CN113145427B - Vacuum electroplating process for surface of shaft sleeve - Google Patents
Vacuum electroplating process for surface of shaft sleeve Download PDFInfo
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- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
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- B05D1/36—Successively applying liquids or other fluent materials, e.g. without intermediate treatment
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- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
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- B05D7/58—No clear coat specified
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3435—Applying energy to the substrate during sputtering
- C23C14/345—Applying energy to the substrate during sputtering using substrate bias
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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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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Abstract
The invention discloses a vacuum plating process for the surface of a shaft sleeve. The method specifically comprises the steps of surface pretreatment, in-situ synthesis of a polydopamine/UIO-66 film, grafting, vacuum metal plating, coating of a protective film and the like, so that the surface of the shaft sleeve is modified, the corrosion resistance of the shaft sleeve is improved, the surface friction coefficient is reduced, and the wear resistance is improved. Has the advantages that: (1) the polydopamine/UIO-66 film is synthesized in situ on the metal surface, so that the pickling step is omitted, the corrosion resistance of the shaft sleeve is improved, and the adhesive force of the metal film layer is increased. (2) The zinc-molybdenum oxide mixed metal layer is sputtered by using a vacuum sputtering process, and the molybdenum oxide has self-lubricating property, so that the zinc-molybdenum oxide mixed metal layer can be effectively adhered to the zinc metal layer, the tightness is improved, and the corrosion resistance is improved. (3) The protective film is arranged, the metal film layer is effectively fixed, and meanwhile, the friction coefficient of the surface of the shaft sleeve is reduced and the wear resistance is improved by using filler orange gel and boron nitride/molybdenum disulfide.
Description
Technical Field
The invention relates to the technical field of shaft sleeve surface treatment, in particular to a vacuum electroplating process for the surface of a shaft sleeve.
Background
A sleeve is a metal part requiring long-term friction work, and is generally enhanced in wear resistance or corrosion resistance using a surface treatment. Common processes include electroplating processes including water electroplating and vacuum electroplating, and water electroplating is gradually replaced by vacuum electroplating due to the problems of high pollution, large film crystal grains, uneven crystal grain distribution and the like. Vacuum plating is a process of separating target materials by using an argon loading machine to form molecules to be physically deposited on the surface.
In the existing shaft sleeve vacuum plating process, an acid solution is generally used for activation before plating and then plating is carried out, a large amount of acid is consumed in the treatment mode, the loss of metal quality is caused, and the treatment problem of waste acid and waste metal is also generated. The hydrogen chemical grade in the pickling solution is higher than that of the pickled steel, and the generated hydrogen can permeate into the steel to accumulate hydrogen brittleness, so that the mechanical property of the metal is reduced. Meanwhile, the problems of poor corrosion resistance, poor adhesion and the like of a single metal coating exist in the electroplating process. In addition, the coating is often used for protection and fixation after the metal layer is sputtered, but most coatings have poor wear resistance and too high viscosity, so that the shaft sleeve has the problem of viscous accumulation in the display use process.
Therefore, the vacuum plating process for the surface of the shaft sleeve is of great significance in solving the problems.
Disclosure of Invention
The invention aims to provide a vacuum plating process for the surface of a shaft sleeve, which aims to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a vacuum plating process for the surface of a shaft sleeve comprises the following steps:
step 1: surface pretreatment: ultrasonically cleaning the surface of the shaft sleeve by using acetone, ethanol and deionized water respectively, and drying; obtaining a shaft sleeve A;
step 2: preparation of polydopamine/UIO-66 film: soaking the shaft sleeve in a dopamine solution for a period of time, washing and drying, placing the shaft sleeve in a hydrothermal reaction kettle containing a UIO-66 precursor solution, setting reaction conditions, and generating a polydopamine/UIO-66 film on the surface of the shaft sleeve in situ to obtain a shaft sleeve B;
and step 3: grafting: uniformly dispersing a silane coupling agent in an ethanol solution to obtain a spraying liquid; placing the shaft sleeve B on a rotary spraying machine, setting parameters, and performing spraying to obtain a shaft sleeve C;
and 4, step 4: vacuum metal film electroplating: placing the shaft sleeve C on a target table, and taking metal zinc as a target A and molybdenum trioxide as a target B; setting process parameters, and setting the target A and the target B to perform sputtering on the targets to obtain a shaft sleeve D;
and 5: coating a protective film: diluting epoxy resin with a water-acetone mixed solvent, sequentially adding boron nitride/molybdenum disulfide, orange gel and a curing agent, and uniformly mixing to obtain an epoxy resin coating; and (3) placing the shaft sleeve D on a rotary spraying machine, spraying an epoxy resin coating, and curing for 2-10 hours at the set temperature of 80-150 ℃ to obtain a shaft sleeve E.
Preferably, in step 2, the preparation of the dopamine solution: dissolving dopamine in a buffer solution to obtain a dopamine solution with the concentration of 3-6 mg/L; preparation of the UIO-66 precursor solution: respectively dissolving zirconium chloride solution and terephthalic acid solution in deionized water and DMF solution to form zirconium chloride solution and terephthalic acid solution; and mixing and stirring the two solutions for 8-12 hours to obtain a UIO-66 precursor solution.
Preferably, in step 2, the reaction conditions are as follows: the reaction temperature was 120 ℃ and the reaction time was 72 hours.
Preferably, in step 3, the parameters are: the spraying distance is 15cm, and the temperature is 55-60 ℃.
Preferably, in step 4, the process parameters are as follows: setting the vacuum degree of the vacuum chamber to 10-4～10-2Pa, introducing argon-nitrogen mixed gas with the gas flow ratio of 5-10: 1, the matrix bias voltage of-70 to-50V, the sputtering temperature of 200-300 ℃ and the sputtering time of 1-2 hours.
Preferably, in step 5, the raw materials of the epoxy resin coating comprise the following components: by weight, 90-105 parts of bisphenol A epoxy resin, 55-65 parts of anhydride curing agent, 7-10 parts of orange gel and 5-8 parts of boron nitride/molybdenum disulfide.
Preferably, in step 5, the preparation method of the orange gel comprises the following steps: washing oranges with clear water, and squeezing to obtain fruit juice; pasteurizing at 85-90 ℃ for 20 minutes; transferring the mixture into a reaction kettle, heating to 65-70 ℃, dropwise adding a sodium hydroxide solution, stirring for reacting for 2 hours, thermally filtering the solution, cooling to room temperature, and adding hydrochloric acid to adjust the pH value to 7-7.5; and transferring the orange gel into a reaction kettle, and aging for 8-9 hours at the set temperature of 65-70 ℃ to obtain the orange gel.
Preferably, in step 5, the preparation method of the molybdenum disulfide/boron nitride comprises the following steps: placing boron nitride into a sodium hydroxide solution, refluxing for 5-5.5 hours at the temperature of 60-62 ℃, filtering, washing to be neutral, and drying to obtain hydroxylated boron nitride; ultrasonically dispersing the mixture in deionized water for 30-40 minutes, sequentially adding ammonium molybdate tetrahydrate and thiourea, and continuously stirring for 1-2 hours to completely dissolve the ammonium molybdate tetrahydrate and the thiourea; and transferring the mixture into a high-pressure reaction kettle, setting the temperature to be 205-210 ℃, reacting for 24 hours, centrifugally washing, and drying to obtain the boron nitride/molybdenum disulfide.
Preferably, the thickness of the metal film is 2-10 μm.
Preferably, the thickness of the protective film is 40-60 μm.
In the technical scheme, a polydopamine/UIO-66 film is synthesized on the surface of the shaft sleeve in situ, and a metal film of zinc-molybdenum trioxide is electroplated by vacuum sputtering, so that corrosion is effectively prevented in a synergistic manner; and a silane coupling agent is grafted on the polydopamine/UIO-66 film, so that the adhesive force of the metal film layer is effectively increased, and finally, a layer of protective film is coated on the outer layer, so that the friction force is reduced, and the smoothness and the wear resistance are increased. The shaft sleeve is subjected to a series of treatment modes, so that the wear resistance and the corrosion resistance are effectively improved.
The shaft sleeve is a mechanical part made of metal steel, and due to the corrosivity of metal, the shaft sleeve is easy to corrode and cause frictional wear when operated in a harsher environment for a long time. Generally, the wear resistance is enhanced by adopting an electroplated zinc layer, but the adhesion is poor and the falling is generated when the electroplated metal film layer is directly plated, and the corrosion resistance of the shaft sleeve is poor after a single zinc layer is electroplated. At present, the acid treatment is commonly used before the electroplating to remove the oxide on the surface of the metal and increase the roughness, thereby increasing the adhesive force and the slow release property of the electroplated layer. However, pickling consumes a large amount of acid and loses metal quality, thereby causing problems in the treatment of waste acid and waste metal; further, the hydrogen chemical level in the pickling solution is higher than that of the steel to be pickled, and the generated hydrogen permeates into the steel to be accumulated to cause hydrogen embrittlement, thereby deteriorating the mechanical properties of the metal. Therefore, in the scheme, the excellent adhesive property and self-aggregation property of dopamine on the metal surface are utilized, the hot melt adhesive reaction is utilized in a combined manner, the UIO-66 film layer is generated on the polydopamine in situ, and the high-density catechol group in the polydopamine has chelation on the active metal center, so that in-situ heterogeneous nucleation is facilitated, and the polydopamine/UIO-66 film with high crystallinity, uniformity and compactness is grown. The film layer is covered on the metal surface in the mode, the adhesive force is strong, the film layer has excellent corrosion resistance, the adhesive force of a subsequent metal film layer can be increased by a large amount of hydroxyl on the UIO-66 surface, and the adhesive force of the metal film layer can be further increased by performing surface modification on the hydroxyl. Thereby replacing the slow release effect and the effect of increasing the adhesive force generated by acid cleaning.
In the scheme, the silane coupling agent is grafted on the surface of UIO-66, so that the adhesion of the sputtered metal film layer is increased while the compactness is increased. The sputtered metal layer is mainly zinc metal and is assisted by molybdenum oxide. If zinc is used as a metal independently, the corrosion resistance is weak, the corrosion resistance of the metal film layer can be effectively improved by using the mixed metal layer, the surface impedance can be effectively increased by adding molybdenum oxide, so that the corrosion resistance is improved, meanwhile, the molybdenum oxide has self-lubricating property, the molybdenum oxide can be effectively adhered between zinc metal layers, the tightness of the metal layer is increased, the immersion rate of corrosive liquid is reduced, the corrosion rate is effectively reduced, and the service life is prolonged. In the sputtering process, the sputtered crystal grain has small size, can be effectively filled in the pores and gaps of the polydopamine/UIO-66 film, reduces the porosity, and simultaneously, due to the uniform dispersion of UIO-66, sputtered metal can be uniformly distributed, the non-uniform phenomenon is effectively reduced, and the roughness is reduced.
In order to reduce the surface friction coefficient of the shaft sleeve and increase the wear resistance, and simultaneously, in order to fix the metal film layer, a protective film is arranged above the metal film layer. The protective film takes polyepoxy resin with higher Vickers hardness as a main body, and two fillers of orange gel and boron nitride/molybdenum disulfide are added. The method comprises the following specific steps: (1) the orange gel has better compatibility with the epoxy resin in a water-acetone solvent. The orange gel contains silicon dioxide hard compounds, so that the rigidity, strength and hardness of the protective film are effectively improved; secondly, the higher surface roughness of the epoxy resin coating is attributed to the layer structure with the rough surface, and the reductive citrate is contained in the layer structure, so that the layer structure is damaged and decomposed into fine grains, the dislocation of the fine grain structure is generated, the density is increased, and the strength of the coating is increased; and the dislocation of the crystal grain structure also increases the adhesive force between the crystal grain structure and the metal film layer. The porosity and the pore space are reduced, the surface cracks are reduced, and the smoothness and the surface wear resistance of the coating are improved. (2) The boron nitride and the molybdenum disulfide both have good wear resistance and self-lubricating property, and can remarkably increase the wear resistance of the coating and reduce the friction force. According to the technical scheme, the surface of boron nitride is hydroxylated, and then the supported molybdenum disulfide is directly synthesized on the surface of the boron nitride by taking hydroxyl as a site to form boron nitride/molybdenum disulfide, so that the agglomeration of the molybdenum disulfide is successfully inhibited. And because of the molybdenum disulfide load, the surface roughness of the boron nitride is increased, and the interface compatibility between the filler and the epoxy resin is further improved. Thereby synergistically generating maximized self-lubricity, reducing the friction coefficient of the surface of the shaft sleeve and enhancing the mechanical strength and the wear resistance.
Compared with the prior art, the invention has the following beneficial effects: (1) the polydopamine/UIO-66 film is synthesized in situ on the metal surface, so that the pickling step is omitted, the corrosion resistance of the shaft sleeve is improved, and the adhesive force of the metal film layer is increased. (2) The zinc-molybdenum oxide mixed metal layer is sputtered by using a vacuum sputtering process, and the molybdenum oxide has self-lubricating property, so that the zinc-molybdenum oxide mixed metal layer can be effectively adhered to the zinc metal layer, the tightness is improved, and the corrosion resistance is improved. (3) The protective film is arranged, the metal film layer is effectively fixed, and meanwhile, the friction coefficient of the surface of the shaft sleeve is reduced and the wear resistance is improved by using filler orange gel and boron nitride/molybdenum disulfide.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
step 1: ultrasonically cleaning the surface of the shaft sleeve by using acetone, ethanol and deionized water respectively, and drying; obtaining a shaft sleeve A;
step 2: dissolving dopamine in a buffer solution to obtain a dopamine solution with the concentration of 4.5 mg/L; soaking the shaft sleeve in a dopamine solution for a period of time, washing and drying, placing the shaft sleeve in a hydrothermal reaction kettle containing a UIO-66 precursor solution, setting reaction conditions, and generating a polydopamine/UIO-66 film on the surface of the shaft sleeve in situ to obtain a shaft sleeve B; respectively dissolving zirconium chloride solution and terephthalic acid solution in deionized water and DMF solution to form zirconium chloride solution and terephthalic acid solution; the two solutions were mixed and stirred for 10 hours to obtain a UIO-66 precursor solution. The reaction temperature was 120 ℃ and the reaction time was 72 hours.
And step 3: uniformly dispersing a silane coupling agent in an ethanol solution to obtain a spraying liquid; placing the shaft sleeve B on a rotary spraying machine, setting parameters, and performing spraying to obtain a shaft sleeve C; the spraying distance was 15cm and the temperature was 58 ℃.
And 4, step 4: placing the shaft sleeve C on a target table, and taking metal zinc as a target A and molybdenum trioxide as a target B; setting the vacuum degree of the vacuum chamber to 10-3Pa, introducing argon-nitrogen mixed gas with the gas flow ratio of 8:1, the matrix bias voltage of-60V, the sputtering temperature of 250 ℃ and the sputtering time of 1.5 hours; target a and target B were set to perform sputtering on the targets, resulting in sleeve D.
And 5: (1) washing oranges with clear water, and squeezing to obtain fruit juice; pasteurizing at 88 deg.C for 20 min; transferring the mixture into a reaction kettle, heating the mixture to a temperature of 68 ℃, dropwise adding a sodium hydroxide solution, stirring the mixture for reaction for 2 hours, thermally filtering the solution, cooling the solution to room temperature, and adding hydrochloric acid to adjust the pH value to 7.2; transferring the orange gel into a reaction kettle, and aging for 8.5 hours at the set temperature of 68 ℃ to obtain orange gel for later use. (2) Placing boron nitride into a sodium hydroxide solution, refluxing for 5.25 hours at the set temperature of 61 ℃, filtering, washing to be neutral, and drying to obtain hydroxylated boron nitride; ultrasonically dispersing the mixture in deionized water for 35 minutes, sequentially adding ammonium molybdate tetrahydrate and thiourea, and continuously stirring for 1.5 hours to completely dissolve the ammonium molybdate tetrahydrate and the thiourea; transferring the mixture into a high-pressure reaction kettle, setting the temperature at 208 ℃, reacting for 24 hours, centrifugally washing, and drying to obtain the boron nitride/molybdenum disulfide for later use. (3) Diluting 98 parts of water-acetone mixed solvent of bisphenol A epoxy resin, sequentially adding 6 parts of boron nitride/molybdenum disulfide, 8 parts of orange gel and 60 parts of anhydride curing agent, and uniformly mixing to obtain epoxy resin coating; and (3) placing the shaft sleeve D on a rotary spraying machine, spraying an epoxy resin coating, and curing for 8 hours at the set temperature of 120 ℃ to obtain a shaft sleeve E.
Example 2:
step 1: ultrasonically cleaning the surface of the shaft sleeve by using acetone, ethanol and deionized water respectively, and drying; obtaining a shaft sleeve A;
step 2: dissolving dopamine in a buffer solution to obtain a dopamine solution with the concentration of 3 mg/L; soaking the shaft sleeve in a dopamine solution for a period of time, washing and drying, placing the shaft sleeve in a hydrothermal reaction kettle containing a UIO-66 precursor solution, setting reaction conditions, and generating a polydopamine/UIO-66 film on the surface of the shaft sleeve in situ to obtain a shaft sleeve B; respectively dissolving zirconium chloride solution and terephthalic acid solution in deionized water and DMF solution to form zirconium chloride solution and terephthalic acid solution; the two solutions were mixed and stirred for 8 hours to obtain a UIO-66 precursor solution. The reaction temperature was 120 ℃ and the reaction time was 72 hours.
And step 3: uniformly dispersing a silane coupling agent in an ethanol solution to obtain a spraying liquid; placing the shaft sleeve B on a rotary spraying machine, setting parameters, and performing spraying to obtain a shaft sleeve C; the spraying distance was 15cm and the temperature was 55 ℃.
And 4, step 4: placing the shaft sleeve C on a target table, and taking metal zinc as a target A and molybdenum trioxide as a target B; setting the vacuum degree of the vacuum chamber to 10-4Pa, introducing argon-nitrogen mixed gas with the gas flow ratio of 5:1, the matrix bias voltage of-70V, the sputtering temperature of 200 ℃ and the sputtering time of 2 hours; target a and target B were set to perform sputtering on the targets, resulting in sleeve D.
And 5: (1) washing oranges with clear water, and squeezing to obtain fruit juice; pasteurizing at 85 deg.C for 20 min; transferring the mixture into a reaction kettle, heating the mixture to 65 ℃, dropwise adding a sodium hydroxide solution, stirring the mixture for reaction for 2 hours, thermally filtering the solution, cooling the solution to room temperature, and adding hydrochloric acid to adjust the pH value to 7; transferring the orange gel into a reaction kettle, and aging for 8 hours at the set temperature of 65 ℃ to obtain orange gel for later use. (2) Placing boron nitride into a sodium hydroxide solution, refluxing for 5 hours at the set temperature of 60 ℃, filtering, washing to be neutral, and drying to obtain hydroxylated boron nitride; ultrasonically dispersing the mixture in deionized water for 30-40 minutes, sequentially adding ammonium molybdate tetrahydrate and thiourea, and continuously stirring for 1 hour to completely dissolve the ammonium molybdate tetrahydrate and the thiourea; transferring the mixture into a high-pressure reaction kettle, setting the temperature to be 205 ℃, reacting for 24 hours, centrifugally washing, and drying to obtain the boron nitride/molybdenum disulfide for later use. (3) Diluting 90 parts of water-acetone mixed solvent of bisphenol A epoxy resin, sequentially adding 5 parts of boron nitride/molybdenum disulfide, 7 parts of orange gel and 55 parts of anhydride curing agent, and uniformly mixing to obtain epoxy resin coating; and (3) placing the shaft sleeve D on a rotary spraying machine, spraying an epoxy resin coating, and curing for 10 hours at the set temperature of 80 ℃ to obtain a shaft sleeve E.
Example 3:
step 1: ultrasonically cleaning the surface of the shaft sleeve by using acetone, ethanol and deionized water respectively, and drying; obtaining a shaft sleeve A;
step 2: dissolving dopamine in a buffer solution to obtain a dopamine solution with the concentration of 6 mg/L; soaking the shaft sleeve in a dopamine solution for a period of time, washing and drying, placing the shaft sleeve in a hydrothermal reaction kettle containing a UIO-66 precursor solution, setting reaction conditions, and generating a polydopamine/UIO-66 film on the surface of the shaft sleeve in situ to obtain a shaft sleeve B; respectively dissolving zirconium chloride solution and terephthalic acid solution in deionized water and DMF solution to form zirconium chloride solution and terephthalic acid solution; the two solutions were mixed and stirred for 12 hours to obtain a UIO-66 precursor solution. The reaction temperature was 120 ℃ and the reaction time was 72 hours.
And step 3: uniformly dispersing a silane coupling agent in an ethanol solution to obtain a spraying liquid; placing the shaft sleeve B on a rotary spraying machine, setting parameters, and performing spraying to obtain a shaft sleeve C; the spraying distance was 15cm and the temperature was 60 ℃.
And 4, step 4: placing the shaft sleeve C on a target table, and taking metal zinc as a target A and molybdenum trioxide as a target B; setting the vacuum degree of the vacuum chamber to 10-2Pa, introducing argon-nitrogen mixed gas with the gas flow ratio of 10:1, the matrix bias voltage of-50V, the sputtering temperature of 300 ℃ and the sputtering time of 1 hour; target a and target B were set to perform sputtering on the targets, resulting in sleeve D.
And 5: (1) washing oranges with clear water, and squeezing to obtain fruit juice; pasteurizing at 90 deg.C for 20 min; transferring the mixture into a reaction kettle, heating the mixture to 70 ℃, dropwise adding a sodium hydroxide solution, stirring the mixture for reaction for 2 hours, thermally filtering the solution, cooling the solution to room temperature, and adding hydrochloric acid to adjust the pH value to 7.5; transferring the orange gel into a reaction kettle, and aging for 9 hours at the set temperature of 70 ℃ to obtain orange gel for later use. (2) Placing boron nitride into a sodium hydroxide solution, setting the temperature at 62 ℃ for refluxing for 5.5 hours, filtering and washing to be neutral, and drying to obtain hydroxylated boron nitride; ultrasonically dispersing the mixture in deionized water for 40 minutes, sequentially adding ammonium molybdate tetrahydrate and thiourea, and continuously stirring for 2 hours to completely dissolve the mixture; transferring the mixture into a high-pressure reaction kettle, setting the temperature to be 210 ℃, reacting for 24 hours, centrifugally washing, and drying to obtain the boron nitride/molybdenum disulfide for later use. (3) Diluting 105 parts of water-acetone mixed solvent of bisphenol A epoxy resin, sequentially adding 8 parts of boron nitride/molybdenum disulfide, 10 parts of orange gel and 65 parts of anhydride curing agent, and uniformly mixing to obtain epoxy resin coating; and (3) placing the shaft sleeve D on a rotary spraying machine, spraying an epoxy resin coating, and curing for 10 hours at the set temperature of 150 ℃ to obtain a shaft sleeve E.
Example 4: no polydopamine/UIO-66 film is arranged, and hydrochloric acid is used for surface activation; the rest is the same as in example 1.
Example 5: molybdenum oxide is not added as an auxiliary metal in the metal film; the rest is the same as in example 1.
Example 6: in the protective film, the epoxy resin is changed into acrylic ester; the rest is the same as in example 1.
Example 7: in the protective film, no orange gel is added; the rest is the same as in example 1.
Example 8: in the protective film, molybdenum sulfide-supported boron nitride was not added, and both were separately added to the coating, and the rest was the same as in example 1.
Experiment: the shaft sleeves subjected to surface treatment in examples 1 to 8 are used as samples, and salt spray resistance experiments are carried out on the shaft sleeves subjected to surface treatment according to the standard method of GB/T1771-2007, so as to characterize the corrosion resistance. And (3) referring to the standard method of GB1720-79, the adhesion of the surface film layer of the shaft sleeve is characterized. According to the GB/T1786-2006 standard method, under the condition of a load of 40N, setting the friction to be 1000m, setting the friction speed to be 1.6m/s, obtaining the abrasion loss according to the mass difference, and performing abrasion resistance on the surface of the shaft sleeve by using a friction abrasion tester to obtain the friction coefficient of the surface. The data obtained are shown in the following table:
and (4) conclusion: as can be seen from the data of the embodiments 1 to 3, a series of film layers are arranged on the surface of the shaft sleeve, so that the adhesive force is strong and can reach 0 grade, and the corrosion resistance is good and can reach more than 5700 hours; has better wear resistance, the friction coefficient of the surface is as low as 0.035, and the abrasion loss is only 0.7 mg.
Comparing the data of example 4 with the data of example 1, it can be found that: the adhesion and the salt spray resistance were reduced due to the high crystallinity, compact and uniform structure of the polydopamine/UIO-66 film. The strong adhesive force between the polydopamine and the metal and the excellent corrosion resistance of the film layer are utilized, and the adhesive force of the subsequent metal film layer and the adhesive force of the sputtered metal film layer can be increased by a large amount of hydroxyl on the surface of UIO-66.
Comparing the data of example 5 with the data of example 1, it can be found that: the salt spray resistance is reduced because the single zinc metal film has low corrosivity, the added molybdenum oxide can effectively increase the surface impedance, so that the corrosion resistance is increased, meanwhile, the molybdenum oxide has self-lubricating property, the molybdenum oxide can be effectively adhered between zinc metal layers, the tightness of the metal layers is increased, the immersion rate of corrosive liquid is reduced, the corrosion rate is effectively reduced, and the service life is prolonged.
Comparing the data of examples 6-7 with example 1, it can be found that: the wear resistance of the surface of the sleeve in example 6 was reduced because the epoxy resin, which is the highest hardness polymer among many polymers, had better wear resistance. The abrasion resistance of the protective film is also remarkably reduced in example 7, because the orange gel contains silica-based hard compounds, the rigidity, strength and hardness of the protective film are effectively improved; the coating also contains citrate, so that the laminated structure is damaged and decomposed into fine grains, the dislocation of the fine grain structure is generated, the density is increased, the gap is reduced, the surface cracks are reduced, and the smoothness and the surface wear resistance of the coating are improved; and the dislocation of the crystal grain structure also increases the adhesive force between the crystal grain structure and the metal film layer, so that the layers are more compact. The data of example 8 can show that the corrosion resistance is reduced and the friction resistance is reduced because the surface of boron nitride is hydroxylated, and then molybdenum disulfide is directly synthesized and loaded on the surface of the boron nitride/molybdenum disulfide by taking hydroxyl as a site to form boron nitride/molybdenum disulfide. And the loaded molybdenum disulfide and the boron nitride form a flat lubrication layer with dense dispersion. And because of the molybdenum disulfide load, the surface roughness of the boron nitride is increased, the interface compatibility between the filler and the epoxy resin is further improved, and the propagation of cracks is inhibited. The two have a synergistic effect and form a uniform and hard film, and the friction and abrasion performance is still better even under the condition of high load or sliding speed.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. 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 (1)
1. The vacuum plating process for the surface of the shaft sleeve is characterized by comprising the following steps: the method comprises the following steps: step 1: surface pretreatment: ultrasonically cleaning the surface of the shaft sleeve by using acetone, ethanol and deionized water respectively, and drying; obtaining a shaft sleeve A; step 2: preparation of polydopamine/UIO-66 film: soaking the shaft sleeve in a dopamine solution for a period of time, washing and drying, placing the shaft sleeve in a hydrothermal reaction kettle containing a UIO-66 precursor solution, setting reaction conditions, and generating a polydopamine/UIO-66 film on the surface of the shaft sleeve in situ to obtain a shaft sleeve B; and step 3: grafting: uniformly dispersing a silane coupling agent in an ethanol solution to obtain a spraying liquid; placing the shaft sleeve B on a rotary spraying machine, setting parameters, and performing spraying to obtain a shaft sleeve C; and 4, step 4: vacuum metal film electroplating: placing the shaft sleeve C on a target table, and taking metal zinc as a target A and molybdenum trioxide as a target B; setting process parameters, and setting the target A and the target B to perform sputtering on the targets to obtain a shaft sleeve D; and 5: coating a protective film: diluting epoxy resin with a water-acetone mixed solvent, sequentially adding boron nitride/molybdenum disulfide, orange gel and a curing agent, and uniformly mixing to obtain an epoxy resin coating; placing the shaft sleeve D on a rotary spraying machine, spraying an epoxy resin coating, and curing at the temperature of 80-150 ℃ for 2-10 hours to obtain a shaft sleeve E;
in step 2, preparing the dopamine solution: dissolving dopamine in a buffer solution to obtain a dopamine solution with the concentration of 3-6 mg/L; preparation of the UIO-66 precursor solution: respectively dissolving zirconium chloride solution and terephthalic acid solution in deionized water and DMF solution to form zirconium chloride solution and terephthalic acid solution; mixing and stirring the two solutions for 8-12 hours to obtain a UIO-66 precursor solution;
in step 2, the reaction conditions are as follows: the reaction temperature is 120 ℃, and the reaction time is 72 hours;
in step 3, the parameters are: the spraying distance is 15cm, and the temperature is 55-60 ℃;
in step 4, the process parameters are as follows: setting the vacuum degree of the vacuum chamber to 10-4 ～10-2 Pa, introducing argon-nitrogen mixed gas with the gas flow ratio of 5-10: 1, the matrix bias voltage of-70 to-50V, the sputtering temperature of 200-300 ℃ and the sputtering time of 1-2 hours;
in step 5, the raw materials of the epoxy resin coating comprise the following components: 90-105 parts of bisphenol A epoxy resin, 55-65 parts of anhydride curing agent, 7-10 parts of orange gel and 5-8 parts of boron nitride/molybdenum disulfide by weight;
in the step 5, the preparation method of the orange gel comprises the following steps: washing oranges with clear water, and squeezing to obtain fruit juice; pasteurizing at 85-90 ℃ for 20 minutes; transferring the mixture into a reaction kettle, heating to 65-70 ℃, dropwise adding a sodium hydroxide solution, stirring for reacting for 2 hours, thermally filtering the solution, cooling to room temperature, and adding hydrochloric acid to adjust the pH value to 7-7.5; transferring the orange gel into a reaction kettle, and aging for 8-9 hours at the set temperature of 65-70 ℃ to obtain orange gel; in step 5, the preparation method of the molybdenum disulfide/boron nitride comprises the following steps: placing boron nitride into a sodium hydroxide solution, refluxing for 5-5.5 hours at the temperature of 60-62 ℃, filtering, washing to be neutral, and drying to obtain hydroxylated boron nitride; ultrasonically dispersing the mixture in deionized water for 30-40 minutes, sequentially adding ammonium molybdate tetrahydrate and thiourea, and continuously stirring for 1-2 hours to completely dissolve the ammonium molybdate tetrahydrate and the thiourea; transferring the mixture into a high-pressure reaction kettle, setting the temperature to be 205-210 ℃, reacting for 24 hours, centrifugally washing, and drying to obtain boron nitride/molybdenum disulfide;
the thickness of the metal film is 2-10 mu m;
the thickness of the protective film is 40-60 mu m.
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