CN109632849A - A kind of transmission electron microscope imaging method for distinguishing different type dislocation - Google Patents
A kind of transmission electron microscope imaging method for distinguishing different type dislocation Download PDFInfo
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Abstract
The invention discloses the transmission electron microscope imaging methods that one kind can distinguish different type dislocation, comprising: under common transmission electron microscope mode, vert sample, makes electron beam along the incidence of the first crystal zone axis, shoots diffraction spectra and demarcate；It is verted sample according to calibration, sample is made to be in the two-beam diffraction state of the first diffraction vector；Electronic Speculum is switched into dark-field imaging mode, the diffraction contrast image of the first diffraction vector diffracted beam is collected using detector；Vert sample, shoots sample along the diffraction spectra of the second crystal zone axis, and demarcate；It is verted sample according to calibration, the dislocation region to be seen of sample is set successively to be in the two-beam diffraction state of two different diffraction vectors, and Electronic Speculum is switched into dark-field imaging mode, collect the diffraction contrast image of the two different diffraction vector diffracted beams respectively using detector.The present invention solves the problems, such as that the Types of Dislocations of a variety of Burgers vectors cannot be distinguished in traditional " two-beam " diffraction, is conducive to the dislocation development law that sample is disclosed deeper into ground.
Description
Technical field
The present invention relates to material microstructures to test and analyze technical field, more particularly to one kind can distinguish different type dislocation
Transmission electron microscope imaging method.
Background technique
The rapid development of modern science and technology, it is desirable that material science worker can provide in time with excellent mechanical performances
Structural material and functional material with various physical and chemical performances, and the performance of material is often depending on its microstructure
And component distributing.Therefore, in order to study new material or improve traditional material, it is necessary to as high as possible resolution capability observation and
Analysis of material is under preparation, processing and use condition (including in phase transition process, under applied stress and the effect of various environmental factors
Deng) variation of microstructure and micro-area composition, and relationship between material composition-technique-microstructure-performance is disclosed in turn
Rule, establish and develop material science basic theories.
Transmission electron microscope (TEM) is exactly such a resolution capability that can reach atomic scale, while providing physical analysis
With the instrument of repertoire needed for chemical analysis.The especially application of selective electron diffraction technology, so that micro-raman spectra and microcell
Crystal structure analysis combines, then is equipped with power spectrum or wave spectrum progress microsection component analyzing, obtains comprehensive information.Utilize transmission
Electronic Speculum carries out imaging to dislocation, the Evolution of dislocation is analyzed according to the type of dislocation, configuration, to group III-nitride
Semiconductor material growing has important directive significance.
" two-beam " diffraction contrast image technology is the more mature technology with transmission electron microscope observing material dislocation.Its basic step is
Sample is set to be in " two-beam " diffraction locations --- the brightness of the transmission spot in sample diffraction spectrum and a specific diffraction spot is remote at this time
Greater than other diffraction spots, recycles lens isis to choose diffraction spot or transmit the diffraction contrast imaging that spot carries out dislocation.It utilizes
" two-beam " diffraction contrast image of different diffracted beam g, acquisition can distinguish dislocation class to the imaging of material the same area different type dislocation
The form of type and observation dislocation.
There are three types of hexagonal structure group III-nitride dislocation basal dislocations, and c type, a type and a+c type, Burgers vector are respectively
<0001>, 1/3<11-20>and 1/3<11-23>.It is traditional, spread out lining for " two-beam " of hexagonal structure group III-nitride dislocation
As observation, the dislocation of these three types can be distinguished using two kinds of diffraction vectors g=0002, g=11-20, as shown in table 1.Table 1
In, ticking indicates contrast, it can be observed that dislocation under the diffraction vector；Cross indicates no contrast, under the diffraction vector
It cannot observe dislocation.
Table 1
However, Burgers vector is a type dislocation of 1/3<11-20>according to the symmetry of hexagonal structure group III-nitride
It is ± 1/3 [1-210], ± 1/3 [11-20], three kinds of ± 1/3 [2-1-10] that Burgers vector, which can be subdivided into,.In general, extension is raw
Most of dislocation is a type dislocation in long group III-nitride, and accurate three kinds of forms for differentiating a type dislocation are to deep understanding a type
Origin of the dislocation in Material growth, proliferation, developing and burying in oblivion is of great significance.However, from table 1 it follows that tradition
Observation dislocation method cannot further to Burgers vector be ± 1/3 [1-210], ± 1/3 [11-20], ± 1/3 [2-1-10]
Three kinds of a type dislocations distinguish.
Summary of the invention
In view of the shortcomings of the prior art, the present invention provides one kind can distinguish the transmission electron microscope of different type dislocation at
Image space method, facilitate people deeper into study sample in different dislocations interaction rule.
In order to achieve the above purpose, present invention employs the following technical solutions:
A kind of transmission electron microscope imaging method for distinguishing different type dislocation, comprising:
Under common transmission electron microscope mode, vert sample, makes electron beam along the incidence of the first crystal zone axis, shoots diffraction spectra, and
Carry out first time calibration；
The sample that verts is demarcated according to the first time, observation in real time and shooting diffraction spectra determine that sample is in the first diffraction
The two-beam diffraction state of vector；
Electronic Speculum is switched into dark-field imaging mode, the diffraction of the first diffraction vector diffracted beam is collected using detector
Contrast image；
Vert sample, so that electron beam shoots the diffraction spectra of sample along the incidence of the second crystal zone axis, and carries out second and marks
Fixed, first crystal zone axis is different from second crystal zone axis；
The sample that verts is demarcated according to described second, observation in real time and shooting diffraction spectra make the dislocation area to be seen of sample
Domain is in the two-beam diffraction state of the second diffraction vector；
Electronic Speculum is switched into dark-field imaging mode, the diffraction of the second diffraction vector diffracted beam is collected using detector
Contrast image；
The sample that verts is demarcated according to described second, observation in real time and shooting diffraction spectra make the dislocation area to be seen of sample
Domain is in the two-beam diffraction state of third diffraction vector；
Electronic Speculum is switched into dark-field imaging mode, the diffraction of the third diffraction vector diffracted beam is collected using detector
Contrast image.
As one of embodiment, the sample is the group III-nitride of hexagonal structure.
As one of embodiment, first crystal zone axis is [11-20] crystal orientation.
As one of embodiment, second crystal zone axis is [- 5,10, -5,3] crystal orientation.
As one of embodiment, first diffraction vector corresponds to g=10-10.
As one of embodiment, second diffraction vector corresponds to g=1-105.
As one of embodiment, the third diffraction vector corresponds to g=0-115.
The present invention is imaged by supplementing a variety of diffraction vectors in traditional imaging mode, is advised using the delustring of dislocation
Rule, solves the problems, such as that the Types of Dislocations of a variety of Burgers vectors cannot be distinguished in traditional " two-beam " diffraction, can be to dislocation
Type, configuration and interaction are analyzed, deeper into ground disclose sample, such as group III-nitride dislocation development law.
Detailed description of the invention
Fig. 1 is the diffraction spectra and calibration result when the sample of the embodiment of the present invention is in the first crystal zone shaft position；
Fig. 2 is that the sample of the embodiment of the present invention is in " two-beam " diffraction state schematic diagram of diffraction vector g=10-10；
Fig. 3 is the sample diffraction contrast image under different diffraction vectors respectively of the embodiment of the present invention, in figure, (a)-
It (e) is respectively g=10-10, g=1-105, g=01-15, the diffraction contrast image of g=0002, g=11-20；
Fig. 4 is the diffraction spectra and calibration result when the sample of the embodiment of the present invention is in the second crystal zone shaft position；
Fig. 5 is the diffraction spectra that the sample of the embodiment of the present invention is in " two-beam " diffraction state of diffraction vector g=1-105；
Fig. 6 is the diffraction spectra that the sample of the embodiment of the present invention is in " two-beam " diffractive shape of diffraction vector g=0-115.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further described.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and do not have to
It is of the invention in limiting.
Transmission electron microscope imaging method of the invention can be used for distinguishing the different type dislocation of sample, and main includes following step
It is rapid:
S01, under common transmission electron microscope mode, find the dislocation region to be seen of sample, vert sample, makes electron beam edge
First crystal zone axis is incident, shoots the diffraction spectra of sample, and carry out first time calibration.
Preferably, sample of the invention is the group III-nitride of hexagonal structure, such as AlN, GaN, InN.For convenience of description,
The present embodiment is illustrated by taking AlN sample as an example.
It in actual operation, is the characteristic for cooperating AlN sample, which is [11-20] crystal orientation, the present embodiment
When AlN sample is in the position the first crystal zone axis [11-20], calibrated diffraction spectrogram picture is as shown in Figure 1.
S02, verted according to first time calibration sample, in real time observation and shooting diffraction spectra, determine that sample is in the first diffraction
The two-beam diffraction state of vector.
It is after crystal orientation carries out first time calibration with the first crystal zone axis [11-20], it is only necessary to which small range is verted AlN sample, i.e.,
The dislocation not of the same race of AlN sample can be made successively to be under the two-beam diffraction state of the first diffraction vector, as shown in Figure 2, it is preferable that
First diffraction vector corresponds to g=10-10.As shown in table 2 below, at first diffraction vector g=10-10, only Burgers
Vector is that both a type dislocations of ± 1/3 [11-20], ± 1/3 [2-1-10] can be imaged, and Burgers vector is ± 1/3
The a type dislocation of [1-210] can not be imaged.
Table 2
S03, Electronic Speculum is switched into dark-field imaging mode, the diffraction of the first diffraction vector diffracted beam is collected using detector
Contrast image.
AlN sample is shown in (a) image such as in Fig. 3 of the diffraction contrast image under the first diffraction vector g=10-10.
S04, vert sample, makes electron beam along the incidence of the second crystal zone axis, shoots the diffraction spectra of sample, and carries out second and mark
It is fixed.
Here, the first crystal zone axis is different from the second crystal zone axis, and the second crystal zone axis is [- 5,10, -5,3] crystal orientation.The present embodiment
AlN sample when being in the second crystal zone axis [- 5,10, -5,3] position, calibrated diffraction spectra is as shown in Figure 4.
S05, verted according to second of calibration sample, in real time observation and shooting diffraction spectra, make the dislocation area to be seen of sample
Domain is in the two-beam diffraction state of the second diffraction vector.
S06, Electronic Speculum is switched into dark-field imaging mode, the diffraction of the second diffraction vector diffracted beam is collected using detector
Contrast image.
S07, verted according to second of calibration sample, in real time observation and shooting diffraction spectra, make the dislocation area to be seen of sample
Domain is in the two-beam diffraction state of third diffraction vector.
S08, Electronic Speculum is switched into dark-field imaging mode, the diffraction of the second diffraction vector diffracted beam is collected using detector
Contrast image.
With the second crystal zone axis [- 5,10, -5,3] be crystal orientation carry out second demarcate after, it is only necessary to small range is verted AlN sample
Product can make the dislocation not of the same race of AlN sample successively be respectively at the two-beam diffraction of the second diffraction vector and third diffraction vector
Under state, as shown in Figure 5, Figure 6, it is preferable that the second diffraction vector and third diffraction vector respectively correspond as g=1-105 and g=
0-115。
In conjunction with shown in table 2, at diffraction vector g=1-105, Burgers vector is ± 1/3 [1-210], ± 1/3 [2-
1-10] both a type dislocations can be imaged, and Burgers vector be ± 1/3 [11-20] a type dislocation can not be imaged；At this
Under diffraction vector g=0-115, Burgers vector is that both a type dislocations of ± 1/3 [1-210], ± 1/3 [11-20] can be at
Picture, and a type dislocation that Burgers vector is ± 1/3 [2-1-10] can not be imaged.And combine the first diffraction vector g=of front
10-10 imaging contexts: at the first diffraction vector g=10-10, Burgers vector is ± 1/3 [11-20], ± 1/3 [2-1-10]
Both a type dislocations can be imaged, and a type dislocation that Burgers vector is ± 1/3 [1-210] can not be imaged, therefore, can be with
Both a type dislocations that Burgers vector is ± 1/3 [11-20], ± 1/3 [2-1-10] are distinguished easily.
As in Fig. 3 (b), shown in (c) image, respectively AlN sample is in the second diffraction vector g=1-105, third diffraction
Diffraction contrast image under vector g=0-115.(d), it is under g=0002, g=11-20 that (e) image, which is respectively diffraction vector,
Diffraction contrast image can be clear c type, a type and a for distinguishing hexagonal structure group III-nitride by combining table 2 and Fig. 3
+ c type dislocation.
The imaging of traditional diffraction vector g=0002, g=11-20 can be distinguished using above-mentioned similar imaging method,
The present invention is not intended to limit.Such as: under common transmission electron microscope mode, vert sample, shoots the diffraction spectra of sample, rower of going forward side by side
It is fixed；Then, according to the calibration, vert sample, and the dislocation region to be seen of sample is made successively to be in diffraction vector g=0002, g=
The two-beam diffraction state of 11-20；Finally, Electronic Speculum is switched into dark-field imaging mode, diffraction vector g=is collected using detector
0002, the diffraction contrast image of g=11-20 diffracted beam.
The embodiment of the present invention introduces g=10-10, tri- kinds of diffraction of g=1-105, g=0-115 on the basis of conventional method
Vector imaging, using the delustring rule of dislocation diffraction contrast image, solving traditional " two-beam " diffraction contrast image be cannot be distinguished in group III-nitride
The problem of different a type dislocation (Burgers vector is respectively ± 1/3 [11-20], ± 1/3 [1-210], ± 1/3 [2-1-10]), have
Help people deeper into research group III-nitride in different dislocations interaction rule.
The above is only the specific embodiment of the application, it is noted that for the ordinary skill people of the art
For member, under the premise of not departing from the application principle, several improvements and modifications can also be made, these improvements and modifications are also answered
It is considered as the protection scope of the application.
Claims (6)
1. the transmission electron microscope imaging method that one kind can distinguish different type dislocation characterized by comprising
Under common transmission electron microscope mode, vert sample, makes electron beam along the incidence of the first crystal zone axis, shoots the diffraction spectra of sample,
And carry out first time calibration；
The sample that verts is demarcated according to the first time, sample is made to be in the two-beam diffraction state of the first diffraction vector；
Electronic Speculum is switched into dark-field imaging mode, the diffraction contrast of the first diffraction vector diffracted beam is collected using detector
Image；
Vert sample, makes electron beam along the incidence of the second crystal zone axis, shoots the diffraction spectra of sample, and carries out second and demarcate, described
First crystal zone axis is different from second crystal zone axis；
The sample that verts is demarcated according to described second, the two-beam for making the dislocation region to be seen of sample be in the second diffraction vector spreads out
Penetrate state；
Electronic Speculum is switched into dark-field imaging mode, the diffraction contrast of the second diffraction vector diffracted beam is collected using detector
Image；
The sample that verts is demarcated according to described second, sample is made to be in the two-beam diffraction state of third diffraction vector；
Electronic Speculum is switched into dark-field imaging mode, the diffraction contrast of the third diffraction vector diffracted beam is collected using detector
Image.
2. the transmission electron microscope imaging method according to claim 1 for distinguishing different type dislocation, which is characterized in that described
Sample is the group III-nitride of hexagonal structure.
3. the transmission electron microscope imaging method according to claim 2 for distinguishing different type dislocation, which is characterized in that described
First crystal zone axis is [11-20] crystal orientation.
4. the transmission electron microscope imaging method according to claim 3 for distinguishing different type dislocation, which is characterized in that described
Second crystal zone axis is [- 5,10, -5,3] crystal orientation.
5. the transmission electron microscope imaging method according to claim 1 to 4 for distinguishing different type dislocation, feature exist
In first diffraction vector corresponds to g=10-10.
6. the transmission electron microscope imaging method according to claim 5 for distinguishing different type dislocation, which is characterized in that described
Second diffraction vector, third diffraction vector respectively correspond as g=1-105 and g=0-115.
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Cited By (5)
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| CN110986802A (en) * | 2019-12-14 | 2020-04-10 | 燕山大学 | Method for measuring thickness of transmission electron microscope sample |
| CN111982945A (en) * | 2019-05-24 | 2020-11-24 | 北京纳米能源与系统研究所 | Method for acquiring time-resolved dark field image based on ultrafast transmission electron microscope system and application |
| CN112505071A (en) * | 2020-12-29 | 2021-03-16 | 重庆大学 | Dislocation three-dimensional quantitative characterization method and system based on transmission electron microscope |
| CN116577340A (en) * | 2023-05-28 | 2023-08-11 | 兰州大学 | Method for distinguishing threading screw dislocation and threading edge dislocation in silicon carbide |
| CN118112027A (en) * | 2024-04-30 | 2024-05-31 | 中国科学院苏州纳米技术与纳米仿生研究所 | Electron back scattering diffraction imaging characterization method of crystal defect |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111982945A (en) * | 2019-05-24 | 2020-11-24 | 北京纳米能源与系统研究所 | Method for acquiring time-resolved dark field image based on ultrafast transmission electron microscope system and application |
| CN111982945B (en) * | 2019-05-24 | 2023-04-28 | 北京纳米能源与系统研究所 | Method for acquiring time resolution dark field image based on ultra-fast transmission electron microscope system and application |
| CN110986802A (en) * | 2019-12-14 | 2020-04-10 | 燕山大学 | Method for measuring thickness of transmission electron microscope sample |
| CN112505071A (en) * | 2020-12-29 | 2021-03-16 | 重庆大学 | Dislocation three-dimensional quantitative characterization method and system based on transmission electron microscope |
| CN112505071B (en) * | 2020-12-29 | 2024-04-16 | 重庆大学 | Dislocation three-dimensional quantitative characterization method and system based on transmission electron microscope |
| CN116577340A (en) * | 2023-05-28 | 2023-08-11 | 兰州大学 | Method for distinguishing threading screw dislocation and threading edge dislocation in silicon carbide |
| CN116577340B (en) * | 2023-05-28 | 2024-01-05 | 兰州大学 | Method for distinguishing threading screw dislocation and threading edge dislocation in silicon carbide |
| CN118112027A (en) * | 2024-04-30 | 2024-05-31 | 中国科学院苏州纳米技术与纳米仿生研究所 | Electron back scattering diffraction imaging characterization method of crystal defect |
| CN118112027B (en) * | 2024-04-30 | 2024-06-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Electron back scattering diffraction imaging characterization method of crystal defect |
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Application publication date: 20190416 |