CN114134469A - Aluminum alloy target material for photovoltaic reflective film and preparation method thereof - Google Patents
Aluminum alloy target material for photovoltaic reflective film and preparation method thereof Download PDFInfo
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C01B32/182—Graphene
- C01B32/194—After-treatment
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/24—Alkaline-earth metal silicates
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C21/00—Alloys based on aluminium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0089—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with other, not previously mentioned inorganic compounds as the main non-metallic constituent, e.g. sulfides, glass
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
The invention discloses an aluminum alloy target material for a photovoltaic reflective film, which comprises aluminum, a metal additive, a corrosion-resistant regulator and a refining modifier, wherein the mass ratio of the aluminum to the metal additive to the corrosion-resistant regulator to the refining modifier is (5-9): (1-2): (0.5-1.5): 0.5; wherein the metal additive is one or more of manganese, zirconium, yttrium, tantalum, titanium, technetium and scandium. The aluminum alloy target material is prepared by compounding aluminum, a metal additive, a corrosion-resistant regulator and a refining modifier, an oxidation film layer can be formed in the middle of a product to prevent external media of the product from entering the product and improve the corrosion-resistant performance of the product, and the special needle-shaped structure of the active wollastonite has the penetrating function, fills the gap of the oxidation film layer and plays a role in filling, so that the corrosion-resistant performance of the product is further improved.
Description
Technical Field
The invention relates to the technical field of aluminum alloy targets, in particular to an aluminum alloy target for a photovoltaic reflective film and a preparation method thereof.
Background
The coating target is a sputtering source which forms various functional films on a substrate by sputtering through magnetron sputtering, multi-arc ion plating or other types of coating systems under proper process conditions. In short, the target material is a target material bombarded by high-speed charged energy particles, and when the target material is used in a high-energy laser weapon, lasers with different power densities, different output waveforms and different wavelengths interact with different target materials, different killing and damaging effects can be generated. For example, the evaporation magnetron sputtering coating is a heating evaporation coating, an aluminum film and the like. Different target materials (such as aluminum, copper, stainless steel, titanium, nickel targets and the like) are replaced, and different film systems (such as superhard, wear-resistant and corrosion-resistant alloy films and the like) can be obtained.
The existing aluminum alloy target material is simple in raw material proportion, the prepared target material is poor in corrosion resistance, and the service life of the target material is influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an aluminum alloy target material for a photovoltaic reflective film and a preparation method thereof, so as to solve the problems in the background art.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides an aluminum alloy target material for a photovoltaic reflective film, which comprises aluminum, a metal additive, a corrosion-resistant regulator and a refining modifier, wherein the mass ratio of the aluminum to the metal additive to the corrosion-resistant regulator to the refining modifier is (5-9): (1-2): (0.5-1.5): 0.5; wherein the metal additive is one or more of manganese, zirconium, yttrium, tantalum, titanium, technetium and scandium;
the corrosion-resistant regulator comprises a first regulator and a second regulator, and the first regulator and the second regulator are optimized to obtain the corrosion-resistant regulator;
the preparation method of the first regulator comprises the following steps: sending graphene into a ball mill for ball milling treatment, calcining at the temperature of 100-120 ℃ for 10-20min, then cooling to 80-90 ℃, continuing to preserve heat for 25-35min, finally cooling to room temperature at the speed of 1-3 ℃/min, then washing for 1-3 times by using boiling water, and drying to obtain a first regulator;
the preparation method of the second regulator comprises the following steps: calcining the bentonite at the temperature of 200-300 ℃ for 20-30min, then carrying out radiation treatment, wherein the radiation dose is 100-150KGy, ending the radiation, and then naturally cooling to the room temperature to obtain the second regulator.
Preferably, the optimization treatment method of the first and second regulators comprises the following steps: and respectively placing the first regulator and the second regulator in a dispersing agent for high-degree dispersion treatment, and washing and drying after dispersion is finished.
Preferably, the preparation method of the dispersant is as follows: adding an ethanol medium into a magnetic stirrer, adding glacial acetic acid, adjusting the pH value of the solution to 4.0-5.0, then adding GaNP metal quantum dots accounting for 10-20% of the total amount of the ethanol and an alkyl sodium sulfonate wetting agent accounting for 5-10%, continuing stirring for 10-20min at the stirring speed of 200-400r/min, and obtaining the dispersing agent after the stirring is finished.
Preferably, the specific operation steps of the high-degree dispersion treatment are as follows: stirring at the rotation speed of 1500r/min for 10-20min and at the rotation speed of 300r/min for 200-40 min, and finally performing ultrasonic oscillation for 1-3 times with the ultrasonic power of 500W.
Preferably, the preparation method of the refining alterant comprises the following steps:
s1: preparation of a first reaction material:
the method comprises the following steps: mixing aluminum nitride and tin powder according to the weight ratio of 2:1, then sending the mixture into ethanol with the weight 2-3 times of the total weight of the aluminum nitride for ultrasonic dispersion, then adding polyethylene glycol with the weight 10-20% of the total weight of the ethanol, performing ultrasonic dispersion for 10-20min, wherein the ultrasonic power is 100-;
step two: then adding sodium dodecyl sulfate accounting for 1-5% of the total amount of the aluminum nitride, and stirring at the rotating speed of 100-;
s2: preparation of a second reaction material: mixing La, Ce and Sm according to the weight ratio of 3:2:1 to form a rare earth material, adding modified wollastonite powder accounting for 10-20% of the total weight of the rare earth material, and mixing at the rotating speed of 100-500r/min to obtain a second reaction material;
s3: adding the second reaction material into the first reaction material, firstly stirring at the rotation speed of 500-.
Preferably, the modification method of the modified wollastonite powder comprises the following steps: mixing wollastonite powder and silicon dioxide emulsion according to the weight ratio of 3:1, adopting proton irradiation with the irradiation power of 100-500W and the irradiation time of 10-20min, adding the mixture into a grinding machine for grinding at the grinding speed of 1000-1500r/min and the grinding time of 30-40min, finishing grinding, and then washing and drying to obtain the modified wollastonite powder.
Preferably, the silicon dioxide emulsion is formed by mixing silicon dioxide and polystyrene microsphere emulsion according to the weight ratio of 1: 2.
Preferably, the polystyrene microsphere emulsion is prepared by reacting ethanol as a medium, styrene as a monomer, azobisisobutyronitrile as an initiator, divinylbenzene as a crosslinking agent and sodium dodecyl sulfate as an emulsifier.
A manufacturing method of an aluminum alloy target material for a photovoltaic reflective film comprises the following steps:
the method comprises the following steps: melting and smelting aluminum and metal conditioning agents to be completely melted, then cooling and forming, and then grinding to powder, and sieving with a sieve of 100 meshes and 300 meshes;
step two: then adding a refining alterant, sintering for 10-20min at the temperature of 400-;
step three: then, continuously sintering at the temperature of 300-400 ℃ for 10-20min, and obtaining a sintered material after sintering is finished;
step four: carrying out heat treatment on the sintering material, and finally cooling to room temperature to obtain the heat-treated sintering material;
step five: and spraying the sintered material obtained in the fourth step onto stainless steel to a spraying thickness of 1-3mm to obtain the target material.
Preferably, the treatment temperature in the heat treatment is 260-300 ℃, the treatment is 15-25min, then the temperature is reduced to 180-220 ℃, and the treatment is continued for 10-20 min.
Compared with the prior art, the invention has the following beneficial effects:
the aluminum alloy target material is prepared by compounding aluminum, a metal additive, a corrosion-resistant regulator and a refining modifier; the first regulator and the second regulator in the corrosion-resistant regulator and the refining alterant are added in product sintering, the first reaction material in the refining alterant is prepared by adopting raw materials such as aluminum nitride, tin powder and the like, the tin powder and the aluminum nitride can promote crystal refining in sintering, the mixed rare earth in the second reaction material has excellent activity and can form an oxidation film layer in the middle of the product to prevent external media of the product from entering the product and improve the corrosion-resistant performance of the product, and the active wollastonite has a special needle-shaped structure and has an interpenetration function to fill the gap of the oxidation film layer and play a role in filling, thereby further improving the corrosion-resistant performance of the product;
in the modification of wollastonite powder, the wollastonite powder and the silica emulsion are modified in a matching way, so that the silica in the silica emulsion has high specific surface area, and the wollastonite is polished in the matching way of the polystyrene microsphere emulsion, and meanwhile, the wollastonite and the polystyrene microsphere emulsion are incompatible and in an independent state, so that the modified wollastonite has high purity and high activity needle-shaped bodies, and a high-quality medium environment is provided for the modification of corrosion resistance;
first regulator and second regulator cooperation are used, graphite alkene in the first regulator is through the ball-milling, the activity reinforcing after calcining, bentonite in the second regulator is through a series of processings back, the lamella interval enlarges, the activity reinforcing, after optimizing again, the dispersibility reinforcing, thereby the application effect of first regulator and second regulator is better, better application is in the raw materials, the lamellar structure of graphite alkene and the lamellar structure of bentonite play high two-dimentional dislocation cooperation, thereby fill in the product, the barrier property of further improvement product, thereby play efficient corrosion resistance.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The aluminum alloy target material for the photovoltaic reflective film comprises aluminum, a metal additive, a corrosion-resistant regulator and a refining modifier, wherein the mass ratio of the aluminum to the metal additive to the corrosion-resistant regulator to the refining modifier is (5-9): (1-2): (0.5-1.5): 0.5; wherein the metal additive is one or more of manganese, zirconium, yttrium, tantalum, titanium, technetium and scandium;
the corrosion-resistant regulator comprises a first regulator and a second regulator, and the first regulator and the second regulator are optimized to obtain the corrosion-resistant regulator;
the preparation method of the first regulator comprises the following steps: sending graphene into a ball mill for ball milling treatment, calcining at the temperature of 100-120 ℃ for 10-20min, then cooling to 80-90 ℃, continuing to preserve heat for 25-35min, finally cooling to room temperature at the speed of 1-3 ℃/min, then washing for 1-3 times by using boiling water, and drying to obtain a first regulator;
the preparation method of the second regulator comprises the following steps: calcining the bentonite at the temperature of 200-300 ℃ for 20-30min, then carrying out radiation treatment, wherein the radiation dose is 100-150KGy, ending the radiation, and then naturally cooling to the room temperature to obtain the second regulator.
The optimization processing method of the first regulator and the second regulator in the embodiment comprises the following steps: and respectively placing the first regulator and the second regulator in a dispersing agent for high-degree dispersion treatment, and washing and drying after dispersion is finished.
The preparation method of the dispersant of the embodiment comprises the following steps: adding an ethanol medium into a magnetic stirrer, adding glacial acetic acid, adjusting the pH value of the solution to 4.0-5.0, then adding GaNP metal quantum dots accounting for 10-20% of the total amount of the ethanol and an alkyl sodium sulfonate wetting agent accounting for 5-10%, continuing stirring for 10-20min at the stirring speed of 200-400r/min, and obtaining the dispersing agent after the stirring is finished.
The specific operation steps of the high dispersion treatment in this embodiment are as follows: stirring at the rotation speed of 1500r/min for 10-20min and at the rotation speed of 300r/min for 200-40 min, and finally performing ultrasonic oscillation for 1-3 times with the ultrasonic power of 500W.
The preparation method of the refining alterant comprises the following steps:
s1: preparation of a first reaction material:
the method comprises the following steps: mixing aluminum nitride and tin powder according to the weight ratio of 2:1, then sending the mixture into ethanol with the weight 2-3 times of the total weight of the aluminum nitride for ultrasonic dispersion, then adding polyethylene glycol with the weight 10-20% of the total weight of the ethanol, performing ultrasonic dispersion for 10-20min, wherein the ultrasonic power is 100-;
step two: then adding sodium dodecyl sulfate accounting for 1-5% of the total amount of the aluminum nitride, and stirring at the rotating speed of 100-;
s2: preparation of a second reaction material: mixing La, Ce and Sm according to the weight ratio of 3:2:1 to form a rare earth material, adding modified wollastonite powder accounting for 10-20% of the total weight of the rare earth material, and mixing at the rotating speed of 100-500r/min to obtain a second reaction material;
s3: adding the second reaction material into the first reaction material, firstly stirring at the rotation speed of 500-.
The modification method of the modified wollastonite powder of this embodiment is as follows: mixing wollastonite powder and silicon dioxide emulsion according to the weight ratio of 3:1, adopting proton irradiation with the irradiation power of 100-500W and the irradiation time of 10-20min, adding the mixture into a grinding machine for grinding at the grinding speed of 1000-1500r/min and the grinding time of 30-40min, finishing grinding, and then washing and drying to obtain the modified wollastonite powder.
The silica emulsion of the embodiment is formed by mixing silica and polystyrene microsphere emulsion according to the weight ratio of 1: 2.
The polystyrene microsphere emulsion of the embodiment is prepared by reacting ethanol as a medium, styrene as a monomer, azobisisobutyronitrile as an initiator, divinylbenzene as a crosslinking agent, and sodium dodecyl sulfate as an emulsifier.
The manufacturing method of the aluminum alloy target material for the photovoltaic reflective film comprises the following steps:
the method comprises the following steps: melting and smelting aluminum and metal conditioning agents to be completely melted, then cooling and forming, and then grinding to powder, and sieving with a sieve of 100 meshes and 300 meshes;
step two: then adding a refining alterant, sintering for 10-20min at the temperature of 400-;
step three: then, continuously sintering at the temperature of 300-400 ℃ for 10-20min, and obtaining a sintered material after sintering is finished;
step four: carrying out heat treatment on the sintering material, and finally cooling to room temperature to obtain the heat-treated sintering material;
step five: and spraying the sintered material obtained in the fourth step onto stainless steel to a spraying thickness of 1-3mm to obtain the target material.
The treatment temperature in the heat treatment of the embodiment is 260-300 ℃, the treatment is carried out for 15-25min, then the temperature is reduced to 180-220 ℃, and the treatment is continued for 10-20 min.
Example 1
The aluminum alloy target material for the photovoltaic reflective film comprises aluminum, a metal additive, a corrosion-resistant regulator and a refining modifier, wherein the mass ratio of the aluminum to the metal additive to the corrosion-resistant regulator to the refining modifier is 5: 1: 0.5: 0.5; wherein the metal additive is a composition of manganese, zirconium, yttrium, tantalum and scandium;
the corrosion-resistant regulator comprises a first regulator and a second regulator, and the first regulator and the second regulator are optimized to obtain the corrosion-resistant regulator;
the preparation method of the first regulator comprises the following steps: sending graphene into a ball mill for ball milling treatment, then calcining at 100 ℃ for 10min, then cooling to 80 ℃, continuing to preserve heat for 25min, ending the heat preservation, finally cooling to room temperature at 1 ℃/min, then washing for 1 time by using boiling water, and drying to obtain a first regulator;
the preparation method of the second regulator comprises the following steps: calcining the bentonite for 20min at 200 ℃, then carrying out radiation treatment, wherein the radiation dose is 100KGy, finishing the radiation, and then naturally cooling to room temperature to obtain the second regulator.
The optimization processing method of the first regulator and the second regulator in the embodiment comprises the following steps: and respectively placing the first regulator and the second regulator in a dispersing agent for high-degree dispersion treatment, and washing and drying after dispersion is finished.
The preparation method of the dispersant of the embodiment comprises the following steps: adding an ethanol medium into a magnetic stirrer, adding glacial acetic acid, adjusting the pH value of the solution to 4.0, adding GaNP metal quantum dots accounting for 10% of the total amount of the ethanol and an alkyl sodium sulfonate wetting agent accounting for 5%, continuously stirring for 10-20min at the stirring speed of 200r/min, and obtaining the dispersing agent after the stirring is finished.
The specific operation steps of the high dispersion treatment in this embodiment are as follows: stirring at 1000r/min for 10min, then stirring at 200r/min for 30min, and finally performing ultrasonic oscillation for 1 time, wherein the ultrasonic power is 500W.
The preparation method of the refining alterant comprises the following steps:
s1: preparation of a first reaction material:
the method comprises the following steps: mixing aluminum nitride and tin powder according to the weight ratio of 2:1, then sending into ethanol with the weight 2-3 times of the total weight of the aluminum nitride for ultrasonic dispersion, then adding polyethylene glycol with the weight 10% of the total weight of the ethanol, performing ultrasonic dispersion for 10min, wherein the ultrasonic power is 100W, and finishing the ultrasonic treatment;
step two: then adding sodium dodecyl sulfate accounting for 1-5% of the total amount of the aluminum nitride, and stirring at the rotating speed of 100r/min for 10min to obtain a first reaction material;
s2: preparation of a second reaction material: mixing La, Ce and Sm according to the weight ratio of 3:2:1 to form a rare earth material, adding modified wollastonite powder accounting for 10% of the total weight of the rare earth material, and mixing at the rotating speed of 100r/min to obtain a second reaction material;
s3: and adding the second reaction material into the first reaction material, stirring at a rotating speed of 500r/min for 10-30min, then stirring at a low speed of 300r/min for 45min, finishing stirring, and then washing and drying to obtain the refined alterant.
The modification method of the modified wollastonite powder of this embodiment is as follows: mixing the wollastonite powder and the silicon dioxide emulsion according to the weight ratio of 3:1, adopting proton irradiation with the irradiation power of 100W and the irradiation time of 10min, adding the mixture into a grinding machine for grinding at the grinding rotation speed of 1000r/min for 30min, finishing grinding, and then washing and drying to obtain the modified wollastonite powder.
The silica emulsion of the embodiment is formed by mixing silica and polystyrene microsphere emulsion according to the weight ratio of 1: 2.
The polystyrene microsphere emulsion of the embodiment is prepared by reacting ethanol as a medium, styrene as a monomer, azobisisobutyronitrile as an initiator, divinylbenzene as a crosslinking agent, and sodium dodecyl sulfate as an emulsifier.
The manufacturing method of the aluminum alloy target material for the photovoltaic reflective film comprises the following steps:
the method comprises the following steps: melting and smelting aluminum and metal conditioning agents to be completely melted, then cooling and forming, then grinding to powder, and sieving with a 100-mesh sieve;
step two: adding a refining alterant, sintering at 400 ℃ for 10min, sequentially adding a first regulator and a second regulator in the corrosion-resistant regulator, stirring at a high speed for 10min at a stirring speed of 300r/min, and finishing stirring;
step three: then continuously sintering at 300 ℃ for 10min, and obtaining a sintering material after sintering is finished;
step four: carrying out heat treatment on the sintering material, and finally cooling to room temperature to obtain the heat-treated sintering material;
step five: and (4) spraying the sintered material obtained in the fourth step onto stainless steel, wherein the spraying thickness is 1mm, and thus the target material can be obtained.
The treatment temperature in the heat treatment of this example was 260 ℃ for 15min, and then the temperature was reduced to 180 ℃ for 10 min.
Example 2
The aluminum alloy target material for the photovoltaic reflective film comprises aluminum, a metal additive, a corrosion-resistant regulator and a refining modifier, wherein the mass ratio of the aluminum to the metal additive to the corrosion-resistant regulator to the refining modifier is 9: 2: 1.5: 0.5; wherein the metal additive is a composition of manganese, tantalum, titanium, technetium and scandium;
the corrosion-resistant regulator comprises a first regulator and a second regulator, and the first regulator and the second regulator are optimized to obtain the corrosion-resistant regulator;
the preparation method of the first regulator comprises the following steps: sending graphene into a ball mill for ball milling treatment, then calcining at 120 ℃ for 20min, then cooling to 90 ℃, continuing to preserve heat for 35min, ending the heat preservation, finally cooling to room temperature at 3 ℃/min, then washing for 3 times by using boiling water, and drying to obtain a first regulator;
the preparation method of the second regulator comprises the following steps: calcining the bentonite at 300 ℃ for 30min, then carrying out radiation treatment, wherein the radiation dose is 150KGy, finishing the radiation, and then naturally cooling to room temperature to obtain the second regulator.
The optimization processing method of the first regulator and the second regulator in the embodiment comprises the following steps: and respectively placing the first regulator and the second regulator in a dispersing agent for high-degree dispersion treatment, and washing and drying after dispersion is finished.
The preparation method of the dispersant of the embodiment comprises the following steps: adding an ethanol medium into a magnetic stirrer, adding glacial acetic acid, adjusting the pH value of the solution to 5.0, adding GaNP metal quantum dots accounting for 20% of the total amount of ethanol and an alkyl sodium sulfonate wetting agent accounting for 10%, continuing stirring for 20min, wherein the stirring speed is 400r/min, and finishing stirring to obtain the dispersing agent.
The specific operation steps of the high dispersion treatment in this embodiment are as follows: stirring at 1500r/min for 20min, stirring at 300r/min for 40min, and ultrasonically oscillating for 3 times with ultrasonic power of 500W.
The preparation method of the refining alterant comprises the following steps:
s1: preparation of a first reaction material:
the method comprises the following steps: mixing aluminum nitride and tin powder according to the weight ratio of 2:1, then sending into ethanol with the amount of 3 times of the total amount of the aluminum nitride for ultrasonic dispersion, then adding polyethylene glycol with the amount of 20% of the total amount of the ethanol, performing ultrasonic dispersion for 20min, wherein the ultrasonic power is 500W, and finishing the ultrasonic treatment;
step two: then adding sodium dodecyl sulfate accounting for 5 percent of the total amount of the aluminum nitride, and stirring at the rotating speed of 500r/min for 20min to obtain a first reaction material;
s2: preparation of a second reaction material: mixing La, Ce and Sm according to the weight ratio of 3:2:1 to form a rare earth material, adding modified wollastonite powder accounting for 20% of the total weight of the rare earth material, and mixing at the rotating speed of 500r/min to obtain a second reaction material;
s3: and adding the second reaction material into the first reaction material, stirring at a rotating speed of 1000r/min for 30min, then stirring at a rotating speed of 400r/min for 55min at a low speed, and then washing and drying to obtain the refined alterant after the stirring is finished.
The modification method of the modified wollastonite powder of this embodiment is as follows: mixing the wollastonite powder and the silicon dioxide emulsion according to the weight ratio of 3:1, adopting proton irradiation with the irradiation power of 500W and the irradiation time of 20min, adding the mixture into a grinding machine for grinding at the grinding rotation speed of 1500r/min for 40min, finishing grinding, and then washing and drying to obtain the modified wollastonite powder.
The silica emulsion of the embodiment is formed by mixing silica and polystyrene microsphere emulsion according to the weight ratio of 1: 2.
The polystyrene microsphere emulsion of the embodiment is prepared by reacting ethanol as a medium, styrene as a monomer, azobisisobutyronitrile as an initiator, divinylbenzene as a crosslinking agent, and sodium dodecyl sulfate as an emulsifier.
The manufacturing method of the aluminum alloy target material for the photovoltaic reflective film comprises the following steps:
the method comprises the following steps: melting and smelting aluminum and metal conditioning agents to be completely melted, then cooling and forming, then grinding to powder, and sieving with a 300-mesh sieve;
step two: adding a refining alterant, sintering at 500 ℃ for 20min, sequentially adding a first regulator and a second regulator in the corrosion-resistant regulator, stirring at a high speed for 40min at a stirring speed of 500r/min, and finishing stirring;
step three: then, continuously sintering at 400 ℃ for 20min, and obtaining a sintering material after sintering is finished;
step four: carrying out heat treatment on the sintering material, and finally cooling to room temperature to obtain the heat-treated sintering material;
step five: and spraying the sintered material obtained in the fourth step onto stainless steel to a spraying thickness of 1-3mm to obtain the target material.
The treatment temperature in the heat treatment of this example was 300 ℃, the treatment was carried out for 25min, and then the temperature was reduced to 220 ℃, and the treatment was continued for 20 min.
Example 3
The aluminum alloy target material for the photovoltaic reflective film comprises aluminum, a metal additive, a corrosion-resistant regulator and a refining modifier, wherein the mass ratio of the aluminum to the metal additive to the corrosion-resistant regulator to the refining modifier is 7: 1.5: 1: 0.5; wherein the metal additive is a plurality of compositions of manganese, zirconium, yttrium, tantalum, titanium, technetium and scandium;
the corrosion-resistant regulator comprises a first regulator and a second regulator, and the first regulator and the second regulator are optimized to obtain the corrosion-resistant regulator;
the preparation method of the first regulator comprises the following steps: sending graphene into a ball mill for ball milling treatment, then calcining at 110 ℃ for 15min, then cooling to 85 ℃, continuing to preserve heat for 30min, ending the heat preservation, finally cooling to room temperature at the speed of 2 ℃/min, then washing for 2 times by using boiling water, and drying to obtain a first regulator;
the preparation method of the second regulator comprises the following steps: calcining the bentonite at 250 ℃ for 25min, then carrying out radiation treatment, wherein the radiation dose is 125KGy, finishing the radiation, and then naturally cooling to room temperature to obtain the second regulator.
The optimization processing method of the first regulator and the second regulator in the embodiment comprises the following steps: and respectively placing the first regulator and the second regulator in a dispersing agent for high-degree dispersion treatment, and washing and drying after dispersion is finished.
The preparation method of the dispersant of the embodiment comprises the following steps: adding an ethanol medium into a magnetic stirrer, adding glacial acetic acid, adjusting the pH value of the solution to 4.5, adding GaNP metal quantum dots accounting for 15% of the total amount of the ethanol and an alkyl sodium sulfonate wetting agent accounting for 7.5%, continuously stirring for 15min at the stirring speed of 300r/min, and obtaining the dispersing agent after the stirring is finished.
The specific operation steps of the high dispersion treatment in this embodiment are as follows: stirring at 1250r/min for 15min, then stirring at 250r/min for 35min, and finally performing ultrasonic oscillation for 2 times, wherein the ultrasonic power is 500W.
The preparation method of the refining alterant comprises the following steps:
s1: preparation of a first reaction material:
the method comprises the following steps: mixing aluminum nitride and tin powder according to the weight ratio of 2:1, then sending into ethanol with the weight 2.5 times of the total weight of the aluminum nitride for ultrasonic dispersion, then adding polyethylene glycol with the weight 15% of the total weight of the ethanol, performing ultrasonic dispersion for 15min, wherein the ultrasonic power is 300W, and finishing the ultrasonic treatment;
step two: then adding sodium dodecyl sulfate accounting for 3 percent of the total amount of the aluminum nitride, and stirring at the rotating speed of 300r/min for 15min to obtain a first reaction material;
s2: preparation of a second reaction material: mixing La, Ce and Sm according to the weight ratio of 3:2:1 to form a rare earth material, adding modified wollastonite powder accounting for 15% of the total weight of the rare earth material, and mixing at the rotating speed of 300r/min to obtain a second reaction material;
s3: and adding the second reaction material into the first reaction material, stirring at a rotating speed of 750r/min for 20min, then stirring at a low speed of 350r/min for 50min, and then washing and drying to obtain the refined alterant after stirring.
The modification method of the modified wollastonite powder of this embodiment is as follows: mixing the wollastonite powder and the silicon dioxide emulsion according to the weight ratio of 3:1, adopting proton irradiation with the irradiation power of 300W and the irradiation time of 15min, adding the mixture into a grinding machine for grinding at the grinding rotation speed of 1250r/min for 35min, finishing grinding, and then washing and drying to obtain the modified wollastonite powder.
The silica emulsion of the embodiment is formed by mixing silica and polystyrene microsphere emulsion according to the weight ratio of 1: 2.
The polystyrene microsphere emulsion of the embodiment is prepared by reacting ethanol as a medium, styrene as a monomer, azobisisobutyronitrile as an initiator, divinylbenzene as a crosslinking agent, and sodium dodecyl sulfate as an emulsifier.
The manufacturing method of the aluminum alloy target material for the photovoltaic reflective film comprises the following steps:
the method comprises the following steps: melting and smelting aluminum and metal conditioning agents to be completely melted, then cooling and forming, then grinding to powder, and sieving with a 200-mesh sieve;
step two: adding a refining alterant, sintering at 450 ℃ for 15min, sequentially adding a first regulator and a second regulator in the corrosion-resistant regulator, stirring at a high speed for 20min at a stirring speed of 400r/min, and finishing stirring;
step three: then, continuously sintering for 15min at 350 ℃, and obtaining a sintering material after sintering is finished;
step four: carrying out heat treatment on the sintering material, and finally cooling to room temperature to obtain the heat-treated sintering material;
step five: and (4) spraying the sintered material obtained in the fourth step onto stainless steel, wherein the spraying thickness is 2mm, and thus the target material can be obtained.
The treatment temperature in the heat treatment of this example was 280 ℃ for 20min, and then the temperature was lowered to 200 ℃ for further 15 min.
Comparative example 1
Unlike example 3, no refining modifier was added.
Comparative example 2
In contrast to example 3, no first regulator was added.
Comparative example 3
In contrast to example 3, no second regulator was added.
The results of the performance measurements of examples 1 to 3 and comparative examples 1 to 3 are as follows
From examples 1-3 and comparative examples 1-3, the product of example 3 of the present invention has excellent relative density and oxygen content, and the product performance can be significantly improved after modification.
Performing an electrochemical experiment on the product, adopting a standard three-electrode system, taking a platinum sheet as an auxiliary electrode, taking a saturated calomel electrode as a reference electrode, taking a product as a working electrode, soaking the product in a sodium chloride solution with the concentration of 3.0 percent for 30min, and measuring the corrosion current density;
from examples 1-3 and comparative examples 1-3, the corrosion current density of the product of example 3 of the present invention was minimized, and the product had excellent corrosion resistance.
The preparation method of the refining alterant comprises the following steps:
s1: preparation of a first reaction material:
the method comprises the following steps: mixing aluminum nitride and tin powder according to the weight ratio of 2:1, then sending into ethanol with the weight 2.5 times of the total weight of the aluminum nitride for ultrasonic dispersion, then adding polyethylene glycol with the weight 15% of the total weight of the ethanol, performing ultrasonic dispersion for 15min, wherein the ultrasonic power is 300W, and finishing the ultrasonic treatment;
step two: then adding sodium dodecyl sulfate accounting for 3 percent of the total amount of the aluminum nitride, and stirring at the rotating speed of 300r/min for 15min to obtain a first reaction material;
s2: preparation of a second reaction material: mixing La, Ce and Sm according to the weight ratio of 3:2:1 to form a rare earth material, adding modified wollastonite powder accounting for 15% of the total weight of the rare earth material, and mixing at the rotating speed of 300r/min to obtain a second reaction material;
s3: and adding the second reaction material into the first reaction material, stirring at a rotating speed of 750r/min for 20min, then stirring at a low speed of 350r/min for 50min, and then washing and drying to obtain the refined alterant after stirring.
The invention further explores the corrosion resistance of the product by refining the alterant
Experimental example 1.
Modified wollastonite powder is not added into the refining alterant.
Experimental example 2.
Rare earth materials are not added into the refining alterant.
Experimental example 3.
Tin powder is not added into the refining alterant.
As can be seen from the experimental examples 1-3, the modified wollastonite powder, the rare earth material and the tin powder in the refined alterant have certain influence on the corrosion resistance of the product, and on the basis, the refined alterant has a positive improvement effect on the corrosion resistance of the product.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. The aluminum alloy target material for the photovoltaic reflective film is characterized by comprising aluminum, a metal additive, a corrosion-resistant regulator and a refining modifier, wherein the mass ratio of the aluminum to the metal additive to the corrosion-resistant regulator to the refining modifier is (5-9): (1-2): (0.5-1.5): 0.5; wherein the metal additive is one or more of manganese, zirconium, yttrium, tantalum, titanium, technetium and scandium;
the corrosion-resistant regulator comprises a first regulator and a second regulator, and the first regulator and the second regulator are optimized to obtain the corrosion-resistant regulator;
the preparation method of the first regulator comprises the following steps: sending graphene into a ball mill for ball milling treatment, calcining at the temperature of 100-120 ℃ for 10-20min, then cooling to 80-90 ℃, continuing to preserve heat for 25-35min, finally cooling to room temperature at the speed of 1-3 ℃/min, then washing for 1-3 times by using boiling water, and drying to obtain a first regulator;
the preparation method of the second regulator comprises the following steps: calcining the bentonite at the temperature of 200-300 ℃ for 20-30min, then carrying out radiation treatment, wherein the radiation dose is 100-150KGy, ending the radiation, and then naturally cooling to the room temperature to obtain the second regulator.
2. The aluminum alloy target material for the photovoltaic reflective film as recited in claim 1, wherein the optimization processing method of the first and second regulators comprises: and respectively placing the first regulator and the second regulator in a dispersing agent for high-degree dispersion treatment, and washing and drying after dispersion is finished.
3. The aluminum alloy target material for the photovoltaic reflective film as claimed in claim 2, wherein the preparation method of the dispersant comprises the following steps: adding an ethanol medium into a magnetic stirrer, adding glacial acetic acid, adjusting the pH value of the solution to 4.0-5.0, then adding GaNP metal quantum dots accounting for 10-20% of the total amount of the ethanol and an alkyl sodium sulfonate wetting agent accounting for 5-10%, continuing stirring for 10-20min at the stirring speed of 200-400r/min, and obtaining the dispersing agent after the stirring is finished.
4. The aluminum alloy target material for the photovoltaic reflective film as recited in claim 2, wherein the specific operation steps of the high-dispersion treatment are as follows: stirring at the rotation speed of 1500r/min for 10-20min and at the rotation speed of 300r/min for 200-40 min, and finally performing ultrasonic oscillation for 1-3 times with the ultrasonic power of 500W.
5. The aluminum alloy target material for the photovoltaic reflective film as claimed in claim 1, wherein the preparation method of the refining alterant comprises the following steps:
s1: preparation of a first reaction material:
the method comprises the following steps: mixing aluminum nitride and tin powder according to the weight ratio of 2:1, then sending the mixture into ethanol with the weight 2-3 times of the total weight of the aluminum nitride for ultrasonic dispersion, then adding polyethylene glycol with the weight 10-20% of the total weight of the ethanol, performing ultrasonic dispersion for 10-20min, wherein the ultrasonic power is 100-;
step two: then adding sodium dodecyl sulfate accounting for 1-5% of the total amount of the aluminum nitride, and stirring at the rotating speed of 100-;
s2: preparation of a second reaction material: mixing La, Ce and Sm according to the weight ratio of 3:2:1 to form a rare earth material, adding modified wollastonite powder accounting for 10-20% of the total weight of the rare earth material, and mixing at the rotating speed of 100-500r/min to obtain a second reaction material;
s3: adding the second reaction material into the first reaction material, firstly stirring at the rotation speed of 500-.
6. The aluminum alloy target material for the photovoltaic reflective film according to claim 5, wherein the modification method of the modified wollastonite powder comprises the following steps: mixing wollastonite powder and silicon dioxide emulsion according to the weight ratio of 3:1, adopting proton irradiation with the irradiation power of 100-500W and the irradiation time of 10-20min, adding the mixture into a grinding machine for grinding at the grinding speed of 1000-1500r/min and the grinding time of 30-40min, finishing grinding, and then washing and drying to obtain the modified wollastonite powder.
7. The aluminum alloy target material for the photovoltaic reflective film as recited in claim 5, wherein the silica emulsion is formed by mixing silica and polystyrene microsphere emulsion according to a weight ratio of 1: 2.
8. The aluminum alloy target material for the photovoltaic reflective film as recited in claim 7, wherein the polystyrene microsphere emulsion is prepared by reacting ethanol as a medium, styrene as a monomer, azobisisobutyronitrile as an initiator, divinylbenzene as a crosslinking agent, and sodium dodecyl sulfate as an emulsifier.
9. The method for manufacturing the aluminum alloy target material for the photovoltaic reflective film according to any one of claims 1 to 8, comprising the following steps:
the method comprises the following steps: melting and smelting aluminum and metal conditioning agents to be completely melted, then cooling and forming, and then grinding to powder, and sieving with a sieve of 100 meshes and 300 meshes;
step two: then adding a refining alterant, sintering for 10-20min at the temperature of 400-;
step three: then, continuously sintering at the temperature of 300-400 ℃ for 10-20min, and obtaining a sintered material after sintering is finished;
step four: carrying out heat treatment on the sintering material, and finally cooling to room temperature to obtain the heat-treated sintering material;
step five: and spraying the sintered material obtained in the fourth step onto stainless steel to a spraying thickness of 1-3mm to obtain the target material.
10. The method as claimed in claim 9, wherein the temperature of the heat treatment is 260-300 ℃, the treatment is carried out for 15-25min, and then the temperature is decreased to 180-220 ℃, and the treatment is continued for 10-20 min.
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