CN102345968B - Device and method for drying supercritical carbon dioxide microemulsion - Google Patents
Device and method for drying supercritical carbon dioxide microemulsion Download PDFInfo
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- CN102345968B CN102345968B CN2010102421539A CN201010242153A CN102345968B CN 102345968 B CN102345968 B CN 102345968B CN 2010102421539 A CN2010102421539 A CN 2010102421539A CN 201010242153 A CN201010242153 A CN 201010242153A CN 102345968 B CN102345968 B CN 102345968B
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Abstract
The invention discloses a device and a method for drying supercritical carbon dioxide microemulsion. The method comprises the following steps of: displacing a water-based cleaning fluid by using liquid carbon dioxide; adding a surfactant; heating the carbon dioxide to reach a supercritical state; and drying a photoresist or a microstructure in a micro-electromechanical system (MEMS). In the method, because a gas-liquid interface and the surface tension are prevented, high depth-to-width ratio or porous structures and the like can be cleaned and dried without damage. Compared with the conventional supercritical carbon dioxide drying method, the method has the advantages that: an organic solution is not required to be used, so that the photoresist and the like cannot be damaged; the drying time is greatly reduced, so that the problem of pattern collapse can be effectively solved. The method meets the requirements of reducing the consumption of the organic solution, saving energy and the like in an international semiconductor technology blueprint, and is easily compatible with the conventional integrated circuit (IC) process.
Description
Technical field
The present invention relates to semiconductor and clean and technical field of drying, relate in particular to a kind of based on supercritical carbon dioxide (SCCO
2) device and method of microemulsion drying.
Background technology
In the manufacture process of microelectronic component, along with characteristic size further reduce further raising with the complex structure degree, subsiding of device architecture becomes serious day by day problem.With water is that primary solvent cleans device afterwards when drying, and the more weak photoresist figure as microcomputer electric component and high-aspect-ratio of its mechanicalness structure can be destroyed.
Carbon dioxide is as a kind of environmental friendliness and cheap solvent, its above-critical state has and approaches zero surface tension and high diffusibility, be suitable for very much the semiconductor cleaning, clean in semiconductor and the micro-electromechanical technology and dry novel green solvent so ITRS in 2006 (ITRS) is considered as supercritical fluid can solve.Though utilize liquid carbon dioxide to replace organic solution, enter above-critical state then and carry out the problem that dry method can effectively solve present structural collapse.But still remain in the device architecture for fear of a certain amount of organic solution or water, what often need to carry out pulsed repeatedly repeats displacement, not only consuming time, and the consumption of carbon dioxide is very big.In carbon dioxide, add some special surfactants, when carbon dioxide runs into water, can form micro emulsion under certain condition and drip, will increase the solubility of water in carbon dioxide greatly.The microemulsion system that utilizes liquid carbon dioxide displacement deionized water and form with supercritical carbon dioxide and surfactant can carry out drying fast and efficiently.
Therefore based on the proposition of supercritical carbon dioxide microemulsion system, will be an effective way that addresses this problem.
Summary of the invention
(1) technical problem that will solve
In view of this, main purpose of the present invention is to provide a kind of device and method based on supercritical carbon dioxide microemulsion drying.
(2) technical scheme
For achieving the above object, the invention provides a kind of device based on supercritical carbon dioxide microemulsion drying, comprising:
The fluid reservoir 1 and the air accumulator 2 that high-purity carbon dioxide is provided of surfactant are housed, and the two is connected in magnetic valve 5 by second booster pump 3 and first booster pump 4 respectively, and the other end of magnetic valve 5 is connected in the inlet of reaction chamber 6;
Be connected in observation window 10 by first hand-operated valve 9 on the export pipeline of reaction chamber 6, be connected in second heat exchanger 18 by first expansion valve 19 on another export pipeline;
The outlet of observation window 10 is connected in first separator 13, is connected to one second expansion valve 11 and first heat exchanger 12 on the connecting line of the observation window 10 and first separator 13; The outlet of first separator 13 is connected in the first filtration purification devices, 15, the first filtration purification devices 15 and is connected in reaction chamber 6 by the 3rd booster pump 23 and the 4th heat exchanger 24;
The outlet of second heat exchanger 18 is connected in the 3rd separator 17, the three separators 17 and is connected in reaction chamber 6 by the 3rd heat exchanger 21, second separator 20, cooling device 22, the 3rd booster pump 23 and the 4th heat exchanger 24 successively;
An outlet of second separator 20 is filtered purification devices 26 by the 4th hand-operated valve 25 and second and is connected in surfactant storage tank 1.
In the such scheme, described reaction chamber 6 internal fixation have turning and rotary-tray 8, its outside that cold circulation 29 systems, heating system 30, temperature measuring equipment 27 and device for pressure measurement 28 are installed.
In the such scheme, described the 3rd separator 17, its first end is connected with the outlet of second heat exchanger 18, and second end is connected with second separator 20 by the 3rd heat exchanger 21, and the 3rd termination has the 3rd hand-operated valve 16.
In the such scheme, this device has a carbon dioxide and recycles system, comprising:
Be connected to first hand-operated valve 9 of reaction chamber 6 bottoms, its other end is connected in observation window 10, the outlet of observation window 10 is connected with second expansion valve 11 and first heat exchanger 12, the carbon dioxide that comes out from first heat exchanger 12 flows in first separator 13, filters purification devices 15 through first again and flows in the reaction chamber 6 by the 3rd booster pump 23 and the 4th heat exchanger 24;
Be connected to first expansion valve 19 of reaction chamber 6 bottoms, its other end is connected in second heat exchanger 18, the carbon dioxide that comes out from second heat exchanger 18 flows in the 3rd separator 17, the carbon dioxide that comes out from the 3rd separator 17 flows in second separator 20 through the 3rd heat exchanger 21 again, the other end of second separator 20 is connected in cooling device 22, and the carbon dioxide that comes out from cooling device 22 flows in the reaction chamber 6 by the 3rd booster pump 23 and the 4th heat exchanger 24.
In the such scheme, this device has a surfactant and recycles system, comprising:
Be connected to first expansion valve 19 of reaction chamber 6 bottoms, its other end is connected in second heat exchanger 18, second heat exchanger 18 is connected with the 3rd separator 17, the top exit of the 3rd separator 17 is connected through the inlet of the 3rd heat exchanger 21 and second separator 20, and surfactant filters purification devices 26 through the 4th hand-operated valve 25 and second again from the outlet of second separator 20 and flows back to the surfactant storage tank 1.
For achieving the above object, the present invention also provides a kind of drying means based on the supercritical carbon dioxide microemulsion, and this method is to utilize liquid carbon dioxide displacement deionized water, then utilizes based on SCCO
2Microemulsion structure graph is carried out drying, feed the pure carbon dioxide purge then.
In the such scheme, described water is deionized water, and uses carbon dioxide source purity to reach more than the 5N, and the selection of surfactant can not cause damage to structure graph.
(3) beneficial effect
From technique scheme as can be seen, the present invention has following beneficial effect:
1, this drying device and method provided by the invention based on the supercritical carbon dioxide microemulsion, supercritical carbon dioxide is owing to have peculiar properties such as quite low coefficient of viscosity, high diffusibility and insignificant surface tension, can do not destroyed trickleer structure by surface tension and capillary pulling force yet, therefore can effectively solve the problem of structural collapse in the dry run, and clean and dry device is provided.Therefore supercritical carbon dioxide is cleaned and dry solvent as semiconductor novel green of future generation, not only reduced organic solvent a large amount of uses, protected environment, reduced consumption the energy, and meet the development trend of ITRS.Directly use liquid carbon dioxide replacing water solution, and in supercritical carbon dioxide microemulsion environment, carry out drying, avoided a large amount of uses of organic solution and carbon dioxide, shortened scavenging period, improved efficient.Therefore no matter still be economic benefit from environmental issue, the supercritical carbon dioxide microemulsion system all has good development and application prospect, is expected to be used on the microelectronics machining production line.
2, this drying device and method provided by the invention based on the supercritical carbon dioxide microemulsion, mainly utilize liquid carbon dioxide displacement water-base cleaning liquid, add surfactant then and heat carbon dioxide and make it reach above-critical state the micro-structural among photoresist or the MEMS etc. is carried out drying.This method can be cleaned with drying high-aspect-ratio or loose structure etc. and not damage owing to avoided the generation of gas-liquid interface and prevented capillary effect.Therefore compare with present supercritical carbon dioxide drying means, this method need not used organic solution, can not damage photoresist etc.; And drying time reduce greatly, can effectively prevent the problem that figure subsides.This method meets in the ITRS about reducing requirements such as organic solution consumption and energy savings, and easily and present IC process compatible.
Description of drawings
Fig. 1 is the schematic representation of apparatus based on supercritical carbon dioxide microemulsion drying provided by the invention;
Fig. 2 is liquid carbon dioxide displacement and SCCO among the present invention
2The schematic diagram of microemulsion dry run;
Wherein, 1 is the surfactant storage tank, and 2 is the carbon dioxide air accumulator, 3 is second booster pump, and 4 is first booster pump, and 5 is magnetic valve, 6 is reaction chamber, and 7 are the print that is dried, and 8 is pallet turning and rotation, 9 is first hand-operated valve, 10 is observation window, and 11 is second expansion valve, and 12 is first heat exchanger, 13 is first separator, 14 is second hand-operated valve, and 15 is the first filtration purification devices, and 16 is the 3rd hand-operated valve, 17 is the 3rd separator, 18 is second heat exchanger, and 19 is first expansion valve, and 20 is second separator, 21 is the 3rd heat exchanger, 22 is cooling device, and 23 is the 3rd booster pump, and 24 is the 4th heat exchanger, 25 is the 4th hand-operated valve, and 26 is the second filtration purification devices; 27 is temperature sensor; 28 is pressure sensor; 29 is the cold circulatory system; 30 is heating system.
The specific embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
As shown in Figure 1, Fig. 1 is the schematic representation of apparatus based on supercritical carbon dioxide microemulsion drying provided by the invention, and this device comprises:
The fluid reservoir 1 and the air accumulator 2 that high-purity carbon dioxide is provided of surfactant are housed, and the two is connected in magnetic valve 5 by second booster pump 3 and first booster pump 4 respectively, and the other end of magnetic valve 5 is connected in the inlet of reaction chamber 6;
Be connected in observation window 10 by first hand-operated valve 9 on the export pipeline of reaction chamber 6, be connected in second heat exchanger 18 by first expansion valve 19 on another export pipeline;
The outlet of observation window 10 is connected in first separator 13, is connected to one second expansion valve 11 and first heat exchanger 12 on the connecting line of the observation window 10 and first separator 13; The outlet of first separator 13 is connected in the first filtration purification devices, 15, the first filtration purification devices 15 and is connected in reaction chamber 6 by the 3rd booster pump 23 and the 4th heat exchanger 24;
The outlet of second heat exchanger 18 is connected in the 3rd separator 17, the three separators 17 and is connected in reaction chamber 6 by the 3rd heat exchanger 21, second separator 20, cooling device 22, the 3rd booster pump 23 and the 4th heat exchanger 24 successively;
An outlet of second separator 20 is filtered purification devices 26 by the 4th hand-operated valve 25 and second and is connected in surfactant storage tank 1.
Wherein, described reaction chamber 6 internal fixation have turning and rotary-tray 8, its outside that cold circulation 29 systems, heating system 30, temperature measuring equipment 27 and device for pressure measurement 28 are installed.Described the 3rd separator 17, its first end is connected with the outlet of second heat exchanger 18, and second end is connected with second separator 20 by the 3rd heat exchanger 21, and the 3rd termination has the 3rd hand-operated valve 16.
Device based on supercritical carbon dioxide microemulsion drying provided by the invention, have a carbon dioxide and recycle system, comprise: first hand-operated valve 9 that is connected to reaction chamber 6 bottoms, its other end is connected in observation window 10, the outlet of observation window 10 is connected with second expansion valve 11 and first heat exchanger 12, the carbon dioxide that comes out from first heat exchanger 12 flows in first separator 13, filters purification devices 15 through first again and flows in the reaction chamber 6 by the 3rd booster pump 23 and the 4th heat exchanger 24; Be connected to first expansion valve 19 of reaction chamber 6 bottoms, its other end is connected in second heat exchanger 18, the carbon dioxide that comes out from second heat exchanger 18 flows in the 3rd separator 17, the carbon dioxide that comes out from the 3rd separator 17 flows in second separator 20 through the 3rd heat exchanger 21 again, the other end of second separator 20 is connected in cooling device 22, and the carbon dioxide that comes out from cooling device 22 flows in the reaction chamber 6 by the 3rd booster pump 23 and the 4th heat exchanger 24.
Device based on supercritical carbon dioxide microemulsion drying provided by the invention, also have a surfactant and recycle system, comprise: first expansion valve 19 that is connected to reaction chamber 6 bottoms, its other end is connected in second heat exchanger 18, second heat exchanger 18 is connected with the 3rd separator 17, the top exit of the 3rd separator 17 is connected through the inlet of the 3rd heat exchanger 21 and second separator 20, and surfactant filters purification devices 26 through the 4th hand-operated valve 25 and second again from the outlet of second separator 20 and flows back to the surfactant storage tank 1.
Referring again to Fig. 1, the annexation based on each parts in the device of supercritical carbon dioxide microemulsion drying provided by the invention is: the outlet of surfactant storage tank 1 is connected to an end of magnetic valve 5 by second booster pump 3; The outlet of carbon dioxide storage tank 2 is connected to an end of magnetic valve 5 by first booster pump 4; The other end of magnetic valve 5 links to each other with the arrival end of reaction chamber 6; The print 7 that is dried is fixed on the pallet 8 of rotatable and upset; The outlet of reaction chamber 6 is positioned at the bottom, is connected with observation window 10 by first hand-operated valve 9; The outlet of observation window 10 is connected to second expansion valve 11, links to each other with the inlet of first separator 13 through first heat exchanger 12 then, and its outlet at bottom is connected to second hand-operated valve 14; The top exit of first separator 13 connects first and crosses filtration purification devices 15, and the inlet with the 3rd booster pump 23 is connected then; The outlet of the 3rd booster pump 23 is connected to reaction chamber 6 via the 4th heat exchanger 24; Another outlet of reaction chamber 6 is communicated with the inlet of the 3rd separator 17 by first expansion valve 19 and second heat exchanger 18; Waste liquid in the 3rd separator 17 is discharged by the 3rd hand-operated valve 16, and its top exit is connected to the import of second separator 20 through the 3rd heat exchanger 21; The top exit of second separator 20 is connected with the 3rd booster pump 23 by cooling device 22, is connected with magnetic valve 5 through the 4th heat exchanger 24 then; The outlet at bottom of second separator 20 links together and is communicated with surfactant storage tank 1 through the 4th hand-operated valve 25 and the second mistake filtration purification devices 26; Temperate zone sensor 27 is positioned at the top of reaction chamber 6, and pressure sensor 28 is positioned at the top of reaction chamber 6; The cold circulatory system 29 is wrapped in the outer wall of reaction chamber 6, and heating system 30 is fixed on the outside of reaction chamber 6.
In conjunction with Fig. 1, the effect based on each parts in the device of supercritical carbon dioxide microemulsion drying provided by the invention is respectively: first, second and the 3rd booster pump are used for reactant being pumped into chamber and chamber being pressurizeed; Temperate zone sensor 27 is used for measuring in real time and shows temperature in the reaction chamber 6; Pressure sensor 28 is used for measuring in real time and shows pressure in the reaction chamber 6; Pallet 8 is designed to rotatable and upset is that most water breaks away from silicon chip in the print 7 that is dried under the effect of mechanical force in order to make; Thereby the cold circulatory system 29 is to be used for keeping the carbon dioxide that enters to reaction chamber 6 refrigeration to be liquid state; Thereby heating system 30 is to be used for heating to reaction chamber 6 making carbon dioxide reach above-critical state; The effect of observation window 10 is whether be used for observing displacement complete; The effect of expansion valve is to make that warm material becomes the low-temp low-pressure state in the high pressure; The first, second, third and the 4th heat exchanger further strengthens gas-liquid separation; First, second and the 3rd separator are realized gas-liquid separation and are collected liquid; Cooling device 22 is used for making it become liquid state to the gaseous carbon dioxide refrigeration; First and second filter purification devices is used for the material that needs recycle is filtered and purifies.
As shown in Figure 2, Fig. 2 is liquid carbon dioxide displacement and SCCO among the present invention
2The schematic diagram of microemulsion dry run should be based on SCCO
2The dry run of microemulsion system is: structure after will corroding or figure are put on the silicon chip chuck of reaction chamber, and use the deionized water submergence, prevent gas-liquid interface.With reaction chamber sealing and refrigeration, make temperature reach 5 ℃ then, pressure maintains 4MPa, and this process can be measured in real time and shows by the temperature and pressure sensor; The carbon dioxide that enter chamber this moment is a liquid, and its density is 0.893g/cm
3, less than the density of water, so liquid carbon dioxide pumps into chamber from the top of reaction chamber.Because the solubility of water in pure liquid carbon dioxide is very little, easily replaced by liquid carbon dioxide; In course of reaction, at regular intervals, just first hand-operated valve is slowly opened, make observation window be full of mixing material, and whether analyze displacement according to the interface location of mixes liquid in the form abundant; Mixing material in the form enters in first separator by expansion valve and heat exchanger; Gaseous carbon dioxide in first separator is by after filtering purifier and filter and purifying, by the booster pump pressurization be injected into carry out in the chamber recycling; Waste liquid in first separator can be discharged from by second hand-operated valve; After replacement completion, silicon chip is opened second booster pump this moment just by the submergence of liquid carbon dioxide institute, adds surfactant, closes the cold circulatory system then, opens heating system, and reaction chamber is heated; After carbon dioxide reaches above-critical state, with holding the pallet reversing of silicon chip, be rotated simultaneously, allow the most of water that covers silicon chip surface under action of centrifugal force, leave silicon chip surface, fraction water then since the effect meeting of surfactant at SCCO
2The middle micro emulsion that forms drips, and silicon chip is carried out drying; After dry a period of time, feed the gaseous state pure carbon dioxide, with the SCCO in the chamber
2Microemulsion is discharged in the 3rd separator and second separator by expansion valve; Waste liquid in the 3rd separator can be discharged by the control of the 3rd hand-operated valve; The gaseous carbon dioxide of separating from the 3rd separator and second separator becomes liquid state after the cooler refrigeration, finally inject reaction chamber by booster pump and recycle; Surfactant in second separator can recycle by filtering purification devices purification filtration.Behind dry the end, the chamber pressure release to normal pressure, is needed in pressure leak process to guarantee that chamber temp is all the time greater than critical-temperature; Print can be taken out then and carry out subsequent analysis.At last the waste liquids such as water in the separator are discharged.
Above-described specific embodiment; purpose of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the above only is specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. the device based on supercritical carbon dioxide microemulsion drying is characterized in that, comprising:
The fluid reservoir (1) of surfactant is housed and the air accumulator (2) of high-purity carbon dioxide is provided, the two is connected in magnetic valve (5) by second booster pump (3) and first booster pump (4) respectively, and the other end of magnetic valve (5) is connected in the inlet of reaction chamber (6);
Be connected in observation window (10) by first hand-operated valve (9) on the export pipeline of reaction chamber (6), be connected in second heat exchanger (18) by first expansion valve (19) on another export pipeline; Reaction chamber (6) internal fixation has turning and rotary-tray (8), and its outside is equipped with cold circulation (29) system, heating system (30), temperature measuring equipment (27) and device for pressure measurement (28);
The outlet of observation window (10) is connected in first separator (13), is connected to one second expansion valve (11) and first heat exchanger (12) on the connecting line of observation window (10) and first separator (13); The outlet of first separator (13) is connected in first and filters purification devices (15), and first filters purification devices (15) is connected in reaction chamber (6) by the 3rd booster pump (23) and the 4th heat exchanger (24);
The outlet of second heat exchanger (18) is connected in the 3rd separator (17), and the 3rd separator (17) is connected in reaction chamber (6) by the 3rd heat exchanger (21), second separator (20), cooling device (22), the 3rd booster pump (23) and the 4th heat exchanger (24) successively;
An outlet of second separator (20) is filtered purification devices (26) by the 4th hand-operated valve (25) and second and is connected in surfactant storage tank (1).
2. the device based on supercritical carbon dioxide microemulsion drying according to claim 1, it is characterized in that, described the 3rd separator (17), its first end is connected with the outlet of second heat exchanger (18), second end is connected with second separator (20) by the 3rd heat exchanger (21), and the 3rd termination has the 3rd hand-operated valve (16).
3. the device based on supercritical carbon dioxide microemulsion drying according to claim 1 is characterized in that, this device has a carbon dioxide and recycles system, comprising:
Be connected to first hand-operated valve (9) of reaction chamber (6) bottom, its other end is connected in observation window (10), the outlet of observation window (10) is connected with second expansion valve (11) and first heat exchanger (12), the carbon dioxide that comes out from first heat exchanger (12) flows in first separator (13), filters purification devices (15) through first again and flows in the reaction chamber (6) by the 3rd booster pump (23) and the 4th heat exchanger (24);
Be connected to first expansion valve (19) of reaction chamber (6) bottom, its other end is connected in second heat exchanger (18), the carbon dioxide that comes out from second heat exchanger (18) flows in the 3rd separator (17), the carbon dioxide that comes out from the 3rd separator (17) flows in second separator (20) through the 3rd heat exchanger (21) again, the other end of second separator (20) is connected in cooling device (22), and the carbon dioxide that comes out from cooling device (22) flows in the reaction chamber (6) by the 3rd booster pump (23) and the 4th heat exchanger (24).
4. the device based on supercritical carbon dioxide microemulsion drying according to claim 1 is characterized in that, this device has a surfactant and recycles system, comprising:
Be connected to first expansion valve (19) of reaction chamber (6) bottom, its other end is connected in second heat exchanger (18), second heat exchanger (18) is connected with the 3rd separator (17), the top exit of the 3rd separator (17) is connected through the 3rd heat exchanger (21) and the inlet of second separator (20), and surfactant filters purification devices (26) through the 4th hand-operated valve (25) and second again from the outlet of second separator (20) and flows back to the surfactant storage tank (1).
5. the drying means based on the supercritical carbon dioxide microemulsion is applied to the described device of claim 1, it is characterized in that, this method is to utilize liquid carbon dioxide displacement deionized water, then utilizes based on SCCO
2Microemulsion structure graph is carried out drying, feed the pure carbon dioxide purge then.
6. the drying means based on the supercritical carbon dioxide microemulsion according to claim 5 is characterized in that, described water is deionized water, and uses carbon dioxide source purity to reach more than the 5N, and the selection of surfactant can not cause damage to structure graph.
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