CN116145076B - A MoNbZr/Zr nano-layered material and preparation method thereof - Google Patents
A MoNbZr/Zr nano-layered material and preparation method thereof Download PDFInfo
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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
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- 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
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Abstract
The invention discloses MoNbZr/Zr nanometer layered material and a preparation method thereof, wherein MoNbZr/Zr nanometer layered material is prepared on a clean silicon substrate by a magnetron sputtering deposition method, ar+ ions bombard a target material to elastically collide with MoNbZr/Zr atoms, collision cascade is further generated, and sample atoms are excited by the collision cascade and reversely deposited on the substrate. MoNbZr atoms and Zr atoms are sequentially deposited to alternately form a multilayer nano lamellar material with different interface structures and different phase compositions in different modulation periods, and secondary electrons and other high-density plasmas generated by sputtering circularly move in a rotation line mode under the combined action of mutually perpendicular electromagnetic fields and are not contacted with a matrix. Therefore, the ionization efficiency is high and the deposition rate is fast. The invention not only successfully prepares the nano lamellar material with different phase compositions, but also obtains the nano lamellar material which is uniform and compact, has clear interface structure and excellent comprehensive performance.
Description
Technical Field
The invention belongs to the field of material surface modification, and particularly relates to MoNbZr/Zr nano lamellar material and a preparation method thereof.
Background
The high-speed development of society puts more stringent requirements on the comprehensive properties of metal structural materials, such as high plasticity, high thermal stability, high strength and the like. In order to increase the mechanical strength of the metal material, grain refinement and amorphization methods are generally employed, but at the same time the plasticity is sacrificed. The strength and plasticity are largely dependent on dislocation-defect interactions in the crystalline material and shear band deformation in the metallic glass. To address these challenges, nanostructured materials are important candidate materials.
The nanostructure material is known as a new material in twenty-first century, and the interface becomes a main structural unit of the nanostructure material due to the reduction of the characteristic size of the microstructure to the nanoscale. In recent years, interface engineering for regulating performance by designing an interface structure is becoming an important way for improving the performance of a nano-structure material. The nano lamellar material has strong designability, such as component selection and layer thickness control, can fully play the regulation and control of the interface on the performance, and in addition, most of the nano lamellar materials which are not mutually soluble in the components can form a clear heterogeneous interface on the atomic scale, so that the research on the interface effect is facilitated. And a great deal of researches prove that the high-entropy alloy film/coating in the BCC structure shows excellent oxidation resistance, corrosion resistance and irradiation resistance similar to those of the alloy under irradiation conditions, and is one of effective ways for preparing the protective film/coating of the cladding material.
In summary, for the nano lamellar material, the interface structure is one of the important factors for determining the performance of the nano lamellar material, and the comprehensive performance of the nano lamellar material, including mechanics, radiation damage resistance, thermal stability and the like, is regulated and controlled by designing the interface structure, so that the nano lamellar material has important research significance. However, the current methods for preparing nano layered materials with various interface structures are very limited and the prepared nano layered materials have poor comprehensive properties, so that it is necessary to research a preparation method of nano layered materials with different interface structures to improve the comprehensive properties of nano layered materials.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the MoNbZr/Zr nano lamellar material and the preparation method thereof, the nano lamellar material prepared by the interface regulation and control process has high purity, the deposited nano lamellar material is even and compact, the interface binding force is strong, and the comprehensive performance of the nano lamellar material is improved.
The invention is realized by the following technical scheme:
a preparation method of MoNbZr/Zr nanometer lamellar material comprises the following steps:
step 1, removing impurities and oxide films on the surface of a silicon substrate;
Step 2, in a high vacuum environment, sputtering the etched silicon substrate by adopting MoNbZr targets and Zr targets alternately, and cooling to room temperature along with a furnace after sputtering and depositing to a preset thickness to obtain a MoNbZr/Zr nano lamellar material;
In each modulation period, the formed MoNbZr component layers and Zr layers have the same thickness, the thickness is 5nm-75nm, and the thickness of the MoNbZr/Zr nano lamellar material is less than 1.4um-1.6um.
Preferably, in the step 1, the polished silicon substrate is sequentially ultrasonically cleaned in acetone and absolute ethyl alcohol and then dried, and impurities on the surface of the silicon substrate are removed;
and then, corroding the dried silicon substrate by adopting hydrofluoric acid aqueous solution, and removing the oxide film on the surface of the silicon substrate.
Preferably, the vacuum degree of the high vacuum environment in the step 2 is less than 4.0X10 -4 Pa.
Preferably, in step 2, the MoNbZr target and Zr target have a power of 200W, the argon flow rate during deposition is 60sccm, and the air pressure is 1.0Pa.
Preferably, in the step 2, the sputtering time of each modulation period MoNbZr target and Zr target is 40 to 580s and 30 to 400s, respectively.
Preferably, in step 2, the surface of the substrate is etched by using Ar+ ions under vacuum, and then pre-sputtering is performed, wherein the argon gas is introduced for at least 30s before the pre-sputtering, and the pre-sputtering time is at least 10s.
Preferably, the rotating speed of the silicon substrate in the magnetron sputtering deposition process in the step 2 is 15r/min.
A MoNbZr/Zr nanometer lamellar material comprises MoNbZr component layers and Zr layers which are alternately laminated, wherein the thicknesses of the MoNbZr component layers and the Zr layers in each modulation period are the same, the thickness of the MoNbZr/Zr nanometer lamellar material is about 1.5 mu m, and the hardness of the MoNbZr/Zr nanometer lamellar material is 5.25 GPa-6.95 GPa.
Preferably, when the layer thicknesses of MoNbZr layers and the pure Zr layers in one modulation period are 5nm respectively, the interlayer interface type formed by sputtering is a crystal/crystal non-coherent type, and the intra-MoNbZr-layer structure is a crystal/amorphous alternating double-phase structure;
When the layer thicknesses of the MoNbZr layer and the pure Zr layer in one modulation period are respectively 10-75 nm, the interlayer interface formed by sputtering is of a crystal/crystal non-coherent type, and the MoNbZr layer is of a double-phase structure with crystals embedded in an amorphous state.
Preferably, the element ratio of the MoNbZr alloy component layers is Mo: nb: zr=1:1:1.
Compared with the prior art, the invention has the following beneficial technical effects:
The invention relates to a preparation method of MoNbZr/Zr nanometer lamellar material, which comprises the steps of firstly removing impurities and oxide films on the surface of a silicon substrate through ultrasonic cleaning and erosion, so that metal atoms and silicon atoms are directly combined, and the epitaxial growth of a composite material in an oriented manner is facilitated. And then under the action of positive and negative electrode voltages, ar gas between the electrodes is ionized in a large quantity to enable Ar atoms to be ionized into Ar+ and electrons, the electrons are accelerated to fly to a substrate of the anode, and positively charged Ar+ rapidly flies to a target of the cathode under the action of an electric field and a magnetic field to bombard the target to elastically collide with sample (MoNbZr/Zr) atoms, so that a part of kinetic energy is transferred, and the out-of-position atoms are excited. The delocalized atoms further repeatedly collide with surrounding sample atoms in sequence, creating a collision cascade. When the collision cascade reaches the sample surface, the kinetic energy of the atoms far exceeds their surface binding energy, escaping into the vacuum forming a vapor. Sample atoms reversely move to a substrate (anode) for deposition, and high-density plasmas such as secondary electrons and the like with lower energy generated by collision circularly move in a spiral form under the combined action of mutually perpendicular electromagnetic fields and do not contact with the substrate. The invention adopts magnetron sputtering to deposit in turn, improves ionization rate and deposition rate, has weak scattering effect of working gas on sputtered atoms, and further improves deposition efficiency and layer interface binding force, thus, the deposition rate is fast, the ionization efficiency is high, and the prepared nano lamellar material has high purity, the deposited nano lamellar material is uniform and compact, has few defects, high purity and strong interface binding force.
The method utilizes an alloying strategy to improve the composition complexity of the BCC structural alloy, particularly the multi-principal-element medium (high) entropy alloy, and can effectively inhibit the defect induced by irradiation. This phenomenon is attributed to the composition complexity and lattice distortion effects of medium (high) entropy alloys, which can effectively alter the migration behavior of defects, thereby improving their irradiation resistance. In addition, the nano layered material prepared by the magnetron sputtering method can control the layer thickness by changing the sputtering time, so that the interface is increased, the interface is an effective trap for absorbing dislocation and capturing defects generated in the irradiation process, and the existence of the grain boundary/interface reduces the mean free path of defect migration and reduces the density of free migration defects. Therefore, the nano lamellar material with the high-density interface is beneficial to improving the irradiation resistance.
Further, the interfacial structure of MoNbZr/Zr nano-layered materials is adjusted by controlling the deposition time. In the deposition process, the collision probability among sputtered Mo atoms, nb atoms and Zr atoms in the MoNbZr alloy target is higher, and the energy is larger when the sputtering target is deposited on a substrate, so that a part of metastable amorphous structure can be formed, but the whole structure is still crystal, the sputtered Zr atoms in the Zr target are deposited to form a crystal layer, and the interface structure is of a crystal/crystal type. With the change of the deposition time, the monolayer thickness of the nano lamellar material MoNbZr/Zr changes, but it is notable that the interface between layers still keeps the crystal/crystal non-coherent interface, indicating that the interface structure is very stable, and in addition, the MoNbZr layer still keeps the crystal/amorphous dual-phase structure, except that at shorter deposition times, the layer interface has a restraining effect on the growth of crystal grains, and the crystal grain size is smaller. When the deposition time is longer, the grain size increases, and the alternating crystalline/amorphous dual phase structure in MoNbZr layers changes to a crystalline "mosaic" with an amorphous dual phase structure. The thickness and interface are important factors affecting the performance and deformation mechanism of the nano layered material, the critical shear stress required by dislocation transmission at the crystal/amorphous position can affect the hardness of the sample, and when the thickness is small, the amorphous layer is approximately transparent to dislocation movement in the crystal/amorphous alternating phase, so the layered material of the crystal/amorphous alternating phase has low hardness and good plasticity. And the layered material with the crystal embedded in the amorphous structure has high hardness and poor plasticity. Meanwhile, the interface is an effective defect absorbing well, and defects generated by helium ions and the like can be absorbed. Therefore, moNbZr/Zr nanometer lamellar materials with a multi-interface structure have guiding significance for researching and developing corrosion-resistant materials and radiation-resistant materials and exploring the motion rules of dislocation at different interface structures.
Furthermore, after the deposition is finished, the material is naturally cooled in a high-vacuum coating chamber to stabilize the interface structure of the layer, and meanwhile, the falling off of the nano lamellar material and the possible oxidation under the high-temperature condition caused by the difference of the thermal expansion coefficients of the material are avoided.
A MoNbZr/Zr nano lamellar material is characterized by that its morphology is cylindrical crystal, its size is stable in nano crystal range, its interface structure and mechanical property are changed with the change of layer thickness, moNbZr layers are made into crystal/amorphous alternate structure, its hardness is low, and MoNbZr layers are made into crystal "inlaid" in amorphous structure, its hardness is high. Uniform and compact in the layer and excellent comprehensive performance.
Drawings
FIG. 1 is a XRD pattern diagram of MoNbZr/Zr nanometer layered materials prepared by magnetron sputtering according to the invention.
FIG. 2 is a TEM sectional view of MoNbZr/Zr nanometer layered materials prepared by magnetron sputtering according to the present invention.
FIG. 3 is a graph showing nanoindentation hardness results for various modulation periods MoNbZr/Zr nanolayered materials of the invention.
Detailed Description
The invention will now be described in further detail with reference to the accompanying drawings, which illustrate but do not limit the invention.
A preparation method of MoNbZr/Zr nanometer lamellar material comprises the following steps:
step 1, removing impurities and oxide films on the surface of a silicon substrate;
specifically, firstly polishing a silicon substrate, then sequentially ultrasonically cleaning the polished silicon substrate in acetone and absolute ethyl alcohol, then drying to remove impurities on the surface of the silicon substrate, and then eroding the dried silicon substrate by adopting hydrofluoric acid aqueous solution for 60 seconds to remove an oxide film on the surface of the silicon substrate.
And 2, in a high vacuum environment, firstly, utilizing Ar+ ions to etch to further remove impurities on the surface of a substrate, then sequentially starting MoNbZr targets and Zr targets for direct current power supplies to perform pre-sputtering and formal sputtering, starting only one power supply of the targets in each modulation period, and cooling along with a furnace after the two components are alternately deposited to a preset thickness to obtain the nano layered material formed by MoNbZr and Zr alternately.
Specifically, the power of Ar+ ion etching is 200W, the etching time is at least 5min, the argon gas introducing time is at least 30s before pre-sputtering, and the pre-sputtering time is at least 10s.
The MoNbZr target power was set to 200W, the purity was not less than 99.9wt.%, and the Zr target power was set to 200W, the purity was not less than 99.9wt.%. The argon flow rate during the deposition process is set to 60sccm, the air pressure is set to 1.0Pa, the silicon substrate rotating speed during the deposition process is 15r/min, and the sputtering time is 40+/-5 s and 30+/-5 s, 80+/-5 s and 50+/-5 s, 190+/-5 s and 130+/-5 s, or 390s-270s and 580s-400s respectively. The element ratio of MoNbZr alloy component layer is Mo: nb: zr apprxeq 1:1:1.
As shown in figures 1-3, the grain morphology of the MoNbZr/Zr nano lamellar material prepared is columnar crystal, the size is stable in the range of the nano crystal, the interface structure and the mechanical property are changed along with the change of the layer thickness, wherein the MoNbZr layer is of a crystal/amorphous alternating structure in small layer thickness, the hardness is lower, and the MoNbZr layer is of a crystal embedded in an amorphous structure in large layer thickness, and the hardness is higher. Uniform and compact in the layer and excellent comprehensive performance. The thickness of the nano lamellar material is about 1.5 mu m, and the nano lamellar material is uniform and compact and has excellent comprehensive performance.
According to the preparation method of the MoNbZr/Zr nano lamellar material, firstly, a Si- (111) substrate subjected to single-sided polishing is respectively soaked in acetone and absolute ethyl alcohol solution and is subjected to ultrasonic cleaning for at least 15min, so that organic stains and dust on the surface are removed, and the interface binding force is improved. Then soaking the treated matrix in hydrofluoric acid water solution to erode for about 60s so as to remove the oxide on the surface of the matrix, thereby being beneficial to the oriented epitaxial growth of the nano lamellar material. A MoNbZr/Zr nanometer lamellar material is deposited on the surface of a clean matrix by adopting a magnetron sputtering technology, and the principle is that Ar+ ions bombard a target material (cathode) to elastically collide with atoms of a sample (MoNbZr/Zr), and a part of kinetic energy is transferred, so that off-site atoms are excited. The delocalized atoms further repeatedly collide with surrounding sample atoms in sequence, creating a collision cascade. When the collision cascade reaches the sample surface, the kinetic energy of the atoms far exceeds their surface binding energy, escaping into the vacuum forming a vapor. Sample atoms reversely move to a substrate (anode) for deposition, and high-density plasmas such as secondary electrons and the like with lower energy generated by collision circularly move in a spiral form under the combined action of mutually perpendicular electromagnetic fields and do not contact with the substrate. By adopting the magnetron sputtering deposition technology, the MoNbZr target and the Zr target both adopt direct current power supplies, and the power is 200W. The grain size of MoNbZr/Zr nano lamellar material is adjusted by controlling the deposition time, so as to change the distribution of crystal/amorphous two phases in the MoNbZr layer. When the deposition time is short, moNbZr layers are of crystal/amorphous alternating structures, and when the deposition time is long, the grain size in MoNbZr layers is increased, so that crystals are embedded in the amorphous structures. And finally, naturally cooling in a high vacuum coating chamber to avoid the falling of the nano lamellar material caused by the difference of the thermal expansion coefficients of the materials. The nano lamellar material is prevented from being oxidized when being contacted with air under the high temperature condition, and MoNbZr/Zr nano lamellar material with different modulation periods and different structures is finally formed.
Example 1
A preparation method of MoNbZr/Zr nanometer lamellar material comprises the following steps:
S1, sequentially removing impurities on the surfaces of the target and the substrate by using acetone and absolute ethyl alcohol, and then removing impurities and oxides on the surfaces of the target and the substrate by using hydrofluoric acid aqueous solution.
S2, fixing the substrate on the substrate by using conductive adhesive, mechanically and automatically conveying the substrate into a magnetron sputtering vacuum coating chamber, and pumping the substrate until the back vacuum degree is 3.6X10-4 Pa, wherein the etching power is 200W, and the etching time is 5min.
S3, starting formal sputtering after etching is finished, namely firstly introducing argon for 30 seconds, pre-sputtering for 10 seconds, and then sequentially sputtering by using a double direct current power supply to deposit MoNbZr/Zr nano lamellar materials on a clean silicon substrate;
Wherein, the power of MoNbZr targets (purity 99.95 wt.%) and Zr targets (purity 99.99 wt.%) are 200W, the flow rate of argon is 60sccm, the deposition pressure is set to 1.0Pa, the deposition temperature is room temperature, the rotating speed of a base plate is 15r/min, a MoNbZr target power supply and a Zr target power supply are sequentially started for deposition, the deposition time of MoNbZr targets is 40s, the deposition time of Zr targets is 30s, the deposition is 150 times in a circulating way, and the total deposition time is 14400s;
S4, naturally cooling the sample in a high vacuum coating chamber for 2-3 hours to room temperature, and withdrawing to obtain the nanocrystalline MoNbZr/Zr nano lamellar material with the modulation period thickness of lambda=10nm, the MonbZr layer thickness of hA=5nm (A-MoNbZr) and the Zr layer thickness of hb=5nm (B-Zr), wherein the thickness of the nano lamellar material is about 1.5 mu m.
And carrying out microstructure characterization and mechanical property test on the MoNbZr/Zr nano lamellar material, wherein crystal grains are columnar crystals, the type of an interlayer interface is crystal/crystal non-coherent, moNbZr layers are crystal/amorphous alternating structures, and the hardness of the nano lamellar material is 5.25+/-0.04 GPa when nano-indentation is measured under the load of 6000 mu N.
Example 2
A preparation method of MoNbZr/Zr nanometer lamellar material comprises the following steps:
S1, sequentially removing impurities on the surfaces of the target and the substrate by using acetone and absolute ethyl alcohol, and then removing impurities and oxides on the surfaces of the target and the substrate by using hydrofluoric acid aqueous solution.
S2, fixing the substrate on the substrate by using conductive adhesive, mechanically and automatically conveying the substrate into a magnetron sputtering vacuum coating chamber, and pumping the substrate until the back vacuum degree is 2.4X10-4 Pa, wherein the etching power is 200W, and the etching time is 5min.
S3, starting formal sputtering after etching is finished, namely firstly introducing argon for 30 seconds, pre-sputtering for 10 seconds, and then sequentially sputtering by using a double direct current power supply to deposit MoNbZr/Zr nano lamellar materials on a clean silicon substrate, wherein the power of a MoNbZr target (purity is 99.95 wt.%) and the power of a Zr target (purity is 99.99 wt.%) are 200W, the flow rate of the argon is 60sccm, the deposition air pressure is set to be 1.0Pa, the deposition temperature is room temperature, the rotating speed of the substrate is 15r/min, a MoNbZr target power supply and a Zr target power supply are sequentially started for deposition, the deposition time of the MoNbZr target in one modulation period is 80 seconds, the deposition time of the Zr target is 50 seconds, the cyclic deposition is 75 times, and the total deposition time is 11700 seconds.
S4, naturally cooling the sample in a high vacuum coating chamber for 2-3 hours to room temperature, and withdrawing to obtain the nanocrystalline MoNbZr/Zr nano lamellar material with the modulation period thickness lambda=20nm, the MonbZr layer thickness hA=10nm and the Zr layer thickness hB=10nm, wherein the thickness of the nano lamellar material is about 1.5 mu m.
And carrying out microstructure characterization and mechanical property test on the MoNbZr/Zr nano lamellar material, wherein crystal grains are columnar crystals, the type of an interlayer interface is crystal/crystal non-coherent, moNbZr layers are crystal embedded in an amorphous structure, and the hardness of the nano lamellar material is 5.51+/-0.06 GPa measured by nano indentation under the load of 6000 mu N.
Example 3
A preparation method of MoNbZr/Zr nanometer lamellar material comprises the following steps:
S1, sequentially removing impurities on the surfaces of the target and the substrate by using acetone and absolute ethyl alcohol, and then removing impurities and oxides on the surfaces of the target and the substrate by using hydrofluoric acid aqueous solution.
S2, fixing the substrate on the substrate by using conductive adhesive, mechanically and automatically conveying the substrate into a magnetron sputtering vacuum coating chamber, and pumping the substrate until the back vacuum degree is 3.2X10-4 Pa, wherein the etching power is 200W, and the etching time is 5min.
S3, starting formal sputtering after etching is finished, namely firstly introducing argon for 30S, pre-sputtering for 10S, then sequentially sputtering by using a double direct current power supply to deposit MoNbZr/Zr nano lamellar materials on a clean silicon substrate, wherein the power of a MoNbZr target (purity is 99.95 wt.%) and the power of a Zr target (purity is 99.99 wt.%) are 200W, the argon flow rate is 60sccm, the deposition air pressure is set to be 1.0Pa, the deposition temperature is room temperature, the rotating speed of the substrate is 15r/min, the MoNbZr target direct current power supply and the Zr target direct current power supply are sequentially started for deposition, the deposition time of the MoNbZr target is 190s in one modulation period, the deposition time of the Zr target is 130S, the cyclic deposition is 30 times, and the total deposition time is 10380S.
S4, naturally cooling the sample in a high vacuum coating chamber for 2-3 hours to room temperature, and withdrawing to obtain the nanocrystalline MoNbZr/Zr nano lamellar material with the modulation period thickness lambda=50nm, the MonbZr layer thickness hA=25nm and the Zr layer thickness hB=25nm, wherein the thickness of the nano lamellar material is about 1.5 mu m.
And carrying out microstructure characterization and mechanical property test on the MoNbZr/Zr nano lamellar material, wherein crystal grains are columnar crystals, the type of an interlayer interface is crystal/crystal non-coherent, moNbZr layers are crystal embedded in an amorphous structure, and the hardness of the nano lamellar material is 6.95+/-0.07 GPa when nano-indentation is measured under 6000 mu N load.
Example 4
A preparation method of MoNbZr/Zr nanometer lamellar material comprises the following steps:
S1, sequentially removing impurities on the surfaces of the target and the substrate by using acetone and absolute ethyl alcohol, and then removing impurities and oxides on the surfaces of the target and the substrate by using hydrofluoric acid aqueous solution.
S2, fixing the substrate on the substrate by using conductive adhesive, mechanically and automatically conveying the substrate into a magnetron sputtering vacuum coating chamber, and pumping the substrate until the back vacuum degree is 2.7X10-4 Pa, wherein the etching power is 200W, and the etching time is 5min.
S3, starting formal sputtering after etching is finished, namely firstly introducing argon for 30S, pre-sputtering for 10S, then sequentially sputtering by using a double direct current power supply to deposit MoNbZr/Zr nano lamellar materials on a clean silicon substrate, wherein the power of a MoNbZr target (purity is 99.95 wt.%) and the power of a Zr target (purity is 99.99 wt.%) are 200W, the argon flow rate is 60sccm, the deposition air pressure is set to be 1.0Pa, the deposition temperature is room temperature, the rotating speed of the substrate is 15r/min, the MoNbZr target direct current power supply and the Zr target direct current power supply are sequentially started for deposition, the deposition time of the MoNbZr target is 390S, the deposition time of the Zr target is 270S, the cyclic deposition is 15 times, and the total deposition time is 10290S.
S4, naturally cooling the sample in a high vacuum coating chamber for 2-3 hours to room temperature, and withdrawing to obtain the nanocrystalline MoNbZr/Zr nano lamellar material with the modulation period thickness lambda=100 nm, the MonbZr layer thickness hA=50 nm and the Zr layer thickness hB=50 nm, wherein the thickness of the nano lamellar material is about 1.5 mu m.
And carrying out microstructure characterization and mechanical property test on the MoNbZr/Zr nano lamellar material, wherein crystal grains are columnar crystals, the type of an interlayer interface is crystal/crystal non-coherent, moNbZr layers are crystal embedded in an amorphous structure, and the hardness of the nano lamellar material is 6.55+/-0.06 GPa measured by nano indentation under the load of 6000 mu N.
Example 5
A preparation method of MoNbZr/Zr nanometer lamellar material comprises the following steps:
S1, sequentially removing impurities on the surfaces of the target and the substrate by using acetone and absolute ethyl alcohol, and then removing impurities and oxides on the surfaces of the target and the substrate by using hydrofluoric acid aqueous solution.
S2, fixing the substrate on the substrate by using conductive adhesive, mechanically and automatically conveying the substrate into a magnetron sputtering vacuum coating chamber, and pumping the substrate until the back vacuum degree is 1.0X10-4 Pa, wherein the etching power is 200W, and the etching time is 5min.
S3, starting formal sputtering after etching is finished, namely firstly introducing argon for 30S, pre-sputtering for 10S, and then sequentially sputtering by using a double direct current power supply to deposit MoNbZr/Zr nano lamellar materials on a clean silicon substrate, wherein the power of a MoNbZr target (purity is 99.95 wt.%) and the power of a Zr target (purity is 99.99 wt.%) are 200W, the flow rate of the argon is 60sccm, the deposition air pressure is set to be 1.0Pa, the deposition temperature is room temperature, the rotating speed of the substrate is 15r/min, a MoNbZr target power supply and a Zr target power supply are sequentially started for deposition, the deposition time of the MoNbZr target in one modulation period is 580S, the deposition time of the Zr target is 400S, the cyclic deposition is 10 times, and the total deposition time is 10060S.
S4, naturally cooling the sample in a high vacuum coating chamber for 2-3 hours to room temperature, and withdrawing to obtain the nanocrystalline MoNbZr/Zr nano lamellar material with the modulation period thickness lambda=150 nm, the MonbZr layer thickness hA=75 nm and the Zr layer thickness hB=75 nm, wherein the thickness of the nano lamellar material is about 1.5 mu m.
And carrying out microstructure characterization and mechanical property test on the MoNbZr/Zr nano lamellar material, wherein crystal grains are columnar crystals, the type of an interlayer interface is crystal/crystal non-coherent, moNbZr layers are crystal embedded in an amorphous structure, and the hardness of the nano lamellar material is 6.38+/-0.14 GPa when nano-indentation is measured under 6000 mu N load.
The invention discloses MoNbZr/Zr nanometer layered material and a preparation method thereof, wherein MoNbZr/Zr nanometer layered material is prepared on a clean silicon substrate by a magnetron sputtering deposition method, ar+ ions bombard a target material (cathode) to elastically collide with sample (MoNbZr/Zr) atoms, collision cascade is further generated, and the sample atoms are excited and reversely deposited on the substrate. MoNbZr atoms and Zr atoms are sequentially deposited to alternately form a multilayer nano lamellar material with different interface structures and different phase compositions in different modulation periods, and secondary electrons and other high-density plasmas generated by sputtering circularly move in a rotation line mode under the combined action of mutually perpendicular electromagnetic fields and are not contacted with a matrix. Therefore, the ionization efficiency is high and the deposition rate is fast. The invention not only successfully prepares the nano lamellar material with different interface structures, but also obtains the nano lamellar material which is even and compact, has clear interface structure and excellent comprehensive performance.
The above is only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present invention falls within the protection scope of the claims of the present invention.
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