CN108914075B - Preparation method of W-based nanocrystalline thin film material based on helium - Google Patents
Preparation method of W-based nanocrystalline thin film material based on helium Download PDFInfo
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- CN108914075B CN108914075B CN201810764894.XA CN201810764894A CN108914075B CN 108914075 B CN108914075 B CN 108914075B CN 201810764894 A CN201810764894 A CN 201810764894A CN 108914075 B CN108914075 B CN 108914075B
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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
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- 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
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- 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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- 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
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- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
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Abstract
The invention discloses a preparation method of a W-based nanocrystalline film material containing helium, which comprises the steps of firstly adopting a magnetron sputtering method to sputter and deposit a W-based target material in He/Ar mixed atmosphere, thereby realizing the preparation of the W-based nanocrystalline film material containing helium on a substrate. The preparation method can effectively overcome the problem that the crystal grains of the W-based block prepared by the traditional powder metallurgy method and other methods are thick, realize the preparation of the W-based sample with the nanometer-level crystal grain size, effectively overcome the problems that the temperature is uncontrollable, the helium atoms are not uniformly distributed in the depth direction of the material surface and the like caused by the temperature rise of the material surface when an accelerator is used for injecting He in the traditional method, and realize the uniform and controllable injection of the He atoms in the W-based material.
Description
Technical Field
The invention relates to a preparation method of a metal-based nanocrystalline film material containing helium, in particular to a preparation method of a W-based nanocrystalline film material containing helium.
Background
Nuclear energy is considered to be an ideal energy source which can replace fossil energy sources on a large scale, meet the ever-increasing power demand of people and improve energy consumption structures at present. The nuclear fusion energy is obtained mainly by using the way that deuterium and tritium isotopes of hydrogen undergo polymerization reaction under special conditions to release high-energy particles (neutrons and helium), namely 2D + 3T Ò 4He (3.5 MeV) + n0 (14.1 MeV). Materials in a fusion reactor, particularly a first wall facing to plasma and a divertor material, are subjected to high-energy neutron irradiation to generate serious lattice atom dislocation damage, and helium with the concentration of 10-15 appm He/dpa generated in the fusion reaction process is easy to diffuse into the materials and is gathered to form helium bubbles, so that the reduction of the properties of swelling, bubbling, hardening, embrittlement, creep, fatigue and the like of the materials is caused, namely the phenomenon of helium brittleness.
Tungsten has been considered as one of the main candidate materials for the first wall material facing plasma of future nuclear fusion reactors due to its advantages of high melting point, low sputtering rate, good mechanical properties, and low tritium retention. However, the problem of helium embrittlement caused by the irradiation of tungsten with helium is more pronounced than with other metals. The main reasons are as follows: 1) the potential energy barrier of helium atoms penetrating through the surface of tungsten into the interior is only 5 eV, so that helium irradiated with high energy easily enters the interior of tungsten crystal lattice; 2) helium migrates extremely easily after entering the interior of tungsten; 3) tungsten atoms are easy to generate dislocation damage phenomenon when the particle irradiation energy exceeds 500 eV, so that a large number of vacancies and interstitial tungsten atoms are generated, and helium atom-vacancy complexes and helium atom clusters are more easily formed than other metals. In addition, nanostructured materials have shown excellent radiation resistance due to their higher dislocation density and grain boundary volume ratio, which can become important radiation-induced defect traps. Therefore, the preparation of the W-based nanocrystalline material containing helium has important significance for researching the nucleation growth and evolution process of He bubbles in the material.
Heretofore, there have been many methods of introducing helium atoms into W materials, including ion implantation, tritium decay, neutron irradiation, and the like. With respect to the above methods, they have many disadvantages. For example, while helium ion implantation can introduce controlled, quantitative helium atoms into a sample, it is difficult to uniformly distribute helium atoms in a material; for the tritium decay method, although it can uniformly introduce helium atoms into the material, the experimental procedure requires a long half-life (about 12.3 years); neutron irradiation also causes a series of irradiation induced damage, complicating research experiments on helium behavior in W.
Magnetron sputtering is a commonly used method for preparing thin films, and the method is characterized in that a small amount of inert gas is introduced into a vacuum system, inert gas ions generated by discharge bombard a cathode target after being accelerated by cathode bias voltage, so that target atoms are sputtered onto a substrate to finally form the thin film. The prior prepared helium-containing aluminum or titanium film adopts a direct-current magnetron sputtering method. However, the dc magnetron sputtering can only sputter conductive targets, and the dc magnetron sputtering preparation method cannot be used for W-based targets such as oxide dispersion W and carbide dispersion W.
The application range of the radio frequency magnetron sputtering method is wider, and almost all solid targets can be sputtered. At present, radio frequency magnetron sputtering is not seen in the literature for preparing the W-based thin film material.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a helium-containing nanocrystalline tungsten-based film material with adjustable He concentration and controllable W grain size, which can effectively overcome the problem that W-based bulk grains prepared by the traditional method are thick on one hand, and can introduce a helium-containing W-based nanocrystalline film with controllable He concentration and uniformly distributed helium bubbles on the other hand.
The invention also provides a preparation method of the W-based nanocrystalline film material containing helium, which comprises the following steps:
the method comprises the following steps: carrying out surface treatment and polishing on the W-based target material, and removing metal oxides and oil stains on the surface to obtain a target material to be sputtered;
step two: carrying out ultrasonic cleaning on a single crystal Si substrate, a ceramic wafer substrate, a quartz substrate or other metal substrates (such as a W substrate or a Mo substrate) by using a mixed solution of alcohol and acetone, finally washing by using deionized water, and drying;
step three: and (3) mounting the W-based target obtained in the first step on a permanent magnet target subjected to magnetron sputtering, placing the substrate obtained in the second step on a substrate in a magnetron sputtering instrument, vacuumizing to a certain degree, introducing He/Ar mixed atmosphere, and carrying out sputtering deposition for a certain time to obtain the W-based nanocrystalline thin film material containing helium.
Preferably, the W-based target material of the first step is a W target and a W alloy target material (the thickness is 0.1mm-5 mm).
Preferably, the organic solvent of the second step is ethanol and acetone, and the substrate of the second step is a single crystal Si sheet, a ceramic substrate, a quartz substrate or other metal substrate (W substrate or Mo substrate).
Preferably, the total pressure of the He/Ar mixed gas in the third step is 0.1Pa-5Pa, the pressure ratio of the He/Ar is 0.1-10, and the sputtering time is 0.5-50 h; the thickness of the film is 10nm-100 μm.
Preferably, the preparation method is a radio frequency magnetron sputtering method, wherein the deposition temperature is normal temperature to 600 ℃, and the deposition is carried out under He/Ar mixed gas; the sputtering power is 50-150W.
According to the invention, through a large amount of experimental work, the radio frequency magnetron sputtering method is firstly applied to the preparation of the W-based nanocrystalline thin film material containing helium, He with uniform concentration can be introduced into the W-based material, and the method is particularly suitable for researching the He brittleness problem of the W-based material in nuclear fusion reaction, and compared with the prior art, the method has the following specific advantages:
the preparation method of the W-based nanocrystalline film material containing helium disclosed by the invention can be used for preparing a W-based film containing helium, the grain size of which is below 100nm, and the problem that tungsten-based block bodies prepared by a traditional method are large in grains is solved.
The preparation method of the W-based nanocrystalline thin film material containing helium disclosed by the invention overcomes the problems of uncontrollable temperature caused by the temperature rise of the surface of the material, uneven distribution of helium atoms in the depth direction of the surface of the material and the like when an accelerator is used for injecting He, can prepare the W-based nanocrystalline thin film containing He with uniform and thicker concentration, and is more beneficial to simulating and researching the evolution process of formation of helium bubbles in tungsten.
The invention discloses a preparation method of a W-based nanocrystalline film material, which can regulate and control the He concentration in the W-based nanocrystalline film by regulating the He partial pressure in the mixed atmosphere, so that the He concentration can be controllably introduced.
The preparation method disclosed by the invention has the advantages of simple preparation process, easiness in operation, time saving, energy saving, high efficiency, safety and no need of expensive ion irradiation equipment, and meets the requirement of large-scale sample research.
Drawings
FIG. 1 is a schematic diagram of a W-type nanocrystalline thin film material containing helium prepared according to the present invention;
FIG. 2 is a scanning electron micrograph of the surface morphology of the W nanocrystalline thin film material containing helium prepared by the present invention;
FIG. 3 is a scanning electron micrograph of the cross-sectional morphology of the W nanocrystalline thin film material containing helium prepared by the present invention;
FIG. 4 is a transmission electron micrograph of a cross section of the W nanocrystalline thin film material containing helium prepared by the present invention.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
The embodiment provides a preparation method of a W-based nanocrystalline thin film material containing helium, as shown in fig. 1, comprising the following steps:
the method comprises the following steps: carrying out surface treatment on the W target (the thickness of the W target is 2 mm), and removing surface metal oxides and impurities to obtain a metal W target to be sputtered;
step two: ultrasonically cleaning a single crystal Si substrate by using a mixed solution of alcohol and acetone, finally washing by using deionized water, and drying;
step three, installing the W target in the step one on a permanent magnet target of magnetron sputtering, placing the substrate in the step two on a substrate in a magnetron sputtering instrument, vacuumizing to 8 × 10-5Pa, introducing He/Ar mixed atmosphere for sputtering deposition for 5 hours, wherein the total pressure of He/Ar mixed gas is 2Pa, the pressure ratio of He/Ar is 5, the deposition temperature of the single crystal Si substrate is normal temperature-600 ℃, and the sputtering power is 100W, thus obtaining the W-based nanocrystalline thin film material containing helium.
The test of the W-based nanocrystalline thin film material containing helium obtained by the method of this embodiment specifically includes:
A. the surface morphology of the helium-containing W-based nanocrystalline thin film is analyzed, pure W is used as a target material, the helium-containing nanocrystalline thin film material is prepared by a radio frequency magnetron sputtering method at normal temperature, the surface morphology of the helium-containing W nanocrystalline thin film material is measured by a scanning electron microscope, the result is shown in figure 2, the figure shows that after deposition sputtering, the grain size of the helium-containing W nanocrystalline thin film material is basically below 100nm and is approximate to about 10nm in some cases, the average grain size is about 70nm through statistical calculation, and the size range of the helium-containing W nanocrystalline thin film material is met.
B. The sectional morphology of the helium-containing W-based nanocrystalline thin-film material is analyzed, pure W is used as a target material, the helium-containing nanocrystalline thin-film material is prepared at normal temperature by using a radio frequency magnetron sputtering method, and the section of the helium-containing nanocrystalline thin-film material is measured by a scanning electron microscope, and the result is shown in figure 3, wherein the crystal structure of the helium-containing W nanocrystalline thin-film material is typical nano columnar crystal after deposition sputtering, and the thickness of the thin-film is within the range of 10nm-100 mu m.
C. Analyzing the distribution of helium bubbles in the helium-containing W-based nanocrystalline thin film material, determining the nanocrystalline thin film material in the third step, namely, the surface of the thin film is faced to the surface and then is ground to be less than 20 mu m, then carrying out ion thinning and perforation to prepare a transmission sample of the section of the thin film material, and then carrying out transmission electron microscope observation and measurement on the transmission sample to obtain a result shown in figure 4, wherein the helium bubbles in the helium-containing W nanocrystalline thin film material prepared by deposition are uniformly distributed, and the average size of the helium bubbles is about 1 nm.
Example 2
This example provides a method for preparing a W-based nanocrystalline thin film material containing helium, compared with example 1, the process parameters in step 2 and step 3 are the same, except that the W-based target material used in step 1 is a W alloy target (oxide dispersed W or carbide dispersed W).
The test of the W-based nanocrystalline thin film material containing helium obtained by the method of this example by the method of example 1 shows that:
the grain size of the W-based nanocrystalline film material containing helium is about 100nm, which accords with the size range of nanocrystalline materials;
the crystal structure of the helium-containing W nanocrystalline film material is typical nano columnar crystal, and the thickness of the film is in the range of 10nm-100 mu m.
The helium bubbles in the helium-containing W nanocrystalline thin film material are uniformly distributed, and the average size of the helium bubbles is about 1 nm.
Example 3
This example provides a method for preparing a W-based nanocrystalline thin film material containing helium, and compared with example 1, the process parameters of step 1 and step 3 are the same, except that the substrate in step 2 is a ceramic substrate.
The test of the W-based nanocrystalline thin film material containing helium obtained by the method of this example by the method of example 1 shows that:
the grain size of the W-based nanocrystalline film material containing helium is about 100nm, which accords with the size range of nanocrystalline materials;
the crystal structure of the helium-containing W nanocrystalline film material is typical nano columnar crystal, and the thickness of the film is in the range of 10nm-100 mu m.
The helium bubbles in the helium-containing W nanocrystalline thin film material are uniformly distributed, and the average size of the helium bubbles is about 1 nm.
Example 4
This example provides a method for preparing a W-based nanocrystalline thin film material containing helium, compared with example 1, the process parameters of step 1 and step 3 are the same, except that the substrate in step 2 is a quartz substrate.
The test of the W-based nanocrystalline thin film material containing helium obtained by the method of this example by the method of example 1 shows that:
the grain size of the W-based nanocrystalline film material containing helium is about 100nm, which accords with the size range of nanocrystalline materials;
the crystal structure of the helium-containing W nanocrystalline film material is typical nano columnar crystal, and the thickness of the film is in the range of 10nm-100 mu m.
The helium bubbles in the helium-containing W nanocrystalline thin film material are uniformly distributed, and the average size of the helium bubbles is about 1 nm.
Example 5
This example provides a method for preparing a W-based nanocrystalline thin film material containing helium, and compared with example 1, the process parameters of step 1 and step 3 are the same, except that the substrate in step 2 is a W substrate.
The test of the W-based nanocrystalline thin film material containing helium obtained by the method of this example by the method of example 1 shows that:
the grain size of the W-based nanocrystalline film material containing helium is about 100nm, which accords with the size range of nanocrystalline materials;
the crystal structure of the helium-containing W nanocrystalline film material is typical nano columnar crystal, and the thickness of the film is in the range of 10nm-100 mu m.
The helium bubbles in the helium-containing W nanocrystalline thin film material are uniformly distributed, and the average size of the helium bubbles is about 1 nm.
Example 6
This example provides a method for preparing a W-based nanocrystalline thin film material containing helium, and compared with example 1, the process parameters in step 1 and step 3 are the same, except that the substrate in step 2 is a Mo substrate.
The test of the W-based nanocrystalline thin film material containing helium obtained by the method of this example by the method of example 1 shows that:
the grain size of the W-based nanocrystalline film material containing helium is about 100nm, which accords with the size range of nanocrystalline materials;
the crystal structure of the helium-containing W nanocrystalline film material is typical nano columnar crystal, and the thickness of the film is in the range of 10nm-100 mu m.
The helium bubbles in the helium-containing W nanocrystalline thin film material are uniformly distributed, and the average size of the helium bubbles is about 1 nm.
Although particular embodiments of the invention have been described and illustrated in detail, it should be understood that various equivalent changes and modifications could be made to the above-described embodiments in accordance with the spirit of the invention, and the resulting functional effects would still fall within the scope of the invention.
Claims (4)
1. A preparation method of a W-based nanocrystalline film material containing helium adopts a radio frequency magnetron sputtering method, and is characterized by comprising the following steps:
the method comprises the following steps: carrying out surface treatment on the W-based target material to remove surface metal oxides and impurities;
step two: ultrasonically cleaning the substrate with a mixed solution of alcohol and acetone, finally washing with deionized water, and drying;
step three: mounting the W-based target material in the first step on a permanent magnet target or an electromagnetic target for magnetron sputtering, placing the substrate in the second step on a substrate in a magnetron sputtering instrument, vacuumizing to a certain degree, introducing a mixed atmosphere consisting of helium and argon, and performing sputtering deposition on the substrate by adjusting proper sputtering power and time to obtain the W-based nanocrystalline film containing helium;
the W-based target material in the step one is a pure W target or a W alloy target, and the thickness of the W-based target material is 0.1mm-5 mm;
the substrate in the second step is a single crystal Si sheet, a ceramic substrate, a quartz substrate or a W substrate or a Mo substrate;
the sputtering atmosphere in the third step is He/Ar mixed gas, the total pressure of the He/Ar mixed gas is 0.1Pa-5Pa, and the pressure ratio of He/Ar is 0.1-10;
the sputtering time in the third step is 0.5-10 h;
in the third step, the deposition temperature of the substrate is normal temperature-600 ℃, and the sputtering power is 50-150W.
2. The method according to claim 1, wherein the thickness of the W-based nano-crystalline film is 10nm-100 μm.
3. The method according to claim 1, wherein the grain size of the W-based nano-crystalline film material is less than 1 μm.
4. The method according to claim 1, wherein the W-based nano-crystalline film material containing helium contains target atoms and He atoms, and the ratio of the He atoms to the target atoms is 0-0.8.
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