CN112899686A - Preparation method of super-hydrophobic aluminum-magnesium alloy material - Google Patents
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- 239000000956 alloy Substances 0.000 title claims abstract description 50
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 46
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 37
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 37
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 238000007670 refining Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 238000007872 degassing Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000011068 loading method Methods 0.000 claims abstract description 8
- 230000010355 oscillation Effects 0.000 claims abstract description 8
- 238000003892 spreading Methods 0.000 claims abstract description 8
- 230000007480 spreading Effects 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 14
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 14
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 14
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 239000000919 ceramic Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 7
- 239000001103 potassium chloride Substances 0.000 claims description 7
- 235000011164 potassium chloride Nutrition 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 239000011592 zinc chloride Substances 0.000 claims description 7
- 235000005074 zinc chloride Nutrition 0.000 claims description 7
- 238000000643 oven drying Methods 0.000 claims description 2
- 238000009832 plasma treatment Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 239000000843 powder Substances 0.000 abstract 2
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 238000002791 soaking Methods 0.000 description 6
- 238000005096 rolling process Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 240000002853 Nelumbo nucifera Species 0.000 description 2
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 2
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910018134 Al-Mg Inorganic materials 0.000 description 1
- 229910018467 Al—Mg Inorganic materials 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000010336 energy treatment Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- XPBBUZJBQWWFFJ-UHFFFAOYSA-N fluorosilane Chemical compound [SiH3]F XPBBUZJBQWWFFJ-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/20—Acidic compositions for etching aluminium or alloys thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- 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
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- 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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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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
- C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
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Abstract
The invention provides a preparation method of a super-hydrophobic aluminum magnesium alloy material. The preparation steps are as follows: respectively carrying out thermal oxidation on the aluminum magnesium powder to obtain oxidized aluminum magnesium powder; loading the oxidized aluminum powder into a crucible, and heating the crucible along with a resistance furnace to completely melt the aluminum powder; adding magnesium powder into a crucible until the magnesium powder is completely melted, and then degassing and refining; after refining, standing, and pouring the alloy liquid into an aluminum-magnesium alloy material; sequentially carrying out ultrasonic oscillation cleaning on the aluminum-magnesium alloy material by using acetone and deionized water, and then immersing the aluminum-magnesium alloy material into a hydrofluoric acid solution for treatment; taking out, washing with deionized water, drying, and spreading on an earth electrode in a low-temperature plasma treatment device for treatment; taking out, putting into an oven under a humid condition, and treating at high temperature. The super-hydrophobic aluminum-magnesium alloy prepared by the invention has good super-hydrophobic performance, and has very high application value on clean surfaces of satellite antennas and radars, surfaces of aviation materials and automobile shells and the like.
Description
Technical Field
The invention relates to the field of alloy materials, in particular to a preparation method of a super-hydrophobic aluminum-magnesium alloy material.
Background
Surface wettability is an important property of a solid and is one of the important features of a solid surface, which is determined by the chemical composition and the micro-geometry of the surface. In recent years, researchers have paid high attention to the study of the wettability of superhydrophobic surfaces and solids. By superhydrophobic surface is generally meant a surface having a contact angle greater than 150 °. The contact angle and the rolling angle of a water drop on the surface of the lotus leaf are 161.0 degrees and 2 degrees respectively, and the phenomenon is caused because the lotus leaf has a special surface micro-nano composite structure.
The super-hydrophobic surface has extremely wide application prospect in industrial and agricultural production and daily life of people: such as clean surfaces of satellite antennas and radars, drag reduction materials of submarine water bodies, pipe wall modification in the field of petrochemical industry and the like, and has very high application value. The preparation of superhydrophobic surfaces can be started from two aspects: on one hand, the low surface energy substance is modified on the rough surface; another aspect is the building of a rough structure on the surface of the hydrophobic material. However, on smooth surfaces only by changing the surface energy, the contact angle can typically only be increased up to 120 °, whereas the contact angle of a surface with fine roughness can exceed 150 °. Much research is now focused on how to form suitable roughness structures on the surface.
At present, there are many reports on methods for producing a rough surface, such as: sol-gel methods, vapor deposition methods, electrochemical methods, nanotube array methods, and the like. However, most of these methods require a special apparatus or control of a complicated experimental process. Therefore, it is important to develop a method which is simple in operation process, easy to control the reaction, and does not require large-scale equipment.
Disclosure of Invention
The technical problem to be solved is as follows: the invention aims to provide a preparation method of a super-hydrophobic aluminum-magnesium alloy material, and the prepared super-hydrophobic aluminum-magnesium alloy material has good super-hydrophobic performance and very high application value on clean surfaces of satellite antennas and radars, surfaces of aviation materials and automobile shells and the like.
The technical scheme is as follows: a preparation method of a super-hydrophobic aluminum magnesium alloy material comprises the following steps:
step 1: respectively placing aluminum powder and magnesium powder with the total weight of 100g in an evaporating dish, flatly paving, placing in a drying box at 75 ℃, and oxidizing for 10-24h in a normal-pressure air environment to obtain oxidized aluminum powder and magnesium powder;
step 2: loading oxidized aluminum powder into a crucible, heating the crucible along with a resistance furnace, and scattering a layer of covering agent consisting of potassium chloride and magnesium chloride on the liquid surface after the aluminum powder is completely melted;
and step 3: adding magnesium powder into the crucible in the step 2 until the magnesium powder is completely melted, and then adding aluminum chloride or zinc chloride for degassing and refining;
and 4, step 4: after refining, standing, filtering the alloy liquid through a porous ceramic plate twice, and pouring into an aluminum magnesium alloy material;
and 5: sequentially carrying out ultrasonic oscillation cleaning on the aluminum-magnesium alloy material by using acetone and deionized water, and then immersing the aluminum-magnesium alloy material into a hydrofluoric acid solution for treatment for 10 min;
step 6: taking out, washing with deionized water, oven drying, spreading on an earth electrode in a low temperature plasma processing device, and processing for 10-15 min;
and 7: taking out, placing into an oven under humid condition, and treating at high temperature for 5-8 min.
Further, the mass ratio of the aluminum powder to the magnesium powder in the step 1 is 1-8: 1.
Further, the concentration of the hydrofluoric acid solution in the step 5 is 3.75 mol/L.
Further, the processing conditions in the step 6 are as follows: the power frequency is 10-15kHz, the working voltage is 20kV, and the discharge power is 70-80W.
Further, the temperature of the oven in the step 7 is 140-.
Has the advantages that:
1. according to the invention, the super-hydrophobic surface can be prepared on the aluminum-magnesium alloy substrate through simple etching and high-temperature treatment, and the preparation method is simple and efficient.
2. The aluminum-magnesium alloy is treated by hydrofluoric acid solution and low-temperature plasma to form a surface structure with a micron-scale coarse structure, and then is oxidized at high temperature to generate related oxides, so that a nano structure is constructed again on the basis of the prior art, and a micro-nano dual-composite coarse structure is constructed.
3. The method of the invention does not have the step of low surface energy treatment, can save resources and simultaneously improve the processing technology and the processing effect.
4. The contact angle of the super-hydrophobic aluminum-magnesium alloy is higher than 165 degrees, the rolling angle is lower than 5 degrees, the contact angle of the embodiment 3 is 168.3 degrees at most, and the super-hydrophobic aluminum-magnesium alloy has good super-hydrophobic performance.
Drawings
FIG. 1 shows droplets on the surface of a superhydrophobic aluminum-magnesium alloy, which are observed by a video optical contact angle measuring instrument in example 3.
Detailed Description
Example 1
A preparation method of a super-hydrophobic aluminum magnesium alloy material comprises the following steps:
step 1: respectively placing aluminum powder and magnesium powder with the total weight of 100g in an evaporating dish, flatly paving, placing in a drying box at 75 ℃, and oxidizing for 10 hours in a normal-pressure air environment to obtain oxidized aluminum powder and magnesium powder, wherein the mass ratio of the aluminum powder to the magnesium powder is 1: 1;
step 2: loading oxidized aluminum powder into a crucible, heating the crucible along with a resistance furnace, and scattering a layer of covering agent consisting of potassium chloride and magnesium chloride on the liquid surface after the aluminum powder is completely melted;
and step 3: adding magnesium powder into a crucible until the magnesium powder is completely melted, and then adding aluminum chloride or zinc chloride for degassing and refining;
and 4, step 4: after refining, standing, filtering the alloy liquid through a porous ceramic plate twice, and pouring into an aluminum magnesium alloy material;
and 5: sequentially carrying out ultrasonic oscillation cleaning on the aluminum-magnesium alloy material by using acetone and deionized water, and then soaking the aluminum-magnesium alloy material into a hydrofluoric acid solution with the concentration of 3.75 mol/L for treatment for 10 min;
step 6: taking out, washing with deionized water, drying, spreading on an earth electrode in a low-temperature plasma treatment device, and treating for 10min at a power frequency of 10kHz, a working voltage of 20kV and a discharge power of 70W;
and 7: taking out, placing into a 140 deg.C oven under humid condition, and treating at high temperature for 5 min.
Example 2
A preparation method of a super-hydrophobic aluminum magnesium alloy material comprises the following steps:
step 1: respectively placing aluminum powder and magnesium powder with the total weight of 100g in an evaporating dish, flatly paving, placing in a drying box at 75 ℃, and oxidizing for 14h in a normal-pressure air environment to obtain oxidized aluminum powder and magnesium powder, wherein the mass ratio of the aluminum powder to the magnesium powder is 3: 1;
step 2: loading oxidized aluminum powder into a crucible, heating the crucible along with a resistance furnace, and scattering a layer of covering agent consisting of potassium chloride and magnesium chloride on the liquid surface after the aluminum powder is completely melted;
and step 3: adding magnesium powder into a crucible until the magnesium powder is completely melted, and then adding aluminum chloride or zinc chloride for degassing and refining;
and 4, step 4: after refining, standing, filtering the alloy liquid through a porous ceramic plate twice, and pouring into an aluminum magnesium alloy material;
and 5: sequentially carrying out ultrasonic oscillation cleaning on the aluminum-magnesium alloy material by using acetone and deionized water, and then soaking the aluminum-magnesium alloy material into a hydrofluoric acid solution with the concentration of 3.75 mol/L for treatment for 10 min;
step 6: taking out, washing with deionized water, drying, spreading on an earth electrode in a low-temperature plasma treatment device, and treating for 12min under the conditions of power frequency of 12kHz, working voltage of 20kV and discharge power of 75W;
and 7: taking out, placing in oven at 145 deg.C under humid condition, and treating at high temperature for 6 min.
Example 3
A preparation method of a super-hydrophobic aluminum magnesium alloy material comprises the following steps:
step 1: respectively placing aluminum powder and magnesium powder with the total weight of 100g in an evaporating dish, flatly paving, placing in a drying box at 75 ℃, and oxidizing for 18h in a normal-pressure air environment to obtain oxidized aluminum powder and magnesium powder, wherein the mass ratio of the aluminum powder to the magnesium powder is 5: 1;
step 2: loading oxidized aluminum powder into a crucible, heating the crucible along with a resistance furnace, and scattering a layer of covering agent consisting of potassium chloride and magnesium chloride on the liquid surface after the aluminum powder is completely melted;
and step 3: adding magnesium powder into a crucible until the magnesium powder is completely melted, and then adding aluminum chloride or zinc chloride for degassing and refining;
and 4, step 4: after refining, standing, filtering the alloy liquid through a porous ceramic plate twice, and pouring into an aluminum magnesium alloy material;
and 5: sequentially carrying out ultrasonic oscillation cleaning on the aluminum-magnesium alloy material by using acetone and deionized water, and then soaking the aluminum-magnesium alloy material into a hydrofluoric acid solution with the concentration of 3.75 mol/L for treatment for 10 min;
step 6: taking out, washing with deionized water, drying, spreading on an earth electrode in a low-temperature plasma treatment device, and treating for 14min at a power frequency of 14kHz, a working voltage of 20kV and a discharge power of 75W;
and 7: taking out, placing in oven at 145 deg.C under humid condition, and treating at high temperature for 7 min.
Example 4
A preparation method of a super-hydrophobic aluminum magnesium alloy material comprises the following steps:
step 1: respectively placing aluminum powder and magnesium powder with the total weight of 100g in an evaporating dish, flatly paving, placing in a drying box at 75 ℃, and oxidizing for 24 hours in a normal-pressure air environment to obtain oxidized aluminum powder and magnesium powder, wherein the mass ratio of the aluminum powder to the magnesium powder is 8: 1;
step 2: loading oxidized aluminum powder into a crucible, heating the crucible along with a resistance furnace, and scattering a layer of covering agent consisting of potassium chloride and magnesium chloride on the liquid surface after the aluminum powder is completely melted;
and step 3: adding magnesium powder into a crucible until the magnesium powder is completely melted, and then adding aluminum chloride or zinc chloride for degassing and refining;
and 4, step 4: after refining, standing, filtering the alloy liquid through a porous ceramic plate twice, and pouring into an aluminum magnesium alloy material;
and 5: sequentially carrying out ultrasonic oscillation cleaning on the aluminum-magnesium alloy material by using acetone and deionized water, and then soaking the aluminum-magnesium alloy material into a hydrofluoric acid solution with the concentration of 3.75 mol/L for treatment for 10 min;
step 6: taking out, washing with deionized water, drying, spreading on an earth electrode in a low-temperature plasma treatment device, and treating for 15min under the conditions of power frequency of 15kHz, working voltage of 20kV and discharge power of 80W;
and 7: taking out, placing in a 150 deg.C oven under humid condition, and treating at high temperature for 8 min.
Comparative example 1
A preparation method of a super-hydrophobic aluminum magnesium alloy material comprises the following steps:
step 1: respectively placing aluminum powder and magnesium powder with the total weight of 100g in an evaporating dish, flatly paving, placing in a drying box at 75 ℃, and oxidizing for 10 hours in a normal-pressure air environment to obtain oxidized aluminum powder and magnesium powder, wherein the mass ratio of the aluminum powder to the magnesium powder is 1: 1;
step 2: loading oxidized aluminum powder into a crucible, heating the crucible along with a resistance furnace, and scattering a layer of covering agent consisting of potassium chloride and magnesium chloride on the liquid surface after the aluminum powder is completely melted;
and step 3: adding magnesium powder into a crucible until the magnesium powder is completely melted, and then adding aluminum chloride or zinc chloride for degassing and refining;
and 4, step 4: after refining, standing, filtering the alloy liquid through a porous ceramic plate twice, and pouring into an aluminum magnesium alloy material;
and 5: sequentially carrying out ultrasonic oscillation cleaning on the aluminum-magnesium alloy material by using acetone and deionized water, and then soaking the aluminum-magnesium alloy material into a hydrofluoric acid solution with the concentration of 3.75 mol/L for treatment for 10 min;
step 6: taking out, washing with deionized water, drying, spreading on an earth electrode in a low-temperature plasma treatment device, and treating for 10min at a power frequency of 10kHz, a working voltage of 20kV and a discharge power of 70W;
and 7: taking out, placing into prepared 1.0wt% fluorosilane ethanol solution, soaking for 30 min, then placing into a drying oven, and drying at 120 deg.C.
The contact angle is measured by adopting an OCA20 video optical contact angle measuring instrument, the water drop used in the measurement is 5 mu L, the average value of the measurement is obtained at 5 different positions, the advancing contact angle and the retreating contact angle are measured by a method for increasing or reducing the volume of the water drop, and the change rate of the volume of the water drop is 2.0 mu L/s.
TABLE 1 contact and roll angles on the surface of Al-Mg alloys
As can be seen from Table 1, the contact angles of all the examples are higher than 165 degrees, higher than 150 degrees of the conventional superhydrophobic material, the rolling angles are lower than 5 degrees, the contact angle of the example 3 is at most 168.3 degrees, and the superhydrophobic performance is good.
Claims (5)
1. The preparation method of the super-hydrophobic aluminum-magnesium alloy material is characterized by comprising the following steps of:
step 1: respectively placing aluminum powder and magnesium powder with the total weight of 100g in an evaporating dish, flatly paving, placing in a drying box at 75 ℃, and oxidizing for 10-24h in a normal-pressure air environment to obtain oxidized aluminum powder and magnesium powder;
step 2: loading oxidized aluminum powder into a crucible, heating the crucible along with a resistance furnace, and scattering a layer of covering agent consisting of potassium chloride and magnesium chloride on the liquid surface after the aluminum powder is completely melted;
and step 3: adding magnesium powder into the crucible in the step 2 until the magnesium powder is completely melted, and then adding aluminum chloride or zinc chloride for degassing and refining;
and 4, step 4: after refining, standing, filtering the alloy liquid through a porous ceramic plate twice, and pouring into an aluminum magnesium alloy material;
and 5: sequentially carrying out ultrasonic oscillation cleaning on the aluminum-magnesium alloy material by using acetone and deionized water, and then immersing the aluminum-magnesium alloy material into a hydrofluoric acid solution for treatment for 10 min;
step 6: taking out, washing with deionized water, oven drying, spreading on an earth electrode in a low temperature plasma processing device, and processing for 10-15 min;
and 7: taking out, placing into an oven under humid condition, and treating at high temperature for 5-8 min.
2. The method for preparing the superhydrophobic aluminum-magnesium alloy material according to claim 1, wherein the mass ratio of the aluminum powder to the magnesium powder in the step 1 is 1-8: 1.
3. The method for preparing a superhydrophobic aluminum magnesium alloy material according to claim 1, wherein the concentration of the hydrofluoric acid solution in the step 5 is 3.75 mol/L.
4. The method for preparing the superhydrophobic aluminum magnesium alloy material according to claim 1, wherein the treatment conditions in the step 6 are as follows: the power frequency is 10-15kHz, the working voltage is 20kV, and the discharge power is 70-80W.
5. The method as claimed in claim 1, wherein the oven temperature in step 7 is 140-150 ℃.
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|---|---|---|---|---|
| CN117531045A (en) * | 2024-01-04 | 2024-02-09 | 华融科创生物科技（天津）有限公司 | Preparation method of composite coating on magnesium alloy surface and biomedical implant magnesium alloy |
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