JP6082361B2 - Gas supply method - Google Patents

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JP6082361B2
JP6082361B2 JP2014095002A JP2014095002A JP6082361B2 JP 6082361 B2 JP6082361 B2 JP 6082361B2 JP 2014095002 A JP2014095002 A JP 2014095002A JP 2014095002 A JP2014095002 A JP 2014095002A JP 6082361 B2 JP6082361 B2 JP 6082361B2
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gas supply
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JP2015212558A (en
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一大 柿木
一大 柿木
明宏 市川
明宏 市川
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Taiyo Nippon Sanso Corp
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Description

本発明は、ガス供給方法に関し、詳しくは、高圧充填されている容器から消費設備へ減圧手段を介してフッ素混合ガスを供給するガス供給方法に関する。   The present invention relates to a gas supply method, and more particularly, to a gas supply method for supplying a fluorine mixed gas from a container filled with high pressure to a consumption facility through a decompression unit.

従来、半導体製造装置のクリーニングガスとして三フッ化窒素ガスが使用されてきたが、三フッ化窒素ガスの地球温暖化係数が17200と高く、環境問題を考慮し、地球温暖化係数が0のフッ素ガスの使用量が近年増加傾向にある。また、クリーニングガスの供給設備における各機器や配管の連結部分での漏れを防止するために、形状追従性の良い樹脂材料がシール材として用いられている。しかしながら、高圧充填された容器から高圧ガスを供給する場合、配管内にガスが導入された際の断熱圧縮による発熱や衝撃波により、樹脂材料が熱変形、溶損又は焼損するおそれがあった。   Conventionally, nitrogen trifluoride gas has been used as a cleaning gas for semiconductor manufacturing equipment. However, nitrogen trifluoride gas has a high global warming potential of 17200, and in consideration of environmental problems, fluorine with a global warming potential of 0 is used. The amount of gas used has been increasing in recent years. In addition, a resin material having good shape following property is used as a sealing material in order to prevent leakage at the connecting portion of each device and piping in the cleaning gas supply facility. However, when high-pressure gas is supplied from a high-pressure filled container, the resin material may be thermally deformed, melted, or burned out due to heat generated by adiabatic compression and shock waves when the gas is introduced into the pipe.

そこで、樹脂材料が熱変形、溶損又は焼損するのを防ぐため、高圧充填された容器から衝撃波減衰機構を介して消費設備へ供給するガス供給方法が提案されている(例えば、特許文献1,2参照。)。   Therefore, in order to prevent the resin material from being thermally deformed, melted or burned out, a gas supply method has been proposed in which a high-pressure filled container is supplied to a consumption facility via a shock wave attenuation mechanism (for example, Patent Document 1, Patent Document 1). 2).

特開2012−154429号公報JP 2012-154429 A 特開2012−167813号公報JP 2012-167813 A

特許文献1,2に記載されている方法では、衝撃波減衰機構をわざわざ設ける必要があり、供給設備における装置構成が複雑となるだけでなく、消費設備へ必要十分な流量を確保できないことがある。   In the methods described in Patent Documents 1 and 2, it is necessary to bother to provide a shock wave attenuating mechanism, which not only complicates the apparatus configuration in the supply facility, but also may not ensure a necessary and sufficient flow rate to the consumption facility.

そこで本発明は、複雑な装置構成とならずに、構成機器中の樹脂材料が熱変形、溶損又は焼損するのを確実に防ぐことができ、十分な流量を消費設備に供給可能なガス供給方法を提供することを目的としている。   Therefore, the present invention is capable of reliably preventing the resin material in the constituent equipment from being thermally deformed, melted or burned out without having a complicated apparatus configuration, and capable of supplying a sufficient flow rate to the consumption facility. It aims to provide a method.

上記目的を達成するため、本発明のガス供給方法は、容器に高圧充填されているフッ素混合ガスを減圧手段を介して減圧した後に消費設備へ供給するガス供給方法であって、前記容器の容器弁から減圧手段までの配管内に、消費設備への供給圧力よりも高い圧力で、かつ、前記容器の充填圧力よりも低い圧力の不活性ガスを充填する充填封入工程を行い、該充填封入工程後に、前記配管内に前記不活性ガスが封入されたままの状態で前記消費設備へ前記フッ素混合ガスの供給を開始することを特徴としている。 In order to achieve the above object, a gas supply method of the present invention is a gas supply method for supplying a consumption facility after depressurizing a fluorine mixed gas filled in a container with high pressure through a decompression means, the container of the container Filling and filling the pipe from the valve to the decompression means with an inert gas having a pressure higher than the supply pressure to the consuming equipment and lower than the filling pressure of the container, After that , the supply of the fluorine mixed gas to the consuming equipment is started in a state where the inert gas is sealed in the pipe .

また、前記充填封入工程の前に、前記配管内を不活性ガスで置換するパージ処理工程を行うことが好ましく、前記充填封入工程における不活性ガスの圧力が、前記供給圧力の5〜10倍であると好ましい。 Further, it is preferable to perform a purge process step of replacing the inside of the pipe with an inert gas before the filling and sealing step, and the pressure of the inert gas in the filling and sealing step is 5 to 10 times the supply pressure. Preferably there is.

さらに、前記減圧手段のシート材質が三フッ化エチレン樹脂であり、前記消費設備が半導体製造装置であると本発明のガス供給方法を適用するのに好適である。   Furthermore, it is suitable for applying the gas supply method of the present invention that the sheet material of the decompression means is an ethylene trifluoride resin and the consuming equipment is a semiconductor manufacturing apparatus.

本発明によれば、容器の容器弁から減圧手段までの配管内に、消費設備への供給圧力よりも高い圧力で、かつ、前記容器の充填圧力よりも低い圧力の不活性ガスを充填することにより、ガス供給時における配管内での断熱圧縮及び衝撃波を緩和することができるので、樹脂材料の熱変形、溶損又は焼損を確実に防ぐことができる。また、充填封入工程の前に、配管内を不活性ガスで置換するパージ処理工程を行うことにより、不純物の混入を防止することができる。また、充填封入工程における不活性ガスの圧力を供給圧力の5〜10倍にすることで、余剰な不活性ガスを使用することがなく経済性も高い。   According to the present invention, the inert gas having a pressure higher than the supply pressure to the consumption facility and lower than the filling pressure of the container is filled in the pipe from the container valve to the pressure reducing means. Thus, since adiabatic compression and shock waves in the pipe during gas supply can be mitigated, it is possible to reliably prevent thermal deformation, melting or burning of the resin material. Further, by performing a purge process step of replacing the inside of the pipe with an inert gas before the filling and enclosing step, it is possible to prevent impurities from being mixed. In addition, by making the pressure of the inert gas in the filling and enclosing process 5 to 10 times the supply pressure, excessive inert gas is not used and the economy is high.

本発明のガス供給方法を適用した供給設備の一形態例を示す説明図である。It is explanatory drawing which shows one example of the supply equipment to which the gas supply method of this invention is applied.

図1は、本発明のガス供給方法を適用した供給設備の一形態例を示す説明図である。供給設備1は、高圧ガス容器10に高圧充填されているフッ素混合ガスを、減圧手段である圧力調整器11により減圧し、図示しない消費設備、例えば、半導体製造装置に供給するものである。   FIG. 1 is an explanatory diagram showing an example of a supply facility to which the gas supply method of the present invention is applied. The supply facility 1 decompresses the fluorine mixed gas filled in the high-pressure gas container 10 with a pressure regulator 11 as decompression means, and supplies it to a consumption facility (not shown) such as a semiconductor manufacturing apparatus.

高圧ガス容器10の容器弁10aから圧力調整器11までの配管には、上流側から順に第1三方弁12、第1圧力計13、第1フィルター14、第2三方弁15、第1仕切弁16が設けられている。   In the piping from the container valve 10a to the pressure regulator 11 of the high-pressure gas container 10, the first three-way valve 12, the first pressure gauge 13, the first filter 14, the second three-way valve 15, and the first gate valve are sequentially arranged from the upstream side. 16 is provided.

また、圧力調整器11から消費設備までの配管には、上流側から順に、第2圧力計17、第3三方弁18、第2フィルター19、第2仕切弁20、流量計21、第3仕切弁22が設けられている。   In addition, the pipe from the pressure regulator 11 to the consuming equipment has a second pressure gauge 17, a third three-way valve 18, a second filter 19, a second gate valve 20, a flow meter 21, and a third partition in order from the upstream side. A valve 22 is provided.

第1三方弁12の各ポートは、高圧ガス容器10、図示しない不活性ガス供給源及び第1フィルター14にそれぞれ接続されている。   Each port of the first three-way valve 12 is connected to the high-pressure gas container 10, an inert gas supply source (not shown), and the first filter 14.

また、第2三方弁15の2つのポートは、第1フィルター14及び第1仕切弁16に接続され、残りの1つのポートは、排気用管路23に接続されている。第3三方弁18の2つのポートは、圧力調整器11及び第2フィルター19に接続され、残りの1つのポートは、排気用管路24に接続されている。   The two ports of the second three-way valve 15 are connected to the first filter 14 and the first gate valve 16, and the remaining one port is connected to the exhaust pipe 23. Two ports of the third three-way valve 18 are connected to the pressure regulator 11 and the second filter 19, and the remaining one port is connected to the exhaust pipe 24.

次に、本発明のガス供給方法について説明する。まず、高圧ガス容器10の容器弁10a及び圧力調整器11を閉じ、第1仕切弁16を開け、高圧ガス容器10から圧力調整器10までの配管が連通した状態とする。   Next, the gas supply method of the present invention will be described. First, the container valve 10a and the pressure regulator 11 of the high-pressure gas container 10 are closed, the first gate valve 16 is opened, and the piping from the high-pressure gas container 10 to the pressure regulator 10 is in a communicating state.

次に、第1三方弁12の不活性ガス供給源に繋がるポートを開け、配管内に不活性ガスを導入した後、不活性ガス供給源に繋がるポートを再び閉じる。第2三方弁15の排気用管路23に繋がるポートを開け、配管内のガスを放出排気した後、排気用管路23に繋がるポートを再び閉じる。この不活性ガスの導入と排気とを複数回繰り返し行うことにより、配管内に存在した空気が不活性ガスで置換される(本発明のパージ処理工程)。   Next, the port connected to the inert gas supply source of the first three-way valve 12 is opened, and after introducing the inert gas into the pipe, the port connected to the inert gas supply source is closed again. The port connected to the exhaust pipe 23 of the second three-way valve 15 is opened to discharge and exhaust the gas in the pipe, and then the port connected to the exhaust pipe 23 is closed again. By repeatedly introducing and evacuating the inert gas a plurality of times, the air existing in the pipe is replaced with the inert gas (purge process step of the present invention).

パージ処理工程終了後に、第1三方弁12の不活性ガス供給源に繋がるポートを開け、不活性ガスを配管内に充填する。充填された不活性ガスの圧力が、圧力計13により、消費設備への供給圧力よりも高く、かつ、高圧ガス容器10の充填圧力よりも低い所定の圧力になったら、不活性ガス供給源に繋がるポートを閉じ、配管内に不活性ガスを封入する(本発明の充填封入工程)。   After the purge process step is completed, the port connected to the inert gas supply source of the first three-way valve 12 is opened, and the inert gas is filled into the pipe. When the pressure of the filled inert gas becomes a predetermined pressure that is higher than the supply pressure to the consumption equipment and lower than the filling pressure of the high-pressure gas container 10 by the pressure gauge 13, the pressure is supplied to the inert gas supply source. The connecting port is closed and the inert gas is sealed in the pipe (filling and sealing step of the present invention).

その後、第2仕切弁20及び第3仕切弁22を開状態にし、高圧ガス容器10の容器弁を開け、配管内にフッ素混合ガスを導入し、圧力調整器11を開状態に操作することで、消費設備へのガス供給を開始する。   Thereafter, the second gate valve 20 and the third gate valve 22 are opened, the container valve of the high-pressure gas container 10 is opened, the fluorine mixed gas is introduced into the piping, and the pressure regulator 11 is operated to be opened. , Start gas supply to consumption equipment.

以下、実施例と比較例とを比較することにより、本発明の効果について説明する。   Hereinafter, the effect of the present invention will be described by comparing an example and a comparative example.

フッ素ガスを窒素で容積比20%に希釈した混合ガスを10MPaで充填した高圧ガス容器10を用意し、不活性ガスには窒素ガスを用いた。また、圧力調整器11の二次側の圧力を0.2MPaに設定し、圧力調整器11のシート材質にPCTFE(三フッ化エチレン樹脂)を用いた。パージ処理工程後の充填封入工程における窒素ガスの充填圧力を2MPaとした。   A high-pressure gas container 10 filled with a mixed gas obtained by diluting fluorine gas with nitrogen to a volume ratio of 20% was prepared at 10 MPa, and nitrogen gas was used as the inert gas. Further, the pressure on the secondary side of the pressure regulator 11 was set to 0.2 MPa, and PCTFE (ethylene trifluoride resin) was used as the sheet material of the pressure regulator 11. The filling pressure of nitrogen gas in the filling and sealing step after the purge treatment step was set to 2 MPa.

上述のような方法でガス供給を開始し、流量計21にて通ガス量を測定し、500L通ガス毎に窒素ガスにて圧力調整器11のシートリーク検査を実施したところ、23500Lを通ガスさせてもシートリークは認められなかった。   Gas supply was started by the method as described above, the amount of gas passed was measured with the flow meter 21, and the sheet leak inspection of the pressure regulator 11 was performed with nitrogen gas for every 500 L passed gas. No seat leak was observed even when it was used.

<比較例>
一方、比較例として、実施例と同様にパージ処理工程は実施したものの、配管内に窒素ガスを充填することなく、ガス供給を開始した。実施例と同様に、流量計21にて通ガス量を測定し、500L通ガス毎に窒素ガスにて圧力調整器11のシートリーク検査を実施したところ、500Lを通ガスさせた段階でシートリークが確認された。
<Comparative example>
On the other hand, as a comparative example, the purge process was performed in the same manner as in the example, but the gas supply was started without filling the pipe with nitrogen gas. As in the example, the amount of gas flow was measured with the flow meter 21 and the sheet leak inspection of the pressure regulator 11 was performed with nitrogen gas for every 500 L of gas passed. Was confirmed.

比較例において、シートリークが確認されたのは、圧力調整器11のシートのPCTFEが熱的な損傷を受けたものと推察される。一方、実施例のように、配管内に窒素ガスを充填することで、断熱圧縮及び衝撃波の影響は十分緩和できることが確認された。   In the comparative example, it was assumed that the sheet leak was confirmed that the PCTFE of the sheet of the pressure regulator 11 was thermally damaged. On the other hand, it was confirmed that the effects of adiabatic compression and shock waves can be sufficiently mitigated by filling the pipe with nitrogen gas as in the examples.

なお、不活性ガスとしては、窒素ガス以外にアルゴン、ヘリウム、ネオン、キセノン、クリプトン等のガスも使用できるが、安価で購入可能な窒素を利用することが経済的な面から好ましい。   In addition to the nitrogen gas, argon, helium, neon, xenon, krypton, and other gases can be used as the inert gas. However, it is preferable from the economical aspect to use inexpensive and commercially available nitrogen.

また、充填封入工程における圧力は、高圧ガス容器10の充填圧力、消費設備への供給圧圧力(圧力調整器11の二次側圧力)、シート材料の耐熱温度、配管の長さや径等から適宜定めることができる。充填封入工程における圧力が高いほど断熱圧縮や衝撃波が緩和されるといえるが、あまり圧力が高いと供給ガスの濃度低下の要因ともなるし、余剰のガスとなってしまうことから、消費設備の供給圧力の5〜10倍であることが好ましい。   Further, the pressure in the filling and sealing step is appropriately determined from the filling pressure of the high-pressure gas container 10, the supply pressure pressure to the consumption equipment (secondary pressure of the pressure regulator 11), the heat resistant temperature of the sheet material, the length and diameter of the pipe, and the like. Can be determined. It can be said that the higher the pressure in the filling and sealing process, the more adiabatic compression and shock wave will be mitigated. It is preferably 5 to 10 times the pressure.

なお、本形態例の供給設備1における第1三方弁12、第2三方弁15、第3三方弁18は、それぞれ通常の仕切弁を複数組み合わせて構成してもよい。   The first three-way valve 12, the second three-way valve 15, and the third three-way valve 18 in the supply facility 1 of this embodiment may be configured by combining a plurality of normal gate valves.

1…供給設備、10…高圧ガス容器、10a…容器弁、11…圧力調整器、12…第1三方弁、13…第1圧力計、14…第1フィルター、15…第2三方弁、16…第1仕切弁、17…第2圧力計、18…第3三方弁、19…第2フィルター、20…第2仕切弁、21…流量計、22…第3仕切弁、23,24…排気用管路 DESCRIPTION OF SYMBOLS 1 ... Supply equipment, 10 ... High pressure gas container, 10a ... Container valve, 11 ... Pressure regulator, 12 ... First three-way valve, 13 ... First pressure gauge, 14 ... First filter, 15 ... Second three-way valve, 16 ... 1st gate valve, 17 ... 2nd pressure gauge, 18 ... 3rd three-way valve, 19 ... 2nd filter, 20 ... 2nd gate valve, 21 ... Flow meter, 22 ... 3rd gate valve, 23, 24 ... Exhaust Pipeline

Claims (5)

容器に高圧充填されているフッ素混合ガスを減圧手段を介して減圧した後に消費設備へ供給するガス供給方法であって、
前記容器の容器弁から減圧手段までの配管内に、消費設備への供給圧力よりも高い圧力で、かつ、前記容器の充填圧力よりも低い圧力の不活性ガスを充填する充填封入工程を行い、該充填封入工程後に、前記配管内に前記不活性ガスが封入されたままの状態で前記消費設備へ前記フッ素混合ガスの供給を開始するガス供給方法。
A gas supply method for supplying to a consumption facility after depressurizing a fluorine mixed gas filled in a container with high pressure through a depressurization means,
In the pipe from the container valve of the container to the pressure reducing means, a filling and sealing step of filling an inert gas at a pressure higher than the supply pressure to the consuming equipment and lower than the filling pressure of the container, A gas supply method for starting supply of the fluorine mixed gas to the consuming equipment in a state where the inert gas is sealed in the pipe after the filling and sealing step.
前記充填封入工程の前に、前記配管内を不活性ガスで置換するパージ処理工程を行うことを特徴とする請求項1記載のガス供給方法。   2. The gas supply method according to claim 1, wherein a purge process step of replacing the inside of the pipe with an inert gas is performed before the filling and sealing step. 前記充填封入工程における不活性ガスの圧力が、前記供給圧力の5〜10倍であることを特徴とする請求項1又は2記載のガス供給方法。   The gas supply method according to claim 1 or 2, wherein the pressure of the inert gas in the filling and sealing step is 5 to 10 times the supply pressure. 前記減圧手段のシート材質が三フッ化エチレン樹脂であることを特徴とする請求項1乃至3のいずれか1項記載のガス供給方法。   The gas supply method according to any one of claims 1 to 3, wherein a sheet material of the decompression means is an ethylene trifluoride resin. 前記消費設備が半導体製造装置であることを特徴とする請求項1乃至4のいずれか1項記載のガス供給方法。   The gas supply method according to any one of claims 1 to 4, wherein the consumption facility is a semiconductor manufacturing apparatus.
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