JP2003042395A - Gas supply method and gas supply device - Google Patents
Gas supply method and gas supply deviceInfo
- Publication number
- JP2003042395A JP2003042395A JP2001226303A JP2001226303A JP2003042395A JP 2003042395 A JP2003042395 A JP 2003042395A JP 2001226303 A JP2001226303 A JP 2001226303A JP 2001226303 A JP2001226303 A JP 2001226303A JP 2003042395 A JP2003042395 A JP 2003042395A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- pressure
- gas supply
- cylinder
- hydrogen chloride
- 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.)
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Classifications
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- 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
- Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
- Chemical Vapour Deposition (AREA)
- Drying Of Semiconductors (AREA)
- Filling Or Discharging Of Gas Storage Vessels (AREA)
- Pipeline Systems (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、液化ガスが充填さ
れたボンベからガスを供給するガス供給装置に関し、特
に気相成長装置に適したガス供給装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a gas supply device for supplying gas from a cylinder filled with liquefied gas, and more particularly to a gas supply device suitable for a vapor phase growth device.
【０００２】[0002]
【従来の技術】半導体製造プロセスにおいて、各種ガス
が使用される。例えばシリコンエピタキシャルウェーハ
を製造する気相成長装置では、シリコン単結晶ウェーハ
（以下単に「ウェーハ」と称する）上に所定のガスを供
給し、シリコンエピタキシャル層を気相エピタキシャル
成長させる。即ち、図５に示すように、気相成長装置１
０の反応炉１１内に備えられるサセプタ１１ａ上にウェ
ーハＷを載置し、反応炉１１内を所定温度まで昇温す
る。この状態で、反応炉１１内に、ジクロロシラン（Ｓ
ｉＨ2Ｃｌ2：ｄichlorosilane）等の原料ガス、アルシ
ン（ＡｓＨ3：arsine）やホスフィン（ＰＨ3：ｐhosphi
ne）等のドーパントガス、キャリアガスとしての水素ガ
ス等からなる混合ガス（「プロセスガス」と称する）を
供給し、ウェーハＷの主表面にシリコンエピタキシャル
層を形成する。その際、反応炉１１の内壁面やサセプタ
１１ａ等にシリコンが堆積するので、反応炉１１内にエ
ッチングガスを供給して堆積したシリコンを除去する。2. Description of the Related Art Various gases are used in the semiconductor manufacturing process. For example, in a vapor phase growth apparatus for producing a silicon epitaxial wafer, a predetermined gas is supplied onto a silicon single crystal wafer (hereinafter simply referred to as “wafer”) to grow a silicon epitaxial layer by vapor phase epitaxial growth. That is, as shown in FIG.
The wafer W is placed on the susceptor 11a provided in the reaction furnace 11 of 0 temperature, and the inside of the reaction furnace 11 is heated to a predetermined temperature. In this state, dichlorosilane (S
Source gas such as iH 2 Cl 2 : dichlorosilane), arsine (AsH 3 : arsine) and phosphine (PH 3 : phosphi)
A mixed gas (referred to as a “process gas”) including a dopant gas such as ne) and hydrogen gas as a carrier gas is supplied to form a silicon epitaxial layer on the main surface of the wafer W. At that time, since silicon is deposited on the inner wall surface of the reaction furnace 11 and the susceptor 11a, etching gas is supplied into the reaction furnace 11 to remove the deposited silicon.
【０００３】こうしたシリコンエピタキシャルウェーハ
の製造におけるエッチングガスとして、例えば塩化水素
（ＨＣｌ）ガスが使用される。図５に示すように、塩化
水素ガスは、例えばボンベ３０より供給される。このボ
ンベ３０内には、液化塩化水素Ｌが高圧で充填されてい
る。この液化塩化水素Ｌから気化した塩化水素ガスは、
ボンベ３０のガス供給口３０ａから減圧弁３１に導かれ
て、気相成長装置１０で使用される圧力にまで減圧され
る。そして開閉弁３２が開かれると、配管３３を介して
塩化水素ガスが反応炉１１内に供給される。シリコンエ
ピタキシャルウェーハの製造では、塩化水素ガスは、例
えば温度３００Ｋにおいて内圧５０ｋｇｆ／ｃｍ
2（４．９ＭＰａ）であるボンベ３０から減圧弁３１に
おいて１０ｋｇｆ／ｃｍ2（０．９８ＭＰａ）以下の圧
力まで減圧されて反応炉１１に供給される。Hydrogen chloride (HCl) gas, for example, is used as an etching gas in the production of such a silicon epitaxial wafer. As shown in FIG. 5, hydrogen chloride gas is supplied from, for example, a cylinder 30. The cylinder 30 is filled with liquefied hydrogen chloride L at high pressure. The hydrogen chloride gas vaporized from this liquefied hydrogen chloride L is
The pressure is introduced from the gas supply port 30a of the cylinder 30 to the pressure reducing valve 31 and reduced to the pressure used in the vapor phase growth apparatus 10. When the on-off valve 32 is opened, hydrogen chloride gas is supplied into the reaction furnace 11 via the pipe 33. In the production of silicon epitaxial wafers, hydrogen chloride gas is used at an internal pressure of 50 kgf / cm at a temperature of 300 K, for example.
The pressure is reduced from a cylinder 30 of 2 (4.9 MPa) to a pressure of 10 kgf / cm 2 (0.98 MPa) or less by a pressure reducing valve 31 and supplied to the reaction furnace 11.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、ボンベ
３０から供給される塩化水素ガス中に、不純物として水
分が含まれてしまい、その純度が低下する場合がある。
そして、塩化水素ガスの純度が低下すると、反応炉１１
内に水分が不純物として供給されてしまうだけでなく、
塩化水素ガスに含まれる水分によって配管３３の内面が
腐蝕してしまう場合もある。このために、高純度ガスを
安定して供給できるガス供給方法およびガス供給装置が
望まれていた。However, the hydrogen chloride gas supplied from the cylinder 30 may contain water as an impurity and its purity may be lowered.
When the purity of hydrogen chloride gas decreases, the reaction furnace 11
Not only will water be supplied as impurities inside,
The water contained in the hydrogen chloride gas may corrode the inner surface of the pipe 33. Therefore, a gas supply method and a gas supply device capable of stably supplying a high-purity gas have been desired.
【０００５】本発明の課題は、不純物として含まれる水
分の量が低減された高純度ガスを安定して供給できるガ
ス供給方法およびガス供給装置を提供することである。An object of the present invention is to provide a gas supply method and a gas supply device capable of stably supplying a high-purity gas in which the amount of water contained as impurities is reduced.
【０００６】[0006]
【課題を解決するための手段】液化塩化水素Ｌは、ボン
ベ３０内の液化塩化水素Ｌ自体から熱を奪いながら気化
してその温度を低下させる。こうして液化塩化水素Ｌの
温度が水の凝固点以下まで低下すると、液化塩化水素Ｌ
中に僅かに含まれる水分から微細な氷が生成する。液化
塩化水素Ｌの密度１．２ｋｇ／ｍ3に比べると、氷の密
度が１ｋｇ／ｍ3と軽いことから、微細な氷は、気化す
る塩化水素の蒸気に容易に同伴されてしまう。この微細
な氷が、液化塩化水素Ｌの蒸気に同伴されると、ボンベ
３０から供給される塩化水素ガス中に水分が含まれるよ
うになり、その純度が低下してしまうのである。Liquefied hydrogen chloride L vaporizes while absorbing heat from the liquefied hydrogen chloride L itself in the cylinder 30 to lower its temperature. When the temperature of liquefied hydrogen chloride L falls below the freezing point of water in this way, liquefied hydrogen chloride L
Fine ice is generated from a small amount of water contained therein. Compared to the density 1.2 kg / m 3 of liquefied hydrogen chloride L, since the density of the ice is light and 1 kg / m 3, fine ice, will be readily entrained in the vapor of the hydrogen chloride vaporized. When this fine ice is entrained in the vapor of the liquefied hydrogen chloride L, the hydrogen chloride gas supplied from the cylinder 30 will contain water, and its purity will decrease.
【０００７】そこで、上記課題を解決するため、本発明
のガス供給方法は、ボンベの内圧が、該ボンベに充填さ
れた液化ガスに含まれる水分を液体に保つことができる
圧力以上の時にのみ、前記ボンベからガスを供給するこ
とを特徴とする。Therefore, in order to solve the above-mentioned problems, the gas supply method of the present invention, the internal pressure of the cylinder, only when the water contained in the liquefied gas filled in the cylinder is equal to or higher than the pressure capable of keeping the liquid as a liquid, It is characterized in that gas is supplied from the cylinder.
【０００８】本発明のガス供給方法において、ボンベよ
り導かれるガスを、該ボンベ内の液化ガスに含まれる水
分を液体に保つことができる圧力以上に設定された第１
減圧弁によって減圧し、該第１減圧弁によって減圧され
たガスを、第２減圧弁によって減圧して供給することが
好ましい。In the gas supply method of the present invention, the gas introduced from the cylinder is set to a pressure equal to or higher than the pressure at which the water contained in the liquefied gas in the cylinder can be kept liquid.
It is preferable that the pressure of the gas reduced by the pressure reducing valve and reduced by the first pressure reducing valve be reduced and supplied by the second pressure reducing valve.
【０００９】ここで、液化ガスとしては、例えばアルシ
ン（ＡｓＨ3）、ホスフィン（ＰＨ3）、ジクロロシラン
（ＳｉＨ2Ｃｌ2）、塩化水素ガスが挙げられる。例え
ば、液化ガスが塩化水素ガスである場合には、第１減圧
弁は２．９ＭＰａ以上に設定することが好ましい。Here, examples of the liquefied gas include arsine (AsH 3 ), phosphine (PH 3 ), dichlorosilane (SiH 2 Cl 2 ), and hydrogen chloride gas. For example, when the liquefied gas is hydrogen chloride gas, the first pressure reducing valve is preferably set to 2.9 MPa or more.
【００１０】また、本発明のガス供給装置は、液化ガス
を充填した複数本のボンベからガスを供給するガス供給
装置において、前記ボンベの内圧が、該ボンベ内の液化
ガスに含まれる水分を液体に保つことができる圧力以上
の状態の時にのみ、該ボンベからガスを供給するように
構成されているガス供給制御手段を備えたことを特徴と
する。Further, the gas supply device of the present invention is a gas supply device for supplying gas from a plurality of cylinders filled with liquefied gas, wherein the internal pressure of the cylinder is such that moisture contained in the liquefied gas in the cylinder becomes liquid. The gas supply control means is configured to supply the gas from the cylinder only when the pressure is equal to or higher than the pressure that can be maintained.
【００１１】本発明のガス供給装置において、ガス供給
制御手段は、並列に接続した前記複数本のボンベと第２
減圧弁との間に第１減圧弁をそれぞれ介在させ、これら
第１減圧弁の下流側を互いに接続すると共に、これら第
１減圧弁を、前記ボンベ内の液化ガスに含まれる水分を
液体に保つことができる圧力以上でかつ互いに異なる圧
力に設定することにより構成しても良い。In the gas supply apparatus of the present invention, the gas supply control means includes the plurality of cylinders connected in parallel and the second cylinder.
The first pressure reducing valves are respectively interposed between the pressure reducing valves and the downstream sides of the first pressure reducing valves are connected to each other, and the first pressure reducing valves keep the water contained in the liquefied gas in the cylinder liquid. Alternatively, the pressure may be set to a pressure higher than the above pressure and different from each other.
【００１２】また、本発明において、ガス供給制御手段
を、前記複数のボンベと第２減圧弁との間にそれぞれ介
在される圧力制御弁として、該圧力制御弁は、前記複数
のボンベのうちいずれかの内圧が、該ボンベ内の液化ガ
スに含まれる水分を液体に保つことができる圧力よりも
低下したときに閉弁して、該ボンベから前記第２減圧弁
へのガス供給を停止させるように構成しても良い。In the present invention, the gas supply control means is a pressure control valve interposed between the plurality of cylinders and the second pressure reducing valve, and the pressure control valve is any one of the plurality of cylinders. When the internal pressure of the cylinder becomes lower than the pressure at which the water contained in the liquefied gas in the cylinder can be kept liquid, the valve is closed to stop the gas supply from the cylinder to the second pressure reducing valve. It may be configured to.
【００１３】本発明によれば、ガスの供給は、液化ガス
中に含まれる水分を液体に保った状態でなされる。即
ち、ガスの供給に際して、液化ガス中に含まれる水分か
ら微細な氷を生じさせない。すると、水は液化ガスより
も極めて高沸点であるため、液体に保たれている水は気
化せず、液化ガスだけが気化するようになる。これによ
り、化学処理装置等に供給されるガス中に水分が含まれ
ることを抑制できる。以上から、高純度のガスを安定し
て供給できる。According to the present invention, the gas is supplied in a state where the water contained in the liquefied gas is kept liquid. That is, when the gas is supplied, fine ice is not generated from the water contained in the liquefied gas. Then, since water has a boiling point extremely higher than that of the liquefied gas, the water held in the liquid does not evaporate, but only the liquefied gas evaporates. As a result, it is possible to suppress the inclusion of water in the gas supplied to the chemical treatment device or the like. From the above, a high-purity gas can be stably supplied.
【００１４】[0014]
【発明の実施の形態】〔第１の実施の形態〕以下、図
１、図４を参照して、第１の実施の形態のガス供給装置
１を詳細に説明する。このガス供給装置１は、シリコン
エピタキシャルウェーハを製造する気相成長装置８に、
エッチングガスとして使用する塩化水素ガスを供給する
ものである。図１に示すように、ガス供給装置１は、液
化塩化水素（液化ガス）２Ｌ、３Ｌが充填された２本の
ボンベ２、３を備える。これらボンベ２、３が設置され
る雰囲気Ｆは、その温度が室温（３００Ｋ）に保たれて
いる。そしてボンベ２、３のガス供給口２ａ、３ａに
は、減圧弁（第１減圧弁）４、５がそれぞれ配管１ａ、
１ｂを介して接続されている。これら配管１ａ、１ｂに
は、それぞれ逆止弁１ｅ、１ｆが設けられている。そし
て減圧弁４、５の下流側は、それぞれ配管１ｃを介して
減圧弁６（第２減圧弁）に接続されている。この減圧弁
６は、開閉弁７を有する配管１ｄを介して気相成長装置
８に接続されている。こうして、ボンベ２、３は互いに
並列に接続されている。この結果、減圧弁４、５は、配
管１ｃでのガス圧がスプリング４ａ、５ａに設定した設
定圧Ａ、Ｂよりも小さい時にはそれぞれ開弁している
が、配管１ｃでのガス圧が設定圧Ａ、Ｂよりも大きくな
ると閉弁する。この設定圧Ａ、Ｂは、後述する所定圧Ｐ
０以上で、かつ、およそ１ｋｇｆ／ｃｍ2（９．８×１
０-2ＭＰａ）程度互いに僅かにずれるように設定されて
いる。BEST MODE FOR CARRYING OUT THE INVENTION [First Embodiment] Hereinafter, a gas supply device 1 according to a first embodiment will be described in detail with reference to FIGS. 1 and 4. This gas supply device 1 is applied to a vapor phase growth device 8 for manufacturing a silicon epitaxial wafer,
A hydrogen chloride gas used as an etching gas is supplied. As shown in FIG. 1, the gas supply device 1 includes two cylinders 2 and 3 filled with liquefied hydrogen chloride (liquefied gas) 2L and 3L. The temperature of the atmosphere F in which these cylinders 2 and 3 are installed is kept at room temperature (300K). Pressure reducing valves (first pressure reducing valves) 4 and 5 are provided at the gas supply ports 2a and 3a of the cylinders 2 and 3, respectively.
It is connected via 1b. Check valves 1e and 1f are provided in the pipes 1a and 1b, respectively. The downstream sides of the pressure reducing valves 4 and 5 are connected to the pressure reducing valve 6 (second pressure reducing valve) via the pipes 1c, respectively. The pressure reducing valve 6 is connected to the vapor phase growth apparatus 8 via a pipe 1d having an opening / closing valve 7. Thus, the cylinders 2 and 3 are connected in parallel with each other. As a result, the pressure reducing valves 4 and 5 are opened when the gas pressure in the pipe 1c is smaller than the set pressures A and B set in the springs 4a and 5a, respectively, but the gas pressure in the pipe 1c is set to the set pressure. When it becomes larger than A and B, it closes. The set pressures A and B are predetermined pressures P described later.
0 or more and about 1 kgf / cm 2 (9.8 × 1
It is set to be slightly deviated from each other by about 0 -2 MPa.
【００１５】この所定圧Ｐ０は、以下のように設定され
ている。液化塩化水素２Ｌ、３Ｌは、塩化水素ガスとし
て気化する際に、液化塩化水素２Ｌ、３Ｌ自体から気化
熱を奪う。この気化熱の消費が著しいと、ボンベ２、３
が設置される雰囲気Ｆから流入する熱量Ｑ１（図１参
照）だけでは補うことができず、液化塩化水素２Ｌ、３
Ｌの温度Ｔは、塩化水素の蒸気圧曲線（図４に実線で図
示）に沿って下降する。これに伴って、ボンベ２、３の
内圧Ｐが蒸気圧曲線に沿って下降していく。具体的に
は、図４に示すように、Ａ点で示される内圧Ｐ１（この
場合には５ＭＰａ）から塩化水素ガスを気化させると、
ボンベの内圧Ｐは蒸気圧曲線に沿って下降する。さらに
内圧Ｐが下降すると、水の状態図における固体／液体の
境界線と塩化水素の蒸気圧曲線との交点（Ｂ点）で示さ
れる内圧Ｐ２に至る。この内圧Ｐ２は、およそ２．５Ｍ
Ｐａである。この状態で塩化水素ガスをさらに気化させ
ると、液化塩化水素２Ｌ、３Ｌの温度が水の状態図にお
ける固体／液体の境界線よりも低下し、液化塩化水素２
Ｌ、３Ｌ中に微細な氷を生成させてしまう。そこで前記
所定圧Ｐ０は、Ｐ２よりも高圧、すなわち、ボンベ２、
３内の液化塩化水素２Ｌ、３Ｌに含まれる水分を常に液
体に保つことができる２．９ＭＰａ以上の圧力に設定す
る。The predetermined pressure P0 is set as follows. The liquefied hydrogen chlorides 2L and 3L take heat of vaporization from the liquefied hydrogen chlorides 2L and 3L themselves when vaporized as hydrogen chloride gas. When the consumption of this heat of vaporization is remarkable, the cylinders 2, 3
The quantity of heat Q1 (see FIG. 1) flowing from the atmosphere F in which the gas is installed cannot be compensated for, and liquefied hydrogen chloride 2L, 3
The temperature T of L falls along the vapor pressure curve of hydrogen chloride (shown by the solid line in FIG. 4). Along with this, the internal pressure P of the cylinders 2 and 3 decreases along the vapor pressure curve. Specifically, as shown in FIG. 4, when the hydrogen chloride gas is vaporized from the internal pressure P1 indicated by point A (5 MPa in this case),
The internal pressure P of the cylinder falls along the vapor pressure curve. When the internal pressure P further decreases, the internal pressure P2 shown by the intersection (point B) between the solid / liquid boundary line and the vapor pressure curve of hydrogen chloride in the water phase diagram is reached. This internal pressure P2 is about 2.5M
Pa. When the hydrogen chloride gas is further vaporized in this state, the temperatures of the liquefied hydrogen chloride 2L and 3L become lower than the solid / liquid boundary line in the water phase diagram, and the liquefied hydrogen chloride 2L
Fine ice is generated in L and 3L. Therefore, the predetermined pressure P0 is higher than P2, that is, the cylinder 2,
The pressure is set to 2.9 MPa or more so that the water contained in 2 L and 3 L of liquefied hydrogen chloride in 3 can always be kept liquid.
【００１６】このようなガス供給装置１によれば、各ボ
ンベ２、３の内圧Ｐを所定圧Ｐ０以上に制御しながら、
減圧弁４、５および減圧弁６を介して塩化水素ガスが気
相成長装置８に供給される。以下、ガス供給装置１によ
って気相成長装置８に塩化水素ガスが供給される様子を
より具体的に説明する。但し以下の説明では、一例とし
て減圧弁４、５の設定圧をＡ＞Ｂとした場合を説明す
る。According to such a gas supply device 1, while controlling the internal pressure P of each cylinder 2, 3 to a predetermined pressure P0 or higher,
Hydrogen chloride gas is supplied to the vapor phase growth apparatus 8 via the pressure reducing valves 4 and 5 and the pressure reducing valve 6. Hereinafter, the manner in which the hydrogen chloride gas is supplied to the vapor phase growth apparatus 8 by the gas supply apparatus 1 will be described more specifically. However, in the following description, the case where the set pressure of the pressure reducing valves 4 and 5 is A> B will be described as an example.
【００１７】先ず、減圧弁４、５のうち配管１ｃ側のガ
ス圧が最も大きく設定されているボンベ２からのみガス
が供給され始める。これにより、配管１ｃのガス圧力は
設定圧Ａとなる。この時、減圧弁５は閉弁している。こ
うしてボンベ２からのみガス供給されると、気化熱によ
り液化塩化水素２Ｌの温度がしだいに下る為、ボンベ２
の内圧Ｐが下降していく。そして、ボンベ２の内圧Ｐが
設定圧Ａよりさらに下降してＢに至ると、減圧弁５が開
弁してボンベ３からガスが供給され始めるとともに、ボ
ンベ２からのガス供給が一旦停止する。なおこの時、他
の減圧弁４は開弁しているが逆止弁１ｅによってガスの
逆流が防止される。一方、ボンベ３からガスを供給して
いる間に、ガス供給が停止したボンベ２は、雰囲気Ｆか
ら流入する熱量Ｑ１によって液化塩化水素２Ｌの温度を
上昇させながら、内圧Ｐがそれぞれの設定圧Ａを越える
まで回復させる。こうして、ボンベ２、３の内圧が、該
ボンベ２、３に充填された液化塩化水素２Ｌ、３Ｌに含
まれる水分を液体に保つことができる所定圧Ｐ０以上の
時にのみ、何れかのボンベ２、３から継続してガスが供
給される。即ち、第１の実施の形態では、減圧弁４、５
と、減圧弁６と、これらを接続する配管１ｃとからガス
供給制御手段が構成される。First, gas starts to be supplied only from the cylinder 2 of the pressure reducing valves 4 and 5 in which the gas pressure on the side of the pipe 1c is set to the maximum. As a result, the gas pressure in the pipe 1c becomes the set pressure A. At this time, the pressure reducing valve 5 is closed. When gas is supplied only from the cylinder 2 in this way, the temperature of the liquefied hydrogen chloride 2 L gradually drops due to the heat of vaporization, so that the cylinder 2
The internal pressure P of is decreasing. When the internal pressure P of the cylinder 2 further falls below the set pressure A and reaches B, the pressure reducing valve 5 opens and gas is supplied from the cylinder 3 and the gas supply from the cylinder 2 is temporarily stopped. At this time, the other pressure reducing valve 4 is opened, but the check valve 1e prevents the reverse flow of gas. On the other hand, while the gas is being supplied from the cylinder 3, the cylinder 2 in which the gas supply is stopped raises the temperature of the liquefied hydrogen chloride 2L by the heat quantity Q1 flowing in from the atmosphere F, while the internal pressure P is set to the respective set pressure A. Restore until it exceeds. Thus, only when the internal pressure of the cylinders 2, 3 is equal to or higher than the predetermined pressure P0 capable of keeping the water contained in the liquefied hydrogen chloride 2L, 3L filled in the cylinders 2, 3 as a liquid, Gas is continuously supplied from 3. That is, in the first embodiment, the pressure reducing valves 4, 5
The gas supply control means is composed of the pressure reducing valve 6 and the pipe 1c connecting them.
【００１８】〔第２の実施の形態〕第２の実施の形態の
ガス供給装置１は、図２に示すように、ボンベ２、３の
ガス供給口２ａ、３ａに、それぞれ配管１ａ、１ｂを介
して圧力制御弁（ガス供給制御手段）１１、１２が接続
されている。これら圧力制御弁１１、１２は、それぞれ
配管１ａ、１ｂでのガス圧がスプリング１１ａ、１２ａ
に設定した所定圧Ｐ０以上の時には開弁しているが、配
管１ａ、１ｂでのガス圧が所定圧Ｐ０よりも小さくなる
と閉弁する。そして圧力制御弁１１、１２の下流側はそ
れぞれ配管１ｃを介して減圧弁６（第２減圧弁）に接続
されている。[Second Embodiment] As shown in FIG. 2, a gas supply apparatus 1 according to a second embodiment is provided with pipes 1a and 1b at gas supply ports 2a and 3a of cylinders 2 and 3, respectively. Pressure control valves (gas supply control means) 11 and 12 are connected via the pressure control valves. In these pressure control valves 11 and 12, the gas pressures in the pipes 1a and 1b are the springs 11a and 12a, respectively.
The valve is opened when the pressure is equal to or higher than the predetermined pressure P0 set to 1. However, the valve is closed when the gas pressure in the pipes 1a and 1b becomes lower than the predetermined pressure P0. The downstream sides of the pressure control valves 11 and 12 are respectively connected to the pressure reducing valve 6 (second pressure reducing valve) via the pipe 1c.
【００１９】このガス供給装置１によって、気相成長装
置８に塩化水素ガスを供給するうちに、気化熱により液
化塩化水素２Ｌの温度がしだいに下り、例えばボンベ２
の内圧Ｐが前記所定圧Ｐ０よりも低下すると、このボン
ベ２に対応する圧力制御弁１１が閉弁してガス供給を停
止させる。そして、ガス供給が停止したボンベ２内の液
化塩化水素２Ｌに雰囲気Ｆから熱量Ｑ１が流入し、その
内圧Ｐが所定圧Ｐ０を越えるまで回復すると、圧力制御
弁１１が開弁してガス供給が再開される。このボンベ２
と同様にして、ボンベ３からも塩化水素ガスが供給され
る。こうして、複数のボンベ２、３から長期間に渡って
継続して塩化水素ガスが供給される。While the hydrogen chloride gas is being supplied to the vapor phase growth apparatus 8 by the gas supply apparatus 1, the temperature of the liquefied hydrogen chloride 2L gradually drops due to the heat of vaporization, for example, the cylinder 2
When the internal pressure P of the cylinder 2 becomes lower than the predetermined pressure P0, the pressure control valve 11 corresponding to the cylinder 2 is closed to stop the gas supply. Then, when the heat quantity Q1 flows from the atmosphere F into the liquefied hydrogen chloride 2L in the cylinder 2 in which the gas supply is stopped and the internal pressure P recovers until it exceeds the predetermined pressure P0, the pressure control valve 11 opens and the gas supply is stopped. It will be restarted. This cylinder 2
Similarly to the above, hydrogen chloride gas is also supplied from the cylinder 3. Thus, hydrogen chloride gas is continuously supplied from the plurality of cylinders 2 and 3 for a long period of time.
【００２０】〔第３の実施の形態〕第３の実施の形態の
ガス供給装置１は、図３に示すように、ボンベ２、３の
ガス供給口２ａ、３ａに、それぞれ配管１ａ、１ｂを介
して電磁弁２３、２４が接続されている。これら電磁弁
２３、２４の下流側はそれぞれ配管１ｃを介して減圧弁
６（第２減圧弁）に接続されている。そして電磁弁２
３、２４は制御部２５に接続されている。この制御部２
５には、ボンベ２、３の内圧Ｐをモニタする圧力センサ
２１、２２が接続されている。そして、例えばボンベ２
の内圧Ｐが前記所定圧Ｐ０より低くなると、圧力センサ
２１から信号が出力され、この出力信号を受けた制御部
２５が、電磁弁２３を閉弁させる。こうしてボンベ２か
らのガス供給が停止される。そして、雰囲気Ｆから流入
する熱量Ｑ１によってボンベ２の内圧Ｐが回復すると、
制御部２５による制御の下で電磁弁２３が開弁し、ボン
ベ２からのガス供給が再開される。即ち、第３の実施の
形態では、圧力センサ２１、２２と、制御部２５と、電
磁弁２３、２４とからガス供給制御手段が構成される。[Third Embodiment] As shown in FIG. 3, a gas supply device 1 according to a third embodiment has pipes 1a and 1b at gas supply ports 2a and 3a of cylinders 2 and 3, respectively. The solenoid valves 23 and 24 are connected via the. Downstream sides of these electromagnetic valves 23 and 24 are connected to a pressure reducing valve 6 (second pressure reducing valve) via a pipe 1c. And solenoid valve 2
3, 24 are connected to the control unit 25. This control unit 2
Pressure sensors 21 and 22 for monitoring the internal pressure P of the cylinders 2 and 3 are connected to 5. And, for example, the cylinder 2
When the internal pressure P becomes lower than the predetermined pressure P0, a signal is output from the pressure sensor 21, and the control unit 25 receiving this output signal closes the solenoid valve 23. In this way, the gas supply from the cylinder 2 is stopped. Then, when the internal pressure P of the cylinder 2 is recovered by the heat quantity Q1 flowing from the atmosphere F,
The solenoid valve 23 is opened under the control of the control unit 25, and the gas supply from the cylinder 2 is restarted. That is, in the third embodiment, the gas supply control means is composed of the pressure sensors 21 and 22, the control unit 25, and the electromagnetic valves 23 and 24.
【００２１】［実施例］２５ｋｇの液化塩化水素を内圧
５０ｋｇｆ／ｃｍ2（４．９ＭＰａ）で充填した４本の
ボンベを使用して、第１の実施の形態に示した通りにガ
ス供給装置１を構成する。これらボンベに接続される第
１減圧弁の設定圧は、何れも３０ｋｇｆ／ｃｍ2（２．
９ＭＰａ）以上で互いに１ｋｇｆ／ｃｍ2（９．８×１
０-2ＭＰａ）ずらして設定する。またボンベを設置する
雰囲気は３００Ｋ程度の室温に保たれている。ここで図
４に示すように、ボンベの内圧が３０ｋｇｆ／ｃｍ
2（２．９ＭＰａ）であるとき（図４に示すＤ点）、ボ
ンベの内圧Ｐは、前記Ｐ２（水の状態図における固体／
液体の境界線と塩化水素の蒸気圧曲線との交点（Ｂ点）
で示される内圧）よりも高圧に保たれることになる。こ
のガス供給装置１により塩化水素ガスを気相成長装置１
０に供給したところ、ボンベ１本あたりの液化塩化水素
の残渣量が５ｋｇとなるまで、露点は−４０℃を確保で
きていた。従来、液化塩化水素の残渣量が５ｋｇ程度に
なるまで使用すると、露点は−３０℃以上になる。こう
して、不純物として含まれる水分の量が低減された高純
度の塩化水素ガスを長期間に渡って安定して供給するこ
とができる。[Example] Using four cylinders filled with 25 kg of liquefied hydrogen chloride at an internal pressure of 50 kgf / cm 2 (4.9 MPa), the gas supply device 1 was used as shown in the first embodiment. Make up. The set pressure of the first pressure reducing valve connected to these cylinders is 30 kgf / cm 2 (2.
9 MPa) or more and 1 kgf / cm 2 (9.8 × 1) to each other
0 -2 MPa) Set the offset. The atmosphere in which the cylinder is installed is kept at room temperature of about 300K. Here, as shown in FIG. 4, the internal pressure of the cylinder is 30 kgf / cm.
2 (2.9 MPa) (point D in FIG. 4), the internal pressure P of the cylinder is P2 (solid / solid in the state diagram of water /
Intersection of liquid boundary line and vapor pressure curve of hydrogen chloride (point B)
Will be maintained at a higher pressure. This gas supply device 1 is used for vapor phase growth device 1 for hydrogen chloride gas.
When it was supplied to 0, a dew point of -40 ° C was secured until the amount of liquefied hydrogen chloride residue per cylinder reached 5 kg. Conventionally, when used until the amount of liquefied hydrogen chloride residue reaches about 5 kg, the dew point becomes -30 ° C or higher. In this way, high-purity hydrogen chloride gas in which the amount of water contained as impurities is reduced can be stably supplied over a long period of time.
【００２２】なお、本発明は上記実施の形態に限定され
るものではない。例えば、本実施の形態では、２本のボ
ンベ２、３を用いる構成としたが、ボンベの本数は同様
にして任意に設計できる。また、本実施の形態では、第
１の実施の形態における減圧弁４、５の設定圧Ａ、Ｂ、
および、第２の実施の形態における圧力制御弁１１、１
２の所定圧Ｐ０は、それぞれスプリング４ａ、５ａ、１
１ａ、１２ａにより設定するように構成したが、その他
にも、油圧、空気圧等により設定するように構成しても
良い。さらに、本実施の形態では、気相成長装置８にエ
ッチングガスとして塩化水素ガスを供給する場合を例示
したが、ジクロロシラン等の原料ガスや、アルシンある
いはホスフィン等のドーパントガスについても同様に適
用できる。さらに本発明は、気相成長装置とは異なる他
の化学処理装置に、水分量を低減して高純度に各種ガス
を供給する場合にも適用できる。その他、本発明の趣旨
を逸脱しない範囲において、適宜に変更可能であること
は勿論である。The present invention is not limited to the above embodiment. For example, in this embodiment, two cylinders 2 and 3 are used, but the number of cylinders can be similarly designed arbitrarily. Further, in the present embodiment, the set pressures A, B of the pressure reducing valves 4, 5 in the first embodiment,
Also, the pressure control valves 11 and 1 according to the second embodiment.
The predetermined pressure P0 of 2 is the springs 4a, 5a, 1 respectively.
Although it is configured to be set by 1a and 12a, it may be configured by hydraulic pressure, air pressure or the like. Further, in the present embodiment, the case where hydrogen chloride gas is supplied as the etching gas to the vapor phase growth apparatus 8 is illustrated, but the same applies to a source gas such as dichlorosilane or a dopant gas such as arsine or phosphine. . Furthermore, the present invention can also be applied to the case of supplying various gases with high purity by reducing the amount of water to another chemical processing apparatus different from the vapor phase growth apparatus. Of course, other changes can be made without departing from the spirit of the present invention.
【００２３】[0023]
【発明の効果】本発明によれば、液化ガス中に微細な氷
を生じさせないため、この微細な氷がガス中に同伴され
ることがない。さらに、液化ガス中に含まれる水分が液
体状態に保たれるので、液化ガスだけが気化する。従っ
て、水分量が低減された高純度のガスを安定して化学処
理装置に供給できる。According to the present invention, since fine ice is not produced in the liquefied gas, the fine ice is not entrained in the gas. Furthermore, since the water contained in the liquefied gas is kept in a liquid state, only the liquefied gas is vaporized. Therefore, a high-purity gas having a reduced water content can be stably supplied to the chemical treatment device.
【図１】本発明を適用した第１の実施の形態のガス供給
装置１を示す配管図である。FIG. 1 is a piping diagram showing a gas supply device 1 of a first embodiment to which the present invention is applied.
【図２】本発明を適用した第２の実施の形態のガス供給
装置１を示す配管図である。FIG. 2 is a piping diagram showing a gas supply device 1 according to a second embodiment of the present invention.
【図３】本発明を適用した第３の実施の形態のガス供給
装置１を示す配管図である。FIG. 3 is a piping diagram showing a gas supply device 1 according to a third embodiment of the present invention.
【図４】本発明のガス供給装置１により塩化水素ガスが
高純度に供給される理由を説明するための塩化水素と水
の状態図を示す図である。FIG. 4 is a diagram showing a state diagram of hydrogen chloride and water for explaining the reason why hydrogen chloride gas is supplied with high purity by the gas supply device 1 of the present invention.
【図５】従来のガス供給装置を概念的に示した図であ
る。FIG. 5 is a diagram conceptually showing a conventional gas supply device.
１ ガス供給装置 ２、３ ボンベ ２Ｌ、３Ｌ 液化塩化水素（液化ガス） ４、５ 減圧弁（第１減圧弁） ６ 減圧弁（第２減圧弁） １１、１２ 圧力制御弁（ガス供給制御手段） ２１、２２ 圧力センサ（ガス供給制御手段の一部） ２３、２４ 電磁弁（ガス供給制御手段の一部） ２５ 制御部（ガス供給制御手段の一部） 1 gas supply device A few cylinders 2L, 3L Liquefied hydrogen chloride (liquefied gas) 4, 5 pressure reducing valve (first pressure reducing valve) 6 Pressure reducing valve (second pressure reducing valve) 11, 12 Pressure control valve (gas supply control means) 21, 22 Pressure sensor (a part of gas supply control means) 23, 24 Solenoid valve (part of gas supply control means) 25 Control part (a part of gas supply control means)
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｈ０１Ｌ 21/3065 Ｈ０１Ｌ 21/302 Ｎ ５Ｆ０４５ (72)発明者 寺嶋 誠一 群馬県安中市磯部２丁目13番１号 信越半 導体株式会社磯部工場内 Ｆターム(参考） 3E072 DB03 3J071 AA01 BB11 BB14 CC11 DD01 EE02 EE24 FF11 4G068 AA01 AB02 AC20 AD40 AF06 4K030 AA03 CA04 EA01 5F004 AA13 BC08 BD04 DA29 DB02 EA38 5F045 AA03 AB02 AC12 EB06 EE02─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 7 Identification code FI theme code (reference) H01L 21/3065 H01L 21/302 N 5F045 (72) Inventor Seiichi Terashima 2-13, Isobe, Annaka-shi, Gunma No. 1 Shin-Etsu Semiconductor Co., Ltd. Isobe Factory F-term (Reference) 3E072 DB03 3J071 AA01 BB11 BB14 CC11 DD01 EE02 EE24 FF11 4G068 AA01 AB02 AC20 AD40 AF06 4K030 AA03 CA04 EA01 5F004 AA13 BC08 BD04 5F02 A02 A02 A02 A45 A02 A45 A02 A02 A45 A02 A45 A02 A45 A02
Claims (7)
液化ガスに含まれる水分を液体に保つことができる圧力
以上の時にのみ、前記ボンベからガスを供給することを
特徴とするガス供給方法。1. A gas supply method characterized in that gas is supplied from the cylinder only when the internal pressure of the cylinder is equal to or higher than a pressure capable of keeping the water contained in the liquefied gas filled in the cylinder as a liquid. .
の液化ガスに含まれる水分を液体に保つことができる圧
力以上に設定された第１減圧弁によって減圧し、該第１
減圧弁によって減圧されたガスを、第２減圧弁によって
減圧して供給することを特徴とする請求項１記載のガス
供給方法。2. The gas introduced from the cylinder is decompressed by a first pressure reducing valve set to a pressure equal to or higher than a pressure at which water contained in the liquefied gas in the cylinder can be kept in a liquid state.
The gas supply method according to claim 1, wherein the gas whose pressure has been reduced by the pressure reducing valve is reduced in pressure by the second pressure reducing valve before being supplied.
記第１減圧弁は２．９ＭＰａ以上に設定することを特徴
とする請求項２記載のガス供給方法。3. The gas supply method according to claim 2, wherein the liquefied gas is liquefied hydrogen chloride, and the first pressure reducing valve is set to 2.9 MPa or more.
ガスを供給するガス供給装置において、 前記ボンベの内圧が、該ボンベ内の液化ガスに含まれる
水分を液体に保つことができる圧力以上の状態の時にの
み、該ボンベからガスを供給するように構成されている
ガス供給制御手段を備えたことを特徴とするガス供給装
置。4. A gas supply device for supplying gas from a plurality of cylinders filled with liquefied gas, wherein the internal pressure of the cylinder is equal to or higher than a pressure at which water contained in the liquefied gas in the cylinder can be kept liquid. A gas supply device comprising gas supply control means configured to supply gas from the cylinder only in the state.
に第１減圧弁をそれぞれ介在させ、 これら第１減圧弁の下流側を互いに接続すると共に、こ
れら第１減圧弁を、前記ボンベ内の液化ガスに含まれる
水分を液体に保つことができる圧力以上でかつ互いに異
なる圧力に設定することにより構成されていることを特
徴とする請求項４記載のガス供給装置。5. The gas supply control means includes a first pressure reducing valve interposed between the plurality of cylinders connected in parallel and a second pressure reducing valve, and the downstream sides of the first pressure reducing valves are connected to each other. In addition, the first pressure reducing valve is configured to have a pressure higher than or equal to a pressure at which the water contained in the liquefied gas in the cylinder can be kept in a liquid state and different from each other. 4. The gas supply device according to 4.
ンベと第２減圧弁との間にそれぞれ介在される圧力制御
弁であり、 該圧力制御弁は、前記複数のボンベのうちいずれかの内
圧が、該ボンベ内の液化ガスに含まれる水分を液体に保
つことができる圧力よりも低下したときに閉弁して、該
ボンベから前記第２減圧弁へのガス供給を停止させるこ
とを特徴とする請求項４記載のガス供給装置。6. The gas supply control means is a pressure control valve interposed between the plurality of cylinders and a second pressure reducing valve, and the pressure control valve is one of the plurality of cylinders. A valve is closed when the internal pressure is lower than a pressure at which water contained in the liquefied gas in the cylinder can be kept in a liquid state, and the gas supply from the cylinder to the second pressure reducing valve is stopped. The gas supply device according to claim 4.
を特徴とする請求項４〜６のいずれか一つに記載のガス
供給装置。7. The gas supply device according to claim 4, wherein the liquefied gas is liquefied hydrogen chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001226303A JP4815711B2 (en) | 2001-07-26 | 2001-07-26 | Gas supply method and gas supply apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001226303A JP4815711B2 (en) | 2001-07-26 | 2001-07-26 | Gas supply method and gas supply apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2003042395A true JP2003042395A (en) | 2003-02-13 |
| JP4815711B2 JP4815711B2 (en) | 2011-11-16 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014152869A (en) * | 2013-02-08 | 2014-08-25 | Air Water Plant & Engineering Inc | Liquefied gas supply device and method |
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| JPS585596A (en) * | 1981-06-30 | 1983-01-12 | Toshiba Corp | Method of supplying gas in vessel |
| JPH01163534U (en) * | 1988-05-02 | 1989-11-15 | ||
| JPH02201509A (en) * | 1989-01-31 | 1990-08-09 | Yazaki Corp | Gas pressure governing/weigher |
| JPH0675011U (en) * | 1993-03-24 | 1994-10-21 | 株式会社ユタカ | Pressure regulator |
| JPH0972495A (en) * | 1995-08-31 | 1997-03-18 | Toshiba Eng Co Ltd | Liquefied gas feeding device |
| JPH1043575A (en) * | 1996-02-23 | 1998-02-17 | L'air Liquide | Bulk transportation of ultrahigh purity gas at high flow velocity |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014152869A (en) * | 2013-02-08 | 2014-08-25 | Air Water Plant & Engineering Inc | Liquefied gas supply device and method |
Also Published As
| Publication number | Publication date |
|---|---|
| JP4815711B2 (en) | 2011-11-16 |
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