JPH06104177B2 - Pressure vessel for high-purity gas storage - Google Patents
Pressure vessel for high-purity gas storageInfo
- Publication number
- JPH06104177B2 JPH06104177B2 JP61234786A JP23478686A JPH06104177B2 JP H06104177 B2 JPH06104177 B2 JP H06104177B2 JP 61234786 A JP61234786 A JP 61234786A JP 23478686 A JP23478686 A JP 23478686A JP H06104177 B2 JPH06104177 B2 JP H06104177B2
- Authority
- JP
- Japan
- Prior art keywords
- gas
- adsorbent
- pressure vessel
- purity
- purity gas
- 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
- F17C11/00—Use of gas-solvents or gas-sorbents in vessels
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Filling Or Discharging Of Gas Storage Vessels (AREA)
- Separation Of Gases By Adsorption (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、各種の高純度ガスを貯蔵する圧力容器に関す
る。TECHNICAL FIELD The present invention relates to a pressure vessel for storing various high-purity gases.
従来、圧力容器の内面に金や樹脂の特殊なコーテングを
施しているに過ぎず、不純ガスを除去する手段を備えて
いなかった。Conventionally, a special coating of gold or resin is merely applied to the inner surface of the pressure vessel, and no means for removing the impure gas is provided.
〔発明が解決しようとする問題点〕 しかし、例えば、O2,CO,CO2，H2Oなどの不純ガスが、容
器内壁からの脱離、容器への高純度ガス充填時の洩れ込
み、容器の出口側に備えられたバルブからの洩れ込み等
によって、圧力容器内の高純度ガスに混入し、いかに純
度の高いガス精製装置から圧力容器に充填しても、圧力
容器から供給されるガスの純度を、例えば、不純ガスが
1ppb以下というような超高純度に維持できない欠点があ
った。[Problems to be solved by the invention] However, for example, impure gases such as O 2 , CO, CO 2 , and H 2 O are desorbed from the inner wall of the container, leak when the container is filled with high-purity gas, Gas that is supplied from the pressure vessel no matter how high-purity the gas purification device fills the pressure vessel due to mixing with the high-purity gas in the pressure vessel due to leakage from the valve provided on the outlet side of the vessel. The purity of, for example, impure gas
There was a drawback that it could not be maintained in ultra-high purity such as 1 ppb or less.
本発明の目的は、圧力容器における純度低下を阻止し、
圧力容器から供給されるガスを確実に高純度に維持でき
るようにする点にある。An object of the present invention is to prevent a decrease in purity in a pressure vessel,
This is to ensure that the gas supplied from the pressure vessel can be maintained in high purity.
本発明の特徴構成は、不純ガスに対する吸着剤の充填層
を、容器内空間と容器出口の間で流動する高純度ガスが
前記充填層を通過するようにバルブより内方側に配置し
たことにあり、その作用効果は次の通りである。The characteristic configuration of the present invention is that the packed bed of the adsorbent for the impure gas is arranged on the inner side of the valve so that the high-purity gas flowing between the space inside the container and the container outlet passes through the packed bed. Yes, its effects are as follows.
つまり、容器内壁からの脱離で容器内の高純度ガスに不
純ガスが混入しても、貯蔵時のガス拡散によって不純ガ
スが吸着剤で除去されると共に、圧力容器からのガス供
給時に高純度ガスが吸着剤の充填層を通過するから、不
純ガスが確実に除去され、圧力容器からの供給ガスを確
実に高純度にできる。In other words, even if the impure gas is mixed with the high-purity gas in the container due to desorption from the inner wall of the container, the impure gas is removed by the adsorbent due to the gas diffusion during storage, and the high-purity gas is supplied when the gas is supplied from the pressure container. Since the gas passes through the packed bed of the adsorbent, the impure gas can be surely removed, and the supply gas from the pressure vessel can be surely made highly pure.
また、圧力容器への高純度ガス充填時に不純ガスが洩れ
込んでも、高純度ガスが吸着剤の充填層を通過するか
ら、不純ガスが確実に除去され、さらに、貯蔵時に圧力
容器の出口側に備えられたバルブから不純ガスが洩れ込
んでも、ガス拡散によって不純ガスが吸着剤で除去さ
れ、全体として、圧力容器におけるガスの純度低下を十
分に阻止できる。Further, even if the impure gas leaks when the high-purity gas is filled into the pressure vessel, the high-purity gas passes through the packed bed of the adsorbent, so that the impure gas is reliably removed. Even if the impure gas leaks from the provided valve, the impure gas is removed by the adsorbent due to the gas diffusion, and the purity of the gas in the pressure vessel can be sufficiently prevented from being lowered as a whole.
その結果、従来の圧力容器では不可能であった超高純度
のガス、つまり99.9999％（ドライベース）より高純度
のガスを、長期にわたって確実に供給でき、例えば不純
ガスが1ppb以下の不活性ガスを必要とする超々LSI製造
などの、超高純度ガスを必要とする業界へのガス供給に
極めて有効な高純度ガス貯蔵用圧力容器を提供できるよ
うになった。As a result, it is possible to reliably supply ultra-high purity gas, which is impossible with conventional pressure vessels, that is, gas with a purity higher than 99.9999% (dry base), for a long period of time. For example, the impure gas is an inert gas of 1 ppb or less. It has become possible to provide a pressure vessel for storing high-purity gas, which is extremely effective for gas supply to industries that require ultra-high-purity gas, such as ultra-ultra-chip manufacturing that requires.
次に実施例を示す。 Next, examples will be shown.
第１図に示すように、圧力容器（１）にバルブ（Ｖ）付
の給排管（２）を接続し、圧力容器（１）にその内部に
位置する状態でパンチングメタルや金網などから成る多
孔状容器（３）を取付け、その多孔状容器（３）内に不
純ガスに対する吸着剤の充填層（４）を形成し、容器内
空間（５）と容器出口（６）の間で流動する高純度ガス
が充填層（４）を通するように、充填層（４）を配置し
てある。As shown in FIG. 1, a pressure vessel (1) is connected to a supply / discharge pipe (2) with a valve (V), and is made of punching metal, wire mesh or the like while being located inside the pressure vessel (1). A porous container (3) is attached, an adsorbent filling layer (4) for impure gas is formed in the porous container (3), and flows between the container internal space (5) and the container outlet (6). The packed bed (4) is arranged so that the high-purity gas passes through the packed bed (4).
吸着剤の種類は貯蔵される高純度ガスの種類に見合って
適当に選定され、以下に具体例を示す。The type of adsorbent is appropriately selected according to the type of high-purity gas stored, and specific examples are shown below.
（イ） N2,Ar,He等の不活性ガス 第VIII族金属系化学吸着剤、ゼオライト系物理吸着剤の
両方又はいずれか一方 （ロ） O2及びH2、あるいは、それと不活性ガスの混合
ガス ゼオライト系物理吸着剤 （ハ） NH3，PH3，AsH3等のVa族水素化物、あるいは、
それと不活性ガスの混合ガスゼオライト系物理吸着剤あ
るいは活性炭系物理吸着剤あるいはCu系化学吸着剤 （ニ） SiH4，Si2H6の硅素水素化物、あるいは、それ
と不活性ガスの混合ガス ゼオライト系物理吸着剤あるいはCu系化学吸着剤 （ホ） CF4，CH2F2等のハロゲン化炭素、あるいは、そ
れと不活性ガスの混合ガス ゼオライト系物理吸着剤あるいはNi,Cu等の還元金属系
吸収剤あるいは活性炭系物理吸着剤 〔実施例〕 次に実施例を示す。(B) N 2, Ar, inert gas Group VIII metal-based chemical adsorbent such as He, whereas both or either zeolitic physical adsorbent (b) O 2 and H 2 or, the same inert gas Mixed gas Zeolite-based physical adsorbent (C) Va group hydrides such as NH 3 , PH 3 , and AsH 3 , or
Mixed gas of it and inert gas Zeolite physical adsorbent or activated carbon physical adsorbent or Cu chemical adsorbent (d) SiH 4 , Si 2 H 6 silicon hydride, or mixed gas of it and inert gas Zeolite Physical adsorbents or Cu-based chemical adsorbents (e) Carbon halides such as CF 4 and CH 2 F 2 , or mixed gas of them with inert gas Zeolite-based physical adsorbents or reduced metal-based adsorbents such as Ni and Cu Alternatively, activated carbon-based physical adsorbents [Examples] Next, Examples will be shown.
本発明の圧力容器は、内容積が50lで吸着剤の充填層容
積が2lであり、従来の圧力容器は吸着剤充填層の無いも
のである。The pressure vessel of the present invention has an inner volume of 50 liters and an adsorbent packed bed volume of 2 liters, and the conventional pressure vessel has no adsorbent packed bed.
配管に本発明の圧力容器と従来の圧力容器を各別に接続
し、それら配管を同種の通常グレードのガスでパージ
し、その後、同じ純度の高純度ガスを貯蔵した圧力容器
から配管に容器内の高純度ガスを10Nl/minの流量で供給
し、10分後に配管から供給される高純度ガス中に不純ガ
スの濃度を分析した。尚、O2，CH4はガスクロマトグラ
フ質量分析計で、かつ、H2O,COは半導体レーザー赤外分
光光度計で分析した。The pressure vessel of the present invention and the conventional pressure vessel are separately connected to the pipes, the pipes are purged with a gas of the same kind of normal grade, and then the pressure vessel storing the high-purity gas of the same purity is piped into the pipe. The high-purity gas was supplied at a flow rate of 10 Nl / min, and after 10 minutes, the concentration of the impure gas in the high-purity gas supplied from the pipe was analyzed. In addition, O 2 and CH 4 were analyzed by a gas chromatograph mass spectrometer, and H 2 O and CO were analyzed by a semiconductor laser infrared spectrophotometer.
実施例１ 高純度のN2を対象にし、吸着剤をNi系吸着剤とゼオライ
ト系吸着剤の混合物にし、下記表の結果を得た。Example 1 Targeting high purity N 2 , the adsorbent was a mixture of Ni adsorbent and zeolite adsorbent, and the results shown in the following table were obtained.
実験例２ 高純度のArを対象にし、実験例１と同様の吸着剤にし、
下記表に示す結果を得た。 Experimental Example 2 Targeting high-purity Ar, the same adsorbent as in Experimental Example 1 was used.
The results shown in the table below were obtained.
実験例３ 高純度のHeを対象にし、実験例１と同様の吸着剤にし、
下記表に示す結果を得た。 Experimental Example 3 Targeting high-purity He, using the same adsorbent as in Experimental Example 1,
The results shown in the table below were obtained.
実験例４ 高純度のO2を対象にし、吸着剤をゼオライト系吸着剤に
し、H2O濃度を調べた結果、本発明の圧力容器ではH2O＜
400ppbであり、従来の圧力容器ではH2O＜100ppmであっ
た。 Experimental Example 4 As a result of investigating high purity O 2 and using a zeolite-based adsorbent as the adsorbent and examining the H 2 O concentration, it was found that H 2 O <in the pressure vessel of the present invention.
It was 400 ppb, and H 2 O <100 ppm in the conventional pressure vessel.
実験例５ 高純度のNH3を対象にし、吸着剤をCu系化学吸着剤と活
性炭系吸着剤の混合物にし、下記表に示す結果を得た。Experimental Example 5 Targeting high-purity NH 3 , the adsorbent was a mixture of Cu-based chemical adsorbent and activated carbon-based adsorbent, and the results shown in the following table were obtained.
実験例６ 高純度のAsH3を対象にし、実験例５と同様の吸着剤に
し、下記表に示す結果を得た。 Experimental Example 6 A high-purity AsH 3 was used as a target and the same adsorbent as in Experimental Example 5 was used, and the results shown in the following table were obtained.
実験例７ 高純度のSiH4を対象にし、吸着剤をゼオライト系吸着剤
にし、H2O濃度を調べた結果、本発明の圧力容器ではH2O
＜400ppbであり、従来の圧力容器ではH2O＜1ppmであっ
た。 Experimental Example 7 Targeting high-purity SiH 4 , the adsorbent was a zeolite-based adsorbent, and the H 2 O concentration was examined. As a result, in the pressure vessel of the present invention, H 2 O was used.
<400 ppb and H 2 O <1 ppm in the conventional pressure vessel.
実験例８ 高純度のCF4を対象にし、吸着剤をCu系化学吸収剤とゼ
オライト系吸着剤の混合物にし、下記表に示す結果を得
た。Experimental Example 8 Targeting high-purity CF 4 , the adsorbent was a mixture of a Cu-based chemical absorbent and a zeolite-based adsorbent, and the results shown in the following table were obtained.
実験例９ 高純度のCHF3を対象にし、実施例８と同様の吸着剤に
し、下記表に示す結果を得た。 Experimental Example 9 A high-purity CHF 3 was used as an adsorbent similar to that in Example 8, and the results shown in the following table were obtained.
以上、いずれの実験例においても、本発明の圧力容器を
利用すると従来よりも大巾に純度の高いガスを供給でき
る。 As described above, in any of the experimental examples, by using the pressure vessel of the present invention, a gas having a much higher purity than the conventional one can be supplied.
次に別実施例を示す。 Next, another embodiment will be described.
吸着剤の充填層（４）を設けるに、構造や配置等におい
て適宜変更が可能であり、例えば第２図に示すように、
バルブ（Ｖ）付給排管（２）の複数本を圧力容器（１）
に接続して、吸着剤の充填層（４）を給排管（２）に対
して各別に設けてもよい。また、第３図に示すように、
給排管（２）を圧力容器（１）内に突出させて、粒状吸
着剤が沈降して、充填層（４）の上面と圧力容器（１）
の間に隙間（７）が生じても、圧力容器（１）内の高純
度ガスが確実に充填層（４）を通って給排管（２）に送
られるようにし、そして、粒状吸着剤が給排管（２）内
に入らないように、網などの適当なフィルター（８）を
設けてもよい。The structure and arrangement of the adsorbent filling layer (4) can be appropriately changed. For example, as shown in FIG.
A plurality of supply / discharge pipes (2) with valves (V) are installed in a pressure vessel (1)
The adsorbent filling layer (4) may be separately provided for the supply / discharge pipe (2). Also, as shown in FIG.
The supply / discharge pipe (2) is projected into the pressure vessel (1), and the granular adsorbent is settled, and the upper surface of the packed bed (4) and the pressure vessel (1).
Even if a gap (7) is formed between the two, it is ensured that the high-purity gas in the pressure vessel (1) is sent to the supply / discharge pipe (2) through the packed bed (4), and the granular adsorbent A suitable filter (8) such as a net may be provided to prevent the water from entering the supply / discharge pipe (2).
尚、特許請求の範囲の項に図面との対照を便利にする為
に符号を記すが、該記入により本発明は添付図面の構造
に限定されるものではない。It should be noted that reference numerals are added to the claims for convenience of comparison with the drawings, but the present invention is not limited to the structures of the accompanying drawings by the entry.
第１図は本発明の実施例を示す概念図、第２図及び第３
図は本発明の各別の実施例を示す概念図である。 （４）……吸着剤の充填層、（５）……容器内空間、
（６）……容器出口、（Ｖ）……バルブ。FIG. 1 is a conceptual diagram showing an embodiment of the present invention, FIG. 2 and FIG.
The drawings are conceptual diagrams showing different embodiments of the present invention. (4) ... adsorbent packed bed, (5) ... internal container space,
(6) …… Vessel outlet, (V) …… Valve.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 松本 勝 大阪府大阪市東区平野町５丁目１番地 大 阪瓦斯株式会社内 (72)発明者 和田 昌夫 大阪府大阪市東区平野町５丁目１番地 大 阪瓦斯株式会社内 (72)発明者 木村 正城 大阪府大阪市東区平野町５丁目１番地 近 畿冷熱株式会社内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Masaru Matsumoto, 5-1, Hirano-cho, Higashi-ku, Osaka, Osaka Prefecture, Osaka, Osaka Gas Co., Ltd. (72) Masao Wada, 5--1, Hirano-cho, Higashi-ku, Osaka, Osaka Inside Han Gas Co., Ltd. (72) Inventor Masaki Kimura 5-1, Hiranocho, Higashi-ku, Osaka City, Osaka Prefecture
Claims (1)
を、容器内空間（５）と容器出口（６）の間で流動する
高純度ガスが前記充填層（４）を通過するようにバルブ
（Ｖ）より内方側に配置してある高純度ガス貯蔵用圧力
容器。1. A packed bed of adsorbent for impure gas (4).
Is a high-purity gas arranged inside the valve (V) so that the high-purity gas flowing between the container internal space (5) and the container outlet (6) passes through the packed bed (4). Storage pressure vessel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61234786A JPH06104177B2 (en) | 1986-10-02 | 1986-10-02 | Pressure vessel for high-purity gas storage |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61234786A JPH06104177B2 (en) | 1986-10-02 | 1986-10-02 | Pressure vessel for high-purity gas storage |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6388017A JPS6388017A (en) | 1988-04-19 |
| JPH06104177B2 true JPH06104177B2 (en) | 1994-12-21 |
Family
ID=16976355
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61234786A Expired - Lifetime JPH06104177B2 (en) | 1986-10-02 | 1986-10-02 | Pressure vessel for high-purity gas storage |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06104177B2 (en) |
Families Citing this family (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5704967A (en) * | 1995-10-13 | 1998-01-06 | Advanced Technology Materials, Inc. | Fluid storage and delivery system comprising high work capacity physical sorbent |
| US6132492A (en) * | 1994-10-13 | 2000-10-17 | Advanced Technology Materials, Inc. | Sorbent-based gas storage and delivery system for dispensing of high-purity gas, and apparatus and process for manufacturing semiconductor devices, products and precursor structures utilizing same |
| US5518528A (en) * | 1994-10-13 | 1996-05-21 | Advanced Technology Materials, Inc. | Storage and delivery system for gaseous hydride, halide, and organometallic group V compounds |
| US6083298A (en) * | 1994-10-13 | 2000-07-04 | Advanced Technology Materials, Inc. | Process for fabricating a sorbent-based gas storage and dispensing system, utilizing sorbent material pretreatment |
| US6204180B1 (en) | 1997-05-16 | 2001-03-20 | Advanced Technology Materials, Inc. | Apparatus and process for manufacturing semiconductor devices, products and precursor structures utilizing sorbent-based fluid storage and dispensing system for reagent delivery |
| US5707424A (en) * | 1994-10-13 | 1998-01-13 | Advanced Technology Materials, Inc. | Process system with integrated gas storage and delivery unit |
| US5676735A (en) * | 1996-10-31 | 1997-10-14 | Advanced Technology Materials, Inc. | Reclaiming system for gas recovery from decommissioned gas storage and dispensing vessels and recycle of recovered gas |
| US6027547A (en) * | 1997-05-16 | 2000-02-22 | Advanced Technology Materials, Inc. | Fluid storage and dispensing vessel with modified high surface area solid as fluid storage medium |
| US5985008A (en) * | 1997-05-20 | 1999-11-16 | Advanced Technology Materials, Inc. | Sorbent-based fluid storage and dispensing system with high efficiency sorbent medium |
| US5851270A (en) * | 1997-05-20 | 1998-12-22 | Advanced Technology Materials, Inc. | Low pressure gas source and dispensing apparatus with enhanced diffusive/extractive means |
| US6406519B1 (en) * | 1998-03-27 | 2002-06-18 | Advanced Technology Materials, Inc. | Gas cabinet assembly comprising sorbent-based gas storage and delivery system |
| US6660063B2 (en) | 1998-03-27 | 2003-12-09 | Advanced Technology Materials, Inc | Sorbent-based gas storage and delivery system |
| US7105037B2 (en) | 2002-10-31 | 2006-09-12 | Advanced Technology Materials, Inc. | Semiconductor manufacturing facility utilizing exhaust recirculation |
| US6991671B2 (en) | 2002-12-09 | 2006-01-31 | Advanced Technology Materials, Inc. | Rectangular parallelepiped fluid storage and dispensing vessel |
| US8002880B2 (en) | 2002-12-10 | 2011-08-23 | Advanced Technology Materials, Inc. | Gas storage and dispensing system with monolithic carbon adsorbent |
| US8679231B2 (en) | 2011-01-19 | 2014-03-25 | Advanced Technology Materials, Inc. | PVDF pyrolyzate adsorbent and gas storage and dispensing system utilizing same |
| US9126139B2 (en) | 2012-05-29 | 2015-09-08 | Entegris, Inc. | Carbon adsorbent for hydrogen sulfide removal from gases containing same, and regeneration of adsorbent |
-
1986
- 1986-10-02 JP JP61234786A patent/JPH06104177B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6388017A (en) | 1988-04-19 |
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