JPS6235445A - Device for analyzing sample surface - Google Patents
Device for analyzing sample surfaceInfo
- Publication number
- JPS6235445A JPS6235445A JP60172780A JP17278085A JPS6235445A JP S6235445 A JPS6235445 A JP S6235445A JP 60172780 A JP60172780 A JP 60172780A JP 17278085 A JP17278085 A JP 17278085A JP S6235445 A JPS6235445 A JP S6235445A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- sample surface
- electron beam
- ray
- crystal
- 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
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
Description
【発明の詳細な説明】
イ 産業上の利用分野
本発明はＸ線マイクロアナライザ等の、荷電粒子のマイ
クロビームで試料を励起し、試料から放射されるＸ線等
を検出することにより試料表面の広域の元素分布を測定
する装置に関する。DETAILED DESCRIPTION OF THE INVENTION A. Industrial Application Field The present invention excites a sample with a microbeam of charged particles, such as an X-ray microanalyzer, and detects the X-rays emitted from the sample. This invention relates to a device for measuring element distribution over a wide area.
口 従来の技術
］ンピュータの利用により、試料面の元素の濃度分布等
のカラー表示が行われるようになり、Ｘ線マイクロアナ
ライザ等による、試料表面の広い面積における定性分析
及び特定元素の定量分析が求められるようになってきた
。[Background technology] With the use of computers, color display of the concentration distribution of elements on the sample surface has become possible, and qualitative analysis and quantitative analysis of specific elements over a wide area of the sample surface using X-ray microanalyzers, etc. have become possible. It's starting to be sought after.
しかしＸ線マイクロアナライザのような装置は本来、試
料の局所分析（１μｓｎ程度）を行う装置であり、広域
の分析としては、Ｘ線分光器の波長を特定の元素の特性
Ｘ線の波長に合せて設定しておき、試料の方を駆動して
広い面積の走査を行い、特定元素の濃度分布を求めるこ
とが行われている。However, equipment such as the X-ray microanalyzer is originally a device that performs local analysis (about 1 μsn) of a sample, and for wide-area analysis, it is necessary to adjust the wavelength of the X-ray spectrometer to the characteristic X-ray wavelength of a specific element. The concentration distribution of a specific element is determined by setting the sample to scan a wide area by driving the sample.
しかしこの方法は、分析面積を画素点に分割して、一画
素点毎にＸ線測定を行わねばならないから非常な時間が
か＼る。Ｘ線測定の所要時間は一画素点当り１０ｍＳ程
度で、仮に測定面積を縦横夫々５００の画素に分割する
と全部で２５００００個の画素になり、正味のＸ線測定
時間は４０分余りである。しかし試料を止めては動かす
と云う動作を繰返すので、機構の慣性のため高速駆動は
できず、スロースタート、スローストップを繰返すこと
になり、−走査線の終りの折返し点では機構のバックラ
ッシュを除くため余分の移動を行わせねばならないから
、試料の移動のために実測定時間の何倍もの時間を消費
し、所定面積の測定に１０時間もか＼ることがあった。However, this method requires a considerable amount of time because the analysis area must be divided into pixel points and X-ray measurement must be performed for each pixel point. The time required for X-ray measurement is approximately 10 mS per pixel point, and if the measurement area is divided into 500 vertical and horizontal pixels, there will be a total of 250,000 pixels, and the net X-ray measurement time will be over 40 minutes. However, since the sample is stopped and moved repeatedly, high-speed drive is not possible due to the inertia of the mechanism, and slow starts and slow stops are repeated. Since extra movement must be performed to remove the sample, it takes many times the actual measurement time to move the sample, and it sometimes takes up to 10 hours to measure a given area.
ハ 発明が解決しようとする問題点
上述したように荷電粒子のマイクロビームラ用いる分析
装置で広い面積における指定元素の定量分布の測定を行
うことが求められているが適当な方法がなかった。本発
明は荷電粒子マイクロビームを用いる分析装置で数ｍｍ
〜数σ平方程度の広□面積における指定元素の濃度分布
を精度良くかつ短時間で行い得るようにしようとするも
のである。C. Problems to be Solved by the Invention As mentioned above, there is a need to measure the quantitative distribution of specified elements over a wide area using an analyzer using a microbeam laser of charged particles, but there has been no suitable method. The present invention is an analyzer that uses a charged particle microbeam to
The purpose is to make it possible to measure the concentration distribution of a designated element in a wide square area of approximately several sigma squares with high accuracy and in a short time.
二 問題点解決のための手段
試料を回転させると共に、回転の半径方向に移動させ、
Ｘ線分光器は定量をしようとする元素の特性Ｘ線の波長
位置に設定して上記試料面上の空間的に固定した一定点
をにらむようにした。即ちＸ線分光器は試料面を渦巻線
状に走査しながらＸ線検出出力を、試料上のマイクロビ
ーム照射点の位置のデータに対応させて記録するように
した。(ii) means for solving the problem, rotating the sample and moving it in the radial direction of the rotation;
The X-ray spectrometer was set at the wavelength position of the characteristic X-ray of the element to be quantified so as to aim at a spatially fixed point on the sample surface. That is, the X-ray spectrometer was configured to record the X-ray detection output while scanning the sample surface in a spiral manner in correspondence with data on the position of the microbeam irradiation point on the sample.
ホ 作用
本発明は試料を一方向の回転と一方向の直線運動との組
合せで動かし、マイクロビームにょる試査の場合のよう
なバックラッシュ消六の動作が不要であり、余分な試料
運動がなく、一方向運動であるから慣性の問題がなく、
そのため起動停止に要する時間消費がない。試料の運動
期間を全部実分析時間に当てることができるので、分析
所要時間が短縮できるのである。E. Function The present invention moves the sample by a combination of rotation in one direction and linear motion in one direction, eliminating the need for backlash elimination operations as in the case of testing using a microbeam, and eliminating unnecessary sample movement. , since it is a unidirectional motion, there is no problem of inertia,
Therefore, there is no time consumption required for starting and stopping. Since the entire sample movement period can be used as the actual analysis time, the time required for analysis can be shortened.
へ 実施例
図は本発明の一実施例を示す。１は試料で、電子ビーム
２を試料ｌの表面に収束させる。５は試料面の電子ビー
ム照射点から放射されるＸ線で、分光結晶３で分光され
、Ｘ線検出器４に入射せしめられる。試料１の電子ビー
ム照射点と分光結晶３とＸ線検出器４の曲面スリットが
共通のローランド円Ｒ上に位置するように、分光結晶と
Ｘ線検出器とは機構的に連結され、波長走査用モータＭ
によって駆動され指定元素の特性Ｘ線の波長位置に設定
される。試料１は試料ホルダ６に保持される。試料ホル
ダ６はＸ方向微動台７、Ｙ方向微動台８によって位置調
節可能である。Ｘ方向微動台、Ｙ方向微動台は回転テー
ブル９の中央に載置固定されている。回転テーブル９は
一方向移動ステージ１４に垂直軸によって回転自在に保
持され、同ステージに固定されたモータ１１により歯車
１０を介して回転駆動される。一方移動ステージ１４は
、基台Ｂ上に一方向ガイドにより一方向摺動可能に載置
されており、同ステージに固定されたナツトが基台Ｂに
保持された送りねじ１６に螺合しており、送りねじ１６
をモータ１７で駆動することにより、一方向、図では左
右方向に移動せしめられる。Embodiment The figure shows an embodiment of the present invention. 1 is a sample, and an electron beam 2 is focused on the surface of the sample 1. Reference numeral 5 indicates X-rays emitted from an electron beam irradiation point on the sample surface, which is separated by a spectroscopic crystal 3 and made incident on an X-ray detector 4. The spectroscopic crystal and the X-ray detector are mechanically connected so that the electron beam irradiation point of the sample 1, the curved slit of the spectroscopic crystal 3, and the X-ray detector 4 are located on a common Rowland circle R, and wavelength scanning is performed. Motor M
is driven by and set at the wavelength position of the characteristic X-ray of the specified element. The sample 1 is held in a sample holder 6. The position of the sample holder 6 can be adjusted by an X-direction fine movement table 7 and a Y-direction fine movement table 8. The X-direction fine movement table and the Y-direction fine movement table are mounted and fixed at the center of the rotary table 9. The rotary table 9 is rotatably held on a one-way moving stage 14 by a vertical axis, and is rotationally driven via a gear 10 by a motor 11 fixed to the stage. On the other hand, the moving stage 14 is placed on the base B so as to be slidable in one direction by a one-way guide, and a nut fixed to the stage is screwed into a feed screw 16 held on the base B. cage, feed screw 16
By driving it with a motor 17, it can be moved in one direction, in the left and right directions in the figure.
上述溝造で、回転テーブル９を回転させながら一方向移
動ステージ１４を例えば左方向に移動させると、試料ｌ
上の電子ビーム照射点は空間的には不動であるが、試料
面に対しては局線を画いて移動し、試料面の円形領域が
電子ビームによって走査されることになる。In the above-mentioned groove structure, when the one-way moving stage 14 is moved, for example, to the left while rotating the rotary table 9, the sample l
The upper electron beam irradiation point does not move spatially, but moves along a line with respect to the sample surface, and a circular area on the sample surface is scanned by the electron beam.
回転テーブル９の周縁には磁気テープが貼設してあり、
一方向移動ステージ１４に固定された磁気ヘッド１３が
この磁気テープに対向させである。Magnetic tape is attached to the periphery of the rotary table 9.
A magnetic head 13 fixed to a one-way moving stage 14 faces this magnetic tape.
上記磁気テープには回転テーブル９の回転角を示すため
の情報が記録しである。この情報は例えば、回転テーブ
ル９の回転角表示の起点を表わす符号と円周を１０２４
等分する一定ピッチのパルス状符号とで、ＣＰＵ１８は
磁気ヘッド１３によりこれらの符号を読取り、回転角の
起点からのパルス符号の数を計数して回転テーブル９の
回転位置を検出している。送りねじ１６を駆動するモー
タ１７はパルスモータで、ＣＰＵ１８は回転テーブル９
の回転中心が電子ビーム２の光軸と一致する位置にある
ときの移動ステージ１４の位置を起点にして、パルスモ
ータ１７の駆動パルスを計数して回転テーブル９の中心
の図で左右方向の位置を検出している。移動ステージ１
４の起点位置は移動ステージ１４がリミットスイッチＳ
に当接することによって検出される。以上の構成により
試料ｌ上の任意の位置は回転テーブル９の回転角と移動
ステージの起点からの距離を座標データとして表ＣＰＵ
は上述した試料運動によってマイクロビームで試料面の
走査を行いながらＸ線検出器４の出力を試料１上の各点
でサンプリングし、サンプリングしたデータを試料１の
Ｘ線強度サンプリング点の座標に対応するメモリ１９の
アドレスに格納する。このようにして試料表面の所定面
積における指定元素の濃度分布のデータが得られ、これ
に基いて試料面の目的元素の濃度分布のカラー表示等が
できる。マイクロビームの光学系の周囲に複数台のＸ線
分光器が配置されている場合には上述方法で同時に複数
元素の濃度分布を測定することができる。Information indicating the rotation angle of the rotary table 9 is recorded on the magnetic tape. This information includes, for example, a code representing the starting point of the rotation angle display of the rotary table 9 and a circumference of 1024.
The CPU 18 reads these codes with the magnetic head 13 and counts the number of pulse codes from the starting point of the rotation angle to detect the rotational position of the rotary table 9. The motor 17 that drives the feed screw 16 is a pulse motor, and the CPU 18 drives the rotary table 9.
Starting from the position of the movable stage 14 when the center of rotation is at a position that coincides with the optical axis of the electron beam 2, drive pulses of the pulse motor 17 are counted to determine the horizontal position of the center of the rotary table 9 in the diagram. is being detected. Moving stage 1
4, the moving stage 14 is at the limit switch S.
It is detected by coming into contact with the With the above configuration, any position on the sample l can be determined by the CPU using the rotation angle of the rotary table 9 and the distance from the starting point of the moving stage as coordinate data.
samples the output of the X-ray detector 4 at each point on the sample 1 while scanning the sample surface with a microbeam by the sample movement described above, and the sampled data corresponds to the coordinates of the X-ray intensity sampling point on the sample 1. The data is stored at the address in the memory 19. In this way, data on the concentration distribution of the designated element in a predetermined area of the sample surface is obtained, and based on this data, the concentration distribution of the target element on the sample surface can be displayed in color. When a plurality of X-ray spectrometers are arranged around the microbeam optical system, the concentration distribution of a plurality of elements can be measured simultaneously by the above-described method.
ト 効果
本発明によれば、試料面をマイクロビームで走査するの
に試料の一方向の回転と一方向の移動との組合せを用い
ているので、Ｘ方向、Ｙ方向のジグザグ走査に比し走査
機構が簡単になり、往復運動が少いから高速走査が可能
となって、大面積の分析が能率的に行われる。Ｘ線分析
では測定精度を上げるためには一つの点について成る程
度時間をかける必要があるが、試料面を画素に区分し、
画素毎に分析を行って行く方法では、試料を一画素分ず
つ送っては停止すると云う動作を繰返し、起動、停止の
度に慣性吸収のためスロースタート、スローストップを
行うので、実測定時間よりこの移動時間の方が多くなり
、実測定時間が２〜３時間である場合でも全所要時間は
１０時間もか＼ると云うのが実情であるが、本発明によ
れば、略実測定時間で分析を完了することができる。G. Effect According to the present invention, since a combination of rotation in one direction and movement in one direction of the specimen is used to scan the specimen surface with a microbeam, the scanning speed is lower than that in zigzag scanning in the X and Y directions. The mechanism is simple and there is little reciprocating movement, so high-speed scanning is possible, and analysis of large areas can be performed efficiently. In order to improve measurement accuracy in X-ray analysis, it is necessary to spend time on each point, but by dividing the sample surface into pixels,
In the method of performing analysis pixel by pixel, the sample is sent one pixel at a time and then stopped, which is repeated, and each time the sample is started and stopped, slow starts and slow stops are performed due to inertia absorption, so it takes longer than the actual measurement time. The actual situation is that this travel time is longer, and even if the actual measurement time is 2 to 3 hours, the total time required is about 10 hours, but according to the present invention, the actual measurement time is approximately 10 hours. The analysis can be completed with
図は本発明の一実施例の要部側面図である。 The figure is a side view of essential parts of an embodiment of the present invention.
Claims (1)
る放射線を検出する構成で、試料を回転させる台と、こ
の台を一方向に往復移動させる手段を有し、上記台を一
方向に移動させながら試料をこの移動速度に比し高速に
回転させて試料面を渦線伏走査線に沿って上記荷電粒子
ビームで走査するようにし、試料面の各位置から放射さ
れる放射線の検出信号を試料面上を移動する荷電粒子ビ
ーム照射点の各位置と対応させたメモリ上の各アドレス
に格納するようにした試料面分析装置。The sample surface is irradiated with a charged particle beam and the radiation emitted from the sample surface is detected.The sample surface is irradiated with a charged particle beam and the radiation emitted from the sample surface is detected. While moving, the sample is rotated at a high speed compared to this moving speed so that the sample surface is scanned by the charged particle beam along the vortex line scanning line, and detection signals of radiation emitted from each position on the sample surface are detected. A sample surface analysis device in which the information is stored in each address on a memory corresponding to each position of a charged particle beam irradiation point moving on the sample surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60172780A JPH0642357B2 (en) | 1985-08-05 | 1985-08-05 | Sample surface analyzer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60172780A JPH0642357B2 (en) | 1985-08-05 | 1985-08-05 | Sample surface analyzer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6235445A true JPS6235445A (en) | 1987-02-16 |
| JPH0642357B2 JPH0642357B2 (en) | 1994-06-01 |
Family
ID=15948212
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60172780A Expired - Lifetime JPH0642357B2 (en) | 1985-08-05 | 1985-08-05 | Sample surface analyzer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0642357B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63318055A (en) * | 1987-06-19 | 1988-12-26 | Shimadzu Corp | Measured data displaying method for epma |
| JPH01102839A (en) * | 1987-10-15 | 1989-04-20 | Hitachi Ltd | Electron microscope with analytical function |
| JPH0424544A (en) * | 1990-05-18 | 1992-01-28 | Motohiro Iwami | Soft x-ray spectrochemical analysis apparatus |
| WO2021240675A1 (en) * | 2020-05-27 | 2021-12-02 | 株式会社日立ハイテク | Nucleic acid analysis device |
-
1985
- 1985-08-05 JP JP60172780A patent/JPH0642357B2/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63318055A (en) * | 1987-06-19 | 1988-12-26 | Shimadzu Corp | Measured data displaying method for epma |
| JPH01102839A (en) * | 1987-10-15 | 1989-04-20 | Hitachi Ltd | Electron microscope with analytical function |
| JPH0424544A (en) * | 1990-05-18 | 1992-01-28 | Motohiro Iwami | Soft x-ray spectrochemical analysis apparatus |
| WO2021240675A1 (en) * | 2020-05-27 | 2021-12-02 | 株式会社日立ハイテク | Nucleic acid analysis device |
| JPWO2021240675A1 (en) * | 2020-05-27 | 2021-12-02 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0642357B2 (en) | 1994-06-01 |
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