JP2010052952A - Method for purifying silicon - Google Patents
Method for purifying silicon Download PDFInfo
- Publication number
- JP2010052952A JP2010052952A JP2008216225A JP2008216225A JP2010052952A JP 2010052952 A JP2010052952 A JP 2010052952A JP 2008216225 A JP2008216225 A JP 2008216225A JP 2008216225 A JP2008216225 A JP 2008216225A JP 2010052952 A JP2010052952 A JP 2010052952A
- Authority
- JP
- Japan
- Prior art keywords
- silicon
- purity
- purifying
- combustion flame
- mass
- 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
Landscapes
- Silicon Compounds (AREA)
Abstract
Description
本発明は、純度が９５〜９９質量％程度の、所謂粗シリコンを原料として、より高純度の金属シリコンに精製する方法に関するものである。 The present invention relates to a method for refining metal silicon of higher purity using so-called crude silicon having a purity of about 95 to 99% by mass as a raw material.
近年、特に太陽電池の普及により、その主要な材料であるシリコンの需要は拡大している。シリコンは半導体材料として高純度のものが求められ、太陽電池用は半導体材料のＮＧ品や端材を使用することが多かった。しかし、半導体材料の精製法は高価であり、太陽電池用の需要が高まっていることから、太陽電池専用の生産や精製法が求められている。 In recent years, the demand for silicon, which is the main material, has been increasing due to the spread of solar cells. Silicon is required to have a high purity as a semiconductor material, and for solar cells, NG products and scraps of semiconductor materials are often used. However, the purification method for semiconductor materials is expensive, and the demand for solar cells is increasing. Therefore, production and purification methods dedicated to solar cells are required.
例えば半導体に用いられるような高純度シリコンの精製法には、モノシランガス等を原料にしたプラズマＣＶＤ法(特許文献１参照)あるいは単結晶を原料にした赤外線や高周波誘導コイル加熱溶融法(特許文献２参照)等がある。 For example, a high-purity silicon purification method used in semiconductors includes a plasma CVD method using monosilane gas or the like as a raw material (see Patent Document 1) or an infrared or high-frequency induction coil heating and melting method using a single crystal as a raw material (Patent Document 2). See).
また、太陽電池などに利用可能なより安価な製造方法として、プラズマを用いる方法(特許文献３参照)が提案されている。 Moreover, a method using plasma (see Patent Document 3) has been proposed as a cheaper manufacturing method that can be used for solar cells and the like.
また、他に希薄な弗化水素酸中に浸漬して精製する方法(特許文献４参照)や溶融状態のシリコンにＡｒ、Ｈ２あるいはこれらの混合ガスに１ｖｏｌ％以下のＮ２を混合したガスを吹き込むことで精製する方法(特許文献５参照)等が提案されている。
例えば上記特開２００５−２４４０９８号公報や米国特許第４１８８１７７号公報に記載の方法は、非常に高価なものである上に、太陽電池用としては純度が高すぎて必要以上の精製が施されたものとなっている。 For example, the methods described in JP-A-2005-244098 and U.S. Pat. No. 4,188,177 are very expensive, and the purity is too high for solar cells, and the purification is performed more than necessary. It has become a thing.
また、上記特開昭６３−２１８５０６号公報に記載のプラズマを用いる方法は、プラズマを用いるため高価なＡｒガスと電力を多量に消費するため精製コストが高くなる。 Further, the method using plasma described in JP-A-63-218506 increases the purification cost because it consumes a large amount of expensive Ar gas and electric power because it uses plasma.
また、上記特開２００８−５０１８０号公報に記載の方法は、弗化水素酸の取り扱いや廃液処理などの問題点がある。 In addition, the method described in JP-A-2008-50180 has problems such as handling of hydrofluoric acid and waste liquid treatment.
さらに、上記特開平５−３３０８１５号公報に記載の方法も、高価なＡｒガスを使用することや、Ｈ２ガスの取り扱い等、簡易な方法とは言い難い。 Further, the method described in JP-A-5-330815 is also not a simple method such as using expensive Ar gas or handling H 2 gas.
このように、シリコンの需要が高まっているのにもかかわらず、安価な方法で、かつ簡易で純度の高いシリコンを精製する方法は未だに得られていないのが現状である。 As described above, in spite of the increasing demand for silicon, there has not yet been obtained a method for purifying silicon that is inexpensive and simple and high in purity.
本発明は、純度９５質量％以上の金属シリコン粒子を、酸素燃焼炎を形成する燃焼炎ノズル中央部に供給することで、シリコン中の不純物を除去することを特徴とするシリコンの精製方法である。 The present invention is a method for purifying silicon characterized in that impurities in silicon are removed by supplying metal silicon particles having a purity of 95% by mass or more to the center of a combustion flame nozzle that forms an oxyfuel combustion flame. .
また、前記シリコン粒子の径が１〜５００μｍであることを特徴とする上記のシリコンの精製方法である。 The silicon purification method is characterized in that the silicon particles have a diameter of 1 to 500 μm.
本発明によれば、大量の電力を消費せずに、純度９５質量％程度の粗シリコンから純度の高いシリコンを連続でかつ効率的に精製して得ることが可能となる。 According to the present invention, high-purity silicon can be continuously and efficiently purified from crude silicon having a purity of about 95% by mass without consuming a large amount of power.
図１は、本発明を実施するのに用いる装置の基本的な構成の一例であり、９５質量％以上の金属シリコン粒子を燃焼炎ノズル２の中央部の原料供給口３から連続的に供給し、１５００〜３０００℃の酸素燃焼炎４を通過させる。この酸素燃焼炎を通過する間に金属シリコンは酸化されること無く瞬時に溶解するため、蒸気圧の高いＰ、Ｃａ、Ａｌ、Ｍｇなどの不純物は優先蒸発し、また酸素燃焼炎であるため酸化生成物の蒸気圧が高いＢやＣも気相への除去が可能となる。このことにより、金属シリコン中の不純物（特に、Ｂ、Ｃ、Ｐ）を除去できた精製シリコン６を排出口５より連続的に取り出すことが可能となる。 FIG. 1 shows an example of a basic configuration of an apparatus used for carrying out the present invention, in which 95% by mass or more of metal silicon particles are continuously supplied from a raw material supply port 3 at the center of a combustion flame nozzle 2. The oxygen combustion flame 4 at 1500 to 3000 ° C. is passed. Metal silicon dissolves instantly without being oxidized while passing through this oxycombustion flame, so impurities such as P, Ca, Al, and Mg having high vapor pressure preferentially evaporate, and because it is an oxyfuel combustion flame, it is oxidized. B and C having a high vapor pressure of the product can also be removed to the gas phase. As a result, the purified silicon 6 from which impurities (particularly B, C, P) in the metal silicon can be removed can be continuously taken out from the discharge port 5.
ここで、原料となる金属シリコン粒子の径は１〜５００μｍとする。金属シリコン粒子が１μｍ未満では金属シリコンの粉砕に多大な時間やコストがかかるため望ましくない。また５００μｍを超えると、原料供給時の空気搬送が困難となり、また酸素燃焼炎中での不純物の除去効率が悪くなるため好ましくない。より好ましくは１０〜３００μｍである。 Here, the diameter of the metal silicon particles used as a raw material is 1 to 500 μm. If the metal silicon particles are less than 1 μm, it takes a long time and costs to pulverize the metal silicon, which is not desirable. On the other hand, if it exceeds 500 μm, it is difficult to carry the air at the time of supplying the raw material, and the impurity removal efficiency in the oxyfuel flame is deteriorated, which is not preferable. More preferably, it is 10-300 micrometers.
酸素燃焼においては、火炎温度が好ましくはシリコンの融点である１４００℃以上で、かつシリコンの沸点である２３００℃以下になるように燃焼量などを調整する必要があり、また燃焼における酸素比は０．８０〜１．２０、シリコンの酸化や不純物の除去効率を考慮して好ましくは０．９０〜１．１０程度にする。 In oxyfuel combustion, it is necessary to adjust the amount of combustion so that the flame temperature is preferably 1400 ° C. or higher, which is the melting point of silicon, and 2300 ° C. or lower, which is the boiling point of silicon, and the oxygen ratio in combustion is 0 .80 to 1.20, and preferably about 0.90 to 1.10 in consideration of silicon oxidation and impurity removal efficiency.
燃焼に使用する燃料はＬＮＧ、ＬＰＧや灯油などいずれでも良い。しかし、先に述べたように多くの不純物が蒸発されて除かれるとはいえ、精製したシリコンに出来る限り不純物が移行しないように、燃料中にはＢ、Ｃ、Ｐなどの不純物が少ない方が望ましい。 The fuel used for combustion may be LNG, LPG, kerosene, or the like. However, as described above, although many impurities are evaporated and removed, the amount of impurities such as B, C, and P is less in the fuel so that the impurities are not transferred to the purified silicon as much as possible. desirable.
１ シリコンの製造置
２ 燃焼炎ノズル
３ 原料供給口
４ 酸素燃焼炎
５ 精製シリコン排出口
６ 精製シリコン
1 Silicon production site
2 Combustion flame nozzle
3 Raw material supply port
4 Oxyfuel flame
5 Purified silicon outlet
6 Purified silicon
Claims (2)
2. The method for purifying silicon according to claim 1, wherein the silicon particles have a diameter of 1 to 500 [mu] m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008216225A JP2010052952A (en) | 2008-08-26 | 2008-08-26 | Method for purifying silicon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008216225A JP2010052952A (en) | 2008-08-26 | 2008-08-26 | Method for purifying silicon |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2010052952A true JP2010052952A (en) | 2010-03-11 |
Family
ID=42069268
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2008216225A Pending JP2010052952A (en) | 2008-08-26 | 2008-08-26 | Method for purifying silicon |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2010052952A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS627619A (en) * | 1985-07-03 | 1987-01-14 | Mitsubishi Chem Ind Ltd | Method and apparatus for producing silicon |
| JPS63218506A (en) * | 1985-07-31 | 1988-09-12 | フォトワット・インタナショナル・ソシエテ・アノニム | How to purify split silicon under plasma |
| JPH10203812A (en) * | 1997-01-22 | 1998-08-04 | Kawasaki Steel Corp | Refining of metallic silicon |
| JPH10251007A (en) * | 1997-03-11 | 1998-09-22 | Kawasaki Steel Corp | Method for melting metal silicon and method for oxidation refining using the same |
| JP2001089130A (en) * | 1999-09-14 | 2001-04-03 | Denki Kagaku Kogyo Kk | Production of fine spherical silica powder |
| WO2008031229A1 (en) * | 2006-09-14 | 2008-03-20 | Silicium Becancour Inc. | Process and apparatus for purifying low-grade silicon material |
-
2008
- 2008-08-26 JP JP2008216225A patent/JP2010052952A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS627619A (en) * | 1985-07-03 | 1987-01-14 | Mitsubishi Chem Ind Ltd | Method and apparatus for producing silicon |
| JPS63218506A (en) * | 1985-07-31 | 1988-09-12 | フォトワット・インタナショナル・ソシエテ・アノニム | How to purify split silicon under plasma |
| JPH10203812A (en) * | 1997-01-22 | 1998-08-04 | Kawasaki Steel Corp | Refining of metallic silicon |
| JPH10251007A (en) * | 1997-03-11 | 1998-09-22 | Kawasaki Steel Corp | Method for melting metal silicon and method for oxidation refining using the same |
| JP2001089130A (en) * | 1999-09-14 | 2001-04-03 | Denki Kagaku Kogyo Kk | Production of fine spherical silica powder |
| WO2008031229A1 (en) * | 2006-09-14 | 2008-03-20 | Silicium Becancour Inc. | Process and apparatus for purifying low-grade silicon material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100369811C (en) | Comprehensive utilization method of by-product for poycrystalline silicon production process | |
| CN103482623B (en) | Method for preparing nano diamonds by using direct-current arc process | |
| JP2007145663A (en) | Method for producing high purity polycrystalline silicon | |
| JP2010100508A (en) | Production method of high purity silicon | |
| JP6124374B2 (en) | Method for producing isopropyl alcohol | |
| JP4692324B2 (en) | High purity polycrystalline silicon production equipment | |
| JP2010052952A (en) | Method for purifying silicon | |
| JP6746580B2 (en) | Optimized methods and equipment for melting vitrifiable materials in flame-fired furnaces | |
| JP2010269992A (en) | Method and apparatus for refining metallic silicon | |
| JP2010052960A (en) | Method for production of high-purity silicon, production apparatus, and high-purity silicon | |
| Karabanov et al. | Mathematical modeling and experimental research of the method of plasma chemical purification of metallurgical-grade silicon | |
| CN101311660A (en) | Polycrystalline silicon reducing furnace water cooled electrode | |
| CN105502405B (en) | A kind of method of carbon insulation quilt surface dephosphorization in polysilicon handle wafer stove | |
| TWI619855B (en) | Method for purifying high-purity silicon by fractionation | |
| RU2327639C2 (en) | Method of producing high purity silicon | |
| CN101386413B (en) | Method for reducing oxygen and carbon content in metal silicon | |
| RU2010146688A (en) | METHOD FOR REFINING METALLURGIC SILICON BY PLASMA OF DRY ARGON WITH INJECTION OF WATER ON THE SURFACE OF THE MELT WITH THE FOLLOWING DIRECTED DIRECTIONAL CRYSTALLIZATION | |
| JP2010052951A (en) | Method for producing silicon | |
| JP2008081387A (en) | Manufacturing method of high purity silicon | |
| RU2010146687A (en) | METHOD FOR CLEANING METALLURGIC SILICON MOISTURIZED BY AC PLASMA IN VACUUM | |
| JP4392671B2 (en) | Silicon production equipment | |
| JP2010042955A (en) | Inert gas recovery device in single crystal pulling device | |
| RU2707053C1 (en) | Method of cleaning metallurgical silicon from carbon | |
| JPH0416504A (en) | Method for purifying silicon | |
| CN103833037B (en) | A kind of polysilicon dephosphorization apparatus and method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| RD04 | Notification of resignation of power of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7424 Effective date: 20100325 |
|
| RD02 | Notification of acceptance of power of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7422 Effective date: 20100326 |
|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20110516 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20120912 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20120918 |
|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20121024 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20121127 |
|
| A02 | Decision of refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A02 Effective date: 20130326 |