JP3123860B2 - Elemental analyzer using wavelength dispersive spectrometer and energy dispersive spectrometer - Google Patents
Elemental analyzer using wavelength dispersive spectrometer and energy dispersive spectrometerInfo
- Publication number
- JP3123860B2 JP3123860B2 JP05178964A JP17896493A JP3123860B2 JP 3123860 B2 JP3123860 B2 JP 3123860B2 JP 05178964 A JP05178964 A JP 05178964A JP 17896493 A JP17896493 A JP 17896493A JP 3123860 B2 JP3123860 B2 JP 3123860B2
- Authority
- JP
- Japan
- Prior art keywords
- measurement
- dispersive spectrometer
- eds
- wds
- spectrometer
- 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 - Fee Related
Links
- 238000005259 measurement Methods 0.000 claims description 51
- 238000001514 detection method Methods 0.000 claims description 6
- 239000013078 crystal Substances 0.000 description 11
- 230000003595 spectral effect Effects 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 9
- 238000010586 diagram Methods 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 6
- 239000008186 active pharmaceutical agent Substances 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
Description
【０００１】[0001]
【産業上の利用分野】本発明は元素分析装置に係わり、
特に波長分散型分光器（ＷＤＳ）およびエネルギ分散型
分光器（ＥＤＳ）が付いている分析型電子顕微鏡を用い
た元素分析装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an elemental analyzer,
Particularly, the present invention relates to an elemental analyzer using an analytical electron microscope equipped with a wavelength dispersive spectrometer (WDS) and an energy dispersive spectrometer (EDS).
【０００２】[0002]
【従来の技術】試料に電子線を照射し、分析対象の元素
が検出される位置に分光結晶を移動して特性Ｘ線を測定
するＷＤＳ、および半導体検出器等の検出素子を特定位
置に固定して試料から出てくるＸ線を検出し、エネルギ
のピーク位置から元素分析するＥＤＳが付いている分析
型電子顕微鏡を用いて複数元素のピーク強度を測定する
ことが行われている。図５はこのようなＷＤＳおよびＥ
ＤＳが付いている分析型電子顕微鏡による分析装置を示
す図である。電子銃１から発生した電子線２は、収束レ
ンズ３、対物レンズ４を通り、収束されてステージ６上
の試料５に照射される。このとき試料からは含有元素特
有の特性Ｘ線が発生する。ＷＤＳでは、測定する特性Ｘ
線が検出できる位置に分光結晶７を移動した後、検出器
８で計測する。ＥＤＳでは固定位置の半導体検出器９で
その元素特有の特性Ｘ線を検出すると、特性Ｘ線の各エ
ネルギ位置にピークとして計測される。通常、ＥＤＳに
おいて元素のピークカウントデータとして使用する場合
には、一定時間計測した後、注目元素の特性Ｘ線が検出
できるピーク全体のカウント値をその元素のカウント値
として使用している。ＥＤＳ／ＷＤＳを用いた分析で
は、あらかじめ測定する元素を決めてＷＤＳ／ＥＤＳで
測定すべき元素を分担し、順次必要な元素の特性Ｘ線を
計測する。実際の操作においては、測定時間を短縮する
ためＥＤＳではＸ線を照射してすぐに指定した時間Ｘ線
の計測に入り、半導体検出器９の検出結果が測定回路１
０で測定される。ＷＤＳでは、ＥＤＳが測定を行ってい
る間に指定したピーク位置に分光結晶７を移動させる。
この移動は分光器制御回路１１からの指示により行わ
れ、指定した時間計測後、次の元素の特性Ｘ線を計測す
るためにその元素のピーク位置に分光結晶を移動する。
このようなプロセスをＷＤＳで分担した元素が無くなる
まで実行する。したがって、ＷＤＳはＥＤＳが測定を行
っている間に分光結晶の移動、測定を繰り返すことにな
る。このようにＷＤＳおよびＥＤＳが付いている分析型
電子顕微鏡では複数元素のピーク強度等を測定する場
合、測定効率を上げるためＥＤＳとＷＤＳとを同時に行
っていた。2. Description of the Related Art A WDS for irradiating a sample with an electron beam and moving a spectral crystal to a position where an element to be analyzed is detected and measuring characteristic X-rays, and a detecting element such as a semiconductor detector are fixed at a specific position. X-rays emitted from a sample are detected, and the peak intensities of a plurality of elements are measured using an analytical electron microscope equipped with an EDS for performing elemental analysis from an energy peak position. FIG. 5 shows such a WDS and E
It is a figure which shows the analyzer by the analytical electron microscope with DS. An electron beam 2 generated from an electron gun 1 passes through a converging lens 3 and an objective lens 4 and is converged and irradiated on a sample 5 on a stage 6. At this time, characteristic X-rays specific to the contained elements are generated from the sample. In WDS, the characteristic X to be measured
After moving the spectral crystal 7 to a position where a line can be detected, measurement is performed by the detector 8. In the EDS, when the characteristic X-ray peculiar to the element is detected by the semiconductor detector 9 at the fixed position, the characteristic X-ray is measured as a peak at each energy position. Normally, when used as peak count data of an element in EDS, after counting for a certain period of time, the count value of the entire peak at which characteristic X-rays of the element of interest can be detected is used as the count value of the element. In the analysis using EDS / WDS, an element to be measured is determined in advance, an element to be measured by WDS / EDS is shared, and characteristic X-rays of necessary elements are sequentially measured. In an actual operation, in order to shorten the measurement time, the EDS irradiates X-rays and immediately starts measuring the X-rays for a designated time, and the detection result of the semiconductor detector 9 is used as a measurement circuit
It is measured at zero. In the WDS, the spectral crystal 7 is moved to a specified peak position while the EDS is performing the measurement.
This movement is performed in accordance with an instruction from the spectrometer control circuit 11, and after the specified time measurement, the spectral crystal is moved to the peak position of the next element in order to measure the characteristic X-ray of the next element.
Such a process is executed until the elements shared by the WDS disappear. Therefore, in the WDS, the movement and the measurement of the spectral crystal are repeated while the EDS is performing the measurement. As described above, in the analytical electron microscope equipped with WDS and EDS, when measuring peak intensities of a plurality of elements, etc., EDS and WDS were simultaneously performed in order to increase measurement efficiency.
【０００３】[0003]
【発明が解決しようとする課題】しかし、ＥＤＳ測定中
にＷＤＳ分光器を動作させると、ＷＤＳ分光器はモータ
駆動により移動させているため、機械的振動が発生し、
この振動が半導体検出器に影響してＥＤＳのデータがブ
ロードになり、データのＳ／Ｎが低下し、分析結果に悪
い影響を与えるという問題があった。本発明は上記課題
を解決するためのもので、ＷＤＳとＥＤＳが付いている
分析型電子顕微鏡を用い、ＷＤＳとＥＤＳとの同時測定
を行い、かつＷＤＳ分光器の移動による影響を無くし、
測定データのＳ／Ｎ比を向上させることができる波長分
散型分光器とエネルギ分散型分光器を用いた元素分析装
置を提供することを目的とする。However, when the WDS spectrometer is operated during the EDS measurement, the WDS spectrometer is moved by driving the motor, so that mechanical vibration occurs.
This vibration affects the semiconductor detector, so that the data of the EDS becomes broad and the S / N of the data is reduced, which has a problem that the analysis result is adversely affected. The present invention has been made to solve the above-described problems, and performs simultaneous measurement of WDS and EDS using an analytical electron microscope equipped with WDS and EDS, and eliminates the influence of moving the WDS spectrometer,
It is an object of the present invention to provide an elemental analyzer using a wavelength dispersive spectrometer and an energy dispersive spectrometer that can improve the S / N ratio of measurement data.
【０００４】[0004]
【課題を解決するための手段】本発明は、波長分散型分
光器とエネルギ分散型分光器を有する元素分析装置にお
いて、波長分散型分光器およびエネルギ分散型分光器の
検出データを取り込む測定回路と、波長分散型分光器を
駆動制御する分光器制御回路と、分光器制御回路および
測定回路を制御する制御手段とを備え、前記制御手段
は、分光器制御回路からの動作信号を基に測定回路を制
御し、波長分散型分光器動作中はエネルギ分散型分光器
の動作を停止させるようにしたことを特徴とする。SUMMARY OF THE INVENTION The present invention relates to an elemental analyzer having a wavelength dispersive spectrometer and an energy dispersive spectrometer, and a measuring circuit for capturing detection data of the wavelength dispersive spectrometer and the energy dispersive spectrometer. A spectroscope control circuit for driving and controlling the wavelength dispersion type spectroscope, and control means for controlling the spectroscope control circuit and the measurement circuit, wherein the control means includes a measurement circuit based on an operation signal from the spectroscope control circuit. And the operation of the energy dispersive spectroscope is stopped during the operation of the wavelength dispersive spectroscope.
【０００５】[0005]
【作用】本発明はＷＤＳ分光器からの動作信号を基にＥ
ＤＳの測定を制御するようにしたものであり、ＷＤＳ分
光器の移動中にはＥＤＳの測定を停止し、ＷＤＳ分光器
の移動が停止したときにＥＤＳの測定を行うようにした
ので、ＷＤＳ分光器の移動に伴う振動の影響がなくな
り、測定データのＳ／Ｎ比を向上させ、分析精度を向上
させることが可能となる。According to the present invention, E is calculated based on operation signals from a WDS spectrometer.
Since the DS measurement is controlled, the EDS measurement is stopped while the WDS spectroscope is moving, and the EDS measurement is performed when the WDS spectrometer stops moving. The influence of the vibration accompanying the movement of the instrument is eliminated, and the S / N ratio of the measurement data can be improved, and the analysis accuracy can be improved.
【０００６】[0006]
【実施例】図１は本発明のＸ線検出回路の構成を示す
図、図２は測定回路の構成を示す図、図３は測定のタイ
ミングチャートを示す図、図４は測定結果を示す図であ
る。図１において、図５と同一参照番号は同一内容を示
している。ＷＤＳで分析を行う場合、まず分光結晶７を
分析元素が検出される位置に移動した後に検出器８でＸ
線を測定する。この時分光結晶７と検出器８との位置は
分光器制御回路１１によって制御されている。ＥＤＳで
分析する場合は、あるエネルギ位置にピークとして検出
されるので、分光結晶を移動するような物理的動作は必
要なく、半導体検出器９でＸ線を検出し、測定回路１０
で測定することになる。通常、複数元素を複数のＷＤＳ
分光器、１つのＥＤＳで分担して測定するが、分析効率
を上げるために、ＷＤＳ、ＥＤＳの測定を同時に開始し
ている。そのためＥＤＳで測定中にＷＤＳ分光結晶７、
検出器８が次の元素の測定のために移動を開始すると、
その振動等の影響でＥＤＳの特性Ｘ線ピークのＳ／Ｎは
低下する。FIG. 1 is a diagram showing a configuration of an X-ray detection circuit of the present invention, FIG. 2 is a diagram showing a configuration of a measurement circuit, FIG. 3 is a diagram showing a timing chart of measurement, and FIG. It is. 1, the same reference numerals as those in FIG. 5 indicate the same contents. In the case of performing analysis by WDS, first, the spectral crystal 7 is moved to a position where an element to be analyzed is detected, and then X
Measure the line. At this time, the positions of the spectral crystal 7 and the detector 8 are controlled by the spectrometer control circuit 11. In the case of analysis by EDS, since a peak is detected at a certain energy position, there is no need to perform a physical operation such as moving the dispersive crystal, and the semiconductor detector 9 detects X-rays and the measurement circuit 10
Will be measured. In general, multiple WDS
The spectrometer and the EDS share the measurement, but the WDS and EDS measurements are started simultaneously to increase the analysis efficiency. Therefore, during measurement by EDS, WDS
When the detector 8 starts moving to measure the next element,
The S / N of the characteristic X-ray peak of EDS decreases due to the influence of the vibration and the like.
【０００７】本発明では分光器制御回路１１からの動作
信号を基に測定回路１０でＥＤＳの測定を制御して、効
率よく測定するとともに、お互いが影響を受けないよう
にしたものである。この測定方法について図２、図３を
参照して説明する。図２は測定回路１０の主な要素を示
したもので、指定された測定時間、計測を行うために測
定制御回路２０は計測すべき指定時間をタイマー制御回
路２２に指示する。この指示に従ってタイマー制御回路
２２は、検出パルスの出入りを制御するゲート２３とカ
ウンタ２４とに測定開始信号を送り、測定開始を指示す
る。指定した時間測定した後、タイマー制御回路２２は
ゲート２３を閉じ、カウンタ２４による計測を終了させ
る。さらに測定制御回路２０の指示によりタイマーゲー
ト制御回路２１はＷＤＳ分光器制御回路１１から発生す
る分光器動作信号を基に、その信号ラインが動作中であ
るときには、タイマー制御回路２２とゲート２３に一時
測定停止信号を送り、測定を一時停止させる。従って、
ＷＤＳ分光器が動作中の時は測定が進行しないことにな
る。In the present invention, the measurement of the EDS is controlled by the measurement circuit 10 based on the operation signal from the spectroscope control circuit 11, so that the EDS can be measured efficiently and not affected by each other. This measuring method will be described with reference to FIGS. FIG. 2 shows main elements of the measurement circuit 10. The measurement control circuit 20 instructs the timer control circuit 22 to specify the designated measurement time and the designated time to be measured in order to perform the measurement. In accordance with this instruction, the timer control circuit 22 sends a measurement start signal to the gate 23 and the counter 24 for controlling the input and output of the detection pulse, and instructs to start the measurement. After the measurement for the specified time, the timer control circuit 22 closes the gate 23 and terminates the measurement by the counter 24. Further, based on the instruction from the measurement control circuit 20, the timer gate control circuit 21 temporarily stores the signal line in operation based on the spectroscope operation signal generated from the WDS spectroscope control circuit 11 when the signal line is in operation. Send a measurement stop signal to pause the measurement. Therefore,
When the WDS spectrometer is in operation, the measurement will not proceed.
【０００８】この動作について図３のタイムチャートに
より説明すると、例えば、ＷＤＳ分光器−１，分光器−
２，分光器−３からなる３チャンネルが装備されている
場合、分光器−１、分光器−２、分光器−３の何れかの
分光結晶が移動中には測定停止信号が発せられ、ゲート
２３が閉じられて測定が停止され、分光器−１、分光器
−２、分光器−３の何れもが移動中でない間に測定停止
信号が解除されてＥＤＳ測定が行われることになる。図
４（ａ）はＷＤＳの分光結晶の移動を停止させ、振動を
与えなかったときのＥＤＳ波形例であり、図４（ｂ）は
同一の条件で測定し、ＷＤＳ分光器を移動して振動を与
えた時のＥＤＳ波形例であり、図４（ｃ）は図４
（ａ），（ｂ）を重ねてその違いを示したものである。
ＥＤＳで求めるある元素のＸ線カウント値は、その元素
のピークの積分値を使用するため、図４（ｂ）のように
ピーク波形が崩れると、真のピークが求められないばか
りか、隣接するピークの値が求めようとするピークの値
として計測されてしまう場合もある。本発明によりこの
振動の影響を無くすと、図４（ｃ）の実線に示すように
ピークがシャープとなり、分析精度を向上させることが
可能となる。This operation will be described with reference to the time chart of FIG. 3. For example, WDS spectroscope-1, spectroscope
In the case where three channels of the spectroscope-3 and the spectroscope-3 are provided, a measurement stop signal is issued while any of the spectroscope-1, the spectroscope-2, and the spectroscope-3 is moving, and the gate is stopped. 23 is closed to stop the measurement, and while none of the spectroscope-1, the spectroscope-2, and the spectroscope-3 are moving, the measurement stop signal is released and the EDS measurement is performed. FIG. 4A shows an example of the EDS waveform when the movement of the WDS spectral crystal is stopped and no vibration is applied, and FIG. 4B shows the measurement under the same conditions, and the WDS spectrometer is moved to vibrate. FIG. 4 (c) is an example of the EDS waveform when
(A) and (b) are overlapped to show the difference.
The X-ray count value of an element determined by EDS uses the integrated value of the peak of the element. Therefore, if the peak waveform is distorted as shown in FIG. The peak value may be measured as the peak value to be obtained. When the influence of this vibration is eliminated by the present invention, the peak becomes sharp as shown by the solid line in FIG. 4C, and the analysis accuracy can be improved.
【０００９】[0009]
【発明の効果】以上のように本発明によれば、ＷＤＳと
ＥＤＳによる測定を効率よく行うことができると共に、
ＥＤＳがＷＤＳ分光結晶の移動の影響を受けることがな
いため、ＥＤＳの特性Ｘ線ピーク測定のＳ／Ｎ比を良く
し、分析精度を向上させることが可能となる。As described above, according to the present invention, measurement by WDS and EDS can be performed efficiently,
Since the EDS is not affected by the movement of the WDS spectral crystal, the S / N ratio of the characteristic X-ray peak measurement of the EDS can be improved, and the analysis accuracy can be improved.
【図１】 本発明のＸ線検出回路の構成を示す図であ
る。FIG. 1 is a diagram showing a configuration of an X-ray detection circuit of the present invention.
【図２】 測定回路の構成を示す図である。FIG. 2 is a diagram illustrating a configuration of a measurement circuit.
【図３】 測定のタイミングチャートを示す図である。FIG. 3 is a diagram showing a timing chart of measurement.
【図４】 測定結果を示す図である。FIG. 4 is a diagram showing measurement results.
【図５】 ＷＤＳとＥＤＳが付いている分析型電子顕微
鏡による分析を説明する図である。FIG. 5 is a diagram for explaining analysis by an analytical electron microscope equipped with WDS and EDS.
７…分光結晶、８…検出器、９…半導体検出器、１０…
測定回路、１１…分光器制御回路、１２…制御回路、２
０…測定制御回路、２１…タイマ・ゲート制御回路、２
２…タイマ制御回路、２３…ゲート、２４…カウンタ。7: spectral crystal, 8: detector, 9: semiconductor detector, 10 ...
Measurement circuit, 11: spectrometer control circuit, 12: control circuit, 2
0: measurement control circuit, 21: timer / gate control circuit, 2
2 ... Timer control circuit, 23 ... Gate, 24 ... Counter.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) H01J 37/252 H01J 37/244 G01N 23/00 - 23/227 ──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int.Cl. 7 , DB name) H01J 37/252 H01J 37/244 G01N 23/00-23/227
Claims (1)
器を有する元素分析装置において、波長分散型分光器お
よびエネルギ分散型分光器の検出データを取り込む測定
回路と、波長分散型分光器を駆動制御する分光器制御回
路と、分光器制御回路および測定回路を制御する制御手
段とを備え、前記制御手段は、分光器制御回路からの動
作信号を基に測定回路を制御し、波長分散型分光器動作
中はエネルギ分散型分光器の動作を停止させるようにし
たことを特徴とする波長分散型分光器とエネルギ分散型
分光器を用いた元素分析装置。An element analyzer having a wavelength dispersive spectrometer and an energy dispersive spectrometer, a measuring circuit for capturing detection data of the wavelength dispersive spectrometer and the energy dispersive spectrometer, and driving the wavelength dispersive spectrometer A spectroscope control circuit for controlling the spectroscope control circuit and a control circuit for controlling the measurement circuit, wherein the control means controls the measurement circuit based on an operation signal from the spectroscope control circuit, and An elemental analyzer using a wavelength dispersive spectrometer and an energy dispersive spectrometer, wherein the operation of the energy dispersive spectrometer is stopped during operation of the spectrometer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05178964A JP3123860B2 (en) | 1993-07-20 | 1993-07-20 | Elemental analyzer using wavelength dispersive spectrometer and energy dispersive spectrometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05178964A JP3123860B2 (en) | 1993-07-20 | 1993-07-20 | Elemental analyzer using wavelength dispersive spectrometer and energy dispersive spectrometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0737539A JPH0737539A (en) | 1995-02-07 |
| JP3123860B2 true JP3123860B2 (en) | 2001-01-15 |
Family
ID=16057748
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP05178964A Expired - Fee Related JP3123860B2 (en) | 1993-07-20 | 1993-07-20 | Elemental analyzer using wavelength dispersive spectrometer and energy dispersive spectrometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3123860B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102621170B (en) * | 2012-03-09 | 2013-11-06 | 湖北方圆环保科技有限公司 | Method for automatically determining measurement time in detection of energy spectrometer |
-
1993
- 1993-07-20 JP JP05178964A patent/JP3123860B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0737539A (en) | 1995-02-07 |
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