JPS6351623A - Realtime manufacturing, analyzing and evaluating device for crystal - Google Patents
Realtime manufacturing, analyzing and evaluating device for crystalInfo
- Publication number
- JPS6351623A JPS6351623A JP19609186A JP19609186A JPS6351623A JP S6351623 A JPS6351623 A JP S6351623A JP 19609186 A JP19609186 A JP 19609186A JP 19609186 A JP19609186 A JP 19609186A JP S6351623 A JPS6351623 A JP S6351623A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- laser
- state
- diffraction
- ray
- 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
- 239000013078 crystal Substances 0.000 title claims abstract description 7
- 238000012394 real-time manufacturing Methods 0.000 title 1
- 238000002441 X-ray diffraction Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 5
- 230000010355 oscillation Effects 0.000 claims description 4
- 238000011156 evaluation Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 abstract description 12
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 2
- -1 aqueous vapor Chemical compound 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 239000013307 optical fiber Substances 0.000 abstract description 2
- 239000005304 optical glass Substances 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000001451 molecular beam epitaxy Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は単結晶および多結晶材料の高温における挙動の
追求や、新材料の探索に用いるリアルタイム結晶製作・
解析評価装置に関する。[Detailed Description of the Invention] [Industrial Field of Application] The present invention is directed to real-time crystal production and use for investigating the behavior of single-crystalline and polycrystalline materials at high temperatures, and for searching for new materials.
Regarding analysis and evaluation equipment.
単結晶および多結晶材料を高温に加へする過程や、それ
らの材料の製作過程等をリアルタイムにＸ線回折により
評価する従来の装置には、以下にのべるような大きな制
約や欠点があった。たとえば、付加すべき加熱装置が大
体積のため、収集できるデータが室温の場合に比べて著
しく制限されたり、高温保持用の耐熱容器がないために
、最高設定温度が低く抑えられたり、あるいは、測温の
困難さのために、温度制御が不可能であるといった欠点
である。また、特に、空気中以外での実験は大きな制約
を受けていた。何故ならば、試料雰囲気を真空にしたり
、試料室に各種の不活性ガスや反応ガスを導入したりす
ると、そのために、装置の大型化が避けられなくなり、
また、それ等のガス回路系の複雑さのために、肝心のデ
ータの収集が著しく制約されたりするからである。これ
等原因のために、従来の装置では、ｆ＠便にリアルタイ
ムに材料探索を行うことはできなかった。Conventional equipment that evaluates the process of subjecting single-crystalline and polycrystalline materials to high temperatures, the manufacturing process of these materials, etc. using X-ray diffraction in real time has the following major limitations and drawbacks. For example, due to the large volume of the heating device that must be added, the data that can be collected is significantly limited compared to the case at room temperature, or the maximum set temperature is kept low because there is no heat-resistant container for maintaining high temperatures, or The disadvantage is that temperature control is impossible due to the difficulty of temperature measurement. Additionally, experiments in environments other than air were subject to significant restrictions. This is because if you make the sample atmosphere a vacuum or introduce various inert gases or reactive gases into the sample chamber, it becomes inevitable that the equipment becomes larger.
In addition, the complexity of such gas circuit systems significantly limits the collection of essential data. Due to these reasons, it has not been possible to search for materials in real time using conventional devices.
本発明が提供するリアルタイム結晶製作・解析装置とは
、簡便に材料探索を行うためのものである。もっとも、
大がかりにこれを行おうとすると、ＭＢＥ（分子線エピ
タキシー装置）（ジャーナル・オブ・ツ゛アキューム・
サイエンス・テクノロジー（Ｊ、 Ｖａｃ。The real-time crystal production/analysis device provided by the present invention is for easily searching for materials. However,
If you try to do this on a large scale, MBE (molecular beam epitaxy equipment) (Journal of
Science and Technology (J, Vac.
Ｓｃｉ、 Ｔｅｃｈｎｏｌ、、６ （１９６９）、５４
５．）に、その例を見るように、超高真空や大型物理分
析装置との結合を必要とする。しかしながら、材料探索
や新材料発見の殆どの場合には、該材料固有の性質を明
らかにすることが、第一段階の目的であるから、徒らに
、装置の大型化や、雰囲気のきびしい制御等は本来不要
である。Sci, Technol, 6 (1969), 54
5. ), as shown in the example above, requires coupling with an ultra-high vacuum or large-scale physical analysis equipment. However, in most cases of material exploration and new material discovery, the purpose of the first stage is to clarify the unique properties of the material, so it is unnecessary to increase the size of the equipment and to strictly control the atmosphere. etc. are essentially unnecessary.
本発明の目的は、市販の回折用Ｘ線発生装置。The object of the present invention is to provide a commercially available X-ray generator for diffraction.
加熱用レーザ・発振装置、光ファイバー、温度センサー
、ガス噴（２）器等を備えた系を用いて上記目的を簡便
、迅速かつ十分な経済性をもって果せる装置を提供する
ことにある。The object of the present invention is to provide a device that can accomplish the above objectives simply, quickly, and with sufficient economy using a system equipped with a heating laser/oscillator, optical fiber, temperature sensor, gas jet (2), and the like.
本発明は試料表面にレーザビームを照射して加熱するレ
ーザ発振装置と、試料を含む一定範囲に真空又は特定の
ガス雰囲気を形成する装置と、試料にＸ線を入射するＸ
線照射装置と、試料の表面状態の回折Ｘ線パターンを観
測する装置とを有することを特徴とするリアルタイム結
晶製作・解析評価装置である。The present invention consists of a laser oscillation device that heats a sample surface by irradiating it with a laser beam, a device that forms a vacuum or a specific gas atmosphere in a certain area including the sample, and an X-ray device that injects X-rays into the sample.
This is a real-time crystal production/analysis/evaluation device characterized by having a radiation irradiation device and a device for observing the diffraction X-ray pattern of the surface state of a sample.
第１図は本発明の構成概念図である。先ず、Ｎｄ：ＹＡ
Ｇレーザがレーザ発振装置１から、光ガラス・ファイバ
ー２によって、集光レンズ３まで導かれた後、被検査試
料４上に焦点が結ばれ、該試料４が加熱される。該試料
４上のレーザ・ビーム・スポットの直径は、０．５ｍ乃
至１０＋ｎｏ＋の範囲で可変である。一方、赤外線温度
センサー５により、試料温度が測温され、結果はレーザ
・発振装置１にフィード・バックされ、予め設定された
温度に制御される。ラウェ法Ｘ線回折のように試料が静
止している場合には、その安定度は±１０℃程度である
。FIG. 1 is a conceptual diagram of the structure of the present invention. First, Nd:YA
After the G laser is guided from the laser oscillation device 1 to the condenser lens 3 by the optical glass fiber 2, it is focused on the sample to be inspected 4, and the sample 4 is heated. The diameter of the laser beam spot on the sample 4 is variable in the range from 0.5 m to 10+no+. On the other hand, the temperature of the sample is measured by the infrared temperature sensor 5, and the result is fed back to the laser/oscillation device 1, which controls the temperature to a preset temperature. When the sample is stationary as in Laue X-ray diffraction, the stability is about ±10°C.
一方、試料４の被加熱状態は、拡大レンズ６を通してａ
察できる。加熱に加えて１本発明では、さらに、雰囲気
制御が可能となる。即ち、試料４の斜上方に設置された
ノズル７からは、酸素、窒素、水蒸気、アンモニア・ガ
スその外、空気中に放出しても、発火性や引火性がなく
、また人体にとって有害でないガスが、試料４に向かっ
て噴射される。その際第１図に示す如く、噴射コーンが
十分試料４を被っている場合には、該試料４は該噴射ガ
スの気流中にあることになる。気流中にない場合は、Ｘ
線、レーザ光線、および被検査試料から発する赤外線に
対して、十分透明である耐熱ガラスで構成された豆電球
状の試料支持器（図示路）中に封じ込む、この際、該支
持器内は真空に保たれるか、または、任意のガスにより
封じこまれる。On the other hand, the heated state of the sample 4 can be seen through the magnifying lens 6.
I can understand it. In addition to heating, the present invention further allows for atmospheric control. In other words, from the nozzle 7 installed diagonally above the sample 4, oxygen, nitrogen, water vapor, ammonia gas, and other gases are not ignitable or flammable, and are not harmful to the human body even if released into the air. is injected toward the sample 4. In this case, as shown in FIG. 1, if the injection cone sufficiently covers the sample 4, the sample 4 will be in the air stream of the injection gas. If not in the airflow, X
The sample is enclosed in a miniature bulb-shaped sample support (the path shown in the figure) made of heat-resistant glass that is sufficiently transparent to radiation, laser beams, and infrared rays emitted from the sample to be inspected. Maintained under vacuum or enclosed by any gas.
前者の場合、試料は空気中に曝されたまま上下あるいは
、左右からガスを高速で噴射され、試料４はガス流中で
閉じ込められた状態になる。その際。In the former case, gas is injected from above and below or from the left and right at high speed while the sample is exposed to air, and the sample 4 becomes trapped in the gas flow. that time.
試料近辺の空気は排除されて、実験中に該試料４は空気
に接触しない状態となる。また、該試料の加熱による化
学変化の様子は、同時にＸ線照射装置８から試料４に入
射されるＸ線の回折Ｘ線パターンの変化をパターン１ｅ
ｔｉ！１１装置９にて’ｉｎ ５ｉｔｕ’に観測するこ
とができる。また、被加熱試料の急冷時の化学変化を観
測したい場合には、レーザ・ビームの照射を止めると同
時に、先に述べたノズルから水蒸気を噴出させてやれば
よい。The air near the sample is removed so that the sample 4 does not come into contact with air during the experiment. Furthermore, the state of the chemical change due to heating of the sample is determined by the change in the diffraction X-ray pattern of the X-rays incident on the sample 4 from the X-ray irradiation device 8 at the same time.
Ti! It can be observed 'in 5 itu' with No. 11 equipment 9. Furthermore, if it is desired to observe chemical changes during rapid cooling of a heated sample, water vapor may be ejected from the aforementioned nozzle at the same time as stopping the laser beam irradiation.
以下に本発明の実施例を示す。 Examples of the present invention are shown below.
ＧａＡｓウェー八を試へとして前述の方法により局部加
熱したところ、ＧａＡｓ酸化膜が表面に形成された。そ
の際、水蒸気ガスをノズルから吹き付けたところ、酸化
膜の形成が著しく促進された。この酸化膜の結晶状態は
直ちにＸ線回折パターンの変化として捉えることができ
た。When a GaAs wafer was locally heated using the method described above, a GaAs oxide film was formed on the surface. At that time, when water vapor gas was sprayed from a nozzle, the formation of an oxide film was significantly promoted. The crystalline state of this oxide film could be immediately detected as a change in the X-ray diffraction pattern.
以上のように本発明によれば、従来困難とされていた結
晶製作のプロセスおよび結果を熱的ならびに雰囲気的環
境を変化させながら、リアルタイムに、しかも極めて簡
便に観測でき、したがって材料探索に大きく貢献できる
効果を有するものである。As described above, according to the present invention, the process and results of crystal production, which were conventionally considered difficult, can be observed in real time and extremely easily while changing the thermal and atmospheric environment, thus greatly contributing to material exploration. It has the effect that it can.
第１図は本発明の概念を示す装置および試料の配置図で
ある。FIG. 1 is a layout diagram of an apparatus and a sample showing the concept of the present invention.
Claims (1)
ザ発振装置と、試料を含む一定範囲に真空又は特定のガ
ス雰囲気を形成する装置と、試料にＸ線を入射するＸ線
照射装置と、試料の表面状態の回折Ｘ線パターンを観測
する装置とを有することを特徴とするリアルタイム結晶
製作・解析評価装置。(1) A laser oscillation device that irradiates the sample surface with a laser beam to heat it, a device that forms a vacuum or a specific gas atmosphere in a certain area including the sample, and an X-ray irradiation device that injects X-rays into the sample; 1. A real-time crystal production/analysis/evaluation device comprising: a device for observing a diffraction X-ray pattern of a surface state of a sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19609186A JPS6351623A (en) | 1986-08-20 | 1986-08-20 | Realtime manufacturing, analyzing and evaluating device for crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19609186A JPS6351623A (en) | 1986-08-20 | 1986-08-20 | Realtime manufacturing, analyzing and evaluating device for crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6351623A true JPS6351623A (en) | 1988-03-04 |
Family
ID=16352061
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19609186A Pending JPS6351623A (en) | 1986-08-20 | 1986-08-20 | Realtime manufacturing, analyzing and evaluating device for crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6351623A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002057763A2 (en) * | 2000-10-19 | 2002-07-25 | Structural Genomix, Inc. | Apparatus and method for identification of crystals by in-situ x-ray diffraction |
| KR20030000411A (en) * | 2001-06-25 | 2003-01-06 | 주식회사 에셀텍 | Tft-lcd repair method using nd:yag laser |
-
1986
- 1986-08-20 JP JP19609186A patent/JPS6351623A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002057763A2 (en) * | 2000-10-19 | 2002-07-25 | Structural Genomix, Inc. | Apparatus and method for identification of crystals by in-situ x-ray diffraction |
| WO2002057763A3 (en) * | 2000-10-19 | 2003-01-23 | Structural Genomix Inc | Apparatus and method for identification of crystals by in-situ x-ray diffraction |
| KR20030000411A (en) * | 2001-06-25 | 2003-01-06 | 주식회사 에셀텍 | Tft-lcd repair method using nd:yag laser |
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