CN116536538A - Preparation method of ultrasonic-assisted self-infiltration aluminum oxide reinforced magnesium-based composite material - Google Patents
Preparation method of ultrasonic-assisted self-infiltration aluminum oxide reinforced magnesium-based composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 47
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 35
- 239000011777 magnesium Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims description 17
- 238000001764 infiltration Methods 0.000 title abstract description 15
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 82
- 239000000956 alloy Substances 0.000 claims abstract description 82
- 239000007788 liquid Substances 0.000 claims abstract description 77
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000009766 low-temperature sintering Methods 0.000 claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- 239000011248 coating agent Substances 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 238000003723 Smelting Methods 0.000 claims description 12
- 238000007872 degassing Methods 0.000 claims description 12
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 238000007710 freezing Methods 0.000 claims description 12
- 230000008014 freezing Effects 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 239000007790 solid phase Substances 0.000 claims description 12
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 11
- 229910052742 iron Inorganic materials 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 125000003158 alcohol group Chemical group 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 239000010431 corundum Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000011268 mixed slurry Substances 0.000 claims description 4
- 229920000193 polymethacrylate Polymers 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 abstract description 20
- 230000008595 infiltration Effects 0.000 abstract description 10
- 238000011049 filling Methods 0.000 abstract description 6
- 239000011148 porous material Substances 0.000 abstract description 5
- 238000005266 casting Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 7
- 238000005470 impregnation Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000012595 freezing medium Substances 0.000 description 2
- 238000009715 pressure infiltration Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 208000033830 Hot Flashes Diseases 0.000 description 1
- 206010060800 Hot flush Diseases 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
- C22C1/1021—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform the preform being ceramic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
- B22D23/04—Casting by dipping
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/12—Making non-ferrous alloys by processing in a semi-solid state, e.g. holding the alloy in the solid-liquid phase
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0036—Matrix based on Al, Mg, Be or alloys thereof
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Composite Materials (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
A preparation method of an ultrasonic-assisted self-impregnating alumina reinforced magnesium-based composite material belongs to the technical field of magnesium-based composite material preparation, and solves the technical problems of single preparation method, long time, high cost, incomplete pore filling and uncoordinated strong plasticity promotion of the existing magnesium-based composite material, and the solution is as follows: first, a layered porous alumina ceramic preform having a certain strength and a high porosity is produced by low-temperature sintering based on a freeze casting method. Then, an ultrasonic mechanical vibration ultrasonic composite mode is introduced on the basis of pressureless infiltration, so that alloy liquid is more fully filled between the ceramic sheet layer and the ceramic framework, a good interface bonding effect is achieved, and the strong plasticity collaborative promotion of the composite material is realized. The invention can realize the high-flux preparation of composite materials with different proportions, cooling rates and dimensions at one time, has short operation time and high infiltration speed, can prepare composite materials in batches, and can also prepare specific workpieces.
Description
Technical Field
The invention belongs to the technical field of magnesium-based composite material preparation, and particularly relates to a preparation method of an ultrasonic-assisted self-infiltration aluminum oxide reinforced magnesium-based composite material.
Background
The resource and the environment become the primary precondition of sustainable development of human beings, magnesium and magnesium alloy are taken as a new material with important strategic significance, and the development and application of hot flashes are promoted in the global scope, and the magnesium alloy is determined as one of important directions for future research and development in the fields of transportation, electronic industry, military industry, biomedical use, aerospace and the like. The magnesium alloy is used as a metal structural material, has good performances of dimensional stability, heat conduction and electric conductivity, high damping, electromagnetic shielding and the like, and is called as a '21 st century green engineering material' because of the characteristic of easy recycling. The magnesium alloy has the defects of low strength, low elastic modulus, high thermal expansion coefficient, poor thermal stability, wear resistance and the like when being used as an ideal light material. The ceramic has the advantages of high strength, high melting point, good heat stability, high hardness, wear resistance, low cost and the like. Therefore, the magnesium-based composite material prepared by adding the ceramic particles into the magnesium alloy has excellent properties of high specific strength, high specific modulus, wear resistance, heat resistance, electric conduction, heat conduction, radiation resistance, low thermal expansion coefficient and the like.
Early scholars found that the shell was made by 95vol.% CaCO 3 And 5vol.% of organics constitute a soft, hard, alternating layered structure similar to "brick and mud", with a fracture strength of pure CaCO 3 More than 20 times of (a). Based on the above, a novel porous ceramic preparation technology, namely a freeze casting method, is adopted by a learnerPreparing the lamellar porous ceramic, then impregnating the alloy into the porous ceramic by a pressureless impregnation or pressure impregnation method to finish the preparation of the composite material, and providing a new idea for manufacturing the bionic composite material with the lamellar structure.
In the prior report, on one hand, researchers adopt a pressure infiltration method to infiltrate molten alloy into a ceramic preform under the action of pressure so as to prepare a composite material, but the alumina preform prepared by a freeze casting method is often low in strength, and the strength required in the pressure infiltration process is difficult to meet. On the other hand, the prepared preform is directly immersed into the molten alloy liquid by a scholars by adopting a pressureless impregnation method, and the molten alloy liquid is spontaneously impregnated into the ceramic skeleton by utilizing the wettability of the preform and the molten alloy liquid, but the sintering temperature is higher (usually 1200 ℃ -1500 ℃) when the porous alumina ceramic is prepared, the compressive strength of the composite material prepared by pressureless impregnation is 500-700 MPa, and the compressive strain is 2% -4%.
In summary, the magnesium-based composite material prepared in the prior art is impregnated by means of wettability, but the pressure impregnation method has high requirement on the strength of the preform, and the pressureless impregnation method is only used for impregnating by means of wettability, so that molten alloy is difficult to completely introduce into a ceramic skeleton, and therefore, the prepared composite material has obvious defects such as air holes and the like, and the application and development of the magnesium-based composite material are limited.
Disclosure of Invention
The invention mainly aims to overcome the defects in the prior art, solve the technical problems of single preparation method, long time, high cost, incomplete pore filling and uncoordinated strong plasticity promotion of the existing magnesium-based composite material, and provide the preparation method of the ultrasonic-assisted self-infiltration aluminum oxide reinforced magnesium-based composite material.
The design concept of the invention is as follows: first, a layered porous alumina ceramic preform having a certain strength and a high porosity is produced by improving the internal components of the ceramic and sintering at a low temperature based on a freeze casting method. Then, a mechanical vibration and ultrasonic composite mode is introduced on the basis of pressureless infiltration, the porosity is reduced in a mechanical vibration mode, air holes in the prefabricated body are further removed by means of the cavity effect of ultrasonic waves, alloy liquid is fully filled between the ceramic sheet layer and the ceramic skeleton, a good interface bonding effect is achieved, and strong plasticity collaborative promotion of the composite material is achieved.
The invention is realized by the following technical scheme: the preparation method of the ultrasonic-assisted self-impregnating aluminum oxide reinforced magnesium-based composite material comprises the following steps:
s1, placing alumina powder, silica sol, a dispersing agent and deionized water into a corundum ball milling tank, and ball milling for 10-20 hours at 100-400 rpm by using a ball mill to prepare uniformly mixed slurry; wherein the mass percent of the dispersing agent accounts for 0.5-2 wt% of the total mass of the raw material, the volume percent of the solid phase accounts for 30 vol% of the total volume of the raw material, the volume percent of the alumina powder accounts for 15-30 vol% of the volume percent of the solid phase, and the volume percent of the silicon dioxide in the silica sol accounts for 0-15 vol% of the volume percent of the solid phase;
s2, placing the slurry prepared in the step S1 into a vacuum box for degassing treatment, wherein the air pressure in the vacuum box is-0.08 MPa to-0.1 MPa, and the degassing time is 10-20 min;
s3, pouring the slurry subjected to the degassing treatment in the step S2 into a pipe-shaped die, and placing the pipe-shaped die on a copper plate in a low-temperature constant-temperature tank for freezing at the freezing temperature of-10 ℃ to-80 ℃ to obtain a frozen green body;
s4, placing the frozen green body obtained in the step S3 in a vacuum freeze dryer to sublimate ice, wherein the vacuum degree of the vacuum freeze dryer is 10 Pa-50 Pa, and the freeze drying time is 24 h-170 h;
s5, performing low-temperature sintering on the green body subjected to freeze drying in the step S4, heating to 800-1000 ℃ from room temperature, wherein the heating rate is 5-10 ℃/min, and preserving heat for 2-4 hours; then cooling to room temperature along with a furnace to obtain a porous alumina ceramic preform;
s6, fixing the porous alumina ceramic preform prepared in the step S5 on a net-shaped mechanical vibration platform through iron wires, and then placing the porous alumina ceramic preform into a heating furnace for heat preservation for 1-3 hours, wherein the temperature is as follows: the temperature is 520-600 ℃ and is kept for later use;
s7, firstly, preheating a crucible at a preheating temperature of 500-550 ℃; secondly, taking out the preheated crucible, and uniformly coating a coating agent on the inner wall of the crucible; thirdly, placing the crucible with the coating agent coated on the inner wall into a smelting furnace until the temperature of the crucible is raised to 740-800 ℃; finally, placing the magnesium alloy into a crucible, continuously introducing protective gas into a smelting furnace, cooling to 700-740 ℃ after the solid alloy is completely melted into alloy liquid, and preserving heat for later use;
s8, taking out the porous alumina ceramic preform subjected to heat preservation in the step S6, hanging the porous alumina ceramic preform on a mechanical vibration platform above a smelting furnace, and ensuring that the temperature of the porous alumina ceramic preform is consistent with the temperature of alloy liquid for later use;
s9, firstly, marking scale marks at the position 2 cm-4 cm away from the lower end of the ultrasonic rod; then preheating an ultrasonic rod for 20-40 min at a preheating temperature of 600-700 ℃; finally, the lower end of the ultrasonic rod is placed into the alloy liquid completely melted in the step S7, the scale mark is level with the liquid level of the alloy liquid, the ultrasonic device is turned on for searching frequency for at least 2 times, a switch of an ultrasonic vibration controller is turned on after the ultrasonic rod is stabilized at the Hertz, the ultrasonic rod is used for carrying out ultrasonic vibration on the alloy liquid for 5-15 min, the switch of the ultrasonic vibration controller is turned off after the gas in the alloy liquid is removed, and the ultrasonic rod stops working;
s10, firstly, removing impurities on the surface of the alloy liquid after ultrasonic vibration in the step S9; then, immediately descending a mesh-shaped mechanical vibration platform prepared in the step S8, wherein the mesh-shaped mechanical vibration platform drives the porous alumina ceramic preform to move downwards until the porous alumina ceramic preform is completely immersed in the alloy liquid, and continuously shaking for 5-10 min; finally, turning on an ultrasonic device to seek frequency for at least 2 times, turning on a switch of an ultrasonic vibration controller after the Hertz is stable, and performing secondary ultrasonic vibration on the alloy liquid for 5-15 min by using an ultrasonic rod;
and S11, cooling the alloy liquid to 550-600 ℃ after the second ultrasonic vibration in the step S10, taking out the alloy liquid until cooling to room temperature when the alloy liquid is in a semi-solid state, and keeping the alloy liquid in a protective gas atmosphere all the time in the process of solidifying the alloy liquid to the semi-solid state to prepare the self-impregnating alumina reinforced magnesium-based composite material.
Further, in the step S1, the particle diameter of the alumina powder is 1 μm to 10 μm, and the particle diameter of the silica in the silica sol is 5nm to 30nm.
Further, in the step S1, the dispersant is sodium polymethacrylate.
Further, in the step S3, the frozen medium is alcohol.
Further, in the step S6, the iron wire and the mesh-shaped mechanical vibration platform are both coated with a coating agent.
Further, in the step S9, the hertz range of the ultrasonic vibration controller is adjusted to 19300hz to 19950hz, the current coefficient is adjusted to 50%, and the operation mode is selected to be a continuous mode.
Further, in the step S10, the mesh-shaped mechanical vibration platform is immersed in the alloy liquid all the time in the continuous shaking process.
Compared with the prior art, the invention has the beneficial effects that:
on one hand, the porous alumina ceramic preform is prepared based on a freeze-drying method, but the preparation process creatively adopts a low-temperature sintering method, so that the sintering temperature is reduced while the preform has certain strength, and meanwhile, the pores are loose and the sheet spacing is large, so that an excellent framework is provided for subsequent alloy liquid infiltration.
On the other hand, in the method, the mechanical vibration and ultrasonic vibration combined mode is adopted, the alloy liquid is fully infiltrated into the porous alumina ceramic preform, the gas generated in the melting process of the alloy liquid can be effectively removed through primary ultrasonic vibration, the infiltration of the alloy liquid is completed to a greater extent when the alloy liquid enters the preform through the mechanical vibration, the gas aggregation formed in the preform in the infiltration process can be further removed through secondary ultrasonic vibration, and the negative effects brought by the mechanical vibration are counteracted.
In summary, the invention provides the preparation method of the self-impregnating aluminum oxide reinforced magnesium-based composite material, which has the advantages of simple and reliable process, low production cost, low sintering temperature requirement, applicability to batch production and capability of impregnating specific workpieces, and solves the problems of high impregnating equipment requirement, high impregnating atmosphere requirement, high cost, inconsistent strong plasticity promotion and the like in the existing preparation of the aluminum oxide reinforced magnesium-based composite material. The method has the following advantages:
1. excellent performance: the aluminum oxide reinforced magnesium-based composite material prepared by the method has high compressive strength reaching 550-750 MPa and a compression ratio reaching 4-7%, and has the characteristics of complete filling of a ceramic skeleton, complete filling of pores and the like;
2. and (3) impregnating completely: in the traditional pressureless infiltration method, the infiltration of the middle part is incomplete due to the influence of wettability, and the method combines a mechanical vibration and ultrasonic vibration compound auxiliary mode, so that the pore filling is complete, the interface combination is excellent and the strong plasticity is improved and coordinated on the premise that the method can be completed by a self-infiltration method;
3. the production cost is reduced: the porous alumina ceramic preform is sintered at low temperature in the preparation process, so that the production cost is saved;
4. the preparation method is simple and efficient, and can be used for mass production and preparation of specific workpieces: the invention can realize the high-flux preparation of composite materials with different proportions, cooling rates and dimensions at one time, has short operation time and high infiltration speed, can prepare composite materials in batches, and can also prepare specific workpieces.
Drawings
FIG. 1 is a microstructure of a self-infiltrated alumina-reinforced magnesium-based composite prepared in example 1;
FIG. 2 is a facial sweep of a self-impregnating alumina-reinforced magnesium-based composite prepared in example 1;
fig. 3 is a graph comparing stress-strain curves of self-impregnating alumina-reinforced magnesium-based composites prepared under different conditions of examples 1 and 2.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples.
Example 1
The preparation method of the ultrasonic-assisted self-impregnating aluminum oxide reinforced magnesium-based composite material comprises the following steps:
s1, placing alumina powder, silica sol, a dispersing agent and deionized water into a corundum ball milling tank, and ball milling for 20 hours by using a ball mill at a rotating speed of 100rpm to prepare uniformly mixed slurry; wherein the dispersing agent is sodium polymethacrylate, the mass percent of the dispersing agent accounts for 1wt.% of the total mass of the raw materials, the volume percent of the solid phase accounts for 30vol.% of the total volume of the raw materials, the volume percent of the alumina powder (with the particle size of 5 μm) accounts for 25vol.% of the volume percent of the solid phase, and the volume percent of the silicon dioxide (with the particle size of 10 nm) in the silica sol accounts for 5vol.% of the volume percent of the solid phase;
s2, placing the slurry prepared in the step S1 into a vacuum box for degassing treatment, wherein the degassing time is 10min;
s3, pouring the slurry subjected to the degassing treatment in the step S2 into a pipe-shaped die, and placing the pipe-shaped die on a copper plate in a low-temperature constant-temperature tank for freezing, wherein a freezing medium is alcohol, and the freezing temperature is-20 ℃ to prepare a frozen green body;
s4, placing the frozen green body obtained in the step S3 in a vacuum freeze dryer to sublimate ice, wherein the vacuum degree of the vacuum freeze dryer is 20Pa, the freezing temperature is minus 20 ℃, the drying time is 72h, the freezing temperature is minus 50 ℃, and the drying time is 120h;
s5, performing low-temperature sintering on the green body subjected to freeze drying in the step S4, heating to 900 ℃ from room temperature, wherein the heating rate is 5 ℃/min, and preserving heat for 2 hours; then cooling to room temperature along with a furnace to prepare a porous alumina ceramic preform with a loose ceramic skeleton and a certain strength;
s6, fixing the porous alumina ceramic preform prepared in the step S5 on a net-shaped mechanical vibration platform through iron wires, coating the iron wires and the net-shaped mechanical vibration platform with a coating agent to prevent iron from reacting with magnesium alloy, and then placing the porous alumina ceramic preform into a heating furnace to be insulated for 2 hours, wherein the temperature is as follows: 540 ℃ for later use;
s7, firstly, preheating a crucible, wherein the preheating temperature is 520 ℃; secondly, taking out the preheated crucible, and uniformly coating a coating agent on the inner wall of the crucible; thirdly, placing the crucible with the coating agent coated on the inner wall into a smelting furnace until the temperature of the crucible is raised to 760 ℃; finally, placing the magnesium alloy into a crucible, continuously introducing protective gas into a smelting furnace, cooling to 740 ℃ after the solid alloy is completely melted into alloy liquid, and preserving heat for later use;
s8, taking out the porous alumina ceramic preform subjected to heat preservation in the step S6, hanging the porous alumina ceramic preform on a mechanical vibration platform above a smelting furnace, and ensuring that the temperature of the porous alumina ceramic preform is consistent with the temperature of alloy liquid for later use;
s9, firstly, marking scale marks at the position 3cm away from the lower end of the ultrasonic rod; then preheating an ultrasonic rod for 30min, wherein the preheating temperature is 650 ℃; finally, placing the lower end of the ultrasonic rod into the alloy liquid completely melted in the step S7, enabling the scale mark to be level with the liquid level of the alloy liquid, adjusting the Hertz range of the ultrasonic vibration controller to 19300 Hz-19950 Hz, adjusting the current coefficient to 50%, selecting a continuous mode in an operation mode, switching on the ultrasonic device to seek frequencies for at least 2 times, switching on a switch of the ultrasonic vibration controller after the Hertz is stable, performing ultrasonic vibration on the alloy liquid for 10min by using the ultrasonic rod, switching off the switch of the ultrasonic vibration controller after removing gas in the alloy liquid, and stopping working of the ultrasonic rod;
s10, firstly, removing impurities on the surface of the alloy liquid after ultrasonic vibration in the step S9; then, the mesh-shaped mechanical vibration platform prepared in the step S8 immediately descends, the mesh-shaped mechanical vibration platform drives the porous alumina ceramic preform to move downwards until the porous alumina ceramic preform is completely immersed in the alloy liquid, the mesh-shaped mechanical vibration platform continuously shakes for 10 minutes, and the mesh-shaped mechanical vibration platform is always immersed in the alloy liquid in the continuous shaking process; finally, turning on an ultrasonic device to seek frequency for at least 2 times, turning on a switch of an ultrasonic vibration controller after the Hertz is stable, and performing secondary ultrasonic vibration on the alloy liquid for 10 minutes by using an ultrasonic rod;
s11, cooling the alloy liquid to 550 ℃ after the alloy liquid is subjected to secondary ultrasonic vibration in the step S10, taking out the alloy liquid until the alloy liquid is cooled to room temperature when the alloy liquid is in a semi-solid state, and keeping the alloy liquid in a protective gas atmosphere all the time in the process of solidifying the alloy liquid to the semi-solid state to prepare the self-impregnating alumina reinforced magnesium-based composite material, wherein the micro-morphology of the self-impregnating alumina reinforced magnesium-based composite material is shown in a graph 1, the surface scanning graph is shown in a graph 2, and the micro-morphology can be seen from the graph 1 and the graph 2: the pressureless infiltration is helpful to ensure the integrity of the material, the bright layer is an alloy layer, the dark layer is a ceramic layer, and the ceramic skeleton in the preform is complete and has no fracture phenomenon; meanwhile, the ceramic skeleton is loose under the low-temperature sintering condition, so that alloy filling of gaps of the ceramic layer is obviously observed under a metallographic microscope.
Example 2
The preparation method of the ultrasonic-assisted self-impregnating aluminum oxide reinforced magnesium-based composite material comprises the following steps:
s1, placing alumina powder, silica sol, a dispersing agent and deionized water into a corundum ball milling tank, and ball milling for 20 hours by using a ball mill at a rotating speed of 100rpm to prepare uniformly mixed slurry; wherein the dispersing agent is sodium polymethacrylate, the mass percent of the dispersing agent accounts for 1wt.% of the total mass of the raw materials, the volume percent of the solid phase accounts for 30vol.% of the total volume of the raw materials, the volume percent of the alumina powder (with the particle size of 1 μm) accounts for 25vol.% of the volume percent of the solid phase, and the volume percent of the silicon dioxide (with the particle size of 10 nm) in the silica sol accounts for 5vol.% of the volume percent of the solid phase;
s2, placing the slurry prepared in the step S1 into a vacuum box for degassing treatment, wherein the degassing time is 10min;
s3, pouring the slurry subjected to the degassing treatment in the step S2 into a pipe-shaped die, and placing the pipe-shaped die on a copper plate in a low-temperature constant-temperature tank for freezing, wherein a freezing medium is alcohol, and the freezing temperature is minus 30 ℃ to prepare a frozen green body;
s4, placing the frozen green body obtained in the step S3 in a vacuum freeze dryer to sublimate ice, wherein the vacuum degree of the vacuum freeze dryer is 20Pa, the freezing temperature is minus 30 ℃, the drying time is 72h, the freezing temperature is minus 50 ℃, and the drying time is 120h;
s5, performing low-temperature sintering on the green body subjected to freeze drying in the step S4, heating to 900 ℃ from room temperature, wherein the heating rate is 5 ℃/min, and preserving heat for 2 hours; then cooling to room temperature along with a furnace to prepare a porous alumina ceramic preform with a loose ceramic skeleton and a certain strength;
s6, fixing the porous alumina ceramic preform prepared in the step S5 on a net-shaped mechanical vibration platform through iron wires, coating the iron wires and the net-shaped mechanical vibration platform with a coating agent to prevent iron from reacting with magnesium alloy, and then placing the porous alumina ceramic preform into a heating furnace to be insulated for 2 hours, wherein the temperature is as follows: 540 ℃ for later use;
s7, firstly, preheating a crucible, wherein the preheating temperature is 520 ℃; secondly, taking out the preheated crucible, and uniformly coating a coating agent on the inner wall of the crucible; thirdly, placing the crucible with the coating agent coated on the inner wall into a smelting furnace until the temperature of the crucible is raised to 760 ℃; finally, placing the magnesium alloy into a crucible, continuously introducing protective gas into a smelting furnace, cooling to 740 ℃ after the solid alloy is completely melted into alloy liquid, and preserving heat for later use;
s8, taking out the porous alumina ceramic preform subjected to heat preservation in the step S6, hanging the porous alumina ceramic preform on a mechanical vibration platform above a smelting furnace, and ensuring that the temperature of the porous alumina ceramic preform is consistent with the temperature of alloy liquid for later use;
s9, firstly, marking scale marks at the position 3cm away from the lower end of the ultrasonic rod; then preheating an ultrasonic rod for 30min, wherein the preheating temperature is 650 ℃; finally, placing the lower end of the ultrasonic rod into the alloy liquid completely melted in the step S7, enabling the scale mark to be level with the liquid level of the alloy liquid, adjusting the Hertz range of the ultrasonic vibration controller to 19300 Hz-19950 Hz, adjusting the current coefficient to 50%, selecting a continuous mode in an operation mode, switching on the ultrasonic device to seek frequencies for at least 2 times, switching on a switch of the ultrasonic vibration controller after the Hertz is stable, performing ultrasonic vibration on the alloy liquid for 10min by using the ultrasonic rod, switching off the switch of the ultrasonic vibration controller after removing gas in the alloy liquid, and stopping working of the ultrasonic rod;
s10, firstly, removing impurities on the surface of the alloy liquid after ultrasonic vibration in the step S9; then, the mesh-shaped mechanical vibration platform prepared in the step S8 immediately descends, the mesh-shaped mechanical vibration platform drives the porous alumina ceramic preform to move downwards until the porous alumina ceramic preform is completely immersed in the alloy liquid, the mesh-shaped mechanical vibration platform continuously shakes for 10 minutes, and the mesh-shaped mechanical vibration platform is always immersed in the alloy liquid in the continuous shaking process; finally, turning on an ultrasonic device to seek frequency for at least 2 times, turning on a switch of an ultrasonic vibration controller after the Hertz is stable, and performing secondary ultrasonic vibration on the alloy liquid for 10 minutes by using an ultrasonic rod;
and S11, cooling the alloy liquid to 550 ℃ after the second ultrasonic vibration in the step S10, taking out the alloy liquid until the alloy liquid is cooled to room temperature when the alloy liquid is in a semi-solid state, and keeping the alloy liquid in a protective gas atmosphere all the time in the process of solidifying the alloy liquid to the semi-solid state to prepare the self-impregnating alumina reinforced magnesium-based composite material.
Fig. 3 is a graph showing stress-strain curve comparison of the self-impregnating alumina-reinforced magnesium-based composite material prepared under different conditions of examples 1 and 2, as can be seen from fig. 3: the ultrasonic assistance is obviously helpful to promote the strong plastic matching of the material, so that the material exhibits more excellent performance.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the scope of the present invention should be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (7)
1. The preparation method of the ultrasonic-assisted self-impregnating aluminum oxide reinforced magnesium-based composite material is characterized by comprising the following steps of:
s1, placing alumina powder, silica sol, a dispersing agent and deionized water into a corundum ball milling tank, and ball milling for 10-20 hours at 100-400 rpm by using a ball mill to prepare uniformly mixed slurry; wherein the mass percent of the dispersing agent accounts for 0.5-2 wt% of the total mass of the raw material, the volume percent of the solid phase accounts for 30 vol% of the total volume of the raw material, the volume percent of the alumina powder accounts for 15-30 vol% of the volume percent of the solid phase, and the volume percent of the silicon dioxide in the silica sol accounts for 0-15 vol% of the volume percent of the solid phase;
s2, placing the slurry prepared in the step S1 into a vacuum box for degassing treatment, wherein the air pressure in the vacuum box is-0.08 MPa to-0.1 MPa, and the degassing time is 10-20 min;
s3, pouring the slurry subjected to the degassing treatment in the step S2 into a pipe-shaped die, and placing the pipe-shaped die on a copper plate in a low-temperature constant-temperature tank for freezing at the freezing temperature of-10 ℃ to-80 ℃ to obtain a frozen green body;
s4, placing the frozen green body obtained in the step S3 in a vacuum freeze dryer to sublimate ice, wherein the vacuum degree of the vacuum freeze dryer is 10 Pa-50 Pa, and the freeze drying time is 24 h-170 h;
s5, performing low-temperature sintering on the green body subjected to freeze drying in the step S4, heating to 800-1000 ℃ from room temperature, wherein the heating rate is 5-10 ℃/min, and preserving heat for 2-4 hours; then cooling to room temperature along with a furnace to obtain a porous alumina ceramic preform;
s6, fixing the porous alumina ceramic preform prepared in the step S5 on a net-shaped mechanical vibration platform through iron wires, and then placing the porous alumina ceramic preform into a heating furnace for heat preservation for 1-3 hours, wherein the temperature is as follows: 520-560 ℃ for later use;
s7, firstly, preheating a crucible at a preheating temperature of 500-550 ℃; secondly, taking out the preheated crucible, and uniformly coating a coating agent on the inner wall of the crucible; thirdly, placing the crucible with the coating agent coated on the inner wall into a smelting furnace until the temperature of the crucible is raised to 740-800 ℃; finally, placing the magnesium alloy into a crucible, continuously introducing protective gas into a smelting furnace, cooling to 700-740 ℃ after the solid alloy is completely melted into alloy liquid, and preserving heat for later use;
s8, taking out the porous alumina ceramic preform subjected to heat preservation in the step S6, hanging the porous alumina ceramic preform on a mechanical vibration platform above a smelting furnace, and ensuring that the temperature of the porous alumina ceramic preform is consistent with the temperature of alloy liquid for later use;
s9, firstly, marking scale marks at the position 2 cm-4 cm away from the lower end of the ultrasonic rod; then preheating an ultrasonic rod for 20-40 min at a preheating temperature of 600-700 ℃; finally, the lower end of the ultrasonic rod is placed into the alloy liquid completely melted in the step S7, the scale mark is level with the liquid level of the alloy liquid, the ultrasonic device is turned on for searching frequency for at least 2 times, a switch of an ultrasonic vibration controller is turned on after the ultrasonic rod is stabilized at the Hertz, the ultrasonic rod is used for carrying out ultrasonic vibration on the alloy liquid for 5-15 min, the switch of the ultrasonic vibration controller is turned off after the gas in the alloy liquid is removed, and the ultrasonic rod stops working;
s10, firstly, removing impurities on the surface of the alloy liquid after ultrasonic vibration in the step S9; then, immediately descending a mesh-shaped mechanical vibration platform prepared in the step S8, wherein the mesh-shaped mechanical vibration platform drives the porous alumina ceramic preform to move downwards until the porous alumina ceramic preform is completely immersed in the alloy liquid, and continuously shaking for 5-10 min; finally, turning on an ultrasonic device to seek frequency for at least 2 times, turning on a switch of an ultrasonic vibration controller after the Hertz is stable, and performing secondary ultrasonic vibration on the alloy liquid for 5-15 min by using an ultrasonic rod;
and S11, cooling the alloy liquid to 550-600 ℃ after the second ultrasonic vibration in the step S10, taking out the alloy liquid until cooling to room temperature when the alloy liquid is in a semi-solid state, and keeping the alloy liquid in a protective gas atmosphere all the time in the process of solidifying the alloy liquid to the semi-solid state to prepare the self-impregnating alumina reinforced magnesium-based composite material.
2. The method for preparing the ultrasonic-assisted self-impregnating aluminum oxide reinforced magnesium-based composite material, which is characterized by comprising the following steps of: in the step S1, the particle size of the alumina powder is 1-10 μm, and the particle size of the silica in the silica sol is 5-30 nm.
3. The method for preparing the ultrasonic-assisted self-impregnating aluminum oxide reinforced magnesium-based composite material, which is characterized by comprising the following steps of: in the step S1, the dispersant is sodium polymethacrylate.
4. The method for preparing the ultrasonic-assisted self-impregnating aluminum oxide reinforced magnesium-based composite material, which is characterized by comprising the following steps of: in the step S3, the frozen medium is alcohol.
5. The method for preparing the ultrasonic-assisted self-impregnating aluminum oxide reinforced magnesium-based composite material, which is characterized by comprising the following steps of: in the step S6, the iron wires and the net-shaped mechanical vibration platform are coated with the coating agent.
6. The method for preparing the ultrasonic-assisted self-impregnating aluminum oxide reinforced magnesium-based composite material, which is characterized by comprising the following steps of: in the step S9, the Hertz range of the ultrasonic vibration controller is adjusted to 19300 Hz-19950 Hz, the current coefficient is adjusted to 50%, and the operation mode is selected to be a continuous mode.
7. The method for preparing the ultrasonic-assisted self-impregnating aluminum oxide reinforced magnesium-based composite material, which is characterized by comprising the following steps of: in the step S10, the mesh-shaped mechanical vibration platform is immersed in the alloy liquid all the time in the continuous shaking process.
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