CN115386839A - Anti-irradiation high-entropy alloy/ceramic multilayer film and preparation method thereof - Google Patents

Anti-irradiation high-entropy alloy/ceramic multilayer film and preparation method thereof Download PDF

Info

Publication number
CN115386839A
CN115386839A CN202210839902.9A CN202210839902A CN115386839A CN 115386839 A CN115386839 A CN 115386839A CN 202210839902 A CN202210839902 A CN 202210839902A CN 115386839 A CN115386839 A CN 115386839A
Authority
CN
China
Prior art keywords
entropy alloy
multilayer film
ceramic multilayer
layer
radiation
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.)
Granted
Application number
CN202210839902.9A
Other languages
Chinese (zh)
Other versions
CN115386839B (en
Inventor
魏东博
刘建华
张平则
胡玉锦
李逢昆
杨凯
党博
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing University of Aeronautics and Astronautics
Original Assignee
Nanjing University of Aeronautics and Astronautics
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nanjing University of Aeronautics and Astronautics filed Critical Nanjing University of Aeronautics and Astronautics
Priority to CN202210839902.9A priority Critical patent/CN115386839B/en
Publication of CN115386839A publication Critical patent/CN115386839A/en
Application granted granted Critical
Publication of CN115386839B publication Critical patent/CN115386839B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • 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
    • C23C14/08—Oxides
    • C23C14/081—Oxides of aluminium, magnesium or beryllium
    • 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
    • C23C14/3435—Applying energy to the substrate during sputtering
    • C23C14/345—Applying energy to the substrate during sputtering using substrate bias
    • 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
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • 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
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses an irradiation-resistant high-entropy alloy/ceramic multilayer film, which comprises a TaWTIVMo high-entropy alloy layer and an aluminum oxide layer which are alternately deposited; the high-entropy alloy layer comprises the following elements in percentage by mass: from 28% to 32% Ta, from 30% to 36% by weight of W, from 15% to 20% by weight of Ti, from 8% to 13% by weight of V, the balance being Mo, the TaWTIVMo high entropy alloy layer being of body centred cubic structure; the alumina layer has nano-holes therein. The invention also discloses a preparation method of the anti-irradiation high-entropy alloy/ceramic multilayer filmThe method is carried out. The invention utilizes the high-entropy alloy film and Al 2 O 3 The film is used for preparing the multi-layer film with the nanometer scale, the grain boundary density of the multi-layer composite material formed by the film and the film is increased, and the anti-irradiation performance of the electronic equipment element working in the irradiation environment is obviously improved.

Description

Anti-irradiation high-entropy alloy/ceramic multilayer film and preparation method thereof
Technical Field
The invention belongs to a composite film and a preparation method thereof, and particularly relates to an anti-irradiation high-entropy alloy/ceramic multilayer film and a preparation method thereof.
Background
Under the condition of rapid development of modern science, electronic equipment is widely used in both high-precision aerospace and modern war. The electronic components that make up the electronic device are inevitably exposed to both spatial and nuclear radiation, and failure of the electronic components may result in failure of the entire electronic device. In order to realize the periodic protection and the radiation resistance of the key devices, some technical means adopted in the past have long period and may sacrifice some inherent advantages. The improvement of the anti-irradiation performance of the key parts of the electronic equipment needs to be solved urgently.
Al 2 O 3 Film ionization radiation resistance capability ratio of SiO 2 The film is more than one order of magnitude higher because of Al 2 O 3 The film has a large number of vacancy defects as a defect sink for absorbing irradiation particles, al 2 O 3 Film dielectric constant ratio SiO 2 High. Al (Al) 2 O 3 Being ceramic is inherently brittle.
The Chinese patent with the application number of 202010719235.1 discloses a molybdenum disulfide/yttrium stabilized zirconia composite film with high wear resistance and radiation resistance and a preparation method thereof, wherein a radiation resistant film layer mainly comprises a Ti transition layer and a molybdenum disulfide/yttrium composite film, vacancy defects are increased through doping to reduce the radiation resistance, and the change of amorphousness after radiation is reduced through adopting a new technology and annealing, but the radiation resistance is reduced due to insufficient radiation resistance dose and defects after radiation.
The high-entropy alloy is composed of elements with close molar ratios, the content of each element is 5% -35%, and the larger mixed entropy inhibits the formation of intermetallic compounds and promotes the formation of simple crystal phases. Due to the unique macroscopic properties, high mixed entropy, slow diffusion of lattice distortion and the cocktail effect of the high entropy alloy. High entropy alloys have attracted considerable attention in advanced material design and application due to their superior properties compared to conventional alloys, such as high hardness/strength, high fatigue and fracture toughness, high temperature oxidation resistance, corrosion resistance, radiation resistance, and unique electrical and magnetic properties. Numerous studies have shown that high-entropy alloys with excellent physicochemical properties have a wide potential for use in different fields, such as aeroengines, tool coatings and nuclear protection. Previous studies have shown that films and coatings exhibit properties that differ from those of bulk due to intrinsic structural features resulting from differences in apparent geometry, and that films and coatings are limited in dimensional thickness, resulting in very limited grain growth space. The crystal grain volume is small and the number of grain boundaries is large.
At present, the anti-radiation performance of the high-entropy alloy multilayer film becomes a research hotspot in China. Alumina and high-entropy alloy are difficult to be effectively combined due to large difference of elastic modulus. Therefore, the problem of how to combine the aluminum oxide and the high-entropy alloy to further improve the radiation resistance of the high-entropy alloy multilayer needs to be solved urgently.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects of the prior art, the invention aims to provide a radiation-resistant high-entropy alloy/ceramic multilayer film with good stability and strong interface bonding force, and the invention also aims to provide a convenient and controllable preparation method of the radiation-resistant high-entropy alloy/ceramic multilayer film.
The technical scheme is as follows: the invention relates to an irradiation-resistant high-entropy alloy/ceramic multilayer film, which comprises TaWTIVMo high-entropy alloy layers and aluminum oxide layers which are alternately deposited; the high-entropy alloy layer comprises the following elements in percentage by mass: from 28% to 32% Ta, from 30% to 36% by weight of W, from 15% to 20% by weight of Ti, from 8% to 13% by weight of V, the balance being Mo, the TaWTIVMo high entropy alloy layer being of body centred cubic structure; the alumina layer is provided with nano holes, and the nano holes preset in advance are used as polymerization points for absorbing defects generated by irradiation, so that irradiation swelling is inhibited, the structure is kept stable, and the irradiation resistance is improved.
Further, the thickness of the high-entropy alloy layer is 300nm to 500nm, and the thickness of the aluminum oxide layer is 100nm to 200nm.
Furthermore, the total number of layers of the high-entropy alloy/ceramic multilayer film is 6-16, and the total thickness is 1.2-5.6 μm. When the content of the W element in the high-entropy alloy layer is larger than that of Ta, ti, V and Mo, the irradiation resistance is the best, because the W element has the characteristics of high melting point, low sputtering rate, high thermal conductivity, low tritium retention and the like.
The preparation method of the radiation-resistant high-entropy alloy/ceramic multilayer film comprises the following steps:
(a) After the surface of a silicon substrate polished on one side is cleaned, etching liquid is used for surface pretreatment under ultrasonic stirring, so that the surface roughness is 1-5 nm;
(b) In a vacuum environment, cleaning impurities and oxides on the surfaces of the aluminum oxide target material and the high-entropy alloy target material in the sputtering cavity, and after pre-sputtering is finished, closing the baffles of the aluminum oxide target material and the high-entropy alloy target material;
(c) In a vacuum environment, depositing a high-entropy alloy layer on a silicon substrate, then depositing an aluminum oxide layer, and sequentially and alternately depositing for 3-8 periods;
(d) And (c) annealing the product obtained in the step (c) in vacuum at 190-200 ℃ for 2-4 h in an argon atmosphere to obtain the anti-radiation high-entropy alloy/ceramic multilayer film.
Further, in the step (a), the silicon substrate is a monocrystalline silicon wafer, and the crystal orientation is (100). The etching liquid is prepared by mixing 1-3M KOH and 18-20 vol% isopropyl alcohol aqueous solution, the power of ultrasonic stirring is 100-120 KHz, and the intensity is 50-60W/L. By etching liquid pretreatment, the roughness of the silicon substrate is increased, and the adhesive force between films is effectively improved.
Further, the step (b) specifically comprises the following steps: pumping the vacuum degree of the sputtering cavity to be lower than 5 multiplied by 10 -6 pa, introducing argon with the gas flow of 15-25 sccm, and adjusting the deposition pressure to 1.5-1.9 pa; regulatingThe pre-sputtering rate of a power supply is 100-110W, the pre-sputtering time is 10-15 min, the alumina target baffle is in a closed state when the high-entropy alloy target is pre-sputtered, and the high-entropy alloy target baffle is in a closed state when the alumina target is pre-sputtered.
Further, in the step (c), when the high-entropy alloy layer is deposited, the baffle plate of the alumina target is in a closed state, the power supply power is 83-100W, the deposition time is 10-15 min, the rotating speed of the silicon substrate is 10-12 r/min, and the bias voltage of the silicon substrate is-50V-40V. When the aluminum oxide layer is deposited, the baffle of the high-entropy alloy target is in a closed state, the power supply power is 80-92 w, the deposition time is 8-10 min, the rotating speed of the silicon substrate is 10-12 r/min, and the bias voltage of the silicon substrate is-50V-40V.
Further, the high-entropy alloy target material is Ta 20 W 20 Ti 24 V 26 Mo 10 High entropy alloy.
The reaction principle is as follows: the multilayer film has a large number of interfaces, defects generated by irradiation can be annihilated, and nucleation and growth of bubbles generated by irradiation are inhibited. The dimensional effects present in multilayer films result in a higher radiation resistance for smaller periodic thicknesses of the multilayer film. Under the condition that the specific gravity of the W element is the maximum, the characteristics of low tritium retention and the like are that the radiation resistance of the high-entropy alloy layer is improved. The pretreatment of the substrate before preparation increases the binding force between the substrate and the film, increases the integrity of the whole film and has excellent anti-irradiation effect. Under the action of the preset cavity for inhibiting radiation swelling, the body-centered cubic structure is kept intact. Compared with the traditional material, the interfaces of the multi-layer nanoscale material are increased, a large number of defects generated by irradiation annihilate at the interfaces, and irradiation damage is reduced.
Has the beneficial effects that: compared with the prior art, the invention has the following remarkable characteristics:
1. using high entropy alloy films and Al 2 O 3 The film is used for preparing a multi-layer film with a nano scale, and the multi-layer composite material formed by the film and the film increases the grain boundary density, so that the anti-irradiation performance of an electronic equipment element working in an irradiation environment is obviously improved;
2. the density of an interface is increased by the preparation of different film layers, the micro roughness is increased by treating the silicon substrate with the etching liquid, and the binding force between the film layers and the silicon substrate is increased;
3. the nano-holes preset in advance in the film are used as the defects preset in advance, can absorb polymerization points of the defects generated by radiation induction, inhibit aggregation and growth of radiation swelling, reduce radiation hardening and defects, maintain the stability of the structure, improve the radiation resistance, and reduce the radiation swelling rate by 50 percent compared with a single-layer alumina film under the same thickness;
4. the high-entropy alloy has good mechanical property, and the radiation resistance can be improved and the mechanical property can be improved by adding a layer of radiation-proof high-entropy alloy mixed coating;
5. the vacuum annealing is favorable for keeping the stability of crystal lattices, and the structure of the body-centered cubic is also favorable for improving the anti-irradiation performance;
6. the multilayer film and the preset nano-cavities are prepared by utilizing a magnetron sputtering technology, so that irradiation particles can be absorbed, the anti-irradiation performance is improved by blending different film layers, the mechanical property is also improved, and the supersaturation defect generated by irradiation can be absorbed and inhibited due to higher grain boundary density of the multilayer film;
7. the invention can be applied to the field of radiation-proof coatings on the surfaces of electronic components, can also improve the radiation-proof stability of thermonuclear fusion devices, and widens the application of high-entropy alloy to components in the fields of aircraft engines, tool coatings and nuclear protection.
Drawings
FIG. 1 is a schematic structural view of embodiment 1 of the present invention;
FIG. 2 is a scanning electron micrograph of example 6 of the present invention;
FIG. 3 is a pictorial view of embodiment 6 of the present invention;
FIG. 4 shows that the surface of the alumina layer 2 is 9X 10 in example 6 of the present invention 5 Transmission electron micrographs at magnification;
FIG. 5 shows that the surface of the alumina layer 2 of example 6 of the present invention is 3.6X 10 6 Transmission electron micrographs at magnification;
FIG. 6 is an XRD pattern for example 6 of the present invention;
FIG. 7 is a transmission electron micrograph after irradiation of example 6 of the present invention;
Detailed Description
In the following embodiments, one cycle refers to repeating a set of steps (4) and (5). With high purity Ta 20 W 20 Ti 24 V 26 Mo 10 The high-entropy alloy is used as a high-entropy alloy target material, and the purity is 99.9%; high-purity alumina is used as an alumina target material, and the purity is 99.9%. The silicon substrate 3 is a monocrystalline silicon wafer, and has a crystal orientation (100). The magnetron sputtering device is the existing device, and the target material I of the magnetron sputtering furnace is placed from left to right, the left side is the high-entropy alloy target material, and the right side is the alumina target material.
Example 1
A preparation method of a radiation-resistant high-entropy alloy/ceramic multilayer film comprises the following steps:
(1) Preparing a matrix: adding isopropanol with the concentration of 18vol% into a 1M KOH solution to serve as an etching solution, carrying out surface pretreatment on the silicon substrate 3 with the single-sided polished under ultrasonic stirring to ensure that the surface roughness is 1nm, the ultrasonic stirring frequency is 100 kilohertz, and the ultrasonic intensity is 50 watts/liter, and drying a surface water film;
(2) Adjusting air pressure: the vacuum degree of the sputtering cavity is pumped to be lower than 5 multiplied by 10 -6 Introducing inert gas argon as protective gas, wherein the gas flow is 15sccm, the gas purity is 99.9%, and the deposition pressure is adjusted to be 1.5pa;
(3) Pre-sputtering: cleaning impurities and oxides on the surfaces of the high-entropy alloy target and the alumina target in a sputtering cavity, adjusting the pre-sputtering rate of a power supply to be 100W, adjusting the pre-sputtering time to be 10min, continuously observing the color of plasma in the cavity in the pre-sputtering process, and after the pre-sputtering is finished, keeping material baffles on the upper parts of the high-entropy alloy target and the alumina target in a closed state;
(4) Depositing a high-entropy alloy layer 1: closing a baffle on the upper part of the alumina target, opening a baffle on the upper part of the high-entropy alloy target, wherein the rotating speed of a matrix is 10r/min, the bias voltage of the matrix is-50V, the deposition distance is 10cm, the deposition power is 83W, the matrix is kept unchanged at room temperature in the whole deposition process, and the deposition is carried out for 10min;
(5) Depositing an aluminum oxide layer 2: closing a baffle on the upper part of the high-entropy alloy target, opening a baffle on the upper part of the alumina target, keeping the working pressure at 1.5pa, the rotating speed of the matrix at 10r/min, the bias voltage of the matrix at-50V, the deposition distance at 10cm, the deposition power at 80W, keeping the room temperature of the matrix unchanged in the whole deposition process, and depositing for 8min;
(6) Repeating the steps (4) and (5) for 2 times to obtain a 300 nm-thick high-entropy alloy layer 1 and a 100 nm-thick aluminum oxide layer 2 with an alternating period of 3 times;
(7) And (4) putting the product obtained in the step (6) into a vacuum annealing furnace, introducing argon as protective gas, and carrying out vacuum annealing at 190 ℃ for 2h to obtain the radiation-resistant high-entropy alloy/ceramic multilayer film with 6 total layers and a total thickness of 1.2 mu m.
The irradiation-resistant high-entropy alloy/ceramic multilayer film prepared in this example is subjected to EDS energy spectrum analysis, and the high-entropy alloy layer 1 includes the following elements in percentage by mass: 28% Ta,30% W,15% Ti,13% V,14% Mo.
Example 2
A preparation method of a radiation-resistant high-entropy alloy/ceramic multilayer film comprises the following steps:
(1) Preparing a matrix: adding isopropanol with the concentration of 20vol% into a 3M KOH solution to serve as an etching solution, carrying out surface pretreatment on the silicon substrate 3 with the single-side polished under ultrasonic stirring to ensure that the surface roughness is 5nm, the ultrasonic stirring frequency is 120 kilohertz and the ultrasonic intensity is 60 watts/liter, and drying a surface water film;
(2) Adjusting the air pressure: pumping the vacuum degree of the sputtering cavity to be lower than 5 multiplied by 10 -6 pa, introducing inert gas argon as protective gas, wherein the gas flow is 25sccm, the gas purity is 99.9%, and the deposition pressure is adjusted to be 1.9pa;
(3) Pre-sputtering: cleaning impurities and oxides on the surfaces of the high-entropy alloy target material and the alumina target material in a sputtering cavity, adjusting the pre-sputtering rate of a power supply to be 110W, adjusting the pre-sputtering time to be 15min, continuously observing the color of plasma in the cavity in the pre-sputtering process, and after the pre-sputtering is finished, closing material baffles on the upper parts of the high-entropy alloy target material and the alumina target;
(4) Depositing a high-entropy alloy layer 1: closing a baffle on the upper part of the alumina target, opening the baffle on the upper part of the high-entropy alloy target, controlling the rotating speed of a substrate to be 12r/min, the bias voltage of the substrate to be 40V, the deposition distance to be 15cm, the deposition power to be 100W, keeping the room temperature of the substrate unchanged in the whole deposition process, and depositing for 15min;
(5) Depositing an aluminum oxide layer 2: closing a baffle on the upper part of the high-entropy alloy target, opening a baffle on the upper part of the alumina target, keeping the working pressure at 1.9pa, the rotating speed of the matrix at 12r/min, the bias voltage of the matrix at minus 40V, the deposition distance at 10cm and the deposition power at 92W, keeping the room temperature of the matrix unchanged in the whole deposition process, and depositing for 10min;
(6) Repeating the steps (4) and (5) for 7 times to obtain a 500 nm-thick high-entropy alloy layer 1 and a 200 nm-thick aluminum oxide layer 2 with 8 alternating periods;
(7) And (5) putting the product obtained in the step (6) into a vacuum annealing furnace, introducing argon as protective gas, and carrying out vacuum annealing at 200 ℃ for 4 hours to obtain the radiation-resistant high-entropy alloy/ceramic multilayer film with 16 total layers and 5.6 mu m total thickness.
The irradiation-resistant high-entropy alloy/ceramic multilayer film prepared in this example is subjected to EDS energy spectrum analysis, and the high-entropy alloy layer 1 includes the following elements in percentage by mass: 32% Ta,36% W,20% Ti,8% V,4% Mo.
Example 3
A preparation method of a radiation-resistant high-entropy alloy/ceramic multilayer film comprises the following steps:
(1) Preparing a matrix: adding isopropanol with the concentration of 19vol% into a 2M KOH solution to serve as an etching solution, carrying out surface pretreatment on the silicon substrate 3 with the single-side polished under ultrasonic stirring to ensure that the surface roughness is 3nm, the ultrasonic stirring frequency is 110 kilohertz, and the ultrasonic intensity is 55 watts/liter, and drying a surface water film;
(2) Adjusting air pressure: the vacuum degree of the sputtering cavity is pumped to be lower than 5 multiplied by 10 -6 Introducing inert gas argon as protective gas, wherein the gas flow is 20sccm, the gas purity is 99.9%, and the deposition pressure is adjusted to be 1.7pa;
(3) Pre-sputtering: cleaning impurities and oxides on the surfaces of the high-entropy alloy target material and the alumina target material in a sputtering cavity, adjusting the pre-sputtering rate of a power supply to be 105W, adjusting the pre-sputtering time to be 13min, continuously observing the color of plasma in the cavity in the pre-sputtering process, and after the pre-sputtering is finished, closing material baffles on the upper parts of the high-entropy alloy target material and the alumina target;
(4) Depositing a high-entropy alloy layer 1: closing a baffle on the upper part of the alumina target, opening a baffle on the upper part of the high-entropy alloy target, wherein the rotating speed of a matrix is 11r/min, the bias voltage of the matrix is-45V, the deposition distance is 12cm, the deposition power is 92W, the room temperature of the matrix is kept unchanged in the whole deposition process, and the deposition is carried out for 13min;
(5) Depositing an aluminum oxide layer 2: closing a baffle on the upper part of the high-entropy alloy target, opening a baffle on the upper part of the alumina target, keeping the working pressure at 1.7pa, the rotating speed of the matrix at 11r/min, the bias voltage of the matrix at-45V, the deposition distance at 10cm and the deposition power at 86W, keeping the room temperature of the matrix unchanged in the whole deposition process, and depositing for 9min;
(6) Repeating the steps (4) and (5) for 5 times to obtain a 400 nm-thick high-entropy alloy layer 1 and a 150 nm-thick aluminum oxide layer 2 with an alternating period of 6 times;
(7) And (5) putting the product obtained in the step (6) into a vacuum annealing furnace, introducing argon as protective gas, and carrying out vacuum annealing at 195 ℃ for 6 hours to obtain the radiation-resistant high-entropy alloy/ceramic multilayer film with 12 total layers and 3.3 mu m total thickness.
The irradiation-resistant high-entropy alloy/ceramic multilayer thin film prepared in this embodiment is subjected to EDS energy spectrum analysis, and the high-entropy alloy layer 1 obtained includes the following elements in percentage by mass: 30% Ta,33% W,17% Ti,10% Mo.
Example 4
A preparation method of a radiation-resistant high-entropy alloy/ceramic multilayer film comprises the following steps:
(1) Preparing a matrix: adding isopropanol with the concentration of 19vol% into a 1M KOH solution to serve as an etching solution, carrying out surface pretreatment on the silicon substrate 3 with the single-sided polished under ultrasonic stirring to ensure that the surface roughness is 2nm, the ultrasonic stirring frequency is 105 kilohertz, and the ultrasonic intensity is 53 watts/liter, and drying a surface water film;
(2) Adjusting air pressure: pumping the vacuum degree of the sputtering cavity to be lower than 5 multiplied by 10 -6 pa, introducing inert gas argon as protective gas, wherein the gas flow is 18sccm, and the gas isThe purity is 99.9 percent, and the deposition pressure is adjusted to be 1.6pa;
(3) Pre-sputtering: cleaning impurities and oxides on the surfaces of the high-entropy alloy target material and the alumina target material in a sputtering cavity, adjusting the pre-sputtering rate of a power supply to be 102W, adjusting the pre-sputtering time to be 12min, continuously observing the color of plasma in the cavity in the pre-sputtering process, and after the pre-sputtering is finished, closing material baffles on the upper parts of the high-entropy alloy target material and the alumina target;
(4) Depositing a high-entropy alloy layer 1: closing a baffle on the upper part of the alumina target, opening a baffle on the upper part of the high-entropy alloy target, wherein the rotating speed of a matrix is 10r/min, the bias voltage of the matrix is-42V, the deposition distance is 11cm, the deposition power is 85W, the room temperature of the matrix is kept unchanged in the whole deposition process, and the deposition is carried out for 12min;
(5) Depositing an aluminum oxide layer 2: closing a baffle on the upper part of the high-entropy alloy target, opening a baffle on the upper part of the alumina target, keeping the working pressure at 1.6pa, the rotating speed of the matrix at 10r/min, the bias voltage of the matrix at-44V, the deposition distance at 10cm and the deposition power at 84W, keeping the room temperature of the matrix unchanged in the whole deposition process, and depositing for 8min;
(6) Repeating the steps (4) and (5) for 3 times to obtain a 350 nm-thick high-entropy alloy layer 1 and a 120 nm-thick aluminum oxide layer 2 with 4 alternating periods;
(7) And (4) putting the product obtained in the step (6) into a vacuum annealing furnace, introducing argon as protective gas, and carrying out vacuum annealing at 192 ℃ for 2.5h to obtain the radiation-resistant high-entropy alloy/ceramic multilayer film with 8 total layers and a total thickness of 1.88 mu m.
The irradiation-resistant high-entropy alloy/ceramic multilayer film prepared in this example is subjected to EDS energy spectrum analysis, and the high-entropy alloy layer 1 includes the following elements in percentage by mass: 29% Ta,34% W,16% Ti,12% Mo.
Example 5
A preparation method of an irradiation-resistant high-entropy alloy/ceramic multilayer film comprises the following steps:
(1) Preparing a matrix: adding isopropanol with the concentration of 20vol% into 2.5M KOH solution to serve as etching liquid, carrying out surface pretreatment on the silicon substrate 3 with the single-side polished under ultrasonic stirring to ensure that the surface roughness is 4nm, the ultrasonic stirring frequency is 115 kilohertz and the ultrasonic intensity is 58 watts/liter, and drying a surface water film;
(2) Adjusting air pressure: the vacuum degree of the sputtering cavity is pumped to be lower than 5 multiplied by 10 -6 Introducing inert gas argon as protective gas, wherein the gas flow is 23sccm, the gas purity is 99.9%, and the deposition pressure is adjusted to be 1.8pa;
(3) Pre-sputtering: cleaning impurities and oxides on the surfaces of the high-entropy alloy target material and the alumina target material in a sputtering cavity, adjusting the pre-sputtering rate of a power supply to be 108W, adjusting the pre-sputtering time to be 14min, continuously observing the color of plasma in the cavity in the pre-sputtering process, and after the pre-sputtering is finished, closing material baffles on the upper parts of the high-entropy alloy target material and the alumina target;
(4) Depositing a high-entropy alloy layer 1: closing a baffle on the upper part of the alumina target, opening a baffle on the upper part of the high-entropy alloy target, wherein the rotating speed of a matrix is 12r/min, the bias voltage of the matrix is-46V, the deposition distance is 14cm, the deposition power is 95W, the matrix is kept at room temperature in the whole deposition process, and the deposition is carried out for 14min;
(5) Depositing an aluminum oxide layer 2: closing a baffle on the upper part of the high-entropy alloy target, opening a baffle on the upper part of the alumina target, keeping the working pressure at 1.8pa, the rotating speed of the matrix at 12r/min, the bias voltage of the matrix at-41V, the deposition distance at 10cm, the deposition power at 90W, keeping the room temperature of the matrix unchanged in the whole deposition process, and depositing for 9min;
(6) Repeating the steps (4) and (5) for 6 times to obtain a high-entropy alloy layer 1 with the thickness of 450nm and an aluminum oxide layer 2 with the thickness of 190nm, wherein the alternating period is 7 times;
(7) And (4) putting the product obtained in the step (6) into a vacuum annealing furnace, introducing argon as protective gas, and carrying out vacuum annealing at 198 ℃ for 3.5h to obtain the radiation-resistant high-entropy alloy/ceramic multilayer film with 14 total layers and 4.48 mu m total thickness.
The irradiation-resistant high-entropy alloy/ceramic multilayer film prepared in this example is subjected to EDS energy spectrum analysis, and the high-entropy alloy layer 1 includes the following elements in percentage by mass: 30% Ta,31W,18% Ti,9% by weight, mo.
Example 6
A preparation method of an irradiation-resistant high-entropy alloy/ceramic multilayer film comprises the following steps:
(1) Preparing a matrix: adding isopropanol with the concentration of 20vol% into a 3M KOH solution to serve as an etching solution, carrying out surface pretreatment on the silicon substrate 3 with the single-side polished under ultrasonic stirring to ensure that the surface roughness is 5nm, the ultrasonic stirring frequency is 100 kilohertz and the ultrasonic intensity is 50 watts/liter, and drying a surface water film;
(2) Adjusting air pressure: pumping the vacuum degree of the sputtering cavity to be lower than 5 multiplied by 10 -6 pa, introducing inert gas argon as protective gas, wherein the gas flow is 25sccm, the gas purity is 99.9%, and the deposition pressure is adjusted to be 1.9pa;
(3) Pre-sputtering: cleaning impurities and oxides on the surfaces of the high-entropy alloy target material and the alumina target material in a sputtering cavity, adjusting the pre-sputtering rate of a power supply to be 110W, adjusting the pre-sputtering time to be 15min, continuously observing the color of plasma in the cavity in the pre-sputtering process, and after the pre-sputtering is finished, closing material baffles on the upper parts of the high-entropy alloy target material and the alumina target;
(4) Depositing a high-entropy alloy layer 1: closing a baffle on the upper part of the alumina target, opening a baffle on the upper part of the high-entropy alloy target, wherein the rotating speed of a matrix is 10r/min, the bias voltage of the matrix is-50V, the deposition distance is 10cm, the deposition power is 90W, the room temperature of the matrix is kept unchanged in the whole deposition process, and the deposition is carried out for 15min;
(5) Depositing an aluminum oxide layer 2: closing a baffle on the upper part of the high-entropy alloy target, opening a baffle on the upper part of the alumina target, keeping the working pressure at 1.9pa, the rotating speed of the matrix at 10r/min, the bias voltage of the matrix at-50V, the deposition distance at 10cm and the deposition power at 82W, keeping the room temperature of the matrix unchanged in the whole deposition process, and depositing for 8min;
(6) Repeating the steps (4) and (5) for 3 times to obtain a high-entropy alloy layer 1 with the thickness of 500nm and an aluminum oxide layer 2 with the thickness of 200nm, wherein the alternating period is 4 times;
(7) And (5) putting the product obtained in the step (6) into a vacuum annealing furnace, introducing argon as protective gas, and carrying out vacuum annealing at 200 ℃ for 2 hours to obtain the radiation-resistant high-entropy alloy/ceramic multilayer film with 8 total layers and 3.1 mu m total thickness.
The irradiation-resistant high-entropy alloy/ceramic multilayer film prepared in this example is subjected to EDS energy spectrum analysis, and the high-entropy alloy layer 1 includes the following elements in percentage by mass: 30% Ta,32% W,20% Ti,13% V,5% Mo.
As shown in FIG. 1, a silicon substrate 3 is provided with high entropy alloy layers 1 and aluminum oxide layers 2 alternately from bottom to top to obtain a total of 6 tightly bonded films.
As shown in fig. 2 to 3, the silicon substrate 3 has good adhesion with the high-entropy alloy layer 1, and the interface with the aluminum oxide layer 2 is flat and clear, the interface of the thin film layer is complete, the preparation quality of the multilayer film is good, and the layering is complete and the macroscopic effect is good.
As shown in fig. 4 to 5, the nano-voids 4 are successfully preset in the multilayer film in advance and are located in the alumina layer 2, and it can be seen from the figure that the voids are large in number and are randomly distributed in the film.
As shown in fig. 6, the XRD pattern of the multilayer film can be seen as bcc crystal type.
Comparative example 1
The remainder of the comparative example was the same as example 6 except that: and (5) is cancelled, and the step (4) is only operated once to obtain the single-layer high-entropy alloy layer 1.
Comparative example 2
The remainder of the operation of this comparative example is the same as example 6, except that: and (4) the step (4) is eliminated, the step (5) is operated only once, and the deposition time is replaced by 30min to obtain a single-layer aluminum oxide layer 2.
Comparative example 3
The remainder of the comparative example was the same as example 6 except that: the argon flow in the step (2) is 15sccm, the deposition pressure is 0.5pa, the sputtering condition power in the steps (4) and (5) is 90W, and the rotating speed of the substrate is 50r/min.
Comparative example 4
The remainder of the operation of this comparative example is the same as example 6, except that: the deposition time of the high-entropy alloy in the step (4) is 10min, and the deposition time of the aluminum oxide in the step (5) is 10min.
Comparative example 1 irradiation dose 3.2 x 10 15 The film is yellow and cracked by naked eyes when the helium particles are irradiated.
Comparative example 2 irradiation dose of 3.2 x 10 15 Helium pelletsThe film is seriously yellowed by irradiation, the thickness of a sem image is increased, swelling is obvious after the irradiation, the electric conductivity of the film is 300m omega cm, and a certain swelling rate exists when the film is 900m omega cm after the irradiation.
Example 6 irradiation dose of 3.2 x 10 15 The helium particle irradiation is carried out, the surface of the film is unchanged, the decomposition of the film layer is obvious, the thickness change is small, the conductivity is about 133 mu omega cm, the difference between the conductivity and the conductivity before irradiation is not large, the difference between the conductivity and the conductivity before irradiation is small, the difference between the conductivity and the conductivity before irradiation is large, and the swelling rate after irradiation is inhibited. Helium bubbles are absorbed in the nano-voids preset in advance as shown in fig. 7.
The multilayer films prepared in the comparative examples 3-4 have weak adhesion, the macroscopic surfaces slightly fall off, the sputtering power of the two targets in the comparative example 3 is consistent, the deposition thickness does not reach an ideal effect, and the adhesion between the films and the matrix is reduced due to too low working air pressure. In contrast, the deposition time of the two targets in the comparative example 4 is the same, so that the deposition stress is increased, and the adhesion between the film and the substrate and between the film and each layer of the substrate is reduced, so that slight separation can be observed macroscopically, and the process parameters adopted in the example 6 avoid the defect.

Claims (10)

1. An irradiation-resistant high-entropy alloy/ceramic multilayer film is characterized in that: comprises TaWTiVMo high-entropy alloy layers (1) and aluminum oxide layers (2) which are alternately deposited; the high-entropy alloy layer (1) comprises the following elements in percentage by mass: from 28% to 32% Ta, from 30% to 36% by weight of W, from 15% to 20% by weight of Ti, from 8% to 13% by weight of V, the balance being Mo, said TaWTIVMo high entropy alloy layer (1) being of body centered cubic structure; the alumina layer (2) is provided with nano holes.
2. A radiation-resistant high-entropy alloy/ceramic multilayer film according to claim 1, wherein: the thickness of the high-entropy alloy layer (1) is 300 nm-500 nm, and the thickness of the aluminum oxide layer (2) is 100 nm-200 nm.
3. A radiation-resistant high entropy alloy/ceramic multilayer film of claim 2, wherein: the total number of layers of the high-entropy alloy/ceramic multilayer film is 6-16, and the total thickness is 1.2-5.6 mu m.
4. The preparation method of the radiation-resistant high-entropy alloy/ceramic multilayer film according to any one of claims 1 to 3, characterized by comprising the following steps:
(a) After the surface of a silicon substrate (3) with a single-side polished surface is cleaned, etching liquid is used for surface pretreatment under ultrasonic stirring to ensure that the surface roughness is 1-5 nm, and the silicon substrate is placed into a magnetron sputtering chamber after the pretreatment is finished;
(b) In a vacuum environment, cleaning impurities and oxides on the surfaces of an aluminum oxide target material and a high-entropy alloy target material in a pre-sputtering cavity, and after pre-sputtering is finished, closing baffles on the upper parts of the aluminum oxide target material and the high-entropy alloy target material, wherein the high-entropy alloy target material is positioned on the left side in the sputtering cavity, and the aluminum oxide target material is positioned on the right side in the sputtering cavity;
(c) In a vacuum environment, firstly depositing a high-entropy alloy layer (1) on a silicon substrate (3), then depositing an aluminum oxide layer (2), and sequentially and alternately depositing for 3-8 periods;
(d) And (c) annealing the product obtained in the step (c) in vacuum at 190-200 ℃ for 2-4 h in an argon atmosphere to obtain the anti-irradiation high-entropy alloy/ceramic multilayer film.
5. The preparation method of the radiation-resistant high-entropy alloy/ceramic multilayer film as claimed in claim 4, characterized in that: in the step (a), the silicon substrate (3) is a monocrystalline silicon wafer with a crystal orientation (100).
6. The preparation method of the radiation-resistant high-entropy alloy/ceramic multilayer film as claimed in claim 4, characterized in that: in the step (a), the etching solution is mixed by 1-3M KOH and 18-20 vol% isopropanol water solution, the power of ultrasonic stirring is 100-120 KHz, and the intensity is 50-60W/L.
7. The preparation method of the radiation-resistant high-entropy alloy/ceramic multilayer film as claimed in claim 4, characterized in that: the step (b) specifically comprises the following steps: pumping the vacuum degree of the sputtering chamber to be lower than5×10 -6 pa, introducing argon with the gas flow of 15-25 sccm, and adjusting the deposition pressure to 1.5-1.9 pa; adjusting the pre-sputtering rate of a power supply to be 100-110W, and the pre-sputtering time to be 10-15 min, wherein when the high-entropy alloy target is pre-sputtered, the alumina target baffle is in a closed state, and when the alumina target is pre-sputtered, the high-entropy alloy target baffle is in a closed state.
8. The method for preparing the radiation-resistant high-entropy alloy/ceramic multilayer film of claim 4, wherein: in the step (c), when the high-entropy alloy layer (1) is deposited, the baffle of the alumina target is in a closed state, the power supply power is 83-100W, the deposition time is 10-15 min, the rotating speed of the silicon substrate (3) is 10-12 r/min, and the bias voltage of the silicon substrate is-50V-40V.
9. The method for preparing the radiation-resistant high-entropy alloy/ceramic multilayer film of claim 4, wherein: in the step (c), when the aluminum oxide layer (2) is deposited, the baffle of the high-entropy alloy target is in a closed state, the power of a power supply is 80-92 w, the deposition time is 8-10 min, the rotating speed of the silicon substrate (3) is 10-12 r/min, and the bias voltage of the silicon substrate is-50V-40V.
10. The method for preparing the radiation-resistant high-entropy alloy/ceramic multilayer film of claim 4, wherein: the high-entropy alloy target material is Ta 20 W 20 Ti 24 V 26 Mo 10 High entropy alloy.
CN202210839902.9A 2022-07-18 2022-07-18 Anti-radiation high-entropy alloy/ceramic multilayer film and preparation method thereof Active CN115386839B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210839902.9A CN115386839B (en) 2022-07-18 2022-07-18 Anti-radiation high-entropy alloy/ceramic multilayer film and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210839902.9A CN115386839B (en) 2022-07-18 2022-07-18 Anti-radiation high-entropy alloy/ceramic multilayer film and preparation method thereof

Publications (2)

Publication Number Publication Date
CN115386839A true CN115386839A (en) 2022-11-25
CN115386839B CN115386839B (en) 2023-07-04

Family

ID=84116513

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210839902.9A Active CN115386839B (en) 2022-07-18 2022-07-18 Anti-radiation high-entropy alloy/ceramic multilayer film and preparation method thereof

Country Status (1)

Country Link
CN (1) CN115386839B (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180128952A1 (en) * 2016-11-04 2018-05-10 National Tsing Hua University Multi-Film Structure
CN108380892A (en) * 2018-04-03 2018-08-10 武汉理工大学 A kind of ceramics/high-entropy alloy laminated material and preparation method thereof
CN113151795A (en) * 2021-03-30 2021-07-23 西安交通大学 NbMoTaWAl refractory high-entropy alloy film and preparation method thereof
CN113445041A (en) * 2021-07-15 2021-09-28 山东理工大学 Preparation method of low-cost light high-entropy alloy/aluminum oxide composite coating on surface of magnesium alloy

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180128952A1 (en) * 2016-11-04 2018-05-10 National Tsing Hua University Multi-Film Structure
CN108380892A (en) * 2018-04-03 2018-08-10 武汉理工大学 A kind of ceramics/high-entropy alloy laminated material and preparation method thereof
CN113151795A (en) * 2021-03-30 2021-07-23 西安交通大学 NbMoTaWAl refractory high-entropy alloy film and preparation method thereof
CN113445041A (en) * 2021-07-15 2021-09-28 山东理工大学 Preparation method of low-cost light high-entropy alloy/aluminum oxide composite coating on surface of magnesium alloy

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
O. EL-ATWANI等: "Helium implantation damage resistance in nanocrystalline W-Ta-V-Cr high entropy alloys" *
王辉: ""含纳米空洞 YSZ/Al2O3 多层膜和纳米孔道Al0.1 FeCoNiCr 高熵合金薄膜的制备及抗辐照性能研究"" *

Also Published As

Publication number Publication date
CN115386839B (en) 2023-07-04

Similar Documents

Publication Publication Date Title
JP5968479B2 (en) Method for forming a sputtering target
CN114703452B (en) CoCrFeNi high-entropy alloy doped amorphous carbon film and preparation method thereof
CN110144484B (en) Cu-NbMoTaW alloy and preparation method thereof
JP7372312B2 (en) SiC composite substrate and composite substrate for semiconductor devices
CN113355580A (en) FeCoNiCrTiV high-entropy alloy film and preparation method thereof
CN115386839A (en) Anti-irradiation high-entropy alloy/ceramic multilayer film and preparation method thereof
Tu et al. Structure, composition and mechanical properties of reactively sputtered (TiVCrTaW) Nx high-entropy films
CN115305443B (en) Preparation method and application of zirconium-based amorphous multicomponent oxide coating
JP7272653B2 (en) STRUCTURE, LAMINATED STRUCTURE, LAMINATED STRUCTURE MANUFACTURING METHOD AND LAMINATED STRUCTURE MANUFACTURING APPARATUS
CN112962060B (en) Cr (chromium)3Al/Zr multilayer film and preparation method thereof
ZHANG et al. Influence of substrate bias on microstructure and morphology of ZrN thin films deposited by arc ion plating
CN112746256B (en) High-strength high-plasticity layered heterogeneous aluminum-based composite material and preparation method thereof
Yuk et al. Formation mechanisms of metallic Zn nanodots by using ZnO thin films deposited on n-Si substrates
CN113846303B (en) W-containing low-activation high-entropy alloy and preparation method thereof
CN113802100A (en) Method for regulating and controlling processing hardening capacity of amorphous/amorphous nano multilayer film
KR100682416B1 (en) Process for producing alumina coating composed mainly of ?-type crystal structure, alumina coating composed mainly of ?-type crystal structure, laminate coating including the alumina coating, member clad with the alumina coating or laminate coating, process for producing the member, and physical evaporation apparatus
Peifang et al. Control of growth and structure of Ag films by the driving frequency of magnetron sputtering
CN110144485B (en) Cu-Ta alloy and preparation method thereof
Jung et al. Effect of ion-beam assisted deposition on resistivity and crystallographic structure of Cr/Cu
CN114703458B (en) Application of CoCrFeNi high-entropy alloy doped amorphous carbon film in preparation of material under heavy-load working condition
CN116354739B (en) Ceramic connecting piece and preparation method and application thereof
CN113430488B (en) Nano composite coating for nuclear reactor fuel cladding and preparation method thereof
Chuang et al. Low-Temperature Die Bonding of SiC Chips with DBC Ceramic Substrates Using High-Density Ag (111) Nanotwinned Films
Jing et al. Dependence of characteristics of LaB6 films on DC magnetron sputtering power
TW202309313A (en) Metallic nano-twinned thin film structure and method for forming the same

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