WO2008052112A2

WO2008052112A2 - Multiple pin mixing apparatus and methods of using

Info

Publication number: WO2008052112A2
Application number: PCT/US2007/082522
Authority: WO
Inventors: Matthew F. Smith; Justin Fisher; Parvinder Walia; Matt Bishop
Original assignee: Symyx Technologies, Inc.; Dow Chemical Company
Priority date: 2006-10-25
Filing date: 2007-10-25
Publication date: 2008-05-02
Also published as: WO2008052112A3

Abstract

The present invention is directed to a four-rotor mixer and methods for blending materials using the mixer. The four-rotor mixer is a system that can heat, mix, and extrude multi-component chemistry systems of materials, such as polymers and additives (fillers, pigments, catalysts, etc.) optionally with automation and under software control.

Description

MULTIPLE PIN MIXING APPARATUS AND METHODS OF USING

[0001] This application claims priority from U.S. Provisional patent application number 60/854,588, filed October 25, 2006, which is incorporated herein by reference in its entirety.

FIELD OF THE INVENTION [0002] The present invention generally relates to apparatus and methods for blending materials, and specifically, to apparatus and methods for providing good dispersion and distribution of blended materials.

BACKGROUND OF INVENTION

[0003] The discovery of new materials with novel chemical and physical properties often leads to the development of new and useful technologies. Over forty years ago, for example, the preparation of single crystal semiconductors transformed the electronics industry. Currently, there is a tremendous amount of activity being carried out in the areas of new materials. Unfortunately, even though the chemistry of extended solids has been extensively explored, few general principles have emerged that allow one to predict with certainty composition, structure and reaction pathways for the synthesis of such solid state compounds, compositions or structures. Moreover, it is difficult to predict a priori the physical properties or the microstructure that a particular material will possess. [0004] Polymeric blends comprise at least two components—a major and a minor component. Producing polymeric blends comprising at least two components mandates dispersing the minor component into the major component. Conventional manufacturing processes typically utilize single or twin screw extruders to this end. When the minor component is thoroughly mixed into the major component, it is otherwise known as the dispersed minor phase. The morphology— general size and shape—of the dispersed minor phase affects the overall mechanical and chemical properties of the polymeric system. The smaller the dispersed-phase morphologies tend to be, the better the resulting mechanical and chemical properties; clearly, relatively small dispersed-phase morphologies provide a commercial advantage because of the polymeric blend's improved mechanical and chemical properties.

[0005] Extruders are conventionally used in dispersion processes to produce dispersed- phase morphologies having an order of magnitude of approximately 1 micron. An explanation for current polymeric systems generally having consistent dispersed-phase morphologies of 1 micron is that a particular extruder's viscous and interfacial forces acting on the polymeric system's minor components are of the same magnitude as any other. For a typical continuous phase extrusion process (viscosity equal to 100 Pa-second and shear rate equal to 100 sec.sup.-l), the shear (viscous) stresses responsible for breaking up the minor component into smaller domains are about 10,000 Pa. and have to balance the interfacial stresses acting on the surface of the dispersed particles (or polymer-polymer interfacial tension divided by the length scale of the dispersed phase). For a typical surface tension of about 0.01 N/m, the characteristic dimension of the dispersed particles to balance the characteristic viscous stresses is about 10.sup.-6 m (or 1 micron). Because of the inherent mechanical limitations—a typical extrusion process is incapable of producing polymeric systems having dispersed-phase morphologies less than 1 micron. It would therefore be of great scientific and commercial importance to design a commercially viable process comprising a mixing method yielding polymeric systems having dispersed-phase morphologies less than 1 micron-dispersed-phase morphologies smaller than those currently produced by conventional methods. [0006] There are screw-type micro-extruders commercially available that are designed to blend small batches of polymer melts. These systems are typically very expensive. Moreover, they are difficult to clean and maintain. Furthermore, they do not provide both good dispersive mixing and distributive mixing.

[0007] Methods and apparatus utilizing chaotic mixing to obtain unusual morphologies in polymer blends, which are not typically obtained by conventional blending in single and twin screw extruders have been recently developed. Chaotic mixing systems (those whose designs provide mixing that will evolve over time so that any given region or open set of its phase space will eventually overlap with any other given region) have been utilized and investigated. Blends produced within batch chaotic mixers, such as those including two vertical, spaced apart rotors in a cavity, have been shown to have enhanced physical properties. Enhanced properties have been measured in blends produced by chaotic mixing even when the component phases have poor interfacial cohesion. Experimental and numerical studies of chaotic mixing in various geometries have so far shown agreement and provide a strong foundation for the practical application of chaos theory to polymer systems. However, these designs and methods do not provide an opportunity for superior dispersive and distributive mixing, or the ability to tailor a blended system by designing different blending modes. [0008] A thorough understanding is still being developed on the effects of mixer designs, forms of chaotic motion, viscosity ratios, compositions, etc. There is still a need to produce apparatus and methods that produce good distributive and dispersive mixing of systems, such as filled polymer or polymer-polymer systems. There is also a need for these systems to be usable on a small scale and provide high yields. See also WO 2007/095036.

[0009] This invention provides methods and apparatus for the formation and testing of blended materials by effectively utilizing a certain combination of steps or structures. The invention can be used to make known materials or new materials.

SUMMARY OF INVENTION

[0010] Briefly, therefore, the present invention is directed to a four-rotor mixer and methods for blending materials using the mixer. The four-rotor mixer is a system that can heat, mix, and extrude multi-component chemistry systems of materials, such as polymers and additives (fillers, pigments, catalysts, etc.) optionally with automation and under software control. The system has the ability to mix and extrude different total volumes of mixtures i.e. 1-1000 ml. The device has gas and vacuum ports to evacuate and add gasses. The mixing and extrusion process are optionally automated. The device can be configured in a parallel arrangement utilizing multiple devices. [0011] The present invention is its various embodiments provides all of some of the following benefits: it provides the ability to monitor mixing during the mixing process to monitor and/or adjust blend properties to a predetermined level (including characterizing the morphology of the blend, characterizing the composition of the blend, and/or screening the blend for at least one property of interest), it provides the ability to adjust blend compositions to commercially significant properties (such as cost), it provides the ability to perform reactive chemistry in a mixing module, it provides customized mixing protocols, it provides for complete flexibility for mixing protocols, and it provides for mixing of variable material volumes (including volumes that change during mixing). [0012] Therefore, the invention is directed toward an apparatus for blending two or more materials, the apparatus comprising: a body defining a chamber for blending the materials, the body comprising a first end comprising an inlet for introducing materials into the chamber and a second end; a base located on the second end of the body; comprising four rotary element throughbores; four rotary elements configured for rotation and linear movement within the chamber for blending the materials and configured for movement into and out of the chamber through the rotary element throughbores of the base; a rotary assembly adapted to rotate each of the four rotary elements independently from each other; a linear actuation assembly adapted to linearly move each of the four rotary elements independently from each other through the throughbores; an outlet in selective fluid communication with the chamber through which materials are removed from the chamber; and a by-pass valve in fluid communication with the outlet that provides an optional flow path for materials exiting the chamber.

[0013] Also, the invention is directed to an apparatus including a body defining a chamber for blending the materials, a system for introducing or removing gases from the chamber, the system comprising a gas channel in the body and a gas pin channel located in the body and in selective fluid communication with the gas channel and in fluid communication with the chamber, wherein the gas channel and the gas pin channel are located relative to each other (e.g., at about 90 degrees), and wherein a gas pin located in the gas pin channel, is configured to move between a first and a second position to open and close gas flow between the chamber and the gas channel, and four rotary elements configured for rotation and/or linear movement within the chamber for blending the materials.

[0014] Optionally, the apparatus for blending two or more materials where the apparatus includes a body constructed of a transparent material defining the chamber for blending the materials and four rotary elements configured for rotation within the chamber for blending the materials. The transparent body allows for an analysis assembly to view the materials in the chamber while mixing.

[0015] Also optionally, the apparatus includes i)a cylindrical body defining a cylindrical chamber for blending the materials, where the body includes a first end comprising an inlet for introducing materials into the chamber and a second end, ii)a base located on the second end of the body, including four rotary element throughbores, iii)four rotary elements configured for rotation within the chamber for blending the materials and configured for movement into and out of the chamber through the rotary element throughbores of the base, and iv)a pressurized seal in each rotary element throughbore of the base around each rotary element, to prevent materials from leaving the chamber through the rotary element throughbores. [0016] The invention is also directed to a method of blending at least two materials. The method includes providing an apparatus as described herein, providing a first material, providing a second material, delivering the first and second materials to the chamber and blending the materials in the chamber with the four rotary elements. [0017] Other features, objects and advantages of the present invention will be in part apparent to those skilled in art and in part pointed out hereinafter. All references cited in the instant specification are incorporated by reference for all purposes. Moreover, as the patent and non-patent literature relating to the subject matter disclosed and/or claimed herein is substantial, many relevant references are available to a skilled artisan that will provide further instruction with respect to such subject matter.

BRIEF DESCRIPTION OF THE DRAWINGS

[0018] FIG. 1 is a side view of an exemplary embodiment of an apparatus of the present invention.

[0019] FIG. 2 is a perspective view of an exemplary embodiment of a blending assembly of the present invention.

[0020] FIG. 3 A is a top view of an exemplary embodiment of a blending assembly of the present invention. FIG. 3B is a cross-sectional side view of the embodiment of FIG. 3 A. [0021] FIG. 4 is an illustrative top view of a blending chamber and rotor geometric configuration.

[0022] FIG. 5 A is a cross-sectional side view of an exemplary embodiment of a blending assembly of the present invention. FIG. 5B is a perspective view of an exemplary heated bottom block for use with the embodiment of FIG. 5 A. FIG. 5B is a perspective, exploded view of an exemplary embodiment of an outlet port and outlet port pin for use with the embodiment of FIG. 5 A. FIG. 5C is a cross-sectional side view of a sealing and bearing element for use in the embodiment of FIG. 5 A.

[0023] FIG. 6 A is a cross-sectional side view of an exemplary embodiment of a pressurized seal assembly for use in a blending assembly of the present invention. FIG. 6B is a perspective view of the embodiment of FIG. 6A without the base. [0024] FIG. 7 is an exploded perspective view of an exemplary embodiment of a blending assembly of the present invention. [0025] FIG. 8 is a cross-sectional side view of an exemplary embodiment of an extruder pin embodiment of the present invention. FIG. 8 A is a cross-sectional view of a by-pass valve and excess material flow path.

[0026] FIG. 9 A is a perspective view of an exemplary embodiment of a gas port pin of the present invention. FIG. 9B is a partial, cross-sectional top view of an exemplary embodiment of the gas flow system of the blending assembly in a closed position. FIG.

9C is a partial, cross-sectional top view of an exemplary embodiment of the gas flow system of the blending assembly in an open position.

[0027] FIG. 1OA is a cross-sectional side view of part of an exemplary embodiment of a rotor assembly. FIG. 1OB is a perspective view of the embodiment of FIG. 1OA.

[0028] FIG. 1 IA is a perspective view of an exemplary embodiment of a rotary and linear actuation assembly of the present invention. FIG. 1OB is a cross-sectional side view of the rotor actuator assembly of the embodiment of FIG. 1OA, showing only one rotor assembly. FIG. 11C is a side view of the embodiment of FIG. 1 IB.

[0029] FIG. 12 is a perspective view of an exemplary embodiment of a linear actuation assembly of the present invention.

[0030] FIG. 13 A is a perspective view of an exemplary embodiment of a plunger assembly of the present invention. FIG. 13B is a top view of the plunger assembly of

FIG. 13 A placed over a blending assembly in place for blending. FIG. 13C is a top view of the plunger assembly of FIG. 13 A over a blending assembly retracted for access to the chamber of the blending assembly. FIG. 13D is a cross-sectional side view of an exemplary embodiment of the present invention showing a plunger collar disengaged with a mixer body. FIG. 13E is a cross-sectional side view of an exemplary embodiment of the present invention showing a plunger collar engaged with a mixer body.

[0031] FIG. 14 is a cross-sectional side view of an exemplary embodiment of the present invention.

[0032] FIG. 15 is a perspective view of an exemplary embodiment of the present invention, with FIG. 15A being a top view and FIG. 15B being a bottom view.

[0033] FIG. 16 is a top view illustration for rotor numbering in the blending chamber for the explanation of blending modes in FIGS. 17-19.

[0034] FIG. 17 is a chart displaying exemplary rotary blending modes of the present invention.

[0035] FIG. 18 is a chart displaying exemplary time periodic motion blending modes of the present invention. [0036] FIG. 19 is a chart displaying exemplary linear blending modes of the present invention.

[0037] FIG. 20 is a perspective view of an exemplary embodiment of a system of the present invention.

[0038] FIG. 21 is a perspective view of an exemplary embodiment of a system of the present invention.

[0039] FIG. 22 is a perspective view of an exemplary embodiment of a system of the present invention.

[0040] FIGS. 23A-23M are timed photographs of the Example.

DETAILED DESCRIPTION OF THE INVENTION

Detailed Description Of Preferred Embodiment

[0041] The present invention provides an apparatus and method for the research and development of commercially attractive blend materials, including the steps of: a. Providing a body defining a chamber and four rotary elements; b. Providing a first material; c. Providing a second material; d. Delivering the first and second materials to the chamber; and e. Blending the materials in the chamber with the four rotary elements [0042] The method can further include characterizing the morphology of the blend, characterizing the composition of the blend, screening the blend for at least one property of interest, or a combination thereof.

[0043] As used herein the term "blend" shall refer to a macro scopically homogeneous mixture of at least two chemically or physically different materials. In a preferred embodiment, but not necessarily required in the practice of the present invention, at least one of the materials is a polymer ("polymers" shall encompass homopolymers, copolymers, oligomers, co-oligomers, polymer blends or the like). Blends herein may be homogeneous, or otherwise include at least two materials that are substantially miscible and compatible relative to each other for a given condition. Blends may be heterogeneous or otherwise include at least two materials that differ in form, composition, processability, surface characteristic, diffusion, morphology, phase separation behavior, or some other characteristic that renders the materials immiscible but compatible relative to each other. Blends of the present invention may be mono- phase or may take any of a number of different multi-phase forms, examples of which include lamellar, dispersions, composites with other polymers, interpenetrating networks, or the like. Blends may also include polymer alloys that include a modified interface between polymers. The different materials in a blend need not be compositionally distinct to form a blend; however, blends will, in most instances, include at least two materials of different architecture.

[0044] In one embodiment, the method of the present invention is employed as part of a research and development program for the discovery or optimization of materials that are made in bulk quantities (e.g., greater than about 10 kg, more preferably greater than about 100 kg, still more preferably greater than about 1000 kg, and still more preferably greater than about 10,000 kg), such as that amount sufficient for meeting commercial or industrial demands.

[0045] As the following will illustrate, the invention involves various aspects that, independently or in combination, may contribute to this result, or conversely, the elimination during research and development of certain materials from consideration for bulk production. For example, in one aspect, the present invention is directed toward methods for the physical mixing of two or more materials for forming a blend composition. Further aspects will be ascertainable from review of the discussion herein. As will be appreciated, some of the apparatus and methods disclosed herein may be employed for either or both of forming a blend of a plurality of different materials by mixing or forming material samples of one material or a plurality of different materials. Thus, discussion herein of a method in one context is not intended to exclude application of the method in another context. Further, it will be appreciated that material samples or blends prepared in accordance with the methods herein may be subjected to additional art-disclosed processing techniques, such as thermal exposure, surface treatment or the like.

[0046] One feature of the present invention is the ability to employ the methods for the preparation of miniature scale material samples, thereby enabling rapid throughput analysis and cost-effective use of equipment, materials and other resources. [0047] The present invention may be useful for forming and screening combinatorial libraries chosen from a wide variety of materials, including but not limited to, metals, ceramics, composites, organic materials, inorganic materials, flocculated materials, colloids, non- volatile materials, soluble materials, combinations thereof and the like.

Other materials appropriate for combinatorial research may include, for instance, catalysts, products of various polymerization reaction conditions, lubricants, gels, adhesives, coatings and/or products of new post-synthesis processing conditions. Materials appropriate for combinatorial research according to the present invention may be also selected from foodstuffs, cosmetics, beverages, lotions, creams, pharmaceuticals, inks, body fluids, fuels, additives, detergents, surfactants, shampoos, conditioners, other hair styling products, dyes, waxes, fuel cell electrolytes, photoresist, semiconductor material, wire coatings, or the like.

[0048] According to one highly preferred aspect, though applicable to other materials, the present invention has been found particularly useful in connection with the processing and testing of, amongst other materials, polymeric materials or blends including the same. In this regard, the present invention can be employed to investigate any of a number of different types of materials including homogeneous blends, heterogeneous blends, interpenetrating networks, copolymers, composites, or other materials. Preferably, the blends will include a first material and a second material, one or both of which may be polymers. The blends need not be homogeneous materials or homogeneous polymer materials, and may include, for instance, organic or inorganic constituents. Further, the blends may be of non-polymers, inorganic materials, organic materials, biological materials, pharmaceutical compounds and polymorphs thereof, salts of small organic molecules or other non-biological or biological materials. [0049] Without intending to be limited thereby, the present invention is contemplated for use in connection with research or other activities addressing thermoset polymers, thermoplastic polymers, or mixtures thereof. The polymers also may be thermosets that become crosslinked. For example, among the popular industrial polymers for which the present invention is useful are polymers selected from one or more types of polymers including, for example, polyolefins (e.g., polyethylene, polypropylene, polyethylene terephthalate, or the like), vinyls (e.g., polyvinyl chloride), polyamides (e.g., NYLON®), polyimides, polyurethanes, acrylics, polyesters, celluloses, acetates, melamines, thermoplastic rubbers, thermosetting rubbers, fluorocarbons (e.g. PTFE or TEFLON ®), polystyrenes, nitriles, phenolics, polycarbonates, epoxies, A.BS, polyethylene ether ketones, acetals, or otherwise. The polymers may be high molecular weight, medium molecular weight, low molecular weight, high density (HD), low density (LD) or medium density (MD), conductive polymers, insulative polymers, ionomers or the like. [0050] Examples of other polymeric materials may include various polyolefin resins, mixtures of polylefins with other thermoplastics, mixtures of polyethylene (e.g., LDPE, VLDPE, or HDPE), polypropylene, ethylene/α-olefin copolymer, and/or polybutene-1 with ethylene alkyl (meth)acrylate copolymers, ionomers, nylon and polycarbonates. Other particularly attractive materials may include, for example, a polyolefm selected from poly(4-methylpentene- I)(PMP), 4-methylpentene-l (4-MP-l)/decene-l copolymer, polybutene-1 (PB), ultra-high molecular weight polyethylene, high density polyethylene or combinations thereof.

[0051] In some instances, it is possible that the polymer materials prepared or analyzed in accordance with the present invention may be substantially pure; that is consisting essentially of its constituent polymers. However, the present invention also lends itself well to the preparation and analysis of polymer materials that include additional ingredients, such as additives (e.g., light or temperature stabilizers, performance enhancers, biocides, fungicides, flame retardants, impact modifiers, foaming agents, or the like) colorants, reinforcements (e.g., fibers, particles, rovings, mats, foams, or the like, which may be any suitable composition such as carbon, aramid or otherwise). [0052] In general, though one aspect of the present invention contemplates rapid formation, synthesis and/or characterization of individual material samples in isolation, the method and system of the present invention also contemplates forming a library of a plurality of the same or different materials using rapid-serial synthesis techniques, parallel synthesis techniques or a combination thereof. In the formation of libraries in accordance with the present invention, one or a plurality of ingredients may be selected to form a desired material or may be selected to explore a compositional or process parameter range or phase space potentially useful as a desired material. [0053] It will be appreciated that materials also contemplate different materials having the same composition, such as isomers, polymorphs, or being selected of different molecular weights, polydispersities, weight distributions, chain branching or the like. It will also be appreciated that many parameters can be altered to produce a wide range of materials, such as the number of different component ingredients, the relative amounts of each component, the co-monomer content of a component, the nature and extent of chain branching or the like. The component ingredients may be the product of a single reactor or plural reactors (e.g., a tandem, serial reactor for producing bimodal molecular weight distribution polymers).

[0054] According to one aspect, the present method contemplates the use of the apparatus of the present invention for mixing at least two materials together to form a blend. In one embodiment, in general, two or more materials are provided and energy is applied to physically bring the materials together as the blend. How the energy is applied,and the means for minimizing the amount of energy necessary is specifically discussed herein. Typically, the energy is applied by a mechanical mixing, and more preferably by mixing that imparts shear flow, elongational flow or a combination thereof to the mixed materials. Examples of such mixing include, rotary mixing, periodic mixing, linear mixing and combinations thereof utilizing four rotary elements. The starting materials may be provided in any suitable form. For example, they may be provided as a block, a plate, a bale, a sheet, a rod, a fiber, a powder, a pellet, a fine particulate, a granule, a solution, a fluid, a gel, a melt, an emulsion or dispersion or the like.

[0055] Blending may take place at any suitable temperature. In one aspect of the present invention, in the context of a polymer containing material, it is preferred that any mechanical mixing occurs at or above the glass transition temperature (and more preferably at or above the melting point) of at least one and preferably all of the polymer materials being mixed.

[0056] Referring to Figure 1, there is illustrated one embodiment of an apparatus of the present invention. The apparatus includes an optional plunger assembly 100, a mixing assembly 102, a mixing element rotary actuation assembly 104, and an optional mixing element linear actuation assembly 106. Each assembly will be discussed in more detail below. Figures 2-9 discuss various aspects of the mixer assembly 102 shown in Figure 1. [0057] Figure 2 shows a perspective view of one embodiment of the mixer assembly 102 of the present invention. The mixing assembly generally includes a body 200 which defines a chamber 202 in fluid communication with an inlet 204 through which materials are introduced to the chamber 202 in which materials are blended via four or more rotary elements (not shown). The chamber can be configured so that materials are introduced and removed from the chamber through the inlet 204. The assembly can also include an outlet 206 in selective fluid communication with the chamber 202, separate from the inlet 204, through which materials are removed from the chamber 202 after blending. As shown and further discussed in connection with Figure 8, the outlet 206 is opened and closed via an outlet actuator 208. The mixer also optionally includes a chamber gas port 300 (shown in Figure 9) in selective fluid communication with the chamber 202 for introducing a gas, such as an inert or reactive gas, to the chamber 202, or for removing gas from the chamber 202. As discussed in Figure 7, the gas port is opened and closed via a gas port actuator 210. The assembly also optionally includes a base gas port 212 for introducing a gas into a sealing element to pressurize an area of sealing around the rotary elements to aid in sealing the point of entry of the rotary elements into the chamber 202. This aspect is shown in more detail in Figure 6. The assembly also optionally includes a base element 214, which supports the body 200 and can also provide the outlet 206 and the gas port 212 for the sealing elements. [0058] The volume of the chamber 202 is not critical. In one embodiment, the volume is less than 1 liter, more specifically less than 500 ml, more specifically, less than 250 ml, more specifically, less than 100 ml, more specifically, less than 50 ml, more specifically, less than 25 ml, more specifically, less than 20 ml, more specifically, less than 10 ml, and even more specifically, less than 5 ml. In another embodiment, the volume is between about 1 ml and 1 liter, more specifically, between about 1 ml and 500 ml, more specifically, between about 1 ml and 250 ml, more specifically, between about 1 ml and 100 ml, more specifically, between about 1 ml and 50 ml, more specifically, between about 1 ml and 25 ml, more specifically, between about 1 ml and 10 ml, and even more specifically, between about 1 ml and 5 ml.

[0059] The shape of the cavity is not critical. In one embodiment, the chamber 202 is a cylindrical cavity.

[0060] In one embodiment, the body is configured to operate at temperatures between about -20⁰C and 400⁰C, more specifically between about 0°C and 300°C, more specifically between about 50°C and 300°C, more specifically between about 100⁰C and 300°C, and even more specifically between about 150°C and 300°C. In another embodiment, the body is configured to operate at temperatures above about 100°C, more specifically above about 150°C, more specifically above about 200°C, more specifically above about 250°C, more specifically above about 300°C, and even more specifically above about 350°C. In one embodiment, this is accomplished using a heating element around the body 200, such as a band heater 216. In other embodiments, the body 200 can be placed in a heating or cooling chamber, such as an oven, or freezer or can have heating or cooling elements embedded within the body 200.

[0061] The body 200 can be constructed of materials suitable for operating at the desired operating temperatures and which are typically inert with respect to the materials being blended. Such materials include, but are not limited to, various grades of steel, such as stainless steel and hastaloy, titanium, aluminum, polyether ether ketone, glass, quartz, ceramics, and other like materials that will be recognized by those of skill in the art. [0062] In one embodiment, the chamber 202 can include a sensor or an array of different sensors used individually or simultaneously (not shown) for detecting various properties of the chamber or material, such as a liquid level sensor, pressure sensor, temperature sensor, and/or electrochemical sensors for detecting toxic and/or corrosive byproducts. [0063] Figure 3 A shows a top view of one embodiment of the present invention, and Figure 3B shows a side cross-sectional view of the embodiment of Figure 3 A. Figure 3 A shows one location for a gas port 300 for introducing or removing gases from the chamber 202 through the body 200. The mixer assembly of the present invention includes at least four rotary elements. In the embodiment shown in Figures 3 A and 3B, the rotary elements are preferably vertical cylinders 302, (rotors or pins), that are at least partially within the chamber 202. The rotors 302 can be introduced into the chamber 202 through the base 214 as shown in Figure 3B, or can be introduced into the chamber 202 through the inlet 204. Introducing the rotors 302 through the base 214 is advantageous in embodiments that include a plunger assembly 100. In those embodiments, it may be desirable to have the rotors 302 configured such that they are able to be moved into and out of the chamber 202 either during blending or prior/subsequent to blending. One blending mode, which will be discussed below, includes moving the rotors 302 into and out of the chamber 202 during blending. Also, in embodiments in which a plunger assembly 100 is utilized, it could be desirable to be able to retract the rotors out of the chamber 202 as a plunger is introduced towards the bottom of the chamber 202. For those embodiments in which the rotors 302 are introduced at least partially into the chamber 202 through the base 214, the base 214 includes a bore 304 for each rotary element 302 to pass through into the chamber 202. Each bore 304, optionally includes a seal 306 to prevent material in the chamber 202 from passing through the bore 304 either during blending or as the rotors 302 are at least partially retracted from the chamber 202. [0064] The geometry of the chamber 202 and rotary elements 302 can be configured to provide good dispersive and/or distributive mixing. In one embodiment as shown in Figure 4, where the rotary elements A B C and D are cylindrical rotors inside a cylindrical chamber 202, the rotary elements 302 in the chamber are designed to have a height (hi) and a radius (R₁) (R_1A5Ri_B, Ric and R₁D respectively). The chamber 202 is designed to have a radius (R₀) and a height (h₂). When in the chamber 202, each rotor 302 has a respective distance from the center of the chamber 202 to the center of the rotor (d_l5 d₂, d₃ and (U) and a shortest distance from the edge of the rotor 302 to the chamber wall (X₁, x₂, X₃ and X₄, respectively). The shortest distance between the edge of two rotors is designated y_Aβ, yAc, Y_AD, YB_C, YBD and V_CD- In one embodiment, di, d₂, d₃ and d_i are equal. In another embodiment R₁AjRiB, Ric and R₁D are equal. In another embodiment, R_1A5RiB, Ric and R,_D, are all different, in another embodiment, two rotors have the same R, and the other two rotors have an equal R; different from the Ri for the other two rotors, and in another embodiment, one rotor has an R₁ different from the R₁ of the other three rotors, which have an equal R₁. In another embodiment X₁, x₂, x₃ and x₄ are equal. In another embodiment, the ratio of hi :h₂ is between about 1 : 10 to about 9.9:10, more specifically between about 1 :2 to about 4:5. One of skill in the art will recognize that different geometries and ratios are possible to optimize the system by eliminating stagnation zones, maximizing elongational and shear flows and combinations thereof for various mixing systems, depending on temperature, viscosities, etc. [0065] In one embodiment, the four rotary elements are a first rotor, a second rotor, a third rotor and a fourth rotor, and are arranged in an array such that the first and third rotors have a first center-to-center distance between them, the second and fourth rotors have a second center-to center distance between them equal to the first center-to center distance, the first and second rotors have a third center-to-center distance between them that is less than the first center-to center distance, the first and fourth rotors have a fourth center-to-center distance between them that is less than the first center-to center distance, the second and third rotors have a fifth center-to-center distance between them that is less than the first center-to center distance, and the third and fourth rotors have a sixth center- to-center distance between them that is less than the first center-to center distance. Specifically the rotary elements are in a square configuration, meaning the third center-to center distance, the fourth center-to center distance, the fifth center-to center distance, and the sixth center-to center distance are equal.

[0066] Figure 5 A shows one embodiment of a mixer assembly in which the assembly is heated using a cartridge heater 500 or other type of heating element embedded in the body 200 and/or a bottom heating element 502 for heating the base 214. The bottom heating element 502, which is shown in Figure 5B, can be a separate piece from the base 214 and be connected to the base, or can be can be the same piece as the base 214. The outlet 206 can have a threaded end 504 and includes a removable pin 506, shown in Figure 5C, which engages the threaded portion 504 for closing off the outlet 206 during blending, and can be removed in order to remove blended material from the chamber 202. The sealing element 306 includes a wiper seal 508 that surrounds the rotor 302 in the bore 304. As shown in Figure 5D, the seal is held in place by a spacer 510 located between the seal 508 and a bearing 512.

[0067] An embodiment shown in Figures 6 A and 6B is the sealing element 306 for the rotors 302 in the bores 304 is a pressurized double seal. The pressurized double seal includes two lip seals 600, 602 separated by a spacer 604. The spacer includes a channel 606 which is in fluid communication with a gas inlet channel 610 which is fed by the base gas port 212. In one embodiment, the two lip seals 600, 602 and spacer 604 are held on a retaining plate 608 as shown in Figure 6B. The retaining plate 608 includes the sealing elements for all four rotors and is engaged with the base 214 as shown in Figure 6 A. In another embodiment, the seals are retained by the base 214. The gas inlet channel 610 and optionally a seal connection channel 612 are integral with the base 214. In one embodiment, when the seals are engaged with the base 214, two of the sealing elements are in fluid communication with one gas channel 610 and port 212. Thus, there are two gas channels 610 and ports 212, one for each set of two seal elements, hi another embodiment, there is one gas channel 610 and port 212 for each sealing element. In another embodiment, one channel 610 and port 212 feeds all four seal elements. In operation, a gas is fed through the channels 610 and 606 engaging the lip seals 600, 602 against the base 214 and creating a pressurized seal environment. As can be seen in Figures 6A and 6B, in one embodiment, it is preferable to mount the seals 600, 602 with what would be considered the front faces facing each other, so that when pressurized, there exists little if any dead volume for material to accumulate in the area between the seal element and the chamber 202.

[0068] Figure 7 shows an exploded view of an embodiment where a band heater 216 is used to heat the body 200 and chamber 202. It has been found that in embodiments where the blended materials leave the chamber 202 through a chamber outlet 708 in the base 214, the materials can lose heat traveling through the base 214, which can cause problems if the material solidifies or becomes too viscous to flow well. Thus, it is desirable to heat the base 214 so that materials being sent from the chamber outlet 708 to the assembly outlet 206 in the base 214 are maintained at a desirable temperature, such as above the glass transition temperature, and preferably above the melting point. This can be accomplished with a base heating element as shown in Figure 5B. In other embodiments, as shown in Figure 7, a heating element, such as a mica heater 700 can be used to heat the base 214. In the embodiment shown, the heater 700 has a first surface in contact with the base 214 and a second surface in contact with a piece of heater ceramic paper 702. The paper 702 and heater 700 are held against the base 214 using appropriate fastening elements, such as a clamp 703, which can be fastened to the base 214, holding the heater 702 in place. The assembly can also optionally include thermocouples 704 for monitoring the temperature in the base 214, the body 200 and/or the chamber 202. The base 214, in one embodiment, includes bores 304 for the rotors, the assembly outlet 206, and a base sealing element 706, such as an O-ring, for sealing the connection of the body 200 and the base 214. For higher pressures, other sealing elements will be apparent to those of skill in the art.

[0069] Figure 8 shows an enlarged view of an embodiment for maintaining materials in the chamber 202 during blending and removing materials from the chamber 202 using an exit pin 800. In one embodiment, an exit pin 800 is set into an outlet channel 802, such that it blocks or closes off the chamber outlet 708 during blending. When removing the material from the assembly, the exit pin 800 is pulled back by a driving element, such as a linear actuator 208, essentially opening the chamber outlet 708. Material is forced through the chamber outlet 708 and into an outlet channel 802 via a plunger 1300 which drives into the chamber from the inlet towards the outlet. As material is forced into the outlet, it passes through the outlet channel 802 and out of the assembly outlet 206 of the base 214. When the plunger reaches the bottom of the chamber 202, all of the material is either in the outlet channel 802, or has passed out of the assembly. In order to remove the material from the outlet channel 802, the exit pin 800, connected to the driving element, such as a linear actuator 208 is driven through the channel 802 pushing the remaining material out of the outlet 206 of the base 214. This provides very high yields of blended materials, which can be very important when materials are being investigated on a small scale or are expensive.

[0070] Figure 8 A shows an embodiment of a system that includes a by-pass valve 810 in fluid communication with the outlet 206 that generally resides between the outlet 206 and a mold or other container 850 that receives the material contents from the chamber. The by-pass valve 810 includes a flow path 811 and a valve 812 that allows material that may not physically fit into the mold or other container 850 into a container. The by-pass valve provides the ability to mix materials of unknown volume or materials that may change volume during mixing (such as during reactive mixing). The by-pass valve also aides in packing of the materials into the mold. One can vary the pressures seen the in mold cavity by changing the size of the exit hole on the by-pass valve body. Typically, the valve 812 is controlled by the software that controls the overall system, and can allow for controlled or fully open or completely closed flow through the by-pass flow path 811.

[0071] Figure 9 shows an embodiment of a system for introducing gas to or removing gas from the chamber 202. Generally, introduction or removal of gases into a mixing chamber as described herein is counter-intuitive to those of skill in the art because an additional port in the mixing chamber provides a leak path and increases the size required of the chamber (to accommodate the port). The port provides the ability to perform reactive chemistry in the chamber. Figure 9A shows the gas pin, Figure 9B shows the gas pin in a closed position, and Figure 9C shows the gas pin in an open position. In one embodiment, gas is fed to or removed from a chamber gas port 300 via a gas channel 902 in the body 200. A gas pin channel 904 is located in the body 200 and is in selective fluid communication with the gas channel 902 and in fluid communication with the chamber 202. In one embodiment, as shown in Figures 9B and 9C, the gas channel 902 and the gas pin channel 904 are located at about 90 degrees relative to each other, and the gas pin 900 located in the gas pin channel 904, moves between first and second position to open and close the gas flow between the chamber 202 and the chamber gas port 300. In one embodiment, the gas pin is a cylindrical pin having a first section 906 with a first radius and a second section 908 having a second radius smaller than the first radius. The gas pin channel 904 also has a first section 910 and a second section 912, designed to accommodate the gas pin as shown. The gas pin 900 is supported in the gas pin channel 904 by a spring 914 and a seal 916, such as an O-ring which is held into the body 200 by a retaining element 920. The spring 914 biases the gas pin 900 into a closed position as shown in Figure 9B. To open the channel, a driving element, such as a linear actuator 210 drives the pin forward into position as shown in figure 9C. The gas pin 900 has a channel 918 in the second section 908 that engages the gas channel 902 when in the open position and allows gas to flow between the gas channel 902 and the chamber 202. The gas pin is designed to allow the flow of gas into and out of the chamber 202, and essentially prevents solids from leaving the chamber 202.

[0072] The invention includes at least four rotary elements and an assembly for rotating and optionally linearly moving the elements, individually or together, in the mixing assembly. In one embodiment, as shown in Figures 1OA and 1OB, the rotary elements 302 are vertical cylindrical shafts, or pins, that are supported by one, and preferably two bearings 1000 in a bearing block 1002. One bearing 1000 is sufficient for embodiments in which the rotors 302 only rotate. In embodiments in which the rotors also linearly move into and out of the chamber 202, such as through wiper seals, two bearings 1000 facilitate rotational and linear stability to the rotor 302, although other designs will be apparent to those of skill in the art. The bearing block 1002 is attached to a support 1006, and the rotor 302 is connected to a linear actuator, either directly, or through couplings 1004, such as universal joint couplings and flex couplings. In one embodiment, the bearings 1000 are constructed of sintered bronze, which helps reduce friction at the joint. Other friction reduction designs will be understood by those of skill in the art.

[0073] The rotary elements (e.g., pins) are preferably driven by a suitable motor, and in one embodiment, a suitable controller or suitable software is employed for controlling and varying rotation speed as desired, e.g., up to about 1000 rpm, more specifically up to about 800 rpm, more specifically up to about 600 rpm, more specifically up to about 400 rpm, and still more specifically up to about 200 rpm. In one embodiment, the rotation speed is controllable by the user and through input based upon library or material sample design criteria that has been inputted. A suitable axial load measurement device, torque measurement device or both can be also employed for providing feedback to the user about processing conditions. Feed back can also be obtained as the condition of the joint assembly, such as high current draw that might indicate a linear or rotary drive issue. [0074] Figure 1 IA is a perspective view of one embodiment of the rotary and linear actuation assembly, and Figure 1 IB is a partial cross-sectional view of the embodiment showing the rotary assembly 102 and one rotor 302 and actuator of the assembly. In the embodiment shown, the rotors are designed to be used in a small chamber 202, such that the rotors 302 may be in close proximity to each other (as described elsewhere herein). Due to size constraints, the rotary actuators 1100 are set at an angle with respect to the rotors 302. Various types of couplings 1102 and joints can be utilized to connect the rotary actuator 1100 with the rotor 302. In one embodiment, the rotary actuator is a motor having appropriate gear head ratios to attain the desired rotational accelerations, speeds and torques. In one embodiment, a motor support 1101 supports each actuator 1100 and a rotary actuator assembly pillar 1103 acts as a linear guide for each rotary actuator 1100 to help keep the rotary actuation assembly in line as it is driven linearly. [0075] In one embodiment, the rotational actuator assembly 104 is coupled to the linear actuation assembly 106 to provide linear movement of the rotors 302 within the chamber

202. hi one embodiment, the linear drive assembly 106 includes a connection element 1104 that connects the linear actuator assembly 106 with the rotary actuator assembly 104, such as with a rod 1104 that connects to the motor support 1101 with appropriate fastening means, such as a connection pin 1106. The linear actuation assembly also optionally includes a pair of optical limit switches 1108 for defining maximum and minimum linear movement. An example of the linear actuation assembly is shown in Figure 12. In one embodiment, the linear actuators are roller screw type elements directly connected to motors.

[0076] In the embodiment described, there is one rotary actuator and one linear actuator for each rotary element 302. This provides individual control of speed, acceleration, rotary direction and linear movement of each rotary element. In other embodiments, it may be desirable to have one actuator control two rotary elements or all four rotary elements.

[0077] Figure 13 A shows an embodiment of the plunger assembly 100. The plunger assembly 100 includes a plunger 1300 designed to fit into the chamber 202 of the mixer through the inlet. Specifically, the plunger 1300 is designed to seal the chamber 202, by being shaped to fit tightly into the chamber 202 and through the use of sealing elements that interact with the walls of the chamber 202, such as O-rings 1312. The assembly also includes a driving element 1302, such as a linear actuator, for moving the plunger 1300 into and out of the chamber 202, a support 1306 for holding the assembly in an elevated position over the mixing apparatus 102, and a slide table 1304, configured to move the plunger 1300 over the mixer assembly to engage the chamber 202, and away from the mixer assembly such as for cleaning or loading the chamber 202 with materials. A top view of the plunger assembly 100 in a position to engage the chamber 202 for mixing is shown in Figure 13B, and a top view of the plunger assembly 100 in a retracted position to enable access to the chamber 202, is shown in Figure 13C.

[0078] Figures 13D and 13E show an embodiment which utilizes a plunger collar 1310 that interfaces with the inlet of the chamber 202 to provide additional sealing of the chamber 202. The collar 1310 is attached to the plunger shaft via a return spring 1314, and engages the body 200 at the inlet as the plunger is driven into the chamber. If the sealing element on the plunger head (such as an O-ring) is compromised, the interfacing surfaces of the collar 1310 are held tightly against the body to effectively seal the chamber 202. The design of the collar is not critical but should be designed so that it can form a seal when engaged with the body. For example, in Figures 13D and 13E, the inlet of the body is chamfered and the collar 1310 is designed in such a manner as to engage the chamfered inlet and seal the chamber 202. The collar 1310 can be constructed of any material suitable for forming a seal when engaged with the body 200. In one embodiment, the collar 1310 is constructed of a first material 1316 to form the collar body, and a second material 1318, such as rubber, for forming a seal with the body 200. Figure 13D shows the embodiment with the collar 1310 disengaged from the body 200. Figure 13E shows an embodiment with the collar 1310 engaged with the body 200. [0079] In one embodiment it may be desirable to visually observe the blending while using a plunger. A transparent plunger (not shown) such as constructed of a material suitable to the temperature of blending, such as borosilicate, glass, quartz or acrylic can be used and manually pressed into the chamber 202 to provide an essentially sealed environment, allowing a direct overhead view into the chamber 202 during blending. [0080] Figure 14 illustrates an embodiment of engagement of the plunger 1200 with the chamber 202. After loading of materials into the chamber 202, the plunger engages the chamber 202, sealing the chamber 202. In one embodiment, after mixing, the rotors are retracted using a linear actuator assembly 106, and the plunger 1200 is driven into the chamber 202 to force the blended material out of the outlet 206. When the plunger 1200 reaches the bottom of the chamber 202, an extruder pin can drive the remaining material out of the outlet 206. The plunger can also include an adjustable tip. [0081] Figure 15 illustrates an embodiment of a system in which no plunger assembly 100 or linear actuation assembly 106 is used. This embodiment includes a mixing assembly which includes a body 200 defining a chamber 202 which is open at the top 1500 where materials can be added and removed from the system. The rotor and rotary actuation assembly includes at least four rotary elements 302, such as rotors driven by actuators 1100, such as DC motors. The rotary elements 302 are introduced to the chamber 202 through the opening 1500. In one embodiment, the assembly includes a bearing block 1502, which includes bearings 1506 through which the rotors 302 pass. The bearing block 1502 acts to hold the rotors 302 in a specific spatial relationship and acts as a top to the chamber 202 when brought into contact as shown in the figure. The bearing block 1502 also optionally includes grooves 1504 for moving the rotors 302 to provide different configurations for blending. In one embodiment, the body 200 is constructed of a transparent material, such as borosilicate, glass, quartz or acrylic. This allows for visual monitoring of the blending in order to observe the various real-time effects of rotor configurations and material properties, such as viscosity. This embodiment can also optionally include a linear actuation assembly (not shown) for moving the rotors linearly within the chamber 202. This embodiment can also include a plunger assembly designed to seal the chamber and provide access for the rotary elements into the chamber through the plunger assembly. Furthermore, it is within the scope of the invention that a body constructed of a clear material as described above can be implemented into the other various embodiments described herein. [0082] The rotary elements of the present invention can be configured and run in various ways to provide different modes of blending, as beneficially discussed herein. For illustrative purposes, the rotary elements 302, which in one embodiment are cylindrical shafts (cylinders or pins), will be designated by numbers 1 , 2, 3, and 4 by position for explanation of the various modes of operation. Figure 16 shows this designation. [0083] In one embodiment, as illustrated in Figure 17, during blending, the rotors can be run in a regular mode, meaning all 4 rotors (pins) are rotating at the same time for a blending period of time. The speed and direction can be varied from one rotor to another. In one embodiment, all four rotors rotate in the same direction (in phase) 1700. In another embodiment, rotors 1 and 3 rotate in a first direction, while rotors 2 and 4 rotate in a second direction 1702. In another embodiment, rotors 1 and 4 rotate in a first direction, while rotors 2 and 3 rotate in a second direction 1704. In another embodiment, rotor 1 rotates in a first direction, while rotors 2, 3 and 4 rotate in a second direction 1706.

[0084] In one embodiment, as illustrated in Figure 18, during blending, the rotors can be run in a time periodic mode, meaning that the rotors spin in pairs in separate or overlapping time periods during blending. The rotor pairings, directions, speed and time periods can be varied. In one embodiment, the rotors are grouped so that rotors 1 and 2 spin together during a first time period and rotors 3 and 4 spin together during a second time period 1800. In another embodiment the rotors are grouped so that rotors 1 and 3 spin together during a first time period and rotors 2 and 4 spin together during a second time period 1802. The first and second time periods can overlap or be distinct, such that one set of rotors stops before the second set starts. In either of these time periodic embodiments, the speed and direction can be varied from one rotor to another. In one embodiment, all four rotors rotate in the same direction (in phase) 1804. In another embodiment, rotors 1 and 3 rotate in a first direction, while rotors 2 and 4 rotate in a second direction 1806. In another embodiment, rotors 1 and 4 rotate in a first direction, while rotors 2 and 3 rotate in a second direction 1808. .In another embodiment, rotors 1 and 2 rotate in a first direction, while rotors 3 and 4 rotate in a second direction 1810. hi another embodiment, rotor 1 rotates in a first direction, and rotors 2, 3 and 4 rotate in a second direction 1812.

[0085] In one embodiment, as illustrated in Figure 19, during blending, the rotors can be run in a linear mode, meaning the rotors move linearly in the chamber 202 during blending to assist in vertical mixing of the materials. The rotor pairings, directions, speed (linear and rotational) and time periods can be varied. For example, as shown in Figure 19, in one embodiment, rotors 1 and 2 can be paired to move linearly together at the same rate and speed, and pins 3 and 4 can be grouped together to move linearly within the chamber 1900. In another embodiment, rotors 1, 2, 3 and 4 can move linearly together at the same rate and speed 1902. In another embodiment, rotors 1 and 3 can be paired to move linearly together at the same rate and speed, and pins 2 and 4 can be grouped together to move linearly within the chamber 1904.

[0086] Those of skill in the art will recognize, in view of the teaching above, that the various modes can be combined to create many different blending modes that include rotor direction, rotor speed, rotor acceleration, linear speed, linear acceleration, time periodic motion, pairing and linear movement. The above embodiments are illustrative and not intended to be limiting to all of the possible combinations of the various embodiments. The independent control of rotor direction, rotor speed, rotor acceleration, linear speed, linear acceleration, time periodic motion, pairing and linear movement is of great benefit in that the materials can be stopped from achieving steady state or allowed to achieve steady state. This control gives the benefit of morphology or other property tuning. However, this independent control would be counter-intuitive to those of skill in the art without the teachings herein in that the design is complicated for a small volume apparatus, as described herein.

[0087] Figures 20, 21 and 22 show different embodiments of the system for dispensing materials, blending materials, preparing the blended materials for analysis, and the like. In one embodiment, as shown in Figure 20, the system 2000 includes one or more blending apparatus 2002 and a dispensing apparatus 2004 (such as an articulated arm robot equipped with a vial gripper, or a three-axis robot for dispensing liquids or solids). Figure 21 shows a system for introducing powder samples (materials having a particle sizes between about 1 and 500 microns) to a blending apparatus 2100. The system includes a suitable powder dispensing apparatus, such as a Many- to-Many Powdernium (available from Symyx Technologies, Inc., Sunnyvale, California) 2104 which dispenses powder samples into vials, a balance 2106 for weighing samples and an articulated arm robot 2102 equipped with a vial gripper for transferring powder samples to the blending apparatus 2100. Figure 22 shows a system including sources 2200 of material samples (such as a liquid, powder or pellet in an array of vials), and a dispensing apparatus 2202 (e.g., an articulated arm robot equipped with a vial gripper, or a Symyx liquid dispensing robot) for transferring the material samples to a blending apparatus 2204 in which the material samples are brought into contact. By way of illustration, in one embodiment, a material is provided as a powder from one or more 20 ml vials 2206 (which optionally are integrated in a single structure, such as a microtiter plate). Materials to be blended typically include at least two components. The two components can be located in separate vials to be individually delivered to the blending apparatus 2204 for mixing, or alternatively, they can be combined beforehand into a single vial and be delivered together to the blending apparatus 2204. The system also optionally includes a balance 2208 for weighing the vials before delivery, after delivery, or both in order to determine the volume or weight of each material or combination of materials delivered to the blending apparatus 2204. After mixing, the blended material is optionally sent to a transfer vessel 2210 and to a mold 2212 in which the blended material is molded into a desired shape for characterization. Molding or shaping may be accomplished using any other art-disclosed molding technique, including but not limited to injection molding, solution film casting, capillary extrusion, or the like. Additionally, bulk shapes can be molded using art-disclosed techniques and then machined or otherwise processed to the final desired shape.

[0088] The dispensing apparatus 2004, 2102, 2202 may be operated manually. Preferably it is automated and is in controlling communication with a computer or other suitable programmable controller, and is directed to transfer samples in predetermined amounts and then to deliver the materials to the blending apparatus. For example, the dispensing apparatus will receive instructions from IMPRESSIONIST™ software, based upon information inputted by a user through LIBRARY STUDIO^®, where a library is initially designed (with system operational software being available from Symyx Technologies, Inc., Sunnyvale, California, e.g., EPOCH). [0089] Samples can be prepared for mixing by numerous methods that will be recognized by those of skill in the art. For example, in one embodiment, solid samples (such as in the form of pellets) can be ground in a device such as a freezer mill into a powder. The powder can be dispensed by a powder dispensing device (such as a Many- to-Many Powdernium, Symyx Technologies, Inc., Sunnyvale, California) into vials for delivery to the blending apparatus 106.

[0090] Once dispensed and blended, the resulting blended material can be obtained for analysis. For materials characterization, the samples may be formed in a variety of sizes and weights. For example, samples may be pressed by a vacuum press to thicknesses as low as about 0.1 micron to about 25 mm. Moreover, exemplary ranges of weights for samples include ranges of about 1 microgram to about 0.5 kilogram or about 1 mg to about 100 mg or about 10 mg to about 80 mg. Materials in accordance with the present invention can be analyzed for any of a number of its characteristics, including for instance chemical composition, morphology (including distribution and dispersion), physical property, decomposition, turbidity or other property of interest. [0091] The material made in accordance with the present invention lend themselves to any of a number of art-disclosed characterization techniques including but not limited to those employing beam radiation analysis, such as x-ray diffraction, high-throughput x- ray scattering, scattering from experimental systems, viscometry, failure or strength testing, adhesion testing, birefrigerance, rheo-optics, electron radiation, neutron radiation, sychotron radiation, or the like, infrared techniques (e.g., FTIR, IR detection or otherwise), thermal analysis techniques (such as differential scanning calorimetry, differential thermal analysis or the like), chromatographic techniques, resonance, spectroscopy, light scatter, spectrometry, microscopy, nuclear magnetic resonance, optical measurements, electrochemical measurements, and calorimetry, such as pyrolisis combustion flow calorimetry. By way of example, optical microscopy and image analysis can be used in combination to determine the material particle size distribution and dispersion, respectively. When the chamber is transparent, those characterization techniques that are useful through the transparent material may be used in a analysis assembly that views the materials in the chambers while mixing. [0092] Samples may also be analyzed using art-disclosed techniques, for any of a number of different physical properties, such as tensile strength testing, impact strength testing, tear resistance testing, density testing, tack testing, viscoelastic modulus testing, rheology testing, viscosity testing, bulge testing, probe perturbation testing, flexure testing, optical testing, hardness testing, melt index testing, flow index testing, glass transition testing, melting point testing, flow impedance testing, surface roughness testing, light scattering property testing, die swell testing, order-disorder transition temperature testing, order-order transition temperature testing, fluid permeability testing, electrical property testing (e.g., dielectric constant) or other testing. Other thermal or electrical properties may be analyzed such as conductivity, resistivity, or the like. [0093] Samples may also be analyzed for response to cyclic loading, solvent/chemical resistance, weatherability, or other conditions for simulating actual operating conditions for a particular application. In yet another embodiment, materials are analyzed for their recycleability attributes.

[0094] It is also expected that characterization may also be employed using other art- disclosed techniques, including optical microscopy, scanning electron microscopy, or other microscopy techniques.

[0095] Other examples of sample formation and characterizations for blended materials can be found in U.S. Patent 6,881 ,363, which is hereby incorporated by reference in its entirety.

[0096] Though manual methods are possible, in a particularly preferred embodiment, the preparation and analysis of material samples is performed in at least a partially automated manner, and is facilitated by the use of suitable software. Though it is possible that several functions may be combined into an integrated software package, it is anticipated that the software will likely be packaged as separate modules, or as a group of separate modules together in a suite. Though any suitable software may be employed, preferred software is that available from Symyx Technologies, Inc. (Sunnyvale, CA), under the designations identified parenthetically in the following discussion. [0097] In general, software is employed in at least the following processing:

1) designing an experiment, such as a library of samples (e.g., LIBRARY STUDIO™)

2) translating a library design into commands for directing robots or other instrumentation to prepare material samples and thereafter process them (e.g., IMPRESSIONIST™)

3) acquiring data about material samples in a library (e.g., EPOCH™); and

4) organizing and displaying material sample data for search or analysis (e.g., POLY VIEW™).

[0098] A more detailed discussion of the features and operation of sample preparation or processing software can be found in U.S. Patent Application Serial Nos. 09/420,334 (filed October 18, 1999); 09/174,856 (filed October 19, 1998); and U.S. Patent No. 6,507,945, incorporated by reference herein in their entirety. [0099] Further, it is also contemplated that any suitable commercially available software can be employed for storing and retrieving material sample data (e.g., database software available from ORACLE), correlating material sample data with information about a material sample or other material samples in a library, or both. For example, for each material sample, the information obtained preferably is inputted and stored into a computer, which can retrieve such information for subsequent analysis or comparison with other library members.

[0100] The accompanying Figures and this description depict and describe embodiments of the reactor system and method of the present invention, and features and components thereof. Fastening, mounting, attaching or connecting the components of the present invention to form the apparatus or device as a whole, unless specifically described otherwise, are intended to encompass conventional fasteners such as machine screws, nut and bolt connectors, machine threaded connectors, snap rings, clamps such as screw clamps and the like, rivets, nuts and bolts, toggles, pins and the like. Components may also be connected by welding, friction fitting or deformation, if appropriate. Unless specifically otherwise disclosed or taught, materials for making components of the present invention are selected from appropriate materials such as metal, metallic alloys, fibers, plastics and the like, and appropriate manufacturing or production methods including casting, extruding, coating, molding and machining may be used. [0101] Also part of this invention is an apparatus for blending two or more materials, the apparatus comprising: a cylindrical body defining a cylindrical chamber for blending the materials, the body comprising a first end comprising an inlet for introducing materials into the chamber and a second end; a base located on the second end of the body; comprising four rotary element throughbores; four rotary elements configured for rotation within the chamber for blending the materials and configured for movement into and out of the chamber through the rotary element throughbores of the base; and a pressurized seal in each rotary element throughbore of the base around each rotary element, to prevent materials from leaving the chamber through the rotary element throughbores. Also part of this invention is an apparatus for blending two or more materials, the apparatus comprising: a body constructed of a transparent material defining a chamber for blending the materials; and four rotary elements configured for rotation within the chamber for blending the materials. These inventions can be combined with any of the dependent claims as listed below. [0102] Any references herein to front and back, right and left, top and bottom, upper and lower and horizontal and vertical are intended for convenience of description only, not to limit the present invention or its components to any one positional or spatial orientation.

Such terms are to be read and understood with their conventional meanings. In the

Figures, elements common to the embodiments of the invention are commonly identified.

[0103] It is contemplated that various changes may be made without deviating from the spirit and scope of the present invention. Accordingly, it is intended that the scope of the present invention not be limited strictly to that of the above description of the present invention.

[0104] The following example illustrates the principles and advantages of the invention.

EXAMPLE

[0105] A viscosity standard (N270000, available from Canon Instrument Company) was combined with carbon black in an amount of 0.25% of the total weight to a blending apparatus of the present invention as shown in Figure 15, with the addition of linear actuation of the rotors. The viscosity standard was first manually added to the chamber, followed by the carbon black. The rotation speed for the rotors was set at 200 rpm, the rotational acceleration at 10 rev/s², the linear speed was set at 50 rrrm/s and the linear acceleration was set at 0.4mm/s². The blending time was set at 4 minutes. The rotors were set to run in a regular mode, with all rotors rotating at the same time, with rotors 1 and 2 rotating in a first direction and rotors 3 and 4 rotating in a second direction (Rotor numbering as per Figure 16), and a linear mode with rotors 1 and 3 moving linearly together and rotors 2 and 4 moving linearly together. Pictures were taken every 20 seconds for the run duration and are shown in figures 23 A-23M. [0106] In light of the detailed description of the invention and the examples presented above, it can be appreciated that the several objects of the invention are achieved. [0107] The explanations and illustrations presented herein are intended to acquaint others skilled in the art with the invention, its principles, and its practical application. Those skilled in the art may adapt and apply the invention in its numerous forms, as may be best suited to the requirements of a particular use. Accordingly, the specific embodiments of the present invention as set forth are not intended as being exhaustive or limiting of the invention.

Claims

We claim:

1. An apparatus for blending two or more materials, the apparatus comprising: a body defining a chamber for blending the materials, the body comprising a first end comprising an inlet for introducing materials into the chamber and a second end; a base located on the second end of the body; comprising four rotary element throughbores; four rotary elements configured for rotation and linear movement within the chamber for blending the materials and configured for movement into and out of the chamber through the rotary element throughbores of the base; a rotary assembly adapted to rotate each of the four rotary elements independently from each other; a linear actuation assembly adapted to linearly move each of the four rotary elements independently from each other through the throughbores; an outlet in selective fluid communication with the chamber through which materials are removed from the chamber; and a by-pass valve in fluid communication with the outlet that provides an optional flow path for materials exiting the chamber.

2. An apparatus for blending two or more materials, the apparatus comprising: a body defining a chamber for blending the materials; a system for introducing or removing gases from the chamber, the system comprising a gas channel in the body and a gas pin channel located in the body and in selective fluid communication with the gas channel and in fluid communication with the chamber, wherein the gas channel and the gas pin channel are located at about 90 degrees relative to each other, and wherein a gas pin located in the gas pin channel, is configured to move between a first and a second position to open and close gas flow between the chamber and the gas channel; and four rotary elements configured for independent rotation and linear movement within the chamber for blending the materials.

3. An apparatus for blending two or more materials, the apparatus comprising: a body defining a transparent chamber for blending the materials, the body comprising a first end comprising an inlet for introducing materials into the chamber and a second end; a base located on the second end of the body; comprising four rotary element throughbores; four rotary elements configured for rotation and linear movement within the chamber for blending the materials and configured for movement into and out of the chamber through the rotary element throughbores of the base; a rotary assembly adapted to rotate each of the four rotary elements independently from each other; a linear actuation assembly adapted to oscillate each of the four rotary elements independently from each other through the throughbores; an outlet in selective fluid communication with the chamber through which materials are removed from the chamber; and an analysis assembly for viewing materials in said transparent chamber.

4. The apparatus of any of claim 1-3, wherein the chamber has a volume from about 1 to about 1000 ml.

5. The apparatus of any of claims 1-4, wherein the four rotary elements are vertical pins configured for rotation within the chamber for blending the materials.

6. The apparatus of any of claims 1-5, wherein the body comprises an inlet in fluid communication with the chamber.

7. The apparatus of claim 2, wherein the body comprises an outlet in fluid communication with the chamber.

8. The apparatus of any of claims 1-7, wherein one of the materials is a powder having a particle size range between about 1 and 500 microns .

9. The apparatus of any of claims 1-8, wherein at least one of the materials is a polymer.

10. The apparatus of any of claims 1-9, wherein at least two of the materials are polymers.

11. The apparatus of any of claims 1-10, further comprising an automated powder dispensing device configured for dispensing a predetermined amount of a powder material to be blended.

12. The apparatus of any of claims 1- 11, further comprising a plunger and an extruding element, configured for dispensing the blended material out of the outlet of the chamber of the body.

13. The apparatus of claim 12, wherein the plunger is driven by a linear actuator.

14. The apparatus of claim 12, wherein the plunger comprises a spring loaded plunger collar configurerd to engage the body and provide additional sealing when the plunger is driven into the chamber.

15. The apparatus of any of claims 12-14, wherein the extruding element is an extruder pin configured to extrude the blended material through the outlet port after the plunger is driven into the chamber.

16. The apparatus of any of claims 1-15, wherein the chamber is configured to operate at temperatures from about -20 to about 100°C.

17. The apparatus of any of claims 1-15, wherein the chamber is configured to operate at temperatures above about 150°C.

18. The apparatus of any of claims 1-15, wherein the chamber is configured to operate at temperatures above about 200⁰C.

19. The apparatus of any of claims 1-15, wherein the chamber is configured to operate at temperatures above about 250°C.

20. The apparatus of any of claims 1-19, wherein the rotary elements are configured for a rotational speed between about 1 and 1000 rotations per minute.

21. The apparatus of any of claims 1-20, wherein the four rotary elements are a first pin, a second pin, a third pin and a fourth pin, and wherein the four pins are arranged in an array such that the first and third pins have a first center-to-center distance between them; the second and fourth pins have a second center-to center distance between them equal to the first center-to center distance; the first and second pins have a third center-to-center distance between them that is less than the first center-to center distance; the first and fourth pins have a fourth center-to-center distance between them that is less than the first center-to center distance; the second and third pins have a fifth center-to-center distance between them that is less than the first center-to center distance; and the third and fourth pins have a sixth center-to-center distance between them that is less than the first center-to center distance.

22. The apparatus of any of claims 1-21, wherein the four rotary elements are configured for rotation at the same time during blending of the materials.

23. The apparatus of claim 22, wherein the first, second, third and fourth pins are all configured for rotation at the same speed in the same direction.

24. The apparatus of claim 22, wherein the first and third pins are configured for rotation at the same speed in a first direction and the second and fourth pins are configured for rotation at the same speed in a second direction different than the first direction.

25. The apparatus of claim 22, wherein the first and fourth pins are configured for rotation at the same speed in a first direction and the second and third pins are configured for rotation at the same speed in a second direction different than the first direction.

26. The apparatus of claim 22, wherein the first pin is configured for rotation in a first direction and the second, third and fourth pins are configured for rotation at the same speed in a second direction different than the first direction.

27. The apparatus of any of claims 1-21, wherein the first and second pins are configured for rotation at the same time during a first time period during blending of the materials and the third and fourth pins are configured for rotation at the same time during a second time period during blending of the materials.

28. The apparatus of claim 27, wherein the first, second, third and fourth pins are all configured for rotation at the same speed in the same direction.

29. The apparatus of claim 27, wherein the first and third pins are configured for rotation at the same speed in a first direction and the second and fourth pins are configured for rotation at the same speed in a second direction different than the first direction.

30. The apparatus of claim 27, wherein the first and fourth pins are configured for rotation at the same speed in a first direction and the second and third pins are configured for rotation at the same speed in a second direction different than the first direction.

31. The apparatus of claim 27, wherein the first and second pins are configured for rotation at the same speed in a first direction and the third and fourth pins are configured for rotation at the same speed in a second direction different than the first direction.

32. The apparatus of claim 27, wherein the first pin is configured for rotation in a first direction and the second, third and fourth pins are configured for rotation at the same speed in a second direction different than the first direction.

33. The apparatus of any of claims 1-21, wherein first and third pins are configured for rotation at the same time during a first time period during blending of the materials and the second and fourth pins are configured for rotation at the same time during a second time period during blending of the materials.

34. The apparatus of claim 33, wherein the first, second, third and fourth pins are all configured for rotation at the same speed in the same direction.

35. The apparatus of claim 33, wherein the first and third pins are configured for rotation at the same speed in a first direction and the second and fourth pins are configured for rotation at the same speed in a second direction different than the first direction.

36. The apparatus of claim 33, wherein the first and fourth pins are configured for rotation at the same speed in a first direction and the second and third pins are configured for rotation at the same speed in a second direction different than the first direction.

37. The apparatus of claim 36, wherein the first and second pins are configured for rotation at the same speed in a first direction and the third and fourth pins are configured for rotation at the same speed in a second direction different than the first direction.

38. The apparatus of claim 33, wherein the first pin is configured for rotation in a first direction and the second, third and fourth pins are configured for rotation at the same speed in a second direction different than the first direction.

39. The apparatus of any of claims 27-38, wherein the first time period and the second time period do not overlap.

40. The apparatus of any of claims 27-38, wherein the first time period and the second time period overlap.

41. The apparatus of any of claims 1-40, wherein the four pins are configured for vertical movement in and out of the chamber.

42. The apparatus of any of claims 1-21, wherein each pin is individually configured to rotate in a first or second direction; rotate at a variable speed; linearly move into and out of the chamber; and combinations thereof during blending of the materials.

43. The apparatus of any of claims 21-42, wherein the third center-to center distance, the fourth center-to center distance, the fifth center-to center distance, and the sixth center-to center distance are equal.

44. A method of blending at least two materials, the method comprising; providing an apparatus defined by any of claims 1-43; providing a first material; providing a second material; delivering the first and second materials to the chamber; and blending the materials in the chamber with the four rotary elements.

45. The method of claim 44, wherein the four rotary elements are a first pin, a second pin, a third pin and a fourth pin, and wherein the four pins are arranged in an array such that the first and third pins have a first center-to-center distance between them; the second and fourth pins have a second center-to center distance between them equal to the first center-to center distance; the first and second pins have a third center-to-center distance between them that is less than the first center-to center distance; the first and fourth pins have a fourth center-to-center distance between them that is less than the first center-to center distance; the second and third pins have a fifth center-to-center distance between them that is less than the first center-to center distance; and the third and fourth pins have a sixth center-to-center distance between them that is less than the first center-to center distance.

46. The method of claim 45, wherein the blending step comprises rotating the four pins at the same time.

47. The method of claim 46, wherein the first, second, third and fourth pins all rotate at the same speed in the same direction.

48. The method of claim 46, wherein the first and third pins rotate at the same speed in a first direction and the second and fourth pins rotate at the same speed in a second direction different than the first direction.

49. The method of claim 46, wherein the first and fourth pins rotate at the same speed in a first direction and the second and third pins rotate at the same speed in a second direction different than the first direction.

50. The method of claim 46, wherein the first pin rotates in a first direction and the second, third and fourth pins rotate at the same speed in a second direction different than the first direction.

51. The method of claim 45, wherein the blending step comprises rotating the first and second pins together during a first time period and rotating the third and fourth pins together during a second time period.

52. The method of claim 51, wherein the first, second, third and fourth pins rotate at the same speed in the same direction.

53. The method of claim 51, wherein the first and third pins rotate at the same speed in a first direction and the second and fourth pins rotate at the same speed in a second direction different than the first direction.

54. The method of claim 51 , wherein the first and fourth pins rotate at the same speed in a first direction and the second and third pins rotate at the same speed in a second direction different than the first direction.

55. The method of claim 51, wherein the first and second pins rotate at the same speed in a first direction and the third and fourth pins rotate at the same speed in a second direction different than the first direction.

56. The method of claim 51, wherein the first pin rotates in a first direction and the second, third and fourth pins rotate at the same speed in a second direction different than the first direction.

57. The method of claim 45, wherein the blending step comprises rotating the first and third pins together during a first time period and rotating the second and fourth pins together during a second time period.

58. The method of claim 57, wherein the first, second, third and fourth pins rotate at the same speed in the same direction.

59. The method of claim 57, wherein the first and third pins rotate at the same speed in a first direction and the second and fourth pins rotate at the same speed in a second direction different than the first direction.

60. The method of claim 57, wherein the first and fourth pins rotate at the same speed in a first direction and the second and third pins rotate at the same speed in a second direction different than the first direction.

61. The method of claim 57, wherein the first and second pins rotate at the same speed in a first direction and the third and fourth pins rotate at the same speed in a second direction different than the first direction.

62. The method of claim 57, wherein the first pin rotates in a first direction and the second, third and fourth pins rotate at the same speed in a second direction different than the first direction.

63. The method of any of claims 51-62, wherein the first time period and the second time period do not overlap.

64. The method of any of claims 51-62, wherein the first time period and the second time period overlap.

65. The method of any of claims 44-64, wherein the four pins move in and out of the chamber during blending.

66. The method of any of claims 44-65, further comprising dispensing the blended materials out of the chamber through an outlet.

67. The method of claim 66, wherein the blended material is extruded out of the chamber.

68. The method of any of claims 44-67, wherein each rotary element individually rotates in a first or second direction; rotates at a variable speed; linearly moves into and out of the chamber; and combinations thereof during blending of the materials.

69. The method of any of claims 44-68, wherein the chamber has a volume from about 1 to about 10 ml.

70. The method of any of claims 44-69, wherein one of the materials is a powder.

71. The method of claim 70, wherein the powder is dispensed into the chamber via an automated powder dispensing apparatus.

72. The method of any of claims 44-71, wherein at least one of the materials is a polymer.

73. The method of any of claims 44-72, wherein at least two of the materials are polymers.

74. The method of any of claims 44-73, wherein the blending step occurs at temperatures above about 100⁰C.

75. The method of any of claims 44-73, wherein the blending step occurs at temperatures above about 150⁰C.

76. The method of any of claims 44-73, wherein the blending step occurs at temperatures above about 200°C.

77. The method of any of claims 44-73, wherein the blending step occurs at temperatures above about 250°C.

78. The method of any of claims 44-73, wherein the blending step occurs at temperatures above about 300°C.

79. The method of any of claims 44-78, wherein the rotary elements rotate between about 1 and 600 rotations per minute.

80. The method of any of claims 44-79, wherein the chamber is constructed of an infrared-transparent material.

81. The method of any of claims 77 -80, wherein the method is automated.

82. The method of any of claims 44-81, further comprising characterizing the material.