CN110670069A - Method for improving hydrophobic corrosion resistance of aluminum alloy surface - Google Patents
Method for improving hydrophobic corrosion resistance of aluminum alloy surface Download PDFInfo
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Abstract
The invention discloses a method for improving the hydrophobic corrosion-resistant performance of an aluminum alloy surface, and particularly relates to the technical field of aluminum alloys. The surface of the self-made aluminum-aluminum oxide composite fiber contains hydroxyl, and the hydroxyl can be subjected to esterification reaction with hydroxyl in dodecanedioic acid, and simultaneously the residual carboxyl is grafted to the surface of the aluminum alloy, so that the aluminum-aluminum oxide composite fiber is introduced to the surface of the aluminum alloy, and after high-temperature calcination at the temperature of 570-580 ℃, aluminum powder is softened to play a role in adhesion, so that the aluminum-aluminum oxide composite fiber is firmly adhered to the surface of the aluminum alloy, the corrosion resistance of the surface of the aluminum alloy is greatly improved, and meanwhile, the formed uniform micro-pit surface and the ester group exist, so that the hydrophobic property of the surface of the aluminum alloy is greatly improved.
Description
Technical Field
The invention belongs to the technical field of aluminum alloy, and particularly relates to a method for improving the hydrophobic corrosion resistance of the surface of aluminum alloy.
Background
Aluminum alloys are the most widely used class of non-ferrous materials in industry and are used in large numbers in the aerospace, automotive, mechanical manufacturing, and chemical industries. With the rapid development of science and technology and industrial economy, the demand on the performance of aluminum alloy materials is increasing day by day. The super-hydrophobic surface is a surface with a contact angle with water of more than 150 degrees and a rolling angle of less than 10 degrees, and the super-hydrophobic functional surface is constructed on an aluminum alloy material and can be widely applied to the scientific research and industrial fields of self-cleaning, ice coating prevention, oil-water separation, corrosion prevention, drag reduction, transportation increase and the like.
Patent publication No. CN109680252A discloses a hydrophobic aluminum alloy composite material, an epoxy resin protective layer is coated on an aluminum alloy substrate layer, and a first molybdenum disulfide layer, a first silicon dioxide layer, a second molybdenum disulfide layer, a second silicon dioxide layer, a third molybdenum disulfide layer and a third silicon dioxide layer are deposited on the epoxy resin protective layer in sequence.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a method for improving the hydrophobic corrosion resistance of the surface of the aluminum alloy.
The invention is realized by the following technical scheme:
a method for improving the hydrophobic corrosion resistance of the surface of an aluminum alloy specifically comprises the following steps:
(1) cutting aluminum alloy into the size of 20mm multiplied by 10mm multiplied by 2mm, then adding the aluminum alloy into acetone, heating to boil, carrying out reflux treatment for 1-2h, then cooling and taking out the aluminum alloy, adding the aluminum alloy into deionized water, heating and refluxing for 2-4h again, cooling and taking out; acetone and deionized water are utilized to carry out reflux treatment on the aluminum alloy, so that not only can grease on the surface of the aluminum alloy be thoroughly taken out, but also the surface of the aluminum alloy can be roughened preliminarily, and hydroxyl groups can be grafted on the surface of the aluminum alloy, so that subsequent esterification reaction of dodecanedioic acid and the dodecanedioic acid is facilitated, and the grafting purpose is achieved;
(2) adding the aluminum alloy obtained in the step (1) into the modified material, heating to 82-85 ℃, stirring at 200rpm of 100-.
Further, the preparation method of the modified material in the step (2) comprises the following steps:
(1) dissolving 50-60 parts by weight of polyvinyl alcohol in distilled water with the volume 10-15 times of that of the polyvinyl alcohol, stirring for 30-35min at 91-93 ℃ and 140rpm of 120-;
(2) spinning the spinning solution obtained in the step (1) by an electrostatic spinning method, and shearing and spinning the spinning solution to a size of 1-3 microns to obtain spinning fibers;
(3) transferring the spinning fiber obtained in the step (2) into a vacuum drying box, drying at 60-70 ℃ for 3-4h, then transferring into a resistance furnace, roasting at 580-590 ℃ for 2-3h, then roasting at 635-642 ℃ for 1-2h, then cooling to room temperature at the rate of 3-5 ℃/min, soaking for 2-3h by using deionized water, filtering, and drying to obtain the aluminum-aluminum oxide composite fiber;
(4) adding 30-50 parts of the aluminum-aluminum oxide composite fiber obtained in the step (3) into ethanol with the volume 5-8 times of that of the aluminum-aluminum oxide composite fiber, dispersing for 20-30min under the ultrasonic condition of 50-55KHz, then adding 30-50 parts of dodecanedioic acid, heating to 70-80 ℃, and reacting for 3-4h under 200-300rpm to obtain the modified material. The preparation method comprises the steps of carrying out a cross-linking reaction on polyvinyl alcohol and sodium alginate to prepare a spinning solution, wherein the spinning solution comprises aluminum powder and aluminum nitrate, converting the aluminum nitrate into aluminum hydroxide to be attached to the surface of the aluminum powder under the action of ammonia water, spinning the aluminum hydroxide into fibers, calcining the fibers at high temperature to form aluminum-aluminum oxide composite fibers, wherein the surfaces of the aluminum-aluminum oxide composite fibers contain hydroxyl groups, the hydroxyl groups can be subjected to an esterification reaction with hydroxyl groups in dodecanedioic acid, and simultaneously the remaining carboxyl groups are grafted to the surface of aluminum alloy, so that the aluminum-aluminum oxide composite fibers are introduced to the surface of the aluminum alloy, and after the aluminum-aluminum oxide composite fibers are calcined at high temperature of 570-580 ℃, the aluminum powder is softened to play.
Further, the specific spinning process parameters in the step (2) are as follows: the direct current voltage is 18-25kV, the receiving distance is 15-18cm, the relative humidity is 52-55%, and the spinning supply rate is 1.5-1.8 ml/h.
The invention has the beneficial effects that: the method provided by the embodiment of the invention can improve the water contact angle to a greater extent, and ensure that the rolling angle is less than or equal to 5 degrees, so that the surface of the aluminum alloy is super-hydrophobic, and meanwhile, the corrosion resistance of the aluminum alloy is obviously improved. According to the invention, acetone and deionized water are firstly utilized to carry out reflux treatment on the aluminum alloy, so that not only can grease on the surface of the aluminum alloy be thoroughly taken out, but also the surface of the aluminum alloy can be roughened preliminarily, and hydroxyl groups can be grafted on the surface of the aluminum alloy, thereby facilitating the subsequent esterification reaction of dodecanedioic acid and the aluminum alloy, and achieving the grafting purpose; the polyvinyl alcohol and the sodium alginate are subjected to cross-linking reaction to prepare spinning solution, wherein the spinning solution comprises aluminum powder and aluminum nitrate, under the action of ammonia water, aluminum nitrate is converted into aluminum hydroxide to be attached to the surface of aluminum powder, then the aluminum hydroxide is spun into fiber shape, the fiber shape is calcined at high temperature to form aluminum-aluminum oxide composite fiber, the surface of the fiber contains hydroxyl which can be esterified with the hydroxyl in the dodecanedioic acid, and the residual carboxyl is grafted to the surface of the aluminum alloy, so that the aluminum-aluminum oxide composite fiber is introduced to the surface of the aluminum alloy, after high-temperature calcination at the temperature of 570-580 ℃, the aluminum powder is softened to play a role in adhesion, and the aluminum-alumina composite fiber is firmly adhered to the surface of the aluminum alloy, so that the corrosion resistance of the surface of the aluminum alloy is greatly improved, and simultaneously, the surface of the formed uniform micro-pits and the existence of ester groups greatly improve the hydrophobic property of the surface of the aluminum alloy.
Detailed Description
The invention is illustrated by the following specific examples, which are not intended to be limiting.
Example 1
A method for improving the hydrophobic corrosion resistance of the surface of an aluminum alloy specifically comprises the following steps:
(1) cutting aluminum alloy into the size of 20mm multiplied by 10mm multiplied by 2mm, then adding the aluminum alloy into acetone, heating to boil, carrying out reflux treatment for 1h, then cooling and taking out the aluminum alloy, adding the aluminum alloy into deionized water, heating again and refluxing for 2h, cooling and taking out;
(2) adding the aluminum alloy obtained in the step (1) into the modified material, heating to 82 ℃, stirring at 100rpm for reaction for 5h, taking out, putting the obtained aluminum alloy into a roasting furnace preheated to 60 ℃, introducing nitrogen for protection, heating to 570 ℃ at 3 ℃/min, keeping for 5min, reducing to 250 ℃ at the speed of 6 ℃/min, taking out, quickly putting into water for quenching, continuing to put back into the roasting furnace, cooling from 250 ℃, taking out again for quenching when the temperature is reduced to 150 ℃, then putting back into the roasting furnace again, and continuing to reduce to room temperature.
Further, the preparation method of the modified material in the step (2) comprises the following steps:
(1) dissolving 50 parts by weight of polyvinyl alcohol in distilled water with the volume being 10 times of that of the polyvinyl alcohol, stirring the solution at 91 ℃ and 120rpm for 30min, then adding 10 parts of aluminum powder and 20 parts of aluminum nitrate solution with the concentration being 1mol/L, continuously stirring the solution for 20min, cooling the solution to 50 ℃, adding 20 parts of sodium alginate, reacting the solution for 2h at 200rpm, dropwise adding saturated ammonia water solution into the solution while stirring the solution until no precipitate is generated, stopping dropwise adding ammonia water, and continuously stirring the solution for 2h to obtain spinning solution;
(2) spinning the spinning solution obtained in the step (1) by an electrostatic spinning method, and shearing and spinning the spinning solution to a size of 1-3 microns to obtain spinning fibers;
(3) transferring the spinning fiber obtained in the step (2) into a vacuum drying oven, drying at 60 ℃ for 3h, then transferring into a resistance furnace, roasting at 580 ℃ for 2h, then roasting at 635 ℃ for 1h, then cooling to room temperature at the speed of 3 ℃/min, soaking for 2h by using deionized water, filtering, and drying to obtain the aluminum-aluminum oxide composite fiber;
(4) and (3) adding 30 parts of the aluminum-aluminum oxide composite fiber obtained in the step (3) into ethanol with the volume 5 times that of the aluminum-aluminum oxide composite fiber, dispersing for 20min under the ultrasonic condition of 50KHz, then adding 30 parts of dodecanedioic acid, heating to 70-80 ℃, and reacting for 3h at 200rpm to obtain the modified material.
Further, the specific spinning process parameters in the step (2) are as follows: the DC voltage was 18kV, the take-up distance was 15cm, the relative humidity was 52%, and the spinning feed rate was 1.5 ml/h.
And (3) performance testing: according to tests, the contact angle of the sample obtained in the embodiment is 158 degrees, the rolling angle is 4 degrees, and the maximum corrosion depth is 87 micrometers through an intergranular corrosion test.
Example 2
A method for improving the hydrophobic corrosion resistance of the surface of an aluminum alloy specifically comprises the following steps:
(1) cutting aluminum alloy into the size of 20mm multiplied by 10mm multiplied by 2mm, then adding the aluminum alloy into acetone, heating to boil, carrying out reflux treatment for 2 hours, then cooling and taking out the aluminum alloy, adding the aluminum alloy into deionized water, heating again and refluxing for 3 hours, cooling and taking out;
(2) adding the aluminum alloy obtained in the step (1) into the modified material, heating to 84 ℃, stirring at 150rpm for reaction for 6h, taking out, putting the obtained aluminum alloy into a roasting furnace preheated to 65 ℃, introducing nitrogen for protection, heating to 575 ℃ at 4 ℃/min, keeping for 6min, reducing to 255 ℃ at the speed of 8 ℃/min, taking out, rapidly putting into water for quenching, continuing to put back into the roasting furnace, cooling from 255 ℃, taking out again for quenching when the temperature is reduced to 153 ℃, then putting back into the roasting furnace again, and continuing to reduce to room temperature.
Further, the preparation method of the modified material in the step (2) comprises the following steps:
(1) dissolving 55 parts by weight of polyvinyl alcohol in distilled water with the volume being 12 times of that of the polyvinyl alcohol, stirring at 92 ℃ and 130rpm for 32min, then adding 13 parts of aluminum powder and 25 parts of aluminum nitrate solution with the concentration being 1.1mol/L, continuously stirring for 25min, cooling to 55 ℃, adding 23 parts of sodium alginate, reacting at 210rpm for 3h, then dropwise adding saturated ammonia water solution while stirring until no precipitate is generated, stopping dropwise adding ammonia water, and continuously stirring for 3h to obtain spinning solution;
(2) spinning the spinning solution obtained in the step (1) by an electrostatic spinning method, and shearing and spinning the spinning solution to a size of 1-3 microns to obtain spinning fibers;
(3) transferring the spinning fiber obtained in the step (2) into a vacuum drying oven, drying at 65 ℃ for 4h, then transferring into a resistance furnace, roasting at 585 ℃ for 2.5h, then roasting at 638 ℃ for 1.5h, then cooling to room temperature at the rate of 4 ℃/min, soaking for 2.5h by using deionized water, filtering, and drying to obtain the aluminum-aluminum oxide composite fiber;
(4) and (3) adding 40 parts of the aluminum-aluminum oxide composite fiber obtained in the step (3) into ethanol with the volume 7 times that of the aluminum-aluminum oxide composite fiber, dispersing for 25min under the ultrasonic condition of 53KHz, then adding 40 parts of dodecanedioic acid, heating to 75 ℃, and reacting for 4h at 250rpm to obtain the modified material.
Further, the specific spinning process parameters in the step (2) are as follows: the DC voltage was 22kV, the take-up distance was 17cm, the relative humidity was 54%, and the spinning feed rate was 1.6 ml/h.
And (3) performance testing: according to the test, the contact angle of the sample obtained in the embodiment is 159 degrees, the rolling angle is 4 degrees, and the maximum corrosion depth is 86 μm through the intergranular corrosion test.
Example 3
A method for improving the hydrophobic corrosion resistance of the surface of an aluminum alloy specifically comprises the following steps:
(1) cutting aluminum alloy into the size of 20mm multiplied by 10mm multiplied by 2mm, then adding the aluminum alloy into acetone, heating to boil, carrying out reflux treatment for 2 hours, then cooling and taking out the aluminum alloy, adding the aluminum alloy into deionized water, heating again and refluxing for 4 hours, cooling and taking out;
(2) adding the aluminum alloy obtained in the step (1) into the modified material, heating to 85 ℃, stirring at 200rpm for 8h, taking out, putting the aluminum alloy into a roasting furnace preheated to 70 ℃, introducing nitrogen for protection, heating to 580 ℃ at 5 ℃/min, keeping for 8min, reducing to 260 ℃ at the speed of 10 ℃/min, taking out, rapidly putting into water for quenching, continuing to put back into the roasting furnace, cooling from 260 ℃, taking out again for quenching when the temperature is reduced to 155 ℃, then putting back into the roasting furnace again, and continuing to reduce to room temperature.
Further, the preparation method of the modified material in the step (2) comprises the following steps:
(1) dissolving 60 parts by weight of polyvinyl alcohol in distilled water 15 times of the volume of the polyvinyl alcohol, stirring at 93 ℃ and 140rpm for 35min, then adding 15 parts of aluminum powder and 30 parts of aluminum nitrate solution with the concentration of 1.2mol/L, continuously stirring for 30min, cooling to 60 ℃, adding 25 parts of sodium alginate, reacting at 230rpm for 3h, then dropwise adding saturated ammonia water solution while stirring until no precipitate is generated, stopping dropwise adding ammonia water, and continuously stirring for 3h to obtain spinning solution;
(2) spinning the spinning solution obtained in the step (1) by an electrostatic spinning method, and shearing and spinning the spinning solution to a size of 1-3 microns to obtain spinning fibers;
(3) transferring the spinning fiber obtained in the step (2) into a vacuum drying oven, drying at 70 ℃ for 4h, then transferring into a resistance furnace, roasting at 590 ℃ for 3h, then roasting at 642 ℃ for 2h, then cooling to room temperature at the speed of 5 ℃/min, soaking for 3h by using deionized water, filtering, and drying to obtain the aluminum-aluminum oxide composite fiber;
(4) and (3) adding 50 parts of the aluminum-aluminum oxide composite fiber obtained in the step (3) into ethanol with the volume 8 times that of the aluminum-aluminum oxide composite fiber, dispersing for 30min under the ultrasonic condition of 55KHz, then adding 50 parts of dodecanedioic acid, heating to 80 ℃, and reacting for 4h at 300rpm to obtain the modified material.
Further, the specific spinning process parameters in the step (2) are as follows: the DC voltage was 25kV, the take-up distance was 18cm, the relative humidity was 55%, and the spinning feed rate was 1.8 ml/h.
And (3) performance testing: through tests, the contact angle of the sample obtained in the embodiment is 156 degrees, the rolling angle is 5 degrees, and the maximum corrosion depth is 88 μm through an intergranular corrosion test.
Comparative example 1
In this comparative example, the acetone heating reflux step and the deionized water heating reflux step of step (1) were omitted as compared with example 1, except that the steps were the same.
According to the test, the contact angle of the sample obtained in the comparative example is 135 degrees, the rolling angle is 9 degrees, and the maximum corrosion depth is 90 μm through the intergranular corrosion test.
Comparative example 2
In this comparative example, the procedure was the same as in example 1 except that the modifier was replaced with deionized water.
The contact angle and the rolling angle of the sample obtained in the comparative example are 124 degrees and 11 degrees respectively, and the maximum corrosion depth is 116 microns through an intergranular corrosion test.
Comparative example 3
In this comparative example, compared with example 1, the steps of the method are the same except that the addition of the aluminum-alumina composite fiber in the modifier is omitted.
According to the test, the contact angle of the sample obtained in the comparative example is 130 degrees, the rolling angle is 10 degrees, and the maximum corrosion depth is 114 μm through the intergranular corrosion test.
Comparative example 4
The procedure is the same as in example 1 except that the addition of dodecanedioic acid to the modifier is omitted.
According to the test, the contact angle of the sample obtained in the comparative example is 131 degrees, the rolling angle is 10 degrees, and the maximum corrosion depth is 102 μm through the intergranular corrosion test.
The test results of each group of examples and comparative examples are compared, so that the method provided by the embodiment of the invention can improve the water contact angle to a greater extent, and ensure that the rolling angle is less than or equal to 5 degrees, so that the surface of the aluminum alloy is super-hydrophobic, and meanwhile, the corrosion resistance of the aluminum alloy is obviously improved.
Note: the experimental specific conditions of the application are as follows:
contact angle test: the contact angle of a water drop on the surface of a test sample is measured by a contact angle goniometer (DSA 100, Kruss, Germany) at room temperature, and the measurement result is the average value of the contact angles of the water drop at five different points on the surface of the test sample.
And (3) rolling angle testing: placing a super-hydrophobic surface sample on a sample table of a contact angle measuring instrument (DSA 100, Kruss, Germany), dripping 5.0 mu L of water drops on the surface of the sample by using a micro-injector, and then inclining the sample table from 0 DEG, wherein the inclination angle when the water drops roll on the sample table is the rolling angle of the water drops on the super-hydrophobic surface. A photograph was taken with a digital camera to observe the contact angle of a water drop on the surface of the sample.
Intergranular corrosion test: the intergranular corrosion is carried out according to the GB/T7998-2005 standard, samples of the examples and the comparative examples with the same specification are hung in a corrosive liquid (40 g/L sodium chloride +6mol/L hydrogen peroxide and distilled water are added to 1L) and are completely immersed, the mutual contact between the samples and a container is prevented, the ratio of the surface area of the samples to the volume of the solution is less than 20 mm/ml, the corrosion is carried out at a constant temperature of 35 ℃, the corrosion time is 8h, then the samples are taken out, 5mm is removed from one end in the direction perpendicular to the main deformation direction, and the corrosion depth of the cut sections is observed under a metallographic microscope.
Claims (3)
1. The method for improving the hydrophobic corrosion resistance of the surface of the aluminum alloy is characterized by comprising the following steps:
(1) cutting aluminum alloy into the size of 20mm multiplied by 10mm multiplied by 2mm, then adding the aluminum alloy into acetone, heating to boil, carrying out reflux treatment for 1-2h, then cooling and taking out the aluminum alloy, adding the aluminum alloy into deionized water, heating and refluxing for 2-4h again, cooling and taking out;
(2) adding the aluminum alloy obtained in the step (1) into the modified material, heating to 82-85 ℃, stirring at 200rpm of 100-.
2. The method for improving the hydrophobic corrosion resistance of the surface of the aluminum alloy according to claim 1, wherein the modified material prepared in the step (2) is prepared by the following steps:
(1) dissolving 50-60 parts by weight of polyvinyl alcohol in distilled water with the volume 10-15 times of that of the polyvinyl alcohol, stirring for 30-35min at 91-93 ℃ and 140rpm of 120-;
(2) spinning the spinning solution obtained in the step (1) by an electrostatic spinning method, and shearing and spinning the spinning solution to a size of 1-3mm to obtain spinning fibers;
(3) transferring the spinning fiber obtained in the step (2) into a vacuum drying box, drying at 60-70 ℃ for 3-4h, then transferring into a resistance furnace, roasting at 580-590 ℃ for 2-3h, then roasting at 635-642 ℃ for 1-2h, then cooling to room temperature at the rate of 3-5 ℃/min, soaking for 2-3h by using deionized water, filtering, and drying to obtain the aluminum-aluminum oxide composite fiber;
(4) adding 30-50 parts of the aluminum-aluminum oxide composite fiber obtained in the step (3) into ethanol with the volume 5-8 times of that of the aluminum-aluminum oxide composite fiber, dispersing for 20-30min under the ultrasonic condition of 50-55KHz, then adding 30-50 parts of dodecanedioic acid, heating to 70-80 ℃, and reacting for 3-4h under 200-300rpm to obtain the modified material.
3. The method for improving the hydrophobic corrosion resistance of the surface of the aluminum alloy according to claim 2, wherein the specific spinning process parameters in the step (2) are as follows: the direct current voltage is 18-25kV, the receiving distance is 15-18cm, the relative humidity is 52-55%, and the spinning supply rate is 1.5-1.8 ml/h.
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| CN112501605A (en) * | 2020-12-01 | 2021-03-16 | 湖北超卓航空科技股份有限公司 | Preparation method of functional composite cold spray coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112501605A (en) * | 2020-12-01 | 2021-03-16 | 湖北超卓航空科技股份有限公司 | Preparation method of functional composite cold spray coating |
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