JPH04184155A - Total reflection spectrum measuring device - Google Patents
Total reflection spectrum measuring deviceInfo
- Publication number
- JPH04184155A JPH04184155A JP2312463A JP31246390A JPH04184155A JP H04184155 A JPH04184155 A JP H04184155A JP 2312463 A JP2312463 A JP 2312463A JP 31246390 A JP31246390 A JP 31246390A JP H04184155 A JPH04184155 A JP H04184155A
- Authority
- JP
- Japan
- Prior art keywords
- light
- ray
- white
- measurement
- energy
- 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
- 238000001228 spectrum Methods 0.000 title claims abstract description 22
- 238000005259 measurement Methods 0.000 claims abstract description 34
- 239000013078 crystal Substances 0.000 claims abstract description 19
- 238000001514 detection method Methods 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims description 7
- 230000004907 flux Effects 0.000 claims description 5
- 230000003595 spectral effect Effects 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims 1
- 239000010409 thin film Substances 0.000 abstract description 23
- 238000010586 diagram Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000005469 synchrotron radiation Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000192 extended X-ray absorption fine structure spectroscopy Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000001028 reflection method Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本５１明は、測定試料表面の方位を入射ｘｉ光線に対し
連続的に回転させながら全反射スペクトルを同時に測定
する装置に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to an apparatus for simultaneously measuring a total reflection spectrum while continuously rotating the orientation of a surface of a measurement sample with respect to an incident xi light beam.
〔従来の技術及び発明が解決しようとする課題〕拡張Ｘ
線吸収微細構造（ＥＸＡＦＳ）測定装置は、分光結晶と
して曲結晶を用いた実験室系の装置（テクノス社製等）
が実用化されている。光源として放射光を用いる場合に
は、１つのチャンネルカット分光結晶を用いた高分解能
装置が得られるが、実験室に入手可能な強力光源（回転
対陰極）を用いる限り、感度を落とさずに高分解能を達
成すること実現していない。[Problems to be solved by conventional technology and invention] Expansion X
The line absorption fine structure (EXAFS) measurement device is a laboratory-type device (manufactured by Technos, etc.) that uses a curved crystal as a spectroscopic crystal.
has been put into practical use. When synchrotron radiation is used as a light source, a high-resolution device using a single channel-cut spectroscopic crystal can be obtained, but as long as a powerful light source (rotating anticathode) available in the laboratory is used, high resolution can be obtained without reducing sensitivity. Achieving resolution has not been achieved.
また、全反射を用いた薄膜計測法は、今日の材料デバイ
スで必須な薄膜の構造解析、およびその場観察の技術と
して最適のものである。この計測装置においては、薄膜
に入射するＸ線光束のエネルギーを変化させながら、各
エネルギーごとに、基板上の薄膜に対する入射Ｘ線光束
の入射角を連絖的に変化させ反射率を測定することにな
る。Furthermore, the thin film measurement method using total internal reflection is the most suitable technique for structural analysis of thin films, which is essential for today's material devices, and for in-situ observation. In this measurement device, while changing the energy of the X-ray beam incident on the thin film, the reflectance is measured by continuously changing the angle of incidence of the incident X-ray beam on the thin film on the substrate for each energy. become.
しかしながら、従来の方法では、各エネルギーごとに薄
膜方位（θ）を０−６０分程度走査し反射率の測定を行
なうことになり、また次の走査に移る前に初期のθ：０
に戻さなければならないので、放射光源（シンクロトロ
ン放射）などの高輝度のＸ線源を用いないかぎり、測定
に非常な長時間を必要とするため実現困難である。However, in the conventional method, the reflectance is measured by scanning the thin film orientation (θ) for about 0 to 60 minutes for each energy, and before moving on to the next scan, the initial θ: 0
Therefore, unless a high-brightness X-ray source such as a synchrotron radiation source is used, it is difficult to realize this because the measurement requires a very long time.
本発明はこの点に鑑みなされたもので、回転対陰極Ｘ線
源を用いた実験室系装置で、全反射を用いた薄膜計測を
短時間で測定出来るようにする全反射スペクトル測定装
置を提供することを目的とする。The present invention has been made in view of this point, and provides a total reflection spectrum measuring device that enables thin film measurements using total internal reflection to be performed in a short time using a laboratory device using a rotating anticathode X-ray source. The purpose is to
上記目的を達成するため、本発明によれば、Ｘ線を基板
上の測定試料面に照射し、その吸収、反射あるいは回折
スペクトルを測定することにより基板上の測定試料の構
造評価を行なう全反射スペクトル測定装置において、Ｘ
線源から放出された光束を白色光のまま平行光として測
定試料面に照射させるコリメータ系と、測定試料面から
の反射光束の全エネルギーを各単色光成分ごとに検出す
る分光検出手段と、測定試料面のＸ線光束に対する入射
角を連続的に変化させる機構とを有することを特徴とす
る全反射スペクトル測定装置が提供される。In order to achieve the above object, the present invention provides a total reflection method for evaluating the structure of the measurement sample on the substrate by irradiating the surface of the measurement sample on the substrate with X-rays and measuring its absorption, reflection, or diffraction spectrum. In the spectrum measuring device,
A collimator system that irradiates the light flux emitted from the radiation source as parallel light onto the measurement sample surface as white light; a spectral detection means that detects the total energy of the light flux reflected from the measurement sample surface for each monochromatic light component; A total reflection spectrum measuring device is provided, which is characterized by having a mechanism for continuously changing the incident angle of an X-ray beam on a sample surface.
本発明では、Ｘ線源から放出された光束がコリメータ系
により白色光のまま平行光として測定試料面に照射され
、前記機構により測定試料面が傾けられながら、分光検
出手段が測定試料面からの反射光束の全エネルギーを一
挙にマルチヤンネル検圧する。したがって、１回のθ走
金で計測が行なえるようになり、測定時間が大幅に短縮
される。In the present invention, the light flux emitted from the X-ray source is irradiated onto the measurement sample surface as parallel light while remaining white light by the collimator system, and while the measurement sample surface is tilted by the mechanism, the spectral detection means detects the light beam from the measurement sample surface. The total energy of the reflected light beam is measured in multiple channels at once. Therefore, measurement can be performed with one θ run, and the measurement time is significantly shortened.
以下本発明を実施例により詳細に説明する。 The present invention will be explained in detail below using examples.
、先ず、第２図により、本発明者らが先に提案した全反
射スペクトル測定装置の説明を行なう。同図において１
はＸ線源、２は分光結晶、４は試料系、５は基板、６は
薄膜試料、９は検出器、１０はビームストッパー、５１
−３３はスリット系を示す。Ｘ線源Ｉより射出された白
色Ｘ線は、スリット系Ｓ１により整形され、例えば３１
などの完全に近い単結晶よりなる分光結晶２に入射する
。分光結晶２は、所定の結晶面（例えば、（１１１））
を入射Ｘ線光束に対し所定の方位にセットされ、分光結
晶２により所定のエネルギーのＸ線がブラッグ反射を起
こし射出されるようになっている。こうして、スリット
系Ｓ２を通過したＸ線光束は単色化される。分光結晶２
にはチャンネルカット結晶や複数の結晶を組み合わせた
ものが用いられる。スリットＳ２を通過後の単色、平行
のＸ線光束は、測定すべき薄膜試料６表面に入射され、
薄膜試料６表面からの反射光束がスリット系Ｓ３を介し
て検出器９に入り、反射Ｘ線強度が測定される。薄膜試
料６表面からのＸ線反射率はＸ線光束の入射角度に依存
するので、入射角を変化させながら測定が行なわれる。First, with reference to FIG. 2, a total reflection spectrum measurement apparatus previously proposed by the present inventors will be explained. In the same figure, 1
is an X-ray source, 2 is a spectroscopic crystal, 4 is a sample system, 5 is a substrate, 6 is a thin film sample, 9 is a detector, 10 is a beam stopper, 51
-33 indicates a slit system. The white X-rays emitted from the X-ray source I are shaped by a slit system S1, for example 31
The light enters a spectroscopic crystal 2 made of a nearly perfect single crystal such as . The spectroscopic crystal 2 has a predetermined crystal plane (for example, (111))
is set in a predetermined direction with respect to the incident X-ray beam, and X-rays of a predetermined energy are emitted by the spectroscopic crystal 2 after causing Bragg reflection. In this way, the X-ray beam passing through the slit system S2 is made monochromatic. Spectroscopic crystal 2
Channel-cut crystals or combinations of multiple crystals are used. The monochromatic, parallel X-ray beam after passing through the slit S2 is incident on the surface of the thin film sample 6 to be measured,
The reflected light flux from the surface of the thin film sample 6 enters the detector 9 via the slit system S3, and the reflected X-ray intensity is measured. Since the X-ray reflectance from the surface of the thin film sample 6 depends on the incident angle of the X-ray beam, measurement is performed while changing the incident angle.
すなわち、薄膜試料６表面へのＸ線光束の入射角がθの
とき、検出器９の方位は２θとなるように、薄膜試料６
表面のＸ線光束入射点（ナイフェツジの位ｙｌ（第２図
の８）〕を中心に連動回転を行なう。That is, when the angle of incidence of the X-ray beam on the surface of the thin film sample 6 is θ, the orientation of the detector 9 is 2θ.
Interlocking rotation is performed around the X-ray beam incident point on the surface (knifetsu position yl (8 in FIG. 2)).
ところが、薄膜の全反射スペクトル測定のためには、こ
のような測定を複数エネルギーのＸ線光束に対して繰り
返す必要がある。第３図には３種類のエネルギーＪ＋Ｅ
２＋Ｅ３の場合を示しであるが、分解能を更に向上させ
るためにはより多くのエネルギーのＸ線光束について測
定を繰り返さなければならず、これには莫大な時間がか
かるため改善の余地があった。However, in order to measure the total reflection spectrum of a thin film, it is necessary to repeat such measurements for X-ray beams of multiple energies. Figure 3 shows three types of energy J+E.
The case of 2+E3 is shown, but in order to further improve the resolution, measurements must be repeated for X-ray beams with more energy, and this takes a huge amount of time, so there is room for improvement.
第１図はこのような問題を解決する本発明による全反射
スペクトル測定装置の一実施例の概念図である。同図に
おいて、１１はＸ線源、１２は試料系、１３は基板、】
４は測定すべき薄膜試料、】５は薄膜試料１４表面への
Ｘ線光束入射点、１Ｇはビームストッパ、１７は分光結
晶、１８は位置敏感型Ｘ線検出器、５１１−３１２はス
リット系を示す。FIG. 1 is a conceptual diagram of an embodiment of a total reflection spectrum measuring device according to the present invention that solves such problems. In the figure, 11 is an X-ray source, 12 is a sample system, 13 is a substrate,
4 is a thin film sample to be measured, 5 is an incident point of the X-ray beam onto the surface of the thin film sample 14, 1G is a beam stopper, 17 is a spectroscopic crystal, 18 is a position-sensitive X-ray detector, and 511-312 is a slit system. show.
動作について説明するとＸ線光源１１より射出された白
色Ｘ線はスリット系Ｓｌｌ、３１２により平行光束に整
形された後、白色光のまま薄膜試料１４表面に入射する
。薄膜試料１４表面に対する白色Ｘ線光束の入射角θと
反射された白色Ｘ線光束を検出すべき検出系の方位２θ
は周知の技術で容易に構成しうる機構（図示せず）によ
り連動回転される。なお、実際はθは数十分程度の微小
角であるので回転させる必要はない場合も多い。薄膜試
料１４表面より反射された白色Ｘ線光束は、分光結晶１
７により分光され、位置敏感型Ｘ線検出器１８により受
光される。この位置敏感型Ｘ線検出器１８は単色光成分
ごとにその各受光部位（チャンネル）に検出しうる構成
となっているため、全エネルギースペクトルが同時に検
出される。したがって、本装置によれば、同時に各エネ
ルギーに対し薄膜試料１４表面よりの反射率を測定して
いることになるので、短時間に測定を行なうことが可能
となる。To explain the operation, white X-rays emitted from the X-ray light source 11 are shaped into a parallel beam by the slit system Sll, 312, and then enter the surface of the thin film sample 14 as white light. Incident angle θ of the white X-ray beam with respect to the surface of the thin film sample 14 and orientation 2θ of the detection system that should detect the reflected white X-ray beam
are rotated in conjunction with each other by a mechanism (not shown) that can be easily constructed using well-known technology. Note that in reality, θ is a small angle of about several tens of minutes, so there is often no need to rotate it. The white X-ray beam reflected from the surface of the thin film sample 14 is transmitted to the spectroscopic crystal 1
7 and received by a position-sensitive X-ray detector 18. Since this position-sensitive X-ray detector 18 is configured to be able to detect each monochromatic light component at each light receiving site (channel), the entire energy spectrum is detected simultaneously. Therefore, according to this apparatus, the reflectance from the surface of the thin film sample 14 is measured for each energy at the same time, so that the measurement can be carried out in a short time.
なお、上記実施例では測定試料面からの反射光束の全エ
ネルギーを各単色光成分ごとに検出する手段として、分
光結晶１７と位置敏感型Ｘ線検出器１８との組合せを用
いたが、これに代えてエネルギー分解能を有する半導体
固体素子検出器（ＳＳＤ）を用いることもできる。In the above embodiment, a combination of the spectroscopic crystal 17 and the position-sensitive X-ray detector 18 was used as a means for detecting the total energy of the reflected light beam from the measurement sample surface for each monochromatic light component. Alternatively, a semiconductor solid-state detector (SSD) with energy resolution can also be used.
また、上記では分光結晶１７は透過型（ラウェケース）
の回折を用いているが、反射型（ブラッグケース）の回
折を用いることもできる。In addition, in the above, the spectroscopic crystal 17 is a transmission type (Lawe case).
However, reflection type (Bragg case) diffraction can also be used.
本発明によれば前記構成としたので以下のような効果が
得られる。According to the present invention, with the above configuration, the following effects can be obtained.
実験室で利用できるＸ線源を用いて、薄膜表面からの全
反射スペクトルを複数のエネルギーに対して測定するこ
とが短時間にできるようになる。Using an X-ray source available in the laboratory, it becomes possible to measure the total reflection spectrum from the surface of a thin film for multiple energies in a short time.
従来技術では、莫大な時間を要することになり、同等の
データを得ることは事実上不可能であるが、本装置によ
れば、ただ１回の薄膜試料方位スキャンにより同時の各
エネルギーに対する反射率データが得られるので、各エ
ネルギーごとにスキャンを繰り返し行なった場合に比べ
て、角度の誤差が全く生じない点で優れている。With conventional technology, it takes a huge amount of time and it is virtually impossible to obtain equivalent data, but with this device, the reflectance for each energy simultaneously can be calculated by scanning the thin film sample orientation once. Since data can be obtained, this method is superior to the case where scans are repeatedly performed for each energy in that there is no angular error at all.
また、反射スペクトルの各エネルギー成分をそれぞれ同
時に検出することができるので、莫大な時間を要して反
射スペクトルの測定がほとんど瞬時に出来るようになる
。Furthermore, since each energy component of the reflection spectrum can be detected simultaneously, the measurement of the reflection spectrum can be performed almost instantaneously, instead of requiring a huge amount of time.
第１図は本発明の全反射スペクトル測定装置の一実施例
の概念図、第２図は本発明者が先に提案した全反射スペ
クトル測定装置の概念図、第３図は従来の全反射スペク
トル測定の説明図である。
１１ ・Ｘ線源
１４・・・薄膜試料
１７・・・分光結晶
１８・・位置敏感型Ｘ線検出器
Ｓｌｌ、Ｓｉ２・・・スリット系
特許出願人 株式会社 リ コ −Fig. 1 is a conceptual diagram of an embodiment of the total reflection spectrum measurement device of the present invention, Fig. 2 is a conceptual diagram of the total reflection spectrum measurement device previously proposed by the present inventor, and Fig. 3 is a conceptual diagram of a total reflection spectrum measurement device of the present invention. It is an explanatory diagram of measurement. 11 ・X-ray source 14... Thin film sample 17... Spectroscopic crystal 18... Position-sensitive X-ray detector Sll, Si2... Slit system patent applicant Rico Co., Ltd. -
Claims (3)
反射あるいは回折スペクトルを測定することにより基板
上の測定試料の構造評価を行なう全反射スペクトル測定
装置において、Ｘ線源から放出された光束を白色光のま
ま平行光として測定試料面に照射させるコリメータ系と
、測定試料面からの反射光束の全エネルギーを各単色光
成分ごとに検出する分光検出手段と、測定試料面のＸ線
光束に対する入射角を連続的に変化させる機構とを有す
ることを特徴とする全反射スペクトル測定装置。(1) Irradiate the measurement sample surface on the substrate with X-rays, absorb the
In a total internal reflection spectrum measuring device that evaluates the structure of a measurement sample on a substrate by measuring reflection or diffraction spectra, a collimator system that irradiates the surface of the measurement sample with the light flux emitted from the X-ray source as parallel light while remaining white light. and a spectral detection means for detecting the total energy of the reflected light beam from the measurement sample surface for each monochromatic light component, and a mechanism for continuously changing the incident angle of the measurement sample surface with respect to the X-ray beam. A total reflection spectrum measurement device.
の結合であることを特徴とする請求項１に記載の全反射
スペクトル測定装置。(2) The total reflection spectrum measuring device according to claim 1, wherein the spectroscopic detection means is a combination of a spectroscopic crystal and a position-sensitive detector.
導体固体素子検出器（ＳＳＤ）であることを特徴とする
請求項１記載の全反射スペクトル測定装置。(3) The total reflection spectrum measuring device according to claim 1, wherein the spectroscopic detection means is a semiconductor solid state device detector (SSD) having energy resolution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2312463A JP2921597B2 (en) | 1990-11-17 | 1990-11-17 | Total reflection spectrum measurement device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2312463A JP2921597B2 (en) | 1990-11-17 | 1990-11-17 | Total reflection spectrum measurement device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04184155A true JPH04184155A (en) | 1992-07-01 |
| JP2921597B2 JP2921597B2 (en) | 1999-07-19 |
Family
ID=18029504
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2312463A Expired - Lifetime JP2921597B2 (en) | 1990-11-17 | 1990-11-17 | Total reflection spectrum measurement device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2921597B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004086018A1 (en) * | 2003-03-27 | 2004-10-07 | Rigaku Industrial Corporation | X-ray fluorescence analyzer |
| JP2013514527A (en) * | 2009-12-17 | 2013-04-25 | サーモ フィッシャー サイエンティフィック （エキュブラン） エスアーエールエル | Method and apparatus for performing X-ray analysis of sample |
| DE102016014213A1 (en) * | 2015-12-08 | 2017-07-06 | Shimadzu Corporation | X-RAY SPECTROSCOPIC ANALYSIS DEVICE AND ELEMENTARY ANALYSIS METHOD |
-
1990
- 1990-11-17 JP JP2312463A patent/JP2921597B2/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004086018A1 (en) * | 2003-03-27 | 2004-10-07 | Rigaku Industrial Corporation | X-ray fluorescence analyzer |
| JPWO2004086018A1 (en) * | 2003-03-27 | 2006-06-29 | 理学電機工業株式会社 | X-ray fluorescence analyzer |
| JP2013514527A (en) * | 2009-12-17 | 2013-04-25 | サーモ フィッシャー サイエンティフィック （エキュブラン） エスアーエールエル | Method and apparatus for performing X-ray analysis of sample |
| US9031187B2 (en) | 2009-12-17 | 2015-05-12 | Thermo Fisher Scientific (Ecublens) Sarl | Method and apparatus for performing X-ray analysis of a sample |
| DE102016014213A1 (en) * | 2015-12-08 | 2017-07-06 | Shimadzu Corporation | X-RAY SPECTROSCOPIC ANALYSIS DEVICE AND ELEMENTARY ANALYSIS METHOD |
| US10948434B2 (en) | 2015-12-08 | 2021-03-16 | Shimadzu Corporation | X-ray spectroscopic analysis apparatus and elementary analysis method |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2921597B2 (en) | 1999-07-19 |
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