JP2004061316A - Apparatus and method for analyzing surface reaction process of diffusing material - Google Patents

Apparatus and method for analyzing surface reaction process of diffusing material Download PDF

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JP2004061316A
JP2004061316A JP2002220383A JP2002220383A JP2004061316A JP 2004061316 A JP2004061316 A JP 2004061316A JP 2002220383 A JP2002220383 A JP 2002220383A JP 2002220383 A JP2002220383 A JP 2002220383A JP 2004061316 A JP2004061316 A JP 2004061316A
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diffusion material
chamber
storage chamber
analyzing
hydrogen
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JP3659943B2 (en
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Takehiko Ito
伊藤　岳彦
Mitsuru Sakano
坂野　充
Tomotsugu Sakai
坂井　智嗣
Taro Ichihara
市原　太郎
Yasuhiro Iwamura
岩村　康弘
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Mitsubishi Heavy Industries Ltd
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Mitsubishi Heavy Industries Ltd
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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
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    • Y02E30/10—Nuclear fusion reactors

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Abstract

<P>PROBLEM TO BE SOLVED: To provide an apparatus and a method for analyzing the surface reaction processes of a diffusing material and capable of lowering costs. <P>SOLUTION: The apparatus for analyzing the surface reaction processes of the diffusing material is provided with an occlusion chamber 2 and a discharge chamber 3 for airtightly sandwiching and arranging a sample (the diffusing material) 1 capable of diffusing gaseous hydrogen and an analyzing means for analyzing the surface of the sample 1. The apparatus is provided with both a hydrogen supply system 8 for supplying hydrogen in the inside of the occlusion chamber 2 and an evacuating system (a circulating device) 9 for returning gases, which have transmitted through the sample 1 and flowed into the discharge chamber 3 from the occlusion chamber 2, to the occlusion chamber 2. The evacuating system 9 is provided with both a channel 9a for communicate with the discharge chamber 3 and the occlusion chamber 2 and a circulating pump 9c provided at a midpoint in the channel 9a for feeding gases from the side of the discharge chamber 2 to the side of the occlusion chamber 3. <P>COPYRIGHT: (C)2004,JPO

Description

【０００１】
【発明の属する技術分野】
本発明は、水素あるいは重水素が拡散材料中に拡散しながら透過したとき、その拡散試料の反応状態を観察して解析する拡散材料の表面反応過程分析装置および方法に関する。
【０００２】
【従来の技術】
水素あるいは重水素を用いて試料に反応させる従来技術として、特開平８−１６６４７６号公報，同８−１６６４７７号公報に示される技術がある。上記特開平８−１６６４７６号公報（以下、第一の従来技術という）には、パラジウムなどの金属やその合金等の固体に、軽水素と重水素との何れか一方を含ませて作成した試料を、真空容器内でヒーターにより加熱して、試料中で前記何れか一方のガスを移動させ、人為的に核融合反応を引き起こす技術が開示されている。
【０００３】
また、上記特開平８−１６６４７７号公報（以下、第二の従来技術という）には、電解溶液側の電気分解セルと、真空容器と、パラジウム等からなる試料としての陰極電極との間が気密的に閉じられるように装置を構成し、陰極電極と陽極電極とにより電解溶液の電気分解を行うことにより、その際の核反応によって生成された、電解溶液内を通過できない荷電粒子やＸ線を検出できるようにした技術が開示されている。
しかしながら、第一の従来技術では、真空容器を用いその中で核融合反応を誘発するものの、水素或いは重水素を長時間連続的に拡散させることが出来ない。また、この従来技術は、核融合反応の結果発生する放射線を計測するものであり、各反応生成物質（元素変換）を計測するものではない。他方、第二の従来技術では、電解吸蔵を用いているため、核反応生成物が大量に生成される場合を除いて、不純物混入のおそれがあり、計測の正確性に欠けるという問題がある。
【０００４】
【発明が解決しようとする課題】
そこで、特開２００１−１６５８５１にはこのような問題点を解決する拡散材料の表面反応過程分析方法及びその装置が提案されている。
この技術においては吸蔵室と放出室との間の圧力差を利用して試料への重水素の注入を行っているが、試料を透過した重水素を放出室から取り除いている一方、吸蔵室には重水素を供給しつづける必要がある。したがって比較的高価な重水素のコストがかさむという問題があった。また、水素としてトリチウムを用いた場合、安全な排気処理を行う必要があるため、安全性を確保するためにコストがかさむという問題があった。
【０００５】
本発明は上記事情に鑑みてなされたものであり、コストを下げることができる拡散材料の表面反応過程分析装置および方法を提供することを目的とする。
【０００６】
【課題を解決するための手段】
請求項１に記載の発明は、水素ガスを拡散し得る拡散材料を互いに気密状態で挟んで配置する吸蔵室及び放出室と、拡散材料の表面を分析する分析手段とを備えた拡散材料の表面反応過程分析装置において、吸蔵室内に水素を供給する水素供給系と、前記拡散材料を透過して前記吸蔵室から放出室に流入したガスを前記吸蔵室に戻す循環装置とを備え、該循環装置は放出室と吸蔵室とを連通する流路と、該流路途中に設けられ前記放出室側から吸蔵室側へガスを送る循環ポンプとを備えていることを特徴とする。
【０００７】
この発明においては、拡散材料を透過して吸蔵室から放出室に流れ込んだ水素ガスを、再び吸蔵室に戻す。これによって水素ガスを再利用することができる。また、水素としてトリチウムを用いた場合は、トリチウムを外に排出せず循環させて再利用することで、高い安全性を得ることができる。
【０００８】
請求項２に記載の発明は、請求項１に記載の拡散材料の表面反応過程分析装置において、不純物を除去するフィルタが前記流路途中に設けられていることを特徴とする。
【０００９】
この発明においては、循環ポンプや配管系から発生する不純物をフィルタにより除去した後に水素ガスを吸蔵室に戻す。
【００１０】
請求項３に記載の発明は、請求項１または２に記載の拡散材料の表面反応過程分析装置において、昇圧用の圧縮機が前記流路途中に設けられていることを特徴とする。
【００１１】
この発明においては、吸蔵室の圧力に合わせて昇圧した後のガスを吸蔵室に戻す。
【００１２】
請求項４に記載の発明は、請求項１から３いずれかに記載の拡散材料の表面反応過程分析装置において、前記水素としてトリチウムが用いられ、前記吸蔵室内のトリチウム量を検出するトリチウム検出手段が設けられていることを特徴とする。
【００１３】
この発明においては、水素としてトリチウムを含むガスを用いる場合に、系内におけるトリチウムの増減を監視しておく。これにより、核種変換、漏れ等があった場合に検出することができる。
【００１４】
請求項５に記載の発明は、請求項４に記載の拡散材料の表面反応過程分析装置において、前記トリチウム検出手段は、前記吸蔵室から出て該吸蔵室に戻る流路と、該流路途中に設けられた循環ポンプと、トリチウムモニターとを備えていることを特徴とする。
【００１５】
この発明においては、吸蔵室内のガスは循環ポンプにより流路内に取り込まれ、トリチウムモニターでガスに含まれているトリチウム量を検出する。
【００１６】
請求項６に記載の発明は、吸蔵室と放出室との境界位置に、水素を拡散し得る拡散材料を互いに気密状態で挟んで配置し、前記ガスを吸蔵室から拡散材料中を経て放出室に放出させ、該拡散材料の表面を分析する拡散材料の表面反応過程分析方法であって、真空状態の吸蔵室内に露出した前記拡散材料に水素を注入する工程と、該拡散材料を透過した前記水素を再び前記吸蔵室に戻す工程とを有することを特徴とする。
【００１７】
この発明においては、拡散材料を透過して吸蔵室から放出室に流れ込んだ水素ガスを、再び吸蔵室に戻す。これによって水素ガスを再利用することができる。
【００１８】
請求項７に記載の発明は、請求項６に記載の拡散材料の表面反応過程分析方法において、前記水素としてトリチウムが用いられ、前記吸蔵室内のトリチウム量を検出するトリチウム検出工程を有することを特徴とする。
【００１９】
この発明においては、水素としてトリチウムを含むガスを用いる場合に、系内におけるトリチウムの増減を監視しておく。これにより、核種変換、漏れ等があった場合に検出することができる。
【００２０】
【発明の実施の形態】
次に、本発明の実施形態について、図面を参照して説明する。
図１において、符号１は水素拡散材料である試料、２は吸蔵室、３は放出室であり、吸蔵室２と放出室３との境界位置には試料１が配置され、両室２，３間は不純物等が混入しないよう気密保持されている。
【００２１】
なお、試料１としては、水素を拡散しながら透過させる材料であるなら何でもよく、例えばパラジウム，チタン，バナジウム等がある。また、吸蔵室２及び放出室３等の構成材料は、水素や拡散材料と触れても何等悪影響を受けることのない材質で構成されている。
なお、本実施形態においては重水素を用いて説明しているが、これに限らず軽水素で代用することも可能である。
【００２２】
本装置においては、真空排気系７と、水素供給系８と、圧力計１９とが備えられ、また放出室３には真空排気系（循環装置）９と、真空真空排気系ゲージ２０とが備えられている。
真空排気系７は、重水素ガスの供給に際し、予め吸蔵室２を高真空状態に保つためのものであり、ロータリポンプ７ａ，真空バルブ７ｂ、ロータリポンプ７ａと真空バルブ７ｂとの間に設けられたターボ分子ポンプ７ｃ、真空バルブ７ｂと吸蔵室２間に設けられた吸蔵室用の真空ゲージ７ｄを備える。
また、水素供給系８は、真空状態にある吸蔵室２に重水素ガスを充填するものであり、重水素ガスボンベ８ａ、バリアブルリークバルブ８ｂからなっている。
真空排気系９は、放出室３を常に真空状態に保つものであり、放出室３から出て吸蔵室２に戻る流路９ａを備えている。さらに、該流路９ａに対して、放出室３を真空引きするターボ分子ポンプ９ｂと、放出室３側から吸蔵室２側にガスを送る循環ポンプ９ｃと、循環ポンプ９ｃから送られてきたガスを圧縮する圧縮機９ｄと、圧縮機９ｄにより昇圧されたガスを、吸蔵室３に送る流路と、別途の排出系に送る流路とに切り替える外部排気弁９ｅと、不純物を除去するフィルタ９ｆとを、放出室３から吸蔵室２に向かってこの順で備えている。フィルタ９ｆは液体窒素等により流路９ａを冷却することにより、循環ポンプ９ｃや配管系から発生する不純物を除去するものである。なお、吸蔵室２の圧力が高くない場合には圧縮機９ｄを設けなくても良い場合がある。同様に、循環ポンプ９ｃや配管系から発生する不純物が極めて少ない場合にはフィルタ９ｆを設けなくても良い場合がある。
【００２３】
図に示すように、試料１が吸蔵室２と放出室３間の境界位置に互いに気密状態のままで配置される。その際、図２に示すように試料１の成膜面側が吸蔵室２を向くようにセットされる。図において、符号４は真空フランジ、６はＯリングである。
【００２４】
そして、吸蔵室２には、分析手段として静電アナライザー２１及びＸ線銃２２からなるＸＰＳ計測装置と、放射線計測器としてのＸ線検出器１４とが備えられている。
【００２５】
Ｘ線検出器１４は、大気中に設置しているため、真空と大気を仕切り、しかもＸ線を透過させることができるよう、Ｘ線源と吸蔵室２との間にベリリウム窓１４ａが設けられている。
【００２６】
本実施の形態においては、まず試料１が吸蔵室２と放出室３間にセットされる。試料１のセット後、吸蔵室２側の真空排気系７及び放出室３側の真空排気系９をそれぞれ駆動し、両室を所定圧の高真空状態とする。真空排気系９は、ターボ分子ポンプ９ｂにより排気を行い、外部排気弁９ｅを経て外部に排気される。
次いで、所定の高真空状態となったところで、ＸＰＳ計測装置により吸蔵室２内の試料表面の状態を計測し、試料表面に存在する物質を計測する。かかる計測後、吸蔵室２内の真空排気系７の真空バルブ７ｂを閉じる一方、水素供給系８により吸蔵室２内に重水素ガスを導入する。所定量導入後は水素の供給を停止し、真空排気系９により放出室３に透過した水素を吸蔵室２に戻す運転を行う。このとき、外部排気弁９ｅは吸蔵室２側へ切り替え、循環ポンプ９ｃにより送られる水素ガスが吸蔵室２側へ導入されるようにする。
【００２７】
なお、ＸＰＳ計測装置は高真空でのみ計測可能な装置であるので、この時間内では動作させないでおき、Ｘ線検出器１４を動作させ、該Ｘ線検出器１４により試料１から放出されるＸ線量を検出可能としている。
【００２８】
放出室３はターボ分子ポンプ９ｂにより排気されている状態とする。したがって試料１を透過したガスはターボ分子ポンプ９ｂにより吸引され、循環ポンプ９ｃにより吸蔵室２側に送られる。このとき、ガスはまず圧縮機９ｄにより吸蔵室２の圧力に合わせて昇圧され、次いでフィルタ９ｆにより不純物が除去された後、吸蔵室２に導入される。
しかる後、所定時間が経過した後は、真空排気系７の真空バルブ７ｂを開くことにより、吸蔵室２を再び真空排気する。また、外部排気弁９ｅを排気側に切り替える。
そして、吸蔵室２内が高真空となった後、再度ＸＰＳ計測装置を駆動し、試料１表面側の元素分析を行う。
【００２９】
このように、真空排気系９により放出室３のガスが吸蔵室２に戻され、重水素が吸蔵室２と放出室３との間を循環する。したがって、重水素を繰り返し使用することができ、コストを抑えることができるという効果を得ることができる。また、水素としてトリチウムを用いた場合、排気の処理に高い安全性が要求されコストがかかるトリチウムを循環して利用することができるから、これによってもコストを抑えることができる。
また、圧縮機９ｄによって圧縮することで、吸蔵室２に戻す水素ガスを吸蔵室２の圧力に合わせることができ、フィルタ９ｆを通すことにより、不純物を除去することができる。
また、重水素を透過する前の試料表面の状態と、重水素透過した後の試料表面の状態とを計測するので、試料１の反応前後の状態を分析することができ、また試料１の表面に物質が生成されたことを確実に解明することができる。しかも、長時間に渡り、吸蔵室２，試料１，放出室３間が気密に保持され、またその間で試料１を取り出さないので、実験中に外部から不純物が混入するというおそれがなく、そのため、試料１の表面で生成された物質を正確かつ的確に分析することができる。
【００３０】
次に、本発明の第２実施形態について説明する。なお、上記第１実施形態と同一の構成については同一の符号を用い、その説明を省略する。
図３は本実施形態の構成を示した図である。本実施形態においては、重水素ガスボンベ８ａ内には水素としてトリチウムが含まれている。
そして、トリチウム検出手段２０が設けられている。トリチウム検出手段２０は、前記吸蔵室２から出て該吸蔵室２に戻る循環流路２０ａを備え、該循環流路２０ａには、上流側から下流に向かって、トリチウムモニター２０ｂと、循環ポンプ２０ｃと、フィルタ２０ｄとがこの順で設けられている。
トリチウムモニター２０ｂはトリチウムの量を検出する装置であり、フィルタ２０ｄは液体窒素等により循環流路２０ａを冷却することで循環ポンプ２０ｃや配管系から発生する不純物を取り除く装置である。なお、循環ポンプ２０ｃや配管系から発生する不純物が極めて少ない場合にはフィルタ２０ｄを設けなくても良い場合がある。
【００３１】
次に、本実施形態の動作について説明する。
本実施形態においては、上記第１実施形態と同様に、吸蔵室２に水素供給系８から水素が供給され、試料１の内部を水素が拡散しつつ透過する。このとき、上記と同様に真空排気系９により、放出室３のガスが吸蔵室２に戻され、重水素が吸蔵室２と放出室３との間を循環する。したがって、重水素を繰り返し使用することができ、コストを抑えることができる。
また、水素供給系８からの水素供給を停止した後において、循環ポンプ２０ｃを駆動して吸蔵室２内のガスについてトリチウムモニター２０ｂにより測定する。トリチウムモニター２０ｂは、ガスに含まれるトリチウムの量を検出する。したがって、系内（吸蔵室２および放出室３）におけるトリチウムの量の変動を検出することができ、核種変換、漏れがあった場合に検出することができる。
このように、トリチウムを外部に排気せず循環して再利用することで、高い安全性と低いコストを実現することができる。
【００３２】
なお、これまでの図示実施の形態では、吸蔵室２内に各種分析装置を設けた構成を示したが、放出室３側に設けても良いのはもちろんである。また、これら核分析手段は解析目的に応じて使用すれば、種々の解析目的を実現することができるものである。従って、上記実施形態に挙げた例に限らず、少なくとも解析すべき内容に応じたものを設置し、使用することができる。
さらに、分析手段は必ずしも吸蔵室２または放出室３と一体である必要はなく、吸蔵室２および放出室３とは別個に設けてもよい。すなわち、試料１に水素を透過させた後、試料１を吸蔵室２及び放出室３から取出し、外部に設けられた分析手段に試料１を移して分析を行っても良い。
【００３３】
【発明の効果】
以上説明したように、本発明によれば拡散材料を透過して吸蔵室から放出室に流れ込んだガスを再び吸蔵室に戻す。これによって水素ガスを再利用することができ、コストを下げることができる。また、また、水素としてトリチウムを用いた場合は、トリチウムを外に排出せず循環させて再利用することで、高い安全性を得ることができる。
また、フィルタを設けることで、循環ポンプや配管系から出る不純物を取り除くことができる。
また、圧縮機が設けられているから、吸蔵室の圧力に合わせて圧縮した水素を吸蔵室に導入することができる。
さらにまた、水素としてトリチウムを用いた場合には、トリチウム検出手段を用いることで、核種変換、漏れ等を検出することができる。
【図面の簡単な説明】
【図１】本発明の第１実施形態による表面反応過程分析装置を示す構成図である。
【図２】図１における吸蔵室と試料と放出室間の機密保持構造を示す断面図である。
【図３】本発明の第２実施形態による表面反応過程分析装置を示す構成図である。
【符号の説明】
１　試料（拡散材料）
２　吸蔵室
３　放出室
９　真空排気系（循環装置）
９ａ　流路
９ｃ　循環ポンプ
９ｄ　圧縮機
９ｆ　フィルタ
２０　トリチウム検出手段
２０ａ　流路
２０ｂ　トリチウムモニター
２０ｃ　循環ポンプ
２０ｄ　フィルタ[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to an apparatus and a method for analyzing a surface reaction process of a diffusion material, in which when hydrogen or deuterium is transmitted while diffusing into a diffusion material, the reaction state of the diffusion sample is observed and analyzed.
[0002]
[Prior art]
As a conventional technique for reacting a sample with hydrogen or deuterium, there are techniques disclosed in JP-A-8-166476 and JP-A-8-166577. Japanese Patent Application Laid-Open No. 8-166476 (hereinafter referred to as first prior art) discloses a sample prepared by adding one of light hydrogen and deuterium to a solid such as a metal such as palladium or an alloy thereof. Is heated by a heater in a vacuum vessel to move any one of the gases in a sample, thereby causing a nuclear fusion reaction artificially.
[0003]
Japanese Patent Application Laid-Open No. Hei 8-166577 (hereinafter referred to as second prior art) discloses that the space between an electrolytic cell on the electrolytic solution side, a vacuum vessel, and a cathode electrode as a sample made of palladium or the like is airtight. The device is configured to be closed in a closed manner, and electrolysis of the electrolytic solution is performed by the cathode electrode and the anode electrode, so that charged particles and X-rays generated by the nuclear reaction at that time and which cannot pass through the electrolytic solution are removed. There is disclosed a technique capable of detecting the same.
However, in the first prior art, although a fusion reaction is induced in a vacuum vessel, hydrogen or deuterium cannot be continuously diffused for a long time. Further, this conventional technique measures radiation generated as a result of a nuclear fusion reaction, and does not measure each reaction product (element conversion). On the other hand, in the second prior art, since electrolytic occlusion is used, there is a possibility that impurities may be mixed in, except for a case where a large amount of nuclear reaction products are generated, and there is a problem that measurement accuracy is lacking.
[0004]
[Problems to be solved by the invention]
Therefore, Japanese Patent Application Laid-Open No. 2001-165851 proposes a method and an apparatus for analyzing a surface reaction process of a diffusion material which solves such a problem.
In this technique, deuterium is injected into the sample using the pressure difference between the storage chamber and the release chamber.However, while deuterium permeating the sample is removed from the release chamber, Need to keep supplying deuterium. Therefore, there has been a problem that the cost of relatively expensive deuterium increases. Further, when tritium is used as hydrogen, it is necessary to perform safe exhaust treatment, so that there is a problem that costs are increased in order to ensure safety.
[0005]
The present invention has been made in view of the above circumstances, and an object of the present invention is to provide an apparatus and method for analyzing a surface reaction process of a diffusion material, which can reduce the cost.
[0006]
[Means for Solving the Problems]
According to a first aspect of the present invention, there is provided a surface of a diffusion material, comprising: a storage chamber and a discharge chamber in which a diffusion material capable of diffusing hydrogen gas is disposed in an airtight manner with each other, and analysis means for analyzing a surface of the diffusion material. The reaction process analyzer, comprising: a hydrogen supply system for supplying hydrogen into the storage chamber; and a circulator for returning the gas permeating the diffusion material and flowing from the storage chamber to the discharge chamber to the storage chamber. Is characterized by comprising a flow path communicating between the discharge chamber and the occlusion chamber, and a circulation pump provided in the middle of the flow path and for sending gas from the discharge chamber side to the occlusion chamber side.
[0007]
In the present invention, the hydrogen gas that has passed through the diffusion material and flowed from the storage chamber to the release chamber is returned to the storage chamber again. Thereby, the hydrogen gas can be reused. When tritium is used as hydrogen, high safety can be obtained by circulating and recycling tritium without discharging it.
[0008]
According to a second aspect of the present invention, in the surface reaction process analyzer for a diffusion material according to the first aspect, a filter for removing impurities is provided in the middle of the flow path.
[0009]
In this invention, the hydrogen gas is returned to the storage chamber after the impurities generated from the circulation pump and the piping system are removed by the filter.
[0010]
According to a third aspect of the present invention, in the apparatus for analyzing a surface reaction process of a diffusion material according to the first or second aspect, a compressor for increasing pressure is provided in the middle of the flow path.
[0011]
In the present invention, the gas that has been pressurized in accordance with the pressure of the storage chamber is returned to the storage chamber.
[0012]
According to a fourth aspect of the present invention, in the apparatus for analyzing a surface reaction process of a diffusion material according to any one of the first to third aspects, tritium is used as the hydrogen, and tritium detecting means for detecting an amount of tritium in the storage chamber is provided. It is characterized by being provided.
[0013]
In the present invention, when a gas containing tritium is used as hydrogen, the increase or decrease of tritium in the system is monitored. This makes it possible to detect when there is nuclide conversion, leakage, or the like.
[0014]
According to a fifth aspect of the present invention, in the surface reaction process analyzer for a diffusion material according to the fourth aspect, the tritium detecting means includes a flow path that exits the storage chamber and returns to the storage chamber, and And a tritium monitor.
[0015]
In this invention, the gas in the storage chamber is taken into the flow channel by the circulation pump, and the tritium monitor detects the amount of tritium contained in the gas.
[0016]
According to a sixth aspect of the present invention, a diffusion material capable of diffusing hydrogen is disposed in a boundary position between the occlusion chamber and the release chamber in an airtight state with respect to each other, and the gas is discharged from the occlusion chamber through the diffusion material. A method for analyzing the surface reaction process of a diffusion material, wherein the surface of the diffusion material is analyzed, wherein hydrogen is injected into the diffusion material exposed in a storage chamber in a vacuum state; and Returning hydrogen to the storage chamber again.
[0017]
In the present invention, the hydrogen gas that has passed through the diffusion material and flowed from the storage chamber to the release chamber is returned to the storage chamber again. Thereby, the hydrogen gas can be reused.
[0018]
According to a seventh aspect of the present invention, in the method for analyzing a surface reaction process of a diffusion material according to the sixth aspect, tritium is used as the hydrogen, and the method further comprises a tritium detecting step of detecting an amount of tritium in the storage chamber. And
[0019]
In the present invention, when a gas containing tritium is used as hydrogen, the increase or decrease of tritium in the system is monitored. This makes it possible to detect when there is nuclide conversion, leakage, or the like.
[0020]
BEST MODE FOR CARRYING OUT THE INVENTION
Next, an embodiment of the present invention will be described with reference to the drawings.
In FIG. 1, reference numeral 1 denotes a sample which is a hydrogen diffusion material, 2 denotes an occlusion chamber, 3 denotes a release chamber, and a sample 1 is disposed at a boundary position between the occlusion chamber 2 and the release chamber 3. The space is kept airtight so that impurities and the like do not enter.
[0021]
The sample 1 may be any material as long as it is a material that transmits hydrogen while diffusing it, such as palladium, titanium, and vanadium. The constituent materials of the occlusion chamber 2 and the release chamber 3 are made of a material that does not have any adverse effect even when it comes into contact with hydrogen or a diffusion material.
In the present embodiment, the description is made using deuterium. However, the present invention is not limited to this, and light hydrogen can be used instead.
[0022]
In this apparatus, a vacuum exhaust system 7, a hydrogen supply system 8, and a pressure gauge 19 are provided, and the discharge chamber 3 is provided with a vacuum exhaust system (circulation device) 9 and a vacuum vacuum exhaust system gauge 20. Have been.
The vacuum evacuation system 7 is for maintaining the storage chamber 2 in a high vacuum state before supplying the deuterium gas, and is provided between the rotary pump 7a, the vacuum valve 7b, and the rotary pump 7a and the vacuum valve 7b. And a vacuum gauge 7d provided between the vacuum valve 7b and the storage chamber 2 for the storage chamber.
The hydrogen supply system 8 fills the storage chamber 2 in a vacuum state with deuterium gas, and includes a deuterium gas cylinder 8a and a variable leak valve 8b.
The evacuation system 9 always keeps the discharge chamber 3 in a vacuum state, and includes a flow path 9 a that exits from the discharge chamber 3 and returns to the storage chamber 2. Further, a turbo-molecular pump 9b for evacuating the discharge chamber 3 to the flow passage 9a, a circulation pump 9c for sending gas from the discharge chamber 3 to the storage chamber 2, and a gas sent from the circulation pump 9c. 9d for compressing the gas, an external exhaust valve 9e for switching between a flow path for sending the gas pressurized by the compressor 9d to the storage chamber 3 and a flow path for sending to a separate discharge system, and a filter 9f for removing impurities. Are provided in this order from the discharge chamber 3 to the occlusion chamber 2. The filter 9f removes impurities generated from the circulation pump 9c and the piping system by cooling the flow path 9a with liquid nitrogen or the like. When the pressure in the storage chamber 2 is not high, the compressor 9d may not be provided in some cases. Similarly, when the amount of impurities generated from the circulation pump 9c and the piping system is extremely small, the filter 9f may not be provided in some cases.
[0023]
As shown in the figure, the sample 1 is arranged in a boundary position between the occlusion chamber 2 and the discharge chamber 3 while keeping the airtight state therebetween. At this time, the sample 1 is set so that the film formation surface side of the sample 1 faces the storage chamber 2 as shown in FIG. In the figure, reference numeral 4 is a vacuum flange, and 6 is an O-ring.
[0024]
The storage chamber 2 is provided with an XPS measuring device including an electrostatic analyzer 21 and an X-ray gun 22 as analysis means, and an X-ray detector 14 as a radiation measuring device.
[0025]
Since the X-ray detector 14 is installed in the atmosphere, a beryllium window 14a is provided between the X-ray source and the storage chamber 2 so as to separate the vacuum from the atmosphere and transmit X-rays. ing.
[0026]
In the present embodiment, first, the sample 1 is set between the occlusion chamber 2 and the release chamber 3. After the sample 1 is set, the vacuum evacuation system 7 on the storage chamber 2 side and the vacuum evacuation system 9 on the release chamber 3 side are driven to bring both chambers into a high vacuum state at a predetermined pressure. The vacuum evacuation system 9 is evacuated by a turbo molecular pump 9b, and is evacuated to the outside via an external exhaust valve 9e.
Next, when a predetermined high vacuum state is reached, the state of the sample surface in the storage chamber 2 is measured by the XPS measuring device, and the substance present on the sample surface is measured. After the measurement, the vacuum valve 7b of the evacuation system 7 in the storage chamber 2 is closed, and deuterium gas is introduced into the storage chamber 2 by the hydrogen supply system 8. After the introduction of the predetermined amount, the supply of hydrogen is stopped, and an operation of returning the hydrogen permeated to the discharge chamber 3 by the vacuum exhaust system 9 to the storage chamber 2 is performed. At this time, the external exhaust valve 9e is switched to the storage chamber 2 side so that the hydrogen gas sent by the circulation pump 9c is introduced to the storage chamber 2 side.
[0027]
Since the XPS measuring device is a device that can only measure in a high vacuum, it is not operated during this time, the X-ray detector 14 is operated, and the X-rays emitted from the sample 1 by the X-ray detector 14 are The dose can be detected.
[0028]
The release chamber 3 is in a state of being exhausted by the turbo molecular pump 9b. Therefore, the gas permeating the sample 1 is sucked by the turbo molecular pump 9b and sent to the storage chamber 2 side by the circulation pump 9c. At this time, the gas is first pressurized by the compressor 9d in accordance with the pressure of the storage chamber 2, and then introduced into the storage chamber 2 after the impurities are removed by the filter 9f.
Thereafter, after a predetermined time has elapsed, the storage chamber 2 is evacuated again by opening the vacuum valve 7b of the evacuation system 7. Further, the external exhaust valve 9e is switched to the exhaust side.
Then, after the inside of the storage chamber 2 becomes high vacuum, the XPS measuring device is driven again to perform elemental analysis on the surface side of the sample 1.
[0029]
As described above, the gas in the discharge chamber 3 is returned to the storage chamber 2 by the vacuum exhaust system 9, and deuterium circulates between the storage chamber 2 and the release chamber 3. Therefore, the effect that deuterium can be used repeatedly and the cost can be reduced can be obtained. In addition, when tritium is used as hydrogen, since high safety is required for the treatment of exhaust gas and expensive tritium can be circulated and used, the cost can also be reduced.
The hydrogen gas returned to the storage chamber 2 can be adjusted to the pressure of the storage chamber 2 by being compressed by the compressor 9d, and impurities can be removed by passing through the filter 9f.
In addition, since the state of the sample surface before the permeation of deuterium and the state of the sample surface after the permeation of deuterium are measured, the state of the sample 1 before and after the reaction can be analyzed. Can be ascertained that the substance has been generated. Moreover, for a long time, the space between the storage chamber 2, the sample 1, and the discharge chamber 3 is kept airtight, and the sample 1 is not taken out between them, so that there is no danger that impurities are mixed in from outside during the experiment. The substance generated on the surface of the sample 1 can be analyzed accurately and accurately.
[0030]
Next, a second embodiment of the present invention will be described. The same components as those in the first embodiment are denoted by the same reference numerals, and description thereof is omitted.
FIG. 3 is a diagram showing the configuration of the present embodiment. In the present embodiment, tritium is contained as hydrogen in the deuterium gas cylinder 8a.
And, a tritium detecting means 20 is provided. The tritium detecting means 20 includes a circulation flow path 20a that exits from the storage chamber 2 and returns to the storage chamber 2. The circulation flow path 20a includes a tritium monitor 20b and a circulation pump 20c from upstream to downstream. And the filter 20d are provided in this order.
The tritium monitor 20b is a device that detects the amount of tritium, and the filter 20d is a device that removes impurities generated from the circulation pump 20c and the piping system by cooling the circulation channel 20a with liquid nitrogen or the like. When impurities generated from the circulation pump 20c and the piping system are extremely small, the filter 20d may not be provided in some cases.
[0031]
Next, the operation of the present embodiment will be described.
In the present embodiment, as in the first embodiment, hydrogen is supplied to the storage chamber 2 from the hydrogen supply system 8, and the hydrogen diffuses and permeates inside the sample 1. At this time, the gas in the release chamber 3 is returned to the storage chamber 2 by the vacuum exhaust system 9 as described above, and deuterium circulates between the storage chamber 2 and the release chamber 3. Therefore, deuterium can be used repeatedly, and costs can be reduced.
After the supply of hydrogen from the hydrogen supply system 8 is stopped, the circulation pump 20c is driven to measure the gas in the storage chamber 2 with the tritium monitor 20b. The tritium monitor 20b detects the amount of tritium contained in the gas. Therefore, it is possible to detect a change in the amount of tritium in the system (the storage chamber 2 and the release chamber 3), and it is possible to detect when there is nuclide conversion or leakage.
In this way, by recycling and recycling tritium without exhausting it to the outside, high safety and low cost can be realized.
[0032]
In the illustrated embodiments described above, a configuration in which various analyzers are provided in the occlusion chamber 2 has been described. However, it is a matter of course that the analyzers may be provided on the release chamber 3 side. In addition, if these nuclear analysis means are used according to the analysis purpose, various analysis purposes can be realized. Therefore, the present invention is not limited to the examples described in the above embodiments, and can be installed and used in accordance with at least the contents to be analyzed.
Further, the analysis means does not necessarily need to be integrated with the storage chamber 2 or the release chamber 3 and may be provided separately from the storage chamber 2 and the release chamber 3. That is, after permeating hydrogen into the sample 1, the sample 1 may be taken out from the storage chamber 2 and the release chamber 3, and the sample 1 may be transferred to analysis means provided outside for analysis.
[0033]
【The invention's effect】
As described above, according to the present invention, the gas that has passed through the diffusion material and flowed from the storage chamber to the discharge chamber is returned to the storage chamber. As a result, the hydrogen gas can be reused, and the cost can be reduced. Further, when tritium is used as hydrogen, high safety can be obtained by circulating and recycling tritium without discharging the tritium to the outside.
Further, by providing a filter, impurities emitted from the circulation pump and the piping system can be removed.
Further, since the compressor is provided, hydrogen compressed according to the pressure of the storage chamber can be introduced into the storage chamber.
Furthermore, when tritium is used as hydrogen, nuclide conversion, leakage, and the like can be detected by using tritium detection means.
[Brief description of the drawings]
FIG. 1 is a configuration diagram illustrating a surface reaction process analyzer according to a first embodiment of the present invention.
FIG. 2 is a cross-sectional view showing a confidentiality maintaining structure between the storage chamber, the sample, and the release chamber in FIG.
FIG. 3 is a configuration diagram illustrating a surface reaction process analyzer according to a second embodiment of the present invention.
[Explanation of symbols]
1 sample (diffusion material)
2 Storage room 3 Release room 9 Vacuum exhaust system (circulation device)
9a flow path 9c circulation pump 9d compressor 9f filter 20 tritium detection means 20a flow path 20b tritium monitor 20c circulation pump 20d filter

Claims (7)

水素ガスを拡散し得る拡散材料を互いに気密状態で挟んで配置する吸蔵室及び放出室と、拡散材料の表面を分析する分析手段とを備えた拡散材料の表面反応過程分析装置において、
吸蔵室内に水素を供給する水素供給系と、前記拡散材料を透過して前記吸蔵室から放出室に流入したガスを前記吸蔵室に戻す循環装置とを備え、該循環装置は放出室と吸蔵室とを連通する流路と、該流路途中に設けられ前記放出室側から吸蔵室側へガスを送る循環ポンプとを備えていることを特徴とする拡散材料の表面反応過程分析装置。In an analyzer for a surface reaction process of a diffusion material, comprising an absorption chamber and an emission chamber in which a diffusion material capable of diffusing hydrogen gas is disposed sandwiching each other in an airtight state, and analysis means for analyzing the surface of the diffusion material,
A hydrogen supply system for supplying hydrogen into the storage chamber; and a circulating device for returning gas permeating the diffusion material and flowing from the storage chamber to the discharge chamber to the storage chamber, the circulator comprising a discharge chamber and a storage chamber. And a circulation pump which is provided in the middle of the flow path and sends gas from the discharge chamber side to the storage chamber side. 請求項１に記載の拡散材料の表面反応過程分析装置において、
不純物を除去するフィルタが前記流路途中に設けられていることを特徴とする拡散材料の表面反応過程分析装置。The apparatus for analyzing a surface reaction process of a diffusion material according to claim 1,
An apparatus for analyzing a surface reaction process of a diffusion material, wherein a filter for removing impurities is provided in the middle of the flow path. 請求項１または２に記載の拡散材料の表面反応過程分析装置において、
昇圧用の圧縮機が前記流路途中に設けられていることを特徴とする拡散材料の表面反応過程分析装置。The apparatus for analyzing a surface reaction process of a diffusion material according to claim 1 or 2,
An apparatus for analyzing a surface reaction process of a diffusion material, wherein a pressure increasing compressor is provided in the middle of the flow path. 請求項１から３いずれかに記載の拡散材料の表面反応過程分析装置において、
前記水素としてトリチウムが用いられ、前記吸蔵室内のトリチウム量を検出するトリチウム検出手段が設けられていることを特徴とする拡散材料の表面反応過程分析装置。The apparatus for analyzing a surface reaction process of a diffusion material according to any one of claims 1 to 3,
An apparatus for analyzing a surface reaction process of a diffusion material, wherein tritium is used as the hydrogen, and tritium detecting means for detecting an amount of tritium in the storage chamber is provided. 請求項４に記載の拡散材料の表面反応過程分析装置において、
前記トリチウム検出手段は、前記吸蔵室から出て該吸蔵室に戻る流路と、該流路途中に設けられた循環ポンプと、トリチウムモニターとを備えていることを特徴とする拡散材料の表面反応過程分析装置。The apparatus for analyzing a surface reaction process of a diffusion material according to claim 4,
The tritium detecting means includes a flow path that exits the storage chamber and returns to the storage chamber, a circulation pump provided in the middle of the flow path, and a tritium monitor. Process analyzer. 吸蔵室と放出室との境界位置に、水素を拡散し得る拡散材料を互いに気密状態で挟んで配置し、前記ガスを吸蔵室から拡散材料中を経て放出室に放出させ、該拡散材料の表面を分析する拡散材料の表面反応過程分析方法であって、真空状態の吸蔵室内に露出した前記拡散材料に水素を注入する工程と、該拡散材料を透過した前記水素を再び前記吸蔵室に戻す工程とを有することを特徴とする拡散材料の表面反応過程分析方法。A diffusion material capable of diffusing hydrogen is disposed in a boundary position between the occlusion chamber and the release chamber in an airtight manner with respect to each other, and the gas is released from the occlusion chamber through the diffusion material to the release chamber, and the surface of the diffusion material is discharged. A step of injecting hydrogen into the diffusion material exposed in the storage chamber in a vacuum state, and a step of returning the hydrogen permeated through the diffusion material to the storage chamber again. A method for analyzing a surface reaction process of a diffusion material, comprising: 請求項６に記載の拡散材料の表面反応過程分析方法において、
前記水素としてトリチウムが用いられ、前記吸蔵室内のトリチウム量を検出するトリチウム検出工程を有することを特徴とする拡散材料の表面反応過程分析方法。The method for analyzing a surface reaction process of a diffusion material according to claim 6,
A method for analyzing a surface reaction process of a diffusion material, wherein tritium is used as the hydrogen, and the method further comprises a tritium detecting step of detecting an amount of tritium in the storage chamber.
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