JP6110519B2 - 顕微鏡サンプルからサンプル表面層を改変する方法 - Google Patents
顕微鏡サンプルからサンプル表面層を改変する方法 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims description 35
- 239000002344 surface layer Substances 0.000 title claims description 13
- 239000007788 liquid Substances 0.000 claims description 120
- 230000004048 modification Effects 0.000 claims description 19
- 238000012986 modification Methods 0.000 claims description 19
- 238000002347 injection Methods 0.000 claims description 15
- 239000007924 injection Substances 0.000 claims description 15
- 239000012620 biological material Substances 0.000 claims description 12
- 238000007747 plating Methods 0.000 claims description 11
- 238000010894 electron beam technology Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 238000005530 etching Methods 0.000 claims description 8
- 238000010884 ion-beam technique Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 238000009713 electroplating Methods 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 5
- 102000004190 Enzymes Human genes 0.000 claims description 3
- 108090000790 Enzymes Proteins 0.000 claims description 3
- 125000000524 functional group Chemical group 0.000 claims description 3
- 239000002086 nanomaterial Substances 0.000 claims description 3
- 239000002070 nanowire Substances 0.000 claims description 3
- 230000009257 reactivity Effects 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 claims description 3
- 238000007772 electroless plating Methods 0.000 claims description 2
- 230000003746 surface roughness Effects 0.000 claims description 2
- 238000003780 insertion Methods 0.000 claims 2
- 230000037431 insertion Effects 0.000 claims 2
- 239000000523 sample Substances 0.000 description 75
- 230000008020 evaporation Effects 0.000 description 17
- 238000001704 evaporation Methods 0.000 description 17
- 150000002500 ions Chemical class 0.000 description 8
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 3
- 241000446313 Lamella Species 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 238000004070 electrodeposition Methods 0.000 description 3
- 229910052733 gallium Inorganic materials 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000003550 marker Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000012472 biological sample Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
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- 238000011065 in-situ storage Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
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- 238000007787 electrohydrodynamic spraying Methods 0.000 description 1
- 238000000866 electrolytic etching Methods 0.000 description 1
- 238000011066 ex-situ storage Methods 0.000 description 1
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- 102000034287 fluorescent proteins Human genes 0.000 description 1
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- 230000008014 freezing Effects 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
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- 238000007689 inspection Methods 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
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- 238000002844 melting Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 229910000489 osmium tetroxide Inorganic materials 0.000 description 1
- 239000012285 osmium tetroxide Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
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- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910001927 ruthenium tetroxide Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/60—Electroplating characterised by the structure or texture of the layers
- C25D5/605—Surface topography of the layers, e.g. rough, dendritic or nodular layers
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C3/00—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material
- B05C3/02—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material
- B05C3/09—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material for treating separate articles
- B05C3/10—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material for treating separate articles the articles being moved through the liquid or other fluent material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0493—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases using vacuum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/02—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain a matt or rough surface
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- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/04—Removal of gases or vapours ; Gas or pressure control
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/12—Semiconductors
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- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
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- H01J37/30—Electron-beam or ion-beam tubes for localised treatment of objects
- H01J37/317—Electron-beam or ion-beam tubes for localised treatment of objects for changing properties of the objects or for applying thin layers thereon, e.g. for ion implantation
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30604—Chemical etching
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/32051—Deposition of metallic or metal-silicide layers
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- G—PHYSICS
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- G—PHYSICS
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- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
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- H—ELECTRICITY
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- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
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- H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
- H01J2237/206—Modifying objects while observing
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- H01J2237/317—Processing objects on a microscale
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Description
・マニピュレータに取付けられた顕微鏡サンプルを提供するステップと、
・第1の温度における第1の液体を提供するステップと、
・前記第1の液体内にサンプルを浸漬し、それによりサンプル表面改変を生じるステップと、
・前記第1の液体からサンプルを除去するステップと、
・第2の温度における第2の液体を提供するステップと、
・前記第2の液体内にサンプルを浸漬するステップと、
・前記第2の液体からサンプルを除去するステップと、
を有する。
・例えばステージの凹部における小体積の(温度制御された)液体を提供し、使用後、液体の温度、及び従って蒸発速度を下げるステップ、
・使用しないときは、真空から密閉される、小体積の液体を提供するステップ、
・ステージ内の小さいチャネルを介して液体を提供するステップ、
・表面上に液滴をエレクトロスプレーするステップ、
・(チャネル内に小蒸気バブルを形成するステップ、又はピエゾ結晶を使用してチャネルの変形をして、液滴を絞り出すステップを包含する)インクジェットテクニックを使用して液滴を適用するステップ、等。
これらの実施形態において、第1の液体は、エッチング液(etchant)もしくはメッキ液である。エッチ除去は、エッチング液化学物質(chemical)、沈没時間(浸漬時間)、液体濃度、及び液体温度(及び電気化学エッチングの場合は電流)のパラメータを制御することにより制御可能である。
同様に、メッキ厚さは、メッキ化学物質、沈没時間(浸漬時間)、液体濃度、及び液体温度(及び電気メッキの場合は電流)のパラメータを制御することにより制御可能である。
これにより、エッチ除去もしくはメッキ厚さについて微細な制御が達成可能であって、当該方法を、厚さ10nm未満を有する表面層を除去もしくは追加するのによく適したものにする。
電気メッキ及び電解エッチングの場合、液体に対して、サンプルにバイアスをかける。当該液体は、例えばそれが置かれている表面から、その電位を導出する。
第2の液体は、前記活性サイトに材料を提供することを有する。
表1: 異なるサンプル材料の場合のエッチング液。
使用に依存して、第1の液体及び第2の液体は、同一の(制御された)温度もしくは異なる(制御された)温度を有し得る。
同様に、メッキ用(化学もしくは電気化学)化学物質及び溶媒が、当業者に知られる。
図1は、本発明によるSEMを概略的に表す。
当該方法は、(ガリウム)FIBでラメラを加工した後、そのラメラをエッチングするのに特に有用であり、ガリウム注入が行われた、もしくは結晶格子が乱れている(disturbed)表面層を除去する。
[1] SJ Randolph et al., ‘Capsule−free fluid delivery and beam−induced electrodeposition in a scanning electron microscope’, RSC Adv., 2013, p 20016−23.
[2] 米国特許第5,270,552号,Hitachi.
[3] J. Mayer et al., ‘TEM Sample Preparation and FIB−Induced Damage’, MRS BULLETIN, Vol. 32 (May 2007), p. 400−407.
[4] http://www.nanotechnik.com/mis−em.html
[5] 米国特許第8,919,902号,Ricoh Company Ltd.
[6] 米国特許第8,919,938号,Hewlett Packard Development Company L.P.
110A 第1の液体注入システム
110B 第2の液体注入システム
112 サンプルステージ
116 マニピュレータ
118 先端
120 サンプル
122A 第1の液体
122B 第2の液体
124 ヒータ/クーラー
Claims (17)
- 粒子光学装置内のサンプルからサンプル表面層を改変する方法であって、当該方法は、真空内で実施され、且つ
1)マニピュレータに取付けられた顕微鏡サンプルを提供するステップと、
2)第1の温度における第1の液体を提供するステップと、
3)前記第1の液体内にステップ1)で提供された前記サンプルを浸漬し、それによりサンプル表面改変を生じるステップと、
4)前記第1の液体から前記サンプルを除去するステップと、
5)第2の温度における第2の液体を提供するステップと、
6)前記第2の液体内にステップ4)で得られた前記サンプルを浸漬するステップと、
7)前記第2の液体から前記サンプルを除去するステップと、
を有する、方法。 - 前記サンプル表面改変は、サンプル表面粗さ、親水性、表面電荷、表面エネルギー、生体適合性、もしくは反応性の改変、官能基の追加、生体物質の追加、サンプル表面をメッキすること又はサンプル表面層の除去である、請求項1に記載の方法。
- ビーム誘起堆積を使用して溶接部を形成することにより、前記顕微鏡サンプルはマニピュレータに取付けられ、前記ビーム誘起堆積は、レーザービーム、電子ビームもしくはイオンビームにより誘起される、請求項1乃至2のいずれか一項に記載の方法。
- 前記サンプルは、いずれの方向において10μm未満の寸法を有し、且つ前記第1の液体及び前記第2の液体は、体積1ピコリットル未満を有する液滴としてデポジットされる、請求項1乃至3のいずれか一項に記載の方法。
- 前記サンプルは、半導体サンプルである、請求項1乃至4のいずれか一項に記載の方法。
- マニピュレータに取付けられた顕微鏡サンプルを提供するステップ1)は、以下の:
・ワークピースを提供するステップと、
・前記サンプルを前記マニピュレータに取付けるステップと、
・集束イオンビームを使用して、前記ワークピースから前記サンプルを切除するステップと、
を有する、請求項1乃至5のいずれか一項に記載の方法。 - 前記サンプル表面改変は、エッチング、電気化学エッチング、無電解メッキもしくは電気メッキにより引き起こされ、前記電気メッキは、非仮想カソードを使用する、請求項1乃至6のいずれか一項に記載の方法。
- 除去されたもしくは追加されたサンプル表面層の厚さは10nm未満である、請求項7に記載の方法。
- 前記第2の液体は、リンス用液体であり、及び前記第2の液体内に前記サンプルを浸漬するステップ6)は、前記サンプルをリンスする、請求項1乃至8のいずれか一項に記載の方法。
- 前記サンプルは繰り返しリンスされる、請求項9に記載の方法。
- リンスの各ステップは、新しいリンス用液体において行われる、請求項10に記載の方法。
- 前記第1の液体は、生体物質を含有し、前記サンプル表面改変は、前記サンプルの表面に生体物質を提供するステップを有し、及び前記第2の液体は、前記サンプルの表面に前記生体物質を結合するステップを生じる、請求項1乃至6のいずれか一項に記載の方法。
- 前記サンプル表面改変は、酵素、ナノワイヤもしくはその他のナノ構造のデポジットにより生じた活性サイトを形成することにより、前記サンプルを官能化するステップを有し、及び
前記第2の液体は、前記活性サイトに材料を提供することを有する、請求項1乃至6のいずれか一項に記載の方法。 - 2つの液体は1つの表面上に提供され、前記マニピュレータは前記表面に対して移動可能である、請求項1乃至13のいずれか一項に記載の方法。
- 前記サンプル表面層の改変の際及び/もしくは後、前記サンプル表面は荷電粒子のビームを使用して検査される、請求項1乃至14のいずれか一項に記載の方法。
- 第1の液体挿入システム及び第2の液体挿入システムを使用して、前記2つの液体が適用される、請求項1乃至15のいずれか一項に記載の方法。
- 前記第1の液体注入システム及び前記第2の液体注入システムは、1つの構造的液体注入システムに統合される、請求項16に記載の方法。
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