JPH0459518B2 - - Google Patents
Info
- Publication number
- JPH0459518B2 JPH0459518B2 JP59182773A JP18277384A JPH0459518B2 JP H0459518 B2 JPH0459518 B2 JP H0459518B2 JP 59182773 A JP59182773 A JP 59182773A JP 18277384 A JP18277384 A JP 18277384A JP H0459518 B2 JPH0459518 B2 JP H0459518B2
- Authority
- JP
- Japan
- Prior art keywords
- monosilane
- container
- nitrogen
- storage tank
- filling
- 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.)
- Expired - Lifetime
Links
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C6/00—Methods and apparatus for filling vessels not under pressure with liquefied or solidified gases
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2221/00—Handled fluid, in particular type of fluid
- F17C2221/01—Pure fluids
- F17C2221/012—Hydrogen
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2221/00—Handled fluid, in particular type of fluid
- F17C2221/03—Mixtures
- F17C2221/037—Containing pollutant, e.g. H2S, Cl
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2223/00—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel
- F17C2223/01—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel characterised by the phase
- F17C2223/0146—Two-phase
- F17C2223/0153—Liquefied gas, e.g. LPG, GPL
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2227/00—Transfer of fluids, i.e. method or means for transferring the fluid; Heat exchange with the fluid
- F17C2227/01—Propulsion of the fluid
- F17C2227/0128—Propulsion of the fluid with pumps or compressors
- F17C2227/0135—Pumps
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2227/00—Transfer of fluids, i.e. method or means for transferring the fluid; Heat exchange with the fluid
- F17C2227/01—Propulsion of the fluid
- F17C2227/0128—Propulsion of the fluid with pumps or compressors
- F17C2227/0157—Compressors
-
- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Filling Or Discharging Of Gas Storage Vessels (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、高純度モノシランの容器充填方法に
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容器に充填
する方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for filling containers with high purity monosilane. More specifically, the present invention relates to a method of filling a container with monosilane that does not contain gases having a boiling point lower than that of monosilane, such as oxygen, nitrogen, hydrogen, argon, helium, and methane.
エレクトロニクス産業市場の急成長に伴いモノ
シラン、はIC、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を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 electronics industry market, demand for monosilane has increased rapidly in recent years as a raw material gas for forming semiconductor thin films in ICs, solar cells, photosensitive drums, etc. Common methods for producing monosilane gas include reducing chlorosilanes such as silicon tetrachloride or silicon trichloride with an alkali metal hydride or alkyl aluminum hydride, or reacting Mg 2 Si 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、活性炭やモレキユラーシーブ等の吸着剤を用
いて吸着精製したり、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。 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 are based on the boiling point of monosilane (-
It has a sufficient purification effect on impurities with a boiling point higher than 112℃), but it has a sufficient purification effect on impurities with a boiling point lower than monosilane, such as oxygen, nitrogen, hydrogen, argon, helium, and methane. is not obtained.
従つて、このような微量の不純物が混入したま
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。 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、ヘ
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
すことを見出した。
However, for applications such as semiconductors, solar cells, and photoreceptor drums that require high purity, contamination of low-boiling point substances such as oxygen, nitrogen, hydrogen, argon, helium, and methane in the product monosilane gas is a problem. It has a significant impact on the quality of the product in its application. The present inventors have found that, especially for amorphous silicon solar cells, the presence of very small amounts of impurities such as oxygen and nitrogen in the raw material monosilane has a significant effect on the performance of the cell, especially its aging characteristics. It was found that
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 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. .
本発明の上記目的は、低沸点ガスを含有しない
モノシランを容器に充填するにあたり、液体モノ
シランの貯槽内でモノシランを還流下に保持した
後、該貯槽から容器に充填することにより達成さ
れる。
The above object of the present invention is achieved by, when filling a container with monosilane that does not contain a low boiling point gas, by holding the monosilane under reflux in a liquid monosilane storage tank and then filling the container from the storage tank.
以下、本発明を詳細に説明する。 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。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ラシンは、凝縮され
て製品ホルダー（貯槽）に貯液される。 Monosilanes to which the present invention can be applied include those produced by reducing chlorosilanes using a reducing agent;
Any material manufactured by reacting an alloy such as Mg 2 Si with hydrochloric acid or ammonium chloride may also be used. Regardless of the manufacturing process, monolasin entrained with purified hydrogen is condensed and stored in a 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−
112℃付近に沸騰状態に保持し、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
るものである。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
抜き出し、容器に充填してもよい。 In the present invention, the monosilane is refluxed in this storage tank, preferably at the boiling point of the monosilane.
It is kept in a boiling state at around 112°C, and then 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 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.
以下本発明を実施例により具体的に説明する。 The present invention will be specifically explained below using examples.
実施例 １
40のジヤケツト付液体シランホルダーに３m2
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、５Kg／cm2Ｇの圧力の液
体窒素で冷却した。ホルダー部分は、75mm厚のウ
レタンホームで保冷した。ジヤケツトには液体窒
素を流さない。このホルダーに毎時10Nm3のキア
リアガス（窒素1500ppm、酸素とアルゴン
100ppmを含有する水素）を用いて毎時1.2Kgのシ
ランを10時間供給し、液体シラン12Kg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。Example 1 3m2 liquid silane holder with 40 jackets
A countercurrent condenser with a heat transfer area of The counterflow condenser was cooled with liquid nitrogen at a pressure of 5 Kg/cm 2 G. The holder part was kept cool with a 75mm thick urethane foam. Do not pour liquid nitrogen into the jacket. 10Nm3 of Chiaria gas (nitrogen 1500ppm, oxygen and argon) per hour to this holder
Hydrogen containing 100 ppm was used to supply 1.2 Kg of silane per hour for 10 hours, and 12 Kg of liquid silane was stored. 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、47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0.7ppm、酸素とアルゴンの和
0.3ppm、水素5ppm、メタン不検出であつた。 Liquid silane was extracted from the bottom of the storage tank using a pump, vaporized, and then filled into two 47 cylinders with silane gas. Analysis of impurities in the cylinder revealed 0.7 ppm of nitrogen, the sum of oxygen and argon.
0.3ppm, hydrogen 5ppm, and no methane detected.
比較例 １
ホルダーのジヤケツ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12ppm、酸素とアルゴンの和4ppmで
あつた。Comparative Example 1 Pass liquid nitrogen through the jacket of the holder and -
A cylinder was filled with monosilane in the same manner as in Example 1 except that the temperature was maintained at 120°C. As a result, the impurities in the cylinder were 12 ppm of nitrogen and 4 ppm of oxygen and argon.
本発明方法によれば、例えば47ボンベに10Kg
のモノシランを充填した場合、窒素の混入量は
1ppm以下、酸素の混入量は0.5ppm以下とするこ
とができ、水素も10ppm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。したがつて、このようにして容器に充填
されたモノシランは、IC、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。
According to the method of the present invention, for example, 10 kg in 47 cylinders
When filled with monosilane, the amount of nitrogen mixed in is
It is possible to fill containers with ultra-high purity silicon, which can reduce the amount of mixed oxygen to 1ppm or less, the amount of oxygen mixed in to 0.5ppm or less, and the hydrogen content to 10ppm or less, and furthermore, argon, helium, methane, etc. are not detected. Become. Therefore, the monosilane filled into the container in this manner can be effectively used for applications such as ICs, solar cells, and photosensitive drums.
第１図は、本発明の高純度モノシランの容器充
填に用いた装置の一例を示す図である。
１……シランホルダー、２……シランホルダー
ジヤケツト、３……逆流コンデンサー、４……低
沸成分を含むモノシランガスの入口、５……低沸
成分ガスの出口、６……液体シランの抜き出しラ
イン（液体シランの充填ライン）、７……液体窒
素の入口、８……液体窒素の出口。
FIG. 1 is a diagram showing an example of an apparatus used for filling containers with high-purity monosilane of the present invention. 1... Silane holder, 2... Silane holder jacket, 3... Backflow condenser, 4... Inlet for monosilane gas containing low-boiling components, 5... Outlet for low-boiling component gas, 6... Liquid silane extraction line (liquid silane filling line), 7...liquid nitrogen inlet, 8...liquid nitrogen outlet.
Claims (1)
充填するにあたり、液体モノシランの貯槽内でモ
ノシランを還流下に保持した後、該貯槽から容器
に充填することを特徴とする高純度モノシランの
容器充填方法。1. A method for filling a container with high-purity monosilane, which is characterized in that when filling a container with monosilane that does not contain a low-boiling point gas, the monosilane is held under reflux in a liquid monosilane storage tank, and then the container is filled from the storage tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59182773A JPS6162699A (en) | 1984-09-03 | 1984-09-03 | Method of filling container with high-purity monosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59182773A JPS6162699A (en) | 1984-09-03 | 1984-09-03 | Method of filling container with high-purity monosilane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6162699A JPS6162699A (en) | 1986-03-31 |
| JPH0459518B2 true JPH0459518B2 (en) | 1992-09-22 |
Family
ID=16124164
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59182773A Granted JPS6162699A (en) | 1984-09-03 | 1984-09-03 | Method of filling container with high-purity monosilane |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6162699A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107539990B (en) * | 2016-07-22 | 2019-08-02 | 南京大学 | A kind of porous silicon nanomaterial and its preparation method and application |
-
1984
- 1984-09-03 JP JP59182773A patent/JPS6162699A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6162699A (en) | 1986-03-31 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |