CN107677694B - Method for in-situ observation of metal martensite phase transformation - Google Patents
Method for in-situ observation of metal martensite phase transformation Download PDFInfo
- Publication number
- CN107677694B CN107677694B CN201710654259.1A CN201710654259A CN107677694B CN 107677694 B CN107677694 B CN 107677694B CN 201710654259 A CN201710654259 A CN 201710654259A CN 107677694 B CN107677694 B CN 107677694B
- Authority
- CN
- China
- Prior art keywords
- sample
- situ
- phase
- tensile
- stretched
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/624—Specific applications or type of materials steel, castings
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The method for observing the low-plasticity high-strength metal martensite phase transformation in situ comprises the steps of mechanically polishing a sample; searching a chrysanthemum pool pattern by using EBSD (electron back scattering device), and etching a marking line along a grain boundary for crystal grains with a [200] channel in the chrysanthemum pool pattern; cutting a tensile sample from the crystal grains within the range of the marking line; preparing a clamping groove on a sample substrate stretched in situ, and extracting and transferring a stretched sample into the clamping groove; punching a hole on the midline of the bone sample in the length direction; gradually thinning the tensile sample; finely adjusting the tilting angle of the sample rod to obtain a [200] normal incidence diffraction pattern, and shooting a high-resolution lattice fringe image; carrying out tensile deformation on the sample substrate, shooting a video of a central dark field image and recording the formation and growth process of an HCP phase; and moving the front edge of the phase interface to the center of the picture, and shooting a video of the lattice fringe image in a high-resolution mode. The invention has the advantage that the body-centered cubic metal phase-change close-packed hexagonal metal can be directly observed under a transmission electron microscope.
Description
Technical Field
The invention relates to a method for in-situ observation of a metal phase change process under a transmission electron microscope.
Background
Phase change refers to the change of a material from one atomic configuration to another atomic configuration, and almost all materials have phase change behavior. There are many classification methods for phase change, and if the phase change process is changed, the phase change process is divided into two categories, namely diffusion phase change and non-diffusion phase change. The phase change often causes the material to show distinct physicochemical properties, and provides wide regulation and control possibility for people to obtain various functions. Taking the famous non-diffusion phase transformation-martensite phase transformation as an example, the common carbon steel is rapidly cooled to the martensite phase transformation temperature from an austenite temperature zone, so that all or part of martensite structures can be obtained, and the carbon steel has extremely high hardness. If the martensitic structure steel is further tempered at medium temperature, carbide precipitated phases are formed in martensite, the martensite is converted into tempered sorbite, and the material has high hardness and good toughness. Therefore, various performance designs of the material can be realized by regulating and controlling the phase change.
The phase change behavior directly determines the structure and the property of a phase change product, so people show great research interest in the phase change process, and hope to understand the phase change mechanism and further refine key factors for controlling the phase change to realize the free phase change design by thoroughly understanding the phase change process. For the diffusion phase change, due to the diffusion process, people can easily track the transformation of each factor in the phase change process, and can easily master the phase change process. For non-diffusion phase transformation, such as the aforementioned martensite phase transformation, the phase transformation process is usually fast (the fastest speed can reach the sound velocity), the overall phase transformation rule is the atom uniform shear, and there is no component change, so that it is relatively difficult to capture the phase transformation process. This is why martensitic transformation has been still widely known for over 120 years since now, 32429.
In the research of the non-diffusion phase transition method, various research means are developed at present. For example, in-situ X-ray diffraction and in-situ neutron diffraction can reveal changes in the crystal structure of the material during phase change, in-situ scanning electron microscopy and optical microscopy can show changes in the morphology of the material during phase change, in-situ electrical resistance or magnetic testing can reflect changes in the physical properties of the material, and the like. The results obtained by the in-situ methods can provide important basis for conjecture of the phase change mechanism, and greatly deepens the understanding of people on the diffusion-free phase change.
However, there is no effective means for revealing how an atom is transformed from a parent phase to a new phase, which is the most core element of a phase transition without diffusion. Transmission electron microscopes, especially high-resolution transmission electron microscopes, can directly observe the atomic arrangement mode and have important advantages in the research of atomic mechanisms without diffusion phase change. However, no mature method is available for realizing in-situ high-resolution observation of the phase transition process.
Disclosure of Invention
The invention aims to provide a method for directly observing body-centered cubic metal phase-change close-packed hexagonal metal under a transmission electron microscope.
The method for in-situ observation of the low-plasticity high-strength metal martensite transformation comprises the following steps:
step 1: carrying out mechanical polishing on the sample, and then carrying out electrolytic polishing to obtain a sample with a smooth surface and no strain layer;
step 2: putting the sample into a Focused Ion Beam (FIB) system equipped with Electron Back Scattering Diffraction (EBSD), obtaining the morphological size and orientation of the surface crystal grains of the sample by using an EBSD test, and finding out the Kikuchi pattern; etching a circle of marking lines on crystal grains with [200] channels in the chrysanthemum pool pattern along a grain boundary by using ion beams;
and step 3: depositing a Pt deposition layer or a W deposition layer with the width of 3-10 microns and the length penetrating through the crystal grains in the direction of a [200] channel in the marking line;
and 4, step 4: cutting a tensile sample from crystal grains within the range of the marking line by utilizing a focused ion beam, wherein the tensile sample is in a bone shape with two large ends and a slender middle part in the overlooking direction, the direction from one large end of the tensile sample to the other large end is taken as the length direction, the outer surface of the tensile sample along the length direction is parallel to the [200] channel, and the two large ends and the middle part of the tensile sample are in right-angle transition respectively;
and 5: preparing a clamping groove on the sample substrate stretched in situ, wherein the shape and the size of the clamping groove enable a tensile sample to be placed in the clamping groove, and the depth of the clamping groove is lower than that of the tensile sample;
step 6: extracting and transferring a tensile sample into a clamping groove, spraying tungsten on the root of the bone sample for solidification, wherein the root refers to a connecting part between a large end and the middle part;
and 7: punching a hole on the midline of the bone sample in the length direction;
and 8: carrying out ion cutting on the middle part of the tensile sample, and gradually thinning the middle part to 50-200 nm in the width direction;
and step 9: loading an in-situ stretched substrate into a stretched sample rod of an in-situ transmission electron microscope, inserting the stretched sample rod into the middle area of a transmission electron microscope observation stretched sample, representing that the initial state is a BCC (Body-centered cubic) structure by matching a central bright field image with a diffraction pattern, finely adjusting the tilting angle of the sample rod to obtain a [200] normal incidence diffraction pattern, and shooting a high-resolution lattice fringe image;
step 10: the method comprises the steps of utilizing the stretching function of an in-situ TEM stretching sample rod to control stretching step length and speed, carrying out stretching deformation on a sample substrate, driving a stretching sample to deform by the sample substrate, observing whether new spots appear in a diffraction pattern to judge whether an HCP (Hexagonal close packing) phase is generated in the stretching process, representing the position and the form of the HCP phase by using a central dark field image, and shooting a video of the central dark field image to record the formation and growth process of the HCP phase;
step 11: moving the front edge of the phase interface to the center of the picture, amplifying the front edge to 40-60 ten thousand times, and shooting a video of the lattice fringe image in a high-resolution mode;
step 12: the process of converting the atomic lattice from BCC arrangement to HCP arrangement was analyzed using the Burgers phase transition mechanism.
Further, in step 7, a hole or holes are punched in the midline.
Further, the orientation of the slot prepared in step 5 is: ion beam grooving is carried out on the sample substrate stretched in situ, the plane dimension of the groove is 1.2 times of the top view dimension of the tensile sample, and the depth of the groove is 0.2 times of the height of the tensile sample.
Further, the thickness of both ends of this tensile sample is 2 ~ 10 microns, and length is 2 ~ 5 microns, and the thickness of middle part is 0.5 ~ 2 microns, and the length of middle part is 2 ~ 5 microns.
According to the invention, the EBSD observation sample finds out the crystal grains with the [200] channel in the Juju chi pattern for marking, and the crystal grains with the [200] channel in the Juju chi pattern are taken as the range for taking the tensile sample, so that the taken tensile sample is ensured to have the crystal grains with the [200] channel certainly. The [200] channel is chosen in the present invention because, according to previous theoretical studies, the most abundant phase transformation processes can be observed along the [200] direction when the metal material with the body-centered cubic structure is subjected to phase transformation. Then, a mark in the [200] channel direction is made in the sampling range, the outer side surface of the tensile sample in the length direction is parallel to the [200] channel direction during sampling, and then the [200] channel direction can be found only along the length direction of the tensile test during later observation. The tensile sample is made to be thick at two ends and thin in the middle, and root reinforcement is performed when the tensile sample is transferred onto a sample substrate, so that the deformation and fracture positions of the tensile sample are ensured to be positioned in the middle during a tensile test. The reason why the middle line of the middle part in the length direction needs to be perforated is that the crack of the low-plasticity high-strength material is very fast to spread when being stretched, and even if the crack is generated, the phase change process of the front edge of the crack is not always observed. The crack propagation energy can be absorbed by punching, so that the crack is temporarily stopped at the hole, and conditions are created for in-situ observation. Meanwhile, the punching is beneficial to locking the crack initiation position, and the problem of extremely small view field caused by too high multiple of the transmission electron microscope is solved.
The invention has the advantages that: 1. the processed tensile specimen inevitably has crystal grains with [200] channels. 2. The [200] channel is parallel to the outer side surface of the tensile sample in the length direction, and the [200] channel is easy to find under an electron microscope. 3. As the sample is ensured to have a [200] channel and to be parallel to the outer side surface of the sample, the [200] band axis incidence can be obtained when the electron microscope is stretched in situ, the lattice fringes of the {110} crystal face with the largest crystal face spacing can be conveniently obtained, and a high-quality and high-resolution picture can be obtained. 4. As the [200] band axis incidence is the core observation direction of the Booth phase change theory, the verification by the Booth phase change theory is very favorable. 5. The crack propagation energy can be absorbed by punching, so that the crack is temporarily stopped at the hole, and conditions are created for in-situ observation. Meanwhile, the punching is beneficial to locking the crack initiation position, and the problem of extremely small view field caused by too high multiple of the transmission electron microscope is solved.
Drawings
FIG. 1 is a photograph of a tensile specimen under a transmission electron microscope.
FIG. 1-1 is a photograph of a tensile specimen with a hole punched in the middle.
FIG. 2 shows the diffraction pattern of BCC incident on the [200] channel band axis.
FIG. 3 is the BCC and HCP mixed diffraction patterns obtained during phase transformation.
FIG. 4 is a dark field image at the beginning of phase transition.
FIG. 5 is a dark field image of the middle phase transition.
Fig. 6 is a starting frame of a lattice fringe image video.
Fig. 7 is frame 90 of the lattice fringe image video.
Detailed Description
The method for in-situ observation of the low-plasticity high-strength metal martensite transformation comprises the following steps:
step 1: and performing mechanical polishing on the sample, and then performing electrolytic polishing to obtain the sample with a smooth surface and no strain layer.
Step 2: putting the sample into a Focused Ion Beam (FIB) system equipped with Electron Back Scattering Diffraction (EBSD), obtaining the morphological size and orientation of the surface crystal grains of the sample by using an EBSD test, and finding out the Kikuchi pattern; etching a circle of marking lines on crystal grains with [200] channels in the chrysanthemum pool pattern along a grain boundary by using ion beams; so that the range of the crystal grains can be identified when the sample is observed by SEM (Scanning electron microscope) and cut by FIB (focused ion beam) later, and the cut position is ensured to be positioned inside the selected crystal grains with [200] channels.
And step 3: depositing a Pt deposition layer or a W deposition layer with the width of 3-10 microns and the length penetrating through the crystal grains in the direction of the [200] channel in the marking line, wherein the Pt deposition layer or the W deposition layer is used as the marking line of the [200] channel; when the FIB cuts out the sample, the sample which is in accordance with the [002] band axis incidence can be ensured to be cut out only along the length direction which is parallel to the deposition layer.
And 4, step 4: cutting a tensile sample from crystal grains within the range of the marking line by utilizing a focused ion beam, wherein the tensile sample is in a bone shape with two large ends and a slender middle part in the overlooking direction, the direction from one large end of the tensile sample to the other large end is taken as the length direction, the outer surface of the tensile sample along the length direction is parallel to the [200] channel, and the two large ends and the middle part of the tensile sample are in right-angle transition respectively; the shape of the tensile sample is shown in figure 1, wherein the surface a is the outer surface of the tensile sample along the length direction, and the surface a is parallel to a [200] channel.
And 5: and preparing a clamping groove on the sample substrate stretched in situ, wherein the shape and the size of the clamping groove enable the tensile sample to be just placed in the clamping groove, and the depth of the clamping groove is lower than that of the tensile sample.
Step 6: and extracting and transferring the tensile sample into a clamping groove, and spraying tungsten on the root of the bone sample for solidification, wherein the root refers to a connecting part between the large end and the middle part.
And 7: the bone specimen is perforated at the midline of the length thereof with one or more holes, 2 holes being perforated at the midline as shown in fig. 1-1. The reason for perforating the middle line in the length direction of the middle part is that the crack of the low-plasticity high-strength material is rapidly propagated during stretching, and even if the crack is generated, the phase change process of the front edge of the crack is not easy to observe. The crack propagation energy can be absorbed by punching, so that the crack is temporarily stopped at the hole, and conditions are created for in-situ observation. Meanwhile, the punching is beneficial to locking the crack initiation position, and the problem of extremely small view field caused by too high multiple of the transmission electron microscope is solved. The phase change process can be observed in a segmented and multiple manner by punching a plurality of holes.
And 8: and carrying out ion cutting on the middle part of the tensile sample, and gradually thinning the middle part to 50-200 nm in the width direction. Preferably stepwise thinning to 100 nm.
And step 9: the in-situ stretched substrate is placed in a stretched sample rod of an in-situ transmission electron microscope, the stretched sample rod is inserted into the middle area of a transmission electron microscope observation stretched sample, a pure BCC structure is represented in the initial state by matching a central bright field image with a diffraction pattern, a [200] normal incidence diffraction pattern is obtained by finely adjusting the tilting angle of the sample rod, and a high-resolution lattice fringe image is shot. FIG. 2 shows the diffraction pattern of BCC incident on the band axis of the [200] channel observed in SEM.
Step 10: controlling the stretching step length and the stretching speed by utilizing the stretching function of an in-situ TEM stretching sample rod, carrying out stretching deformation on a sample substrate, driving a stretching sample to deform by a sample gold plate, observing whether new spots appear in a diffraction pattern to judge whether an HCP (host-control) phase is generated in the stretching process, representing the position and the form of the HCP phase by using a central dark field image, and shooting a video of the central dark field image to record the formation and the growth process of the HCP phase; BCC and HCP mixed diffraction patterns obtained during phase transformation as shown in FIG. 3, dark field image of initial phase transformation as shown in FIG. 4, and white part as new HCP phase; the dark field image in the middle phase transition stage is shown in fig. 5. An increase in the white light fraction, i.e., a growth of HCP phase, is seen in FIG. 5. From fig. 6 and 7, it can be seen that from the start frame to the 90 th frame of the image, the HCP-covered region gradually expands, and the BCC-covered region gradually shrinks.
Step 10: and moving the front edge of the phase interface to the center of the picture, amplifying the front edge to 40-60 ten thousand times, and shooting a video of the lattice fringe image in a high-resolution mode.
Step 11: the process of converting the atomic lattice from BCC arrangement to HCP arrangement was analyzed using the Burgers phase transition mechanism.
The orientation of the slot prepared in the step 5 is as follows: ion beam grooving is carried out on the sample substrate stretched in situ, the plane dimension of the groove is 1.2 times of the top view dimension of the tensile sample, and the depth of the groove is 0.2 times of the height of the tensile sample.
The thickness of both ends of this tensile sample is 2 ~ 10 microns, and length is 2 ~ 5 microns, and the thickness at middle part is 0.5 ~ 2 microns, and the length at middle part is 2 ~ 5 microns.
Claims (5)
1. A method for observing the martensitic transformation of metal in situ, comprising the steps of:
step 1: carrying out mechanical polishing on the sample, and then carrying out electrolytic polishing to obtain a sample with a smooth surface and no strain layer;
step 2: putting the sample into an FIB system assembled with EBSD, obtaining the shape size and orientation of the crystal grains on the surface of the sample by EBSD test, and finding out the Juzu pattern; etching a circle of marking lines on crystal grains with [200] channels in the chrysanthemum pool pattern along a grain boundary by using ion beams;
and step 3: depositing a Pt deposition layer or a W deposition layer with the width of 3-10 microns and the length penetrating through the crystal grains in the direction of a [200] channel in the marking line;
and 4, step 4: cutting a tensile sample from crystal grains within the range of the marking line by utilizing a focused ion beam, wherein the tensile sample is in a bone shape with two large ends and a slender middle part in the overlooking direction, the direction from one large end of the tensile sample to the other large end is taken as the length direction, the outer surface of the tensile sample along the length direction is parallel to the [200] channel, and the two large ends and the middle part of the tensile sample are in right-angle transition respectively;
and 5: preparing a clamping groove on the sample substrate stretched in situ, wherein the shape and the size of the clamping groove enable a tensile sample to be placed in the clamping groove, and the depth of the clamping groove is lower than that of the tensile sample;
step 6: extracting and transferring a tensile sample into a clamping groove, spraying tungsten on the root of the bone sample for solidification, wherein the root refers to a connecting part between a large end and the middle part;
and 7: punching a hole on the midline of the bone sample in the length direction;
and 8: carrying out ion cutting on the middle part of the tensile sample, and gradually thinning the middle part to 50-200 nm in the width direction;
and step 9: loading an in-situ stretched substrate into a stretched sample rod of an in-situ transmission electron microscope, inserting the stretched sample rod into the middle area of a transmission electron microscope observation stretched sample, representing that the initial state is a BCC structure by using a central bright field image and a diffraction pattern, finely adjusting the tilting angle of the sample rod to obtain a [200] normal incidence diffraction pattern, and shooting a high-resolution lattice fringe image;
step 10: controlling the stretching step length and the stretching speed by utilizing the stretching function of an in-situ TEM (transverse electric and magnetic field) stretched sample rod, carrying out stretching deformation on a sample substrate, driving a stretching sample to deform by the sample substrate, observing whether new spots appear in a diffraction pattern to judge whether an HCP (host-P) phase is generated in the stretching process, representing the position and the form of the HCP phase by using a central dark field image, and shooting a video of the central dark field image to record the formation and the growth process of the HCP phase;
step 11: and moving the front edge of the phase interface to the center of the picture, amplifying the front edge to 40-60 ten thousand times, and shooting a video of the lattice fringe image in a high-resolution mode.
2. The method for observing the martensitic phase transformation of metal in situ as claimed in claim 1, wherein: and 9 and 10: the process of converting the atomic lattice from BCC arrangement to HCP arrangement was analyzed using the Burgers phase transition mechanism.
3. The method for observing the martensitic transformation of metal in situ as claimed in claim 1 or 2, wherein: one or more holes are punched in the midline.
4. The method of observing metal martensitic transformation in situ as claimed in claim 3 wherein: ion beam grooving is carried out on the sample substrate stretched in situ, the plane dimension of the groove is 1.2 times of the top view dimension of the tensile sample, and the depth of the groove is 0.2 times of the height of the tensile sample.
5. The method of observing metal martensitic transformation in situ as claimed in claim 4 wherein: the thickness of both ends of this tensile sample is 2 ~ 10 microns, and length is 2 ~ 5 microns, and the thickness at middle part is 0.5 ~ 2 microns, and the length at middle part is 2 ~ 5 microns.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710654259.1A CN107677694B (en) | 2017-08-03 | 2017-08-03 | Method for in-situ observation of metal martensite phase transformation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710654259.1A CN107677694B (en) | 2017-08-03 | 2017-08-03 | Method for in-situ observation of metal martensite phase transformation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107677694A CN107677694A (en) | 2018-02-09 |
| CN107677694B true CN107677694B (en) | 2020-05-19 |
Family
ID=61134460
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710654259.1A Active CN107677694B (en) | 2017-08-03 | 2017-08-03 | Method for in-situ observation of metal martensite phase transformation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107677694B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111999323A (en) * | 2020-08-13 | 2020-11-27 | 中国科学院金属研究所 | In-situ EBSD observation method for microscopic orientation evolution of magnesium alloy recrystallized grains |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108593690B (en) * | 2018-04-19 | 2020-12-15 | 南京腾元软磁有限公司 | Sample surface structure imaging method based on transmission electron microscope |
| WO2020096279A1 (en) * | 2018-11-09 | 2020-05-14 | 주식회사 엘지화학 | Method for quantitatively analyzing crystalline fraction in amorphous oxide semiconductor layer |
| CN110196258A (en) * | 2019-05-07 | 2019-09-03 | 宜特(上海)检测技术有限公司 | The defect image pickup method of planar sample based on TEM diffraction theory |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103954487A (en) * | 2014-04-28 | 2014-07-30 | 浙江大学 | Method for preparing in-situ tensile sample for transmission electron microscope |
| CN105928961A (en) * | 2016-06-13 | 2016-09-07 | 北京工业大学 | In-situ testing sample stage and in-situ testing method |
| CN106198226A (en) * | 2016-09-19 | 2016-12-07 | 中国科学院地质与地球物理研究所 | In conjunction with the method that EBSD technology characterizes crystal grain strain in situ |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8785850B2 (en) * | 2010-01-19 | 2014-07-22 | National Research Counsel Of Canada | Charging of a hole-free thin film phase plate |
-
2017
- 2017-08-03 CN CN201710654259.1A patent/CN107677694B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103954487A (en) * | 2014-04-28 | 2014-07-30 | 浙江大学 | Method for preparing in-situ tensile sample for transmission electron microscope |
| CN105928961A (en) * | 2016-06-13 | 2016-09-07 | 北京工业大学 | In-situ testing sample stage and in-situ testing method |
| CN106198226A (en) * | 2016-09-19 | 2016-12-07 | 中国科学院地质与地球物理研究所 | In conjunction with the method that EBSD technology characterizes crystal grain strain in situ |
Non-Patent Citations (2)
| Title |
|---|
| 体心立方Mo单晶纳米线拉伸塑性变形行为的原位TEM研究;卢艳;<中国优秀硕士学位论文全文数据库>;20141231;第31-38页 * |
| 背散射电子衍射与透射电镜在单晶铝形变组织研究中的应用;黄晓旭等;<电子显微学报>;20020831;第21卷(第4期);第449-454页 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111999323A (en) * | 2020-08-13 | 2020-11-27 | 中国科学院金属研究所 | In-situ EBSD observation method for microscopic orientation evolution of magnesium alloy recrystallized grains |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107677694A (en) | 2018-02-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107677694B (en) | Method for in-situ observation of metal martensite phase transformation | |
| CN107703164B (en) | Method for in-situ observation of body-centered cubic metal phase change into close-packed hexagonal metal by transmission electron microscope | |
| Yang et al. | Evolution of functional properties realized by increasing laser scanning speed for the selective laser melting fabricated NiTi alloy | |
| Zhou et al. | Morphology and microstructure of M 2 C carbide formed at different cooling rates in AISI M2 high speed steel | |
| Liu et al. | Effects of the crystallographic and spatial orientation of α lamellae on the anisotropic in-situ tensile behaviors of additive manufactured Ti–6Al–4V | |
| Matsuda et al. | Multiple-shocks induced nanocrystallization in iron | |
| Gao et al. | Twin boundary-dislocation interactions in nanocrystalline Cu-30% Zn alloys prepared by high pressure torsion | |
| Warren et al. | Method for fabricating depth-specific TEM in situ tensile bars | |
| US8420185B1 (en) | Method for forming metal film with twins | |
| CN108070837A (en) | Metal material and the method for manufacturing metal material | |
| Field et al. | Microstructural development in asymmetric processing of tantalum plate | |
| Li et al. | Micropillar compression investigation on the mechanical behavior of Ni manufactured using laser powder bed fusion | |
| Kim et al. | Effect of initial textures on texture formation in AA 3004 sheets during continuous confined strip shearing and subsequent annealing | |
| Liu | Time-resolved and three-dimensional study of dislocation-particle interactions in aluminum and copper alloys | |
| CN107664593B (en) | A method of preparing transmission electron microscope original position stretching sample | |
| US7374613B2 (en) | Single crystal material having high density dislocations arranged one-dimensionally in straight line form, functional device using said single crystal material, and method for their preparation | |
| Soni et al. | Origins of saccharin-induced stress reduction based on observed fracture behavior of electrodeposited Ni films | |
| Hou | Nanoscale Nickel-Titanium Shape Memory Alloys Thin Films Fabricated by Using Biased Target Ion Beam Deposition | |
| Hu et al. | WITHDRAWN: Application of atom probe tomography in understanding high entropy alloys: 3D local chemical compositions in atomic scale analysis | |
| Suehiro et al. | Change in magnetic property of Cu-6.5 mass% Co alloy through processing by ECAP | |
| Xue | Plasticity of Nanotwinned Aluminum and Aluminum Alloy | |
| Hong et al. | Shear-induced directional grain growth in Ag nanocrystalline films under nanoindentation | |
| Wang et al. | The grain refinement mechanism of electrodeposited copper | |
| Cui | Design of Metallic Nanocomposites for High-Strength, Plasticity and Fracture Resistance | |
| Rifai et al. | Microstructure Quantification and Mechanical Properties of Ultrafine Grained Fe-Cr Alloys and Pure Copper by Equal Channel Angular Pressing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |