JPH0136901B2 - - Google Patents
Info
- Publication number
- JPH0136901B2 JPH0136901B2 JP57208075A JP20807582A JPH0136901B2 JP H0136901 B2 JPH0136901 B2 JP H0136901B2 JP 57208075 A JP57208075 A JP 57208075A JP 20807582 A JP20807582 A JP 20807582A JP H0136901 B2 JPH0136901 B2 JP H0136901B2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- generating means
- ray generating
- housing
- cover member
- 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.)
- Expired
Links
- 238000002955 isolation Methods 0.000 claims description 4
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 238000011109 contamination Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/227—Measuring photoelectric effect, e.g. photoelectron emission microscopy [PEEM]
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Description
【発明の詳細な説明】
本発明はＸ線を励起源とし、試料から放出され
る光電子により試料の元素分析を行なう光電子分
光分析装置に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a photoelectron spectrometer that uses X-rays as an excitation source and performs elemental analysis of a sample using photoelectrons emitted from the sample.
従来のこの種の光電子分光分析装置には、第１
図に示すように、フイラメントb1、アノードc1、
電極d1等からなるＸ線発生手段a1を試料室e1内に
むき出しにしたいわゆる解放型のものが広く採用
されている。この様な従来のものにおいて、試料
室e1内を真空ポンプf1で分析可能な、たとえば
10-8Torr程度の真空度に真空引きした後、Ｘ線
発生手段a1を稼動させると、フイラメントb1の表
面やその近傍に吸着されたガスがフイラメントb1
で加熱されて多量に放出される。Ｘ線発生手段a1
に対しては何ら遮蔽物が設けられていないので、
上記放出されたガスは試料室e1内に拡散されてＸ
線発生手段a1に近接配置された試料g1の表面を容
易に汚染する。特に数10Åの極表面を分析する場
合には汚染の影響が大きく、分析精度が損なわれ
るという不具合を生じる。この不具合を改善する
ため、第２図に示すように、試料室e2に対して、
Ｘ線発生手段a2を収容する差動排気室h2を並設
し、両室e2，h2にそれぞれ真空ポンプf2，f3を連
設するとともに、両室e2，h2をバルブv2によつて
連通するようにしたものも試みられている。この
構造のものでは、Ｘ線発生手段a2が差動排気室h2
を構成する隔壁i2で覆われているので上述した不
具合は解消される。しかしながら試料室e2と差動
排気室h2とはそれぞれ別個に真空状態を保持する
必要があるので気密性のある構造とせねばなら
ず、また、真空ポンプf2，f3も各室e2，h2に設け
ねばならないため非常に高価なものとなる。さら
に、真空引きに際しては薄膜のＸ線窓ｊを破損し
ないよう両室e2，h2内の真空バランスを保たねば
ならない。このためにバルブv2の操作が新たに必
要となつて分析の操作が煩雑になるという問題が
ある。 This type of conventional photoelectron spectrometer has a first
As shown in the figure, filament b 1 , anode c 1 ,
A so-called open type in which the X-ray generating means a 1 consisting of the electrode d 1 etc. is exposed inside the sample chamber e 1 is widely used. In such conventional devices, the inside of the sample chamber e 1 can be analyzed using a vacuum pump f 1 , for example.
After evacuation to a degree of vacuum of about 10 -8 Torr, when the X-ray generating means a 1 is operated, the gas adsorbed on the surface of the filament b 1 and its vicinity is transferred to the filament b 1
is heated and released in large quantities. X-ray generation means a 1
Since no shield is provided for
The released gas is diffused into the sample chamber e1 and
This easily contaminates the surface of the sample g 1 placed close to the ray generating means a 1 . Particularly when analyzing the extreme surface of several tens of angstroms, the influence of contamination is large, resulting in problems such as loss of analysis accuracy. In order to improve this problem, as shown in Figure 2, for sample chamber e 2 ,
Differential pumping chambers h 2 accommodating the X-ray generating means a 2 are arranged side by side, vacuum pumps f 2 and f 3 are connected to both chambers e 2 and h 2 , respectively, and both chambers e 2 and h 2 are Attempts have also been made to provide communication via valve v2 . In this structure, the X-ray generating means a 2 is connected to the differential exhaust chamber h 2
Since it is covered with the partition wall i 2 that constitutes the partition wall i 2 , the above-mentioned problem is solved. However, since the sample chamber e 2 and the differential pumping chamber h 2 need to be maintained in a vacuum state separately, they must have an airtight structure, and the vacuum pumps f 2 and f 3 are also connected to each chamber e 2 . , h 2 , making it extremely expensive. Furthermore, during evacuation, the vacuum balance within both chambers e 2 and h 2 must be maintained so as not to damage the thin film X-ray window j. For this reason, there is a problem that the operation of valve v2 is newly required, making the analysis operation complicated.
本発明は上記の問題点に鑑みてなされたもので
あつて、Ｘ線発生手段の加熱にともなう試料表面
のガスによる汚染を防止するとともに安価で、か
つ排気の操作も容易な光電子分光分析装置を提供
することを目的とする。 The present invention has been made in view of the above-mentioned problems, and provides a photoelectron spectrometer that prevents gas contamination of the sample surface due to heating of the X-ray generating means, is inexpensive, and has easy exhaust operation. The purpose is to provide.
本発明は、上記の目的を達成するため、真空室
を構成するハウジング内には、試料配置用の試料
台と、前記試料にＸ線を照射するＸ線発生手段と
がそれぞれ設けられる一方、前記ハウジング内を
真空引きする真空ポンプを備えた光電子分光分析
装置において、次の構成を採る。 In order to achieve the above object, the present invention includes a sample stage for placing a sample and an X-ray generating means for irradiating the sample with X-rays, each of which is provided in a housing constituting a vacuum chamber. A photoelectron spectrometer equipped with a vacuum pump that evacuates the inside of the housing has the following configuration.
すなわち、本発明の光電子分光分析装置は、ハ
ウジング内に、前記Ｘ線発生手段を覆つて該Ｘ線
発生手段と試料台との間を隔離するカバー部材が
設けられ、このカバー部材の前記Ｘ線発生手段と
試料台との間に位置する隔離部には、前記Ｘ線発
生手段からのＸ線を試料に向けて透過させるＸ線
窓が形成され、また、このカバー部材からはパイ
プ部が延設され、このパイプ部の解放端はハウジ
ング内の前記真空ポンプに近接した位置に開口さ
れていることを特徴としている。 That is, in the photoelectron spectrometer of the present invention, a cover member is provided in the housing to cover the X-ray generating means and isolate between the X-ray generating means and the sample stage, and the X-ray of the cover member An X-ray window that transmits the X-rays from the X-ray generating means toward the sample is formed in the isolation section located between the generating means and the sample stage, and a pipe section extends from the cover member. The open end of this pipe portion is characterized in that it opens at a position in the housing adjacent to the vacuum pump.
以下、本発明の構成を第３図に示す実施例に基
づいて説明する。 Hereinafter, the configuration of the present invention will be explained based on the embodiment shown in FIG.
第３図は本発明の光電子分光分析装置１の断面
図である。同図において、１は光電子分光分析装
置の全体を示し、２は真空室、３はこの真空室２
を構成するハウジングで、このハウジング内３に
は、試料４の配置用の試料台５、試料４にＸ線を
照射するＸ線発生手段９および試料４からＸ線に
より励起されて放出される光電子を検出、分析す
る分析手段１０がそれぞれ収容されている。そし
て、上記のＸ線発生手段９は、フイラメント６、
電極７、ターゲツト８からなる。また、１１は真
空室２内を真空引きするため、ハウジング３内に
バルブ１２を介して連設された真空ポンプであ
る。 FIG. 3 is a sectional view of the photoelectron spectrometer 1 of the present invention. In the figure, 1 shows the entire photoelectron spectrometer, 2 is a vacuum chamber, and 3 is this vacuum chamber 2.
This housing 3 contains a sample stage 5 for placing the sample 4, an X-ray generating means 9 for irradiating the sample 4 with X-rays, and photoelectrons excited and emitted from the sample 4 by the X-rays. Analyzing means 10 for detecting and analyzing are housed in each case. The above-mentioned X-ray generating means 9 includes a filament 6,
It consists of an electrode 7 and a target 8. Further, reference numeral 11 denotes a vacuum pump that is connected to the housing 3 via a valve 12 in order to evacuate the inside of the vacuum chamber 2 .
さらに、上記のハウジング３内には、Ｘ線発生
手段９を覆つて該Ｘ線発生手段９と試料台５との
間を隔離するカバー部材１６が設けられている。
そして、このカバー部材１６のＸ線発生手段９と
試料台５との間を位置する隔離部１８には貫通穴
２２が形成されるとともに、この貫通穴２２を閉
鎖してＸ線発生手段９からのＸ線を試料４に向け
て透過させるアルミ箔等でできたＸ線窓２４が固
着されている。さらに、このカバー部材１６の下
部からはその下方に向かつてパイプ部２０が延設
されており、このパイプ部２０の解放端２６はハ
ウジング３内の真空ポンプ１１に近接した位置に
開口されている。 Furthermore, a cover member 16 is provided in the housing 3 to cover the X-ray generating means 9 and isolate the X-ray generating means 9 from the sample stage 5.
A through hole 22 is formed in the isolation part 18 of the cover member 16 located between the X-ray generating means 9 and the sample stage 5, and the through hole 22 is closed so that the X-ray generating means 9 can be isolated from the X-ray generating means 9. An X-ray window 24 made of aluminum foil or the like is fixed to the sample 4 and transmits the X-rays toward the sample 4. Further, a pipe section 20 extends downward from the lower part of the cover member 16, and an open end 26 of the pipe section 20 is opened at a position in the housing 3 close to the vacuum pump 11. .
したがつて、上記構成において、試料４の分析
に際しては、バルブ１２を開いて真空ポンプ１１
で真空室２内を真空引きすると、カバー部材１６
内も同時に真空引きされる。そして、所定の真空
度たとえば108Torr程度になつた時点でＸ線発生
手段９のフイラメント６を点灯する。これによ
り、フイラメント６およびその周辺に吸着してい
たガスは、フイラメント６に加熱されて放出され
る。その場合、放出ガスは、カバー部材１６によ
つて真空室２内への拡散が制限され、真空ポンプ
１１に吸引されて直ちにハウジング３外に排気さ
れる。すなわち、フイラメント６の点灯時点で
は、その真空度が既に有る程度高くなつているの
で大気中に比べると放出ガスの平均自由行程は大
きく、したがつて、ガスの真空室２内への拡散よ
りも真空ポンプ１１により吸引される方が優先さ
れることになる。 Therefore, in the above configuration, when analyzing the sample 4, the valve 12 is opened and the vacuum pump 11 is turned on.
When the inside of the vacuum chamber 2 is evacuated, the cover member 16
The inside is also vacuumed at the same time. Then, when the degree of vacuum reaches a predetermined degree, for example, about 10 8 Torr, the filament 6 of the X-ray generating means 9 is turned on. As a result, the gas adsorbed on the filament 6 and its surroundings is heated by the filament 6 and released. In that case, the released gas is restricted from diffusing into the vacuum chamber 2 by the cover member 16, is sucked into the vacuum pump 11, and is immediately exhausted to the outside of the housing 3. In other words, when the filament 6 is turned on, the degree of vacuum has already reached a certain level, so the mean free path of the emitted gas is larger than that in the atmosphere. Priority is given to the suction by the vacuum pump 11.
以上のように本発明によれば、試料室内にＸ線
発生手段を覆うカバー部材を設け、しかもその開
放端を真空ポンプに近接し、かつ、試料室内に開
口するようにしたのでＸ線発生手段のフイラメン
トの加熱による放出ガスによつて試料表面が汚染
されることが防止される。しかも、真空ポンプを
余分に設置する必要もなく、かつ、カバー部材も
気密性を必要としないので、機械的強度も要求さ
れず、薄肉のものが適用できる。従つて、安価な
費用で試料汚染が防止できる。さらに、排気に際
してのバルブ操作の煩雑さもないという実用上優
れた効果が発揮される。 As described above, according to the present invention, a cover member that covers the X-ray generating means is provided in the sample chamber, and the open end thereof is close to the vacuum pump and opens into the sample chamber, so that the X-ray generating means This prevents the surface of the sample from being contaminated by the gas emitted by the heating of the filament. Furthermore, there is no need to install an extra vacuum pump, and the cover member does not need to be airtight, so mechanical strength is not required, and a thin-walled cover member can be used. Therefore, sample contamination can be prevented at low cost. Furthermore, an excellent practical effect is achieved in that there is no need for complicated valve operations during exhaust.
第１図および第２図は従来の光電子分光分析装
置を示す断面図、第３図は本発明の光電子分光分
析装置の実施例を示す断面図である。
１…光電子分光分析装置、２…真空室、３…ハ
ウジング、４…試料、９…Ｘ線発生手段、１１…
真空ポンプ、１６…カバー部材、１６…隔離部、
２０…パイプ部、２４…Ｘ線窓、２６…解放端。
1 and 2 are cross-sectional views showing a conventional photoelectron spectrometer, and FIG. 3 is a cross-sectional view showing an embodiment of the photoelectron spectrometer of the present invention. DESCRIPTION OF SYMBOLS 1... Photoelectron spectrometer, 2... Vacuum chamber, 3... Housing, 4... Sample, 9... X-ray generation means, 11...
Vacuum pump, 16...cover member, 16...isolation part,
20...Pipe section, 24...X-ray window, 26...Open end.
Claims (1)
置用の試料台と、前記試料にＸ線を照射するＸ線
発生手段とがそれぞれ設けられる一方、前記ハウ
ジング内を真空引きする真空ポンプを備えた光電
子分光分析装置において、 前記ハウジング内には、前記Ｘ線発生手段を覆
つて該Ｘ線発生手段と試料台との間を隔離するカ
バー部材が設けられ、このカバー部材の前記Ｘ線
発生手段と試料台との間に位置する隔離部には、
前記Ｘ線発生手段からのＸ線を試料に向けて透過
させるＸ線窓が形成され、また、このカバー部材
からはパイプ部が延設され、このパイプ部の解放
端はハウジング内の前記真空ポンプに近接した位
置に開口されていることを特徴とする光電子分光
分析装置。[Scope of Claims] 1 A housing constituting a vacuum chamber is provided with a sample stage for placing a sample and an X-ray generating means for irradiating the sample with X-rays, while the housing is evacuated. In the photoelectron spectrometer equipped with a vacuum pump, a cover member is provided in the housing to cover the X-ray generating means and isolate between the X-ray generating means and the sample stage, and the cover member The isolation section located between the X-ray generating means and the sample stage includes:
An X-ray window is formed for transmitting X-rays from the X-ray generating means toward the sample, and a pipe section extends from the cover member, and the open end of the pipe section is connected to the vacuum pump in the housing. A photoelectron spectrometer characterized in that the aperture is located close to the .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57208075A JPS5997046A (en) | 1982-11-26 | 1982-11-26 | Photoelectronic spectroscopic analysis apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57208075A JPS5997046A (en) | 1982-11-26 | 1982-11-26 | Photoelectronic spectroscopic analysis apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5997046A JPS5997046A (en) | 1984-06-04 |
| JPH0136901B2 true JPH0136901B2 (en) | 1989-08-03 |
Family
ID=16550222
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57208075A Granted JPS5997046A (en) | 1982-11-26 | 1982-11-26 | Photoelectronic spectroscopic analysis apparatus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5997046A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0668474B2 (en) * | 1985-06-07 | 1994-08-31 | 日電アネルバ株式会社 | Photoelectron analyzer |
-
1982
- 1982-11-26 JP JP57208075A patent/JPS5997046A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5997046A (en) | 1984-06-04 |
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