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CN113088904A - Metal Cr coating with nano multilevel structure and preparation method thereof - Google Patents

Metal Cr coating with nano multilevel structure and preparation method thereof Download PDF

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CN113088904A
CN113088904A CN202110227118.8A CN202110227118A CN113088904A CN 113088904 A CN113088904 A CN 113088904A CN 202110227118 A CN202110227118 A CN 202110227118A CN 113088904 A CN113088904 A CN 113088904A
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coating
metal
nano
deposition
multilevel structure
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CN113088904B (en
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王亚强
肖珣
张金钰
吴凯
刘刚
孙军
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Xian Jiaotong University
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Xian Jiaotong University
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/16Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
    • C23C14/021Cleaning or etching treatments
    • C23C14/022Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target

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  • Engineering & Computer Science (AREA)
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Abstract

本发明公开了一种具有纳米多级结构的金属Cr涂层及其制备方法,通过磁控溅射在洁净的硅基体上沉积制备具有纳米多级结构的金属Cr涂层,其原理是Ar气经辉光放电后产生高密度Ar+,Ar+在电场的作用下被强烈吸引到负电极并以高速率轰击两个金属Cr直流靶,形成碰撞级联过程溅射出靶原子和二次电子,Cr原子最终反向运动至阳极的硅基体上沉积,而二次电子在正交电磁场的运动方向与电场、磁场垂直,以旋轮线的形式循环运动,提高了Ar的电离率,增加了离子密度和能量,从而实现高速率溅射。最终本发明在不同的沉积气压下制备出具有纳米多级结构的金属Cr涂层。

Figure 202110227118

The invention discloses a metal Cr coating with a nanometer multi-level structure and a preparation method thereof. The metal Cr coating with a nanometer multilevel structure is deposited and prepared on a clean silicon substrate by magnetron sputtering. The principle is Ar gas After glow discharge, high-density Ar + is generated, and Ar + is strongly attracted to the negative electrode under the action of the electric field and bombards two metal Cr DC targets at a high rate, forming a collision cascade process to sputter target atoms and secondary electrons, The Cr atoms move in the opposite direction to deposit on the silicon substrate of the anode, while the movement direction of the secondary electrons in the orthogonal electromagnetic field is perpendicular to the electric and magnetic fields, and circulates in the form of cycloids, which improves the ionization rate of Ar and increases the ionization rate of ions. density and energy, enabling high-rate sputtering. Finally, the present invention prepares metal Cr coating with nano-multilevel structure under different deposition pressure.

Figure 202110227118

Description

Metal Cr coating with nano multilevel structure and preparation method thereof
Technical Field
The invention belongs to the field of material surface modification, and particularly relates to a metal Cr coating with a nano multilevel structure and a preparation method thereof.
Background
The metal Cr coating has good corrosion resistance, higher melting point, excellent mechanical strength and wear resistance, and good chemical inertness, high-temperature oxidation performance and substrate adhesion. At present, various preparation methods are used for depositing the metal Cr coating, wherein the magnetron sputtering method is a mature coating preparation technology due to low energy, controllable deposition rate and good process repeatability. The metal Cr coating prepared by magnetron sputtering usually shows the growth morphology of columnar crystals, and the continuous crystal boundary of the columnar crystals is a defect which is easy to cause the cracking and peeling of the coating under the action of external force, so that the continuous growth of the columnar crystals is not beneficial to the improvement of the performance of the metal Cr coating.
The change of the preparation technology and the process parameters of the coating can obviously influence the surface diffusion capability and the bulk diffusion capability in the deposition growth process of the metal Cr coating, and further determine the microstructure of the metal Cr coating, thereby improving and enhancing the quality and the performance of the coating. In order to provide effective protection in extreme environments such as high-temperature oxidation, the metallic Cr coating must have a uniform and dense microstructure and excellent properties, which depend on the preparation technology and process parameters of the metallic Cr coating. How to select proper magnetron sputtering process parameters and prepare the metal Cr coating with excellent performance by regulating and controlling the microstructure of the coating is the key point of the current research.
Disclosure of Invention
Aiming at the problem that the metal Cr coating is easy to crack and peel off under the action of external force in the prior art, the invention provides the metal Cr coating with the nano multistage structure and the preparation method thereof, so that the microstructure of the metal Cr coating is regulated and controlled, and the adhesive force of the high coating is enhanced.
The invention is realized by the following technical scheme:
the metal Cr coating with the nanometer multilevel structure is characterized in that the crystal grain appearance of the metal Cr coating is columnar crystal, the surface of the columnar crystal is of a carambola-shaped structure with the multilevel micro-nano scale, and the thickness of the columnar crystal is 3.92-4.80 microns.
Preferably, the grain size of the metal Cr coating is 180-315 nm.
A preparation method of a metal Cr coating with a nano multilevel structure comprises the steps of etching a clean matrix in a vacuum environment, then carrying out direct-current magnetron sputtering on the etched silicon matrix by adopting two metal Cr targets, and cooling to room temperature along with a furnace after sputtering deposition to obtain the metal Cr coating with the nano multilevel structure;
the deposition power is 200W, the deposition pressure is 0.5-1.5Pa, and the argon flow rate is set to 40-90sccm during the deposition process.
Preferably, the degree of vacuum is 1.0X 10-4Pa or less.
Preferably, the etching power is 200W, the etching pressure is 1.0Pa, and the etching time is 5 min.
Preferably, the substrate is etched and then pre-sputtered, argon is firstly introduced, the gas introduction time is at least 30s, and the pre-sputtering time is at least 10 s.
Preferably, the rotating speed of the silicon substrate in the magnetron sputtering deposition process is 10 r/min.
Preferably, the magnetron sputtering deposition time is 15000 s.
Preferably, the polished silicon substrate is ultrasonically cleaned in acetone and absolute ethyl alcohol for 10min respectively and then dried to remove impurities on the surface of the substrate, so as to obtain a crystallized substrate.
Preferably, the substrate is a silicon substrate.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention relates to a preparation method of a metal Cr coating with a nano multilevel structure, which is used for preparing the metal Cr coating with the nano multilevel structure on a clean silicon substrate by deposition through a magnetron sputtering deposition method. Firstly removing impurities on the surface of a silicon substrate to improve the binding capacity of a coating and the substrate, and then generating high-density Ar after glow discharge of Ar gas+,Ar+Is strongly attracted to the negative under the action of the electric fieldThe electrode bombards two Cr direct current targets at a high rate, partial kinetic energy is transferred to target atoms, and then the target atoms collide with other target atoms to form a cascade process. In the cascade process, target atoms near some surfaces obtain enough kinetic energy to move outwards, so that the target atoms and secondary electrons are sputtered, Cr atoms finally move reversely to a silicon substrate of an anode for deposition, and the secondary electrons move circularly in a form of a cycloidal line in the movement direction of an orthogonal electromagnetic field, which is vertical to an electric field and a magnetic field, so that the ionization rate of Ar is improved, the ion density and energy are increased, and high-speed sputtering is realized. And finally, the coating is cooled to room temperature in a vacuum coating chamber, so that the coating is prevented from peeling off due to small temperature rise and different thermal expansion coefficients of the coating and a substrate in the sputtering process, and the finally deposited coating has few defects and strong adhesive force.
The microstructure of the metal Cr coating is regulated and controlled by controlling the deposition air pressure. When the deposition pressure is lower, the Ar partial pressure is lower, Ar ions bombarding the target after ionization are fewer, sputtered particles are fewer, the deposition rate is lower, the thickness of the deposited metal Cr coating is smaller, and meanwhile, the deposition rate is lower, so that sputtered atoms are favorably deposited on the surface of the substrate without causing holes, and the coating quality is favorably improved; when the deposition gas pressure is increased, the average free path of gas molecules is reduced, the number of times of collision between sputtered atoms and gas molecules is increased, the secondary electron emission is enhanced, the sputtering capacity is enhanced, the deposition rate is increased, the thickness of the coating is increased in the same deposition time, and meanwhile, the average kinetic energy of the sputtered atoms is also reduced due to the increase of the number of times of collision between the sputtered atoms and the gas molecules, the migration capacity on the surface of the coating is reduced, so that the probability of filling the coating into pores on the surface of the coating is reduced, therefore, the coating deposited under the deposition gas pressure is rough, and the pores between columnar crystals are large; when the deposition pressure is too high, the number of collisions between the sputtered atoms and the gas molecules is greatly increased with the increase of the Ar gas molecules, which results in greater loss of energy of the sputtered atoms during the collisions, resulting in a decrease in the number of particles reaching the silicon substrate, a decrease in the deposition rate, a decrease in the thickness of the coating at the same deposition time, and an improvement in the surface quality of the coating. Thus, changes in deposition gas pressure affect changes in the coating deposition rate and surface topography as well as changes in the properties of the coating. The microstructure of the coating is regulated and controlled by controlling the deposition air pressure, and the metal Cr coating with excellent performance is prepared, so that the method has great significance.
Furthermore, after the deposition is finished, the coating is placed in a high vacuum coating chamber to be cooled along with the furnace, so that the phenomenon that the coating falls off from the substrate due to thermal stress caused by different thermal expansion coefficients of the coating and the substrate is avoided, and the coating is prevented from being oxidized at high temperature.
A metal Cr coating with a nano multistage structure is provided, the shape of a crystal grain is columnar crystal, the size of the columnar crystal is stabilized in the range of the nanocrystalline, and the surface of the columnar crystal is of a carambola-shaped structure with multistage micro-nano dimensions. The microstructure of the coating changes with the deposition pressure: at low air pressure, the coating has larger grain size and loose structure; as the air pressure is increased, the grain size of the coating is reduced, and the structure density is increased.
Drawings
FIG. 1 is a SEM surface photograph of a metallic Cr coating prepared by the method;
FIG. 1a is a SEM surface photograph of a metallic Cr coating produced at a pressure of 0.5Pa, and FIG. 1b is a SEM surface photograph of a metallic Cr coating produced at a pressure of 1 Pa.
FIG. 2 is a SEM cross-sectional photograph of a metallic Cr coating prepared by the present invention;
FIG. 2a is a SEM cross-sectional photograph of a metallic Cr coating produced at a pressure of 0.5Pa, and FIG. 2b is a SEM cross-sectional photograph of a metallic Cr coating produced at a pressure of 1 Pa.
FIG. 3 is a high magnification SEM cross section of a metallic Cr coating prepared by the present invention;
FIG. 3a is a high SEM cross-section photograph of a metallic Cr coating produced at 0.5Pa gas pressure, and FIG. 3b is a high SEM cross-section photograph of a metallic Cr coating produced at 1Pa gas pressure.
Detailed Description
The present invention will now be described in further detail with reference to the attached drawings, which are illustrative, but not limiting, of the present invention.
A preparation method of a metallic Cr coating with a nano-multilevel structure comprises the following steps:
step 1, carrying out ultrasonic cleaning and drying on the surface of a silicon substrate;
specifically, polishing one surface of a silicon substrate, respectively ultrasonically cleaning the silicon substrate in acetone and ethanol for 10min, and then quickly drying the silicon substrate to ensure that the surface of the silicon substrate is clean, has no stain and no dust attachment and has the roughness of below 0.5-0.8 nm.
Step 2, utilizing Ar in a high vacuum environment+The ions are etched to remove impurities on the surface of the matrix,
then, two metal Cr targets are adopted for magnetron sputtering, and a metal Cr coating with a nano multistage structure is obtained by deposition on the surface of the substrate.
Wherein, the two metal Cr targets adopt direct current power supplies, the power is 200W, and the target purity is not less than 99.95 wt.%; the deposition pressure is 0.5-1.5Pa, the flow rate of argon gas is set to 40-90sccm during deposition, the deposition temperature is room temperature, and the deposition time is 15000 s.
Concretely, the cleaned and dried silicon substrate is fixed on a base plate and sent into a vacuum coating chamber, and then the vacuum degree of the back bottom is pumped to 1.0 multiplied by 10-4Pa or less.
The etching power is 200W, the etching pressure is 1.0Pa, and the etching time is 5 min; before the pre-sputtering, the argon gas is introduced for at least 30s, the pre-sputtering time is at least 10s, and the rotating speed of the silicon substrate in the deposition process is 10 r/min.
Referring to fig. 1-3, the thickness of the metallic Cr coating with a nano-scale structure prepared by the above method is 3.92 μm to 4.80 μm, the crystal grain morphology of the coating is carambola-like columnar crystals with a nano-scale structure, and the size of the columnar crystals is stabilized in the range of the nanocrystal.
The microstructure of the metal Cr coating changes along with the change of deposition air pressure, the grain size of columnar crystals is 180-315 nm, the grain size decreases along with the increase of the deposition air pressure, and the grain size of the layer crystals is larger and the structure is loose under low air pressure, but the grain size of the coating decreases along with the increase of the deposition air pressure, and the structure density increases.
A process for preparing the metallic Cr coating with nano-class structure includes such steps as polishing Si (111) substrate in acetoneAnd respectively ultrasonically cleaning the substrate in an absolute ethyl alcohol solution for 10min to remove surface stains and dust and improve the binding force of the coating and the substrate. The principle of preparing the metal Cr coating with the nano multistage structure by depositing on a clean silicon substrate through a magnetron sputtering deposition method is that Ar gas generates high-density Ar ions after glow discharge, and Ar+The metal Cr target material is strongly attracted to a negative electrode under the action of an electric field and bombards two metal Cr target materials at a high rate, partial kinetic energy is transferred to target atoms, and then the target atoms collide with other target atoms to form a cascade process. In the cascade process, target atoms near some surfaces obtain enough kinetic energy to move outwards, so that the target atoms and secondary electrons are sputtered, Cr atoms finally move reversely to a silicon substrate of an anode for deposition, and the secondary electrons move circularly in a form of a cycloidal line in the movement direction of an orthogonal electromagnetic field, which is vertical to an electric field and a magnetic field, so that the ionization rate of Ar is improved, the ion density and energy are increased, and high-speed sputtering is realized. The invention adopts two metal Cr direct current targets to carry out magnetron sputtering deposition on the Cr coating, the deposition power is 200W, and the microstructure of the metal Cr coating with the nanometer multilevel structure is regulated and controlled by adopting the same deposition time and different deposition air pressures. And finally, cooling the metal Cr coating to room temperature in a vacuum coating chamber, so that the coating is prevented from peeling off due to small temperature rise and different thermal expansion coefficients of the coating and a substrate in the sputtering process, and finally the metal Cr coating with a nano multistage structure, few defects and strong adhesion is formed by deposition.
Example 1
A preparation method of a metal Cr coating with a nano multilevel structure comprises the following specific preparation processes:
firstly, respectively ultrasonically cleaning a polished Si (111) matrix in acetone and absolute ethyl alcohol for 10min, and drying to remove impurities on the surface of the silicon matrix; then fixing the silicon substrate on a base plate, mechanically and automatically feeding the silicon substrate into a magnetron sputtering vacuum coating chamber in a tracing manner, and pumping the silicon substrate until the vacuum degree of the back bottom is 1.0 multiplied by 10-4And starting etching below Pa, wherein the etching power is 200W, the etching pressure is 1.0Pa, and the etching time is 5 min.
Then, carrying out magnetron sputtering to deposit a metal Cr coating, firstly introducing argon gas for 30s, carrying out pre-sputtering for 10s, adopting two metal Cr direct current targets (with the purity of 99.95 wt.%) to jointly deposit, wherein the deposition power is 200W, the rotating speed of a substrate is 10r/min, the deposition pressure is set to be 0.5Pa, the flow rate of the argon gas is 40sccm, the deposition temperature is room temperature, and the deposition time is 15000 s.
And finally, naturally cooling the sample in a vacuum coating chamber for 2-3 hours to room temperature, and taking out the sample to obtain the metal Cr coating with the nano multistage structure and the thickness of about 4.37 mu m.
And the microstructure representation is carried out on the prepared metal Cr coating, the crystal grain appearance of the metal Cr coating is carambola-shaped columnar crystal with a nano multistage structure, the size of the columnar crystal is stable in the range of the nanocrystal, the size of the crystal grain is larger, and the structure is loose.
Example 2
A preparation method of a metal Cr coating with a nano multilevel structure comprises the following specific preparation processes:
firstly, respectively ultrasonically cleaning a polished Si (111) matrix in acetone and absolute ethyl alcohol for 10min, and drying to remove impurities on the surface of the silicon matrix; then fixing the silicon substrate on a base plate, mechanically and automatically feeding the silicon substrate into a magnetron sputtering vacuum coating chamber in a tracing manner, and pumping the silicon substrate until the vacuum degree of the back bottom is 1.0 multiplied by 10-4And starting etching below Pa, wherein the etching power is 200W, the etching pressure is 1.0Pa, and the etching time is 5 min.
Then, carrying out magnetron sputtering deposition on the metal Cr coating, firstly introducing argon for 60s, carrying out pre-sputtering for 20s, adopting two metal Cr direct current targets (with the purity of 99.95 wt.%) to carry out co-deposition, wherein the deposition power is 200W, the rotating speed of a substrate is 10r/min, the deposition pressure is set to be 1.0Pa, the flow rate of the argon is 70sccm, the deposition temperature is room temperature, and the deposition time is 15000 s.
And finally, naturally cooling the sample in a vacuum coating chamber for 2-3 hours to room temperature, and taking out the sample to obtain the metal Cr coating with the nano multistage structure and the thickness of about 4.80 mu m.
The microstructure representation is carried out on the prepared metal Cr coating with the nano multilevel structure, the crystal grain appearance of the metal Cr coating is carambola-shaped columnar crystal with the nano multilevel structure, the size of the columnar crystal is stable in the range of the nanocrystal, the size of the crystal grain is larger, and the structure is loose.
Example 3
A preparation method of a metal Cr coating with a nano multilevel structure comprises the following specific preparation processes:
firstly, respectively ultrasonically cleaning a polished Si (111) matrix in acetone and absolute ethyl alcohol for 10min, and drying to remove impurities on the surface of the silicon matrix; then fixing the silicon substrate on a base plate, mechanically and automatically feeding the silicon substrate into a magnetron sputtering vacuum coating chamber in a tracing manner, and pumping the silicon substrate until the vacuum degree of the back bottom is 1.0 multiplied by 10-4And starting etching below Pa, wherein the etching power is 200W, the etching pressure is 1.0Pa, and the etching time is 5 min.
Then, carrying out magnetron sputtering deposition on the metal Cr coating, firstly introducing argon for 90s, carrying out pre-sputtering for 30s, adopting two metal Cr direct current targets (with the purity of 99.95 wt.%) to carry out co-deposition, wherein the deposition power is 200W, the rotating speed of a substrate is 10r/min, the deposition pressure is set to be 1.5Pa, the flow rate of the argon is 90sccm, the deposition temperature is room temperature, and the deposition time is 15000 s.
And finally, naturally cooling the sample in a vacuum coating chamber for 2-3 hours to room temperature, and taking out the sample to obtain the metal Cr coating with the nano multistage structure, wherein the thickness of the metal Cr coating is about 3.92 mu m.
The microstructure representation is carried out on the prepared metal Cr coating with the nano multilevel structure, the crystal grain appearance of the metal Cr coating is carambola-shaped columnar crystal with the nano multilevel structure, the size of the columnar crystal is stabilized in the range of the nanocrystal, the size of the crystal grain is smaller, and the structural density is increased.
The invention discloses a metal Cr coating with a nano multilevel structure and a preparation method thereof, wherein the metal Cr coating with the nano multilevel structure is prepared by depositing on a clean silicon substrate through magnetron sputtering deposition, as shown in figures 1-3, the microstructure structures of the metal Cr coatings prepared under different deposition air pressures are different, so that the metal Cr coating with excellent performance can be prepared by controlling the microstructure structure of the metal Cr coating through controlling the magnetron sputtering deposition air pressure.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (10)

1.一种具有纳米多级结构的金属Cr涂层,其特征在于,所述金属Cr涂层的晶粒形貌为柱状晶,且柱状晶表面为具有多级微纳尺度的杨桃状结构,厚度为3.92μm-4.80μm。1. a metal Cr coating with a nano-multilevel structure, characterized in that the grain morphology of the metal Cr coating is a columnar crystal, and the surface of the columnar crystal is a star fruit-like structure with a multi-level micro-nano scale, The thickness is 3.92μm-4.80μm. 2.根据权利要求1所述的一种具有纳米多级结构的金属Cr涂层,其特征在于,所述金属Cr涂层的晶粒尺寸为180~315nm。2 . The metal Cr coating having a nano-multilevel structure according to claim 1 , wherein the grain size of the metal Cr coating is 180-315 nm. 3 . 3.一种权利要求1或2所述的具有纳米多级结构的金属Cr涂层的制备方法,其特征在于,在真空环境下,对洁净的基体进行刻蚀,然后采用两个金属Cr靶对刻蚀后的硅基体进行直流磁控溅射,溅射沉积后随炉冷却至室温,得到具有纳米多级结构的金属Cr涂层;3. the preparation method of the metal Cr coating with nanometer multi-level structure described in claim 1 or 2, it is characterized in that, under vacuum environment, the clean substrate is etched, and then two metal Cr targets are adopted DC magnetron sputtering is performed on the etched silicon substrate, and after the sputter deposition is cooled to room temperature in a furnace, a metallic Cr coating with a nano-multilevel structure is obtained; 沉积功率均为200W,沉积气压为0.5-1.5Pa,沉积过程中氩气流速设定为40-90sccm。The deposition power is all 200W, the deposition pressure is 0.5-1.5Pa, and the argon gas flow rate is set to 40-90sccm during the deposition process. 4.根据权利要求3所述的具有纳米多级结构的金属Cr涂层的制备方法,其特征在于,所述真空度在1.0×10-4Pa以下。4 . The method for preparing a metal Cr coating with a nano-multilevel structure according to claim 3 , wherein the vacuum degree is below 1.0×10 −4 Pa. 5 . 5.根据权利要求3所述的具有纳米多级结构的金属Cr涂层的制备方法,其特征在于,所述刻蚀的功率为200W,刻蚀气压为1.0Pa,刻蚀时间为5min。5 . The method for preparing a metal Cr coating with a nano-multilevel structure according to claim 3 , wherein the etching power is 200W, the etching gas pressure is 1.0Pa, and the etching time is 5min. 6 . 6.根据权利要求3所述的具有纳米多级结构的金属Cr涂层的制备方法,其特征在于,对基体刻蚀后进行预溅射,先通入氩气,通气时间至少为30s,预溅射时间至少为10s。6. the preparation method of the metal Cr coating with nano-multilevel structure according to claim 3, it is characterized in that, carry out pre-sputtering after the substrate is etched, pass argon gas first, the ventilation time is at least 30s, pre-sputtering is carried out. The sputtering time is at least 10s. 7.根据权利要求3所述的具有纳米多级结构的金属Cr涂层的制备方法,其特征在于,所述磁控溅射沉积过程中硅基体转速为10r/min。7 . The method for preparing a metal Cr coating with a nano-multilevel structure according to claim 3 , wherein the rotational speed of the silicon substrate during the magnetron sputtering deposition process is 10 r/min. 8 . 8.根据权利要求3所述的具有纳米多级结构的金属Cr涂层的制备方法,其特征在于,所述磁控溅射沉积时间均为15000s。8 . The method for preparing a metal Cr coating with a nano-multilevel structure according to claim 3 , wherein the magnetron sputtering deposition time is 15000 s. 9 . 9.根据权利要求3所述的具有纳米多级结构的金属Cr涂层的制备方法,其特征在于,将抛光后的硅基体在丙酮和无水乙醇中分别超声清洗10min后并烘干,以去除基体表面的杂质,得到结晶的基体。9. the preparation method of the metal Cr coating with nano-multilevel structure according to claim 3, is characterized in that, the silicon substrate after polishing is respectively ultrasonically cleaned 10min in acetone and dehydrated alcohol and oven dry, with The impurities on the surface of the substrate are removed to obtain a crystallized substrate. 10.根据权利要求3所述的具有纳米多级结构的金属Cr涂层的制备方法,其特征在于,所述基体为硅基体。10 . The method for preparing a metal Cr coating with a nano-multilevel structure according to claim 3 , wherein the substrate is a silicon substrate. 11 .
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