JP2008297130A - Method for concentrating ozone gas - Google Patents

Method for concentrating ozone gas Download PDF

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JP2008297130A
JP2008297130A JP2007141184A JP2007141184A JP2008297130A JP 2008297130 A JP2008297130 A JP 2008297130A JP 2007141184 A JP2007141184 A JP 2007141184A JP 2007141184 A JP2007141184 A JP 2007141184A JP 2008297130 A JP2008297130 A JP 2008297130A
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gas
ozone
adsorbent
ozone gas
oxygen
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JP5183099B2 (en
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Kunihiko Koike
国彦 小池
Goichi Inoue
吾一 井上
Sadanori Nakamura
貞紀 中村
Koichi Izumi
浩一 泉
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Iwatani International Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To produce ozone gas which inhibits an ozonolysis reaction in concentration and can safely be concentrated. <P>SOLUTION: In a method for concentrating ozone gas which includes feeding an ozone-oxygen mixed gas produced by an ozonizer into an adsorption tube (2) internally packed with an adsorbent (1) to selectively adsorb the ozone gas on the adsorbent (1), and desorbing the selectively adsorbed ozone gas to concentrate and purify ozone gas, the ozone-oxygen mixed gas fed into the adsorption tube (2) is made free of NOx and this NOx-free ozone-oxygen mixed gas is allowed to act on the adsorbent (1) in an uncooled state to selectively adsorb the ozone gas on the adsorbent (1), and in ozone gas desorption operation, the adsorption tube (2) is evacuated to desorb the ozone gas from the adsorbent (1). <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

本発明は、半導体製造設備等のオゾン消費設備に、所定濃度範囲に濃縮されたオゾンガスを供給する方法に関し、特にオゾン発生器(オゾナイザー)で発生させたオゾンガスを精製して所定濃度範囲の濃縮オゾンガスとして供給する方法に関する。   The present invention relates to a method for supplying ozone gas concentrated in a predetermined concentration range to ozone consuming equipment such as semiconductor manufacturing equipment, and in particular, purified ozone gas generated by an ozone generator (ozonizer) to concentrate ozone gas in a predetermined concentration range. As a method of supplying as.

一般に、オゾンガスは、酸素ボンベからの酸素ガスや大気分離した酸素ガスをオゾン発生器に供給して発生させているが、酸素ガスボンベからの酸素ガスでオゾンガスを発生させても、オゾンガスは酸素ガス中に5〜10 vol%程度の濃度にしかならない。しかも、オゾンガスは自己分解性が強いことから、オゾンガス供給経路中で自己分解し、オゾンガス消費設備に供給された段階では、もっと低濃度になるうえ、その供給濃度も安定しないという性質がある。近年、半導体の製造分野では、基板等での酸化膜形成にオゾンの酸化力を利用することが増えているが、この場合、短時間のうちに適切な厚みの酸化膜を安定的に製膜するには、安定した中濃度のオゾンガスの供給が望まれる。   In general, ozone gas is generated by supplying oxygen gas from an oxygen cylinder or oxygen gas separated into the atmosphere to an ozone generator. However, even if ozone gas is generated by oxygen gas from an oxygen gas cylinder, ozone gas is not contained in oxygen gas. The concentration is only about 5 to 10 vol%. In addition, since ozone gas is highly self-decomposable, it has the property that when it is self-decomposed in the ozone gas supply path and supplied to the ozone gas consuming equipment, the concentration becomes lower and the supply concentration is not stable. In recent years, in the field of semiconductor manufacturing, the use of the oxidizing power of ozone for forming an oxide film on a substrate or the like has increased. In this case, an oxide film having an appropriate thickness can be stably formed in a short time. For this purpose, it is desired to supply a stable medium concentration of ozone gas.

そこで、近年オゾン発生器から発生するオゾンガスの濃度を少しでも高めるために、原料酸素中に少量の窒素ガスを添加するものが提案されている(特許文献1)。
特許第3628461号公報
Therefore, in recent years, there has been proposed a method in which a small amount of nitrogen gas is added to the raw material oxygen in order to increase the concentration of ozone gas generated from the ozone generator as much as possible (Patent Document 1).
Japanese Patent No. 3628461

ところが、原料酸素中に窒素ガスを添加した場合、オゾンガス供給経路を流れている間にオゾン濃度が低下しやすくなる。これは、オゾン発生時に生じたNOxがオゾン分解触媒として作用するためと考えられる。
さらに、その発生したオゾンガスの濃度が求める濃度に達していない場合には、オゾン吸着剤を使用するなどして濃縮することになるが、窒素ガスを添加させて生成したオゾンガスを濃縮すると、異常分解する危険性が高まるという問題もある。
However, when nitrogen gas is added to the raw material oxygen, the ozone concentration tends to decrease while flowing through the ozone gas supply path. This is presumably because NOx generated when ozone is generated acts as an ozone decomposition catalyst.
Furthermore, if the concentration of the generated ozone gas does not reach the required concentration, it will be concentrated by using an ozone adsorbent, etc. However, if the ozone gas generated by adding nitrogen gas is concentrated, abnormal decomposition will occur. There is also a problem that the risk of doing so increases.

本発明は、このような点に着目して、濃縮時でのオゾン分解反応を抑制し、かつ安全に濃縮できるオゾンガスを生成することを目的とする。   The present invention pays attention to such a point, and an object of the present invention is to generate an ozone gas that can be concentrated safely while suppressing the ozone decomposition reaction during concentration.

上述の目的を達成するために請求項1に記載の本発明は、内部に吸着剤を充填してなる吸着筒にオゾン・酸素混合ガスを作用させて、吸着剤にオゾンガスを選択吸着させ、この選択吸着されたオゾンガスを脱離させることでオゾンガスを濃縮精製するオゾンガス濃縮方法において、吸着筒(2)に供給するオゾン・酸素混合ガスをNOxレスとし、このNOxレスのオゾン・酸素混合ガスを非冷却の状態の吸着剤(1)に作用させてオゾンガスを吸着剤(1)に選択吸着させるとともに、オゾンガス脱離操作時に吸着筒を真空引きすることで吸着剤からオゾンガスを脱離させるようにしたことを特徴としている。   In order to achieve the above-mentioned object, the present invention according to claim 1 is configured such that an ozone / oxygen mixed gas acts on an adsorption cylinder filled with an adsorbent inside to selectively adsorb ozone gas to the adsorbent. In the ozone gas concentration method of concentrating and purifying ozone gas by desorbing the selectively adsorbed ozone gas, the ozone / oxygen mixed gas supplied to the adsorption cylinder (2) is made NOx-less, and this NOx-less ozone / oxygen mixed gas is made non- The ozone gas is selectively adsorbed on the adsorbent (1) by acting on the adsorbent (1) in a cooled state, and ozone gas is desorbed from the adsorbent by evacuating the adsorption cylinder during the ozone gas desorption operation. It is characterized by that.

ここで非冷却状態にある吸着剤とは、吸着剤の吸着性能を高めるために外部から熱エネルギーを供給することをやめる状態を指している。このため、吸着剤がオゾンと反応して発生する反応熱で昇温することを防止するための僅かな冷却は非冷却の範疇にある。   Here, the adsorbent in an uncooled state refers to a state in which the supply of heat energy from the outside is stopped in order to enhance the adsorption performance of the adsorbent. For this reason, slight cooling for preventing the temperature of the adsorbent from rising due to reaction heat generated by reaction with ozone is in the range of non-cooling.

請求項2に記載の本発明は、純酸素ガスを原料としてオゾンガスと酸素ガスとの混合ガスを生成することにより、NOxレスの混合ガスとしたことを特徴とし、請求項3に記載の発明は、窒素ガスを添加した原料ガスをオゾン発生器に供給して生成したオゾンガスと酸素ガスとの混合ガスからNOxを除去することによリNOxレスの混合ガスとしたことを特徴としている。   The present invention described in claim 2 is characterized in that a mixed gas of ozone gas and oxygen gas is produced using pure oxygen gas as a raw material to form a NOx-less mixed gas, and the invention described in claim 3 is characterized in that The raw material gas to which nitrogen gas is added is supplied to an ozone generator, and NOx is removed from the mixed gas of ozone gas and oxygen gas generated to form a NOx-less mixed gas.

本発明では、吸着筒に供給するオゾン・酸素混合ガスをNOxレスとし、冷却をすることなくいわゆる常温状態に保持した吸着剤に、そのNOxレスのオゾン・酸素混合ガスを作用させてオゾンガスを選択吸着させ、この選択吸着されたオゾンガスを吸着剤から脱離させることでオゾンガスを濃縮精製しているので、オゾン発生器でのオゾン発生時にNOxの発生がなくなるから、オゾンガスの自己分解を抑制することができるうえ、オゾンガスの濃縮時にも異常分解反応を抑制することができる。   In the present invention, the ozone / oxygen mixed gas supplied to the adsorption cylinder is made NOx-less, and the ozone gas is selected by allowing the NOx-less ozone / oxygen mixed gas to act on the adsorbent kept at a so-called normal temperature state without cooling. Since the ozone gas is concentrated and purified by adsorbing and desorbing this selectively adsorbed ozone gas from the adsorbent, NOx generation is eliminated when ozone is generated in the ozone generator, thus suppressing the self-decomposition of ozone gas. In addition, the abnormal decomposition reaction can be suppressed even when the ozone gas is concentrated.

図1は本発明方法を実施する装置の一例を示す系統図である。このオゾンガス濃縮装置は、内部にオゾンガスを選択吸着するシリカゲル等の吸着剤(1)を充填した吸着筒(2)と、純酸素ガスからなるオゾン原料ガス源(図示略)と吸着筒(2)とを連通接続するガス導入路(3)と、吸着筒(2)から導出された精製オゾンガス導出路(4)と、吸着筒(2)から導出されたスルーガスのガス排出路(5)とを有している。なお、本実施形態では吸着筒(2)は2基並列して配置してあり、一方の吸着筒が吸着工程時には他方の吸着筒が脱離工程になるように構成してある。   FIG. 1 is a system diagram showing an example of an apparatus for carrying out the method of the present invention. This ozone gas concentrator includes an adsorption cylinder (2) filled with an adsorbent (1) such as silica gel for selectively adsorbing ozone gas, an ozone source gas source (not shown) made of pure oxygen gas, and an adsorption cylinder (2). A gas introduction path (3) that communicates with each other, a purified ozone gas lead-out path (4) derived from the adsorption cylinder (2), and a gas discharge path (5) for the through gas derived from the adsorption cylinder (2). Have. In the present embodiment, two adsorption cylinders (2) are arranged in parallel, and when one adsorption cylinder is in the adsorption process, the other adsorption cylinder is in the desorption process.

ガス導入路(3)は各吸着筒(2)にそれぞれガス導入弁を介して接続されており、このガス導入路(3)には上流側から順に、オゾン発生器(6)とマスフローコントローラとが配置してある。そして、オゾン発生器(6)で発生したオゾン・酸素混合ガスを一定の流量で各吸着筒(2)にガス導入弁の切換え制御により択一的に供給するようにしてある。   The gas introduction path (3) is connected to each adsorption cylinder (2) via a gas introduction valve. The gas introduction path (3) is connected to an ozone generator (6), a mass flow controller, and the like in order from the upstream side. Is arranged. The ozone / oxygen mixed gas generated by the ozone generator (6) is alternatively supplied to each adsorption cylinder (2) at a constant flow rate by switching control of the gas introduction valve.

一方、精製オゾンガス導出路(4)は各吸着筒(2)にガス導出弁を介して接続されており、この精製オゾンガス導出路(4)には、ダイアフラム型真空ポンプ(7)、バッファタンク(8)、マスフローコントローラ(9)、流路開閉弁(10)が吸着筒側から順に配置してある。そして、吸着筒(2)とダイアフラム型真空ポンプ(7)とがガス導出弁の切換え制御により択一的に連通するようにしてある。   On the other hand, the purified ozone gas lead-out path (4) is connected to each adsorption cylinder (2) via a gas lead-out valve. The purified ozone gas lead-out path (4) includes a diaphragm vacuum pump (7), a buffer tank ( 8) A mass flow controller (9) and a flow path opening / closing valve (10) are arranged in this order from the adsorption cylinder side. The adsorption cylinder (2) and the diaphragm type vacuum pump (7) are alternatively communicated by switching control of the gas outlet valve.

また、ガス排出路(5)は精製オゾンガス導出路(4)から分岐する状態で連出されており、このガス排出路(5)にはオゾン分解器(11)が配置してあり、このオゾン分解器(11)の出口は大気に開口している。そして、また、ガス排出路(5)のオゾン分解器(11)よりも上流側から分岐導出された循環路(12)には循環ポンプ(13)が装着してあり、この循環路(12)はオゾン発生器(6)の上流側に接続されている。   Moreover, the gas discharge path (5) is continuously led out from the purified ozone gas lead-out path (4), and an ozone decomposer (11) is arranged in the gas discharge path (5). The outlet of the decomposer (11) is open to the atmosphere. In addition, a circulation pump (13) is attached to the circulation path (12) branched and led out from the upstream side of the ozone decomposing unit (11) of the gas discharge path (5), and this circulation path (12) Is connected to the upstream side of the ozone generator (6).

このように構成したオゾンガス濃縮装置では、例えば液体酸素を気化させることで得られた純酸素をオゾン発生器(6)に供給することで、オゾン発生器(6)で純酸素ガスをオゾン化してオゾン・酸素混合ガスを生成する。純酸素を原料ガスとしてオゾン化した場合には、生成されたオゾン・酸素混合ガスにはNOxは含まれていない。このオゾン・酸素混合ガスを一方の吸着筒(2)に供給して、吸着筒(2)内を流通させる。このとき、吸着剤(1)は外部から加熱や冷却の熱エネルギーを付与されることなく、いわゆる常温状態(自然放置状態)を維持している。吸着筒(2)に供給されたオゾン・酸素混合ガスは、そのうちのオゾンガス成分が吸着剤(1)に吸着され、吸着され残った一部のオゾンガスとキャリアガスとしての酸素ガスがガス排出路(5)からオゾン分解器(11)に送り込まれる。   In the ozone gas concentrator thus configured, for example, pure oxygen obtained by vaporizing liquid oxygen is supplied to the ozone generator (6), so that the ozone generator (6) ozonizes the pure oxygen gas. Generates ozone / oxygen mixed gas. When pure oxygen is ozonized as a raw material gas, the generated ozone / oxygen mixed gas does not contain NOx. This ozone / oxygen mixed gas is supplied to one adsorption cylinder (2) and circulated in the adsorption cylinder (2). At this time, the adsorbent (1) maintains a so-called normal temperature state (natural standing state) without being given heat energy for heating and cooling from the outside. The ozone / oxygen mixed gas supplied to the adsorption cylinder (2) has its ozone gas component adsorbed by the adsorbent (1), and a part of the remaining ozone gas and oxygen gas as the carrier gas are discharged into the gas discharge channel ( 5) is sent to the ozonolysis device (11).

オゾン・酸素混合ガスを吸着筒(2)に所定時間流して、吸着剤(1)での吸着量が所定量になると、今まで、オゾン・酸素混合ガスを流していた吸着筒(2)でのガス導入弁とガス排出弁とを閉弁するとともに、ガス導出弁を開弁して、吸着筒(2)内を真空ポンプ(7)に連通させて、真空脱離により吸着剤(1)からオゾン成分を脱離し、その脱離した精製オゾンガスをバッファタンク(8)に送給する。   When the ozone / oxygen mixed gas is allowed to flow through the adsorption cylinder (2) for a predetermined time and the adsorbed amount in the adsorbent (1) reaches a predetermined amount, The gas inlet valve and the gas discharge valve of the gas generator are closed, the gas outlet valve is opened, the inside of the adsorption cylinder (2) is connected to the vacuum pump (7), and the adsorbent (1) is removed by vacuum desorption The ozone component is desorbed from the water and the purified ozone gas desorbed is sent to the buffer tank (8).

バッファタンク(8)に一旦貯留することで、吸着筒(2)からの脱離オゾンガス濃度に濃度変化があっても、バッファタンク(8)内で平均化させることができ、一定範囲の濃度を維持した状態でオゾン消費設備等に供給することができる。   Once stored in the buffer tank (8), even if there is a change in the concentration of desorbed ozone gas from the adsorption cylinder (2), it can be averaged in the buffer tank (8), and a certain range of concentrations can be obtained. It can be supplied to ozone consuming equipment or the like in a maintained state.

この一方の吸着筒(2)が脱離操作を行っている間に他方の吸着筒(2)は吸着操作を行い、2基の吸着筒(2)で吸着−脱離を交互に行うことにより、連続して精製オゾンガスを取り出すようにしている。なお、この吸着筒(2)は3基以上であってもよく、3基以上の吸着筒(2)での各弁切換えタイミングを制御することで、連続的に精製オゾンガスを取り出すことができる。   While the one adsorption cylinder (2) is performing the desorption operation, the other adsorption cylinder (2) is performing the adsorption operation, and the adsorption-desorption is alternately performed by the two adsorption cylinders (2). The purified ozone gas is taken out continuously. Note that the number of the adsorption cylinders (2) may be three or more, and the purified ozone gas can be continuously taken out by controlling the valve switching timing of the three or more adsorption cylinders (2).

なお、この場合の吸着剤としては、金属成分の少ない高純度シリカゲルが好ましいが、一般的なシリカゲルやゼオライト等の吸着剤であってもよい。   In this case, the adsorbent is preferably high-purity silica gel having a small amount of metal components, but may be an adsorbent such as general silica gel or zeolite.

また、オゾン生成原料としての純酸素としては、前述の液体酸素を気化させたもののほか、不純物の混合濃度が100ppmよりも少ない高純度酸素ガスを使用することができる。   Moreover, as pure oxygen as an ozone production | generation raw material, in addition to what vaporized the above-mentioned liquid oxygen, the high purity oxygen gas with a mixed concentration of impurities less than 100 ppm can be used.

さらに、オゾン生成原料として空気分離等で得られた酸素ガスを用いたり、窒素ガスを微量添加した酸素ガスを用いたりし、オゾン発生器(6)でオゾン−酸素混合ガス生成直後にNOx除去するようにしてもよい。   Further, oxygen gas obtained by air separation or the like is used as an ozone generation raw material, or oxygen gas to which a small amount of nitrogen gas is added is used, and NOx is removed immediately after the ozone-oxygen mixed gas is generated by the ozone generator (6). You may do it.

図2は、窒素ガスを0.5 vol%添加した酸素ガスを原料として放電式オゾン発生器に供給して生成したオゾン−酸素混合ガスと、窒素ガスを添加することなく酸素ガスを原料として放電式オゾン発生器に供給して生成したオゾン−酸素混合ガスとをそれぞれ内容積10リットルのステンレス容器に封入圧力約0.147MPa(1100Torr)で封入した場合のオゾンガス濃度の時間変化を示す。   FIG. 2 shows an ozone-oxygen mixed gas produced by supplying 0.5 vol% of nitrogen gas as a raw material to a discharge-type ozone generator and a discharge using oxygen gas as a raw material without adding nitrogen gas. The time-dependent change of the ozone gas concentration when the ozone-oxygen mixed gas generated by supplying to the ozone generator is sealed in a stainless steel container having an internal volume of 10 liters at a sealing pressure of about 0.147 MPa (1100 Torr) is shown.

図2からも分かるように、窒素ガスを添加した酸素ガスを原料としてオゾンガスを生成すると、時間の経過とともに、オゾンガス濃度が低下しているのに対し、窒素ガスを添加しないものでは、時間経過にかかわらず、ほとんどオゾンガス濃度に変化がない。これは、オゾン発生器でオゾンを発生させる際に、窒素酸化物(NOx)が生成され、このNOxがオゾンの自己分解に対する分解触媒として作用していると考えられる。   As can be seen from FIG. 2, when ozone gas is generated using oxygen gas added with nitrogen gas as a raw material, the ozone gas concentration decreases with the passage of time. Regardless, there is almost no change in ozone gas concentration. This is considered that nitrogen oxide (NOx) is generated when ozone is generated by the ozone generator, and this NOx acts as a decomposition catalyst for the self-decomposition of ozone.

図3は、オゾン発生器から発生したオゾンを濃縮する場合での異常分解発生状態に関する生成したオゾンガスの発生濃度と添加した窒素濃度との関係を示す関係図である。この場合、オゾン濃度が400g/m(18.7 vol%)となるように濃縮した。 FIG. 3 is a relational diagram showing the relationship between the concentration of generated ozone gas and the concentration of added nitrogen regarding the abnormal decomposition occurrence state in the case of concentrating ozone generated from an ozone generator. In this case, it concentrated so that ozone concentration might be set to 400 g / m < 3 > (18.7 vol%).

図3から分かるように、窒素ガスを100ppm(0.01 vol%)よりも多く添加して、発生時のオゾンガス濃度を高めると、濃縮時に異常分解(爆発)を起こすが、窒素ガスの添加量が100ppm(0.01 vol%)よりも少ない場合には、濃縮しても異常分解は起こらないことが確認できた。   As can be seen from Fig. 3, adding more nitrogen gas than 100 ppm (0.01 vol%) and increasing the ozone gas concentration during generation causes abnormal decomposition (explosion) during concentration, but the amount of nitrogen gas added Was less than 100 ppm (0.01 vol%), it was confirmed that no abnormal decomposition occurred even when concentrated.

本発明の技術は、安定した濃度のオゾンガスを必要とする半導体製造設備等のオゾン消費設備に利用することができる。   The technology of the present invention can be used for ozone consuming equipment such as semiconductor manufacturing equipment that requires ozone gas having a stable concentration.

本発明方法を実施する装置の一例を示す系統図である。It is a systematic diagram which shows an example of the apparatus which implements the method of this invention. 発生オゾンガスの時間経過による濃度変化を示すグラフである。It is a graph which shows the density | concentration change with time passage of generated ozone gas. 発生したオゾンガスの濃縮に伴う異常分解発生状況を説明する図である。It is a figure explaining the abnormal decomposition | disassembly generation | occurrence | production situation accompanying the concentration of the generated ozone gas.

符号の説明Explanation of symbols

1…吸着剤、2…吸着筒。
1 ... adsorbent, 2 ... adsorption cylinder.

Claims (4)

内部に吸着剤(1)を充填してなる吸着筒(2)にオゾン発生器で生成したオゾン・酸素混合ガスを作用させて、吸着剤(1)にオゾンガスを選択吸着させ、この選択吸着されたオゾンガスを脱離させることでオゾンガスを濃縮精製するオゾンガス濃縮方法において、
吸着筒(2)に供給するオゾン・酸素混合ガスをNOxレスとし、このNOxレスのオゾン・酸素混合ガスを非冷却の状態の吸着剤(1)に作用させてオゾンガスを吸着剤(1)に選択吸着させるとともに、オゾンガス脱離操作時に吸着筒(2)を真空引きすることで吸着剤(1)からオゾンガスを脱離させるようにしたことを特徴とするオゾンガス濃縮方法。
The ozone / oxygen mixed gas generated by the ozone generator is allowed to act on the adsorption cylinder (2) filled with the adsorbent (1), and the adsorbent (1) is selectively adsorbed with ozone gas. In the ozone gas concentration method of concentrating and purifying ozone gas by desorbing the ozone gas,
The ozone / oxygen mixed gas supplied to the adsorption cylinder (2) is made NOx-less, and this ozone / oxygen mixed gas is made to act on the uncooled adsorbent (1) to convert the ozone gas into the adsorbent (1). A method of concentrating ozone gas, wherein the ozone gas is desorbed from the adsorbent (1) by selectively adsorbing and evacuating the adsorption cylinder (2) during the ozone gas desorption operation.
純酸素ガスを原料ガスとしてオゾン発生器に供給してオゾンガスと酸素ガスとの混合ガスを生成することにより、NOxレスのオゾン・酸素混合ガスとした請求項1に記載のオゾンガス濃縮方法。   The ozone gas concentration method according to claim 1, wherein pure oxygen gas is supplied to an ozone generator as a raw material gas to generate a mixed gas of ozone gas and oxygen gas, thereby producing a NOx-less ozone / oxygen mixed gas. 窒素ガスを添加した原料ガスをオゾン発生器に供給して生成したオゾンガスと酸素ガスとの混合ガスからNOxを除去することにより、NOxレスのオゾン・酸素混合ガスとした請求項1に記載のオゾンガス濃縮方法。   2. The ozone gas according to claim 1, wherein NOx is removed from a mixed gas of ozone gas and oxygen gas generated by supplying a raw material gas added with nitrogen gas to an ozone generator to form a NOx-less ozone / oxygen mixed gas. Concentration method. 吸着剤(1)を高純度シリカゲルで構成した請求項1〜4のいずれか1項に記載のオゾンガス濃縮方法。   The ozone gas concentration method according to any one of claims 1 to 4, wherein the adsorbent (1) is composed of high-purity silica gel.
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