WO2005040778A1 - 電子分光分析方法及び分析装置 - Google Patents
電子分光分析方法及び分析装置 Download PDFInfo
- Publication number
- WO2005040778A1 WO2005040778A1 PCT/JP2004/015930 JP2004015930W WO2005040778A1 WO 2005040778 A1 WO2005040778 A1 WO 2005040778A1 JP 2004015930 W JP2004015930 W JP 2004015930W WO 2005040778 A1 WO2005040778 A1 WO 2005040778A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- sample
- analyzed
- fullerene
- energy
- irradiated
- Prior art date
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Classifications
-
- 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
- G01N23/225—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 using electron or ion
- G01N23/2251—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 using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
- G01N23/2252—Measuring emitted X-rays, e.g. electron probe microanalysis [EPMA]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
- G01N23/2202—Preparing specimens therefor
Definitions
- the present invention provides a method of irradiating a sample with high energy particles in a vacuum atmosphere, detecting the number and kinetic energy of electrons emitted from the sample by the photoelectric effect,
- the present invention relates to an electron spectroscopic analysis method and an analyzer for performing desired analysis on a surface or a depth direction thereof.
- Electron spectroscopy analyzers are used for, for example, functional property correlation analysis, quality control, and process analysis for improving the product performance of various samples produced in the development process and manufacturing process of various materials. ing.
- X-ray photoelectron spectroscopy analyzers that use characteristic X-rays for high-energy particles are widely used to analyze contamination, composition ratios, and the like at a depth of about 5 nm in the sample surface layer. .
- an ultraviolet photoelectron spectroscopy analyzer using ultraviolet rays as high energy particles is widely used for analyzing a change in work function, a chemical state of a composition, and the like at a depth of about 5 nm in a sample surface layer.
- the high-energy particle source electrons, gamma rays, synchrotron radiation, laser light, ions, positrons, and the like may be used.
- Photoelectron spectroscopy is an analysis method in which the surface of a sample is irradiated with high energy and the number of electrons emitted by the photoelectric effect and the kinetic energy are measured to analyze the elements in the sample. is there. Since such photoelectron spectroscopy is excellent in analyzing the chemical state of a material without merely examining the elemental composition of the sample surface, the oxidation state of an organic thin film sample and the acidity of silicon on the surface of a semiconductor device are excellent. It is used for analyzing the state of the dani. At this time, since the sample surface is inevitably covered with contaminants such as oils and fats, water, etc., it is common to perform a pre-cleaning treatment to remove these contaminants using a sputtering ion source. There are many.
- Patent Document 1 discloses an analysis method in which a sample is cut with a known tool such as a diamond cutter to produce a sample indicating information in a depth direction.
- Non-Patent Document 2 describes that a method of exposing the inside of a sample to the surface by cleaving or scribing the sample and analyzing the inside of the sample by a surface analysis method is widely known. ing.
- Patent Document 3 discloses that etching of a sample surface using cluster ions composed of 100 or more atoms or molecules removes contamination with little damage.
- Non-Patent Document 4 describes that the sample surface is cleaned by hitting fine powder of dry ice on the sample surface.
- Patent Document 1 JP-A-2002-365183
- Non-Patent Document 2 U.S. Standard International Standard ASTM E1078-97, Article 11, 3, 4, 1996 Patent Document 3: JP-A-8-122283
- Non-Patent Document 4 Vac.Sci. Technol., B9, p. 1970, 1991
- Non-Patent Document 4 since neutral particles are used instead of ions, it is difficult to quantitatively evaluate the amount of etching with which the operation is not reproducible.
- this non-patent document 4 in order to apply this non-patent document 4 to the surface analysis of a sample, it is necessary to use an analyzer in an ultra-high vacuum, and as with the cluster ions described above, large-scale equipment is required. And the cost will increase.
- the present invention provides an electron spectroscopic analysis method and an analyzer capable of etching a sample surface uniformly with good reproducibility, and requiring no large-scale equipment and capable of etching at low cost.
- the purpose is to provide.
- the invention according to claim 1 irradiates a sample with high energy particles in a vacuum atmosphere, and the sample is released from the sample by the photoelectric effect.
- the method is characterized in that the surface of the sample to be analyzed is irradiated by ion irradiation to remove contaminants present on the surface of the sample to be analyzed.
- the invention according to claim 2 irradiates the analyte with high energy particles in a vacuum atmosphere, and determines the number and kinetic energy of electrons emitted from the analyte by the photoelectric effect.
- An electron spectroscopic analysis method for detecting and performing a desired analysis in a depth direction of the sample to be analyzed, wherein the fullerene is ionized before irradiating the sample with high energy particles. Irradiating the surface of the sample to be analyzed to ion-etch the surface of the sample to be analyzed.
- the invention according to claim 6 irradiates the sample with high energy particles from a high energy energy particle irradiation device in a vacuum atmosphere, and emits electrons emitted from the sample by the photoelectric effect.
- An electron spectrometer for performing a desired analysis on the surface of the sample to be analyzed by detecting the number and kinetic energy of the high-energy particles by ionizing and irradiating fullerene.
- the ion gun force is also applied to the surface of the sample to be analyzed by ionizing fullerene to remove contaminants present on the surface of the sample to be analyzed.
- the invention according to claim 7 irradiates a sample to be analyzed with high-energy particles from a high-energy energy particle irradiation device in a vacuum atmosphere, and emits electrons emitted from the sample by the photoelectric effect.
- the ion gun force is also applied to the surface of the sample to be analyzed by ionizing fullerene, thereby ion-etching the surface of the sample to be analyzed.
- the surface of the sample to be analyzed is irradiated with a fullerene ion beam before the surface of the sample to be analyzed is irradiated with the high-energy particles. Since the surface of the sample to be analyzed can be uniformly etched to such an extent that the damage to the surface of the sample to be analyzed can be neglected, the analysis of the composition of the sample to be analyzed and the condition of the sample can be accurately performed.
- an ion gun that irradiates a fullerene ion beam is not large compared to a device (ion source) that forms a cluster, so that large-scale equipment is not required and cost increase can be suppressed.
- FIG. 1 is a schematic configuration diagram showing an electron spectroscopy analyzer according to Embodiment 1 of the present invention.
- the electron spectroscopic analyzer 1 according to the present embodiment (Shown) is connected, and a sample stage 5 for arranging and fixing a sample (analyte) 4 transferred from outside by a transfer device 3 is provided in the vacuum tank 2. ing.
- a high energy particle irradiation device 6 for irradiating the sample 4 placed on the sample stage 5 with high energy particles is provided above the vacuum chamber 2.
- An ion gun 8 for irradiating an ion beam (carbon 60 cluster ion beam) is provided.
- the ion gun 8 for irradiating the C60 ion beam a known ion gun can be used.
- a dual characteristic X-ray source equipped with aluminum and copper targets was used as the high energy particle irradiation device 6.
- the transfer arm 3a in the transfer device 3 which is evacuated and adjusted to a predetermined pressure (degree of vacuum) by vacuum evacuation by a vacuum evacuation device system (not shown) is driven.
- the sample 4 is placed on the sample stage 5 in the vacuum chamber 2 adjusted to the pressure of.
- pressure inside the vacuum chamber 2 is preferably not more than 1 X 10- 5 Pa.
- the pressure in the vacuum chamber 2 and 5 X 10- 7 Pa is preferably not more than 1 X 10- 5 Pa.
- the ion gun 8 is operated to irradiate the C60 ion beam to the surface of the sample (PTFE (polytetrafluoroethylene) ((CF)) 4, and the C60 ion beam collides with the surface of the sample 4.
- PTFE polytetrafluoroethylene
- the irradiation conditions of the C60 ion beam in the present embodiment were as follows: acceleration voltage: 2 kV, ion current: 10 nA, irradiation time: 60 sec, and scanning range on the surface of the sample 4: 5 mm ⁇ 5 mm.
- the high energy particle irradiation device (dual characteristic X-ray source) 6 is activated to The surface of sample 4 is irradiated with X-rays, and the composition and chemical state changes in the surface or depth direction of sample 4 are analyzed by electron energy analyzer 7 using the electrons emitted from sample 4 (X-ray photoelectron spectroscopy ).
- the characteristic X-rays irradiated in this embodiment were energy: 1.4867 keV, and aluminum was used as the target of the characteristic X-rays.
- the preferable acceleration voltage of the C60 ion beam is 30 kV or less, more preferably 10 kV or less, and 300 V or more.
- Embodiment 1 of the present invention before irradiating the surface of the sample 4 with characteristic X-rays from the high-energy energy particle irradiation device (dual characteristic X-ray source) 6, the C60 ion beam is irradiated from the ion gun 8.
- PTFE polytetrafluoroethylene
- the etching treatment was performed to remove contaminants such as water, oils and fats, inorganic substances, etc., and an oxide film adhered to the surface of Sample 4.
- the quantitative values of the surface of sample 4 were examined.As a result, carbon was approximately 35%, fluorine was approximately 65%, and most of the other elements were No power detected.
- the surface of the sample 4 is irradiated with the C60 ion beam so that damage to the surface of the sample 4 is negligible.
- the sample 4 can be uniformly etched to remove the contamination on the surface of the sample 4 and the acid coating, so that accurate qualitative and quantitative analysis of the sample 4 can be performed.
- the ion gun 8 for irradiating the C60 ion beam is not large as compared with a device (ion source) for forming a cluster, a large-scale facility is not required, and an increase in cost can be suppressed.
- the configuration of the electron spectroscopic analyzer 1 is substantially the same as that of the first embodiment, and redundant description will be omitted.
- the transfer arm 3a of the transfer device 3 is driven, and the sample 4 is placed on the sample stage 5 in the vacuum chamber 2 through the opened gate valve 9. Thereafter, the gate valve 9 is closed, and the inside of the vacuum chamber 2 is evacuated to a predetermined pressure (degree of vacuum) by a connected evacuation system (not shown). In this embodiment, the pressure in the vacuum chamber 2 and 5 X 10- 7 Pa. [0037] Then, the ion gun 8 is actuated to irradiate the C60 ion beam to the surface of the sample (PTFE (polytetrafluoroethylene) ((CF))) 4 so that the C60 ion beam collides with the sample 4 surface.
- PTFE polytetrafluoroethylene
- the irradiation conditions of the C60 ion beam in the present embodiment were as follows: acceleration voltage: 200 V to 30 kV, ion current: 10 nA, irradiation time: 60 sec, and scanning range on the surface of the sample 4: 5 mm ⁇ 5 mm.
- the high energy particle irradiation device (dual characteristic X-ray source) 6 is operated to irradiate the surface of the sample 4 with characteristic X-rays, and the electrons emitted from the sample 4 cause the surface or the surface of the sample 4 to be irradiated.
- the composition and chemical state change in the depth direction are analyzed by the electron energy analyzer 7 (X-ray photoelectron spectroscopy).
- the characteristic X-ray irradiated in the present embodiment was energy: 8.048 keV, and copper was used as the target of the characteristic X-ray.
- FIG. 2 shows that the surface of sample 4 is etched by irradiating a C60 ion beam having an accelerating voltage of 10 kV (a in the figure), 2 kV (b in the figure), and 200 V (c in the figure) on the surface of sample 4.
- X-ray photoelectron spectroscopy analysis of carbon Is line XPS (X-ray photoelectron spectroscopy analysis of carbon Is line
- the irradiation conditions of the C60 ion beam at this time were an ion current of 10 nA and an irradiation time of 60 sec.
- d in Fig. 2 shows the results of X-ray photoelectron spectroscopy (XPS) of the carbon Is line after irradiating the surface of sample 4 with Ar ions at an accelerating voltage of 500 V and etching the surface of sample 4. Vector).
- the Ar ion irradiation conditions at this time were an ion current of 100 nA and an irradiation time of 60 sec.
- the C60 ion beam when the C60 ion beam was irradiated at an acceleration voltage of 10 kV (a in the figure), slight alteration of the sample was observed (no problem in practical use).
- the C60 ion beam was set to 200 V ( When the sample was irradiated at the acceleration voltage of c), the sample surface was hardly etched, and a peak was observed in the XPS spectrum due to contamination of the sample surface.
- the C60 ion beam was irradiated at an accelerating voltage of 300 V, the sample surface was etched and almost no alteration of the sample was observed.
- a preferable acceleration voltage of the irradiated C60 ion beam is 30 kV or less, more preferably 10 kV or less. And 300V or more.
- a characteristic X-ray source for irradiating characteristic X-rays is used as the high-energy particle irradiating device 6, but other than this, an ultraviolet photoelectron spectroscopy device for irradiating ultraviolet light, An Auger electron spectrometer that irradiates electrons, a positron excitation Auger electron spectrometer that irradiates positrons, and the like can be used.
- the vacuum chamber 2 is evacuated to a predetermined pressure (degree of vacuum) by evacuating the vacuum chamber 2 by a vacuum exhaust system (not shown), and then the sample 4 is placed in the vacuum chamber 2. Conversely, after the sample 4 is placed in the vacuum chamber 2, the inside of the vacuum chamber 2 is evacuated by a vacuum evacuation system (not shown) to a predetermined pressure (degree of vacuum). It may be adjusted.
- the C60 ion beam is irradiated from the ion gun 8.
- fullerenes such as C70 and C84 and metal element-containing fullerenes may be ionized.
- a configuration in which irradiation is performed is also possible.
- FIG. 1 is a schematic configuration diagram showing an electron spectroscopic analyzer according to Embodiments 1 and 2 of the present invention.
- FIG. 2 is a diagram showing the results of X-ray photoelectron spectroscopy analysis of carbon is lines after irradiating a sample surface with a C60 ion beam while changing an acceleration voltage.
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Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP04793042A EP1679505A1 (en) | 2003-10-29 | 2004-10-27 | Electronic spectral analyzing method and analyzer |
US10/595,614 US20080042057A1 (en) | 2003-10-29 | 2004-10-27 | Electron Spectroscopy Analysis Method and Analytical Apparatus |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2003-368372 | 2003-10-29 | ||
JP2003368372A JP4497889B2 (ja) | 2003-10-29 | 2003-10-29 | 電子分光分析方法及び分析装置 |
Publications (1)
Publication Number | Publication Date |
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WO2005040778A1 true WO2005040778A1 (ja) | 2005-05-06 |
Family
ID=34510345
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2004/015930 WO2005040778A1 (ja) | 2003-10-29 | 2004-10-27 | 電子分光分析方法及び分析装置 |
Country Status (4)
Country | Link |
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US (1) | US20080042057A1 (ja) |
EP (1) | EP1679505A1 (ja) |
JP (1) | JP4497889B2 (ja) |
WO (1) | WO2005040778A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20150079796A1 (en) * | 2006-10-31 | 2015-03-19 | Fei Company | Charged-Particle-Beam Processing Using a Cluster Source |
Families Citing this family (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4205122B2 (ja) * | 2006-07-19 | 2009-01-07 | 株式会社日立ハイテクノロジーズ | 荷電粒子線加工装置 |
GB0720901D0 (en) * | 2007-10-24 | 2007-12-05 | Shimadzu Res Lab Europe Ltd | Charged particle energy analysers |
JPWO2009131022A1 (ja) * | 2008-04-23 | 2011-08-18 | 株式会社アルバック | 分析方法 |
GB2460855B (en) * | 2008-06-11 | 2013-02-27 | Kratos Analytical Ltd | Electron spectroscopy |
JP2010048584A (ja) * | 2008-08-19 | 2010-03-04 | Univ Of Yamanashi | X線光電子分光装置及び全反射x線光電子分光装置並びに角度分解x線光電子分光装置 |
JPWO2010029929A1 (ja) * | 2008-09-10 | 2012-02-02 | 株式会社アルバック | イオン照射装置 |
JP5692497B2 (ja) * | 2009-07-29 | 2015-04-01 | 福岡県 | 表面加工方法及び表面加工装置 |
DE102009036701A1 (de) * | 2009-08-07 | 2011-03-03 | Carl Zeiss Nts Gmbh | Teilchenstrahlsystem und Untersuchungsverfahren hierzu |
US8976932B2 (en) * | 2010-07-09 | 2015-03-10 | Bsr Co., Ltd. | X-ray generating device |
GB2484488B (en) | 2010-10-12 | 2013-04-17 | Vg Systems Ltd | Improvements in and relating to ion guns |
US8552369B2 (en) * | 2011-05-03 | 2013-10-08 | International Business Machines Corporation | Obtaining elemental concentration profile of sample |
JP2015138667A (ja) | 2014-01-22 | 2015-07-30 | アルバック・ファイ株式会社 | イオン源、イオン銃、分析装置 |
KR102257901B1 (ko) * | 2014-09-19 | 2021-05-31 | 삼성전자주식회사 | 반도체 검사 장비 및 이를 이용한 반도체 소자의 검사 방법 |
JP6331960B2 (ja) * | 2014-10-21 | 2018-05-30 | 住友金属鉱山株式会社 | 薄膜状の試料の前処理方法および分析方法 |
Citations (1)
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JP2001312994A (ja) * | 2000-04-26 | 2001-11-09 | Jeol Ltd | 電子分光装置 |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
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EP0570720A1 (en) * | 1992-05-20 | 1993-11-24 | Sumitomo Electric Industries, Ltd. | Stabilized carbon cluster conducting or superconducting material, its production, and use thereof |
US5558903A (en) * | 1993-06-10 | 1996-09-24 | The Ohio State University | Method for coating fullerene materials for tribology |
GB9510699D0 (en) * | 1995-05-26 | 1995-07-19 | Fisons Plc | Apparatus and method for surface analysis |
US5990476A (en) * | 1996-12-17 | 1999-11-23 | Physical Electronics Inc | Control of surface potential of insulating specimens in surface analysis |
US6743481B2 (en) * | 2000-06-01 | 2004-06-01 | Seagate Technology Llc | Process for production of ultrathin protective overcoats |
JP2002195965A (ja) * | 2000-12-27 | 2002-07-10 | Matsushita Electric Ind Co Ltd | オージェ電子分光分析装置およびそれを用いた分析方法 |
US6768120B2 (en) * | 2001-08-31 | 2004-07-27 | The Regents Of The University Of California | Focused electron and ion beam systems |
US20030080291A1 (en) * | 2001-10-26 | 2003-05-01 | Physical Electronics, Inc. | System and method for characterization of thin films |
GB2386747A (en) * | 2001-11-08 | 2003-09-24 | Ionoptika Ltd | Fullerene ion gun |
US7235796B2 (en) * | 2004-11-24 | 2007-06-26 | Technion Research & Development Foundation Ltd. | Method and apparatus for the generation of anionic and neutral particulate beams and a system using same |
-
2003
- 2003-10-29 JP JP2003368372A patent/JP4497889B2/ja not_active Expired - Fee Related
-
2004
- 2004-10-27 US US10/595,614 patent/US20080042057A1/en not_active Abandoned
- 2004-10-27 EP EP04793042A patent/EP1679505A1/en not_active Withdrawn
- 2004-10-27 WO PCT/JP2004/015930 patent/WO2005040778A1/ja active Application Filing
Patent Citations (1)
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JP2001312994A (ja) * | 2000-04-26 | 2001-11-09 | Jeol Ltd | 電子分光装置 |
Non-Patent Citations (2)
Title |
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POSTAWA Z. ET AL.: "Enhancement of sputtering yields due to C60 versus Ga bombardement of Ag{111} as explored by molecular dynamics simulations", ANALYTICAL CHEMISTRY, vol. 75, no. 17, 1 September 2003 (2003-09-01), pages 4402 - 4407, XP002983740 * |
SANADA N. ET AL.: "C60 ion sputter shori shita yuki kobunshi shiryo no ESCA bunseki", 2004 NEN (HEISEI 16 NEN) SHUNKI DAI 51 KAI OYO BUTSURIGAKU KANKEI RENGO KOENKAI KOEN YOKOSHU DAI 2 BUNSATSU, 28 March 2004 (2004-03-28), pages 761, XP002996975 * |
Cited By (1)
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---|---|---|---|---|
US20150079796A1 (en) * | 2006-10-31 | 2015-03-19 | Fei Company | Charged-Particle-Beam Processing Using a Cluster Source |
Also Published As
Publication number | Publication date |
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JP2005134170A (ja) | 2005-05-26 |
EP1679505A1 (en) | 2006-07-12 |
JP4497889B2 (ja) | 2010-07-07 |
US20080042057A1 (en) | 2008-02-21 |
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