JPS63144110A - Production of polycrystalline silicon - Google Patents
Production of polycrystalline siliconInfo
- Publication number
- JPS63144110A JPS63144110A JP29116686A JP29116686A JPS63144110A JP S63144110 A JPS63144110 A JP S63144110A JP 29116686 A JP29116686 A JP 29116686A JP 29116686 A JP29116686 A JP 29116686A JP S63144110 A JPS63144110 A JP S63144110A
- Authority
- JP
- Japan
- Prior art keywords
- hydrogen
- hydrogen chloride
- polycrystalline silicon
- concentration
- chloride
- 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.)
- Pending
Links
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 58
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 45
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 44
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 34
- 239000001257 hydrogen Substances 0.000 claims abstract description 34
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000007789 gas Substances 0.000 claims abstract description 8
- 230000003211 malignant effect Effects 0.000 claims description 14
- 239000003344 environmental pollutant Substances 0.000 claims description 12
- 231100000719 pollutant Toxicity 0.000 claims description 12
- 238000006722 reduction reaction Methods 0.000 claims description 11
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 abstract description 10
- 238000011109 contamination Methods 0.000 abstract description 9
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 239000000356 contaminant Substances 0.000 abstract description 6
- 230000006378 damage Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 230000002411 adverse Effects 0.000 abstract 4
- 229910003822 SiHCl3 Inorganic materials 0.000 abstract 1
- 150000002431 hydrogen Chemical class 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 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 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000005049 silicon tetrachloride Substances 0.000 description 2
- 238000010186 staining Methods 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、水素による還元反応により多結晶シリコンを
製造する方法に関し、更に詳しくは還元反応において生
した排ガスを活性炭層に通し、水素を精製して再利用す
るようにした多結晶シリコンの製造方法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing polycrystalline silicon by a reduction reaction using hydrogen, and more specifically, the present invention relates to a method for producing polycrystalline silicon by a reduction reaction using hydrogen. The present invention relates to a method for producing polycrystalline silicon that can be recycled.
このような製造方法を第１図により説明すると、還元炉
ｌに三塩化シラン（ＳｉＨＣｌｓ）、水素（Ｈｔ）を供
給することにより下記の還元反応が起こり、多結晶シリ
コン（Ｓｉ）が製造されると同時に、四塩化ケイ素（Ｓ
ｉＣ１４）、塩化水素（ＨＣ／ｌ）、水素（Ｈ２）等を
排出する。To explain this manufacturing method with reference to Figure 1, by supplying silane trichloride (SiHCls) and hydrogen (Ht) to the reduction furnace 1, the following reduction reaction occurs, and polycrystalline silicon (Si) is manufactured. At the same time, silicon tetrachloride (S
iC14), hydrogen chloride (HC/l), hydrogen (H2), etc.
４ＳｉＨＣ１ｘ→Ｓｉ＋３ＳｒＣ１ａ ＋２ＨｚＳＩＨ
ＣＩｊ＋Ｈｚ→Ｓｉ＋３ＨＣ１
排出された四塩化ケイ素、塩化水素、水素と更に未反応
の三塩化シラン、水素とを含んだ排ガスは、水素回収装
置２に送られ、ここで活性炭による塩化物の吸着を受け
、水素のみが精製されて還元炉１に送られ、上記の還元
反応に再利用される。4SiHC1x→Si+3SrC1a +2HzSIH
CIj+Hz→Si+3HC1 The exhaust gas containing silicon tetrachloride, hydrogen chloride, hydrogen, and unreacted trichlorosilane and hydrogen is sent to the hydrogen recovery device 2, where the chloride is adsorbed by activated carbon. Only hydrogen is purified and sent to the reduction furnace 1, where it is reused in the above-mentioned reduction reaction.
この場合、水素は多結晶シリコンの汚染を防止する意味
から、高純度のものが要求され、そのために活性炭を使
用しているわけであるが、活性炭は一定量の物質を吸着
すると、その段階を境に一気に吸着不能に陥る。この現
象は、活性炭の破過と呼ばれ、吸着物質の種類によって
段階的に生じてゆくものである。In this case, hydrogen must be of high purity in order to prevent contamination of polycrystalline silicon, and activated carbon is used for this purpose. Once activated carbon has absorbed a certain amount of material, it stops at that stage. It suddenly becomes impossible to absorb. This phenomenon is called breakthrough of activated carbon, and occurs in stages depending on the type of adsorbent.
第１図の製造系統においてこのような破過が生じると、
破過を生じさせた物質が活性炭に吸着されずにそのまま
還元炉ｌに流入し、多結晶シリコンを汚染することにな
る。汚染物質のなかでもシリコンの電気伝導度に影響を
与える物質、例えば塩化物による破過に起因して活性炭
から生じるリン塩化′ＪＩｙＪ（ｐｃｚゴ）、ボロン塩
化物（ＢＣｊ！３）等は特に有害で、これによる破過は
絶対に回避されなければならず、シリコン中の混入量は
０．１ｐｐｂａ （１０−” ）程度までしか許容さ
れない。If such a breakthrough occurs in the manufacturing system shown in Figure 1,
The substances that caused the breakthrough flow into the reduction furnace 1 as they are without being adsorbed by the activated carbon, contaminating the polycrystalline silicon. Among the contaminants, substances that affect the electrical conductivity of silicon, such as phosphorus chloride 'JIyJ (pczgo) and boron chloride (BCj!3), which are generated from activated carbon due to chloride breakthrough, are particularly harmful. Therefore, breakthrough due to this must be absolutely avoided, and the amount of contamination in the silicon is only allowed to be about 0.1 ppba (10-'').
ところが、現実にこのようなオーダーでリン塩化物等を
検出できる簡易計測器は存在しない、そこで、例えばリ
ン塩化物等の悪性汚染物質による破過の時期を活性炭の
使用期間から経験的に推定して、活性炭の再生を行うと
いうことが考えられるが、当然のことながら再生時期が
安定化せず、再生時期が早すぎた場合は活性炭が無駄に
なり、万一再生時期が遅れた場合は多結晶シリコンが汚
染によって欠陥品となり一層大きな無駄を生じることに
なる。However, in reality, there is no simple measuring instrument that can detect phosphorus chloride, etc. on this order of magnitude, so the time of breakthrough due to malignant pollutants such as phosphorus chloride is estimated empirically from the period of use of activated carbon. Therefore, it is possible to regenerate the activated carbon, but of course the regeneration time is not stabilized, and if the regeneration time is too early, the activated carbon will be wasted, and if the regeneration time is delayed, there will be many problems. Contamination of the crystalline silicon results in defective products and even greater waste.
本発明は、リン塩化物等の悪性汚染物質による汚染を確
実に防止し、しかも活性炭が使用限界近くまで効率よく
使用することができる多結晶シリコンの製造方法を提供
するものである。The present invention provides a method for producing polycrystalline silicon that reliably prevents contamination by malignant pollutants such as phosphorus chloride, and allows activated carbon to be used efficiently up to its usage limit.
〔問題点を解決するための手段）
ところで、第１図に示したような水素還元による多結晶
シリコンの製造においては、前述したように排ガスとし
て塩化水素が生じる。この塩化水素は多結晶シリコンの
品質への影響はなく著しい高濃度になると生産性への影
響はあるが、１０ｐｐｍ程度では問題はない。[Means for Solving the Problems] By the way, in the production of polycrystalline silicon by hydrogen reduction as shown in FIG. 1, hydrogen chloride is produced as exhaust gas, as described above. This hydrogen chloride does not affect the quality of polycrystalline silicon, and if the concentration is extremely high, it may affect productivity, but at about 10 ppm there is no problem.
しかも、この塩化水素は好都合なことに、沸点が−８４
，８℃（ｌａｔｍ）と、リン塩化物等の悪性汚染物質の
沸点（Ｐ Ｃｌ ｓで７４．２℃）に比べて低い。つま
り、活性炭は沸点の低い物質から破過を起こすので、リ
ン塩化物等の悪性汚染物質による破過が発生する前に塩
化水素による破過を生じるのである。Moreover, this hydrogen chloride conveniently has a boiling point of -84
, 8°C (latm), which is lower than the boiling point of malignant pollutants such as phosphorus chloride (74.2°C for P Cl s). In other words, since activated carbon causes breakthrough from substances with low boiling points, breakthrough from hydrogen chloride occurs before breakthrough from malignant pollutants such as phosphorus chloride occurs.
本発明の方法は、この多結晶シリコンの製造における塩
化水素と悪性汚染物質との特長的関係に着目してなされ
たもので、その特徴とするところは、活性炭層を通すこ
とにより精製された水素中の塩化水素濃度を連続的また
は間欠的に定量測定し、定量測定された塩化水素濃度の
上昇からリン塩化物等の悪性汚染物質による活性炭の破
過を未然に検知し、多結晶シリコンへの悪性汚染物質の
混入を防止する点にある。The method of the present invention was developed by focusing on the characteristic relationship between hydrogen chloride and malignant pollutants in the production of polycrystalline silicon. The concentration of hydrogen chloride in the carbon is measured continuously or intermittently, and from the increase in the quantitatively measured hydrogen chloride concentration, breakthrough of activated carbon by malignant pollutants such as phosphorus chloride can be detected in advance, and it is possible to detect The purpose is to prevent the contamination of malignant pollutants.
前述したように、塩化水素はリン塩化物等の悪性Ｉη染
動物質りも早く活性炭に破過を生じさせる。As mentioned above, hydrogen chloride causes a rapid breakthrough in activated carbon even from malignant Iη staining substances such as phosphorus chloride.
塩化水素による破過が生じると、水素中の塩化水素ＩＱ
度が上昇するが、その濃度はｔｏｐｐｍ程度まで許容さ
れる。ｐｐｍオーダーは簡易計測器で十分検出が可能な
量であるので、水素中の塩化水素濃度を定量的に監視す
ることにより、塩化水素による破過が即座に検知され、
これによりこの破過に続く悪性物質による破過を未然に
、しかも正確かつ自動的に知ることができるのである。When hydrogen chloride breakthrough occurs, hydrogen chloride IQ in hydrogen
Although the concentration increases, the concentration is allowed up to about TOPPM. Since the ppm order is a quantity that can be sufficiently detected with a simple measuring instrument, by quantitatively monitoring the hydrogen chloride concentration in hydrogen, a breakthrough due to hydrogen chloride can be detected immediately.
This makes it possible to accurately and automatically detect breakthroughs caused by malignant substances following this breakthrough.
また、塩化水素による破過が生しても、水素中の混入量
が１０ｐｐｍＪＳｆ度まで許容されているので、この濃
度に至るまでに製造を中止し、活性炭を再生すれば、塩
化水素による汚染を生じることもない。In addition, even if breakthrough occurs due to hydrogen chloride, the amount of hydrogen mixed in is allowed up to 10 ppm JSf, so if production is stopped and activated carbon is regenerated before this concentration is reached, contamination by hydrogen chloride can be avoided. It never happens.
第２図は本発明の方法を実施するために検知系統を例示
したフローシートである。FIG. 2 is a flow sheet illustrating a detection system for carrying out the method of the present invention.
図中、３は活性炭により精製された水素の母管を表わし
ている。母管３を通過する水素の一部はバルブ４を経て
例えばテフロンチューブ等の導管５により連続的または
間欠的にサンプリングされる。サンプリングされた水素
はフィルター６を通過後、センサ７にて塩化水素濃度が
測定され、サンプリング用ポンプ８を経て系外に放出さ
れる。In the figure, 3 represents the main pipe of hydrogen purified by activated carbon. A portion of the hydrogen passing through the main pipe 3 is sampled continuously or intermittently via a valve 4 through a conduit 5, such as a Teflon tube. After the sampled hydrogen passes through the filter 6, the hydrogen chloride concentration is measured by the sensor 7, and is discharged to the outside of the system via the sampling pump 8.
測定された塩化水素濃度は例えば中央計器室等で遠隔か
ら監視される。The measured hydrogen chloride concentration is monitored remotely, for example in a central control room.
なお、９は塩化水素ガスボンベで、センサ７の精度を定
期的にチェックするためのものである。Note that 9 is a hydrogen chloride gas cylinder, which is used to periodically check the accuracy of the sensor 7.
第３図は塩化水素濃度センサの一例についてその動作原
理を示したものである。このセンサは、隔膜電極式電解
法の原理に基づくもので、水素等の可燃性ガス中の塩化
水素濃度を安全にしかもｌｐｐｍ単位で測定できる。FIG. 3 shows the operating principle of an example of a hydrogen chloride concentration sensor. This sensor is based on the principle of diaphragm electrode electrolysis and can safely measure the concentration of hydrogen chloride in combustible gases such as hydrogen in lppm units.
同図において、塩化水素を含んだ水素は隔膜ｌＯを通過
し、作用電極１１との間の極めて薄い電解液ＦＪ１２に
塩化水素のみが溶解Ｍ、離する（下式溶解電離によって
生じた０ｆｆ−イオンは、上記作用極１１上で酸化され
（、ＣＲ−−”Ｃ１ｌ＋ｅ−）、これによって生しる電
流を測定することにより塩化水素濃度が定量的に測定さ
れる。電解電離によって塩化水素を失った水素はケース
１３外に放出される。In the figure, hydrogen containing hydrogen chloride passes through the diaphragm IO, only hydrogen chloride dissolves in the extremely thin electrolyte FJ12 between it and the working electrode 11, and is separated (0ff- ions generated by dissolution ionization using the following formula). is oxidized on the working electrode 11 (CR--"C1l+e-), and the hydrogen chloride concentration is quantitatively measured by measuring the current generated. Hydrogen chloride is lost by electrolytic ionization. Hydrogen is released outside the case 13.
なお、１４は対極、１５は基準極を示し、基ｉ％極１５
は、作用型ｉｌｌを他の可燃性ガス、有機溶剤などに反
応しない電位に保つためのものであ第２図の検知系統に
おいて、水素中の塩化水素濃度をセンサ７により監視す
るようにすれば、活性炭に塩化水素による破過が生じて
ない状態では、上記塩化水素は検出されない、この状態
では当然、リン塩化物等の悪性汚染物質による破過も生
じていない。In addition, 14 shows the counter electrode, 15 shows the reference electrode, and the basic i% electrode 15
is to maintain the active type ill at a potential that does not react with other combustible gases, organic solvents, etc. In the detection system shown in Fig. 2, if the hydrogen chloride concentration in hydrogen is monitored by sensor 7, In a state in which hydrogen chloride does not cause breakthrough in the activated carbon, the hydrogen chloride is not detected. In this state, naturally, no breakthrough occurs in malignant pollutants such as phosphorus chloride.
活性炭の塩化水素による破過が生じ始めると、活性炭の
塩化水素に対する吸着能力が急激に劣え始め、これに対
応して水素中の塩化水素濃度が上昇し始める。そして、
この水素中の塩化水素濃度の上昇を許容値到達前にセン
サ７により捉え、多結晶シリコンの製造を停止して活性
炭を再生すれば、リン塩化物等の悪性汚染物質によるｌ
η染が未然に防止される。When breakthrough of activated carbon by hydrogen chloride begins to occur, the adsorption capacity of activated carbon for hydrogen chloride begins to deteriorate rapidly, and correspondingly, the hydrogen chloride concentration in hydrogen begins to increase. and,
If this increase in the concentration of hydrogen chloride in hydrogen is detected by sensor 7 before it reaches a permissible value, and production of polycrystalline silicon is stopped and activated carbon is regenerated, the increase in the concentration of hydrogen chloride in hydrogen can be detected.
η staining is prevented.
確認のため塩化水素を検出した時点で活性炭を取り出し
調査したところ、汚染物質による破過は認められなかっ
た。For confirmation, when hydrogen chloride was detected, the activated carbon was taken out and examined, and no breakthrough due to contaminants was observed.
以上の説明から明らかなように、本発明の方法は水素中
の塩化水素濃度を測定することにより、活性炭の使用限
界が遠隔から正確かつ節華に予知され、これにより活性
炭の悪性汚染物質による破過を未然に防止し、悪性汚染
物質によるシリコン汚染を防いで、シリコンの高品’ｆ
ＧＩＭ保に大きな効果を奏するものである。As is clear from the above explanation, the method of the present invention allows the use limit of activated carbon to be predicted remotely, accurately and conveniently by measuring the concentration of hydrogen chloride in hydrogen, and thereby enables the destruction of activated carbon by malignant pollutants. It prevents silicon pollution from occurring due to malignant pollutants, and improves the quality of silicone.
This has a great effect on GIM maintenance.
また、活性炭が必要以上に早く交換されるといった事態
も回避され、活性炭の使用コストも低減させることがで
きる。Furthermore, a situation in which activated carbon is replaced sooner than necessary can be avoided, and the cost of using activated carbon can also be reduced.
第１図は多結晶シリコンの製造方法を示すフローシート
、第２図は本発明に係る塩化水素濃度検知系統のフロー
シート、第３図は同しく塩化水素濃度センサの原理図で
ある。
図中、ｌ：還元炉、２：水素回収袋；η、３：水素母管
、７：センサ。
第 １ 図
第 ２ 図
第 ３ 凶FIG. 1 is a flow sheet showing a method for manufacturing polycrystalline silicon, FIG. 2 is a flow sheet of a hydrogen chloride concentration detection system according to the present invention, and FIG. 3 is a diagram of the principle of the hydrogen chloride concentration sensor. In the figure, l: reduction furnace, 2: hydrogen recovery bag; η, 3: hydrogen main tube, 7: sensor. Figure 1 Figure 2 Figure 3
Claims (1)
する際に生じる排ガスを活性炭層に通し、水素を精製し
て前記還元反応工程に還元させる多結晶シリコンの製造
において、精製された水素中の塩化水素濃度を連続的ま
たは間欠的に定量測定し、定量測定された塩化水素濃度
の上昇から悪性汚染物質による活性炭の破過を未然に検
知し、多結晶シリコンへの悪性汚染物質の混入を防止す
ることを特徴とする多結晶シリコンの製造方法。(1) In the production of polycrystalline silicon, the exhaust gas generated during the production of polycrystalline silicon through a reduction reaction with hydrogen is passed through an activated carbon layer, the hydrogen is purified, and then reduced in the reduction reaction step. Quantitatively measures hydrogen concentration continuously or intermittently, detects the breakthrough of activated carbon by malignant pollutants from the quantitatively measured increase in hydrogen chloride concentration, and prevents malignant pollutants from entering polycrystalline silicon. A method for producing polycrystalline silicon, characterized by:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29116686A JPS63144110A (en) | 1986-12-05 | 1986-12-05 | Production of polycrystalline silicon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29116686A JPS63144110A (en) | 1986-12-05 | 1986-12-05 | Production of polycrystalline silicon |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63144110A true JPS63144110A (en) | 1988-06-16 |
Family
ID=17765299
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP29116686A Pending JPS63144110A (en) | 1986-12-05 | 1986-12-05 | Production of polycrystalline silicon |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63144110A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006131491A (en) * | 2004-10-05 | 2006-05-25 | Tokuyama Corp | Silicon production method |
| JP2008143776A (en) * | 2006-11-14 | 2008-06-26 | Mitsubishi Materials Corp | Hydrogen purification/collection method and hydrogen purification/collection facility |
| JP2009227514A (en) * | 2008-03-24 | 2009-10-08 | Tokuyama Corp | Silicon production process |
| JP2010275162A (en) * | 2009-05-29 | 2010-12-09 | Mitsubishi Materials Corp | Method and apparatus for producing polycrystalline silicon |
| US8241401B2 (en) | 2010-11-02 | 2012-08-14 | Mitsubishi Polycrystalline Silicon America Corporation (MIPSA) | Apparatus and method for producing purified hydrogen gas by a pressure swing adsorption processes |
| CN104928761A (en) * | 2014-03-19 | 2015-09-23 | 新特能源股份有限公司 | Preparation method of silicon wafer master alloy |
-
1986
- 1986-12-05 JP JP29116686A patent/JPS63144110A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006131491A (en) * | 2004-10-05 | 2006-05-25 | Tokuyama Corp | Silicon production method |
| JP2008143776A (en) * | 2006-11-14 | 2008-06-26 | Mitsubishi Materials Corp | Hydrogen purification/collection method and hydrogen purification/collection facility |
| JP2009227514A (en) * | 2008-03-24 | 2009-10-08 | Tokuyama Corp | Silicon production process |
| JP2010275162A (en) * | 2009-05-29 | 2010-12-09 | Mitsubishi Materials Corp | Method and apparatus for producing polycrystalline silicon |
| US8241401B2 (en) | 2010-11-02 | 2012-08-14 | Mitsubishi Polycrystalline Silicon America Corporation (MIPSA) | Apparatus and method for producing purified hydrogen gas by a pressure swing adsorption processes |
| US8431082B2 (en) | 2010-11-02 | 2013-04-30 | Mitsubishi Polycrystalline Silicon America Corporation (MIPSA) | Apparatus and method for producing purified hydrogen gas by a pressure swing adsorption processes |
| CN104928761A (en) * | 2014-03-19 | 2015-09-23 | 新特能源股份有限公司 | Preparation method of silicon wafer master alloy |
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