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JPH0136061B2 - - Google Patents
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JPH0136061B2 - - Google Patents

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Publication number
JPH0136061B2
JPH0136061B2 JP55164464A JP16446480A JPH0136061B2 JP H0136061 B2 JPH0136061 B2 JP H0136061B2 JP 55164464 A JP55164464 A JP 55164464A JP 16446480 A JP16446480 A JP 16446480A JP H0136061 B2 JPH0136061 B2 JP H0136061B2
Authority
JP
Japan
Prior art keywords
sample
slit
ray
straight line
rays
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
Application number
JP55164464A
Other languages
Japanese (ja)
Other versions
JPS5788354A (en
Inventor
Teruji Hirai
Gen Date
Fukuo Zenitani
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shimadzu Corp
Original Assignee
Shimadzu Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp filed Critical Shimadzu Corp
Priority to JP55164464A priority Critical patent/JPS5788354A/en
Publication of JPS5788354A publication Critical patent/JPS5788354A/en
Publication of JPH0136061B2 publication Critical patent/JPH0136061B2/ja
Granted legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/20Investigating 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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/207Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
    • G01N23/2076Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions for spectrometry, i.e. using an analysing crystal, e.g. for measuring X-ray fluorescence spectrum of a sample with wavelength-dispersion, i.e. WDXFS
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/22Investigating 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
    • G01N23/223Investigating 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 by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence

Landscapes

  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Dispersion Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Description

【発明の詳細な説明】 本発明は比較的広い範囲の分析を行うX線分析
装置に関する。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an X-ray analyzer that performs analysis over a relatively wide range.

試料面をX線或は電子線等の励起線で照射し試
料から放射されるX線を分光する分析法によつて
比較的大きな試料の広い面全体にわたつて含有元
素の濃度分布を測定する場合、元来この分析方法
は試料の微小面積部分の分析を行う方法なので、
試料面を2次元的に走査しながら分析する必要が
ある。今一例として鋼材の100×100mmの範囲につ
いて、S(硫横)の濃度分布を感度0.005%で、1
mm角の分解能で分析する場合、励起線として電子
線を用いると照射電流1μAでSの特性X線SKαの
S100%における信号強度は10CPS/μAであり、
S/N比500の場合一点の分析に約4秒を要し、
100×100mmの面積を1mmずつ4秒かけて分析する
と全体で約11時間を要することになる。
The concentration distribution of contained elements is measured over the entire wide surface of a relatively large sample using an analysis method that irradiates the sample surface with excitation rays such as X-rays or electron beams and spectrally spectra the X-rays emitted from the sample. In this case, this analysis method originally analyzes a small area of the sample, so
It is necessary to analyze the sample surface while scanning it two-dimensionally. As an example, for an area of 100 x 100 mm of steel material, the concentration distribution of S (sulfur side) is calculated at a sensitivity of 0.005%.
When analyzing with a resolution of mm square, when an electron beam is used as the excitation beam, the characteristic X-ray SKα of S is
The signal strength at S100% is 10CPS/μA,
When the S/N ratio is 500, it takes about 4 seconds to analyze one point.
If you analyze an area of 100 x 100 mm every 1 mm in 4 seconds, it will take about 11 hours in total.

本発明は広い面積を有する試料のその面積全体
にわたる元素の濃度分布測定を短時間で完了し得
るようにしたX線分析装置を提供しようとするも
のである。
The present invention aims to provide an X-ray analyzer that can complete the measurement of the concentration distribution of elements over the entire area of a sample having a large area in a short time.

本発明X線分析装置は平面分光結晶或は円筒状
湾曲分光結晶と波長分解のためのスリツトと同ス
リツトの後方に置かれたX線検出器とよりなるX
線分光器において、上記スリツトの前方或は後方
でX線検出器との間に、上記スリツトの長さ方向
に一定間隔でかつ上記長さ方向と直交するように
複数の仕切板を配置し、上記X線検出器を上記ス
リツトの長さ方向に位置分解能を有するX線検出
器とし、試料をその表面が上記X線分光器がにら
む一直線に沿うように配置して、同試料表面の上
記一直線に沿い、或はその一直線を含む二次元的
広がりを有する領域に励起線を照射するように励
起線源を配置し、試料面上で上記一直線が自身と
直交する方向に移動するよう試料を移動させるよ
うにしたものである。
The X-ray analyzer of the present invention consists of a flat spectroscopic crystal or a cylindrical curved spectroscopic crystal, a slit for wavelength resolution, and an X-ray detector placed behind the slit.
In the line spectrometer, a plurality of partition plates are arranged between the X-ray detector and the front or rear of the slit at regular intervals in the length direction of the slit and perpendicular to the length direction, The X-ray detector is an X-ray detector having a positional resolution in the length direction of the slit, and the sample is arranged so that its surface is along the straight line that the X-ray spectrometer faces, and the sample surface is aligned with the straight line. An excitation radiation source is arranged so as to irradiate an excitation radiation to a two-dimensional area that includes the straight line or along the straight line, and the sample is moved so that the straight line moves in a direction perpendicular to itself on the sample surface. It was designed to let you do so.

上記構成によるとスリツトの前方或は後方にス
リツトの長さ方向と直交して多数の仕切板が一定
間隔で配置され、X線検出器が上記スリツトの長
さ方向に位置分解能を有するので、X線分光器は
試料面上で上記スリツトと平行な一本の直線をに
み、かつ、X線分光器の位置分解能によつて試料
面上の上記一直線に沿う元素分布が一度に測定で
き、試料面上で上記一直線を自身と直角の方向に
移動させるように試料或はX線分光器を移動させ
れば、試料面の一次元的な走査で試料面の面分析
ができることになる。以下実施例によつて本発明
を説明する。
According to the above configuration, a large number of partition plates are arranged at regular intervals in front of or behind the slit, perpendicular to the length direction of the slit, and the X-ray detector has positional resolution in the length direction of the slit. The line spectrometer observes a straight line parallel to the slit on the sample surface, and the positional resolution of the X-ray spectrometer allows the element distribution along the straight line on the sample surface to be measured at once. If the sample or the X-ray spectrometer is moved so as to move the above-mentioned straight line on the surface in a direction perpendicular to itself, the surface of the sample surface can be analyzed by one-dimensional scanning of the sample surface. The present invention will be explained below with reference to Examples.

第1図は本発明の一実施例を示す。1はX線源
で試料2表面を全面的に照射している。3は円筒
面湾曲結晶であり、湾曲結晶の表面中心を通る円
筒面の一母線を図に鎖線で示す。試料面上の一直
線xはこの母線と平行であり、4はスリツト群
で、上記母線と平行方向に延びた波長分解のため
の一つのスリツト41と、このスリツト41の長
さ方向に一定間隔、例えば1mm間隔で長さ方向と
直交するように並べられた、試料面上の位置分解
のための仕切板42とよりなり、この仕切板で仕
切られた一区切ずつを一個のスリツトとしたもの
で、仕切板42の背後にX線検出器5を配置して
ある。このX線検出器はX線用一次元固体撮像素
子である。
FIG. 1 shows an embodiment of the invention. 1 is an X-ray source that irradiates the entire surface of the sample 2. 3 is a cylindrical curved crystal, and one generatrix of the cylindrical surface passing through the center of the surface of the curved crystal is shown by a chain line in the figure. A straight line x on the sample surface is parallel to this generatrix, and 4 is a group of slits, including one slit 41 for wavelength resolution extending in a direction parallel to the generatrix, and slits 41 arranged at regular intervals in the length direction of this slit 41. For example, it consists of partition plates 42 arranged perpendicularly to the length direction at 1 mm intervals for position resolution on the sample surface, and each section separated by the partition plates is one slit. , an X-ray detector 5 is arranged behind the partition plate 42. This X-ray detector is a one-dimensional solid-state imaging device for X-rays.

試料面上の一直線xと分光結晶3とスリツト群
内のスリツト41とは直線xと直交する一平面上
に想定されたローランド円上にあるように機構的
に連結されてX線分光器を構成している。従つて
試料面上の直線xは上記分光器がにらんでいる直
線である。試料2はX線で照射され試料からは蛍
光X線が放射される。この蛍光X線が上記分光器
によつて分光される。分光結晶3とスリツト群4
との位置関係を変えると蛍光X線が分光される。
そこで例えば鋼材の断面のSの濃度分布を測定す
る場合、分光結晶3およびスリツト群4の位置を
適当に調正してSの特性X線SKαがスリツト4
1を通して検出器5に入射するようにすればよ
い。仕切板42はスリツト41の長さ方向と直交
しているので、相隣る二枚の仕切板の延長平面が
試料面上で直線xと交わる2点間から放射された
X線が上記二枚の仕切板間を通つてX線検出器5
に入射する。従つて、X線検出器5の受線面には
試料面上の直線xに沿うSのSKα線による分布
像が形成されている。検出器5はX線用固体撮像
素子でその出力を順次読出してメモリに記憶させ
る。試料面上の一本の線xについてデータをとり
終つたら試料2を線xと直角の方向に所定量、例
えば1mm移動させて再びデータをとる。一本の線
につき4秒位かければよい。固体撮像素子の代り
にスリツト4の背後に蛍光板を配置し、蛍光像を
イメージインテンシフアイヤで増強して感光フイ
ルムに記録し或は蛍光像を固体撮像素子を用いて
映像信号に変換したりメモリに記録させるように
してもよい。
A straight line x on the sample surface, the spectroscopic crystal 3, and the slit 41 in the slit group are mechanically connected so that they are on a Rowland circle assumed to be on a plane orthogonal to the straight line x, forming an X-ray spectrometer. are doing. Therefore, the straight line x on the sample surface is the straight line that the spectroscope is looking at. The sample 2 is irradiated with X-rays and fluorescent X-rays are emitted from the sample. This fluorescent X-ray is separated into spectra by the spectroscope. Spectroscopic crystal 3 and slit group 4
By changing the positional relationship with the fluorescent X-rays, the fluorescent X-rays are separated into spectra.
For example, when measuring the concentration distribution of S in a cross section of a steel material, the positions of the spectroscopic crystal 3 and the slit group 4 are adjusted appropriately so that the characteristic X-rays SKα of S
1 and enter the detector 5. Since the partition plate 42 is perpendicular to the length direction of the slit 41, the X-rays emitted from the two points where the extended planes of two adjacent partition plates intersect with the straight line x on the sample surface The X-ray detector 5 passes between the partition plates of
incident on . Therefore, a distribution image of S SKα rays along the straight line x on the sample surface is formed on the receiving surface of the X-ray detector 5. The detector 5 is an X-ray solid-state imaging device, and its output is sequentially read out and stored in a memory. When data have been taken for one line x on the sample surface, the sample 2 is moved by a predetermined amount, for example 1 mm, in a direction perpendicular to the line x, and data is taken again. It should take about 4 seconds for each line. A fluorescent screen is placed behind the slit 4 instead of the solid-state image sensor, and the fluorescent image is intensified with an image intensifier and recorded on a photosensitive film, or the fluorescent image is converted into a video signal using the solid-state image sensor or stored in a memory. It may also be possible to have it recorded.

第2図は本発明の他の実施例装置を示す。1は
励起線源、6は一次元スリツトで試料2面上の一
直線xに沿つて微小幅の範囲にだけ励起線が照射
されるようにする。3は平面分光結晶、4は第1
図の4と同じスリツト群であり、スリツト群4よ
り後の構成は第1図の実施例と同じである。分光
結晶3及びスリツト群4はリンク機構7に取付け
られ、スリツト群4をガイド8に沿つて左右に動
かすと、角度θが変わり、スリツト群4のガイド
8上の或る位置で試料2から放射される特定波長
のX線についてブラツグの回析条件が成立し、そ
の波長のX線を出す元素の直線xに沿う分布が測
定できる。試料2が直線xと直角の方向に移動で
きることは云うまでもない。
FIG. 2 shows another embodiment of the invention. 1 is an excitation line source, and 6 is a one-dimensional slit so that the excitation line is irradiated only over a very narrow range along a straight line x on the surface of the sample 2. 3 is a plane spectroscopic crystal, 4 is the first
This is the same slit group as 4 in the figure, and the structure after slit group 4 is the same as the embodiment in FIG. The spectroscopic crystal 3 and the slit group 4 are attached to a link mechanism 7, and when the slit group 4 is moved left and right along the guide 8, the angle θ changes, and the radiation from the sample 2 is emitted from the sample 2 at a certain position on the guide 8 of the slit group 4. Bragg's diffraction conditions are established for X-rays of a specific wavelength, and the distribution of elements that emit X-rays of that wavelength along the straight line x can be measured. It goes without saying that the sample 2 can move in a direction perpendicular to the straight line x.

上述実施例では仕切板42はスリツト41の後
側に配置されているが、これはスリツト41の前
側でもよい。本発明X線分析装置は上述したよう
な構成で試料面上の一直線に沿つて同時に分析を
完了できるから広い面の二次元的な分析でも時間
的には一方向走査による一次元的な領域の分析と
同じ時間を要するだけであり、始めに述べた例に
ついて例えば点状領域毎に一万点について分析す
るのに11時を要する所をその1/100の約7分程し
か要しないで、大型試料の広い面積の全体にわた
る分析が非常に能率化される。
In the above embodiment, the partition plate 42 is arranged at the rear side of the slit 41, but it may also be arranged at the front side of the slit 41. The X-ray analyzer of the present invention has the above-mentioned configuration and can simultaneously complete analysis along a straight line on the sample surface, so even two-dimensional analysis of a wide surface can be performed in a one-dimensional area by scanning in one direction. It only takes the same amount of time as the analysis, and in the example mentioned at the beginning, for example, it would take 11 o'clock to analyze 10,000 points for each point area, but it takes only about 7 minutes, 1/100 of that time. Analysis over large areas of large samples is greatly streamlined.

【図面の簡単な説明】[Brief explanation of drawings]

第1図は本発明の一実施例装置の斜視図、第2
図は本発明の他の実施例装置の斜視図である。 1……励起線源、2……試料、3……分光結
晶、4……スリツト群、5……X線検出器。
FIG. 1 is a perspective view of an apparatus according to an embodiment of the present invention, and FIG.
The figure is a perspective view of a device according to another embodiment of the present invention. 1... Excitation ray source, 2... Sample, 3... Spectroscopic crystal, 4... Slit group, 5... X-ray detector.

Claims (1)

【特許請求の範囲】[Claims] 1 平面分光結晶或は円筒状湾曲分光結晶と波長
分解のための細長スリツトと、同スリツトの後方
に置かれ、上記スリツトの長さ方向に位置分解能
を有するX線検出器と、同X線検出器の前方に配
置され、上記スリツトをその長さ方向に複数の区
画に区分する仕切板とでX線分光器を構成し、試
料をその表面が上記X線分光器がにらむ一直線に
沿うように配置して、同試料表面上の上記一直線
に沿い、或は試料面全面に励起線を照射するよう
に励起線源を配置し、試料面上で上記一直線が自
身と直交する方向に移動するように試料を移動さ
せるようにしたX線分析装置。
1. A flat spectroscopic crystal or a cylindrical curved spectroscopic crystal, an elongated slit for wavelength resolution, an X-ray detector placed behind the slit and having a positional resolution in the longitudinal direction of the slit, and the same X-ray detector. An X-ray spectrometer is configured with a partition plate that is placed in front of the device and divides the slit into a plurality of sections in the length direction, and the sample is placed so that the surface thereof is along a straight line that the X-ray spectrometer faces. The excitation radiation source is placed so as to irradiate the excitation ray along the straight line on the sample surface or the entire surface of the sample, and so that the straight line moves in a direction perpendicular to itself on the sample surface. An X-ray analyzer that moves the sample.
JP55164464A 1980-11-21 1980-11-21 X-ray analysing apparatus Granted JPS5788354A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP55164464A JPS5788354A (en) 1980-11-21 1980-11-21 X-ray analysing apparatus

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP55164464A JPS5788354A (en) 1980-11-21 1980-11-21 X-ray analysing apparatus

Publications (2)

Publication Number Publication Date
JPS5788354A JPS5788354A (en) 1982-06-02
JPH0136061B2 true JPH0136061B2 (en) 1989-07-28

Family

ID=15793666

Family Applications (1)

Application Number Title Priority Date Filing Date
JP55164464A Granted JPS5788354A (en) 1980-11-21 1980-11-21 X-ray analysing apparatus

Country Status (1)

Country Link
JP (1) JPS5788354A (en)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63139238A (en) * 1986-12-01 1988-06-11 Natl Inst For Res In Inorg Mater Simple one-dimensional scanning X-ray diffraction microscope
JPS63139298A (en) * 1986-12-01 1988-06-11 科学技術庁無機材質研究所長 Simple one-dimensional scanning X-ray diffraction microscope with monochromator
JPH0727080B2 (en) * 1986-12-02 1995-03-29 科学技術庁無機材質研究所長 One-dimensional scanning X-ray diffraction microscope
JPH077120B2 (en) * 1986-12-02 1995-01-30 科学技術庁無機材質研究所長 Scanning X-ray diffraction microscope with one-dimensional position detector
EP0553911A1 (en) * 1992-01-27 1993-08-04 Koninklijke Philips Electronics N.V. Position-sensitive X-ray analysis
KR20200002951A (en) * 2017-05-18 2020-01-08 가부시키가이샤 시마즈세이사쿠쇼 X-ray spectroscopy device
JP2019211252A (en) * 2018-05-31 2019-12-12 キヤノン株式会社 Identification device
DE102024111885A1 (en) * 2024-04-27 2025-10-30 Institut für angewandte Photonik e. V. Method and apparatus for detecting the element lithium

Also Published As

Publication number Publication date
JPS5788354A (en) 1982-06-02

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