CN104132955A - TEM diffraction spot pattern sharpening processing method - Google Patents
TEM diffraction spot pattern sharpening processing method Download PDFInfo
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- CN104132955A CN104132955A CN201410272154.6A CN201410272154A CN104132955A CN 104132955 A CN104132955 A CN 104132955A CN 201410272154 A CN201410272154 A CN 201410272154A CN 104132955 A CN104132955 A CN 104132955A
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Abstract
The invention discloses a TEM diffraction spot pattern sharpening processing method which comprises the following steps: a, shooting a TEM sample, to obtain a TEM diffraction pattern; b, converting the TEM diffraction pattern into a radial intensity distribution curve by a center rotating average method; c, carrying out mirror symmetry on half a central peak formed by the TEM diffraction pattern center spots by a symmetry method, to form a complete peak; d, then fitting the complete center peak by a Gauss peak, to obtain a desired point spread function; e, processing the radial intensity distribution curve by a maximum entropy principle or a maximum likelihood method, to obtain a sharpened diffraction peak; and f, measuring the position of the sharpened diffraction peak. The method has accurate measurement results, especially can improve the measurement accuracy during measurement of lattice constants or interplanar crystal spacing by the TEM diffraction method, and has a great help on micro zone phase analysis and nano beam strain analysis.
Description
Technical field
The present invention relates to a kind of TEM diffraction image disposal route, particularly a kind of sharp keenization of TEM diffraction spot point diagram disposal route.
Background technology
In some TEM diffraction analysis method, for example nanometer bundle strain analysis, the size of diffraction spot is subject to the impact of converging half-angle of electron beam.Converge half-angle larger, diffraction spot is also larger.Excessive diffraction spot will certainly affect the accuracy of diffraction spot position measurement.Be subject to the restriction of instrument, especially the TEM equipment of low side, when carrying out nanometer bundle strain analysis, converges half-angle and cannot be transferred to desirable numerical value, causes the diffraction spot obtaining to appear to diffraction discs.This diffraction image cannot carry out accurate lattice and interplanar distance is measured.And the concept that is applied in the maximum likelihood method adopting in the sharpening of EELS collection of illustrative plates cannot directly apply to sharp keenization of TEM diffraction spot point diagram, need first diffraction spot image to be converted into collection of illustrative plates and just can carry out sharp keenization processing.
Summary of the invention
For above-mentioned technical matters, the present invention discloses a kind of sharp keenization of TEM diffraction spot point diagram disposal route, comprises the following steps: a, use selected diffraction or nanometer bundle diffraction method are taken TEM sample, obtain TEM diffracting spectrum; B, the use central rotation method of average are converted to radial intensity distribution curve by described TEM diffracting spectrum; C, use balanced method carry out Mirror Symmetry by half central peak of described TEM diffracting spectrum center spot formation, form a complete peak; D, use the complete central peak of Gaussian peak matching or other diffraction peak again, obtain required point spread function; The point spread function obtaining in e, use steps d, utilizes principle of maximum entropy or maximum likelihood method to process described radial intensity distribution curve, and the diffraction peak after processing in described radial intensity distribution curve can be by sharp keenization; F, finally measure the position of the diffraction peak after sharp keenization, the accuracy of measuring to improve lattice.
Preferably, the TEM thickness of sample in described step a is 10nm ~ 1000nm, and the time shutter of described shooting is 0.01s ~ 1s.
Preferably, the central rotation method of average in described step b, adopts the auxiliary realization of Diff Tools kit.
Preferably, in described step c, the intensity of central peak of usining is reduced to the position of background intensity as the end position of central peak, and the null position of usining carries out Mirror Symmetry operation as symcenter, obtains complete central peak.
The invention has the beneficial effects as follows by take center spot as the center of circle, whole diffracting spectrum is done to central rotation to handle averagely, obtain with EELS collection of illustrative plates and have homophylic diffracting spectrum, then carry out sharp keenization processing by maximum likelihood method.The measurement result of sharp keenization of TEM diffraction spot point diagram disposal route of the present invention is accurate, particularly when by TEM diffraction measurement grating constant or interplanar distance, can improve measuring accuracy, the analytical approach that depends on accurate measurement diffraction spot position for microcell facies analysis and nanometer bundle strain analysis etc. has very great help.
Embodiment
Below the present invention is described in further detail, to make those skilled in the art can implement according to this with reference to instructions word.
The present invention discloses a kind of sharp keenization of TEM diffraction spot point diagram disposal route, comprises the following steps: a, use selected diffraction or nanometer bundle diffraction method or other diffraction method are taken TEM sample, obtain TEM diffracting spectrum; B, the use central rotation method of average are converted to radial intensity distribution curve by described TEM diffracting spectrum; C, use balanced method carry out Mirror Symmetry by half central peak of described TEM diffracting spectrum center spot formation, form a complete peak; D, use the complete central peak of Gaussian peak matching or other diffraction peak again, obtain required point spread function; The point spread function obtaining in e, use steps d, utilizes principle of maximum entropy or maximum likelihood method to process described radial intensity distribution curve, and the diffraction peak after processing in described radial intensity distribution curve can be by sharp keenization; F, finally measure the position of the diffraction peak after sharp keenization, the accuracy of measuring to improve lattice.
Preferably, the TEM thickness of sample in described step a is 10nm ~ 1000nm, and the time shutter of described shooting is 0.01s ~ 1s.
Preferably, the central rotation method of average in described step b, adopts the auxiliary realization of Diff Tools kit.
Preferably, in described step c, the intensity of central peak of usining is reduced to the position of background intensity as the end position of central peak, and the null position of usining carries out Mirror Symmetry operation as symcenter, obtains complete central peak.
Specifically tell about sharp keenization of TEM diffraction spot point diagram disposal route of the present invention below.
Embodiment 1
This method for be TEM diffracting spectrum, especially nanoelectronic bundle diffracting spectrum, carries out sharp keenization processing by the method for the invention, can effectively improve measuring accuracy.Described sharp keenization of TEM diffraction spot point diagram disposal route comprises the following steps:
A, use nanometer bundle diffraction method are taken TEM sample, obtain TEM diffracting spectrum, and the TEM thickness of sample in described step a is 10nm ~ 1000nm, and the time shutter of described shooting is 0.01s ~ 1s.Guarantee that TEM sample can not be blocked up, and diffraction spot wants shooting clear, and select the correct time shutter, the basic demand of exposure is that diffraction spot can not overexposure or under-exposure;
B, the use central rotation method of average are converted to radial intensity distribution curve by described TEM diffracting spectrum, and accurately location is wanted carefully in the center of diffraction spot, can do to assist with donut and accurately locate, and guarantee that diffraction spot of the same type is on same circumference.The described central rotation method of average, adopts the auxiliary realization of Diff Tools kit, and Diff Tools kit is to be installed on Digital Micrograph
tMa module in software, or adopt the software of other similar functions to realize the conversion of collection of illustrative plates;
C, the intensity of central peak of usining are reduced to the position of background intensity as the end position of central peak, using null position as symcenter, use balanced method that half central peak of described TEM diffracting spectrum center spot formation is carried out to Mirror Symmetry, form a complete peak, must guarantee that be a complete peak by half central peak symmetrical treatment before sharpening is processed, otherwise follow-up sharpening processing may be failed;
D, use the complete central peak of Gaussian peak matching again, obtain required point spread function;
The point spread function obtaining in e, use steps d, utilize principle of maximum entropy or maximum likelihood method to process described radial intensity distribution curve, diffraction peak after processing in described radial intensity distribution curve can be by sharp keenization, wherein, described maximum likelihood method basic calculating principle has specific descriptions in existing document.The maximum likelihood method that the present invention adopts is according to this basic calculating principle, realizes, and carried out the necessary modification of part with Phython programming language, makes it be applicable to the sharpening needs of the radial intensity distribution curve that the central rotation method of average obtains;
F, finally measure the position of the diffraction peak after sharp keenization, improve the accuracy that lattice is measured.
So operation, by take center spot as the center of circle, whole diffracting spectrum is done to central rotation to handle averagely, obtained with EELS collection of illustrative plates and had homophylic diffracting spectrum, the maximum likelihood method of application enhancements is carried out sharp keenization processing again, collection of illustrative plates measurement result after sharp keenization processed is accurate, particularly when by TEM diffraction measurement grating constant or interplanar distance, can improve measuring accuracy, the analytical approach that depends on accurate measurement diffraction spot position for microcell facies analysis and nanometer bundle strain analysis etc. has very great help.
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in instructions and embodiment, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other modification, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the embodiment describing.
Claims (4)
1. sharp keenization of a TEM diffraction spot point diagram disposal route, is characterized in that, comprises the following steps:
A, use selected diffraction or nanometer bundle diffraction method are taken TEM sample, obtain TEM diffracting spectrum;
B, the use central rotation method of average are converted to radial intensity distribution curve by described TEM diffracting spectrum;
C, use balanced method carry out Mirror Symmetry by half central peak of described TEM diffracting spectrum center spot formation, form a complete peak;
D, use the complete central peak of Gaussian peak matching or other diffraction peak again, obtain required point spread function;
The point spread function obtaining in e, use steps d, utilizes principle of maximum entropy or maximum likelihood method to process described radial intensity distribution curve, and the diffraction peak after processing in described radial intensity distribution curve can be by sharp keenization;
F, measure the position of the diffraction peak after sharp keenization, the accuracy of measuring to improve lattice.
2. sharp keenization of TEM diffraction spot point diagram disposal route according to claim 1, is characterized in that: the TEM thickness of sample in described step a is 10nm ~ 1000nm, and the time shutter of described shooting is 0.01s ~ 1s.
3. sharp keenization of TEM diffraction spot point diagram disposal route according to claim 1, is characterized in that: the central rotation method of average in described step b, adopts the auxiliary realization of Diff Tools kit.
4. sharp keenization of TEM diffraction spot point diagram disposal route according to claim 1, it is characterized in that: in described step c, the intensity of central peak of usining is reduced to the position of background intensity as the end position of central peak, the null position of usining carries out Mirror Symmetry operation as symcenter, obtains complete central peak.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107247061A (en) * | 2017-06-02 | 2017-10-13 | 中国工程物理研究院核物理与化学研究所 | Neutron powder diffractometer detector Zero calibration method |
| CN112105918A (en) * | 2018-05-14 | 2020-12-18 | 株式会社理学 | Method, device and program for discriminating graphene precursor |
| CN112461866A (en) * | 2020-11-18 | 2021-03-09 | 浙江大学 | Electronic diffraction auxiliary measuring method for main exposed surface of nano powder crystal |
| CN112649453A (en) * | 2020-12-09 | 2021-04-13 | 北京大学 | Method for measuring four-dimensional electron energy loss spectrum of sample to be measured |
-
2014
- 2014-06-18 CN CN201410272154.6A patent/CN104132955A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| D.R.G. MITCHELL: "《DiffTools: Electron Diffraction Software Tools for DigitalMicrographTM》", 《MICROSCOPY RESEARCH AND TECHNIQUE》 * |
| P.N.H. NAKASHIMA,ETAL: "《Measuring the PSFfrom aperture images of arbitrary shape—an algorithm》", 《ULTRAMICROSCOPY》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107247061A (en) * | 2017-06-02 | 2017-10-13 | 中国工程物理研究院核物理与化学研究所 | Neutron powder diffractometer detector Zero calibration method |
| CN112105918A (en) * | 2018-05-14 | 2020-12-18 | 株式会社理学 | Method, device and program for discriminating graphene precursor |
| CN112461866A (en) * | 2020-11-18 | 2021-03-09 | 浙江大学 | Electronic diffraction auxiliary measuring method for main exposed surface of nano powder crystal |
| CN112649453A (en) * | 2020-12-09 | 2021-04-13 | 北京大学 | Method for measuring four-dimensional electron energy loss spectrum of sample to be measured |
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