CN110042353B - Nano laminated aluminum-based composite material and preparation method thereof - Google Patents

Nano laminated aluminum-based composite material and preparation method thereof Download PDF

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CN110042353B
CN110042353B CN201910269098.3A CN201910269098A CN110042353B CN 110042353 B CN110042353 B CN 110042353B CN 201910269098 A CN201910269098 A CN 201910269098A CN 110042353 B CN110042353 B CN 110042353B
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aluminum
composite material
based composite
alloy foil
nano laminated
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CN110042353A (en
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孙士阳
孙守业
徐平平
丁闯
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Inner Mongolia University of Science and Technology
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Inner Mongolia University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B1/00Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/38Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B3/00Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0688Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B3/00Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
    • B21B2003/001Aluminium or its alloys

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Products (AREA)
  • Pressure Welding/Diffusion-Bonding (AREA)
  • Physical Vapour Deposition (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention discloses a nano laminated aluminum-based composite material and a preparation method thereof, belonging to the field of preparation of aluminum-based composite materials.A physical vapor deposition technology is utilized to carry out magnetron co-sputtering on Al and a ceramic material in an argon atmosphere, and composite layers with the thickness of 2 microns and nano-sized ceramic particles are respectively formed on the double-layer surfaces of an Al alloy foil substrate; then preparing a laminated Al-based composite layer plate by using a high-temperature diffusion bonding technology; the invention has the advantages that: the Al alloy foil is sputtered with the magnetron co-sputtering Al and the ceramic material, so that the ceramic phase reaches the nanoscale and is uniformly distributed in the Al matrix, the common defects of air holes, impurities and the like in the composite material are avoided, and the particle size and the distribution of the ceramic phase can be controlled by high-temperature annealing to change the performance of the material; the optimized lamination period, the optimized layer thickness ratio and the optimized number of the lamination layers are bonded by adopting a high-temperature diffusion bonding technology, so that the strength of the composite structure film obtained by vapor deposition can be further improved, and the application of the composite structure film in the macroscopic field is greatly expanded.

Description

Nano laminated aluminum-based composite material and preparation method thereof
Technical Field
The invention relates to the technology in the field of composite materials, in particular to a nano laminated aluminum-based composite material and a preparation method thereof.
Background
The performance of the aluminum-based composite material is determined by the aluminum alloy substrate and the particle reinforced phase, so that the aluminum-based composite material has the high toughness of a metal material and the high hardness and high wear resistance of a ceramic material, becomes an important direction for the development of modern materials, and has wide application and huge prospects in the fields of aerospace, transportation, electronic and electrical appliances and the like.
Through development for many years, the preparation of the aluminum-based composite material is mature gradually, but the existing process has the problems that the particle size of a ceramic reinforcing phase is large, the microstructure is uneven, bubbles, impurities and the like are often mixed in the preparation process, mainly because the ceramic phase cannot be added uniformly and in high quality under the traditional preparation process, and although the addition of the ceramic phase at the atomic level can be realized through gas phase (chemical) deposition, the method is greatly limited in the application field due to the narrow space scale of a film.
The laminated material can obtain more excellent performance than the composite material with the same component through the modulation period and the layer thickness ratio among different components, but the optimization and connection of lamination become complicated due to a plurality of influencing factors, so that the performance of the real laminated material is greatly dispersed due to different preparation processes.
Disclosure of Invention
The invention aims to provide a nano laminated aluminum-based composite material and a preparation method thereof, which can realize the uniformity and size control of ceramic phase addition and the combination of multi-component thin layers; in the preparation process, the TiN ceramic phase is uniformly distributed in the film, the component ratio in the composite film is convenient to control, and the film layer is tightly combined with the substrate; the performance of the composite material is improved; in addition, the defects of common air holes, impurities and the like in the composite material can be avoided; in addition, the heat preservation time of the composite precast slab can be greatly prolonged.
The nano laminated TiN/aluminum-based composite material is realized by the following technical scheme:
a preparation method of a nano laminated aluminum-based composite material based on a vapor deposition technology and a high-temperature diffusion bonding technology. The method specifically comprises the following steps:
the method comprises the following steps: firstly, cleaning the surface of an aluminum alloy foil, sequentially carrying out ultrasonic cleaning in alcohol, acetone and alcohol solution for 10min, cleaning dirt on the surface of a substrate, and then drying; fixing the cleaned aluminum alloy foil on a workbench in a vacuum chamber;
step two: in vacuum or protective gas atmosphere, high-purity aluminum with the purity of 99.99 percent and high-purity TiN ceramic are used as target materials. Controlling the magnetron sputtering power to enable the content of TiN particles in the film to be 5-10 at%;
step three: when setting upThe vacuum of the standby substrate reaches 2 x 10-3And after Pa, introducing argon with the purity of 99.99 percent into the vacuum chamber as working gas. Then starting a radio frequency magnetron sputtering power supply to carry out aluminum and TiN ceramic co-sputtering deposition on the aluminum alloy foil;
step four: plating double-layer films consisting of 2 mu mTiN and aluminum on the surface of the aluminum alloy foil respectively to be used as a composite material prefabricated plate;
step five: cleaning the obtained composite material precast slab in an alcohol solution, cleaning dirt on the surface, and drying;
step six: and (4) placing at least two composite material precast slabs prepared in the fifth step in a vacuum hot pressing furnace, applying 8MPa of pressure to the sample by adopting a pressure head, heating under the condition of keeping the pressure until the temperature reaches 450 ℃, keeping the temperature for 1h, then cutting off the power, cooling to the temperature lower than 80 ℃, and taking out the micro-nano laminated aluminum-based composite material with high performance.
Preferably, the aluminum alloy foil in the first step adopts a commercial aluminum alloy foil with a double-optical-surface thickness of 30 μm.
Preferably, the aluminum alloy foil has an aluminum content of more than 80% and an alloy content of less than 20%.
Preferably, the process conditions for deposition in the second step are a gas pressure of 0.4Pa and a substrate bias voltage of 250V.
Preferably, the layer thickness ratio of the double-layer film to the aluminum alloy foil in the fourth step is 0.13.
Preferably, the number of the nano laminated aluminum-based composite material layers in the sixth step is 12.
The invention has the advantages that the magnetron co-sputtering aluminum and the ceramic material are adopted on the aluminum alloy foil, so that the ceramic phase reaches the nano scale and is uniformly distributed in the aluminum matrix, the common defects of air holes, impurities and the like in the composite material are avoided, and in addition, the particle size and the distribution of the ceramic phase can be controlled through high-temperature annealing, so that the performance of the material is changed; the optimized lamination period, the optimized layer thickness ratio and the optimized number of the lamination layers are bonded by adopting a high-temperature diffusion bonding technology, so that the strength of the composite structure film obtained by vapor deposition can be further improved, and the application of the composite structure film in the macroscopic field is greatly expanded.
In the preparation process, the component ratio in the composite film is convenient to control, and the film layer is tightly combined with the substrate; meanwhile, the multilayer films can be effectively bonded together by utilizing a high-temperature diffusion technology, the size of TiN particles can be controlled in the bonding process, and the performance of the composite material is improved; the multi-element thin layers are combined to form the composite board, so that the application range of the film is expanded.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Fig. 2 is a schematic diagram of the longitudinal structure of the nanolaminate of the present invention.
Fig. 3 is a lateral structure of a nanolaminate of the present invention.
Detailed Description
Example 1
(1) The surface of a commercial double-optical-surface aluminum alloy foil with the thickness of 30 mu m is pretreated, the aluminum content is required to be higher than 80%, the alloy content is required to be less than 20%, the aluminum foil is sequentially ultrasonically cleaned in alcohol, acetone and alcohol solution for 10min, dirt on the surface of a substrate is cleaned and then dried, and the aluminum foil is fixed on a workbench in a vacuum chamber and dried by a machine.
(2) In vacuum or protective gas atmosphere, ceramic of high-purity aluminum and high-purity TiN with the purity of 99.99 percent is used as a target material.
(3) When the equipment background vacuum reaches 2 x 10-3And after Pa, introducing argon with the purity of 99.99 percent into the vacuum chamber as working gas. And then starting a radio frequency magnetron sputtering power supply to carry out co-sputtering deposition of aluminum and TiN ceramics, wherein the deposition process conditions are as follows: the pressure was 0.4Pa and the substrate bias was 250V.
(4) After deposition, the aluminum alloy foil was coated with 2 μm each of two thin films of TiN and aluminum as a composite material preform.
(5) And (3) cleaning the plurality of composite prefabricated plates in an alcohol solution, cleaning dirt on the surface, and drying.
(6) The composite layer is an aluminium alloy foil plated with a certain gradient composition, so that it can be diffusion-bonded in argon environment, 12 prefabricated plates plated with TiN/aluminium double-layer film aluminium alloy foils on both surfaces are placed in a vacuum hot-pressing furnace, a pressure head is used to apply 8MPa pressure to the sample, and the sample is heated under the condition of keeping the pressure until the temperature reaches 450 ℃. And keeping the temperature for 1h, then cutting off the power, cooling to the temperature lower than 80 ℃, and taking out to obtain the high-performance micro-nano laminated aluminum-based composite material.

Claims (6)

1. A preparation method of a nano laminated aluminum-based composite material is characterized by comprising the following steps:
the method comprises the following steps: firstly, cleaning the surface of an aluminum alloy foil, sequentially carrying out ultrasonic cleaning in alcohol, acetone and alcohol solution for 10min, cleaning dirt on the surface of a substrate, and then drying; fixing the cleaned aluminum alloy foil on a workbench in a vacuum chamber;
step two: under the vacuum or protective gas atmosphere, 99.99% of high-purity aluminum and high-purity TiN ceramic are used as targets, and the content of TiN particles in the film is controlled to be 5-10 at.% by controlling the magnetron sputtering power;
step three: when the equipment background vacuum reaches 2 x 10-3After Pa, argon with the purity of 99.99 percent is introduced into the vacuum chamber as working gas,
then starting a radio frequency magnetron sputtering power supply to carry out aluminum and TiN ceramic co-sputtering deposition on the aluminum alloy foil;
step four: plating double-layer films consisting of 2 mu mTiN and aluminum on the surface of the aluminum alloy foil respectively to be used as a composite material prefabricated plate;
step five: cleaning the obtained composite material precast slab in an alcohol solution, cleaning dirt on the surface, and drying;
step six: and (4) placing at least two composite material precast slabs prepared in the fifth step into a vacuum hot pressing furnace, applying 8-10MPa pressure to the sample by adopting a pressure head, heating under the condition of keeping the pressure until the temperature reaches 400-450 ℃, keeping the temperature for 1h, then cutting off the power, cooling to the temperature lower than 80 ℃, and taking out the nano laminated aluminum-based composite material with high performance.
2. The method for preparing a nano laminated aluminum-based composite material according to claim 1, characterized in that: the aluminum alloy foil in the first step is a commercial aluminum alloy foil with double optical surfaces of 30 microns in thickness.
3. The method for preparing a nano laminated aluminum-based composite material according to claim 2, characterized in that: in the aluminum alloy foil, the content of aluminum is higher than 80%, and the content of alloy is less than 20%.
4. The method for preparing a nano laminated aluminum-based composite material according to claim 1, characterized in that: the process conditions of the deposition in the third step are that the air pressure is 0.4Pa and the substrate bias voltage is 250V.
5. The method for preparing a nano laminated aluminum-based composite material according to claim 1, characterized in that: and the layer thickness ratio of the double-layer film to the aluminum alloy foil in the fourth step is 0.13.
6. The method for preparing a nano laminated aluminum-based composite material according to claim 1, characterized in that: and the number of the nano laminated aluminum-based composite material layers in the sixth step is 12.
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CN113025962B (en) * 2021-03-23 2022-09-06 内蒙古科技大学 Silicon-based porous anodic alumina template and preparation method thereof

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