CN109183024B - Laser cladding method for aluminum oxide-coated graphene oxide/magnesium-based material surface - Google Patents
Laser cladding method for aluminum oxide-coated graphene oxide/magnesium-based material surface Download PDFInfo
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- CN109183024B CN109183024B CN201811083470.3A CN201811083470A CN109183024B CN 109183024 B CN109183024 B CN 109183024B CN 201811083470 A CN201811083470 A CN 201811083470A CN 109183024 B CN109183024 B CN 109183024B
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- C—CHEMISTRY; METALLURGY
- 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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- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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Abstract
A laser cladding method for coating the surface of graphene oxide/magnesium-based material with aluminum oxide is characterized in that in an anhydrous environment, Al ions are adsorbed under the action of self-carried functional groups of graphene oxide by utilizing hydrothermal high pressure, and gamma-type GO @ aluminum oxide is obtained in later-stage roasting. The obtained powder is mixed with Fe powder, Si powder and glycerol according to a certain proportion to obtain the mixed powder in an adhesive state. And (3) polishing the matrix alloy magnesium by using sand paper, and uniformly coating the sticky mixed powder on the surface of the matrix. Then a flame gun is used for quickly and uniformly presintering the powder on the surface of the substrate. The material is then treated by laser cladding. The magnesium-based surface cladding material treated by the method has the characteristics of low wear rate, high surface hardness, good reinforcing combination property and the like, and has the advantages of simplicity, safety, low cost, easiness in operation, controllability and the like.
Description
Technical Field
The invention belongs to the technical field of material preparation.
Background
The graphene nano-sheet is prepared from sp2A two-dimensional material of a thickness of a monoatomic layer composed of hybridized carbon atoms, which exhibits a range of unusual physical properties. The graphene nanosheets have special two-dimensional structures, so that great interest of researchers in the physical, chemical and material science communities is brought, and basic research and engineering application research related to graphene become research hotspots in recent years. Due to the fact that graphene has high strength and tensile strength of 130GPa, the graphene has a huge application space in material application research.
Research into enhancing the strength and other mechanical properties of metal-based materials using carbon materials such as carbon nanotubes or graphene has advanced to some extent. However, due to their outstanding physical properties such as strength, their excellent properties in terms of material wear and hardness have been neglected. A large number of researches show that the correct selection of the reinforcing phase can directly improve the wear resistance and hardness of the composite material. And due to the basic properties of the carbon material, the Graphene Oxide (GO) naturally inherits the characteristics of self-lubrication, better heat dissipation and the like different from other reinforced materials. Proper use can effectively reduce material loss.
However, the defects of the graphene oxide are also obvious. The structure of graphene oxide similar to CNT shows very poor wettability, which directly results in poor interfacial bonding with aluminum matrix, and is not favorable for preparation of composite materials. Thus, improving its wettability with the substrate and choosing the right process method become the key to using graphene to enhance the wear of aluminum-based materials.
The existing method for improving the wettability of graphene oxide comprises surface coating and the like, such as chemical nickel plating, and mainly comprises the steps of sensitizing and activating carboxylated graphene, putting the activated graphene into chemical plating solution for plating, and obtaining a granular coating on the surface of the graphene oxide along with the reaction.
In published patent No. CN106148949A, the name is: laser-induction composite cladding graphene reinforced Ni3Method of Ti composite material ". And pretreating the graphene by chemical plating to obtain the nickel-plated graphene. And mixing the powder and performing conventional laser sintering. In fact, the method has great harm to human bodies due to the limitation of chemical plating, and the graphene needs to be carboxylated independently, so that the production period is long, and meanwhile, the powder waste degree is high due to the utilization of a powder spraying sintering method, and the method has certain limitation.
Therefore, an economical and effective surface coating technology for enhancing the surface wear performance of the magnesium-based composite material by using the graphene oxide is still lacked.
Disclosure of Invention
In order to overcome the technical difficulty of the preparation and molding of the traditional graphene oxide composite material, the invention provides a cladding technology for enhancing the wear resistance of a magnesium-based surface by using graphene oxide. The method is characterized in that mixed powder is added on the surface of a base material, and laser with specific power is utilized to enable the powder to form a protective layer or combine the powder with a matrix. Compared with traditional surface treatment processes such as electroplating and the like, the method has the advantages of wide selection range of applicable base materials, high controllability of a cladding layer, strong customization performance, good bonding performance and the like.
The laser deposition technology comprises three key links of powder selection and proportioning, environment control and process parameter determination, and the three links are linked with each other in a ring-to-ring manner and directly influence the quality of products.
According to the invention, graphene oxide is pretreated by a hydrothermal method, and then the viscosity of glycerol is utilized to keep the dispersibility and the material adhesiveness, so that the non-uniformity caused by different densities in the powder mixing process is reduced.
The specific principle of the invention is as follows:
3Mg+4Al2O3＝3MgAl2O4+2Al
the spinel is generated by introducing alumina on the surface of a magnesium matrix and directly reacting the alumina with magnesium at high temperature. And the self-lubricating property and the extremely high thermal conductivity of the graphene oxide are utilized, so that the surface hardness of the material is linearly improved, and meanwhile, the surface abrasion of the material is effectively reduced.
The invention is realized by the following technical scheme.
The method for cladding the magnesium alloy substrate by using the alumina-coated graphene oxide comprises the following steps.
(1) Carrying out ultrasonic pre-dispersion on graphene oxide in analytically pure ethanol for 1-3 h at room temperature, and controlling the whole process to be free of water vapor. The proportion is strictly controlled to be 0.2-0.4 g:50 ml.
(2) Pouring the graphene oxide dispersion liquid pretreated in the step (1) into a precursor liquid composed of acetylacetone and aluminum nitrate, sealing, and carrying out ultrasonic treatment again for 1-2 hours. Of these, acetylacetone and aluminum nitrate (Al (NO)3)3) The proportion is 0.2-0.4: 1 mol.
(3) And (3) introducing the precursor suspension obtained in the step (2) into a hydrothermal reaction kettle, wherein the ratio of graphene oxide to aluminum nitrate is 1: 1-1.2 mol, and the volume of the suspension accounts for 35% -70% of the volume of the reaction kettle. Heating the mixture in a reaction furnace, heating the mixture to 50-80 ℃ at a speed of 1-5 ℃/min, preserving heat for 1-2 hours, heating the mixture to 150-160 ℃ at a speed of 1-3 ℃/min, and preserving heat for 3-5 hours; taking out, sealing the reaction kettle and air cooling.
(4) And (4) taking out the solution obtained in the step (3), centrifuging, pouring analytically pure ethanol, and centrifuging for multiple times until the solution is colorless, wherein the rotating speed is controlled at 9000-16000 rpm. The whole process is sealed to ensure no water vapor.
(5) And (4) drying the mixed powder obtained in the step (4) in vacuum, and roasting the powder at 450-500 ℃ under the protection of argon. The time is controlled to be 1-3 h. The graphene oxide with the gamma-alumina coating on the surface can be obtained.
(6) And (3) putting the powder obtained in the step (5) into a beaker, adding a certain amount of fine silicon powder and iron powder, and adding a certain amount of glycerol, wherein the silicon powder accounts for 4-8% of the total mass of the powder, the mass ratio of the graphene oxide accounts for 4-7%, the balance is the iron powder, and the size is controlled to be 5-30 μm. The glycerol accounts for 2-6% of the total volume ratio to reduce air holes, no water vapor is generated in the whole treatment process, and then ultrasonic treatment is performed for 1 hour to obtain the mixed powder in an adhesive state.
(7) And (3) polishing the base magnesium-based material alloy plate by using 1500-2000 # abrasive paper, and cleaning and drying by using alcohol. And (4) uniformly coating the adhesive mixed powder obtained in the step (6) on the surface of the substrate, wherein the prefabricated thickness is controlled to be 0.7-1.2 mm. Then a flame gun is used for quickly and uniformly presintering the powder on the surface of the substrate.
(8) And (5) putting the material obtained in the step (7) into an argon protective box, and processing the material by laser cladding. The technological parameters are controlled as follows: the laser power is 0.5-1.2 Kw, the scanning speed is 5-8 mm/s, the diameter of a light spot is 2-5 mm, and the inclination angle is more critical and is controlled to be 20-35 degrees.
The inner lining of the hydrothermal reaction kettle in the step (3) is made of polytetrafluoroethylene.
The invention has the following technical effects: (1) the method reduces the layering phenomenon caused by density difference in the conventional powder mixing process. (2) The dust pollution caused by conventional powder spraying can be reduced by using the viscosity of the lipid, and the powder spraying device is more environment-friendly. (3) The method has the advantages of low reaction temperature and low risk coefficient. (4) The graphene oxide with the transition layer reacts with the matrix on the surface of the magnesium-based material to form a spinel structure, so that the agglomeration probability of the graphene oxide is further reduced while a better interface is provided. (5) The graphene oxide coating has a certain protection effect on the high temperature of laser.
Detailed Description
The invention will be further illustrated by the following examples.
Example 1:
carrying out ultrasonic pre-dispersion on graphene oxide in analytically pure ethanol for 1h at room temperature, and controlling the whole process to be free of water vapor. The mixture ratio is strictly controlled at 0.2g:50ml, and then precursor liquid consisting of acetylacetone and aluminum nitrate is led into the dispersion liquid to be sealed and ultrasonically treated for 1 h. Among these, acetylacetone is reacted with aluminum nitrate (Al (NO)3)3) The mixture ratio is 0.2:1 mol. Then carrying out hydrothermal treatment, wherein the volume of the suspension accounts for 50% of the volume of the reaction kettle. Heating in a reaction furnace at 5 deg.C/min to 80 deg.C, maintaining for 2 hr, and collecting the supernatant at 3 deg.CAfter the temperature is increased to 160 ℃ in min, the temperature is kept for 5 h. Taking out the reaction kettle and then cooling in air. The resulting solution was taken out, centrifuged and centrifuged several times by pouring analytically pure ethanol until the solution was colorless. The whole process is sealed to ensure no water vapor. Then, the obtained powder is roasted at 450 ℃ under the protection of argon. The time is controlled to be 2 h. The surface can be obtained with the surface having the gamma-Al2O3Coated graphene oxide.
And then, proportioning the obtained powder, iron powder and silicon powder in a beaker, and adding a certain amount of glycerol, wherein the mass ratio of the silicon powder to the total powder is controlled to be 4%, the mass ratio of GO to the total powder is controlled to be 5%, the balance is the iron powder, and the size is controlled to be 5 μm. The glycerol accounts for 2-6% of the total volume, no water vapor exists in the whole treatment process, and ultrasonic treatment is carried out for one hour. To obtain a mixed powder in a sticky state. And (3) polishing the substrate aluminum AM60 by using 1500-2000 # abrasive paper, and cleaning and drying by using alcohol. The obtained adhesive state mixed powder is uniformly coated on the surface of a matrix, and the prefabricated thickness is controlled to be 0.7 mm. Then a flame gun is used for quickly and uniformly presintering the powder on the surface of the substrate. And then processing the material by laser cladding in an argon protection box. The technological parameters are controlled as follows: the laser power was 0.7Kw, the scanning speed was 6mm/s, and the spot diameter was 3mm, wherein the tilt angle was controlled to be 20 °.
Example 2.
Carrying out ultrasonic pre-dispersion on graphene oxide in analytically pure ethanol for 1h at room temperature, and controlling the whole process to be free of water vapor. The mixture ratio is strictly controlled at 0.2g:50ml, and then precursor liquid consisting of acetylacetone and aluminum nitrate is led into the dispersion liquid to be sealed and ultrasonically treated for 1 h. Among these, acetylacetone is reacted with aluminum nitrate (Al (NO)3)3) The mixture ratio is 0.3:1 mol. Then, hydrothermal treatment is carried out, wherein the volume of the suspension accounts for 60% of the volume of the reaction kettle. Then putting the mixture into a reaction furnace for heating, heating to 60 ℃ at the speed of 3 ℃/min, preserving heat for 2h, heating to 150 ℃ at the speed of 3 ℃/min, and preserving heat for 3 h. Taking out the reaction kettle and then cooling in air. The resulting solution was taken out, centrifuged and centrifuged several times by pouring analytically pure ethanol until the solution was colorless. The whole process is sealed to ensure no water vapor. Then, the obtained powder is roasted at 500 ℃ under the protection of argon. The time is controlled to be 1 h. The surface can be obtained with the surface having the gamma-Al2O3Coated oxidized stoneGraphene.
Then, the obtained powder is matched with iron powder and silicon powder in a beaker, and a certain amount of glycerol is added, wherein the silicon powder accounts for 6% of the total mass of the powder, the mass ratio of the graphene oxide accounts for 6%, the balance is the iron powder, and the size is controlled to be about 15 microns. The glycerol accounts for 3 percent of the total volume, no water vapor exists in the whole treatment process, and ultrasonic treatment is carried out for one hour. To obtain a mixed powder in a sticky state. And (3) polishing the magnesium AZ61 matrix by using No. 1500-2000 abrasive paper, cleaning by using alcohol and drying. The obtained adhesive state mixed powder is uniformly coated on the surface of a matrix, and the prefabricated thickness is controlled to be 0.9 mm. Then a flame gun is used for quickly and uniformly presintering the powder on the surface of the substrate. And then processing the material by laser cladding in an argon protection box. The technological parameters are controlled as follows: the laser power was 0.9Kw, the scanning speed was 7mm/s, and the spot diameter was 4mm, wherein the tilt angle was controlled to be 25 °.
Example 3.
Carrying out ultrasonic pre-dispersion on graphene oxide in analytically pure ethanol for 1h at room temperature, and controlling the whole process to be free of water vapor. The mixture ratio is strictly controlled at 0.2g:50ml, and then precursor liquid consisting of acetylacetone and aluminum nitrate is led into the dispersion liquid to be sealed and ultrasonically treated for 1 h. Among these, acetylacetone is reacted with aluminum nitrate (Al (NO)3)3) The mixture ratio is 0.4:1 mol. Then carrying out hydrothermal treatment, wherein the volume of the suspension accounts for 40% of the volume of the reaction kettle. Then putting the mixture into a reaction furnace for heating, heating to 80 ℃ at the speed of 3 ℃/min, preserving heat for 1h, heating to 160 ℃ at the speed of 2 ℃/min, and preserving heat for 3 h. Taking out the reaction kettle and then cooling in air. The resulting solution was taken out, centrifuged and centrifuged several times by pouring analytically pure ethanol until the solution was colorless. The whole process is sealed to ensure no water vapor. Then, the obtained powder is roasted at 480 ℃ under the protection of argon. The time is controlled to be 2 h. The surface can be obtained with the surface having the gamma-Al2O3Coated graphene oxide.
And then, proportioning the obtained powder, iron powder and silicon powder in a beaker, and adding a certain amount of glycerol, wherein the mass ratio of the silicon powder to the GO is controlled to be 7% of the total mass of the powder, the mass ratio of the GO is 5%, the balance is the iron powder, and the size is controlled to be about 10 mu m. The glycerol accounts for 6 percent of the total volume, no water vapor exists in the whole treatment process, and ultrasonic treatment is carried out for one hour. To obtain a mixed powder in a sticky state. And (3) polishing the substrate AZ91D by using No. 1500-2000 abrasive paper, cleaning by using alcohol and drying. The obtained adhesive state mixed powder is uniformly coated on the surface of a matrix, and the prefabricated thickness is controlled to be 1.1 mm. Then a flame gun is used for quickly and uniformly presintering the powder on the surface of the substrate. And then processing the material by laser cladding in an argon protection box. The technological parameters are controlled as follows: the laser power was 1.2Kw, the scanning speed was 8mm/s, and the spot diameter was 5mm, wherein the tilt angle was controlled to be 30 °.
Claims (1)
1. A laser cladding method for coating the surface of graphene oxide/magnesium-based material by using aluminum oxide comprises the following steps:
(1) carrying out ultrasonic pre-dispersion on graphene oxide in analytically pure ethanol for 1-3 h at room temperature, controlling the whole process to be free of water vapor, and strictly controlling the mixture ratio to be 0.2-0.4 g:50 mL;
(2) pouring the graphene oxide dispersion liquid pretreated in the step (1) into a precursor liquid consisting of acetylacetone and aluminum nitrate, sealing, and carrying out ultrasonic treatment for 1-2 hours again, wherein the ratio of the acetylacetone to the aluminum nitrate is 0.2-0.4: 1 mol;
(3) introducing the precursor suspension obtained in the step (2) into a hydrothermal reaction kettle, wherein the ratio of graphene oxide to aluminum nitrate is 1: 1-1.2 mol, and the volume of the suspension accounts for 35% -70% of the volume of the reaction kettle; heating the mixture in a reaction furnace, heating the mixture to 50-80 ℃ at a speed of 1-5 ℃/min, preserving heat for 1-2 hours, heating the mixture to 150-160 ℃ at a speed of 1-3 ℃/min, and preserving heat for 3-5 hours; taking out, sealing the reaction kettle and air cooling;
(4) taking out the solution obtained in the step (3), centrifuging, pouring analytically pure ethanol, centrifuging for multiple times until the solution is colorless, controlling the rotating speed at 9000-16000 rpm, and sealing the whole process to ensure that no water vapor exists;
(5) vacuum drying the mixed powder obtained in the step (4), and roasting the powder at 450-500 ℃ under the protection of argon for 1-3 h; graphene oxide with a gamma-alumina coating on the surface can be obtained;
(6) putting the powder obtained in the step (5) into a beaker, adding fine silicon powder and iron powder, and adding glycerol, wherein the silicon powder is controlled to be 4-8% of the total mass of the powder, the mass ratio of graphene oxide is 4-7%, the balance is iron powder, and the size is controlled to be 5-30 μm; the glycerol accounts for 2-6% of the total volume ratio to reduce air holes, no water vapor is generated in the whole treatment process, and then ultrasonic treatment is performed for 1 hour to obtain mixed powder in an adhesive state;
(7) polishing the base magnesium-based material alloy plate by using No. 1500-2000 abrasive paper, cleaning and drying by using alcohol, then uniformly coating the adhesive mixed powder obtained in the step (6) on the surface of the base, controlling the prefabricated thickness to be 0.7-1.2 mm, and rapidly and uniformly pre-sintering the powder on the surface of the base by using a flame gun;
(8) putting the material obtained in the step (7) into an argon protective box, and processing the material by laser cladding, wherein the process parameters are controlled as follows: the laser power is 0.5-1.2 kW, the scanning speed is 5-8 mm/s, the spot diameter is 2-5 mm, and the inclination angle is more critical and is controlled to be 20-35 degrees;
and (4) the lining of the hydrothermal reaction kettle in the step (3) is polytetrafluoroethylene.
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