JPS6163517A - Method of purifying monosilane - Google Patents
Method of purifying monosilaneInfo
- Publication number
- JPS6163517A JPS6163517A JP18277584A JP18277584A JPS6163517A JP S6163517 A JPS6163517 A JP S6163517A JP 18277584 A JP18277584 A JP 18277584A JP 18277584 A JP18277584 A JP 18277584A JP S6163517 A JPS6163517 A JP S6163517A
- Authority
- JP
- Japan
- Prior art keywords
- monosilane
- storage tank
- hydrogen
- nitrogen
- oxygen
- 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.)
- Granted
Links
Landscapes
- Silicon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
〔技術分野〕
本発明は、モノシランの精製方法に関する。更に詳しく
は、酸素、窒素、水素、アルゴン、ヘリウム、メタン等
のモノシランより沸点の低いガスを含有しないモノシラ
ンを取得する方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Technical Field] The present invention relates to a method for purifying monosilane. More specifically, the present invention relates to a method for obtaining monosilane that does not contain gases having a boiling point lower than monosilane, such as oxygen, nitrogen, hydrogen, argon, helium, and methane.
エレクトロ産業市場の急成長に伴いモノシランは、■Ｃ
１太陽電池、光感光体ドラム等における半導体薄膜を形
成するための原料ガスとして近年急激に需要が増加して
いる。モノシランガスの製造方法としては、四塩化硅素
又は三塩化硅素等のクロロシラン類、アルカリ金属ハイ
ドライド又はアルキルアルミニウムハイドライドで還元
する方法あるいは、Ｍｇ２Ｓｉと塩酸又は塩化アンモニ
ウム等を反応させる方法が一般的である。With the rapid growth of the electronic industry market, monosilane has become
1. Demand has increased rapidly in recent years as a raw material gas for forming semiconductor thin films in solar cells, photosensitive drums, etc. A common method for producing monosilane gas is a method of reduction with chlorosilanes such as silicon tetrachloride or silicon trichloride, an alkali metal hydride or an alkyl aluminum hydride, or a method of reacting Mg2Si with hydrochloric acid or ammonium chloride.
これらの方法により得られるモノシランガスは、活性炭
やモレキュラーシーブ等の吸着剤を用いて １吸着
精製したり、蒸留により精製したり、あるいは、これら
を組み合わせて精製し、実用に供していた。これらの精
製方法は、モノシランの沸点（−１１２℃）よりも高い
沸点の不純物に対しては、充分な精製効果があるが、酸
素、窒素、水素、アルゴン、ヘリウム、メタン等の、モ
ノシランより沸点の低い不純物に対しては、充分な精製
効果が得られない。従って、このような微量の不純物の
混入したまま、ボンベ等の容器に充填されて各種用途に
使用されていた。Monosilane gas obtained by these methods has been purified by adsorption using an adsorbent such as activated carbon or molecular sieve, purified by distillation, or purified by a combination of these methods for practical use. These purification methods have a sufficient purification effect on impurities with a boiling point higher than that of monosilane (-112°C), but impurities with boiling points higher than monosilane, such as oxygen, nitrogen, hydrogen, argon, helium, and methane, A sufficient purification effect cannot be obtained for impurities with low . Therefore, it has been filled into containers such as cylinders and used for various purposes with such trace amounts of impurities mixed in.
しかしながら、高純度を要求される半導体、太陽電池、
光感光体ドラム等の用途には、製品モノシランガス中の
酸素、窒素、水素、アルゴン、へリウム、メタン等の低
沸点物質の不純物の混入は、当該用途における製品の品
質に大きな影響を与える。本発明者らは、とくに、非晶
質シリコン太陽電池用には、原料モノシラン中に酸素や
窒素等の不純物が、非常に微小量存在しただけで該電池
の性能、とくに経日劣化特性に著しい影響を及ぼすこと
を見い出した。However, semiconductors, solar cells, etc. that require high purity,
For applications such as photoreceptor drums, contamination of impurities with low boiling point substances such as oxygen, nitrogen, hydrogen, argon, helium, and methane in the product monosilane gas has a significant impact on the quality of the product in the application. The present inventors have found that, in particular, for amorphous silicon solar cells, the presence of very small amounts of impurities such as oxygen and nitrogen in the raw material monosilane significantly affects the performance of the cell, especially its aging characteristics. found that it has an effect.
しかして、本発明の目的は、かかる非晶質シリコン太陽
電池のごとき特に高品質を要求される分野に好適に使用
できるように、高純度のモノシランガスを容器に充填貯
蔵する方法を提供することである。Therefore, an object of the present invention is to provide a method for filling and storing a container with high-purity monosilane gas so that it can be suitably used in fields that require particularly high quality, such as amorphous silicon solar cells. be.
すなわち、本発明の上記目的は液体モノシランの貯槽内
でモノシランの還流下に保持することにより達成される
。以下、本発明の詳細な説明する。That is, the above objects of the present invention are achieved by maintaining monosilane under reflux in a storage tank of liquid monosilane. The present invention will be explained in detail below.
本発明の適用しうるモノシランは、クロロシラン類を還
元剤を用いて還元して製造したものも、Ｍｇ２Ｓｉのご
とき合金と塩酸又は塩化アンモニウム等を反応させて製
造したものも、いずれでもよい。The monosilane to which the present invention can be applied may be one produced by reducing chlorosilanes using a reducing agent, or one produced by reacting an alloy such as Mg2Si with hydrochloric acid or ammonium chloride.
いかなる製造プロセスを経るにせよ、精製された水素を
同伴しているモノシランは、凝縮されて製品ホルダーに
貯液される。Regardless of the manufacturing process, the monosilane entrained with purified hydrogen is condensed and stored in the product holder.
本発明においては、この貯槽内で、モノシランを還流下
、好ましくは、モノシランの沸点である一１１２°Ｃ付
近に保持することにより精製が行なわれる。しかるのち
、貯槽から、好適には、貯槽の下部から、ポンプで抜き
出し、気化器で加熱してボンベ等の容器に充填する。ポ
ンプで抜き出す際には、モノシランを液状で抜き出して
もよいが、また、還流下に保持した貯槽の気相部からモ
ノシランを圧縮器で抜出し、容器に充填してもよい。In the present invention, purification is carried out by maintaining monosilane under reflux in this storage tank, preferably at around -112°C, which is the boiling point of monosilane. Thereafter, it is extracted from the storage tank, preferably from the lower part of the storage tank, with a pump, heated with a vaporizer, and filled into a container such as a cylinder. When extracting monosilane with a pump, monosilane may be extracted in liquid form, but monosilane may also be extracted with a compressor from the gas phase of a storage tank held under reflux and filled into a container.
（実施例） 以下本発明を実施例により具体的に説明する。(Example) The present invention will be specifically explained below using examples.
（実施例 １）
４０／のジャケット付液体シランホルダーに３−の伝熱
面積を有する逆流コンデンサーを設置した。逆流コンデ
ンサーは、５ ｋｇ ／ ｔｒｉ Ｇの圧力の液体窒素
で冷却した。ホルダ一部分は、７５朋厚のウレタンフオ
ームで保冷した。シャケナトには液体窒素を流さない。(Example 1) A backflow condenser having a heat transfer area of 3-2 was installed in a 40-mm jacketed liquid silane holder. The counterflow condenser was cooled with liquid nitrogen at a pressure of 5 kg/tri G. A portion of the holder was kept cool with 75 mm thick urethane foam. Do not pour liquid nitrogen into Shakenat.
このホルダーに、毎時ｔｏＮｍ’のキャリアガス（窒素
１５００Ｆ。This holder was filled with toNm' of carrier gas (nitrogen 1500F) per hour.
酸素とアルゴン１００Ｐを含有する水素）を用いて毎時
１．２ ｋｑのシランを１０時間供給し、液体シラン１
２に９を貯液した。ホルダー内のシランは沸騰状態に保
持され逆流コンデンサーで還流される。1.2 kq of silane was supplied per hour using hydrogen containing oxygen and 100 P of argon, and liquid silane 1
9 was stored in 2. The silane in the holder is kept at boiling point and refluxed in a counterflow condenser.
この貯槽下部からポンプにより液体シランを抜き出し、
気化させたのち、４７１ボンベ２本にシランガスを充填
した。ボンベ中の不純物を分析したところ、窒素０．７
Ｆ、酸素とアルゴンの和０．３１Ｆ。Liquid silane is extracted from the bottom of this storage tank using a pump,
After vaporization, two 471 cylinders were filled with silane gas. Analysis of impurities in the cylinder revealed that nitrogen was 0.7
F, the sum of oxygen and argon is 0.31F.
水素５１Ｆ、メタン不検出であった。Hydrogen 51F and methane were not detected.
比較例 １
ホルダーのジャケットに液体窒素を通して、−１２０℃
に保持した以外は実施例１と同様にしてモノシランをボ
ンベに充填した結果、ボンベ中の不純物は、窒素１２２
、酸素とアルゴンの和４Ｐであった。Comparative example 1 Liquid nitrogen was passed through the jacket of the holder at -120°C.
As a result of filling a cylinder with monosilane in the same manner as in Example 1 except that the impurities in the cylinder were nitrogen 122
, the sum of 4P of oxygen and argon.
〔発明の効果及び産業上の利用可能性〕本発明方法によ
り精製されたモノシランを、例えば、４７１ボンベに充
填した場合、窒素の混入量は、ＩＰ１以下、酸素の混入
量は、０．５１１ｐ以下とすることができ、水素も１０
−以下となり、さらに、アルゴン、ヘリウム、メタン等
は不検出というような超高純度シリコンを容器に充填す
ることが可能となる。したがって、このようにして容器
に充填されたモノシランは、Ｉ０１太陽電池、光感光体
ドラム等の用途に、効果的に供されるものである。[Effects and industrial applicability of the invention] When monosilane purified by the method of the present invention is filled into a 471 cylinder, for example, the amount of nitrogen mixed in is IP1 or less, and the amount of oxygen mixed in is 0.511p or less. and hydrogen is also 10
- or less, and furthermore, it becomes possible to fill a container with ultra-high purity silicon in which argon, helium, methane, etc. are not detected. Therefore, the monosilane filled into the container in this way can be effectively used for applications such as I01 solar cells and photosensitive drums.
Claims (1)
保持することを特徴とするモノシランの精製方法。(1) A method for purifying monosilane, which comprises maintaining monosilane under reflux in a liquid monosilane storage tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18277584A JPS6163517A (en) | 1984-09-03 | 1984-09-03 | Method of purifying monosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18277584A JPS6163517A (en) | 1984-09-03 | 1984-09-03 | Method of purifying monosilane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6163517A true JPS6163517A (en) | 1986-04-01 |
| JPH0443845B2 JPH0443845B2 (en) | 1992-07-17 |
Family
ID=16124198
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18277584A Granted JPS6163517A (en) | 1984-09-03 | 1984-09-03 | Method of purifying monosilane |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6163517A (en) |
-
1984
- 1984-09-03 JP JP18277584A patent/JPS6163517A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0443845B2 (en) | 1992-07-17 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |