WO2010004516A1 - System and methods for in-line monitoring of particles in opaque flows and selective object manipulation in multi-component flow - Google Patents

System and methods for in-line monitoring of particles in opaque flows and selective object manipulation in multi-component flow Download PDF

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Publication number
WO2010004516A1
WO2010004516A1 PCT/IB2009/052974 IB2009052974W WO2010004516A1 WO 2010004516 A1 WO2010004516 A1 WO 2010004516A1 IB 2009052974 W IB2009052974 W IB 2009052974W WO 2010004516 A1 WO2010004516 A1 WO 2010004516A1
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WIPO (PCT)
Prior art keywords
flow
component
sample
manipulating
manipulation
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PCT/IB2009/052974
Other languages
French (fr)
Inventor
Rashid Mavliev
Andrew Mavliev
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Ipgrip, Inc.
Schweiger, Martin
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Filing date
Publication date
Priority claimed from US12/169,500 external-priority patent/US7738101B2/en
Application filed by Ipgrip, Inc., Schweiger, Martin filed Critical Ipgrip, Inc.
Priority to JP2011517300A priority Critical patent/JP2011527751A/en
Publication of WO2010004516A1 publication Critical patent/WO2010004516A1/en

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/10Investigating individual particles
    • G01N15/14Electro-optical investigation, e.g. flow cytometers
    • G01N15/1404Fluid conditioning in flow cytometers, e.g. flow cells; Supply; Control of flow
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D43/00Separating particles from liquids, or liquids from solids, otherwise than by sedimentation or filtration
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/10Investigating individual particles
    • G01N15/14Electro-optical investigation, e.g. flow cytometers
    • G01N15/1425Electro-optical investigation, e.g. flow cytometers using an analyser being characterised by its control arrangement
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
    • G01N35/1095Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices for supplying the samples to flow-through analysers
    • G01N35/1097Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices for supplying the samples to flow-through analysers characterised by the valves
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N2015/0092Monitoring flocculation or agglomeration

Definitions

  • the subject matter presented herein relates generally to the field of detection and characterization of particles in concentrated liquid systems, such as slurries, emulsions and suspensions as well as to the field of manipulation, including filtration or separation of multiple components in a flow carrier, e.g., a liquid or a gas. More specifically it relates to the field of manipulation, including filtration or separation of multiple components in a flow carrier at industrial flow rates.
  • a flow carrier e.g., a liquid or a gas. More specifically it relates to the field of manipulation, including filtration or separation of multiple components in a flow carrier at industrial flow rates.
  • CMP chemical mechanical planarization
  • Flow-through separation devices such as filters or other types of mechanical separators are known. Separation efficiency can depend on the difference in characteristics of the components to be separated. In some cases, one of the components to be separated may be different by one or more measurable parameters and may have a lower concentration in the flow carrier than the other components.
  • One of such cases is filtration of polishing slurry from oversized particles. Typical polishing slurry consist of ensemble of particles of high concentration (up to 10 ⁇ 12 per cc) and desired size (typically 50 - 500 nm): these particles are required to perform polishing process. At certain situation much bigger particles with size of 1 to 100 um may be present in slurries because of agglomeration, malfunction, contamination or other reason.
  • the method requires specifically influencing and separating of the particles, by means of dielectrophoresis, a measuring channel area for characterizing the particles, and a sorting area for sorting the particles identified in the measuring channel area by dielectrophoresis.
  • the sorting includes switching elements which permit active guidance of the particles into two or more subchannels corresponding to the criteria which have been registered in the measuring channel area. While method allows quick and precise sorting of particles, in particular biological cells in a suspension, it can not be implemented to sort particles in multi-component flows such a slurry, especially at industrial flow rates.
  • a particle monitoring system comprises a cuvette configured to confine a flowable sample, the flowable sample being opaque to at least a first range of wavelengths of light waves and a transparent flow compression element located within the cuvette and configured to compress the flowable sample in a first direction while controlling the sample in a second direction parallel to the direction of flow and orthogonal to the first direction while elongating the sample in a third direction orthogonal to the first and second directions, wherein when the sample is compressed in the first direction it becomes transparent to at least one of the wavelengths in the range of wavelengths of light waves.
  • a method of particle monitoring comprises confining a flowable sample, the flowable sample being opaque to at least a first range of wavelengths of light waves, measuring transparency of the flowable sample, compressing the flowable sample in a first direction while controlling the sample in a second direction parallel to the direction of flow and orthogonal to the first direction while elongating the sample in a third direction orthogonal to the first and second directions, wherein when the sample is compressed in the first direction it becomes transparent to at least one of the wavelengths in the range of wavelengths of light waves and identifying characteristics of particles contained in the compressed sample.
  • a system for selective object manipulation in multi-component flow comprises means for detecting and mapping a component in a flow carrier, means for manipulation the component in the flow carrier, wherein the component manipulation means is configured to eliminate or separate the detected component from other components in the flow carrier and means for controlling the manipulation of the detected component, wherein the controlling means is configured to synchronize the manipulation means with the detecting means.
  • the detecting and mapping means comprises a cuvette configured to confine a flowable sample, the flowable sample being opaque to at least a first range of wavelengths of light waves, a transparent flow compression element located within the cuvette and configured to compress the flowable sample in a first direction while controlling the sample in a second direction parallel to the direction of flow and orthogonal to the first direction while elongating the sample in a third direction orthogonal to the first and second directions, wherein when the sample is compressed in the first direction it becomes transparent to at least one of the wavelengths in the range of wavelengths of light waves and a monitor for monitoring the flowable sample using the at least one wavelength.
  • a method of selective object manipulation in multi-component flow comprises detecting and mapping a component in a flow carrier and manipulating the detected component in the flow carrier including elimination or separation from other components, wherein the step of manipulating of the detected component is synchronized with the step of detecting and mapping the component.
  • the step of detecting and mapping comprises confining a flowable sample, the flowable sample being opaque to at least a first range of wavelengths of light waves, measuring transparency of the flowable sample, compressing the flowable sample in a first direction while confining the sample in a second direction parallel to a flow direction of the flowable sample and orthogonal to the first direction, while elongating the sample in a third direction orthogonal to the first and second directions, wherein when the sample is compressed in the first direction, the sample becomes transparent to at least one of the wavelengths in the first range of wavelengths and identifying characteristics of particles contained in the sample that has been compressed.
  • FIG. 1 shows an exemplary embodiment of a system with flow separation.
  • FIG. 2 shows an exemplary embodiment of a system with component manipulation.
  • FIG. 3 shows an exemplary embodiment with coordinate conversion.
  • FIG. 4 shows an exemplary embodiment for selective particle removal in a Chemical
  • FIG. 5 shows an example of time delay and spreading factor in one embodiment of a system with selective object manipulation in a multi-component flow such as a slurry used in a CMP process.
  • FIG. 6A shows an overview of flow in one embodiment of a particle monitoring system;
  • FIG. 6B shows an overview of the system and parameters for numerical estimations in one embodiment a particle monitoring system;
  • FIG. 6C shows an overview of examples of cuvettes according to a first embodiment
  • FIG. 7A shows an overview of an exemplary particle monitoring system according to a first embodiment
  • FIG. 7B shows a more detailed cross-sectional view of an exemplary particle monitoring system according to a first embodiment
  • FIGs. 7C and 7D show a cross-sectional view of an exemplary particle monitoring system according to the first embodiment incorporating surrounding flow.
  • FIG. 8A shows an overview of an exemplary particle monitoring system according to a second embodiment
  • FIG. 8B shows a more detailed cross-sectional view of an exemplary particle monitoring system according to a second embodiment.
  • FIG. 9 A shows an overview of an exemplary particle monitoring system according to a third embodiment
  • FIG. 9B shows a more detailed cross-sectional view of an exemplary particle monitoring system according to a third embodiment
  • FIG. 9C shows a more detailed view of a cuvette in an exemplary particle monitoring system according to a third embodiment.
  • FIG. 10 shows a view of an exemplary optical cuvette according to a fourth embodiment.
  • FIG. 11 shows a view of an exemplary optical cuvette according to a fifth embodiment.
  • FIGs. 12A, 12B, 12C and 12D show views of an exemplary particle monitoring system according to a sixth embodiment employing a bi-concave cylindrical lens as a waveguide.
  • FIG. 1 shows system 1, which comprises a means for the detection and mapping 2, i.e., localization, of a component ("Component B") in a flow carrier, e.g., liquid or gas.
  • the means for detection and mapping can be an optical system for the in-situ and/or in-line or off-line monitoring of particles in a flowable sample, such as a slurry, emulsion or suspension, such as systems disclosed in Figures 6 to 12.
  • the system 1 can include a flow separation means 3, such as a mechanical device (e.g., a valve or actuator), an electrical process (e.g., dielec- trophoresis), magnetic fields or a chemical process.
  • a flow separation means 3 such as a mechanical device (e.g., a valve or actuator), an electrical process (e.g., dielec- trophoresis), magnetic fields or a chemical process.
  • the flow separation means can be used to separate the detected component from other components in the flow carrier.
  • the system 1 can include a flow affecting means, such as a mechanical device (e.g., an actuator), an electromechanical device (e.g., an ultra or megasonic actuator), an electrical process (e.g., electrical discharge), electromagnetic fields (e.g., laser or X-ray), or a chemical process.
  • a flow affecting means such as a mechanical device (e.g., an actuator), an electromechanical device (e.g., an ultra or megasonic actuator), an electrical process (e.g., electrical discharge), electromagnetic fields (e.g., laser or X-ray), or a chemical process.
  • the flow affecting means can be used to alternate the detected component from other components in the flow carrier by eliminating or selectively changing desired properties.
  • the system 1 can include a control means 4 so that the flow manipulation means, i.e., particle elimination, diversion or removal, can be synchronized with the detection means.
  • the control means 4 can include, for example, a computer, a controller or other processor known in the art.
  • the control means can receive and process, for example, detected image data and distinguish a component of interest from the remaining suspension. Once the particle is recognized, the control means 4 can trigger the flow manipulation means 3 to separate Component B 5 from the flow comprising component B 5 and component A such as a suspension or eliminate it. Downstream of the flow manipulation means 3, the flow is free from component B 6.
  • an input can be received from the detection means 2 monitoring a target region for a component or particle of interest.
  • the target region may be monitored to detect any known attribute (or absence thereof) that can be used to distinguish a particle from the remaining suspension.
  • the particle monitoring system may be utilized to capture a stream of images that may be used to identify a particle by its particular attributes.
  • signatures, fingerprints or indices such as a fluorescent signature, light scattering signature, optical fingerprint, X- ray diffraction signature or index of refraction, and the like, or any combination of these, may be used to distinguish the particle from the remaining suspension.
  • Surface charges of particles may also be used to distinguish the particle by observing the reaction of the particle to an applied electric or magnetic field.
  • FIG. 2 shows another exemplary embodiment in which the flow separation means 3 can be replaced or supplemented with a component manipulation means 7.
  • a component manipulation means can include, for example, a laser or other radiation source for destroying dangerous cells while letting other components pass through.
  • Other examples of component manipulation means can include radiation sources or sources that can produce other destructive effects, e.g., Shockwaves, to break up agglomerates of particles.
  • FIG. 3 illustrates an exemplary method using coordinate conversion of detected components. Detection can be done by exemplary particle monitoring systems as illustrated in Figures 6 to 12 and the accompanying description.
  • the sample flow can be shaped into a thin "thread" form using the same technique for both Component B detection and for the subsequent flow separation or manipulation (using a flow of minimal thickness can allow for easier detection and mapping and for easier separation or manipulation).
  • Exemplary techniques for shaping the flow can include the use of two prisms with opposing tips, two cylindrical lenses and two optical blocks with minimal overlap on the Z axis as illustrated in Figure 6, for example.
  • the prisms can be configured to compress the flowable sample in a first direction (X) while limiting the sample in a second direction (Z) parallel to the direction of flow and orthogonal to the first direction while elongating the sample in a third direction (Y) orthogonal to the first and second directions.
  • X first direction
  • Z parallel to the direction of flow
  • Y orthogonal to the first direction
  • the sample When the sample is compressed in the first direction, it can become transparent to light of at least one wavelength.
  • Component B's coordinates (y, t) can be determined.
  • Component B's coordinates (y', t') can be determined by second detection system.
  • the plurality of the component B and B' coordinates are then can be converted to the manipulation system transfer function T linking (y, t) to (y', t').
  • transfer function T With known transfer function T, the detection of an object by detection system at coordinate Y 1 and time ti allows to generate the coordinate Y 1 ' at which point the appropriate action can be applied at the predetermined time (V 1 ).
  • FIG. 4 shows a non-limiting exemplary embodiment for selective particle removal in a Chemical Mechanical Planarization (CMP) system 12.
  • CMP can be used, for example, in semiconductor wafer fabrication.
  • CMP can use an abrasive and corrosive chemical slurry 16 (commonly a colloid) in conjunction with a polishing pad and retaining ring, typically of a greater diameter than the semiconductor wafer 9.
  • CMP process slurries typically consist of SiO.sub.2 or Al.sub.2 O.sub.3 particles suspended in an acid or base solution at a concentration of 4% to 18% solids by weight.
  • the CMP slurry can include a broad range of particle sizes, e.g., from 0.03 .mu.m (microns) to over 1.0 .mu.m (microns) diameter particles.
  • slurry may contain particles of bigger size due to contamination or agglomeration of slurry particles. It is confirmed correlation between the number of oversized particles and number of scratch defects on polished wafers, so it is important to control such particles. It is difficult to check the quality the particle size distributions within these slurries due to the small number of the oversized particles and the substantially opaque nature of the slurry.
  • Particles having dimensions that exceed a delimiting value for a particular application are analogous to sandpaper having grit that is too large, and disadvan- tageously score or scratch the surface that is being smoothed. Thus, it is an essential quality control process to eliminate the use of slurries having particles that are too large.
  • the pad and wafer 9 can be pressed together by a dynamic polishing head 8 and held in place by a plastic retaining ring.
  • the dynamic polishing head 8 is rotated with different axes of rotation (i.e., not concentric). This removes material and tends to even out any irregular topography, making the wafer flat or planar. This may be necessary in order to set up the wafer for the formation of additional circuit elements.
  • the slurry delivery line 15 of CMP polishing system has particle detection system 2, which in one embodiment is the particle detection system illustrated in Figure 7B, and particle separation system 3 comprising a three-way valve.
  • detection and mapping can be performed with use of one or more of the embodiments illustrated in Figures 6 to 12 and described in the accompanying description.
  • the system for in-line monitoring of particles in opaque flows of one of the embodiments illustrated in Figures 6 to 12 is connected to slurry delivery line 11 of CMP polishing system 12 preferably few meters before slurry distribution nozzle 13.
  • the inline monitoring system 2 has predetermined detection limit and means to generate the ALARM signal at each occasion of detection of particle with size above of prede- termined limit.
  • the ALARM signal can be an electrical signal accompanied with audible and visible indication.
  • the ALARM electrical signal can be used by main control PC or other devices.
  • the ALARM signal can be used to trigger the three-way valve 3 located further downstream so that particles having a size larger than the predetermined size are removed from the slurry and fed into the waster container 14.
  • the triggering of the valve 3 will be delayed for predetermined time offset after the detection of the particles having a size larger than the pre-determined size by the diction means 2.
  • the predetermined time offset or time delay depends on additional process conditions such as the flow rate of the slurry through the supply line 11 for example. For higher flow rates, the time offset is shorter as the particles take less lime to travel through the supply line 11 from the detection means 2 to the valve 3. Such conditions could be that particle detection and manipulation will take place during polishing process when it is essential to eliminate scratch causing big particles; particle detection and manipulation can be omitted during, for example, idle cycle.
  • the 3-way valve 3 is integrated to slurry line preferably close to slurry delivery nozzle 13.
  • the 3-way valve typically has the inlet and two outlets - "ALWAYS ON” (1) and “ALWAYS OFF”(2).
  • Slurry line 15 is connected to the inlet of the valve 3 and to "ALWAYS ON” outlet of the valve connected to slurry line which goes to polishing platen.
  • the 3-way valve 3 can be a pneumatic 3-way valve of small body type from Swagelok, for example, model number NXT-DRP41YFCFCFC-S, activated by pneumatic manifold which is controlled by main process PC.
  • the particle detection system generates ALARM signal for main process PC, which processes signal, verifies the necessity of action and activates three-way valve for predetermined duration of time. Valve activation will cause redirection of slurry flow to waste container where it can be further analyzed to find the cause of problem if necessary.
  • a second in-line monitor (not shown) can be temporarily connected to the 3-way valve and the time delay can be determined for typical flow rates (approximate exemplary value ⁇ 1 min for a 3 m line).
  • the time delay value the slurry flow will be monitored for certain time period and correlation will be made of these two system readings.
  • the reading of the first particle detection system will correlate with readings of the second system with time delay necessary for particles to travel from first detection point to second. Due to flow turbulence and irregularities the time delay may vary in certain limit which can be introduced as spreading factor S.
  • An example of exercise to determine the time delay and time spreading factor is presented in FIG.5.
  • a "packet" of particles e.g., a change in the particle concentration from 0 to a certain predetermined value for fixed time duration, can be used to determine the time delay.
  • the time delay and "packet" spreading factor S can be determined by comparing signals from the two in-line monitors.
  • the control unit 4 e.g., PC
  • exemplary embodiments are directed to examining a flow carrier containing components desired to be separated, locating in the flow the positions of a particular component to be separated and selectively removing the fraction of the flow with the component to be separated while minimizing effects on the portion of the flow that does not contain the component to be separated.
  • particle diversion or removal can be synchronized with particle detection.
  • the separated component can be concentrated for further analysis or utilization.
  • the exemplary embodiments can separate components that may not be separable by filtration, e.g., living and dead cells that may be distinguished by fluorescence but may not be separable by filtration.
  • FIGs. 6A, 6B, 6C and 6D are provided as an introductory overview of an in-line particle detection system.
  • the in-line particle detection system may be used to monitor the flow continuously.
  • the particle detection system of one of the embodiments illustrated in figures 6 to 12 may be used in a selective object manipulation system such as the system of one of Figures 1 to 4, for example, the CMP system illustrated in Figure 4.
  • the sample flow with inclusions or particles to be detected can have converging and diverging parts. Arrows represent light penetration depth that depends on optical properties of the sample, e.g., sample turbidity. A goal can be to provide light penetration in the narrowest part of the flow (1). In that case, an optical technique, such as dynamic light scattering, light extinction, light scattering, or a combination of techniques, can be used to detect and characterize the impurities (particles, inclusions) in the flow.
  • FIG. 6B shows an overview of an exemplary particle monitoring system and parameters for numerical estimations that will be discussed later.
  • FIG. 6C shows an overview of examples of cuvettes according to a first group.
  • FIG. 6D shows an overview of examples of cuvettes according to a second group.
  • These designs may include, for example, a monolithic waveguide structure with a slit for flow that is limited in the Z direction.
  • Another group of designs could include a combination of features. For example, one optical element could have substantial curvature in the Z direction and another element could include a flat section.
  • the transparency of the sample flow can be arranged in the form of a "sheet" flow, which can be relatively thin in first (X) and second (Z) orthogonal dimensions and long in a third (Y) orthogonal dimension.
  • Exemplary optimal sample thicknesses can be determined using, for example, two criteria.
  • a first criterion can be based either on the absence of significant multiple scattering of light by the sample or the existence of relatively high sample transparency; this criterion can determine thickness in the first dimension.
  • a second criterion can be based on desired pressure drop of the optical cuvette at required flow rates.
  • Pressure drop inside of an optical cuvette can be an important factor for method applicability in industry. There may be an acceptable range of pressure drops that can be introduced by a device (like in-line monitoring device) into flow lanes. This range can vary from application to application and depends from process parameters.
  • Pressure drop inside of a cuvette can be a reverse function of flow thicknesses in the first and third dimensions and which can determine the cross section of the cuvette. Because the flow thickness in the first dimension X can be determined by optical transparency criterion and may not be varied freely, the flow width in third dimension Y can be used to keep the pressure drop at a desired level.
  • the pressure drop can be directly proportional to the flow dimension in the second direction Z and this also can be used to affect the pressure drop in the cuvette in a desired manner.
  • X 5-500 ⁇ m
  • Z 0.1-5 mm
  • width of Y 5-25 mm in the third dimension
  • a diverging angle in the output part of cuvette can also affect pressure drop in the cuvette at a given flow rate and may be chosen accordingly. Another criterion to choose the diverging angle can be its affect on flow structure. For example, a high diverging angle (an extreme case is a right angle, i.e., slit in flat material) most likely generates turbulent motion in the flow. When turbulence is not desirable it can be prevented by choosing proper diverging angle of cuvette.
  • laser light extinction and multiple light scattering by the particles can be negligible for a "sheet" of a typical slurry.
  • the slurry flow may require no dilution and therefore the size distribution of the particles in the slurry can have minimum distortion.
  • flow parameters at a measuring point are width Y, thickness X, flowrate Q.
  • a laser beam of Lp (not shown) power has width Y and thickness Z.
  • a measuring area Z*Y is projected by an optical system with magnification k to a camera type sensor with Py*Pz pixels (pixel sizes are z p and y p ) and signal accumulation time t c .
  • Optical magnification is chosen for whole flow observation:
  • F(d) is light scattering function for particle of size d.
  • the detection limit is determined by signal/noise ratio rather by signal value itself.
  • Signal/noise ratio can be affected by two parameters - the volume of scattering media illuminating the single pixel and ratio of signal and noise accumulation times. Multiplying these two factors for signal/noise ratio results in:
  • d m is median particle size in the scattering media.
  • SN does not necessarily depend on flow spatial parameters. This allows varying flow thickness X to achieve flow transparency without affecting signal/noise ratio.
  • the range of acceptable sample optical thickness can be extended up to five or more at small signal collection angles. In that case, the correction of the Beer- Lambert light scattering law can be modified.
  • the parameters of the sensor can also be as important as the total flow rate.
  • Some exemplary calculation results for two cameras (1024 and 2048 pixels) and two flow rates are shown in Table 1.
  • FIGs. 7 A, 7B, 7C and 7D show an exemplary particle monitoring system 200 according to a first embodiment.
  • particle monitoring system 200 comprises a cuvette 210, e.g., a transparent optical flow cell, configured to confine a flowable sample.
  • the flowable sample may be opaque to at least a first range of wavelengths of light waves.
  • a transparent flow compression element 220 e.g., prisms, can be located within the cuvette 210 and configured to compress the flowable sample in a first (X) direction while controlling the sample in a second direction (Z) parallel to the direction of flow and orthogonal to the first direction while elongating the sample in a third direction (Y) orthogonal to the first and second directions.
  • the sample When the sample is compressed in the first direction, it may become transparent to at least one of the wavelengths in the range of wavelengths of light waves.
  • exemplary dimensions for the X, Z and Y directions may be about 50 ⁇ m to 3 mm in the first (X) direction, about 10 ⁇ m to 3 mm in the second (Z) direction and about 5 mm to 25 mm in the third (Y) dimension.
  • an optical flow cell such as a cuvette 210
  • a cuvette 210 can be used to form a focused flow of the sample fluid.
  • the cuvette 210 can include a flow converging part, a measuring part, a sample introduction part and a sample discharge part.
  • the width of the flow channel in the measuring part of the cuvette 210 can be narrow in the first dimension (e.g., 0.1 mm ⁇ 10% or lesser or greater) and wide in the third orthogonal dimension (for example, approximately 10 mm ⁇ 10% or lesser or greater).
  • the effective flow dimension in the second orthogonal direction may be determined by the curvature of the flow focusing elements and can be in the range of, for example, 10 ⁇ m to 3 mm.
  • the flow channel parameters can be substantially constant (e.g., ⁇ 10% flow channel width in any direction) along the whole length of this measuring part of the cuvette 210.
  • the measuring part of the cuvette 210 can be optically transparent and may be used for characterization of the sample transparency and for the optical characterization of particles in the focused sample fluid.
  • sample fluid flow can also be placed into operable communication (e.g., at least partially surrounded) with a flow of clean (i.e. relatively particle-free) transparent liquid (e.g., water) or other appropriate liquid.
  • a flow of clean (i.e. relatively particle-free) transparent liquid e.g., water
  • This method can be used to avoid the contamination of optical parts or as another method to control sample flow thickness and transparency.
  • An exemplary optical cuvette having symmetrical surrounding flow inlets is illustrated in FIGs. 7C and 7D.
  • Main sample flow can be in- troduced through the flow inlet and discharged through the sensing area formed by the tips of the prisms 220.
  • a surrounding flow of clean liquid compatible with sample liquid parameters can form a boundary layer on the prism 220 surfaces preventing particle deposition on optical surfaces.
  • Surrounding flow can be chosen compatible with sample flow and flow rates can be minimal so as not to affect the sample flow properties.
  • FIGs. 85 an exemplary way of compressing flow is represented in FIGs.
  • optical elements e.g., prisms 220
  • the tips of the prisms 220 may be designed to provide the necessary optical quality.
  • Prisms as flow forming optical elements can satisfy the parameters mentioned above: elongation by axis Y and short distance by axis Z.
  • the optical signal can be collected through the flat surface of the prism opposing the sensing volume forming tip.
  • the prism angle from tip to flat surface can be chosen depending on requirements of the signal detection system - for light transmission schemes the angle can be small, for light scattering schemes bigger angles can be used for scattered light collection.
  • Symmetrical or asymmetrical prisms can be used depending on requirements for converging and diverging angles of the flow.
  • the cuvette can be configured using two optical elements, such as two equilateral (or other) prisms to produce a flow cell for compressing the sample in at least one dimension to render the sample transparent to light waves of a predetermined wavelength.
  • the system also can include a way to identify characteristics of individual particles contained in the compressed sample.
  • the identifying device is represented in FIG. 7B as an optical camera or detector 230 (e.g., a CCD camera, CMOS, photodiode or other optically sensitive device) in optical communication with the cuvette 210.
  • An associated light source 240 e.g., a laser, which produces a beam of light 250, can also be in optical communication with the cuvette 210.
  • the sample transparency can be measured by light extinction, and the sample fluid thickness in the flat part of the cuvette 210 can be adjusted to obtain a predetermined transparency value or sensing volume value.
  • Conventional light scattering and/or light extinction techniques can be used to measure the parameters of single particles having diameters above the detection limit.
  • a CCD (charge-coupled device) or CMOS detector/camera 230, together with appropriate frame-capture electronics and data- handling software, can be used to suppress the influence of background scattering on the quantitative detection of the signal produced by individual particles passing through the optical sensing volume.
  • FIGs. 7C and 7D shows more details of an exemplary cuvette 210 according to a first embodiment.
  • the cuvette 210 can include the body assembly for the parts, prisms 220 attached to actuators 260, and two symmetrical holders. Proper sealing in the holder- prism interface can be provided by o-rings (e.g., Kalrez or Chemrez material). To achieve a variation in the channel thickness, the cuvette 210 can be configured using two symmetrical optical parts, such as prisms 220, separated by an elastic spacer formed of, for example, O-ring cord or any elastic material.
  • o-rings e.g., Kalrez or Chemrez material
  • Prisms 220 e.g., sapphire or glass, coated with diamond like carbon
  • actuators 260 can be attached to actuators 260 allowing the prisms' displacement to adjust the sensing area width.
  • Externally controlled pressure can be applied on these two opposing parts using, for example, screws, hydraulic or pneumatic actuators, electromagnetic actuators or any other way to control displacement to cause shrinkage in the spacer to a level that depends on the applied pressure and Young's modulus of elasticity for the spacer. This can allow control of the sample transparency, because the focused fluid sample thickness can have a known relationship (e.g., be proportional) to the flow channel thickness.
  • Actuators 260 can also be used to provide high frequency (ultra- or megasonic) vibration of the prisms 220 to reduce possible particle deposition on optical parts.
  • This exemplary embodiment allows a measurement of the sample transparency as a function of sample thickness in a single experiment. These measurements can permit a determination of the particle size parameters in the sample fluid using an integral scattering approach. At the same time, the parameters of the largest particles can be determined using a single-particle approach. The combination of these two different approaches (that is, integral and differential) can permit an improvement in the accuracy and reliability of the measurements.
  • the sample fluid flow can be introduced into a flat part of the cuvette 310, which can be formed by two flat optical waveguides 320.
  • a monolithic waveguide structure with a slit for flow that is limited in the Z direction from the second group of designs mentioned previously can be used.
  • the second embodiment can allow for a simple mechanical design of a cuvette in several possible embodiments. However, optical measurements can be made in transmission mode and flow may have substantial recirculation after passage through measuring area.
  • the sample fluid in the flat part of the cuvette 310 can be illuminated with a light beam 350 of appropriate shape from a laser 340 or any other suitable light source.
  • the beam shape can be chosen using criteria such as being wide enough to cover the whole flow width and narrow enough to go through optical waveguides 320.
  • the intensity of the transmitted light can be measured and analyzed to determine the sample transparency.
  • the width of the focused sample fluid flow can be adjusted to reach the desired level of sample transparency.
  • the size parameters of the particles for example, the particle size distribution above a given threshold diameter
  • the sample fluid can be measured by known optical and electronic methods with relatively high accuracy.
  • the sample fluid flow can be introduced into the flat part of the cuvette 410 which can be formed by a flat optical window 470 and a cylindrical lens 480.
  • This embodiment can allow a bigger optical signal collection angle but may have challenges in mechanical design of the cuvette 410.
  • Dimension Z can be determined by lens diameter and may be substantially bigger than in the first or second embodiments.
  • FIG. 10 shows an example of a fourth embodiment.
  • the sample flow can be a circular "thread" of flow with thickness X.
  • An exemplary light guide and scattering light collection system can be made of glass, sapphire or quartz. Scattered light can be delivered to a light detection and signal processing system by a fiber optic guide. This guide can be used to connect (convert) a circularly distributed signal with a linear optical detector.
  • FIG. 11 shows a fifth embodiment similar to the fourth embodiment.
  • FIGs. 12A, 12B, 12C and 12D show views of an exemplary particle monitoring system according to a sixth embodiment.
  • the waveguide can be formed using a bi-concave cylindrical lens.
  • the slit can be cut in the middle of lens and polished for light passage.
  • the slit width can be fixed.
  • FIGs. 9A, 9B and 9C An example of this optical cuvette is shown in FIGs. 9A, 9B and 9C.
  • the width of flow was 10 mm and sample thickness (X, measured with a shim) was -100 ⁇ m.
  • the diameter of the cylindrical lens was 5 mm and the window diameter was 20 mm.
  • the cylindrical lens was used to partially focus the laser beam in the cylinder- window vicinity (sensing area). The laser beam was widened before approaching the optical cuvette by another cylindrical lens to provide uniform irradiation along whole sample length in the Y axis.
  • the housing was made of black Delrin material and the windows were partially glued or rubber-tight sealed.
  • the measured pressure drop at these cell parameters was -1.5 psi for a flowrate of 100 ml/min. This pressure, which translates to 7.5 psi at 500 ml/min, should be acceptable, for example, for most semiconductor applications.
  • the sample was irradiated with a laser to which custom modi- fications were made to reduce pulse length to eliminate the image "smearing" of moving particles.
  • the laser beam was stopped at the collection lens plane and a collection lens was used to direct forward scattering light to a video camera (WT-502 by Watec Corp.).
  • the images were recorded on a PC with Airlink+ frame grabber.
  • the experimental results showed that non-diluted slurry looks like "milky" uniformly scattering media. Because of the small thickness the slurry was transparent. 1588 nm polymer microspheres from Duke Scientific Corp. in DI water were used to test for optical system sensitivity and the ability to record particles of such size. The same concentration of 1588 nm microspheres was also placed in a slurry. The results showed that the added particles are clearly detectable in DIW as well as in slurry.
  • Slurry becomes transparent at a certain thickness and optical methods can be applied for particle characterization.
  • the cuvette resistance to flow can be kept low to facilitate the operation at relatively high flow rates, e.g., 500 ml/min.
  • exemplary embodiments are directed to non-intrusive systems and methods for in-line or off-line monitoring of single particles over a wide range of sizes and concentrations, contained in systems comprised mostly of smaller particles. Exemplary methods can accommodate mixtures without requiring their dilution, and mixtures wherein the "tail" of largest particles in the particle size distribution can be accurately measured. Optical characterization of particles over a wide range of sizes and concentrations in concentrated systems may be achieved using exemplary embodiments of an optical flow cell, such as a cuvette, wherein the sample flow is made relatively transparent to apply an optical technique for particle characterization.
  • an optical flow cell such as a cuvette
  • a system for chemical.mechanical polishing of a semiconductor wafer illustrated in Figure 4 comprises a slurry source 17 comprising SiO.sub.2 or Al.sub.2 O.sub.3 particles suspended in an acid or base solution at a concentration of 4% to 18% solids by weight.
  • the particle sizes range, e.g., from 0.03 .microns to over 1.0 micron in diameter.
  • portions of the slurry 16 may contain particles of bigger size due to contamination or agglomeration of slurry particles. It is desirable to remove particles or agglomerations of particles from the slurry 16 before the slurry 16 reaches the semiconductor wafer 9 where these larger particles may damage the semiconductor wafer.
  • the chemical mechanical polishing system 12 includes an inline particle detection monitor 2 which is able to detect the size of the particles flowing through the slurry delivery line 15.
  • the in-line particle size detection monitor 2 is provided by system 200 illustrated in Figure 7B which includes a cuvette 210 comprising two prisms 220, an identifying device comprising an optical camera or detector 230 (e.g., a CCD camera, CMOS, photodiode or other optically sensitive device) in optical communication with the cuvette 210.
  • An associated light source 240 e.g., a laser, which produces a beam of light 250, can also be in optical communication with the cuvette 210.
  • the sample transparency can be measured by light extinction, and the sample fluid thickness in the flat part of the cuvette 210 can be adjusted to obtain a predetermined transparency value or sensing volume value.
  • Conventional light scattering and/or light extinction techniques can be used to measure the parameters of single particles having diameters above the detection limit.
  • a CCD (charge-coupled device) or CMOS detector/camera 230, together with appropriate frame-capture electronics and data- handling software, can be used to suppress the influence of background scattering on the quantitative detection of the signal produced by individual particles passing through the optical sensing volume.
  • a control unit 4 activates the three-way valve 3 positioned in the slurry delivery line 15 downstream of the particle detection monitor 2 in order to redirect the portion of the slurry 16 containing these particles having a size greater than the predetermined size into the slurry waste container 14. Portions of the slurry 16 which do not contain particles above the predetermined size are directed into slurry delivery arm 11 where they are directed on to the wafer 9 and used to chemically mechanically polish the surface of the wafer 9.
  • the detection system 2 and the timing of the actuation of the three-way valve 3 are synchronized so that the portion of the slurry detected by the detection means 2 at point C of the slurry line 15 is directed into waste container 14 when this portion of the slurry reaches the three-way valve 3 at point D in the slurry line 15.
  • the portion of the slurry containing the undesirable large particles may spread due to turbulence and flow.non-unifomity during its travel from point C to point D. This spreading of the portion or packet of particles may be compensated as disclosed in connection with Figure 5 by adjusting the time delay before actuating the three-way valve 3 and/or by adjusting the length of time that the slurry flow is directed into the waste container 14.
  • An exemplary system can include a detection system for the monitoring of a component, such as a particle in a flow carrier.
  • the system can also include a device (e.g., a valve or actuator) to manipulate the detected component from other components in the flow carrier.
  • a controller or other processor can receive and process detected component data and distinguish a component of interest from the remaining flowable sample. Once the component is recognized, the controller synchronizes the flow manipulation device with the detection system to manipulate the detected component from the flow carrier.

Abstract

Systems and methods are disclosed for particle monitoring, in particular in-line particle monitoring and selective object manipulation in multi-component flow. An exemplary system can include a detection system for the monitoring of a component, such as a particle in a opaque flow carrier. An exemplary system includes confining a flowable sample which is opaque to at least a first range of wavelengths of light waves; compressing the flowable sample in a first direction while confining the sample in a second direction parallel to a flow direction of the flowable sample and orthogonal to the first direction, while elongating the sample in a third direction orthogonal to the first and second directions. When the sample is compressed in the first direction, the sample becomes transparent to at least one of the wavelengths in the first range of wavelengths enabling optical means for particle detection. The system can also include a device such as a valve or actuator to manipulate the detected component from other components in the flow carrier. A controller or other processor can receive and process detected component data and distinguish a component of interest from the remaining flowable sample. Once the component is recognized, the controller synchronizes the flow manipulation device with the detection system to manipulate the detected component from the flow carrier.

Description

Description
Title of Invention: SYSTEM AND METHODS FOR IN-LINE MONITORING OF PARTICLES IN OPAQUE FLOWS AND SELECTIVE OBJECT MANIPULATION IN MULTI- COMPONENT FLOW
[1] BACKGROUND
[2] The subject matter presented herein relates generally to the field of detection and characterization of particles in concentrated liquid systems, such as slurries, emulsions and suspensions as well as to the field of manipulation, including filtration or separation of multiple components in a flow carrier, e.g., a liquid or a gas. More specifically it relates to the field of manipulation, including filtration or separation of multiple components in a flow carrier at industrial flow rates.
[3] Liquid systems with high particulate concentrations are widely used in industry.
Examples of such systems are slurries used in chemical mechanical planarization (CMP) processes for the semiconductor industry and emulsions used in the pharmaceutical industry.
[4] Optical methods of detection and characterization have been used for monitoring particle parameters in gas and liquid media. U.S. Patent No. 6,710,874 to Mavliev discloses an apparatus and method for the optical characterization of particles in highly concentrated systems and is hereby incorporated by reference in its entirety.
[5] Flow-through separation devices, such as filters or other types of mechanical separators are known. Separation efficiency can depend on the difference in characteristics of the components to be separated. In some cases, one of the components to be separated may be different by one or more measurable parameters and may have a lower concentration in the flow carrier than the other components. One of such cases is filtration of polishing slurry from oversized particles. Typical polishing slurry consist of ensemble of particles of high concentration (up to 10Λ12 per cc) and desired size (typically 50 - 500 nm): these particles are required to perform polishing process. At certain situation much bigger particles with size of 1 to 100 um may be present in slurries because of agglomeration, malfunction, contamination or other reason. The presence of big particles can cause substrate scratch during polishing resulting in "killer defects" and manufacturing yield reduction. One of the well accepted solutions to eliminate the big particles is filtration. In situations of slurry or other emulsion filtration, the other different (useful) components can also accumulate in the filtering device, possibly leading to secondary big particle generation and to necessity of the frequent maintenance and replacement of the filtering device. [6] A method for separating particles is disclosed in U.S. Patent No. 7,294,249 to
Gawad. The method requires specifically influencing and separating of the particles, by means of dielectrophoresis, a measuring channel area for characterizing the particles, and a sorting area for sorting the particles identified in the measuring channel area by dielectrophoresis. The sorting includes switching elements which permit active guidance of the particles into two or more subchannels corresponding to the criteria which have been registered in the measuring channel area. While method allows quick and precise sorting of particles, in particular biological cells in a suspension, it can not be implemented to sort particles in multi-component flows such a slurry, especially at industrial flow rates.
[7] Methods for separating particles, disclosed in U.S. Patent No. 7,318,902 and
7 ' ,Al '2,791A to Oakey, which are incorporated herein by reference in their entirety are employing the laminar nature of fluid flows in microfluidic flow devices with the flow obstacles. External means are used to modulate flow rate which makes these inventions not applicable to the scope of this patent. The flow obstacles are especially not desired in manipulations of flow with high particular content such as slurries and emulsions. US patent No.s 7,428,971 by Hirano, et al. 7,366,377 by Getin, et al 7,068,874 by Wang, et al are dedicated to particles manipulation in flow using optical means. These methods may be useful in the field of cell sorting but are not useful for object manipulation in opaque flows with high particle content (such a slurries and emulsions) especially at industrial flow rates.
[8] So there is a need for methods and apparatus for in-line monitoring of particles in opaque flow as well as filtration or particles separation from multi-component flows including flows with components (particles) to be preserved and flows with high particle content such as slurries and emulsions. Methods which do not depend on flow parameters such as optical transparency, viscosity, flow rate or laminarity, and methods and apparatus which can operate at industrial conditions are also desirable.
[9] SUMMARY
[10] A particle monitoring system comprises a cuvette configured to confine a flowable sample, the flowable sample being opaque to at least a first range of wavelengths of light waves and a transparent flow compression element located within the cuvette and configured to compress the flowable sample in a first direction while controlling the sample in a second direction parallel to the direction of flow and orthogonal to the first direction while elongating the sample in a third direction orthogonal to the first and second directions, wherein when the sample is compressed in the first direction it becomes transparent to at least one of the wavelengths in the range of wavelengths of light waves.
[11] A method of particle monitoring comprises confining a flowable sample, the flowable sample being opaque to at least a first range of wavelengths of light waves, measuring transparency of the flowable sample, compressing the flowable sample in a first direction while controlling the sample in a second direction parallel to the direction of flow and orthogonal to the first direction while elongating the sample in a third direction orthogonal to the first and second directions, wherein when the sample is compressed in the first direction it becomes transparent to at least one of the wavelengths in the range of wavelengths of light waves and identifying characteristics of particles contained in the compressed sample.
[12] A system for selective object manipulation in multi-component flow comprises means for detecting and mapping a component in a flow carrier, means for manipulation the component in the flow carrier, wherein the component manipulation means is configured to eliminate or separate the detected component from other components in the flow carrier and means for controlling the manipulation of the detected component, wherein the controlling means is configured to synchronize the manipulation means with the detecting means.
[13] In one embodiment, the detecting and mapping means comprises a cuvette configured to confine a flowable sample, the flowable sample being opaque to at least a first range of wavelengths of light waves, a transparent flow compression element located within the cuvette and configured to compress the flowable sample in a first direction while controlling the sample in a second direction parallel to the direction of flow and orthogonal to the first direction while elongating the sample in a third direction orthogonal to the first and second directions, wherein when the sample is compressed in the first direction it becomes transparent to at least one of the wavelengths in the range of wavelengths of light waves and a monitor for monitoring the flowable sample using the at least one wavelength.
[14] A method of selective object manipulation in multi-component flow comprises detecting and mapping a component in a flow carrier and manipulating the detected component in the flow carrier including elimination or separation from other components, wherein the step of manipulating of the detected component is synchronized with the step of detecting and mapping the component.
[15] In one embodiment, the step of detecting and mapping comprises confining a flowable sample, the flowable sample being opaque to at least a first range of wavelengths of light waves, measuring transparency of the flowable sample, compressing the flowable sample in a first direction while confining the sample in a second direction parallel to a flow direction of the flowable sample and orthogonal to the first direction, while elongating the sample in a third direction orthogonal to the first and second directions, wherein when the sample is compressed in the first direction, the sample becomes transparent to at least one of the wavelengths in the first range of wavelengths and identifying characteristics of particles contained in the sample that has been compressed.
[16] BRIEF DESCRIPTION OF THE DRAWINGS
[17] As will be realized, different embodiments are possible, and the details disclosed herein are capable of modification in various respects, all without departing from the scope of the claims. Accordingly, the drawings and descriptions are to be regarded as illustrative in nature and not as restrictive. Like reference numerals have been used to designate like elements.
[18] FIG. 1 shows an exemplary embodiment of a system with flow separation.
[19] FIG. 2 shows an exemplary embodiment of a system with component manipulation.
[20] FIG. 3 shows an exemplary embodiment with coordinate conversion.
[21] FIG. 4 shows an exemplary embodiment for selective particle removal in a Chemical
Mechanical Planarization (CMP) process. [22] FIG. 5 shows an example of time delay and spreading factor in one embodiment of a system with selective object manipulation in a multi-component flow such as a slurry used in a CMP process. [23] FIG. 6A shows an overview of flow in one embodiment of a particle monitoring system; [24] FIG. 6B shows an overview of the system and parameters for numerical estimations in one embodiment a particle monitoring system; [25] FIG. 6C shows an overview of examples of cuvettes according to a first embodiment
(two optical elements with Y axis elongation and Z axis curvature); FIG 6D shows an overview of examples of cuvettes according to a second embodiment (optical elements with flow passages elongated in the Y axis and confined in Z axis). [26] FIG. 7A shows an overview of an exemplary particle monitoring system according to a first embodiment; [27] FIG. 7B shows a more detailed cross-sectional view of an exemplary particle monitoring system according to a first embodiment; [28] FIGs. 7C and 7D show a cross-sectional view of an exemplary particle monitoring system according to the first embodiment incorporating surrounding flow. [29] FIG. 8A shows an overview of an exemplary particle monitoring system according to a second embodiment; [30] FIG. 8B shows a more detailed cross-sectional view of an exemplary particle monitoring system according to a second embodiment. [31] FIG. 9 A shows an overview of an exemplary particle monitoring system according to a third embodiment; [32] FIG. 9B shows a more detailed cross-sectional view of an exemplary particle monitoring system according to a third embodiment; [33] FIG. 9C shows a more detailed view of a cuvette in an exemplary particle monitoring system according to a third embodiment.
[34] FIG. 10 shows a view of an exemplary optical cuvette according to a fourth embodiment.
[35] FIG. 11 shows a view of an exemplary optical cuvette according to a fifth embodiment.
[36] FIGs. 12A, 12B, 12C and 12D show views of an exemplary particle monitoring system according to a sixth embodiment employing a bi-concave cylindrical lens as a waveguide.
[37] DETAILED DESCRIPTION
[38] FIG. 1 shows system 1, which comprises a means for the detection and mapping 2, i.e., localization, of a component ("Component B") in a flow carrier, e.g., liquid or gas. In one embodiment, the means for detection and mapping can be an optical system for the in-situ and/or in-line or off-line monitoring of particles in a flowable sample, such as a slurry, emulsion or suspension, such as systems disclosed in Figures 6 to 12.
[39] In one embodiment, the system 1 can include a flow separation means 3, such as a mechanical device (e.g., a valve or actuator), an electrical process (e.g., dielec- trophoresis), magnetic fields or a chemical process. The flow separation means can be used to separate the detected component from other components in the flow carrier.
[40] In one embodiment, the system 1 can include a flow affecting means, such as a mechanical device (e.g., an actuator), an electromechanical device (e.g., an ultra or megasonic actuator), an electrical process (e.g., electrical discharge), electromagnetic fields (e.g., laser or X-ray), or a chemical process. The flow affecting means can be used to alternate the detected component from other components in the flow carrier by eliminating or selectively changing desired properties.
[41] In one embodiment, the system 1 can include a control means 4 so that the flow manipulation means, i.e., particle elimination, diversion or removal, can be synchronized with the detection means. The control means 4 can include, for example, a computer, a controller or other processor known in the art. The control means can receive and process, for example, detected image data and distinguish a component of interest from the remaining suspension. Once the particle is recognized, the control means 4 can trigger the flow manipulation means 3 to separate Component B 5 from the flow comprising component B 5 and component A such as a suspension or eliminate it. Downstream of the flow manipulation means 3, the flow is free from component B 6.
[42] In exemplary system 1, an input can be received from the detection means 2 monitoring a target region for a component or particle of interest. The target region may be monitored to detect any known attribute (or absence thereof) that can be used to distinguish a particle from the remaining suspension. The particle monitoring system, for example, may be utilized to capture a stream of images that may be used to identify a particle by its particular attributes. Alternatively, signatures, fingerprints or indices such as a fluorescent signature, light scattering signature, optical fingerprint, X- ray diffraction signature or index of refraction, and the like, or any combination of these, may be used to distinguish the particle from the remaining suspension. Surface charges of particles may also be used to distinguish the particle by observing the reaction of the particle to an applied electric or magnetic field.
[43] FIG. 2 shows another exemplary embodiment in which the flow separation means 3 can be replaced or supplemented with a component manipulation means 7. Examples of a component manipulation means can include, for example, a laser or other radiation source for destroying dangerous cells while letting other components pass through. Other examples of component manipulation means can include radiation sources or sources that can produce other destructive effects, e.g., Shockwaves, to break up agglomerates of particles.
[44] FIG. 3 illustrates an exemplary method using coordinate conversion of detected components. Detection can be done by exemplary particle monitoring systems as illustrated in Figures 6 to 12 and the accompanying description. The sample flow can be shaped into a thin "thread" form using the same technique for both Component B detection and for the subsequent flow separation or manipulation (using a flow of minimal thickness can allow for easier detection and mapping and for easier separation or manipulation).
[45] Exemplary techniques for shaping the flow can include the use of two prisms with opposing tips, two cylindrical lenses and two optical blocks with minimal overlap on the Z axis as illustrated in Figure 6, for example. In the embodiment of two prisms with opposing tips, such as that illustrated in Figure 6B the prisms can be configured to compress the flowable sample in a first direction (X) while limiting the sample in a second direction (Z) parallel to the direction of flow and orthogonal to the first direction while elongating the sample in a third direction (Y) orthogonal to the first and second directions. When the sample is compressed in the first direction, it can become transparent to light of at least one wavelength.
[46] A coordinate conversion factor can be established between the detection and manipulation systems (y=>y') using the detection system and second detection system in the place of the manipulation system. Similarly, a time delay factor (t=>f) can be determined between the two systems. After detection of Component B on the detection system, Component B's coordinates (y, t) can be determined. Component B's coordinates (y', t') can be determined by second detection system. The plurality of the component B and B' coordinates are then can be converted to the manipulation system transfer function T linking (y, t) to (y', t'). With known transfer function T, the detection of an object by detection system at coordinate Y1 and time ti allows to generate the coordinate Y1 ' at which point the appropriate action can be applied at the predetermined time (V1).
[47] FIG. 4 shows a non-limiting exemplary embodiment for selective particle removal in a Chemical Mechanical Planarization (CMP) system 12. CMP can be used, for example, in semiconductor wafer fabrication. CMP can use an abrasive and corrosive chemical slurry 16 (commonly a colloid) in conjunction with a polishing pad and retaining ring, typically of a greater diameter than the semiconductor wafer 9. CMP process slurries typically consist of SiO.sub.2 or Al.sub.2 O.sub.3 particles suspended in an acid or base solution at a concentration of 4% to 18% solids by weight. The CMP slurry can include a broad range of particle sizes, e.g., from 0.03 .mu.m (microns) to over 1.0 .mu.m (microns) diameter particles. Occasionally slurry may contain particles of bigger size due to contamination or agglomeration of slurry particles. It is confirmed correlation between the number of oversized particles and number of scratch defects on polished wafers, so it is important to control such particles. It is difficult to check the quality the particle size distributions within these slurries due to the small number of the oversized particles and the substantially opaque nature of the slurry.
[48] Particles having dimensions that exceed a delimiting value for a particular application are analogous to sandpaper having grit that is too large, and disadvan- tageously score or scratch the surface that is being smoothed. Thus, it is an essential quality control process to eliminate the use of slurries having particles that are too large.
[49] The pad and wafer 9 can be pressed together by a dynamic polishing head 8 and held in place by a plastic retaining ring. The dynamic polishing head 8 is rotated with different axes of rotation (i.e., not concentric). This removes material and tends to even out any irregular topography, making the wafer flat or planar. This may be necessary in order to set up the wafer for the formation of additional circuit elements.
[50] In a non-limiting exemplary embodiment shown in FIG. 4 the slurry delivery line 15 of CMP polishing system has particle detection system 2, which in one embodiment is the particle detection system illustrated in Figure 7B, and particle separation system 3 comprising a three-way valve. In the FIG. 4 embodiment, detection and mapping can be performed with use of one or more of the embodiments illustrated in Figures 6 to 12 and described in the accompanying description.
[51] The system for in-line monitoring of particles in opaque flows of one of the embodiments illustrated in Figures 6 to 12 is connected to slurry delivery line 11 of CMP polishing system 12 preferably few meters before slurry distribution nozzle 13. The inline monitoring system 2 has predetermined detection limit and means to generate the ALARM signal at each occasion of detection of particle with size above of prede- termined limit. The ALARM signal can be an electrical signal accompanied with audible and visible indication. The ALARM electrical signal can be used by main control PC or other devices. In one embodiment the ALARM signal can be used to trigger the three-way valve 3 located further downstream so that particles having a size larger than the predetermined size are removed from the slurry and fed into the waster container 14. The slurry reaching the wafer is then free of these larger particles which may cause damage to the wafer. The triggering of the valve 3 will be delayed for predetermined time offset after the detection of the particles having a size larger than the pre-determined size by the diction means 2. In one embodiment, the predetermined time offset or time delay depends on additional process conditions such as the flow rate of the slurry through the supply line 11 for example. For higher flow rates, the time offset is shorter as the particles take less lime to travel through the supply line 11 from the detection means 2 to the valve 3. Such conditions could be that particle detection and manipulation will take place during polishing process when it is essential to eliminate scratch causing big particles; particle detection and manipulation can be omitted during, for example, idle cycle.
[52] In one embodiment, the 3-way valve 3 is integrated to slurry line preferably close to slurry delivery nozzle 13. The 3-way valve typically has the inlet and two outlets - "ALWAYS ON" (1) and "ALWAYS OFF"(2). Slurry line 15 is connected to the inlet of the valve 3 and to "ALWAYS ON" outlet of the valve connected to slurry line which goes to polishing platen. The "ALWAYS OFF" outlet of the valve connected to waste container 14.
[53] In one embodiment, the 3-way valve 3 can be a pneumatic 3-way valve of small body type from Swagelok, for example, model number NXT-DRP41YFCFCFC-S, activated by pneumatic manifold which is controlled by main process PC. In the this case the particle detection system generates ALARM signal for main process PC, which processes signal, verifies the necessity of action and activates three-way valve for predetermined duration of time. Valve activation will cause redirection of slurry flow to waste container where it can be further analyzed to find the cause of problem if necessary.
[54] In one embodiment, in a test mode, a second in-line monitor (not shown) can be temporarily connected to the 3-way valve and the time delay can be determined for typical flow rates (approximate exemplary value ~1 min for a 3 m line). To determine the time delay value the slurry flow will be monitored for certain time period and correlation will be made of these two system readings. The reading of the first particle detection system will correlate with readings of the second system with time delay necessary for particles to travel from first detection point to second. Due to flow turbulence and irregularities the time delay may vary in certain limit which can be introduced as spreading factor S. An example of exercise to determine the time delay and time spreading factor is presented in FIG.5.
[55] As illustrated in FIG. 5, a "packet" of particles, e.g., a change in the particle concentration from 0 to a certain predetermined value for fixed time duration, can be used to determine the time delay. The time delay and "packet" spreading factor S (due to turbulence and flow non-uniformity) can be determined by comparing signals from the two in-line monitors.
[56] In operational mode, after the detection of a particle by the in-line monitor 2, the control unit 4, e.g., PC, can generate an event alarm, determine the time delay factor (t=>t') and activate the 3-way valve 3 at a predetermined time (f) for a time exceeding the "packet" spreading factor T, thus delivering a portion of the slurry with the detected component, e.g., big particles capable of affecting the polishing process and causing wafer scratch, to a waste container 14.
[57] As described, exemplary embodiments are directed to examining a flow carrier containing components desired to be separated, locating in the flow the positions of a particular component to be separated and selectively removing the fraction of the flow with the component to be separated while minimizing effects on the portion of the flow that does not contain the component to be separated. In the exemplary embodiments, particle diversion or removal can be synchronized with particle detection. The separated component can be concentrated for further analysis or utilization. The exemplary embodiments can separate components that may not be separable by filtration, e.g., living and dead cells that may be distinguished by fluorescence but may not be separable by filtration.
[58] FIGs. 6A, 6B, 6C and 6D are provided as an introductory overview of an in-line particle detection system. The in-line particle detection system may be used to monitor the flow continuously.
[59] In further embodiments, the particle detection system of one of the embodiments illustrated in figures 6 to 12 may be used in a selective object manipulation system such as the system of one of Figures 1 to 4, for example, the CMP system illustrated in Figure 4.
[60] In the exemplary particle monitoring system shown FIG. 6A, the sample flow with inclusions or particles to be detected (represented as dots) can have converging and diverging parts. Arrows represent light penetration depth that depends on optical properties of the sample, e.g., sample turbidity. A goal can be to provide light penetration in the narrowest part of the flow (1). In that case, an optical technique, such as dynamic light scattering, light extinction, light scattering, or a combination of techniques, can be used to detect and characterize the impurities (particles, inclusions) in the flow. [61] FIG. 6B shows an overview of an exemplary particle monitoring system and parameters for numerical estimations that will be discussed later.
[62] There can be several basic groupings into which exemplary designs for a particle monitoring system can be categorized. FIG. 6C shows an overview of examples of cuvettes according to a first group. Here, there can be two optical elements with Y axis elongation and Z axis curvature. Examples include two prisms with opposing tips, two cylindrical lenses and two optical blocks with minimal overlap on the Z axis. FIG. 6D shows an overview of examples of cuvettes according to a second group. Here, there can be optical elements with flow passages elongated in the Y axis and confined in Z axis. These designs may include, for example, a monolithic waveguide structure with a slit for flow that is limited in the Z direction. Another group of designs could include a combination of features. For example, one optical element could have substantial curvature in the Z direction and another element could include a flat section.
[63] The transparency of the sample flow can be arranged in the form of a "sheet" flow, which can be relatively thin in first (X) and second (Z) orthogonal dimensions and long in a third (Y) orthogonal dimension. Exemplary optimal sample thicknesses can be determined using, for example, two criteria. A first criterion can be based either on the absence of significant multiple scattering of light by the sample or the existence of relatively high sample transparency; this criterion can determine thickness in the first dimension.
[64] A second criterion can be based on desired pressure drop of the optical cuvette at required flow rates. Pressure drop inside of an optical cuvette can be an important factor for method applicability in industry. There may be an acceptable range of pressure drops that can be introduced by a device (like in-line monitoring device) into flow lanes. This range can vary from application to application and depends from process parameters. Pressure drop inside of a cuvette can be a reverse function of flow thicknesses in the first and third dimensions and which can determine the cross section of the cuvette. Because the flow thickness in the first dimension X can be determined by optical transparency criterion and may not be varied freely, the flow width in third dimension Y can be used to keep the pressure drop at a desired level. The pressure drop can be directly proportional to the flow dimension in the second direction Z and this also can be used to affect the pressure drop in the cuvette in a desired manner.
[65] In one example, a sample fluid flow having a thickness in the range of approximately
X = 5-500 μm, Z = 0.1-5 mm and width of Y = 5-25 mm in the third dimension can be established.
[66] A diverging angle in the output part of cuvette can also affect pressure drop in the cuvette at a given flow rate and may be chosen accordingly. Another criterion to choose the diverging angle can be its affect on flow structure. For example, a high diverging angle (an extreme case is a right angle, i.e., slit in flat material) most likely generates turbulent motion in the flow. When turbulence is not desirable it can be prevented by choosing proper diverging angle of cuvette.
[67] In exemplary embodiments, laser light extinction and multiple light scattering by the particles can be negligible for a "sheet" of a typical slurry. At the same time, the slurry flow may require no dilution and therefore the size distribution of the particles in the slurry can have minimum distortion.
[68] Numerical Estimations
[69] In one embodiment, referring again to FIG. 6B, flow parameters at a measuring point are width Y, thickness X, flowrate Q. A laser beam of Lp (not shown) power has width Y and thickness Z. A measuring area Z*Y is projected by an optical system with magnification k to a camera type sensor with Py*Pz pixels (pixel sizes are zp and yp) and signal accumulation time tc. Optical magnification is chosen for whole flow observation:
[70] Y = k*Py* yp .
[71] Particle velocity in the measuring area is V= Q/(X*Y). Signal registration time is t =
Z/V or t = Zp /k/V , which one is smaller. Assuming t< tc (valid for most cases) the signal amplitude is:
[72] S = Lp*F(d)*X/Q*( zp IkTL),
[73] where F(d) is light scattering function for particle of size d. For particles in scattering media, the detection limit is determined by signal/noise ratio rather by signal value itself. Signal/noise ratio can be affected by two parameters - the volume of scattering media illuminating the single pixel and ratio of signal and noise accumulation times. Multiplying these two factors for signal/noise ratio results in:
[74] SN = Py/ tc /Q*(F(d)/F(dm)),
[75] where dm is median particle size in the scattering media. SN does not necessarily depend on flow spatial parameters. This allows varying flow thickness X to achieve flow transparency without affecting signal/noise ratio.
[76] Multiple light scattering may be negligible for sample optical thicknesses below one
(i.e., transmission>exp(-l)). The range of acceptable sample optical thickness can be extended up to five or more at small signal collection angles. In that case, the correction of the Beer- Lambert light scattering law can be modified.
[77] The parameters of the sensor (e.g., detecting camera) can also be as important as the total flow rate. Some exemplary calculation results for two cameras (1024 and 2048 pixels) and two flow rates are shown in Table 1. Detectable particle size dp is estimated in assumption of Raleigh scattering (F(d)~d 6) and signal to noise ratio of 1 (slurry parameters are d=100 nm and N= Ie 12 1/cc).
[78] It can be seen from Table 1 that with simple assumptions it should be possible to detect individual particles as small as 600-1000 nm. It should be mentioned that detectable particle size can be reduced if necessary by operating at S/N ratios below 1, which may be technically feasible.
[79] FIGs. 7 A, 7B, 7C and 7D show an exemplary particle monitoring system 200 according to a first embodiment. In this embodiment, particle monitoring system 200 comprises a cuvette 210, e.g., a transparent optical flow cell, configured to confine a flowable sample. The flowable sample may be opaque to at least a first range of wavelengths of light waves. A transparent flow compression element 220, e.g., prisms, can be located within the cuvette 210 and configured to compress the flowable sample in a first (X) direction while controlling the sample in a second direction (Z) parallel to the direction of flow and orthogonal to the first direction while elongating the sample in a third direction (Y) orthogonal to the first and second directions. When the sample is compressed in the first direction, it may become transparent to at least one of the wavelengths in the range of wavelengths of light waves.
[80] In one embodiment, exemplary dimensions for the X, Z and Y directions may be about 50 μm to 3 mm in the first (X) direction, about 10 μm to 3 mm in the second (Z) direction and about 5 mm to 25 mm in the third (Y) dimension.
[81] In one embodiment, an optical flow cell, such as a cuvette 210, can be used to form a focused flow of the sample fluid. The cuvette 210 can include a flow converging part, a measuring part, a sample introduction part and a sample discharge part. The width of the flow channel in the measuring part of the cuvette 210 can be narrow in the first dimension (e.g., 0.1 mm ± 10% or lesser or greater) and wide in the third orthogonal dimension (for example, approximately 10 mm ± 10% or lesser or greater).
[82] The effective flow dimension in the second orthogonal direction may be determined by the curvature of the flow focusing elements and can be in the range of, for example, 10 μm to 3 mm. The flow channel parameters can be substantially constant (e.g., ± 10% flow channel width in any direction) along the whole length of this measuring part of the cuvette 210. The measuring part of the cuvette 210 can be optically transparent and may be used for characterization of the sample transparency and for the optical characterization of particles in the focused sample fluid.
[83] In one embodiment, as shown in FIGs. 7C and 7D, sample fluid flow can also be placed into operable communication (e.g., at least partially surrounded) with a flow of clean (i.e. relatively particle-free) transparent liquid (e.g., water) or other appropriate liquid. This may be accomplished by introducing and removing the clean transparent liquid via surrounding flow inlets and outlets, for example. This method can be used to avoid the contamination of optical parts or as another method to control sample flow thickness and transparency. An exemplary optical cuvette having symmetrical surrounding flow inlets is illustrated in FIGs. 7C and 7D. Main sample flow can be in- troduced through the flow inlet and discharged through the sensing area formed by the tips of the prisms 220. A surrounding flow of clean liquid compatible with sample liquid parameters can form a boundary layer on the prism 220 surfaces preventing particle deposition on optical surfaces. Surrounding flow can be chosen compatible with sample flow and flow rates can be minimal so as not to affect the sample flow properties.
[84] In one embodiment, an exemplary way of compressing flow is represented in FIGs.
7A, 7B, 7C and 7D as two optical elements (e.g., prisms 220) having a gap formed between the tips, to compress the sample and render the sample transparent to at least one wavelength of light waves. The tips of the prisms 220 may be designed to provide the necessary optical quality. Prisms as flow forming optical elements can satisfy the parameters mentioned above: elongation by axis Y and short distance by axis Z. The optical signal can be collected through the flat surface of the prism opposing the sensing volume forming tip. The prism angle from tip to flat surface can be chosen depending on requirements of the signal detection system - for light transmission schemes the angle can be small, for light scattering schemes bigger angles can be used for scattered light collection.
[85] Symmetrical or asymmetrical prisms can be used depending on requirements for converging and diverging angles of the flow. Those skilled in the art will appreciate that in any or all of the foregoing embodiments, as well as variations thereof, the cuvette can be configured using two optical elements, such as two equilateral (or other) prisms to produce a flow cell for compressing the sample in at least one dimension to render the sample transparent to light waves of a predetermined wavelength.
[86] The system also can include a way to identify characteristics of individual particles contained in the compressed sample. In one embodiment, the identifying device is represented in FIG. 7B as an optical camera or detector 230 (e.g., a CCD camera, CMOS, photodiode or other optically sensitive device) in optical communication with the cuvette 210. An associated light source 240, e.g., a laser, which produces a beam of light 250, can also be in optical communication with the cuvette 210.
[87] The sample transparency can be measured by light extinction, and the sample fluid thickness in the flat part of the cuvette 210 can be adjusted to obtain a predetermined transparency value or sensing volume value. Conventional light scattering and/or light extinction techniques can be used to measure the parameters of single particles having diameters above the detection limit. A CCD (charge-coupled device) or CMOS detector/camera 230, together with appropriate frame-capture electronics and data- handling software, can be used to suppress the influence of background scattering on the quantitative detection of the signal produced by individual particles passing through the optical sensing volume. [88] FIGs. 7C and 7D shows more details of an exemplary cuvette 210 according to a first embodiment. The cuvette 210 can include the body assembly for the parts, prisms 220 attached to actuators 260, and two symmetrical holders. Proper sealing in the holder- prism interface can be provided by o-rings (e.g., Kalrez or Chemrez material). To achieve a variation in the channel thickness, the cuvette 210 can be configured using two symmetrical optical parts, such as prisms 220, separated by an elastic spacer formed of, for example, O-ring cord or any elastic material.
[89] Prisms 220 (e.g., sapphire or glass, coated with diamond like carbon) can be attached to actuators 260 allowing the prisms' displacement to adjust the sensing area width. Externally controlled pressure can be applied on these two opposing parts using, for example, screws, hydraulic or pneumatic actuators, electromagnetic actuators or any other way to control displacement to cause shrinkage in the spacer to a level that depends on the applied pressure and Young's modulus of elasticity for the spacer. This can allow control of the sample transparency, because the focused fluid sample thickness can have a known relationship (e.g., be proportional) to the flow channel thickness. Actuators 260 can also be used to provide high frequency (ultra- or megasonic) vibration of the prisms 220 to reduce possible particle deposition on optical parts.
[90] This exemplary embodiment allows a measurement of the sample transparency as a function of sample thickness in a single experiment. These measurements can permit a determination of the particle size parameters in the sample fluid using an integral scattering approach. At the same time, the parameters of the largest particles can be determined using a single-particle approach. The combination of these two different approaches (that is, integral and differential) can permit an improvement in the accuracy and reliability of the measurements.
[91] In a second embodiment, as shown in FIGs. 8 A and 8B, the sample fluid flow can be introduced into a flat part of the cuvette 310, which can be formed by two flat optical waveguides 320. In a variation of this embodiment, a monolithic waveguide structure with a slit for flow that is limited in the Z direction from the second group of designs mentioned previously can be used. The second embodiment can allow for a simple mechanical design of a cuvette in several possible embodiments. However, optical measurements can be made in transmission mode and flow may have substantial recirculation after passage through measuring area.
[92] The sample fluid in the flat part of the cuvette 310 can be illuminated with a light beam 350 of appropriate shape from a laser 340 or any other suitable light source. The beam shape can be chosen using criteria such as being wide enough to cover the whole flow width and narrow enough to go through optical waveguides 320. The intensity of the transmitted light can be measured and analyzed to determine the sample transparency. The width of the focused sample fluid flow can be adjusted to reach the desired level of sample transparency. When the desired level of sample transparency is achieved, the size parameters of the particles (for example, the particle size distribution above a given threshold diameter) in the sample fluid can be measured by known optical and electronic methods with relatively high accuracy.
[93] In a third embodiment, as shown in FIGs. 9A, 9B and 9C, the sample fluid flow can be introduced into the flat part of the cuvette 410 which can be formed by a flat optical window 470 and a cylindrical lens 480. This embodiment can allow a bigger optical signal collection angle but may have challenges in mechanical design of the cuvette 410. Dimension Z can be determined by lens diameter and may be substantially bigger than in the first or second embodiments.
[94] FIG. 10 shows an example of a fourth embodiment. As shown, the sample flow can be a circular "thread" of flow with thickness X. An exemplary light guide and scattering light collection system can be made of glass, sapphire or quartz. Scattered light can be delivered to a light detection and signal processing system by a fiber optic guide. This guide can be used to connect (convert) a circularly distributed signal with a linear optical detector. FIG. 11 shows a fifth embodiment similar to the fourth embodiment.
[95] FIGs. 12A, 12B, 12C and 12D show views of an exemplary particle monitoring system according to a sixth embodiment. In this embodiment, the waveguide can be formed using a bi-concave cylindrical lens. The slit can be cut in the middle of lens and polished for light passage. In this embodiment, the slit width can be fixed.
[96] Experimental results suggest the feasibility of the concepts described herein. For example, experiments were performed with an optical cuvette of the third embodiment (i.e., formed by a flat window and a cylindrical lens). An example of this optical cuvette is shown in FIGs. 9A, 9B and 9C. In this exemplary embodiment, the width of flow was 10 mm and sample thickness (X, measured with a shim) was -100 μm. The diameter of the cylindrical lens was 5 mm and the window diameter was 20 mm. The cylindrical lens was used to partially focus the laser beam in the cylinder- window vicinity (sensing area). The laser beam was widened before approaching the optical cuvette by another cylindrical lens to provide uniform irradiation along whole sample length in the Y axis.
[97] In this exemplary experimental embodiment, the housing was made of black Delrin material and the windows were partially glued or rubber-tight sealed. The measured pressure drop at these cell parameters was -1.5 psi for a flowrate of 100 ml/min. This pressure, which translates to 7.5 psi at 500 ml/min, should be acceptable, for example, for most semiconductor applications.
[98] In this embodiment, the sample was irradiated with a laser to which custom modi- fications were made to reduce pulse length to eliminate the image "smearing" of moving particles. The laser beam was stopped at the collection lens plane and a collection lens was used to direct forward scattering light to a video camera (WT-502 by Watec Corp.). The images were recorded on a PC with Airlink+ frame grabber.
[99] In this embodiment, the experimental results showed that non-diluted slurry looks like "milky" uniformly scattering media. Because of the small thickness the slurry was transparent. 1588 nm polymer microspheres from Duke Scientific Corp. in DI water were used to test for optical system sensitivity and the ability to record particles of such size. The same concentration of 1588 nm microspheres was also placed in a slurry. The results showed that the added particles are clearly detectable in DIW as well as in slurry.
[100] In this embodiment, the experimental data suggests that:
[101] Slurry becomes transparent at a certain thickness and optical methods can be applied for particle characterization.
[102] The cuvette resistance to flow can be kept low to facilitate the operation at relatively high flow rates, e.g., 500 ml/min.
[103] The whole flow can be irradiated and surveyed for the presence of big particles.
[104] Background scattering from slurry does not prevent the registration of big particles.
[105] Thus, in one embodiment, experimental results suggest that it may be possible to monitor 100% of the slurry flow at flowrates up to 500 ml/min.
[106] As described, exemplary embodiments are directed to non-intrusive systems and methods for in-line or off-line monitoring of single particles over a wide range of sizes and concentrations, contained in systems comprised mostly of smaller particles. Exemplary methods can accommodate mixtures without requiring their dilution, and mixtures wherein the "tail" of largest particles in the particle size distribution can be accurately measured. Optical characterization of particles over a wide range of sizes and concentrations in concentrated systems may be achieved using exemplary embodiments of an optical flow cell, such as a cuvette, wherein the sample flow is made relatively transparent to apply an optical technique for particle characterization.
[107] In an embodiment, a system for chemical.mechanical polishing of a semiconductor wafer illustrated in Figure 4 comprises a slurry source 17 comprising SiO.sub.2 or Al.sub.2 O.sub.3 particles suspended in an acid or base solution at a concentration of 4% to 18% solids by weight. The particle sizes range, e.g., from 0.03 .microns to over 1.0 micron in diameter. Occasionally, portions of the slurry 16 may contain particles of bigger size due to contamination or agglomeration of slurry particles. It is desirable to remove particles or agglomerations of particles from the slurry 16 before the slurry 16 reaches the semiconductor wafer 9 where these larger particles may damage the semiconductor wafer. [108] The chemical mechanical polishing system 12 includes an inline particle detection monitor 2 which is able to detect the size of the particles flowing through the slurry delivery line 15. The in-line particle size detection monitor 2 is provided by system 200 illustrated in Figure 7B which includes a cuvette 210 comprising two prisms 220, an identifying device comprising an optical camera or detector 230 (e.g., a CCD camera, CMOS, photodiode or other optically sensitive device) in optical communication with the cuvette 210. An associated light source 240, e.g., a laser, which produces a beam of light 250, can also be in optical communication with the cuvette 210.
[109] The sample transparency can be measured by light extinction, and the sample fluid thickness in the flat part of the cuvette 210 can be adjusted to obtain a predetermined transparency value or sensing volume value. Conventional light scattering and/or light extinction techniques can be used to measure the parameters of single particles having diameters above the detection limit. A CCD (charge-coupled device) or CMOS detector/camera 230, together with appropriate frame-capture electronics and data- handling software, can be used to suppress the influence of background scattering on the quantitative detection of the signal produced by individual particles passing through the optical sensing volume.
[110] If particles having a size of greater than a predetermined size, such as 1 micron, are detected, a control unit 4 activates the three-way valve 3 positioned in the slurry delivery line 15 downstream of the particle detection monitor 2 in order to redirect the portion of the slurry 16 containing these particles having a size greater than the predetermined size into the slurry waste container 14. Portions of the slurry 16 which do not contain particles above the predetermined size are directed into slurry delivery arm 11 where they are directed on to the wafer 9 and used to chemically mechanically polish the surface of the wafer 9.
[I l l] The detection system 2 and the timing of the actuation of the three-way valve 3 are synchronized so that the portion of the slurry detected by the detection means 2 at point C of the slurry line 15 is directed into waste container 14 when this portion of the slurry reaches the three-way valve 3 at point D in the slurry line 15. The portion of the slurry containing the undesirable large particles may spread due to turbulence and flow.non-unifomity during its travel from point C to point D. This spreading of the portion or packet of particles may be compensated as disclosed in connection with Figure 5 by adjusting the time delay before actuating the three-way valve 3 and/or by adjusting the length of time that the slurry flow is directed into the waste container 14.
[112] To summarize, systems and methods are disclosed for selective object manipulation in multi-component flow. An exemplary system can include a detection system for the monitoring of a component, such as a particle in a flow carrier. The system can also include a device (e.g., a valve or actuator) to manipulate the detected component from other components in the flow carrier. A controller or other processor can receive and process detected component data and distinguish a component of interest from the remaining flowable sample. Once the component is recognized, the controller synchronizes the flow manipulation device with the detection system to manipulate the detected component from the flow carrier. The above description is presented to enable a person skilled in the art to make and use the systems and methods described herein, and it is provided in the context of a particular application and its requirements. Various modifications to the embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments and applications without departing from the spirit and scope of the claims. Thus, there is no intention to be limited to the embodiments shown, but rather to be accorded the widest scope consistent with the principles and features disclosed herein.

Claims

Claims
[Claim 1] What is claimed is:
A system for selective object manipulation in multi-component flow, comprising: means for detecting and mapping a component in a flow carrier; means for manipulating the flow component, wherein manipulating the flow component means is configured to eliminate or separate the detected component from other components in the flow carrier; and means for controlling the manipulation of the detected component, wherein the controlling means is configured to synchronize the manipulating means with the detecting means.
[Claim 2] The system of claim 1, wherein the object is particle.
[Claim 3] The system of claim 1, wherein the object is agglomerate of particles.
[Claim 4] The system of claim 1, wherein the object is cell.
[Claim 5] The system of claim 1, wherein the object is the part of the multi- component flow with one or more parameters deviated from required value.
[Claim 6] The system of claim 1, wherein the multi-component flow comprising liquid or mixture of liquids.
[Claim 7] The system of claim 1, wherein the multi-component flow comprising liquid with particles.
[Claim 8] The system of claim 1, wherein the multi-component flow comprising liquid with bubbles.
[Claim 9] The system of claim 1, wherein the multi-component flow comprising liquid with dissolved substances.
[Claim 10] The system of claim 1, wherein the multi-component flow comprising liquid with biological substances.
[Claim 11] The system of claim 1, wherein the multi-component flow is slurry.
[Claim 12] The system of claim 1, wherein the multi-component flow is emulsion.
[Claim 13] The system of claim 1, wherein the multi-component flow is ink.
[Claim 14] The system of claim 1, wherein the multi-component flow is blood.
[Claim 15] The system of claim 1, wherein the detecting means designed to detect the presence of particle or object with particular characteristics while ignoring the presence of other objects (particles) with different characteristics.
[Claim 16] The system of claim 2, wherein the detecting means comprises optical method based on irradiation scattering (especially suitable for particle detection).
[Claim 17] The system of claim 1, wherein the detecting means comprises optical method based on polarization or wavelength change.
[Claim 18] The system of claim 1, wherein the detecting means comprises a ultrasonic or megasonic sensor.
[Claim 19] The system of claim 1, wherein the detecting means comprises X-ray scattering or reflection.
[Claim 20] The system of claim 1, wherein the detecting means comprises an electrical or electromagnetic sensor (e.g. capacitance sensor).
[Claim 21] The system of claim 16, wherein the detecting means comprises: a cuvette configured to confine a flowable sample, the flowable sample being opaque to at least a first range of wavelengths of light waves; a transparent flow compression element located within the cuvette and configured to compress the flowable sample in a first direction while controlling the sample in a second direction parallel to the direction of flow and orthogonal to the first direction while elongating the sample in a third direction orthogonal to the first and second directions, wherein when the sample is compressed in the first direction it becomes transparent to at least one of the wavelengths in the range of wavelengths of light waves; and a monitor for monitoring the flowable sample using the at least one wavelength.
[Claim 22] The system of claim 1, wherein the detected component mapping means is comprising of labeling each detection event with time stamp.
[Claim 23] The system of claim 1, wherein the flow manipulating means is configured to separate the detected component from other components in the flow carrier.
[Claim 24] The system of claim 1, wherein the flow manipulating means is configured to eliminate or destroy the detected component in the flow carrier.
[Claim 25] The system of claim 23, wherein the flow separating means comprises a flow split device for two or more subflows.
[Claim 26] The system of claim 25, wherein the flow split device for two or more subflows has valves in each subflow.
[Claim 27] The system of claim 25, wherein at least one of subflows is directed to main flow line.
[Claim 28] The system of claim 25, wherein at least one of subflows is directed to waste or waste collection system.
[Claim 29] The system of claim 23, wherein the flow separating means comprises a 3-way valve.
[Claim 30] The system of claim 29, wherein the flow separating 3-way valve "always ON" outlet is connected to main flow line.
[Claim 31] The system of claim 29, wherein the flow separating 3-way valve "always OFF" outlet is connected to waste flow line.
[Claim 32] The system of claim 24, wherein the flow component eliminating means comprises an injector of special chemistry for local change of flow properties.
[Claim 33] The system of claim 24, wherein the flow component eliminating means comprises a laser or other source of electromagnetic irradiation.
[Claim 34] The system of claim 1, wherein the flow manipulating means comprises a means for controlling the manipulation of the detected component, wherein the controlling means is configured to synchronize the manipulating means with the detecting means.
[Claim 35] The system of claim 34, wherein the controlling means is part of component detection means.
[Claim 36] The system of claim 34, wherein the controlling means is part of flow component manipulation means.
[Claim 37] The system of claim 34, wherein the controlling means is computer.
[Claim 38] The system of claim 34, wherein the controlling means is data accusation system.
[Claim 39] The system of claim 34, wherein the synchronization of the manipulating means with the detecting means includes predetermined time delay between detection and manipulating of component.
[Claim 40] The system of claim 39, wherein the time delay is the function of the flow rate, wherein the time delay function of the flow rate is determined as flow rate divided to cross section of flow connector line between detection and manipulation systems.
[Claim 41] The system of claim 34, wherein the synchronization of the manipulating means with the detecting means includes predetermined time duration for manipulating of component.
[Claim 42] The system of claim 41, wherein the predetermined time duration for manipulating of component is function of the flow rate, the activation time for flow manipulation system, turbulence of the flow and desired waste minimization factor.
[Claim 43] The system of claim 41, wherein the time duration for manipulating of component is determined experimentally using second detection system in the place of the flow manipulation system.
[Claim 44] A system for selective object manipulation in multi-component flow, comprising: means for detecting and mapping a component in a flow carrier; means for manipulating flow, wherein the flow manipulating means is configured to manipulate the detected component while preserving other components in the flow carrier; and means for controlling the manipulation of the detected component, wherein the controlling means is configured to synchronize the manipulating means with the detecting and mapping means.
[Claim 45] A method of selective object manipulation in multi-component flow, comprising: detecting and mapping a component in a flow carrier; and manipulating the detected component while preserving other components in the flow carrier, wherein the step of manipulating the detected component is synchronized with the step of detecting and mapping the component.
[Claim 46] The method of claim 45, wherein the object is particle.
[Claim 47] The method of claim 45, wherein the object is agglomerate of particles.
[Claim 48] The method of claim 45, wherein the object is cell.
[Claim 49] The method of claim 45, wherein the object is the part of the multi- component flow with one or more parameters deviated from required value.
[Claim 50] The method of claim 45, wherein the multi-component flow comprising liquid or mixture of liquids.
[Claim 51] The method of claim 45, wherein the multi-component flow comprising liquid with particles.
[Claim 52] The method of claim 45, wherein the multi-component flow comprising liquid with bubbles.
[Claim 53] The method of claim 45, wherein the multi-component flow comprising liquid with dissolved substances
[Claim 54] The method of claim 45, wherein the multi-component flow comprising liquid with biological substances.
[Claim 55] The method of claim 45, wherein the multi-component flow is slurry.
[Claim 56] The method of claim 45, wherein the multi-component flow is emulsion.
[Claim 57] The method of claim 45, wherein the multi-component flow is ink.
[Claim 58] The method of claim 45, wherein the multi-component flow is blood.
[Claim 59] The method of claim 45, wherein the detecting means designed to detect the presence of particle or object with particular characteristics while ignoring the presence of other objects (particles) with different characteristics.
[Claim 60] The method of claim 45, wherein the detecting means comprises optical method based on irradiation scattering (especially suitable for particle detection).
[Claim 61] The method of claim 45, wherein the detecting means comprises optical method based on polarization or wavelength change.
[Claim 62] The method of claim 45, wherein the detecting means comprises a ultrasonic or megasonic sensor.
[Claim 63] The method of claim 45, wherein the detecting means comprises X-ray scattering or reflection.
[Claim 64] The method of claim 45, wherein the detecting means comprises an electrical or electromagnetic sensor (e.g. capacitance sensor).
[Claim 65] The method of claim 59, wherein the detecting means comprises: a cuvette configured to confine a flowable sample, the flowable sample being opaque to at least a first range of wavelengths of light waves; a transparent flow compression element located within the cuvette and configured to compress the flowable sample in a first direction while controlling the sample in a second direction parallel to the direction of flow and orthogonal to the first direction while elongating the sample in a third direction orthogonal to the first and second directions, wherein when the sample is compressed in the first direction it becomes transparent to at least one of the wavelengths in the range of wavelengths of light waves; and a monitor for monitoring the flowable sample using the at least one wavelength.
[Claim 66] The method of claim 45, wherein the detected component mapping means is comprising of labeling each detection event with time stamp.
[Claim 67] The method of claim 45, wherein the flow manipulating means is configured to separate the detected component from other components in the flow carrier.
[Claim 68] The method of claim 45, wherein the flow manipulating means is configured to eliminate or destroy the detected component in the flow carrier.
[Claim 69] The method of claim 67, wherein the flow separating means comprises a flow split device for two or more subflows.
[Claim 70] The method of claim 69, wherein the flow split device for two or more subflows has valves in each subflow.
[Claim 71] The method of claim 69, wherein at least one of subflows is directed to main flow line.
[Claim 72] The method of claim 69, wherein at least one of subflows is directed to waste or waste collection system.
[Claim 73] The method of claim 67, wherein the flow separating means comprises a 3-way valve.
[Claim 74] The method of claim 73, wherein the flow separating 3-way valve "always ON" outlet is connected to main flow line.
[Claim 75] The method of claim 73, wherein the flow separating 3-way valve "always OFF" outlet is connected to waste flow line.
[Claim 76] The method of claim 68, wherein the flow component eliminating means comprises an injector of special chemistry for local change of flow properties.
[Claim 77] The method of claim 68, wherein the flow component eliminating means comprises a laser or other source of electromagnetic irradiation.
[Claim 78] The method of claim 45, wherein the flow manipulating means comprises a means for controlling the manipulation of the detected component, wherein the controlling means is configured to synchronize the manipulating means with the detecting means.
[Claim 79] The method of claim 78, wherein the controlling means is part of component detection means.
[Claim 80] The method of claim 78, wherein the controlling means is part of flow component manipulation means.
[Claim 81] The method of claim 78, wherein the controlling means is computer.
[Claim 82] The method of claim 78, wherein the controlling means is data accusation system.
[Claim 83] The method of claim 78, wherein the synchronization of the manipulating means with the detecting means includes predetermined time delay between detection and manipulating of component.
[Claim 84] The method of claim 83, wherein the time delay is the function of the flow rate, wherein the time delay function of the flow rate is determined as flow rate divided to cross section of flow connector line between detection and manipulation systems.
[Claim 85] The method of claim 45, wherein the synchronization of the manipulating means with the detecting means includes predetermined time duration for manipulating of component.
[Claim 86] The method of claim 85, wherein the predetermined time duration for manipulating of component is function of the flow rate, the activation time for flow manipulation system, turbulence of the flow and desired waste minimization factor.
[Claim 87] The method of claim 85, wherein the time duration for manipulating of component is determined experimentally using second detection system in the place of the flow manipulation system.
[Claim 88] A particle monitoring system, comprising: a cuvette configured to confine a flowable sample, the flowable sample being opaque to at least a first range of wavelengths of light waves; a transparent flow compression element located within the cuvette and configured to compress the flowable sample in a first direction while controlling the sample in a second direction parallel to the direction of flow and orthogonal to the first direction while elongating the sample in a third direction orthogonal to the first and second directions, wherein when the sample is compressed in the first direction it becomes transparent to at least one of the wavelengths in the range of wavelengths of light waves; and a monitor for monitoring the flowable sample using the at least one wavelength.
[Claim 89] The system of claim 88, wherein the transparent flow compression element comprises one or more optical elements.
[Claim 90] The system of claim 88, wherein the one or more optical elements comprise two prisons or two waveguides or a cylindrical lens and an optical window or a first light guide and a second light guide, wherein the second light guide is configured to deliver scattered light, or an optical waveguide configured with a hole through which the flowable sample flows.
[Claim 91] The system of claim 89, wherein the one or more optical elements comprise a protective coating.
[Claim 92] The system of claim 88, comprising a mechanism operatively connected to the one or more optical elements and configured to adjust a distance between the one or more optical elements.
[Claim 93] The system of claim 92, wherein the mechanism comprises at least one of a screw, a hydraulic actuator, a pneumatic actuator and an electromagnetic actuator.
[Claim 94] The system of claim 92, wherein the mechanism is configured to vibrate the one or more optical elements.
[Claim 95] The system of claim 88, comprising a light source in optical communication with the cuvette.
[Claim 96] The system of claim 95, wherein the light source comprises a laser.
[Claim 97] The system of claim 88, the monitor comprising a detector in optical communication with the cuvette.
[Claim 98] The system of claim 97, wherein the detector comprises at least one of a line scanner, a CCD camera, a CMOS camera and a photo diode camera.
[Claim 99] A method of particle monitoring, comprising: confining a flowable sample, the flowable sample being opaque to at least a first range of wavelengths of light waves; measuring transparency of the flowable sample; compressing the flowable sample in a first direction while confining the sample in a second direction parallel to a flow direction of the flowable sample and orthogonal to the first direction, while elongating the sample in a third direction orthogonal to the first and second directions, wherein when the sample is compressed in the first direction, the sample becomes transparent to at least one of the wavelengths in the first range of wavelengths; and
Identifying characteristics of particle is contained in the sample that has been compressed.
[Claim 100] A method of claim 99, wherein the compressing comprises compressing to about 50 microns to 3 millimeters in the first direction while confining the flowable sample for about 10 microns to 3 millimeters in the second direction and the elongating the flowable sample to about 5 millimeters to 25 millimetres in the third direction.
[Claim 101] The method of claim 100, wherein compressing comprises using a transparent flow compression element.
[Claim 102] The method of claim 101, wherein the transparent flow compression element comprises: one or more optical elements.
[Claim 103] The method of claim 99, comprising adjusting a distance between the one or more optical elements using a mechanism operatively connected to the one or more optical elements.
[Claim 104] The method of claim 103, wherein the mechanism is configured to vibrate the one or more optical elements.
[Claim 105] The method of claim 99, wherein measuring transparency comprises irradiating the sample with a light source in optical communication with a cuvette used for confining the flowable sample.
[Claim 106] The method of claim 99, where identifying characteristics of particles comprises detecting an optical signal using a detector in optical communication with the cuvette.
[Claim 107] The method of claim 106, wherein the optical signal is transmitted through the sample.
[Claim 108] The method of claim 106, wherein the optical signal is reflected from the sample.
[Claim 109] The method of claim 99, comprising supply a slurry to a process that utilizes the wherein the entire slurry utilized by the process is monitored as the flowable sample.
[Claim 110] Use of the apparatus of one of claims 1 to 44 and 88 to 98 for chemical mechanical polishing. [Claim 111] Use of the method of one of claims 45 to 87 and 99 to 109 for chemical mechanical polishing.
PCT/IB2009/052974 2008-07-08 2009-07-08 System and methods for in-line monitoring of particles in opaque flows and selective object manipulation in multi-component flow WO2010004516A1 (en)

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