CN1563455A - Method for fabricating aluminum based composite material through composite reinforcement by in situ titanium diboride and dialuminum dioxide - Google Patents
Method for fabricating aluminum based composite material through composite reinforcement by in situ titanium diboride and dialuminum dioxide Download PDFInfo
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- CN1563455A CN1563455A CN 200410031169 CN200410031169A CN1563455A CN 1563455 A CN1563455 A CN 1563455A CN 200410031169 CN200410031169 CN 200410031169 CN 200410031169 A CN200410031169 A CN 200410031169A CN 1563455 A CN1563455 A CN 1563455A
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- 239000002131 composite material Substances 0.000 title claims abstract description 58
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 25
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 12
- 229910033181 TiB2 Inorganic materials 0.000 title description 17
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 title description 3
- WHOPEPSOPUIRQQ-UHFFFAOYSA-N oxoaluminum Chemical compound O1[Al]O[Al]1 WHOPEPSOPUIRQQ-UHFFFAOYSA-N 0.000 title 1
- 230000002787 reinforcement Effects 0.000 title 1
- 239000002245 particle Substances 0.000 claims abstract description 22
- 239000000956 alloy Substances 0.000 claims abstract description 18
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 18
- 239000011159 matrix material Substances 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 239000000376 reactant Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000002844 melting Methods 0.000 claims abstract description 11
- 230000008018 melting Effects 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 230000006698 induction Effects 0.000 claims abstract description 6
- 238000007670 refining Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000007872 degassing Methods 0.000 claims abstract description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract 4
- 238000000465 moulding Methods 0.000 claims abstract 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract 2
- 239000000203 mixture Substances 0.000 claims abstract 2
- 239000000843 powder Substances 0.000 claims description 16
- 229910052796 boron Inorganic materials 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000004512 die casting Methods 0.000 claims description 2
- 239000004576 sand Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 13
- 239000011156 metal matrix composite Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 abstract 1
- 238000004904 shortening Methods 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 16
- 229910052593 corundum Inorganic materials 0.000 description 16
- 229910001845 yogo sapphire Inorganic materials 0.000 description 16
- 239000010936 titanium Substances 0.000 description 10
- 239000013078 crystal Substances 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000155 melt Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000003014 reinforcing effect Effects 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- VHHHONWQHHHLTI-UHFFFAOYSA-N hexachloroethane Chemical compound ClC(Cl)(Cl)C(Cl)(Cl)Cl VHHHONWQHHHLTI-UHFFFAOYSA-N 0.000 description 3
- 239000010953 base metal Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910001008 7075 aluminium alloy Inorganic materials 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
本发明提供了一种原位TiB2颗粒和Al2O3晶须复合强化铝基复合材料的制备方法，其特征在于：工艺过程包括制备预制块和熔制铝基复合材料两个阶段：制备预制块可选择三类反应物为：Al+2Ti+4B+3O2→2Al2O3+2TiB2、4Al+2B+2O2+TiO2→2Al2O3+TiB2、8Al+3Ti+2B+3O2+2B2O3→4Al2O3+3TiB2将原材料按化学计量比放入混料机中混合均匀，再将混合均匀的原料在室温下压制成型。熔制复合材料是将基体合金Al及其合金放入中频感应炉中加热、保温、精炼除气后成型，获得原位反应TiB2颗粒和Al2O3晶须复合强化铝基复合材料。本发明的优点在于：明显缩短复合材料制备工艺流程、降低金属基复合材料的制造成本，可广泛用于要求轻质高强复合材料的场合。
The invention provides a method for preparing an in-situ TiB 2 particle and Al 2 O 3 whisker composite strengthened aluminum matrix composite material, which is characterized in that: the process includes two stages of preparing a prefabricated block and melting an aluminum matrix composite material: preparing Three types of reactants can be selected for prefabricated blocks: Al+2Ti+4B+3O 2 →2Al 2 O 3 +2TiB 2 , 4Al+2B+2O 2 +TiO 2 →2Al 2 O 3 +TiB 2 , 8Al+3Ti+2B +3O 2 +2B 2 O 3 →4Al 2 O 3 +3TiB 2 Put the raw materials into the mixer according to the stoichiometric ratio and mix them uniformly, and then press the uniformly mixed raw materials at room temperature for molding. The melting composite material is formed by placing the matrix alloy Al and its alloy in a medium frequency induction furnace for heating, heat preservation, refining and degassing, and then obtaining in situ reaction TiB 2 particles and Al 2 O 3 whiskers composite strengthened aluminum matrix composite material. The invention has the advantages of significantly shortening the composite material preparation process and reducing the manufacturing cost of the metal matrix composite material, and can be widely used in occasions requiring lightweight and high-strength composite materials.
Description
Technical Field
The invention belongs to the field of metal matrix composite materials, and particularly provides an in-situ TiB2Particles and Al2O3The preparation method of whisker composite reinforced aluminum-based composite material can melt matrix alloy and enhance phaseThe generation is carried out synchronously, the preparation process flow of the composite material is obviously shortened, the manufacturing cost of the metal-based composite material is reduced, and the method can be widely applied to occasions requiring light high-strength composite materials.
Background
The development of modern science and technology has increasingly raised requirements on materials, and the materials are expected to have certain special properties and excellent comprehensive properties, so that the common single material is increasingly difficult to meet the requirements. The composite material has the advantages of exerting the synergistic effect of the raw materials, integrating the advantages of various materials, and having great freedom of material design, thereby showing strong vitality and being rapidly developed in the past decades.
According to the principle of material design, the reinforcing phase particles and the reinforcing and toughening whiskers which are dispersed and distributed are introduced into the matrix at the same time, so that the strength, the wear resistance and the creep resistance of the composite material can be improved at the same time. Songchuntai et al (self-reinforced SiC)w/Si3N4Preparation and performance studies of composite materials, proceedings for silicates, 1993, 1: 1-8) investigating SiCw/Si3N4Composite material, 15 vol% SiC obtainedw/Si3N4The composite material has excellent mechanical property, a steep peak and the like (crystal characteristics and internal defects of β -SiC crystal whisker prepared by a carbothermic method, silicate report, 1993, 2: 33-36) synthesizes β -SiC crystal whisker by using ultrafine carbon powder to thermally reduce kaolin, and the result shows that the synthesis temperature has obvious influence on the crystal morphology of the crystal whisker2O3The crystal whisker has excellent comprehensive performance, melting point of 2040 deg.c and density of 3.96 x 103kg/m3Tensile Strength (σ)b) Is 21X 103MPa，σbA/[ rho]of 53X 104m, elastic modulusThe amount (E) is 4.3X 105MPa, E/rho of 11 x 105m。TiB2The alloy has high melting point, hardness and modulus, and good corrosion resistance, and is increasingly widely applied as a reinforcing phase in metal matrix composite materials. The applicant's research shows (Effect of Ti/catalysis on the formation of Al3Ti of in situ TiC/Al composites，Materials&Design，2001，22(8)：645-650；Effect of Ti/B Additions on the Foration of Al3Ti of insitu TiB2Al Composites, Journal of University of Science and Technology Beijing, 1999, 4: 285-2The performance of the particle reinforced aluminum matrix composite material is superior to that of the TiC particle reinforced aluminum matrix composite material. In the invention, an in-situ TiB is provided2Particles and Al2O3The preparation method of the whisker composite reinforced aluminum-based composite material can be widely applied to occasions requiring light-weight high-strength composite materials.
Disclosure of Invention
The invention aims to: providing an in-situ TiB2Particles and Al2O3The preparation method of the whisker composite reinforced aluminum-based composite material is used in occasions requiring light high-strength composite materials.
The invention is composed of: fusion casting-in-situ reaction TiB2Particles and Al2O3The preparation method of the whisker composite reinforced aluminum-based composite material is characterized by comprising the following steps of: the process comprises two stages of preparing a precast block and melting an aluminum-based composite material:
a. preparing a precast block: al produced by fusion casting-in-situ reaction method2O3Whiskers in which the oxygen originates mainly from: oxygen in the air, impurity oxygen brought by the in-situ reactant, oxygen adsorbed on the surface of the powder, oxygen adsorbed on the surface of the precast block and oxygen brought by the in-situ reactant. In order to increase Al in the composite material2O3The amount of whiskers is necessary to further increase the oxygen content of the preform. To this end, three classes of reactants may be selected (of course, of the second class of reactantsB may also be added2O3TiO can also be added into the third reactant2)：
The first type: ；
the second type: ；
in the third category: 。
ti, B, TiO mentioned in the above first, second and third categories2And B2O3The powder is powder, the particle size range is 10-250 mu m, and the purity is more than 96.0 weight percent.
When the first type of reactants are combined, the ratio (weight ratio) of Ti to B is 1.5-2.8: 1; when combined as a second type of reactant, TiO2The proportion range (weight ratio) of B and B is 2.8-4.2: 1; when combined as a third type of reactant, Ti, B and B2O3The ratio (weight ratio) of the components is 1: 5.5-7: 1.
Putting the raw materials into a mixer according to a stoichiometric ratio, uniformly mixing, and then pressing and forming the uniformly mixed raw materials at room temperature, wherein the pressure range is 25-100 MPa;
b. melting the composite material: putting 70-99.9% of matrix alloy Al and alloy thereof into a medium-frequency induction furnace for heating, wherein the heating temperature is 150-250 ℃ above the melting point of the alloy; then, the prefabricated block accounting for 1-10 wt% of the alloy is put into a furnacePressing into an alloy melt, and preserving heat: 1-30 minutes. Refining, degassing and forming, wherein the forming mode is pouring metal mold and sand mold or forming by using extrusion and die casting methods to obtain in-situ reaction TiB2Particles and Al2O3The whisker is compounded and strengthened with the aluminum-based composite material.
In situ reaction TiB2Particles and Al2O3The principle of the whisker composite reinforced aluminum-based composite material preparation technology is as follows: according to the requirements of material design, proper reactants are selected, and at proper temperature, by means of the chemical reaction between the base metal or alloy and the base metal or alloy, the in-situ generated material has fine size and uniform distributionThe reinforcing phase of (1). Compared with the traditional composite technology of the metal matrix composite material, the technology has the advantages that: (1) the reinforced phase is generated in situ in the matrix, and the surface is free of pollution; (2) the number of the enhancement phases can be adjusted within a certain range; (3) the strength and the elastic modulus of the composite material can be greatly improved while the higher toughness of the composite material is kept.
The invention has the advantages that: (1) TiB2Particles and Al2O3The crystal whisker is generated by in-situ reaction in the melt, the utilization rate of the reinforced phase is high, and the crystal whisker and the particles are distributed more uniformly in the alloy matrix. (2) Simple process, low cost and easy realization of industrialization.
Drawings
FIG. 1 is an X-ray diffraction pattern of a Ti-B-Al reaction block in the present invention. As can be seen, the reaction mass is represented by TiB2、Al2O3And Al. The scanning electron microscope tissue observation and the energy spectrum analysis confirm the generated Al2O3Whiskers rather than particles.
FIG. 2 is an in situ TiB of the present invention2Particles and Al2O3And scanning the structure of the whisker composite reinforced aluminum-based composite material.
Detailed Description
Example 1
Preparation of Al2O3Whiskers (indeterminate weight%, the same applies hereinafter) and 3 wt% TiB2Industrial pure aluminum composite material. Al powder, Ti powder and B powder with purity of 98%, 96% and 99% and particle size of 75 μm, 45 μm and 1 μm respectively are weighed according to the proportion of Al, Ti and B of 50: 35: 15 (weight percent) and mixed uniformly. Pressing into cylindrical prefabricated blocks with the diameter of 20X 30mm on a 50-ton press. 2 kg of industrial pure aluminum is melted in a medium frequency induction furnace and heated to 850 ℃. And pressing 0.12 kg of prefabricated blocks into the aluminum liquid by using a graphite bell jar, and keeping the temperature for 10 minutes. When the temperature is reduced to 750 ℃, hexachloroethane accounting for 0.4 weight percent of the molten liquid is added for refining. When the temperature of the melt is 720 ℃, pouring the melt into a metal moldTo obtain Al2O3Whiskers and 3 wt% TiB2Industrial pure aluminum composite material. Composite material sigmab168MPa and an elongation delta of 13%.
Example 2
Preparation of Al2O3Whiskers and 5% by weight of TiB2The Al-21Si-2.5Cu composite material. In the ratio of Al to TiO2Weighing appropriate amount of Al powder and TiO powder with purity of 98%, 96% and 99% and particle size of 75 μm, 75 μm and 1 μm respectively at a ratio of B to B of 50: 40: 10 (weight%)2Mixing the powder with the powder B, and mixing uniformly. Pressing into cylindrical prefabricated blocks with the diameter of 20X 30mm on a 50-ton press. 4 kg of Al-21Si-2.5Cu alloy is put into a medium frequency induction furnace to be melted and heated to 950 ℃. And pressing 0.40 kg of prefabricated blocks into the aluminum liquid by using a graphite bell jar, and keeping the temperature for 15 minutes. When the temperature is reduced to 740 ℃, hexachloroethane accounting for 0.4 percent of the weight of the molten liquid is added for refining. Pouring into a metal mold when the temperature of the melt is 730 ℃ to obtain Al2O3Whiskers and 5 wt% TiB2The Al-21Si-2.5Cu composite material. Composite material sigmabIs 420 MPa.
Example 3
Preparation of Al2O3Whiskers and 5% by weight of TiB2The/7075 composite material. According to the ratio of Al to Ti to B2O3Weighing appropriate amount of Al powder and TiO powder with purity of 98%, 96% and 99% and particle size of 75 μm, 45 μm and 1 μm at 35: 30: 5: 30 (wt.%), respectively2Mixing the powder, Ti powder and B powder. Pressing into cylindrical prefabricated blocks with the diameter of 20X 30mm on a 50-ton press. 4 kg of 7075 aluminum alloy is melted in a medium frequency induction furnace and heated to 900 ℃. And pressing 0.50 kg of prefabricated block into the aluminum liquid by using a graphite bell jar, and keeping the temperature for 10 minutes. Adding hexachloroethane accounting for 0.3 percent of the weight of the molten liquid for refining. Pouring into a metal mold when the temperature of the melt is 730 ℃ to obtain Al2O3Whiskers and 5 wt% TiB2The/7075 composite material. Composite material sigma after extrusionb685 MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB200410031169XA CN100554463C (en) | 2004-04-14 | 2004-04-14 | The preparation method of a kind of original position TiB2 and the compound reinforced aluminum matrix composites of aluminium sesquioxide |
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| CNB200410031169XA CN100554463C (en) | 2004-04-14 | 2004-04-14 | The preparation method of a kind of original position TiB2 and the compound reinforced aluminum matrix composites of aluminium sesquioxide |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100443605C (en) * | 2006-12-28 | 2008-12-17 | 上海交通大学 | Preparation Method of Particle Hybrid Reinforced Aluminum Matrix Composite |
| CN102534314A (en) * | 2012-01-19 | 2012-07-04 | 山东大学 | Lanthanum-hexaboride-reinforced aluminum-silicon-base composite material and preparation method thereof |
| CN103589913A (en) * | 2013-11-04 | 2014-02-19 | 无锡鸿祥热导科技股份有限公司 | Method for in situ preparation of nano particle reinforced aluminum-based composite material |
| CN103589893A (en) * | 2013-11-04 | 2014-02-19 | 无锡鸿祥热导科技股份有限公司 | Method for production of in situ aluminum-based composite material by high-yielding-rate reaction system |
| CN106498204A (en) * | 2016-11-08 | 2017-03-15 | 上海航天精密机械研究所 | A kind of generated aluminum-base composite foundry goods preparation method |
| CN107760933A (en) * | 2017-09-11 | 2018-03-06 | 南京航空航天大学 | A kind of 3D printing strengthens Al alloy powder and preparation method thereof with in-situ nano complex phase ceramic |
| CN110129641A (en) * | 2019-05-13 | 2019-08-16 | 贵州航天风华精密设备有限公司 | A kind of high-performance original position TiB2Particle enhanced aluminum-based composite material and preparation method thereof |
| CN110331311A (en) * | 2019-04-22 | 2019-10-15 | 江苏大学 | A kind of continuous preparation method of in-situ ceramic particle enhanced aluminum-based composite material |
| CN111663061A (en) * | 2020-06-23 | 2020-09-15 | 江苏大学 | Method for preparing Al-Si alloy grain refiner |
-
2004
- 2004-04-14 CN CNB200410031169XA patent/CN100554463C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100443605C (en) * | 2006-12-28 | 2008-12-17 | 上海交通大学 | Preparation Method of Particle Hybrid Reinforced Aluminum Matrix Composite |
| CN102534314A (en) * | 2012-01-19 | 2012-07-04 | 山东大学 | Lanthanum-hexaboride-reinforced aluminum-silicon-base composite material and preparation method thereof |
| CN103589913A (en) * | 2013-11-04 | 2014-02-19 | 无锡鸿祥热导科技股份有限公司 | Method for in situ preparation of nano particle reinforced aluminum-based composite material |
| CN103589893A (en) * | 2013-11-04 | 2014-02-19 | 无锡鸿祥热导科技股份有限公司 | Method for production of in situ aluminum-based composite material by high-yielding-rate reaction system |
| CN103589913B (en) * | 2013-11-04 | 2016-01-13 | 无锡鸿祥热导科技股份有限公司 | A kind of original position prepares the method for nanoparticle reinforced aluminum-based composite |
| CN103589893B (en) * | 2013-11-04 | 2016-05-11 | 无锡鸿祥热导科技股份有限公司 | A kind of high recovery rate reaction system is prepared the method for in-situ Al-base composition |
| CN106498204A (en) * | 2016-11-08 | 2017-03-15 | 上海航天精密机械研究所 | A kind of generated aluminum-base composite foundry goods preparation method |
| CN107760933A (en) * | 2017-09-11 | 2018-03-06 | 南京航空航天大学 | A kind of 3D printing strengthens Al alloy powder and preparation method thereof with in-situ nano complex phase ceramic |
| CN110331311A (en) * | 2019-04-22 | 2019-10-15 | 江苏大学 | A kind of continuous preparation method of in-situ ceramic particle enhanced aluminum-based composite material |
| CN110129641A (en) * | 2019-05-13 | 2019-08-16 | 贵州航天风华精密设备有限公司 | A kind of high-performance original position TiB2Particle enhanced aluminum-based composite material and preparation method thereof |
| CN111663061A (en) * | 2020-06-23 | 2020-09-15 | 江苏大学 | Method for preparing Al-Si alloy grain refiner |
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