CN110551927B - In-situ self-generated aluminum-silicon gradient composite material and preparation method thereof - Google Patents
In-situ self-generated aluminum-silicon gradient composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an in-situ self-generated aluminum-silicon gradient composite material and a preparation method thereof. The in-situ authigenic aluminum-silicon gradient composite material provided by the invention is as follows: the silicon content gradually decreases from the surface to the core part to form a gradient composite material, the gradient composite material gradually transits from an outer hypereutectic high-silicon tissue layer to an inner eutectic aluminum-silicon tissue layer or from the outer hypereutectic high-silicon tissue layer to a eutectic aluminum-silicon tissue layer and then transits to a hypoeutectic aluminum-silicon tissue layer or from the outer hypereutectic high-silicon tissue layer to the eutectic aluminum-silicon tissue layer and then transits to the hypoeutectic aluminum-silicon tissue layer, and the core part is a pure aluminum layer. Aiming at the problem that massive primary crystal silicon and needle-shaped eutectic silicon exist in the aluminum-silicon gradient composite material. According to the invention, lanthanum or cerium alterant is added into pure aluminum liquid, and then reacts with silicon dioxide to obtain the aluminum-silicon gradient composite material, so that the shapes of primary silicon and eutectic silicon are improved, and finally the primary silicon and the eutectic silicon with round heads and short rods or round heads and particles are obtained.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a preparation method of an in-situ self-generated aluminum-silicon gradient composite material.
Background
The high-silicon aluminum alloy has high-temperature strength, good thermal stability and high wear resistance, and is an ideal wear-resistant material. The wear-resistant piston is widely applied to the fields of automobiles, motorcycles, military industry and the like, such as wear-resistant parts of pistons, cylinder sleeves, brake discs and the like of tanks, motorcycles and automobiles. The use of aluminum alloy engines has become an important direction for engines with cast iron cylinder liners as a comprehensive replacement for cast iron engines. However, because the microhardness difference between primary crystal silicon (microhardness value is HV 1000-1300) and matrix aluminum (microhardness value of as-cast aluminum is HV 60-100) is large, when a friction load is borne, hard primary crystal silicon particles and the surrounding matrix aluminum are mutually extruded to form a plastic deformation area, so that the primary crystal silicon falls off from the matrix, the advantages of high hardness and high wear resistance of silicon cannot be exerted, and the surface of a workpiece is damaged. In fact, this characteristic of high silicon aluminum alloys is also a critical factor limiting their applications. Accordingly, researchers have adopted casting infiltration, electromagnetic centrifugation, mechanical centrifugation, electromagnetic phase separation, and other methods to prepare aluminum-silicon gradient composite materials or have added silica particles to prepare aluminum-silicon gradient composite materials in situ. The cast-infiltration method is to adhere a casting-infiltration agent mixed with enhanced particles/powder on the inner surface of a mould shell and thermally diffuse the casting-infiltration agent into an aluminum alloy melt, but the formula of the casting-infiltration agent is complex, and the enhanced particles are generally generated in an ex-situ manner; the transition between the external enhancement layer and the internal tissue of the gradient composite material obtained by an electromagnetic centrifugal method, a mechanical centrifugal method and an electromagnetic phase separation method is sharp, is limited by the shape and the structure of a workpiece, and cannot meet the requirement of one-time forming of the workpiece with a complex structure. Therefore, a new method for preparing the aluminum-silicon gradient composite material, which can break through the limitation of the shape and the structure of the workpiece, has simple process and low cost, is developed to meet the preparation requirements of aluminum-silicon wear-resistant workpieces with various shapes and structures.
The electronic packaging material is a base material used for bearing electronic devices and interconnection thereof, and has the functions of mechanical support, sealed environment protection, signal transmission, heat dissipation, shielding and the like. Studies have shown that the failure rate of electronic devices increases dramatically with increasing operating temperature: basically every 10 increases in operating temperatureoThe lifetime of C, gallium arsenide or silicon semiconductor devices will be reduced by one third. Heat dissipation and cooling of electronic devices are typically accomplished using heat sinks, heat spreaders, and electronic packaging materials. Research and development of electronic packaging materials and components having high thermal conductivity and good overall performance have become a key technology in the field of electronic packaging and have affected the development of the electronic industry.
The aluminum-silicon gradient composite material can adjust the volume fraction of silicon in a large range to obtain high-silicon aluminum alloy materials with different properties, and has the characteristics of low thermal expansion coefficient, low density, high thermal conductivity, good electrical conductivity (excellent electromagnetic interference/radio frequency interference shielding performance), high hardness, excellent thermal mechanical stability, high compactness, easy machining, easy plating and coating protection, compatibility with a standard microelectronic assembly process and the like. Therefore, the development of new aluminum-silicon gradient composite materials is expected to meet the increasing electronic packaging requirements.
Disclosure of Invention
Based on the above, the present invention provides an aluminum-silicon gradient composite material, which has the advantages of high thermal conductivity, high mechanical strength, small density, adjustable performance, easy molding and processing, and low cost. Eutectic silicon and primary crystal silicon in the alloy can be simultaneously modified through one modifier, so that the mechanical property is optimized, and the industrial production purpose is met.
The technical scheme adopted by the invention is as follows:
an in-situ self-generated aluminum-silicon gradient composite material is a gradient composite material, wherein the silicon content is gradually reduced from the surface to the core part, at least the gradient composite material is formed by gradually transitioning from an outer layer hypereutectic high-silicon structure to an inner eutectic aluminum-silicon structure, or transitioning from the outer layer hypereutectic high-silicon structure to the eutectic aluminum-silicon structure and then to a hypoeutectic aluminum-silicon structure, or transitioning from the outer layer hypereutectic high-silicon structure to the eutectic aluminum-silicon structure and then to the hypoeutectic aluminum-silicon structure, and the core part is pure aluminum; according to the percentage content, the highest surface silicon content can reach more than 60 percent, and the lowest core silicon content is zero. And lanthanum or cerium metamorphic alloy elements are added to improve the shapes of eutectic silicon and primary crystal silicon, and the mechanical property of the material is optimized.
Wherein, the outer layer hypereutectic high silicon structure has high wear resistance, high thermal conductivity, small thermal expansion coefficient, high specific strength and small density (less than 2.7 g/cm)3) Good conductivity (excellent electromagnetic interference/radio frequency interference shielding performance), high hardness, excellent thermal mechanical stability, high compactness, easy machining, easy coating protection, compatibility with standard microelectronic assembly process and the like; the inner low-silicon or silicon-free aluminum layer has the characteristics of excellent plasticity and toughness, higher thermal conductivity and electrical conductivity, low density and the like; and the contents of silicon and aluminum in the earth crust are respectively 27.7 percent and 8.1 percent, and the content is very rich, so the aluminum-silicon alloy has low cost, no pollution to the environment, no harm to the human body and convenient recycling. Therefore, the aluminum-silicon gradient composite material can meet the requirements of wear-resistant parts and modern electronic packaging on material mechanics, thermophysical properties and process properties, and has wide application prospects in the fields of aviation, aerospace, automobiles, electronics, communication and the like.
The invention relates to a high silicon aluminum silicon alloy andthe low-silicon aluminum silicon alloy is organically combined to form the aluminum silicon gradient composite material with smooth transition of each tissue layer and no obvious interface, so that the aim of making up for deficiencies is fulfilled, on one hand, the high strength and the high wear resistance of the high-silicon aluminum silicon alloy are utilized to provide good mechanical properties for wear-resistant parts and electronic devices, on the other hand, the advantages of easy processing and forming, plating, laser welding and the like of the aluminum silicon alloy are fully exerted, and the processing of the aluminum silicon alloy into workpieces with complex shapes is facilitated. The comprehensive strength and toughness, thermal expansion coefficient and thermal conductivity of the material are adjusted by regulating and controlling proper silicon content distribution. In addition, the in-situ synthesized aluminum-silicon gradient composite material also has the characteristic of light weight (less than 2.7 g/cm)3）。
According to actual use requirements, various designs can be carried out on the gradient structure of the in-situ self-generated aluminum-silicon gradient composite material, and the thicknesses of a hypereutectic silicon tissue layer, a eutectic silicon tissue layer, a hypoeutectic tissue layer and a pure aluminum layer are adjusted by controlling the distribution of silicon content, so that the composite material with different properties can be obtained. Therefore, the in-situ synthesized aluminum-silicon gradient composite material has good controllability.
The in-situ authigenic aluminum-silicon gradient composite material not only retains the high wear resistance, high thermal conductivity and high strength of aluminum-silicon alloy, but also fully utilizes the advantages of easy processability, cladding and laser welding of aluminum-silicon. The composite material has the advantages of high wear resistance, high thermal conductivity, high mechanical strength, small density, adjustable performance, easy forming and processing and low cost, has good comprehensive performance, and can meet various index requirements of wear-resistant structures and electronic packaging. The material is particularly suitable for being used as a wear-resistant structural material and an electronic packaging material, such as wear-resistant parts of pistons, cylinder sleeves, brake discs and the like, packaging materials of high-power density microelectronics and microwave devices and the like, and the service performance of the material can be further improved through the optimized design of a gradient structure.
The percentage and distribution of eutectic silicon and primary silicon are regulated and controlled according to the diffusion temperature and the diffusion time; and lanthanum or cerium metamorphic alloy elements are added to improve the shapes of eutectic silicon and primary crystal silicon, so that the mechanical property of the material is optimized. Solves the problem that the percentage and the distribution of the eutectic silicon and the primary silicon of the traditional preparation of the aluminum-silicon gradient alloy are difficult to control, and the difficulty of simultaneously modifying the eutectic silicon and the primary silicon. The obtained material mainly comprises smooth alpha-Al dendrites, and the dendrite and the crystal boundary are modified round-head short rod-shaped silicon phases, so that the material has excellent obdurability.
Another object of the present invention is to provide a method for preparing an in-situ self-generated aluminum-silicon gradient composite material, comprising the following steps:
(1) high-purity silicon dioxide quartz glass ware with consistent workpiece shape is placed still in a heating furnace and heated to 800 DEGoC-900oPreheating and preserving heat within the range of C;
(2) melting high-purity aluminum in a high-purity aluminum oxide ceramic crucible to obtain pure aluminum liquid or according to the structural requirement required to be met by the mechanical property design requirement of the aluminum-silicon gradient alloy, and adding a certain amount of aluminum lanthanum or aluminum-cerium modifier master alloy into the aluminum liquid.
(3) Heating the aluminum liquid in the step (2) to 800oC, pouring the mixture into the high-purity silica quartz glass ware obtained in the step (1), and standing the mixture at 800 DEGoC-900oKeeping the temperature within the range of C;
(4) controlling the heat preservation time of the step (3) within the range of 0.5-5 hours, ensuring that the aluminum liquid reacts with the silicon dioxide, generating silicon atoms by self and diffusing the silicon atoms into the aluminum liquid, and finally cooling along with the furnace or air cooling;
(5) and (4) removing the residual quartz glass on the surface of the material in the step (4) to obtain the in-situ authigenic aluminum-silicon gradient composite material with the shape consistent with that of a quartz glass vessel.
The invention controls the distribution of silicon content by controlling the reaction temperature and time of the aluminum liquid and the silicon dioxide, thereby obtaining a gradient composite material with a certain gradient phase structure and meeting the performance requirement. The preparation method has the advantages of simple process, easy control and realization, smooth phase structure transition, no abrupt interface and improvement of the integral performance of the gradient composite material.
For a better understanding and practice, the invention is described in detail below with reference to the accompanying drawings.
Drawings
FIG. 1 is a flow chart of the preparation of the in-situ authigenic aluminum-silicon gradient composite material of the present invention;
FIG. 2 is a cross-sectional profile of the in-situ autogenous Al-Si gradient composite made in example 1;
FIG. 3 is a microstructure and morphology diagram of the in-situ authigenic Al-Si gradient composite material prepared in example 1;
FIG. 4 is a microstructure morphology of the in situ authigenic Al-Si gradient composite material prepared in example 1;
FIG. 5 is a cross-sectional profile of the in-situ autogenous Al-Si gradient composite made in example 2;
FIG. 6 is a microstructure and morphology diagram of the in-situ authigenic Al-Si gradient composite material prepared in example 2;
FIG. 7 is a cross-sectional profile of the in-situ autogenous Al-Si gradient composite made in example 3;
FIG. 8 is a microstructure and morphology diagram of the in-situ synthesized Al-Si gradient composite material prepared in example 3
Detailed Description
The in-situ self-generated aluminum-silicon gradient composite material is a gradient composite material which is formed by at least gradually reducing the silicon content from the surface to the core part and gradually transits from an outer hypereutectic high-silicon tissue layer to an inner eutectic aluminum-silicon tissue layer or from an outer hypereutectic high-silicon tissue layer to a eutectic aluminum-silicon tissue layer and then to a hypoeutectic aluminum-silicon tissue layer, wherein the core part is a pure aluminum layer. And lanthanum or cerium metamorphic alloy elements are added to improve the appearance of eutectic silicon or primary silicon and optimize the mechanical property of the material.
The gradient structure of the in-situ self-generated aluminum-silicon gradient composite material can be designed according to actual use requirements, and the composite material with different gradient structure structures and performances can be obtained by adjusting the diffusion reaction temperature and the diffusion reaction time and adding the alterant. Therefore, the in-situ synthesized aluminum-silicon gradient composite material has good controllability, can be processed into workpieces with complex shapes according to drawings, and realizes airtight packaging through surface plating and laser welding.
As shown in fig. 1, after completing the design of the gradient structure, the in-situ self-generated aluminum-silicon gradient composite material is prepared according to the following steps:
(1) high-purity silicon dioxide quartz glass ware with consistent workpiece shape is placed still in a heating furnace and heated to 800 DEGoC-900oPreheating and preserving heat within the range of C;
(2) melting high-purity aluminum in a high-purity aluminum oxide ceramic crucible to obtain pure aluminum liquid or according to the structural requirement required to be met by the mechanical property design requirement of the aluminum-silicon gradient alloy, and adding a certain amount of aluminum lanthanum or aluminum-cerium modifier master alloy into the aluminum liquid.
(3) Heating the aluminum liquid in the step (2) to 800oC, pouring the mixture into the high-purity silica quartz glass ware obtained in the step (1), and standing the mixture at 800 DEGoC-900oKeeping the temperature within the range of C;
(4) controlling the heat preservation time of the step (3) within the range of 0.5-5 hours, ensuring that the aluminum liquid reacts with the silicon dioxide, generating silicon atoms by self and diffusing the silicon atoms into the aluminum liquid, and finally cooling along with the furnace or air cooling;
(5) and (4) removing the residual quartz glass on the surface of the material in the step (4) to obtain the in-situ authigenic aluminum-silicon gradient composite material with the shape consistent with that of a quartz glass vessel.
Example 1
(1) High-purity silicon dioxide quartz glass ware with consistent workpiece shape is placed still in a heating furnace and heated to 800 DEGoC, preheating and heat preservation;
(2) will 800oPouring the C pure aluminum liquid into the high-purity silica quartz glass ware in the step (1), and standing at 800 DEGoC, preserving heat;
(3) controlling the heat preservation time of the step (2) for 2 hours to ensure that the aluminum liquid reacts with the silicon dioxide, silicon atoms are diffused into the aluminum liquid, and finally, cooling along with the furnace;
(4) and (4) removing the residual quartz glass on the surface of the material obtained in the step (3) to obtain the in-situ authigenic aluminum-silicon gradient composite material with the shape consistent with that of a quartz glass vessel.
(5) The macroscopic structure is shown in figure 2, and the massive primary crystal silicon is distributed on the outer ring; the microstructure splicing diagram from outside to inside is shown in fig. 3, and the smooth transition of the layered structure without obvious phase-layer interfaces can be obviously seen. The microstructure of the coexisting part of the primary crystal silicon and the eutectic silicon is shown in figure 4, and the acicular eutectic silicon and the massive primary crystal silicon are obvious without adding the alterant.
Example 2
(1) High-purity silicon dioxide quartz glass ware with consistent workpiece shape is placed still in a heating furnace and heated to 800 DEGoC, preheating and heat preservation;
(2) melting high-purity aluminum in a high-purity aluminum oxide ceramic crucible, and adding 3wt.% of lanthanum into aluminum liquid.
(3) Heating the aluminum liquid in the step (2) to 800oC, pouring the mixture into the high-purity silica quartz glass ware obtained in the step (1), and standing the mixture at 800 DEG CoC, preserving heat;
(4) controlling the heat preservation time of the step (3) for 2 hours to ensure that the aluminum liquid reacts with the silicon dioxide, silicon atoms are diffused into the aluminum liquid, and finally, cooling along with the furnace;
(5) and (4) removing the residual quartz glass on the surface of the material in the step (4) to obtain the in-situ authigenic aluminum-silicon gradient composite material with the shape consistent with that of a quartz glass vessel.
(6) The macroscopic structure diagram is shown in figure 5 (white spots are pits left for measuring hardness and caused by reflection during shooting), coarse primary crystal silicon distribution is avoided, and the structure is more uniform; the microstructure is shown in figure 6, the alterant lanthanum is added, and the silicon phase is mainly distributed among dendrites and is mainly in a round head short rod shape.
Example 3
(1) High-purity silicon dioxide quartz glass ware with consistent workpiece shape is placed still in a heating furnace and heated to 800 DEGoC, preheating and heat preservation;
(2) melting high-purity aluminum in a high-purity aluminum oxide ceramic crucible, and adding 1.00wt.% of cerium into aluminum liquid.
(3) Heating the aluminum liquid in the step (2) to 800oC, pouring the mixture into the high-purity silica quartz glass ware obtained in the step (1), and standing the mixture at 800 DEG CoC, preserving heat;
(4) controlling the heat preservation time of the step (3) for 2 hours to ensure that the aluminum liquid reacts with the silicon dioxide, silicon atoms are diffused into the aluminum liquid, and finally, cooling along with the furnace;
(5) and (4) removing the residual quartz glass on the surface of the material in the step (4) to obtain the in-situ authigenic aluminum-silicon gradient composite material with the shape consistent with that of a quartz glass vessel.
(6) The macroscopic structure diagram is shown in figure 7 (white spots are pits left for measuring hardness and caused by reflection during shooting), coarse primary crystal silicon distribution is avoided, and the structure is more uniform; the microstructure is shown in figure 8, the silicon phase is mainly distributed among dendrites and is mainly round-head granular by adding the modifying agent cerium.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (5)
1. The preparation method of the in-situ self-generated aluminum-silicon gradient composite material is characterized by comprising the following steps of: the method comprises the following steps:
(1) standing a high-purity silica quartz glass ware with a consistent workpiece shape in a heating furnace, heating to 800-900 ℃, and preheating and preserving heat;
(2) melting high-purity aluminum in a high-purity aluminum oxide ceramic crucible to obtain pure aluminum liquid or an organization requirement required to be met according to the mechanical property design requirement of the aluminum-silicon gradient alloy, and adding a certain amount of aluminum lanthanum or aluminum cerium modifier master alloy into the aluminum liquid;
(3) heating the aluminum liquid in the step (2) to 800 ℃, pouring the aluminum liquid into the high-purity silica quartz glassware in the step (1), standing the high-purity silica quartz glassware and preserving heat within the range of 800-900 ℃;
(4) controlling the heat preservation time of the step (3) within the range of 0.5-5 hours, ensuring that the aluminum liquid reacts with the silicon dioxide, generating silicon atoms by self and diffusing the silicon atoms into the aluminum liquid, and finally cooling along with the furnace or air cooling;
(5) and (4) removing the residual quartz glass on the surface of the material in the step (4) to obtain the in-situ authigenic aluminum-silicon gradient composite material with the shape consistent with that of a quartz glass vessel.
2. An in-situ synthesized Al-Si gradient composite material prepared by the method according to claim 1, wherein: the silicon content is gradually reduced from the surface to the core part, the outer layer hypereutectic high-silicon structure is gradually transited to the inner eutectic aluminum-silicon structure, or the outer layer hypereutectic high-silicon structure is transited to the eutectic aluminum-silicon structure and then transited to the hypoeutectic aluminum-silicon structure, and finally the core part is the pure aluminum gradient composite material; according to the percentage content, the highest surface silicon content is 60%, the lowest core silicon content is zero, and the morphology of eutectic silicon or hypereutectic silicon is improved by adding lanthanum or cerium metamorphic alloy elements, so that the mechanical property of the material is optimized.
The added lanthanum or cerium modified alloy element is added in the mode of aluminum lanthanum or aluminum cerium master alloy, wherein the addition amount of lanthanum is 2.50-4.00 wt.%, and the addition amount of cerium is 0.80-1.20 wt.%.
3. The in-situ autogenous aluminum silicon gradient composite according to claim 2, characterized in that: the hypereutectic high-silicon tissue layer is primary crystal silicon and eutectic silicon, the eutectic silicon tissue layer is eutectic silicon, the hypoeutectic silicon tissue layer is primary crystal alpha aluminum and eutectic silicon, the core part is pure aluminum, the eutectic silicon and the primary crystal silicon are enriched between alpha-Al dendrites, the acicular eutectic silicon is converted into fine reticular eutectic silicon, and the petal-shaped sharp-angle primary crystal silicon is converted into fine short rod-shaped primary crystal silicon.
4. The in-situ autogenous Al-Si gradient composite according to claim 3, characterized in that: the width of each alloy layer is determined by the component distribution of silicon diffusion, each tissue layer is in smooth transition without obvious interfaces, and eutectic silicon and primary crystal silicon are changed from the morphology with poor mechanical property to the morphology with excellent mechanical property.
5. The in situ autogenous al-si gradient composite according to any of claims 2-4, characterized in that: the quantity of primary crystal silicon phase and eutectic silicon phase is gradually reduced from the surface to the core part, the quantity of primary crystal alpha aluminum phase and pure aluminum is gradually increased, and lanthanum or cerium metamorphic alloy elements are added to change the shapes of eutectic silicon and primary crystal silicon.
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