JPS6398550A - Exafs apparatus of soft x-ray region - Google Patents
Exafs apparatus of soft x-ray regionInfo
- Publication number
- JPS6398550A JPS6398550A JP61242924A JP24292486A JPS6398550A JP S6398550 A JPS6398550 A JP S6398550A JP 61242924 A JP61242924 A JP 61242924A JP 24292486 A JP24292486 A JP 24292486A JP S6398550 A JPS6398550 A JP S6398550A
- Authority
- JP
- Japan
- Prior art keywords
- rays
- incident
- measuring
- intensity
- transmitted
- 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.)
- Pending
Links
- 238000005259 measurement Methods 0.000 claims abstract description 12
- 238000000192 extended X-ray absorption fine structure spectroscopy Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000000523 sample Substances 0.000 claims description 20
- 238000001228 spectrum Methods 0.000 abstract description 8
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract description 3
- 239000010931 gold Substances 0.000 abstract description 3
- 229910052737 gold Inorganic materials 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000005469 synchrotron radiation Effects 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating 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
- G01N23/02—Investigating 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 transmitting the radiation through the material
- G01N23/06—Investigating 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 transmitting the radiation through the material and measuring the absorption
- G01N23/083—Investigating 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 transmitting the radiation through the material and measuring the absorption the radiation being X-rays
- G01N23/085—X-ray absorption fine structure [XAFS], e.g. extended XAFS [EXAFS]
Landscapes
- Health & Medical Sciences (AREA)
- Toxicology (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)
- Analysing Materials By The Use Of Radiation (AREA)
- X-Ray Techniques (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は軟Ｘ線領域のエクザフス（ＢＸＡＦＳ ：Ｅ
ｘｔｅｎｄｅｄ Ｘ−ｒａｙ Ａｂｓｏｒｐｔｉｏｎ
Ｆｉｎｅ ５ｔｒｕｃｔｕｒｅ）装置に係シ、特に精度
のよい測定を行なうために好適なＸ線測定素子に関する
つ
〔従来の技術〕
波長走査できる単色Ｘ線を試料に照射し、試料を透過し
たＸ線強度を測定することによりＸ線吸収スペクトルを
得ることができる。近年、この吸収スペクトルの微細な
振動構造はエクザフスと呼ばれ、吸収原子の周囲の局所
構造を反映しておシ非晶質等物質の状態解析手段として
知らｎている。[Detailed Description of the Invention] [Industrial Application Field] The present invention is directed to soft X-ray region EXAFS (BXAFS: E
xtended X-ray Absorption
Regarding X-ray measurement elements suitable for fine 5 structure) equipment, particularly for performing highly accurate measurements [Prior art] Monochromatic X-rays that can scan the wavelength are irradiated onto a sample, and the intensity of the X-rays transmitted through the sample is measured. By measuring, an X-ray absorption spectrum can be obtained. In recent years, this fine vibrational structure of the absorption spectrum is called an exafus, and it has become known as a means of analyzing the state of materials such as amorphous materials by reflecting the local structure around the absorbing atoms.
同様にして、試料を透過したＸ線の代シに試料から放射
される二次Ｘ線を信号とする蛍光ｇ ＸＡ Ｆ Ｓや試
料からの反射Ｘ線を利用する反射型ＥＸＡＦＳも用いら
れつつあるう
上記ＥＸＡＦＳ装置のＸ線源として、現在のところ電子
線動、起Ｘ線源、シンクロトロン放射光がある。特にシ
ンクロトロン放射光のＸ線強度は従来に比べ１０３〜１
０４程度強いため、測定時間の大巾な短縮や極めて良好
な８７Ｎ比のスペクトルが得られている。Similarly, fluorescent g At present, as the X-ray source for the above-mentioned EXAFS apparatus, there are an electron beam dynamic source, an excitation X-ray source, and a synchrotron radiation source. In particular, the X-ray intensity of synchrotron radiation is 103 to 1
04, the measurement time was greatly shortened and a spectrum with an extremely good 87N ratio was obtained.
ＥＸＡＦＳ装置では、試料を透過、もしくは試料から放
射される信号Ｘ線強度測定の他に必ず入射Ｘ線の強度測
定を同時に行なう。測定された信号Ｘ線には、モノクロ
メータ（単色分光器）の波長特性、Ｘ線強度の時間的変
動等雑音成分が含まれているが、入射Ｘ線にも含まれる
ため単なる割算等のデータ処理によって雑音成分を取除
くことができるからである。また、通常の装置のＸ線強
度測定子は、Ａｒ、ｔｉ２ガス等を封入した電離箱を用
いる。しかし、電離箱の入射窓、出射窓ｖ′ｉ、Ｂｅ膜
やカプトン膜で仕切られているため、軟Ｘ線領域（１０
Å以上）のｇＸＡＦｓスペクトルを得ることができなか
った。In the EXAFS apparatus, in addition to measuring the intensity of signal X-rays transmitted through or emitted from the sample, the intensity of incident X-rays is always measured at the same time. The measured signal X-ray contains noise components such as the wavelength characteristics of the monochromator (monochromatic spectrometer) and temporal fluctuations in X-ray intensity, but since they are also included in the incident X-ray, simple division etc. This is because noise components can be removed through data processing. Further, the X-ray intensity measuring element of a normal device uses an ionization chamber filled with Ar, Ti2 gas, etc. However, since the entrance window and exit window v′i of the ionization chamber are partitioned by a Be film and a Kapton film, the soft X-ray region (10
It was not possible to obtain a gXAFs spectrum of .
従来、試料から放射される電子を信号とする表面Ｌ’Ｘ
ＡＦＳ装置については、サーフエース サイエンス（３
ｕｒｆａｃｅ、 ３ｃｉｅｎｃｅ ） ５０３頁〜５２
４頁（１９８２年第１１７巻）において論じられている
。Conventionally, the surface L'X uses electrons emitted from the sample as a signal.
For AFS equipment, please contact Surf Ace Science (3
surface, 3science) pages 503-52
4 (Vol. 117, 1982).
上記従来技術はｔａ箱の入射窓、出射窓にｆ３ｅ膜、カ
プトン膜を使っているため、軟Ｘ線領域ではそれらの膜
による吸収が著しく、新しい測定素子を考える必要があ
った。Since the above-mentioned conventional technology uses an F3E film and a Kapton film for the entrance and exit windows of the TA box, absorption by these films is significant in the soft X-ray region, and it was necessary to consider a new measurement element.
本発明の目的は軟Ｘ線領域においてもＥＸＡＦＳスペク
トルが得らｎるようにすることにある。An object of the present invention is to enable EXAFS spectra to be obtained even in the soft X-ray region.
上記目的は、入射及び信号Ｘ線強度測定に同一測定原理
でかつ同一材料である固体測定素子を用いることにより
、達成される。しかし、入射測定子は入射光の大部分全
透過させ、一部を検出できるような構造とする。The above object is achieved by using solid-state measurement elements of the same measurement principle and of the same material for incident and signal X-ray intensity measurements. However, the incident probe has a structure that allows most of the incident light to completely pass through and detects only a portion of the incident light.
Ｘ線強度測定用固体素子の測定原理として、固体にＸ線
を照射すると、Ｘ線の強度に応じて光電子量が変化する
ことを利用している。The measurement principle of solid-state elements for measuring X-ray intensity is based on the fact that when a solid is irradiated with X-rays, the amount of photoelectrons changes depending on the intensity of the X-rays.
従って、入射及び信号Ｘ線強度の測定子の受光面を同一
材料で作り、かつ入射測定子のみ入射光の大部分を通過
させ一部だけしか取込まない点は異なるが構造上も信号
測定子と可能な限シ同一にすれば正確な１ＸｋＦｓスペ
クトルを得ることができる。Therefore, although the light-receiving surfaces of the incident and signal X-ray intensity probes are made of the same material, and only the incident probe passes most of the incident light and only takes in a portion, the structure of the signal probe is also different. An accurate 1XkFs spectrum can be obtained by making it as similar as possible.
もし、再考の測定子受光面の材料もしくは構造が異なる
場合、波長に対して入射Ｘ線が一様だったとしても材料
の違いによる吸収端及び波長に対する吸収の程度の差を
生ずる。そのため、測定子の波長に対する感度特性が変
ってしまい信頼性のあるＥＸＡＦＳスペクトルを得るこ
とができない。If the material or structure of the light-receiving surface of the probe to be reconsidered is different, even if the incident X-rays are uniform with respect to the wavelength, differences in the absorption edge and the degree of absorption with respect to the wavelength will occur due to the difference in the material. Therefore, the wavelength sensitivity characteristics of the probe change, making it impossible to obtain a reliable EXAFS spectrum.
以下、本発明の一実施例を第１図にニジ説明する。本実
施例は光源としてシンクロトロン放射光を利用した例で
、図は軟Ｘ線領域のＥＸＡＦ８装置を示す。An embodiment of the present invention will be described below with reference to FIG. This embodiment is an example in which synchrotron radiation is used as a light source, and the figure shows an EXAF8 apparatus in the soft X-ray region.
図の１はシンクロトロン、２は上記シンクトロンｌから
発生した連続Ｘ線、３は軟Ｘ線領域の波長走査が可能な
モノクロメータ、４は上記モノクロメータ３によって単
色化された軟ＸＳ、Ｓは入射Ｘ線強度測定装置、６は上
記測定装置５の構成要素の一つである測定子で金蒸着し
たメツシュ、７は測定子６から放出された光電子を増幅
するための電子増倍管、８は試料、９は透過Ｘ線強度測
定装置、ｌＯｖ′ｉ上記測定装置９の測定子で金蒸着し
た板、１１は測定子１０から放出された光電子を増幅す
るための電子増倍管、１２は透過Ｘ線強度を入射Ｘ線強
度で割る除算回路、１３は記録するためのＸ−Ｙレコー
ダである。In the figure, 1 is a synchrotron, 2 is a continuous X-ray generated from the synchtron 1, 3 is a monochromator capable of wavelength scanning in the soft X-ray region, and 4 is a soft XS, which is made monochromatic by the monochromator 3. is an incident X-ray intensity measuring device; 6 is a gold-deposited measuring tip which is one of the components of the measuring device 5; 7 is an electron multiplier tube for amplifying photoelectrons emitted from the measuring tip 6; 8 is a sample, 9 is a transmitted X-ray intensity measuring device, lOv'i is a gold-deposited plate with a probe of the measurement device 9, 11 is an electron multiplier tube for amplifying photoelectrons emitted from the probe 10, 12 1 is a division circuit that divides the transmitted X-ray intensity by the incident X-ray intensity, and 13 is an X-Y recorder for recording.
シンクロトロン１から放射された連続軟Ｘ線２のうち、
モノクロメータ３によって特定な波長のＸ線４が試料８
に照射される。試料８を透過したＸ線の強度は測定装置
９によって測定される。除算回路１２を用いて、この出
力を入射Ｘ線強度測定装置５の出力で割算し、その結果
ｔ−ｘ−ｙレコーダ１３に表示し記録する。Of the continuous soft X-rays 2 emitted from the synchrotron 1,
A monochromator 3 sends X-rays 4 of a specific wavelength to a sample 8.
is irradiated. The intensity of the X-rays transmitted through the sample 8 is measured by a measuring device 9. This output is divided by the output of the incident X-ray intensity measuring device 5 using the division circuit 12, and the result is displayed and recorded on the txy recorder 13.
透過Ｘ線の強度は、透過光の光路上に金膜をコーティン
グした板１０を置き、そこから発生する光電子を電子増
倍管１１で増幅した後の電流値を測定することによって
得られる。この時透過Ｘ線の強度と上記電流値は必ずし
も比例関係圧なっていない。測定子である金板１０での
吸収構造が上記電流値に含まれているからである。従っ
て、透過Ｘ線強度測定装置９と全く同一のものを入射Ｘ
線強度測定装置５として使い、測定子による波長の感度
依存の影響を取除けば良い。しかし、大部分の光を透過
させ−る必要があるため、受光面はメツシュあるいは中
心部がくりぬかれている構造でなければならない。以上
本発明の実施例によれば、透過Ｘ線強度測定装置９の出
力を入射Ｘ線強度測定装置ｉｔ５の出力で割れば、測定
子がもつ波長に対する感度特性を取シ除くことができ、
かつモノクロメータ３の感度特性による影響、光源光２
の不安定等の雑音成分を取）除くことができる。The intensity of the transmitted X-rays can be obtained by placing a plate 10 coated with a gold film on the optical path of the transmitted light, and measuring the current value after amplifying photoelectrons generated from the plate 10 with an electron multiplier 11. At this time, the intensity of the transmitted X-rays and the above-mentioned current value are not necessarily in a proportional relationship. This is because the absorption structure of the metal plate 10, which is the measuring element, is included in the above current value. Therefore, the incident X
It is sufficient to use it as the line intensity measuring device 5 to remove the influence of wavelength sensitivity dependence due to the probe. However, since it is necessary to transmit most of the light, the light-receiving surface must have a mesh or a structure in which the center is hollowed out. As described above, according to the embodiment of the present invention, by dividing the output of the transmitted X-ray intensity measuring device 9 by the output of the incident X-ray intensity measuring device it5, it is possible to remove the wavelength sensitivity characteristic of the probe.
and the influence of the sensitivity characteristics of monochromator 3, light source light 2
Noise components such as instability can be removed.
さらに、入射光に対する測定子６及び測定子１０の入射
角も同一にする等構造上においても可能な限シ同一にす
れば、よシ忠実な軟Ｘ線領域のＥＸＡＦ Ｓスペクトル
を得ることができる。Furthermore, if the angles of incidence of the measuring element 6 and measuring element 10 with respect to the incident light are made the same as much as possible in terms of structure, a very faithful EXAF S spectrum in the soft X-ray region can be obtained. .
本発明によれば、入射Ｘ線と信号Ｘ線の測定に同一材料
の受光面、はぼ同一な構造をもつ測定子を用いているの
で精度のよいＥＸＡＦＳスペクトルを得ることができる
。According to the present invention, since a measuring element having a light-receiving surface made of the same material and having almost the same structure is used to measure incident X-rays and signal X-rays, a highly accurate EXAFS spectrum can be obtained.
第１図は不発明の一実施例で、軟Ｘ線領域のＥＸＡＦＳ
装置の構成を示す模式図である。Figure 1 shows an embodiment of the invention, in which EXAFS in the soft X-ray region
FIG. 2 is a schematic diagram showing the configuration of the device.
Claims (1)
軟Ｘ線を単色化し、かつ波長走査できるモノクロメータ
（単色分光器）、試料に入射する単色Ｘ線の一部を検出
できる測定子及び試料を透過した、もしくは試料から放
射された信号Ｘ線強度の測定が可能な検出器から構成さ
れるエクザフス装置において、入射Ｘ線強度をモニター
する固体測定子と信号Ｘ線強度を検出する固体測定子は
同一測定原理でかつ受光面の材料が同一であることを特
徴とする軟Ｘ線領域のエクザフス装置。1. A device that generates continuous X-rays, a monochromator that monochromates the soft X-rays of the generated continuous X-rays and can scan the wavelength, and a measurement device that can detect a portion of the monochromatic X-rays incident on the sample. The EXAFS device consists of a detector capable of measuring the intensity of signal X-rays transmitted through or emitted from the sample. This is an EXAFS device in the soft X-ray region, in which the solid-state probe uses the same measurement principle and the material of the light-receiving surface is the same.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61242924A JPS6398550A (en) | 1986-10-15 | 1986-10-15 | Exafs apparatus of soft x-ray region |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61242924A JPS6398550A (en) | 1986-10-15 | 1986-10-15 | Exafs apparatus of soft x-ray region |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6398550A true JPS6398550A (en) | 1988-04-30 |
Family
ID=17096233
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61242924A Pending JPS6398550A (en) | 1986-10-15 | 1986-10-15 | Exafs apparatus of soft x-ray region |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6398550A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06151089A (en) * | 1992-11-09 | 1994-05-31 | Rigaku Corp | X-ray analyzing device and x-ray analyzing method |
| WO1999015885A1 (en) * | 1997-09-19 | 1999-04-01 | Japan Science And Technology Corporation | High vacuum xafs measuring instrument |
-
1986
- 1986-10-15 JP JP61242924A patent/JPS6398550A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06151089A (en) * | 1992-11-09 | 1994-05-31 | Rigaku Corp | X-ray analyzing device and x-ray analyzing method |
| WO1999015885A1 (en) * | 1997-09-19 | 1999-04-01 | Japan Science And Technology Corporation | High vacuum xafs measuring instrument |
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