CN119243287B - Composite coating preparation method and composite coating - Google Patents
Composite coating preparation method and composite coating Download PDFInfo
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Abstract
本公开是关于一种复合涂层的制备方法及复合涂层，涉及金属涂层技术领域，该方法包括：步骤一：将活化处理后的MoS2纳米粉体均匀分散在电解液中，得到复合电解液；步骤二：将钛合金基体放置到所述复合电解液中进行微弧氧化处理，以在所述钛合金基体表面生成带有TiO2/MoS2的微弧氧化层；步骤三：将带有TiO2/MoS2的微弧氧化层的钛合金基体浸入封孔液中，随后进行干燥处理，得到带有封孔TiO2耐蚀层的基材；步骤四：将带有封孔TiO2耐蚀层的基材放置于气相沉积设备的真空腔室内作为阳极，采用MoS2靶材及Ti靶材作为阴极，在真空度为1Pa的氩气氛围下进行镀膜处理，以在带有封孔TiO2耐蚀层的基材表面形成耐磨蚀的复合涂层。本公开提高了复合涂层的耐腐蚀性。
The present disclosure is about a preparation method of a composite coating and the composite coating, and relates to the technical field of metal coatings. The method comprises: step 1: uniformly dispersing the activated MoS2 nanopowder in an electrolyte to obtain a composite electrolyte; step 2: placing a titanium alloy substrate in the composite electrolyte for micro-arc oxidation treatment to generate a micro-arc oxidation layer with TiO2 / MoS2 on the surface of the titanium alloy substrate; step 3: immersing the titanium alloy substrate with the micro-arc oxidation layer of TiO2 / MoS2 in a sealing liquid, and then performing a drying treatment to obtain a substrate with a sealed TiO2 corrosion-resistant layer; step 4: placing the substrate with the sealed TiO2 corrosion-resistant layer in a vacuum chamber of a vapor deposition device as an anode, using a MoS2 target and a Ti target as a cathode, and performing a coating treatment in an argon atmosphere with a vacuum degree of 1Pa to form a wear-resistant composite coating on the surface of the substrate with the sealed TiO2 corrosion-resistant layer. The present disclosure improves the corrosion resistance of the composite coating.
Description
Technical Field
The embodiment of the disclosure relates to the technical field of metal coatings, in particular to a preparation method of a composite coating and the composite coating.
Background
The titanium alloy has the advantages of light weight, high strength, high temperature resistance and the like, is an ideal material for large-scale industrial equipment, complicated service environment, harsh component working conditions, long-term development of service life requirements, and is widely applied to the fields of aerospace, ocean, nuclear energy, chemical industry, medical treatment and the like. However, in the practical application process, the titanium alloy component has the problems of insufficient wear resistance, galvanic corrosion resistance and insufficient hot salt corrosion resistance in the service process, so that the problem that the reliability and service life of the titanium alloy component are reduced in the use process and even the operation safety of the whole equipment is influenced is easily caused.
To solve this problem, surface strengthening means may be employed to enhance the surface properties of the titanium alloy member. At present, research and development of coating materials on the surface of titanium alloy are mainly focused on improvement of wear resistance, but on the basis of the wear resistance, how to reduce the actions of galvanic corrosion between titanium alloy and dissimilar materials, hot salt corrosion in a high-temperature salt-containing environment and the like is also a problem to be solved.
Disclosure of Invention
The present disclosure aims to provide a method for preparing a composite coating and a composite coating, and further overcome at least to some extent the problems of how to reduce galvanic corrosion between titanium alloy and dissimilar materials and hot salt corrosion in high temperature salt-containing environments due to limitations and drawbacks of the related art.
According to one aspect of the present disclosure, there is provided a method of preparing a composite coating layer, comprising:
uniformly dispersing the activated MoS 2 nano powder in an electrolyte to obtain a composite electrolyte;
Placing a titanium alloy matrix into the composite electrolyte for micro-arc oxidation treatment to generate a micro-arc oxidation layer with TiO 2/MoS2 on the surface of the titanium alloy matrix;
Immersing the titanium alloy substrate with the micro-arc oxidation layer of TiO 2/MoS2 into hole sealing liquid, and then drying to obtain a substrate with a hole sealing TiO 2 corrosion-resistant layer;
And fourthly, placing the substrate with the hole sealing TiO 2 corrosion-resistant layer in a vacuum chamber of vapor deposition equipment to serve as an anode, adopting a MoS 2 target material and a Ti target material as a cathode, and performing film coating treatment under an argon atmosphere with the vacuum degree of 1Pa to form an abrasion-resistant composite coating on the surface of the substrate with the hole sealing TiO 2 corrosion-resistant layer.
In an exemplary embodiment of the present disclosure, the activated MoS 2 nano-powder used in the preparation process of the composite electrolyte is obtained by immersing 10-20g of MoS 2 nano-powder in a mixed solution of 0.05-0.1g of sodium dodecyl sulfate and 200-300g of ethanol, stirring for 2 hours, obtaining an activated mixed solution, and drying and sieving the activated mixed solution to obtain activated MoS 2 nano-powder.
In an exemplary embodiment of the disclosure, the preparation process of the composite electrolyte is obtained by preparing 1-5g/L of activated MoS 2 nano powder, 10-15g/L of sodium silicate, 0.5-1g/L of sodium hypophosphite, 2-5g/L of sodium tungstate and 2-8ml/L of glycerin into the electrolyte, continuously stirring for 1-2h, and ultrasonically oscillating for 0.5-1.5h, so that the activated MoS 2 nano powder is uniformly distributed in the electrolyte.
In an exemplary embodiment of the present disclosure, in the preparation of the micro-arc oxidation layer with TiO 2/MoS2, the frequency used in the micro-arc oxidation process is 400-800Hz, the positive duty cycle is 5-30%, the negative duty cycle is 5-30%, the positive voltage is 350-500V, the negative voltage is 10-50V, and the oxidation time is 20-40min.
In an exemplary embodiment of the present disclosure, the hole sealing liquid is prepared by:
1) Mixing 0.5-1.5g/L of silane coupling agent with 2-10g/L of organic solvent to obtain a solvent mixing result;
2) Stirring the solvent mixing result for 36-48h to activate the solvent mixing result to obtain a solvent activating result;
3) Adding 5-10g/L potassium fluozirconate, 1-3g/L nano titanium dioxide and 1-5g/L triethanolamine into the solvent activation result, and performing ultrasonic vibration for 0.5h to obtain the hole sealing liquid.
In an exemplary embodiment of the disclosure, the substrate with the hole-sealing TiO 2 corrosion-resistant layer is prepared by placing a titanium alloy substrate with a micro-arc oxidation layer of TiO 2/MoS2 in a hole-sealing liquid, soaking for 5-10min, placing the soaked titanium alloy substrate in an oven for 15min at 160 ℃, repeating the baking for 3-5 times, and then drying for 30min again to obtain the substrate with the hole-sealing TiO 2 corrosion-resistant layer.
In an exemplary embodiment of the disclosure, the composite coating is prepared by 1) placing a substrate with a hole-sealing TiO 2 corrosion-resistant layer in a vacuum chamber of a vapor deposition device, keeping the vacuum degree at 1Pa, 2) turning on a MoS 2 target, wherein the power source is a radio frequency power source, the sputtering power of the radio frequency power source is set to be 200-250W, 3) turning on a Ti target, the power source is a direct current power source, the current magnitude of the direct current power source is set to be 50-100A, the bias voltage is set to be-200V to-400V, the duty ratio is 40-60%, and the deposition time is 1-3h, so as to plate the composite coating on the surface of the substrate with the hole-sealing TiO 2 corrosion-resistant layer.
According to one aspect of the present disclosure, there is provided a composite coating obtained by the method for preparing a composite coating according to any one of the above, the composite coating comprising a micro-arc oxidized TiO 2/MoS2 layer, a TiO 2 hole sealing layer, and a vapor deposited Ti/MoS 2 layer.
In one exemplary embodiment of the present disclosure, the micro-arc oxidized TiO 2/MoS2 layer has a thickness of 10-15 μm, the TiO 2 hole sealing layer has a thickness of 1-1.5 μm, and the vapor deposited Ti/MoS 2 layer has a thickness of 1-3 μm.
In an exemplary embodiment of the present disclosure, the atomic percent of Ti in the vapor deposited Ti/MoS 2 layer is 2% -10%.
In the preparation method of the composite coating provided by the embodiment of the disclosure, on one hand, the activated MoS 2 nano powder is uniformly dispersed in an electrolyte to obtain the composite electrolyte, then a titanium alloy substrate is placed in the composite electrolyte to be subjected to micro-arc oxidation treatment to generate a micro-arc oxidation layer with TiO 2/MoS2 on the surface of the titanium alloy substrate, the titanium alloy substrate with the micro-arc oxidation layer of TiO 2/MoS2 is immersed in a hole sealing liquid and then subjected to drying treatment to obtain a substrate with a hole sealing TiO 2 corrosion resistant layer, finally the substrate with the hole sealing TiO 2 corrosion resistant layer is placed in a vacuum chamber of a vapor deposition device to serve as an anode, a MoS 2 target material and a Ti target material serve as a cathode, film plating treatment is performed under an argon atmosphere with the vacuum degree of 1Pa to form an abrasion-resistant composite coating on the surface of the substrate with the hole sealing TiO 2 corrosion resistant layer, and further the abrasion-resistant composite coating can be improved due to the fact that the micro-arc oxidation mode can be adopted on the surface of the titanium alloy substrate to generate the micro-arc oxidation layer with TiO 2/MoS2, and on the other hand, the hole sealing method can be adopted to further improve the abrasion resistance of the titanium alloy.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the disclosure and together with the description, serve to explain the principles of the disclosure. It will be apparent to those of ordinary skill in the art that the drawings in the following description are merely examples of the disclosure and that other drawings may be derived from them without undue effort.
Fig. 1 schematically illustrates a flow chart of a method of preparing a composite coating according to an example embodiment of the present disclosure.
Fig. 2 schematically illustrates an example diagram of a composite coating obtained based on example 2, according to an example embodiment of the present disclosure.
Fig. 3 schematically illustrates an example graph of a micro-arc oxidation layer based on comparative example 1, according to an example embodiment of the present disclosure.
FIG. 4 schematically illustrates a topography obtained after hot salt corrosion of a surface coating of a titanium alloy substrate according to an example embodiment of the present disclosure.
Fig. 5 schematically illustrates a topography obtained after hot salt corrosion of the composite coating obtained based on example 2, according to an example embodiment of the present disclosure.
Fig. 6 schematically illustrates a topography obtained after hot salt etching based on the surface of the micro-arc oxidation layer obtained in comparative example 1, according to an example embodiment of the present disclosure.
Detailed Description
Example embodiments will now be described more fully with reference to the accompanying drawings. However, the exemplary embodiments may be embodied in many forms and should not be construed as limited to the examples set forth herein, but rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of the exemplary embodiments to those skilled in the art. The described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. In the following description, numerous specific details are provided to give a thorough understanding of embodiments of the present disclosure. One skilled in the relevant art will recognize, however, that the aspects of the disclosure may be practiced without one or more of the specific details, or with other methods, components, devices, steps, etc. In other instances, well-known technical solutions have not been shown or described in detail to avoid obscuring aspects of the present disclosure.
The terms "a," "an," "the," and "said" are used in this specification to denote the presence of one or more elements/components, etc., the terms "comprising" and "having" are used in an open-ended fashion and mean that there may be additional elements/components, etc., in addition to the listed elements/components, etc., and the terms "first" and "second," etc., are used merely as labels, and are not limiting in number of their objects.
Aiming at the problem that galvanic corrosion between titanium alloy and dissimilar materials and hot salt corrosion in a high-temperature salt-containing environment cannot be reduced in the related art, the embodiment of the disclosure firstly provides a preparation method of a composite coating. Specifically, referring to fig. 1, the preparation method of the composite coating may include the following steps:
Step S110, uniformly dispersing the MoS 2 nano powder after the activation treatment in an electrolyte to obtain a composite electrolyte;
Step S120, placing a titanium alloy matrix into the composite electrolyte for micro-arc oxidation treatment to generate a micro-arc oxidation layer with TiO 2/MoS2 on the surface of the titanium alloy matrix;
Step S130, immersing the titanium alloy substrate with the micro-arc oxidation layer of TiO 2/MoS2 into hole sealing liquid, and then drying to obtain a substrate with a hole sealing TiO 2 corrosion-resistant layer;
And step S140, placing the substrate with the hole sealing TiO 2 corrosion-resistant layer in a vacuum chamber of vapor deposition equipment to serve as an anode, adopting a MoS 2 target material and a Ti target material as a cathode, and performing film coating treatment under an argon atmosphere with the vacuum degree of 1Pa to form an abrasion-resistant composite coating on the surface of the substrate with the hole sealing TiO 2 corrosion-resistant layer.
According to the preparation method of the composite coating, on one hand, moS 2 nano powder after activation treatment is uniformly dispersed in electrolyte to obtain the composite electrolyte, then a titanium alloy substrate is placed in the composite electrolyte to be subjected to micro-arc oxidation treatment to generate a micro-arc oxidation layer with TiO 2/MoS2 on the surface of the titanium alloy substrate, the titanium alloy substrate with the micro-arc oxidation layer of TiO 2/MoS2 is immersed in hole sealing liquid and then subjected to drying treatment to obtain a base material with a hole sealing TiO 2 corrosion-resistant layer, finally the base material with the hole sealing TiO 2 corrosion-resistant layer is placed in a vacuum chamber of a vapor deposition device to serve as an anode, a MoS 2 target material and a Ti target material serve as a cathode, film plating treatment is performed under an argon atmosphere with the vacuum degree of 1Pa, so that an abrasion-resistant composite coating is formed on the surface of the base material with the hole sealing TiO 2 layer, and further abrasion-resistant performance of the titanium alloy can be improved due to the fact that the micro-arc oxidation mode can be adopted to generate the micro-arc oxidation layer with TiO 2/MoS2 on the surface of the titanium alloy substrate, and on the other hand, the hole sealing method can be adopted to further improve the abrasion-resistant performance of the titanium alloy, and further corrosion-resistant performance of the composite coating with the hole sealing TiO 2 layer can be obtained.
The preparation method of the composite coating provided by the invention further needs to be additionally described, wherein in the practical application process, firstly, a composite micro-arc oxidation layer is prepared in the first stage to improve the antifriction and wear resistance of the composite coating, secondly, the corrosion resistance of the composite coating is improved through multi-step hole sealing in the second stage, the Ti/MoS 2 composite coating is prepared in the third stage through a vapor deposition method, the antifriction performance of the composite coating is further improved, and finally, the problems of insufficient antifriction, galvanic corrosion resistance and hot salt corrosion resistance of the titanium alloy are effectively overcome through the optimal design of the components and the structure of the composite coating on the surface of the titanium alloy.
Hereinafter, each step involved in the preparation method of the composite coating will be explained and described in detail. Specific:
in step S110, the activated MoS 2 nano powder is uniformly dispersed in the electrolyte to obtain a composite electrolyte.
Specifically, the activated MoS 2 nano powder used in the preparation process of the composite electrolyte is obtained by immersing 10-20g of MoS 2 nano powder in a mixed solution of 0.05-0.1g of sodium dodecyl sulfate and 200-300g of ethanol, stirring for 2 hours to obtain an activated mixed solution, and drying and sieving the activated mixed solution to obtain activated MoS 2 nano powder. Further, under the premise, the preparation process of the composite electrolyte is obtained by preparing 1-5g/L of activated MoS 2 nano powder, 10-15g/L of sodium silicate, 0.5-1g/L of sodium hypophosphite, 2-5g/L of sodium tungstate and 2-8ml/L of glycerol into the electrolyte, continuously stirring for 1-2h, ultrasonically oscillating for 0.5-1.5h, and uniformly distributing the activated MoS 2 nano powder in the electrolyte.
In step S120, a titanium alloy substrate is placed in the composite electrolyte to perform micro-arc oxidation treatment, so as to generate a micro-arc oxidation layer with TiO 2/MoS2 on the surface of the titanium alloy substrate.
Specifically, in the preparation process of the micro-arc oxidation layer with the TiO 2/MoS2, the frequency used in the micro-arc oxidation treatment process is 400-800Hz, the positive duty ratio is 5-30%, the negative duty ratio is 5-30%, the positive voltage is 350-500V, the negative voltage is 10-50V, and the oxidation time is 20-40min.
In step S130, the titanium alloy substrate with the micro-arc oxidation layer of TiO 2/MoS2 is immersed in the hole sealing liquid, and then dried to obtain the substrate with the hole sealing TiO 2 corrosion resistant layer.
Specifically, the hole sealing liquid is prepared by 1) mixing 0.5-1.5g/L of silane coupling agent with 2-10g/L of organic solvent to obtain a solvent mixing result, 2) stirring the solvent mixing result for 36-48h to activate the solvent mixing result to obtain a solvent activation result, and 3) adding 5-10g/L of potassium fluozirconate, 1-3g/L of nano titanium dioxide and 1-5g/L of triethanolamine into the solvent activation result, and performing ultrasonic vibration for 0.5h to obtain the hole sealing liquid. The silane coupling agent described here is KH507.
Under the premise, the base material with the hole sealing TiO 2 corrosion-resistant layer is prepared by placing a titanium alloy base body with a micro-arc oxidation layer of TiO 2/MoS2 in hole sealing liquid, soaking for 5-10min, placing the soaked titanium alloy base body in an oven for 15min at 160 ℃, repeating the baking for 3-5 times, and then drying for 30min again, so that the base material with the hole sealing TiO 2 corrosion-resistant layer can be obtained.
In step S140, the substrate with the hole-sealing TiO 2 corrosion-resistant layer is placed in a vacuum chamber of a vapor deposition apparatus as an anode, a MoS 2 target and a Ti target are used as a cathode, and a film plating treatment is performed under an argon atmosphere with a vacuum degree of 1Pa, so as to form an abrasion-resistant composite coating on the surface of the substrate with the hole-sealing TiO 2 corrosion-resistant layer.
Specifically, the composite coating is prepared by 1) placing a substrate with a hole-sealing TiO 2 corrosion-resistant layer in a vacuum chamber of vapor deposition equipment, keeping the vacuum degree at 1Pa, 2) starting a MoS 2 target, wherein the power is a radio frequency power supply, the sputtering power of the radio frequency power supply is set to be 200-250W, 3) starting a Ti target, the power is a direct current power supply, the current of the direct current power supply is set to be 50-100A, the bias voltage is set to be-200V to-400V, the duty ratio is 40-60%, and the deposition time is 1-3h, so that the composite coating is plated on the surface of the substrate with the hole-sealing TiO 2 corrosion-resistant layer.
Further, the composite coating obtained based on the preparation method of the composite coating can comprise a micro-arc oxidation TiO 2/MoS2 layer, a TiO 2 hole sealing layer and a vapor deposition Ti/MoS 2 layer, wherein the thickness of the micro-arc oxidation TiO 2/MoS2 layer is 10-15 mu m, the thickness of the TiO 2 hole sealing layer is 1-1.5 mu m, the thickness of the vapor deposition Ti/MoS 2 layer is 1-3 mu m, the atomic percentage of Ti in the vapor deposition Ti/MoS 2 layer is 2-10%, and the composite coating obtained based on the exemplary embodiment of the disclosure can be used for TA2, TC4, TC6, TC11, ti5331 and other brands of alloys.
The preparation method of the composite coating described in the exemplary embodiments of the present disclosure has been fully achieved so far. Based on the foregoing, it can be seen that the preparation method of the composite coating according to the exemplary embodiment of the disclosure has at least the advantages that, on one hand, the micro-arc oxidation method is adopted to treat the TC6 alloy, the activated MoS 2 nano powder is uniformly dispersed into the electrolyte to obtain the TiO 2/MoS2 coating, so that the antifriction and wear-resistant performances of the TC6 alloy can be greatly improved, on the other hand, the multi-step hole sealing method is adopted to obtain the TiO 2 corrosion-resistant layer, so that the corrosion-resistant performances of the coating are further improved, and finally, the physical vapor deposition method is adopted to prepare the MoS 2/Ti antifriction layer, on the other hand, the exemplary embodiment of the disclosure adopts a typical multi-layer design to prepare the composite coating on the surface of the TC6 alloy by combining micro-arc oxidation with physical vapor deposition, so that the advantages of different coating components are combined, the antifriction and wear-resistant performances and the heat-resistant salt corrosion-resistant performances of the composite coating can be greatly improved, and the use requirements of various complex working conditions can be met, and the composite coating has good applicability.
The method of preparing the composite coating will be further explained and illustrated with reference to specific examples. Specific:
example 1A method for preparing a composite coating and a composite coating comprising the steps of:
Uniformly dispersing the activated MoS 2 nano powder in the electrolyte to obtain the composite electrolyte.
And secondly, placing the clean titanium alloy matrix in the composite electrolyte of the first step for micro-arc oxidation treatment to obtain a TiO 2/MoS2 micro-arc oxidation layer on the surface of the titanium alloy matrix.
And thirdly, immersing the titanium alloy substrate with the TiO 2/MoS2 micro-arc oxidation layer in the hole sealing liquid, and then drying to obtain the substrate with the hole sealing TiO 2 corrosion-resistant layer.
And step four, placing the sample obtained in the step three in a vacuum chamber of vapor deposition equipment to serve as an anode, adopting a MoS 2 target and a Ti target as cathodes, performing film coating treatment under the argon atmosphere with the vacuum degree of 1Pa, and forming a MoS 2/Ti layer on the surface to obtain the abrasion-resistant composite coating.
In the first step of the embodiment, the activation method of the MoS 2 nano powder comprises the steps of immersing 10gMoS 2 nano powder in a mixed solution of 0.05g of sodium dodecyl sulfate and 200g of ethanol, stirring for 2 hours for activation treatment, and then drying and sieving to obtain the activated MoS 2 nano powder.
In the first step of the embodiment, the preparation method of the composite electrolyte comprises the steps of preparing 1g/L of activated MoS 2 nano powder, 10g/L of sodium silicate, 0.5g/L of sodium hypophosphite, 2g/L of sodium tungstate and 4ml/L of glycerin into the electrolyte, continuously stirring for 1h, carrying out ultrasonic vibration for 0.5h, and uniformly distributing the activated MoS 2 nano powder in the electrolyte. Meanwhile, in the second step of the embodiment, the preparation method of the TiO 2/MoS2 micro-arc oxidation layer is 400Hz, the positive duty ratio is 30%, the negative duty ratio is 30%, the positive voltage is 350V, the negative voltage is 10V, and the oxidation time is 40min. Further, in the third step of the embodiment, the hole sealing liquid is prepared by mixing 1.5g/L KH507 with 10g/L organic solvent, stirring for 48h for activation, and then adding 10g/L potassium fluozirconate, 3g/L nano titanium dioxide and 3g/L triethanolamine, and performing ultrasonic vibration for 0.5h. Further, in the third step of the embodiment, the hole sealing layer preparation method is that the base material with the TiO 2/MoS2 micro-arc oxidation layer in the second step is placed in the hole sealing liquid to be soaked for 5min, then is placed in an oven to be dried for 15min at 160 ℃, and is dried for 30min after repeating for 3 times, so that the base material with the hole sealing TiO 2 corrosion resistant layer is obtained. Finally, in the fourth step of this embodiment, the Ti/MoS 2 layer is prepared by placing the substrate obtained in the third step in a vacuum chamber of a vapor deposition apparatus, maintaining the vacuum degree at 1Pa, then starting the MoS 2 target, using a radio frequency power source, and setting the sputtering power to 200W. The Ti target is started, the power supply is a direct current power supply, and the current is set to be 50A. The bias voltage was set at-200V, the duty cycle was 40%, the deposition time was 1h, and the Ti/MoS 2 composite layer was plated.
And, the composite coating in this embodiment is composed of a micro-arc oxidized TiO 2/MoS2 layer, a TiO 2 hole sealing layer and a vapor deposition Ti/MoS 2 layer. Wherein the thickness of the TiO 2/MoS2 layer is 10 mu m, the hole sealing layer of the TiO 2 layer is 1 mu m, the vapor deposition Ti/MoS 2 layer is 1 mu m, and the atomic percentage of Ti in the Ti/MoS 2 layer is 2%.
Example 2A method for preparing a composite coating and a composite coating comprising the steps of:
Uniformly dispersing the activated MoS 2 nano powder in the electrolyte to obtain the composite electrolyte.
And secondly, placing the clean titanium alloy matrix in the composite electrolyte of the first step for micro-arc oxidation treatment to obtain a TiO 2/MoS2 micro-arc oxidation layer on the surface of the titanium alloy matrix.
And thirdly, immersing the titanium alloy substrate with the TiO 2/MoS2 micro-arc oxidation layer in the hole sealing liquid, and then drying to obtain the substrate with the hole sealing TiO 2 corrosion-resistant layer.
And step four, placing the sample obtained in the step three in a vacuum chamber of vapor deposition equipment to serve as an anode, adopting a MoS 2 target and a Ti target as cathodes, performing film coating treatment under the argon atmosphere with the vacuum degree of 1Pa, and forming a MoS 2/Ti layer on the surface to obtain the abrasion-resistant composite coating.
In the first step of the embodiment, the activation method of the MoS 2 nano powder comprises the steps of immersing 20. 20gMoS 2 nano powder in a mixed solution of 0.08g of sodium dodecyl sulfate and 250g of ethanol, stirring for 2 hours for activation treatment, and then drying and sieving to obtain the activated MoS 2 nano powder. Meanwhile, in the first step of the embodiment, the preparation method of the composite electrolyte comprises the steps of preparing 3g/L of activated MoS 2 nano powder, 12g/L of sodium silicate, 0.8g/L of sodium hypophosphite, 4g/L of sodium tungstate and 2ml/L of glycerin into the electrolyte, continuously stirring for 1.5h, carrying out ultrasonic vibration for 1h, and uniformly distributing the activated MoS 2 nano powder in the electrolyte. Secondly, in the second step of the embodiment, the preparation method of the TiO 2/MoS2 micro-arc oxidation layer is that the frequency is 600Hz, the positive duty ratio is 15%, the negative duty ratio is 15%, the positive voltage is 450V, the negative voltage is 30V, and the oxidation time is 30min. Further, in the third step of the embodiment, the hole sealing liquid is prepared by mixing 1g/L KH507 with 5g/L organic solvent, stirring for 48h for activation, and then adding 8g/L potassium fluozirconate, 1.5g/L nano-titanium dioxide and 5g/L triethanolamine, and performing ultrasonic vibration for 0.5h. further, in the third step of the embodiment, the hole sealing layer is prepared by placing the substrate with the TiO 2/MoS2 micro-arc oxidation layer in the second step in the hole sealing liquid, soaking for 5min, placing in an oven, drying for 15min at 160 ℃, repeating for 4 times, and drying for 30min to obtain the substrate with the hole sealing TiO2 corrosion resistant layer. Finally, in step four of this example, the Ti/MoS 2 layer preparation method is to place the substrate obtained in step three in a vacuum chamber of a vapor deposition apparatus, keep the vacuum degree at 1Pa, then turn on the MoS 2 target, the power used is a radio frequency power supply, and the sputtering power is set to 220W. The Ti target is started, the power supply is a direct current power supply, and the current is set to be 100A. The bias voltage was set at-300V, the duty cycle was 50%, the deposition time was 2h, and the Ti/MoS 2 composite layer was plated.
And, the composite coating in this embodiment is composed of a micro-arc oxidized TiO 2/MoS2 layer, a TiO 2 hole sealing layer and a vapor deposition Ti/MoS 2 layer. Wherein the thickness of the TiO 2/MoS2 layer in the composite coating is 12 mu m, the thickness of the TiO 2 hole sealing layer is 1.2 mu m, the thickness of the vapor deposition Ti/MoS 2 layer is 1.8 mu m, and the atomic percentage of Ti in the Ti/MoS 2 layer is 10%. Meanwhile, an electron microscope scan of the composite coating obtained based on this example can be shown with reference to fig. 2.
Example 3A method for preparing a composite coating and a composite coating comprising the steps of:
Uniformly dispersing the activated MoS 2 nano powder in the electrolyte to obtain the composite electrolyte.
And secondly, placing the clean titanium alloy matrix in the composite electrolyte of the first step for micro-arc oxidation treatment to obtain a TiO 2/MoS2 micro-arc oxidation layer on the surface of the titanium alloy matrix.
And thirdly, immersing the titanium alloy substrate with the TiO 2/MoS2 micro-arc oxidation layer in the hole sealing liquid, and then drying to obtain the substrate with the hole sealing TiO 2 corrosion-resistant layer.
And step four, placing the sample obtained in the step three in a vacuum chamber of vapor deposition equipment to serve as an anode, adopting a MoS 2 target and a Ti target as cathodes, performing film coating treatment under the argon atmosphere with the vacuum degree of 1Pa, and forming a MoS 2/Ti layer on the surface to obtain the abrasion-resistant composite coating.
In the first step of the embodiment, the activation method of the MoS 2 nano powder comprises the steps of immersing 20. 20gMoS 2 nano powder in a mixed solution of 0.1g of sodium dodecyl sulfate and 300g of ethanol, stirring for 2 hours for activation treatment, and then drying and sieving to obtain the activated MoS 2 nano powder. Meanwhile, in the first step of the embodiment, the preparation method of the composite electrolyte comprises the steps of preparing 5g/L of activated MoS 2 nano powder, 15g/L of sodium silicate, 1g/L of sodium hypophosphite, 5g/L of sodium tungstate and 4ml/L of glycerin into the electrolyte, continuously stirring for 1.5h, and carrying out ultrasonic vibration for 1.5h to uniformly distribute the activated MoS 2 nano powder in the electrolyte. Secondly, in the second step of the embodiment, the preparation method of the TiO 2/MoS2 micro-arc oxidation layer is that the frequency is 600Hz, the positive duty ratio is 15%, the negative duty ratio is 15%, the positive voltage is 450V, the negative voltage is 30V, and the oxidation time is 30min. Further, in the third step of the embodiment, the hole sealing liquid is prepared by mixing 1g/L KH507 with 5g/L organic solvent, stirring for 48h for activation, and then adding 8g/L potassium fluozirconate, 1.5g/L nano-titanium dioxide and 5g/L triethanolamine, and performing ultrasonic vibration for 0.5h. Further, in the third step of the embodiment, the hole sealing layer is prepared by placing the substrate with the TiO 2/MoS2 micro-arc oxidation layer in the second step in the hole sealing liquid, soaking for 5min, placing in an oven, drying for 15min at 160 ℃, repeating for 4 times, and drying for 30min to obtain the substrate with the hole sealing TiO2 corrosion resistant layer. Finally, in the fourth step of this embodiment, the Ti/MoS 2 layer preparation method is that the substrate obtained in the third step is placed in a vacuum chamber of a vapor deposition apparatus, the vacuum degree is kept at 1Pa, then the MoS 2 target is turned on, the power used is a radio frequency power supply, and the sputtering power is set to 250W. The Ti target is started, the power supply is a direct current power supply, and the current is set to be 100A. The bias voltage was set at-400V, the duty cycle was 60%, the deposition time was 3h, and the Ti/MoS 2 composite layer was plated.
And, the composite coating in this embodiment is composed of a micro-arc oxidized TiO 2/MoS2 layer, a TiO 2 hole sealing layer and a vapor deposition Ti/MoS 2 layer. Wherein the thickness of the TiO 2/MoS2 layer is 13 μm, the hole sealing layer of TiO 2 is 1.2 μm, the vapor deposition Ti/MoS 2 layer is 2 μm, and the atomic percentage of Ti in the Ti/MoS 2 layer is 8%.
Example 4A method for preparing a composite coating and a composite coating comprising the steps of:
Uniformly dispersing the activated MoS 2 nano powder in the electrolyte to obtain the composite electrolyte.
And secondly, placing the clean titanium alloy matrix in the composite electrolyte of the first step for micro-arc oxidation treatment to obtain a TiO 2/MoS2 micro-arc oxidation layer on the surface of the titanium alloy matrix.
And thirdly, immersing the titanium alloy substrate with the TiO 2/MoS2 micro-arc oxidation layer in the hole sealing liquid, and then drying to obtain the substrate with the hole sealing TiO 2 corrosion-resistant layer.
And step four, placing the sample obtained in the step three in a vacuum chamber of vapor deposition equipment to serve as an anode, adopting a MoS 2 target and a Ti target as cathodes, performing film coating treatment under the argon atmosphere with the vacuum degree of 1Pa, and forming a MoS 2/Ti layer on the surface to obtain the abrasion-resistant composite coating.
In the first step of the embodiment, the activating method of the MoS 2 nano powder comprises the steps of immersing 10gMoS 2 nano powder in a mixed solution of 0.1g/L sodium dodecyl sulfate and 200g of ethanol, stirring for 2 hours for activating treatment, and then drying and sieving to obtain the activated MoS 2 nano powder.
In the first step of the embodiment, the preparation method of the composite electrolyte comprises the steps of preparing 5g/L of activated MoS 2 nano powder, 15g/L of sodium silicate, 1g/L of sodium hypophosphite, 5g/L of sodium tungstate and 8ml/L of glycerin into the electrolyte, continuously stirring for 2 hours, ultrasonically oscillating for 1.5 hours, and uniformly distributing the activated MoS 2 nano powder in the electrolyte. Meanwhile, in the second step of the embodiment, the preparation method of the TiO 2/MoS2 micro-arc oxidation layer is that the frequency is 800Hz, the positive duty ratio is 5%, the negative duty ratio is 5%, the positive voltage is 500V, the negative voltage is 50V, and the oxidation time is 20min. Secondly, in the third step of the embodiment, the hole sealing liquid is prepared by mixing 0.5g/L KH507 with 2g/L organic solvent, stirring for 36h for activation, and then adding 5g/L potassium fluozirconate, 1g/L nano titanium dioxide and 1g/L triethanolamine, and carrying out ultrasonic vibration for 0.5h. Further, in the third step of the embodiment, the hole sealing layer preparation method is that the base material with the TiO 2/MoS2 micro-arc oxidation layer in the second step is placed in the hole sealing liquid to be soaked for 5min, then is placed in an oven to be dried for 15min at 160 ℃, and is dried for 30min after repeating for 5 times, so that the base material with the hole sealing TiO 2 corrosion resistant layer is obtained. Finally, in step four of this example, the Ti/MoS 2 layer was prepared by placing the substrate obtained in step three in a vacuum chamber of a vapor deposition apparatus, maintaining the vacuum at 1Pa, then turning on the MoS 2 target, using a radio frequency power source, and setting the sputtering power to 250W. The Ti target is started, the power supply is a direct current power supply, and the current is set to be 100A. The bias voltage was set at-400V, the duty cycle was 60%, the deposition time was 3h, and the Ti/MoS 2 composite layer was plated.
And, the composite coating in this embodiment is composed of a micro-arc oxidized TiO 2/MoS2 layer, a TiO 2 hole sealing layer and a vapor deposition Ti/MoS 2 layer. Wherein the thickness of the TiO 2/MoS2 layer is 15 μm, the thickness of the TiO 2 hole sealing layer is 1 μm, the thickness of the vapor deposition Ti/MoS 2 layer is 2 μm, and the atomic percentage of Ti in the Ti/MoS 2 layer is 8%.
Comparative example 1:
the preparation method of the abrasion-resistant composite coating on the surface of the titanium alloy can comprise the following steps:
Uniformly dispersing the activated MoS 2 nano powder in the electrolyte to obtain the composite electrolyte.
And secondly, placing the clean titanium alloy matrix in the composite electrolyte of the first step for micro-arc oxidation treatment to obtain a TiO 2/MoS2 micro-arc oxidation layer on the surface of the titanium alloy matrix.
In the first step of the embodiment, the activation method of the MoS 2 nano powder comprises the steps of immersing 20. 20gMoS 2 nano powder in a mixed solution of 0.08g of sodium dodecyl sulfate and 250g of ethanol, stirring for 2 hours for activation treatment, and then drying and sieving to obtain the activated MoS 2 nano powder. Meanwhile, in the first step of the embodiment, the preparation method of the composite electrolyte comprises the steps of preparing 3g/L of activated MoS 2 nano powder, 12g/L of sodium silicate, 0.8g/L of sodium hypophosphite, 4g/L of sodium tungstate and 2ml/L of glycerin into the electrolyte, continuously stirring for 1.5h, carrying out ultrasonic vibration for 1h, and uniformly distributing the activated MoS 2 nano powder in the electrolyte.
And, the coating obtained in this comparative example is a micro-arc oxidized TiO 2/MoS2 layer. Meanwhile, an electron microscope scan of the micro-arc oxide layer obtained based on this comparative example can be shown with reference to fig. 3.
Fig. 4 schematically shows a topography obtained after hot salt corrosion on a titanium alloy substrate, fig. 5 schematically shows a topography obtained after hot salt corrosion on a surface of a composite coating layer obtained based on example 2, and fig. 6 schematically shows a topography obtained after hot salt corrosion on a surface of a micro-arc oxidation layer obtained based on comparative example 1. Meanwhile, as can be seen from fig. 4 to fig. 6, on the one hand, for the composite coating obtained by applying the above embodiment 2 in the present disclosure, compared with the titanium alloy substrate and the micro-arc oxidation layer, the corrosion resistance of the titanium alloy can be obviously improved by adopting the coating preparation scheme of embodiment 2. Further, table 1 shows the friction coefficient and wear rate of the titanium alloy substrate, the titanium alloy surface coating in the embodiment 2 of the present invention and the comparative example, and it can be seen that the friction and wear resistance of the composite coating obtained in the embodiment 2 of the present disclosure are significantly improved compared with the titanium alloy substrate. Compared with the comparative example, the composite coating obtained in the embodiment 2 of the invention has similar wear resistance and obviously improved antifriction.
TABLE 1
Furthermore, the above-described figures are only schematic illustrations of processes included in the method according to the exemplary embodiments of the present disclosure, and are not intended to be limiting. It will be readily appreciated that the processes shown in the above figures do not indicate or limit the temporal order of these processes. In addition, it is also readily understood that these processes may be performed synchronously or asynchronously, for example, among a plurality of modules.
Other embodiments of the disclosure will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure disclosed herein. This application is intended to cover any adaptations, uses, or adaptations of the disclosure following, in general, the principles of the disclosure and including such departures from the present disclosure as come within known or customary practice within the art to which the disclosure pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the disclosure being indicated by the following claims.
It is to be understood that the present disclosure is not limited to the precise arrangements and instrumentalities shown in the drawings, and that various modifications and changes may be effected without departing from the scope thereof. The scope of the present disclosure is limited only by the appended claims.
Claims (9)
1. A method of preparing a composite coating, comprising:
uniformly dispersing the activated MoS 2 nano powder in an electrolyte to obtain a composite electrolyte;
Placing a titanium alloy matrix into the composite electrolyte for micro-arc oxidation treatment to generate a micro-arc oxidation layer with TiO 2/MoS2 on the surface of the titanium alloy matrix;
Immersing the titanium alloy substrate with the micro-arc oxidation layer of TiO 2/MoS2 into hole sealing liquid, and then drying to obtain a substrate with a hole sealing TiO 2 corrosion-resistant layer;
Placing the substrate with the hole sealing TiO 2 corrosion-resistant layer in a vacuum chamber of vapor deposition equipment to serve as an anode, adopting a MoS 2 target material and a Ti target material as a cathode, and performing film coating treatment under an argon atmosphere with the vacuum degree of 1Pa to form an abrasion-resistant composite coating on the surface of the substrate with the hole sealing TiO 2 corrosion-resistant layer;
The hole sealing liquid is prepared by 1) mixing 0.5-1.5g/L of silane coupling agent with 2-10g/L of organic solvent to obtain a solvent mixing result, 2) stirring the solvent mixing result for 36-48h to activate the solvent mixing result to obtain a solvent activating result, and 3) adding 5-10g/L of potassium fluozirconate, 1-3g/L of nano titanium dioxide and 1-5g/L of triethanolamine into the solvent activating result, and performing ultrasonic vibration for 0.5h to obtain the hole sealing liquid.
2. The method for preparing the composite coating according to claim 1, wherein the activated MoS 2 nano powder used in the preparation process of the composite electrolyte is obtained by immersing 10-20g of MoS 2 nano powder in a mixture of 0.05-0.1g of sodium dodecyl sulfate and 200-300g of ethanol, stirring for 2h, obtaining an activated mixture, and drying and sieving the activated mixture to obtain activated MoS 2 nano powder.
3. The preparation method of the composite coating according to claim 1, wherein the preparation process of the composite electrolyte is characterized in that 1-5g/L of activated MoS 2 nano powder, 10-15g/L of sodium silicate, 0.5-1g/L of sodium hypophosphite, 2-5g/L of sodium tungstate and 2-8ml/L of glycerin are prepared into the electrolyte, the electrolyte is continuously stirred for 1-2h, ultrasonic vibration is carried out for 0.5-1.5h, and the activated MoS 2 nano powder is uniformly distributed in the electrolyte.
4. The method for preparing a composite coating according to claim 1, wherein in the preparation process of the micro-arc oxidation layer with TiO 2/MoS2, the frequency used in the micro-arc oxidation treatment process is 400-800Hz, the positive duty ratio is 5-30%, the negative duty ratio is 5-30%, the positive voltage is 350-500V, the negative voltage is 10-50V, and the oxidation time is 20-40min.
5. The method for preparing the composite coating according to claim 1, wherein the substrate with the hole-sealing TiO 2 corrosion-resistant layer is prepared by placing a titanium alloy substrate with a micro-arc oxidation layer of TiO 2/MoS2 in hole-sealing liquid, soaking for 5-10min, placing the soaked titanium alloy substrate in an oven for 15min at 160 ℃, repeating the baking for 3-5 times, and then drying for 30min again to obtain the substrate with the hole-sealing TiO 2 corrosion-resistant layer.
6. The method for preparing the composite coating according to claim 1, wherein the composite coating is prepared by 1) placing a substrate with a hole-sealing TiO 2 corrosion-resistant layer in a vacuum chamber of a vapor deposition device, keeping the vacuum degree at 1Pa, 2) starting a MoS 2 target, wherein the power source is a radio frequency power source, the sputtering power of the radio frequency power source is set to be 200-250W, 3) starting a Ti target, the power source is a direct current power source, the current of the direct current power source is set to be 50-100A, the bias voltage is set to be-200V to-400V, the duty ratio is 40% -60%, and the deposition time is 1-3h, so that the composite coating is plated on the surface of the substrate with the hole-sealing TiO 2 corrosion-resistant layer.
7. A composite coating obtained by the method for preparing a composite coating according to any one of claims 1 to 6, wherein the composite coating comprises a micro-arc oxidized TiO 2/MoS2 layer, a TiO 2 hole sealing layer and a vapor deposited Ti/MoS 2 layer.
8. The composite coating according to claim 7, wherein the micro-arc oxidized TiO 2/MoS2 layer has a thickness of 10-15 μm, the TiO 2 pore sealing layer has a thickness of 1-1.5 μm, and the vapor deposited Ti/MoS 2 layer has a thickness of 1-3 μm.
9. The composite coating of claim 7, wherein the atomic percent of Ti in the vapor deposited Ti/MoS 2 layer is 2% -10%.
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