JPS62276448A - Fast atomic bombardment type secondary ion mass spectrograph - Google Patents
Fast atomic bombardment type secondary ion mass spectrographInfo
- Publication number
- JPS62276448A JPS62276448A JP61119061A JP11906186A JPS62276448A JP S62276448 A JPS62276448 A JP S62276448A JP 61119061 A JP61119061 A JP 61119061A JP 11906186 A JP11906186 A JP 11906186A JP S62276448 A JPS62276448 A JP S62276448A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- specimen
- atomic beam
- secondary ions
- fast atomic
- 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
Links
- 150000002500 ions Chemical group 0.000 claims abstract description 41
- 238000004458 analytical method Methods 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract 2
- 239000013078 crystal Substances 0.000 description 6
- 238000004949 mass spectrometry Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 230000001678 irradiating effect Effects 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Description
【発明の詳細な説明】
３、発明の詳細な説明
［発明の目的］
（産業上の利用分野）
この発明は、固体試料の組成分析のための高速原子子ｉ
％！型二次イオン質呈分析泪に関する。Detailed Description of the Invention 3. Detailed Description of the Invention [Object of the Invention] (Field of Industrial Application)
%! Type secondary ion material analysis analysis.
（従来の技術）
分析試料を高速原子線で衝撃し、試料表面から放出する
二次イオンの質量分析を行うことによって、試料の組成
分析を行う高速原子→ｉ撃型二次イオン質吊分析計とし
て、従来は第２図に示すようなものが知られている。(Prior art) A high-speed atom → i bombardment type secondary ion material suspension analyzer that analyzes the composition of a sample by bombarding the analysis sample with a high-speed atomic beam and performing mass spectrometry on the secondary ions released from the sample surface. Conventionally, the one shown in FIG. 2 has been known.
この従来の二次イオン質量分析計は、高速原子線源１に
△１゛ガスを導入して、その内部で運動エネルギーが３
ｋｅＶ程度の八ｒの高速原子を生成さけ、これを高速
原子Ｐｉ１３として放出する。そしてディフレクタ−４
に通すことによって残留づるイオンを除去して純粋な高
速原子線３とし、これを試料ホルダー５の上の試料６に
照射する。そこで、試料６の表面が高速原子線３の衝撃
を受け、スパッターされて二次イオン７８放出する。そ
して、この二次イオン７をエネルギーフィルター８に通
して適切な運動エネルギーのものを選択し、買１分析計
９に導く。’＆ｔｆｆｉ分析計９は、この二次イオン７
の貿示分析を行い、試料６の組成を同定する。This conventional secondary ion mass spectrometer introduces △1゛ gas into the fast atomic beam source 1, and the kinetic energy inside it is 3.
A high speed atom of 8r of about keV is avoided and is emitted as a high speed atom Pi13. and deflector-4
The remaining ions are removed by passing through the sample holder 5 to remove residual ions, resulting in a pure high-speed atomic beam 3, which is irradiated onto the sample 6 on the sample holder 5. Thereupon, the surface of the sample 6 is bombarded by the high-speed atomic beam 3 and is sputtered, emitting secondary ions 78. Then, the secondary ions 7 are passed through an energy filter 8 to select those with appropriate kinetic energy, and are guided to an analyzer 9. '& tffi analyzer 9 uses this secondary ion 7
A trade analysis is performed to identify the composition of Sample 6.
ところが、このような従来の装置では、高速原子線が試
１１を衝撃することによって生ずるスバツター現象を利
用しているために、特に試料が単結晶性の場合には、結
晶方位と高速原子線の入射角によって二次イオンの放出
効率が異なる。However, since these conventional devices utilize the sputtering phenomenon that occurs when a high-speed atomic beam bombards Sample 11, especially when the sample is single crystal, the crystal orientation and high-speed atomic beam The ejection efficiency of secondary ions differs depending on the incident angle.
−例として、結晶配位（１００）の銅の単結晶を１０ｋ
ｅＶあるいは１５ｋｅＶの運動エネルギーを有するＡｒ
イオンで衝撃した際の二次イオン強度を、Ａｒイオンの
入射角を変化させて測定した結果が、第３図に示しであ
る。- As an example, take a single crystal of copper with crystal orientation (100) as 10k
Ar with a kinetic energy of eV or 15 keV
FIG. 3 shows the results of measuring the secondary ion intensity upon bombardment with ions while varying the incident angle of Ar ions.
この図から明らかなように、試料が単結晶の場合には、
同一の物質であってもその結晶方位によって二次イオン
の強度が変わる口と、また試料の取付は角がわずかに異
なっても二次イオンの強度に影響することがわかる。そ
して、このように試料の取付は角によって、生成ザる二
次イオンの強度に変化が出るとすると、試料の組成分析
の精度にも影響する問題がある。As is clear from this figure, when the sample is a single crystal,
It can be seen that even if the material is the same, the intensity of secondary ions changes depending on its crystal orientation, and that even slight differences in the corners of the sample mounting affect the intensity of secondary ions. If the intensity of the generated secondary ions changes depending on the angle at which the sample is mounted, there is a problem that this also affects the accuracy of the compositional analysis of the sample.
さらに、従来の装置では、試料表面に偏析が生じている
場合にも試料上の分析部位によって二次イオンの感度が
異なってくるため、分析精度の低下をまねく恐れもあっ
た。Furthermore, in conventional apparatuses, even when segregation occurs on the sample surface, the sensitivity of secondary ions differs depending on the analysis site on the sample, which may lead to a decrease in analysis accuracy.
（発明が解決しようとする問題点）
上記のように、従来の高速原子衝撃型二次イオン質量分
析計では、試料の取付は角の違いや高速原子線の照明部
位の違いによって組成分析の結果に影響が出るため、高
い分析精度が期待できない問題があった。(Problems to be Solved by the Invention) As mentioned above, in the conventional high-speed atom bombardment type secondary ion mass spectrometer, the mounting of the sample depends on the angle of the specimen and the illumination area of the high-speed atomic beam. There was a problem that high analytical accuracy could not be expected because of the influence on
この発明は、このような従来の問題に鑑みてなされたち
のであって、大出力パルスレーザ−を試料表面に照射し
てアモルファス状態にし、結晶性に起因する二次イオン
の放出強度の変動を抑え、精ＩＩ！の高い組成分析がで
きる高速原子衝撃型二次イオン質量分析計を提供するこ
とを目的とする。This invention was made in view of these conventional problems, and involves irradiating the sample surface with a high-power pulsed laser to turn it into an amorphous state, thereby suppressing fluctuations in the emitted intensity of secondary ions caused by crystallinity. , Sei II! The purpose of the present invention is to provide a high-speed atom bombardment type secondary ion mass spectrometer that can perform high-speed compositional analysis.
（問題点を解決するための手段）
この発明の高速原子衝撃型二次イオン質量分析計は、高
速原子線の試料への入射を一時的に遮断するシャッター
と、このシャッターが閉じている間に照射して試料表面
を溶融させる大出力パルスレーザ−装置とを備え、分析
試料を高速原子線で衝撃し、試料表面から放出する二次
イオンの質量分析を行うものである。(Means for Solving the Problems) The high-speed atom bombardment type secondary ion mass spectrometer of the present invention includes a shutter that temporarily blocks the incidence of high-speed atomic beams into the sample, and a It is equipped with a high-output pulse laser device that irradiates and melts the sample surface, bombards the analysis sample with high-speed atomic beams, and performs mass spectrometry of secondary ions released from the sample surface.
（作用）
この発明の高速原子種ｉ撃型二次イオン質問分析計では
、高速原子線源からの高速原子線を試料に照射して二次
イオンを放出させ、質量分析計によって質量分析するに
あたり、大出力パルスレーザ−を試料の表面に照射して
アモルファス化し、その後で高速原子線を試料の表面に
照射し、放出される二次イオンのＷＥｆｉ分析を行う。(Function) In the high-speed atomic species i-bomb type secondary ion interrogation analyzer of the present invention, a sample is irradiated with a high-speed atomic beam from a high-speed atomic beam source to release secondary ions, which are then subjected to mass analysis by a mass spectrometer. The surface of the sample is irradiated with a high-power pulsed laser to make it amorphous, and then a high-speed atomic beam is irradiated onto the surface of the sample, and the emitted secondary ions are subjected to WEfi analysis.
（実施例）
以下、この発明の実施例を図に基づいて詳説する。第１
図は、一実施例を示すものであって、高速原子＠源１１
、この１１へに置かれたディフレクタ−１２、試料１３
を支持する試料ホルダー１４、この試料１３を収容する
シールドケース１５、試料１３からの二次イオ゛ンを分
析する質量分析計１６を備えている。(Example) Hereinafter, an example of the present invention will be explained in detail based on the drawings. 1st
The figure shows an example, in which fast atoms @ source 11
, the deflector 12 placed on this 11, the sample 13
The sample holder 14 supports the sample 13, the shield case 15 houses the sample 13, and the mass spectrometer 16 analyzes secondary ions from the sample 13.
前記ディフレクタ−１２には、電線１７が接続されてい
る。また、質量分析計１６の前にエネルギーフィルター
１８が投首されている。An electric wire 17 is connected to the deflector 12. Furthermore, an energy filter 18 is placed in front of the mass spectrometer 16.
さらに、ディフレクタ−１２とシールドケース１５の間
には、高速原子線を遮断するシャッター１９が設けられ
ている。シールドケース１５の中の試料１３に対して大
出力のパルスレーザ−を照射り′るためのパルスレー＋
ｙ−装置２０が備えられている。Furthermore, a shutter 19 is provided between the deflector 12 and the shield case 15 to block high-speed atomic beams. A pulse laser + for irradiating the sample 13 inside the shield case 15 with a high-power pulse laser.
A y-device 20 is provided.
上記構成の高速原子衝撃型二次イオン質量分析計の初作
について、次に説明する。高速原子線源］１に対してＡ
ｒガス２１を導入して、従来例と同様に運動エネルギ−
３ｋｅＶ程度の△「の高速原子線２２を放出させる。デ
ィフレクタ−１２には電１ｉｉｉｔ１７によって電圧が
印加されており、ここを通過する高速原子！＄２２に残
留するイオンが除去され、純粋＜ヱ高速原子線がシール
ドケース１５側に放出される。The first high-speed atom bombardment type secondary ion mass spectrometer with the above configuration will be described next. Fast atomic beam source] A for 1
R gas 21 is introduced to generate kinetic energy as in the conventional example.
A high-speed atomic beam 22 of about 3 keV △' is emitted. A voltage is applied to the deflector 12 by an electric current 17, and the ions remaining in the high-speed atoms passing through this are removed, and the pure<ヱhigh-speed The atomic beam is emitted to the shield case 15 side.
大出力パルスレーザ−装置２０からは、レーザー２３が
パルス的に出力され、試料１３に対して照射され、その
表面が溶融ｓｒろ。この人出力パルスレーザー２３に用
いられるものは、例えば０゜５ Ｊ ／ ｎ＋＋Ｉｓｅ
、パルス幅１００ｎｓ 〜１０ｎ＋ｓのＹＡＧレーザ
ーが適当であるが、特に限定されるものではない。A laser 23 is output in pulses from a high-output pulse laser device 20, and is irradiated onto the sample 13, melting the surface of the sample 13. The one used for this human output pulse laser 23 is, for example, 0°5 J/n++Ise
, a YAG laser with a pulse width of 100 ns to 10 n+s is suitable, but is not particularly limited.
このような大出力でパルス幅の狭いレーザーで結晶性の
固体の表面を照射すると、その表面は瞬時に昇温して溶
融し、結晶性が失われる。そして直ちに急冷されて、結
晶性が回復される前に固化し、アモルファスの状態にな
る。このアモルファス層は、上記のレーザーでは０．０
０１〜１μｍの表層部のみに形成される。When the surface of a crystalline solid is irradiated with such a high-power, narrow-pulse laser, the surface instantly heats up, melts, and loses its crystallinity. It is then rapidly cooled and solidified into an amorphous state before its crystallinity is recovered. This amorphous layer is 0.0
It is formed only in the surface layer part of 01 to 1 μm.
二次イオンのＨａ分析に際しては、シャッター１９を閉
じた状態にして、大出力パルスレーザ−装置２０から１
パルスのレーザー２３を試料１３に照射して表面をアモ
ルファス化し、続いてシャッター１９を開き、高速原子
線２２を高速原子線源１１からシールドケース１５に導
き、試Ｆ１１３の表面を衝撃する。When performing Ha analysis of secondary ions, the shutter 19 is closed and the high-output pulse laser device 20 is
The sample 13 is irradiated with a pulsed laser 23 to make the surface amorphous, and then the shutter 19 is opened, and the high-speed atomic beam 22 is guided from the high-speed atomic beam source 11 to the shield case 15 to impact the surface of the sample F113.
この衝撃によって、試料１３の表面から二次イオン２４
が放出され、エネルギーフィルター１８によって適当な
運動エネルギーのものが選択され、質量分析計１６に至
る。質量分析計１６は、入射してくる二次イオンの質量
分析を行い、その結果により試料１３の組成分析がなさ
れる。This impact causes secondary ions 24 from the surface of the sample 13.
is emitted, and those with appropriate kinetic energy are selected by an energy filter 18 and delivered to a mass spectrometer 16. The mass spectrometer 16 performs mass spectrometry on the incident secondary ions, and the composition of the sample 13 is analyzed based on the results.
このにうにして、アモルファス化した試料表面を衝撃し
て二次イオンを放出させるとき、試料１３の表面には結
晶性がないため、衝撃部位による二次イオンの放出効率
に変化がなく、信頼性の高い質量分析を行えることにな
る。In this way, when the amorphous surface of the sample is bombarded to release secondary ions, since the surface of sample 13 has no crystallinity, there is no change in the efficiency of secondary ion release depending on the impact site, and it is reliable. This means that highly accurate mass spectrometry can be performed.
［発明の効果］
この発明は、上記の構成を有するため、試料の表面をパ
ルスレーザ−の照射によりアモルファス化し、その表面
に高速原子線を衝撃して二次イオンを／ｌ！Ｉ出さけ、
質量分析を行うことができる。[Effects of the Invention] Since the present invention has the above-mentioned configuration, the surface of the sample is made amorphous by irradiation with a pulsed laser, and the surface is bombarded with a high-speed atomic beam to generate secondary ions/l! Let me out,
Mass spectrometry can be performed.
そのため、乙との材料に結晶性があったり、偏析があっ
ても、それに起因する分析感度、分析精度のゆらぎを抑
えることかでき、信頼性の高い組成分析ができる。Therefore, even if the material with B has crystallinity or segregation, fluctuations in analytical sensitivity and analytical accuracy due to this can be suppressed, and highly reliable compositional analysis can be performed.
第１図はこの発明の一実施例の概要を示す斜視図、第２
図は従来例の概要を示す斜視図、第３図は結晶性試料の
二次イオン放出強度の二次ビーム入射角依存性を示すグ
ラフである。
１１・・・高速原子線源
１２・・・ディフレクタ−
１３・・・試料
１４・・・試料ホルダー
１５・・・シールドケース
１６・・・質量分析計
１７・・・電源
１８・・・エネルギーフィルター
１９・・・シャッター
２０・・・大出力パルスレーザー装置
２２・・・高速原子線
２３・・・大出力パルスレーザ−
２４・・・二次イオン
第１図
入射角（度）FIG. 1 is a perspective view showing an outline of an embodiment of the present invention, and FIG.
The figure is a perspective view showing an outline of a conventional example, and FIG. 3 is a graph showing the dependence of the secondary ion emission intensity of a crystalline sample on the incident angle of the secondary beam. 11...Fast atomic beam source 12...Deflector 13...Sample 14...Sample holder 15...Shield case 16...Mass spectrometer 17...Power source 18...Energy filter 19 ... Shutter 20 ... High-power pulse laser device 22 ... High-speed atomic beam 23 ... High-power pulse laser - 24 ... Secondary ion Figure 1 Incident angle (degrees)
Claims (1)
を照射する高速原子線源と、 前記高速原子線の照射を阻止するシャッターと、前記試
料に対してパルスレーザーを照射するレーザー装置と、 前記試料からの二次イオンの分析を行う質量分析計とを
備えて成る高速原子衝撃型二次イオン質量分析計。[Scope of Claims] A sample holder that supports an analysis sample; a high-speed atomic beam source that irradiates the sample supported by the sample holder with a high-speed atomic beam; and a shutter that blocks irradiation of the high-speed atomic beam. A high-speed atom impact secondary ion mass spectrometer comprising: a laser device that irradiates the sample with a pulsed laser; and a mass spectrometer that analyzes secondary ions from the sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61119061A JPH076894B2 (en) | 1986-05-26 | 1986-05-26 | Fast atom bombardment type secondary ion mass spectrometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61119061A JPH076894B2 (en) | 1986-05-26 | 1986-05-26 | Fast atom bombardment type secondary ion mass spectrometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62276448A true JPS62276448A (en) | 1987-12-01 |
| JPH076894B2 JPH076894B2 (en) | 1995-01-30 |
Family
ID=14751935
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61119061A Expired - Fee Related JPH076894B2 (en) | 1986-05-26 | 1986-05-26 | Fast atom bombardment type secondary ion mass spectrometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH076894B2 (en) |
-
1986
- 1986-05-26 JP JP61119061A patent/JPH076894B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH076894B2 (en) | 1995-01-30 |
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