JPH0765952B2 - Sample holding method and device - Google Patents
Sample holding method and deviceInfo
- Publication number
- JPH0765952B2 JPH0765952B2 JP61038550A JP3855086A JPH0765952B2 JP H0765952 B2 JPH0765952 B2 JP H0765952B2 JP 61038550 A JP61038550 A JP 61038550A JP 3855086 A JP3855086 A JP 3855086A JP H0765952 B2 JPH0765952 B2 JP H0765952B2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- embedding
- holder
- layer
- test 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
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0409—Sample holders or containers
-
- 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
- G01N23/22—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 measuring secondary emission from the material
- G01N23/2204—Specimen supports therefor; Sample conveying means therefore
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/02—Details
- H01J37/20—Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/14—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
- H01J49/142—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers using a solid target which is not previously vapourised
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (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】 〔発明の利用分野〕 本発明は試料保持方法および装置に係り、時にイオンマ
イクロアナライザ（以下,IMAと略す）に好適な試料保持
方法および装置に関する。Description: FIELD OF THE INVENTION The present invention relates to a sample holding method and apparatus, and sometimes to a sample holding method and apparatus suitable for an ion microanalyzer (hereinafter abbreviated as IMA).
IMA装置の試料室に置かれた、絶縁物の粉末状試料（表
面が酸化された粒子状金属も含む）にイオンビームを照
射すると、粉末状試料の帯電現象が現れ、相互の斥力に
より試料が飛散してしまうという問題がある。When an ion beam is irradiated on a powder sample of an insulator (including a particulate metal whose surface is oxidized) placed in the sample chamber of the IMA device, a charging phenomenon of the powder sample appears, and the sample is repulsed by each other. There is a problem of scattering.
そこで、従来より、IMA装置に用いるための、絶縁物の
粉末状試料および微小ペレット状試料の前処理と取りつ
けに関しては、種々の工夫や提案がなされている。Therefore, conventionally, various ideas and proposals have been made for pretreatment and attachment of powdered samples and micropellet-shaped samples of an insulator for use in an IMA device.
このような試料の前処理と取付けに関連した公知文献と
しては、例えば、染野、安盛著“表面分析”（1976年講
談社発行）第241〜242頁がある。Known documents relating to the pretreatment and mounting of such a sample are, for example, "Surface Analysis" by Someno and Yasumori (published by Kodansha in 1976), pages 241-242.
この文献では、板状（ペレット状）や粉末状の微細片試
料の前処理と取り付けに触れられており、特に粉末試料
の前処理と取りつけ方法として、 （１）試料を両面接着テープで止める方法、 （２）試料をプレスしてペレット状にする方法、および （３）試料を溶媒で溶解する方法、 の３方法があげられている。しかし、各々の方法には、
それぞれ次のような問題がある。This document touches on the pretreatment and mounting of plate-shaped (pellet-shaped) or powder-like fine piece samples. Particularly, as a pretreatment and mounting method for powder samples, (1) a method of fixing the sample with double-sided adhesive tape , (2) a method of pressing the sample into pellets, and (3) a method of dissolving the sample in a solvent. But each method has
Each has the following problems.
（１）の方法ではテープに導電性を持たせるためにスプ
レーするが、試料が汚され、正確な情報が得られなくな
る。In the method of (1), the tape is sprayed in order to make it conductive, but the sample becomes dirty and accurate information cannot be obtained.
（２）の方法は、目の細かい金属網に、試料粉末を均一
に薄く振りかけ、プレスしてペレットにするものである
が、微粉末試料の落ちこぼれや、プレスによる試料形状
の変形などがあり、好ましくない。The method (2) is to sprinkle the sample powder evenly and thinly on a fine mesh and press it into pellets. However, there are spillage of the fine powder sample, deformation of the sample shape due to pressing, etc., Not preferable.
（３）の方法では、溶媒により試料が変質したり、汚さ
れたりする恐れがある。In the method (3), the sample may be denatured or contaminated by the solvent.
上記の外にも、粉末状試料などを銀ペーストで固定する
方法も考えられる。しかし、この方法でも、前記（３）
の方法と同様に、銀ペーストの溶媒により試料の変質、
汚染を生じたり、装置が汚されるという問題がある。In addition to the above, a method of fixing a powdery sample or the like with silver paste can be considered. However, even with this method, (3)
Similar to the method of 1, the deterioration of the sample by the solvent of the silver paste,
There is a problem that it causes pollution and the device is contaminated.
本発明の目的は、純度が高く、蒸気圧の低い液体金属や
低融点金属などを用い、その中に被験試料を包埋状態で
保持することにより、被験試料の帯電を防止して試料の
斥力による飛散を無くすると共に、試料の変質、汚染や
装置の汚染などを実質上完全に防止することのできる試
料保持方法および装置を提供することにある。An object of the present invention is to use a liquid metal or a low melting point metal having a high purity and a low vapor pressure, in which the test sample is held in an embedded state to prevent the charge of the test sample and repulsive force of the sample. It is an object of the present invention to provide a sample holding method and device capable of eliminating scattering due to, and substantially completely preventing alteration of sample, contamination and contamination of the device.
本発明の特徴は、試料ホルダの上面に包埋用In層を形成
し、前記層内に被験試料の微細片を包埋した点にある。The feature of the present invention resides in that an embedding In layer is formed on the upper surface of the sample holder, and fine pieces of the test sample are embedded in the layer.
また、本発明の他の特徴は、試料ホルダの上面に包埋用
Inを載せ、これを加熱溶融して液状とし、その表面を平
滑化した後に被験試料の微細片を振りかけ、必要に応じ
て、さらに適当な押え部材で押込包埋して、特にIMA装
置に用いるに適したように試料を保持するようにした点
にある。Another feature of the present invention is that it is embedded on the upper surface of the sample holder.
Place In, heat and melt it to make it liquid, then smooth the surface and sprinkle fine particles of the test sample, and if necessary, embed it with a suitable holding member and use it especially for the IMA device. The sample is held so that it is suitable for.
以下に、図面を参照して本発明の実施例を説明する。 Embodiments of the present invention will be described below with reference to the drawings.
まず、第１実施例を第１図，第２図で説明する。例えば
SUS（ステンレススチール）で作られたホルダ２上に、
純度99.99％で、融点156℃のInの小さい塊1aを、第１図
（Ａ）に示すように置く。First, the first embodiment will be described with reference to FIGS. For example
On the holder 2 made of SUS (stainless steel),
A small lump 1a of In having a purity of 99.99% and a melting point of 156 ° C. is placed as shown in FIG. 1 (A).
ヒータ３でホルダ２並びにInと塊１を加熱すると、Inの
塊１は溶融する。これを平らな金属板などで、第１図
（Ｂ）に示すように、表面が滑らかなIn層１にした後、
必要に応じて試料ホルダ２を空冷する。When the heater 2 heats the holder 2 and In and the lump 1, the In lump 1 is melted. As shown in FIG. 1 (B), this is formed into an In layer 1 having a smooth surface by using a flat metal plate or the like.
The sample holder 2 is air-cooled if necessary.
次に、絶縁物の粉末状試料４をIn層１上に均一に薄く振
りかけ、適当なローラまたは押え板で上から軽く押した
後In層１を固化し、第２図に示すように、試料４をIn層
１内に押込んで包埋する。このように前処理された試料
４を、In層１およびホルダ２と共にIMA装置の試料室に
装填する。Next, the powdered sample 4 of the insulating material is sprinkled evenly and thinly on the In layer 1, lightly pressed from above with an appropriate roller or a pressing plate, and then the In layer 1 is solidified. As shown in FIG. 4 is pushed into the In layer 1 and embedded. The sample 4 thus pretreated is loaded into the sample chamber of the IMA device together with the In layer 1 and the holder 2.
第２図のように、イオンビーム５を試料４に照射して元
素を分析する場合、イオン衝撃誘起導電現象（Ion Bomb
ardment Induced Conductivity）により、イオン照射時
の絶縁物試料は導電性を帯びる。そして、本実施例によ
れば、試料４の表面に生じた電荷６は、In層１へ伝導す
るので、試料４自体が帯電して分析が妨害されることは
なくなる。As shown in FIG. 2, when the sample 4 is irradiated with the ion beam 5 to analyze elements, the ion impact induced conduction phenomenon (Ion Bomb
ardment Induced Conductivity), the insulator sample becomes conductive during ion irradiation. Then, according to the present embodiment, the charge 6 generated on the surface of the sample 4 is conducted to the In layer 1, so that the sample 4 itself is not charged and the analysis is not disturbed.
本実施例により、次のように効果があることがわかっ
た。It was found that the present example has the following effects.
（１）絶縁物の粉末状試料をIn層へ包埋するのに、適当
な押え部材で軽く押すだけで良く、試料形状が変形しな
い。(1) To embed a powder sample of an insulating material in the In layer, it is sufficient to lightly press it with an appropriate pressing member, and the sample shape is not deformed.
（２）Inは純度が高く、蒸気圧が低いので、不純物や放
出ガスが殆んど無く、試料や装置を汚さない。また、試
料の変質も少ない。(2) Since In has a high purity and a low vapor pressure, it has almost no impurities or released gas and does not contaminate the sample or the apparatus. Also, the quality of the sample is small.
なお、以上では、ホルダ２の下部から、ヒータ３で包埋
用Inを加熱、溶融する例について示したが、ホルダ２の
上方から、適宜の手段でInの塊１を直接に加熱溶融する
方法によっても、同様な効果が得られることはいうまで
もない。In the above, an example of heating and melting the embedding In with the heater 3 from the lower portion of the holder 2 has been described, but a method of directly heating and melting the In lump 1 from above the holder 2 by an appropriate means. It goes without saying that the same effect can be obtained by the above.
次に、本発明の第２実施例を第３図にしたがって述べ
る。第３図は微小ペレット状試料4aをIn層１に包埋した
状態を示す平面図である。その他の構成および技法は、
第１図の場合と同じである。Next, a second embodiment of the present invention will be described with reference to FIG. FIG. 3 is a plan view showing a state in which the minute pellet-shaped sample 4a is embedded in the In layer 1. Other configurations and techniques include
This is the same as in the case of FIG.
なお、試料4aの深さ方向の分析をする場合、イオンビー
ムを試料4aより広い四辺形abcdの領域にわたって掃引さ
せるのが望ましい。When analyzing the sample 4a in the depth direction, it is desirable to sweep the ion beam over a region of the quadrangular abcd wider than the sample 4a.
このようにすれば、イオンビームによる試料のスパッタ
が試料表面に対して必ずしも垂直に行なわれないことに
起因する試料端面エッジの影響がなくなり、簡単な手法
で精度良い深さ方向の分析ができるようになる。By doing so, the influence of the sample end face edge due to the fact that the sample is not sputtered by the ion beam is not always perpendicular to the sample surface, and it is possible to perform accurate depth direction analysis with a simple method. become.
本発明の第３実施例を第４図（Ａ），（Ｂ）にしたがっ
て述べる。本実施例は、ホルダ2aに包埋用Inを貯溜する
ためのウエル７を設けたものである。その他の構成およ
び技法は第１図の場合と同じである。A third embodiment of the present invention will be described with reference to FIGS. 4 (A) and 4 (B). In this embodiment, the holder 2a is provided with the well 7 for storing the embedding In. Other configurations and techniques are the same as in the case of FIG.
前述の実施例と同様に、包埋用Inをウエル７内に置いて
液状とし、その上に粉末試料を載置し、平坦な押え部材
で軽く押して試料４を包埋する。Similarly to the above-described embodiment, the embedding In is placed in the well 7 to be in a liquid state, the powder sample is placed thereon, and the sample 4 is embedded by lightly pressing with a flat holding member.
この場合、試料４がペレット状のように、平坦面を有す
るものであれば、第４図（Ｂ）のようにこの平坦面をウ
エル７の上面に一致させることが容易である。In this case, if the sample 4 has a flat surface like a pellet, it is easy to make the flat surface coincide with the upper surface of the well 7 as shown in FIG. 4 (B).
このようにすれば、試料をホルダと共にIMA装置に装填
した場合に、試料の縦方向（イオンビーム軸方向）の位
置が決まり、イオンビーム照射位置が決まることになる
ので、ホルダ２を移動したり、あるいは試料を交換した
りするごとにイオンビーム調整をする手間が省けるとい
う利点を生ずる。By doing so, when the sample is loaded into the IMA device together with the holder, the position of the sample in the vertical direction (ion beam axis direction) is determined, and the ion beam irradiation position is determined. Alternatively, there is an advantage that the labor of adjusting the ion beam every time the sample is exchanged can be saved.
本発明の第４実施例を、第５図にしたがって述べる。第
５図は、ホルダ２に複数個のウエル７を設けた場合の断
面図である。その他の構成および技法は第１図の場合と
同じである。A fourth embodiment of the present invention will be described with reference to FIG. FIG. 5 is a cross-sectional view when the holder 2 is provided with a plurality of wells 7. Other configurations and techniques are the same as in the case of FIG.
本実施例によれば、第３実施例による前述の効果に加え
てさらに、一度に多種類の試料を前処理し、取りつける
ことができるという利点がある。According to the present embodiment, in addition to the above-described effects of the third embodiment, there is an advantage that many kinds of samples can be pretreated and attached at one time.
本発明により、次のような効果があることがわかった。 The present invention has been found to have the following effects.
（１）In層を試料包埋用として用いるので、スプレーを
行なわなくてすみ、スプレーによる試料の汚れや変質が
無い。(1) Since the In layer is used for embedding the sample, it is not necessary to perform spraying, and there is no contamination or deterioration of the sample due to spraying.
（２）試料を液体状のIn層に包埋するのに、軽く押しつ
けるだけで良く、試料形状の変形がない。(2) To embed the sample in the liquid In layer, it is only necessary to press lightly, and the sample shape is not deformed.
（３）試料を溶媒で溶解しないので、試料が変質、汚染
しない。(3) Since the sample is not dissolved in the solvent, the sample is not altered or contaminated.
（４）In層は純度が高く、蒸気圧が低いので、不純物や
放出ガスによる試料や装置の汚れがない。(4) Since the In layer has a high purity and a low vapor pressure, the sample and the device are not contaminated by impurities and released gas.
第１図は本発明の試料装置を製造する工程を説明するた
めの正面図、第２図は本発明の試料装置の一実施例にイ
オンビームを照射した状態を示す断面図、第３図はIn層
に包埋された微小ペレット状試料に本発明を適用した他
の実施例の上面図、第４図および第５図はそれぞれ、本
発明のさらに他の実施例の断面図である。 １……包埋用Inの金属層、２……ホルダ、３……ヒー
タ、４……絶縁物の粉末状試料および微小ペレット状試
料、５……イオンビーム、６……帯電現象により生じる
電荷、７……ウエルFIG. 1 is a front view for explaining a process for manufacturing a sample device of the present invention, FIG. 2 is a cross-sectional view showing a state in which an ion beam is irradiated to one embodiment of the sample device of the present invention, and FIG. FIG. 4 is a top view of another embodiment in which the present invention is applied to a micropellet-shaped sample embedded in an In layer, and FIGS. 4 and 5 are cross-sectional views of still another embodiment of the present invention. 1 ... Embedding In metal layer, 2 ... Holder, 3 ... Heater, 4 ... Insulator powder sample and fine pellet sample, 5 ... Ion beam, 6 ... Charge generated by charging phenomenon , 7 ... well
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｈ０１Ｊ 37/20 Ａ ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification code Office reference number FI technical display location H01J 37/20 A
Claims (5)
くともその一部が露出する状態で前記包埋用In層内に包
埋されるように構成されたことを特徴とする試料保持装
置。1. A test sample comprising a holder and an embedding In layer held by the holder, wherein the test sample that can be charged by irradiation with a charged particle beam is at least partially exposed. A sample holding device configured to be embedded in an In layer.
形成され、前記ウエルに包埋用In層が設けられたことを
特徴とする前記特許請求の範囲第１項記載の試料保持装
置。2. The sample holding device according to claim 1, wherein at least one well is formed in the holder, and an In layer for embedding is provided in the well.
規定される平面と同一平面内にあることを特徴とする前
記特許請求の範囲第２項記載の試料保持装置。3. The sample holding device according to claim 2, wherein the surface of the test sample is in the same plane as the plane defined by the upper surface of the well.
と、 溶融された包埋用Inの表面に、荷電粒子線の照射によっ
て帯電し得る被験試料を包埋させる工程とよりなること
を特徴とする試料保持装置。4. A step of heating and melting the embedding In on a holder, and a step of embedding a test sample that can be charged by irradiation of a charged particle beam on the surface of the molten Embedding In. A sample holding device.
Inの表面に被験試料を振りかけた後に、当該被験試料を
包埋用Inに向って押しつける工程よりなることを特徴と
する前記特許請求の範囲第４項記載の試料保持方法。5. The step of embedding the test sample is for embedding
The method for holding a sample according to claim 4, comprising a step of sprinkling the test sample on the surface of In and then pressing the test sample toward In for embedding.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61038550A JPH0765952B2 (en) | 1986-02-24 | 1986-02-24 | Sample holding method and device |
| PCT/JP1987/000116 WO1990008312A1 (en) | 1986-02-24 | 1987-02-23 | Holding method for specimen of electric insulation |
| US07/123,114 US4833331A (en) | 1986-02-24 | 1987-02-23 | Method of holding an electrically insulating sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61038550A JPH0765952B2 (en) | 1986-02-24 | 1986-02-24 | Sample holding method and device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62195548A JPS62195548A (en) | 1987-08-28 |
| JPH0765952B2 true JPH0765952B2 (en) | 1995-07-19 |
Family
ID=12528398
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61038550A Expired - Lifetime JPH0765952B2 (en) | 1986-02-24 | 1986-02-24 | Sample holding method and device |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JPH0765952B2 (en) |
| WO (1) | WO1990008312A1 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101047215B1 (en) | 2009-07-30 | 2011-07-06 | 정태승 | Manufacturing method of conductive cold mounting specimen for scanning electron microscope (SEM) |
| JP5687299B2 (en) * | 2012-03-23 | 2015-03-18 | 株式会社住化分析センター | Observation sample, preparation method of observation sample, and observation method |
| JP6392622B2 (en) * | 2014-10-03 | 2018-09-19 | 株式会社トクヤマ | Sample preparation method for observing particles with an electron microscope, and method for observing particles with an electron microscope |
| JP6519459B2 (en) * | 2015-12-04 | 2019-05-29 | 住友金属鉱山株式会社 | Ore observation sample for mineral particle analyzer and method for producing the same |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5063077U (en) * | 1973-10-11 | 1975-06-09 | ||
| JPS57196354U (en) * | 1981-06-09 | 1982-12-13 | ||
| JPS5889847U (en) * | 1981-12-11 | 1983-06-17 | 三菱重工業株式会社 | Sample for film observation |
-
1986
- 1986-02-24 JP JP61038550A patent/JPH0765952B2/en not_active Expired - Lifetime
-
1987
- 1987-02-23 WO PCT/JP1987/000116 patent/WO1990008312A1/en not_active Ceased
Also Published As
| Publication number | Publication date |
|---|---|
| WO1990008312A1 (en) | 1990-07-26 |
| JPS62195548A (en) | 1987-08-28 |
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