JPH0714872Y2 - Low temperature powder X-ray diffractometer - Google Patents
Low temperature powder X-ray diffractometerInfo
- Publication number
- JPH0714872Y2 JPH0714872Y2 JP1988152569U JP15256988U JPH0714872Y2 JP H0714872 Y2 JPH0714872 Y2 JP H0714872Y2 JP 1988152569 U JP1988152569 U JP 1988152569U JP 15256988 U JP15256988 U JP 15256988U JP H0714872 Y2 JPH0714872 Y2 JP H0714872Y2
- Authority
- JP
- Japan
- Prior art keywords
- low temperature
- sample
- ray diffractometer
- temperature powder
- powder
- 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】 本考案は、低温粉末Ｘ線回折装置に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a low temperature powder X-ray diffractometer.
最近、液体窒素温度付近に臨界温度をもつ酸化物高温超
伝導体の発見により、低温においての粉末Ｘ線回折プロ
ファイル測定の必要性が増している。Recently, the discovery of high-temperature oxide superconductors having a critical temperature near the temperature of liquid nitrogen has increased the need for powder X-ray diffraction profile measurement at low temperatures.
低温（４−100K）におけるＸ線回折法は、主に単結晶精
密構造解析に、原子の熱振動抑制手段として用いられて
きた。低温の実現法としては、窒素ガス吹き付け装置に
よる方法等が挙げられるが、氷の付着という欠点があ
り、測定に困難が生じていた。上記に鑑み本考案は、試
料を冷却する際に生ずる試料付近の氷の付着を除去する
ことを目的とする。The X-ray diffraction method at low temperature (4-100K) has been used as a means for suppressing thermal vibration of atoms, mainly for single crystal precision structural analysis. As a method for realizing the low temperature, there is a method using a nitrogen gas blowing device and the like, but there is a drawback that ice adheres, which causes difficulty in measurement. In view of the above, it is an object of the present invention to remove ice adhesion near the sample that occurs when the sample is cooled.
以下、本考案の実施例を図面を参照して説明する。Hereinafter, embodiments of the present invention will be described with reference to the drawings.
第１図は実施例を示す。ホルダー（１）はステンレス材
よりなり、冷媒タンク（３）と試料ホルダー（４）とを
一体化させた構造を有する。FIG. 1 shows an embodiment. The holder (1) is made of stainless steel and has a structure in which the refrigerant tank (3) and the sample holder (4) are integrated.
冷媒タンク（３）上部には、液体窒素等の冷媒を内部に
入れる為の抽入口（２）が設けられている。試料ホルダ
ー（４）は、模型ゴニオメーター（５）に光学系のカバ
ーを取り外すだけで直接取り付けられる。Above the refrigerant tank (3), there is provided an extraction port (2) for putting a refrigerant such as liquid nitrogen therein. The sample holder (4) can be directly attached to the model goniometer (5) simply by removing the optical system cover.
試料ホルダー（４）には試料（６）が取り付けられ、試
料（６）には銅コンスタンタン熱電対等の温度センサー
（７）が埋入されている。A sample (6) is attached to the sample holder (4), and a temperature sensor (7) such as a copper constantan thermocouple is embedded in the sample (6).
温度センサー（７）は外部温度測定装置とリード線（1
5）を介して接続されている。The temperature sensor (7) consists of an external temperature measuring device and a lead wire (1
5) is connected via.
ホルダー（１）は、その周囲をアクリル製の容器（８）
によって密閉されている。The holder (1) has an acrylic container (8) around the holder (1).
Is sealed by.
容器（８）には、循環パイプ（16）の出入口が接続し、
容器（８）の下方には循環パイプ（16）の入口（９）、
容器（８）の上方には循環パイプ（16）の出口（10）が
各々設けられている。The inlet and outlet of the circulation pipe (16) is connected to the container (8),
Below the container (8) is the inlet (9) of the circulation pipe (16),
An outlet (10) of the circulation pipe (16) is provided above the container (8).
循環パイプ（16）の経路には、ポンプ（17）及びゼオラ
イト4A、シリカゲル等の乾燥剤（11）が配置されてい
る。A pump (17) and a desiccant (11) such as zeolite 4A and silica gel are arranged in the path of the circulation pipe (16).
容器（８）には、試料ホルダー（４）に取り付けられた
試料（６）と略平行となる位置に、外部Ｘ線出力装置よ
り出力されるＸ線を試料に照射する為の照射口（12）及
び、試料（６）を通過したＸ線を外部測定装置へ到達せ
しめる為の検出口（13）が設けられている。The container (8) has an irradiation port (12) for irradiating the sample with X-rays output from an external X-ray output device at a position substantially parallel to the sample (6) attached to the sample holder (4). ) And a detection port (13) for allowing the X-rays passing through the sample (6) to reach an external measuring device.
次に上記実施例の動作を説明する。Next, the operation of the above embodiment will be described.
冷媒タンク（３）の抽入口（２）より抽入された液体窒
素等の冷媒により、試料ホルダー（４）を介して試料
（６）が冷やされると同時に、ポンプ（17）が駆動し、
入口（９）から密閉された空間内の大気（14）が、ポン
プ（17）を介して乾燥剤（11）に取り込まれる。大気
（14）は乾燥剤（11）を通過し、通過する際、大気中の
水分が抜き取られ、更に水分の抜き取られた大気は、循
環パイプ（16）を経て出口（10）へ到達する。At the same time as the sample (6) is cooled via the sample holder (4) by the refrigerant such as liquid nitrogen extracted from the extraction port (2) of the refrigerant tank (3), the pump (17) is driven,
The atmosphere (14) in the space sealed from the inlet (9) is taken into the desiccant (11) via the pump (17). The atmosphere (14) passes through the desiccant (11), and when passing through the desiccant (11), moisture in the atmosphere is removed, and the removed atmosphere reaches the outlet (10) through the circulation pipe (16).
ポンプ（17）の駆動を行なうことにより上述の動作が繰
り返され、密閉空間中の大気（14）が乾燥剤を通過循環
して除湿され、冷却中の試料に氷が付着するのを防止す
るものである。The operation described above is repeated by driving the pump (17), and the atmosphere (14) in the closed space is circulated through the desiccant to be dehumidified to prevent ice from adhering to the sample being cooled. Is.
従って、本考案によれば、氷の付着によって生ずるＸ線
回折プロファイル測定の障害は皆無となり、正確な測定
が行なえる等の効果を有するものである。Therefore, according to the present invention, there is no obstacle to the measurement of the X-ray diffraction profile caused by the adhesion of ice, and there is an effect that accurate measurement can be performed.
尚、循環経路、ポンプ、乾燥剤の構造、形状乃至位置関
係は、第１図に示す実施例に限ることはない。又、乾燥
剤は、ここで示すような化学的乾燥の他、機械的、物理
的乾燥による手段も取り得る。ここで大気とは、本実施
例の使用時、ホルダーの周囲に存在する気体、例えば空
気等を示すものである。The structure, shape and positional relationship of the circulation path, the pump and the desiccant are not limited to those in the embodiment shown in FIG. Further, the desiccant may take not only chemical drying as shown here but also mechanical and physical drying means. Here, the atmosphere means a gas existing around the holder when using the present embodiment, such as air.
第１図は、本考案の一実施例を示す構造図であり、第２
図は、第１図に示した構造図の一部を示す斜視図であ
る。 １…ホルダー、２…抽入口、３…冷媒タンク、４…試料
ホルダー、５…ゴニオメーター、６…試料、７…温度セ
ンサー。FIG. 1 is a structural diagram showing an embodiment of the present invention.
The drawing is a perspective view showing a part of the structural view shown in FIG. 1 ... Holder, 2 ... Extractor, 3 ... Refrigerant tank, 4 ... Sample holder, 5 ... Goniometer, 6 ... Sample, 7 ... Temperature sensor.
Claims (2)
した試料ホルダーよりなることを特徴とする低温粉末Ｘ
線回折装置。1. A low temperature powder X comprising a refrigerant tank and a sample holder formed on the surface of the refrigerant tank.
Line diffractometer.
る循環手段、前記循環手段の循環経路中に設けた大気水
分を除去する除去手段よりなることを特徴とする前記第
（１）項記載の低温粉末Ｘ線回折装置。2. The low temperature according to claim 1, further comprising a circulation means for circulating the atmosphere around the sample holder, and a removal means provided in a circulation path of the circulation means for removing atmospheric moisture. Powder X-ray diffractometer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1988152569U JPH0714872Y2 (en) | 1988-11-25 | 1988-11-25 | Low temperature powder X-ray diffractometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1988152569U JPH0714872Y2 (en) | 1988-11-25 | 1988-11-25 | Low temperature powder X-ray diffractometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0272962U JPH0272962U (en) | 1990-06-04 |
| JPH0714872Y2 true JPH0714872Y2 (en) | 1995-04-10 |
Family
ID=31427617
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1988152569U Expired - Lifetime JPH0714872Y2 (en) | 1988-11-25 | 1988-11-25 | Low temperature powder X-ray diffractometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0714872Y2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08304242A (en) * | 1995-05-15 | 1996-11-22 | Rigaku Corp | Sample cooling nozzle |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3781556A (en) * | 1972-09-08 | 1973-12-25 | Atomic Energy Commission | Neutron activation analysis system |
-
1988
- 1988-11-25 JP JP1988152569U patent/JPH0714872Y2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08304242A (en) * | 1995-05-15 | 1996-11-22 | Rigaku Corp | Sample cooling nozzle |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0272962U (en) | 1990-06-04 |
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