JP2532297B2 - Inert gas recovery device for single crystal pulling device - Google Patents
Inert gas recovery device for single crystal pulling deviceInfo
- Publication number
- JP2532297B2 JP2532297B2 JP2199276A JP19927690A JP2532297B2 JP 2532297 B2 JP2532297 B2 JP 2532297B2 JP 2199276 A JP2199276 A JP 2199276A JP 19927690 A JP19927690 A JP 19927690A JP 2532297 B2 JP2532297 B2 JP 2532297B2
- Authority
- JP
- Japan
- Prior art keywords
- inert gas
- gas
- single crystal
- purification unit
- crystal pulling
- 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 - Fee Related
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ この発明は、単結晶引上装置に使用される不活性ガス
（特にアルゴンガス）のリサイクルを可能にする不活性
ガス回収装置に関するものである。TECHNICAL FIELD The present invention relates to an inert gas recovery device that enables recycling of an inert gas (particularly argon gas) used in a single crystal pulling device. .
［従来の技術］ 従来、単結晶引上装置に使用されるアルゴン等の不活
性ガスは、そのまま廃棄されていたが、近年、高価であ
る不活性ガスを回収循環使用する回収装置が種々提案さ
れている。例えば、特開昭59−39800号公報、特公平２
−14315号公報等がある。[Prior Art] Conventionally, the inert gas such as argon used in the single crystal pulling apparatus has been discarded as it is, but in recent years, various recovery apparatuses for recovering and circulating expensive inert gas have been proposed. ing. For example, JP-A-59-39800, Japanese Patent Publication No. 2
-14315 publication.
従来の回収装置は、CO、CO2、O2、H2等の不純物を酸
素または空気と反応させて除去するものである。The conventional recovery device removes impurities such as CO, CO2, O2, and H2 by reacting with oxygen or air.
［発明が解決しようとする課題］ 単結晶引上装置から回収されるアルゴンガス中のCO、
CO2、O2等の不純物は濃度が変化する。つまり、引上炉
中に使用されているカーボンパーツのライフ（使用回
数）や炉内の圧力によって不純物の濃度が非常に変化す
る。このため、回収アルゴンガス中に不純物が回収装置
の処理能力以上に含まれている場合には、回収アルゴン
ガスをそのまま廃棄せざるをえない。廃棄を避けるに
は、不純物濃度によって酸素供給量を変化させる装置を
増設し、かつ不純物吸着塔を増設しなければならない。[Problems to be Solved by the Invention] CO in argon gas recovered from a single crystal pulling apparatus,
The concentration of impurities such as CO2 and O2 changes. That is, the concentration of impurities greatly changes depending on the life (number of times of use) of the carbon parts used in the pulling furnace and the pressure in the furnace. For this reason, when impurities are contained in the recovered argon gas in excess of the processing capacity of the recovery device, the recovered argon gas must be discarded as it is. In order to avoid disposal, it is necessary to add an apparatus that changes the oxygen supply amount depending on the impurity concentration and an impurity adsorption tower.
また、従来の回収装置では、N2成分が除去できず、回
収リサイクル中にN2濃度が高くなり、２回程度の回収リ
サイクルしか実行出来ないことが多かった。Further, in the conventional recovery device, the N2 component cannot be removed, the N2 concentration becomes high during the recovery / recycling, and the recovery / recycling can be performed only about twice.
本発明の目的は不純物濃度に左右されず、しかも多く
の回収リサイクルが可能な単結晶引上装置用不活性ガス
回収装置を提供することである。An object of the present invention is to provide an inert gas recovery apparatus for a single crystal pulling apparatus, which is not affected by the impurity concentration and can be recovered and recycled in large quantities.
［課題を解決するための手段］ 本発明の要旨は、単結晶引上装置から回収されるN2ガ
ス含有の不活性ガス中の不純物を水によって除去するた
めの液封式真空ポンプと、N2ガス含有の不活性ガスをPS
A方式で精製して少くともN2ガスを除去するPSA精製ユニ
ットと、不活性ガスを触媒方式で精製する不活性ガス精
製ユニットを備え、N2ガスを低減した状態で不活性ガス
を回収する構成にしたことを特徴とする単結晶引上用不
活性ガス回収装置である。[Means for Solving the Problems] The gist of the present invention is to provide a liquid-ring vacuum pump for removing impurities in N 2 gas-containing inert gas recovered from a single crystal pulling apparatus with water, 2 Inert gas containing gas PS
It is equipped with a PSA purification unit that purifies by A method to remove at least N 2 gas and an inert gas purification unit that purifies inert gas by a catalytic method, and recovers inert gas with N 2 gas reduced. It is an inert gas recovery apparatus for pulling a single crystal characterized by having a configuration.
［作用］ 単結晶引上装置で使用された不活性ガス（例えばアル
ゴンガス）は、液封式真空ポンプで引かれ、その液封式
真空ポンプ中の水によって、SiO微粉が取り除かれる。
液封式真空ポンプは、油回転式の真空ポンプのようにC
O、CO2、CnHmのガスを発生することがない。[Operation] The inert gas (for example, argon gas) used in the single crystal pulling apparatus is pulled by the liquid ring vacuum pump, and the fine SiO 2 powder is removed by the water in the liquid ring vacuum pump.
The liquid ring vacuum pump is similar to an oil rotary vacuum pump.
Does not generate O, CO2 or CnHm gas.
液封式真空ポンプから送られたアルゴンガスはPSA（P
ressure Swing Absorption:ガスの圧力変化により吸
着・脱着をするガスの分離精製）方式の精製ユニット
（本明細書ではPSA精製ユニットと略称する）によってN
2、CO、CO2ガスが除去される。The argon gas sent from the liquid ring vacuum pump is PSA (P
ressure Swing Absorption: Gas separation and purification that adsorbs and desorbs due to changes in gas pressure) (purification unit in this specification)
2, CO, CO2 gas is removed.
これらの不純物ガスが除去されたあと、アルゴンガス
は、不活性ガス精製ユニットに送られ、そこでO2、H2、
微量残留CO2等とアルゴンガスが分離精製される。After these impurity gases have been removed, the argon gas is sent to an inert gas purification unit where O2, H2,
Trace amount of residual CO2 etc. and argon gas are separated and purified.
このようにして得られた高純度のアルゴンガスを回収
してリサイクル使用する。The high-purity argon gas thus obtained is collected and recycled.
［実施例］ 第１図に示すように、それ自体公知の単結晶引上装置
１で使用されてアルゴンガスは、回収ガスとして液封式
つまり水封式と真空ポンプ２に引かれる。その水封式真
空ポンプ２内の水によって、そこに引かれたアルゴンガ
ス中に含まれるSiO微粉が取り除かれる。しかるのち、
アルゴンガスは一時貯蔵タンク３に貯蔵される。さら
に、アルゴンガスはその一時貯蔵タンク３からPSA精製
ユニット４に送られる。このPSA精製ユニット４で、ア
ルゴンガス中のN2、CO、CO2等の不純物ガス成分が分離
されて除去される。[Example] As shown in FIG. 1, used in a single crystal pulling apparatus 1 known per se, argon gas is drawn as a recovery gas by a liquid ring type, that is, a water ring type and a vacuum pump 2. The water in the water-sealed vacuum pump 2 removes the SiO fine powder contained in the argon gas drawn therein. After a while
The argon gas is stored in the temporary storage tank 3. Further, the argon gas is sent from the temporary storage tank 3 to the PSA purification unit 4. In this PSA purification unit 4, impurity gas components such as N2, CO, CO2 in the argon gas are separated and removed.
第２図に示すように、PSA精製ユニット４では、コン
プレッサー21によってアルゴンガスがゼオライトの吸着
剤の存在する吸着槽22に送られる。アルゴンガスに比べ
て吸着量の多いN2、CO、CO2が吸着槽22内の吸着剤によ
って吸着される。そのあと、アルゴンガスは吸着槽22の
上部から取り出される。As shown in FIG. 2, in the PSA purification unit 4, the compressor 21 sends the argon gas to the adsorption tank 22 in which the zeolite adsorbent is present. The adsorbent in the adsorption tank 22 adsorbs N2, CO, and CO2, which have a larger adsorption amount than the argon gas. After that, the argon gas is taken out from the upper part of the adsorption tank 22.
吸着が完了すると、吸着槽22内は減圧される。そして
真空ポンプ23で減圧脱着を行う。When the adsorption is completed, the pressure inside the adsorption tank 22 is reduced. Then, the vacuum pump 23 performs depressurization desorption.
PSA精製ユニット４で精製されたアルゴンガスは、H
2、O2、微量残留CO2等を含んでいるため、不活性ガス精
製ユニット５に送られる。The argon gas purified by the PSA purification unit 4 is H
Since it contains 2, O2, trace amount of residual CO2, etc., it is sent to the inert gas purification unit 5.
第３図に示すように、不活性ガス精製ユニット５は、
順にコンプレッサー31、パラジウム触媒塔32、脱酸素塔
33、吸着塔34から構成されている。コンプレッサー31に
よって送られたアルゴンガス中のH2、O2や、PSA精製ユ
ニット４で除去されなかった微量のCO、CO2は、触媒塔3
2での酸素添加によりH2O、CO2に変成され、回収ガス中
のH2O、CO2とともに吸着塔34で吸着され、半導体単結晶
引上げに使用できるように除去される。As shown in FIG. 3, the inert gas purification unit 5 is
Compressor 31, palladium catalyst tower 32, deoxidizer tower
33, adsorption tower 34. The H2 and O2 in the argon gas sent by the compressor 31 and the trace amounts of CO and CO2 that were not removed by the PSA purification unit 4 are the catalyst tower 3
It is converted to H2O and CO2 by the oxygen addition at 2, and is adsorbed in the adsorption tower 34 together with H2O and CO2 in the recovered gas and removed so that it can be used for pulling a semiconductor single crystal.
過剰の酸素は脱酸素塔33により反応除去される。 Excess oxygen is removed by reaction by the deoxygenation tower 33.
不純物が除去された高純度アルゴンガスは、貯蔵タン
ク６に貯蔵され、再度、単結晶引上装置１に送られて使
用される。７は貯蔵タンク６へのバックアップラインを
示す。The high-purity argon gas from which impurities have been removed is stored in the storage tank 6 and sent to the single crystal pulling apparatus 1 again for use. Reference numeral 7 denotes a backup line to the storage tank 6.
［変形例］ 本発明は前述の実施例に限定されない。[Modification] The present invention is not limited to the above embodiment.
PSA精製ユニット４と不活性ガス精製ユニット５の順
序を逆にして、PSA精製ユニット４を不活性ガス精製ユ
ニット５の後方に設けても、同様の効果が得られる。Even if the order of the PSA purification unit 4 and the inert gas purification unit 5 is reversed and the PSA purification unit 4 is provided behind the inert gas purification unit 5, the same effect can be obtained.
PSA精製のユニット４の吸着剤は第２図の実施例のゼ
オライトに限らず適宜選択することができる。同様に、
不活性ガス精製ユニット５の触媒塔32、脱酸素塔33、吸
着塔34に使用する材料も、第３図の実施例のものに限ら
ず適宜選択できる。The adsorbent of the PSA refining unit 4 is not limited to the zeolite of the embodiment shown in FIG. 2 and can be appropriately selected. Similarly,
The materials used for the catalyst tower 32, the deoxygenation tower 33, and the adsorption tower 34 of the inert gas purification unit 5 are not limited to those of the embodiment shown in FIG.
［発明の効果］ この発明の不活性ガス回収装置によれば、CO、CO2、O
2等の不純物の濃度変化に関係なく、それらの不純物を
除去できる。[Effects of the Invention] According to the inert gas recovery apparatus of the present invention, CO, CO2, O
It is possible to remove impurities such as 2 regardless of the concentration change of the impurities.
本発明の好ましい不活性ガス回収装置（第１図の例）
の各箇所Ａ、Ｂ、Ｃにおける不純物濃度（ppm）を表１
に示す。Preferred Inert Gas Recovery Device of the Present Invention (Example of FIG. 1)
Table 1 shows the impurity concentration (ppm) at each point A, B, and C
Shown in
表１からも分かるように、本発明の単結晶引上装置用
不活性ガス回収装置によれば、従来の回収装置では除去
できなかったN2を除去でき、しかも何度も回収ガスのリ
サイクル利用が可能である。As can be seen from Table 1, according to the inert gas recovery apparatus for a single crystal pulling apparatus of the present invention, N2 which could not be removed by the conventional recovery apparatus can be removed, and the recovered gas can be reused many times. It is possible.
第１図は本発明による単結晶引上装置用不活性ガス回収
装置の一例を示す概略系統図、第２図は第１図の不活性
ガス回収装置に使用するPSA精製ユニットの系統図、第
３図は第１図の不活性ガス回収装置に使用する不活性ガ
ス精製ユニットの系統図である。 １……単結晶引上装置 ２……液封式真空ポンプ ３……一時貯蔵タンク ４……PSA精製ユニット ５……不活性ガス精製ユニット ６……貯蔵タンク 21……コンプレッサー 22……吸着槽 23……真空ポンプ 31……コンプレッサー 32……触媒塔 33……脱酸素塔 34……吸着塔1 is a schematic system diagram showing an example of an inert gas recovery apparatus for a single crystal pulling apparatus according to the present invention, FIG. 2 is a system diagram of a PSA purification unit used in the inert gas recovery apparatus of FIG. 1, FIG. 3 is a system diagram of an inert gas purification unit used in the inert gas recovery device of FIG. 1 …… Single crystal pulling device 2 …… Liquid-ring vacuum pump 3 …… Temporary storage tank 4 …… PSA purification unit 5 …… Inert gas purification unit 6 …… Storage tank 21 …… Compressor 22 …… Adsorption tank 23 …… Vacuum pump 31 …… Compressor 32 …… Catalyst tower 33 …… Deoxidizing tower 34 …… Adsorption tower
───────────────────────────────────────────────────── フロントページの続き (72)発明者 今 美紀夫 山形県西置賜郡小国町大字小国町378番 地 東芝セラミックス株式会社小国製造 所内 (56)参考文献 特公 平２−14315（ＪＰ，Ｂ２) 特公 昭50−8999（ＪＰ，Ｂ２) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Mikio Ima, Oguni Town, Oguni Town, Nishikitama District, Yamagata Prefecture, 378 Oguni Town, Toshiba Ceramics Co., Ltd. (56) Reference Japanese Patent Publication No. 2-14315 (JP, B2) Japanese Patent Publication Sho 50-8999 (JP, B2)
Claims (1)
の不活性ガス中の不純物を水によって除去するための液
封式真空ポンプと、N2ガス含有の不活性ガスをPSA方式
で精製して少くともN2ガスを除去するPSA精製ユニット
と、不活性ガスを触媒方式で精製する不活性ガス精製ユ
ニットを備え、N2ガスを低減した状態で不活性ガスを回
収する構成にしたことを特徴とする単結晶引上用不活性
ガス回収装置。1. A liquid-ring vacuum pump for removing impurities in N 2 gas-containing inert gas recovered from a single crystal pulling apparatus by water, and a PSA method for N 2 gas-containing inert gas. A PSA purification unit that purifies at least N 2 gas and an inert gas purification unit that purifies the inert gas by a catalytic method are provided, and the inert gas is recovered with the N 2 gas reduced. An inert gas recovery device for pulling a single crystal characterized by the above.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2199276A JP2532297B2 (en) | 1990-07-30 | 1990-07-30 | Inert gas recovery device for single crystal pulling device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2199276A JP2532297B2 (en) | 1990-07-30 | 1990-07-30 | Inert gas recovery device for single crystal pulling device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0489387A JPH0489387A (en) | 1992-03-23 |
| JP2532297B2 true JP2532297B2 (en) | 1996-09-11 |
Family
ID=16405098
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2199276A Expired - Fee Related JP2532297B2 (en) | 1990-07-30 | 1990-07-30 | Inert gas recovery device for single crystal pulling device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2532297B2 (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5706674A (en) * | 1997-01-17 | 1998-01-13 | Air Products And Chemicals, Inc. | Argon recovery from silicon crystal furnace |
| JP4717184B2 (en) * | 2000-07-14 | 2011-07-06 | Ｓｕｍｃｏ Ｔｅｃｈｘｉｖ株式会社 | Inert gas recovery equipment for single crystal pulling equipment |
| US6838066B2 (en) | 2002-09-13 | 2005-01-04 | Air Products And Chemicals, Inc. | Process for recovery, purification, and recycle of argon |
| JP5500650B2 (en) * | 2010-11-10 | 2014-05-21 | 住友精化株式会社 | Argon gas purification method and purification apparatus |
| JP2012140254A (en) * | 2010-12-28 | 2012-07-26 | Covalent Materials Corp | Inert gas recovery apparatus |
| CN113277488B (en) * | 2021-07-23 | 2021-10-08 | 苏州市兴鲁空分设备科技发展有限公司 | Method and device for recovering and purifying argon tail gas |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3933576A (en) * | 1973-05-17 | 1976-01-20 | Whiting Corporation | Evaporation of radioactive wastes |
| JPH0214315A (en) * | 1988-12-12 | 1990-01-18 | Wacom Co Ltd | Electronic blackboard marker |
-
1990
- 1990-07-30 JP JP2199276A patent/JP2532297B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0489387A (en) | 1992-03-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR100192690B1 (en) | The use of nitrogen from an air separation plant in carbon dioxide removal from a feed gas to further process | |
| US5039500A (en) | Process for producing xenon | |
| JPS5922625A (en) | Method for removing gaseous nitrogen contained in gaseous carbon monoxide or gaseous mixture of carbon monoxide and carbon dioxide by adsorption method | |
| GB1574801A (en) | Gas separation | |
| JP5498661B2 (en) | Blast furnace gas separation method | |
| JP2532297B2 (en) | Inert gas recovery device for single crystal pulling device | |
| JPH0372566B2 (en) | ||
| JPH0490819A (en) | Air separation method | |
| JP2005246137A (en) | Method and apparatus for gas separation | |
| JP3294067B2 (en) | Krypton manufacturing method | |
| JPH09187622A (en) | Method for separating and recovering concentrated carbon dioxide | |
| JP3219612B2 (en) | Method for co-producing carbon monoxide and hydrogen from mixed gas | |
| JPS59116115A (en) | Method for recovering carbon monoxide | |
| JP2587334B2 (en) | Method of separating CO gas not containing CH4 | |
| JP2000239007A (en) | Method and apparatus for recovering and cleaning nitrous oxide included in waste gas | |
| JPH07275631A (en) | Substitution-reduction method for impurity in product in pressure swing adsorption method | |
| JP3256811B2 (en) | Method for purifying krypton and xenon | |
| JP3026103B2 (en) | Argon recovery method | |
| JP7191619B2 (en) | Carbon monoxide gas separation device and carbon monoxide gas separation method | |
| JPH02283608A (en) | Method for separating and recovering carbon monoxide | |
| JPH0463804B2 (en) | ||
| JPH0112529B2 (en) | ||
| JPH1025102A (en) | Chlorine removal apparatus and oxygen separation by pressure swing adsorption | |
| JP3191113B2 (en) | Argon recovery method | |
| JPH0768119A (en) | Method for separation and recovery of carbon monoxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| S531 | Written request for registration of change of domicile |
Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080627 Year of fee payment: 12 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313111 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080627 Year of fee payment: 12 |
|
| R371 | Transfer withdrawn |
Free format text: JAPANESE INTERMEDIATE CODE: R371 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313111 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080627 Year of fee payment: 12 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080627 Year of fee payment: 12 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090627 Year of fee payment: 13 |
|
| LAPS | Cancellation because of no payment of annual fees |