CN108914075A - A kind of preparation method based on the base nanometer crystal thin-film material of W containing helium - Google Patents
A kind of preparation method based on the base nanometer crystal thin-film material of W containing helium Download PDFInfo
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- CN108914075A CN108914075A CN201810764894.XA CN201810764894A CN108914075A CN 108914075 A CN108914075 A CN 108914075A CN 201810764894 A CN201810764894 A CN 201810764894A CN 108914075 A CN108914075 A CN 108914075A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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Abstract
The invention discloses a kind of preparation methods of the base nanometer crystal of W containing helium thin-film material, i.e., sputter W base target using the method for magnetron sputtering for the first time in He/Ar mixed atmosphere, deposited, to realize the preparation of the base nanometer crystal thin-film material of W containing helium on substrate.This preparation method can effectively overcome the problems, such as the W matrix body coarse grains of the methods of prior powder metallurgy preparation, realize the preparation with the W based specimen of nanometer scale crystallite dimension, it effectively overcomes caused by increasing when injecting He using accelerator in conventional method due to material surface temperature that temperature is uncontrollable, helium atom the problems such as depth direction is unevenly distributed on the surface of the material, realizes that He atom is uniform in W sill, controllably injects.
Description
Technical field
The present invention relates to a kind of preparation methods of crystal film material of metal-based nano containing helium, especially one kind W containing helium
The preparation method of base nanometer crystal thin-film material.
Background technique
Nuclear energy is considered as that can substitute fossil energy on a large scale at present, meet the ever-increasing electricity needs of people, change
The ideal energy of kind energy consumption structure.It is poly- that nuclear fusion energy mainly utilizes the isotope deuterium of hydrogen and tritium to occur under specific condition
Reaction is closed to release high energy particle（Neutron and helium）Mode obtain energy, i.e.,2D + 3TÒ 4He（3.5 MeV）+
n0（14.1 MeV）.Material in fusion reactor, especially the first wall and Divertor Materials towards plasma, in addition to by
To high-energy neutron irradiation generate serious lattice atoms off normal damage it is outer, during fusion reaction caused by concentration up to 10
The helium of ~ 15 appm He/dpa, which is easy to diffuse to material internal and assembles, forms helium bubble, causes material swelling, blistering, hardening, crisp
Change and the reduction of the performances such as creep and fatigue, i.e. " helium is crisp " phenomenon.
Tungsten due to its high-melting-point, low sputtering raste, good mechanical performance and low tritium be detained the advantages that, have always been considered as be
Main candidate material one of of the following fusion reactor towards plasma facing materials.But during helium irradiation tungsten
The caused crisp problem of helium seems more prominent than other metals.The main reason is that：1) helium atom enters inside across tungsten surface
Potential energy barrier be only 5 eV, the helium for resulting in high-energy irradiation is easily accessible tungsten intracell；2) helium pole after entering tungsten inside
It is easy migration；3) tungsten atom is easy to happen when particle irradiation energy is more than 500 eV offs normal damage phenomenon and generates a large amount of
Vacancy and gap tungsten atom, are more easier to form helium atom-vacancy complex and helium atom cluster than other metals.In addition, receiving
Rice structural material is due to having the higher dislocation density and crystal boundary volume ratio that can become important radiation-induced defect trap,
Through showing excellent anti-radiation performance.Therefore, the forming core that W base nanometer crystal material of the preparation containing helium steeps He in research material is long
Big and evolution process has great importance.
So far, the method that helium atom is introduced into W material is had very much, including ion implanting, tritium decay and neutron
Irradiation etc..For the above method, there are many disadvantages for they.Although although for example, He isotopic geochemistry can introduce it is controllable,
Quantitative helium atom enters sample, but it is difficult to be uniformly distributed helium atom in the material；For the method for tritium decay, although
Helium atom can be equably introduced into material by it, but experimentation needs a very long half-life period (about 12.3 years)；
And neutron irradiation can also cause a series of radiation-induced damages, so that the research experiment about helium behavior in W be made to become complicated.
Magnetron sputtering is a kind of method for commonly preparing film, and this method in vacuum system by leading into a small amount of lazy
Property gas, electric discharge generate inert gas ion bombarding cathode target after cathode bias accelerates, so that target atom is splashed to
Film is eventually formed on substrate.The aluminium containing helium or titanium film of existing preparation, use is all DC magnetron sputtering method.But
Magnetically controlled DC sputtering can only sputter target that can be conductive, not for the W base such as dispersed oxide W and carbide dispersion W target
Magnetically controlled DC sputtering preparation method can be used.
And the range of radio frequency magnetron sputtering method application is more extensive, can sputter most solid-state target.Currently,
The preparation that rf magnetron sputtering is used for W based film material is had not seen in document.
Summary of the invention
That it is an object of the invention to overcome the deficiencies of the prior art and provide a kind of He concentration is adjustable, W crystal particle scale is controllable
The nanocrystalline tungsten based film material containing helium preparation method, on the one hand can effectively overcome conventional method prepare W matrix body crystal grain
Coarse problem, on the other hand can introduce that He concentration is controllable, and helium steeps the equally distributed base nanometer crystal of W containing helium film.
The present invention also provides a kind of preparation methods of the above-mentioned base nanometer crystal of W containing helium thin-film material, include the following steps：
Step 1：Surface treatment polishing is carried out to W base target, surface metal oxide and greasy dirt is removed, obtains target to be sputtered
Material；
Step 2：By single crystal Si substrate, potsherd substrate, quartz substrate or other metal substrates (such as W substrate or Mo substrate
Deng) be cleaned by ultrasonic with alcohol and acetone mixed solution, it is finally rinsed, is dried with deionized water；
Step 3：The W base target of step 1 is installed on the permanent magnetism target of magnetron sputtering, the substrate of step 2 is placed on magnetron sputtering
On substrate inside instrument, it is evacuated to and is passed through He/Ar mixed atmosphere to a certain degree and carries out sputtering sedimentation certain time to get to institute
State the base nanometer crystal thin-film material of W containing helium.
Preferably, the W base target of the step 1 is W target and W alloy target (with a thickness of 0.1mm-5mm).
Preferably, the organic solvent of the step 2 is ethyl alcohol and acetone, and the substrate of the step 2 is single crystalline Si piece, pottery
Ceramic liner bottom, quartz substrate or other metal substrates (W substrate or Mo substrate).
Preferably, the total gas pressure of the He/Ar mixed gas of the step 3 is 0.1Pa-5Pa, and He/Ar air pressure ratio is 0.1-
10, the time of sputtering is 0.5-50h；Film with a thickness of 10nm-100 μm.
Preferably, the preparation method of a kind of base nanometer crystal of W containing helium thin-film material according to claim 1, feature
It is, the method for the preparation is radio-frequency magnetron sputter method, wherein depositing temperature is -600 DEG C of room temperature, must be in He/Ar gaseous mixture
It is carried out under body；Sputtering power is 50-150W.
The present invention is worked by many experiments, and it is thin that the method for rf magnetron sputtering is applied to the base nanometer crystal of W containing helium for the first time
In the preparation of membrane material, the He of uniform concentration can be introduced into W sill, especially suitable for studying W in nuclear fusion reaction
The crisp problem of the He of sill, compared with prior art, specific advantage is as follows：
1. the preparation method of the base nanometer crystal of W containing helium thin-film material disclosed by the invention can prepare crystallite dimension in 100nm or less
The base film of W containing helium, overcome conventional method preparation tungsten matrix body coarse grains the problem of.
2. the preparation method of the base nanometer crystal of W containing helium thin-film material disclosed by the invention, which overcomes, injects He using accelerator
When increased due to material surface temperature caused by temperature is uncontrollable, depth direction is unevenly distributed etc. and to ask helium atom on the surface of the material
Topic, can prepare even concentration containing He, thicker nanocrystalline W base film, be more conducive to helium in analog study tungsten and steep to be formed
Evolutionary process.
3. the preparation method that the present invention discloses W base nanometer crystal thin-film material can be by point of He in adjusting mixed atmosphere
Pressure is to regulate and control the He concentration in W base nanometer crystal film, so that He concentration be made to realize controllable introducing.
4. preparation method disclosed by the invention, preparation process is simple to operation, time-saving energy-saving, highly effective and safe, without high
Your ion irradiation equipment meets the needs of extensive sample research.
Detailed description of the invention
Fig. 1 is the schematic diagram of the nano crystal thin film material of W containing helium prepared by the present invention；
Fig. 2 is the stereoscan photograph of the nano crystal thin film material of W containing helium surface topography prepared by the present invention；
Fig. 3 is the stereoscan photograph of the nano crystal thin film material of W containing helium cross-section morphology prepared by the present invention；
Fig. 4 is the section transmission electron microscope photo of the nano crystal thin film material of W containing helium prepared by the present invention.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
The preparation method for present embodiments providing a kind of base nanometer crystal of W containing helium thin-film material, as shown in Figure 1, including the following steps：
Step 1：W target is surface-treated（W target with a thickness of 2mm）, remove surface metal oxide and impurity, obtain to
The metal W target of sputtering；
Step 2：Single crystal Si substrate is cleaned by ultrasonic with alcohol and acetone mixed solution, is finally rinsed with deionized water, is dried
It is dry；
Step 3：The W target of step 1 is installed on the permanent magnetism target of magnetron sputtering, the substrate of step 2 is placed on magnetic control sputtering device
On the substrate of the inside, it is evacuated to 8 × 10-5Pa is passed through He/Ar mixed atmosphere and carries out sputtering sedimentation 5h, wherein He/Ar mixing
The total gas pressure of gas is that 2Pa, He/Ar air pressure ratio are 5；The depositing temperature of single crystal Si substrate is -600 DEG C of room temperature, sputtering power is
100W is to get the base nanometer crystal thin-film material of W containing helium described in.
The base nanometer crystal thin-film material of W containing helium obtained to the present embodiment the method is tested, specially：
A, the Analysis of Surface Topography of the base nanometer crystal of W containing helium film
To using pure W as target, using preparing nano crystal thin film material containing helium under radio frequency magnetron sputtering method room temperature to its surface
Pattern is scanned Electronic Speculum measurement, as a result as shown in Fig. 2, can be seen that in figure, after deposition sputtering, and the nano-crystal film of W containing helium
Material grains size is substantially all in 100nm hereinafter, some are close to 10nm or so, by the way that its average crystal grain ruler is calculated
Very little about 70nm, meets the size range of nanocrystalline material.
B, the cross-section morphology analysis of the base nanometer crystal of W containing helium thin-film material
To using pure W as target, using preparing nano crystal thin film material containing helium under radio frequency magnetron sputtering method room temperature to its section
It is scanned Electronic Speculum measurement, as a result as shown in figure 3, can be seen that in figure, after deposition sputtering, the nano crystal thin film material of W containing helium
Crystal structure is typical nanometer column crystal, and film thickness is in 10nm-100 μ m.
C, the distribution situation analysis that helium steeps in the base nanometer crystal of W containing helium thin-film material
The nano crystal thin film material of determination step three, film surface are as thin as 20 μm hereinafter, carrying out ion again to viscous regrind face-to-face
Perforation is thinned and makes its section transmission sample, obtains after then carrying out transmission electron microscope observing measurement to its transmission sample such as Fig. 4 institute
Showing as a result, can be seen that in figure, what helium steeped in the nano crystal thin film material of W containing helium by deposition preparation is evenly distributed, helium bubble
Average-size is about 1nm or so.
Embodiment 2
A kind of preparation method of the base nanometer crystal of W containing helium thin-film material is present embodiments provided, compared with Example 1, step 2 and step
Rapid 3 technological parameter is identical, the difference is that the W base target that step 1 uses is W alloy target（Dispersed oxide W or carbide
Disperse W）.
To the base nanometer crystal thin-film material of W containing helium that the present embodiment the method obtains, carried out by method described in embodiment 1
Test, as the result is shown：
The crystallite dimension of the base nanometer crystal thin-film material of W containing helium meets the size range of nanocrystalline material in 100nm or so；
The crystal structure of the nano crystal thin film material of W containing helium is typical nanometer column crystal, and film thickness is in 10nm-100 μ m.
What helium steeped in the nano crystal thin film material of W containing helium is evenly distributed, and the average-size of helium bubble is also about 1nm or so.
Embodiment 3
A kind of preparation method of the base nanometer crystal of W containing helium thin-film material is present embodiments provided, compared with Example 1, step 1 and step
Rapid 3 technological parameter is identical, the difference is that the substrate in step 2 is ceramic substrate.
To the base nanometer crystal thin-film material of W containing helium that the present embodiment the method obtains, carried out by method described in embodiment 1
Test, as the result is shown：
The crystallite dimension of the base nanometer crystal thin-film material of W containing helium meets the size range of nanocrystalline material in 100nm or so；
The crystal structure of the nano crystal thin film material of W containing helium is typical nanometer column crystal, and film thickness is in 10nm-100 μ m.
What helium steeped in the nano crystal thin film material of W containing helium is evenly distributed, and the average-size of helium bubble is also about 1nm or so.
Embodiment 4
A kind of preparation method of the base nanometer crystal of W containing helium thin-film material is present embodiments provided, compared with Example 1, step 1 and step
Rapid 3 technological parameter is identical, the difference is that the substrate in step 2 is quartz substrate.
To the base nanometer crystal thin-film material of W containing helium that the present embodiment the method obtains, carried out by method described in embodiment 1
Test, as the result is shown：
The crystallite dimension of the base nanometer crystal thin-film material of W containing helium meets the size range of nanocrystalline material in 100nm or so；
The crystal structure of the nano crystal thin film material of W containing helium is typical nanometer column crystal, and film thickness is in 10nm-100 μ m.
What helium steeped in the nano crystal thin film material of W containing helium is evenly distributed, and the average-size of helium bubble is also about 1nm or so.
Embodiment 5
A kind of preparation method of the base nanometer crystal of W containing helium thin-film material is present embodiments provided, compared with Example 1, step 1 and step
Rapid 3 technological parameter is identical, the difference is that the substrate in step 2 is W substrate.
To the base nanometer crystal thin-film material of W containing helium that the present embodiment the method obtains, carried out by method described in embodiment 1
Test, as the result is shown：
The crystallite dimension of the base nanometer crystal thin-film material of W containing helium meets the size range of nanocrystalline material in 100nm or so；
The crystal structure of the nano crystal thin film material of W containing helium is typical nanometer column crystal, and film thickness is in 10nm-100 μ m.
What helium steeped in the nano crystal thin film material of W containing helium is evenly distributed, and the average-size of helium bubble is also about 1nm or so.
Embodiment 6
A kind of preparation method of the base nanometer crystal of W containing helium thin-film material is present embodiments provided, compared with Example 1, step 1 and step
Rapid 3 technological parameter is identical, the difference is that the substrate in step 2 is Mo substrate.
To the base nanometer crystal thin-film material of W containing helium that the present embodiment the method obtains, carried out by method described in embodiment 1
Test, as the result is shown：
The crystallite dimension of the base nanometer crystal thin-film material of W containing helium meets the size range of nanocrystalline material in 100nm or so；
The crystal structure of the nano crystal thin film material of W containing helium is typical nanometer column crystal, and film thickness is in 10nm-100 μ m.
What helium steeped in the nano crystal thin film material of W containing helium is evenly distributed, and the average-size of helium bubble is also about 1nm or so.
Although the detailed description and description of the specific embodiments of the present invention are given above, it should be noted that
We can carry out various equivalent changes and modification to above embodiment according to the concept of the present invention, and generated function is made
It, should all be within protection scope of the present invention when with the spirit still covered without departing from specification.
Claims (9)
1. a kind of preparation method of the base nanometer crystal of W containing helium thin-film material, using the method for rf magnetron sputtering, it is characterised in that packet
Include following steps：
Step 1：W base target is surface-treated, surface metal oxide and impurity are removed；
Step 2：Substrate is cleaned by ultrasonic with alcohol and acetone mixed solution, is finally rinsed with deionized water, is dried；
Step 3：W base target described in step 1 is installed on the permanent magnetism target or electromagnetism target of magnetron sputtering, by step 2
Described in substrate be placed on the substrate inside magnetic control sputtering device, be evacuated to be passed through afterwards to a certain degree helium and argon gas composition
Mixed atmosphere sputter deposited on substrate by adjusting suitable sputtering power and time to get the Ji Na of W containing helium described in
The brilliant film of rice.
2. a kind of preparation method of the base nanometer crystal of W containing helium thin-film material according to claim 1, which is characterized in that described
W base target in step 1 is pure W target or W alloy target, with a thickness of 0.1mm-5mm.
3. a kind of preparation method of the base nanometer crystal of W containing helium thin-film material according to claim 1, which is characterized in that described
Substrate in step 2 is single crystalline Si piece, ceramic substrate, quartz substrate or W substrate or Mo substrate.
4. a kind of preparation method of the base nanometer crystal of W containing helium thin-film material according to claim 1, which is characterized in that described
Sputtering atmosphere in step 3 is He/Ar mixed gas, and the total gas pressure of He/Ar mixed gas is 0.1Pa-5Pa, He/Ar air pressure
Than for 0.1-10.
5. a kind of preparation method of the base nanometer crystal of W containing helium thin-film material according to claim 1, which is characterized in that described
Sputtering time in step 3 is 0.5-10h.
6. a kind of preparation method of the base nanometer crystal of W containing helium thin-film material according to claim 1, which is characterized in that described
The depositing temperature of substrate is -600 DEG C of room temperature in step 3, sputtering power 50-150W.
7. a kind of preparation method of the base nanometer crystal of W containing helium thin-film material according to claim 1, which is characterized in that described
The base nanometer crystal thin-film material of W containing helium film thickness be 10nm-100 μm.
8. a kind of preparation method of the base nanometer crystal of W containing helium thin-film material according to claim 1, which is characterized in that described
The nano crystal thin film material of W containing helium crystallite dimension at 1 μm or less.
9. a kind of preparation method of the base nanometer crystal of W containing helium thin-film material according to claim 1, which is characterized in that described
The base nanometer crystal thin-film material of W containing helium in ingredient target atom and He atom, wherein He atom and target atom ratio are 0-0.8.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112289532A (en) * | 2020-09-23 | 2021-01-29 | 贵州凯里经济开发区中昊电子有限公司 | Method for preparing nanocrystalline film electrode by using copper alloy as material and application |
| CN112725748A (en) * | 2020-11-10 | 2021-04-30 | 北京工业大学 | Preparation method of superfine nanocrystalline tungsten material |
| CN114196928A (en) * | 2021-12-01 | 2022-03-18 | 合肥工业大学 | Tungsten coating with excellent plasma irradiation resistance and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0845846A (en) * | 1994-07-26 | 1996-02-16 | Tokyo Electron Ltd | Sputtering method and apparatus |
| CN101323946A (en) * | 2008-07-15 | 2008-12-17 | 南京大学 | Preparation of nanocrystalline metal Ta film having out phase structure |
| CN107250425A (en) * | 2015-02-23 | 2017-10-13 | 应用材料公司 | The automated capacitive current regulator for controlling one or more film characters by target validity period is compensated |
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2018
- 2018-07-12 CN CN201810764894.XA patent/CN108914075B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0845846A (en) * | 1994-07-26 | 1996-02-16 | Tokyo Electron Ltd | Sputtering method and apparatus |
| CN101323946A (en) * | 2008-07-15 | 2008-12-17 | 南京大学 | Preparation of nanocrystalline metal Ta film having out phase structure |
| CN107250425A (en) * | 2015-02-23 | 2017-10-13 | 应用材料公司 | The automated capacitive current regulator for controlling one or more film characters by target validity period is compensated |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112289532A (en) * | 2020-09-23 | 2021-01-29 | 贵州凯里经济开发区中昊电子有限公司 | Method for preparing nanocrystalline film electrode by using copper alloy as material and application |
| CN112289532B (en) * | 2020-09-23 | 2023-09-01 | 贵州凯里经济开发区中昊电子有限公司 | Method for preparing nanocrystalline thin film electrode by using copper alloy as material and application |
| CN112725748A (en) * | 2020-11-10 | 2021-04-30 | 北京工业大学 | Preparation method of superfine nanocrystalline tungsten material |
| CN112725748B (en) * | 2020-11-10 | 2022-09-09 | 北京工业大学 | Preparation method of superfine nanocrystalline tungsten material |
| CN114196928A (en) * | 2021-12-01 | 2022-03-18 | 合肥工业大学 | Tungsten coating with excellent plasma irradiation resistance and preparation method thereof |
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| CN108914075B (en) | 2020-07-17 |
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