CN110904479B - Gradient multistage nanometer twin crystal structure and preparation method thereof - Google Patents
Gradient multistage nanometer twin crystal structure and preparation method thereof Download PDFInfo
- Publication number
- CN110904479B CN110904479B CN201911236984.2A CN201911236984A CN110904479B CN 110904479 B CN110904479 B CN 110904479B CN 201911236984 A CN201911236984 A CN 201911236984A CN 110904479 B CN110904479 B CN 110904479B
- Authority
- CN
- China
- Prior art keywords
- gradient
- twin crystal
- twin
- nanometer
- directions
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Automation & Control Theory (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention relates to a gradient multistage nanometer twin crystal structure and a preparation method thereof, belonging to the technical field of nanometer structure metal material engineering. The gradient multistage nanometer twin crystal structure comprises a gradient nanometer structure in the direction vertical to the surface of the material and multistage nanometer twin crystal structures in different directions in the gradient nanometer structure, and the multistage nanometer twin crystal structure with crystal orientation grows in the gradient nanometer structure in multiple directions. The preparation method comprises the following steps: in the process of preparing the gradient nano structure by adopting an electroplating deposition technology, an external electric field is introduced to change and guide the direction of material deposition, so that gradient multistage nano twin crystal structures with different positions formed in multiple directions are obtained. The invention is characterized in that the gradient multistage nanometer twin crystal structure is prepared by innovatively designing on the basis of preparing the gradient nanometer structure by the traditional electroplating deposition technology and adding an external electric field, the mechanical properties of the material in the aspects of strength, hardness and the like are effectively improved by the structure, and the plasticity of the material is effectively guaranteed.
Description
Technical Field
The invention relates to the technical field of nano-structure metal material engineering, in particular to a gradient multistage nano twin crystal structure and a preparation method thereof.
Background
The strength and toughness of materials in the field of scientific and technological engineering are always main factors for further improving the modernization efficiency of national economy, for example, an aerospace engine which is in service under extremely severe conditions has the service life and the safety factor which are mainly determined by the strength and the toughness of the engine.
In recent decades, materials scientists have continually sought and studied ways and methods to improve the mechanical properties of materials. Theoretical studies and analysis indicate that a perfect crystal structure material has very high theoretical strength, but the actual material strength is far lower than the strength. The microstructure characterization of the material finds that various defects (dislocations, twin crystals, grain boundaries and the like) exist in the material, and the distribution of the defects and the movement under the loading condition enable the strength of the material to be far lower than the theoretical strength.
According to the traditional Hall-Petch relationship, the strength of the material is closely related to the grain size. The material strength shows positive correlation improvement along with the reduction of the grain size, which is due to the fact that the proportion of defects such as grain boundaries and the like is improved due to the reduction of the grain size, the blocking effect on dislocation is enhanced, and the material strength is improved, namely fine grain strengthening is realized. In this case, the state and motion of dislocations dominate the strengthening of the material. According to the theory, people continuously change the distribution state of the microstructure and the defects in the material, and improve the mechanical property of the toughness of the material. According to different theories, the strength of the material is continuously improved in different ways, but the improvement of the strength of the material is accompanied by the obvious reduction of plasticity, so that the application range of the material is greatly limited. Especially, when the grain size is reduced to 20-30 nm, the material strength deviates from the Hall-Petch relation, and a softening phenomenon, namely an abnormal Hall-Petch effect, occurs. In the size range, the material has the phenomena of grain boundary migration, grain rotation, even grain growth and the like under the loading condition, the movement of the grain boundary occupies a dominant position, and the strengthening can not be effectively realized. Therefore, the improvement of the comprehensive mechanical properties of the material needs further exploration.
In recent years, the gradient nano structure and the nano twin structure attract people to pay attention due to the remarkable improvement of the toughness of the material. In the gradient nano structure, nano crystal grains and coarse crystal grains with different sizes are distributed in sequence from the surface to the inside, the nano crystal mainly causes dislocation product, stress concentration at the crystal grains is caused to a certain degree, and simultaneously the nano crystal is effectively regulated by the coarse crystal grains in the inside, so that the comprehensive toughness of the material can be improved finally, but the plasticity is reduced to some extent. In the nanometer twin crystal structure, the twin crystal has the same function of blocking dislocation movement with the grain boundary to improve the material strength, and the atoms on the twin crystal interface are regularly arranged, and the slip, movement and annihilation of the dislocation at the position form interaction with the twin grain boundary. If the gradient nano structure is combined with the nano twin structure, the advantages can be complemented, so that the material shows more excellent performance, and the preparation of the gradient nano twin structure is gradually an attention object.
A gradient nanometer twin crystal structure is prepared by utilizing a direct current electrolytic deposition technology and taking a pure copper material as a research object. The strength of the gradient nanometer twin crystal and the work hardening rate are synchronously improved along with the increase of the structural gradient, and when the structural gradient is large enough, the strength of the gradient material even exceeds the strongest part in the gradient microstructure. Experimental characterization and theoretical simulation analysis show that the improvement of the structural performance is due to a large number of geometrically essential dislocation-rich bundles generated by the constraint of the gradient structure, which are formed in the early stage of deformation and are uniformly distributed in the interior of the crystal grains along the gradient direction. Different from a randomly distributed statistical storage dislocation structure in a uniform structure material, the dislocation rich cluster with ultrahigh dislocation density effectively inhibits the grain boundary strain localization by blocking dislocation motion in the process of dislocation rich cluster deformation, thereby improving the strength and the work hardening of a gradient nanometer twin crystal structure. However, only a twin crystal structure growing in a single direction is researched in the structure, and the improvement space is provided for the strength and plasticity improvement effect of the material.
Disclosure of Invention
The invention aims to provide a gradient multistage nanometer twin crystal structure and a preparation method thereof.
In order to solve the above problems, the present invention provides the following technical solutions:
a gradient multistage nanometer twin crystal structure comprises a gradient nanometer structure in the direction vertical to the surface of a material and multistage nanometer twin crystal structures in different directions in the gradient nanometer structure;
the gradient nano structure is characterized in that the size and the distribution of the grain size show continuous gradient change from large to small or from small to large in the direction vertical to the surface of the material;
twin crystals in the multistage nanometer twin crystal structure have four direction types, which are respectively one direction, two directions, three directions and four directions, and when the twin crystals have 2 or more directions, the optical orientation angles of the twin crystals in the adjacent directions are all 70 degrees;
wherein, when the twin crystal is in one direction, it can be called a first-order twin crystal; when the twin crystal is in two directions, the twin crystal in different directions can be respectively called a first-stage twin crystal and a second-stage twin crystal; when the twin crystal is in three directions, the twin crystal in different directions can be respectively called a first-stage twin crystal, a second-stage twin crystal and a third-stage twin crystal which are adjacent in sequence; when the twin crystal is in four directions, the twin crystal in different directions can be respectively called a first-stage twin crystal, a second-stage twin crystal, a third-stage twin crystal and a fourth-stage twin crystal which are adjacent in sequence.
According to the scheme, the variation range of the grain size is 50-2 mu m.
The preparation method of the gradient multistage nanometer twin crystal structure is provided, and in the process of preparing the gradient nanometer structure by adopting an electroplating deposition technology, the direction of material deposition is changed and guided by introducing an external electric field, so that the gradient multistage nanometer twin crystal structure with different positions formed in multiple directions is obtained.
According to the scheme, the method comprises the following specific steps:
1) placing the cathode and anode electrode plates in electrolyte to build an electrolysis experiment platform;
2) 5 micro electrodes are independently placed in the electrolyte, evenly distributed in a horizontal 360-degree range around the positive and negative electrode plates and used for introducing an external electric field;
3) the gradient multistage nanometer twin crystal structure is obtained by electroplating deposition by controlling the gradient change of the temperature of the electrolyte along with time and introducing an external electric field.
According to the scheme, the current density of the external electric field is 30-60 mA/cm2。
According to the scheme, the micro electrode in the step 2) adopts an atomic force microscope probe.
According to the scheme, the distance between the tip of the microelectrode probe and the center of the electrode plate in the horizontal direction is controlled to be 2.5-3.5 mm, and the distance between the tip of the microelectrode probe and the cathode plate and the distance between the tip of the microelectrode probe and the anode plate in the vertical direction are controlled to be equal.
According to the scheme, the micro electrode is precisely moved in the step 2) through the high-precision three-dimensional moving platform.
According to the scheme, the step of controlling the temperature of the electrolyte to change along with the time gradient in the step 3) refers to controlling the temperature of the electrolyte to increase or decrease along with the time gradient within the range of 20-50 ℃, and the total deposition time is 15-25 hours.
According to the scheme, the anode and cathode electrode plates required by electroplating deposition in the step 1) are vertically and symmetrically distributed in the electrolyte, the anode plate is arranged above the cathode plate, the distance is 10-15 mm, the anode plate is made of graphite, the cathode plate is made of pure copper, and the area ratio of the anode and cathode electrode plates is 0.5-2; the concentration of the electrolyte is 140-160 g/L, and the pH is 1.5-2.5.
According to the scheme, the cathode and anode electrode plates in the step 1) are circular, and the diameter of the cathode and anode electrode plates is 10-20 mm.
For a Face Centered Cubic (FCC) crystal with a plurality of sliding systems, the twin crystal orientation is rich, the twin crystals distributed in different directions and twin crystal boundaries have far-reaching influence on dislocation movement, and the twin crystals with different crystal orientation in a multistage nanometer twin crystal structure (the parts in the crystal grains are different twin crystals) enable the interaction between the twin crystals and the twin crystals, and between the twin crystals and the dislocations to be rich. The processes of dislocation formation, blockage, slippage and the like enable stress distribution under the loading condition to be more uniform, so that the strength and plasticity of the material are greatly improved.
The invention has the beneficial effects that:
according to the invention, innovative design is carried out on the basis of preparing a gradient nano structure by a traditional electroplating deposition technology, an external electric field is added, the movement of metal cations in an electrolyte is guided by applying the external electric field, multi-stage nano twin crystal structures with crystal orientation are grown in the gradient nano structure in different directions, and finally the gradient multi-stage nano twin crystal structure is prepared in a material.
Drawings
FIG. 1 is a schematic diagram of the grain structure of 4 different regions in the gradient nanostructure according to the embodiment of the present invention.
FIG. 2 is a schematic diagram of an applied electric field introduced in an electrolysis experiment platform according to an embodiment of the present invention.
FIG. 3 is a schematic diagram of the mutual angles between different twin directions in the embodiment of the present invention.
FIG. 4 is a typical electron microscope image of a region having 1 twin direction in example 1 of the present invention.
FIG. 5 is a typical electron microscope image of the region having 2 twin directions in example 1 of the present invention.
FIG. 6 is a typical electron microscope image of the region having 3 twin directions in example 1 of the present invention.
FIG. 7 is a typical electron microscope photograph of a region having 4 twin directions in example 1 of the present invention.
FIG. 8 is a comparative graph of strength and mechanical properties of copper materials with gradient multistage nanometer twin crystal structures and other structures in the embodiment of the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
Example 1
Taking Cu as an example, the preparation method of the gradient multistage nanometer twin crystal structure specifically comprises the following steps:
1. the growth of the copper metal material gradient nanostructure is realized by adopting an electroplating deposition technology.
An electrolysis experiment platform for growing a copper gradient nanostructure is built, and the electrolysis experiment platform mainly comprises a positive and negative electrode plate, electrolyte, an LDX-K30010 adjustable direct current stabilized power supply and an AIJ high-precision temperature controller.
Wherein, electrolysis experiment platform's negative and positive electrode piece longitudinal symmetry distributes in electrolyte, and the positive pole piece is last, and the negative pole piece is under, apart from 10mm, and the positive pole piece adopts graphite preparation, and the negative pole piece adopts pure copper material (99.99%, mass fraction) as base member deposit growth copper material, and in order to receive the electricity evenly simultaneously, make electrode piece overall dimension circular, diameter 10mm, the area ratio of negative and positive electrode piece is 1: 1.
the electrolyte is prepared from high-purity deionized water and CuSO4Is used as main component (concentration is 150g/L) and concentrated H is used2SO4The pH of the electrolyte was adjusted to 2 and the volume was 1L.
For Cu by electroplating deposition technique2+The oxidation-reduction reaction of (2) realizes the generation of copper, and the current density is set to be 30mA/cm by a direct current stabilized power supply2Controlling the reaction temperature to be increased in a gradient manner within the range of 20-50 ℃ by a temperature controllerThe initial temperature is 20 ℃, the temperature is increased by 10 ℃ every 5 hours, the total deposition time is 20 hours, the experimental environment temperature is about 293K, and finally the gradient nano structure is formed under control.
Since the material grows from the bottom to the top, the gradient change of the size and the distribution of the grain size and the twin lamella thickness is larger along with the rise of the temperature, so that the average grain size shows continuous gradient change from large to small (the grain size is 29.8-2.3 μm, the twin lamella thickness is 2nm-800nm) in the direction vertical to the surface of the material from top to bottom, and the regions with the same thickness in 4 groups are respectively cut in the direction for comparison, as shown in fig. 1, each layer has a thickness of about 30 μm, and the average grain size of the regions from top to bottom in 4 groups is respectively about: 21.2 μm, 10.7 μm, 5.8 μm, 3.5. mu.m.
2. The improvement is carried out on the basis of the traditional electroplating device, and an external electric field is introduced in the electroplating process to guide Cu2+The material in the same gradient grows along different crystallographic directions, and the growth of the gradient multistage nanometer twin crystal structure material is realized, wherein:
the current density of the external electric field is 60mA/cm2。
The external electric field is 5 micro electrodes independently placed in the electrolyte, the micro electrodes are atomic force microscope probes, the distribution of the electric field is shown in figure 2a, the micro electrodes are accurately moved in position through a high-precision three-dimensional moving platform, so that the micro electrodes are evenly distributed around the positive electrode plate and the negative electrode plate within 360 degrees horizontally, the distance between the needle point of the probe and the center of the electrode plate in the horizontal direction is controlled to be 3mm, and the distance between the needle point of the probe and the center of the electrode plate in the vertical direction is 5mm from the cathode plate and the anode plate, as shown in figure 2b, so that the purpose of applying and influencing the electric field in different directions is achieved according to the distribution of twin crystal positions in crystallography in the direction.
Different twin crystal structures are distributed in different directions in the gradient nano structure, the obtained twin crystal has four direction types, namely one direction, two directions, three directions and four directions, and when the twin crystal has more than 2 directions, the optical orientation angles of the twin crystal in adjacent directions are all 70 degrees, as shown in figure 3. Wherein, when the twin crystal is in one direction, the twin crystal is a first-level twin crystal; when the twin crystal is in two directions, the twin crystal in different directions is a first-stage twin crystal and a second-stage twin crystal respectively; when the twin crystal is in three directions, the twin crystal in different directions is a first-stage twin crystal, a second-stage twin crystal and a third-stage twin crystal which are adjacent in sequence; when the twin crystal is in four directions, the twin crystal in different directions is respectively a first-stage twin crystal, a second-stage twin crystal, a third-stage twin crystal and a fourth-stage twin crystal which are adjacent in sequence.
3. And (3) performing microstructure and appearance characterization, and tensile and compressive mechanical tests on the prepared sample.
The sample was processed into a standard dog-bone shape by means of wire cutting with a cutter.
The microstructure and morphology characterization of the sample is carried out under a scanning electron microscope and an in-situ transmission electron microscope, and as the pure copper metal material has lower stacking fault energy and the energy required by the growth condition of the twin crystal is relatively less, the structural morphology of the multistage twin crystal can be observed when the sample is observed under a high-power scanning electron microscope, namely clear strip included angles in a plurality of directions, and typical electron microscope pictures with one direction, two directions, three directions and four directions of the twin crystal are respectively shown in figures 4-7.
In-situ scanning and transmission technology is utilized to carry out tensile and compression mechanical strength performance test under in-situ conditions, Deben Microtest and Hystron PI-85 type nano-indentors are adopted as in-situ mechanical test equipment and are respectively integrated in a scanning electron microscope, in the process of performance test, firstly observation is carried out under low power condition, then real-time dynamic observation and analysis are carried out under high resolution state, finally, the strength mechanical performance test curve 3 of the prepared copper material with gradient multistage nano-twin structure is measured, and simultaneously, compared with annealed copper 1, copper 2 containing gradient nano-structure, copper 4 containing multistage nano-twin structure, copper 5 containing gradient (one-stage) nano-twin structure and copper 6 in polycrystalline state, as shown in figure 8, the state copper 6 has the highest polycrystalline strength but the worst plasticity, the plasticity of the copper 4 containing multistage nano-twin structure improves the plasticity while ensuring the high strength, but still worse, the annealed copper 1 and the copper 2 containing the gradient nano structure have good plasticity, but the strength also has a promotion space, the strength and the plasticity of the gradient (primary) nano twin structure copper 5 formed after the twin structure is introduced into the gradient structure are balanced, and the comprehensive performance of the mechanical strength and the plasticity of the further gradient multi-stage nano twin structure copper 3 is best.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (6)
1. A method for preparing a gradient multistage nanometer twin crystal structure is characterized in that in the process of preparing the gradient nanometer structure by adopting an electroplating deposition technology, an external electric field is introduced to change and guide the direction of material deposition, so that gradient multistage nanometer twin crystal structures with different positions formed in multiple directions are obtained; the method comprises the following specific steps:
1) placing the cathode and anode electrode plates in electrolyte to build an electrolysis experiment platform;
2) independently placing 5 tiny electrodes in the electrolyte, and evenly distributing the tiny electrodes around the cathode and anode electrode plates within 360 degrees of the horizontal direction for introducing an external electric field, wherein: the microelectrode adopts an atomic force microscope probe, the distance between the tip of the microelectrode probe and the center of the electrode slice in the horizontal direction is controlled to be 2.5-3.5 mm, and the microelectrode is equidistant from the cathode slice and the anode slice in the vertical direction;
3) the gradient multistage nanometer twin crystal structure is obtained by controlling the temperature of the electrolyte to change along with time gradient and introducing an external electric field for electroplating deposition, wherein the current density of the external electric field is 30-60 mA/cm2The current density of the electroplating deposition is 30mA/cm2。
2. The method according to claim 1, wherein the controlling of the temperature gradient of the electrolyte in step 3) is controlling of the temperature gradient of the electrolyte to increase or decrease in the range of 20 to 50 ℃ in time gradient, and the total deposition time is 15 to 25 hours.
3. The preparation method according to claim 1, wherein the cathode and anode electrode sheets required for electroplating deposition in the step 1) are vertically and symmetrically distributed in the electrolyte, the anode sheet is arranged above the cathode sheet, and the distance between the anode sheet and the cathode sheet is 10-15 mm; the anode sheet is made of graphite, the cathode sheet is made of pure copper, and the area ratio of the anode sheet to the cathode sheet is 0.5-2; the concentration of the electrolyte is 140-160 g/L, and the pH is 1.5-2.5.
4. The preparation method according to claim 1, wherein the cathode and anode electrode plates in the step 1) are circular and have a diameter of 10-20 mm.
5. The production method according to claim 1, wherein the gradient multistage nano-twin structure includes a gradient nano-structure in a direction perpendicular to a surface of the material and a multistage nano-twin structure in different directions within the gradient nano-structure, wherein:
the gradient nano structure is characterized in that the size and the distribution of the grain size show continuous gradient change from large to small or from small to large in the direction vertical to the surface of the material;
twin crystals in the multistage nanometer twin crystal structure have four direction types, which are respectively one direction, two directions, three directions and four directions, and when the twin crystals have more than 2 directions, the crystal orientation angles of the twin crystals in adjacent directions are all 70 degrees.
6. The method according to claim 5, wherein the variation of the grain size is 50 to 2 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911236984.2A CN110904479B (en) | 2019-12-05 | 2019-12-05 | Gradient multistage nanometer twin crystal structure and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911236984.2A CN110904479B (en) | 2019-12-05 | 2019-12-05 | Gradient multistage nanometer twin crystal structure and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110904479A CN110904479A (en) | 2020-03-24 |
| CN110904479B true CN110904479B (en) | 2021-08-10 |
Family
ID=69823142
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911236984.2A Active CN110904479B (en) | 2019-12-05 | 2019-12-05 | Gradient multistage nanometer twin crystal structure and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110904479B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112522784B (en) * | 2020-11-10 | 2022-05-06 | 中国科学院金属研究所 | Metal material with crystal space structure stable under high-temperature condition |
| CN112620927B (en) * | 2020-12-09 | 2022-03-22 | 北京理工大学 | Method for preparing twin crystal quantum dots by electric field assisted femtosecond laser shaping pulse |
| CN113621999B (en) * | 2021-05-08 | 2023-03-24 | 中国科学院金属研究所 | High-extensibility electrolytic copper foil and preparation method thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109136987B (en) * | 2017-06-19 | 2020-05-05 | 中国科学院金属研究所 | Gradient nano twin crystal copper block material and temperature control preparation method thereof |
| CN108362959A (en) * | 2018-01-05 | 2018-08-03 | 中山大学 | A kind of detecting system and method detecting film memristor characteristic using conducting atomic force microscopy device |
| CN108677213B (en) * | 2018-05-31 | 2021-01-12 | 中国科学院金属研究所 | Method for improving mechanical property of material by changing gradient nanometer twin crystal structure of metal material |
| CN108913854B (en) * | 2018-09-06 | 2020-08-14 | 中国科学院金属研究所 | Gradient nanostructure with excellent comprehensive high-cycle and low-cycle fatigue performance |
| CN110408976B (en) * | 2019-08-09 | 2021-05-25 | 常州大学 | Graphene/nano twin crystal composite material with controllable tissue and preparation method thereof |
-
2019
- 2019-12-05 CN CN201911236984.2A patent/CN110904479B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN110904479A (en) | 2020-03-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110904479B (en) | Gradient multistage nanometer twin crystal structure and preparation method thereof | |
| Li et al. | Nano-scale twinned Cu with ultrahigh strength prepared by direct current electrodeposition | |
| CN110592621B (en) | Method for preparing nano twin copper layer by adopting high-frequency pulse | |
| CN104928649A (en) | Local-area carbon supply device and method for manufacturing wafer-level graphene monocrystalline based on local-area carbon supply | |
| CN115058667B (en) | Preparation method of nano twin crystal high-entropy alloy with low temperature and high strength and toughness | |
| Shen et al. | The mechanical behavior of a layered nanostructured Ni with an alternating growth of ultrafine grains and nano-sized grains fabricated by electrodeposition | |
| CN112195366B (en) | High-thermal-stability equiaxial nanocrystalline Ti-Zr-Ag alloy and preparation method thereof | |
| CN112342433B (en) | High-thermal-stability equiaxial nanocrystalline Ti-Zr-W alloy and preparation method thereof | |
| CN112063892B (en) | High-thermal-stability equiaxial nanocrystalline Ti-Zr-Mn alloy and preparation method thereof | |
| CN112342431B (en) | High-thermal-stability equiaxial nanocrystalline Ti6Al4V-Cu alloy and preparation method thereof | |
| CN112063889B (en) | High-thermal-stability equiaxed nanocrystalline Ti6Al4V-Cr alloy and preparation method thereof | |
| CN112251640A (en) | Nanocrystalline Ti6Al4V-Ag alloy and additive manufacturing and preparing method thereof | |
| CN112342435B (en) | High-thermal-stability equiaxial nanocrystalline Ti-Zr-Ni alloy and preparation method thereof | |
| CN114606465B (en) | Method for preparing cutting line and cutting line | |
| CN112251645B (en) | High-thermal-stability equiaxial nanocrystalline Ti-Co alloy and preparation method thereof | |
| CN112195368B (en) | High-thermal-stability equiaxial nanocrystalline Ti-Ni alloy and preparation method thereof | |
| CN112251637B (en) | High-thermal-stability equiaxial nanocrystalline Ti-Fe alloy and preparation method thereof | |
| CN112342432B (en) | High-thermal-stability equiaxial nanocrystalline Ti-W alloy and preparation method thereof | |
| CN112195365B (en) | High-thermal-stability equiaxial nanocrystalline Ti-Zr-Fe alloy and preparation method thereof | |
| CN112063891B (en) | High-thermal-stability equiaxial nanocrystalline Ti-Zr-Cr alloy and preparation method thereof | |
| CN112251638B (en) | High-thermal-stability equiaxial nanocrystalline Ti-Cu alloy and preparation method thereof | |
| CN112143937B (en) | High-thermal-stability equiaxial nanocrystalline Ti-Zr-Co alloy and preparation method thereof | |
| CN112251635B (en) | High-thermal-stability equiaxed nanocrystalline Ti6Al4V-Ni alloy and preparation method thereof | |
| CN112063890B (en) | High-thermal-stability equiaxial nanocrystalline Ti-Ag alloy and preparation method thereof | |
| CN112251644B (en) | High-thermal-stability equiaxial nanocrystalline Ti6Al4V-Ag alloy and preparation method thereof |
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 |