Aluminum alloy material easy to oxidize and color and preparation method thereof

Abstract

The invention discloses an aluminum alloy material easy to oxidize and color and a preparation method thereof.The aluminum alloy material is prepared from, by weight, 20-25 parts of aluminum alloy powder, 5-10 parts of graphene, 4-6 parts of p-nitrophenol, 0.5-1 part of concentrated bromine water and 4-7 parts of magnesium powder. And graphene treatment, aluminum alloy and graphene dispersion treatment, drying, water washing and vacuum hot pressing are carried out. Graphene is doped with the aluminum alloy, the comprehensive performance of the aluminum alloy can be remarkably improved, the hardness can be improved, the electrical conductivity and the thermal conductivity can be remarkably improved, halogen elements are introduced, the activity of the aluminum alloy is improved, the oxidized capacity is improved, the coloring efficiency is improved, and the flame retardant property is improved; and the magnesium powder is added, so that the stability of the system is protected, and the hardness of the system is improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of aluminum alloy materials, in particular to an aluminum alloy material easy to be oxidized and colored and a preparation method thereof. BACKGROUND

[0002] Aluminum alloy is an important metal material in industry and life, and has a wide application in the fields of automobile, aerospace, machinery, ship and chemistry. The main method for coloring aluminum alloy is to oxidize aluminum alloy as an anode, and after oxidation, fine cavities appear on the surface of the aluminum alloy, and then the aluminum alloy is placed in the dye prepared in advance with water, so that the dye is adsorbed into the cavities to achieve the purpose of coloring.

[0003] The perfect degree of coloring of aluminum alloy depends on the number of cavities on the surface of the aluminum alloy after oxidation. Aluminum forms a dense oxide film on the surface in air and water, thereby reducing the occurrence of oxidation. The general solution is to add a lively metal to achieve the purpose of being oxidized, but this method has certain limitations. The requirement for electrolyte is getting higher and higher, and the efficiency of oxidation also has a certain upper limit, which cannot meet the production needs of people. In the process of electrolysis, a part of metal ions cannot be attached to the surface of the aluminum alloy, causing a certain loss and reducing the comprehensive performance of the product. Therefore, it is particularly important to invent a new type of aluminum alloy material. SUMMARY

[0004] The present application aims to provide an aluminum alloy material easy to be oxidized and colored and a preparation method thereof to solve the problems in the background art.

[0005] In order to solve the above technical problems, the present application provides the following technical scheme: an aluminum alloy material easy to be oxidized and colored, the raw materials of the aluminum alloy material are as follows, in terms of weight fraction, including 20-25 parts of aluminum alloy powder, 5-10 parts of graphene, 4-6 parts of p-nitrophenol, 0.5-1 part of concentrated bromine water and 4-7 parts of magnesium powder.

[0006] A preparation method of an aluminum alloy material easy to be oxidized and colored, the steps are as follows, (1) Dissolve graphene into ice water, add concentrated sulfuric acid, stir at 500-600 r / min, add sodium nitrate and potassium permanganate, stir for 2-3 h, add hydrogen peroxide, stir for 30-60 min, filter to obtain composition A; (2) Ultrasonically treat composition A to dissolve it in anhydrous ethanol, add p-nitrophenol, stir at 500-600 r / min, add concentrated bromine water to obtain composition B; (3) Add aluminum alloy powder into acetone solution, stir at 500-600 r / min, and stir for 20-30 min to obtain composition C; (4) Mix composition B with composition C, disperse by mechanical grinding, to obtain dispersion liquid A; (5) Add magnesium powder into dispersion liquid A, add in 3 times, stir at 500-600 r / min, disperse until uniform; (6) Filter dispersion liquid A, rinse with deionized water, repeat 3 times, to obtain filter cake, put the filter cake into inert gas drying box, dry for 1-2 h, after drying, put into stainless steel mold; (7) Put the stainless steel mold containing the product into vacuum hot press, vacuumize, heat up to 200-300℃, pressurize, pressure 50-60 MPa, keep temperature and pressure for 3-5 h, start to cool down; (8) Slowly cool down the furnace, take out the mold, take out the product to obtain aluminum alloy material.

[0007] Further, the reaction temperature in steps (2) to (4) is kept at 20-25℃.

[0008] Further, in step (5), the magnesium powder is added in 3 times, 1 / 6 of the total amount in the first time, 1 / 3 of the total amount in the second time, and 1 / 2 of the total amount in the third time.

[0009] Further, in step (6), the temperature of the drying box is 150-250℃, and the inert gas is argon or xenon.

[0010] Further, in step (7), the vacuum degree is 10-20 KPa, and the heating rate is controlled at 30-50℃ / h.

[0011] Further, in step (8), the cooling rate is controlled at 50-60℃ / h.

[0012] Further, in step (6), the filter screen is selected to be 30-50 μm.

[0013] Compared with the prior art, the present application has the advantages that: in industrial production, the hardness of common aluminum alloy materials cannot meet people's needs, in the present application, graphene is doped with aluminum alloy, which can significantly improve the comprehensive performance of aluminum alloy, improve the hardness, and significantly improve the electrical conductivity and thermal conductivity, the present application compares graphene and carbon nanotubes when selecting materials, and finally selects graphene, the reason is that graphene has smaller porosity than carbon nanotubes, and when doped with aluminum alloy, the breaking of carbon-carbon bonds can be reduced, thereby causing the structure of graphene to change, however, graphene still has high porosity, therefore, the graphene is treated first, and the treated graphene has multiple functional groups, such as hydroxyl and carboxyl groups, the addition of functional groups can fill the voids of nucleation sites on one hand, and the addition of functional groups can better improve the aluminum alloy-graphene.

[0014] When dispersing and dissolving the aluminum powder, the solvent added is acetone, but acetone is not a substance required by the product, the general treatment method is to heat to 60-80 DEG C, and evaporate, but this operation will cause the functional groups on the graphene to decompose, and the structure of the graphene and its functional groups is destroyed, therefore, the present application selects p-nitrophenol, on one hand, p-nitrophenol can absorb acetone in the presence of concentrated sulfuric acid, on the other hand, the formation of a new polymer can protect the metal from corrosion by acid and alkali, and on the other hand, the hydroxyl group of p-nitrophenol and the hydroxyl group of the treated graphene can be complexed with the metal added later, which can improve the hardness and stability of the aluminum alloy-graphene system.

[0015] When coloring the aluminum alloy material, the electrolytic method is usually used, the aluminum alloy is oxidized as an anode, and then is put into a dye solution, so as to achieve the purpose of dyeing. Therefore, the present application treats p-nitrophenol, and adds concentrated bromine water drop by drop, to ensure that bromine completely replaces the hydrogen atoms on the benzene ring, so that p-nitrophenol carries halogen, on one hand, the product acts as an anode, during ionization, the aluminum alloy surface will form a cavity, and free bromide ions will also be generated, the part of bromide ions can be adsorbed on the cavity of the aluminum alloy material, improve the adsorption capacity of free metal ions, change the surface distribution of the aluminum alloy, make the oxide film on the surface of the aluminum alloy more easily form a cavity, increase the activity of the aluminum alloy, thereby improve the oxidation ability and the coloring efficiency, on the other hand, it can be used as an excellent flame retardant, which can volatilize flame retardant gas when burning to inhibit combustion. The treated graphene has hydroxyl and carboxyl groups, the carboxyl group will produce hydrogen ions with acid when ionized, the hydrogen ions will combine with the ionized bromide ions, causing the rupture of the metal oxide film, the added magnesium powder can react with the carboxyl groups on the graphene, thereby achieving the purpose of removing the carboxyl groups on the graphene.

[0016] In the presence of concentrated sulfuric acid, the concentrated sulfuric acid will react with other metals in the aluminum alloy which is added first, mainly containing copper, magnesium, zinc and other metals, to generate copper sulfate, zinc sulfate and other metal salts, thereby destroying the metal structure of the aluminum alloy and failing to achieve the purpose of enhancing the hardness of the aluminum alloy. According to the activity of the metal, the magnesium powder is selected and added in three times. The reason is that copper sulfate and zinc sulfate will undergo displacement reaction with the added magnesium powder. In order to ensure that the system does not contain copper sulfate and zinc sulfate, the magnesium powder needs to be added in batches and also needs to be continuously stirred and ground to ensure that the precipitated copper and zinc are uniformly dispersed in the anhydrous ethanol. After subsequent vacuum hot pressing, the content of copper, magnesium, zinc and other metal elements in the aluminum alloy can still be maintained, thereby ensuring the stability of the system and improving the hardness of the system. During the heating operation of the vacuum hot press, the heating rate needs to be controlled. If the heating rate is too fast, the product will be unevenly heated, thereby causing the hardness of the product to decrease and the product yield to decrease.

[0017] The hydroxyl and carboxyl groups of the anhydrous ethanol can undergo esterification reaction in the presence of concentrated sulfuric acid. This reaction is reversible and also brings in new impurities. Therefore, the product system of the present application does not contain ester impurities, thereby improving the hardness of the aluminum alloy and the yield of the product. DETAILED DESCRIPTION

[0018] The technical solutions in the embodiments of the present application will be described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present application, not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.

[0019] Embodiment one An aluminum alloy material easy to oxidize and color, raw materials of each component of the aluminum alloy material are as follows, by weight fraction, including aluminum alloy powder 20 parts, graphene 5 parts, p-nitrophenol 4 parts, concentrated bromine water 0.5 parts, magnesium powder 4 parts.

[0020] A preparation method of an aluminum alloy material easy to oxidize and color, steps are as follows, (1) Dissolve the graphene into ice water, add concentrated sulfuric acid, stir at 500 r / min, add sodium nitrate and potassium permanganate, stir for 2 h, add hydrogen peroxide, stir for 30 min, filter to obtain composition A; (2) Ultrasonic treatment is performed on the composition A to dissolve it in anhydrous ethanol, add p-nitrophenol, stir at 500 r / min, temperature 20℃, add concentrated bromine water to obtain composition B; (3) aluminum alloy powder is added into acetone solution, stirring at 500 r / min, temperature 20℃, stirring time 20 min, to obtain composition C; (4) composition B is mixed with composition C, temperature 20℃, dispersion by mechanical grinding, to obtain dispersion liquid A; (5) magnesium powder is added into dispersion liquid A, adding in 3 times, 1 / 6 of total fraction in the first time, 1 / 3 of total fraction in the second time, 1 / 2 of total fraction in the third time, stirring at 500 r / min, dispersion until uniform; (6) dispersion liquid A is filtered, filter screen 30 μm, deionized water washing, repeated 3 times, to obtain filter cake, the filter cake is put into inert gas drying box, temperature of drying box 150℃, inert gas argon, xenon, drying for 1 h, after drying, the product is loaded into stainless steel mold; (7) the stainless steel mold loaded with product is put into vacuum hot press, vacuum degree 10 KPa, temperature rising speed controlled at 30℃ / h, temperature rising 200℃, pressurizing, pressure 50 MPa, holding time 3 h, starting cooling; (8) furnace cooling, slow cooling, temperature dropping speed should be controlled, keeping 50℃ / h, taking out the mold, taking out the product, to obtain aluminum alloy material.

[0021] Example two An aluminum alloy material easy to be oxidized and colored, raw materials of each component are as follows, by weight fraction, including aluminum alloy powder 23 parts, graphene 6 parts, p-nitrophenol 5 parts, concentrated bromine water 0.8 parts, magnesium powder 5 parts.

[0022] A preparation method of an aluminum alloy material easy to be oxidized and colored, steps are as follows, (1) graphene is dissolved into ice water, concentrated sulfuric acid is added, stirring at 550 r / min, sodium nitrate, potassium permanganate are added, stirring for 2.5 h, hydrogen peroxide is added, stirring for 50 min, filtering, to obtain composition A; (2) composition A is ultrasonically treated, to be dissolved in anhydrous ethanol, p-nitrophenol is added, stirring at 550 r / min, temperature 20-25℃, concentrated bromine water is added, to obtain composition B; (3) aluminum alloy powder is added into acetone solution, stirring at 550 r / min, temperature 23℃, stirring time 25 min, to obtain composition C; (4) composition B is mixed with composition C, temperature 22℃, dispersion by mechanical grinding, to obtain dispersion liquid A; (5) magnesium powder is added to the dispersion liquid A, added in 3 times, 1 / 6 of the total fraction is added in the first time, 1 / 3 of the total fraction is added in the second time, 1 / 2 of the total fraction is added in the third time, stirring 550 r / min, dispersed until uniform; (6) the dispersion liquid A is filtered, a 40 μm filter screen is selected, washed with deionized water, repeated 3 times, a filter cake is obtained, the filter cake is placed into an inert gas drying box, the temperature of the drying box is 200℃, the inert gas is argon and xenon, dried for 1.5 h, after drying, the filter cake is loaded into a stainless steel mold; (7) the stainless steel mold loaded with the product is placed into a vacuum hot press, vacuumized, the vacuum degree is 15 KPa, the temperature rising speed is controlled at 40℃ / h, the temperature is raised to 250℃, pressurized, the pressure is 55 MPa, the temperature and pressure are kept for 4 h, the temperature is started to be lowered; (8) the hearth is cooled, slowly cooled, the temperature lowering speed is controlled, the temperature is lowered at 55℃ / h, the mold is taken out, the product is taken out, an aluminum alloy material is obtained.

[0023] Example three An aluminum alloy material easy to be oxidized and colored, raw materials of each component of the aluminum alloy material are as follows, by weight fraction, including aluminum alloy powder 25 parts, graphene 10 parts, p-nitrophenol 6 parts, concentrated bromine water 1 part, magnesium powder 7 parts.

[0024] A preparation method of an aluminum alloy material easy to be oxidized and colored, steps are as follows, (1) graphene is dissolved into ice water, concentrated sulfuric acid is added, stirring 600 r / min, sodium nitrate and potassium permanganate are added, stirring 3 h, hydrogen peroxide is added, stirring 60 min, filtered, a composition A is obtained; (2) the composition A is ultrasonically treated, dissolved in anhydrous ethanol, p-nitrophenol is added, stirring 600 r / min, the temperature is 25℃, concentrated bromine water is added, a composition B is obtained; (3) aluminum alloy powder is added into an acetone solution, stirring 600 r / min, the temperature is 25℃, the stirring time is 30 min, a composition C is obtained; (4) the composition B is mixed with the composition C, the temperature is 25℃, dispersed by mechanical grinding, a dispersion liquid A is obtained; (5) magnesium powder is added to the dispersion liquid A, added in 3 times, 1 / 6 of the total fraction is added in the first time, 1 / 3 of the total fraction is added in the second time, 1 / 2 of the total fraction is added in the third time, stirring 600 r / min, dispersed until uniform; (6) the dispersion liquid A is filtered, a 50 μm filter screen is selected, washed with deionized water, repeated 3 times, a filter cake is obtained, the filter cake is placed into an inert gas drying box, the temperature of the drying box is 250℃, the inert gas is argon and xenon, dried for 2 h, after drying, the filter cake is loaded into a stainless steel mold; (7) Put the stainless steel mold containing the product into the vacuum hot press, vacuumize, vacuum degree 20 KPa, temperature rising speed control at 50℃ / h, temperature rising 300℃, pressurize, pressure 60MPa, temperature and pressure preservation, time 5h, start cooling; (8) Perform hearth cooling, slowly cool, control cooling speed when cooling, maintain 60℃ / h cooling, take out the mold, take out the product to obtain the aluminum alloy material.

[0025] Comparative Example 1 An aluminum alloy material easy to oxidize and color, raw materials of each component are as follows, including aluminum alloy powder 25 parts, graphene 10 parts, concentrated bromine water 1 part, magnesium powder 7 parts.

[0026] A method for preparing an aluminum alloy material easy to oxidize and color, steps are as follows, (1) Dissolve graphene into ice water, add concentrated sulfuric acid, stir 600r / min, add sodium nitrate and potassium permanganate, stir 3h, add hydrogen peroxide, stir 60min, filter to obtain composition A; (2) Ultrasonically treat composition A to dissolve in anhydrous ethanol, stir 600r / min, temperature 25℃, add concentrated bromine water to obtain composition B; (3) Add aluminum alloy powder into acetone solution, stir 600r / min, temperature 25℃, stir for 30min to obtain composition C; (4) Mix composition B and composition C, temperature 25℃, disperse by mechanical grinding to obtain dispersion liquid A; (5) Add magnesium powder into dispersion liquid A, add in three times, add 1 / 6 of total parts in the first time, add 1 / 3 of total parts in the second time, add 1 / 2 of total parts in the third time, stir 600r / min, disperse until uniform; (6) Filter dispersion liquid A, select 50μm filter screen, rinse with deionized water for 3 times to obtain filter cake, put the filter cake into inert gas drying box, temperature of the drying box 250℃, inert gas is argon and xenon, dry for 2h, after drying, put into stainless steel mold; (7) Put the stainless steel mold containing the product into the vacuum hot press, vacuumize, vacuum degree 20 KPa, temperature rising speed control at 50℃ / h, temperature rising 300℃, pressurize, pressure 60MPa, temperature and pressure preservation, time 5h, start cooling; (8) Perform hearth cooling, slowly cool, control cooling speed when cooling, maintain 60℃ / h cooling, take out the mold, take out the product to obtain the aluminum alloy material.

[0027] Comparative Example 2 An aluminum alloy material easy to oxidize coloring, the aluminum alloy material raw materials are as follows, including aluminum alloy powder 25 parts, graphene 10 parts, p-nitrophenol 6 parts, magnesium powder 7 parts.

[0028] An aluminum alloy material easy to oxidize coloring preparation method, the steps are as follows, (1) graphene is dissolved in ice water, concentrated sulfuric acid is added, stirring 600r / min, sodium nitrate, potassium permanganate is added, stirring 3h, hydrogen peroxide is added, stirring 60min, filtration, get composition A; (2) composition A is treated by ultrasonic, it is dissolved in anhydrous ethanol, p-nitrophenol is added, stirring 600r / min, temperature 25 DEG C, get composition B; (3) aluminum alloy powder is added to acetone solution, stirring 600r / min, temperature 25 DEG C, stirring time 30min, get composition C; (4) composition B and composition C are mixed, temperature 25 DEG C, by mechanical grinding, dispersion, get dispersion liquid A; (5) magnesium powder is added to dispersion liquid A, in 3 times, the first time adds 1 / 6 of total fraction, the second time adds 1 / 3 of total fraction, the third time adds 1 / 2 of total fraction, stirring 600r / min, dispersion, until uniform; (6) dispersion liquid A is filtered, filter screen selects 50 μm, deionized water is washed, repeat 3 times, get filter cake, the filter cake is placed into inert gas drying box, the temperature of drying box is 250 DEG C, inert gas is argon, xenon, dry 2h, after drying, is loaded into stainless steel mould; (7) the stainless steel mould loaded with product is placed into vacuum hot press, vacuum, vacuum degree 20 KPa, temperature rising speed control is at 50 DEG C / h, temperature rises 300 DEG C, pressurizes, pressure 60MPa, keeps temperature and pressure, time 5h, starts cooling; (8) furnace hearth cooling, slow cooling, when cooling, temperature drop speed is controlled, maintains 60 DEG C / h, takes out product and gets aluminum alloy material.

[0029] Comparative example 3 An aluminum alloy material easy to oxidize coloring, the aluminum alloy material raw materials are as follows, including aluminum alloy powder 25 parts, graphene 10 parts, p-nitrophenol 6 parts, concentrated bromine water 1 part, magnesium powder 7 parts.

[0030] An aluminum alloy material easy to oxidize coloring preparation method, the steps are as follows, (1) graphene is dissolved in ice water, concentrated sulfuric acid is added, stirring 600r / min, sodium nitrate, potassium permanganate is added, stirring 3h, hydrogen peroxide is added, stirring 60min, filtration, get composition A; (2) ultrasonic treatment of composition A, dissolved in anhydrous ethanol, adding p-nitrophenol, stirring 600 r / min, temperature 25℃, adding concentrated bromine water, 1 time, to obtain composition B; (3) aluminum alloy powder is added to acetone solution, stirring 600 r / min, temperature 25℃, stirring time 30 min, to obtain composition C; (4) composition B is mixed with composition C, temperature 25℃, dispersed by mechanical grinding, to obtain dispersion A; (5) magnesium powder is added to dispersion A, 3 times, 1 / 6 of the total fraction is added the first time, 1 / 3 of the total fraction is added the second time, 1 / 2 of the total fraction is added the third time, stirring 600 r / min, dispersed until uniform; (6) dispersion A is filtered, filter screen 50 μm, deionized water is used for washing, repeated 3 times, to obtain filter cake, the filter cake is placed into an inert gas drying box, temperature of the drying box 250℃, inert gas argon, xenon, dried for 2 h, after drying, loaded into a stainless steel mold; (7) the stainless steel mold loaded with the product is placed into a vacuum hot press, vacuumed, vacuum degree 20 KPa, temperature rising speed controlled at 50℃ / h, temperature raised to 300℃, pressurized, pressure 60 MPa, holding temperature and pressure, time 5 h, temperature starts to decrease; (8) furnace hearth temperature is decreased, slowly, temperature decreasing speed is controlled, maintained at 60℃ / h, the product is taken out, to obtain an aluminum alloy material.

[0031] Comparative Example 4 An aluminum alloy material easy to be oxidized and colored, raw materials of each component are as follows, by weight fraction, including aluminum alloy powder 25 parts, graphene 10 parts, p-nitrophenol 6 parts, concentrated bromine water 1 part.

[0032] A method for preparing an aluminum alloy material easy to be oxidized and colored, steps are as follows, (1) graphene is dissolved into ice water, concentrated sulfuric acid is added, stirring 600 r / min, sodium nitrate, potassium permanganate are added, stirring 3 h, hydrogen peroxide is added, stirring 60 min, filtered, to obtain composition A; (2) ultrasonic treatment of composition A, dissolved in anhydrous ethanol, adding p-nitrophenol, stirring 600 r / min, temperature 25℃, adding concentrated bromine water, to obtain composition B; (3) aluminum alloy powder is added to acetone solution, stirring 600 r / min, temperature 25℃, stirring time 30 min, to obtain composition C; (4) composition B is mixed with composition C, temperature 25℃, dispersed by mechanical grinding, to obtain dispersion A; (5) The dispersion liquid A is filtered with a 50 μm filter screen, washed with deionized water for 3 times, and a filter cake is obtained. The filter cake is placed in an inert gas drying oven with a temperature of 250℃, and argon or xenon is used as the inert gas. The drying is performed for 2 hours. After drying, the product is loaded into a stainless steel mold; (6) The stainless steel mold loaded with the product is placed in a vacuum hot press. Vacuum is applied with a vacuum degree of 20 KPa. The temperature is raised at a speed of 50℃ / h to 300℃. Pressure is applied at a pressure of 60 MPa. The temperature and pressure are maintained for 5 hours. The temperature is then lowered; (7) The furnace is cooled slowly. The cooling speed is controlled to maintain a cooling speed of 60℃ / h. The product is taken out to obtain an aluminum alloy material.

[0033] Comparative Example 5 An aluminum alloy material easy to be oxidized and colored, which comprises, by weight fraction, 25 parts of aluminum alloy powder, 10 parts of graphene, 6 parts of p-nitrophenol, 1 part of concentrated bromine water, and 7 parts of magnesium powder.

[0034] A method for preparing an aluminum alloy material easy to be oxidized and colored, which comprises the following steps, (1) The graphene is dissolved in ice water. Concentrated sulfuric acid is added. The mixture is stirred at a speed of 600 r / min. Sodium nitrate and potassium permanganate are added. The mixture is stirred for 3 hours. Hydrogen peroxide is added. The mixture is stirred for 60 minutes. The mixture is filtered to obtain a composition A; (2) The composition A is subjected to ultrasonic treatment and dissolved in anhydrous ethanol. P-nitrophenol is added. The mixture is stirred at a speed of 600 r / min at a temperature of 25℃. Concentrated bromine water is added to obtain a composition B; (3) The aluminum alloy powder is added to an acetone solution. The mixture is stirred at a speed of 600 r / min at a temperature of 25℃ for 30 minutes to obtain a composition C; (4) The composition B and the composition C are mixed at a temperature of 25℃. The mixture is dispersed by mechanical grinding to obtain a dispersion liquid A; (5) The magnesium powder is added to the dispersion liquid A in one time. The mixture is stirred at a speed of 600 r / min until it is uniformly dispersed; (6) The dispersion liquid A is filtered with a 50 μm filter screen. The filter cake is washed with deionized water for 3 times. The filter cake is placed in an inert gas drying oven with a temperature of 250℃. Argon or xenon is used as the inert gas. The drying is performed for 2 hours. After drying, the product is loaded into a stainless steel mold; (7) The stainless steel mold loaded with the product is placed in a vacuum hot press. Vacuum is applied with a vacuum degree of 20 KPa. The temperature is raised at a speed of 50℃ / h to 300℃. Pressure is applied at a pressure of 60 MPa. The temperature and pressure are maintained for 5 hours. The temperature is then lowered; (8) furnace temperature reduction, slow cooling, cooling to control the cooling rate, keep 60 ℃ / h cooling, remove the mold, remove the product to get aluminum alloy material.

[0035] Comparative Example 6 An aluminum alloy material easy to oxidize coloring, the aluminum alloy material each component raw material is as follows, by weight fraction, including aluminum alloy powder 25 parts, graphene 10 parts, p-nitrophenol 6 parts, concentrated bromine water 1 part, magnesium powder 7 parts.

[0036] An aluminum alloy material easy to oxidize coloring preparation method, the steps are as follows, (1) the graphene is dissolved in ice water, add concentrated sulfuric acid, stirring 600 r / min, add sodium nitrate, potassium permanganate, stirring 3h, add hydrogen peroxide, stirring 60 min, filtration, get composition A; (2) composition A is treated by ultrasonic, make it dissolved in anhydrous ethanol, add p-nitrophenol, stirring 600 r / min, temperature 25 ℃, add concentrated bromine water, get composition B; (3) aluminum alloy powder is added to acetone solution, stirring 600 r / min, temperature 25 ℃, stirring time 30 min, get composition C; (4) composition B and composition C are mixed, temperature 25 ℃, through mechanical grinding, dispersion, get dispersion liquid A; (5) magnesium powder is added to dispersion liquid A, add in 3 times, the first time adds 1 / 6 of the total fraction, the second time adds 1 / 3 of the total fraction, the third time adds 1 / 2 of the total fraction, stirring 600 r / min, dispersion, until uniform; (6) the dispersion liquid A is filtered, the filter screen is selected to be 50 μm, and deionized water is used for washing, which is repeated 3 times, to obtain a filter cake, which is placed into an inert gas drying box, the temperature of the drying box is 250 ℃, the inert gas is argon or xenon, and drying is performed for 2 h, after drying, the filter cake is loaded into a stainless steel mold; (7) the stainless steel mold loaded with the product is placed into a vacuum hot press, vacuumizing is performed, the vacuum degree is 20 KPa, the temperature rising speed is controlled to be 50 ℃ / h, the temperature is raised to 600 ℃, pressurizing is performed, the pressure is 60 MPa, the temperature is kept for 5 h, and then cooling starts; (8) furnace temperature reduction, slow cooling, cooling to control the cooling rate, keep 60 ℃ / h cooling, remove the mold, remove the product to get aluminum alloy material.

[0037] Comparative Example 7 An aluminum alloy material easy to oxidize coloring, the aluminum alloy material each component raw material is as follows, by weight fraction, including aluminum alloy powder 25 parts, graphene 10 parts, p-nitrophenol 6 parts, concentrated bromine water 1 part, magnesium powder 7 parts.

[0038] A method for preparing an aluminum alloy material susceptible to oxidation coloring, comprising the following steps, (1) Dissolve graphene into ice water, add concentrated sulfuric acid, stir at 600 r / min, add sodium nitrate and potassium permanganate, stir for 3 h, add hydrogen peroxide, stir for 60 min, and filter to obtain composition A; (2) Ultrasonically treat composition A, dissolve it in anhydrous ethanol, add p-nitrophenol, stir at 600 r / min at a temperature of 25℃, and add concentrated bromine water to obtain composition B; (3) Add aluminum alloy powder into an acetone solution, stir at 600 r / min at a temperature of 25℃ for 30 min to obtain composition C; (4) Mix composition B with composition C at a temperature of 25℃, and disperse by mechanical grinding to obtain dispersion liquid A; (5) Add magnesium powder into dispersion liquid A, add 1 / 6 of the total amount of magnesium powder at the first time, add 1 / 3 of the total amount of magnesium powder at the second time, and add 1 / 2 of the total amount of magnesium powder at the third time, and stir and disperse at 600 r / min until uniform; (6) Filter dispersion liquid A using a filter screen with a mesh size of 50 μm, and wash with deionized water for 3 times to obtain a filter cake, place the filter cake into an inert gas drying box, set the temperature of the drying box to 250℃, use argon or xenon as the inert gas, and dry for 2 h, then place the dried filter cake into a stainless steel mold; (7) Place the stainless steel mold containing the product into a vacuum hot press, perform vacuumization, control the vacuum degree to be 20 KPa, control the temperature rising speed to be 100℃ / h, raise the temperature to 300℃, apply pressure, and control the pressure to be 60 MPa, and perform heat preservation and pressure maintaining for 5 h, and then start to reduce the temperature; (8) Slowly reduce the temperature of the furnace, control the temperature reducing speed to be 60℃ / h, and take out the product to obtain an aluminum alloy material.

[0039] Experiment Example 3 as a control, set up the following comparative examples: comparative example 1, comparative example 2, comparative example 3, comparative example 4, comparative example 5, comparative example 6, and comparative example 7.

[0040] The differences between example 3 and the comparative examples are as follows: comparative example 1, p-nitrophenol is not added; comparative example 2, concentrated bromine water is not added; comparative example 3, bromine water is added at one time instead of dropwise; comparative example 4, magnesium powder is not added; comparative example 5, magnesium powder is added at one time instead of in three times; comparative example 6, the hot pressing temperature exceeds 500℃; and comparative example 7, the temperature rising speed during vacuum hot pressing is 100℃ / h.

[0041] Hardness test was carried out on each sample of Example 1, Example 2, Example 3, Comparative Example 1, Comparative Example 4, Comparative Example 5, Comparative Example 6, Comparative Example 7, and aluminum alloy 6061-T6, 3 samples each, with the experimental standard being GB5237-2004, YB / T420-2000, Table I

[0042] Example 1, Example 2, Example 3, Comparative Example 2, Comparative Example 3, each sample 6 samples, 3 samples for ion oxidation, 3 samples for ion oxidation coloring, and then placed under a SEM microscope for observation, Table II

[0043] Data analysis and conclusion Analysis of Table I shows that the hardness values of Example 1, Example 2, and Example 3 remain in the range of 135-140 hb, the hardness value of Comparative Example 1 remains in the range of 120-125 hb, the hardness value of Comparative Example 4 remains in the range of 110-115 hb, the hardness value of Comparative Example 5 remains in the range of 115-120 hb, the hardness value of Comparative Example 6 remains in the range of 80-85 hb, the hardness value of Comparative Example 7 remains in the range of 105-110 hb, and the hardness value of aluminum alloy 6061-T6 remains in the range of 90-95 hb. The hardness value range is arranged as Example 1, Example 2, and Example 3 > Comparative Example 1 > Comparative Example 5 > Comparative Example 4 > Comparative Example 7 > aluminum alloy 6061-T6 > Comparative Example 6.

[0044] It is concluded that no p-nitrophenol is added in Comparative Example 1, which leads to the decrease of the stability of the aluminum alloy-graphene system, and the rupture occurs when the subsequent processing steps are carried out, resulting in the decrease of the hardness of the product, which shows that the addition of p-nitrophenol in the present application has effect and can improve the stability of the aluminum alloy-graphene and the hardness of the product. In Comparative Example 4, no magnesium powder is contained, and the concentrated sulfuric acid added in the preparation process corrodes other metal elements in the aluminum alloy, which changes the metal content of the aluminum alloy and reduces the hardness of the product, which shows the importance of adding magnesium powder in the present application, which can ensure the content of the remaining metals in the aluminum alloy-graphene and further ensure the hardness of the product within the index range. In Comparative Example 5, the magnesium powder is added at one time, although there is a subsequent stirring and dispersion process, but the actual reaction effect is poorer than that of Example 1, Example 2 and Example 3, and part of the metal still exists in the system in the form of metal salt, which leads to the decrease of the hardness of the product, which shows that the way of adding magnesium powder in the present application in three times is very necessary. In Comparative Example 6, the temperature of hot pressing reaches 600℃, and the hardness is 84hb, which is even less than 93hb of the bulk aluminum alloy 6061-T6, the reason is that the temperature is too high, and the magnesium and copper in the aluminum alloy are sintered, the metal hardness is decreased, and the graphene and its functional groups are decomposed, which finally leads to the decrease of the overall performance of the product, which shows the necessity of confirming that the temperature of vacuum hot pressing in the present application should not be higher than 500℃, which can ensure that the metal will not be sintered, and the graphene and its functional groups will not be decomposed, and further ensure the yield and hardness of the product. In Comparative Example 7, the heating speed is too fast during hot pressing, and the heating is uneven, which makes the hot pressing degree of each part of the aluminum alloy-graphene different, so that the hardness of the product is decreased, so in the operation of vacuum hot pressing, the heating speed should be slow to ensure uniform heating, and further ensure the hardness and yield of the product.

[0045] According to the analysis of Table 2, the surface texture of Example 1, Example 2 and Example 3 is uniform after ion oxidation, and the color of the coloring appearance is uniform, the surface texture of Comparative Example 2 is not uniform after ion oxidation, and the color of the coloring appearance is not uniform, the surface texture of Comparative Example 3 is locally not uniform after ion oxidation, and the color of the coloring appearance is locally not uniform, and the arrangement of coloring and oxidation degree is Example 1, Example 2 and Example 3 > Comparative Example 3 > Comparative Example 2. It is concluded that the aluminum alloy surface in example 1, example 2 and example 3 contains bromine, and in the ionization process, the aluminum alloy surface will form a cavity, and free bromide ions will also be produced, and the free bromide ions can be adsorbed on the cavity of the aluminum alloy material, improve the adsorption capacity of free metal ions, change the surface distribution of the aluminum alloy, make the aluminum alloy surface oxide film more easily form a cavity, increase the activity of the aluminum alloy, and the oxidation ability and the coloring efficiency are higher than those of the comparative example 2, and in the adding process, example 1, example 2 and example 3 adopt dropwise adding, while comparative example 3 adopts one-time adding, so that in the preparation process, the contact between the concentrated bromine water and the p-nitrophenol is not sufficient, so that the surface texture and the coloring appearance after oxidation produce local uneven phenomenon, therefore, it is necessary for the application to selectively add concentrated bromine water and adopt dropwise adding.

[0046] Finally, it should be noted that: the above only for the preferred embodiments of the present application, and not for limiting the present application, although the foregoing embodiments of the present application are described in detail, for those skilled in the art, it still can be modified, or equivalent replacement of part of the technical features described in the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. within the spirit and principles of the present application shall be included in the protection scope of the present application.

Claims

1. An easily oxidatively colorable aluminum alloy material, characterized by: The aluminum alloy material raw materials are as follows, by weight fraction, including aluminum alloy powder 20-25 parts, graphene 5-10 parts, p-nitrophenol 4-6 parts, concentrated bromine water 0.5-1 part, magnesium powder 4-7 parts.

2. A method of producing an easily oxidatively colorable aluminum alloy material, characterized by: The steps are as follows, (1) dissolve graphene into ice water, add concentrated sulfuric acid, stir at 500-600 r / min, add sodium nitrate and potassium permanganate, stir for 2-3 h, add hydrogen peroxide, stir for 30-60 min, filter to obtain composition A; (2) ultrasonic treatment is performed on composition A to dissolve it in anhydrous ethanol, add p-nitrophenol, stir at 500-600 r / min, add concentrated bromine water to obtain composition B; (3) add aluminum alloy powder into acetone solution, stir at 500-600 r / min, stir for 20-30 min to obtain composition C; (4) mix composition B with composition C, disperse by mechanical grinding to obtain dispersion liquid A; (5) add magnesium powder into dispersion liquid A, add in 3 times, stir at 500-600 r / min, disperse until uniform; (6) filter dispersion liquid A, rinse with deionized water for 3 times to obtain filter cake, put the filter cake into an inert gas drying box, dry for 1-2 h, after drying, put into a stainless steel mold; (7) put the stainless steel mold containing the product into a vacuum hot press, vacuumize, heat up to 200-300℃, control the heating rate, pressurize, pressure 50-60 MPa, keep temperature and pressure for 3-5 h, start cooling; (8) cool down the furnace, slowly cool down, take out the mold, take out the product to obtain the aluminum alloy material.

3. The method of claim 2, wherein the aluminum alloy material is prepared by the steps of: The reaction temperature in steps (2) to (4) is kept at 20-25℃. ​ 4. The method of claim 2, wherein the aluminum alloy material is prepared by the steps of: In step (5), the magnesium powder is added in 3 times, 1 / 6 of the total fraction in the first time, 1 / 3 of the total fraction in the second time, and 1 / 2 of the total fraction in the third time. ​ 5. The method of claim 2, wherein the aluminum alloy material is prepared by the steps of: In step (6), the temperature of the drying box is 150-250℃, and the inert gas is argon or xenon. ​ 6. The method of claim 2, wherein the aluminum alloy material is prepared by the steps of: In step (7), vacuumize, vacuum degree 10-20 KPa, control the heating rate at 30-50℃ / h. ​ 7. The method of claim 2, wherein the aluminum alloy material is prepared by the steps of: In step (8), control the cooling rate when cooling down, keep the cooling rate at 50-60℃ / h. ​ 8. The method of claim 2, wherein the method further comprises: In step (6), the filter screen is selected to be 30-50 μm. ​

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