GB2028289A - Producing silicon - Google Patents
Producing silicon Download PDFInfo
- Publication number
- GB2028289A GB2028289A GB7915583A GB7915583A GB2028289A GB 2028289 A GB2028289 A GB 2028289A GB 7915583 A GB7915583 A GB 7915583A GB 7915583 A GB7915583 A GB 7915583A GB 2028289 A GB2028289 A GB 2028289A
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- GB
- United Kingdom
- Prior art keywords
- silicon
- reactor
- hydrogen
- trihalosilane
- bed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229910052710 silicon Inorganic materials 0.000 title claims description 43
- 239000010703 silicon Substances 0.000 title claims description 43
- 238000000034 method Methods 0.000 claims abstract description 60
- 230000008569 process Effects 0.000 claims abstract description 57
- 239000004065 semiconductor Substances 0.000 claims abstract description 14
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 43
- 239000001257 hydrogen Substances 0.000 claims description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 18
- 230000008021 deposition Effects 0.000 claims description 5
- 238000010924 continuous production Methods 0.000 claims description 4
- 239000005046 Chlorosilane Substances 0.000 claims 1
- VQPFDLRNOCQMSN-UHFFFAOYSA-N bromosilane Chemical group Br[SiH3] VQPFDLRNOCQMSN-UHFFFAOYSA-N 0.000 claims 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical group Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 22
- 239000000203 mixture Substances 0.000 abstract description 6
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 5
- 229910052794 bromium Chemical group 0.000 abstract description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical group [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 abstract 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical group BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 abstract 1
- 229910052801 chlorine Inorganic materials 0.000 abstract 1
- 239000000460 chlorine Substances 0.000 abstract 1
- 125000001309 chloro group Chemical group Cl* 0.000 abstract 1
- 239000006227 byproduct Substances 0.000 description 11
- IBOKZQNMFSHYNQ-UHFFFAOYSA-N tribromosilane Chemical compound Br[SiH](Br)Br IBOKZQNMFSHYNQ-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000010923 batch production Methods 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- AIFMYMZGQVTROK-UHFFFAOYSA-N silicon tetrabromide Chemical compound Br[Si](Br)(Br)Br AIFMYMZGQVTROK-UHFFFAOYSA-N 0.000 description 5
- 239000011856 silicon-based particle Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 238000004821 distillation Methods 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 230000006911 nucleation Effects 0.000 description 4
- 238000010899 nucleation Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 3
- 239000005052 trichlorosilane Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910003822 SiHCl3 Inorganic materials 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 238000005243 fluidization Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000006200 vaporizer Substances 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- 229910003826 SiH3Cl Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 230000036962 time dependent Effects 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 230000004584 weight gain Effects 0.000 description 1
- 235000019786 weight gain Nutrition 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
A low temperature, closed loop, thermal decomposition process for producing a controllable mixture of heterogeneously and homogeneously nucleated ultrahigh purity polycrystalline silicon suitable for use in the manufacture of semi-conductor devices and photovoltaic solar cells uses the chemical reaction: <IMAGE> where X is chlorine or bromine.c
Description
SPECIFICATION
Process for producing polycrystalline silicon technical field
United States Patent 4,084,024 which issued April 11, 1978, in the name of Joseph C. Schumacher, and which is assigned to the present assignee, discloses and claims a process for the production of semiconductor grade silicon using hydrogen reduction at relatively high temperatures, for example, within a temperature range of from 900"C - 1 200"C. The process of the present invention, on the other hand, involves a process for producing semiconductor grade silicon involving the use of thermal decomposition which is carried out at a lower and more economical temperature range of, for exaple, 500"C - 900"C.
BACKGROUND OF THE PRIOR ART
As pointed out in the patent, recent developments in the semiconductor industry have created a growing demand for a low cost single crystal silicon of extremely high purity, which is known as semiconductor grade silicon, and which is used in the manufacture of semiconductor devices and silicon voltaic solar cells. For that reason, a multitude of prior art processes have been conceived for the production of semiconductor grade silicon, including the process covered by the patent. The prior art processes can be classified into the following six basic approaches:
1. The Siemens process described in GDR Patents 1,066,564; 1,102,117; 1,233,815 and British Patent 904,239 by which essentially all current semiconductor grade polycrystalline silicon is produced, is expressed by the following chemical reaction.
o Si (MG) + HCI Cu Catalyst SiCL4 + SiHC13 + other byproducts o SiHCl3 + H2 1 0000C Si + SiCI4 + HCI + explosive polymer Si-H-X byproducts This is a high temperature batch process providing heterogeneously nucleated silicon growth Si filaments and large volumes of SiCI4 and explosive polymeric byproducts which must be disposed of. The process is as a result of these byproducts not a closed-loop process. In addition a 20/l excess of H2 over stoichiometry is required.
2. Silicon tetrachloride - hydrogen reduction is utilized in some cases because of the availability of byproduct SiC14 from the Siemens process. An alternative SiCI4 production reaction is included here since it may be used as a source.
SiCI4 + 2H2 1 200"C C > Si + 4HCI + polymers This again is a high temperature, non-closed-loop, batch process providing heterogeneously nucleated growth on a heated substrate and requires a large H2 excess.
3. The DuPont process as described in U.S. Patents 3,012,862 and 4,084,024 where in SiX4 or SiHX3 (where X = Cl,Br,l) is reduced in a fluid or moving bed by H2, Zn, or Cd The reaction chemistry is as follows: I Feed preparation
with SiX4 here a byproduct
II Ultrapure silicon production by
+ polymers for X = Cl or
SiX4 + H2 > Si + HX + polymers
These are moderately high temperature, non-closed loop processes with the byproducts varying with the particular process chemistry, and which require large hydrogen excesses where it is used.
4. The lodide process described in U.S. Patent 3,020,129 expressed as follows:
and thermal decomposition to produce Si
This is a moderate-temperature closed-loop batch process in which polycrystalline or single crystal silicon is grown on a seed particle or heated filament.
5. The Union carbide process expressed as follows:
Trichlorosilane preparation
lon exchange redistribution to silane according to
o 2SiHCI3 Amt SiH2C12 + SiHC14 '" + SiHCl4 o2SiH2Cl2 50-1000C SiH3Cl + SiHCl3 Am be rite 50-1 000C o 4SiH3CI Amberlite3SiH4 + SiC14 withappropriatebvnroductrecvcle followed bv silane thermal decomDosition.
This is a low temperature, closed-loop process involving an ion exchange intermediate redistribution and produces homogeneously nucleated product.
6. The thermal decomposition of trichlorosilane according to
is described in U.S. Patents 2,943,918 and 3,012,861. Presumably the trichlorosilane is prepared according to
Si + HCI S SiHC13 SiCI4 + other products so that a non-closed process would result. Only batch type operation is proposed to promote heterogeneous nucleation and homogeneous nucleation is avoided and thought harmful.
Many other techniques and slight modifications of the techniques presented are contained within the prior art; however none would appear to have a material bearing on the present invention.
An important feature of the process of the invention is that it is a continuous process unlike the prior art batch process 1, 2, 4 and 6 described briefly above. As is well known, the continuous process represents an improvement over the batch processes in the reduction of capital costs and operating expenses per unit of product.
Another important feature of the process of the present invention is that it is a ciosed-loop low temperature process; whereas the prior art processes 1, 2, 3 and 6, supra, are high temperature, open-loop processes. The prior art processes represent higher operating expenses due to their excessive energy requirements and the need for the disposal of corrosive and hazardous byproducts.
Another feature of the process of the invention is that it utilizes a direct high yield thermal decomposition of trihalosilane in contrast to the low yield thermal decomposition process of U.S. Patents 2,943,918 and 3,012,861, rather than going through the ion exchange redistribution of prior art process 5 in order to obtain a material suitable for thermal decomposition. The inherent simplicity of the process of the present invention results in a reduction in complexity and operating costs and an improvement in yield capabilities.
Another important feature of the process of the invention is the avoidance of wall build-up in the thermal decomposition reaction by maintaining a critical temperature differential between the bed and the surrounding walls.
Brief description of the drawing
Figure lisa schematic representation of one embodiment of the process of the invention.
Detailed description of the invention
In the first process step, in accordance with the invention, metallurgical grade silicon metal of approximately 95% or greater purity is reacted with hydrogen (H2) and the appropriate silicon tetrahalide (SiX4) in a crude silicon converter 10 to produce trihalosilane, and in which the reaction:
is carried out. The converter may be a first stage fluid bed reactor maintained within a temperature range of substantially 400 Co - 650on, and at atmospheric or greater pressure. The converter may be of the type described, for example, in U.S. Patent 2,993,762.
The metallurgical grade silicon may be generated locally in an electrothermic silicon generator of known construction, as described in U.S. Patent 4,084,024, or it may be obtained from usual commercial sources.
The metallurgical grade silicon is preferably in the particle size range of 50-500 microns to provide good fluidization characteristics. Fluidization is provided by hydrogen gas containing tetrahalide vapor which is introduced into the reactor through an inlet vaporizer 12. Conversion efficiencies of 30% or g reater stoichiometric are achieved in the reactor.
A mixture of trihalosiline (SiHX3) and unreacted hydrogen (H2) and tetrahalosilane is carried from the top of the reactor 10 in vapor phase to a condenser 14. Impurity metal halides are removed from the bottom of reactor 10.
The hydrogen and trihalosilane are separated out in a separator 16, with the hydrogen being returned to the reactor 10. The trihalosilane is introduced to a refiner 18 in which it is purified in accordance with the second step of the process. During the second step unreacted silicon tetrahalide is recovered and returned to the feed system for the reactor 10 through a surge drum 20.
It is important to recognize that the conversion reaction in reactor 10 in accordance with the first step of the process of the invention occurs in a non-equilibrium manner. That is to say, the reaction at 400"-650"C in the reactor of
has a positive free energy of 5-20 Kcal per mole and an equilibrium constant less than unity since AF = -RTf nKp. As a result, the reaction products must be continuously removed from the reactor. The production of trihalosilane (SiHX3) thereby occurs as a result of the operation of the law of mass action under non-equilibrium conditions.
The second step of the process involves the purification of the trihalosilane in a refiner 18 by the distillation of the trihalosilane prior to the further processing thereof into ultra-high purity polycrystalline silicon.
Refiner 18 may be a simple, multi-plate distillation column, and it is utilized to separate the feed trihalosilane into ixtu re of less than 5% tetrahalosilane in trihalosilane of metallic and organic impurity content less than 100 parts per billion total; and a mixture oftrihalosilane and tetrahalosilanewhich has significantly greater than 100 parts per billion metallic and organic impurities, as bottoms. The bottoms are returned to the first stage reactor 10 through the surge drum 20, as explained above. The overhead is fed to reactor 28 through a condenser 22 and separator 24, and through an inlet vaporizer 26, so that the third step of the process may be carried out. As in the previous stage, the hydrogen from separator 24 is recycled to the feed for the first stage reactor 10.Refiner 18 may be of the type described in detail in Adcock et al U.S. Patent 3,120,128.
The third step of the process of the invention effectuates the thermal decomposition of trihalosilane in a reactor 28 within a temperature range of the order of 600 - 800 , and at atmospheric or reduced pressure.
The thermal decomposition is in accordance with the reaction
The product, ultrapure semiconductor grade silicon is produced in reactor 28 along with the by-products hydrogen and tetrahalosilane. The byproducts are recovered and separated by a condenser 30 and separator 32, and they are recycled as feed for the first stage reacltor 10, as illustrated, to achieve a closed-loop process.
The recycled hydrogen is purified in an activated carbon filter 34 of known construction, and is compressed by a compressor 36. The purified and compressed hydrogen is then passed to a mixing eductor 38, in which it is mixed with the silicon tetrahalide from surge drum 20 and fed to the first stage reactor 10.
Make-up hydrogen may also be added, as indicated.
Reactor 28 may be a moving bed reactor of the type described in detail in U.S. Patent 4,084,024; or it may be a fluid bed reactor of the type described in U.S. Patents 3,012,861; 3,012,862 or 3,963,838.
An important feature of the process of the present invention is the production of ultra-pure semiconductor grade silicon in reactor 28 at a relatively low temperature lying, for example, within a range of essentially 500 - 800"C, without the introduction of hydrogen into the reactor; as compared with the high temperature (900"C - 1500"C) hydrogen reduction in the reactor as described in U.S. Patent 4,084,024.The process of the present invention is predicated upon the premise that the chemical reaction
occurs in a temperature range of the order of 600 -800 C producing a high yield (80% - 100%) of purified semi-conductor grade silicon deposited on a substrate consisting of fine particles of the purified silicon.
Above 900"C, for example, the mechanism of reactor 28 changes and the yield of silicon falls to a low value, of the order of 10%, as described, for example, in U.S. Patent 3,012,861. Hydrogen must be added in the high temperature range above 900"C, as described in U.S. Patent 4,084,024, in order to produce high quality silicon in accordance with the reaction
Another important feature of the process of the invention is its "closed loop" aspect, which makes the process economically feasible. Specifically, there are essentially no byproducts produced by the process which are not recycled back for re-use, and the only material actually "consumed" in the process is impure silicon, which is converted into ultra-pure semi-conductor grade silicon.
Accordingly, in the process of the invention, product silicon from trihalosilane thermal decomposition is produced as a mixture of homogeneously nucleated fine powder and heterogeneously nucleated silicon growth upon the fluid or moving bed substrate particles in reactor 28. The relative proportion of homogeneous to deterogeneous nucleation is controlled by several factors including, but not limited to, (1) feed stock (tribromosilane ortrichlorosilane); (2) decomposition temperature and pressure; (3) bed (substrate) particle size distribution and surface pre-treatment; (4) bed velocity and vapor-particle relative velocity; and (5) bed depth and residence time.
It is important to control the ratio of homogeneous to heterogeneous nucleation to (1) achieve a self-perpetuating bed wherein growth substrate particles are grown in situ rather than being prepared from the product in a separate grinding operation and (2) to maximize conversion efficiency and rate. Conversion efficiencies of greater than 80-90% of theoretical are routinely achieved.
In the practice og the process of the invention, it is advantageous to hold wall temperatures in the fluid or moving bed reactor 28 at greater than 900"C while maintaining bed temperature between 700"C and 800"C.
Wall deposits and reactor plugging are thereby avoided. In most fluid or moving bed reactors, reaction heat for endothermic chemical reactions is obtained by heating the reactor walls by gas firing, resistance heating, induction heating or by various other means. However, reaction rate and extent are generally directly proportional to temperature so that considerable reaction and deposition takes place on the walls as described in U.S. Patent 3,963,838. These deposits generally occur at the highest temperature portion of the reactor. Wall deposits, thus formed, in time build up and cause, not only time-dependent heat transfer characteristics, but also reduced heat transfer and eventual reactor plugging. It has been found that silicon deposition from the thermal decomposition of trihalosilane ceases at a temperature of 900"C-1000"C.Thus, wall deposition in the process of the present invention is avoided by holding wall temperatures in a range of 900"C-1000"C, while maintaining bed temperatures in a range extending from 700" to 850into establish maximum silicon deposition rate and yield.
A specific example of the conversion of tetrabromosilane to tribromosilane in the first stage reactor 10 is as follows:
A combined gaseous stream of hydrogen and tetrabromosilane were introduced into reactor 10 which contained a heated bed of silicon particles. The gaseous stream had a composition of 2.23 moles of hydrogen per mole of tetrabromosilane. The silicon bed had a cross-sectional area of 4.54 square centimeters and a length of 40 centimeters. The bed temperature was maintained at 650"C, and the average residence time of the gaseous stream was 5.1 seconds. The silicon particles introduced into the reactor 10 were metallurgical grade.Condensation of the exit stream from the reactor in condenser 14, followed by subsequent distillation of the condensate in the purification distillation column 18 indicated a 36% conversion of the tetrabromosilane into tribromosilane. Conversion is defined as the moles of tribromosilane obtained from the reaction divided by the initial number of moles of tetrabromosilane introduced into the reactor.
Specific example of the decomposition of tribromosilane to silicon in reactor 28.
A gaseous stream of argon and tribromosilane having a composition of 7.7 moles of argon per mole of tribromosilane was introduced into a fluidized bed reactor. Although not essential to the practice of the invention, the argon served as both the tribomosilane carrier and fluidizing gas for the bed of silicon particles within the reactor. The bed of silicon particles consisted of 50 mesh particles and had a total mass at the start of the reaction of 258 grams. The bed was maintained at a temperature of 786"C-800"C during the reaction.
A total of 1.57 moles of tribromosilane was introduced into the reactor during the run. Removal of the silicon particles at the end of the run showed that the bed had a mass of 268.1 grams or a weight gain of 10.1 grams or a yield of 91%, based on the decomposition reaction
The invention provides, therefore, a low-temperature, closed-loop continuous process for the economical production of high purity semiconductor grade silicon. The process of the invention, as described, utilizes the direct thermal decomposition of trihalosilane at relatively low temperatures (below 900"C) to produce ultra-pure silicon. The process also avoids silicon wall build-up in the reactor by maintaining a temperature differential between the bed and the surrounding wall such that the lowest temperature of the wall is above the threshold temperature at which silicon is deposited thereon.
It will be appreciated that although a particular embodiment of the invention has been shown and described, modifications may be made. It is intended in the claims to cover the modifications which come within the true spirit and scope of the invention.
Claims (8)
1. A process for the production of high purity silicon comprising: thermally decomposing trihalosilane in a temperature range of substantially 600"-800"C to produce ultra-pure semiconductor grade silicon.
2. The process for the production of high purity silicon as claimed in Claim 1, wherein said process comprises, before said decomposing step, the preparatory steps of: reacting silicon, silicon tetrahalide and hydrogen to produce trihalosilane, and purifying the trihalosilane.
3. The process defined in Claim 2, in which hydrogen and unreacted silicon tetrahalide are recycled to the reacting step to form a closed-loop continuous process.
4. The process defined in claim 1, in which the thermal decomposition step is carried out in a reactor, and which includes the step of maintaining the wall of the reactor at a temperature above 900"C to obviate the deposition of silicon on the wall of the reactor.
5. The process defined in Claim 1, in which the halosilane is bromosilane.
6. The process defined in Claim 1, in which the halosilane is chlorosilane.
7. The process defined in Claim 2, in which the silicon, silicon tetrahalide and hydrogen are reacted in a temperature range of substantially 400"C-650"C.
8. A process for production of high purity silicon as claimed in any preceding claim and substantially as hereinbefore described.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US93500978A | 1978-08-18 | 1978-08-18 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| GB2028289A true GB2028289A (en) | 1980-03-05 |
| GB2028289B GB2028289B (en) | 1982-09-02 |
Family
ID=25466438
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB7915583A Expired GB2028289B (en) | 1978-08-18 | 1979-05-04 | Producing silicon |
Country Status (6)
| Country | Link |
|---|---|
| JP (1) | JPS5527890A (en) |
| CA (1) | CA1145117A (en) |
| DE (2) | DE2954368C2 (en) |
| FR (1) | FR2433479B1 (en) |
| GB (1) | GB2028289B (en) |
| IT (1) | IT1193203B (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4696834A (en) * | 1986-02-28 | 1987-09-29 | Dow Corning Corporation | Silicon-containing coatings and a method for their preparation |
| US4743344A (en) * | 1986-03-26 | 1988-05-10 | Union Carbide Corporation | Treatment of wastes from high purity silicon process |
| US4871524A (en) * | 1987-09-03 | 1989-10-03 | Ethyl Corporation | Hydrogen purification process |
| WO2007120871A2 (en) * | 2006-04-13 | 2007-10-25 | Cabot Corporation | Production of silicon through a closed-loop process |
| WO2008027101A1 (en) * | 2006-08-30 | 2008-03-06 | Hemlock Semiconductor Corporation | Silicon production with a fluidized bed reactor integrated into a siemens-type process |
| WO2009017780A2 (en) * | 2007-07-31 | 2009-02-05 | Donald Shaum | Electronic apparatus with multiple data input modes |
| US20110262338A1 (en) * | 2008-03-31 | 2011-10-27 | Schmid Silicon Technology Gmbh | Method and system for the production of pure silicon |
| WO2012054170A1 (en) * | 2010-10-22 | 2012-04-26 | Memc Electronic Materials, Inc. | Production of polycrystalline silicon in substantially closed-loop processes and systems |
| US8449848B2 (en) | 2010-10-22 | 2013-05-28 | Memc Electronic Materials, Inc. | Production of polycrystalline silicon in substantially closed-loop systems |
| US9394180B2 (en) | 2010-10-22 | 2016-07-19 | Sunedison, Inc. | Production of polycrystalline silicon in substantially closed-loop systems |
Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4676967A (en) * | 1978-08-23 | 1987-06-30 | Union Carbide Corporation | High purity silane and silicon production |
| US4374182A (en) * | 1980-07-07 | 1983-02-15 | Dow Corning Corporation | Preparation of silicon metal through polymer degradation |
| US4390510A (en) | 1982-02-16 | 1983-06-28 | General Electric Company | Process for treating spent silicon-containing reaction masses to produce halosilanes |
| JPS61101410A (en) * | 1984-10-24 | 1986-05-20 | Hiroshi Ishizuka | Production of polycrystalline silicon and apparatus therefor |
| EP1786730A2 (en) * | 2004-07-16 | 2007-05-23 | Institutt For Energiteknikk | Method and reactor for continuous production of semiconductor grade silicon |
| DE102009032833A1 (en) | 2009-07-08 | 2011-01-13 | Schmid Silicon Technology Gmbh | Process and plant for the production of monosilane |
| DE102009037154B3 (en) * | 2009-08-04 | 2010-12-09 | Schmid Silicon Technology Gmbh | Process for the preparation of monosilane |
| DE102009037155B3 (en) * | 2009-08-04 | 2010-11-04 | Schmid Silicon Technology Gmbh | Process and plant for the production of trichlorosilane |
| DE102010000981A1 (en) | 2010-01-18 | 2011-07-21 | Evonik Degussa GmbH, 45128 | Closed-loop process for the production of trichlorosilane from metallurgical silicon |
| DE102010034469A1 (en) | 2010-08-06 | 2012-02-09 | Schmid Silicon Technology Gmbh | Plant for the production of monosilane |
| DE102011089695A1 (en) | 2011-12-22 | 2013-06-27 | Schmid Silicon Technology Gmbh | Reactor and process for the production of ultrapure silicon |
| DE102015203618A1 (en) | 2015-02-27 | 2016-09-01 | Schmid Silicon Technology Gmbh | Column and process for the disproportionation of chlorosilanes to monosilane and tetrachlorosilane and plant for the production of monosilane |
| DE102015209008A1 (en) | 2015-05-15 | 2016-11-17 | Schmid Silicon Technology Gmbh | Process and plant for the decomposition of monosilane |
| WO2017183487A1 (en) * | 2016-04-21 | 2017-10-26 | 株式会社トクヤマ | Metal powder production method |
| DE102019209898A1 (en) | 2019-07-04 | 2021-01-07 | Schmid Silicon Technology Gmbh | Apparatus and method for forming liquid silicon |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2595620A (en) * | 1948-11-27 | 1952-05-06 | Union Carbide & Carbon Corp | Hydrogenation of halogenosilanes |
| BE554836A (en) * | 1956-02-11 | |||
| BE571013A (en) * | 1957-09-07 | |||
| US3012861A (en) * | 1960-01-15 | 1961-12-12 | Du Pont | Production of silicon |
| GB1498266A (en) * | 1974-05-13 | 1978-01-18 | Texas Instruments Inc | Method of silicon production |
| DE2620739A1 (en) * | 1976-05-11 | 1977-12-01 | Wacker Chemitronic | PROCESS FOR PRODUCING HIGHLY PURE SILICON |
| US4117094A (en) * | 1977-06-13 | 1978-09-26 | Texas Instruments Incorporated | Process for silicon and trichlorosilane production |
-
1979
- 1979-05-04 GB GB7915583A patent/GB2028289B/en not_active Expired
- 1979-05-11 DE DE2954368A patent/DE2954368C2/en not_active Expired
- 1979-05-11 DE DE2919086A patent/DE2919086C2/en not_active Expired
- 1979-05-15 CA CA000327660A patent/CA1145117A/en not_active Expired
- 1979-05-16 FR FR7912469A patent/FR2433479B1/en not_active Expired
- 1979-05-17 IT IT22753/79A patent/IT1193203B/en active
- 1979-05-17 JP JP5980079A patent/JPS5527890A/en active Granted
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4696834A (en) * | 1986-02-28 | 1987-09-29 | Dow Corning Corporation | Silicon-containing coatings and a method for their preparation |
| US4743344A (en) * | 1986-03-26 | 1988-05-10 | Union Carbide Corporation | Treatment of wastes from high purity silicon process |
| US4871524A (en) * | 1987-09-03 | 1989-10-03 | Ethyl Corporation | Hydrogen purification process |
| US7780938B2 (en) | 2006-04-13 | 2010-08-24 | Cabot Corporation | Production of silicon through a closed-loop process |
| WO2007120871A2 (en) * | 2006-04-13 | 2007-10-25 | Cabot Corporation | Production of silicon through a closed-loop process |
| WO2007120871A3 (en) * | 2006-04-13 | 2007-12-21 | Cabot Corp | Production of silicon through a closed-loop process |
| CN101460398B (en) * | 2006-04-13 | 2012-08-29 | 卡伯特公司 | Production of silicon through a closed-loop process |
| US8609058B2 (en) | 2006-08-30 | 2013-12-17 | Hemlock Semiconductor Corporation | Silicon production with a fluidized bed reactor integrated into a Siemens-type process |
| WO2008027101A1 (en) * | 2006-08-30 | 2008-03-06 | Hemlock Semiconductor Corporation | Silicon production with a fluidized bed reactor integrated into a siemens-type process |
| US7935327B2 (en) | 2006-08-30 | 2011-05-03 | Hemlock Semiconductor Corporation | Silicon production with a fluidized bed reactor integrated into a siemens-type process |
| KR101447494B1 (en) | 2006-08-30 | 2014-10-06 | 헴로크세미컨덕터코포레이션 | Silicon production with a fluidized bed reactor integrated into a Siemens-type process |
| WO2009017780A2 (en) * | 2007-07-31 | 2009-02-05 | Donald Shaum | Electronic apparatus with multiple data input modes |
| WO2009017780A3 (en) * | 2007-07-31 | 2010-07-15 | Donald Shaum | Electronic apparatus with multiple data input modes |
| US20110262338A1 (en) * | 2008-03-31 | 2011-10-27 | Schmid Silicon Technology Gmbh | Method and system for the production of pure silicon |
| CN103153855A (en) * | 2010-10-22 | 2013-06-12 | Memc电子材料有限公司 | Production of polycrystalline silicon in substantially closed-loop processes and systems |
| US8449848B2 (en) | 2010-10-22 | 2013-05-28 | Memc Electronic Materials, Inc. | Production of polycrystalline silicon in substantially closed-loop systems |
| WO2012054170A1 (en) * | 2010-10-22 | 2012-04-26 | Memc Electronic Materials, Inc. | Production of polycrystalline silicon in substantially closed-loop processes and systems |
| US9394180B2 (en) | 2010-10-22 | 2016-07-19 | Sunedison, Inc. | Production of polycrystalline silicon in substantially closed-loop systems |
| CN107555438A (en) * | 2010-10-22 | 2018-01-09 | Memc电子材料有限公司 | Polysilicon is prepared in the method and system of basic closed loop |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2433479A1 (en) | 1980-03-14 |
| DE2954368A1 (en) | 1984-07-12 |
| IT7922753A0 (en) | 1979-05-17 |
| JPS6228083B2 (en) | 1987-06-18 |
| CA1145117A (en) | 1983-04-26 |
| IT1193203B (en) | 1988-06-15 |
| DE2954368C2 (en) | 1986-10-16 |
| DE2919086C2 (en) | 1986-10-16 |
| FR2433479B1 (en) | 1985-10-18 |
| GB2028289B (en) | 1982-09-02 |
| JPS5527890A (en) | 1980-02-28 |
| DE2919086A1 (en) | 1980-03-06 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PCNP | Patent ceased through non-payment of renewal fee |
Effective date: 19930504 |