Method for preparing Al-MoS2 composite coating through electro-deposition

Abstract

And preparing the Al-MoS2 composite coating by adopting MoS2 as second-phase particles by utilizing an electro-deposition technology. The preparation method comprises the following steps: putting anhydrous AlCl3, LiAlH4 and MoS2 particles into a glove box filled with argon, weighing 4g of anhydrous AlCl3 and 0.28 g of anhydrous LiAlH4 by using a balance, putting into a beaker, and then weighing a certain amount of MoS2 particles (10g / L-80g / L) and putting into the beaker; and the beaker is sealed, taken out and put into a fuming cupboard. The method comprises the following steps: measuring 20ml of benzene by using a measuring cylinder, pouring the benzene into a sealed beaker by using a guide tube, and then putting the beaker into a magnetic stirrer under an ice bath condition; 5 ml of tetrahydrofuran is measured and slowly poured into the beaker through the guide tube, and in order to prevent the tetrahydrofuran from deteriorating, the process needs to be carried out under an ice bath condition. And adding tetrahydrofuran, sealing the beaker, stirring for 2-3 hours, and carrying out ultrasonic dispersion for 30 minutes. According to the method, an aluminum sheet serves as an anode, a copper sheet serves as a cathode, the current density is controlled to be 30-50 milliamperes / cm < 2 >, the temperature of a plating solution is 20-40 DEG C, the electrodeposition time is 30-75 min, and the Al-MoS2 composite coating with the compact surface and uniform particle distribution can be obtained and mainly comprises Al and MoS2.

Description

Technical Field

[0001] The invention belongs to the field of electrochemical deposition, and in particular relates to a method for preparing a metal composite material Al-MoS2 composite coating. Background Art

[0002] Aluminum and aluminum alloys have attracted widespread attention due to their advantages such as low density and high strength. With the development of modern science and technology, the performance requirements for basic materials are getting higher and higher. Aluminum and its alloys have excellent properties such as light weight, corrosion resistance, and good electrical and thermal conductivity. However, with the continuous improvement of the comprehensive performance requirements of basic materials under modern service conditions, traditional aluminum alloy materials are difficult to meet the requirements. Due to their low surface hardness and poor wear resistance, the further application of aluminum and aluminum alloys is limited. For example, frequent friction between the surfaces of metal parts will greatly reduce the service life of the parts. Aluminum-based composites (AMCs) with aluminum and its alloys as the matrix have become an indispensable component of aerospace materials due to their good comprehensive mechanical, physical and chemical properties.

[0003] Aluminum-based composite materials are new materials that improve the wear resistance, corrosion resistance, fatigue resistance and other properties of materials by adding second-phase particles to aluminum or aluminum alloys. This material combines the light weight, electrical and thermal conductivity of the aluminum metal matrix with the advantages of high strength, high hardness, and high wear resistance of the reinforcing phase to achieve complementary advantages, thereby creating a new material with broad application prospects. Molybdenum disulfide is a ceramic particle with excellent anisotropy, catalytic performance and low friction coefficient. Adding molybdenum disulfide particles to aluminum and aluminum alloys can provide better lubrication performance and greatly improve the wear resistance of the material. There are many methods for preparing aluminum-based composite coating materials at present, mainly including mechanical alloying method, powder metallurgy method, in-situ synthesis method, etc. These methods have the disadvantages of high equipment cost and complex process. The present invention is a technology for enhancing the performance of materials by depositing aluminum-second-phase particle composite coating on the surface of copper matrix by electrochemical deposition method. This method is low in cost and simple in process control compared with other preparation methods. By adding molybdenum disulfide particles to the electrodeposition solution, a composite coating with a high content of molybdenum disulfide particles and a relatively uniform distribution of second-phase particles on the surface can be obtained. Summary of the invention

[0004] The purpose of the present invention is to prepare a new aluminum-based composite coating Al-MoS2 composite coating. The method uses aluminum sheets as anodes, copper as cathodes, and an AlCl3-LiAlH4-benzene-THF organic solvent system with aluminum chloride as the main salt and MoS2 as reinforcing particles for electrodeposition. The system does not need to add other dispersants. AlCl3 and LiAlH4 can form a stable solvation complex in a mixed solvent of benzene and tetrahydrofuran (THF), and the complex helps to improve the dispersibility of powders in organic solvents. Benzene and THF, as non-polar or weakly polar solvents, can reduce the interaction between powders, thereby improving dispersibility. The addition of molybdenum disulfide particles can significantly improve the wear resistance of aluminum and aluminum alloys. The method has low cost and simple process control, and is convenient for large-scale industrial production.

[0005] The specific embodiments of the present invention are as follows: Preparation of plating solution Place anhydrous AlCl3, LiAlH4 and MoS2 particles in a glove box, take out the beaker with the rotor and the medicine spoon from the drying box and place them on the tray, then place the tray in the glove box, seal the glove box and fill it with argon. When the argon fills the entire glove box, weigh the drugs. Use a balance to weigh 4g of anhydrous AlCl3 and 0.28g of anhydrous LiAlH4, put them in a beaker, and then measure a certain amount of MoS2 particles (10g / L~80g / L) and put them in the beaker. Seal the weighed beaker, take it out of the glove box and put it in a fume hood. Use a measuring cylinder to measure 20ml of benzene, pour it into the sealed beaker with a guide tube, and then put the beaker into a magnetic stirrer under ice bath conditions. Measure 5ml of tetrahydrofuran and slowly pour it into the beaker through the guide tube. To prevent tetrahydrofuran from deteriorating, the beaker needs to be placed in an ice bath during this process. After the tetrahydrofuran is completely added, the beaker is sealed, the stirring rate is adjusted to an appropriate value, and the mixture is stirred for 2-3 hours, followed by ultrasonic dispersion for 30 minutes to allow the drug to be fully dissolved and the particles to be evenly dispersed.

[0006] Aluminum substrate treatment The aluminum sheet was polished smooth with 400, 800 and 1200 mesh sandpaper in turn, then chemically degreased to remove oil stains on the surface of the aluminum sheet, and then pre-etched and weakly corroded with dilute hydrochloric acid to remove the oxide film, and then washed with deionized water, and dried in a vacuum drying oven for standby use.

[0007] Copper substrate treatment The copper sheet was polished smooth with 400, 800 and 1200 mesh sandpaper in turn, then chemically degreased to remove oil stains on the surface of the copper sheet, and then pre-etched and weakly corroded with dilute hydrochloric acid to remove the oxide film, and then washed with water, and then placed in a vacuum drying oven to dry for standby use.

[0008] Constant current electrodeposition Using aluminum sheet as anode and copper sheet as cathode, controlling the current density to 30-50 mA / cm2, controlling the plating solution temperature to 20-40°C for electrodeposition, and controlling the electrodeposition time to 30-75 min, an Al-MoS2 composite coating with a dense surface and uniform particle distribution can be obtained.

[0009] The present invention utilizes the electrodeposition preparation technology with low preparation cost and simple process control, and adopts MoS2 particles as the second phase particles to prepare the Al-MoS2 composite coating. The MoS2 particles provide a large number of nucleation sites to refine the grains and improve the coating morphology. The aluminum-based composite coating has high hardness, wear resistance and corrosion resistance. The problems of high preparation cost and complex operation process of aluminum-based composite materials are solved, and the obtained Al-MoS2 composite coating has a dense surface and uniform distribution of MoS2 particles. BRIEF DESCRIPTION OF THE DRAWINGS

[0010] Figure 1 This is a SEM image of the composite coating obtained by the present invention; Figure 2 This is an EDS spectrum diagram of the composite coating obtained by the present invention; Figure 3 The XRD spectrum of the composite coating obtained in the present invention is shown in FIG. DETAILED DESCRIPTION

[0011] In order to better explain the present invention and facilitate understanding, the present invention is described in detail below through specific implementation modes in conjunction with the accompanying drawings.

[0012] The present invention specifically relates to a method for preparing an Al-MoS2 composite coating electroplated on a copper substrate, which is described in detail below through specific examples. The following examples are only part of the examples of the present invention, not all.

[0013] Example 1 (1) Preparation of plating solution Place anhydrous AlCl3, LiAlH4 and MoS2 particles in a glove box, take out the beaker with the rotor and the medicine spoon from the drying box and place them on the tray, then place the tray in the glove box, seal the glove box and fill it with argon. When the argon fills the entire glove box, weigh the drugs. Use a balance to weigh 4g of anhydrous AlCl3 and 0.28g of anhydrous LiAlH4, put them in a beaker, and then measure a certain amount of MoS2 particles (10g / L) and put them in the beaker. Seal the weighed beaker, take it out of the glove box and put it in a fume hood. Use a measuring cylinder to measure 20ml of benzene, pour it into the sealed beaker with a guide tube, and then put the beaker into a magnetic stirrer under ice bath conditions. Measure 5ml of tetrahydrofuran and slowly pour it into the beaker through the guide tube. To prevent tetrahydrofuran from deteriorating, the beaker needs to be placed in an ice bath during this process. After the tetrahydrofuran is completely added, the beaker is sealed, the stirring rate is adjusted to an appropriate value, and the mixture is stirred for 2-3 hours, and then ultrasonically dispersed for 30 minutes to fully dissolve the drug and evenly disperse the particles; (2) Aluminum substrate treatment The aluminum sheet was polished with 400, 800 and 1200 mesh sandpaper in turn, and then chemically degreased to remove the oil stains on the surface of the aluminum sheet, and then pre-etched and weakly etched with dilute hydrochloric acid to remove the oxide film, and then washed with deionized water, and then dried in a vacuum drying oven for standby use; (3) Copper substrate treatment The copper sheet was polished with 400, 800 and 1200 mesh sandpaper in turn, and then chemically degreased to remove the oil stains on the surface of the copper sheet, and then pre-etched and weakly etched with dilute hydrochloric acid to remove the oxide film, and then washed with deionized water, and then dried in a vacuum drying oven for standby use; (4) Constant current electrodeposition With aluminum sheet as anode and copper sheet as cathode, the current density is controlled to be 50 mA / cm2, the bath temperature is 30°C, and the electrodeposition time is 45 min, an Al-MoS2 composite coating with a dense surface and uniform particle distribution can be obtained, and its main components are Al and MoS2. The SEM image, EDS spectrum and XRD spectrum of the sample are shown in Figure 1 , Figure 2 and Figure 3 .

[0014] Example 2 (1) Preparation of plating solution Place anhydrous AlCl3, LiAlH4 and MoS2 particles in a glove box, take out the beaker with the rotor and the medicine spoon from the drying box and place them on the tray, then place the tray in the glove box, seal the glove box and fill it with argon. When the argon fills the entire glove box, weigh the medicine. Use a balance to weigh 4g of anhydrous AlCl3 and 0.28g of anhydrous LiAlH4, put them in a beaker, and then measure a certain amount of MoS2 powder (10g / L) and put it in the beaker. Seal the weighed medicine beaker, take it out of the glove box and put it in a fume hood. Measure 20ml of benzene with a measuring cylinder, pour it into the sealed beaker with a guide tube, and then put the beaker into a magnetic stirrer under ice bath conditions. Measure 5ml of tetrahydrofuran and slowly pour it into the beaker through the guide tube. To prevent tetrahydrofuran from deteriorating, the beaker needs to be placed in an ice bath during this process. After the tetrahydrofuran is completely added, the beaker is sealed, the stirring rate is adjusted to an appropriate value, and the mixture is stirred for 2-3 hours, and then ultrasonically dispersed for 30 minutes to fully dissolve the drug and evenly disperse the particles; (2) Aluminum substrate treatment The aluminum sheet was polished with 400, 800 and 1200 mesh sandpaper in turn, and then chemically degreased to remove the oil stains on the surface of the aluminum sheet, and then pre-etched and weakly etched with dilute hydrochloric acid to remove the oxide film, and then washed with deionized water, and then dried in a vacuum drying oven for standby use; (3) Copper substrate treatment The copper sheet was polished with 400, 800 and 1200 mesh sandpaper in turn, and then chemically degreased to remove the oil stains on the surface of the copper sheet, and then pre-etched and weakly etched with dilute hydrochloric acid to remove the oxide film, and then washed with deionized water, and then dried in a vacuum drying oven for standby use; (4) Constant current electrodeposition Using aluminum sheet as anode and copper sheet as cathode, controlling the current density to 30 mA / cm2, the plating solution temperature to 30°C, and the electrodeposition time to 45 min, an Al-MoS2 composite coating with a dense surface and uniform particle distribution can be obtained.

Claims

1. Preparation of plating solution: put anhydrous AlCl3, LiAlH4 and MoS2 particles into a glove box, take out the beaker with the rotor and the medicine spoon from the drying box and put them on the tray, then put the tray into the glove box, seal the glove box and fill it with argon. When the argon fills the entire glove box, weigh the medicines, weigh 4g of anhydrous AlCl3 and 0.28g of anhydrous LiAlH4 on a balance, put them into a beaker, and then put a certain amount of MoS2 powder (10g / L~80g / L) into the beaker, and put the weighed medicines into the beaker. Seal the beaker containing the drug, take it out of the glove box and put it in a fume hood, use a measuring cylinder to measure 20 ml of benzene, pour it into the sealed beaker with a guide tube, and then put the beaker into a magnetic stirrer under ice bath conditions, measure 5 ml of tetrahydrofuran, and slowly pour it into the beaker through the guide tube. To prevent the tetrahydrofuran from deteriorating, the beaker needs to be placed in an ice bath during this process. After the tetrahydrofuran is completely added, seal the beaker, adjust the stirring rate to an appropriate value, stir for 2-3 hours, and then ultrasonically disperse for 30 minutes to fully dissolve the drug and evenly disperse the particles.

2. Aluminum substrate treatment: Polish the aluminum sheet with 400, 800 and 1200 mesh sandpaper in turn, then perform chemical degreasing to remove oil stains on the surface of the aluminum sheet, and then use dilute hydrochloric acid for pre-etching and weak etching to remove the oxide film, and then use deionized water to wash, and then put it in a vacuum drying oven to dry for standby use.

3. Copper substrate treatment: Polish the copper sheet with 400, 800 and 1200 mesh sandpaper in turn, then perform chemical degreasing to remove oil stains on the surface of the copper sheet, and then use dilute hydrochloric acid for pre-corrosion and weak corrosion to remove the oxide film, and then use deionized water to wash, put it in a vacuum drying oven to dry after washing, and set aside.

4. Constant current electrodeposition: Use aluminum sheet as anode and copper sheet as cathode, control the current density to 30-50 mA / cm2, control the plating solution temperature to 20-40℃ for electrodeposition, and control the electrodeposition time to 30-75min to obtain an Al-MoS2 composite coating with a dense surface and uniform particle distribution.

Images