CN114481099A - Preparation process for alternately depositing soft and hard composite film by electro-fluidic method based on mask plate - Google Patents
Preparation process for alternately depositing soft and hard composite film by electro-fluidic method based on mask plate Download PDFInfo
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- CN114481099A CN114481099A CN202210065072.9A CN202210065072A CN114481099A CN 114481099 A CN114481099 A CN 114481099A CN 202210065072 A CN202210065072 A CN 202210065072A CN 114481099 A CN114481099 A CN 114481099A
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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- C23C18/1216—Metal oxides
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1229—Composition of the substrate
- C23C18/1241—Metallic substrates
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- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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- 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
- C23C24/00—Coating starting from inorganic powder
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Abstract
The invention belongs to the field of antifriction and wear-resistant films, and relates to a preparation process for alternately depositing soft and hard composite films by an electric jet flow method based on a mask plate. The preparation process comprises the following steps: providing a mask plate, wherein the mask plate is provided with a plurality of strip-shaped cavities, covering the mask plate on the surface of a substrate, depositing a hard coating material precursor in the cavities of the mask plate by using an electric jet deposition method, sintering the deposited hard coating material precursor to form a hard strip-shaped structure, covering the mask plate on the surface of the substrate to enable the cavities of the mask plate to be positioned between the hard strip-shaped structures, then depositing a soft coating material in the cavities of the mask plate by using the electric jet deposition method, and carrying out heat treatment on the deposited soft coating material to obtain the mask plate. The invention not only can solve the defect of single material and greatly improve the service life, but also has less material consumption and thinner film layer and is easy to realize industrialized production.
Description
Technical Field
The invention belongs to the field of antifriction and wear-resistant films, and relates to a preparation process for alternately depositing soft and hard composite films by an electric jet method based on a mask plate.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Titanium alloy is widely applied to parts such as flap sliding rails of airplanes, actuator cylinders of aircrafts and the like, and friction pairs are formed between the titanium alloy and stainless steel. However, the titanium alloy has high surface friction coefficient and is easy to generate adhesionWear and tear, etc. In order to improve the antifriction and wear-resistant performance of the titanium alloy and prolong the service life, the surface coating modification is essential. Ceramic material coatings fall into two broad categories, namely hard and soft coating materials. Typical hard coating materials are ZrO2、TiN、Al2O3、SiO2And TiO2And the like, which are characterized by high hardness and good wear resistance, but have the defect of higher friction coefficient of the contact surface. Soft coating materials have a low coefficient of friction but poor shear strength and abrasion resistance, such as WS2、MoS2And the like. The application of single material has certain limitation, and the alternating work of soft and hard is the current research hotspot. And the traditional soft-hard composite coating can be prepared into a laminated pattern, and the mixed friction reduction of materials is realized in the process of wearing layer by layer. However, the inventor researches and discovers that the soft and hard composite coating in a lamination mode needs to coat the surface of a workpiece substrate layer by layer in the preparation process, and the following problems exist: 1. the surface area of the workpiece substrate is large, and after one layer of the workpiece substrate is plated, another layer of the workpiece substrate can be plated continuously, so that more materials are needed; 2. the composition of the hard coating and the soft coating can be finished only by arranging at least two layers of coatings on the surface of a workpiece substrate, and the finally formed film layer is thicker; and so on.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation process for alternately depositing soft and hard composite films by an electro-fluidic method based on a mask plate, which can overcome the defects of a single material, has less material consumption and thinner film layer and is easy to realize industrial production.
In order to achieve the purpose, the technical scheme of the invention is as follows:
on the one hand, a soft or hard composite film, the film is used for adhering to the surface of a substrate, the film comprises a plurality of hard bar structures and a plurality of soft bar structures in an alternative mode, each bar structure and each soft bar structure are connected with the surface of the substrate simultaneously, the hard bar structures are made of hard coating materials, and the soft bar structures are made of soft coating materials.
On the other hand, the preparation process of the soft and hard composite film alternately deposited by the electro-jet deposition method based on the mask plate comprises the steps of providing the mask plate, arranging a plurality of strip-shaped cavities on the mask plate, covering the mask plate on the surface of a base body, depositing a hard coating material precursor in the cavities of the mask plate by the electro-jet deposition method, sintering the deposited hard coating material precursor to form hard strip-shaped structures, covering the mask plate on the surface of the base body, enabling the cavities of the mask plate to be located between the hard strip-shaped structures, depositing a soft coating material in the cavities of the mask plate by the electro-jet deposition method, and carrying out heat treatment on the deposited soft coating material to obtain the soft coating film.
The alternating film prepared by the process can alternately fill soft and hard coating materials, makes up the defect of a single material, provides an antifriction and wear-resistant effect for a substrate, and greatly prolongs the service life. Meanwhile, as the holes are formed in the mask plate, more coating materials are fixed in the holes, and the density of the hard strip-shaped structure and the density of the soft strip-shaped structure are higher after treatment, the overall density of the formed film is improved.
According to the invention, the soft and hard coating materials are alternately arranged in one film layer, so that soft and hard compounding is realized, the number of the film coating layers is reduced, and the thickness of the soft and hard compound film is greatly reduced.
In a third aspect, the soft-hard composite film is applied to the surface of a friction part.
Compared with the prior art, the invention has the following beneficial effects:
the preparation process for alternately depositing the soft and hard composite film by the electro-fluidic method based on the mask plate has the advantages of simple equipment, strong controllability and high deposition rate. Meanwhile, the prepared film has high density, few pores on the surface of the film, lower friction coefficient, easy film formation on various planar substrates, less material consumption and low cost, and is suitable for industrial production.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Fig. 1 is a schematic diagram of a preparation process of alternately depositing soft and hard composite films by electro-jet based on a mask in an embodiment of the invention.
FIG. 2 is a MoS prepared according to an embodiment of the present invention2-TiO2Schematic diagram of the soft and hard composite film, wherein 1 is TiO2Textured surface, 2 MoS2Alternate fillers, 3 being TiO2The transition layer 4 is a metal substrate.
FIG. 3 is a MoS prepared according to example 1 of the present invention2-TiO2The surface appearance and SEM element distribution diagram of the soft and hard composite film.
FIG. 4 is a MoS prepared according to example 1 of the present invention2-TiO2The friction coefficient curve chart of the soft and hard composite film.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In view of the problems of more materials, thick film layer and the like of the existing laminated soft and hard composite coating, the invention provides a preparation process for alternately depositing soft and hard composite films by an electro-jet method based on a mask plate.
In an exemplary embodiment of the present invention, a hard-soft composite film is provided, where the film is used to adhere to a surface of a substrate, the film is composed of a plurality of hard strip-shaped structures and a plurality of soft strip-shaped structures alternately, each strip-shaped structure and each soft strip-shaped structure are simultaneously connected to the surface of the substrate, the hard strip-shaped structures are made of a hard coating material, and the soft strip-shaped structures are made of a soft coating material.
The hard coating material may be ZrO2、TiN、Al2O3、SiO2And TiO2And the like, and has the characteristics of high hardness, good wear resistance and the like. In some examples of this embodiment, the hard coating material is TiO2。
The soft coating material may be WS2、MoS2And the like, and has the characteristic of low friction coefficient. In some examples of this embodiment, the soft coating material MoS2。
Research shows that the soft and hard composite film of the invention is formed by TiO2And MoS2The effect of the alternately formed thin film is better.
In order to increase the bonding force between the substrate and the hard-soft composite film, a transition layer needs to be arranged between the hard-soft composite film and the substrate, and the transition layer is made of a hard coating material.
The invention provides a preparation process for alternately depositing soft and hard composite films by an electro-jet method based on a mask plate, the mask plate is provided with a plurality of strip-shaped cavities, the mask plate is covered on the surface of a matrix, a hard coating material precursor is deposited in the cavities of the mask plate by the electro-jet deposition method, the deposited hard coating material precursor is sintered to form hard strip-shaped structures, the mask plate is covered on the surface of the matrix, the cavities of the mask plate are positioned between the hard strip-shaped structures, then a soft coating material is deposited in the cavities of the mask plate by the electro-jet deposition method, and the deposited soft coating material is subjected to heat treatment to obtain the soft coating material.
In some embodiments of this embodiment, the width of the cavities in the mask is equal to the distance between the cavities. The composition of the soft and hard coating materials is more favorably controlled.
The hard coating material may be ZrO2、TiN、Al2O3、SiO2And TiO2And the like, and has the characteristics of high hardness, good wear resistance and the like. In some examples of this embodiment, the hard coating material is TiO2。
The soft coating material may be WS2、MoS2And the like, and has the characteristic of low friction coefficient. In some examples of this embodiment, the soft coating material MoS2。
In some embodiments of this embodiment, the method comprises the steps of:
preparing hard coating material (ZrO) from hard coating material raw material2、TiN、Al2O3、SiO2、TiO2Etc.) a sol;
applying a soft coating material (WS)2、MoS2Etc.) the powder is uniformly dispersed into the solvent to prepare a soft coating material solution;
cleaning the surface of the substrate;
covering a mask plate on the surface of the substrate after the surface is cleaned, and depositing a hard coating material textured surface on the surface of the substrate in the cavity of the mask plate by using a hard coating material sol through an electro-jet deposition method;
and moving the mask plate to enable the cavities of the mask plate to be aligned to the gaps on the textured surface of the hard coating material, and depositing the soft coating material on the surface of the substrate in the cavities of the mask plate by using a soft coating material solution through an electric jet deposition method.
Specifically, the process of preparing the hard coating material sol from the hard coating material raw material comprises the following steps: under stirring, adding triethanolamine (C)6H15O3N) dropping into absolute ethyl alcohol, simultaneously dropping into hard coating material raw materials (such as butyl titanate, zirconium N-propoxide and the like), continuously stirring, then standing to obtain a solution A, adding deionized water into the solution A, stirring, and standing to obtain a hard coating material sol.
Specifically, the process of uniformly dispersing the soft coating material powder into the solvent to prepare the soft coating material solution comprises the following steps: and fully mixing the soft coating material powder, ethyl cellulose and absolute ethyl alcohol, and uniformly stirring to obtain the coating.
Specifically, the process of cleaning the surface of the substrate is as follows: the substrate is first ground and polished and then cleaned with an alcohol solution.
Specifically, the parameters of the electrojet deposition of the hard coating material sol are as follows: the height of the metal spray needle from the surface of the cutter base body is 1-5 mm, wherein in one embodiment, the height is 2.5 mm; the movement speed of the metal spray needle is 5-20 mm/s, in one embodiment, the movement speed is 15mm/s, and the direct current voltage is 0-10 kV, in one embodiment, the direct current voltage is 2.7 kV;
specifically, the metal spray needle firstly moves along the XY direction and respectively deposits a hard coating material layer as a transition layer for improving the bonding force with a smooth substrate.
Specifically, the mask plate is fixed on a substrate, at least one layer of hard coating material is deposited in the XY direction of a metal spray needle, each layer of deposited hard coating material is placed on a preheating platform for heating, and the mask plate is removed for sintering after deposition is completed. The preheating platform comprises at least two preheating platforms; preferably two preheating temperatures are 200-300 ℃ and 350-450 ℃. Placing the materials in different preheating platforms from low temperature to high temperature in sequence, wherein the placing time is 55-65 s and 55-65 s respectively. The sintering temperature is 350-450 ℃.
Specifically, the parameters of the solution for depositing the soft coating material by the electric jet are as follows: the height of the metal spray needle from the surface of the cutter base body is 1-5 mm, wherein in one embodiment, the height is 2.5 mm; the movement speed of the metal spray needle is 5-20 mm/s, in one embodiment, the movement speed is 10mm/s, and the direct current voltage is 0-10 kV, in one embodiment, the direct current voltage is 3.1 kV.
Process for electrojet deposition of soft coating materials and TiO2The same, except that the sintering process is omitted.
Specifically, the substrate is a TC4 titanium alloy.
The third embodiment of the invention provides an application of the soft-hard composite film on the surface of a friction part.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1
As shown in fig. 1, a preparation process for alternately depositing soft and hard composite films by an electro-fluidic method based on a mask plate includes the following steps: covering a mask plate on the surface of the pretreated metal matrix in an electric jet alternating deposition mode, and sequentially depositing a hard coating TiO2Textured surfaces and MoS2Solid lubricant, eventually forming TiO with an alternating structure2-MoS2The soft and hard composite film, as shown in FIG. 2, comprises TiO2Textured surface 1, MoS2Alternate filler 2, TiO2Transition layer 3, metal matrix 4.
The preparation process comprises the following steps:
(1)TiO2preparing sol: under stirring, 1mL triethanolamine (C)6H15O3N) was slowly dropped into 12mL of anhydrous ethanol, and 3mL of butyl titanate (C) was slowly dropped16H36O4Ti) is dropped into the solution, the solution is placed on a magnetic stirrer at the temperature of 25 ℃ and stirred for 30min at the speed of 300r/min, and then the solution is kept still for 30min to obtain solution A. Then adding 1mL of deionized water into the solution A at the same temperature, placing the solution A on a magnetic stirrer, stirring the solution A at the speed of 500r/min for 60min, and standing the solution A for 24h to obtain stable and uniform TiO2And (3) sol.
(2)MoS2Preparing a solution: 0.5g of MoS with a particle size of 100nm2The powder, 0.1g of ethylcellulose and 2.5g of absolute ethanol are mixed thoroughly and stirred at a temperature of 25 ℃ for 10h at a speed of 400r/min on a magnetic stirrer, and stirring is continued before use in order to prevent precipitation of the powder.
(3) And (3) grinding and polishing the TC4 metal substrate, and then cleaning the TC4 metal substrate in an alcohol solution for 15min to finish the pretreatment of the substrate surface.
(4)TiO2Preparation of textured surface: adopting an electric jet deposition method, firstly depositing TiO on the surface of a pretreated substrate by using a mask plate2Texturing the surface, selecting a spray needle with an inner diameter of 0.4mm, adjusting the distance between the needle head and the substrate to be about 2.5mm, and uniformly spraying TiO at a speed of 6 muL/min by using an injection pump2Injecting the sol into a spray needle, and adjusting a high-voltage power supply to 2.7 kV. The metal spray needle firstly moves along the XY direction to deposit a layer of TiO respectively2Layer as overAnd the transition layer is used for improving the bonding force between the alternating layer and the smooth substrate. Fixing the mask on the substrate, and depositing 6 layers of TiO according to the above method2And sequentially placing each deposited layer on a preheating platform at 250 ℃ and 400 ℃ for heating for 60s respectively, removing the mask plate after deposition is finished, placing the mask plate in a muffle furnace for sintering at 400 ℃, and cooling the mask plate to room temperature along with the furnace to obtain a sample B.
(5)MoS2Deposition of alternating fillers: selecting a spray needle with an inner diameter of 0.6mm, adjusting the distance between the needle head and the matrix to be about 0.5mm, and uniformly spraying MoS at a speed of 6 mu L/min by using an injection pump2Injecting the solution into a spray needle, adjusting a high-voltage power supply to 3.1kV, and fixing the mask plate in the obtained TiO by translating for 1mm2On textured surface sample B, 4 layers of MoS were deposited as described above2And each deposited layer is sequentially placed on a preheating platform at the temperature of 150 ℃ and 300 ℃ for heating for 60 s. And removing the mask plate after the deposition is finished to obtain the stable alternative thin film.
The characterization of the alternating films obtained is shown in FIG. 3, indicating that the above process produces the desired MoS with alternating structure2-TiO2A soft and hard composite film. MoS2-TiO2Graph of coefficient of friction of soft and hard composite film, MoS, as shown in FIG. 42-TiO2The friction coefficient curve of the soft and hard composite film is positioned in MoS2Below the curve of coefficient of friction for the film, the MoS prepared in this example is shown2-TiO2The soft and hard composite film has a MoS ratio2Lower coefficient of friction for the film, demonstrating the MoS prepared in this example2-TiO2The soft and hard composite film has better friction reduction and wear resistance.
Example 2
(1)TiO2Preparing sol: under stirring, 1mL triethanolamine (C)6H15O3N) was slowly dropped into 12mL of anhydrous ethanol, and 3mL of butyl titanate (C) was slowly dropped16H36O4Ti) is dropped into the solution, the solution is placed on a magnetic stirrer at the temperature of 25 ℃ and stirred for 30min at the speed of 300r/min, and then the solution is kept still for 30min to obtain solution B. Then adding 1mL of deionized water into the solution B at the same temperature, placing the solution B on a magnetic stirrer, stirring the solution B at the speed of 500r/min for 60min, and standing the solution BAfter 24 hours, stable and uniform TiO is obtained2And (3) sol.
(2)MoS2Preparing a solution: 0.5g of MoS with a particle size of 100nm2The powder, 0.1g of ethylcellulose and 2.5g of absolute ethanol are mixed thoroughly and stirred at a temperature of 25 ℃ for 10h at a speed of 400r/min on a magnetic stirrer, and stirring is continued before use in order to prevent precipitation of the powder.
(3) Grinding and polishing a TC4 metal matrix, and then cleaning the metal matrix in an alcohol solution for 15min to finish the pretreatment of the surface of the matrix;
(4)TiO2deposition of textured surface: depositing TiO on the surface of the pretreated substrate by adopting an electric jet deposition method2Texturing the surface, selecting a spray needle with an inner diameter of 0.4mm, adjusting the distance between the needle head and the substrate to be about 2mm, and uniformly spraying TiO at a speed of 6 muL/min by using an injection pump2Injecting the sol into a spray needle, and adjusting a high-voltage power supply to 2.8 kV. The metal nozzle first deposits a layer of TiO at a speed of 15mm/s in the XY direction2The layer serves as a transition layer to improve the bonding force with the smooth substrate. Fixing the mask on the substrate, and depositing 8 layers of TiO according to the above method2And sequentially placing each deposited layer on a preheating platform at 250 ℃ and 400 ℃ for heating for 60s respectively, removing the mask plate after deposition is finished, placing the mask plate in a muffle furnace for sintering at 600 ℃, and cooling the mask plate to room temperature along with the furnace to obtain a sample A.
(5)MoS2Deposition of alternating fillers: selecting a spray needle with an inner diameter of 0.6mm, adjusting the distance between the needle head and the matrix to be about 5mm, and uniformly spraying MoS at a speed of 7 mu L/min by using an injection pump2Injecting the solution into a spray needle, adjusting a high-voltage power supply to 3.2kV, and fixing the mask plate in the obtained TiO by translating for 1mm2On textured surface sample A, 5 layers of MoS were deposited on the XY stage at a rate of 15mm/s in the manner described above2Each deposited layer is sequentially placed on a preheating platform at the temperature of 150 ℃ and 300 ℃ for heating for 70 s. And removing the mask plate after the deposition is finished to obtain the stable soft and hard composite film.
Example 3
(1)ZrO2Preparing sol: selecting zirconium (C) n-propoxide under the stirring state12H28O4Zr)2g, acetic acid 0.5g and absolute ethyl alcohol 9g are fully mixed,placing the mixture on a magnetic stirrer at room temperature, stirring the mixture for 1h at a speed of 500r/min, standing the mixture for 24h to obtain stable and uniform ZrO2And (3) sol.
(2)WS2Preparing a solution: 0.5g of WS having a particle size of 100nm2The powder, 0.1g of ethylcellulose and 2.5g of absolute ethanol are mixed thoroughly and stirred at a temperature of 25 ℃ for 10h at a speed of 400r/min on a magnetic stirrer, and stirring is continued before use in order to prevent precipitation of the powder.
(3) Grinding and polishing a TC4 metal matrix, and then cleaning the metal matrix in an alcohol solution for 15min to finish the pretreatment of the surface of the matrix;
(4)ZrO2deposition of textured surface: firstly depositing ZrO on the surface of the pretreated matrix by adopting an electric jet deposition method2Texturing the surface, selecting a spray needle with an inner diameter of 0.4mm, adjusting the distance between a needle head and a substrate to be about 2mm, and uniformly spraying ZrO at a speed of 6 mu L/min by using an injection pump2Injecting the sol into a spray needle, and adjusting a high-voltage power supply to 2.7 kV. The metal nozzle first deposits a layer of ZrO at a rate of 15mm/s in each case in the XY direction2The layer serves as a transition layer to improve the bonding force between the alternating and smooth substrates. Fixing the mask on the substrate, and depositing 6 layers of ZrO according to the above method2And sequentially placing each deposited layer on a preheating platform at 250 ℃ and 400 ℃ for heating for 60s respectively, removing the mask plate after deposition is finished, placing the mask plate in a muffle furnace for sintering at 600 ℃, and cooling the mask plate to room temperature along with the furnace to obtain a sample A.
(5)WS2Deposition of alternating fillers: selecting a spray needle with an inner diameter of 0.6mm, adjusting the distance between the needle head and the substrate to be about 5mm, and uniformly spraying WS at a speed of 7 muL/min by using an injection pump2Injecting the solution into a spray needle, adjusting a high-voltage power supply to 3.2kV, and fixing the mask plate in the obtained ZrO at a distance of 1mm in a translation manner2On the textured surface sample A, 4 layers of WS were deposited by means of the XY-stage in the manner described above at a speed of 10mm/s2And each deposited layer is sequentially placed on a preheating platform at the temperature of 150 ℃ and 300 ℃ for heating for 60 s. And removing the mask plate after the deposition is finished to obtain the stable soft and hard composite film.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The utility model provides a soft or hard composite film, the film is used for adhering to at the base member surface, characterized by, the film comprises a plurality of stereoplasm bar structures and a plurality of soft bar structure in turn, and every bar structure and every soft bar structure are connected with the base member surface simultaneously, stereoplasm bar structure's material is the hard coating material, soft bar structure's material is the soft coating material.
2. The soft-hard composite film according to claim 1, wherein the hard coating material is TiO2；
Or, soft coating material MoS2。
3. A preparation process for alternately depositing soft and hard composite films by an electro-jet method based on a mask plate is characterized in that the mask plate is provided, a plurality of strip-shaped cavities are formed in the mask plate, the mask plate covers the surface of a base body, a hard coating material precursor is deposited in the cavities of the mask plate by the electro-jet deposition method, the deposited hard coating material precursor is sintered to form hard strip-shaped structures, the mask plate covers the surface of the base body, the cavities of the mask plate are located between the hard strip-shaped structures, then a soft coating material is deposited in the cavities of the mask plate by the electro-jet deposition method, and the deposited soft coating material is subjected to heat treatment to obtain the soft coating material.
4. The mask-based process for alternately depositing soft and hard composite films by an electro-fluidic method according to claim 3, wherein the width of the holes in the mask is equal to the distance between the holes.
5. The mask-based process for preparing soft and hard composite films by alternate electrojet deposition according to claim 3, wherein the hard coating material is TiO2(ii) a Or, soft coating material MoS2。
6. The mask-based process for preparing soft and hard composite films by alternate deposition of an electro-fluidic method according to claim 3, which comprises the following steps:
preparing a hard coating material sol from a hard coating material raw material;
uniformly dispersing the soft coating material powder into a solvent to prepare a soft coating material solution;
cleaning the surface of the substrate;
covering a mask plate on the surface of the substrate after the surface is cleaned, and depositing a hard coating material textured surface on the surface of the substrate in the cavity of the mask plate by using a hard coating material sol through an electro-jet deposition method;
and moving the mask plate to enable the cavities of the mask plate to be aligned with the gaps on the textured surface of the hard coating material, and depositing the soft coating material on the surface of the substrate in the cavities of the mask plate by using a soft coating material solution through an electric jet deposition method.
7. The mask-based process for preparing soft and hard composite films by alternate deposition through an electro-fluidic method according to claim 6, wherein the process of preparing hard coating material raw materials into hard coating material sol comprises the following steps: under the stirring state, dripping triethanolamine into absolute ethyl alcohol, simultaneously dripping a hard coating material raw material, continuously stirring, standing to obtain a solution A, adding deionized water into the solution A, stirring, and standing to obtain a hard coating material sol;
or, the process of uniformly dispersing the soft coating material powder into the solvent to prepare the soft coating material solution is as follows: and fully mixing the soft coating material powder, ethyl cellulose and absolute ethyl alcohol, and uniformly stirring to obtain the coating.
8. The mask-based process for preparing soft and hard composite films by alternate deposition of an electro-fluidic method according to claim 6, wherein the process of cleaning the surface of the substrate comprises: firstly, grinding and polishing a substrate, and then cleaning the substrate by adopting an alcohol solution;
or, the metal spray needle firstly moves along the XY direction to deposit a hard coating material layer as a transition layer.
9. The mask-based process for preparing soft and hard composite films by alternate electrojet deposition according to claim 6, wherein the mask is fixed on a substrate, at least one layer of hard coating material is deposited in XY direction of a metal nozzle, each layer is heated on a preheating platform, and the mask is removed for sintering after deposition;
or the substrate is TC4 titanium alloy.
10. The application of the soft-hard composite film as defined in claim 1 or 2 or the soft-hard composite film obtained by the preparation process as defined in any one of claims 3 to 9 on the surface of a friction part.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114717515A (en) * | 2022-04-06 | 2022-07-08 | 北京理工大学 | Hard coating toughening structure and toughness evaluation method |
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| CN108866541A (en) * | 2018-07-17 | 2018-11-23 | 山东大学 | A kind of preparation method of laser assisted electricity jet stream deposition soft and rigid composite coating layer |
| CN111411358A (en) * | 2020-05-18 | 2020-07-14 | 青岛科技大学 | Preparation method of transverse soft-hard alternated self-lubricating coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108866541A (en) * | 2018-07-17 | 2018-11-23 | 山东大学 | A kind of preparation method of laser assisted electricity jet stream deposition soft and rigid composite coating layer |
| CN111411358A (en) * | 2020-05-18 | 2020-07-14 | 青岛科技大学 | Preparation method of transverse soft-hard alternated self-lubricating coating |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114717515A (en) * | 2022-04-06 | 2022-07-08 | 北京理工大学 | Hard coating toughening structure and toughness evaluation method |
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