JP2503670Y2 - Sample holder for X-ray diffractometer - Google Patents
Sample holder for X-ray diffractometerInfo
- Publication number
- JP2503670Y2 JP2503670Y2 JP1990102600U JP10260090U JP2503670Y2 JP 2503670 Y2 JP2503670 Y2 JP 2503670Y2 JP 1990102600 U JP1990102600 U JP 1990102600U JP 10260090 U JP10260090 U JP 10260090U JP 2503670 Y2 JP2503670 Y2 JP 2503670Y2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- ray
- sample container
- exposure surface
- sample holder
- 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 - Lifetime
Links
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Description
【考案の詳細な説明】 〈産業上の利用分野〉 本考案は、Ｘ線回折装置用の試料ホルダに関する。DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to a sample holder for an X-ray diffraction apparatus.
〈従来の技術〉 Ｘ線回折装置において、粉末状の未知試料を分析する
には、従来、第３図に示すような試料ホルダが使用され
る。すなわち、この試料ホルダａは、平板部ａ1の略中
央に透孔ａ2あるいは凹部が形成されており、この透孔
ａ2あるいは凹部に試料ｄを充填した後、これを加圧し
て試料ｄを定着させるとともに、試料ｄのＸ線露光面ｄ
1が平坦になるようにしている。このように、試料ｄの
Ｘ線露光面ｄ1を予め平坦にするのは、この露光面ｄ1が
平板部ａ1より凹んでいたり、凸になっていたりする
と、この試料ホルダａを図外のゴニオメータにセットし
た際に、そのＸ線露光面ｄ1がゴニオメータの回転軸中
心から外れるので、その結果、Ｘ線の回折角（２θ）の
ピーク位置がずれたり、検出強度が変化する等の不具合
を生じるためである。<Prior Art> In an X-ray diffractometer, a sample holder as shown in FIG. 3 is conventionally used to analyze an unknown powdery sample. That is, in this sample holder a, a through hole a 2 or a concave portion is formed substantially in the center of the flat plate portion a 1 , and after filling the through hole a 2 or the concave portion with the sample d, the sample d is pressed to press the sample d. X-ray exposure surface d of sample d
1 is flat. In this way, the X-ray exposure surface d 1 of the sample d is made flat in advance by making the sample holder a out of the drawing when the exposure surface d 1 is concave or convex from the flat plate portion a 1. When it is set on the goniometer, the X-ray exposure surface d 1 deviates from the center of the rotation axis of the goniometer, and as a result, the peak position of the X-ray diffraction angle (2θ) shifts or the detected intensity changes. This is because it causes a problem.
〈考案が解決しようとする課題〉 ところで、試料ｄの種類によっては、測定中に、その
環境変化によって試料ｄの体積が変わったり、粒度が変
化したりするものがある。たとえば、水素吸蔵合金の粉
末試料では、水素の吸収、排出によりその体積が変化す
る。<Problems to be Solved by the Invention> By the way, depending on the type of the sample d, the volume of the sample d may change or the particle size may change due to environmental changes during measurement. For example, in a powder sample of a hydrogen storage alloy, its volume changes due to absorption and discharge of hydrogen.
したがって、このような試料ｄでは、測定中にそのＸ
線露光面ｄ1が平板部ａ1から突出したり、逆に試料ｄが
試料ホルダａから脱落してしまう。そうすると、上述し
たように、そのＸ線露光面ｄ1がゴニオメータの回転軸
中心から外れてしまい、精度良い測定結果が得られなく
なる。Therefore, in such a sample d, the X
The line exposure surface d 1 projects from the flat plate portion a 1 , or conversely the sample d falls off from the sample holder a. Then, as described above, the X-ray exposure surface d 1 deviates from the center of the rotation axis of the goniometer, and accurate measurement results cannot be obtained.
〈課題を解決するための手段〉 本考案は、このような事情に鑑みてなされたものであ
って、測定中に試料が体積変化等を起こした場合でも、
それに影響されずに精度良い分析結果が得られるように
するものである。<Means for Solving the Problem> The present invention has been made in view of such circumstances, and even when the sample undergoes a volume change or the like during measurement,
It is intended to obtain accurate analysis results without being affected by it.
そのため、本考案のＸ線回折装置用試料ホルダは、Ｘ
線透過率の高い材料でできた試料容器を備え、この試料
容器は、その上方部が開口した凹状の試料充填部を有
し、この試料充填部の内側壁のＸ線露光面は、平面状に
形成されるとともに、試料容器をゴニオメータにセット
した状態においてその回転軸中心に一致するように設定
されている。Therefore, the sample holder for the X-ray diffraction device of the present invention is
A sample container made of a material having a high linear transmittance is provided, and this sample container has a concave sample filling portion whose upper portion is open, and the X-ray exposure surface of the inner wall of the sample filling portion is flat. And is set so as to coincide with the center of the rotation axis when the sample container is set in the goniometer.
〈作用〉 上記構成において、試料容器の上方部は開口されてい
るので、測定中に体積変化等が起こっても、試料が上方
に迫り出すか、あるいは下方に没入するだけで、Ｘ線が
露光される部分は変わらない。しかも、試料容器は、Ｘ
線透過率の高い材料でできており、かつ、試料充填部の
Ｘ線露光面は、平面状に形成され、かつ、このＸ線露光
面は試料容器をゴニオメータにセットした状態において
その回転軸中心に一致するから、Ｘ線の回折角（２θ）
のピーク位置がずれる等の不具合はなく、精度良い分析
結果が得られる。<Operation> In the above configuration, since the upper portion of the sample container is open, even if the volume changes during measurement, the sample is squeezed upward or immersed downward, and the X-ray is exposed. The part that is said does not change. Moreover, the sample container is X
The X-ray exposure surface of the sample filling part is made of a material having a high linear transmittance, and the X-ray exposure surface is the center of its rotation axis when the sample container is set in the goniometer. X-ray diffraction angle (2θ)
There is no problem such as a shift in the peak position of, and accurate analysis results can be obtained.
〈実施例〉 第１図は本発明のＸ線回折装置用試料ホルダの正面断
面図、第２図は第１図のII-II線に沿う断面図である。<Example> FIG. 1 is a front sectional view of a sample holder for an X-ray diffraction apparatus of the present invention, and FIG. 2 is a sectional view taken along line II-II of FIG.
これらの図において、１はＸ線回折装置用試料ホルダ
の全体を示し、２は有底円筒状をしたヒータブロックで
あり、このヒータブロック２には、図示省略したヒータ
が埋設されて試料ｓを加熱できるようになっている。そ
して、このヒータブロック２の周壁部分は、水平に180
度の範囲に渡って切り欠いて外壁から内壁にまで連通す
るＸ線窓部４が形成されている。６は試料容器であっ
て、この試料容器６は、BeやプラスチックなどのＸ線透
過率の高い材料でできており、その内部には試料充填部
6aが形成されている。この試料充填部6aは、上方部が開
口した凹状をしており、かつ、水平断面が略長円形に形
成されている。そして、この試料充填部6aの内側壁のＸ
線露光面6bは、平面状に形成されるとともに、ヒータブ
ロック２と試料容器６とを共に図外のゴニオメータにセ
ットした状態においてその回転軸中心ｏに一致するよう
に予め設定されている。また、この試料容器６の上部に
は、この試料容器６と同じ外径をもつ補助円筒８がろう
付けされており、上記の試料容器６と補助円筒８とが共
にヒータブロック２の内壁に嵌入され、これによって、
試料容器６のＸ線露光面6bがＸ線窓部４に臨んでいる。
そして、分析に際しては、試料容器６の試料充填部6aと
補助円筒８とにわたって試料ｓが充填される。In these figures, 1 is the whole sample holder for the X-ray diffractometer, 2 is a heater block having a cylindrical shape with a bottom, and a heater (not shown) is embedded in the heater block 2 to hold the sample s. It can be heated. Then, the peripheral wall portion of the heater block 2 is horizontally
An X-ray window portion 4 is formed by cutting out over a range of degrees and communicating from the outer wall to the inner wall. Reference numeral 6 denotes a sample container, which is made of a material having a high X-ray transmittance such as Be or plastic, and has a sample filling portion inside thereof.
6a is formed. The sample filling portion 6a has a concave shape with an open upper portion, and has a horizontal cross section formed into a substantially oval shape. Then, X on the inner wall of the sample filling portion 6a
The line exposure surface 6b is formed in a planar shape and is preset so as to coincide with the rotation axis center o of the heater block 2 and the sample container 6 set in a goniometer (not shown). An auxiliary cylinder 8 having the same outer diameter as that of the sample container 6 is brazed to the upper portion of the sample container 6, and the sample container 6 and the auxiliary cylinder 8 are both fitted into the inner wall of the heater block 2. And by this,
The X-ray exposure surface 6b of the sample container 6 faces the X-ray window portion 4.
Then, in the analysis, the sample s is filled over the sample filling portion 6a of the sample container 6 and the auxiliary cylinder 8.
上記構成において、試料容器６の上方部は開口されて
いるので、測定中に試料ｓを加熱したり、あるいは冷却
したりすることにより体積変化が起こっても、試料ｓが
上方に迫り出すか、あるいは下方に没入するだけで、Ｘ
線露光面6bの位置は変わらない。しかも、試料容器６
は、Ｘ線透過率の高い材料でできており、かつ、試料充
填部6aのＸ線露光面6bは、平面状に形成され、かつ、こ
のＸ線露光面6bはヒータブロック２と試料容器６とを共
にゴニオメータにセットした状態においてその回転軸中
心ｏに一致するから、Ｘ線の回折角（２θ）のピーク位
置がずれる等の不具合はなく、精度良い分析結果が得ら
れる。In the above configuration, since the upper portion of the sample container 6 is open, even if the sample s is heated or cooled during the measurement to cause a volume change, the sample s will squeeze upward, Or just immerse yourself down
The position of the line exposure surface 6b does not change. Moreover, the sample container 6
Is made of a material having a high X-ray transmittance, the X-ray exposure surface 6b of the sample filling portion 6a is formed in a flat shape, and the X-ray exposure surface 6b is formed on the heater block 2 and the sample container 6 Since both coincide with the rotation axis center o when both are set in the goniometer, there is no problem such as a shift in the peak position of the X-ray diffraction angle (2θ), and accurate analysis results can be obtained.
なお、試料ｓの充填状態によっては、体積変化が生じ
ても試料ｓが上下方向に円滑に移行し難いことがあるの
で、その場合には、第１図および第２図において破線で
示すように、試料充填部6aの近接位置に空間部6eを形成
し、試料充填部6aと空間部6eの間の隔壁部分を一種のダ
イアフラムとして作用させて試料体積変化を吸収するよ
うにしてもよい。また、本例ではヒータブロック２を設
けているが、これを省略することもできる。Note that, depending on the filling state of the sample s, it may be difficult for the sample s to move smoothly in the vertical direction even if a volume change occurs. In that case, as shown by the broken lines in FIGS. 1 and 2. Alternatively, the space 6e may be formed in the vicinity of the sample filling part 6a, and the partition wall portion between the sample filling part 6a and the space 6e may act as a kind of diaphragm to absorb the sample volume change. Further, although the heater block 2 is provided in this example, it may be omitted.
〈考案の効果〉 本考案によれば、測定中に試料が体積変化等を起こし
た場合でも、それに影響されずに精度良い分析結果が得
られるようになる等の優れた効果が発揮される。<Effect of the Invention> According to the present invention, even if the sample undergoes a volume change or the like during measurement, an excellent analysis result can be obtained without being influenced by the change.
第１図は本発明のＸ線回折装置用試料ホルダの正面断面
図、第２図は第１図のII-II線に沿う断面図、第３図は
従来の試料ホルダの斜視図である。 １……Ｘ線回折装置用試料ホルダ、６……試料容器、6a
……試料充填部、6b……Ｘ線露光面、ｓ……試料、ｏ…
…ゴニオメータの回転軸中心。FIG. 1 is a front sectional view of a sample holder for an X-ray diffraction apparatus of the present invention, FIG. 2 is a sectional view taken along line II-II of FIG. 1, and FIG. 3 is a perspective view of a conventional sample holder. 1 ... Sample holder for X-ray diffractometer, 6 ... Sample container, 6a
…… Sample filling part, 6b …… X-ray exposure surface, s …… Sample, o…
… Center of rotation of goniometer.
Claims (1)
備え、この試料容器は、その上方部が開口した凹状の試
料充填部を有し、この試料充填部の内側壁のＸ線露光面
は、平面状に形成されるとともに、試料容器をゴニオメ
ータにセットした状態においてその回転軸中心に一致す
るように設定されていることを特徴とするＸ線回折装置
用試料ホルダ。1. A sample container made of a material having a high X-ray transmittance is provided, and the sample container has a concave sample filling portion whose upper portion is open, and an X-ray on an inner wall of the sample filling portion. The sample holder for an X-ray diffractometer, wherein the exposure surface is formed in a flat shape and is set so as to coincide with the center of the rotation axis of the sample container set in the goniometer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1990102600U JP2503670Y2 (en) | 1990-09-29 | 1990-09-29 | Sample holder for X-ray diffractometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1990102600U JP2503670Y2 (en) | 1990-09-29 | 1990-09-29 | Sample holder for X-ray diffractometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0461047U JPH0461047U (en) | 1992-05-26 |
| JP2503670Y2 true JP2503670Y2 (en) | 1996-07-03 |
Family
ID=31846988
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1990102600U Expired - Lifetime JP2503670Y2 (en) | 1990-09-29 | 1990-09-29 | Sample holder for X-ray diffractometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2503670Y2 (en) |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01168856U (en) * | 1988-05-20 | 1989-11-28 |
-
1990
- 1990-09-29 JP JP1990102600U patent/JP2503670Y2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0461047U (en) | 1992-05-26 |
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