JPS642214B2 - - Google Patents
Info
- Publication number
- JPS642214B2 JPS642214B2 JP15447781A JP15447781A JPS642214B2 JP S642214 B2 JPS642214 B2 JP S642214B2 JP 15447781 A JP15447781 A JP 15447781A JP 15447781 A JP15447781 A JP 15447781A JP S642214 B2 JPS642214 B2 JP S642214B2
- Authority
- JP
- Japan
- Prior art keywords
- sample surface
- sample
- data
- discharge
- 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.)
- Expired
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
Landscapes
- Health & Medical Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (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)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Description
【発明の詳細な説明】
本発明はスパーク光源を用いた発光分光分析に
よつて試料面における元素分布を測定する装置に
関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for measuring element distribution on a sample surface by emission spectrometry using a spark light source.
試料面における元素等の分布を測定し得る装置
として、電子線で試料面を走査するＸ線マイクロ
アナライザ等の電子的な装置があるが、この種の
装置は実際上試料面上の走査範囲がせま過ぎてミ
クロの分析には適しているが、構造材断面におけ
る成分元素の偏析状態とか不純物の分布状態をマ
クロに測定すると云つた目的には適さない。しか
し現在、このような試料面のマクロの解析に適す
る装置は余り知られていない。螢光Ｘ線分光装置
が或る程度この目的に適するが、分析面が大き
く、分析に長時間を要し、特に材料の生産ライン
の管理等の生産場面には不向きなものである。 There are electronic devices such as X-ray microanalyzers that scan the sample surface with an electron beam as devices that can measure the distribution of elements on the sample surface. Although it is suitable for microscopic analysis because it is too narrow, it is not suitable for macroscopic measurements of the segregation state of component elements or the distribution state of impurities in a cross section of a structural material. However, at present, there are not many known devices suitable for such macroscopic analysis of a sample surface. Although a fluorescent X-ray spectrometer is suitable for this purpose to some extent, it has a large analysis surface and requires a long time for analysis, making it particularly unsuitable for production situations such as management of material production lines.
本発明は上述したような現況に鑑み試料面のマ
クロの分析に適した装置を提供しようとするもの
である。スパーク放電を光源とする発光分光分析
は試料面における放電点が一放電毎に異るが数mm
の範囲に分布するので、この分析法はそれ自身mm
のオーダの位置的分解能を有している。従来はス
パーク光源を用いる発光分光分析は試料面の一乃
至複数の点について分析を行い、試料に関して代
表的な分析データを得るにとどまり、試料面にお
ける元素の分布状態を把握し表示すると云う方向
への応用はなされていなかつた。本発明はスパー
ク放電を光源とする発光分析が上述したようにそ
れ自身位置的分解能を有していることに着眼し、
放電電極で試料面を走査することにより、目的と
する元素の分布を測定できるようにした分析装置
に関するものである。以下実施例によつて本発明
を説明する。 In view of the current situation as described above, the present invention aims to provide an apparatus suitable for macroscopic analysis of a sample surface. In emission spectroscopic analysis using spark discharge as a light source, the discharge point on the sample surface varies for each discharge, but is several mm.
distribution in the range of mm, this analytical method itself
It has a positional resolution on the order of . Conventionally, emission spectrometry analysis using a spark light source only analyzes one or more points on the sample surface and obtains representative analytical data about the sample, but the trend is toward understanding and displaying the distribution of elements on the sample surface. had not been applied. The present invention focuses on the fact that optical emission analysis using spark discharge as a light source has positional resolution as described above,
The present invention relates to an analyzer that can measure the distribution of a target element by scanning a sample surface with a discharge electrode. The present invention will be explained below with reference to Examples.
第１図は本発明の一実施例装置を示す。１は試
料、２は発光スタンドでＰは放電電極である。３
は試料走査制御装置で与えられたプログラムに従
い試料１をＸ方向、Ｙ方向に駆動する。この構成
によつてスパーク放電における試料面の放電点が
試料面を走査することになる。４は分光器、５は
測光装置で、分光器のスペクトル面上で検出定量
しようとする元素の輝線位置に受光素子を配置し
てあり、同時に複数の元素に関して測定が可能で
ある。６は放電発光回路で400回／秒程度の速さ
でスパーク放電を行わせる。試料走査制御装置３
による試料１の送り速度は１mm／秒程度である。
測光装置は各輝線毎に測光を行い、積分回路で毎
回のスパーク発光における測光出力を積分する。
積分回路は例えばスパーク発光10回毎にクリヤさ
れる。従つて測光装置５からは例えばスパーク発
光10回における平均の輝線強度が出力される。７
は中央制御装置で、放電発光回路６からの放電信
号をカウントし、測光装置５における積分回路を
クリヤし、また試料走査制御装置３に制御信号を
送つて試料面上に所定の走査軌跡を画かせる。更
に中央制御装置７は測光装置５の出力をＡ−Ｄ変
換して同制御装置内のRAMに記憶させる。
RAMのアドレスはスパーク発光10回を一単位と
して数えた発光回数によつて指定され、このアド
レスと試料面上の位置との関係はプログラムによ
つて与えられる。８はCRTを備えたシステムコ
ンソール、９はグラフイツクプリンタ、１０はＸ
−Ｙプロツタである。中央制御装置は試料面走査
期間中上述した所によつてRAMに測光データを
記憶させて行き、走査が終了するとRAM内のデ
ータに基き各元素の含有％を算出する。この演算
は内部標準元素の輝線強度と目的元素の輝線強度
の比と検量線のデータとによつて行う通常の方法
に従えばよい。このようにして得られた各元素の
含有％はプリンタ９によつて印字し、或はRAM
のアドレスと試料面上の位置との対応関係が走査
プログラムから決つて来るからＸ−Ｙプロツタ−
１０によつて目的元素の濃度分布の等高線として
記憶表示させることもできる。或は濃度を輝度に
変換してCRTによつて表示させることもできる。 FIG. 1 shows an embodiment of the present invention. 1 is a sample, 2 is a light emitting stand, and P is a discharge electrode. 3
drives the sample 1 in the X and Y directions according to a program given by the sample scanning controller. With this configuration, the discharge point on the sample surface in spark discharge scans the sample surface. 4 is a spectrometer, and 5 is a photometer, in which a light-receiving element is arranged at the emission line position of the element to be detected and quantified on the spectrum plane of the spectrometer, and it is possible to measure a plurality of elements at the same time. 6 is a discharge light emitting circuit that causes spark discharge to occur at a speed of about 400 times/second. Sample scanning control device 3
The feeding speed of sample 1 is about 1 mm/sec.
The photometric device performs photometry for each bright line, and an integrating circuit integrates the photometric output for each spark emission.
The integral circuit is cleared, for example, every 10 times the spark is emitted. Therefore, the photometric device 5 outputs, for example, the average bright line intensity of 10 spark emissions. 7
is a central control device that counts the discharge signal from the discharge light emitting circuit 6, clears the integrating circuit in the photometer 5, and sends a control signal to the sample scanning control device 3 to draw a predetermined scanning locus on the sample surface. Let it happen. Furthermore, the central control device 7 converts the output of the photometric device 5 from analog to digital and stores it in the RAM within the control device.
The address of the RAM is specified by the number of flashes counted with 10 spark flashes as one unit, and the relationship between this address and the position on the sample surface is given by the program. 8 is a system console with CRT, 9 is a graphics printer, 10 is an X
-Y Protsuta. The central controller stores the photometric data in the RAM as described above during the sample surface scanning period, and when the scanning is completed, calculates the content percentage of each element based on the data in the RAM. This calculation may be performed in a conventional manner using the ratio of the bright line intensity of the internal standard element and the target element and the data of the calibration curve. The content percentage of each element obtained in this way is printed by the printer 9 or written in the RAM.
Since the correspondence between the address and the position on the sample surface is determined from the scanning program, the X-Y plotter
10 can also be stored and displayed as contour lines of the concentration distribution of the target element. Alternatively, the density can be converted to luminance and displayed on a CRT.
第２図は試料面の走査軌跡の例を示し、分析目
的によつて同図ａのような円周軌跡或はｂのよう
なジグザグ経路による試料面全面の走査等任意の
走査軌跡が可能である。 Figure 2 shows an example of the scanning trajectory of the sample surface. Depending on the purpose of analysis, any scanning trajectory can be used, such as a circular trajectory as shown in Figure a or a zigzag path as shown in Figure b. be.
本発明装置は上述したような構成で、スパーク
発光分光分析法が有する測定位置局限性を利用し
て試料面を走査するので、マクロの分布測定が可
能となり、試料における介在物解析、偏析状態の
解析等に威力を発揮するものであり、またわづか
ずつずらせた多数点の測定データを扱い得るの
で、いわゆるサンプリング誤差の少い高確度の分
析が可能となる。また平均の輝線強度のデータは
位置のデータと共に一旦メモリに格納されるの
で、測定結果に種々の演算加工を施して表示する
ことができ、分析結果の活用に大へん便利であ
る。 The device of the present invention has the above-mentioned configuration and scans the sample surface by utilizing the measurement position localization characteristic of spark emission spectrometry, making it possible to measure the macroscopic distribution and to analyze inclusions in the sample and determine the state of segregation. It is very effective in analysis and the like, and because it can handle measurement data from multiple points that are slightly shifted, highly accurate analysis with little sampling error is possible. Furthermore, since the average bright line intensity data is temporarily stored in the memory together with the position data, the measurement results can be subjected to various calculation processing and displayed, which is very convenient for utilizing the analysis results.
なお毎回のスパーク発光による測光値の平均化
の方法として上述実施例では10点毎に算述平均を
とつているが、これに限られるものではなく、
色々な平均化のプログラムが適用可能であること
は云うまでもない。 In addition, as a method of averaging the photometric values due to each spark emission, in the above embodiment, an arithmetic average is taken every 10 points, but the method is not limited to this.
Needless to say, various averaging programs can be applied.
第１図は本発明の一実施例装置の構成を示すブ
ロツク図、第２図は試料面の走査軌跡を例示する
平面図である。
１……試料、２……発光スタンド、３……試料
走査制御装置、４……分光器、５……測光装置、
６……放電発光回路、７……中央制御装置、８…
…システムコンソール、９……グラフイツクプリ
ンタ、１０……Ｘ−Ｙプロツタ。
FIG. 1 is a block diagram showing the configuration of an apparatus according to an embodiment of the present invention, and FIG. 2 is a plan view illustrating a scanning locus of a sample surface. 1... Sample, 2... Light emitting stand, 3... Sample scanning control device, 4... Spectrometer, 5... Photometry device,
6...Discharge light emitting circuit, 7...Central control unit, 8...
...System console, 9...Graphics printer, 10...X-Y plotter.
Claims (1)
極との間に任意の軌跡に沿つて相対的移動を行わ
せる二次的走査装置と、測定データを記憶させる
メモリと、二次元的な表示手段と、試料面におけ
る上記放電電極の位置のデータとその位置におけ
る分析データとして複数回の発光における光検出
出力の平均値とを上記メモリに格納し、同メモリ
に格納されたデータに演算加工を施して上記表示
手段に表示させる制御装置とよりなる発光分光分
析による濃度分布解析装置。1. A secondary scanning device that allows relative movement along an arbitrary trajectory between the sample and the discharge electrode for spark discharge along the sample surface, a memory that stores measurement data, and a two-dimensional display means. Then, the data on the position of the discharge electrode on the sample surface and the average value of the photodetection output in multiple light emissions as analysis data at that position are stored in the memory, and the data stored in the memory is subjected to arithmetic processing. and a control device for displaying information on the display means.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15447781A JPS5855736A (en) | 1981-09-28 | 1981-09-28 | Analyzing apparatus of density distribution by emission spectrochemical analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15447781A JPS5855736A (en) | 1981-09-28 | 1981-09-28 | Analyzing apparatus of density distribution by emission spectrochemical analysis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5855736A JPS5855736A (en) | 1983-04-02 |
| JPS642214B2 true JPS642214B2 (en) | 1989-01-17 |
Family
ID=15585102
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15447781A Granted JPS5855736A (en) | 1981-09-28 | 1981-09-28 | Analyzing apparatus of density distribution by emission spectrochemical analysis |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5855736A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0629857B2 (en) * | 1986-01-13 | 1994-04-20 | 新日本製鐵株式会社 | Judgment method of surface flaw factor of steel |
| JP2722852B2 (en) * | 1991-04-08 | 1998-03-09 | 住友金属工業株式会社 | Emission spectral analysis method and emission spectral analyzer |
| EP1351049A3 (en) * | 2002-04-01 | 2004-02-25 | Central Iron & Steel Research Institute | Analyzer for metal |
| FR2838827B3 (en) * | 2002-04-19 | 2004-04-02 | Central Iron & Steel Res Inst | ANALYSIS METHOD OF STATISTICAL DISTRIBUTION OF ORIGINAL POSITION FOR A METAL |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57122351A (en) * | 1981-01-21 | 1982-07-30 | Nippon Steel Corp | Method of spectrochemical analysis wherein continuous light emission is utilized |
-
1981
- 1981-09-28 JP JP15447781A patent/JPS5855736A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5855736A (en) | 1983-04-02 |
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