CN114318041B - SiC particle reinforced aluminum-based composite bar with size gradient and preparation method thereof - Google Patents
SiC particle reinforced aluminum-based composite bar with size gradient and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of high-temperature high-strength wear-resistant metal materials, and particularly relates to a SiC particle reinforced aluminum-based composite bar with a size gradient and a preparation method thereof. The method comprises the following steps: (1) Preparing a submicron SiC particle reinforced aluminum matrix composite material by adopting an in-situ synthesis method, hot extruding the composite material into bars with required diameters, and placing the bars into a die groove with a cylindrical cavity; (2) Adding preheated SiC particles with the diameter of 2-3 mu m into the aluminum melt for mechanical stirring; (3) Pouring the mixture into a mold after stirring, filling a cavity, air-cooling to room temperature to obtain a composite sample, and hot-extruding the composite sample again to obtain a bar with a specified diameter; (4) homogenizing annealing the obtained sample. The SiC particle reinforced aluminum matrix composite material with the size gradient structure can realize the high-strength performance of the core part of the bar, the heat resistance and wear resistance of the surface layer of the bar, and certain plastic toughness can be ensured, so that the comprehensive performance of the material is integrally optimized.
Description
Technical Field
The invention belongs to the field of high-temperature high-strength wear-resistant metal materials, and particularly relates to a SiC particle reinforced aluminum-based composite bar with a size gradient and a preparation method thereof.
Background
With the progress of technology and the continuous development of industrial production, the metal matrix composite material gradually replaces the traditional metal material, and has great potential in the fields of aerospace, military national defense, mechanical transportation and the like. The metal matrix composite material is formed by compounding one or more materials serving as a reinforcing body through various technological means by taking metal as a matrix, and the respective performance advantages of the matrix and the reinforcing body are combined. Aluminum has the characteristics of light weight, small density, good plasticity and the like, so that the aluminum-based composite material becomes the most common metal-based composite material and is widely applied to aspects of production and living.
The particle reinforced aluminum matrix composite is the most widely studied and most mature metal matrix composite at present. The SiC particle reinforced aluminum matrix composite material has light weight, high specific strength, high specific modulus, low thermal expansion coefficient and good abrasion resistance, and becomes a hot spot of current research. The preparation methods of the SiC particle reinforced aluminum matrix composite material are numerous: stirring casting method, powder metallurgy method, spray deposition method, in situ synthesis method, etc. Different preparation methods have different characteristics, are suitable for different environments, and can influence the performance of the material more or less. The size of the SiC particles has a critical impact on the performance of the composite. The nano-sized and submicron particles can improve the strength, and the micron particles have good wear resistance while ensuring certain strength.
"Ceramic waste SiC particle-reinforced Al matrix composite brake materials with a high friction coefficient"( High coefficient of friction ceramic waste SiC particle reinforced aluminum matrix composite brake material published by k.l. zheng et al) in one paper, studies show that: compared with aluminum alloy, the SiC particle reinforced aluminum matrix composite material has improved Brinell hardness and bending strength, and ceramic particles participate in the formation of a mechanical transfer layer of the SiC particle reinforced aluminum matrix composite material, which is beneficial to preserving superfine abrasive dust on the wear surface so as to effectively protect the matrix and provide a high friction coefficient and ensure good wear resistance.
However, the present materials are not limited to single excellent performance, and the appearance of the gradient structure can enable the properties and functions of the materials to be changed in a gradient manner so as to meet more complex and changeable working conditions. For example: the Chinese patent with publication number CN107805728A discloses an aluminum-based composite material with a multi-level gradient structure, wherein the content of B 4 C particles is in gradient change, and a preparation method thereof, and the aluminum-based composite material is a high-density block material. The composite material plays a role in load transmission due to the gradient change of the B 4 C particle reinforced phase. However, this preparation method has the following disadvantages: the B 4 C particle reinforced aluminum matrix composite material prepared by adopting the powder metallurgy method has complex process, higher cost of raw materials and equipment, and the plasticity of the second layer material can be reduced and the secondary processing formability is poor along with the increase of the content of the B 4 C particles. In the preparation process, the particle size of B 4 C is greatly different from that of the matrix, and the particles are easily unevenly distributed in the matrix. In addition, the shape and the size of the material prepared by the powder metallurgy method are limited, and the material cannot be prepared into large-scale products.
Disclosure of Invention
The invention aims to provide an SiC particle reinforced aluminum matrix composite bar with a gradient structure and a preparation method thereof. The gradient structure composite bar of the submicron SiC aluminum-based composite material wrapped by the micron SiC particle reinforced aluminum-based composite material is obtained by controlling the particle size of the SiC reinforced phase to be in gradient change, so that the core of the bar has high strength performance, the heat resistance and the wear resistance of the surface layer of the bar are realized, and meanwhile, certain plastic toughness is ensured, so that the comprehensive performance of the material is integrally optimized.
The technical solution for realizing the purpose of the invention is as follows: a size gradient SiC particle reinforced aluminum-based composite bar consists of a core and an outer layer, wherein the core contains submicron SiC particles prepared by an in-situ synthesis method, and the outer layer contains micron SiC particles cast by stirring.
Further, the thickness of the outer layer is less than the diameter of the core.
The method for preparing the composite bar comprises the following steps:
Step (1): preparing a submicron SiC particle reinforced aluminum matrix composite material by adopting an in-situ synthesis method, and hot extruding the composite material into bars with required diameters;
Step (2): placing the mixture into a mold groove with a cylindrical cavity, and adding preheated micron-sized SiC particles into aluminum melt for mechanical stirring;
step (3): pouring the mixture into a mould after stirring, filling a cavity, and performing hot extrusion again to obtain a bar with a required diameter after air cooling to room temperature;
Step (4): and (3) carrying out homogenization heat treatment on the bar material obtained in the step (3).
Further, the preparation of the submicron SiC particle reinforced aluminum matrix composite material by adopting the in-situ synthesis method in the step (1) is specifically as follows: and (3) putting the industrial pure aluminum powder, the industrial pure silicon powder and the graphite powder into a ball mill according to the required proportion for ball milling and sintering.
Further, the specific process parameters of ball milling and sintering are as follows: ball milling for 1 h+/-10 min at a rotating speed of 350-400 r/min; sintering in an argon protection atmosphere furnace at 600-800 ℃ for 2 h+/-30 min.
Further, "hot extrusion into a rod of a desired diameter" in step (1) is specifically: the process is carried out at 300-400 ℃ under the protection of inert gas, and the diameter of the obtained bar is 5-20 mm.
Further, the oxide skin on the surface of the bar is removed before the bar is placed in the die groove with the cylindrical cavity in the step (1).
Further, "mechanical stirring" in the step (2) is specifically: stirring temperature is 680-720 ℃, stirring time is 25+/-10 min, stirring speed is 600-900 rpm, and reversing interval time is 5min;
the particle diameter of the "micron-sized SiC particles" in the step (2) is 2 to 3 μm.
Further, in the step (3) 'hot extrusion into bars with required diameters' is specifically: the process is carried out at 300-450 ℃ under the protection of inert gas, and the diameter of the obtained bar is 10-30 mm.
Further, the homogenizing heat treatment in the step (4) specifically comprises the following steps: and then carrying out homogenizing annealing treatment for 2-3 hours at 400-500 ℃.
Further, repeating the steps (2) - (3), and determining the size of the SiC particles added in the step (2) according to the requirement to obtain the multi-layer SiC particle size gradient structure composite material.
Compared with the prior art, the invention has the remarkable advantages that:
(1) The inner core and the outer layer of the composite bar are both made of SiC particle reinforced aluminum matrix composite materials, the inner core is prepared by adopting an in-situ synthesis method, siC particles can be more uniformly and diffusely distributed in an aluminum matrix, and the particles are fine and are not easy to agglomerate. Submicron-level SiC particles are difficult to directly pass through when dislocation encounters reinforcing phase particles by using an Orowan reinforcing mechanism, so that the particles are bypassed, dislocation loops released by dislocation lines increase dislocation density and strength, and the high-strength performance of the material inner core is realized. The outer layer adopts a stirring casting mode, micron-grade SiC particles are added into the aluminum matrix, and the load can be transferred to the reinforcing body from the matrix through interfacial shear stress, so that the strength of the bar is improved again, and the overall strength of the bar is higher than that of a common reinforcing body bar and a bar with graded content.
(2) The surface layer of the bar prepared by the invention is an SiC particle reinforced aluminum matrix composite material with the particle size of 2-3 mu m, siC particles have bearing property, the soft aluminum matrix is prevented from participating in the friction process as much as possible, and the abrasion of the matrix is reduced, so that the wear resistance of the material is improved; when the aluminum matrix is inevitably worn, the SiC particles are exposed, and are hard particles with the micron-sized particles, so that the SiC particles are not easy to wear and drop, and the wear resistance of the material is improved.
(3) The invention adopts two steps of stirring casting and hot extrusion to successfully combine the inner core and the outer layer to obtain the size gradient bar with strong inner and outer layer combining capability and good combining interface; the stirring casting is used as an extra-particle addition method, the size of the extra-particle can be flexibly selected, the used equipment is simple, and the required cost is low; after the composite casting is obtained, the composite casting is subjected to hot extrusion again, so that not only can the preset shape and size be realized, but also the binding force of the inner layer and the outer layer can be further enhanced; in addition, the casting is subjected to the three-dimensional compressive stress in the plastic deformation area, and the shearing force caused by deformation can lead SiC particles to be distributed more uniformly, matrix grains to be thinned, holes and other defects to be eliminated, thereby effectively preventing crack source from sprouting and crack propagation, being beneficial to exerting the plasticity of the material and obviously improving the thermoforming performance of the material. Similarly, the material with a multilayer gradient structure can be flexibly realized by adopting the mode, and meanwhile, the shape and the size of the material are easy to regulate and control.
(4) The invention finally carries out homogenization heat treatment, reduces the segregation of chemical components and the tissue non-uniformity of the bar, removes residual stress, and further ensures that the material has certain plasticity and toughness on the basis of realizing high-strength wear resistance of the bar, thereby obtaining good comprehensive mechanical properties.
Drawings
FIG. 1 is a schematic cross-sectional view of an aluminum-based composite rod with SiC particle size gradient obtained by the present invention.
Reference numerals illustrate:
1-Al matrix, 2-submicron SiC particles, 3-micron SiC particles.
Detailed Description
The SiC particle reinforced aluminum-based composite bar with the gradient structure comprises industrial pure aluminum powder, industrial pure silicon powder, graphite powder, siC particles and the like. Firstly, putting industrial pure aluminum powder, industrial pure silicon powder and graphite powder into a ball mill according to a certain proportion, ball milling, sintering, extruding into a rod-shaped material with a specified diameter, and putting the rod-shaped material serving as an inner core into a pre-prepared die groove. The preheated micron-sized SiC particles are then added to the aluminum melt for mechanical agitation. And casting the mixture into a mould after stirring is finished, combining the outer-layer micron-sized SiC particle reinforced aluminum matrix composite material with the inner core, cooling and demoulding. And then the composite bar with the gradient structure, which has good bonding surface, high temperature heat resistance, wear resistance and easy regulation of shape and size, is obtained through extrusion deformation and homogenization heat treatment.
The preparation method of the SiC particle reinforced aluminum matrix composite bar with the size gradient specifically comprises the following steps:
(1): firstly, preparing raw materials of industrial pure aluminum powder (99.7 wt%), industrial pure silicon powder (99.9 wt%) and graphite powder according to a certain proportion, fully mixing the raw materials, and placing the mixture into a planetary ball mill for ball milling for 1 h+/-10 min at the rotating speed of 350-400 r/min. Sintering in an argon protective atmosphere furnace after ball milling is finished, wherein the sintering temperature is 600-800 ℃ and the time is 2 h+/-30 min. The sintered sample is hot extruded into bars with the diameter of 5-20 mm at the temperature of 300-400 ℃, and inert gas protection is needed in the process.
(2): And polishing the prepared bar so as to remove the oxide layer on the outer surface, and then placing the bar into a die groove with a cylindrical cavity.
(3): Melting industrial pure aluminum ingot into aluminum melt at 660-700 ℃, and adding preheated micron-sized SiC particles into the aluminum melt for mechanical stirring. The stirring temperature is 630 ℃, the stirring time is 25+/-10 min, the stirring speed is 600-900 rpm, and the reversing interval time is 5min.
(4): Pouring the mixture into a mold after stirring, filling a cavity, and air-cooling to room temperature to obtain an as-cast composite sample.
(5): And (3) hot extruding the as-cast sample of the as-cast composite sample again to obtain a diameter of 10-30 mm, and carrying out the hot extrusion at 300-450 ℃ under the protection of inert gas.
(6): The obtained sample is subjected to homogenizing annealing treatment for 2 to 3 hours at the temperature of 400 to 500 ℃.
Example 1
(1): Firstly, preparing industrial pure aluminum powder, industrial pure silicon powder and graphite powder into raw materials according to a certain ratio, fully mixing the raw materials, and then ball-milling for 1h at the rotating speed of 350r/min. Sintering in an argon protective atmosphere furnace after ball milling is finished, wherein the sintering temperature is 650 ℃ and the time is 2 hours. Hot extruding the sintered sample into bars with the diameter of 15mm at the temperature of 300 ℃ and the extrusion ratio of 6;
(2): polishing the prepared bar to remove an oxide layer on the outer surface, and then placing the bar into a cylindrical groove at the bottom of a die, wherein the inner diameter of the die is 60mm, the depth of the die is 300mm, the diameter of the groove is 15mm, and the depth of the groove is 10mm;
(3): melting industrial pure aluminum ingot into aluminum melt at 680 ℃, adding preheated micron-sized SiC particles into the aluminum solution, and mechanically stirring. Stirring temperature is 700 ℃, stirring time is 20mins, stirring speed is 700rpm, and reversing interval time is 5mins;
(4): pouring the mixture into a mold after stirring is completed, filling a cavity, and air-cooling to room temperature to obtain an as-cast composite sample;
(5): hot extruding the cast composite sample again to form bars with the diameter of 24mm, wherein the extrusion temperature is 350 ℃, and the extrusion ratio is 6.25;
(6): the resulting sample was homogenized at 400℃for 2h.
The inner and outer layers of the prepared gradient structure bar are all made of SiC particle reinforced aluminum matrix composite materials, as shown in figure 1, and the radius ratio of the inner and outer layers is 1:1.6.
Example 2
(1): Firstly, preparing industrial pure aluminum powder, industrial pure silicon powder and graphite powder into raw materials according to a certain ratio, fully mixing the raw materials, and then ball-milling for 1h at the rotating speed of 350r/min. Sintering in an argon protective atmosphere furnace after ball milling is finished, wherein the sintering temperature is 600 ℃ and the time is 2 hours. Hot extruding the sintered sample into bars with the diameter of 8mm at the temperature of 350 ℃ and the extrusion ratio of 6;
(2): polishing the prepared bar to remove an oxide layer on the outer surface, and then placing the bar into a cylindrical groove at the bottom of a die, wherein the inner diameter of the die is 25mm, the depth of the die is 280mm, the diameter of the groove is 8mm, and the depth of the groove is 10mm;
(3): melting industrial pure aluminum ingot into aluminum melt at 690 ℃, adding preheated micron-sized SiC particles into the aluminum melt, and mechanically stirring. Stirring temperature is 700 ℃, stirring time is 25min, stirring speed is 700rpm, and reversing interval time is 5min;
(4): pouring the mixture into a mold after stirring is completed, filling a cavity, and air-cooling to room temperature to obtain an as-cast composite sample;
(5): hot extruding the cast composite sample again to form a bar with the diameter of 10mm, wherein the extrusion temperature is 400 ℃, and the extrusion ratio is 6.25;
(6): the resulting sample was homogenized at 450℃for 2h.
The inner and outer layers of the prepared gradient structure bar are all made of SiC particle reinforced aluminum matrix composite materials, and the radius ratio of the inner layer to the outer layer is 1:1.25.
Example 3
(1): Firstly, preparing industrial pure aluminum powder, industrial pure silicon powder and graphite powder into raw materials according to a certain ratio, fully mixing the raw materials, and then ball-milling for 1h at the rotating speed of 350r/min. Sintering in an argon protective atmosphere furnace after ball milling is finished, wherein the sintering temperature is 800, and the time is 2h. Hot extruding the sintered sample into bars with the diameter of 20mm at the temperature of 400 ℃ and the extrusion ratio of 6.5;
(2): polishing the prepared bar to remove an oxide layer on the outer surface, and then placing the bar into a cylindrical groove at the bottom of a die, wherein the inner diameter of the die is 68mm, the depth of the die is 350mm, the diameter of the groove is 20mm, and the depth of the groove is 10mm;
(3): melting industrial pure aluminum ingot into aluminum solution at 690 ℃, adding preheated micron-sized SiC particles into the aluminum solution, and mechanically stirring. Stirring temperature is 680 ℃, stirring time is 30min, stirring speed is 800rpm, and reversing interval time is 5min;
(4): pouring the mixture into a mold after stirring is completed, filling a cavity, and air-cooling to room temperature to obtain an as-cast composite sample;
(5): hot extruding the cast composite sample again to form a bar with the diameter of 28mm, wherein the extrusion temperature is 400 ℃, and the extrusion ratio is 5.9;
(6): the resulting sample was homogenized at 450℃for 2h.
The inner and outer layers of the prepared gradient structure bar are all made of SiC particle reinforced aluminum matrix composite materials, and the radius ratio of the inner layer to the outer layer is 1:1.4.
Claims (1)
1. The SiC particle reinforced aluminum-based composite bar with the size gradient is characterized by comprising a core part and an outer layer, wherein the core part contains submicron SiC particles prepared by an in-situ synthesis method, and the outer layer contains micron SiC particles cast by stirring;
The method comprises the following steps:
Step (1): preparing a submicron SiC particle reinforced aluminum matrix composite material by adopting an in-situ synthesis method, hot extruding the composite material into bars with required diameters, and placing the bars into a die groove with a cylindrical cavity;
step (2): adding the preheated micron-sized SiC particles into the aluminum melt for mechanical stirring;
step (3): pouring the mixture into a mould after stirring, filling a cavity, and performing hot extrusion again to obtain a bar with a required diameter after air cooling to room temperature;
Step (4): homogenizing the bar obtained in the step (3);
the step (1) of preparing the submicron SiC particle reinforced aluminum matrix composite material by adopting an in-situ synthesis method comprises the following concrete steps: placing the industrial pure aluminum powder, the industrial pure silicon powder and the graphite powder into a ball mill according to the required proportion for ball milling and sintering;
the specific technological parameters of ball milling and sintering are as follows: ball milling for 1 h+/-10 min at a rotating speed of 350-400 r/min; sintering in an argon protection atmosphere furnace at 600-800 ℃ for 2 h+/-30 min;
The "rod material hot extruded to the required diameter" in the step (1) is specifically: the process is carried out at 300-400 ℃ under the protection of inert gas, the diameter of the obtained bar is 5-20 mm, and the extrusion ratio is 6 or 6.5;
Removing oxide skin on the surface of the bar before the bar is placed in a die groove with a cylindrical cavity in the step (1);
the mechanical stirring in the step (2) is specifically as follows: stirring temperature is 680-720 ℃, stirring time is 25+/-10 min, stirring speed is 600-900 rpm, and reversing interval time is 5min;
the particle diameter of the micron-sized SiC particles in the step (2) is 2-3 mu m;
In the step (3), the step of hot extrusion into bars with required diameters is specifically as follows: the process is carried out at 300-450 ℃ under the protection of inert gas, the diameter of the obtained bar is 10-30 mm, and the extrusion ratio is 5.9 or 6.25;
The homogenization heat treatment in the step (4) is specifically as follows: homogenizing and annealing at 400-500 deg.c for 2-3 hr;
repeating the steps (2) - (3), and determining the size of the SiC particles added in the step (2) according to the requirement to obtain the multi-layer SiC particle size gradient structure composite material.
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