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Similar standardsJY/T 011-1996: General rules for transmission electron microscopy---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/JYT011-1996JY INDUSTRY STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA General rules for transmission electron microscopy Issued on. JANUARY 22, 1997 Implemented on. APRIL 1, 1997 Approved by. State Education Commission Table of ContentsForeword... 3 1 Scope... 4 2 Definitions... 4 3 Principle... 4 4 Instruments... 6 5 Specimen... 8 6 Analytical procedures... 8 7 Expression of analysis results... 14 8 Safety precautions... 14ForewordThe drafting format and method of this Standard complies with the requirements of GB/T 1.1-1993 "Directives for the work of standardization - Unit 1.Drafting and presentation of standards - Part 1.General rules for drafting standards" and GB/T 1.4-88 "Directives for the work of standardization - rules for drafting chemical analysis standards". The drafting organization of this Standard. The State Education Commission. Main drafters of this Standard. Zhang Datong and Wang Yongrui. Participating drafters of this Standard. Wan Derui, Lin Chengyi and Zhou Shanyuan. General rules for transmission electron microscopy1 ScopeThis General Rules specify the conventional analytical method of transmission electron microscopy; it is are applicable to high-voltage transmission electron microscopy, high-resolution transmission electron microscopy, ordinary transmission electron microscopy AND simple transmission electron microscopy (hereinafter referred to as TEM).2 DefinitionsThis Standard adopts the following definitions. 2.1 Resolution TEM's capability that can clearly distinguish the minimum distance between two object points and crystal faces. 2.2 Astigmatism An image blurring that is caused by non-rotational symmetry of electromagnetic lenses' magnetic field, in which the lenses have different focusing ability in mutually perpendicular directions.3 PrincipleThe determinant of TEM imaging is the specimen scattering to incident electron, including elastic scattering and inelastic scattering. When thin-specimen is imaging, the un-scattered electrons shall constitute the background. However, the image contrast depends on different scattering characteristics of each part of the specimen to the electrons. Different experimental conditions shall produce different image contrasts. 3.1 Imaging modality Electron beams go into objective lens via specimen, then the first electronic image is formed on its image plane. The intermediate lens enlarges this image to form the image on its own image plane. The projector lens enlarges the image of the intermediate lens to form the final image on the phosphor screen. Its magnification M is the product of each imaging lens magnification. If the specimen is crystal, its electron diffraction pattern shall be presented on the focal plane of the objective lens.4 Instruments4.1 Instrument structure 4.1.1 Lighting system It is composed of electron gun and condenser. Electron gun provides stable electron source of small size and emits high-brightness electron beams. Condenser converges electron beams and irradiates the specimen. 4.1.4 Other systems and accessories Other systems and accessories include vacuum system, power system, security system and cooling system. Some are equipped with scanning accessories, micro diffraction apparatus, electron energy loss spectrometer (EELS) and X-ray energy dispersive spectrometer (EDS), etc. 4.2 Technical indicators 4.3 Environmental conditions 4.3.1 Ambient temperature. 20±5°C. 4.3.5 The ambient spurious magnetic field does not exceed 5×10-7T. 4.3.6 Ground vibration does not exceed 5 µm (when frequency is 5 Hz~20 Hz). 4.3.7 Cooling water pressure is not less than 5×104Pa; water flow is appropriate; water temperature is less than 25°C.5 Specimen5.1 Specimen Requirements The specimen shall not volatilize nor transform in vacuum or under bombardment of high-energy electron beams. It shall be chemically and physically stable, non-radioactive and non-corrosive. 5.2 Specimen preparation 5.2.1 Replica Copy the morphology on the surface of a solid specimen to the film, e.g. two- stage plastic-carbon replica and carbon extraction replica. 5.2.5 Micro-particles Cover the supporting film or micro-sieve membrane on the copper grid. Drip or spray the particle suspension scattered by ultrasound on the supporting film, and leave it to dry.6 Analytical procedures6.1 Power on Successively turn on the regulated power supply, cooling water system and main power switch. After vacuum degree meets the requirements, proceed to the next step. 6.2 Test preparation 6.2.1 Centering adjustment Increase high voltage and filament current. After light spot appears on the phosphor screen, center the lighting system and imaging system. Adjustment of “current center” or “voltage center” shall be strictly in accordance with the instructions for use. 6.2.4 Camera constant calibration Camera constant is the product of diffraction camera length L and wavelength of the incident electron beams k. Because of uncertainty of the length of TEM camera, it needs to use a gold polycrystalline thin film to calibrate. 6.2.5 Magnetic rotation calibration In the selective-area, when diffraction modality is switched to imaging modality, the change on excitation conditions of intermediate lens shall make the image and the diffraction pattern rotate at different angles, comparing to the actual orientation of specimen crystal. If the magnetic rotation of the image is Φi and the magnetic rotation of the pattern is Φd. 6.2.6 Specimen height calibration During magnification calibration and selective-area diffraction, in order to reduce the error, it shall need "Z Height" knob of side specimen-station to adjust the specimen height or standard specimen height, so as to make the specimen film surface and X tilting axis of side specimen-holder to coincide, and realize the equal height tilting. 6.3 Selection of working conditions 6.3.1 Acceleration voltage For general specimen, try to use the highest voltage. When detecting metal thin film or replica specimen, the acceleration voltage shall be at least 100 kV. For specimen of lower inherent contrast, it shall appropriately reduce the acceleration voltage. 6.4 Observation and determination 6.4.1 Mass-thickness contrast image When observing amorphous specimen - such as surface replica of metal or inorganic material, small object or particle, ultra-thin sections of biological tissue or replica of freeze etching - the greater the mass thickness in the area of specimen is, the stronger the scattering to incident electron shall be. 6.4.2 Electron diffraction and micro-diffraction in selective-area Usually, the crystallographic information of some micro-area of specimen is provided by electron diffraction of selective-area. In imaging modality, push the aperture of selective-area above the objective lens surface. Select the micro- area of specimen where it is going to generate diffraction. Limit its size. 6.4.3 Bright-field image and dark-field image of diffraction contrast Usually, the analysis on bright-field imaging and dark-field imaging is always combined with electron diffraction of selective-area, so as to determine the phase's microscopic morphology, lattice type and parameters. 6.4.4 Dark-field image of weak-beam It is widely used in studies on crystal defects, for example, the bright-field image and central dark-field image have higher resolution. In experiment, make specimen relatively far away from Bragg reflection position, comparing to electron beam. 6.4.5 High-resolution image It is used to study the details of atomic scale. The arrangement of atoms in the material can be directly observed. High-resolution imaging techniques are not only applied to measuring the resolution of TEM, but also has been widely used in biology, organic compounds, metals, super-conducting materials, silicates, etc. in order to study microcrystalline structure, crystal defects, interface structure and others. 6.4.6 Electron diffraction of convergent beam Convergent beam is incident to the specimen with its convergence angle which is large enough. Its transmission beam and the diffraction beam are expanded into discs. Within the disc, there are definite intensity distributions. And that is electron diffraction image of convergent beam. The image can precisely adjust crystallite orientation, determine crystal symmetry, lattice parameters of thin crystal area and thickness of thin crystal. Also, it can provide three-dimensional information of crystal structure.7 Expression of analysis results7.1 TEM image is usually provided in photo and interpreted according to mass- thickness contrast, diffraction contrast and phase contrast imaging theory. 7.3 Provide results of qualitative or quantitative analysis on chemical composition in micro-area of specimen.8 Safety precautions8.1 Operating rules of TEM must be strictly obeyed. JY/T 011-1996 JY INDUSTRY STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA General rules for transmission electron microscopy Issued on. JANUARY 22, 1997 Implemented on. APRIL 1, 1997 Approved by. State Education CommissionTable of ContentsForeword... 3 1 Scope... 4 2 Definitions... 4 3 Principle... 4 4 Instruments... 6 5 Specimen... 8 6 Analytical procedures... 8 7 Expression of analysis results... 14 8 Safety precautions... 14ForewordThe drafting format and method of this Standard complies with the requirements of GB/T 1.1-1993 "Directives for the work of standardization - Unit 1.Drafting and presentation of standards - Part 1.General rules for drafting standards" and GB/T 1.4-88 "Directives for the work of standardization - rules for drafting chemical analysis standards". The drafting organization of this Standard. The State Education Commission. Main drafters of this Standard. Zhang Datong and Wang Yongrui. Participating drafters of this Standard. Wan Derui, Lin Chengyi and Zhou Shanyuan. General rules for transmission electron microscopy1 ScopeThis General Rules specify the conventional analytical method of transmission electron microscopy; it is are applicable to high-voltage transmission electron microscopy, high-resolution transmission electron microscopy, ordinary transmission electron microscopy AND simple transmission electron microscopy (hereinafter referred to as TEM).2 DefinitionsThis Standard adopts the following definitions. 2.1 Resolution TEM's capability that can clearly distinguish the minimum distance between two object points and crystal faces. 2.2 Astigmatism An image blurring that is caused by non-rotational symmetry of electromagnetic lenses' magnetic field, in which the lenses have different focusing ability in mutually perpendicular directions.3 PrincipleThe determinant of TEM imaging is the specimen scattering to incident electron, including elastic scattering and inelastic scattering. When thin-specimen is imaging, the un-scattered electrons shall constitute the background. However, the image contrast depends on different scattering characteristics of each part of the specimen to the electrons. Different experimental conditions shall produce different image contrasts. 3.1 Imaging modality Electron beams go into objective lens via specimen, then the first electronic image is formed on its image plane. The intermediate lens enlarges this image to form the image on its own image plane. The projector lens enlarges the image of the intermediate lens to form the final image on the phosphor screen. Its magnification M is the product of each imaging lens magnification. If the specimen is crystal, its electron diffraction pattern shall be presented on the focal plane of the objective lens.4 Instruments4.1 Instrument structure 4.1.1 Lighting system It is composed of electron gun and condenser. Electron gun provides stable electron source of small size and emits high-brightness electron beams. Condenser converges electron beams and irradiates the specimen. 4.1.4 Other systems and accessories Other systems and accessories include vacuum system, power system, security system and cooling system. Some are equipped with scanning accessories, micro diffraction apparatus, electron energy loss spectrometer (EELS) and X-ray energy dispersive spectrometer (EDS), etc. 4.2 Technical indicators 4.3 Environmental conditions 4.3.1 Ambient temperature. 20±5°C. 4.3.5 The ambient spurious magnetic field does not exceed 5×10-7T. 4.3.6 Ground vibration does not exceed 5 µm (when frequency is 5 Hz~20 Hz). 4.3.7 Cooling water pressure is not less than 5×104Pa; water flow is appropriate; water temperature is less than 25°C.5 Specimen5.1 Specimen Requirements The specimen shall not volatilize nor transform in vacuum or under bombardment of high-energy electron beams. It shall be chemically and physically stable, non-radioactive and non-corrosive. 5.2 Specimen preparation 5.2.1 Replica Copy the morphology on the surface of a solid specimen to the film, e.g. two- stage plastic-carbon replica and carbon extraction replica. 5.2.5 Micro-particles Cover the supporting film or micro-sieve membrane on the copper grid. Drip or spray the particle suspension scattered by ultrasound on the supporting film, and leave it to dry.6 Analytical procedures6.1 Power on Successively turn on the regulated power supply, cooling water system and main power switch. After vacuum degree meets the requirements, proceed to the next step. 6.2 Test preparation 6.2.1 Centering adjustment Increase high voltage and filament current. After light spot appears on the phosphor screen, center the lighting system and imaging system. Adjustment of “current center” or “voltage center” shall be strictly in accordance with the instructions for use. 6.2.4 Camera constant calibration Camera constant is the product of diffraction camera length L and wavelength of the incident electron beams k. Because of uncertainty of the length of TEM camera, it needs to use a gold polycrystalline thin film to calibrate. 6.2.5 Magnetic rotation calibration In the selective-area, when diffraction modality is switched to imaging modality, the change on excitation conditions of intermediate lens shall make the image and the diffraction pattern rotate at different angles, comparing to the actual orientation of specimen crystal. If the magnetic rotation of the image is Φi and the magnetic rotation of the pattern is Φd. 6.2.6 Specimen height calibration During magnification calibration and selective-area diffraction, in order to reduce the error, it shall need "Z Height" knob of side specimen-station to adjust the specimen height or standard specimen height, so as to make the specimen film surface and X tilting axis of side specimen-holder to coincide, and realize the equal height tilting. 6.3 Selection of working conditions 6.3.1 Acceleration voltage For general specimen, try to use the highest voltage. When detecting metal thin film or replica specimen, the acceleration voltage shall be at least 100 kV. For specimen of lower inherent contrast, it shall appropriately reduce the acceleration voltage. 6.4 Observation and determination 6.4.1 Mass-thickness contrast image When observing amorphous specimen - such as surface replica of metal or inorganic material, small object or particle, ultra-thin sections of biological tissue or replica of freeze etching - the greater the mass thickness in the area of specimen is, the stronger the scattering to incident electron shall be. 6.4.2 Electron diffraction and micro-diffraction in selective-area Usually, the crystallographic information of some micro-area of specimen is provided by electron diffraction of selective-area. In imaging modality, push the aperture of selective-area above the objective lens surface. Select the micro- area of specimen where it is going to generate diffraction. Limit its size. 6.4.3 Bright-field image and dark-field image of diffraction contrast Usually, the analysis on bright-field imaging and dark-field imaging is always combined with electron diffraction of selective-area, so as to determine the phase's microscopic morphology, lattice type and parameters. 6.4.4 Dark-field image of weak-beam It is widely used in studies on crystal defects, for example, the bright-field image and central dark-field image have higher resolution. In experiment, make specimen relatively far away from Bragg reflection position, comparing to electron beam. 6.4.5 High-resolution image It is used to study the details of atomic scale. The arrangement of atoms in the material can be directly observed. High-resolution imaging techniques are not only applied to measuring the resolution of TEM, but also has been widely used in biology, organic compounds, metals, super-conducting materials, silicates, etc. in order to study microcrystalline structure, crystal defects, interface structure and others. 6.4.6 Electron diffraction of convergent beam Convergent beam is incident to the specimen with its convergence angle which is large enough. Its transmission beam and the diffraction beam are expanded into discs. Within the disc, there are definite intensity distributions. And that is electron diffraction image of convergent beam. The image can precisely adjust crystallite orientation, determine crystal symmetry, lattice parameters of thin crystal area and thickness of thin crystal. Also, it can provide three-dimensional information of crystal structure.7 Expression of analysis results7.1 TEM image is usually provided in photo and interpreted according to mass- thickness contrast, diffraction contrast and phase contrast imaging theory. 7.3 Provide results of qualitative or quantitative analysis on chemical composition in micro-area of specimen.8 Safety precautions8.1 Operating rules of TEM must be strictly obeyed. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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