CN111926303A - Preparation method of high-entropy alloy film - Google Patents
Preparation method of high-entropy alloy film Download PDFInfo
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- CN111926303A CN111926303A CN202010843942.1A CN202010843942A CN111926303A CN 111926303 A CN111926303 A CN 111926303A CN 202010843942 A CN202010843942 A CN 202010843942A CN 111926303 A CN111926303 A CN 111926303A
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- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 13
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- 238000000137 annealing Methods 0.000 claims abstract description 9
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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
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Abstract
The invention relates to a preparation method of a high-entropy alloy film, which comprises the following steps: cleaning the substrate; placing the substrate on a sample table of a vacuum chamber of a magnetron sputtering instrument; putting the high-entropy alloy target material at a sputtering cathode of a vacuum chamber; vacuumizing the vacuum chamber to make the vacuum degree less than 1 x 10‑4Pa; introducing argon into a vacuum chamber; starting a magnetron sputtering instrument, adjusting sputtering power, ionizing argon under the action of a radio-frequency electric field, bombarding the surface of the target by ionized argon ions, sputtering a large amount of target atoms from the target, and depositing on a substrate to form a film; sampling and annealing to obtain the high-entropy alloy film. According to the invention, argon is ionized under the action of a radio frequency electric field, and ionized argon ions bombard the surface of the target material to sputter a large amount of metal atoms on the surface of the target material, so as to form the alloy film. The preparation method has good repeatability, and the prepared film has high bonding degree with the substrate, small porosity, good stability, smooth appearance and good continuity。
Description
Technical Field
The invention relates to the technical field of high-entropy alloy film preparation, in particular to a preparation method of a high-entropy alloy film.
Background
In recent years, a material named as high-entropy alloy is receiving more and more attention from researchers. Generally, an alloy material is obtained by adding a small amount of other elements to a certain main metal material element. Different from the design of the traditional alloy, the high-entropy alloy is a new material which is different from the original metal performance and is formed by mixing a plurality of (five or more) metal elements with high concentration (about 5 to 35 percent of each element).
The "cocktail effect" originally means that two wines mixed together may exhibit one or two tastes according to different proportions, and sometimes may produce another completely new taste. Similarly, when designing the high-entropy alloy, a plurality of metal elements are uniformly mixed in the same or different proportions by using a certain preparation method, and the prepared high-entropy alloy material may show one or more excellent properties. According to related research reports, the high-entropy alloy film generally has the characteristics of good mechanical property, electricity property, corrosion resistance, wear resistance, corrosion resistance, high temperature resistance and the like, and can be applied to a plurality of fields such as high-speed cutting tools, oil pressure air pressure rods, golf ball head striking surfaces, hard surfaces of steel pipes and rolling cylinders, high-frequency soft magnetic films and the like. The good corrosion resistance of the high-entropy alloy also enables the high-entropy alloy to be widely applied to chemical plants and ship industries. In addition, the method has wider application prospect in advanced manufacturing industrial fields of electrothermal materials, hydrogen storage materials, IC diffusion barrier layers, micro-electro-mechanical system components and the like.
However, the existing preparation method is not only uncontrollable in preparation process, but also unsatisfactory in the prepared high-entropy alloy film.
Disclosure of Invention
The invention aims to provide a preparation method of a high-entropy alloy film, which has good repeatability, and the prepared high-entropy alloy film has higher stability.
In order to achieve the purpose, the invention provides the following scheme:
a preparation method of a high-entropy alloy thin film comprises the following steps:
cleaning the substrate; placing the substrate on a sample table of a vacuum chamber of a magnetron sputtering instrument; putting the high-entropy alloy target material at a sputtering cathode of a vacuum chamber;
vacuumizing the vacuum chamber to make the vacuum degree less than 1 x 10-4Pa；
Introducing nitrogen into the vacuum chamber for cleaning; introducing argon into the vacuum chamber after cleaning, and adjusting the pressure of the vacuum chamber to working pressure;
starting a magnetron sputtering instrument, adjusting sputtering power, ionizing argon under the action of a radio-frequency electric field, bombarding the surface of the target by ionized argon ions, sputtering a large amount of target atoms from the target, and depositing on a substrate to form a film;
sampling and annealing to obtain the high-entropy alloy film.
Optionally, the high-entropy alloy target is an AlFeNiCrCu target, and the purity is greater than 99.9%.
Optionally, the substrate cleaning specifically comprises: the substrate was ultrasonically cleaned in acetone, absolute ethanol and deionized water for 15min, respectively, and then the surface moisture of the substrate was dried with a suction bulb.
Optionally, the substrate is high-purity Si or SiO2(ii)/Si, size 4 x 4cm2。
Optionally, the high-purity Si substrate is a single-side polished Si single crystal wafer, the resistivity is 10K omega cm, and the purity is more than 99.9%.
Optionally, the SiO2Si is a layer of SiO with the thickness of 300nm grown on a high-purity Si substrate2And (3) a membrane.
Optionally, the sputtering power is 120W, and the sputtering time is 60 min. The sputtering mode is radio frequency magnetron sputtering.
Optionally, the flow rate of the introduced argon gas is 30 sccm.
Optionally, the working pressure is 1 Pa.
Optionally, the annealing temperature is 800 DEG C
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention discloses a preparation method of a high-entropy alloy film, which comprises the following steps: cleaning the substrate; placing the substrate on a sample table of a vacuum chamber of a magnetron sputtering instrument; putting the high-entropy alloy target material at a sputtering cathode of a vacuum chamber; vacuumizing the vacuum chamber to make the vacuum degree less than 1 x 10-4Pa; introducing nitrogen into the vacuum chamber for cleaning; introducing argon into the vacuum chamber after cleaning, and adjusting the pressure of the vacuum chamber to working pressure; starting a magnetron sputtering instrument, adjusting sputtering power, ionizing argon under the action of a radio-frequency electric field, bombarding the surface of the target by ionized argon ions, sputtering a large amount of target atoms from the target, and depositing on a substrate to form a film; sampling and annealing to obtain the high-entropy alloy film. According to the invention, argon is ionized under the action of a radio frequency electric field, ionized argon ions bombard the surface of a target material, a large number of metal atoms on the surface of the target material are sputtered, deposited on a substrate to form a film, and annealed in the air to form a high-entropy alloy film. The method has good repeatability, and the prepared film has high bonding degree with the substrate, small porosity, good stability, smooth appearance and good continuity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is a flow chart of a method for preparing a high-entropy alloy thin film according to an embodiment of the present invention;
FIG. 2 is a cross-sectional scanning electron microscope image of a high-entropy alloy thin film prepared according to an embodiment of the present invention;
FIG. 3 is another scanning electron microscope cross-sectional view of the prepared high-entropy alloy thin film provided by the embodiment of the invention;
FIG. 4 is an XRD spectrum of the prepared high-entropy alloy thin film provided by the embodiment of the invention;
FIG. 5 is a Raman spectrum of the prepared high-entropy alloy thin film provided by the embodiment of the invention;
FIG. 6 is a diagram of Al element distribution of a high-entropy alloy thin film prepared according to an embodiment of the present invention;
FIG. 7 is a diagram of a distribution of Fe element in a high-entropy alloy thin film prepared according to an embodiment of the present invention;
FIG. 8 is a distribution diagram of Ni element of the prepared high-entropy alloy thin film provided by the embodiment of the invention;
FIG. 9 is a diagram of a distribution of Cr elements in a high-entropy alloy thin film prepared according to an embodiment of the present invention;
FIG. 10 is a Cu element distribution diagram of a prepared high-entropy alloy thin film provided by an embodiment of the invention;
FIG. 11 is a diagram of distribution of O element in the prepared high-entropy alloy thin film provided by the embodiment of the invention;
FIG. 12 is a diagram of the overall element distribution of the prepared high-entropy alloy thin film provided by the embodiment of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a preparation method of a high-entropy alloy film, which has good repeatability, and the prepared high-entropy alloy film has higher stability.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1
Fig. 1 is a flowchart of a method for preparing a high-entropy alloy thin film according to an embodiment of the present invention, and as shown in fig. 1, the method includes:
step 101: and cleaning the substrate. The substrate is placed on a sample stage of a vacuum chamber of a magnetron sputtering apparatus. The high-entropy alloy target is placed at the sputtering cathode of a vacuum chamber.
Preferably, the substrate in this embodiment is high purity Si or SiO2(ii)/Si, size 4 x 4cm2Or larger in size. Wherein the high-purity Si substrate is a single-side polished Si single crystal wafer, the resistivity is 10K omega cm, and the purity is more than 99.9%. SiO 22Si is a layer of SiO with the thickness of 300nm grown on a high-purity Si substrate2The film, the remaining parameters were consistent with the high purity Si substrate.
Preferably, the high-entropy alloy target is an AlFeNiCrCu target, and the purity is more than 99.9%.
In this example, the substrate cleaning process was as follows: the substrate was ultrasonically cleaned in acetone, absolute ethanol and deionized water for 15min, respectively, and then the surface moisture of the substrate was dried with a suction bulb.
Step 102: vacuumizing the vacuum chamber to make the vacuum degree less than 1 x 10-4Pa. Alternatively, it may be greater than 1 x 10-4Pa。
Step 103: the vacuum chamber was purged with nitrogen gas. And introducing argon into the vacuum chamber after cleaning, and adjusting the pressure of the vacuum chamber to working pressure. Preferably, the flow rate of the argon gas is 30sccm, and the working pressure is 1 Pa.
Step 104: starting the magnetron sputtering instrument, adjusting the sputtering power, ionizing the argon under the action of a radio-frequency electric field, bombarding the surface of the target by ionized argon ions, sputtering a large amount of target atoms from the target, and depositing on the substrate to form a film. Preferably, the sputtering power is 120W and the sputtering time is 60 min. The sputtering mode is radio frequency sputtering.
Step 105: sampling and annealing to obtain the high-entropy alloy film. Wherein the annealing temperature is 800 ℃.
The principle of the invention is as follows:
under the vacuum condition, argon atoms are subjected to the action of a radio frequency electric field, electrons move in an accelerated manner, so that the argon atoms are ionized to generate a large amount of argon ions and free electrons. The ionized electrons move to the radio frequency anode and continuously collide with argon atoms to ionize the argon atoms, and more argon ions and electrons are generated. The argon ions move in an accelerated manner under the action of an electric field to bombard the surface of a sputtering cathode (AlFeNiCrCu target), so that a large number of metal atoms on the surface of the target are sputtered off, and an AlFeNiCrCu film is deposited on the substrate. Fig. 2 is a sectional scanning electron microscope image of the prepared high-entropy alloy thin film provided by the embodiment of the invention, and fig. 3 is another sectional scanning electron microscope image of the prepared high-entropy alloy thin film provided by the embodiment of the invention, as shown in fig. 2 and fig. 3, the prepared high-entropy alloy thin film has uniform thickness, flat, continuous, smooth and compact surface appearance, and the thin film is tightly combined with a substrate material.
After the preparation was completed, analysis was performed using an X-ray diffractometer, a Raman spectrometer, and a Scanning Electron Microscope (SEM). Fig. 4 is an XRD spectrum of the prepared high-entropy alloy thin film provided by the embodiment of the present invention, and as shown in fig. 4, diffraction peaks of XRD appear at about 36 °, 44 °, 52 ° and 63 °. By analyzing the diffraction peaks, it was found that a solid solution phase of FCC (face centered cubic) structure was formed in the alloy thin film, and no complex intermetallic compound was formed.
FIG. 5 is a Raman spectrum of the high-entropy alloy thin film prepared according to the embodiment of the present invention, wherein the high-purity Si and SiO are processed under the same conditions2Raman spectrum of AlFeNiCrCu system high entropy alloy prepared on/Si substrate, which can be seen at 715cm-1Has a weak peak which is gamma-Fe of cubic phase2O3(related literature: Begonia populi. Steel atmospheric corrosion rust layer laser Raman Spectroscopy study [ J)]Optical scattering journal 2007, 19 (2): 134-04) is generated by annealing and oxidation in air. Otherwise located at 521cm-1And 950cm-1The peak represents a Si peak, and no other diffraction peaks exist in the whole view, which indicates that the prepared AlFeNiCrCu high-entropy alloy does not generate a complex compound which can be detected by a Raman spectrum and is mutually verified with the XRD spectrum result.
As can be seen from FIGS. 6 to 12, the sample elements are uniformly distributed, and no composition segregation occurs, so that the prepared alloy thin film is a uniform single solid solution. Due to the high mixing entropy effect, the mixing entropy is larger, but the system is stable, the intermiscibility among various elements is increased, the uniform mixing among various elements is facilitated, and the formation of intermetallic compounds is also inhibited, so that a single cubic phase structure is formed.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention directly utilizes the magnetron sputtering instrument to deposit high-purity silicon or SiO2Depositing an AlFeNiCrCu system high-entropy alloy film on a Si substrate. Compared with other methods, the method has the advantages of good repeatability, high bonding degree of the prepared film and the substrate, small porosity, good stability, smooth appearance and good continuity.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to assist in understanding the core concepts of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. A preparation method of a high-entropy alloy film is characterized by comprising the following steps:
cleaning the substrate; placing the substrate on a sample table of a vacuum chamber of a magnetron sputtering instrument; putting the high-entropy alloy target material at a sputtering cathode of a vacuum chamber;
vacuumizing the vacuum chamber to make the vacuum degree less than 1 x 10-4Pa；
Introducing nitrogen into the vacuum chamber for cleaning; introducing argon into the vacuum chamber after cleaning, and adjusting the pressure of the vacuum chamber to working pressure;
starting a magnetron sputtering instrument, adjusting sputtering power, ionizing argon under the action of a radio-frequency electric field, bombarding the surface of the target by ionized argon ions, sputtering a large amount of target atoms from the target, and depositing on a substrate to form a film;
sampling and annealing to obtain the high-entropy alloy film.
2. The method according to claim 1, wherein the high entropy alloy target is an AlFeNiCrCu target with a purity of more than 99.9%.
3. The method according to claim 1, wherein the cleaning of the substrate is in particular: the substrate was ultrasonically cleaned in acetone, absolute ethanol and deionized water for 15min, respectively, and then the surface moisture of the substrate was dried with a suction bulb.
4. The method according to claim 1, wherein the substrate is high purity Si or SiO2(ii)/Si, size 4 x 4cm2。
5. The production method according to claim 4, wherein the high purity Si substrate is a single-side polished Si single crystal wafer having a resistivity of 10K Ω -cm and a purity of more than 99.9%.
6. The method of claim 4, wherein the SiO is2Si is a layer of SiO with the thickness of 300nm grown on a high-purity Si substrate2And (3) a membrane.
7. The method according to claim 1, wherein the sputtering power is 120W and the sputtering time is 60 min. The sputtering mode is radio frequency magnetron sputtering.
8. The method according to claim 1, wherein the argon gas is introduced at a flow rate of 30 sccm.
9. The method of claim 1, wherein the operating pressure is 1 Pa.
10. The method of claim 1, wherein the annealing temperature is 800 ℃.
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Cited By (2)
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| CN116237214A (en) * | 2022-12-13 | 2023-06-09 | 中国科学院合肥物质科学研究院 | Al-Y-Cr-Fe-Er-O high-entropy composite oxide hydrogen-resistant coating and preparation method thereof |
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| CN113802101A (en) * | 2021-08-25 | 2021-12-17 | 西安交通大学 | Method for regulating and controlling creep property of nanocrystalline high-entropy alloy |
| CN116237214A (en) * | 2022-12-13 | 2023-06-09 | 中国科学院合肥物质科学研究院 | Al-Y-Cr-Fe-Er-O high-entropy composite oxide hydrogen-resistant coating and preparation method thereof |
| CN116237214B (en) * | 2022-12-13 | 2024-01-26 | 中国科学院合肥物质科学研究院 | Al-Y-Cr-Fe-Er-O high-entropy composite oxide hydrogen-resistant coating and preparation method thereof |
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