JPH01167642A - Thin-film x-ray diffraction device - Google Patents
Thin-film x-ray diffraction deviceInfo
- Publication number
- JPH01167642A JPH01167642A JP62328011A JP32801187A JPH01167642A JP H01167642 A JPH01167642 A JP H01167642A JP 62328011 A JP62328011 A JP 62328011A JP 32801187 A JP32801187 A JP 32801187A JP H01167642 A JPH01167642 A JP H01167642A
- Authority
- JP
- Japan
- Prior art keywords
- ray
- sample
- angle
- slit
- diffracted
- 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
- 238000002233 thin-film X-ray diffraction Methods 0.000 title claims description 9
- 238000002441 X-ray diffraction Methods 0.000 claims description 6
- 230000035515 penetration Effects 0.000 abstract description 13
- 239000010409 thin film Substances 0.000 abstract description 9
- 101700004678 SLIT3 Proteins 0.000 abstract description 2
- 102100027340 Slit homolog 2 protein Human genes 0.000 abstract description 2
- 101710133576 Slit homolog 2 protein Proteins 0.000 abstract description 2
- 102100027339 Slit homolog 3 protein Human genes 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 abstract description 2
- 230000003247 decreasing effect Effects 0.000 abstract 2
- 230000003287 optical effect Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 238000004381 surface treatment 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〕
本発明は薄膜試料や表面処理材の構造解析、及び金属表
面酸化膜等の評価に適用されるＸ線回折装置に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to an X-ray diffraction apparatus that is applied to structural analysis of thin film samples and surface treatment materials, and evaluation of metal surface oxide films and the like.
従来の薄膜Ｘ線回折装置における光学系の一例を第３図
に、またＸ線の侵入深さと回折Ｘ線が試料面とのなす角
の関係を示すグラフを第４図に各々示す。An example of the optical system in a conventional thin film X-ray diffraction apparatus is shown in FIG. 3, and FIG. 4 is a graph showing the relationship between the penetration depth of X-rays and the angle formed by the diffracted X-rays with the sample surface.
第３図において０１は所定の対陰極を有するＸ線管球、
０２は入射側ソーラスリット、ｏ３は発散スリット、０
４は試料、０５は散乱スリット、０６は受光側ソーラス
リット、０７はモノクロメータ、０８はＸ線検出器であ
る。In Fig. 3, 01 is an X-ray tube having a predetermined anticathode;
02 is the incident side solar slit, o3 is the divergence slit, 0
4 is a sample, 05 is a scattering slit, 06 is a solar slit on the light receiving side, 07 is a monochromator, and 08 is an X-ray detector.
上記の構成でＸ線管球０１から発生したＸ線０９は、ソ
ーラスリット０２、発散スリット０３を通り試料０４表
面に照射される。試料０４表面で回折された回折Ｘ線０
１０は更に散乱スリブ）０５受光側ンーラスリツト０６
を通り、モノクロメータ０７で反射されてＸ線検出器０
８に到達する。ここで、Ｘ線管球０１から発生したＸ線
ｏ９と試料０４面のなす角αは機構的にＸ線０９の侵入
深さを小さくし、回折に寄与する薄膜の相対的体積を増
大させるため、低角度（通常α＝２°〜２．５°）に固
定される。また、試料０４面と回折Ｘ線０１０のなす角
βは回折パターン（回折角βとＸ線検出器０８に導かれ
たＸ線量の関係）を得るために任意に変えられる。With the above configuration, X-rays 09 generated from the X-ray tube 01 pass through the solar slit 02 and the divergent slit 03 and are irradiated onto the surface of the sample 04. Diffracted X-ray 0 diffracted on the surface of sample 04
10 is a scattering slit) 05 light receiving side slit 06
is reflected by the monochromator 07 and sent to the X-ray detector 0.
Reach 8. Here, the angle α between the X-ray o9 generated from the X-ray tube 01 and the surface of the sample 04 mechanically reduces the penetration depth of the X-ray 09 and increases the relative volume of the thin film contributing to diffraction. , is fixed at a low angle (usually α=2° to 2.5°). Further, the angle β between the surface of the sample 04 and the diffracted X-rays 010 can be arbitrarily changed in order to obtain a diffraction pattern (the relationship between the diffraction angle β and the amount of X-rays guided to the X-ray detector 08).
（発明が解決しようとする問題点〕
前述のように従来の薄膜Ｘ線回折装置では、入射Ｘ線を
低角入射して、機構的にＸ線の侵入深さを小さくし回折
に寄与する薄膜の相対的体積を増大させである。しかし
、更に薄い膜の測定にはこれだけでは不充分なことが多
い。(Problems to be Solved by the Invention) As mentioned above, in conventional thin film X-ray diffraction devices, incident X-rays are incident at a low angle to mechanically reduce the penetration depth of X-rays, and a thin film that contributes to diffraction is used. However, this alone is often insufficient for measurements of thinner films.
次に試料に対するＸ線の侵入深さについて考察してみる
。Next, let's consider the penetration depth of X-rays into the sample.
回折Ｘ線の積分強度は次の第１式で与えられる。The integrated intensity of diffracted X-rays is given by the following first equation.
ただし、■０は入射Ｘ線の強度、ａは入射Ｘ線を反射す
るような正しい方向にある結晶粒の体積比率、ｂは単位
体積の結晶によって回折されるエネルギーの入射エネル
ギーに対する比率、αは入射ｘｉと試料面のなす角、β
は回折Ｘ線と試料面のなす角、μは試料の線吸収係数、
Ｘは回折に寄与する層の表面からの距離、ｄｌは回折に
寄与する層の厚さである。where ■0 is the intensity of the incident X-ray, a is the volume ratio of crystal grains in the correct direction to reflect the incident X-ray, b is the ratio of the energy diffracted by a unit volume of crystal to the incident energy, and α is The angle between the incident xi and the sample surface, β
is the angle between the diffracted X-ray and the sample surface, μ is the linear absorption coefficient of the sample,
X is the distance from the surface of the layer contributing to diffraction, and dl is the thickness of the layer contributing to diffraction.
ここで、無限の厚さの試料によって回折された全回折強
度の比として、上記の層による回折強度を示すと、未知
の定数Ｉ％ａ、ｂが消去されて便利である。Here, it is convenient to express the diffraction intensity by the above layer as a ratio of the total diffraction intensity diffracted by a sample of infinite thickness, as this eliminates the unknown constants I%a,b.
その比をＲｘとすると、次の第２式で与えられる。If the ratio is Rx, it is given by the following second equation.
Ｘ＝ギｘ ｘニー〇ＲＸ ＝ Ｊ
ａｌ、、／Ｊ ｄｌ。X = Gi x x Knee RX = J
al,,/J dl.
ｘ−ｏ ｘ＝。x−o x=.
＝ １−１ｚｐ （−ｐｚ （１βｎα＋ｌ／ｓｉｎβ
））・・第２式第２式から明らかなように、薄膜のＸ線
回折パターンを得るときは入射Ｘ線と試料面のなす角α
を小さくすると同時に、回折Ｘ線と試料面のなす角βも
小さくするのが望ましい。= 1-1zp (-pz (1βnα+l/sinβ
))...2nd equation As is clear from the 2nd equation, when obtaining the X-ray diffraction pattern of a thin film, the angle α between the incident X-ray and the sample surface is
It is desirable to reduce the angle β between the diffracted X-ray and the sample surface at the same time.
Ｘ線の侵入深さの一例として、回折Ｘ線と試料面のなす
角βを変化させた場合について３ｉに対するＣｕＫαの
侵入深さをＲＸ＝０．９９ で算出して第４図に示した
。この第４図からもβを低角度（β＝２°）で固定した
方がＸ線の侵入深さが高角度の約％となり、薄膜試料の
測定に有利なことが分かる。As an example of the penetration depth of X-rays, the penetration depth of CuKα with respect to 3i was calculated as RX=0.99 when the angle β between the diffracted X-rays and the sample surface was changed, and is shown in FIG. It can also be seen from FIG. 4 that when β is fixed at a low angle (β=2°), the X-ray penetration depth is approximately % of that at a high angle, which is advantageous for measuring thin film samples.
本発明は上記問題点を解決するために回折Ｘ線と試料面
のな丁角βを低角度で一定にしてＸ線回折パターンを得
るために散乱スリット、受光側ソーラスリット及びモノ
クロメータを試料面と平行な方向に走査する構造となる
。すなわち、Ｘ線管球、発散スリット、試料保持台、散
乱スリット、Ｘ線検出器等からなるＸ線回折装置におい
て、前記Ｘ線管球から照射された入射Ｘ＠と前記試料保
持台上の試料面とのなす角、及び同試料面で回折された
回折Ｘ線と同試料面とのなす角を低角度に固定し、前記
散乱スリット及び前記Ｘ？ｆｓ検出器等を同試料面と平
行な方向に駆動して前記入射Ｘ線と検出する前記回折Ｘ
線との角度を変化させることを特徴とする薄膜Ｘ線回折
装置を提供するものである。In order to solve the above problems, the present invention provides a scattering slit, a light-receiving solar slit, and a monochromator on the sample surface in order to obtain an X-ray diffraction pattern by keeping the angle β between the diffracted X-ray and the sample surface constant at a low angle. The structure is such that it scans in a direction parallel to the . That is, in an X-ray diffraction apparatus consisting of an X-ray tube, a divergent slit, a sample holder, a scattering slit, an X-ray detector, etc., the incident X@ irradiated from the X-ray tube and the sample on the sample holder are The angle between the scattering slit and the X? The diffraction
The present invention provides a thin film X-ray diffraction device characterized by changing the angle with respect to the X-ray.
本発明の薄膜Ｘ線回折装置は上記のような構造となるの
で散乱スリット、受光側ソーラスリット及びモノクロメ
ータを試料面と平行な方向に走査するため、回折Ｘ線と
試料面のなす角を低角度で、かつ一定に保持することに
より入射Ｘ線と試料面のなす角αを小さ（するとともに
、回折Ｘ線と試料面のなす角βを小さくしてＸ線の試料
への侵入深さを小さくして薄膜のＸ線回折を可能とする
ものである。Since the thin film X-ray diffraction apparatus of the present invention has the above-described structure, the scattering slit, the light-receiving solar slit, and the monochromator are scanned in a direction parallel to the sample surface, so the angle between the diffracted X-rays and the sample surface is reduced. By keeping the angle constant, the angle α between the incident This makes it possible to make X-ray diffraction of thin films possible.
（実施例〕
以下、本発明を図面に示す実施例に基づいて具体的に説
明する。第１図は本発明の一実施例に係る薄膜Ｘ線回折
装置の光学系を示す平面図。(Example) The present invention will be specifically described below based on an example shown in the drawings. Fig. 1 is a plan view showing an optical system of a thin film X-ray diffraction apparatus according to an example of the present invention.
第２図は本実施例に係る第１図の側面図である。FIG. 2 is a side view of FIG. 1 according to this embodiment.
ここで１はＸ線管球、２は入射側ソーラスリット、３は
発散スリット、４は試料、５は散乱スリット、６は受光
側ソーラスリット、７はモノクロメータ、８はＸ線検出
器である。ｒは入射−Ｘ線と試料面のなす角、δは回折
Ｘ線と試料面のなす角、θは回折Ｘ線とモノクロメータ
面のなす角、第２図に示すψは入射Ｘ線と回折Ｘ線のな
す角である。また第１．２図の９は入射Ｘ線、１０は回
折Ｘ線である。Here, 1 is an X-ray tube, 2 is a solar slit on the incident side, 3 is a divergent slit, 4 is a sample, 5 is a scattering slit, 6 is a solar slit on the receiving side, 7 is a monochromator, and 8 is an X-ray detector. . r is the angle between the incident -X-ray and the sample surface, δ is the angle between the diffracted X-ray and the sample surface, θ is the angle between the diffracted X-ray and the monochromator surface, and ψ shown in Figure 2 is the angle between the incident X-ray and the diffraction This is the angle formed by X-rays. Further, 9 in FIG. 1.2 is an incident X-ray, and 10 is a diffracted X-ray.
Ｘ線管球１から発生した入射Ｘ線９は、入射側ソーラス
リット２、発散スリット３を通り試料４表面に照射され
る。試料４表面で回折された回折Ｘ線１０は更に散乱ス
リット５、受光側ソーラスリット６を通りモノクロメー
タ７で反射されてＸ線検出器８に到達する。ここでＸ線
管球１から発生した入射Ｘ線９と試料４面のなす角γと
、回折Ｘ線１０と試料４面のなす角δは試料４への入射
Ｘ線９の侵入深さを小さ（するために低角度に固定され
る。また試料４の回折パターンを得るために、散乱スリ
ット５、受光側ソーラスリット６、モノクロメータ７は
試料４面と平行な方向に走査される。すなわち、第２図
で示す入射Ｘ線９と回折Ｘ線１０の角ψは任意に変えら
れる。Incident X-rays 9 generated from the X-ray tube 1 pass through the incident-side solar slit 2 and the divergence slit 3 and are irradiated onto the surface of the sample 4. The diffracted X-rays 10 diffracted by the surface of the sample 4 further pass through the scattering slit 5 and the light-receiving solar slit 6, are reflected by the monochromator 7, and reach the X-ray detector 8. Here, the angle γ between the incident X-ray 9 generated from the X-ray tube 1 and the surface of the sample 4, and the angle δ between the diffracted X-ray 10 and the surface of the sample 4 define the penetration depth of the incident X-ray 9 into the sample 4. In order to obtain a small diffraction pattern, the diffraction pattern of the sample 4 is fixed at a low angle. Also, in order to obtain the diffraction pattern of the sample 4, the scattering slit 5, the light-receiving side solar slit 6, and the monochromator 7 are scanned in a direction parallel to the surface of the sample 4. , the angle ψ between the incident X-ray 9 and the diffracted X-ray 10 shown in FIG. 2 can be arbitrarily changed.
以上、具体的に説明したように本発明における薄膜Ｘ＠
回折装置は、入射Ｘ線と試料面のなす角、及び回折Ｘ線
と試料面のなす角を低角度に固定し、散乱スリット、受
光側ソーラスリット等を試料面と平行に走査してＸ線回
折パターンを得る構造としたため、試料へのＸ線の侵入
深さが小さくなり、薄膜試料の効果的な測定が可能であ
る。As specifically explained above, the thin film X@ in the present invention
The diffractometer fixes the angle between the incident X-ray and the sample surface and the angle between the diffracted X-ray and the sample surface at a low angle, and scans the scattering slit, light-receiving solar slit, etc. parallel to the sample surface to generate X-rays. Since the structure is designed to obtain a diffraction pattern, the penetration depth of X-rays into the sample is reduced, making it possible to effectively measure thin film samples.
第１図は本発明の一実施例に係る薄膜Ｘ線回折装置の光
学系を示す平面図、第２図は本実施例に係る第１図の側
面図、第３図は従来の薄膜Ｘ線回折装置の光学系を示す
平面図、第４図は回折Ｘｉｌと試料面とのなす角を変化
させた場合のＸｉｌの侵入深さを示すグラフである。
１・・・Ｘ線管球、２・・・入射側ソーラスリット、３
・・・発散スリット、４・・・試料、５・・・散乱スリ
ット、６・・・受光側ソーラスリット、７・・・モノク
ロメータ、８・・・Ｘ線検出器、９・・・入射Ｘ線、１
０・・・回折Ｘ線、γ・・・入射Ｘ線と試料面のなす角
、δ・・・回折Ｘ線と試料面のなす角、θ・・・回折Ｘ
線とモノクロメータ面のなす角、ψ・・・入射Ｘ線と回
折Ｘ線のなす角。FIG. 1 is a plan view showing the optical system of a thin film X-ray diffraction apparatus according to an embodiment of the present invention, FIG. 2 is a side view of FIG. 1 according to this embodiment, and FIG. 3 is a conventional thin film X-ray diffraction device. FIG. 4, which is a plan view showing the optical system of the diffraction device, is a graph showing the penetration depth of Xil when the angle between the diffracted Xil and the sample surface is changed. 1...X-ray tube, 2...Incidence side solar slit, 3
... Diverging slit, 4... Sample, 5... Scattering slit, 6... Solar slit on the receiving side, 7... Monochromator, 8... X-ray detector, 9... Incident X line, 1
0...Diffraction X-ray, γ...Angle between incident X-ray and sample surface, δ...Angle between diffraction X-ray and sample surface, θ...Diffraction X
The angle between the line and the monochromator surface, ψ...The angle between the incident X-ray and the diffracted X-ray.
Claims (1)
Ｘ線検出器等からなるＸ線回折装置において、前記Ｘ線
管球から照射された入射Ｘ線と前記試料保持台上の試料
面とのなす角、及び同試料面で回折された回折Ｘ線と同
試料面とのなす角を低角度に固定し、前記散乱スリット
及び前記Ｘ線検出器等を同試料面と平行な方向に駆動し
て前記入射Ｘ線と検出する前記回折Ｘ線との角度を変化
させることを特徴とする薄膜Ｘ線回折装置。X-ray tube, divergent slit, sample holder, scattering slit,
In an X-ray diffraction device consisting of an X-ray detector or the like, the angle formed between the incident X-ray irradiated from the X-ray tube and the sample surface on the sample holder, and the diffracted X-ray diffracted by the sample surface The angle between the incident X-ray and the detected diffracted X-ray is fixed at a low angle, and the scattering slit and the X-ray detector are driven in a direction parallel to the sample surface. A thin film X-ray diffraction device characterized by changing the angle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62328011A JPH01167642A (en) | 1987-12-24 | 1987-12-24 | Thin-film x-ray diffraction device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62328011A JPH01167642A (en) | 1987-12-24 | 1987-12-24 | Thin-film x-ray diffraction device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01167642A true JPH01167642A (en) | 1989-07-03 |
Family
ID=18205513
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62328011A Pending JPH01167642A (en) | 1987-12-24 | 1987-12-24 | Thin-film x-ray diffraction device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01167642A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007132766A (en) * | 2005-11-10 | 2007-05-31 | Meidensha Corp | Vehicle rolling prevention apparatus of chassis dynamometer |
-
1987
- 1987-12-24 JP JP62328011A patent/JPH01167642A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007132766A (en) * | 2005-11-10 | 2007-05-31 | Meidensha Corp | Vehicle rolling prevention apparatus of chassis dynamometer |
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