CN108359852B - Graphene-reinforced high-silicon aluminum-based composite material and preparation method thereof - Google Patents
Graphene-reinforced high-silicon aluminum-based composite material and preparation method thereof Download PDFInfo
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Abstract
A graphene-reinforced high-silicon aluminum-based composite material and a preparation method thereof are disclosed, wherein the composite material comprises the following components in percentage by mass: silicon: 15.0-20.0%, copper: 2.0-4.0%, magnesium: 0.5 to 1.0%, titanium: 0.05 to 0.07%, boron: 0.02-0.05%, graphene: 0.3-0.6% of aluminum and the balance of aluminum; the preparation method comprises the following steps: 1) mixing the raw materials under the protection of gas to obtain alloy powder; 2) pressing the alloy powder into a blocky sintered blank, and then sintering in vacuum to obtain a sintered blank; 3) carrying out quenching treatment and tempering treatment or multidirectional forging and annealing treatment on the composite material according to different silicon contents to obtain the graphene-reinforced high-silicon aluminum-based composite material; the method of the invention ensures that the particles of the reinforcing phase are distributed more uniformly, and a large amount of dislocation is generated in the material, and dislocation cells are broken into sub-crystals or fine crystals to achieve fine crystal strengthening; the tensile strength is improved to more than 400 MPa; meanwhile, the yield strength of the material is improved to over 236 MPa.
Description
Technical Field
The invention relates to the field of graphene application technology, in particular to a graphene-reinforced high-silicon aluminum-based composite material and a preparation method thereof.
Background
The aluminum-silicon composite material has the advantages of high specific strength and specific rigidity, low thermal expansion coefficient, good wear resistance and volume stability, high enough high-temperature strength and the like, and is widely applied to the aerospace and automobile manufacturing industries. When the silicon content exceeds the aluminum-silicon eutectic point component by 12.6%, although the strength is further improved, the matrix is severely cracked due to the increased size and irregular shape of the silicon particles embedded in the matrix, stress concentration is formed at the tip of the silicon phase, the tensile strength of the material is reduced, and the machinability of the material is deteriorated. At present, the silicon content of the commonly used aluminum-silicon-based composite material is basically lower than that of a eutectic composition, and the reinforcement of the aluminum-silicon-based composite material is mainly divided into particle reinforcement and fiber reinforcement, but the production cost is higher, and the potential of further reinforcing the aluminum-based composite material by utilizing particle reinforcement, fiber reinforcement and the like is smaller and smaller.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a graphene-reinforced high-silicon aluminum-based composite material and a preparation method thereof.
The graphene-reinforced high-silicon aluminum-based composite material comprises the following components in percentage by mass: silicon: 15.0-20.0%, copper: 2.0-4.0%, magnesium: 0.5 to 1.0%, titanium: 0.05 to 0.07%, boron: 0.02-0.05%, graphene: 0.3-0.6% and the balance of aluminum.
The graphene-reinforced high-silicon aluminum-based composite material comprises the following components in percentage by mass according to a first preferred scheme: silicon: 15.0-18.0%, copper: 3.0-4.0%, magnesium: : 0.5 to 1.0%, titanium: 0.05-0.06%, boron: 0.02-0.03%, graphene: 0.3-0.6% and the balance of aluminum.
The graphene-reinforced high-silicon aluminum-based composite material comprises the following components in percentage by mass according to a second preferred scheme: silicon: 18.0-20.0%, copper: 2.0-3.0%, magnesium: 0.5 to 1.0%, titanium: 0.06-0.07%, boron: 0.03-0.05%, graphene: 0.3-0.6% and the balance of aluminum.
The preparation method of the graphene-reinforced high-silicon aluminum-based composite material specifically comprises the following steps:
step 1, mixing materials:
mixing the materials according to the component percentage of the graphene-reinforced high-silicon aluminum-based composite material, loading the mixture into a mixing tank under the protection of inert gas or nitrogen, mixing the materials at a rotating speed of 30-50 r/min for 24-36 h, standing for 1-2 h, mixing the materials at a rotating speed of 30-40 r/min for 24-36 h, standing and radiating to normal temperature to obtain uniformly mixed alloy powder;
step 2, die pressing and sintering:
(1) pouring the uniformly mixed alloy powder into a pressing die under the protection of inert gas, maintaining the pressure at 220-250 MPa for 5-8 min, and demolding to obtain a blocky sintered blank;
(2) carrying out vacuum sintering on the block-shaped sintered blank, wherein the sintering temperature is 560-575 ℃, and after the sintering time is 1.5-2 h, the block-shaped sintered blank is cooled to room temperature along with a furnace to obtain a sintered blank;
step 3, subsequent heat treatment:
aiming at the component proportion of the graphene-reinforced high-silicon aluminum-based composite material in the step 1, when the mass percentage of silicon is more than or equal to 15.0% and less than 18%, the following treatment (a) and (b) are adopted:
(a) quenching the sintered blank at 500 ℃ for 1-3 h, and then cooling with water;
(b) tempering the quenched blank at the temperature of 150-200 ℃ for 1-3 h, and then air-cooling to obtain the graphene-reinforced high-silicon aluminum-based composite material;
aiming at the component proportion of the graphene-reinforced high-silicon aluminum-based composite material in the step 1, when the mass percentage of silicon is more than or equal to 18.0% and less than or equal to 20.0%, the following treatment (c) and (d) are adopted:
(c) carrying out multidirectional forging on the sintered blank, wherein the forging temperature is 480-500 ℃, the deformation speed is 2-4 mm/s, and the forging deformation direction is changed in each forging pass;
(d) and annealing the forged blank at the annealing temperature of 180-200 ℃ for 1-3 h to obtain the graphene-reinforced high-silicon aluminum-based composite material.
The preparation method of the graphene-reinforced high-silicon aluminum-based composite material comprises the following steps:
and in the step 1, the mixing tank is filled in a gas protection glove isolation box.
In the step 1, the inert gas is argon.
In the step 1, mixing is carried out in a three-dimensional space motion mixing ball mill.
In the step 1, the materials are mixed for 24-36 hours at the rotating speed of 30-40 r/min and then are kept stand for 1-2 hours, so that the problem that the temperature of a material mixing tank rises due to long-time continuous rotation, the cold welding phenomenon of powder in the tank is caused, and the time is 1-2 hours.
In the step 2, a 0.5MN double-column manual hydraulic press is adopted for die pressing.
In the step 2, the vacuum sintering adopts a vacuum hot-pressing sintering furnace.
In the step 2, the sintering time is determined according to the amount of the alloy powder.
In the step 3, a resistance furnace is adopted for quenching treatment. The quenching heat preservation time is determined according to the size of the part.
In the step 3, a double-column manual hydraulic press is adopted for multidirectional forging.
And 3, forging for 5-10 times.
Graphene is a high-performance nano material, has high strength, good flexibility, excellent electric and thermal conductivity and optical performance, and has the properties of dirac-fermi characteristics, singular quantum hall effect, minimum quantum conductivity and the like due to the unique structure. Compared with the traditional reinforcement, the composite reinforcement has larger specific strength, specific surface area and lower production cost, and becomes the most ideal reinforcement material for replacing ceramic fibers, carbon nanotubes and hard particles. At present, common high-silicon aluminum alloys such as A390, ZL117, KS282 and the like with silicon content of 15-22% at home and abroad have higher specific strength and lower thermal expansion coefficient, are particularly suitable for aeromodelling and motorcycle piston materials, but with the increase of the silicon content, coarse polygonal block or plate-shaped silicon particles appear, and the mechanical property, particularly the elongation, is obviously reduced. The shape and distribution of silicon particles in an aluminum matrix are improved, and the silicon particles are thinned and dispersed and distributed, so that the improvement of the mechanical property of the high-silicon aluminum-based material is very important. The addition of the graphene obviously improves the form of silicon particles in the high-silicon aluminum-based composite material, has a refining effect on the silicon particles, and improves the comprehensive mechanical property of the aluminum-silicon composite material.
Compared with the prior art, the graphene-reinforced high-silicon aluminum-based composite material and the preparation method thereof have the beneficial effects that:
the high-performance graphene reinforced high-silicon aluminum-based composite material with higher strength and hardness is prepared by selecting a specific formula, has the advantages of light weight, wear resistance, high heat conductivity coefficient, low thermal expansion coefficient and good cutting processing performance, has excellent heat conductivity, and can be widely applied to the fields of aerospace, precision instruments and automobile manufacturing.
The addition of the graphene nano material improves the tensile strength and the yield strength of the high-silicon aluminum-based composite material, and the elongation of the high-silicon aluminum-based composite material is also improved. The addition of the graphene nanosheets enables silicon particles in the high-silicon aluminum-based composite material structure to be refined and dispersed, and the tensile strength of the material is improved from 328MPa to more than 400MPa and is increased by more than 20%; meanwhile, the yield strength of the material is improved from more than 202MPa to more than 236 MPa. The improved effect is obviously better than the strengthening effect of other materials for strengthening the high-silicon aluminum-based composite material. The addition of the graphene improves the morphology and distribution of silicon particles, so that the yield strength and plasticity of the silicon particles are improved.
Along with the increase of the Si content, the thermal cracking resistance of the composite material is improved, in order to release the strength of the graphene aluminum-silicon-based multi-component composite material to the maximum, a multidirectional forging process is adopted for the graphene reinforced high-silicon aluminum-based composite material with the Si content close to 20%, so that the reinforced phase particles are distributed more uniformly, a large amount of dislocation is generated in the material, dislocation cells are broken into sub-crystals or fine crystals, and the effect of fine crystal reinforcement is achieved.
Drawings
Fig. 1 is a microstructure of a graphene-reinforced high-silicon aluminum-based composite material prepared in example 1 of the present invention;
fig. 2 shows the microstructure of the graphene-reinforced high-silicon aluminum-based composite material prepared in example 2 of the present invention;
fig. 3 shows the microstructure of the graphene-reinforced high-silicon aluminum-based composite material prepared in example 3 of the present invention;
fig. 4 shows the microstructure of the graphene-reinforced high-silicon aluminum-based composite material prepared in example 4 of the present invention.
Detailed Description
Example 1
A graphene-reinforced high-silicon aluminum-based composite material comprises the following components in percentage by mass: silicon: 15.0%, copper: 4.0%, magnesium: 1.0%, titanium: 0.06%, boron: 0.03%, graphene: 0.5 percent, and the balance being aluminum.
The preparation method of the graphene-reinforced high-silicon aluminum-based composite material specifically comprises the following steps:
step 1, mixing materials:
the graphene-reinforced high-silicon aluminum-based composite material comprises, by mass, 15.0% of silicon, 4.0% of copper, 1.0% of magnesium, 0.06% of titanium, 0.03% of boron, 0.5% of graphene, and the balance aluminum.
Mixing various raw material powders of 700 meshes according to the mass percentage in a glove isolation box under the protection of argon, loading the raw material powders into a mixing tank, assembling the mixing tank on a ball mill, mixing the raw material powders for 30 hours in a three-dimensional space motion mixing ball mill at the rotating speed of 40r/min, standing for 1 hour to prevent the temperature of the mixing tank from rising due to long-time continuous rotation, causing the cold welding phenomenon of the powders in the tank, repeatedly and continuously rotating the mixing tank for 30 hours again, standing for radiating to normal temperature, and unloading the materials from the ball mill to obtain uniformly mixed alloy powders;
step 2, die pressing and sintering:
(1) pouring the uniformly mixed alloy powder into a pressing die under the protection of argon, maintaining the pressure for 5min at 240MPa by adopting a 0.5MN double-column manual hydraulic press, and demoulding to obtain a blocky sintered blank;
(2) vacuum sintering the massive sintering blank by adopting a vacuum hot-pressing sintering furnace, wherein the sintering temperature is 560 ℃, and after the sintering time is 2 hours, the massive sintering blank is cooled to room temperature along with the furnace to obtain a sintered blank;
step 3, subsequent heat treatment:
(1) quenching the sintered blank by using a resistance furnace, wherein the quenching temperature is 500 ℃, and the heat preservation time is 2 hours (which can be determined according to the size of the sintered part) and then water cooling is carried out;
(2) tempering the quenched blank at 180 ℃, and carrying out air cooling after the heat preservation time is 2h to obtain the graphene-reinforced high-silicon aluminum-based composite material; the microstructure is shown in figure 1, wherein the dark granular material is Si granule, and the gray area is mostly Al2A Cu phase.
Example 2
A graphene-reinforced high-silicon aluminum-based composite material comprises the following components in percentage by mass: silicon: 16.0%, copper: 3.5%, magnesium: 1.0%, titanium: 0.06%, boron: 0.03%, graphene: 0.3 percent of aluminum and the balance of aluminum.
The preparation method of the graphene-reinforced high-silicon aluminum-based composite material specifically comprises the following steps:
step 1, mixing materials:
the graphene-reinforced high-silicon aluminum-based composite material comprises, by mass, 16.0% of silicon, 3.5% of copper, 1.0% of magnesium, 0.06% of titanium, 0.03% of boron, 0.3% of graphene, and the balance aluminum.
Mixing various raw material powders of 700 meshes according to the mass percentage in a glove isolation box under the protection of argon, loading the raw material powders into a mixing tank, assembling the mixing tank on a ball mill, mixing the raw material powders for 30 hours in a three-dimensional space motion mixing ball mill at the rotating speed of 40r/min, standing for 1 hour to prevent the temperature of the mixing tank from rising due to long-time continuous rotation, causing the cold welding phenomenon of the powders in the tank, repeatedly and continuously rotating the mixing tank for 30 hours again, standing for radiating to normal temperature, and unloading the materials from the ball mill to obtain uniformly mixed alloy powders;
step 2, die pressing and sintering:
(1) pouring the uniformly mixed alloy powder into a pressing die under the protection of argon, maintaining the pressure for 5min at 240MPa by adopting a 0.5MN double-column manual hydraulic press, and demoulding to obtain a blocky sintered blank;
(2) vacuum sintering is carried out on the massive sintering blank by adopting a vacuum hot-pressing sintering furnace, the sintering temperature is 575 ℃, and after the sintering time is 1.52h, the massive sintering blank is cooled to room temperature along with the furnace, so as to obtain the sintered blank;
step 3, subsequent heat treatment:
(1) quenching the sintered blank by using a resistance furnace, wherein the quenching temperature is 500 ℃, and the heat preservation time is 2 hours (which can be determined according to the size of the sintered part) and then water cooling is carried out;
(2) tempering the quenched blank at 180 ℃, and carrying out air cooling after the heat preservation time is 2h to obtain the graphene-reinforced high-silicon aluminum-based composite material; the microstructure is shown in figure 2.
Example 3
A graphene-reinforced high-silicon aluminum-based composite material comprises the following components in percentage by mass: silicon: 20.0%, copper: 2.0%, magnesium: 1.0%, titanium: 0.07%, boron: 0.04%, graphene: 0.6 percent, and the balance being aluminum.
The preparation method of the graphene-reinforced high-silicon aluminum-based composite material specifically comprises the following steps:
step 1, mixing materials:
the graphene-reinforced high-silicon aluminum-based composite material comprises, by mass, 20.0% of silicon, 2.0% of copper, 1.0% of magnesium, 0.07% of titanium, 0.04% of boron, 0.6% of graphene, and the balance aluminum.
Mixing various raw material powders of 700 meshes according to the mass percentage in a glove isolation box under the protection of argon, loading the raw material powders into a mixing tank, assembling the mixing tank on a ball mill, mixing the raw material powders for 30 hours in a three-dimensional space motion mixing ball mill at the rotating speed of 40r/min, standing for 1 hour to prevent the temperature of the mixing tank from rising due to long-time continuous rotation, causing the cold welding phenomenon of the powders in the tank, repeatedly and continuously rotating the mixing tank for 30 hours again, standing for radiating to normal temperature, and unloading the materials from the ball mill to obtain uniformly mixed alloy powders;
step 2, die pressing and sintering:
(1) pouring the uniformly mixed alloy powder into a pressing die under the protection of argon, maintaining the pressure for 5min at 240MPa by adopting a 0.5MN double-column manual hydraulic press, and demoulding to obtain a blocky sintered blank;
(2) vacuum sintering is carried out on the blocky sintered blank by adopting a vacuum hot-pressing sintering furnace, the sintering temperature is 565 ℃, after the sintering time is 1.8h, the blocky sintered blank is cooled to room temperature along with the furnace, and a sintered blank is obtained;
step 3, subsequent heat treatment:
(1) performing multidirectional forging on the sintered blank by adopting a double-column manual hydraulic press, performing 5 times of forging in total, wherein the forging temperature is 490 ℃, the deformation speed is 3mm/s, and the forging deformation direction is changed in each time of forging;
(2) and annealing the forged blank at 200 ℃ for 2h to obtain the graphene-reinforced high-silicon aluminum-based composite material. The microstructure is shown in figure 3.
Example 4
A graphene-reinforced high-silicon aluminum-based composite material comprises the following components in percentage by mass: silicon: 19.0%, copper: 2.5%, magnesium: 1.0%, titanium: 0.06%, boron: 0.04%, graphene: 0.5 percent, and the balance being aluminum.
The preparation method of the graphene-reinforced high-silicon aluminum-based composite material specifically comprises the following steps:
step 1, mixing materials:
the graphene-reinforced high-silicon aluminum-based composite material comprises, by mass, 19.0% of silicon, 2.5% of copper, 1.0% of magnesium, 0.06% of titanium, 0.04% of boron, 0.5% of graphene, and the balance aluminum.
Mixing various raw material powders of 700 meshes according to the mass percentage in a glove isolation box under the protection of argon, loading the raw material powders into a mixing tank, assembling the mixing tank on a ball mill, mixing the raw material powders for 30 hours in a three-dimensional space motion mixing ball mill at the rotating speed of 40r/min, standing for 1 hour to prevent the temperature of the mixing tank from rising due to long-time continuous rotation, causing the cold welding phenomenon of the powders in the tank, repeatedly and continuously rotating the mixing tank for 30 hours again, standing for radiating to normal temperature, and unloading the materials from the ball mill to obtain uniformly mixed alloy powders;
step 2, die pressing and sintering:
(1) pouring the uniformly mixed alloy powder into a pressing die under the protection of argon, maintaining the pressure for 5min at 240MPa by adopting a 0.5MN double-column manual hydraulic press, and demoulding to obtain a blocky sintered blank;
(2) vacuum sintering is carried out on the massive sintering blank by adopting a vacuum hot-pressing sintering furnace, the sintering temperature is 570 ℃, the sintering time is 1.5-2 h, and then the massive sintering blank is cooled to room temperature along with the furnace to obtain a sintered blank;
step 3, subsequent heat treatment:
(1) performing multidirectional forging on the sintered blank by adopting a double-column manual hydraulic press, performing forging for 10 times in total, wherein the forging temperature is 490 ℃, the deformation speed is 3mm/s, and the forging deformation direction is changed in each time of forging;
(2) and annealing the forged blank at 200 ℃ for 2h to obtain the graphene-reinforced high-silicon aluminum-based composite material. The microstructure is shown in figure 4.
Claims (6)
1. The preparation method of the graphene-reinforced high-silicon aluminum-based composite material is characterized by comprising the following components in percentage by mass: silicon: 15.0-20.0%, copper: 2.0-4.0%, magnesium: 0.5 to 1.0%, titanium: 0.05 to 0.07%, boron: 0.02-0.05%, graphene: 0.3-0.6% of aluminum and the balance of aluminum;
the method specifically comprises the following steps:
step 1, mixing materials:
mixing the materials according to the mass percentage of the graphene-reinforced high-silicon aluminum-based composite material, loading the materials into a mixing tank under the protection of inert gas or nitrogen, mixing the materials at a rotating speed of 30-50 r/min for 24-36 h, standing for 1-2 h, mixing the materials at a rotating speed of 30-40 r/min for 24-36 h, standing and radiating to normal temperature to obtain uniformly mixed alloy powder;
step 2, die pressing and sintering:
(1) pouring the uniformly mixed alloy powder into a pressing die under the protection of inert gas, maintaining the pressure at 220-250 MPa for 5-8 min, and demolding to obtain a blocky sintered blank;
(2) carrying out vacuum sintering on the block-shaped sintered blank, wherein the sintering temperature is 560-575 ℃, and after the sintering time is 1.5-2 h, the block-shaped sintered blank is cooled to room temperature along with a furnace to obtain a sintered blank;
step 3, subsequent heat treatment:
aiming at the component proportion of the graphene-reinforced high-silicon aluminum-based composite material in the step 1, when the mass percentage of silicon is more than or equal to 15.0% and less than 18%, the following treatment (a) and (b) are adopted:
(a) quenching the sintered blank at 500 ℃ for 1-3 h, and then cooling with water;
(b) tempering the quenched blank at the temperature of 150-200 ℃ for 1-3 h, and then air-cooling to obtain the graphene-reinforced high-silicon aluminum-based composite material;
aiming at the component proportion of the graphene-reinforced high-silicon aluminum-based composite material in the step 1, when the mass percentage of silicon is more than or equal to 18.0% and less than or equal to 20.0%, the following treatment steps (c) and (d) are adopted:
(c) carrying out multidirectional forging on the sintered blank, wherein the forging temperature is 480-500 ℃, the deformation speed is 2-4 mm/s, and the forging deformation direction is changed in each forging pass;
(d) and annealing the forged blank at the annealing temperature of 180-200 ℃ for 1-3 h to obtain the graphene-reinforced high-silicon aluminum-based composite material.
2. The preparation method of the graphene-reinforced high-silicon aluminum-based composite material according to claim 1, wherein the graphene-reinforced high-silicon aluminum-based composite material comprises the following components in percentage by mass: silicon: 15.0-18.0%, copper: 3.0-4.0%, magnesium: 0.5 to 1.0%, titanium: 0.05-0.06%, boron: 0.02-0.03%, graphene: 0.3-0.6% and the balance of aluminum.
3. The preparation method of the graphene-reinforced high-silicon aluminum-based composite material according to claim 1, wherein the graphene-reinforced high-silicon aluminum-based composite material comprises the following components in percentage by mass: silicon: 18.0-20.0%, copper: 2.0-3.0%, magnesium: 0.5 to 1.0%, titanium: 0.06-0.07%, boron: 0.03-0.05%, graphene: 0.3-0.6% and the balance of aluminum.
4. The method for preparing the graphene-reinforced high-silicon aluminum-based composite material according to claim 1, wherein the step 1 is carried out in a gas protection glove box by loading the material into a mixing tank; mixing materials in a three-dimensional moving mixing ball mill; in the step 2, a 0.5MN double-column manual hydraulic press is adopted for die pressing, and a vacuum hot-pressing sintering furnace is adopted for vacuum sintering; in the step 3, a resistance furnace is adopted for quenching treatment, and a double-column manual hydraulic press is adopted for multidirectional forging.
5. The method for preparing the graphene-reinforced high-silicon aluminum-based composite material according to claim 1, wherein in the step 1, the inert gas is argon.
6. The preparation method of the graphene-reinforced high-silicon aluminum-based composite material according to claim 1, wherein in the step 3, the forging is performed for 5-10 times in total.
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| CN106567785A (en) * | 2016-11-10 | 2017-04-19 | 无锡市明盛强力风机有限公司 | Graphene-doped aluminum alloy air cylinder cover |
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| CN107299257A (en) * | 2017-05-16 | 2017-10-27 | 苏州莱特复合材料有限公司 | A kind of modified graphene reinforced aluminum matrix composites and preparation method thereof |
Non-Patent Citations (2)
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| EFFECT OF GRAPHENE ADDITION ON FLEXURAL PROPERTIES OF Al 6061 NANOCOMPOSITES;Prashantha kumar H.G et al;《Materials Today:Proceedings》;20171231;第4卷;第8127–8133页 * |
| Graphene nanoflakes reinforced Al-20Si matrix composites prepared by pressure infiltration method;Wenshu Yang et al;《Materials Science & Engineering A》;20170608;第700卷;第351-357页 * |
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