JY/T 011-1996 PDF English
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General rules for transmission electron microscopy
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JY/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/JYT011-1996
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 Commission
Table of Contents
Foreword... 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... 14
Foreword
The 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 microscopy
1 Scope
This 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 Definitions
This 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 Principle
The 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 Instruments
4.1 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 Specimen
5.1 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 procedures
6.1 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 results
7.1 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 precautions
8.1 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 Commission
Table of Contents
Foreword... 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... 14
Foreword
The 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 microscopy
1 Scope
This 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 Definitions
This 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 Principle
The 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 Instruments
4.1 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 Specimen
5.1 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 procedures
6.1 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 results
7.1 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 precautions
8.1 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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