JPH09161707A - Sample cooling observing device - Google Patents
Sample cooling observing deviceInfo
- Publication number
- JPH09161707A JPH09161707A JP7319951A JP31995195A JPH09161707A JP H09161707 A JPH09161707 A JP H09161707A JP 7319951 A JP7319951 A JP 7319951A JP 31995195 A JP31995195 A JP 31995195A JP H09161707 A JPH09161707 A JP H09161707A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- heating
- heating element
- cooling
- temperature
- 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
Landscapes
- Sampling And Sample Adjustment (AREA)
- Resistance Heating (AREA)
- Devices For Use In Laboratory Experiments (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、走査形電子顕微鏡
及びその類似装置に係り、特に、走査形電子顕微鏡に使
用するに好適な試料冷却観察装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a scanning electron microscope and a device similar thereto, and more particularly to a sample cooling observation device suitable for use in a scanning electron microscope.
【０００２】[0002]
【従来の技術】試料に収束電子線を照射し、走査するこ
とにより、試料から得られる信号をもとに走査像を得る
装置、いわゆる走査形電子顕微鏡（通称ＳＥＭ）では、
試料をできるだけ生の状態で観察したいという要求が最
近ますます多くなってきている。そのための方法の一つ
として、試料を冷却した状態で観察する、いわゆる試料
冷却観察装置が使用されている。また、試料室を１〜２
７０Ｐａ程度の低真空度にして試料からの水分の蒸発を
できるだけ少なくして観察する方法も用いられている。
さらに、この両者を組み合わせる方法も用いられてい
る。しかるに、高分子材料や低融点物質など、試料によ
っては、−２０℃以下の低い温度に素速く冷却し、一定
温度に調節しながら観察する場合があり、できるだけ応
答性の良い冷却装置が望ましい。また、試料室を１〜２
７０Ｐａ程度の低真空度にしても、さらには大気圧状態
にしても容易に温度調整ができるようになっていること
が望ましい。従来技術では、この点での考慮が払われて
おらず、−２０℃以下の低い温度設定が困難であった
り、試料室を１〜２７０Ｐａ程度の低真空度にすると、
温度調整を行うための加熱部材が焼損により寿命が著し
く短くなるなどの難点があった。2. Description of the Related Art An apparatus for obtaining a scanning image based on a signal obtained from a sample by irradiating a sample with a convergent electron beam and scanning the so-called scanning electron microscope (commonly called SEM)
Recently, there has been an increasing demand for observing samples as raw as possible. As one of the methods for that purpose, a so-called sample cooling observation device for observing the sample in a cooled state is used. In addition, the sample chamber is
There is also used a method of observing with a low vacuum degree of about 70 Pa to minimize evaporation of water from the sample.
Furthermore, a method of combining the both is also used. However, depending on the sample such as a polymer material or a low-melting point substance, it may be cooled to a low temperature of −20 ° C. or lower quickly and observed while adjusting to a constant temperature, and a cooling device having a good responsiveness is desirable. In addition, the sample chamber is
It is desirable that the temperature can be easily adjusted even when the degree of vacuum is about 70 Pa or even at atmospheric pressure. In the prior art, no consideration has been given to this point, and it is difficult to set a low temperature of -20 ° C. or lower, or if the sample chamber has a low vacuum degree of about 1 to 270 Pa,
There has been a problem that the life of the heating member for adjusting the temperature is remarkably shortened due to burning.
【０００３】[0003]
【発明が解決しようとする課題】本発明は従来技術の難
点をなくし、−２０℃以下の低い温度設定や調整が容易
で、かつ大気圧状態でも長時間温度調整が可能な試料冷
却観察装置を提供することにある。DISCLOSURE OF THE INVENTION The present invention eliminates the drawbacks of the prior art, and provides a sample cooling observation apparatus capable of easily setting and adjusting a low temperature of −20 ° C. or less and capable of adjusting the temperature for a long time even at atmospheric pressure. To provide.
【０００４】[0004]
【課題を解決するための手段】上記の目的を達成するた
めに、本発明では、試料を冷却状態にして観察する手段
を有する走査形電子顕微鏡及びその類似装置の試料冷却
観察装置において、前記試料を載せる部材の近くに、試
料温度を調節するための加熱手段を設け、前記加熱手段
は、大気圧状態から試料観察時の試料室圧力状態に至る
まで、任意に加熱できる部材で構成する。前記加熱部材
は、白金線と絶縁物からなる発熱体と、前記発熱体を遮
蔽するケースとで構成するか、または、ニクロム線と絶
縁物からなる発熱体と、前記発熱体を遮蔽するケースと
で構成する。あるいは、前記加熱部材は、セラミックヒ
ータで構成した。In order to achieve the above object, the present invention provides a scanning electron microscope having a means for observing a sample in a cooled state and a sample cooling and observing device of an apparatus similar to the scanning electron microscope. A heating unit for adjusting the sample temperature is provided near the member on which the sample is placed, and the heating unit is configured by a member capable of arbitrarily heating from the atmospheric pressure state to the sample chamber pressure state during sample observation. The heating member is composed of a heating element made of a platinum wire and an insulator, and a case for shielding the heating element, or a heating element made of a nichrome wire and an insulator, and a case for shielding the heating element. It consists of. Alternatively, the heating member is composed of a ceramic heater.
【０００５】この構成によれば、−２０℃以下の低い温
度設定や調整が容易で、かつ大気圧状態でも長時間温度
調整が可能な試料冷却観察装置を提供することが可能と
なる。According to this structure, it is possible to provide a sample cooling observation apparatus which can easily set and adjust a temperature as low as −20 ° C. or lower and can adjust the temperature for a long time even at atmospheric pressure.
【０００６】[0006]
【発明の実施の形態】以下で本発明の具体的実施例を図
面を用いて詳述する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Specific embodiments of the present invention will be described in detail below with reference to the drawings.
【０００７】図１は本発明の一実施例である。FIG. 1 shows an embodiment of the present invention.
【０００８】同図において、対物レンズ１によって細く
絞られた電子ビーム２は、試料３上で走査され、この試
料表面より発生した２次電子や反射電子(いずれも図示
せず)が、いわゆるＳＥＭ像としての電子信号となる。
試料３は、試料室４に取付けられた試料冷却装置５によ
って冷却される。すなわち、試料３が載置されている冷
却体６の他端は、断熱材７，カバー８などからなる冷却
容器９とつながっており、例えば、液体窒素のような冷
却剤１０で冷却される。試料の微動は、ステージボデー
１１とつまみ１２，真空Ｏリング１３，１４などからな
る試料微動装置１５によりＸ，Ｙ，Ｚ方向に移動できる
ようになっている。また、試料室には、エアロック手段
１６を介して試料処理室１７が設けられ、試料の交換や
切断などが行えるようになっている。試料の温度制御
は、試料台１８の近くに取付けられた熱電対１９と、加
熱手段２０によって行う。加熱手段２０は、試料台１８
を載せる冷却体６に密着して取付けられた加熱部材２１
と、電流導入線２２などで構成されている。温度制御
は、試料室の外側より、熱電対メータ２３と、ヒータ電
流計２４などから成る温度制御装置２５により行われ
る。加熱部材２１は、図２に示すように、白金線条２６
と絶縁体２７，電流導入端子２８，リード線２９及び遮
蔽用ケース３０などから構成されている。遮蔽用ケース
３０は、加熱時の光もれ防止と、発熱体からの輻射熱
が、試料台１８に効率よく伝わるよう、熱の良導体（金
属）で構成され、上面は冷却体６に密着し、下面には真
空排気用の孔３１を有している。発熱体に用いている白
金線条２６は、空気，水分に対して極めて安定であり、
大気中で通電しても、長時間安定に加熱状態を維持でき
る。また、この構造により、放出ガスが少なく、発熱体
は熱しやすく、冷めやすいので、温度制御の応答性も速
いという利点がある。したがって、大気圧条件から試料
観察条件（通常、２７０Ｐａ〜１０-3Ｐａ）の広い範囲
にわたって、長時間容易に温度制御が可能である。In FIG. 1, an electron beam 2 narrowed down by an objective lens 1 is scanned on a sample 3, and secondary electrons and reflected electrons (neither shown) generated from the sample surface are so-called SEM. It becomes an electronic signal as an image.
The sample 3 is cooled by the sample cooling device 5 attached to the sample chamber 4. That is, the other end of the cooling body 6 on which the sample 3 is placed is connected to a cooling container 9 including a heat insulating material 7, a cover 8 and the like, and is cooled by a coolant 10 such as liquid nitrogen. The fine movement of the sample can be moved in the X, Y, and Z directions by the fine movement device 15 of the stage body 11, the knob 12, the vacuum O-rings 13, 14, and the like. Further, a sample processing chamber 17 is provided in the sample chamber via an air lock means 16 so that the sample can be exchanged or cut. The temperature control of the sample is performed by a thermocouple 19 mounted near the sample table 18 and a heating means 20. The heating means 20 is the sample table 18
The heating member 21 closely attached to the cooling body 6 on which the object is placed
And a current introduction line 22 and the like. The temperature control is performed from the outside of the sample chamber by a temperature control device 25 including a thermocouple meter 23 and a heater ammeter 24. The heating member 21, as shown in FIG.
And an insulator 27, a current introduction terminal 28, a lead wire 29, a shielding case 30, and the like. The shielding case 30 is made of a good heat conductor (metal) so that light leakage during heating is prevented and radiant heat from the heating element is efficiently transmitted to the sample stage 18, and the upper surface thereof is in close contact with the cooling body 6. The lower surface has a hole 31 for evacuation. The platinum filament 26 used for the heating element is extremely stable against air and moisture,
Even if electricity is applied in the atmosphere, the heating state can be stably maintained for a long time. Further, with this structure, the amount of released gas is small, and the heating element is easy to heat and cool, which is advantageous in that the temperature control response is fast. Therefore, temperature control can be easily performed for a long time over a wide range from atmospheric pressure conditions to sample observation conditions (usually 270 Pa to 10 −3 Pa).
【０００９】図３は、本発明における他の一実施例であ
り、ニクロム線３２を、絶縁体３３の中に封じ込み、外
部を遮蔽用ケース３４で囲った加熱部材３５の例であ
る。FIG. 3 shows another embodiment of the present invention, which is an example of a heating member 35 in which a nichrome wire 32 is enclosed in an insulator 33 and the outside is surrounded by a shielding case 34.
【００１０】図４は、本発明における加熱部材の他の一
実施例であり、セラミックヒータ３６で構成したもので
ある。この実施例では、内部に発熱体（図示せず）が密
封されており、加熱部材そのものを薄く、軽量化できる
利点がある。FIG. 4 shows another embodiment of the heating member according to the present invention, which comprises a ceramic heater 36. In this embodiment, a heating element (not shown) is sealed inside, and there is an advantage that the heating member itself can be made thin and lightweight.
【００１１】なお、図１では走査形電子顕微鏡に適用し
た場合についての実施例を示したが、本発明の内容はこ
れに限定されるものではなく、例えば走査像装置を有す
る透過形電子顕微鏡に適用した場合についても同様の効
果を奏しうる。Although FIG. 1 shows an embodiment applied to a scanning electron microscope, the content of the present invention is not limited to this. For example, a transmission electron microscope having a scanning image device is used. The same effect can be obtained when applied.
【００１２】[0012]
【発明の効果】本発明によれば、−２０℃以下の低い温
度設定や調整が容易で、かつ大気圧状態でも長時間温度
調整が可能な試料冷却観察装置を提供することが可能と
なる。According to the present invention, it is possible to provide a sample cooling observation apparatus which can easily set and adjust a temperature as low as −20 ° C. or lower and can adjust the temperature for a long time even at atmospheric pressure.
【図１】本発明の一実施例を示す断面図。FIG. 1 is a sectional view showing an embodiment of the present invention.
【図２】本発明の加熱部材の一実施例を示す断面図。FIG. 2 is a sectional view showing an embodiment of a heating member of the present invention.
【図３】本発明の加熱部材の第二の実施例を示す断面
図。FIG. 3 is a sectional view showing a second embodiment of the heating member of the present invention.
【図４】本発明の加熱部材の第三の実施例を示す断面
図。FIG. 4 is a sectional view showing a third embodiment of the heating member of the present invention.
２…電子ビーム、３…試料、６…冷却体、１８…試料
台、１９…熱電対、２０…加熱手段、２１…加熱部材。2 ... Electron beam, 3 ... Sample, 6 ... Cooling body, 18 ... Sample stand, 19 ... Thermocouple, 20 ... Heating means, 21 ... Heating member.
Claims (4)
る走査形電子顕微鏡及びその類似装置の試料冷却観察装
置において、前記試料を載せる部材の近くに、前記試料
の温度を調節するための加熱手段を設け、前記加熱手段
は、大気圧状態から前記試料の観察時の試料室圧力状態
に至るまで、任意に加熱できる部材で構成したことを特
徴とする試料冷却観察装置。1. A sample cooling observation apparatus of a scanning electron microscope and a similar apparatus having means for observing a sample in a cooled state, and heating for adjusting the temperature of the sample near a member on which the sample is placed. A sample cooling and observation apparatus characterized in that a heating means is provided, and the heating means is constituted by a member capable of arbitrarily heating from an atmospheric pressure state to a sample chamber pressure state at the time of observing the sample.
発熱体と、前記発熱体を遮蔽するケースとで構成した請
求項１に記載の試料冷却観察装置。2. The sample cooling observation apparatus according to claim 1, wherein the heating member includes a heating element made of a platinum wire and an insulator, and a case for shielding the heating element.
なる発熱体と、前記発熱体を遮蔽するケースとで構成し
た請求項１に記載の試料冷却観察装置。3. The sample cooling observation apparatus according to claim 1, wherein the heating member includes a heating element made of a nichrome wire and an insulator, and a case that shields the heating element.
した請求項１に記載の試料冷却観察装置。4. The sample cooling observation apparatus according to claim 1, wherein the heating member is a ceramic heater.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7319951A JPH09161707A (en) | 1995-12-08 | 1995-12-08 | Sample cooling observing device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7319951A JPH09161707A (en) | 1995-12-08 | 1995-12-08 | Sample cooling observing device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH09161707A true JPH09161707A (en) | 1997-06-20 |
Family
ID=18116073
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7319951A Pending JPH09161707A (en) | 1995-12-08 | 1995-12-08 | Sample cooling observing device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH09161707A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7531797B2 (en) | 2003-01-21 | 2009-05-12 | Canon Kabushiki Kaisha | Probe-holding apparatus, sample-obtaining apparatus, sample-processing apparatus, sample-processing method and sample-evaluating method |
| JP2016031928A (en) * | 2014-07-29 | 2016-03-07 | ライカ ミクロジュステーメ ゲーエムベーハー | Manipulation container for cryomicroscopy |
| JP6279692B1 (en) * | 2016-11-07 | 2018-02-14 | 株式会社メルビル | Sample holder |
| CN110475394A (en) * | 2019-08-23 | 2019-11-19 | 杭州源位科技有限公司 | A kind of heating device applied in vacuum equipment |
| KR20200092751A (en) * | 2019-01-25 | 2020-08-04 | 서울대학교산학협력단 | Cryocooler for measuring multiple physical property at low temperature and method for measuring specific heat using the same |
-
1995
- 1995-12-08 JP JP7319951A patent/JPH09161707A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7531797B2 (en) | 2003-01-21 | 2009-05-12 | Canon Kabushiki Kaisha | Probe-holding apparatus, sample-obtaining apparatus, sample-processing apparatus, sample-processing method and sample-evaluating method |
| JP2016031928A (en) * | 2014-07-29 | 2016-03-07 | ライカ ミクロジュステーメ ゲーエムベーハー | Manipulation container for cryomicroscopy |
| JP6279692B1 (en) * | 2016-11-07 | 2018-02-14 | 株式会社メルビル | Sample holder |
| JP2018077953A (en) * | 2016-11-07 | 2018-05-17 | 株式会社メルビル | Specimen holder |
| KR20200092751A (en) * | 2019-01-25 | 2020-08-04 | 서울대학교산학협력단 | Cryocooler for measuring multiple physical property at low temperature and method for measuring specific heat using the same |
| CN110475394A (en) * | 2019-08-23 | 2019-11-19 | 杭州源位科技有限公司 | A kind of heating device applied in vacuum equipment |
| CN110475394B (en) * | 2019-08-23 | 2021-11-16 | 杭州源位科技有限公司 | Heating device applied to vacuum equipment |
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