WO2015045477A1 - 試料ホールダ及び荷電粒子装置 - Google Patents
試料ホールダ及び荷電粒子装置 Download PDFInfo
- Publication number
- WO2015045477A1 WO2015045477A1 PCT/JP2014/063148 JP2014063148W WO2015045477A1 WO 2015045477 A1 WO2015045477 A1 WO 2015045477A1 JP 2014063148 W JP2014063148 W JP 2014063148W WO 2015045477 A1 WO2015045477 A1 WO 2015045477A1
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- WIPO (PCT)
- Prior art keywords
- sample
- charged particle
- sample holder
- holder
- hole
- Prior art date
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Classifications
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- 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 objects or the material; Means for adjusting diaphragms or lenses associated with the support
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- 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
-
- 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
- H01J37/18—Vacuum locks ; Means for obtaining or maintaining the desired pressure within the vessel
-
- 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
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
- H01J37/285—Emission microscopes, e.g. field-emission microscopes
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- 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
- H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
- H01J2237/006—Details of gas supplies, e.g. in an ion source, to a beam line, to a specimen or to a workpiece
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
- H01J2237/18—Vacuum control means
- H01J2237/188—Differential pressure
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
- H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
- H01J2237/2002—Controlling environment of sample
- H01J2237/2003—Environmental cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
- H01J2237/26—Electron or ion microscopes
- H01J2237/28—Scanning microscopes
- H01J2237/2802—Transmission microscopes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
- H01J2237/26—Electron or ion microscopes
- H01J2237/28—Scanning microscopes
- H01J2237/2803—Scanning microscopes characterised by the imaging method
- H01J2237/2806—Secondary charged particle
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
- H01M8/04298—Processes for controlling fuel cells or fuel cell systems
- H01M8/04313—Processes for controlling fuel cells or fuel cell systems characterised by the detection or assessment of variables; characterised by the detection or assessment of failure or abnormal function
- H01M8/04664—Failure or abnormal function
- H01M8/04671—Failure or abnormal function of the individual fuel cell
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Definitions
- the present invention relates to an environment-controlled charged particle observation system.
- a sample with a charged particle device such as an electron microscope
- it is used to efficiently detect secondary electrons generated from the sample and efficiently observe the sample while heating the sample while controlling the pressure in the vicinity of the sample. Is. Therefore, in recent analysis of degradation processes of fuel cells and the like, the observation environment with an electron microscope is set to the actual operating environment, and the structure is greatly useful for observation of dynamic changes when the structure is introduced and heated.
- a charged particle device such as an electron microscope
- a transmission electron image or a secondary electron image depending on the type of charged particle detected for observation the vicinity of the sample is observed in a high vacuum state.
- This is fundamental in the world of electron microscopes.
- it has become necessary to observe a sample in an actual operating environment.
- the charged particle device needs to have no adverse effect on the electron gun, and the pressure in the vicinity of the sample is largely limited to maintain the actual operating environment, that is, the atmospheric pressure, and a holder for mounting the sample is required. It was necessary to provide the structure.
- the above-described technique is specialized for observation with a transmission electron image, and there was no example of simultaneous observation with a secondary electron image. This is because only the vicinity of the sample is held at atmospheric pressure by the diaphragm, and secondary electrons are blocked by the diaphragm, so that secondary electrons cannot be detected.
- a secondary electron detection path is provided on the upper part of the sample using a small orifice with a hole diameter, Equipped with a coil heater for heating the sample through the orifice, controlling the pressure in the vicinity of the sample by introducing gas, and enabling the observation of changes in sample dynamics by detecting secondary electrons while heating the sample Invented and provided.
- the object of the present invention is to hold the vicinity of the sample at atmospheric pressure and detect secondary electrons efficiently.
- the pressure in the vicinity of the sample it is possible to control the pressure in the vicinity of the sample, detect secondary electrons efficiently, and observe dynamic changes in the sample.
- it is a sample holder having a hole for differential evacuation so as not to adversely affect an electron gun of a charged particle device such as an electron microscope, and a micro orifice serving as a secondary electron passage A gas introduction nozzle and a micro vacuum gauge for controlling the pressure in the vicinity of the sample, and a heater for heating the sample.
- the vicinity of the sample is maintained in an atmospheric pressure environment by using a micro-orifice on the upper part of the sample and a diaphragm on the lower part of the charged particle passage, and Observation by secondary electrons becomes possible and the problem is solved.
- the micro-orifice for secondary electron passage can also serve as an exhaust hole for gas introduction, so that a passage hole for charged particles generated from an electron gun of a charged particle device such as an electron microscope. If it overlaps, there is a possibility of adverse effects such as electron gun deterioration, which becomes a problem.
- the problem is solved by shifting the position of the charged particle passage hole from the micro orifice provided in the sample holder so that the gas exhausted from the micro orifice is not directly discharged to the electron gun.
- the sample holder according to the present invention can also mount a micro sample produced by a charged particle device, for example, a focused ion beam processing observation device, so that a series of operations from processing to observation can be performed with one holder. By making it possible, the work time from processing to observation can be greatly shortened, resulting in rapid development of research in various fields.
- (B) is the figure which provided the diaphragm in the lower part of the sample in the sample holder front-end
- (A) is a bird's-eye view of a sample holder front-end
- (B) is a bird's-eye view of the tip of the sample holder, and is a schematic diagram for thin film processing of the sample.
- (C) is a schematic diagram at the time of observing with the cross-sectional view of a sample holder front-end
- FIG. 1 shows a basic conceptual diagram of the present invention.
- the charged particle passage hole through which the charged particles A1 pass through the sample holder tip cap 3. 18 is provided to enable observation of charged particles.
- the charged particle device sample chamber 2 is maintained at a high vacuum by a vacuum pump 5 and a valve 6.
- the sample holder 4 includes a gas introduction pipe 26 and a gas exhaust pipe 25 for changing the pressure in the vicinity of the sample 20, and a gas is supplied via a gas pressure control valve 6 for controlling the flow rate at the time of gas introduction.
- the gas is supplied from the storage unit 10, and the gas is exhausted by the vacuum pump 5 and the valve 6 for exhaust.
- the sample holder 4 is connected to a pressure gauge 11 for detecting the pressure in the vicinity of the sample 20.
- the sample holder 4 is provided with a heater 16 for heating the sample 20, and a sample heating temperature control unit 12 for controlling the temperature of the heater 16 is connected to the sample holder 4.
- FIG. 2 shows a conceptual diagram of the detailed structure of the tip of the sample holder 4 described in FIG.
- the sample holder 4 is provided with an O-ring 21 for shielding the atmosphere of only the vicinity of the sample 20 by the sample holder tip cap 3, and provided with a sample holder tip cap fixing screw 22 for fixing the sample holder tip cap 3.
- the sample holder tip cap 3 is provided with charged particle passage holes (micro orifices) 18 through which the charged particles A1 pass in the upper and lower positions of the sample 20, and the charged particle passage holes (micro orifices) 18 above the sample 20 are emitted from the sample 20. It has a hole diameter through which the secondary electrons 15 can pass, and enables image observation on the image display unit 14 via the secondary electron detector 13.
- Fig. 13 shows an observation example at this time.
- the observation image by the secondary electrons 15 and the observation image by the transmission electrons are contrasted, and in the in-situ observation of the structural change of the sample, not only the internal structure of the substance by the transmission image but also the surface observation by the secondary electron image.
- the sample holder 4 is provided with a heater 16 on which the sample 20 can be mounted, and includes a screw for fixing the heater 16.
- the charged particle passage hole / gas exhaust hole 19 at the lower part of the sample 20 has a larger hole diameter than the charged particle passage hole (micro orifice) 18 at the upper part of the sample 20 in order to enhance the exhaust capability.
- the gas exhausted when the gas is introduced is discharged downward from the direction in which the charged particles A1 are generated, so that the charged particle source 28, for example, the electron gun of the electron microscope is not affected.
- FIG. 5 shows a basic conceptual diagram of the present invention.
- the charged particle passage hole (micro orifice) through which the charged particles A1 pass through the sample holder tip cap 3. 18 is provided to enable observation of charged particles.
- the sample holder tip cap 3 is provided with a charged particle passage hole (micro orifice) 18 through which the charged particle A1 passes in the upper part of the sample 20, and the lower part of the sample 20 is separated from the vicinity of the sample 20 and the charged particle apparatus sample chamber 2 by the diaphragm 32. And the charged particles A1 can pass through.
- the charged particle passage hole (micro orifice) 18 provided in the upper part of the sample 20 of the sample holder tip cap 3 is provided at a position not coaxial with the charged particle passage / gas exhaust hole 31 emitted from the charged particle source 28. It is done. For this reason, since the gas exhausted from the charged particle passage hole (micro orifice) 18 located above the sample 20 of the sample holder tip cap 3 is sprayed in a direction different from the generation direction of the charged particle A1, a charged particle source 28 such as an electron microscope is used. The structure does not affect the electron gun.
- the structure attached to the charged particle device sample chamber 2 and the sample holder 4 has the same structure as FIG.
- FIG. 3 shows an embodiment of the present invention, which shows the tip of the sample holder 4 described in FIG. 1 in detail.
- the sample holder 4 is provided with an O-ring 21 for shielding the atmosphere of only the vicinity of the sample 20 by the sample holder tip cap 3, and for fixing the sample holder tip cap for fixing the sample holder tip cap 3.
- a screw 22 is provided.
- the sample holder tip cap 3 is provided with charged particle passage holes (micro orifices) 18 through which the charged particles A1 pass in the upper and lower positions of the sample 20, and the charged particle passage holes (micro orifices) 18 above the sample 20 are emitted from the sample 20. It has a hole diameter through which the secondary electrons 15 can pass, and enables image observation on the image display unit 14 via the secondary electron detector 13.
- a differential exhaust is actively performed in a direction different from the charged particle A1 source direction.
- the gas exhausted when the gas is introduced is discharged below the generation direction of the charged particles A1, and therefore does not affect the charged particle source 28, for example, the electron gun of an electron microscope.
- FIG. 4 is an embodiment of the present invention and is a detailed view of the tip of the sample holder 4.
- the sample holder 4 is provided with a heater 16 for mounting the sample 20 on which the sample 20 is mounted.
- a gas introduction pipe 26 directed to the sample 20 and a gas exhaust pipe 25 are provided, and the structure includes a minute pressure measuring element 24 that detects the pressure in the vicinity of the sample 20.
- FIG. 6 shows an embodiment of the present invention, and shows the tip of the sample holder 4 described in FIG. 5 in detail.
- FIG. 10 shows an embodiment of the present invention, and the positions of the diaphragm 32 and the charged particle passage hole / gas exhaust hole 19 corresponding to the charged particle A1 passage in the upper and lower parts of the sample 20 at the tip of the sample holder 4 described in FIG.
- the sample holder tip cap 3 is arranged as shown in FIG. 10A in order to avoid failure of the charged particle source 28 due to exhaust from the charged particle passage hole / gas exhaust hole 19.
- the sample holder tip cap 3 is arranged as shown in FIG. 10- (b) on the condition of the arrangement relationship of FIG.
- FIG. 11 shows an embodiment of the present invention.
- FIG. 12 shows an embodiment of the present invention.
- the sample holder 4 has a structure in which a cutout is provided in the charged particle beam irradiation direction, for example, the focused ion beam irradiation direction in order to mount the micro sample 20 produced by the micro sampling method of the charged particle device, for example, the focused ion beam processing apparatus.
- the thin film processing of the sample 20 can be performed with a focused ion beam, and the sample 20 processed with a thin film can be observed with a charged particle device different from the above-described device, for example, an electron microscope, after the sample holder tip cap 3 is attached.
- the sample 20 is positioned in the direction rotated by 90 ° and has an observable structure.
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Abstract
Description
2 荷電粒子装置試料室
3 試料ホールダ先端キャップ
4 試料ホールダ
5 真空ポンプ
6 バルブ
7ガス圧コントロールバルブ
8 微小圧力測定素子用接続コネクタ
9 試料加熱用接続コネクタ
10 ガス貯蔵部
11 圧力計
12試料加熱用温度コントロールユニット
13 二次電子検出器
14画像表示部
15 二次電子
16 加熱用ヒータ(試料搭載部)
17 加熱用ヒータ固定ネジ
18 荷電粒子通路孔(微小オリフィス)
19 荷電粒子通路兼ガス排気孔
20 試料
21 Oリング
22 試料ホールダ先端キャップ固定用ネジ
23 ガス排気孔
24 微小圧力測定素子
25 ガス排出用パイプ
26 ガス導入用パイプ
27 試料ホールダ先端キャップ固定用ネジ穴
28 荷電粒子源
29 コンデンサレンズA
30 コンデンサレンズB
31 荷電粒子通路兼ガス排気孔
32 隔膜
33 試料ホールダ先端キャップ保管箱
34 マイクロプローブ
35 荷電粒子B
Claims (9)
- 荷電粒子装置の試料室において、試料近傍を大気圧環境に制御するためのガス導入パイプとガス排出用パイプを有し、荷電粒子通路孔と試料から発せられる二次電子を検出可能な微小オリフィスを試料上部に共有し、試料上部の微小オリフィスよりも穴径を大きくすることでガス導入時の排気を積極的に行える荷電粒子通路孔を有する試料ホールダ。
- 上記請求項1において、
試料を加熱できるヒータを有することにより、試料加熱時おけるガス雰囲気中での試料の状態を観察可能な試料ホールダ。 - 上記請求項1において、
試料下部に位置する荷電粒子通路孔とは別にガス排気孔を1個以上有する試料ホールダ。 - 上記請求項1において、
試料近傍の圧力を確認するための微小圧力測定素子を有する試料ホールダ。 - 荷電粒子装置において、荷電粒子発生源から発する荷電粒子の照射方向と試料中心が同軸上に位置しないよう荷電粒子通路孔が配置された荷電粒子装置と、試料近傍を大気圧環境に制御するためのガス導入パイプとガス排出用パイプを有し、荷電粒子通路孔と試料から発せられる二次電子を検出可能な微小オリフィスを試料上部に共有し、試料下部に荷電粒子が透過可能な隔膜を有する試料ホールダ。
- 上記請求項5において、
試料ホールダ先端部のキャップは、目的に応じ、試料に対し隔膜部分を上下に入れ替えられる構造を有する。 - 上記請求項1において、
試料ホールダ先端部のキャップは、微小オリフィスの穴径が異なるものを複数準備することで、目的に応じて選択が可能な試料ホールダ。 - 上記請求項1または請求項5において、
異なる荷電粒子により加工から観察まで一連の流れを行うことができ、荷電粒子の照射方向に対し任意に試料方向を変更できる構造を有する試料ホールダ。 - 試料を保持する試料保持部と、該試料保持部を内包し、試料近傍の環境を制御し、該試料の上部に所定の大きさの孔を有する環境制御部と、を有する試料ホールダと、
荷電粒子を発生する荷電粒子発生源と、
該荷電粒子発生源から発生した荷電粒子の照射方向を調整するレンズと、
該試料から発生した二次電子を検出する検出器と、
を備え、
前記荷電粒子発生源から照射される荷電粒子の照射方向と前記試料ホールダの前記孔とは軸がずれており、前記荷電粒子発生源から発生した荷電粒子の照射方向を前記レンズによって調整することにより、前記荷電粒子発生源から発生した荷電粒子が前記孔を通って前記試料に照射され、前記試料から発生した二次電子は前記孔を通って前記試料ホールダから放出され、前記検出器によって検出されるように構成されていること、
を特徴とする荷電粒子装置。
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CN201480046171.6A CN105493225B (zh) | 2013-09-30 | 2014-05-19 | 试样支架以及带电粒子装置 |
US14/912,553 US9721752B2 (en) | 2013-09-30 | 2014-05-19 | Sample holder and charged particle device |
DE112014003586.6T DE112014003586B4 (de) | 2013-09-30 | 2014-05-19 | Probenhalter und mit geladenen Teilchen arbeitende Vorrichtung |
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JP2013202952A JP6364167B2 (ja) | 2013-09-30 | 2013-09-30 | 環境制御型荷電粒子観察システム |
JP2013-202952 | 2013-09-30 |
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JP (1) | JP6364167B2 (ja) |
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NL2015258A (en) | 2014-08-03 | 2016-07-07 | Protochips Inc | Method for safe control of gas delivery to an electron microscope sample holder. |
WO2018207309A1 (ja) * | 2017-05-11 | 2018-11-15 | 株式会社日立ハイテクノロジーズ | 試料ホルダ、電子顕微鏡 |
JP7209372B2 (ja) * | 2017-07-06 | 2023-01-20 | プロトチップス,インコーポレイテッド | 独立して圧力および流量を調節する電子顕微鏡試料ホルダーの流体取扱方法 |
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2013
- 2013-09-30 JP JP2013202952A patent/JP6364167B2/ja active Active
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2014
- 2014-05-19 DE DE112014003586.6T patent/DE112014003586B4/de not_active Expired - Fee Related
- 2014-05-19 WO PCT/JP2014/063148 patent/WO2015045477A1/ja active Application Filing
- 2014-05-19 CN CN201480046171.6A patent/CN105493225B/zh active Active
- 2014-05-19 US US14/912,553 patent/US9721752B2/en active Active
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JP2006313716A (ja) * | 2005-05-09 | 2006-11-16 | Lee Bing Huan | 真空または低圧環境下で気体の操作及び観察を可能にする装置 |
JP2011014244A (ja) * | 2009-06-30 | 2011-01-20 | Hitachi High-Technologies Corp | 荷電粒子銃及び荷電粒子線装置 |
WO2012120726A1 (ja) * | 2011-03-04 | 2012-09-13 | 株式会社日立ハイテクノロジーズ | 電子顕微鏡用試料ホルダーおよび試料観察方法 |
JP2013020747A (ja) * | 2011-07-08 | 2013-01-31 | Jeol Ltd | 試料観察方法、試料観察方法に用いる圧力測定用ホルダ及び電子顕微鏡 |
Also Published As
Publication number | Publication date |
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US20160211109A1 (en) | 2016-07-21 |
JP6364167B2 (ja) | 2018-07-25 |
DE112014003586T5 (de) | 2016-06-02 |
JP2015069832A (ja) | 2015-04-13 |
US9721752B2 (en) | 2017-08-01 |
CN105493225B (zh) | 2017-11-17 |
CN105493225A (zh) | 2016-04-13 |
DE112014003586B4 (de) | 2017-04-06 |
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