JP5832792B2 - 極低温でのビーム誘起堆積 - Google Patents
極低温でのビーム誘起堆積 Download PDFInfo
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- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 3
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- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/46—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for heating the substrate
- C23C16/463—Cooling of the substrate
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/48—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation
- C23C16/486—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation using ion beam radiation
Description
− 前記基板の表面に向かって前駆体気体を導く工程、
− 前記前駆体気体が存在する中で前記基板表面に粒子ビームを照射する工程であって、前記前駆体気体は、前記粒子ビームと反応することで、前記基板表面上に材料を堆積させる、工程、
− 前記基板を-50℃よりも低温である所望の極低温にまで冷却する工程、
を有し、
前記前駆体気体は、前記所望の極低温よりも低い融点を有する化合物からなる群から選ばれることを特徴とする。
− イオンビームを用いて前記基板から試料を解放する工程、
− 前記試料と接触するようにマイクロプローブを動かす工程、
− 前記前駆体気体を前記試料へ向かうように導き、かつ前記前駆体気体が存在する中で前記試料に照射することで、前記試料と前記マイクロプローブとを結合させる工程、
− 前記の基板が結合したマイクロプローブを、前記基板から遠ざかるように持ち上げる工程、
− 前記試料が試料ホルダ上の所望の位置で接触するように前記マイクロプローブを動かす工程、
− 前記前駆体気体を前記試料へ向かうように導き、かつ前記前駆体気体が存在する中で前記試料に照射することで、前記試料と前記マイクロプローブとを付着させる工程、
− 前記マイクロプローブを前記試料から分離する工程、並びに、
− 前記工程が実行されている間、前記試料を-130℃に維持する工程、
を有して良い。
41 堆積物
42 堆積物
43 堆積物
44 堆積物
45 堆積物
46 堆積物
47 堆積物
48 堆積物
49 堆積物
100 工程
102 工程
104 工程
106 工程
108 工程
210 デュアルビームSEM/FIBシステム
211 集束イオンビーム(FIB)システム
212 上部首部分
214 イオン源
215 引き出し電極
216 集束鏡筒
217 集束素子
218 集束イオンビーム
219 システム制御装置
220 偏向素子
222 基板
224 TEM用試料ホルダ
225 X-Y-Zステージ
226 試料チャンバ
230 排気制御装置
232 真空制御装置
234 高電圧電源
236 偏向制御装置及び増幅器
238 パターン生成装置
240 検出器
241 電子ビーム鏡筒
243 電子ビーム
244 モニタ
245 走査型電子顕微鏡の電源及び制御装置
246 気体注入システム(GIS)
247 マイクロマニピュレータ
248 精密電気モータ
249 マイクロマニピュレータの真空チャンバ内部に位置する部分
250 細いプローブ
252 電子源
256 電子光学レンズ
258 電子光学レンズ
260 偏向コイル
261 ドア
262 STEM検出器
268 イオンポンプ
270 針状体
271 基板への前駆体材料の供給を制御する手段
Claims (21)
- 極低温で基板上へ材料を堆積する方法であって、
当該方法は:
前記基板の表面に向かって前駆体気体を導く工程;
前記前駆体気体が存在する中で前記基板の表面に粒子ビームを照射する工程であって、前記前駆体気体は、前記粒子ビームと反応することで、前記基板の表面上に材料を堆積させる、工程;
前記基板を-50℃よりも低温である所定の極低温にまで冷却する工程;
を有し、
前記前駆体気体は、前記所定の極低温よりも低い融点を有する化合物からなる群から選ばれ、かつ、
前記基板は氷を含む生体試料を有する、
ことを特徴とする方法。 - 前記前駆体気体が、前記所定の極低温よりも低い融点を有する化合物の群から選ばれる、請求項1に記載の方法。
- 前記前駆体気体の融点は、前記所定の極低温よりも少なくとも10℃低い、請求項1又は2に記載の方法。
- 前記前駆体気体が、前記粒子ビームが存在する中で分解して、堆積物及び気体状副生成物を生成する分子を有する化合物を有する、請求項1乃至3のいずれか1項に記載の方法。
- 前記気体状副生成物が、前記試料の温度よりも低い融点を有する、請求項1乃至4のいずれか1項に記載の方法。
- 前記前駆体気体が、前記所定の極低温で1.0未満の付着係数を有する化合物の群から選ばれる、請求項1乃至5のいずれか1項に記載の方法。
- 前記前駆体気体が、前記所定の極低温にて0.5以上で0.8以下の付着係数を有する化合物の群から選ばれる、請求項1乃至6のいずれか1項に記載の方法。
- 前記前駆体気体は、前記所定の極低温にて、前記基板の表面に吸着する前駆体分子と前記基板の表面から脱離する前駆体気体分子との間で平衡に到達する化合物の群から選ばれる、請求項1乃至7のいずれか1項に記載の方法。
- 気体分子のうちの1未満乃至2分子層が前記基板の表面上に形成されるときに前記平衡が実現される、請求項8に記載の方法。
- 前記前駆体気体がプロパンを有し、かつ
前記所定の極低温が-130℃から-180℃である、
請求項1に記載の方法。 - 前記前駆体気体がヘキサンを有し、かつ
前記所定の極低温が-50℃から-85℃である、
請求項1に記載の方法。 - 前記前駆体気体が、アルカン、アルケン、又はアルキンを有する、請求項1に記載の方法。
- 前記前駆体気体が、エチレン又はアセチレンを有する、請求項12に記載の方法。
- 前記前駆体気体が、ハロアルカン、フルオロカーボン、又はハロホルムを有する、請求項1に記載の方法。
- 前記前駆体気体が、ジフルオロメタン、カーボンテトラフルオライド、又はカーボントリフルオロライドを有する、請求項14に記載の方法。
- 前記前駆体気体が存在する中で前記基板の表面に粒子ビームを照射することで、前記粒子ビームが前記前駆体気体と反応することで、前記基板の表面上に材料を堆積する工程が、前記前駆体気体が存在する中で前記基板の表面に粒子ビームを照射することで、前記前駆体気体が前記粒子ビームと反応することで、前記試料の一部と他の表面とを結合する工程を有する、請求項1乃至15のいずれか1項に記載の方法。
- 材料が、前記基板の表面上の1μm2 の面積にわたって、少なくとも0.6nm/secの速度で前記基板の表面に堆積される、請求項1乃至16のいずれか1項に記載の方法。
- 前記の堆積された材料が炭素を有する、請求項1乃至17のいずれか1項に記載の方法。
- 前記粒子ビームが、少なくとも5keVのビームエネルギーを有する電子ビームを有する、請求項1乃至18のいずれか1項に記載の方法。
- 前記試料は冷凍保存された生体試料で、前記所定の極低温は130℃よりも低い場合において、
イオンビームを用いて前記基板から試料を解放する工程、
前記試料と接触するようにマイクロプローブを動かす工程、
前記前駆体気体を前記試料へ向かうように導き、かつ前記前駆体気体が存在する中で前記試料に照射することで、前記試料と前記マイクロプローブとを結合させる工程、
前記の基板が結合したマイクロプローブを、前記基板から遠ざかるように持ち上げる工程、
前記試料が試料ホルダ上の所望の位置で接触するように前記マイクロプローブを動かす工程、
前記試料と前記マイクロプローブとを結合させる工程、
前記マイクロプローブを前記試料から分離する工程、並びに、
前記工程が実行されている間、前記試料を-130℃に維持する工程、
を有する、請求項1乃至10のいずれか1項に記載の方法。 - 前記試料は、前記前駆体気体を前記試料へ向かうように導き、かつ前記前駆体気体が存在する中で前記試料に照射することで、前記マイクロプローブに結合される、請求項20に記載の方法。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP10167905.8 | 2010-06-30 | ||
EP10167905A EP2402475A1 (en) | 2010-06-30 | 2010-06-30 | Beam-induced deposition at cryogenic temperatures |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2012012704A JP2012012704A (ja) | 2012-01-19 |
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EP2402475A1 (en) | 2010-06-30 | 2012-01-04 | Fei Company | Beam-induced deposition at cryogenic temperatures |
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US9090973B2 (en) | 2011-01-31 | 2015-07-28 | Fei Company | Beam-induced deposition of low-resistivity material |
EP2694941A4 (en) | 2011-04-04 | 2015-03-04 | Omniprobe Inc | METHOD FOR EXTRACTING FROZEN SPECIMENS AND MANUFACTURE OF SPECIMEN ASSEMBLIES |
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US8859963B2 (en) * | 2011-06-03 | 2014-10-14 | Fei Company | Methods for preparing thin samples for TEM imaging |
US8912490B2 (en) * | 2011-06-03 | 2014-12-16 | Fei Company | Method for preparing samples for imaging |
US8884248B2 (en) * | 2012-02-13 | 2014-11-11 | Fei Company | Forming a vitrified sample for electron microscopy |
CN104303257B (zh) * | 2012-05-21 | 2018-03-30 | Fei 公司 | 用于tem观察的薄片的制备 |
EP2685233A1 (en) * | 2012-07-13 | 2014-01-15 | Fei Company | Forming an electron microscope sample from high-pressure frozen material |
US10023955B2 (en) | 2012-08-31 | 2018-07-17 | Fei Company | Seed layer laser-induced deposition |
EP2706342B1 (en) * | 2012-09-11 | 2015-07-08 | Fei Company | Cooperating capillary and cap for use in a high-pressure freezer |
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US9123506B2 (en) | 2013-06-10 | 2015-09-01 | Fei Company | Electron beam-induced etching |
EP2813835B1 (en) * | 2013-06-14 | 2016-09-07 | Fei Company | Method of welding a frozen aqueous sample to a microprobe |
US9799490B2 (en) * | 2015-03-31 | 2017-10-24 | Fei Company | Charged particle beam processing using process gas and cooled surface |
US10103008B2 (en) | 2016-01-12 | 2018-10-16 | Fei Company | Charged particle beam-induced etching |
US10832895B2 (en) | 2016-05-19 | 2020-11-10 | Plasmotica, LLC | Stand alone microfluidic analytical chip device |
JP7056859B2 (ja) | 2017-07-07 | 2022-04-20 | ウイスコンシン アラムナイ リサーチ ファウンデーシヨン | 低温電子顕微鏡の気相試料調製 |
ES2738911A1 (es) * | 2018-07-25 | 2020-01-27 | Consejo Superior Investigacion | Procedimiento para depositar elementos sobre un sustrato de interes y dispositivo |
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US11728146B2 (en) | 2021-01-13 | 2023-08-15 | Wisconsin Alumni Research Foundation | Retractable ion guide, grid holder, and technology for removal of cryogenic sample from vacuum |
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US8617668B2 (en) | 2009-09-23 | 2013-12-31 | Fei Company | Method of using nitrogen based compounds to reduce contamination in beam-induced thin film deposition |
JP5650234B2 (ja) | 2009-11-16 | 2015-01-07 | エフ・イ−・アイ・カンパニー | ビーム処理システムに対するガス送達 |
EP2402475A1 (en) | 2010-06-30 | 2012-01-04 | Fei Company | Beam-induced deposition at cryogenic temperatures |
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EP2402477A1 (en) | 2012-01-04 |
JP2012012704A (ja) | 2012-01-19 |
US20120003394A1 (en) | 2012-01-05 |
CN102312224B (zh) | 2014-10-22 |
CN102312224A (zh) | 2012-01-11 |
US8796646B2 (en) | 2014-08-05 |
EP2402477B1 (en) | 2014-08-13 |
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