CN107271461B - A method of obtaining annular dark field image under transmission electron microscope - Google Patents
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Abstract
A method of it obtaining annular dark field image under transmission electron microscope, comprises the steps of: the region chosen need to shoot image first, acquire polycrystalline electron diffraction ring；Then the diffraction ring for needing to obtain annular dark field image is chosen, carries out continuous darkfield image acquisition on the semi-ring of this diffraction ring using objective lens of the transmission electron microscope diaphragm；All darkfield images collected are added on a picture using software finally and obtain annular dark field image.This method has the advantages that easy to operate, at low cost and easy to accomplish.
Description
Technical field
The present invention relates to a kind of material microcosmic detection methods, and the side of image is obtained especially under transmission electron microscope
Method.
Background technique
Transmission electron microscope is widely used in the research of material science as a kind of material micro-analysis means,
Advantage are as follows: carry out electronic diffraction object while microstructure observing can be carried out and mutually demarcate.It is microcosmic under transmission electron microscope
Structure observation is divided into bright field image and dark field image: bright field image is the picture for selecting transmitted beam to be formed, and brightness of image is high, contrast is good；Dark field
As the picture to select diffracted beam to be formed, although brightness and contrast have in terms of observation crystal and defect not as good as bright field image
Advantage.
Dark field image obtains extensively, at present in terms of detection the defects of crystalline material and crystal (dislocation, fault, twin)
Many dark field methods have been developed: (1) common dark field image technology: one diffracted beam of selection forms dark field image, is mainly used for low
The second phase in observation crystal particular crystal plane and material again；(2) dual beam technique to be verted based on sample is mainly used for obtaining high lining
Spend darkfield image；(3) the center dark field method based on deflection of a beam of electrons is mainly used for shooting the crystal defect picture of high quality；
(4) there are also the development along with scanning transmission electron microscope (STEM), and produce the ring under scanning transmission electron microscope
Shape dark field method-angle of elevation annular dark (HAADF) and low angle annular dark (LAADF): angle of elevation annular dark has title Z
Contrast image is for observing the defects of material, composition information and the full resolution pricture for reaching atom definition；Low square ring shape
Dark field image acquires low angle elastic scattering electrons, can obtain under scanning transmission electron microscope under similar transmission electron microscope
Darkfield image.
As the development of the development of new material technology of preparing, especially nano material is wanted to what the microstructure of material detected
It asks and further increases, such as powder sintered and large plastometric set can prepare the nanometer material that average grain size is less than 20nm
Material, and the transgranular nanocrystalline material containing nano-second-phase can be prepared.Transmission electron microscope bright field image is unable to satisfy this
The microstructure of a little materials characterizes work, needs by dark field image technology, but the imaging of dark field image can only use a branch of diffraction
The disadvantages of beam or a small amount of diffracted beam, obtained image contrast is not high, characterization information is few.On the other hand, although for these green woods
The microstructure characterization of material can use angle of elevation annular dark and low angle annular dark under scanning transmission electron microscope,
But due to scanning transmission electron microscope somewhat expensive, while being also just volume production in recent years, is not each transmitted electron
The function that microscope all has.
Summary of the invention
It does not need to install hardware device additional the purpose of the present invention is to provide one kind, it can be aobvious with common transmitted electron in material
The acquisition annular under transmission electron microscope that the annular dark field image that simple operations can obtain high quality is carried out on micro mirror is dark
The method of field picture.
The present invention is a kind of method that annular dark field image is obtained under transmission electron microscope, is included the following steps:
Step 1) favored area: sample is put under transmission electron microscope, and selection needs to obtain annular dark field image
Region regulates amplification factor, and acquires this region bright field image.
Step 2) acquires polycrystalline diffraction ring: selected to need to obtain ring using the polycrystalline diffraction ring of constituency diaphragm acquisition sample
The diffraction ring of shape darkfield image.
Step 3) acquires darkfield image: amplification factor, object lens electric current must be kept in the collection process of entire darkfield image
Parameter constant.A part is chosen in the diffraction ring that step (2) are selected using lens isis first, acquires darkfield image；Then
A part of diffraction ring is chosen downwards along the diffraction ring that step (2) are selected using lens isis, acquires darkfield image；It continues on and spreads out
Ring selected part diffraction ring down is penetrated, darkfield image is acquired, until total length selected by lens isis is selected greater than step (2)
The half of diffraction ring, darkfield image acquisition are completed.
Step 4) combines image: being superimposed step (3) all dark field pictures collected, generation step using image software
(2) annular dark of selected diffraction ring.
The invention has the following advantages over the prior art:
1, on conventional transmission electron microscope, withouyt high quality is obtained under conditions of annular probe and control software
Annular dark field image.
2, annular dark field contrast obtained is adjustable, can adjust annular dark field contrast with different size of lens isis.
3, operating process is simple and easy.
Detailed description of the invention
Fig. 1 is the schematic diagram that the annular dark field image of the method for the present invention obtains；
Fig. 2 is the crystal bright field image figure of the embodiment of the present invention 1；
Fig. 3 is the polycrystalline diffraction ring figure of the embodiment of the present invention 1；
Fig. 4 is the annular dark field figure of the embodiment of the present invention 1；
Fig. 5 is the crystal bright field image figure of the embodiment of the present invention 2；
Fig. 6 is the polycrystalline diffraction ring figure of the embodiment of the present invention 2；
Fig. 7 is the annular dark field figure of the embodiment of the present invention 2；
Fig. 8 is the crystal bright field image figure of the embodiment of the present invention 3；
Fig. 9 is the polycrystalline diffraction ring figure of the embodiment of the present invention 3；
Figure 10 is the annular dark field figure of the embodiment of the present invention 3；
Figure 11 is the crystal bright field image figure of the embodiment of the present invention 4；
Figure 12 is the polycrystalline diffraction ring figure of the embodiment of the present invention 4；
Figure 13 is the annular dark field figure of the embodiment of the present invention 4.
Specific embodiment
Below with reference to specific example, the present invention will be described in detail.
Embodiment 1
Detect 5083 aluminium alloys that material is powder sintered state.3mm × 5mm × 0.5mm thin slice is intercepted, is ground with waterproof abrasive paper
Mill, thickness reach 30 μm.The double sprays of interception Φ 3mm sample progress, which are thinned, prepares thin area.Utilize double samples that incline of Jem2010 Electronic Speculum
The above-mentioned sample clamping prepared is 200KV using voltage in Electronic Speculum by bar.
Step 1) favored area: by the lookup to the thin area of sample, selection needs detection zone, adjusts amplification factor 25000
Times, this region bright field image is acquired, as shown in Figure 2；
Step 2) acquires polycrystalline diffraction ring: using maximum selection diaphragm in transmission electron microscope to adopting in step (1)
Electronic diffraction is done in collection region, obtains polycrystalline diffraction ring, as shown in Figure 3.Then needs are selected according to polycrystalline diffraction ring collected
The diffraction ring of dark field image is obtained, { 111 } ring is selected herein and acquires dark field image, as shown in Figure 3；
Step 3) acquires darkfield image: using { 111 } of the polycrystalline diffraction ring that the smallest lens isis is acquired in step (2)
Diffracted beam is selected on ring, then position 1 as shown in Figure 1 acquires dark field image 1.Dark field image 1 has been acquired, return step (2) acquisition
Polycrystalline diffraction ring moves lens isis to position 2 clockwise on { 111 } ring, and position 2 as shown in Figure 1 is kept and acquisition dark field
1 identical transmission electron microscope parameter-i.e. amplification factor, acquisition time and object lens electric current acquires dark field 2.It is then returned to step
Suddenly the polycrystalline diffraction ring of (2) acquisition moves lens isis to position 3 clockwise on { 111 } ring, and position 3 as shown in Figure 1 is protected
Transmission electron microscope parameter-i.e. identical with acquisition dark field 1 amplification factor, acquisition time and object lens electric current is held, dark field is acquired
3.Same method successively moves lens isis to next position, acquires corresponding darkfield image, until lens isis is mobile
To position N, as shown in Figure 1, the dark field of i.e. acquired polycrystalline diffraction ring half, this sample N=15, amount to 15 dark field plots of acquisition
Picture.
Step 4) combines image: image processing software ImageJ is used, step (3) 15 darkfield images collected is folded
Add, generates { 111 } annular dark field image, as shown in Figure 4.
Embodiment 2
Detect 5083 aluminium alloys that material is 5Gpa high-pressure sinter state.3mm × 5mm × 0.5mm thin slice is intercepted, water sand is used
Paper grinding, thickness reach 30 μm.The double sprays of interception Φ 3mm sample progress, which are thinned, prepares thin area.Double using Jem2010 Electronic Speculum incline
The above-mentioned sample clamping prepared is 200KV using voltage in Electronic Speculum by specimen holder.
Step 1) favored area: by the lookup to the thin area of sample, selection needs detection zone, adjusts amplification factor 25000
Times, this region bright field image is acquired, as shown in Figure 5；
Step 2) acquires polycrystalline diffraction ring: using maximum selection diaphragm in transmission electron microscope to adopting in step (1)
Electronic diffraction is done in collection region, obtains polycrystalline diffraction ring, as shown in Figure 6.Then needs are selected according to polycrystalline diffraction ring collected
The diffraction ring of dark field image is obtained, { 111 } ring is selected herein and acquires dark field image, as shown in Figure 6；
Step 3) acquires darkfield image: using { 111 } of the polycrystalline diffraction ring that the smallest lens isis is acquired in step (2)
Diffracted beam is selected on ring, then position 1 as shown in Figure 1 acquires dark field image 1.Dark field image 1 has been acquired, return step (2) acquisition
Polycrystalline diffraction ring moves lens isis to position 2 clockwise on { 111 } ring, and position 2 as shown in Figure 1 is kept and acquisition dark field
1 identical transmission electron microscope parameter-i.e. amplification factor, acquisition time and object lens electric current acquires dark field 2.It is then returned to step
Suddenly the polycrystalline diffraction ring of (2) acquisition moves lens isis to position 3 clockwise on { 111 } ring, and position 3 as shown in Figure 1 is protected
Transmission electron microscope parameter-i.e. identical with acquisition dark field 1 amplification factor, acquisition time and object lens electric current is held, dark field is acquired
3.Same method successively moves lens isis to next position, acquires corresponding darkfield image, until lens isis is mobile
To position N, as shown in Figure 1, the dark field of i.e. acquired polycrystalline diffraction ring half, this sample N=14, amount to 14 dark field plots of acquisition
Picture.
Step 4) combines image: image processing software ImageJ is used, step (3) 14 darkfield images collected is folded
Add, generates { 111 } annular dark field image, as shown in Figure 7.
Embodiment 3
Detect 7075 aluminium alloys that material is high-pressure sinter state.3mm × 5mm × 0.5mm thin slice is intercepted, is ground with waterproof abrasive paper
Mill, thickness reach 30 μm.The double sprays of interception Φ 3mm sample progress, which are thinned, prepares thin area.Utilize double samples that incline of Jem2010 Electronic Speculum
The above-mentioned sample clamping prepared is 200KV using voltage in Electronic Speculum by bar.
Step 1) favored area: by the lookup to the thin area of sample, selection needs detection zone, adjusts amplification factor 30000
Times, this region bright field image is acquired, as shown in Figure 8；
Step 2) acquires polycrystalline diffraction ring: using maximum selection diaphragm in transmission electron microscope to adopting in step (1)
Electronic diffraction is done in collection region, obtains polycrystalline diffraction ring, as shown in Figure 9.Then needs are selected according to polycrystalline diffraction ring collected
The diffraction ring of dark field image is obtained, { 111 } ring is selected herein and acquires dark field image, as shown in Figure 9；
Step 3) acquires darkfield image: using { 111 } of the polycrystalline diffraction ring that the smallest lens isis is acquired in step (2)
Diffracted beam is selected on ring, then position 1 as shown in Figure 1 acquires dark field image 1.Dark field image 1 has been acquired, return step (2) acquisition
Polycrystalline diffraction ring moves lens isis to position 2 clockwise on { 111 } ring, and position 2 as shown in Figure 1 is kept and acquisition dark field
1 identical transmission electron microscope parameter-i.e. amplification factor, acquisition time and object lens electric current acquires dark field 2.It is then returned to step
Suddenly the polycrystalline diffraction ring of (2) acquisition moves lens isis to position 3 clockwise on { 111 } ring, and position 3 as shown in Figure 1 is protected
Transmission electron microscope parameter-i.e. identical with acquisition dark field 1 amplification factor, acquisition time and object lens electric current is held, dark field is acquired
3.Same method successively moves lens isis to next position, acquires corresponding darkfield image, until lens isis is mobile
To position N, as shown in Figure 1, the dark field of i.e. acquired polycrystalline diffraction ring half, this sample N=14, amount to 14 dark field plots of acquisition
Picture.
Step 4) combines image: image processing software ImageJ is used, step (3) 14 darkfield images collected is folded
Add, generates { 111 } annular dark field image, as shown in Figure 10.
Embodiment 4
Detect 7050 aluminium alloys that material is high-pressure sinter state.3mm × 5mm × 0.5mm thin slice is intercepted, is ground with waterproof abrasive paper
Mill, thickness reach 30 μm.The double sprays of interception Φ 3mm sample progress, which are thinned, prepares thin area.Utilize double samples that incline of Jem2010 Electronic Speculum
The above-mentioned sample clamping prepared is 200KV using voltage in Electronic Speculum by bar.
Step 1) favored area: by the lookup to the thin area of sample, selection needs detection zone, adjusts amplification factor 30000
Times, this region bright field image is acquired, as shown in figure 11；
Step 2) acquires polycrystalline diffraction ring: using maximum selection diaphragm in transmission electron microscope to adopting in step (1)
Electronic diffraction is done in collection region, obtains polycrystalline diffraction ring, as shown in figure 12.Then needs are selected according to polycrystalline diffraction ring collected
The diffraction ring of dark field image is obtained, { 111 } ring is selected herein and acquires dark field image, as shown in figure 12；
Step 3) acquires darkfield image: using { 111 } of the polycrystalline diffraction ring that the smallest lens isis is acquired in step (2)
Diffracted beam is selected on ring, then position 1 as shown in Figure 1 acquires dark field image 1.Dark field image 1 has been acquired, return step (2) acquisition
Polycrystalline diffraction ring moves lens isis to position 2 clockwise on { 111 } ring, and position 2 as shown in Figure 1 is kept and acquisition dark field
1 identical transmission electron microscope parameter-i.e. amplification factor, acquisition time and object lens electric current acquires dark field 2.It is then returned to step
Suddenly the polycrystalline diffraction ring of (2) acquisition moves lens isis to position 3 clockwise on { 111 } ring, and position 3 as shown in Figure 1 is protected
Transmission electron microscope parameter-i.e. identical with acquisition dark field 1 amplification factor, acquisition time and object lens electric current is held, dark field is acquired
3.Same method successively moves lens isis to next position, acquires corresponding darkfield image, until lens isis is mobile
To position N, as shown in Figure 1, the dark field of i.e. acquired polycrystalline diffraction ring half, this sample N=15, amount to 15 dark field plots of acquisition
Picture.
Step 4) combines image: image processing software ImageJ is used, step (3) 15 darkfield images collected is folded
Add, generates { 111 } annular dark field image, as shown in figure 13.
Claims (1)
1. a kind of method for obtaining annular dark field image under transmission electron microscope, characterized by the following steps:
(1) favored area: sample is put under transmission electron microscope, and selection needs to obtain the region of annular dark field image, is adjusted
Amplification factor has been saved, and has acquired this region bright field image；
(2) polycrystalline diffraction ring is acquired: selected to need to obtain annular dark field figure using the polycrystalline diffraction ring of constituency diaphragm acquisition sample
The diffraction ring of picture；
(3) acquire darkfield image: must be kept in the collection process of entire darkfield image amplification factor, object lens electric current parameter not
Become, choose a part in the diffraction ring that step (2) are selected using lens isis first, acquires darkfield image；Then object is used
Mirror diaphragm chooses downwards a part of diffraction ring along the diffraction ring that step (2) are selected, and acquires darkfield image；It is past to continue on diffraction ring
Lower selected part diffraction ring acquires darkfield image, until total length selected by lens isis, which is greater than step (2), selectes diffraction ring
Half, darkfield image acquisition complete；
(4) it combines image: being superimposed step (3) all dark field pictures collected using image software, what generation step (2) was selected
The annular dark of diffraction ring.
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| 扫描透射电子显微镜及电子能量损失谱的原理及应用;李超 等;《物理》;20141231;第43卷(第9期);第597-605页 |
| 高分辨扫描透射电子显微镜原理及其引用;贾志宏 等;《物理》;20151231;第44卷(第7期);第446-452页 |
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