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US20070014682A1 - Conversion of high purity silicon powder to densified compacts - Google Patents

Conversion of high purity silicon powder to densified compacts Download PDF

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Publication number
US20070014682A1
US20070014682A1 US11/479,735 US47973506A US2007014682A1 US 20070014682 A1 US20070014682 A1 US 20070014682A1 US 47973506 A US47973506 A US 47973506A US 2007014682 A1 US2007014682 A1 US 2007014682A1
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Prior art keywords
silicon
binder
silicon powder
compact
powder
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Abandoned
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US11/479,735
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English (en)
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Alleppey Hariharan
Mohan Chandra
Jagannathan Ravi
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SEMLUX TECHNOLOGIES Inc
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SEMLUX TECHNOLOGIES Inc
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Priority to US11/479,735 priority Critical patent/US20070014682A1/en
Assigned to SEMLUX TECHNOLOGIES, INC. reassignment SEMLUX TECHNOLOGIES, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CHANDRA, MOHAN, HARIHARAN, ALLEPPEY V., RAVI, JAGANNATHAN
Publication of US20070014682A1 publication Critical patent/US20070014682A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F71/00—Manufacture or treatment of devices covered by this subclass
    • H10F71/121—The active layers comprising only Group IV materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/547—Monocrystalline silicon PV cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the present invention is directed towards conversion of fine silicon powder into densified silicon compacts for use in silicon melting and alloy industries. This conversion process is achieved by the use of selective binders to aid in compacting the powder towards subsequent sintering and densification.
  • the end use for the densified silicon compacts is primarily as feedstock for silicon-based photovoltaic manufacturing industries.
  • Compacting of powders is well known in metallurgical and ceramic process industries and is a highly developed method of manufacturing various parts and shapes.
  • powder metals, ceramics or a mixture of ceramics and metals are compacted into various shapes by operations of cold isostatic pressing, hot isostatic pressing, extrusion, injection molding and such other arts.
  • some binder or additive of an inorganic or organic nature is added to effect particle binding and compaction.
  • sintering aids are purposely added in the compaction process to aid in subsequent sintering of the compacted body.
  • the final sintering operation is usually performed at high temperatures in controlled-atmosphere or air-atmosphere furnace to provide for essentially complete removal of the binders and additives, bond the particles metallurgically and impart strength to the compacted body.
  • Silicon powder is industrially produced by various processes. Nominal purity silicon powder is formed as reaction residues from preparation of organochlorosilanes or chlorosilanes from the reaction of elemental silicon with chlorinated hydrocarbons or hydrogen chloride.
  • the powder is used as alloy feed in ferrous and non-ferrous industries, for manufacture of silicon nitride, and so forth.
  • the powder is agglomerated with a binding agent to form granules of 250-500 microns.
  • the binders are typically organic materials such as starch, and lignin. Other agglomeration methods include microwave heating of the powder to 1200-1500 C.
  • the silicon dust is milled in an aqueous solution of pH>5 to form colloidal silica. This helps to agglomerate the dust.
  • Ultra fine silicon is a by-product of the Fluid Bed process to manufacture high purity electronic grade polysilicon.
  • the granules grow in size from an initial seed size of ⁇ 0.2 mm to ⁇ 3 mm in diameter.
  • the granules are utilized in silicon melting and crystal growth applications.
  • the Fluid Bed process however, also results in a large quantity of ultra fine silicon dust. This is tapped out of the reactor outlet and remains as a process waste. This powder is of high purity, but cannot be recycled or used in silicon melting and crystal growth applications.
  • High-pressure hot pressing of silicon powder with sintering aids and subsequent high temperature sintering of pressed silicon bodies are known in the literature.
  • High-pressure hot pressing of silicon powders is described in the art, such as in “ The Effects of Processing Conditions on the Density and Microstructure of Hot-Pressed Si Powder”, by C. J. Santana and K. S. Jones, J. Materials Sci. 31 (18), 4985-4990 (1996); and “ High Pressure Hot-Pressing of Si Powders”, by K. Takatori, M. Shimada and M. Koizumi, J. Jap. Soc. Powder Metal. 28 (1) 15-19 (1981).
  • silicon powder was hot pressed into polycrystalline wafers 1.5′′ diameter using various process conditions, typically hot pressing at 1300 C./2000 psi in hydrogen gas ambience.
  • the wafers were contaminated with iron, aluminum, carbon and oxygen.
  • sintering silicon compacts at high temperatures, ranging from 1250 C. to close to the melting point of Si (1412 C.), in an inert atmosphere. Silicon sintering with addition of sintering aids such as Boron, or retardants such as Tin, is described in the art, for example “ The effect of small amounts of B and Sn on Sintering of Si” by C. Greskovich, J. Mater. Sci 16 (3), 613-619 (1981).
  • the most important aspect of this invention is the development of a process that provides silicon feed stock material to user industries while maintaining the product purity very close to that of the starting material.
  • the silicon compacts can be produced in regular geometric shapes.
  • the silicon used for crystal growth comes in irregular chunks or granules.
  • the advantages of regular shaped silicon of this invention provide for better packing possible, whether for transportation purposes or in the crucible used for melting silicon prior to growing crystalline silicon ingots.
  • the process of this invention uses selective binders to the silicon powder to aid in powder flow, provide material binding and lubricity in mechanical operations in the process of converting the powders to formed shapes.
  • An effective binder will hold dry powders or aggregate together with exceptional green strength during compacting, burning out cleanly and uniformly and provide sufficient strength during subsequent sintering to densify the parts.
  • the focus is the purity of the formed compacted silicon body after subsequent process steps and near complete elimination of all byproducts and subproducts from the binder.
  • the compacting step itself is performed at ambient temperature to prevent in-process reaction of such binders and die/punch material with the silicon, as occurs in hot pressing operations.
  • a similar application of selective binder is in the manufacture of nuclear fuel oxide pellets by the MOX process.
  • small quantities of zinc stearate are utilized as an additive to provide for initial agglomeration and pellet strength while also serving as a lubricant in the pressing operation. It is removed in the subsequent high temperature sintering step.
  • compacting of powders is well known in metallurgical and ceramic process industries. All such processes utilize some binder or additive to effect compaction. In some instances sintering aids are purposely added in the compacting process. Notably, the binders/additives/aids leave a residue of organic or inorganic nature during subsequent operations that render those methods unuseful in this instance. In addition, compacted bodies are sintered at high temperatures to provide compact strength and densification. Although a simple binder-less process is optimum, if practical, to convert high purity silicon powder to compacted shapes, such a method by itself will hardly be robust in industrial handling and transport simply due to lack of compacted body strength with such silicon.
  • the process of this invention utilizes either silicon-based or carbon-based types of binders, each with its specific advantages for application to silicon powder compaction.
  • Silicon-Based Binders are the following Types
  • the binders (a), (b) and (c) belong to the specific group that contains silica (SiO 2 ) either as added or as the product of binder removal. Both forms of silica, fumed and colloidal, and ethyl silicate have unique properties particularly attractive to silicon powder processing. Apart from their binder properties, their cation silicon is the same as the material processed, its anion oxygen helps to form Si-O-Si type of bonds in the process and also reacts with the silicon at high temperature to form volatile SiO, and thus be removed. Because the cation content of these binders is the same as the element silicon that is intended to be processed, these are the most ideal and preferred binding additive.
  • the additive materials (d) and (e) are used because such binders are easy to remove, leave no or very little residues in the completed process and provide a basis to conserve the purity of the processed silicon compact.
  • the ultra fine silicon powder is transferred into a clean feed hopper attached to a blending system where it is blended with the appropriate binder.
  • a batch compacting machine such as pellet press or tablet press.
  • pellet press or tablet press By design such machines are to be of high quality to handle high purity materials. Controlled quantities of the powder are fed into the die by use of an appropriate powder feeder. Special high purity powder feeder may be required.
  • the powder is pressed by the punch with a press force of several tons.
  • the pressed compact in the form of pellet or tablet is ejected into a clean collection bin and/or transferred into a conveyor system to transport to the next stage.
  • the latter itself may be a sintering furnace if the binder is either fumed silica or zinc stearate, or to a de-binder furnace if the binder is one of the following: colloidal silica, ethyl silicate, polypropylene carbonate or stearic acid.
  • the product from the de-binder furnace is transported to the sintering furnace.
  • the sintered compacts are transferred to a lined storage or shipping container.
  • the powder compacting machinery can be semiautomatic or automated for control of operation.
  • the compacting process machinery is located inside a controlled enclosure to maintain process and environment quality.
  • the process facility also provides controlled ingress and filtered egress for environmental safety.
  • the de-binding and sintering furnaces are of the conventional type suitable for the temperature and thermal requirements and with provisions for operation in inert gases, such as argon or helium, or in reducing gas such as hydrogen or in vacuum.
  • the process load carriers are to be high purity silica boats and trays or such refractory containers lined with silicon sheets.
  • FIG. 1 is a general flow sheet for compaction of silicon powder.
  • FIG. 2 gives some example shapes of the compacted silicon product.
  • FIG. 3 is a process flow sheet for silicon powder compaction with combined de-binder and sinter operation.
  • FIG. 1 A process flow sheet of converting silicon powder to compacted and densified silicon shapes is described in FIG. 1 .
  • the invention is amenable to many embodiments.
  • the compacting or pellet/tablet pressing may be done on a clean multi-station press machine with compression force capacity of up to 25 tons.
  • the actual shape and size of the compact are not critical.
  • a precise quantity by weight of the blended silicon powder and binder is fed into the compacting die as a unit charge, and compressed by a matching punch to the required force to achieve the predesigned dimensions.
  • the process may be operated on the basis of compressing a precise charge by volume of powder. The compaction of the precise charge may be performed, to a pre-determined final pressure, whether by calculation or trial and testing to achieve the desired result.
  • the compressed compact is ejected from the machine through the take-off system.
  • the silicon compact provide a bulk material form of silicon for further operations of de-binding and sintering that provide for binder removal and at the same time add densification and strength to the compacted form.
  • compact is herein inclusive of any form factor and a descriptive term that implies a compacted small volume of the raw powder material. Its shape may include cylindrical or square/rectangular block, rods, disks, flats, slabs, wafers, etc. and sizes that are practical for process machinery and handling ( FIG. 2 ).
  • the invention covers the utilization of the compacted and densified dry silicon as feed material by different industries.
  • Silicon compacts of high purity are intended as feedstock to photovoltaic materials industry to make high purity silicon crystals by various means.
  • Silicon compacts of nominal purity are intended for auxiliary ferrosilicon, aluminosilicon and other alloy manufacturing operations.
  • the basic steps of a preferred method for making high purity silicon compacts is as follows: providing a source of high purity silicon powder, feeding the powder into a blender, and mixing with appropriate binder, providing an in-situ drying if desired, discharging the powder into a hopper, feeding a controlled amount by weight or volume of the powder into a die, compacting the powder with pressure, exclusive of any local additive or lubricating agents, and then discharging the dry compact from the die.
  • the machinery may be configured to operate multiple lines of multiple dies, to meet high volume requirements. Additionally, the parts of the machinery that come into contact with the high purity silicon powder and compact may be provided with protective coating to eliminate contamination from the machinery.
  • Additional steps of processing the compacted shapes are: providing an inert flowing gas environment and temperature of 250-500 C. to de-binder the formed compact and providing an inert, reducing or vacuum environment and temperatures of 1000-1350 C. to effect densification and strength to the compact and further remove any binder-related residues.
  • the further steps of especially making high purity silicon ingots from the sintered silicon compacts is conventional and known to those familiar with the art of crystal growth.
  • the crystal growth processes include methods such as Czochralski (CZ), Edge defined Film Growth (EFG), Heat Exchanger Method (HEM), or other.
  • High purity Silicon powder is mixed with high purity fumed silica as a binder.
  • the fumed silica is in the range 0.01-5 weight percent of the silicon powder, preferably in the range 0.05-0.2 weight percent.
  • fumed silica aids powder flow, by forming a layer on the silicon surface and acts like a lubricant, aiding flow and compression. Due to the hydrophilic nature of the fumed silica it absorbs water off the surface of the particles and prevents caking.
  • the mix is well blended, then formed into compacts or pellets/tablets of required shape.
  • the compacted shape is then sintered in an inert gas or reducing gas such as hydrogen in inert gas or vacuum environment at 1000-1350 C. to produce the compacted densified final product.
  • the fumed silica binder reacts with the silicon matrix to form SiO gas, which vaporizes from the compact.
  • High purity Silicon powder is mixed with high purity colloidal silica as a binder.
  • the high purity colloidal silica is nominally 40-50% by weight SiO 2 in isopropyl alcohol or toluene.
  • the colloidal silica is in the range 0.01-5 weight percent of the silicon powder, preferably in the range 0.05-0.2 weight percent.
  • colloidal silica aids powder agglomeration and particle bonding.
  • the mix is well blended, then dried to remove essentially all carrier solvent, then formed into compacts or pellets/tablets of required shape.
  • the compacted shape is then sintered in an inert gas or reducing gas such as hydrogen in inert gas or vacuum environment at 1000-1350 C. to produce the compacted densified final product.
  • any remaining carrier solvent is removed from the compact ( FIG. 3 ).
  • the silica content of the binder reacts with the silicon matrix to form SiO gas, which vaporizes from the compact.
  • High purity Silicon powder is mixed with high purity ethyl silicate 40 (polydiethoxysiloxane with 40% SiO 2 ) as a binder.
  • the ethyl silicate 40 is in the range 0.01-5 weight percent of the silicon powder, preferably in the range 0.05-0.5 weight percent.
  • the mix is well blended, then formed into compacts or pellets/tablets of required shape.
  • the use of ethyl silicate 40 binder requires a de-binder step prior to sintering.
  • Ethyl silicate 40 decomposes completely at >300 C. to silica and ethyl alcohol. The latter boils off the compacted body without any significant reaction with silicon.
  • the compacted shape is then sintered in an inert gas or reducing gas such as hydrogen in inert gas or vacuum environment at 1000-1350 C. to produce the compacted densified final product.
  • an inert gas or reducing gas such as hydrogen in inert gas or vacuum environment at 1000-1350 C.
  • all volatile decomposition products of ethyl silicate 40 will be released completely from the compact.
  • the silica will react with silicon to form silicon monoxide, SiO, which volatilizes off from the compact.
  • the sintered silicon compact may have only very low levels of carbon and oxygen from the binder incorporated in it (of the order of 20 ppm each).
  • High purity Silicon powder is mixed with high purity polypropylene carbonate (QPAC-40) as a binder.
  • the polypropylene carbonate is in the range 0.01-5 weight percent of the silicon powder, preferably in the range 0.05-1 weight percent.
  • the polypropylene carbonate itself is used as a solution dissolved in solvents of the type acetone, methyl ethyl ketone, etc.
  • the concentration of polypropylene carbonate in the solution is in the range 1-25% based on weight, and preferably 10-20%.
  • polypropylene carbonate binders usually results in higher green strength in compacted bodies. Use of such a binder requires a de-binder step prior to sintering. Polypropylene carbonate binders decompose completely in air below 250 C., at temperatures at least 100 C. less than conventional binders. Complete burnout in nitrogen and argon and reducing atmospheres that contain hydrogen is possible at temperatures as low as 300 C., and under vacuum, Polypropylene carbonate burns out as carbon dioxide and water vapor. At the low temperatures of binder removal these products do not react at all significantly with silicon.
  • the compacted shape is then sintered in an inert gas or reducing gas such as hydrogen in inert gas or vacuum environment at 1000-1350 C. to produce the compacted densified final product.
  • an inert gas or reducing gas such as hydrogen in inert gas or vacuum environment at 1000-1350 C.
  • the sintered silicon compact may have only very low levels of carbon and oxygen from the binder incorporated in it (of the order of 20 ppm each).
  • High purity Silicon powder is mixed with high purity stearic acid or zinc stearate as a binder.
  • the stearic acid or zinc stearate is in the range 0.01-5 weight percent of the silicon powder, preferably in the range 0.05-0.2 weight percent.
  • stearic acid or zinc stearate acts as a binder and like a lubricant in the subsequent compacting process.
  • the mix is well blended, then formed into compacts or pellets/tablets of required shape.
  • the compacted shape is then sintered in an inert gas or reducing gas such as hydrogen in inert gas or vacuum environment at 1000-1350 C. to produce the compacted densified final product.
  • Zinc has also a decontamination factor of 100,000 (C melt /C solid ) in the melting and crystallization process.

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US11/479,735 2005-07-01 2006-06-30 Conversion of high purity silicon powder to densified compacts Abandoned US20070014682A1 (en)

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Cited By (17)

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US20070178675A1 (en) * 2003-04-14 2007-08-02 Alain Straboni Sintered semiconductor material
US20080226489A1 (en) * 2007-03-15 2008-09-18 Seiko Epson Corporation Sintered body and method for producing the same
US20090028740A1 (en) * 2003-04-14 2009-01-29 S'tile Method for the production of semiconductor granules
US20090039319A1 (en) * 2003-04-14 2009-02-12 S'tile Sintered semiconductor material
US20090283875A1 (en) * 2008-05-16 2009-11-19 Commissariat A L'energie Atomique Self-supported film and silicon wafer obtained by sintering
WO2010003456A1 (fr) * 2008-07-09 2010-01-14 Garbo S.R.L. Procédé de purification et de compactage de matières premières pour applications photovoltaïques
WO2010003455A1 (fr) * 2008-07-09 2010-01-14 Degussa Novara Technology S.P.A. Corps crus à base de silicium
US20100084776A1 (en) * 2008-10-06 2010-04-08 Clean Venture 21 Corporation Method for producing semiconductor particles
US20100258172A1 (en) * 2003-04-14 2010-10-14 S'tile Semiconductor structure
US20110027159A1 (en) * 2008-06-24 2011-02-03 Tao Zhang APPLICATION METHOD OF SILICON POWDER AND RAW MATERIAL SILICON BRICK WITH GOOD FILLING PROPERTY IN MONO-CRYSTAL FURNACE OR MULTI-CRYSTAL FURNACE (amended)
US20110186111A1 (en) * 2003-04-14 2011-08-04 S'tile Photovoltaic module including integrated photovoltaic cells
EP2117052A3 (fr) * 2008-05-08 2012-02-15 Motech Americas, LLC Feuilles à semi-conducteur et leur procédé de fabrication
US8713966B2 (en) 2011-11-30 2014-05-06 Corning Incorporated Refractory vessels and methods for forming same
US9067792B1 (en) 2006-11-03 2015-06-30 Semlux Technologies, Inc. Laser conversion of high purity silicon powder to densified granular forms
US9741881B2 (en) 2003-04-14 2017-08-22 S'tile Photovoltaic module including integrated photovoltaic cells
CN112384474A (zh) * 2019-04-03 2021-02-19 瓦克化学股份公司 用于生产含硅金属团块的方法
WO2023062154A1 (fr) * 2021-10-14 2023-04-20 JPM Technologies GmbH Procédé permettant la fabrication de granulés de silicium et la fusion de granulés fabriqués

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Cited By (32)

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US20110186111A1 (en) * 2003-04-14 2011-08-04 S'tile Photovoltaic module including integrated photovoltaic cells
US9741881B2 (en) 2003-04-14 2017-08-22 S'tile Photovoltaic module including integrated photovoltaic cells
US20090028740A1 (en) * 2003-04-14 2009-01-29 S'tile Method for the production of semiconductor granules
US20090039319A1 (en) * 2003-04-14 2009-02-12 S'tile Sintered semiconductor material
US9493358B2 (en) 2003-04-14 2016-11-15 Stile Photovoltaic module including integrated photovoltaic cells
US8405183B2 (en) 2003-04-14 2013-03-26 S'Tile Pole des Eco-Industries Semiconductor structure
US8192648B2 (en) 2003-04-14 2012-06-05 S'tile Method for forming a sintered semiconductor material
US8105923B2 (en) * 2003-04-14 2012-01-31 Centre National De La Recherche Scientifique Sintered semiconductor material
US20070178675A1 (en) * 2003-04-14 2007-08-02 Alain Straboni Sintered semiconductor material
US20100258172A1 (en) * 2003-04-14 2010-10-14 S'tile Semiconductor structure
US9067792B1 (en) 2006-11-03 2015-06-30 Semlux Technologies, Inc. Laser conversion of high purity silicon powder to densified granular forms
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