JP2001153760A - Conveying sample container - Google Patents
Conveying sample containerInfo
- Publication number
- JP2001153760A JP2001153760A JP34002799A JP34002799A JP2001153760A JP 2001153760 A JP2001153760 A JP 2001153760A JP 34002799 A JP34002799 A JP 34002799A JP 34002799 A JP34002799 A JP 34002799A JP 2001153760 A JP2001153760 A JP 2001153760A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- chamber
- lid
- glove box
- analysis
- 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.)
- Pending
Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、真空環境で分析を
行なう分析装置に係わり、特に、特定な環境を保持した
まま、試料を分析室に導入することが出来る搬送用試料
容器に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an analyzer for performing analysis in a vacuum environment, and more particularly to a transport sample container capable of introducing a sample into an analysis chamber while maintaining a specific environment.
【０００２】[0002]
【従来の技術】固体表面を真空環境で、電子やイオン又
はＸ線で励起し、その表面から得られる２次電子、回折
電子、散乱電子、オージェ電子、反射イオン、および、
特性Ｘ線や光電子等の信号を検出することによって、固
体表面にどのような元素が存在し、またどのような化学
結合状態にあるかを知ることができる。この表面分析の
手法を用いた装置として代表的なものに、走査電子顕微
鏡（ＳＥＭ）、Ｘ線マイクロアナライザ（ＥＰＭＡ、Ｘ
ＭＡ）、２次イオン質量分析装置（ＳＩＭＳ）、Ｘ線光
電子分光分析装置（ＸＰＳ、ＥＳＣＡ）等がある。2. Description of the Related Art A solid surface is excited by electrons, ions or X-rays in a vacuum environment, and secondary electrons, diffracted electrons, scattered electrons, Auger electrons, reflected ions, and the like are obtained from the surface.
By detecting signals such as characteristic X-rays and photoelectrons, it is possible to know what elements are present on the solid surface and what kind of chemical bonds are present. Representative devices using this surface analysis method include a scanning electron microscope (SEM) and an X-ray microanalyzer (EPMA, XMA).
MA), secondary ion mass spectrometer (SIMS), X-ray photoelectron spectroscopy (XPS, ESCA) and the like.
【０００３】これらの装置は、基礎研究用の分析のみな
らず、資源、エネルギー、公害などの検査、品質管理の
広い分野に使用され、特に、金属固溶体の相、変態、粒
界、析出物、介在物、地質鉱物の岩石、鉱石、隕石、セ
ラミックス、セメント、ガラス、化学の触媒、塗料、プ
ラスチック、ゴム、石油、生物医学の歯、骨、組織、
葉、根、半導体材料、集積回路等の広い分野の非破壊微
小領域元素分析、観察などに用いられる。これらの試料
の中には、長時間大気中に放置すると、空気中の酸素や
水分と反応して変質するものもあり、その他環境による
コンタミネーションを防止するために、測定する採取し
た試料を、大気と隔離する試料ケース等に保存し、不活
性ガス中や真空中に保管する場合もある。[0003] These devices are used not only in analysis for basic research but also in a wide range of fields such as inspection of resources, energy and pollution, and quality control. In particular, phases, transformations, grain boundaries, precipitates, and the like of metal solid solutions are used. Inclusions, geological mineral rocks, ores, meteorites, ceramics, cement, glass, chemical catalysts, paints, plastics, rubber, petroleum, biomedical teeth, bones, tissues,
It is used for nondestructive micro area elemental analysis and observation in a wide range of fields such as leaves, roots, semiconductor materials, and integrated circuits. Some of these samples, if left in the air for a long time, react with oxygen and moisture in the air and deteriorate, and in order to prevent contamination due to the environment, the collected sample to be measured must be It may be stored in a sample case or the like that is isolated from the atmosphere, and may be stored in an inert gas or vacuum.
【０００４】図６は、従来の表面分析装置の試料導入系
統の平面図を示す。この装置の試料導入系統は、グロー
ブボックス４２と試料導入室３８と分析室１４から構成
されており、各部はゲートバルブ４４及びゲートバルブ
１３で連結されている。グローブボックス４２は、透明
なケースで出来ており、前方にグローブ２９が２つ取り
つけられ内部のものを見ながらグローブ２９で取り扱う
ことが出来る。後方に試料２２や試料台１１などを出し
入れでき、密閉出来るように扉４３が設けられている。
まず、扉４３を開放し、試料台１１と、採取された試料
２２をグローブボックス４２内に置く。そして、グロー
ブ２９で操作して、試料台１１に試料２２をセットす
る。ゲートバルブ４４を開放にし、導入棒４１を前に押
すことで、試料２２を試料導入室３８に送りこむことが
できる。グローブボックス４２内は、バルブ３２を介し
て不活性ガス３３を内部に送り込むことができ、余剰の
不要なガスをバルブ３０を介してポンプで引くこともで
きる。従って、試料２２を大気から分離して、不活性ガ
ス３３中で試料台１１に試料２２をセットまたは充填処
理することが出来る。FIG. 6 is a plan view of a sample introduction system of a conventional surface analyzer. The sample introduction system of this apparatus is composed of a glove box 42, a sample introduction chamber 38, and an analysis chamber 14, and each part is connected by a gate valve 44 and a gate valve 13. The glove box 42 is made of a transparent case, and two gloves 29 are attached to the front, so that the glove 29 can be handled while looking at the inside. A door 43 is provided so that the sample 22 and the sample table 11 can be taken in and out from the rear, and can be sealed.
First, the door 43 is opened, and the sample stand 11 and the collected sample 22 are placed in the glove box 42. Then, the sample 22 is set on the sample stage 11 by operating the glove 29. The sample 22 can be sent to the sample introduction chamber 38 by opening the gate valve 44 and pushing the introduction rod 41 forward. The inert gas 33 can be fed into the glove box 42 through the valve 32, and excess unnecessary gas can be pumped through the valve 30. Therefore, the sample 22 can be separated from the atmosphere and set or filled on the sample stage 11 in the inert gas 33.
【０００５】試料導入室３８は、グローブボックス４２
から測定する試料が送り込まれる。そして、ゲートバル
ブ４４を閉め、バルブ３９を介してポンプ４０で粗引き
排気を行なう。従って、この試料導入室３８は、真空に
常時保たれており、ここからゲートバルブ１３を開放に
して、導入棒３７で試料２２がセットされた試料台１１
ごと分析室１４の所定の位置まで送り込まれる。導入棒
３７を引いてゲートバルブ１３を閉める。[0005] The sample introduction chamber 38 includes a glove box 42.
The sample to be measured is sent from. Then, the gate valve 44 is closed, and the pump 40 performs the rough evacuation through the valve 39. Therefore, the sample introduction chamber 38 is always kept in a vacuum, and the gate valve 13 is opened from here, and the sample stage 11 on which the sample 22 is set by the introduction rod 37 is opened.
Is sent to a predetermined position in the analysis chamber 14. The introduction valve 37 is pulled to close the gate valve 13.
【０００６】分析室１４は、バルブ１９を介してポンプ
１８で粗引き真空にされ、バルブ２１を介してポンプ２
０で高真空に排気され、内部に電子銃と、試料からの２
次電子などを検知する検出器等を備えている。試料導入
室３８とはゲートバルブ１３で隔離され、常時高真空に
保たれている。分析終了後は、バルブ１９、バルブ２１
を閉じ、ゲートバルブ１３を開放にして、導入棒３７に
より分析室１４の試料２２を試料導入室３８に戻す。ゲ
ートバルブ１３を閉め、ゲートバルブ４４を開放にし、
導入棒４１で試料導入室３８の試料２２をグローブボッ
クス４２に戻し、ゲートバルブ４４を閉じる。そして、
扉４３を開放にし、試料台１１ごと外部に取り出す。The analysis chamber 14 is roughly evacuated to a vacuum by a pump 18 via a valve 19, and the pump 2 is
0, it is evacuated to a high vacuum, and an electron gun and 2
It has a detector for detecting the next electron and the like. It is isolated from the sample introduction chamber 38 by the gate valve 13 and is always kept at a high vacuum. After the analysis, the valve 19, the valve 21
Is closed, the gate valve 13 is opened, and the sample 22 in the analysis chamber 14 is returned to the sample introduction chamber 38 by the introduction rod 37. Close the gate valve 13 and open the gate valve 44,
The sample 22 in the sample introduction chamber 38 is returned to the glove box 42 with the introduction rod 41, and the gate valve 44 is closed. And
The door 43 is opened, and the whole sample table 11 is taken out.
【０００７】[0007]
【発明が解決しようとする課題】従来の試料導入系統は
以上のように構成されているが、試料２２の酸化防止の
ために、グローブボックス４２と試料導入室３８が連結
された構造に作られているので、分析装置全体が大きく
なる。また、グローブボックス４２が取りつかない標準
の分析装置の場合、改造部分が多くなる。さらに、グロ
ーブボックス４２が取りつけられていることによって除
振性能が低下し、高倍率像による観察が困難になるとい
う問題がある。The conventional sample introduction system is constructed as described above. However, in order to prevent the sample 22 from being oxidized, the glove box 42 and the sample introduction chamber 38 are connected to each other. Therefore, the entire analyzer becomes large. In the case of a standard analyzer in which the glove box 42 cannot be mounted, the number of remodeled parts increases. Further, there is a problem that the anti-vibration performance is reduced due to the attachment of the glove box 42, and observation with a high-magnification image becomes difficult.
【０００８】本発明は、このような事情に鑑みてなされ
たものであって、分析試料が環境によって変質しないよ
うにして、分析装置全体の寸法を大きくすることなく、
改造部分を少なくし、除振性能を向上し、高倍率像によ
る観察が容易に出来る搬送用試料容器を提供することを
目的とする。The present invention has been made in view of the above circumstances, and is intended to prevent the analysis sample from being deteriorated by the environment and to increase the size of the entire analysis apparatus.
It is an object of the present invention to provide a transport sample container that can reduce the number of remodeled portions, improve vibration isolation performance, and facilitate observation with a high-magnification image.
【０００９】[0009]
【課題を解決するための手段】上記の目的を達成するた
め請求項１の発明の搬送用試料容器は、分析用試料を保
持する試料ホルダと、その試料ホルダに被せられ分析試
料を大気と隔離して密閉し試料ホルダを内置する試料導
入室の外部から操作して開閉もしくは着脱可能な試料蓋
と、その試料蓋または試料ホルダにリリーフ弁とを備え
るものである。According to a first aspect of the present invention, there is provided a transport sample container, comprising: a sample holder for holding an analysis sample; and a sample holder placed on the sample holder to isolate the analysis sample from the atmosphere. It is provided with a sample lid that can be opened and closed or detached by being operated from the outside of the sample introduction chamber in which the sample holder is placed and the sample holder is placed inside, and a relief valve provided on the sample lid or the sample holder.
【００１０】また、請求項２の発明の搬送用試料容器
は、分析用試料を保持する試料ホルダと、その試料ホル
ダを大気と隔離する試料室ケースと、試料室ケースを内
置する試料導入室の外部から操作して試料室ケースに開
閉もしくは着脱可能な密閉できる試料蓋と、試料室ケー
ス内のガスを排気する排気口と、排気停止により閉じる
チェック弁とを備えるものである。[0010] According to a second aspect of the present invention, there is provided a transport sample container comprising a sample holder for holding an analysis sample, a sample chamber case for isolating the sample holder from the atmosphere, and a sample introduction chamber for housing the sample chamber case. It is provided with a sample lid that can be opened / closed to / from the sample chamber case by being operated from the outside and can be hermetically closed, an exhaust port for exhausting gas in the sample chamber case, and a check valve that closes when the exhaust is stopped.
【００１１】請求項１の発明の搬送用試料容器は上記の
ように構成されており、分析試料が試料ホルダにセット
され、その試料ホルダに気密性を保つことが出来る開閉
もしくは着脱可能な試料蓋が設けられ、大気と隔離する
ので試料の酸化などによる影響を受けることがない。そ
して、試料導入室の外部から試料蓋の開閉を操作できる
ので、従来のようにグローブボックスを試料導入室に連
結する必要がない。さらに、試料蓋にリリーフ弁が装着
されているので、外圧が高いときには、試料ホルダの内
部に、外部からガスが侵入することがない。一方、外圧
が低い時、例えば、試料ホルダの置かれている空間が真
空の時、自動的にリリーフ弁が働き内部が真空になる。
従って、試料が外部からのガスで汚染されることはな
い。The sample container for transport according to the first aspect of the present invention is configured as described above, and the sample to be analyzed is set in the sample holder, and the sample holder capable of maintaining airtightness in the sample holder can be opened and closed or detachable. And is isolated from the atmosphere, so that it is not affected by oxidation of the sample. Since the opening and closing of the sample lid can be operated from outside the sample introduction chamber, there is no need to connect the glove box to the sample introduction chamber as in the related art. Further, since the relief valve is mounted on the sample lid, when the external pressure is high, gas does not enter the inside of the sample holder from the outside. On the other hand, when the external pressure is low, for example, when the space where the sample holder is placed is in a vacuum, the relief valve automatically operates and the inside is evacuated.
Therefore, the sample is not contaminated by the gas from the outside.
【００１２】また、請求項２の発明の搬送用試料容器
は、試料を試料ホルダにセットし、それを試料室ケース
に収納し、その試料室ケースに気密性を保つことが出来
る開閉もしくは着脱可能な蓋が設けられ、大気と隔離す
るので試料の酸化などによる影響を受けることがない。
そして、試料導入室の外部から試料室ケースの蓋の開閉
を操作できるので、従来のようにグローブボックスを試
料導入室に連結する必要がない。さらに、試料室ケース
に排気口とチェック弁が装着されているので、試料室ケ
ース内を外気より負圧にすることが出来、チェック弁に
よって外圧が高いときには、試料室ケースの内部に、外
部からガスが侵入することがない。一方、外圧が低い
時、例えば、試料室ケースの置かれている空間が真空の
時、自動的にチェック弁が働き内部が真空になる。従っ
て、試料が外部からのガスで汚染されることはない。The sample container for transfer according to the second aspect of the present invention is capable of setting a sample in a sample holder, storing the sample in a sample chamber case, and opening and closing or detaching the sample chamber case so as to maintain airtightness. Since the lid is provided and isolated from the atmosphere, it is not affected by oxidation of the sample.
Since the lid of the sample chamber case can be opened and closed from the outside of the sample introduction chamber, there is no need to connect the glove box to the sample introduction chamber as in the related art. Furthermore, since the sample chamber case is equipped with an exhaust port and a check valve, the inside of the sample chamber case can be set to a lower pressure than the outside air. No gas enters. On the other hand, when the external pressure is low, for example, when the space in which the sample chamber case is placed is vacuum, the check valve automatically operates and the inside becomes vacuum. Therefore, the sample is not contaminated by the gas from the outside.
【００１３】したがって、分析試料ホルダもしくは試料
室ケースに、特定環境を保持する機構を設けて、グロー
ブボックスを試料導入室に連結せずに、分析装置全体の
寸法を大きくすることなく、改造部分を少なくし、除振
性能を向上し、高倍率像による観察が容易に出来る。Therefore, a mechanism for maintaining a specific environment is provided in the analysis sample holder or the sample chamber case, so that the glove box is not connected to the sample introduction chamber, and the remodeled portion can be formed without increasing the size of the entire analyzer. The vibration reduction performance is improved, and observation with a high-magnification image can be easily performed.
【００１４】[0014]
【発明の実施の形態】本発明の搬送用試料容器の一実施
の形態を、図１、図２を参照しながら説明する。図１
は、本発明の搬送用試料容器３の分析室１４への搬送系
統を示す図である。図２は本発明の搬送用試料容器を示
す図である。本搬送用試料容器は、試料２２を処理して
セットする試料台１１と、試料２２の上方から試料台１
１に被せる気密性の機構を有し上面に着脱ネジ２６を備
えた蓋１０と、蓋１０に設けられ内部の圧力より外圧が
高いときにガスが内部に流入しないような機能を持つリ
リーフ弁２５と、内外の気密性を保つためのＯリング２
３、２４と、試料台１１を装着する基台６とから構成さ
れている。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS One embodiment of the transport sample container of the present invention will be described with reference to FIGS. FIG.
FIG. 3 is a view showing a transfer system of the transfer sample container 3 to the analysis chamber 14 according to the present invention. FIG. 2 is a view showing a transport sample container of the present invention. The transport sample container includes a sample stage 11 for processing and setting the sample 22 and a sample stage 1 from above the sample 22.
1, a lid 10 having an airtight mechanism and a detachable screw 26 on the upper surface, and a relief valve 25 provided on the lid 10 and having a function of preventing gas from flowing into the inside when the external pressure is higher than the internal pressure. And O-ring 2 to keep airtight inside and outside
3 and 24, and the base 6 on which the sample stage 11 is mounted.
【００１５】試料台１１は、下部に平板、上部にリング
状の枠からなるステンレス等の材料が使われる。試料２
２が充填される内径は約３２ｍｍ、深さ約２０ｍｍの円
筒状である（試料サイズ）。従って、分析領域は３２ｍ
ｍφの全面を使用することが出来る。リング状の枠外周
には、Ｏリング２３が嵌めこまれる溝が加工されてい
る。The sample stage 11 is made of a material such as stainless steel having a flat plate at the bottom and a ring-shaped frame at the top. Sample 2
2 has a cylindrical shape with an inner diameter of about 32 mm and a depth of about 20 mm (sample size). Therefore, the analysis area is 32m
The entire surface of mφ can be used. A groove into which the O-ring 23 is fitted is formed on the outer periphery of the ring-shaped frame.
【００１６】蓋１０は、円盤状のステンレス材で出来て
おり、上面に着脱用のネジが挿入される着脱ネジ２６が
設けられ、試料導入室７のつまみ１２によって着脱操作
が行なわれる。下面内部にＯリング２３が嵌めこまれる
溝が加工されている。また、内外のガス圧に応じて動作
するリリーフ弁２５が設けられている。リリーフ弁２５
は、蓋１０に設けられ内部の圧力より外圧が高いときに
ガスが内部に流入しないような機能を持つ。従って、外
圧が高いときには、試料台１１の内部に、外部からガス
が侵入することがない。一方、外圧が低い時、例えば、
試料台１１が置かれている空間が真空の時、自動的にリ
リーフ弁２５が働き内部が真空になる。従って、試料が
外部からのガスで汚染されることはない。The lid 10 is made of a disc-shaped stainless steel material, and is provided with a detachable screw 26 on the upper surface of which a detachable screw is inserted. The detachable operation is performed by the knob 12 of the sample introduction chamber 7. A groove into which the O-ring 23 is fitted is machined inside the lower surface. Further, a relief valve 25 that operates according to the internal and external gas pressures is provided. Relief valve 25
Is provided on the lid 10 and has a function of preventing gas from flowing into the inside when the external pressure is higher than the internal pressure. Therefore, when the external pressure is high, gas does not enter the sample stage 11 from the outside. On the other hand, when the external pressure is low, for example,
When the space in which the sample stage 11 is placed is in a vacuum, the relief valve 25 automatically operates and the inside is evacuated. Therefore, the sample is not contaminated by the gas from the outside.
【００１７】基台６は、試料台１１を装着し、図１に示
すフランジ２の台４に載せられ、試料導入室７で蓋１０
を上部に取り外し、導入棒１により、分析室１４内のガ
イド１７上の所定の位置に移動されセットされる。The base 6 has a sample stage 11 mounted thereon and is mounted on the stage 4 of the flange 2 shown in FIG.
Is moved to a predetermined position on the guide 17 in the analysis chamber 14 by the introduction rod 1 and set.
【００１８】次に、本搬送用試料容器３の操作の方法を
説明する。試料導入系統として、図３に示すグローブボ
ックス２７が分析装置と独立して配置され、ここで試料
２２が試料台１１に充填され、搬送用試料容器３内に試
料２２が保管される。その後図１に示す試料導入系統で
搬送用試料容器３が搬送され、分析室１４に導入され
る。Next, a method of operating the transport sample container 3 will be described. As a sample introduction system, a glove box 27 shown in FIG. 3 is arranged independently of the analyzer, where the sample 22 is filled in the sample table 11 and the sample 22 is stored in the transport sample container 3. Thereafter, the transport sample container 3 is transported by the sample introduction system shown in FIG.
【００１９】グローブボックス２７は、透明なケースで
出来ており前方にグローブ２９が２つ取りつけられ、内
部のものを見ながらグローブ２９で取り扱うことが出来
る。後方に試料２２や試料台１１などを出し入れでき、
密閉出来るように扉３４が設けられている。まず、扉３
４を開放し、試料台１１と、採取された試料２２をグロ
ーブボックス２７内に置く。グローブボックス２７内
は、バルブ３２を介して不活性ガス３３を内部に送り込
むことができ、余剰の不要なガスをバルブ３０を介して
ポンプ３１で引くこともできる。従って試料２２を大気
から分離して、不活性ガス３３中で、試料２２を試料台
１１にセットすることが出来る。従って、グローブボッ
クス２７内を不活性ガス３３に置換して、グローブ２９
で操作して試料２２の処理を行ない、試料台１１に処理
された試料２２をセットする。セットが完了すれば、蓋
１０を上部から被せ、Ｏリング２３によって試料２２の
内部を気密にする。そして、扉３４を開けてグローブボ
ックス２７から外部に試料２２の入った試料台１１を取
り出す。次に、図１に示すフランジ２に設けられた台４
上に、基台６がセットされているので、この上部に試料
台１１を取りつける。The glove box 27 is made of a transparent case. Two gloves 29 are attached to the front of the glove box 27. The glove box 27 can be handled with the glove 29 while looking at the inside. The sample 22 and the sample stage 11 can be taken in and out behind,
A door 34 is provided so as to be able to be sealed. First, door 3
4 is opened, and the sample table 11 and the collected sample 22 are placed in the glove box 27. In the glove box 27, an inert gas 33 can be sent into the inside via a valve 32, and excess unnecessary gas can be drawn by a pump 31 via a valve 30. Therefore, the sample 22 can be set on the sample stage 11 in the inert gas 33 by separating the sample 22 from the atmosphere. Therefore, the inside of the glove box 27 is replaced with the inert gas 33 and the glove 29 is replaced.
To process the sample 22, and set the processed sample 22 on the sample stage 11. When the setting is completed, the lid 10 is put on from above, and the inside of the sample 22 is made airtight by the O-ring 23. Then, the door 34 is opened and the sample table 11 containing the sample 22 is taken out from the glove box 27 to the outside. Next, a table 4 provided on the flange 2 shown in FIG.
Since the base 6 is set on the upper part, the sample base 11 is mounted on the base 6.
【００２０】そして、フランジ２とフランジ５を合わせ
る。これにより、試料導入室７に搬送用試料容器３がセ
ットされ、図４に示す状態になる。搬送用試料容器３が
大気中にあるときは、リリーフ弁２５がばねによって弁
が閉じており、ガスは、容器外に出ることはない。試料
導入室７をバルブ９を介してポンプ８で真空に引き始め
ると、試料導入室７の圧力が搬送用試料容器３内の圧力
よりも低くなるので、搬送用試料容器３内のガスは同時
に排気される。最終的に試料導入室７の圧力とほぼ同じ
になる。この状態でつまみ１２の先端についている着脱
雄ネジ３６を蓋１０の着脱ネジ２６に入れて、蓋１０を
上方に取り外す。そして、ゲートバルブ１３を開放に
し、導入棒１を押しこみ、試料台１１を分析室１４のガ
イド１７上を移動させ所定の位置に送り込む。導入棒１
を元の位置に引きこみ、ゲートバルブ１３を閉じる。分
析室１４は常時バルブ２１を介してポンプ２０によって
高真空にされており、電子銃１５から電子を試料２２の
表面に当てる。その励起された表面からの２次電子やイ
オン、特性Ｘ線などを各種検出器１６で検知してその信
号を処理し、表面の元素や化学結合状態を解明する。Then, the flange 2 and the flange 5 are combined. Thereby, the transport sample container 3 is set in the sample introduction chamber 7, and the state shown in FIG. 4 is obtained. When the transport sample container 3 is in the atmosphere, the relief valve 25 is closed by a spring, and gas does not go out of the container. When the sample introduction chamber 7 starts to be evacuated by the pump 8 via the valve 9, the pressure in the sample introduction chamber 7 becomes lower than the pressure in the transfer sample container 3. Exhausted. Finally, the pressure becomes almost the same as the pressure in the sample introduction chamber 7. In this state, the detachable male screw 36 attached to the tip of the knob 12 is inserted into the detachable screw 26 of the lid 10, and the lid 10 is removed upward. Then, the gate valve 13 is opened, the introduction rod 1 is pushed in, and the sample table 11 is moved on the guide 17 of the analysis chamber 14 and sent to a predetermined position. Introduction rod 1
To the original position, and the gate valve 13 is closed. The analysis chamber 14 is kept in a high vacuum state by a pump 20 via a valve 21 at all times, and an electron gun 15 applies electrons to the surface of a sample 22. Secondary detectors and ions, characteristic X-rays, and the like from the excited surface are detected by various detectors 16 and their signals are processed to elucidate surface elements and chemical bonding states.
【００２１】分析が終了すれば、試料２２をこれまでの
導入過程の逆の手順で取り出す。ゲートバルブ１３を開
け、導入棒１で試料台１１を試料導入室７に引きこむ。
ゲートバルブ１３を閉め、つまみ１２で蓋１０を下方に
下ろし試料台１１に被せる。そして、バルブ９を閉じ
て、試料導入室７をリークさせる。リークさせて大気圧
にしても、搬送用試料容器３内の圧力は真空の状態であ
る。そして、フランジ２をフランジ５から離し、搬送用
試料容器３を外部に取り出す。その搬送用試料容器３を
グローブボックス２７に再び入れて、不活性ガス雰囲気
中でリリーフ弁２５を開放する方法で蓋１０を開け、内
部の分析の完了した試料２２を取り出す。When the analysis is completed, the sample 22 is taken out in the reverse order of the introduction process. The gate valve 13 is opened, and the sample table 11 is pulled into the sample introduction chamber 7 with the introduction rod 1.
The gate valve 13 is closed, and the lid 10 is lowered with the knob 12 to cover the sample table 11. Then, the valve 9 is closed to leak the sample introduction chamber 7. Even if the pressure is leaked to atmospheric pressure, the pressure in the transport sample container 3 is in a vacuum state. Then, the flange 2 is separated from the flange 5, and the transport sample container 3 is taken out. The transport sample container 3 is put into the glove box 27 again, the lid 10 is opened by a method of opening the relief valve 25 in an inert gas atmosphere, and the sample 22 whose internal analysis has been completed is taken out.
【００２２】次に、本発明の搬送用試料容器の他の実施
例について説明する。図５は本搬送用試料容器３が試料
導入室５８に導入された状態を示す外観図（Ａ）と断面
図（Ｂ）である。本搬送用試料容器３は、試料５４を充
填する試料ホルダ５０と、その試料ホルダ５０を収容す
る試料室ケース４９と、その試料室ケース４９の上面に
Ｏリングを備えフランジを有した蓋４８と、試料室ケー
ス４９の側部に、シリコンチューブ５３を連結して、そ
の先に内部の圧力より外圧が高いときにガスが内部に流
入しないような機能を持つチェック弁５２と、試料室ケ
ース４９内を排気する排気口５１と、試料室ケース４９
と排気口５１とチェック弁５２を装着する基台５５とか
ら構成されている。Next, another embodiment of the transport sample container of the present invention will be described. 5A and 5B are an external view (A) and a cross-sectional view (B) showing a state in which the main transport sample container 3 is introduced into the sample introduction chamber 58. The transport sample container 3 includes a sample holder 50 for filling a sample 54, a sample chamber case 49 for accommodating the sample holder 50, a lid 48 having an O-ring on the upper surface of the sample chamber case 49 and having a flange. A check valve 52 having a function of preventing a gas from flowing into the inside of a silicon tube 53 connected to a side portion of the sample chamber case 49 when the external pressure is higher than the internal pressure; An exhaust port 51 for exhausting the inside, and a sample chamber case 49
And a base 55 on which a check valve 52 is mounted.
【００２３】本搬送用試料容器３は、蓋４８が試料室ケ
ース４９に取りつけられる構造である。そして、蓋４８
の取り外し機構は、試料導入室５８の側面に設けられた
蓋操作レバー４５を回転することで、蓋開放金具４７が
上下する。この上下動作により蓋４８が上方に持ち上げ
られ、開放される。試料室ケース４９内の圧力と外圧の
関係は、まず、試料５４が試料ホルダ５０にセットさ
れ、その試料ホルダ５０が試料室ケース４９内に収容さ
れ、蓋４８が閉じられた状態で、排気口から内部のガス
が排気される。排気を止めれば、外圧が高いので、チェ
ック弁５２が働き大気のガスが内部に侵入することが出
来ない。その他に付いては前記の実施例と同様の原理で
取り扱いされる。The transport sample container 3 has a structure in which a lid 48 is attached to a sample chamber case 49. And the lid 48
The mechanism for removing the cover opening lever 47 is moved up and down by rotating the cover operation lever 45 provided on the side surface of the sample introduction chamber 58. The lid 48 is lifted upward by this vertical movement and is opened. The relationship between the pressure in the sample chamber case 49 and the external pressure is as follows. First, the sample 54 is set in the sample holder 50, the sample holder 50 is housed in the sample chamber case 49, and the exhaust port is closed. The gas inside is exhausted from. When the evacuation is stopped, the external pressure is high, so that the check valve 52 operates to prevent atmospheric gas from entering the inside. Others are handled according to the same principle as in the above embodiment.
【００２４】次に、この搬送用試料容器３の試料導入手
順を説明する。まず、シリコンチューブ５３を試料室ケ
ース４９側で取り外し、蓋４８、試料室ケース４９をネ
ジを緩めて取り外す。そして図３に示すグローブボック
ス２７中で、試料ホルダ５０に試料５４を充填する。そ
して、試料室ケース４９を被せ、ネジで固定する。次に
シリコンチューブ５３を接続し、蓋４８を被せる。次に
排気口５１に排気用の吸引器を取りつけ試料室ケース４
９内を排気する。そして、搬送用試料容器３を試料導入
室５８に図５に示すように取りつける。試料導入室５８
を排気し、蓋操作レバー４５を操作して蓋４８を持ち上
げる。試料導入室５８の排気が完了すると図１に示すゲ
ートバルブを１３開け、搬送用試料容器３を分析室１４
の所定の位置に送り込む。ゲートバルブ１３を閉め、分
析を行なう。分析完了後、搬送用試料容器３を同様の手
順で試料導入室５８に戻す。そして蓋４８を閉め、試料
導入室５８をリークさせ大気圧にする。この時、試料室
ケース４９内は真空に保持される。そして、外部に搬送
用試料容器３を取りだし、グローブボックス２７内でシ
リコーンチューブ５３を外し試料室ケース４９内をリー
クさせる。蓋４８、試料室ケース４９を取り外し、試料
４８を交換する。Next, a procedure for introducing a sample into the transport sample container 3 will be described. First, the silicon tube 53 is removed on the sample chamber case 49 side, and the lid 48 and the sample chamber case 49 are loosened and removed. Then, the sample 54 is filled in the sample holder 50 in the glove box 27 shown in FIG. Then, the sample chamber case 49 is covered and fixed with screws. Next, the silicon tube 53 is connected, and the lid 48 is covered. Next, an exhaust suction unit is attached to the exhaust port 51, and the sample chamber case 4
The inside of 9 is exhausted. Then, the transport sample container 3 is attached to the sample introduction chamber 58 as shown in FIG. Sample introduction chamber 58
Is exhausted, and the lid operation lever 45 is operated to lift the lid 48. When the evacuation of the sample introduction chamber 58 is completed, the gate valve 13 shown in FIG.
To a predetermined position. The analysis is performed by closing the gate valve 13. After the analysis is completed, the transport sample container 3 is returned to the sample introduction chamber 58 in the same procedure. Then, the lid 48 is closed to leak the sample introduction chamber 58 to atmospheric pressure. At this time, the inside of the sample chamber case 49 is kept in a vacuum. Then, the transport sample container 3 is taken out, and the silicone tube 53 is removed in the glove box 27 to leak the sample chamber case 49. The lid 48 and the sample chamber case 49 are removed, and the sample 48 is replaced.
【００２５】[0025]
【発明の効果】本発明の搬送用試料容器は上記のように
構成されており、気密性を保つことが出来る開閉もしく
は着脱可能な試料蓋が設けられた試料ホルダ、又は試料
室ケースに、分析試料が充填されるので、環境などによ
る試料の酸化や変質などの影響を受けることがない。The transport sample container of the present invention is constructed as described above, and is provided with a sample holder or a sample chamber case provided with an openable / detachable sample lid capable of maintaining airtightness. Since the sample is filled, the sample is not affected by oxidation or alteration of the sample due to the environment or the like.
【００２６】そして、試料導入室の外部から試料蓋の開
閉を操作できるので、グローブボックスを単独で使用し
て、分析装置をコンパクトに構成することが出来る。さ
らに、試料蓋にリリーフ弁が、もしくは試料室ケースに
排気口とチェック弁が装着されているので、外圧が高い
ときには、試料ホルダの内部に、外部からガスが侵入す
ることがない。一方、外圧が低い時、例えば、試料ホル
ダの置かれている空間が真空の時、自動的にリリーフ
弁、もしくはチェック弁が働き内部が真空になる。従っ
て、試料が外部からのガスで汚染されることはない。Since the opening and closing of the sample lid can be operated from outside the sample introduction chamber, the analyzer can be made compact by using the glove box alone. Furthermore, since a relief valve is mounted on the sample lid or an exhaust port and a check valve are mounted on the sample chamber case, when the external pressure is high, gas does not enter the sample holder from the outside. On the other hand, when the external pressure is low, for example, when the space in which the sample holder is placed is in a vacuum, the relief valve or the check valve is automatically activated to evacuate the inside. Therefore, the sample is not contaminated by the gas from the outside.
【００２７】このように特定環境を保持する機構を設け
て、グローブボックスを単独で使用することができ、分
析装置全体がコンパクトになる。そして、改造部分を少
なくして、グローブボックスを連結しないので除振性能
が向上し、高倍率像による観察を容易にすることが出来
る。By providing a mechanism for maintaining a specific environment as described above, the glove box can be used alone, and the entire analyzer becomes compact. Since the modified portion is reduced and the glove box is not connected, the vibration isolation performance is improved, and observation with a high-magnification image can be facilitated.
【図１】 本発明の搬送用試料容器の一実施例を示す図
である。FIG. 1 is a view showing one embodiment of a transport sample container of the present invention.
【図２】 本発明の搬送用試料容器を示す図である。FIG. 2 is a view showing a transport sample container of the present invention.
【図３】 本発明の搬送用試料容器のグローブボックス
内の操作を説明するための図である。FIG. 3 is a view for explaining an operation of the sample container for transport of the present invention in a glove box.
【図４】 本発明の搬送用試料容器を試料導入室に導入
する操作を説明するための図である。FIG. 4 is a view for explaining an operation of introducing the transport sample container of the present invention into a sample introduction chamber.
【図５】 本発明の搬送用試料容器の他の実施例を示す
図である。FIG. 5 is a view showing another embodiment of the transport sample container of the present invention.
【図６】 従来の分析計における試料導入の手順を説明
するための図である。FIG. 6 is a diagram for explaining a procedure for introducing a sample in a conventional analyzer.
１…導入棒 ２…フランジ ３…搬送用試料容器 ４…台 ５…フランジ ６…基台 ７…試料導入室 ８…ポンプ ９…バルブ １０…蓋 １１…試料台 １２…つまみ １３…ゲートバルブ １４…分析室 １５…電子銃 １６…検出器 １７…ガイド １８…ポンプ １９…バルブ ２０…ポンプ ２１…バルブ ２２…試料 ２３…Ｏリング ２４…Ｏリング ２５…リリーフ弁 ２６…着脱ネジ ２７…グローブボックス ２８…圧力計 ２９…グローブ ３０…バルブ ３１…ポンプ ３２…バルブ ３３…不活性ガス ３４…扉 ３５…蓋着脱ユニット ３６…着脱雄ネジ ３７…導入棒 ３８…試料導入室 ３９…バルブ ４０…ポンプ ４１…導入棒 ４２…グローブボ
ックス ４３…扉 ４４…ゲートバル
ブ ４５…蓋操作レバー ４６…蓋開放位置 ４７…蓋開放金具 ４８…蓋 ４９…試料室ケース ５０…試料ホルダ ５１…排気口 ５２…チェック弁 ５３…シリコンチューブ ５４…試料 ５５…基台 ５６…台 ５７…ガイド ５８…試料導入室DESCRIPTION OF SYMBOLS 1 ... Introducing rod 2 ... Flange 3 ... Sample container for conveyance 4 ... Table 5 ... Flange 6 ... Base 7 ... Sample introduction chamber 8 ... Pump 9 ... Valve 10 ... Lid 11 ... Sample table 12 ... Knob 13 ... Gate valve 14 ... Analysis room 15 ... Electron gun 16 ... Detector 17 ... Guide 18 ... Pump 19 ... Valve 20 ... Pump 21 ... Valve 22 ... Sample 23 ... O-ring 24 ... O-ring 25 ... Relief valve 26 ... Removable screw 27 ... Glove box 28 ... Pressure gauge 29 ... Globe 30 ... Valve 31 ... Pump 32 ... Valve 33 ... Inert gas 34 ... Door 35 ... Lid detachable unit 36 ... Removable male screw 37 ... Introduction rod 38 ... Sample introduction chamber 39 ... Valve 40 ... Pump 41 ... Introduction Rod 42 ... Glove box 43 ... Door 44 ... Gate valve 45 ... Lid operating lever 46 ... Lid opening position 47 ... Lid opening fitting 48 ... Lid 49 ... Postal chamber case 50 ... sample holder 51 ... exhaust port 52 ... check valve 53 ... silicone tube 54 ... sample 55 ... base 56 ... base 57 ... Guide 58 ... sample supply chamber
フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｈ０１Ｌ 21/68 Ｈ０１Ｌ 21/68 Ｔ Ｆターム(参考） 2G001 AA03 BA05 BA07 CA03 GA01 JA12 JA14 KA01 KA12 PA01 PA06 PA07 PA11 PA30 QA02 4M106 AA20 DJ31 5C001 AA01 AA08 CC05 DD01 5F031 EA12 EA14 EA20 MA33 NA05 NA09 Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat II (Reference) H01L 21/68 H01L 21/68 TF term (Reference) 2G001 AA03 BA05 BA07 CA03 GA01 JA12 JA14 KA01 KA12 PA01 PA06 PA07 PA11 PA30 QA02 4M106 AA20 DJ31 5C001 AA01 AA08 CC05 DD01 5F031 EA12 EA14 EA20 MA33 NA05 NA09
Claims (2)
試料ホルダに被せられ分析試料を大気と隔離して密閉し
試料ホルダを内置する試料導入室の外部から操作して開
閉もしくは着脱可能な試料蓋と、その試料蓋または試料
ホルダにリリーフ弁とを備えることを特徴とする搬送用
試料容器。1. A sample holder for holding a sample for analysis, and an analysis sample placed on the sample holder, which is isolated from the atmosphere and sealed, and which can be opened / closed or detached by operating from outside a sample introduction chamber in which the sample holder is placed. A transport sample container comprising a sample lid and a relief valve on the sample lid or the sample holder.
試料ホルダを大気と隔離する試料室ケースと、試料室ケ
ースを内置する試料導入室の外部から操作して試料室ケ
ースに開閉もしくは着脱可能な密閉できる試料蓋と、試
料室ケース内のガスを排気する排気口と、排気停止によ
り閉じるチェック弁とを備えることを特徴とする搬送用
試料容器。2. A sample holder for holding a sample for analysis, a sample chamber case for isolating the sample holder from the atmosphere, and a sample chamber case which is opened and closed or detached from the sample chamber by operating the sample chamber from outside. A transport sample container comprising: a sample lid capable of being hermetically sealed; an exhaust port for exhausting gas in the sample chamber case; and a check valve closed by stopping the exhaust.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34002799A JP2001153760A (en) | 1999-11-30 | 1999-11-30 | Conveying sample container |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34002799A JP2001153760A (en) | 1999-11-30 | 1999-11-30 | Conveying sample container |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2001153760A true JP2001153760A (en) | 2001-06-08 |
Family
ID=18333052
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34002799A Pending JP2001153760A (en) | 1999-11-30 | 1999-11-30 | Conveying sample container |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2001153760A (en) |
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008197109A (en) * | 2007-02-15 | 2008-08-28 | Samsung Electronics Co Ltd | Contamination analyzing apparatus, its method, and reticle washing system using it |
| JP2010038601A (en) * | 2008-08-01 | 2010-02-18 | Toyota Motor Corp | Analyzer |
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