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Method for reconstructing three-dimensional reciprocal space of material with complex structure

A reciprocal space and complex structure technology, applied in the field of characterization of complex structures, can solve the problems of limited recording size and susceptibility to electron radiation damage, and achieve the effect of reducing radiation damage and high efficiency

Inactive Publication Date: 2010-07-07
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the limited recording size of the CCD imaging device and its vulnerability to electron radiation damage, the traditional film and imaging plate recording methods are still irreplaceable.

Method used

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  • Method for reconstructing three-dimensional reciprocal space of material with complex structure
  • Method for reconstructing three-dimensional reciprocal space of material with complex structure
  • Method for reconstructing three-dimensional reciprocal space of material with complex structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] like figure 1 As shown, XYZO is the spatial coordinate of the sample in the transmission electron microscope. Before tilting, the initial crystal plane normal of the sample is set to be parallel to the OZ axis, and the effective tilting axis is selected as OB'. After the main tilting axis of the sample stage is rotated α (the initial crystal plane normal is parallel to OA), the secondary tilting axis of the sample stage is rotated β (initial The crystal plane normal is parallel to OA') and then the first tilt is completed (the total rotation angle is Ф). At this time, if OA=OA'=1, the geometric relationship between the main inclination angle α of the sample stage, the secondary inclination angle β of the sample stage and the effective inclination angle θ can be established: tanθ=sinβ / tanα. The above formula can be rewritten as Δβ i =arcsin(tanΔα i ×tanθ). Selecting the tilt step size Δα for the tilted electron diffraction reconstruction experiment i Finally, calcul...

Embodiment 2

[0055] Embodiment 2: The inverted spatial drum-shaped distribution characteristics of PAN-based carbon fibers determined by the present invention

[0056] Before formally applying this method to the PAN-based carbon fiber sample, first calculate the projection angle of the tilting axis of the sample stage of the transmission electron microscope used on the film through the tilting electron diffraction experiment of the single crystal sample as described in step 1 in Example 1 Under the selected camera constant as figure 2 49° shown.

[0057]In the low-magnification imaging mode of the transmission electron microscope, look for the thin area of ​​the carbon fiber; combine the selected area electron diffraction to determine the selected area of ​​the carbon fiber to be tilted (it is better to have obvious features in the shape, so that it can be identified after tilting) such as Figure 7 shown. According to the method described in step 2 to 5 in embodiment 1, keep as Figur...

Embodiment 3

[0059] Example 3: Inverted spatial umbrella-shaped distribution characteristics of graphite crystallite orientation of pyrolytic carbon determined by the present invention

[0060] Before formally applying this method to the pyrolytic carbon sample in the carbon-carbon composite material, as described in step 1 in Example 1, the tilting axis of the sample stage of the transmission electron microscope used was first calculated through the tilting electron diffraction experiment of the single crystal sample at The projection angle on the film is as follows under the selected camera constant figure 2 49° shown.

[0061] In the low-magnification imaging mode of the transmission electron microscope, look for the thin area of ​​the pyrolytic carbon; combine the selected area electron diffraction to determine the selected area of ​​the pyrolytic carbon to be tilted, such as Figure 7 shown. According to the method described in step 2 to 5 in embodiment 1, keep as Figure 11 The e...

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Abstract

For some materials with complex structures or abnormal flaw distribution, the reciprocal spaces thereof may have locality constitution distribution or local paracycle modulation. The invention provides a method for reconstructing a three-dimensional reciprocal space of a material with a complex structure for confirming the kind of complex structures, the method carries out the pre-quantization through the matched value of a main tilt angle Alpha (titling step Delta Alpha i) and a vice tilt angle Beta ( titling offset angle Delta Beta i) of a sample platform in the process of tilting operation, so the operation and record of the whole tilting reconstruction experiment can be accurate and efficient. The invention solves the problems that the kind of complex structures is time-consuming and has poor precision, and the like. Since the quantity offset of the vice tilt angle Delta Beta i is adopted, the gained serial selected-area electron diffraction spectrum can accurately maintain the same titling axis, and also provides a practical method which can conform the dynamic range of intensity of a negative. On the basis of theoretical analysis, the method can simultaneously be matched with the experiment measurement, and quantificationally confirm the value range of diffracted intensity gray level, which accords with the intensity dynamic range of the record negative.

Description

technical field [0001] The present invention relates to a characterization method for the complex structure of materials, specifically including: (1) the pyrolytic carbon structure in carbon-carbon composite materials, (2) the inverted space structure of textured materials with continuous preferred orientation, (3) the presence of localized 3D reciprocal space reconstruction method for reciprocal space structure with continuous distribution, (4) reciprocal space structure with local quasi-periodic modulation, and (5) more complex distribution of reciprocal space structure. Background technique [0002] The preferred orientation distribution of crystallites in textured materials is closely related to the mechanical and physical properties of materials. In order to meet the material performance requirements of a certain application background, comprehensive and accurate characterization of the preferred orientation distribution characteristics of textured materials is the basi...

Claims

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Application Information

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IPC IPC(8): C04B35/83
Inventor 贺连龙朱媛苑
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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