Ann Arbor, MI, United States
Ann Arbor, MI, United States

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Patent
Wadham Energy Lp and Mayaterials, Inc | Date: 2017-02-06

The present invention discloses glycoxy silanes as a source of silica and silica precipitated by advantageous chemical reactions preferably beginning with biogenic silica. Alkoxy COS_(1 )are hydrolyzed in a controlled fashion to nucleate formation of nanoparticles of silica. The growth rate of the particles is controlled by various parameters such that particles of known sizes, size distributions, specific surface areas and pore sizes and size distributions are recovered.


Ro H.W.,U.S. National Institute of Standards and Technology | Popova V.,Mayaterials, Inc | Chen L.,U.S. National Institute of Standards and Technology | Forster A.M.,U.S. National Institute of Standards and Technology | And 5 more authors.
Advanced Materials | Year: 2011

One-step direct nanoimprinting into cubic-silsesquioxane (SSQ) films create low surface energy, high-modulus, thermally stable, and UV-transparent patterns that can then be used as secondary molds for both thermal and UV versions of nanoimprinting. The optimization of these materials is demonstrated by varying the microstructure of the initial SSQ material. The pattern fidelity for features as small as 10 nm is quantified using X-ray reflectivity and AFM. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.


Grant
Agency: National Science Foundation | Branch: | Program: SBIR | Phase: Phase I | Award Amount: 149.82K | Year: 2016

The broader impact/commercial potential of this Small Business Innovation Research Phase I project is that it offers the potential for a new process technology to produce silicon using a sustainable, natural resource as the starting material. Currently, all silicon used in solar cells and computer chips, and all silicon used in the manufacture of silicon containing chemicals including silicone rubbers, oils, lubricants and fumed silica (paints, paper) etc. is produced in an energy, equipment and CO2-intensive process. Biogenic silica includes diatomaceous earth and many kinds of agricultural waste including rice hull ash, inorganic waste from bioethanol production, corn stover, and wheat chaff. The objectives of this project are to develop economical routes from these silica sources to high purity, high value silica products at significantly lower cost than currently available by using a green and sustainable technology. Key markets include electronic, optical, and photonic applications, specialty chemicals, and consumer products. The technical objectives of this Phase I project are to successfully depolymerize biogenic silicas at temperatures ¡Ü 200¡ãC to produce distillable alkoxysilanes. The primary silica source is rice hull ash (RHA), a sustainable, heavy metal free, silica rich agricultural waste. This process uses catalytic base to dissolved RHA silica in antifreeze at ¡Ö 200¡ãC followed by exchange with alcohol to produce alkoxysilanes. In contrast, traditional alkoxysilanes are made from silicon metal produced by carbothermal reduction of silica with carbon at 1900 ¡ãC in an electric arc furnace; a high energy, capital equipment and CO2 intensive process. A further advantage to this process is that the silica depleted RHA offers direct access to high purity (99.9999 %) photovoltaic grade silicon at multi-kg/day scales. If successful, the proposed project could change how high purity alkoxysilanes, precipitated silica, and fumed silica are produced as multiple RHA sources are available worldwide. The alkoxysilane products can be distilled to very high purity at very low cost compared to the same product made from Silicon metal. The initial goal is to produce tetraethoxysilane to compete against Silicon metal derived product and move thereafter to high purity precipitated silica for electronic and optical products applications.


A method of producing alkoxysilanes and precipitated silicas from biogenic silicas is provided. In a first step, biogenically concentrated silica is mixed with a liquid polyol to obtain a mixture, and then the mixture is heated. In a second step, a base is added to obtain a reaction mixture. In a third step, the reaction mixture is filtered to remove the carbon enriched RHA or other undissolved biogenic silica and recover the solution of alkoxysilane and alcoholate. In a fourth step, alkoxysilane is purified by filtering, distilling, precipitating or extracting from the original reaction solution to precipitate various forms of silica. In a final step, residual base present in alkoxysilane is neutralized to eliminate the residual alkali metal base.


Grant
Agency: NSF | Branch: Standard Grant | Program: | Phase: SMALL BUSINESS PHASE I | Award Amount: 164.80K | Year: 2016

The broader impact/commercial potential of this Small Business Innovation Research Phase I project is that it offers the potential for a new process technology to produce silicon using a sustainable, natural resource as the starting material. Currently, all silicon used in solar cells and computer chips, and all silicon used in the manufacture of silicon containing chemicals including silicone rubbers, oils, lubricants and fumed silica (paints, paper) etc. is produced in an energy, equipment and CO2-intensive process. Biogenic silica includes diatomaceous earth and many kinds of agricultural waste including rice hull ash, inorganic waste from bioethanol production, corn stover, and wheat chaff. The objectives of this project are to develop economical routes from these silica sources to high purity, high value silica products at significantly lower cost than currently available by using a green and sustainable technology. Key markets include electronic, optical, and photonic applications, specialty chemicals, and consumer products.

The technical objectives of this Phase I project are to successfully depolymerize biogenic silicas at temperatures ¡Ü 200¡ãC to produce distillable alkoxysilanes. The primary silica source is rice hull ash (RHA), a sustainable, heavy metal free, silica rich agricultural waste. This process uses catalytic base to dissolved RHA silica in antifreeze at ¡Ö 200¡ãC followed by exchange with alcohol to produce alkoxysilanes. In contrast, traditional alkoxysilanes are made from silicon metal produced by carbothermal reduction of silica with carbon at 1900 ¡ãC in an electric arc furnace; a high energy, capital equipment and CO2 intensive process. A further advantage to this process is that the silica depleted RHA offers direct access to high purity (99.9999 %) photovoltaic grade silicon at multi-kg/day scales. If successful, the proposed project could change how high purity alkoxysilanes, precipitated silica, and fumed silica are produced as multiple RHA sources are available worldwide. The alkoxysilane products can be distilled to very high purity at very low cost compared to the same product made from Silicon metal. The initial goal is to produce tetraethoxysilane to compete against Silicon metal derived product and move thereafter to high purity precipitated silica for electronic and optical products applications.


Grant
Agency: Department of Agriculture | Branch: | Program: SBIR | Phase: Phase II | Award Amount: 398.97K | Year: 2010

The United States particularly through DOE and USDA has very strong and often integrated programs targeting the development of new energy sources (e.g. biofuels, wind energy, geothermal, etc) and improvements to sustainable energy sources especially solar power. Billions of dollars have been invested in diverse programs. In contrast, similar integrated efforts at similar scales directed towards new approaches to energy conservation (aside from lighting) have not received the same emphasis despite the fact that this should be of equal National importance. The byproducts of biofuels and direct burning processes (of agricultural wastes for example) will always contain a major inorganic fraction likely to be primarily silica because plants selectively extract and concentrate silica from the environment excluding heavy metals. Thus, the resulting silica is relatively pure compared with natural silica sources (e.g. sand), amorphous and high surface area allowing it to be chemically extracted at low temperatures with minimal costs. Mayaterials' researchers have developed a low temperature, green and inexpensive process to extract this silica from agricultural wastes, rice hull ash in particular. Using the various products of this process, Mayaterials is proposing to develop a new type of inexpensive vacuum insulation panels (VIPs). The use of VIPs in refrigeration and housing is currently limited in the USA due to their very high cost. By using agricultural waste as the raw ingredient and getting rid of the complex and expensive processes currently used to make good quality VIPs, Mayaterials plans to decrease the cost of VIPs several fold. This would allow for a more widespread use of VIP insulation which has the potential for tremendous energy savings if widely adopted. Just in the home refrigerator market, use of VIPs has the potential to save up to 76 Twh each year (50% higher than the USA total wind power electricity generated in 2008).


Grant
Agency: Department of Agriculture | Branch: | Program: SBIR | Phase: Phase I | Award Amount: 80.00K | Year: 2009

Agricultural products used as alternative energy sources can generate considerable waste. This waste will be enriched in plant extracted inorganics including high surface area silica. Mayaterials has already developed proprietary techniques to synthesize several useful chemicals (including several epoxy resins) from these wastes and proposes to use it to develop a new generation of highly efficient vacuum insulation panels cheap enough to be used for housing, thus providing added value to the biofuels synthesis process and increasing energy conservation.


Grant
Agency: National Science Foundation | Branch: | Program: SBIR | Phase: Phase I | Award Amount: 149.92K | Year: 2009

This Small Business Innovation Research Phase I project is to develop materials that function as semi-permanent mold release for the tooling industry. The coating systems proposed also offer icephobic, hydrophobic (non-stick), antibacterial and corrosion resistant properties. The tooling industry employs numerous combinations of materials and processes that require a release agent to reduce adhesion of parts to the tool. Water or silicone based releases are the conventional solution, but need frequent application incurring high material and labor costs. This solution offers considerable cost savings that will be very valuable for most tool companies.


Patent
Mayaterials, Inc | Date: 2012-10-31

A method of forming a silsesquioxane/Q/siloxane polymer or oligomer system used to form coatings or monoliths, includes the step of mixing silsesquioxane, siloxane and alkoxysilane components having structures as presented below in ratios as presented below with a soluble F^() catalyst and water in a suitable solvent so that on stirring at temperatures of 20 to approximately 100 C. all of the components dissolve producing a solution. A soluble oligomer is formed in equilibribum with single molecules with specific structures including [RSiO_(1.5)]_(x)[RMeSiO]_(y)[RMe_(2)SiOSiO_(1.5)]_(z )(where RR or R or R^(1 )or R^(2 )as denoted below) and where x, y and z are mole fractions whose sum is equal to one.


A method of forming a coating comprising the steps of dissolving an silsesquioxane (e.g., one that is primarily a cage compound with 8, 10, 12, 14 or related complete cages or with partially condensed cages containing primarily Si(O)_(4 )units in the cage) in a solvent to form an silsesquioxane solution; introducing (e.g., dissolving) an additive in the solution (e.g., the additive being selected from a rare earth compound, an acid, an organic moiety, a precious metal or compound thereof, a transition metal compound, or any combination thereof, or any of their ionic constituents); and optionally mixing a diluent with the solution to form a coating that is applied to a substrate, wherein the resulting coating forms crosslinks between resulting pendant Si(OH)_(x )groups and a substrate surface. The present invention also contemplates coatings and coated articles consistent with the present teachings.

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