CN111690841B - Hard aluminum alloy and preparation method thereof - Google Patents

Hard aluminum alloy and preparation method thereof Download PDF

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CN111690841B
CN111690841B CN202010521197.9A CN202010521197A CN111690841B CN 111690841 B CN111690841 B CN 111690841B CN 202010521197 A CN202010521197 A CN 202010521197A CN 111690841 B CN111690841 B CN 111690841B
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aluminum alloy
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李虹
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Beijing Falcon Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/026—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/12—Anodising more than once, e.g. in different baths

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Abstract

The invention belongs to the field of materials, and discloses a hard aluminum alloy which is mainly prepared from aluminum, manganese, magnesium, chromium, calcium, titanium, zirconium and rare earth elements through smelting, extrusion forming and electrochemical oxidation treatment. The invention also discloses a preparation method of the hard aluminum alloy, and the hard aluminum alloy prepared by using manganese, magnesium, chromium, calcium, titanium, zirconium and rare earth elements in a matching way and carrying out smelting, extrusion forming and electrochemical oxidation treatment has strong mechanical property, ageing resistance, wear resistance, corrosion resistance and self-cleaning property.

Description

Hard aluminum alloy and preparation method thereof
Technical Field
The invention belongs to the field of materials, and particularly relates to a hard aluminum alloy and a preparation method thereof.
Background
The earth crust contains 8.3% of aluminum element, which is only lower than oxygen and silicon element, and the content of aluminum element is rich. Aluminum alloys made of aluminum, such as aluminum copper alloys, aluminum magnesium alloys, aluminum manganese alloys, and the like, have excellent electrical conductivity, thermal conductivity, ductility, and machinability, and are widely used in the fields of machinery, electronics, construction, and the like.
In the building industry, steel materials are most widely used, but because the steel materials are not anticorrosive, particularly, ferric trioxide is generated after the steel materials are contacted with oxygen, the corrosion speed of iron is accelerated, and an oxide film is formed on the surface of aluminum alloy, so that the aluminum alloy has certain corrosion resistance and is favored to a certain extent. However, with the improvement of living demands and living quality of people, new requirements are also provided for building materials, for example, for aluminum alloy materials used for doors, windows and decorations, the building materials need to have excellent mechanical properties and ageing resistance, and also need to have corrosion resistance and self-cleaning performance, but the aluminum alloy materials on the market at present cannot meet the requirements at the same time.
Therefore, it is highly desirable to provide a hard aluminum alloy with strong mechanical properties, aging resistance, corrosion resistance, and self-cleaning properties.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides the hard aluminum alloy which has strong mechanical property, ageing resistance, corrosion resistance and self-cleaning property.
A hard aluminium alloy is prepared from Al, Mn, Mg, Cr, Ca, Ti, Zr and rare-earth elements through smelting, extruding shaping and electrochemical oxidizing treatment.
The corrosion resistance, the mechanical property and the ageing resistance of the hard aluminum alloy material are improved by the matching use of manganese, magnesium, chromium, calcium, titanium, zirconium and rare earth elements; zirconium has high melting point, hardness and strength, and is easy to form an oxide film, so that the corrosion resistance and the mechanical property of the hard aluminum alloy material are improved; manganese increases hardenability and wear resistance, and separates oxidation from molten metal to carry away oxygen; the addition of the rare earth metal improves the mechanical property and the ageing resistance of the hard aluminum alloy material; the addition of titanium ensures that the alloy has high elongation, and comprehensively improves the performance of the whole hard alloy material.
Preferably, the hard aluminum alloy comprises the following raw materials in parts by weight:
Figure BDA0002532111510000021
further preferably, the hard aluminum alloy comprises the following raw materials in parts by weight:
Figure BDA0002532111510000022
preferably, the rare earth element is at least 3 of gadolinium (Gd), praseodymium (Pr), lanthanum (La), neodymium (Nd) and ytterbium (Yb).
More preferably, the rare earth elements are Gd, Pr, La and Nd; more preferably, the mass ratio of the rare earth elements Gd, Pr, La and Nd is 1:1:1: 1. When Gd, Pr, La and Nd are selected to be added into the aluminum alloy material, the coordination effect with manganese, magnesium, chromium, calcium, titanium and zirconium is better, and the improvement effect on the mechanical property and the aging resistance of the hard aluminum alloy material is great.
The preparation method of the hard aluminum alloy comprises the following steps:
(1) melting aluminum, manganese, magnesium, chromium, calcium, titanium, zirconium and rare earth elements to prepare a mixture A;
(2) extruding and forming the mixture A to obtain an aluminum alloy primary material;
(3) and carrying out electrochemical oxidation reaction on the aluminum alloy primary material to form an oxide film, thus obtaining the hard aluminum alloy.
Preferably, the temperature of the melting in step (1) is 800-.
Preferably, the two electrochemical oxidation processes comprise a primary electrochemical oxidation and a secondary electrochemical oxidation;
the process of the primary electrochemical oxidation comprises the following steps: the aluminum alloy initial material is put into H3PO4Anodizing in electrolyte composed of water solution and glycerol at 10-25 deg.C and 50-100V for 30-90min to obtain primary oxide; the process of the secondary electrochemical oxidation comprises the following steps: and putting the primary oxidation material into a sulfuric acid solution of 20-100g/L, and oxidizing for 30-90min under the voltage of 20-30V.
The prepared aluminum alloy primary material is subjected to twice electrochemical oxidation treatment, and H is adopted for the first electrochemical oxidation3PO4The solution is matched with glycerol to ensure that the surface of the material presents micropores of a highly ordered nano array, the micropores are vertical to the surface of the matrix, and the pores are parallel to each other; and (3) performing secondary electrochemical oxidation treatment, namely adopting a sulfuric acid solution as an electrolyte, further increasing the thickness of an oxide film, and complementing the efficacy of an inner layer film, and further improving the corrosion resistance, wear resistance and self-cleaning capability of the hard aluminum alloy material.
Preferably, said H3PO4The concentration of the aqueous solution is 0.5-1mol/L, and the H3PO4The volume ratio of the aqueous solution to the glycerol is (3-5) to 1.
Preferably, the thickness of the oxide film in step (3) is 50 to 300 μm.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, manganese, magnesium, chromium, calcium, titanium, zirconium and rare earth elements are used in a matching manner, and the hard aluminum alloy is prepared through smelting, extrusion forming and electrochemical oxidation treatment, and has the advantages of strong mechanical property, ageing resistance, wear resistance, corrosion resistance and self-cleaning property.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
Example 1
The hard aluminum alloy comprises the following raw materials in parts by weight:
Figure BDA0002532111510000031
Figure BDA0002532111510000041
a preparation method of hard aluminum alloy comprises the following steps:
(1) melting aluminum, manganese, magnesium, chromium, calcium, titanium, zirconium and rare earth elements at 850 ℃ to prepare a mixture A;
(2) transferring the mixture A into a hot extruder for hot extrusion molding to prepare an aluminum alloy primary material;
(3) polishing and brightening the aluminum alloy primary material, and cleaning by using ultrasonic waves; 400mL of 0.8mol/L H was taken3PO4Adding 100mL of glycerol into the aqueous solution to prepare electrolyte; then putting the cleaned aluminum alloy primary material into an electrolyte, and electrolyzing for 45min at 10-25 ℃ under 80V current for one time. After the electrolysis, cleaning, drying and secondary oxidation are carried out, and sulfuric acid solution with the mass concentration of 60g/L is used as electrolyte and oxidized for 45min under the voltage of 30V.
Example 2
The hard aluminum alloy comprises the following raw materials in parts by weight:
Figure BDA0002532111510000042
a preparation method of hard aluminum alloy comprises the following steps:
(1) melting aluminum, manganese, magnesium, chromium, calcium, titanium, zirconium and rare earth elements at 850 ℃ to prepare a mixture A;
(2) transferring the mixture A into a hot extruder for hot extrusion molding to prepare an aluminum alloy primary material;
(3) polishing and brightening the aluminum alloy primary material, and cleaning by using ultrasonic waves; 400mL of 0.8mol/L H was taken3PO4Adding 100mL of glycerol into the aqueous solution to prepare electrolyte; then putting the cleaned aluminum alloy primary material into an electrolyte, and electrolyzing for 45min at 10-25 ℃ under 80V current for one time. After the electrolysis, cleaning, drying and secondary oxidation are carried out, and sulfuric acid solution with the mass concentration of 60g/L is used as electrolyte and oxidized for 45min under the voltage of 30V.
Example 3
The hard aluminum alloy comprises the following raw materials in parts by weight:
Figure BDA0002532111510000051
a preparation method of hard aluminum alloy comprises the following steps:
(1) melting aluminum, manganese, magnesium, chromium, calcium, titanium, zirconium and rare earth elements at 850 ℃ to prepare a mixture A;
(2) transferring the mixture A into a hot extruder for hot extrusion molding to prepare an aluminum alloy primary material;
(3) polishing and brightening the aluminum alloy primary material, and cleaning by using ultrasonic waves; 400mL of 0.8mol/L H was taken3PO4Adding 100mL of glycerol into the aqueous solution to prepare electrolyte; then putting the cleaned aluminum alloy primary material into an electrolyte, and electrolyzing for 45min at 10-25 ℃ under 80V current for one time. After the electrolysis, cleaning, drying and secondary oxidation are carried out, and sulfuric acid solution with the mass concentration of 60g/L is used as electrolyte and oxidized for 45min under the voltage of 30V.
Example 4
The hard aluminum alloy comprises the following raw materials in parts by weight:
Figure BDA0002532111510000052
Figure BDA0002532111510000061
a preparation method of hard aluminum alloy comprises the following steps:
(1) melting aluminum, manganese, magnesium, chromium, calcium, titanium, zirconium and rare earth elements at 850 ℃ to prepare a mixture A;
(2) transferring the mixture A into a hot extruder for hot extrusion molding to prepare an aluminum alloy primary material;
(3) polishing and brightening the aluminum alloy primary material, and cleaning by using ultrasonic waves; 400mL of 0.8mol/L H was taken3PO4Adding 100mL of glycerol into the aqueous solution to prepare electrolyte; then putting the cleaned aluminum alloy primary material into an electrolyte, and electrolyzing for 45min at 10-25 ℃ under 80V current for one time. After the electrolysis, cleaning, drying and secondary oxidation are carried out, and sulfuric acid solution with the mass concentration of 60g/L is used as electrolyte and oxidized for 45min under the voltage of 30V.
Example 5
The hard aluminum alloy comprises the following raw materials in parts by weight:
Figure BDA0002532111510000062
a preparation method of hard aluminum alloy comprises the following steps:
(1) melting aluminum, manganese, magnesium, chromium, calcium, titanium, zirconium and rare earth elements at 850 ℃ to prepare a mixture A;
(2) transferring the mixture A into a hot extruder for hot extrusion molding to prepare an aluminum alloy primary material;
(3) polishing and brightening the aluminum alloy primary material, and cleaning by using ultrasonic waves; 400mL of 0.8mol/L H was taken3PO4Adding 100mL of glycerol into the aqueous solution to prepare electrolyte; then putting the cleaned aluminum alloy primary material into an electrolyte, and electrolyzing for 45min at 10-25 ℃ under 80V current for one time. After the electrolysis, cleaning, drying and secondary oxidation are carried out, and a sulfuric acid solution with the mass concentration of 60g/L is adopted as an electrolyte and is put under the voltage of 30VAnd (5) oxidizing for 45 min.
Example 6
The hard aluminum alloy comprises the following raw materials in parts by weight:
Figure BDA0002532111510000071
a preparation method of hard aluminum alloy comprises the following steps:
(1) melting aluminum, manganese, magnesium, chromium, calcium, titanium, zirconium and rare earth elements at 850 ℃ to prepare a mixture A;
(2) transferring the mixture A into a hot extruder for hot extrusion molding to prepare an aluminum alloy primary material;
(3) polishing and brightening the aluminum alloy primary material, and cleaning by using ultrasonic waves; 500mL of 0.6mol/L H was taken3PO4Adding 100mL of glycerol into the aqueous solution to prepare electrolyte; then putting the cleaned aluminum alloy primary material into an electrolyte, and electrolyzing for 60min at 10-25 ℃ under 50V current for one time. After the electrolysis, cleaning, drying and secondary oxidation are carried out, and a sulfuric acid solution with the mass concentration of 50g/L is used as an electrolyte and is oxidized for 60min under the voltage of 30V.
Comparative example 1
The hard aluminum alloy comprises the following raw materials in parts by weight:
Figure BDA0002532111510000072
a preparation method of hard aluminum alloy comprises the following steps:
(1) melting aluminum, manganese, magnesium, chromium, calcium, titanium and zirconium at 850 ℃ to obtain a mixture A;
(2) transferring the mixture A into a hot extruder for hot extrusion molding to prepare an aluminum alloy primary material;
(3) polishing and brightening the aluminum alloy primary material, and cleaning by using ultrasonic waves; 400mL of 0.8mol/L H was taken3PO4Adding 100mL of glycerol into the aqueous solution to prepare electrolyte; then putting the cleaned aluminum alloy primary material into electrolyte at 10-25 DEG CElectrolyzing for 45min at 80V. After the electrolysis, cleaning, drying and secondary oxidation are carried out, and sulfuric acid solution with the mass concentration of 60g/L is used as electrolyte and oxidized for 45min under the voltage of 30V.
Comparative example 2
The hard aluminum alloy comprises the following raw materials in parts by weight:
Figure BDA0002532111510000081
a preparation method of hard aluminum alloy comprises the following steps:
(1) melting aluminum, manganese, magnesium, chromium, calcium, titanium and rare earth elements at 850 ℃ to prepare a mixture A;
(2) transferring the mixture A into a hot extruder for hot extrusion molding to prepare an aluminum alloy primary material;
(3) polishing and brightening the aluminum alloy primary material, and cleaning by using ultrasonic waves; 400mL of 0.8mol/L H was taken3PO4Adding 100mL of glycerol into the aqueous solution to prepare electrolyte; then putting the cleaned aluminum alloy primary material into an electrolyte, and electrolyzing for 45min at 10-25 ℃ under 80V current for one time. After the electrolysis, cleaning, drying and secondary oxidation are carried out, and sulfuric acid solution with the mass concentration of 60g/L is used as electrolyte and oxidized for 45min under the voltage of 30V.
Comparative example 3
The hard aluminum alloy comprises the following raw materials in parts by weight:
Figure BDA0002532111510000082
Figure BDA0002532111510000091
a preparation method of hard aluminum alloy comprises the following steps:
(1) melting aluminum, manganese, magnesium, chromium, calcium, titanium, zirconium and rare earth elements at 850 ℃ to prepare a mixture A;
(2) transferring the mixture A into a hot extruder for hot extrusion molding to prepare an aluminum alloy primary material;
(3) polishing and brightening the aluminum alloy primary material, cleaning by using ultrasonic waves, and drying to obtain the aluminum alloy.
Product effectiveness testing
The hard aluminum alloys obtained in examples 1 to 6 and comparative examples 1 to 3 were subjected to performance tests mainly including the following tests:
1. xenon lamp aging test
And (3) testing conditions are as follows: wavelength of 420nm and irradiation intensity of 0.08W/m2And (4) irradiating.
2. Hardness (HV, Kg/mm)2)
The hardness of the oxide film layer was measured by means of an HV-1000 type microhardness tester with a test load of 100g and a loading time of 10 seconds.
3. Salt spray resistance time
And placing the sample in a NaCl solution with the mass fraction of 3% -5%, and observing the corrosion condition.
4. Abrasion resistance
The surface of No. 2000 abrasive paper is downwards placed on a super-hydrophobic aluminum sample, then 1.25kPa pressure is applied, the abrasive paper is dragged to move for 10cm on the sample along one direction, the sample is rotated for 90 degrees, the abrasive paper is continuously dragged for 10cm, and the 1 cycle is carried out for 5 cycles in total, and the movement distance is 1 m. The contact angle of the surface of the test piece is tested to evaluate the wear resistance.
5. Corrosion resistance
And respectively dropping a drop of 1mol/L hydrochloric acid and a 1mol/L sodium hydroxide solution on the surface of the sample to be measured, and observing the color change of the drop on the surface. The evaluation criteria for corrosion resistance were: the longer the time required for the droplets on the recording surface from the start of the droplet application to the time from yellow to green indicates better corrosion resistance of the film layer.
6. Self-cleaning performance
The carbon powder is taken as a pollution source and is paved on the surface of the aluminum alloy, and the covering state of the carbon powder on the surface is observed after water drops on the surface. The test results are shown in Table 1.
TABLE 1 results of performance test of hard aluminum alloys obtained in examples 1 to 6 and comparative examples 1 to 3
Figure BDA0002532111510000101
As can be seen from Table 1, the aluminum alloys obtained in examples 1 to 6 are significantly superior in performance to the aluminum alloys obtained in comparative examples 1 to 3.

Claims (7)

1. The hard aluminum alloy is characterized by being prepared by smelting, extrusion forming and electrochemical oxidation treatment of 40-80 parts of aluminum, 0.1-5 parts of manganese, 0.1-8 parts of magnesium, 0.1-3 parts of chromium, 0.1-3 parts of calcium, 0.1-5 parts of titanium, 0.1-2 parts of zirconium and 0.1-2 parts of rare earth elements; the rare earth elements are at least 3 of Gd, Pr, La, Nd and Yb.
2. The hard aluminum alloy according to claim 1, wherein the rare earth element is Gd, Pr, La, Nd.
3. The hard aluminum alloy according to claim 2, wherein the mass ratio of the rare earth elements Gd, Pr, La, Nd is 1:1: 1.
4. The method of making the hard aluminum alloy of any of claims 1-3, comprising the steps of:
(1) melting aluminum, manganese, magnesium, chromium, calcium, titanium, zirconium and rare earth elements to prepare a mixture A;
(2) extruding and forming the mixture A to obtain an aluminum alloy primary material;
(3) carrying out electrochemical oxidation treatment on the aluminum alloy primary material to form an oxide film, thus obtaining the hard aluminum alloy; the electrochemical oxidation treatment process in the step (3) comprises primary electrochemical oxidation and secondary electrochemical oxidation; the process of the primary electrochemical oxidation comprises the following steps: the aluminum alloy initial material is put into H3PO4Anodizing in electrolyte composed of water solution and glycerol at 10-25 deg.C and 50-100V for 30-90min to obtain primary oxide; the process of the secondary electrochemical oxidation comprises the following steps: will be one ofThe sub-oxidation material is put into a sulfuric acid solution with the concentration of 20-100g/L and oxidized for 30-90min under the voltage of 20-30V.
5. The method as claimed in claim 4, wherein the melting temperature in step (1) is 800-900 ℃.
6. The method of claim 4, wherein the H is3PO4The concentration of the aqueous solution is 0.5-1mol/L, and the H3PO4The volume ratio of the aqueous solution to the glycerol is (3-5) to 1.
7. The production method according to claim 4, wherein the thickness of the oxide film in the step (3) is 50 to 300 μm.
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JPH06330386A (en) * 1993-05-20 1994-11-29 Fujikura Ltd Formation of hard anodic oxide film and aluminum alloy for forming the film
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