JPH0410022B2 - - Google Patents
Info
- Publication number
- JPH0410022B2 JPH0410022B2 JP56023285A JP2328581A JPH0410022B2 JP H0410022 B2 JPH0410022 B2 JP H0410022B2 JP 56023285 A JP56023285 A JP 56023285A JP 2328581 A JP2328581 A JP 2328581A JP H0410022 B2 JPH0410022 B2 JP H0410022B2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- container
- coolant
- cooling plate
- vacuum
- 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
- 239000002826 coolant Substances 0.000 claims description 27
- 238000001816 cooling Methods 0.000 claims description 24
- 239000000758 substrate Substances 0.000 claims description 16
- 238000002441 X-ray diffraction Methods 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 3
- 239000012780 transparent material Substances 0.000 claims 2
- 230000008878 coupling Effects 0.000 claims 1
- 238000010168 coupling process Methods 0.000 claims 1
- 238000005859 coupling reaction Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 229920002799 BoPET Polymers 0.000 description 12
- 239000005041 Mylar™ Substances 0.000 description 12
- 239000007789 gas Substances 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052790 beryllium Inorganic materials 0.000 description 2
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000000112 cooling gas Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000000110 cooling liquid Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
- G01N23/20033—Sample holders or supports therefor provided with temperature control or heating means
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
Description
【発明の詳細な説明】
本発明は低温の液体試料等のＸ線回折を求める
のに適したＸ線回折装置に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an X-ray diffraction apparatus suitable for determining X-ray diffraction of a low-temperature liquid sample.
比較的低い温度状態で試料のＸ線回折を求めた
いという強い要請がありいくつかの提案が行なわ
れている。冷却ガス吹付法は固体もしくは液体の
試料に液体窒素を気化させた冷却ガスを吹きつけ
て試料の温度を降下させる方法である。この吹付
低温装置は固体もしくは液体の試料を低温にする
ことが可能であるが補助装置を含めて全装置がき
わめて大がかりになり簡便に利用しにくいという
問題がある。断熱のために真空にした容器内に試
料を封入して冷却する装置も実施されている。こ
のような装置は試料が固体である場合は問題がな
いが、液体の場合は試料が真空容器内に散逸して
しまうので液体試料の測定には適しない。軽油中
のある成分は低温で結晶化することが知られてい
るが、このような試料のＸ線回折を求めることは
従来不可能であつた。 There is a strong desire to obtain X-ray diffraction of a sample at a relatively low temperature, and several proposals have been made. The cooling gas spraying method is a method in which a cooling gas made by vaporizing liquid nitrogen is sprayed onto a solid or liquid sample to lower the temperature of the sample. Although this spray cryogenic apparatus is capable of lowering a solid or liquid sample to a low temperature, there is a problem in that the entire apparatus including auxiliary equipment is extremely large-scale, making it difficult to use easily. Devices have also been implemented in which a sample is sealed in a vacuum-filled container for insulation and then cooled. Such an apparatus has no problem when the sample is solid, but when the sample is liquid, the sample dissipates into the vacuum container, so it is not suitable for measuring liquid samples. Although it is known that certain components in gas oil crystallize at low temperatures, it has previously been impossible to obtain X-ray diffraction of such samples.
本発明の目的は低温液体試料等のＸ線回折分析
を可能にするＸ線回折装置における低温液体試料
支持装置を提供することにある。 An object of the present invention is to provide a low-temperature liquid sample support device in an X-ray diffraction apparatus that enables X-ray diffraction analysis of low-temperature liquid samples.
前記目的を達成するために本発明によるＸ線回
折装置における低温試料支持装置は、Ｘ線回折装
置において、
内容器に冷却剤が充填されて外容器間が真空に
保たれ得る冷却剤容器と、
前記内容器内の冷却剤に冷却剤導入管を介して
熱結合させられ、前記冷却剤容器の下方で水平方
向に位置させられている冷却板と、
前記冷却板に垂直に結合させられている試料基
板と、
前記基板の前方に着脱可能であり、前面にＸ線
透過膜が設けられている試料容器と、
前記基板の後方に取りつけられた温度調整のた
めのヒータと、
前方にＸ線透過物質による窓が設けられ、か
つ、ガス封入口が設けられており、前記冷却板に
結合させられて密封された試料室を形成するケー
スと、
前方に前記窓に対応してＸ線透過物質による窓
が設けられ、
真空引出口を有し前記試料室を収容して前記冷
却剤容器の外容器に結合可能な真空室とから構成
されている。 In order to achieve the above object, the present invention provides a low-temperature sample support device for an X-ray diffraction apparatus, which includes: a coolant container in which an inner container is filled with a coolant to maintain a vacuum between the outer containers; a cooling plate thermally coupled to the coolant in the inner container via a coolant introduction pipe and positioned horizontally below the coolant container; and vertically coupled to the cooling plate. a sample substrate; a sample container that is removably attached to the front of the substrate and has an X-ray transmission membrane on the front; a heater for temperature adjustment that is attached to the rear of the substrate; and an X-ray transmission membrane on the front. a case provided with a window made of material and a gas inlet, which is coupled to the cooling plate to form a sealed sample chamber; A vacuum chamber is provided with a window, has a vacuum outlet, accommodates the sample chamber, and is connectable to the outer container of the coolant container.
上記構成によれば試料室は真空空間とは分離さ
れているので前述した問題は完全に解決できる。
また冷却剤容器と真空室とは分離可能であり、真
空室内に位置する試料室内への試料の充填も容易
となり操作性においても秀れている。 According to the above configuration, since the sample chamber is separated from the vacuum space, the above-mentioned problem can be completely solved.
In addition, the coolant container and the vacuum chamber can be separated, and it is easy to fill the sample chamber located within the vacuum chamber, resulting in excellent operability.
以下、図面等を参照して本発明をさらに詳しく
説明する。 Hereinafter, the present invention will be explained in more detail with reference to the drawings and the like.
第１図は本発明の実施例装置の主として冷却剤
容器を破断して示した側面図、第２図は前記容器
の内外容器間に連通する真空室との結合状態を示
す側面図であつてＸ線回折装置の他の構成部分と
の関連を示してある。冷却剤容器１は内容器１ｂ
と外容器１ａからなる、いわゆるデユワー容器を
形成しており、内容器内に上方から冷却液剤であ
る液体窒素が充填され密封可能に構成されてい
る。内容器１ｂの底にはブロツク１ｃが設けられ
ており、このブロツク１ｃには銅の導入管１０が
結合されており、この管１０の内部に液体窒素が
導入されている。この導入管１０の下端には銅の
円板状の冷却板１１が結合させられている。 FIG. 1 is a side view mainly showing a cutaway coolant container of an apparatus according to an embodiment of the present invention, and FIG. 2 is a side view showing a state in which the container is connected to a vacuum chamber communicating between the inner and outer containers. The relationship with other components of the X-ray diffraction device is shown. Coolant container 1 is inner container 1b
and an outer container 1a, forming a so-called dewar container, and the inner container is filled with liquid nitrogen, which is a cooling liquid, from above and is configured to be able to be sealed. A block 1c is provided at the bottom of the inner container 1b, and a copper introduction tube 10 is connected to this block 1c, into which liquid nitrogen is introduced. A copper disc-shaped cooling plate 11 is coupled to the lower end of the introduction pipe 10.
この冷却板１１は相当の熱慣性をもち常時冷却
されて低温度に保たされている。この冷却板１１
には金属パツキング１７を介して試料室ケース１
３が気密に固定される。 This cooling plate 11 has considerable thermal inertia and is constantly cooled and kept at a low temperature. This cooling plate 11
The sample chamber case 1 is connected to the sample chamber case 1 via the metal packing 17.
3 is fixed airtight.
この試料室の内部を第３図以後を参照して説明
する。前記冷却板１１には第３図に示されている
ように試料基板１２が垂直に接合されており、こ
の基板も冷却板１１と熱的に結合しており、同様
に冷却される。この基板１２の前面に試料容器
が、後面には加温装置が固定されている。試料容
器は前面に開く窓を有し、上方に３本の試料注入
孔（第４図参照）を有する試料板１８と試料板押
え２０に展着されて前記試料板１８に結合され前
記窓を封じるマイラー１９により構成されてい
る。 The inside of this sample chamber will be explained with reference to FIG. 3 and subsequent figures. As shown in FIG. 3, a sample substrate 12 is vertically joined to the cooling plate 11, and this substrate is also thermally connected to the cooling plate 11 and is similarly cooled. A sample container is fixed to the front surface of this substrate 12, and a heating device is fixed to the rear surface. The sample container has a window that opens on the front, and is attached to a sample plate 18 having three sample injection holes (see FIG. 4) at the top and a sample plate holder 20, and is connected to the sample plate 18 so that the window opens. It is made of sealing Mylar 19.
前記マイラー１９を試料板押え２０に展着する
さいにはマイラー１９を十分に引き伸す治具を用
いる。試料板押えの接合面に接着剤をつけて伸展
されているマイラー１９に接合することにより均
一なマイラー窓が作られる。試料基板の後面側に
ヒータ２２がヒータ押え２２ａによつて固定され
る。なお、この試料基板１２の温度を知るために
試料基板１２内部に熱電対２３を埋め込んであ
る。（第７図参照）。このヒータに電力を供給する
リードおよび熱電対の電位差を外部に伝達するた
めのリード７は前記冷却板１１を貫通し、冷却剤
容器１の真空部を通り容器１の上方に取り出され
ている。前記冷却板１１を貫通する部分、いわゆ
るハーメチツクシール部１６となつている。第１
図に示すように冷却剤容器１上には中継ボツクス
８が設けられており、そのターミナル６を介して
ヒータに電力が供給され、リード７ａを介して熱
電対の電位差が取り出される。金属性パツキング
１７を介して前記冷却板に気密に固定される試料
室ケース１３の前面にはベリリユウムのＸ線窓が
バンド状のリング１５でケース１３の前方開口部
に固定されている。 When spreading the Mylar 19 onto the sample plate holder 20, a jig is used to sufficiently stretch the Mylar 19. A uniform Mylar window is created by applying adhesive to the joint surface of the sample plate holder and joining it to the stretched Mylar 19. A heater 22 is fixed to the rear side of the sample substrate by a heater holder 22a. Note that in order to know the temperature of this sample substrate 12, a thermocouple 23 is embedded inside the sample substrate 12. (See Figure 7). Leads for supplying power to the heater and leads 7 for transmitting the potential difference between the thermocouples to the outside pass through the cooling plate 11, pass through the vacuum part of the coolant container 1, and are taken out above the container 1. A portion passing through the cooling plate 11 is a so-called hermetic seal portion 16. 1st
As shown in the figure, a relay box 8 is provided on the coolant container 1, and power is supplied to the heater through the terminal 6 of the relay box 8, and the potential difference of the thermocouple is taken out through the lead 7a. A beryllium X-ray window is fixed to the front opening of the case 13 with a band-shaped ring 15 on the front surface of the sample chamber case 13, which is airtightly fixed to the cooling plate via a metal packing 17.
第６図は試料室ケース１３の底面図であつて、
バンド１５の締付け状態が示されている。この試
料室ケース１３には試料室内を乾燥空気または窒
素ガスを充填するためのガス封入口２４が設けら
れている。この封入口２４はガスを充填するとと
もにすでに入つていたガスを取り出すことができ
るように二重口になつており、中央からパイプ２
５を介して充填し外周より上下方からすでに充填
されていたガスを排出し、内部ガスの入れ替えを
可能にしている。このガスの充填は市販のN2ま
たは乾燥空気ボンベを用いることにより簡単に行
なえる。この試料室は第２図に示す真空室の中央
に位置させられる。真空室２の前面開口には金属
蒸着マイラー（ネツト付）のＸ線窓がバンド状の
マイラー押え４により固定されている。この真空
室２と前記冷却剤容器は着脱可能であり固定金具
２４により固定される。前記冷却剤容器１と真空
室２と固定し、真空室２に設けられている真空引
口５を図示しない真空ポンプに接続すると、真空
室内とこれに連通する冷却剤容器１の外周空間は
真空に近づけられる。 FIG. 6 is a bottom view of the sample chamber case 13.
The tightened state of the band 15 is shown. The sample chamber case 13 is provided with a gas filling port 24 for filling the sample chamber with dry air or nitrogen gas. This filling port 24 has a double port so that it can be filled with gas and also take out the gas that has already entered, and the pipe 2 is connected from the center.
5, and the gas already filled is discharged from above and below from the outer periphery, making it possible to replace the internal gas. Filling with this gas can be easily performed using a commercially available N 2 or dry air cylinder. This sample chamber is located in the center of the vacuum chamber shown in FIG. An X-ray window made of metal-deposited mylar (with a net) is fixed to the front opening of the vacuum chamber 2 by a band-shaped mylar holder 4. The vacuum chamber 2 and the coolant container are removable and fixed by a fixing fitting 24. When the coolant container 1 and the vacuum chamber 2 are fixed and the vacuum outlet 5 provided in the vacuum chamber 2 is connected to a vacuum pump (not shown), the vacuum chamber and the outer circumferential space of the coolant container 1 communicating with the vacuum chamber become vacuum. can be approached.
この冷却剤容器と真空室１の組立は第２図破線
で示すゴニオメータ３１上に搭載される。試料と
ゴニオメータ３１との中心合わせは試料位置合わ
せ機構９により微調整することにより行なわれ
る。 This assembly of the coolant container and the vacuum chamber 1 is mounted on a goniometer 31 shown in broken lines in FIG. Center alignment between the sample and the goniometer 31 is performed by finely adjusting the sample positioning mechanism 9.
第２図中に破線でチユーブシールド３０を示し
てある。この中にはＸ線源であるＸ線管が収容さ
れている。 The tube shield 30 is shown in broken lines in FIG. This contains an X-ray tube that is an X-ray source.
本発明による装置は以上のように構成されてい
るので、冷却剤容器１を真空室２から固定金具２
７を操作して分離した状態で冷却板１１から試料
ケースを取りはずすことができる。その状態で試
料室への液体試料の装着を行なう。液体試料を試
料板１８とマイラー１９で形成される空間に充填
し、試料室ケース１３を冷却板１１に固定するこ
とにより独立した試料室空間が形成される。試料
室空間への窒素ガス等の充填は栓２６をはずして
ボンベを接続して充填終了後に栓２６を閉じる。
試料室の準備が完了し、真空室２と冷却容器１を
結合し、図示しない真空ポンプを作動させると試
料室外周および冷却室の外周空間は真空に近づけ
られる。 Since the apparatus according to the present invention is constructed as described above, the coolant container 1 can be moved from the vacuum chamber 2 to the fixture 2.
7 to remove the sample case from the cooling plate 11 in a separated state. In this state, the liquid sample is loaded into the sample chamber. An independent sample chamber space is formed by filling the space formed by the sample plate 18 and Mylar 19 with a liquid sample and fixing the sample chamber case 13 to the cooling plate 11. To fill the sample chamber space with nitrogen gas or the like, the plug 26 is removed, a cylinder is connected, and the plug 26 is closed after filling is completed.
When the preparation of the sample chamber is completed, the vacuum chamber 2 and the cooling container 1 are connected, and a vacuum pump (not shown) is operated, the outer periphery of the sample chamber and the outer circumferential space of the cooling chamber are brought close to vacuum.
冷却容器１には上部から液体窒素などの冷却剤
を充填され密封されており、冷却板１１とこれと
一体に熱結合させられている試料基板１２、試料
板１８およびこれに収容されている液体試料は冷
却される。 The cooling container 1 is filled with a coolant such as liquid nitrogen from above and sealed, and contains a cooling plate 11, a sample substrate 12 which is thermally coupled to the cooling plate 11, a sample plate 18, and the liquid contained therein. The sample is cooled.
冷却剤を用いて冷却しうる最低の温度以上の温
度を得るためにヒータ２２が作動させられ、試料
基板の温度（＝試料温度）は熱電対２３の出力に
より常時監視される。測定温度に達した時に外部
のチユーブシールド３０内Ｘ線源を作動させる
と、Ｘ線は真空室のマイラーの窓３、試料室のケ
ースＸ線窓１４（ベリリウム）、および試料室の
マイラー１９の窓を介して試料液体に達し、回折
させられる。回折Ｘ線は前記とは逆に１９→１４
→３を透過して図示しないＸ線検出器に達し検出
される。 The heater 22 is operated to obtain a temperature higher than the lowest temperature that can be cooled using a coolant, and the temperature of the sample substrate (=sample temperature) is constantly monitored by the output of the thermocouple 23. When the X-ray source in the external tube shield 30 is activated when the measurement temperature is reached, the X-rays are transmitted through the Mylar window 3 in the vacuum chamber, the case X-ray window 14 (beryllium) in the sample chamber, and the Mylar 19 in the sample chamber. The sample liquid is reached through the window and is diffracted. Contrary to the above, diffraction X-rays are 19 → 14
→It passes through 3 and reaches an X-ray detector (not shown), where it is detected.
以上詳しく説明した実施例において、冷媒とし
て液体窒業を用いると試料の温度は−190℃から
＋40℃まで可変できる。取扱いは前述したように
簡単であり、広い応用が期待できる。なお、前述
した実施例は低温液体の例について述べてあるが
液体だけではなく粉末などの分析にも好適に応用
できる。 In the embodiment described in detail above, when liquid nitrogen is used as the refrigerant, the temperature of the sample can be varied from -190°C to +40°C. As mentioned above, it is easy to handle and can be expected to have a wide range of applications. Note that although the above-mentioned embodiments have been described with respect to low-temperature liquids, the present invention can be suitably applied to analysis of not only liquids but also powders.
第１図から第７図は本発明による装置の実施例
を示す図であつて、第１図は冷却剤容器と試料室
の関係を示す側断面図、第２図は前記冷却剤容器
と真空室、Ｘ線管ゴニオメータなどの位置関係を
示す側面図、第３図は試料室の側断面図、第４図
は試料容器の正面図、第５図は試料容器の背面
図、第６図は同底面図、第７図は試料容器を冷却
板との関係を展開的に示した斜視図である。
１……冷却剤容器、２……真空室、３……Ｘ線
窓（真空容器）、４……マイラー押え、５……真
空引口、６……ヒータ端子、７……リード線、８
……中継ボツクス、９……試料位置調整機構、１
０……液体窒素導入管、１１……冷却板、１２…
…試料基板、１３……試料室ケース、１４……ケ
ースＸ線窓、１５……リング、１６……密栓（ハ
ーメチツクシール）、１７……パツキング、１８
……試料板、１９……マイラー、２０……試料板
押え、２１……ねじ、２２……ヒータ、２２ａ…
…ヒータ押え、２３……熱電対、２４……ガス封
入口、２５……パイプ、２６……栓、２７……固
定金具、３０……チユーブシールド、３１……ゴ
ニオメータ。
1 to 7 are views showing an embodiment of the apparatus according to the present invention, in which FIG. 1 is a side sectional view showing the relationship between the coolant container and the sample chamber, and FIG. 2 is a side sectional view showing the relationship between the coolant container and the vacuum chamber. Figure 3 is a side sectional view of the sample chamber, Figure 4 is a front view of the sample container, Figure 5 is a rear view of the sample container, and Figure 6 is a side view showing the positional relationship of the chamber, X-ray tube goniometer, etc. The bottom view and FIG. 7 are perspective views showing the relationship between the sample container and the cooling plate. 1... Coolant container, 2... Vacuum chamber, 3... X-ray window (vacuum container), 4... Mylar presser foot, 5... Vacuum outlet, 6... Heater terminal, 7... Lead wire, 8
... Relay box, 9 ... Sample position adjustment mechanism, 1
0...Liquid nitrogen introduction pipe, 11...Cooling plate, 12...
... Sample substrate, 13 ... Sample chamber case, 14 ... Case X-ray window, 15 ... Ring, 16 ... Hermetic seal, 17 ... Packing, 18
...Sample plate, 19...Mylar, 20...Sample plate holder, 21...Screw, 22...Heater, 22a...
... Heater holder, 23 ... Thermocouple, 24 ... Gas filling port, 25 ... Pipe, 26 ... Plug, 27 ... Fixing metal fittings, 30 ... Tube shield, 31 ... Goniometer.
Claims (1)
保たれ得る冷却剤容器と、 前記内容器内の冷却剤に冷却剤導入管を介して
熱結合させられ、前記冷却剤容器の下方で水平方
向に位置させられている冷却板と、 前記冷却板に垂直に結合させられている試料基
板と、 前記基板の前方に着脱可能であり、前面にＸ線
透過膜が設けられている試料容器と、 前記基板の後方に取りつけられた温度調整のた
めのヒータと、 前方にＸ線透過物質による窓が設けられ、か
つ、ガス封入口が設けられており、前記冷却板に
結合させられて密封された試料室を形成するケー
スと、 前方に前記窓に対応してＸ線透過物質による窓
が設けられ、 真空引出口を有し前記試料室を収容して前記冷
却剤容器の外容器に結合可能な真空室とからなる
Ｘ線回折装置における低温試料支持装置。[Scope of Claims] 1. An X-ray diffraction apparatus comprising: a coolant container in which an inner container is filled with a coolant to maintain a vacuum between the outer containers; and a coolant inlet tube that connects the coolant in the inner container. a cooling plate that is thermally coupled to the cooling plate and positioned horizontally below the coolant container; a sample substrate that is vertically coupled to the cooling plate; and a sample substrate that is detachable in front of the substrate; A sample container with an X-ray transparent membrane on the front, a heater for temperature adjustment attached to the rear of the substrate, a window made of an X-ray transparent material on the front, and a gas filling port. a case that is coupled to the cooling plate to form a sealed sample chamber; a window made of an X-ray transparent material is provided in the front corresponding to the window, and a vacuum outlet is provided to form a sealed sample chamber; and a vacuum chamber capable of accommodating and coupling to an outer container of the coolant container.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56023285A JPS57136149A (en) | 1981-02-18 | 1981-02-18 | Device for supporting low temperature sample in x ray diffraction device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56023285A JPS57136149A (en) | 1981-02-18 | 1981-02-18 | Device for supporting low temperature sample in x ray diffraction device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS57136149A JPS57136149A (en) | 1982-08-23 |
| JPH0410022B2 true JPH0410022B2 (en) | 1992-02-24 |
Family
ID=12106326
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP56023285A Granted JPS57136149A (en) | 1981-02-18 | 1981-02-18 | Device for supporting low temperature sample in x ray diffraction device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS57136149A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01112132A (en) * | 1987-10-27 | 1989-04-28 | Rigaku Denki Kk | Low-temperature device for sample |
| JP2559622Y2 (en) * | 1990-06-22 | 1998-01-19 | 株式会社 マックサイエンス | Sample cryogenic device |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5233263Y2 (en) * | 1974-04-10 | 1977-07-29 |
-
1981
- 1981-02-18 JP JP56023285A patent/JPS57136149A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS57136149A (en) | 1982-08-23 |
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