CN114318232A - Al-coated Al3Ti intermetallic compound nano-particles and preparation method thereof - Google Patents
Al-coated Al3Ti intermetallic compound nano-particles and preparation method thereof Download PDFInfo
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Abstract
Al-coated Al3A Ti intermetallic compound nano-particle material and its preparing process, which features use of physical vapor deposition coating technique, co-deposition of Al and Ti components, and control of Al-Ti ratio and Al-smelting point near Al-smelting point3The two phases of Ti and Al realize separation growth at high temperature and prepare Al3A two-phase structure layer consisting of Ti and Al and a multilayer structure composite film formed by mutually and alternately overlapping Al layers. The Al with wide shape and size variation range and Al-coated surface is prepared by the invention3The Ti nano-particle material is not only easy to be added into molten metal, but also not easy to generate particle aggregation, can obtain a composite material with uniformly dispersed nano-particles, and obviously improves the metal matrix composite material, in particular Al matrix composite materialThe properties of the material.
Description
Technical Field
The invention relates to a technology in the field of metal-based composite nano materials, in particular to Al-coated Al3Ti intermetallic compound nano-particles and a preparation method thereof.
Background
The particle-reinforced metal-based composite material has performance advantages and is more and more widely applied in modern industry, however, when the diameter is reduced to the nanometer level, the specific surface area of the particles is increased sharply, and the particles are difficult to be added into molten metal and obtain uniform dispersion due to surface adsorption, pollution and the like, so that the particle-reinforced metal-based composite material becomes a key difficulty and a problem which are urgently needed to be overcome in the preparation of the nanoparticle-reinforced metal-based composite material. The prior art has good effect of coating the particles with metal to improve the fusion of micron-scale particles into molten metal, but the method is difficult to be used for nano-scale particles because the surfaces of the nano-particles are difficult to treat and are completely covered by the metal due to the extremely small diameter and huge amount of interfaces of the nano-particles, and on the other hand, for some metals with stable oxides, such as Al, Mg, Ti and the like, even if the full-covering coating of the particles can be realized, new oxide films (Al) can be generated on the coating surfaces of the metals2O3、MgO、TiO2Etc.), the problem has not yet been solved. Therefore, in the research and production of the present nanoparticle reinforced metal matrix composite, there is an urgent need for a nanoparticle whose surface is completely coated with metal, which not only requires the particle to have the characteristics of controllable shape and high dimensional accuracy and dimensional uniformity, but also requires that no new metal-coated surface is generatedStabilizing the oxide film, but such nanoparticles and their preparation techniques remain blank.
Disclosure of Invention
The invention provides Al-coated Al, aiming at the problems that the shape and size of ceramic nanoparticles are not wide in variation range and low in size precision and size uniformity in the existing preparation technology of particle-reinforced metal-based composite materials, and particularly, the nanoparticles are difficult to be added into molten metal and uniformly distributed3The Ti intermetallic compound nano-particles and the preparation method thereof have the characteristics of wide variation range of shapes and sizes, high size precision and size uniformity and coating by metal Al without a surface oxide film. These are mixed with Al3Al in the form of Ti/Al composite film3The Ti nano-particles have the advantage of being easy to add into molten metal without aggregation, and can obtain the metal-based composite material with uniformly dispersed nano-particles, thereby obviously improving the performance of the composite material, in particular the Al-based composite material.
The invention is realized by the following technical scheme:
the invention relates to Al with Al-coated surface3A process for preparing the nm-class particles of Ti intermetallic compound includes such steps as codepositing Al and Ti components by physical vapor deposition, and controlling the ratio of Al to Ti and the temp of substrate close to Al smelting point3The two phases of Ti and Al realize separation growth at high temperature and prepare Al3A two-phase structure layer consisting of Ti and Al and a multilayer structure composite film formed by mutually and alternately overlapping Al layers.
The two-phase structure layer is made of mutually insoluble Al3Ti nano columnar crystal phase and Al3The Ti nano columnar crystal is completely coated by Al.
The Al layer adopts a single-component deposition method to block Al3And growing the Ti nano columnar crystal, and further forming a multilayer structure composite film with two phase structure layers and an Al layer which are alternately overlapped by repeated deposition.
The physical vapor deposition coating technology adopts physical methods such as but not limited to vacuum evaporation coating, sputtering coating and the like to gasify metal and then deposit the metal on the surface of a solid to form a film.
The codeposition method of the Al and Ti components comprises the following steps: in the physical vapor deposition process, two metals of Al and Ti are simultaneously gasified and are jointly deposited on a substrate to form a binary alloy film by an Al and Ti gasification source or an Al-Ti alloy gasification source, and the proportion of the two components of Al and Ti is controlled as follows: the atomic percentage of Ti in the film is in the range of 6-12 at.%, and is obtained by controlling the power of two gasification sources of Al and Ti or the component ratio of Al and Ti in the Al-Ti alloy gasification source.
The base material is as follows: and thin metal sheets of Al, Ni, Ti, etc.
The substrate temperature close to the melting point of Al is as follows: throughout the deposition of the film, the substrate was heated and maintained in the range of 600-650 ℃. The invention relates to Al-coated Al prepared by the method3Ti intermetallic compound nanoparticles, the Al3Al with Ti intermetallic compound nano particles in multilayer structure composite film3In the Ti/Al two-phase structure layer, no oxide film and other adsorbed or polluted substances exist on the surface of the coated Al.
Unlike the coating of powdered particles with metals, which are commonly used, these Al-coated Al3Al in which Ti nanoparticles are bonded by Al and arranged in order in the multilayer-structure composite film3In the Ti/Al two-phase structure layer, the problem that the surface of the Al coating layer of common powder particles is oxidized is solved.
The Al is3The Ti intermetallic compound nano particles are granular or needle-rod-shaped particles with the average diameter of 10-30nm and the length of 30-1000nm, and the length error of the particles is less than +/-3 nm.
The Al is3The length of Ti intermetallic compound nanoparticles is controlled and varied by the thickness of the two-phase structure layer to make Al3The Ti nanoparticles have the characteristics of wide length variation range and high size precision and size uniformity.
The present invention relates to the Al coated with Al3Use of Ti intermetallic compound nanoparticles for Al3TiThe metal matrix composite material reinforced by nano particles, especially Al matrix composite material, can make Al3The Ti nano-particles are easy to be added into the metal melt and realize uniform dispersion in the matrix, and the performance of the composite material can be obviously improved.
Technical effects
The invention solves the problem that the prior art is difficult to obtain the Al with variable needle bar-shaped length and high size uniformity3Ti intermetallic compound nano particles, particularly the defect of complete coating of the nano particles, and the defect that the Ti intermetallic compound nano particles are difficult to add and uniformly distribute in a metal melt because a new oxide film is generated on the surface of a coated metal, particularly the surface of Al after the powder particles are coated are overcome, and the Al-Ti intermetallic compound nano particles are prepared by selecting the specific ratio of the Al component to the Ti component, particularly the substrate temperature close to the melting point of Al3Growing a structural layer by separating Ti nano columnar crystal and Al, and growing Al by using a metal Al layer3Blocking of Ti columnar crystals to control acicular Al3The technical means of Ti length are obtained, in the multi-layer structure composite film formed by two-phase structure layer and Al layer3The length variation range of Ti intermetallic compound nano particles is very wide, is 5-1000nm, and can be controlled and changed, so that Al with different shapes such as granular shape, cylindrical shape to needle shape and the like can be obtained3Ti nanoparticles, and these nanoparticles also have the advantage of high dimensional accuracy and dimensional uniformity. The above Al provided by the present invention3The Ti nanoparticles provide a large space for the metal matrix composite material to select the shape and size of the reinforcing body particles. In particular, the adoption of Al to Al is realized3The complete coating of the Ti particles and the elimination of the surface oxide film coating Al. Such Al-coated Al3The Ti nano-particles have the advantages of being easy to add into the metal solution and realizing uniform distribution, can effectively and obviously improve the performance of the metal-based composite material, particularly the mechanical property of the Al-based composite material, and has important value for promoting the development and application of the metal-based composite material.
Drawings
FIG. 1 is a drawing of the present inventionThe Al-coated Al obtained3A structural schematic diagram of the Ti intermetallic compound nanoparticle multilayer structure composite film;
in the figure: 1Al3Ti nano particles, a 2Al matrix, a 3Al layer and 4 base materials;
FIG. 2 is a schematic diagram of the observation result of a two-phase structure of the composite film from the direction of the film surface by a transmission electron microscope;
in the figure: the dark granular region is Al3The cross section of the Ti nano columnar crystal is provided with an Al matrix in a light color area.
Detailed Description
Example 1
In this embodiment, a multi-target magnetron sputtering apparatus is adopted, and two independent cathodes are used to control a pure Al target and a pure Ti target, and the method specifically includes the following steps:
step 1) by pumping the vacuum chamber to 10 deg.C-3Heating the pure Al base material in the vacuum chamber after Pa is lower than Pa (keeping the temperature at 600 ℃ in the whole deposition and coating process), and sputtering and depositing an Al transition layer with the thickness of 100nm on the Al base material;
step 2) filling Ar gas and keeping the pressure at 6 multiplied by 10-1Pa, depositing an Al layer on the Al transition layer; then Ar gas is filled in and the pressure is kept at 6 x 10-1Pa, depositing Al on the Al layer by a co-deposition method3The method comprises the following steps of forming a two-phase structure layer consisting of Ti and Al, controlling the Ti content in the two-phase structure layer by adjusting the power of an Al target and the power of a Ti target, controlling the thickness of the Al layer and the thickness of the two-phase structure layer by the deposition coating time, and carrying out cyclic treatment until a multi-layer structure composite film which is alternately overlapped is obtained.
And 3) plating a 100nm Al covering layer on the surface of the deposited multilayer structure composite film.
In this example, the thickness of the two-phase structure layer was 1000nm, the thickness of the Al layer was 10nm, and the total thickness of the multi-layer structure composite film was about 10 μm by controlling the deposition temperature and the coating time of each layer, so as to obtain acicular Al coated and bonded with Al as shown in FIG. 13Ti nanoparticles, the length of the particles being 1000nm and the average diameter being 10 nm. The observation of the two-phase structure layer of the multilayer structure composite film by a transmission electron microscope is shown in FIG. 2.
Example 2
In this example, compared with example 1, the substrate temperature was maintained at 625 deg.C, the thickness of the two-phase structure layer was 100nm, the thickness of the Al layer was 10nm, and the total thickness of the multi-layer structure composite film was about 10 μm by controlling the deposition coating time, and cylindrical Al coated with Al and bonded together was obtained3Nanoparticles of Ti, Al3The average diameter of the Ti nanoparticles is 20nm, and the length is 100 nm.
Example 3
In this example, compared with example 1, the substrate temperature was maintained at 650 ℃, the thickness of the two-phase structure layer was 30nm, the thickness of the Al layer was 10nm, and the total thickness of the multi-layer structure composite film was about 10 μm by controlling the deposition coating time, so as to obtain equiaxed Al coated and bonded with Al3Nanoparticles of Ti, Al3The average diameter and length of the Ti nanoparticles were 30 nm.
In conclusion, the present invention is based on Al which has a large difference in melting point and temperature and which is wettable but not solid-soluble with each other3The combination of two-phase materials with specific ratio of Ti and Al, in particular, adopts the blank of the prior art that the substrate temperature is deposited at the temperature close to the melting point of Al, and obtains the material with Al3A two-phase structure layer with Ti columnar crystals and Al separated and grown, and further adopts an Al-only plating layer to block Al in the two-phase structure layer3The multilayer structure composite film method for Ti columnar crystal growth obtains Al which is coated by Al and coated with Al surface oxide film is eliminated3Ti nanoparticles, and such Al3The Ti intermetallic compound nanoparticles are also characterized by a wide range of length variation and high dimensional accuracy and dimensional uniformity.
The foregoing embodiments may be modified in many different ways by those skilled in the art without departing from the spirit and scope of the invention, which is defined by the appended claims and all changes that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (10)
1. Al with Al-coated surface3Preparation method of Ti intermetallic compound nanoparticle materialThe method is characterized in that a physical vapor deposition coating technology is adopted, the Al and Ti components are co-deposited by a method of controlling the proportion of the Al and Ti components and the temperature of the base material close to the melting point of the Al3The two phases of Ti and Al realize separation growth at high temperature and prepare Al3A two-phase structure layer consisting of Ti and Al and a multilayer structure composite film formed by mutually and alternately overlapping Al layers.
2. Al-clad Al according to claim 13The preparation method of Ti intermetallic compound nano-particles is characterized in that the two-phase structure layer is formed by mutually insoluble Al3Ti nano columnar crystal phase and Al3The Ti nano columnar crystal is completely coated by Al.
3. Al-clad Al according to claim 13Ti intermetallic compound nano particles and a preparation method thereof, and is characterized in that the Al layer adopts a component deposition method to block Al3And (3) growing Ti nano columnar crystals, and further forming a nano multilayer structure composite film with a two-phase structure layer and an Al layer which are alternately overlapped by repeated deposition.
4. Al-clad Al according to claim 13The Ti intermetallic compound nano-particles and the preparation method thereof are characterized in that the physical vapor deposition coating technology adopts vacuum evaporation coating and sputtering coating to gasify metal and then deposit the metal on the surface of a solid to form a film.
5. Al-clad Al according to claim 13The Ti intermetallic compound nano-particles and the preparation method thereof are characterized in that the codeposition method of the Al and Ti components is as follows: in the physical vapor deposition process, two metals of Al and Ti are simultaneously gasified and jointly deposited on a substrate to form a binary alloy film by two gasification sources of Al and Ti or an Al-Ti alloy.
6. According to claim 1The Al-coated Al3The Ti intermetallic compound nano-particles and the preparation method thereof are characterized in that the control of the proportion of the Al component and the Ti component refers to that: the atomic percentage of Ti in the film is in the range of 6-12 at.%, and is obtained by controlling the power of two gasification sources of Al and Ti or the component ratio of Al and Ti in the Al-Ti alloy gasification source.
7. Al-clad Al according to claim 13The Ti intermetallic compound nano-particles and the preparation method thereof are characterized in that the base material is as follows: al, Ni or Ti flakes.
8. Al-clad Al according to claim 1 or 73The Ti intermetallic compound nano-particles and the preparation method thereof are characterized in that the substrate temperature close to the Al melting point refers to that: throughout the deposition of the film, the substrate was heated and maintained in the range of 600-650 ℃.
9. Al-coated Al prepared by the method according to any one of claims 1 to 83Ti intermetallic compound nanoparticles, characterized in that the Al is3Al with Ti intermetallic compound nano particles in multilayer structure composite film3In the Ti/Al two-phase structure layer, no oxide film and other adsorbed or polluted substances exist on the surface of the coated Al;
the Al is3The Ti intermetallic compound nano particles are in a granular or needle-bar structure with the average diameter of 10-30nm and the length of 30-1000nm, and the error of the length of the particles is less than +/-3 nm.
10. Al-coated Al according to any of the preceding claims3Use of Ti intermetallic compound nanoparticles for Al3Al-based composite material reinforced with Ti nanoparticles3The Ti nano-particles are easy to be added into the metal melt and realize uniform dispersion in the matrix so as to obviously improve the performance of the composite material.
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