CN108315705B - Structure for improving crystallization resistance of amorphous metal film material and preparation method thereof - Google Patents
Structure for improving crystallization resistance of amorphous metal film material and preparation method thereof Download PDFInfo
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- CN108315705B CN108315705B CN201810327894.3A CN201810327894A CN108315705B CN 108315705 B CN108315705 B CN 108315705B CN 201810327894 A CN201810327894 A CN 201810327894A CN 108315705 B CN108315705 B CN 108315705B
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- 239000000463 material Substances 0.000 title claims abstract description 57
- 239000005300 metallic glass Substances 0.000 title claims abstract description 45
- 238000002425 crystallisation Methods 0.000 title claims abstract description 32
- 230000008025 crystallization Effects 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 9
- 239000010408 film Substances 0.000 claims description 64
- 239000013078 crystal Substances 0.000 claims description 43
- FEBJSGQWYJIENF-UHFFFAOYSA-N nickel niobium Chemical compound [Ni].[Nb] FEBJSGQWYJIENF-UHFFFAOYSA-N 0.000 claims description 40
- 229910052721 tungsten Inorganic materials 0.000 claims description 29
- 239000010937 tungsten Substances 0.000 claims description 29
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 28
- 239000000758 substrate Substances 0.000 claims description 19
- 238000000151 deposition Methods 0.000 claims description 15
- 230000008021 deposition Effects 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 238000004544 sputter deposition Methods 0.000 claims description 7
- 239000010409 thin film Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000007769 metal material Substances 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 229910005805 NiNb Inorganic materials 0.000 claims 2
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 230000008707 rearrangement Effects 0.000 abstract description 2
- 230000007704 transition Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 47
- 238000004458 analytical method Methods 0.000 description 6
- 238000000137 annealing Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000013077 target material Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000002524 electron diffraction data Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 150000003657 tungsten Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
- 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
- C23C14/54—Controlling or regulating the coating process
- C23C14/542—Controlling the film thickness or evaporation rate
Abstract
The invention discloses a structure for improving the crystallization resistance of an amorphous metal film material and a preparation method thereof. The crystallization process of amorphous materials is a process of rearrangement and ordering of atoms, which is a thermally activated process. In the film material, the diffusion coefficient and the transition frequency of surface atoms are several times higher than those in the material, so that the atoms originally positioned on the surface can effectively present the properties similar to those of the internal atoms when the surface is covered, thereby obstructing the energy transfer process of the amorphous material and the external environment and reducing the crystallization and instability speeds of the amorphous material. Compared with a single amorphous film with the same component in a control group, the structure of the invention has stronger crystallization resistance. The method adopts the traditional magnetron sputtering means, has low cost, strong controllability and simple operation, and is easy to realize and popularize.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a structure for improving crystallization resistance of an amorphous metal film material and a preparation method thereof.
Background
In recent years, amorphous materials have attracted much attention as a new structural material. Amorphous materials have some unique properties due to their long-range disorder on an atomic scale and the lack of lattice defects like dislocations in crystals: such as high elastic strain limit, good corrosion resistance, ultra-high hardness and the like. In the last decade, the mechanical properties of amorphous materials have become a hotspot in research: it is generally accepted that the mechanical behavior of amorphous materials is influenced by shear banding, shear deformation zone (STZ), free volume or localized plastic deformation.
The properties of the material expressed macroscopically are often closely and directly related to the microstructure, and amorphous materials are not exceptional. The excellent mechanical properties of the amorphous material can be attributed to the disordered atomic structure, and the amorphous material loses advantages when converted into a crystalline structure, so that the stability of the amorphous material is particularly important. The present research suggests that the mechanical properties of amorphous alloys are affected by their structural stability (whether bulk amorphous or amorphous films, may crystallize upon heating). And the amorphous material belongs to a metastable state in thermodynamics, the amorphous material has the possibility of crystallization after annealing, and the amorphous material can be embrittled and failed due to force-induced deformation or high-pressure treatment. Therefore, it is important to improve the structural stability of the amorphous material in a thermally induced environment.
Disclosure of Invention
The invention aims to provide a structure for improving the crystallization resistance of an amorphous metal film material and a preparation method thereof, so as to solve the technical problems. The amorphous metal film material prepared by the invention has a structure that the upper surface and the lower surface of the amorphous layer are both covered by the crystalline layer. The film prepared by the process has a compact structure, and the interface layer of the crystal amorphous layer is clear. The amorphous film structure with stronger crystallization resistance and strong stability can be prepared by the method. Meanwhile, the method adopts the traditional magnetron sputtering method, and has the advantages of low cost, strong controllability, simple operation and easy realization and popularization.
In order to achieve the purpose, the invention adopts the following technical scheme:
a structure for improving the crystallization resistance of an amorphous metal film material comprises an amorphous metal film, wherein the lower surface and the upper surface of the amorphous metal film are both covered with a crystal layer to form a sandwich layer structure.
Further, the crystal layer is a metal material different from the element of the amorphous metal thin film.
Furthermore, the thermal expansion coefficients of the crystal layer material and the amorphous metal film are different.
Furthermore, the crystalline layer is made of tungsten or silver, and the amorphous metal film is made of nickel-niobium.
Furthermore, the amorphous metal film and the crystal layers covered on the lower surface and the upper surface of the amorphous metal film are all prepared by adopting a magnetron sputtering method.
Further, the crystalline layer is made of tungsten, the amorphous metal film is made of nickel niobium, and a W/NiNb/W sandwich layered structure is formed; the thickness of the NiNb amorphous metal film is 600nm, and the thickness of the two tungsten crystal layers is 60 nm.
A method for preparing a structure for improving the crystallization resistance of an amorphous metal film material comprises the following steps:
1) cleaning a substrate, and putting the substrate on a substrate table of ultrahigh vacuum magnetron sputtering equipment; placing a metal target to be sputtered on a target base;
2) the preparation of the crystal layer adopts a continuous deposition coating mode; suspending the equipment after obtaining a crystal layer, and preparing an amorphous metal film after the film is completely cooled;
3) the preparation of the amorphous metal film adopts an intermittent deposition method, the sputtering is suspended for 5-10 minutes every 15-30 minutes of deposition, the film is cooled, and then the preparation of the next amorphous metal film is carried out, wherein the deposition rate is 5-6 nm/s; when the thickness of the amorphous layer reaches a preset value, the preparation of the amorphous metal film is finished;
4) after the film is completely cooled, preparing a crystal layer by the same method in the step 2); finally obtaining the sandwich layered structure.
Compared with the prior art, the invention has the following beneficial effects:
the size of the amorphous film material in the cross section direction is small, and the structure of the amorphous film material can refer to a two-dimensional material under the nanoscale. As the dimensions of a material are reduced to nanometer-even smaller, more subtle dimensions, its specific surface area will grow rapidly. At the moment, the property of the surface of the material plays a great role in the overall performance of the material, and the invention utilizes the surface of the film material to intervene in the crystallization behavior of the amorphous material.
The method adopted by the invention has the main principle that: the crystallization process of amorphous materials is a process of rearrangement and ordering of atoms, which is a thermally activated process. In the film material, the diffusion coefficient and the transition frequency of surface atoms are several times higher than those in the material, so that the atoms originally positioned on the surface can effectively present the properties similar to those of the internal atoms when the surface is covered, thereby obstructing the energy transfer process of the amorphous material and the external environment and reducing the crystallization and instability speeds of the amorphous material.
Compared with the amorphous film prepared by the traditional method, the crystal covering amorphous structure prepared by the invention has higher crystallization resistance.
Drawings
FIG. 1 is a schematic diagram of the NiNb amorphous structure of a tungsten-coated crystal layer prepared according to the present invention, i.e., the above-mentioned "sandwich" layered structure;
FIG. 2 is an XRD structure analysis of the NiNb amorphous annealed state and the NiNb amorphous annealed state coated with the tungsten crystal layer;
FIG. 3 is an electron diffraction pattern analysis view of a selected area in a NiNb amorphous annealed high-resolution transmission photograph;
FIG. 4 is a high resolution transmission image of the amorphous annealed state of NiNb;
FIG. 5 is a TEM image of the NiNb amorphous annealed interface of the tungsten-coated crystal layer and an analysis view of a high-resolution transmission diagram thereof.
Detailed Description
The invention relates to a structure for improving crystallization resistance of an amorphous metal film material, which comprises an amorphous metal film, wherein the lower surface and the upper surface of the amorphous metal film are both covered with crystal layers to form a sandwich layer structure. The method of the invention utilizes the magnetron sputtering technology and combines the continuous deposition and the intermittent deposition coating technology to prepare the amorphous metal film material covered by the crystal so as to improve the crystallization resistance of the amorphous metal film material. In the embodiment, common metal tungsten is used as a sputtering target material to prepare the tungsten/nickel niobium/tungsten thin film material. It should be noted that, according to the preparation method adopted by the present invention, the crystal layer metal may adopt other materials according to the thermal expansion coefficient; not limited to tungsten. In order to illustrate the difference between the method and the conventional magnetron sputtering process, the preparation process characteristics of the metal film material are provided.
1. The specific technological process of the tungsten/nickel-niobium amorphous/tungsten (W/NiNb/W) film material (three layers) comprises the following steps:
1) cutting the single-side polished monocrystalline silicon substrate into required sizes by using a diamond knife, immersing the silicon substrate in acetone, ultrasonically cleaning for 15 minutes, and drying by using a blower; then ultrasonically cleaning the substrate by using ethanol for 15 minutes, drying the substrate and then placing the substrate on a substrate table of ultrahigh vacuum magnetron sputtering equipment.
2) Respectively installing a metal W target material and a NiNb amorphous target material on a target position, closing a sputtering cabin and vacuumizing.
3) When the vacuum degree in the equipment cavity reaches 10-7And when the mbar is in magnitude, the argon bottle valve can be opened. Adjusting the argon flow to 3.0sccm, simultaneously turning on a direct-current pulse power supply and a radio-frequency power supply, and simultaneously pre-sputtering the amorphous alloy target and the metal tungsten target for 15 minutes. The purpose of this step is to remove the oxide layer and contaminants that may be present on the target surface, and to ensure the purity of the components of the plated film.
4) And after the pre-sputtering is finished, adjusting the position of the substrate base to prepare for film coating. And turning on a direct current pulse power supply, and regulating the sputtering power to be 100W for sputtering.
5) The technological parameters of the crystal tungsten layer are as follows: power of the direct current pulse power supply: 100W; rotating the additional substrate table; no substrate bias; deposition temperature: and (4) room temperature. Under the parameters, the deposition is carried out for 5-10 minutes until the required film thickness is reached, and the thickness of the crystalline tungsten layer is 60 nanometers in the embodiment.
6) Deposition process parameters of the NiNb amorphous layer: power of the direct current pulse power supply: 100W; rotating the additional substrate table; no substrate bias; deposition temperature: and (4) room temperature. Under the parameters, the deposition is continuously carried out for 30 minutes, the power supply is turned off, the coating is suspended for 10 minutes, and the deposition is carried out for 30 minutes again after the deposited film is completely cooled. The above steps are repeated until the thickness of the amorphous layer reaches the desired preset thickness value, and the thickness of the amorphous layer is 600nm in the embodiment.
7) And after the amorphous layer is plated and fully cooled, covering a crystal tungsten layer on the amorphous layer, namely repeating the step 5), wherein the thickness is still 60 nanometers, namely one tenth of the thickness of the amorphous layer.
2. In this example, a control group was set to compare the crystallization resistance of the comparative materials: the specific process of the nickel-niobium (NiNb) amorphous film material (single layer) comprises the following steps:
the above 1, the process steps in the examples 1)2)3)4)6) can be simply performed.
The two amorphous materials obtained by the method are simultaneously subjected to high vacuum annealing treatment, and the heat treatment process parameters are that the vacuum degree during annealing is less than 5 × 10-4Pa; annealing temperature: 873K; annealing time: one hour; after heat treatmentAfter the finished product is finished, the furnace is cooled for more than 12 hours to room temperature, and then the product can be taken out.
The invention is described in further detail below with reference to the accompanying drawings:
FIG. 2 is an XRD structure analysis of the NiNb amorphous annealed state and the NiNb amorphous annealed state coated with the tungsten crystal layer; from the results in the figure, it can be found that: the annealed NiNb amorphous has obvious crystal peaks; whereas only the crystal peak of tungsten was observed in the NiNb amorphous in the annealed state of the tungsten-clad crystal layer. From this, it was qualitatively determined that the coverage of the tungsten crystal layer had an effect of suppressing amorphous crystallization.
FIG. 3 is a high-resolution transmission microscope selective diffraction analysis of the annealed NiNb amorphous film, and the result shows that the NiNb amorphous film is crystallized to generate a nanocrystalline phase. The experimental values in the first column of table 1 were obtained by calibrating the interplanar spacing of the selected zone electron diffraction in the photograph.
Table 1 is a comparison graph of the crystal spacing of the NiNb crystallized phase in an annealed state, and the comparison with the standard crystal spacing can confirm that the nanocrystalline phase generated after the crystallization of the NiNb amorphous film is Nb7Ni6I.e., the fourth column of table 1.
Fig. 4 is a high resolution transmission diagram analysis of the NiNb amorphous annealed state, and from the diagram, the crystallization condition in the NiNb amorphous annealing process is observed, and it can be found that: the NiNb amorphous film presents heterogeneous crystallization behavior, namely crystallization occurs near the surface, and crystal grains can be obviously observed; the amorphous structure state of disordered atomic arrangement is still kept near the silicon substrate. The result of this gradient crystallization behavior indicates that amorphous crystallization starts at the surface.
FIG. 5 is a TEM image of the interface of the NiNb amorphous annealed state of the tungsten-coated crystal layer and the analysis of the high-resolution transmission diagram thereof, and the interface between the crystal layer and the amorphous layer of the thin film can be observed to be clear. Further observing the micro-morphology of the tungsten-coated crystal layer, the NiNb amorphous micro-morphology of the tungsten-coated crystal layer is shown as follows: a large amount of nanocrystalline nuclei are embedded in the amorphous substrate in a dispersed mode, and the crystallization condition is light (compared with figure 3). Therefore, the NiNb coated with the tungsten crystal layer is amorphous, and the crystallization resistance is stronger.
The data in table 2 were obtained by quantitative statistics of the average grain size and the number of grains of the NiNb amorphous (fig. 4) and the NiNb amorphous coated with the tungsten crystalline layer (fig. 5). The average grain size in the NiNb amorphous annealed state is about 32 nanometers, while the average grain size in the NiNb amorphous annealed state of the tungsten-coated crystalline layer is only 6 nanometers. The structure of the amorphous film covered by the crystal prepared by the invention can achieve the effect of improving the crystallization resistance of the amorphous metal film material.
TABLE 1 comparison of interplanar spacing of NiNb crystalline phases
TABLE 2 statistics of the grain size and the number of grains of the NiNb amorphous layer and the NiNb amorphous layer coated with the tungsten crystal layer
Claims (5)
1. A structure for improving the crystallization resistance of an amorphous metal film material is characterized by comprising an amorphous metal film, wherein the lower surface and the upper surface of the amorphous metal film are both covered with a crystal layer to form a sandwich layer structure;
the crystal layer is a metal material different from elements of the amorphous metal film;
the material of the crystal layer is different from the thermal expansion coefficient of the amorphous metal film;
the thickness of the amorphous metal film is larger than the thickness of the crystal layer covering the lower surface and the upper surface of the amorphous metal film.
2. The structure of claim 1, wherein the crystalline layer is made of tungsten or silver, and the amorphous metal film is made of nickel-niobium.
3. The structure of claim 1, wherein the amorphous metal film and the crystal layers on the lower surface and the upper surface of the amorphous metal film are prepared by magnetron sputtering.
4. The structure for improving the crystallization resistance of the amorphous metal thin film material according to claim 1, wherein the crystalline layer is made of tungsten, and the amorphous metal thin film is made of nickel-niobium, so as to form a W/NiNb/W sandwich layered structure; the thickness of the NiNb amorphous metal film is 600nm, and the thickness of the two tungsten crystal layers is 60 nm.
5. The method for preparing a structure for improving the crystallization resistance of an amorphous metal thin film material according to any one of claims 1 to 4, comprising the following steps:
1) cleaning a substrate, and putting the substrate on a substrate table of ultrahigh vacuum magnetron sputtering equipment; placing a metal target to be sputtered on a target base;
2) the preparation of the crystal layer adopts a continuous deposition coating mode; suspending the equipment after obtaining a crystal layer, and preparing an amorphous metal film after the film is completely cooled;
3) the preparation of the amorphous metal film adopts an intermittent deposition method, the sputtering is suspended for 5-10 minutes every 15-30 minutes of deposition, the film is cooled, and then the preparation of the next amorphous metal film is carried out, wherein the deposition rate is 5-6 nm/s; when the thickness of the amorphous layer reaches a preset value, the preparation of the amorphous metal film is finished;
4) after the film is completely cooled, preparing a crystal layer by the same method in the step 2); finally obtaining the sandwich layered structure.
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