JP2004163293A - Method and apparatus for measuring ozone gas concentration - Google Patents

Method and apparatus for measuring ozone gas concentration Download PDF

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Publication number
JP2004163293A
JP2004163293A JP2002330152A JP2002330152A JP2004163293A JP 2004163293 A JP2004163293 A JP 2004163293A JP 2002330152 A JP2002330152 A JP 2002330152A JP 2002330152 A JP2002330152 A JP 2002330152A JP 2004163293 A JP2004163293 A JP 2004163293A
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ozone gas
ozone
concentration
ultraviolet
gas flow
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JP4009523B2 (en
Inventor
Kunihiko Koike
国彦 小池
Sadanori Nakamura
貞紀 中村
Shunsuke Hosokawa
俊介 細川
Masaharu Otsuki
雅晴 大槻
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DYLEC Inc
MASUDA KENKYUSHO KK
Iwatani Corp
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DYLEC Inc
MASUDA KENKYUSHO KK
Iwatani International Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method and an apparatus for measuring ozone gas concentration, which can easily and accurately measure the ozone gas concentration even in the case ozone gas is present at high concentrations. <P>SOLUTION: In the method, an ozone concentration measuring apparatus which is an ultraviolet ray absorption type, is disposed in an ozone gas supplying system, and the ozone gas flows through the ozone gas supplying system in a negative pressure condition. The ozone gas concentration of the gas to be measured is determined based on both an absorption value of light being detected by the ultraviolet ray absorption type ozone concentration measuring apparatus and an absolute pressure value being detected at the region where the ultraviolet ray absorption type ozone concentration measuring apparatus is disposed. <P>COPYRIGHT: (C)2004,JPO

Description

【０００１】
【発明の属する技術分野】
本発明は、オゾンガス濃度の計測方法及びその装置に関し、特に、発生したオゾンを濃縮して得られる高濃度オゾンガスや極低流量でオゾナイザーを運転した際に得られる高濃度オゾンガスの濃度計測方法及びその装置に関する。
【０００２】
【従来の技術】
従来から、オゾンガスの濃度を計測する方法として紫外線吸収法が知られている。これは、オゾンが紫外線領域の２５４ｎｍ付近に最大吸収帯を持ち、この２５４ｎｍ域では他の気体の吸収強度が小さいことを利用して濃度を求める方法であり、オゾンを含まない標準ガス（ゼロガス）と、計測対象ガス（試料ガス）とをオゾンガス濃度計の紫外線吸収セル内に個別に流し、それぞれの吸光強度から計測対象ガスのガス濃度を計測するようになっている。
【０００３】
【特許文献１】
特開２０００−１９１０７号公報（段落０００２〜０００４、図４）
【０００４】
【発明が解決しようとする課題】
ところが、従来の紫外線吸収式オゾンガス濃度計は、オゾンガス濃度１０ｖｏｌ ％以下のオゾンガスの濃度測定用に形成してあり、オゾンガス濃度１５ｖｏｌ ％以上の高濃度オゾンガスの濃度を計測できるものは提供されていない。
【０００５】
さらに、オゾンガスの圧力が高い場合、例えば、大気圧下では紫外線吸光光路、すなわち、オゾンガスの厚みを５０μｍと薄くしてもオゾンガス濃度が１０ｖｏｌ ％を超えると大部分の紫外線がオゾンガスに吸収されるため、高精度のオゾン濃度検出ができなかった。
【０００６】
これは従来、純酸素ガスを原料として高能力のオゾン発生器でオゾンを発生させても通常の運転方法では１０ｖｏｌ ％程度の濃度のオゾンガスしか生成することができず、１５ｖｏｌ ％以上の高濃度オゾンガスが実用化されていなかったことに起因していると考えられる。
【０００７】
近年、半導体製造分野等では、酸化膜製造等の用途に使用するために１５ｖｏｌ ％以上の高濃度オゾンが要望されてきている。この場合、オゾンガスの濃度は酸化膜厚形成に大きな影響を及ぼすことになるから、高濃度オゾンガスの濃度を高精度に、しかもインラインで計測できるオゾンガス濃度計測技術が待望されている。
【０００８】
本発明は、このような点に着目してなされたものであり、高濃度のオゾンガスでも、容易に、かつ正確にその濃度を測定することのできるオゾンガス濃度の計測方法並び計測装置を提供することを目的とする。
【０００９】
【課題を解決するための手段】
上述の目的を達成するために請求項１に記載の本発明では、オゾンガス流通路に両面を紫外線透過ガラスで構成した紫外線透過窓を形成し、その一側に紫外線発光部を、他側に紫外線受光部をそれぞれ配置し、オゾンによる紫外線吸光強度を計測することでオゾン濃度を計測するオゾンガス濃度計測方法において、オゾンガス流通路に負圧のオゾンガスを流通させ、このオゾンガス流通路での絶対圧を紫外線吸光強度と同時に計測し、これらの計測値からオゾン濃度を求めるようにしたことを特徴としている。
【００１０】
また、請求項２に記載の発明では、オゾンガス流通路内を流通させるオゾンガスの圧力を１００Ｐａ〜５０ｋＰａとしたことを特徴とし、請求項３に記載の発明では、オゾンガス流通路内を流れるオゾンガス流量を計測し、該ガス通路のコンダクタンスと、計測したオゾンガス流量とに基づき紫外線透過ガラス部の絶対圧力を補正して、オゾンガス濃度を求めるようにしたことを特徴とし、請求項４に記載の発明では、オゾンガス流通路内を流れるオゾンガス流量を計測し、予め求めておいた紫外線透過ガラス部を通過する際に生ずる紫外線照射により分解するオゾン分解率とオゾンガス流量ならびにオゾン濃度の関係からオゾン濃度の補正を行うようにしたことを特徴とし、請求項５に記載の発明では、オゾンガス流通路内を流れるオゾンガス流量を１００ｓｃｃｍ以下に設定したことを特徴とし、請求項６に記載した発明は、オゾンガス流通路内のガス温度とオゾンガス流路自体の温度との少なくとも一方を計測し、オゾン濃度を標準状態に換算することを特徴とし、請求項７に記載した発明は、オゾンガス流通路内を流通するオゾンガスをオゾンガス濃度１５ｖｏｌ ％以上の高濃度オゾンガスにしたことを特徴としている。
【００１１】
さらに、請求項８に記載の発明では、オゾンガス流通路内の絶対ガス圧を１００Ｐａ以下とすることでオゾンガス濃度の零点補正を行うことを特徴とし、請求項９に記載の発明は、オゾンガスを密閉容器に封入し電気火花などでオゾンガスを完全に分解し、その圧力上昇から求めたオゾン濃度を校正値とすることを特徴としている。
【００１２】
請求項１０に記載の本発明は、オゾンガス流通路の両面を紫外線透過ガラスで構成した紫外線透過窓を形成しその一側に紫外線発光部を、他側に紫外線受光部をそれぞれ配置し、オゾンによる紫外線吸光強度を計測することでオゾン濃度を計測するオゾンガス濃度計測装置において、オゾンガス流通路の出口側を真空ポンプで排気するとともに紫外線透過窓近傍に圧力センサーを配して、オゾンガス流通路内の絶対圧を紫外線吸光強度と同時に計測し、これらの計測値をオゾン濃度算出部に伝達してオゾン濃度を求めることを特徴としたものである。
【００１３】
そして、請求項１１に記載した発明では、紫外線透過窓を構成している紫外線透過ガラスの間隔を５０μｍ以上に構成したことを特徴とし、請求項１２に記載した発明は、オゾンガス流通路を流れるオゾンガス流量を制御するとともにオゾンガス流量値をオゾンガス濃度算出部に伝達してオゾン濃度を補正することを特徴とし、請求項１３に記載した発明は、オゾンガス流通路内とオゾンガス流通路を構成している配管との少なくとも一方にオゾンセンサーを取り付けてオゾンガス濃度を計測し、その計測値をオゾンガス濃度算出部に伝達してオゾン濃度を補正することを特徴とし、請求項１４に記載の発明は、オゾンガス算出部では紫外線透過窓におけるオゾンガスの絶対圧、温度がセンサーの計測値から換算されると共に、オゾンガスの濃度と紫外線吸光強度、オゾンガスの絶対圧、温度、オゾンガス流量、紫外線照射によるオゾン分解率との関係が定義されていることを特徴とし、請求項１５に記載の発明は、オゾンガス流通路の出口がオゾン処理をする真空槽に直接接続されており、濃度計測済みのオゾンガスをオゾン処理に使用するようにしたことを特徴とし、請求項１６に記載の発明は、オゾンガス流通路の内面を高濃度オゾンで不動態化処理したことを特徴とし、請求項１７に記載の発明は、オゾンガス流通路の両面に紫外線透過ガラスで構成した紫外線透過窓を形成しその一側に紫外線発光部を、他側に紫外線受光部をそれぞれ配置し、オゾンによる紫外線吸光強度を計測することでオゾン濃度を計測するオゾンガス濃度計測装置において、ガス通路内でのガス圧を１００Ｐａ以下に設定し、オゾンガス濃度のゼロガス構成を行うように構成したことを特徴としている。
【００１４】
【発明の作用】
本発明では、両面を紫外線透過ガラスで構成してある紫外線透過窓の一側に紫外線発光部を、他側に紫外線受光部をそれぞれ配置してなるオゾンガス流通路（紫外線吸収セル）に、測定対象となるオゾンガスを負圧の圧力条件で流通させている。これにより、流通ガス中のオゾン分子数の絶対量が少なくなり、オゾン濃度が高濃度となった場合は特に、僅かな濃度変化があっても、吸光強度に大きな差が現れる。したがって、オゾン濃度を高精度に測定することができることになる。
【００１５】
また、同じオゾン濃度でもオゾン分子数は流通ガスの圧力に比例するため、オゾン濃度を正確に得るためには、紫外線吸収セル部分の絶対圧を正確に測定することが不可欠である。本発明では、オゾンガス流通路の絶対圧を計測し、その計測値を直接用い、または、オゾンガス流量に応じた補正を行うことで紫外線吸収セル部分での絶対圧を算出し、オゾン濃度を求めるように構成している。
【００１６】
さらに、流通ガス流量が小さい場合、特に、１００ｓｃｃｍ以下では紫外線吸光セル部分で紫外線を照射された場合、紫外線の吸光と同時に、オゾン分解が発生するため、紫外線の吸光強度は実際のオゾン濃度よりも小さくなってしまう。そこで、予め、紫外線照射によるオゾン分解率とオゾンガス流量並びにオゾン濃度の関係を求めておき、オゾン濃度を補正する構成としている。
【００１７】
また、オゾンガス流通路内のガス温度を直接計測することで、オゾン濃度を標準状態に換算できる。ただし、流通ガスが負圧で流量が小さい場合、紫外線吸光セル近傍のオゾンガス流路自体の温度自体を計測したほうが、オゾンガス自体の温度の計測点が紫外線吸光セルから離れる場合には、より正確な計測ができる。
【００１８】
さらに、定期的な零点補正は、通常はガス流路を切り替えてオゾンを含まない空気や酸素などを供給した時の紫外線吸光強度をリファレンスとして補正を行っているが、本発明ではオゾンガス流通路の圧力を１００Ｐａ以下とすることで残存するオゾン分子量を非常に少なくすることで零点補正を行うことができる。
【００１９】
一方、オゾン濃度の構成は、負圧のオゾンガスを密閉容器内に封入し電気火花などを用いてオゾンガスを完全に分解し、密閉容器の圧力上昇からオゾン濃度を求める爆発法を基準として行うことで、負圧下のオゾンガス濃度の校正も可能となる。
【００２０】
【発明の実施の形態】
図１は本発明を適用したオゾンガス供給系での濃度測定システムの概略構成図であり、オゾンガス供給源（１）と真空ポンプ（４）との間に、オゾンガス濃度計測装置（２）が装着してある。また、オゾンガス濃度計測装置（２）を校正する場合には、爆発式オゾン濃度校正器（３）を、例えば、オゾンガス濃度計測装置（２）と真空ポンプ（４）に接続すると良い。
【００２１】
オゾンガス濃度計測装置（２）は図２に示すように、内部にオゾンガス流通路（５）を形成しているケーシング（６）に紫外線透過窓（７）を形成し、この紫外線透過窓（７）部分に一対の紫外線透過ガラス（８）を５０μｍ以上の間隔を持たせた状態で対向させて配置し、紫外線透過ガラス（８）間をオゾンガス流通路（５）に形成することで紫外線吸収セルに構成してある。そして、紫外線透過ガラス（８）で形成した紫外線透過窓（７）部分に、紫外線発光部（９）と紫外線受光部（１０）とが紫外線透過ガラス（８）で形成したオゾンガス流通路（５）を挟んで対向する状態に配置してある。そして、オゾンガス濃度計測装置（２）は、そのオゾンガス流通路（５）における出口路部分を図１で示した爆発式オゾン濃度構成器（３）の代わりにオゾンガス消費装置（図示略）を介して前記真空ポンプ（４）に接続し、オゾンガス濃度計測装置（２）でガス濃度を計測されたオゾンガスをオゾンガス消費装置に供給するとよい。
【００２２】
紫外線発光部（９）は、紫外線ランプ（１１）と、紫外線ランプ電源（１２）と、紫外線（３０）を透過光（３１）と反射光（３２）に分割するハーフミラー（１３）とで形成してある。そして、紫外線受光部（１０ａ）での紫外線透過窓（７）を通過した反射光（３２）の紫外線光量と紫外線受光部（１０ｂ）での透過光（３１）の紫外線光量をオゾン濃度算出装置（１４）に伝達するようにしてある。勿論、紫外線発光部（９）の構成により透過光（３１）が紫外線透過窓（７）を通過する場合もある。
【００２３】
オゾンガス濃度計測装置（２）での紫外線透過窓（７）の近傍部にオゾンガス流通路（５）内の圧力を検知する圧力センサー（１５）とオゾンガス流通路（５）内を流れるオゾンガスの温度を検知する温度センサー（１６ａ）とが配置してある。そして、この圧力センサー（１５）で検出した圧力信号と温度センサー（１６ａ）で検出した温度信号は、前記オゾン濃度算出装置（１４）に入力されるようになっている。なお、オゾンガス流量が少ない場合には紫外線透過窓（７）の極近傍のケーシング（６）に取り付けた温度センサー（１６ｂ）を用いた方がオゾンガス温度を正確に計測できる。
【００２４】
また、オゾンガス濃度計測装置（２）の紫外線透過窓（７）を形成している個所よりも下流側に位置するガス出口路（１７）にマスフローコントローラ（１８）が配置してある。なお、オゾンガス濃度計測装置（２）でのオゾンガス流通路（５）やオゾンガス供給路（１９）の内面を高濃度（例えば１５ｖｏｌ％以上）に濃縮処理したオゾンガスで不動態化処理しておくと、オゾンガス流通路（５）やオゾンガス供給路（１９）の内面に酸化不動態膜が形成され、オゾンガスの自然分解や流路壁面との反応によりオゾンガスが分解消費されることを防止することができる。
図中符号（２０）はオゾン濃度算出装置（１４）で算出されたオゾンガス濃度の表示部である。
【００２５】
オゾンガス供給源（１）としては、空気分離装置や酸素ガスシリンダ等の酸素源と、オゾン発生器及びオゾンガス濃縮装置等とで構成したオゾン製造ユニットや、高濃度オゾンガスを貯蔵したガスシリンダなどのガス貯蔵容器が考えられる。
【００２６】
このように構成したオゾンガス濃度測定システムでは、負圧状態（１００Ｐａ〜５０ｋＰａ）でオゾンガス供給路（１９）を所定流量（１００ｓｃｃｍ）で流れているオゾンガスをオゾンガス濃度計測装置（４）に導入して測定した紫外線吸光強度をオゾン濃度算出装置（１４）に入力し、オゾン濃度算出装置（１４）では紫外線吸光強度を温度、圧力及びオゾン流量に基づいて補正して演算することにより、オゾンガス流通路（５）内を流れるオゾンガス濃度を計測して表示部（２０）に表示するようになっている。この場合、オゾンガス流通路（５）のコンダクタンスとオゾンガス流通路（５）内を流れているガス流量とに基づいて紫外線吸収セル部分での絶対圧を補正している。また、オゾンガス流通路（５）内の圧力を１００Ｐａ（０．７Ｔｏｒｒ）以下の真空状態にして紫外線吸光強度を計測することにより、無オゾン状態での紫外線吸光強度を計測してゼロガス校正を行っている。
【００２７】
ここで、測定対象ガス（オゾンガス）での紫外線吸光強度をＩ、標準ガス又は１００Ｐａ以下の真空状態での紫外線吸光強度をＩ０、モル吸光係数をε［Ｌ／ｍｏｌ・ｃｍ］、測定光路長をｄ［ｃｍ］、オゾン濃度をＣ［ｍｏｌ／Ｌ］、測定対象ガスの圧力をＰ［ｋＰａ］、測定対象ガスの温度をＴ［Ｋ］、基準圧をＰＮ（１０１．３ｋＰａ）、基準温度をＴＮ（２７３Ｋ）とした場合、オゾン濃度と紫外線吸光強度との関係は次式で表すことができる。
【式１】

Figure 2004163293
【００２８】
本発明では、負圧状態でオゾンガス濃度を測定するようにしていることから、高濃度のオゾンガスであっても、そのオゾン分子の数が少なく、オゾン濃度の僅かな変動に対しても紫外線吸光強度の変化が大きく表れることになるから、測定対象となっているオゾンガス濃度を高精度に測定することができることになる。
【００２９】
本発明方法では、検出センサーであるオゾンガス濃度計測装置（２）、圧力センサー（１５）、温度センサー（１６ａ）（１６ｂ）、マスフローメータ（１８）と、オゾン濃度算出装置（１４）並びに表示部（２０）を離して配置しておくことができ、また、複数の検出センサー部からの情報を１台のオゾン濃度算出装置（１４）並びに表示部（２０）で処理・表示することもできる。
【００３０】
さらに、上記のオゾンガス濃度測定システムでは、オゾンガス濃度計測装置（２）のオゾンガス流通路（５）内を１００Ｐａ以下の超高真空状態にして紫外線吸光強度を計測することによりゼロガス校正を行っているが、オゾンガス濃度計測装置（２）のオゾンガス流通路（５）内に標準ガスを流して、ゼロガス校正を行うようにしても良い。
【００３１】
オゾン濃度の校正を爆発式オゾン濃度校正器（３）を用いる場合、図１のように爆発式オゾン濃度校正器（３）にオゾン濃度計測装置（２）を通過したオゾンガスを直接導入しても良いし、三方弁（４１）、バイパス（４２）、三方弁（４３）を通過させることでオゾンガス濃度計測装置（２）を軽油させることなく導入しても良い。
【００３２】
爆発式オゾン濃度校正器（３）では導入したオゾンガスを三方弁（４３）とバルブ（４８）を封じ切って電源（４７）より高電圧を供給して火花ギャップ（４６）で火花を飛ばしてオゾンガスを爆発させて完全に分解させる。爆発前後の温度と圧力を温度センサー（４４）と圧力センサー（４５）で計測することでオゾン濃度が得られる。こうして得られたオゾン濃度でオゾンガス濃度計測装置（２）の校正を行うと良い。
【００３３】
【発明の効果】
本発明では、測定対象となるオゾンガスを負圧の圧力条件で紫外線吸収式オゾン濃度計測装置の紫外線吸収セル内を流通させていることから、流通ガス中のオゾン分子の絶対数が少なく、僅かな濃度変化があっても、吸光強度に大きな差が現れる。したがって、計測対象ガス中のオゾンガス濃度を高精度に測定することができる。
【００３４】
また、本発明では、オゾンガス濃度計測装置部分で検出した絶対圧力に基づき濃度を演算算出するようにしてあることから、圧力の影響が現れやすい負圧状態下での測定であっても計測対象ガス中のオゾンガス濃度を高精度に検出することができる。
【図面の簡単な説明】
【図１】本発明を適用したオゾンガス濃度測定システムの概略構成図である。
【図２】オゾンガス濃度計測装置の概略構成図である。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method and an apparatus for measuring the concentration of ozone gas, and in particular, a method and a method for measuring the concentration of high-concentration ozone gas obtained by operating an ozonizer at a very low flow rate or a high-concentration ozone gas obtained by concentrating the generated ozone. Equipment related.
[0002]
[Prior art]
Conventionally, an ultraviolet absorption method has been known as a method for measuring the concentration of ozone gas. In this method, ozone has a maximum absorption band near 254 nm in the ultraviolet region, and the absorption intensity of another gas is small in this 254 nm region, and the concentration is determined by using a standard gas (zero gas) containing no ozone. And the gas to be measured (sample gas) are individually flowed into the ultraviolet absorption cell of the ozone gas concentration meter, and the gas concentration of the gas to be measured is measured from the respective absorption intensities.
[0003]
[Patent Document 1]
JP-A-2000-19107 (paragraphs 0002 to 0004, FIG. 4)
[0004]
[Problems to be solved by the invention]
However, the conventional ultraviolet absorption type ozone gas concentration meter is formed for measuring the concentration of ozone gas having an ozone gas concentration of 10 vol% or less, and there is no device capable of measuring the concentration of a high concentration ozone gas having an ozone gas concentration of 15 vol% or more.
[0005]
Further, when the pressure of the ozone gas is high, for example, under the atmospheric pressure, the ultraviolet ray absorbing optical path, that is, when the ozone gas concentration exceeds 10 vol% even if the thickness of the ozone gas is reduced to 50 μm, most of the ultraviolet rays are absorbed by the ozone gas. , High-precision ozone concentration detection was not possible.
[0006]
Conventionally, even if ozone is generated by a high-capacity ozone generator using pure oxygen gas as a raw material, a normal operation method can only generate ozone gas having a concentration of about 10 vol%, and ozone gas having a high concentration of 15 vol% or more. It is thought that this was caused by the fact that was not put into practical use.
[0007]
In recent years, in the field of semiconductor manufacturing and the like, high-concentration ozone of 15 vol% or more has been demanded for use in applications such as oxide film manufacturing. In this case, since the concentration of the ozone gas has a great influence on the formation of the oxide film, an ozone gas concentration measurement technique capable of measuring the concentration of the high-concentration ozone gas with high accuracy and in-line is demanded.
[0008]
The present invention has been made in view of such a point, and provides a method and apparatus for measuring an ozone gas concentration capable of easily and accurately measuring the concentration of ozone gas even at a high concentration. With the goal.
[0009]
[Means for Solving the Problems]
In order to achieve the above object, according to the present invention, the ozone gas flow passage is formed with an ultraviolet transmitting window having ultraviolet transmitting glass on both sides, an ultraviolet light emitting portion on one side, and an ultraviolet light transmitting portion on the other side. In the ozone gas concentration measurement method of measuring ozone concentration by arranging a light receiving unit and measuring the ultraviolet absorption intensity of ozone, a negative pressure ozone gas is caused to flow through the ozone gas flow passage, and the absolute pressure in the ozone gas flow passage is measured by ultraviolet light. It is characterized in that it is measured at the same time as the absorption intensity and the ozone concentration is determined from these measured values.
[0010]
According to the second aspect of the present invention, the pressure of the ozone gas flowing through the ozone gas flow passage is set to 100 Pa to 50 kPa. According to the third aspect of the invention, the flow rate of the ozone gas flowing through the ozone gas flow passage is reduced. The ozone gas concentration is determined by correcting the absolute pressure of the ultraviolet transmitting glass portion based on the measured and measured conductance of the gas passage and the measured flow rate of the ozone gas. The flow rate of the ozone gas flowing in the ozone gas flow passage is measured, and the ozone concentration is corrected based on the relationship between the ozone decomposition rate, the ozone gas flow rate, and the ozone concentration, which are decomposed by the irradiation of ultraviolet light generated when the light passes through the ultraviolet transmitting glass part. According to the fifth aspect of the present invention, the ozone flowing in the ozone gas flow passage is provided. The gas flow rate is set to 100 sccm or less, and the invention described in claim 6 measures at least one of the gas temperature in the ozone gas flow path and the temperature of the ozone gas flow path itself, and sets the ozone concentration to a standard state. The invention described in claim 7 is characterized in that the ozone gas flowing through the ozone gas flow passage is a high-concentration ozone gas having an ozone gas concentration of 15 vol% or more.
[0011]
Further, the invention according to claim 8 is characterized in that the zero point correction of the ozone gas concentration is performed by setting the absolute gas pressure in the ozone gas flow passage to 100 Pa or less. It is characterized in that ozone gas is completely decomposed by an electric spark or the like enclosed in a container, and the ozone concentration obtained from the pressure rise is used as a calibration value.
[0012]
According to a tenth aspect of the present invention, an ozone gas flow passage is formed on both sides thereof with an ultraviolet transmitting window formed of ultraviolet transmitting glass, an ultraviolet light emitting portion is arranged on one side thereof, and an ultraviolet light receiving portion is arranged on the other side. In an ozone gas concentration measuring device that measures ozone concentration by measuring ultraviolet absorption intensity, the outlet side of the ozone gas flow passage is evacuated with a vacuum pump, and a pressure sensor is disposed near the ultraviolet transmission window, so that an absolute The pressure is measured at the same time as the ultraviolet absorption intensity, and the measured values are transmitted to an ozone concentration calculator to determine the ozone concentration.
[0013]
According to an eleventh aspect of the present invention, the distance between the ultraviolet transmitting glasses forming the ultraviolet transmitting window is set to 50 μm or more. 14. The invention according to claim 13, wherein the flow rate is controlled and the ozone gas flow rate value is transmitted to an ozone gas concentration calculation unit to correct the ozone concentration. An ozone sensor is attached to at least one of the above and the ozone gas concentration is measured, and the measured value is transmitted to an ozone gas concentration calculation unit to correct the ozone concentration. The invention according to claim 14, wherein the ozone gas calculation unit In the system, the absolute pressure and temperature of the ozone gas in the UV transmission window are converted from the measurement values of the sensor, The relationship between the temperature and the ultraviolet light absorption intensity, the absolute pressure of the ozone gas, the temperature, the flow rate of the ozone gas, and the ozone decomposition rate by ultraviolet irradiation is defined. The invention according to claim 15, wherein the outlet of the ozone gas flow passage is 17. The invention according to claim 16, wherein the ozone gas whose concentration has been measured is directly connected to a vacuum tank for performing ozone treatment and is used for ozone treatment. The invention according to claim 17 is characterized in that an ultraviolet light transmitting window made of ultraviolet transmitting glass is formed on both surfaces of the ozone gas flow path, an ultraviolet light emitting portion is provided on one side, and an ultraviolet light emitting portion is provided on the other side. In the ozone gas concentration measurement device that measures the ozone concentration by arranging the ultraviolet ray receiving units and measuring the ultraviolet absorption intensity by ozone, the gas pressure in the gas passage is measured. It is characterized in that the pressure is set to 100 Pa or less and a zero gas composition of the ozone gas concentration is performed.
[0014]
Effect of the Invention
In the present invention, an object to be measured is placed in an ozone gas flow path (ultraviolet absorption cell) in which an ultraviolet light emitting portion is arranged on one side of an ultraviolet ray transmitting window having both surfaces made of ultraviolet ray transmitting glass and an ultraviolet ray receiving portion is arranged on the other side. Is circulated under negative pressure conditions. Thereby, the absolute amount of the number of ozone molecules in the flowing gas decreases, and especially when the ozone concentration becomes high, even if there is a slight concentration change, a large difference appears in the absorption intensity. Therefore, the ozone concentration can be measured with high accuracy.
[0015]
Also, even at the same ozone concentration, the number of ozone molecules is proportional to the pressure of the flowing gas. Therefore, in order to accurately obtain the ozone concentration, it is indispensable to accurately measure the absolute pressure of the ultraviolet absorbing cell part. In the present invention, the absolute pressure in the ultraviolet absorption cell portion is calculated by directly measuring the absolute pressure of the ozone gas flow passage and directly using the measured value, or by performing a correction according to the ozone gas flow rate, thereby obtaining the ozone concentration. It is composed.
[0016]
Further, when the flow rate of the flowing gas is small, particularly when the flow rate of the gas is less than 100 sccm, when the ultraviolet ray is irradiated in the ultraviolet ray absorption cell portion, ozone decomposition occurs simultaneously with the absorption of the ultraviolet ray. It will be smaller. Therefore, the relationship between the ozone decomposition rate due to ultraviolet irradiation, the ozone gas flow rate, and the ozone concentration is determined in advance, and the ozone concentration is corrected.
[0017]
Further, by directly measuring the gas temperature in the ozone gas flow passage, the ozone concentration can be converted to a standard state. However, when the flowing gas is negative pressure and the flow rate is small, it is better to measure the temperature itself of the ozone gas flow path itself near the ultraviolet absorption cell, and when the measurement point of the temperature of the ozone gas itself is far from the ultraviolet absorption cell, more accurate measurement is possible. Can measure.
[0018]
Furthermore, the periodic zero point correction is normally performed by switching the gas flow path and using the ultraviolet absorption intensity when air or oxygen containing no ozone is supplied as a reference, but in the present invention, the ozone gas flow path is corrected. By setting the pressure to 100 Pa or less, the zero point correction can be performed by making the residual ozone molecular weight extremely small.
[0019]
On the other hand, the composition of ozone concentration is based on the explosion method, in which negative pressure ozone gas is sealed in a closed container, the ozone gas is completely decomposed using an electric spark, etc., and the ozone concentration is determined from the pressure increase in the closed container. In addition, the ozone gas concentration under negative pressure can be calibrated.
[0020]
BEST MODE FOR CARRYING OUT THE INVENTION
FIG. 1 is a schematic configuration diagram of a concentration measurement system in an ozone gas supply system to which the present invention is applied. An ozone gas concentration measurement device (2) is mounted between an ozone gas supply source (1) and a vacuum pump (4). It is. When calibrating the ozone gas concentration measuring device (2), the explosion type ozone concentration calibrator (3) may be connected to, for example, the ozone gas concentration measuring device (2) and the vacuum pump (4).
[0021]
As shown in FIG. 2, the ozone gas concentration measuring device (2) forms an ultraviolet transmission window (7) in a casing (6) having an ozone gas flow passage (5) formed therein, and the ultraviolet transmission window (7). A pair of ultraviolet transmitting glasses (8) are arranged facing each other with a space of 50 μm or more at a portion thereof, and an ultraviolet absorbing cell is formed by forming an ozone gas flow path (5) between the ultraviolet transmitting glasses (8). It is composed. An ozone gas flow path (5) in which an ultraviolet light emitting portion (9) and an ultraviolet light receiving portion (10) are formed of an ultraviolet transmitting glass (8) is provided in an ultraviolet transmitting window (7) formed of an ultraviolet transmitting glass (8). Are arranged to face each other. The ozone gas concentration measuring device (2) uses an ozone gas consuming device (not shown) instead of the explosion type ozone concentration composing device (3) shown in FIG. The ozone gas whose gas concentration has been measured by the ozone gas concentration measuring device (2) may be connected to the vacuum pump (4) and supplied to the ozone gas consuming device.
[0022]
The ultraviolet light emitting section (9) is formed by an ultraviolet lamp (11), an ultraviolet lamp power supply (12), and a half mirror (13) for dividing the ultraviolet light (30) into transmitted light (31) and reflected light (32). I have. Then, the ozone concentration calculating device (10) calculates the amount of ultraviolet light of the reflected light (32) passing through the ultraviolet transmitting window (7) in the ultraviolet light receiving portion (10a) and the amount of ultraviolet light of the transmitted light (31) in the ultraviolet light receiving portion (10b). 14). Of course, depending on the configuration of the ultraviolet light emitting section (9), the transmitted light (31) may pass through the ultraviolet transmission window (7).
[0023]
A pressure sensor (15) for detecting the pressure in the ozone gas flow path (5) and a temperature of the ozone gas flowing in the ozone gas flow path (5) are provided near the ultraviolet transmission window (7) in the ozone gas concentration measurement device (2). A temperature sensor (16a) for detection is arranged. The pressure signal detected by the pressure sensor (15) and the temperature signal detected by the temperature sensor (16a) are input to the ozone concentration calculating device (14). When the flow rate of the ozone gas is small, the temperature of the ozone gas can be measured more accurately by using the temperature sensor (16b) attached to the casing (6) in the immediate vicinity of the ultraviolet transmission window (7).
[0024]
In addition, a mass flow controller (18) is disposed in a gas outlet path (17) located downstream of a position where the ultraviolet ray transmitting window (7) of the ozone gas concentration measuring device (2) is formed. If the ozone gas flow path (5) and the inner surface of the ozone gas supply path (19) in the ozone gas concentration measurement device (2) are passivated with ozone gas which has been concentrated to a high concentration (for example, 15 vol% or more), An oxidation passivation film is formed on the inner surfaces of the ozone gas flow path (5) and the ozone gas supply path (19), so that the ozone gas can be prevented from being decomposed and consumed by spontaneous decomposition of the ozone gas or reaction with the flow path wall surface.
Reference numeral (20) in the figure denotes a display section of the ozone gas concentration calculated by the ozone concentration calculating device (14).
[0025]
Examples of the ozone gas supply source (1) include an oxygen source such as an air separation device and an oxygen gas cylinder, an ozone production unit including an ozone generator and an ozone gas concentrator, and a gas cylinder such as a gas cylinder storing high-concentration ozone gas. Storage containers are conceivable.
[0026]
In the ozone gas concentration measurement system thus configured, the ozone gas flowing at a predetermined flow rate (100 sccm) through the ozone gas supply path (19) under a negative pressure state (100 Pa to 50 kPa) is introduced into the ozone gas concentration measurement device (4) for measurement. The obtained ultraviolet absorption intensity is input to the ozone concentration calculating device (14), and the ozone concentration calculating device (14) corrects and calculates the ultraviolet absorption intensity based on the temperature, the pressure, and the ozone flow rate, thereby obtaining the ozone gas flow path (5). The ozone gas concentration flowing in the parentheses is measured and displayed on the display unit (20). In this case, the absolute pressure in the ultraviolet absorbing cell portion is corrected based on the conductance of the ozone gas flow path (5) and the gas flow rate flowing in the ozone gas flow path (5). Further, the pressure in the ozone gas flow path (5) is set to a vacuum state of 100 Pa (0.7 Torr) or less, and the ultraviolet absorption intensity is measured. I have.
[0027]
Here, the ultraviolet light absorption intensity of the gas to be measured (ozone gas) is I, the ultraviolet light absorption intensity in a standard gas or a vacuum state of 100 Pa or less is I 0 , the molar extinction coefficient is ε [L / mol · cm], and the measurement optical path length Is d [cm], the ozone concentration is C [mol / L], the pressure of the gas to be measured is P [kPa], the temperature of the gas to be measured is T [K], the reference pressure is PN (101.3 kPa), and the reference. When the temperature is T N (273 K), the relationship between the ozone concentration and the ultraviolet absorption intensity can be expressed by the following equation.
(Equation 1)
Figure 2004163293
[0028]
In the present invention, since the ozone gas concentration is measured in a negative pressure state, even if the ozone gas has a high concentration, the number of the ozone molecules is small, and even if the ozone concentration is slightly changed, the ultraviolet absorption intensity is small. Changes, the ozone gas concentration to be measured can be measured with high accuracy.
[0029]
In the method of the present invention, the ozone gas concentration measurement device (2), the pressure sensor (15), the temperature sensors (16a) (16b), the mass flow meter (18), the ozone concentration calculation device (14), and the display unit ( 20) can be arranged separately, and information from a plurality of detection sensor units can be processed and displayed on one ozone concentration calculation device (14) and display unit (20).
[0030]
Furthermore, in the above-mentioned ozone gas concentration measurement system, zero gas calibration is performed by measuring the ultraviolet absorption intensity in an ultra-high vacuum state of 100 Pa or less in the ozone gas flow passage (5) of the ozone gas concentration measurement device (2). Alternatively, zero gas calibration may be performed by flowing a standard gas into the ozone gas flow path (5) of the ozone gas concentration measurement device (2).
[0031]
When the explosion-type ozone concentration calibrator (3) is used for the calibration of the ozone concentration, the ozone gas which has passed through the ozone concentration measurement device (2) is directly introduced into the explosion-type ozone concentration calibrator (3) as shown in FIG. Alternatively, the ozone gas concentration measurement device (2) may be introduced without passing light oil by passing through the three-way valve (41), the bypass (42), and the three-way valve (43).
[0032]
In the explosion-type ozone concentration calibrator (3), the introduced ozone gas is closed by closing the three-way valve (43) and the valve (48) and a high voltage is supplied from the power supply (47), and the spark is blown by the spark gap (46). To explode completely. By measuring the temperature and pressure before and after the explosion with the temperature sensor (44) and the pressure sensor (45), the ozone concentration can be obtained. It is preferable to calibrate the ozone gas concentration measuring device (2) with the ozone concentration thus obtained.
[0033]
【The invention's effect】
In the present invention, since the ozone gas to be measured is circulated in the ultraviolet absorption cell of the ultraviolet absorption type ozone concentration measuring device under a negative pressure condition, the absolute number of ozone molecules in the circulating gas is small and slight. Even if the concentration changes, a large difference appears in the absorption intensity. Therefore, the ozone gas concentration in the measurement target gas can be measured with high accuracy.
[0034]
Further, in the present invention, since the concentration is calculated and calculated based on the absolute pressure detected by the ozone gas concentration measuring device, even if the measurement is performed under a negative pressure state where the influence of the pressure is likely to appear, the gas to be measured can be measured. The concentration of ozone gas in the medium can be detected with high accuracy.
[Brief description of the drawings]
FIG. 1 is a schematic configuration diagram of an ozone gas concentration measurement system to which the present invention is applied.
FIG. 2 is a schematic configuration diagram of an ozone gas concentration measurement device.

Claims (17)

オゾンガス流通路の両面に紫外線透過ガラスで構成した紫外線透過窓を配置し、その一側に紫外線発光部を、他側に紫外線受光部をそれぞれ配置し、オゾンによる紫外線吸光強度を計測することでオゾン濃度を計測するオゾンガス濃度計測方法において、
オゾンガス流通路に負圧のオゾンガスを流通させ、このオゾンガス流通路での絶対圧を紫外線吸光強度と同時に計測し、これらの計測値からオゾン濃度を求めるようにしたことを特徴とするオゾンガス濃度計測方法。An ultraviolet transmitting window made of ultraviolet transmitting glass is arranged on both sides of the ozone gas flow passage, an ultraviolet light emitting part is arranged on one side, and an ultraviolet light receiving part is arranged on the other side, and the ultraviolet absorption intensity by ozone is measured. In the ozone gas concentration measurement method to measure the concentration,
A method for measuring ozone gas concentration, characterized in that ozone gas at a negative pressure is passed through an ozone gas flow passage, the absolute pressure in the ozone gas flow passage is measured simultaneously with the ultraviolet absorption intensity, and the ozone concentration is determined from these measured values. . オゾンガス流通路内を流通させるオゾンガスの圧力が１００Ｐａ〜５０ｋＰａである請求項１に記載のオゾンガス濃度計測方法。The ozone gas concentration measurement method according to claim 1, wherein the pressure of the ozone gas flowing through the ozone gas flow passage is 100 Pa to 50 kPa. オゾンガス流通路内を流れるオゾンガス流量を計測し、その値と、絶対圧の計測点と紫外線透過窓の間のコンダクタンスから、絶対圧の計測値を紫外線透過ガラス部の絶対圧力に換算して、オゾンガス濃度を求めるようにした請求項１または２に記載のオゾンガス濃度計測方法。The ozone gas flow rate in the ozone gas flow passage is measured, and the measured value of the absolute pressure is converted into the absolute pressure of the ultraviolet ray transmitting glass part from the measured value and the conductance between the absolute pressure measurement point and the ultraviolet ray transmitting window. 3. The method for measuring ozone gas concentration according to claim 1, wherein the concentration is determined. オゾンガス流通路内を流れるオゾンガス流量を計測し、予め求めておいた紫外線透過ガラス部を通過する際に生じる紫外線照射により分解するオゾン分解率とオゾンガス流量並びにオゾン濃度の関係から請求項１から３のいずれかの方法で求めたオゾン濃度の補正を行うことを特徴とするオゾンガス濃度計測方法。The flow rate of ozone gas flowing through the ozone gas flow passage is measured, and the ozone decomposition rate, which is decomposed by ultraviolet irradiation generated when passing through the ultraviolet transmitting glass part, and the ozone gas flow rate and the ozone concentration are determined in advance. An ozone gas concentration measurement method, wherein the ozone concentration obtained by any one of the methods is corrected. オゾンガス流通路内を流れるオゾンガス流量を１００ｓｃｃｍ以下とした請求項１から４のいずれか１項に記載のオゾンガス濃度計測方法。The method for measuring the concentration of ozone gas according to any one of claims 1 to 4, wherein the flow rate of the ozone gas flowing in the ozone gas flow passage is set to 100 sccm or less. オゾンガス流通路内のガス温度とオゾンガス流路自体の温度との少なくとも一方を計測し、請求項１から５のいずれかの方法で求めたオゾン濃度を標準状態に換算することを特徴とするオゾンガス濃度計測方法。6. An ozone gas concentration characterized by measuring at least one of a gas temperature in an ozone gas flow passage and a temperature of an ozone gas flow passage itself, and converting an ozone concentration obtained by the method according to claim 1 into a standard state. Measurement method. オゾンガス流通路内を流通するオゾンガスが、オゾンガス濃度１５ｖｏｌ ％以上の高濃度オゾンガスである請求項１から６のいずれか１項に記載のオゾンガス濃度計測方法。The ozone gas concentration measuring method according to any one of claims 1 to 6, wherein the ozone gas flowing in the ozone gas flow passage is a high concentration ozone gas having an ozone gas concentration of 15 vol% or more. オゾンガス流通路内の絶対ガス圧を１００Ｐａ以下とすることでオゾンガス濃度の零点補正を行うことを特徴とする請求項１から７のいずれか１項に記載のオゾンガス濃度計測方法。The ozone gas concentration measuring method according to any one of claims 1 to 7, wherein zero point correction of the ozone gas concentration is performed by setting the absolute gas pressure in the ozone gas flow passage to 100 Pa or less. オゾンガスを密閉容器に封入し電気火花などでオゾンガスを完全に分解し、その圧力上昇から求めたオゾン濃度を校正値とすることを特徴とする請求項１から８のいずれか１項に記載のオゾンガス濃度計測方法。The ozone gas according to any one of claims 1 to 8, wherein the ozone gas is sealed in a closed container, the ozone gas is completely decomposed by an electric spark or the like, and the ozone concentration obtained from the pressure rise is used as a calibration value. Concentration measurement method. オゾンガス流通路に両面を紫外線透過ガラスで構成した紫外線透過窓を形成しその一側に紫外線発光部を、他側に紫外線受光部をそれぞれ配置し、オゾンによる紫外線吸光強度を計測することでオゾン濃度を計測するオゾンガス濃度計測装置において、
オゾンガス流通路の出口側を真空ポンプで排気するとともに紫外線透過窓近傍に圧力センサーを配して、オゾンガス流通路内の絶対圧を紫外線吸光強度と同時に計測し、これらの計測値をオゾン濃度算出部に伝達してオゾン濃度を求めることを特徴とするオゾンガス濃度計測装置。In the ozone gas flow path, an ultraviolet transmitting window composed of ultraviolet transmitting glass on both sides is formed, an ultraviolet light emitting part is arranged on one side and an ultraviolet light receiving part is arranged on the other side, and the ozone concentration is measured by measuring the ultraviolet absorption intensity by ozone. In an ozone gas concentration measurement device that measures
The outlet side of the ozone gas flow passage is evacuated by a vacuum pump, and a pressure sensor is disposed near the ultraviolet transmission window to measure the absolute pressure in the ozone gas flow passage at the same time as the ultraviolet light absorption intensity. An ozone gas concentration measuring device characterized in that the ozone gas concentration is obtained by transmitting the ozone gas concentration to an ozone gas. 紫外線透過窓を構成している紫外線透過ガラスの間隔を５０μｍ以上に構成した請求項１０に記載のオゾンガス濃度計測装置。The ozone gas concentration measuring device according to claim 10, wherein the interval between the ultraviolet transmitting glasses forming the ultraviolet transmitting window is set to 50 µm or more. オゾンガス流通路を流れるオゾンガス流量を制御するとともにオゾンガス流量値をオゾンガス濃度算出部に伝達してオゾン濃度を補正することを特徴とする請求項１０又は１１に記載のオゾンガス濃度計測装置。12. The ozone gas concentration measuring device according to claim 10, wherein the ozone gas flow rate flowing through the ozone gas flow passage is controlled and the ozone gas flow rate value is transmitted to an ozone gas concentration calculation unit to correct the ozone concentration. オゾンガス流通路を構成している配管とオゾンガス流通路内との少なくとも一方にオゾンセンサーを取り付けてオゾンガスの濃度を計測し、その計測値をオゾンガス濃度算出部に伝達してオゾン濃度を補正することを特徴とする請求項１０から１２のいずれか１項に記載のオゾンガス濃度計測装置。An ozone sensor is attached to at least one of the piping constituting the ozone gas flow path and the inside of the ozone gas flow path to measure the concentration of ozone gas, and the measured value is transmitted to the ozone gas concentration calculation unit to correct the ozone concentration. The ozone gas concentration measuring device according to any one of claims 10 to 12, wherein: オゾンガス算出部では紫外線透過窓におけるオゾンガスの絶対圧、温度がセンサーの計測値から換算されると共に、オゾンガス濃度と紫外線吸光強度、オゾンガスの絶対圧、温度、オゾンガス流量、紫外線照射によるオゾン分解率との関係が定義されていることを特徴とする請求項１０から１３のいずれか１項に記載のオゾンガス濃度計測装置。The ozone gas calculation unit converts the absolute pressure and temperature of the ozone gas in the ultraviolet transmission window from the measurement values of the sensor, and calculates the ozone gas concentration and the ultraviolet absorption intensity, the absolute pressure of the ozone gas, the temperature, the ozone gas flow rate, and the ozone decomposition rate by ultraviolet irradiation. 14. The ozone gas concentration measuring device according to claim 10, wherein a relationship is defined. オゾンガス流通路の出口がオゾン処理をする真空槽に直接接続されており、濃度計測済みのオゾンガスをオゾン処理に使用するようにしたことを特徴とする請求項１０から１４のいずれか１項に記載のオゾンガス濃度計測装置。The outlet of the ozone gas flow passage is directly connected to a vacuum tank for performing ozone treatment, and the ozone gas whose concentration has been measured is used for the ozone treatment. Ozone gas concentration measurement device. オゾンガス流通路の内面を高濃度オゾンで不動態化処理してある請求項１０から１５のいずれか１項に記載のオゾンガス濃度計測装置。The ozone gas concentration measuring device according to any one of claims 10 to 15, wherein the inner surface of the ozone gas flow passage is passivated with high-concentration ozone. オゾンガス流通路の両面を紫外線透過ガラスで構成した紫外線透過窓を形成しその一側に紫外線発光部を、他側に紫外線受光部をそれぞれ配置し、オゾンによる紫外線吸光強度を計測することでオゾン濃度を計測するオゾンガス濃度計測装置において、
ガス通路内でのガス圧を１００Ｐａ以下に設定し、オゾンガス濃度のゼロガス校正を行うことを特徴とするオゾンガス濃度計測装置。An ultraviolet transmitting window composed of ultraviolet transmitting glass is formed on both sides of the ozone gas flow passage, an ultraviolet light emitting part is arranged on one side and an ultraviolet light receiving part is arranged on the other side, and the ozone concentration is measured by measuring the ultraviolet absorption intensity by ozone. In an ozone gas concentration measurement device that measures
An ozone gas concentration measuring device, wherein a gas pressure in a gas passage is set to 100 Pa or less and zero gas calibration of an ozone gas concentration is performed.
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