CN113463051A - Thin film material and preparation method and application thereof - Google Patents

Thin film material and preparation method and application thereof Download PDF

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CN113463051A
CN113463051A CN202110747162.1A CN202110747162A CN113463051A CN 113463051 A CN113463051 A CN 113463051A CN 202110747162 A CN202110747162 A CN 202110747162A CN 113463051 A CN113463051 A CN 113463051A
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noble metal
film material
present
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mosi
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CN113463051B (en
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任萍
王港港
杨晓阳
邱剑勋
司衍鑫
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Yantai University
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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
    • 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
    • C23C14/06—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

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  • Engineering & Computer Science (AREA)
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Abstract

The invention provides a thin film material and a preparation method and application thereof, belonging to the technical field of protective materials. The invention provides a film material which comprises a molybdenum element, a silicon element and a noble metal element, wherein the noble metal element is gold or silver, the content of the molybdenum element is 28-35 at.%, the content of the silicon element is 60-70 at.%, the content of the noble metal element is 0.5-1.5 at.%, and the noble metal element exists in a single atom form. In the invention, the introduction of the noble metal Au or Ag single atom can regulate and control MoSi2The microstructure of (a), confining MoSi2Grain size of (1), increasing MoSi2The compactness of the film is improved, the intrinsic brittleness of the film is improved, and the toughness of the film is improved, so that the hardness and the fracture toughness of the film material are improved. And the introduction of Au monoatomic or Ag monoatomic can greatly reduce MoSi2The friction coefficient of the film has important significance for the engine transmission mechanism.

Description

Thin film material and preparation method and application thereof
Technical Field
The invention relates to the technical field of protective materials, in particular to a thin film material and a preparation method and application thereof.
Background
With the rapid development of aerospace industry, the premise that the aero-engine can stably run is that whether the transmission mechanism of the aero-engine, such as a gear and a spline, can bear severe working environment. This not only requires the transmission mechanism of the engine to have high hardness, toughness and wear resistance, but also the service life is of great importance. On the other hand, friction between different parts needs to be borne between the transmission mechanisms, the transmission efficiency between the transmission mechanisms can be reduced due to a large friction coefficient, and the transmission efficiency can be improved due to a low friction coefficient. Meanwhile, on the premise of ensuring the stable operation of the engine transmission mechanism, the influence of the engine transmission mechanism on the air environment is reduced. The development of the film technology has obvious effects on improving the surface hardness and toughness of the material and reducing the friction coefficient of the surface.
In recent years, it has been found that a transition metal silicide has high hardness, high wear resistance and oxidation resistance, and has a remarkable effect in improving material properties as a hard protective film. Molybdenum disilicide as a transition metal silicide has the dual properties of metal and ceramic, and has high wear resistance, corrosion resistance and oxidation resistance. Simultaneous MoSi2Is also a renewable, nontoxic and environment-friendly material, which makes the material the first choice of the protective film. However, MoSi2Its inherent brittleness limits further improvement of its mechanical properties.
Disclosure of Invention
In view of the above, the present invention aims to provide a thin film material, and a preparation method and an application thereof. The film material provided by the invention has high hardness and good fracture toughness.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a film material which comprises a molybdenum element, a silicon element and a noble metal element, wherein the noble metal element is gold or silver, the content of the molybdenum element is 28-35 at.%, the content of the silicon element is 60-70 at.%, the content of the noble metal element is 0.5-1.5 at.%, and the noble metal element exists in a single atom form.
Preferably, the content of the noble metal element is 0.8 to 1.0 at.%.
Preferably, the molybdenum element is present in an amount of 30.6 at.%, the silicon element is present in an amount of 68.9 at.%, and the gold is present in an amount of 0.5 at.%.
Preferably, the molybdenum element is present in an amount of 31.7 at.%, the silicon element is present in an amount of 67.5 at.%, and the gold is present in an amount of 0.8 at.%.
Preferably, the molybdenum element is present in an amount of 32.4 at.%, the silicon element is present in an amount of 66.1 at.%, and the gold is present in an amount of 1.5 at.%.
Preferably, the molybdenum element is present in an amount of 32.3 at.%, the silicon element is present in an amount of 66.7 at.%, and the silver is present in an amount of 1.0 at.%.
The invention also provides a preparation method of the film material in the technical scheme, which comprises the following steps:
using MoSi2And carrying out magnetron sputtering deposition on the surface of the substrate simultaneously to obtain the film material, wherein the noble metal target material is an Au target material or an Ag target material.
Preferably, the MoSi is sputtered during the magnetron sputtering deposition2The direct current constant current of the target material is 0.5A, the power for sputtering the noble metal target material is 0-50W, and the power for sputtering the noble metal target material is not 0.
Preferably, the working pressure of the magnetron sputtering deposition is 0.6-0.8 Pa.
The invention also provides the application of the film material in the technical scheme or the film material prepared by the preparation method in the technical scheme in an aircraft engine transmission mechanism.
The invention provides a film material which comprises a molybdenum element, a silicon element and a noble metal element, wherein the noble metal element is gold or silver, the content of the molybdenum element is 28-35 at.%, the content of the silicon element is 60-70 at.%, the content of the noble metal element is 0.5-1.5 at.%, and the noble metal element exists in a single atom form. In the invention, the introduction of the noble metal Au or Ag single atom can regulate and control MoSi2Is smallStructural confinement of MoSi2Grain size of (1), increasing MoSi2The compactness of the film is improved, the intrinsic brittleness of the film is improved, and the toughness of the film is improved, so that the hardness and the fracture toughness of the film material are improved. And a small amount of Au monoatomic or Ag monoatomic is doped to ensure MoSi2The wear resistance of the wear-resistant steel is improved, the toughness of the wear-resistant steel is improved, and the friction coefficient of the wear-resistant steel under the oil lubrication condition is reduced. The invention proves the application potential of the transition metal silicide in the engine transmission mechanism and simultaneously plays a certain role in the lightweight design of the engine transmission mechanism. Therefore, the film material prepared by the method has good development and application prospects in the transmission mechanism of the aircraft engine, and has important significance for the transmission mechanism of the engine.
The invention also provides a preparation method of the film material in the technical scheme, and the film material is prepared by adopting a magnetron sputtering deposition technology, so that the method is simple and rapid, and the flow is short.
Furthermore, the invention can control the content of noble metal single atoms by changing the power of the noble metal target material; the thickness of the film material can be controlled by controlling the time of magnetron sputtering deposition.
Drawings
FIG. 1 is an XRD pattern of various thin film materials prepared in examples 1-3;
FIG. 2 is a high resolution plot of the thin film material prepared in example 2;
FIG. 3 is an electron diffraction pattern of a corresponding selected area of the thin film material prepared in example 2;
FIG. 4 is a high resolution plot of the film material prepared in comparative example 2;
FIG. 5 is a corresponding selected area electron diffraction pattern for the thin film material prepared in comparative example 2;
FIG. 6 is a graph showing the friction coefficient of the films prepared in examples 1 to 3 and comparative examples 1 to 2.
Detailed Description
The invention provides a film material which comprises a molybdenum element, a silicon element and a noble metal element, wherein the noble metal element is gold or silver, the content of the molybdenum element is 28-35 at.%, the content of the silicon element is 60-70 at.%, the content of the noble metal element is 0.5-1.5 at.%, and the noble metal element exists in a single atom form.
In the invention, the thickness of the film material is preferably 1-1.5 μm.
In the present invention, the content of the noble metal element is preferably 0.8 to 1.0 at.%. In the invention, the noble metal element replaces MoSi2Si atom in (1).
In the invention, the molybdenum element and the silicon element are MoSi2Said MoSi being present2Corresponds to a hexagonal structure of C40 and is preferentially oriented to the (111) plane.
In one embodiment of the present invention, the molybdenum element is present in an amount of 30.6 at.%, the silicon element is present in an amount of 68.9 at.%, and the gold is present in an amount of 0.5 at.% or
The content of the molybdenum element is 31.7 at.%, the content of the silicon element is 67.5 at.%, and the content of the gold is 0.8 at.% or
The content of the molybdenum element is 32.4 at.%, the content of the silicon element is 66.1 at.%, and the content of the gold is 1.5 at.% or
The content of the molybdenum element is 32.3 at.%, the content of the silicon element is 66.7 at.%, and the content of the silver is 1.0 at.%.
The invention also provides a preparation method of the film material in the technical scheme, which comprises the following steps:
using MoSi2And carrying out magnetron sputtering deposition on the surface of the substrate simultaneously to obtain the film material, wherein the noble metal target material is an Au target material or an Ag target material.
In the invention, during the magnetron sputtering deposition, the MoSi is sputtered2The DC constant current of the target is preferably 0.5A, the power for sputtering the noble metal target is preferably 0-50W, and the power for sputtering the noble metal target is preferably not 0.
In the invention, the working pressure of the magnetron sputtering deposition is preferably 0.6-0.8 Pa.
In the invention, the distance between the target and the substrate is preferably 10-15 cm independently during magnetron sputtering deposition.
In the invention, before magnetron sputtering deposition, the vacuum degree of the coating chamber is preferably pumped to 1 × 10 by a turbo molecular pump-4Pa, and introducing Ar of 80sccm as sputtering gas. In the present invention, the purity of Ar is preferably 99.99%.
In the present invention, the substrate is preferably a Si wafer. In the present invention, the substrate is preferably not applied with temperature and bias at the time of the magnetron sputtering deposition.
In the invention, the Si sheet is preferably pretreated before use, and the pretreatment is preferably carried out by sequentially carrying out ultrasonic cleaning on the Si sheet by using ethanol, acetone and deionized water and then drying the Si sheet. In the present invention, the time for each of the ultrasonic cleaning is preferably 15 minutes. The specific drying mode is not particularly limited, and deionized water can be completely removed.
In the present invention, the MoSi is2The purity of both the target material and the noble metal target material is preferably 99.95 wt%.
The invention also provides the application of the film material in the technical scheme or the film material prepared by the preparation method in the technical scheme in an aircraft engine transmission mechanism.
The invention is not particularly limited to the described applications, as such may be performed in a manner well known to those skilled in the art.
In order to further illustrate the present invention, the following detailed description of the film material provided by the present invention, its preparation method and application are given by way of examples, which should not be construed as limiting the scope of the present invention.
Example 1
Preparation work:
adopting magnetron sputtering deposition technique to mix MoSi2The target (99.95%) and the Au target (99.95%) were fixed at the sputtering target position 12cm from the substrate, where MoSi2The current of a direct current power supply of the target material is 0.5A, the power of a radio frequency power supply of the Au target material is 10W, the pressure of magnetron sputtering is controlled to be 0.8Pa, the temperature and bias voltage are not applied to the substrate, Ar ions bombard the surface of the target material in the film preparation process, and meanwhile, the argon flow is controlled to be 80 sccm. Will be provided withAnd (3) carrying out mechanical and oil friction and wear tests on the sample, measuring the friction coefficient of the prepared film in the lubricating oil base oil PAO4 by using a friction tester, and collecting the abraded swarf and the sample.
The experimental results are as follows:
by XRD (see FIG. 1) and HRTEM (see FIG. 2) analysis, FIG. 3 is the electron diffraction pattern of the corresponding selected region of the thin film material prepared in example 2, which proves that the obtained Mo-Si-Au thin film structure is C40 hexagonal structure, and no diffraction peak of Au is observed in XRD, and Au exists in MoSi in the form of monoatomic form2In the crystal lattice. The content of Mo atoms, Si atoms, and Au atoms in the prepared film were determined by XPS to be 30.6 at.%, 68.9 at.%, and 0.5 at.%. The hardness was 13.4GPa, and the fracture toughness was 2.36 MPa-m1/2The coefficient of friction was measured to be 0.11 by a friction tester under oil lubrication conditions (see fig. 6).
Example 2
Preparation work:
adopting magnetron sputtering deposition technique to mix MoSi2The target (99.95%) and the Au target (99.95%) were fixed at the sputtering target position 12cm from the substrate, where MoSi2The current of a direct current power supply of the target material is 0.5A, the power of a radio frequency power supply of the Au target material is 15W, the pressure of magnetron sputtering is controlled to be 0.8Pa, the temperature and bias voltage are not applied to the substrate, Ar ions bombard the surface of the target material in the film preparation process, and meanwhile, the argon flow is controlled to be 80 sccm. And (3) carrying out mechanical and oil friction and wear tests on the sample, measuring the friction coefficient of the prepared film in the lubricating oil base oil PAO4 by a friction tester, and collecting the abraded abrasive dust and the sample.
The experimental results are as follows:
the structure of the obtained Mo-Si-Au thin film is proved to be a C40 hexagonal structure by XRD (see figure 1), and no diffraction peak of Au is observed in the XRD, and Au exists in MoSi in a form of monoatomic form2In the crystal lattice. The content of Mo atoms, 67.5 at.% of Si atoms, and 0.8 at.% of Au atoms in the prepared film were determined by XPS. The hardness is 15.4GPa, and the fracture toughness is 2.55 MPa.m1/2The coefficient of friction was measured by a friction tester under oil lubrication conditions to be 0.09 (fig. 6).
Example 3
Preparation work:
adopting magnetron sputtering deposition technique to mix MoSi2The target (99.95%) and the Au target (99.95%) were fixed at the sputtering target position 12cm from the substrate, where MoSi2The current of a direct current power supply of the target material is 0.5A, the power of a radio frequency power supply of the Au target material is 20W, the pressure of magnetron sputtering is controlled to be 0.8Pa, the temperature and bias voltage are not applied to the substrate, Ar ions bombard the surface of the target material in the film preparation process, and meanwhile, the argon flow is controlled to be 80 sccm. And (3) carrying out mechanical and oil friction and wear tests on the sample, measuring the friction coefficient of the prepared film in the lubricating oil base oil PAO4 by a friction tester, and collecting the abraded abrasive dust and the sample.
The experimental results are as follows:
the structure of the obtained Mo-Si-Au thin film is proved to be a C40 hexagonal structure by XRD (see figure 1), and no diffraction peak of Au is observed in the XRD, and Au exists in MoSi in a form of monoatomic form2In the crystal lattice. The content of Mo atoms, the content of Si atoms, and the content of Au atoms in the prepared film were determined by XPS to be 32.4 at.%, 66.1 at.%, and 1.5 at.%, respectively. The hardness was 13.5GPa, and the fracture toughness was 2.47MPa m1/2The coefficient of friction was measured by a friction tester under oil lubrication conditions to be 0.11 (fig. 6).
Example 4
Preparation work:
adopting magnetron sputtering deposition technique to mix MoSi2The target (99.95%) and the Ag target (99.95%) were fixed at the sputtering target position 12cm from the substrate, with MoSi2The current of a direct current power supply of the target material is 0.5A, the power of a radio frequency power supply of the Ag target material is 15W, the pressure of magnetron sputtering is controlled to be 0.8Pa, the temperature and bias voltage are not applied to the substrate, Ar ions bombard the surface of the target material in the film preparation process, and meanwhile, the argon flow is controlled to be 80 sccm. And (3) carrying out mechanical and oil friction and wear tests on the sample, measuring the friction coefficient of the prepared film in the lubricating oil base oil PAO4 by a friction tester, and collecting the abraded abrasive dust and the sample.
The experimental results are as follows:
obtained by XRD and HRTEMThe Mo-Si-Ag thin film structure is a C40 hexagonal structure, no diffraction peak of Ag is observed in XRD, and the Ag exists in MoSi in a form of single atom2In the crystal lattice. The content of Mo atoms, the content of Si atoms, and the content of Ag atoms in the prepared film were determined by XPS to be 32.3 at.%, 66.7 at.%, and 1.0 at.%, respectively. The hardness is 15.2GPa, and the fracture toughness is 2.49 MPa.m1/2The coefficient of friction was 0.09 as measured by a friction tester under oil lubrication conditions.
Comparative example 1
Preparation work:
adopting magnetron sputtering deposition technique to mix MoSi2The target (99.95%) and Au target (99.95%) were fixed at the sputtering target position 12cm away from the substrate, MoSi2The current of the target direct current power supply is 0.5A, the power of the radio frequency power supply of the Au target is 0W, the sputtering pressure is controlled to be 0.8Pa, the temperature and the bias voltage are not applied to the substrate, Ar ions bombard the surface of the target in the film preparation process, and meanwhile, the argon flow is controlled to be 80 sccm. And (3) carrying out mechanical and oil friction and wear tests on the sample, measuring the friction coefficient of the prepared film in the lubricating oil base oil PAO4 by a friction tester, and collecting the abraded abrasive dust and the sample.
The experimental results are as follows:
the MoSi obtained was confirmed by XRD and HRTEM2The film structure is a C40 hexagonal structure. The content of Mo atoms in the prepared film was determined by XPS to be 33.3 at.%, and the content of Si atoms to be 66.7 at.%. The hardness is 10.9GPa, and the fracture toughness is 2.10 MPa.m1/2The coefficient of friction was measured by a friction tester under oil lubrication conditions to be 0.17 (fig. 6).
Comparative example 2
Preparation work:
adopting magnetron sputtering deposition technique to mix MoSi2The target (99.95%) and the Au target (99.95%) were fixed at the sputtering target position 12cm from the substrate, where MoSi2The current of a direct current power supply of the target material is 0.5A, the power of a radio frequency power supply of the Au target material is 50W, the pressure of magnetron sputtering is controlled to be 0.8Pa, the temperature and bias voltage are not applied to the substrate, Ar ions bombard the surface of the target material in the film preparation process, and meanwhile, the argon flow is controlled to be 80 sccm.
The experimental results are as follows:
by XRD and HRTEM (FIG. 4), FIG. 5 is the corresponding selected area electron diffraction pattern of the thin film material prepared in comparative example 2, the obtained Mo-Si-Au thin film structure is proved to be C40 hexagonal structure, and the diffraction ring of Au (111) is observed in high resolution corresponding to the selected area electron diffraction, which indicates that Au atom part forms a group from MoSi2And precipitating in crystal lattices. XPS analysis gave a Mo atom content of 34.6 at.%, a Si atom content of 63.0 at.%, and an Au atom content of 2.4 at.%. The hardness was 9.9GPa, and the fracture toughness was 2.04MPa m1/2The coefficient of friction measured by a friction tester under oil lubrication conditions was 0.14 (fig. 6).
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications should also be construed as the protection scope of the present invention.

Claims (10)

1. A thin film material is characterized by comprising a molybdenum element, a silicon element and a noble metal element, wherein the noble metal element is gold or silver, the content of the molybdenum element is 28-35 at.%, the content of the silicon element is 60-70 at.%, the content of the noble metal element is 0.5-1.5 at.%, and the noble metal element exists in a single atom form.
2. The thin film material according to claim 1, wherein the noble metal element is contained in an amount of 0.8 to 1.0 at.%.
3. The thin film material of claim 1, wherein the molybdenum element is present in an amount of 30.6 at.%, the silicon element is present in an amount of 68.9 at.%, and the gold is present in an amount of 0.5 at.%.
4. The thin film material of claim 1 or 2, wherein the molybdenum element is present in an amount of 31.7 at.%, the silicon element is present in an amount of 67.5 at.%, and the gold is present in an amount of 0.8 at.%.
5. The thin film material of claim 1, wherein the molybdenum element is present in an amount of 32.4 at.%, the silicon element is present in an amount of 66.1 at.%, and the gold is present in an amount of 1.5 at.%.
6. The thin film material of claim 1 or 2, wherein the molybdenum element is present in an amount of 32.3 at.%, the silicon element is present in an amount of 66.7 at.%, and the silver is present in an amount of 1.0 at.%.
7. A method for preparing a film material according to any one of claims 1 to 6, comprising the steps of:
using MoSi2And carrying out magnetron sputtering deposition on the surface of the substrate simultaneously to obtain the film material, wherein the noble metal target material is an Au target material or an Ag target material.
8. The method according to claim 7, wherein the MoSi is sputtered during the magnetron sputtering deposition2The direct current constant current of the target material is 0.5A, the power for sputtering the noble metal target material is 0-50W, and the power for sputtering the noble metal target material is not 0.
9. The preparation method according to claim 7, wherein the working pressure of the magnetron sputtering deposition is 0.6-0.8 Pa.
10. Use of the film material according to any one of claims 1 to 6 or the film material prepared by the preparation method according to any one of claims 7 to 9 in an aircraft engine transmission mechanism.
CN202110747162.1A 2021-07-02 2021-07-02 Film material and preparation method and application thereof Active CN113463051B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114086138A (en) * 2021-11-19 2022-02-25 烟台大学 alpha-CNxPreparation method of/Fe nano composite coating
CN114561621A (en) * 2021-12-10 2022-05-31 吉林大学 High-entropy metal glass film and preparation method and application thereof

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CN108342687A (en) * 2018-01-30 2018-07-31 吉林大学 A kind of Hf of the monatomic doping of noble metal3N4Film and preparation method thereof

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JP2003055761A (en) * 2001-08-13 2003-02-26 Toshiba Corp Sputtering target, production method therefor and electronic parts
CN108342687A (en) * 2018-01-30 2018-07-31 吉林大学 A kind of Hf of the monatomic doping of noble metal3N4Film and preparation method thereof

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Title
赖道辉: ""Al合金化对MoSi2性能的影响：第一性原理计算与实验研究"", 《中国优秀硕士学位论文全文数据库（电子期刊）工程科技Ⅰ辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114086138A (en) * 2021-11-19 2022-02-25 烟台大学 alpha-CNxPreparation method of/Fe nano composite coating
CN114086138B (en) * 2021-11-19 2024-03-15 烟台大学 alpha-CN x Preparation method of Fe nano composite coating
CN114561621A (en) * 2021-12-10 2022-05-31 吉林大学 High-entropy metal glass film and preparation method and application thereof

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