JP2003207500A - Agent and method for detecting germane - Google Patents

Agent and method for detecting germane

Info

Publication number
JP2003207500A
JP2003207500A JP2002008199A JP2002008199A JP2003207500A JP 2003207500 A JP2003207500 A JP 2003207500A JP 2002008199 A JP2002008199 A JP 2002008199A JP 2002008199 A JP2002008199 A JP 2002008199A JP 2003207500 A JP2003207500 A JP 2003207500A
Authority
JP
Japan
Prior art keywords
germane
detecting
agent
detection
detection agent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP2002008199A
Other languages
Japanese (ja)
Other versions
JP3895604B2 (en
Inventor
Yoji Nawa
洋二 名和
Chitsu Arakawa
秩 荒川
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Japan Pionics Ltd
Original Assignee
Japan Pionics Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Japan Pionics Ltd filed Critical Japan Pionics Ltd
Priority to JP2002008199A priority Critical patent/JP3895604B2/en
Priority to PCT/JP2002/013542 priority patent/WO2003060510A1/en
Priority to TW92100844A priority patent/TW200302348A/en
Publication of JP2003207500A publication Critical patent/JP2003207500A/en
Application granted granted Critical
Publication of JP3895604B2 publication Critical patent/JP3895604B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Molecular Biology (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Biophysics (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

<P>PROBLEM TO BE SOLVED: To provide a detecting agent or a detecting method which can sensitively detect germane exhausted from a semiconductor manufacturing process or the like without being affected by atmospheric gas. <P>SOLUTION: The detecting agent is made up of an inorganic carrier which carries permanganate of alkaline metals as a coloring principle. The germane is detected by making the germane contact with the detecting agent and by detecting the change of color of the detecting agent. <P>COPYRIGHT: (C)2003,JPO

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の属する技術分野】本発明は、ゲルマンの検知剤
及び検知方法に関する。さらに詳細には、半導体製造工
程等から排出されるゲルマンを高感度で検知できる検知
剤及び検知方法に関する。
TECHNICAL FIELD The present invention relates to a detecting agent and a detecting method for germane. More specifically, it relates to a detecting agent and a detecting method capable of detecting germane discharged from a semiconductor manufacturing process or the like with high sensitivity.

【0002】[0002]

【従来の技術】半導体製造工業においては、アルシン、
ホスフィン、ジボラン、セレン化水素等とともにゲルマ
ンが原料ガスとして使用されている。ゲルマンを使用し
た際には、半導体製造工程からは、窒素、水素、ヘリウ
ム等のガスで希釈された状態で未反応のゲルマンが排出
されるが、ゲルマンは毒性が高く、大気にそのまま放出
した場合は人体及び環境に悪影響を与えるので、大気に
放出するに先立ってゲルマンを含有するガスを浄化しこ
れが含まれていないことを確認する必要がある。また、
例えば乾式浄化法によりゲルマンを浄化する場合は、浄
化筒の破過を検知する必要がある。このため、取り扱い
が容易で感度が高いゲルマンを検知するための検知剤あ
るいは検知方法が開発されてきた。
In the semiconductor manufacturing industry, arsine,
Germane is used as a source gas together with phosphine, diborane, hydrogen selenide and the like. When germane is used, unreacted germane is discharged from the semiconductor manufacturing process in a state diluted with a gas such as nitrogen, hydrogen, or helium, but germane is highly toxic and is released into the atmosphere as it is. Has a harmful effect on the human body and the environment, so it is necessary to purify the gas containing germane and confirm that it is not contained before it is released into the atmosphere. Also,
For example, when germane is purified by the dry purification method, it is necessary to detect breakthrough of the purification cylinder. Therefore, a detecting agent or a detecting method for detecting germane which is easy to handle and has high sensitivity has been developed.

【0003】従来より、ゲルマン等の水素化物ガスを検
知するための検知剤としては、例えば第二銅塩とパラジ
ウム塩との混合物を変色成分とする検知剤(特開昭62
−22062号公報)、第二銅塩と金塩との混合物を変
色成分とする検知剤(特開平2−32254号公報)、
無機質担体に変色成分としてモリブデン酸及びモリブデ
ン酸塩の少なくとも一種が担持されてなる検知剤(特開
平8−129009号公報)が知られている。また、検
知方法としては、ガラス管にこれらの検知剤を充填した
検知管にサンプリングしたガスを通し、その変色により
水素化物ガスの有無を検知する方法、有害ガスの浄化筒
の覗き窓部等に検知剤を充填し、その変色によって浄化
筒の破過を検知する方法等が一般的に用いられている。
Conventionally, as a detecting agent for detecting a hydride gas such as germane, for example, a detecting agent containing a mixture of a cupric salt and a palladium salt as a color-changing component (JP-A-62-62).
-22062), a detection agent containing a mixture of a cupric salt and a gold salt as a discoloring component (JP-A-2-32254),
A detection agent (Japanese Unexamined Patent Publication (Kokai) No. 8-129090) in which at least one of molybdic acid and molybdate is supported as a discoloring component on an inorganic carrier is known. In addition, as a detection method, a sampled gas is passed through a detector tube filled with these detecting agents in a glass tube, and the presence or absence of hydride gas is detected by its discoloration, and the inspection window of the purification column for harmful gas is used. A method of filling a detection agent and detecting breakthrough of the purifying cylinder based on its color change is generally used.

【0004】[0004]

【発明が解決しようとする課題】しかしながら、第二銅
塩とパラジウム塩との混合物を変色成分とする検知剤
は、水素の存在下では水素により変色するので、水素を
含むガス中のゲルマンを選択的に検知することができな
いほか、ゲルマンと浄化剤が反応して水素を発生するよ
うな浄化筒の破過を検知することができないという不都
合があった。また、第二銅塩と金塩との混合物を変色成
分とする検知剤、無機質担体に変色成分としてモリブデ
ン酸及びモリブデン酸塩の少なくとも一種が担持されて
なる検知剤は、アルシン、ホスフィンを高感度で検知す
ることができるが、ゲルマンの検知については充分な感
度が得られなかった。ゲルマンは他の水素化物に比べて
反応性が低く、短時間で鋭敏に変色するようなゲルマン
の検知剤の開発は困難であった。
However, the detection agent containing a mixture of a cupric salt and a palladium salt as a discoloring component is discolored by hydrogen in the presence of hydrogen, so germane in a gas containing hydrogen is selected. In addition to the above, there is the inconvenience that it is not possible to detect the breakthrough of the purifying cylinder that causes hydrogen to react with germane to generate hydrogen. Further, a detection agent having a mixture of a cupric salt and a gold salt as a color-changing component, a detection agent in which at least one of molybdic acid and molybdate is supported as a color-changing component on an inorganic carrier, arsine and phosphine are highly sensitive. However, sufficient sensitivity was not obtained for the detection of germane. Germane has lower reactivity than other hydrides, and it has been difficult to develop a detecting agent for germane that causes a sharp discoloration in a short time.

【0005】従って、本発明が解決しようとする課題
は、半導体製造工程等から排出されるゲルマンを、雰囲
気ガスに影響されることなく高感度で検知できる検知剤
あるいは検知方法を提供することである。
Therefore, the problem to be solved by the present invention is to provide a detecting agent or a detecting method capable of detecting germane discharged from a semiconductor manufacturing process or the like with high sensitivity without being affected by atmospheric gas. .

【0006】[0006]

【課題を解決するための手段】本発明者らは、これらの
課題を解決すべく鋭意検討した結果、アルカリ金属の過
マンガン酸塩が、感度が高く変色速度が速いゲルマンの
検知剤の変色成分として使用し得ることを見い出し、本
発明のゲルマンの検知剤及び検知方法に到達した。すな
わち本発明は、無機質担体に変色成分としてアルカリ金
属の過マンガン酸塩を担持させたことを特徴とするゲル
マンの検知剤である。また、本発明は、ゲルマンを含有
するガスを、無機質担体に変色成分としてアルカリ金属
の過マンガン酸塩を担持させた検知剤と接触させて、該
検知剤の変色を検知することにより該ガスに含まれるゲ
ルマンを検知することを特徴とするゲルマンの検知方法
でもある。
As a result of intensive studies to solve these problems, the present inventors have found that permanganate of an alkali metal is a color-changing component of a detecting agent for germane having high sensitivity and high color-changing speed. As a result, they have found that they can be used as, and have reached the germane detection agent and detection method of the present invention. That is, the present invention is a germane detection agent characterized in that an inorganic carrier carries an alkali metal permanganate as a discoloring component. Further, the present invention, by contacting a gas containing germane with a detection agent having an alkali metal permanganate as a discoloration component carried on an inorganic carrier, the gas is detected by detecting the color change of the detection agent. It is also a method for detecting germane, which is characterized by detecting contained germane.

【0007】[0007]

【発明の実施の形態】本発明は、窒素、水素、アルゴ
ン、ヘリウム等を含むガス中に存在するゲルマンを検知
する検知剤あるいは検知方法に適用されが、特に水素を
含むガス中のゲルマンの検知に効果が発揮される。尚、
本発明におけるゲルマンは、モノゲルマン(GeH
のほか、ジゲルマン(Ge)、トリゲルマン(G
)を含むものである。
BEST MODE FOR CARRYING OUT THE INVENTION The present invention is applied to a detection agent or a detection method for detecting germane present in a gas containing nitrogen, hydrogen, argon, helium, etc., but particularly to the detection of germane in a gas containing hydrogen. Is effective. still,
The germane in the present invention is monogermane (GeH 4 ).
In addition to Digerman (Ge 2 H 6 ), Trigerman (G
e 3 H 8 ).

【0008】本発明のゲルマンの検知剤は、無機質担体
に変色成分としてアルカリ金属の過マンガン酸塩を担持
させた検知剤である。また、本発明のゲルマンの検知方
法は、ゲルマンを含有するガスを、無機質担体に変色成
分としてアルカリ金属の過マンガン酸塩を担持させた検
知剤と接触させて、検知剤の変色を検知することにより
前記ガスに含まれるゲルマンを検知する検知方法であ
る。
The germane detection agent of the present invention is a detection agent in which an alkali metal permanganate as a discoloring component is carried on an inorganic carrier. Further, the method for detecting germane of the present invention, a gas containing germane is contacted with a detecting agent having an alkali metal permanganate as a discoloring component supported on an inorganic carrier, and the discoloring of the detecting agent is detected. Is a detection method for detecting germane contained in the gas.

【0009】以下、本発明の検知剤について詳細に説明
する。本発明のゲルマンの検知剤においては、アルカリ
金属の過マンガン酸塩が無機質担体に担持せしめられて
検知剤とされる。無機質担体としては、シリカゲル、ア
ルミナ、ジルコニア、チタニア、シリカアルミナ、シリ
カチタニア等を例示することができる。しかし、これら
の無機質担体の中でシリカゲル以外の無機質担体を使用
した場合は、比表面積が大きいものほど無機質担体の作
用により光で過マンガン酸塩が分解しやすくなるので、
高比表面積の無機質担体が使用できず高感度の検知剤が
得られ難いという不都合がある。従って、無機質担体と
してシリカゲルを用いることが好ましい。無機質担体の
形態には特に制限はないが、シリカゲルの場合は、通常
は比表面積が0.1〜400m/gの範囲のものが使
用可能である。
The detection agent of the present invention will be described in detail below. In the germane detection agent of the present invention, an alkali metal permanganate is supported on an inorganic carrier to form a detection agent. Examples of the inorganic carrier include silica gel, alumina, zirconia, titania, silica alumina, silica titania and the like. However, when an inorganic carrier other than silica gel is used among these inorganic carriers, the larger the specific surface area, the more easily the permanganate is decomposed by light due to the action of the inorganic carrier,
There is an inconvenience that it is difficult to obtain a highly sensitive detection agent because an inorganic carrier having a high specific surface area cannot be used. Therefore, it is preferable to use silica gel as the inorganic carrier. The form of the inorganic carrier is not particularly limited, but in the case of silica gel, one having a specific surface area of 0.1 to 400 m 2 / g can be usually used.

【0010】本発明の検知剤における過マンガン酸塩と
しては、過マンガン酸リチウム、過マンガン酸ナトリウ
ム、過マンガン酸カリウムを挙げることができるが、ゲ
ルマンを検知しやすく、また容易に入手できることか
ら、過マンガン酸カリウムを用いることが好ましい。ア
ルカリ金属の過マンガン酸塩の含有量は、無機質担体に
対して、通常は0.001〜0.2wt%、好ましくは
0.005〜0.1wt%である。アルカリ金属の過マ
ンガン酸塩の含有量が無機質担体に対して0.001w
t%未満の場合は、検知剤の変色成分の色が薄すぎて検
知しにくくなる不都合を生じる。また、ゲルマンは他の
水素化物に比べて反応性が低く、ACGIHが定めてい
る許容濃度(0.2ppm)近辺のゲルマンを検知する
際、アルカリ金属の過マンガン酸塩の含有量が無機質担
体に対して0.2wt%を超える場合は検知剤の検出感
度が悪くなる不都合を生じる。
Examples of the permanganate salt in the detecting agent of the present invention include lithium permanganate, sodium permanganate, and potassium permanganate. However, since germane is easily detected and is easily available, Preference is given to using potassium permanganate. The content of alkali metal permanganate is usually 0.001 to 0.2 wt% and preferably 0.005 to 0.1 wt% with respect to the inorganic carrier. The content of alkali metal permanganate is 0.001w based on the inorganic carrier.
If it is less than t%, the color of the discoloring component of the detection agent is too light to be detected easily. Further, germane has lower reactivity than other hydrides, and when detecting germane in the vicinity of the permissible concentration (0.2 ppm) defined by ACGIH, the content of alkali metal permanganate in the inorganic carrier is detected. On the other hand, when it exceeds 0.2 wt%, the detection sensitivity of the detection agent is deteriorated.

【0011】アルカリ金属の過マンガン酸塩を無機質担
体に担持させる方法としては、アルカリ金属の過マンガ
ン酸塩を含む水溶液を無機質担体に含浸させた後乾燥す
る方法、あるいは無機質担体をかき混ぜながら前記水溶
液を振りかけて乾燥させる方法を例示することができ
る。
As a method of supporting the alkali metal permanganate on the inorganic carrier, a method of impregnating an aqueous solution containing the alkali metal permanganate into the inorganic carrier and then drying it, or the above-mentioned aqueous solution while stirring the inorganic carrier is used. The method of sprinkling and drying can be illustrated.

【0012】次に本発明の検知方法について詳細に説明
する。本発明のゲルマンの検知方法においては、半導体
製造工程等から排出されるゲルマンを含有するガスを、
前述の検知剤と接触させることによりガスに含まれるゲ
ルマンが検知される。本発明において、ゲルマンがアル
カリ金属の過マンガン酸塩と接触すると、ゲルマンが酸
化されるとともにアルカリ金属の過マンガン酸塩が変色
するので、この間の検知剤の変色を検知することにより
ガス中のゲルマンを検知することができる。例えば、ゲ
ルマンが白色の無機質担体に過マンガン酸カリウムを担
持させた検知剤と接触した場合、検知剤は赤紫色から白
色に鋭敏に変色する。
Next, the detection method of the present invention will be described in detail. In the germane detection method of the present invention, the gas containing germane discharged from the semiconductor manufacturing process,
Germane contained in the gas is detected by bringing it into contact with the above-mentioned detection agent. In the present invention, when germane is brought into contact with an alkali metal permanganate, the germane is oxidized and the alkali metal permanganate is discolored.Therefore, by detecting the discoloration of the detection agent during this period, germane in the gas is detected. Can be detected. For example, when germane comes into contact with a detection agent in which potassium permanganate is supported on a white inorganic carrier, the detection agent is sensitively changed from red purple to white.

【0013】本発明のゲルマンの検知剤は通常固体であ
り、例えば本発明の検知剤をガラス製の透明管に充填し
て検知管とし、検知対象ガスを配管等のガス採取口より
検知管に吸引することにより目的のゲルマンを検知する
ことができる。また、本発明の検知剤をガラス製あるい
はプラスチック製の透明管に充填し、これを検知対象ガ
スの配管のバイパス管に設置して、透明管の中に検知対
象ガスを通すことにより目的のゲルマンを検知すること
ができる。また、本発明のゲルマンの検知剤を浄化筒の
破過を検知するために使用する場合には、検知剤を浄化
筒内の浄化剤層の下流側、浄化筒の後または複数の浄化
剤層の間などに設けられた透明な覗き窓部に配置して使
用される。
The germane detection agent of the present invention is usually a solid. For example, the detection agent of the present invention is filled in a glass transparent tube to form a detection tube, and the gas to be detected is introduced from a gas sampling port such as a pipe into the detection tube. The target germane can be detected by suction. Further, the detection agent of the present invention is filled in a transparent tube made of glass or plastic, and this is installed in a bypass pipe of the pipe for the gas to be detected, and the target germane is passed by passing the gas to be detected in the transparent tube. Can be detected. When the germane detection agent of the present invention is used to detect breakthrough of the purification tube, the detection agent is used on the downstream side of the purification agent layer in the purification tube, after the purification tube or in a plurality of purification agent layers. It is used by arranging it in a transparent viewing window provided in the space between them.

【0014】本発明の検知剤を透明管に充填し、これを
バイパス管に設置して使用する場合、あるいは本発明の
検知剤を浄化剤等とともに使用する場合等において、検
知剤と接触させる検知対象ガスの速度に特に制限はない
が、通常は空筒線速度で0.01〜100cm/sec
程度とされる。空筒線速度が0.01cm/secより
低い場合は検知が遅くなり、100cm/secより高
い場合は圧力損失が大きくなる虞がある。接触時の検知
対象ガスの温度は通常は−20〜100℃、また、圧力
は通常は常圧であるが1kPa(abs)の減圧から1
MPa(abs)の加圧下においても使用可能である。
When a transparent pipe is filled with the detecting agent of the present invention and is used by being installed in a bypass pipe, or when the detecting agent of the present invention is used together with a purifying agent, etc., detection by contact with the detecting agent The velocity of the target gas is not particularly limited, but is usually 0.01 to 100 cm / sec in the empty cylinder linear velocity.
It is considered as a degree. If the hollow cylinder linear velocity is lower than 0.01 cm / sec, the detection becomes slow, and if it is higher than 100 cm / sec, the pressure loss may increase. The temperature of the gas to be detected at the time of contact is usually −20 to 100 ° C., and the pressure is usually atmospheric pressure, but from a reduced pressure of 1 kPa (abs) to 1
It can also be used under a pressure of MPa (abs).

【0015】本発明の検知剤及び検知方法においては、
水素の存在下でも水素により変色しないので、水素を含
むガス中のゲルマンを選択的に高感度で検知することが
できる。また、半導体製造工程から排出されるゲルマン
を乾式浄化法により浄化する場合、ゲルマンと浄化剤が
反応して水素を発生するような浄化筒の破過も高感度で
検知することができる。
In the detection agent and the detection method of the present invention,
Since hydrogen does not discolor even in the presence of hydrogen, germane in a gas containing hydrogen can be selectively detected with high sensitivity. Further, when the germane discharged from the semiconductor manufacturing process is purified by the dry purification method, breakthrough of the purifying cylinder in which germane and the purifying agent react to generate hydrogen can be detected with high sensitivity.

【0016】[0016]

【実施例】次に、本発明を実施例により具体的に説明す
るが、本発明がこれらにより限定されるものではない。
EXAMPLES Next, the present invention will be specifically described by way of examples, but the present invention is not limited to these.

【0017】実施例1 (検知剤の調製)濃度10g/Lの過マンガン酸カリウ
ム水溶液7.5mlに1000mlの水を加えたもの
を、径1.5〜4mm、比表面積300m/gの球状
シリカゲル500gに含浸させた後、ロータリーエバポ
レーターを用いて80℃の温度で減圧乾燥させて検知剤
(過マンガン酸カリウムの含有量:シリカゲルに対して
0.015wt%)を調製した。
Example 1 (Preparation of detection agent) A solution obtained by adding 1000 ml of water to 7.5 ml of an aqueous potassium permanganate solution having a concentration of 10 g / L was used to obtain spherical particles having a diameter of 1.5 to 4 mm and a specific surface area of 300 m 2 / g. After impregnating 500 g of silica gel, it was dried under reduced pressure at a temperature of 80 ° C. using a rotary evaporator to prepare a detection agent (content of potassium permanganate: 0.015 wt% with respect to silica gel).

【0018】(検知能力の測定)この検知剤20gを内
径20mmのガラス管に充填した検知管を製作し、これ
に10ppmのゲルマン及び10%の水素を含有する窒
素ガスを、25℃、常圧、空筒線速度5cm/secの
条件で接触させ、検知剤が赤紫色から白色に変色し始め
るまでの時間を測定した。その結果を表1に示す。
(Measurement of Detection Ability) A detection tube was prepared by filling 20 g of this detection agent in a glass tube having an inner diameter of 20 mm, and nitrogen gas containing 10 ppm germane and 10% hydrogen was added thereto at 25 ° C. and normal pressure. The contact time was 5 cm / sec, and the time until the detection agent started to change color from red purple to white was measured. The results are shown in Table 1.

【0019】実施例2 実施例1におけるアルカリ金属の過マンガン酸塩を、過
マンガン酸ナトリウムに替えたほかは実施例1と同様に
して検知剤を調製した。この検知剤を用いたほかは実施
例1と同様にして検知能力の測定を行なった。その結果
を表1に示す。
Example 2 A detection agent was prepared in the same manner as in Example 1 except that the alkali metal permanganate in Example 1 was replaced with sodium permanganate. The detection ability was measured in the same manner as in Example 1 except that this detection agent was used. The results are shown in Table 1.

【0020】実施例3,4 実施例1における検知対象ガス中のゲルマンの濃度を、
各々1ppm、20ppmに変えたほかは実施例1と同
様にして検知能力の測定を行なった。その結果を表1に
示す。
Examples 3 and 4 The concentration of germane in the gas to be detected in Example 1 is
The detection ability was measured in the same manner as in Example 1 except that the amounts were changed to 1 ppm and 20 ppm, respectively. The results are shown in Table 1.

【0021】実施例5,6 実施例1における検知対象ガスの空筒線速度を、各々1
cm/sec、50cm/secに変えたほかは実施例
1と同様にして検知能力の測定を行なった。その結果を
表1に示す。
Embodiments 5 and 6 The empty cylinder linear velocity of the gas to be detected in Embodiment 1 is 1
The detection ability was measured in the same manner as in Example 1 except that the values were changed to cm / sec and 50 cm / sec. The results are shown in Table 1.

【0022】実施例7 実施例1における検知対象ガス中のゲルマンの濃度を
0.2ppmに、検知対象ガスの空筒線速度を50cm
/secに変えたほかは実施例1と同様にして検知能力
の測定を行なった。その結果を表1に示す。
Example 7 The concentration of germane in the gas to be detected in Example 1 was 0.2 ppm, and the empty cylinder linear velocity of the gas to be detected was 50 cm.
The detection ability was measured in the same manner as in Example 1 except that the value was changed to / sec. The results are shown in Table 1.

【0023】実施例8〜10 実施例1における過マンガン酸カリウムのシリカゲルに
対する含有量を、各々0.01wt%、0.10wt
%、0.30wt%に変えたほかは実施例1と同様にし
て検知剤を調製した。これらの検知剤を用いたほかは実
施例1と同様にして検知能力の測定を行なった。その結
果を表1に示す。
Examples 8 to 10 The contents of potassium permanganate in Example 1 with respect to silica gel were 0.01 wt% and 0.10 wt, respectively.
%, 0.30 wt%, and the detecting agent was prepared in the same manner as in Example 1. The detection ability was measured in the same manner as in Example 1 except that these detection agents were used. The results are shown in Table 1.

【0024】[0024]

【表1】 [Table 1]

【0025】[0025]

【発明の効果】本発明のゲルマンの検知剤及び検知方法
により、半導体製造工程等から排出されるゲルマンを、
雰囲気ガスに影響されることなく高感度で検知すること
が可能となった。
EFFECT OF THE INVENTION With the detection agent and detection method for germane of the present invention, the germane discharged from the semiconductor manufacturing process,
It has become possible to detect with high sensitivity without being affected by atmospheric gas.

───────────────────────────────────────────────────── フロントページの続き Fターム(参考) 2G042 AA01 BC13 CA01 CB01 DA03 DA08 FA04 FA11 FB04 FB06 GA03 GA04 HA07 2G054 AA01 AB07 CA30 CE01 EA06 FA06 GB04    ─────────────────────────────────────────────────── ─── Continued front page    F term (reference) 2G042 AA01 BC13 CA01 CB01 DA03                       DA08 FA04 FA11 FB04 FB06                       GA03 GA04 HA07                 2G054 AA01 AB07 CA30 CE01 EA06                       FA06 GB04

Claims (7)

【特許請求の範囲】[Claims] 【請求項1】 無機質担体に変色成分としてアルカリ金
属の過マンガン酸塩を担持させたことを特徴とするゲル
マンの検知剤。
1. A detecting agent for germane, comprising an inorganic carrier carrying an alkali metal permanganate as a discoloring component.
【請求項2】 無機質担体が、シリカゲル、アルミナ、
ジルコニア、チタニア、シリカアルミナ、またはシリカ
チタニアである請求項1に記載のゲルマンの検知剤。
2. The inorganic carrier is silica gel, alumina,
The germane detection agent according to claim 1, which is zirconia, titania, silica alumina, or silica titania.
【請求項3】 アルカリ金属の過マンガン酸塩が、過マ
ンガン酸カリウムである請求項1に記載のゲルマンの検
知剤。
3. The germane detection agent according to claim 1, wherein the alkali metal permanganate is potassium permanganate.
【請求項4】 アルカリ金属の過マンガン酸塩の含有量
が、無機質担体に対して0.001〜0.2wt%であ
る請求項1に記載のゲルマンの検知剤。
4. The germane detection agent according to claim 1, wherein the content of the alkali metal permanganate is 0.001 to 0.2 wt% with respect to the inorganic carrier.
【請求項5】 検知対象が、水素を含有するガス中のゲ
ルマンである請求項1に記載のゲルマンの検知剤。
5. The germane detecting agent according to claim 1, wherein the object to be detected is germane in a gas containing hydrogen.
【請求項6】 ゲルマンを含有するガスを、無機質担体
に変色成分としてアルカリ金属の過マンガン酸塩を担持
させた検知剤と接触させて、該検知剤の変色を検知する
ことにより該ガスに含まれるゲルマンを検知することを
特徴とするゲルマンの検知方法。
6. A gas containing germane is included in the gas by detecting the discoloration of the detection agent by bringing the gas containing germane into contact with a detection agent having an alkali metal permanganate as a discoloration component supported thereon. A method for detecting germane, which comprises detecting germane generated.
【請求項7】 検知対象ガスが、ゲルマンとともに水素
を含むガスである請求項6に記載のゲルマンの検知方
法。
7. The method for detecting germane according to claim 6, wherein the gas to be detected is a gas containing hydrogen together with germane.
JP2002008199A 2002-01-17 2002-01-17 Germanium detection agent and detection method Expired - Fee Related JP3895604B2 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
JP2002008199A JP3895604B2 (en) 2002-01-17 2002-01-17 Germanium detection agent and detection method
PCT/JP2002/013542 WO2003060510A1 (en) 2002-01-17 2002-12-25 Agent and method for detecting germane
TW92100844A TW200302348A (en) 2002-01-17 2003-01-16 Detector and method for detecting germane

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2002008199A JP3895604B2 (en) 2002-01-17 2002-01-17 Germanium detection agent and detection method

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008020343A (en) * 2006-07-13 2008-01-31 Japan Pionics Co Ltd Agent for detecting germane and organic silicon compound

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4420567A (en) * 1981-10-22 1983-12-13 Mda Scientific, Inc. Hydride gas detecting tape
JPS6380830A (en) * 1986-09-25 1988-04-11 Osaka Oxygen Ind Ltd Exhaust gas treatment agent in semiconductor industry
JPH03137917A (en) * 1989-10-24 1991-06-12 Iwatani Internatl Corp Dry treatment of hydride type waste gas

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008020343A (en) * 2006-07-13 2008-01-31 Japan Pionics Co Ltd Agent for detecting germane and organic silicon compound

Also Published As

Publication number Publication date
WO2003060510A1 (en) 2003-07-24
JP3895604B2 (en) 2007-03-22
TW200302348A (en) 2003-08-01

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