CN117049545B - Silicon carbide pretreatment method and application thereof in preparation of aluminum-based composite material - Google Patents
Silicon carbide pretreatment method and application thereof in preparation of aluminum-based composite material Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 112
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 68
- 239000002131 composite material Substances 0.000 title claims abstract description 68
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000002203 pretreatment Methods 0.000 title abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 74
- 238000003756 stirring Methods 0.000 claims abstract description 66
- 238000000034 method Methods 0.000 claims abstract description 45
- 230000003647 oxidation Effects 0.000 claims abstract description 40
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 40
- 238000000498 ball milling Methods 0.000 claims abstract description 30
- 238000005266 casting Methods 0.000 claims abstract description 27
- 230000008569 process Effects 0.000 claims abstract description 22
- 230000007704 transition Effects 0.000 claims abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 13
- 239000001301 oxygen Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000012216 screening Methods 0.000 claims abstract description 6
- 238000007670 refining Methods 0.000 claims abstract description 3
- 229910000838 Al alloy Inorganic materials 0.000 claims description 60
- 239000011159 matrix material Substances 0.000 claims description 46
- 238000000227 grinding Methods 0.000 claims description 19
- 239000002994 raw material Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- 239000004677 Nylon Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000010907 mechanical stirring Methods 0.000 claims description 5
- 229920001778 nylon Polymers 0.000 claims description 5
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims 2
- 239000000956 alloy Substances 0.000 abstract description 12
- 238000005054 agglomeration Methods 0.000 abstract description 6
- 230000002776 aggregation Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 239000011777 magnesium Substances 0.000 description 17
- 239000010949 copper Substances 0.000 description 16
- 229910045601 alloy Inorganic materials 0.000 description 10
- 229910003336 CuNi Inorganic materials 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- 239000007788 liquid Substances 0.000 description 7
- 230000003014 reinforcing effect Effects 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000155 melt Substances 0.000 description 5
- 230000002787 reinforcement Effects 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000003607 modifier Substances 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000001133 acceleration Effects 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910000676 Si alloy Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910018125 Al-Si Inorganic materials 0.000 description 1
- 229910021364 Al-Si alloy Inorganic materials 0.000 description 1
- 229910018520 Al—Si Inorganic materials 0.000 description 1
- 229910018566 Al—Si—Mg Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910019018 Mg 2 Si Inorganic materials 0.000 description 1
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 1
- ZGUQGPFMMTZGBQ-UHFFFAOYSA-N [Al].[Al].[Zr] Chemical compound [Al].[Al].[Zr] ZGUQGPFMMTZGBQ-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- WPPDFTBPZNZZRP-UHFFFAOYSA-N aluminum copper Chemical compound [Al].[Cu] WPPDFTBPZNZZRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000009661 fatigue test Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000009715 pressure infiltration Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
- B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
- B07B1/00—Sieving, screening, sifting, or sorting solid materials using networks, gratings, grids, or the like
- B07B1/28—Moving screens not otherwise provided for, e.g. swinging, reciprocating, rocking, tilting or wobbling screens
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
-
- 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
- C22C21/00—Alloys based on aluminium
-
- 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
- C22C32/0047—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 carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—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 carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
- C22C32/0063—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 carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on SiC
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Food Science & Technology (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
The invention relates to the technical field of alloy materials, in particular to a silicon carbide pretreatment method and application thereof in preparation of aluminum-based composite materials, wherein a low-energy ball mill is adopted to ball-mill silicon carbide particles; heating the ball-milled silicon carbide particles, introducing oxygen, and mechanically stirring in the oxidation process to oxidize the surfaces of the ball-milled silicon carbide particles; vibrating and screening the oxidized silicon carbide particles to obtain pretreated silicon carbide particles; preparing materials, preparing melt, adding silicon carbide particles, vacuum transition variable speed stirring, modifying and refining, casting and the like on the basis of the pretreated silicon carbide particles to obtain an aluminum-based composite material; the invention adopts the low-energy ball milling and high-temperature stirring oxidation method, effectively improves the shape of silicon carbide particles, prevents mutual adhesion agglomeration among the particles, and greatly improves the wettability in stirring casting and the interface strength in aluminum-based composite material.
Description
Technical Field
The invention relates to the technical field of alloy materials, in particular to a silicon carbide pretreatment method and application thereof in preparation of an aluminum-based composite material, wherein the aluminum-based composite material is prepared by stirring casting and composite modification refinement.
Background
Aluminum-based composite materials have been a hot spot in recent years because of their excellent properties such as high specific strength, specific stiffness, abrasion resistance, low thermal expansion coefficient, good heat conduction and dimensional stability. The particle reinforced aluminum-based composite material represented by SiC enables the low-cost aluminum-based composite material to realize performance optimization through particle content, size and the like, and breakthrough is continuously realized in the fields of aerospace, electronic packaging, automobile manufacturing, high-speed trains and the like. The main processes for preparing the aluminum-based composite material at present are stirring casting, powder metallurgy, pressure infiltration and the like. The stirring casting method is a method for obtaining a composite material by stirring after a matrix is melted and added reinforcing phase particles are involved to obtain a uniformly distributed melt and casting under certain conditions. The method has the advantages of simple equipment and process, high production efficiency, low cost and capability of mass production of components with complex shapes, and is one of the most potential processes for realizing industrial mass production.
For aluminum-based composites, the degree of uniformity of the dispersion of the reinforcing phase in the matrix and the interfacial bond strength of the reinforcing phase to the matrix can greatly affect the performance of the composite. The thermal fatigue resistance of the aluminum-based composite material developed against the background of high-temperature application is determined by the interface property to a great extent. Under the condition of cold and hot circulation, because of the difference of thermal expansion or contraction characteristics between the matrix and the reinforcing phase of the composite material, local stress concentration is easy to generate at the interface, so that the interface is separated and plastically deformed, and finally, the thermal fatigue failure of the composite material is brought. The difficulty in producing aluminum-based composites by stirring casting is achieving good bonding between the reinforcing phase and the matrix. Since the wettability between the reinforcing phase and the aluminum melt is generally not high, it is difficult to obtain acceptable interfacial strength and weaken the overall strength and thermal fatigue resistance of the aluminum-based composite material. This also makes the powder pretreatment process a popular technique to solve this problem.
For example, in patent CN113502407B, a pretreatment method of silicon carbide particles is disclosed, in which a silicon dioxide layer is formed on the surface of the silicon carbide particles by calcination, and then etched to make surface holes, thereby improving wettability and interfacial bonding strength between the silicon carbide particles and aluminum alloy. However, the method is used for oxidizing particles by a common calcination process, so that a uniform oxide film is difficult to obtain, the outline size of the silicon carbide particles is not round enough, the finally prepared silicon carbide particles are still mainly used for preparing the aluminum-based composite material by a powder metallurgy method, and the performance improvement on the stirring casting production of the aluminum-based composite material is limited.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a silicon carbide pretreatment method and application thereof in preparation of an aluminum matrix composite material, so that the prepared silicon carbide is tightly combined with the aluminum matrix, and the composite material has excellent mechanical property and thermal fatigue resistance.
The aim of the invention is achieved by the following technical scheme:
a method of pretreating silicon carbide, comprising the steps of:
(1) Ball milling: ball milling is carried out on silicon carbide particles by adopting a low-energy ball mill;
(2) Oxidizing: heating the ball-milled silicon carbide particles, introducing oxygen, and mechanically stirring the silicon carbide particles in the oxidation process to oxidize the surfaces of the silicon carbide particles;
(3) And (3) screening: and (3) vibrating and screening the oxidized silicon carbide particles to obtain pretreated silicon oxide particles.
Further, the silicon carbide particles are cleaned before ball milling.
Furthermore, the ball milling adopts a horizontal low-energy ball mill, and adopts a nylon grinding tank and silicon carbide grinding balls to ball mill silicon carbide particles.
Further, the ball milling parameters are as follows: the rotating speed is 100-300 r/min, the ball milling time is 5-30 h, the volume ratio of silicon carbide to grinding balls is 1 (1-3), deionized water is selected as a ball milling medium, and water is injected to 2/5~4/5 of the volume of a grinding tank for ball milling; and after ball milling, taking out the slurry, and drying at 100-300 ℃.
Further, the oxidation is: and placing the ball-milled silicon carbide particles into an oxidation tube for heating and introducing oxygen, wherein a silicon nitride stirring paddle is adopted for mechanical stirring in the oxidation process.
Further, the oxidation temperature is 800-1300 ℃, the oxygen flow is 0.1-0.8L/min, and the oxidation time is 1-8 h; the stirring speed of the stirring paddle is 5-50 r/min.
The silicon carbide obtained by the method has the particle size of 10-40 mu m, the average length-diameter ratio of 1.2-3.5, the oxide film thickness of 10-400nm, less sharp corners and no obvious crack defects.
The preparation method comprises the steps of preparing component raw materials of an aluminum alloy matrix, melting in a vacuum environment to obtain an aluminum alloy melt, adding pretreated silicon carbide particles into the aluminum alloy melt, performing vacuum transition variable speed stirring, refining and modifying the aluminum alloy melt, casting the aluminum alloy melt, and cooling to obtain the silicon carbide reinforced aluminum matrix composite.
The method specifically comprises the following steps:
(1) Preparing raw materials: preparing component raw materials of an aluminum alloy matrix, and cleaning;
(2) Pretreatment of silicon carbide: pretreating silicon carbide particles;
(3) Preparing an aluminum melt: placing the component raw materials of the cleaned aluminum alloy matrix in a crucible, vacuumizing, and heating to melt to obtain an aluminum alloy melt;
(4) Adding silicon carbide: stirring the aluminum alloy melt, and adding the pretreated silicon carbide into the aluminum alloy melt to obtain an aluminum-based composite material melt;
(5) Vacuum transition variable speed stirring: further vacuumizing, and carrying out transition variable speed stirring on the aluminum-based composite material melt for a plurality of times to disperse silicon carbide particles;
(6) Modification and refinement: adding a refiner and an alterant into the aluminum-based composite material melt;
(7) Casting: and (3) raising the temperature, pouring the aluminum-based composite material melt into a preheated mold, and cooling and forming to obtain the silicon carbide aluminum-based composite material.
The beneficial effects of this application are:
1. the silicon carbide pretreatment process adopts a low-energy ball milling and high-temperature stirring oxidation method, effectively improves the shape of silicon carbide particles, and prevents mutual adhesion agglomeration among the particles. The oxide film generated by the surface pretreatment is uniform and has proper thickness, so that the wettability in stirring casting and the interface strength in the aluminum-based composite material are greatly improved.
2. The application adopts a vacuum transition variable speed stirring casting method, adopts multiple frequency transition variable speed stirring to promote the formation of irregular vortex in the melt, and further breaks up the agglomeration of silicon carbide to promote the distribution of the silicon carbide. The material structure is even, and good performances are ensured.
3. The aluminum-based composite material prepared by the method does not contain precious and rare elements, ensures low cost, and has excellent mechanical property and thermal fatigue resistance.
Drawings
Fig. 1 is a schematic structural diagram of a high-temperature oxidation stirring device according to an embodiment of the present invention.
FIG. 2 is a metallographic structure of an aluminum-based composite material made in accordance with the present invention.
FIG. 3 is a thermal fatigue crack of an aluminum-based composite material made in accordance with the present invention.
Detailed Description
The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings, and it is obvious that the described embodiments are only illustrative and not limiting of the present application. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
In a first aspect, the present application provides an effective pretreatment method for modifying a silicon carbide surface, comprising the steps of: cleaning, ball milling, oxidizing and sieving silicon carbide.
In the prior art, the shape optimization of the silicon carbide particles generally adopts high-energy ball milling, the shape improvement effect is limited, sharp corner particles cannot be effectively passivated and rounded, and the sharp corners are further caused by cracking of the particles. The shape of the silicon carbide particles can be effectively improved by the low-energy ball milling method, and the particles can be prevented from cracking by using a proper nylon grinding tank and matching with grinding balls and deionized water in a proper proportion.
In addition, the oxidation method in the application adopts high-temperature stirring oxidation to prevent the adhesion agglomeration of particles which are easy to generate in the general calcination oxidation. The particles in the oxidation process are stirred and the oxygen introducing amount is controlled, so that the oxidation modification of the silicon carbide surface can be effectively realized, the generated oxide film is uniform and has proper thickness, and the wettability in stirring casting and the interface strength in the aluminum-based composite material are further improved.
The silicon carbide is particles with the particle diameter of 5-60 mu m, the purity is more than 99 percent, more preferably 10-40 mu m, and the purity is more than 99.7 percent. Soaking silicon carbide particles in HF solution with the mass concentration of 5% for 24-36 h, mechanically stirring, standing for precipitation after soaking, removing the turbid liquid on the upper layer, and repeatedly washing with distilled water to be neutral to obtain slurry.
The ball milling step adopts a horizontal low-energy ball mill, and silicon carbide slurry with proper quality and grinding balls are put into a nylon grinding tank. The grinding balls are silicon carbide grinding balls for preventing pollution, the rotating speed is 100-300 r/min, the ball milling time is 5-30 h, the volume ratio of silicon carbide to the grinding balls is 1:1-3, the ball milling medium is deionized water, and water is injected to 2/5~4/5 of the volume of the grinding tank. And after ball milling, taking out the slurry, and drying at 100-300 ℃.
The oxidation step adopts a stirring oxidation device, the silicon carbide after ball milling is placed in an oxidation tube, the oxidation temperature is 800-1300 ℃, the oxygen flow is 0.1-0.8L/min, and the oxidation time is 1-8 h. In the oxidation process, mechanical stirring is carried out in the whole process to prevent particles from adhering or from being oxidized unevenly, and the stirring speed is 5-50 r/min. And after the oxidation is finished, naturally cooling and vibrating and screening are carried out to further prevent the particles from adhering and agglomerating.
Preferably, the oxidation tube is a high-temperature resistant corundum tube or a high-purity silicon nitride tube, the stirring paddle is high-purity silicon nitride, the stirring speed is 10r/min, the oxidation temperature is 1000-1100 ℃, the oxygen introducing amount is 0.2L/min, and the oxidation time is 3h.
In a second aspect, the present application provides a method for preparing a silicon carbide reinforced aluminum matrix composite, wherein the pretreated silicon carbide is added into an aluminum alloy solution by adopting a stirring casting method, and then an ingot or a part of the aluminum matrix composite is prepared by vacuum casting.
The aluminum-based composite material comprises 15-35% of SiC particle reinforcement by mass percent based on the total mass of the aluminum-based composite material, and the balance of an aluminum alloy matrix;
wherein the aluminum alloy matrix is hypoeutectic aluminum-silicon alloy, and comprises the following components: the aluminum alloy comprises the following components in percentage by mass based on the total mass of an aluminum alloy matrix: 9 to 12 percent of Si, 1 to 2.5 percent of Cu, 1 to 2 percent of Ni, 0.2 to 1.5 percent of Mg, 1.5 to 2.5 percent of Mn, 0.5 to 1.5 percent of Cr, 0.3 to 0.8 percent of Fe, 0.01 to 0.5 percent of Zr, 0.25 percent of Ce, 0.25 percent of La, 0.3 percent of V, 0.3 percent of Y, 0.4 percent of Ti, 0.04 percent of Sr, and 0.01 percent of B; the balance Al and unavoidable impurities.
According to the mass percentage, the following elements of the aluminum alloy matrix are as follows:（1）
（2）
（3）
in the method, in the process of the invention,is the mass percent of Ni in the aluminum alloy matrix, < >>Is Cu mass percent in the aluminum alloy matrix, < >>Is the mass percent of Mg in the aluminum alloy matrix, < >>Is the mass percent of Mn in the aluminum alloy matrix, < >>The mass percentage of Cr in the aluminum alloy matrix is as follows. Through the component design, the precipitated phase with good high-temperature mechanical property can be obtained to the maximum.
In the aluminum-based composite material, hypoeutectic silicon with better castability and thermal stability is adopted, and meanwhile, the lower Si content is convenient for introducing additional silicon carbide. Further, the aluminum alloy comprises Al 3 CuNi phase, said Al 3 The volume fraction of the CuNi phase is not less than 6%.
Cu and Ni elements are introduced to strengthen the aluminum-silicon alloy, and Al is generated by introducing Cu elements 2 Cu、Al 5 Cu 2 Mg 8 Si 6 Metastable phase, however, the increase of Cu content causes solidification volume shrinkage, and the number of pores increases, so that the mechanical property is deteriorated, and the Cu element content is controlled to be less than 2.5 percent.
Ni element introduction will first generate Al 7 Cu 4 Ni、Al 3 CuNi phase, further increasing Ni content, will generate Al 3 Ni phase, above three Ni-rich phases, al 3 The thermal stability and fatigue resistance of CuNi phase are optimal, therefore, the invention controls 0.5<Ni/Cu<0.7 in order to obtain more Al 3 A CuNi phase.
When the mass of the silicon carbide particle reinforcement accounts for 5% -15% of the total mass of the aluminum-based composite material; in the aluminum alloy matrix, the mass of Mg element accounts for 0.2 to 0.7 percent of the mass of the aluminum alloy matrix.
When the mass of the silicon carbide particle reinforcement accounts for 15% -30% of the total mass of the aluminum-based composite material; in the aluminum alloy matrix, the mass of Mg element accounts for 0.7-1.5% of the mass of the aluminum alloy matrix.
When the mass of the silicon carbide particle reinforcement accounts for 30% -50% of the total mass of the aluminum-based composite material; in the aluminum alloy matrix, the mass of Mg element accounts for 1.5-2% of the mass of the aluminum alloy matrix.
The aluminum alloy comprises Al 5 Cu 2 Mg 8 Si 6 A phase of Al 3 The volume fraction of the CuNi phase is 6.5% -7.4%.
The Mg element can improve the wettability of the aluminum alloy matrix and the silicon carbide interface, a part of Mg exists at the interface of the silicon carbide particles and the aluminum matrix, and a part of Mg exists in the form of intermetallic compounds. In the intermetallic compound, mg is preferentially selected from Al 5 Cu 2 Mg 8 Si 6 Phase precipitation, which occurs as the content of Mg increases 2 Si phase, mg 2 The strengthening mechanism of Si phase in the aluminum-silicon matrix is mainly Orowan strengthening, and the material plasticity is seriously reduced while the room temperature strength is improved.
Thus, the present invention is to control the existence form of Mg element. And controlProper amount of Cu content is reduced, mg content is increased, and Al can be reduced 2 Cu and Mg 2 Si phase is generated to convert Cu and Mg elements into Al with better creep resistance 5 Cu 2 Mg 8 Si 6 And (3) phase (C).
Further, the aluminum alloy comprises dendritic Al 15 (Mn,Fe) 3 Si 2 And (3) phase (C). And Al is 15 (Mn,Fe) 3 Si 2 The grain size is about 20 um. Al (Al) 15 (Mn,Fe) 3 Si 2 The phase and the eutectic silicon matrix form a three-dimensional net structure.
Mn element is added to generate two-dimensional lath Al 13 Mn 4 Si 8 Lath-shaped Al 13 Mn 4 Si 8 Further generating dendritic Al through peritectic reaction 15 Mn 3 Si 2 Phases, dendritic Al 15 Mn 3 Si 2 The high temperature stability and fatigue resistance of the phase are better. To improve Mn-rich phase, proper amount of Fe element is added to promote lath Al 13 Mn 4 Si 8 Conversion to dendritic Al 15 (Mn,Fe) 3 Si 2 . With the increase of Mn content, the size of Mn-rich phase increases to 50-80 um level, but the excessive precipitated phase easily damages the mechanical property of the material, the invention controls 1.5<Mn/Cr<2 because Cr element may be present in the Mn-rich phase and refine the Mn-rich phase to around 20 um.
Al 15 (Mn,Fe) 3 Si 2 Is attached to Al 7 CuNi phase, al 3 The CuNi phase is separated out, a three-dimensional network structure is formed by the CuNi phase and the eutectic silicon matrix, and the network structure is further reinforced by the silicon carbide particle reinforcement, so that the critical stress of crack initiation is improved. The separated hard phase and ceramic particles are used as hard supporting points in the friction process, so that the hard supporting points are not easy to abrade, an Al matrix is protected, and the friction performance of the material is improved.
Further, in the aluminum alloy, the following elements are filled according to mass percentFoot:. In (1) the->Is the mass percentage of Zr in the aluminum alloy matrix,is the mass percent of Ce in the aluminum alloy matrix, < >>Is the mass percentage of La in the aluminum alloy matrix, < >>Is the mass percentage of V in the aluminum alloy matrix, < >>Is the mass percentage of Y in the aluminum alloy matrix.
In the invention, the addition of Zr element can form Al 3 Zr phase, and grain is obviously refined; the Sr element is added in the form of Al-10Sr, clusters at Si liquid interfaces in the modified alloy are formed, the eutectic Si morphology is improved, and the strength and the plasticity of the material are improved; b is added in the form of Al-5Ti-B, and has remarkable effect on grain refinement of Al-Si alloy; part of Ti element exists in the additionally added refiner Al-5Ti-B, and the other part of Ti exists in the high-temperature stable phase Ti 2 Al 20 Ce, ce.
In the prior art, the preparation method of the aluminum-based composite material mainly comprises three methods of casting, powder metallurgy and aluminum liquid infiltration. Compared with powder metallurgy and infiltration, the casting method has the advantages of simple equipment, low production cost, contribution to industrial production and the like, and the aluminum-based composite material prepared by the casting method occupies more than 40 percent of the total amount of the aluminum-based composite material. The stirring casting process is also called stirring composite process, and is characterized by that the reinforcing body is mixed with liquid aluminium alloy matrix by means of mechanical stirring device, then the aluminium alloy matrix is made into cast ingot or component of aluminium base composite material by means of normal pressure casting or vacuum pressure casting or pressure casting, and its advantages are that it adopts conventional smelting equipment, and its cost is low, so that it can prepare precise complex component structure. However, some problems still remain to be solved when preparing the silicon carbide reinforced aluminum-based composite material by stirring and casting, such as: casting defects (mixing of gas and inclusions), uneven particle distribution, and the like. According to the method, a vacuum transition variable speed stirring casting method is adopted, after silicon carbide is added into an aluminum alloy melt, the formation of irregular vortex in the melt is promoted by adopting multi-frequency transition variable speed stirring, and the agglomeration of the silicon carbide is further dispersed so as to promote the distribution of the silicon carbide.
Specifically, the preparation method comprises the following steps:
A. preparing raw materials: preparing component raw materials of an aluminum alloy matrix, and cleaning;
B. pretreatment of silicon carbide: the silicon carbide particles are subjected to the pretreatment;
C. preparing an aluminum melt: placing an aluminum alloy raw material in a crucible, vacuumizing, and heating to melt to obtain an aluminum alloy melt;
D. adding silicon carbide: adding silicon carbide into the aluminum alloy melt in the process of stirring the aluminum alloy melt to obtain an aluminum-based composite material melt;
E. vacuum transition variable speed stirring: further vacuumizing, and thoroughly scattering silicon carbide particles through transition variable speed stirring;
F. modification and refinement: adding a refiner and an alterant into the prepared aluminum-based composite material melt;
G. casting: and (3) raising the temperature, pouring the aluminum-based composite material melt into a preheated mold, and cooling and forming to obtain an ingot.
Preferably, the aluminum alloy in the step A is an Al-Si series or Al-Si-Mg series alloy, and the component raw materials can be pure metal blocks or intermediate alloys, preferably common aluminum-silicon intermediate alloys, aluminum-copper intermediate alloys, aluminum-nickel intermediate alloys, aluminum-zirconium intermediate alloys, pure aluminum, pure magnesium and the like. And ultrasonically cleaning the raw materials by using acetone or absolute ethyl alcohol for 10-30 minutes.
Preferably, the specific steps of the step C are as follows: and (3) placing the raw materials into a vacuum induction melting furnace crucible with a stirring device, vacuumizing to 50-150 Pa, heating to 700-800 ℃, and preserving heat for 0.5-1 h to ensure that all the raw materials are completely melted.
Preferably, the specific steps of the step D are as follows: and (3) reducing the temperature of the melt to a semi-solid temperature range, inserting a stirring head below the liquid level, starting a stirring device to stir at a constant speed, wherein the rotating speed is 300-800 r/min, and adding silicon carbide into the central vortex of the aluminum alloy melt through a secondary feeding device. Further preferably, the semi-solid temperature is 10-30 ℃ above the solidus of the aluminum alloy matrix.
Preferably, the specific steps of the step E are as follows: after the silicon carbide is added, vacuumizing to 30-50 Pa, increasing the rotating speed to 800-2000 r/min, and continuously stirring for 1-3 h in a semi-solid temperature interval. And (3) carrying out transition variable speed stirring for 10-30 times, wherein the rotating speed transition difference value is 300-1500 r/min, and the speed transition is completed within 1-3 s.
Preferably, the refiner and the modifier used in the step F are respectively 0.1-0.5 wt.% of Al-5Ti-B and 0.1-0.5 wt.% of Al-10Sr. And before adding the thinning modifier, reducing the stirring rotation speed to 200-300 r/min, and increasing the temperature of the aluminum-based composite material melt to 700-720 ℃. And (5) after adding the refiner and the modifier, preserving heat for 10-20 min.
The invention adopts transition variable speed stirring mode in the process of mixing and dispersing silicon carbide in aluminum alloy melt. In the prior art, a stirring mode with constant rotation speed is generally adopted, and after the stirring mode is adopted for a period of time, a stable vortex flow field is formed by the melt, so that the partially agglomerated silicon carbide particles are difficult to break up under the stable flow field, and the dispersing effect is poor. Therefore, in order to solve the problems, the invention adopts a transition variable speed stirring mode, and the main idea is that in the stirring process, the stirring rotating speed is enabled to have acceleration higher than a certain critical value, and the acceleration of the rotating speed can form a large shearing force in melt vortex, so that the instability of the original steady-state vortex is facilitated, and further, the agglomerated silicon carbide particles rotating along with the vortex are scoured and scattered, thereby facilitating the uniform distribution of the silicon carbide particles.
Preferably, the specific steps of the step G are as follows: and raising the temperature of the aluminum-based composite material melt to 730-750 ℃, pouring the aluminum-based composite material melt into a die with the preheating temperature of 200-300 ℃, and cooling and forming to obtain an aluminum-based composite material ingot.
Example 1:
an aluminum-based composite material with a total mass of 5kg, wherein: 4kg of aluminum alloy and 1kg of silicon carbide particles. The aluminum alloy comprises the following components in percentage by mass: si:9.21%, mg:0.53%, ti:0.02%, cu:0.02%, sr:0.12%, the balance being Al and unavoidable impurities.
The preparation process comprises the following steps: silicon carbide particles with the purity of more than 99.7% and the particle diameter of 10-20 mu m are selected. Soaking silicon carbide particles for 24 hours by adopting an HF solution with the mass concentration of 5%, mechanically stirring the silicon carbide particles during the soaking, standing for precipitation, removing turbid liquid on the upper layer, and repeatedly washing with distilled water to be neutral to obtain slurry. And placing the slurry and grinding balls into a nylon grinding tank, wherein the grinding balls are silicon carbide grinding balls with diameters of 5-10 mm, and the volume ratio of the silicon carbide to the grinding balls is 1:1.5. Deionized water is selected as the ball milling medium, and water is injected to 4/5 of the volume of the grinding tank. The ball milling adopts a horizontal low-energy ball mill with the rotating speed of 130r/min and the ball milling time of 20h. And after ball milling, taking out the slurry, and drying at 170 ℃. The oxidation uses a high-temperature oxidation stirring device shown in figure 1, the dried silicon carbide is placed in an oxidation cavity 2 in the middle of an oxidation tube 1, high-temperature resistant tube plugs 4 are plugged into two sides of the oxidation tube, oxygen is blown in through an oxygen tube 5, and an air flow valve 6 is adjusted to enable the oxygen flow to be 0.2L/min. The oxidation temperature is 1100 ℃ and the oxidation time is 3 hours. In the oxidation process, the stirring paddle 3 is driven by the motor 7 to stir the silicon carbide, and the mechanical stirring speed is 10r/min. And naturally cooling and vibrating and sieving after the oxidation is finished.
The pretreated silicon carbide is placed in a secondary feeding device of a vacuum induction smelting furnace with a stirring device, and Al-15Si intermediate alloy, al-10Ti intermediate alloy, al-50Cu intermediate alloy, pure Mg and pure Al are placed in a crucible of the smelting furnace. Vacuumizing to 50Pa, and raising the temperature of the smelting furnace to 750 ℃ for 0.5h. And (3) reducing the temperature of the aluminum alloy melt to 570-590 ℃, inserting a stirring device below the liquid level of the aluminum alloy, starting the stirring device at the rotating speed of 600r/min, and adding silicon carbide into the central vortex of the aluminum alloy melt through a secondary feeding device. After the addition is finished, vacuumizing to 30Pa, increasing the rotating speed to 800r/min, and continuously stirring for 1h at 570-600 ℃. 15 transitions are carried out, the transition is carried out between 300r/min and 800r/min, and acceleration is completed within 1.5 s. The stirring speed is reduced to 300r/min, and the temperature of the composite material melt is increased to 700 ℃. 0.2. 0.2 wt percent of Al-5Ti-B refiner and 0.2. 0.2 wt percent of Al-10Sr modifier are added through a secondary feeding device, and the temperature is kept for 20 minutes. Raising the temperature to 750 ℃, pouring the melt into a die with the preheating temperature of 250 ℃, and cooling and forming to obtain the aluminum-based composite ingot.
The microstructure of the aluminum-based composite material prepared in the embodiment is shown in fig. 2, and the silicon carbide is uniformly distributed and has no obvious agglomeration. The tensile strength of the composite material at normal temperature is 230-290 MPa, the elongation is 1.0-2.0%, the thermal fatigue resistance is excellent in thermal fatigue resistance in a thermal fatigue test, and after 600 times of circulation at 30-250 ℃, no obvious thermal fatigue crack is generated in the prefabricated notch, as shown in figure 3.
The foregoing description is only exemplary embodiments of the present application and is not intended to limit the scope of the present application, and all equivalent structures or equivalent processes using the descriptions and the drawings of the present application, or direct or indirect application in other related technical fields are included in the scope of the present application.
Claims (6)
1. The application of silicon carbide in the preparation of aluminum-based composite materials is characterized in that the silicon carbide is pretreated by the following steps:
(1) Ball milling: ball milling is carried out on silicon carbide particles by adopting a low-energy ball mill;
(2) Oxidizing: heating the ball-milled silicon carbide particles, introducing oxygen, and mechanically stirring the silicon carbide particles in the oxidation process to oxidize the surfaces of the silicon carbide particles;
(3) And (3) screening: vibrating and screening the oxidized silicon carbide particles to obtain pretreated silicon carbide particles;
the obtained pretreated silicon carbide has the particle size of 10-40 mu m, the average length-diameter ratio of 1.2-3.5 and the oxide film thickness of 10-400nm;
preparing component raw materials of an aluminum alloy matrix, melting the component raw materials in a vacuum environment to obtain an aluminum alloy melt, adding pretreated silicon carbide particles into the aluminum alloy melt, performing vacuum transition variable speed stirring, then refining and modifying the aluminum alloy melt, casting the aluminum alloy melt, and cooling to obtain the silicon carbide reinforced aluminum matrix composite material.
2. Use of a silicon carbide according to claim 1 for the preparation of an aluminium based composite material, wherein the silicon carbide particles are washed prior to ball milling.
3. The use of silicon carbide in the preparation of an aluminum matrix composite material according to claim 1, wherein the ball milling is performed by a horizontal low energy ball mill, and the silicon carbide particles are ball milled by a nylon milling pot and silicon carbide milling balls.
4. Use of silicon carbide according to claim 3 for the preparation of aluminium-based composites, wherein the ball milling parameters are: the rotating speed is 100-300 r/min, the ball milling time is 5-30 h, the volume ratio of silicon carbide to grinding balls is 1 (1-3), deionized water is selected as a ball milling medium, and after ball milling, the slurry is taken out and dried at 100-300 ℃.
5. Use of a silicon carbide according to claim 1 for the preparation of an aluminium based composite material, wherein the oxidation is: and placing the ball-milled silicon carbide particles into an oxidation tube for heating and introducing oxygen, wherein a silicon nitride stirring paddle is adopted for mechanical stirring in the oxidation process.
6. The application of the silicon carbide in the preparation of the aluminum-based composite material according to claim 5, wherein the oxidation temperature is 800-1300 ℃, the oxygen introducing amount is 0.1-0.8L/min, and the oxidation time is 1-8 h; the stirring speed of the stirring paddle is 5-50 r/min.
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