JPH081423B2 - X-ray diffraction sample heating device - Google Patents
X-ray diffraction sample heating deviceInfo
- Publication number
- JPH081423B2 JPH081423B2 JP62128339A JP12833987A JPH081423B2 JP H081423 B2 JPH081423 B2 JP H081423B2 JP 62128339 A JP62128339 A JP 62128339A JP 12833987 A JP12833987 A JP 12833987A JP H081423 B2 JPH081423 B2 JP H081423B2
- Authority
- JP
- Japan
- Prior art keywords
- resistor
- strip
- legs
- shaped
- sample
- 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
- 238000002441 X-ray diffraction Methods 0.000 title claims description 9
- 238000010438 heat treatment Methods 0.000 title claims description 7
- 239000000498 cooling water Substances 0.000 claims description 5
- 239000012809 cooling fluid Substances 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 239000012212 insulator Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 239000000112 cooling gas Substances 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Description
【発明の詳細な説明】 例えば鉄板その他の薄板状金属材料あるいは粉末状の
無機物質等においては、Ｘ線の回折を利用して高温時の
結晶構造を観測すると同時にその試料を急冷して高温時
の状態を固定した場合の分析を必要とする。しかし従来
は試料を高温に加熱して、しかもその試料を極めて急速
に冷却することが困難で、複雑な大形の装置を必要と
し、かつ充分な成果を得ることができなかった。従って
本発明は極めて簡単小形な装置をもって薄板状の試料を
数百乃至千度以上に加熱し、しかもその試料にＸ線を照
射して回折角の測定を行った状態で、例えば毎分数千度
の速度をもって試料を急速に冷却することにより、結晶
構造を固定してこれを光学的に観測し、あるいはその変
化を研究することのできる試料加熱装置を提供するもの
である。DETAILED DESCRIPTION OF THE INVENTION For example, in the case of an iron plate or other thin plate metal material or powdery inorganic substance, the crystal structure at high temperature is observed by using X-ray diffraction, and at the same time, the sample is rapidly cooled to obtain high temperature. Analysis is required when the state of is fixed. However, in the past, it was difficult to heat the sample to a high temperature and to cool the sample extremely rapidly, which required a complicated and large-sized apparatus and could not obtain sufficient results. Therefore, according to the present invention, a thin plate-shaped sample is heated to several hundreds to 1,000 degrees or more by an extremely simple and compact device, and the diffraction angle is measured by irradiating the sample with X-rays, for example, several thousands per minute. (EN) A sample heating device capable of fixing a crystal structure and optically observing it or studying its change by rapidly cooling a sample at a speed of 10 degrees.
本発明は、Ｘ線回折装置の試料保持機構に関し、帯状
抵抗体をコ字形基台の両脚の先端に取り付けると共にそ
の一方の脚を回動自在に保持して抵抗体の伸縮に伴う湾
曲あるいは破断を防止し、かつ基台の適宜の位置に電気
絶縁体を介挿して上記抵抗体に加熱電流を流すことによ
りこれを例えば数百度乃至千度以上まで加熱する。また
上記基台の両脚には冷却水の流路を設けて基台の温度上
昇を防止し、かつ前記帯状抵抗体の背面に冷却流体を吹
き付けてこれを急冷するためのノズルを設けたもので、
その抵抗体自体を試料とするか、あるいはこれに粉末状
または薄板状の試料を添着してＸ線を照射し、その回折
Ｘ線を検出して回折角の測定を行う。従って試料および
その保持部を極めて簡単で小形に形成しうると共に試料
を極めて高温度まで加熱してその状態でＸ線の回折角を
測定し、あるいは一旦加熱した試料を例えば毎分6000度
程度の高速度で急冷して高温時の結晶状態を固定するこ
とにより光学的観測を行うこと等も可能である。更に再
結晶過程における格子歪の解放あるいは相変態時の結晶
方位変化の観測等にも用いることができる。The present invention relates to a sample holding mechanism for an X-ray diffractometer, in which a band-shaped resistor is attached to the tips of both legs of a U-shaped base and one of the legs is rotatably held to bend or break as the resistor expands or contracts. In addition, a heating current is passed through the resistor by inserting an electric insulator at an appropriate position on the base to heat the resistor to several hundred degrees to 1,000 degrees or more. Also, a cooling water flow path is provided on both legs of the base to prevent the temperature of the base from rising, and a nozzle for spraying a cooling fluid on the back surface of the strip-shaped resistor to rapidly cool it is provided. ,
The resistor itself is used as a sample, or a powdery or thin plate-like sample is attached to the resistor and irradiated with X-rays, and the diffraction X-rays are detected to measure the diffraction angle. Therefore, the sample and its holding portion can be formed in a very simple and small size, and the X-ray diffraction angle can be measured in such a state that the sample is heated to an extremely high temperature, or the sample once heated can be heated to, for example, about 6000 degrees per minute. It is also possible to perform optical observation by rapidly quenching at a high speed and fixing the crystal state at high temperature. Further, it can be used for releasing the lattice strain in the recrystallization process or for observing the crystal orientation change during the phase transformation.
第１図は本発明実施例の縦断面図、第２図はその正面
図で、コ字形をなした試料の取付基台１の両脚の先端に
例えば鋼板等の帯状抵抗体２を配置し、押え金具３で押
さえてねじ４で締め付けるようにしてある。また上記両
脚には冷却水の通路５を設けてそれらの両端に冷却水の
流入または流出口６を形成し、かつ前記帯状抵抗体２の
中央部における背面に温度測定用の熱電対接点７を添着
してある。更にコ字形基台１における一方の脚８は、そ
の基端を軸９によって基台の中央片に結着することによ
り、この基台を含む平面内で僅かに回動し得るようにし
てある。かつ基台１の中央片には電気絶縁体10を介挿し
て両脚の間を絶縁し、その脚の基端部に加熱電流の端子
11を設けて導線12で電源に接続するようにしてある。更
に基台１の中央部には冷却流体、例えば低温度の空気ま
たは窒素等を抵抗体２の中央部背面に高速度で吹き付け
るためのノズル13を取り付けてある。なお上記実施例は
帯状抵抗体２自体の中央部を試料とするものであるが、
例えば粉末状あるいは薄板状の他の試料についてＸ線回
折測定を行う場合は第３図に一部の正面図を、また第４
図にその縦断面図を示したように、必要に応じて抵抗体
２の前面中央部に浅い凹部14を設け、その凹部に上記試
料15を充填することもできる。更に第５図は上述のよう
な試料取付基台１をゴニオメータ16の回転台17上に設置
してＸ線回折測定を行う装置の平面図で、ゴニオメータ
の側部に設置したＸ線管18からＸ線ｘを抵抗体２の中央
部に投射し、回転台17の２倍の角速度で回転するＸ線検
出器19によって回折Ｘ線ｘ′を検出することにより、回
折角の測定を行う。なお必要に応じては上記回転台17上
の基台１を真空装置中に収容してＸ線の減衰散乱を防止
する。FIG. 1 is a longitudinal sectional view of an embodiment of the present invention, and FIG. 2 is a front view thereof, in which a strip-shaped resistor 2 such as a steel plate is arranged at the tips of both legs of a mounting base 1 of a U-shaped sample, It is designed to be held down by the press fitting 3 and tightened with the screw 4. In addition, cooling water passages 5 are provided in the both legs, cooling water inflows or outflows 6 are formed at both ends thereof, and a thermocouple contact 7 for temperature measurement is provided on the back surface in the central portion of the strip-shaped resistor 2. It is attached. Further, one leg 8 of the U-shaped base 1 can be slightly rotated in a plane including the base by connecting its base end to a central piece of the base by a shaft 9. . In addition, an electrical insulator 10 is inserted in the center piece of the base 1 to insulate between the legs, and a heating current terminal is provided at the base end of the legs.
11 is provided and is connected to the power source by the lead wire 12. Further, a nozzle 13 for spraying a cooling fluid such as low temperature air or nitrogen on the rear surface of the central portion of the resistor 2 at a high speed is attached to the central portion of the base 1. In the above embodiment, the central portion of the strip resistor 2 itself is used as a sample.
For example, when performing X-ray diffraction measurement on other powdery or thin plate-shaped samples, a partial front view is shown in FIG.
As shown in the vertical sectional view in the figure, a shallow recess 14 may be provided in the center of the front surface of the resistor 2 and the sample 15 may be filled in the recess as required. Further, FIG. 5 is a plan view of an apparatus for performing X-ray diffraction measurement by installing the sample mounting base 1 as described above on the rotary table 17 of the goniometer 16, and showing the X-ray tube 18 installed on the side of the goniometer. The X-ray x is projected onto the central portion of the resistor 2, and the diffracted X-ray x ′ is detected by the X-ray detector 19 which rotates at twice the angular velocity of the turntable 17, thereby measuring the diffraction angle. If necessary, the base 1 on the rotary table 17 is housed in a vacuum device to prevent X-ray attenuation and scattering.
上記実施例のように本発明の装置は試料で形成した帯
状の抵抗体に直接、または試料を添着した他の帯状抵抗
体に電流を流して加熱するから、小電力をもって効率よ
く、かつ迅速に試料の温度を上昇させることができる。
またコ字形基台の一方の脚を回転自在にしてあるから、
抵抗体の膨張収縮によってこれが屈曲し、あるいは切断
するようなおそれがなく、試料位置の変動を防止するこ
とができる。また試料の冷却に際してはノズル13を例え
ば窒素ボンベに連結して低温度の窒素を帯状抵抗体２の
裏側に吹き付ける。その際ノズルから吹き出した気体が
急激に膨張して、この膨張により温度が急激に低下する
ために、加熱された抵抗体２は極めて有効に効率よく冷
却される。すなわち加熱された試料の温度が例えば毎分
6000度程度の速度で急激に低下して、高温時の結晶状態
が固定されるから、例えばＸ線の回折データと固定され
た結晶状態の光学的観察等の対比を行うことができる。As in the above-mentioned embodiment, the device of the present invention heats by directly applying a current to the strip-shaped resistor formed by the sample or by passing a current to another strip-shaped resistor attached with the sample. The temperature of the sample can be raised.
Also, because one leg of the U-shaped base is rotatable,
There is no risk of the resistor being bent or cut due to the expansion and contraction of the resistor, and it is possible to prevent the sample position from changing. Further, when cooling the sample, the nozzle 13 is connected to, for example, a nitrogen cylinder, and low temperature nitrogen is blown to the back side of the strip-shaped resistor 2. At this time, the gas blown from the nozzle rapidly expands, and the temperature sharply drops due to this expansion, so that the heated resistor 2 is cooled very effectively and efficiently. That is, the temperature of the heated sample is
Since the crystal state is rapidly lowered at a speed of about 6000 degrees and the crystal state at high temperature is fixed, it is possible to compare, for example, X-ray diffraction data and optical observation of the fixed crystal state.
第１図は本発明実施例の縦断面図、第２図は第１図の装
置の正面図、第３図は本発明の他の実施例における帯状
抵抗体の一部の正面図、第４図は第３図の抵抗体の縦断
面図、第５図は本発明の装置をＸ線回折ゴニオメータに
取り付けた状態の平面図である。なお図においてね１は
試料取付基台、２は抵抗体、５は冷却水通路、13は冷却
気体ノズルである。1 is a longitudinal sectional view of an embodiment of the present invention, FIG. 2 is a front view of the apparatus of FIG. 1, FIG. 3 is a front view of a part of a strip-shaped resistor in another embodiment of the present invention, and FIG. FIG. 5 is a vertical cross-sectional view of the resistor of FIG. 3, and FIG. 5 is a plan view of the device of the present invention attached to an X-ray diffraction goniometer. In the figure, 1 is a sample mounting base, 2 is a resistor, 5 is a cooling water passage, and 13 is a cooling gas nozzle.
Claims (1)
折試料加熱装置。 （イ）Ｘ線回折試料を加熱するための帯状抵抗体を有す
る。 （ロ）両脚とその間の中央片とからなるコ字形取付基台
を有する。 （ハ）前記帯状抵抗体の両端が前記両脚の先端に固定さ
れる。 （ニ）前記コ字形取付基台の一方の脚が前記中央片に対
して回動自在に取り付けられる。 （ホ）前記両脚に冷却水の流路が設けられる。 （へ）前記両脚の間を電気的に絶縁する絶縁体が前記コ
字形取付基台に設けられる。 （ト）前記帯状抵抗体に電流を供給するための加熱電流
端子が前記両脚に設けられる。 （チ）前記帯状抵抗体の中央部背面に熱電対接点が固定
される。 （リ）前記帯状抵抗体の中央部背面に向かって冷却流体
を吹き付けるノズルが前記コ字形取付基台に設けられ
る。1. An X-ray diffraction sample heating apparatus having the following features (a) to (i). (A) It has a strip-shaped resistor for heating the X-ray diffraction sample. (B) It has a U-shaped mounting base consisting of both legs and a center piece between them. (C) Both ends of the strip resistor are fixed to the tips of the legs. (D) One leg of the U-shaped mounting base is rotatably attached to the central piece. (E) Flow paths for cooling water are provided on both legs. (V) An insulator that electrically insulates between the legs is provided on the U-shaped mounting base. (G) A heating current terminal for supplying a current to the strip-shaped resistor is provided on the both legs. (H) A thermocouple contact is fixed to the back surface of the central portion of the strip resistor. (I) A nozzle for spraying the cooling fluid toward the rear surface of the central portion of the strip-shaped resistor is provided on the U-shaped mounting base.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62128339A JPH081423B2 (en) | 1987-05-27 | 1987-05-27 | X-ray diffraction sample heating device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62128339A JPH081423B2 (en) | 1987-05-27 | 1987-05-27 | X-ray diffraction sample heating device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63293452A JPS63293452A (en) | 1988-11-30 |
| JPH081423B2 true JPH081423B2 (en) | 1996-01-10 |
Family
ID=14982354
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62128339A Expired - Lifetime JPH081423B2 (en) | 1987-05-27 | 1987-05-27 | X-ray diffraction sample heating device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH081423B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010048618A (en) * | 2008-08-20 | 2010-03-04 | Tokyo Institute Of Technology | Method for measuring phase transition conditions of sample to be subjected to phase transition, and measuring apparatus therefor |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5011583U (en) * | 1973-05-28 | 1975-02-06 | ||
| JPS5816553U (en) * | 1981-07-24 | 1983-02-01 | 理学電機株式会社 | Sample heating device for X-ray small-angle scattering measurement device |
-
1987
- 1987-05-27 JP JP62128339A patent/JPH081423B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010048618A (en) * | 2008-08-20 | 2010-03-04 | Tokyo Institute Of Technology | Method for measuring phase transition conditions of sample to be subjected to phase transition, and measuring apparatus therefor |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63293452A (en) | 1988-11-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP7162206B2 (en) | X-ray analysis cell and X-ray analysis device | |
| US3456490A (en) | Differential thermal analysis | |
| US8371746B2 (en) | Thermal analysis device | |
| JPS59500688A (en) | Low temperature stage for trace analysis | |
| US3527081A (en) | Differential scanning calorimeter | |
| JP3669615B2 (en) | Sample heating / cooling device and thermal analysis device | |
| US3165915A (en) | Determination of thermal properties of materials | |
| JPH081423B2 (en) | X-ray diffraction sample heating device | |
| US6215323B1 (en) | Method and apparatus for temperature-controlled testing of integrated circuits | |
| RU2620028C1 (en) | Thermostatic device for nanocalorimetric measurements on chip with ultra-high heating and cooling rates | |
| JP3129417B2 (en) | Heating / cooling device and electrical characteristic evaluation device | |
| JPH09222404A (en) | Method and device for measuring specific heat capacity | |
| JP3849295B2 (en) | Thermal diffusion coefficient measuring device | |
| JPH0552783A (en) | Thermoelectric characteristic measuring device | |
| US11740194B2 (en) | Measuring mechanism for measuring thermal conductivity | |
| GB1604481A (en) | Process and equipment for the thermal analysis of materials | |
| JPH0518913A (en) | Thermoelectromotive force measuring method and apparatus | |
| JPH0323563Y2 (en) | ||
| US3535913A (en) | Differential thermal analysis apparatus | |
| JPH06201572A (en) | Friction evaluating apparatus | |
| SU920485A1 (en) | Device for investigating metal and alloy properties | |
| US5044211A (en) | Method for determining the effects of oxygen plasma on a specimen | |
| RU2831948C1 (en) | Device for creating temperature gradient and studying structure of polymer samples with thermoelectric properties by x-ray diffraction in geometry of sliding beam | |
| RU2620029C1 (en) | Holder unit for nanocalorimetric sensors for measuring thermophysical and structural parameters of sample | |
| RU2711563C1 (en) | Thermostating device for carrying out nanocalorimetric measurements |