CN1557987A - Preparation method for reinforced aluminum base composite material composed by in situ alpha-Al2O3 crystal whisker and TiC grain - Google Patents

Preparation method for reinforced aluminum base composite material composed by in situ alpha-Al2O3 crystal whisker and TiC grain Download PDF

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Publication number
CN1557987A
CN1557987A CNA2004100011587A CN200410001158A CN1557987A CN 1557987 A CN1557987 A CN 1557987A CN A2004100011587 A CNA2004100011587 A CN A2004100011587A CN 200410001158 A CN200410001158 A CN 200410001158A CN 1557987 A CN1557987 A CN 1557987A
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composite
alloy
whisker
type
tic
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CN1297682C (en
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滨 杨
杨滨
王玉庆
张济山
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Beijing University of Technology
University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Abstract

The preparation process of in-situ alpha-Al2O3 whisker and TiC grain composite reinforcing aluminum-base material features that the technological process includes two stages of preparing prefabricated block and smelting aluminum-base composite material. Three kinds of reactant may be selected, including the first kind of Al+Ti+C+O2, the second kind of Al+ C+O2+TiO2, and the third kind of Al+Ti+C+TiO2. The raw materials in the stoichiometric proportion are mixed homogeneously, pressed to form in the pressure of 25-100 MPa and smelted into the composite material. The present invention has the advantages of simultaneous alloy smelting and reinforced phase formation, shortened composite material preparing process and lowered production cost, and the composite material may be used widely in various fields.

Description

In-situ α -Al2O3Preparation method of whisker and TiC particle composite reinforced aluminum matrix composite material
Technical Field
The invention belongs to the field of metal matrix composite materials, and particularly provides in-situ α -Al2O3The preparation method of the whisker and TiC particle composite reinforced aluminum matrix composite material canThe smelting of the matrix alloy and the generation of the reinforced phase are synchronously carried out, the preparation process flow of the composite material is obviously shortened, the manufacturing cost of the metal matrix 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.
Generally, the composite materials are classified into three major categories, namely ceramic matrix composite materials, resin (polymer) matrix composite materials and metal matrix composite materials, according to the type of matrix material. Ceramics are lighter and harder than metals, do not rust,and can mostly resist high temperatures above 1000 ℃, but have the greatest disadvantage of being brittle. The main problems of the laminated resin-based composite material at present are poor transverse mechanical property, low interlaminar shear strength, easy moisture absorption, aging, creep deformation, burning and the like. Compared with resin-based composite materials, the metal-based composite material has the advantages of high temperature resistance, wear resistance, good electric and thermal conductivity, no moisture absorption, no air release, stable size, no aging and the like. However, the development speed of metal matrix composites is still behind that of resin matrix composites because the process technology of metal matrix composites is complicated and the cost is high. However, in the last two decades, with the rapid development of aviation, aerospace, automobile and electronic technologies, metal matrix composites have been increasingly regarded by the developed countries of various skills in the world.
The development of metal matrix composites is largely closely related to the development of reinforcement. Depending on the shape of the reinforcement, metal matrix composites can be generally classified into three major categories, continuous fiber reinforced metal matrix composites, whisker/short fiber reinforced metal matrix composites, and particle reinforced metal matrix composites.
Whiskers generally refer to whiskers having an aspect ratio (l/d generally greater than 10) and a cross-sectional area of less than 52X 10-5cm2The single crystal fiber material of (1). Because the crystal structure of the whisker is complete and the internal defects are few, the strength and the modulus of the whisker are connectedThe theoretical value of the nearly complete crystal material is a reinforcing and toughening agent of a novel composite material (particularly a metal matrix composite material and a ceramic matrix composite material) with very excellent mechanical property.
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 (the crystallization characteristic and the internal defect of β -SiC whisker are prepared by a carbothermic method, silicate is reported, 1993, 2: 33-36) the β -SiC whisker is synthesized by thermally reducing kaolin with superfine carbon powder, and the result shows that the synthesis temperature has obvious influence on the crystal morphology of the whisker2O3The crystal whisker is one of the excellent comprehensive properties, as shown in the table 1, the invention provides an in-situ α -Al2O3The preparation method of the whisker and TiC particle composite reinforced aluminum matrix composite material can be widely used in occasions requiring light high-strength composite materials.
TABLE 1 Properties of partial whiskers
Density (. rho.) tensile Strength. sigmabσbModulus of elasticity of/[ rho]E E/ρ
Melting Point of whisker (. degree. C.)
(103kg/m3) (103MPa) (104m) (105MPa) (105m)
α-Al2O32040 3.96 21 53 4.3 11
B4C 2450 2.52 14 56 4.9 19
α-SiC 2316 3.15 21 - 4.823 -
β-SiC 2316 3.15 21 - 5.512-8.279 -
Si3N41960 3.18 14 44 3.8 12
TiN - 5.2 7 - 2-3 -
AlN 2199 3.3 - - 3.345 -
Cr 1890 7.20 9 13 2.4 3.4
Cu 1080 8.91 3.3 3.7 1.2 1.4
Fe 1540 7.83 13 17 2.0 2.6
Ni 1450 8.97 3.9 4.3 2.1 2.4
In situ reaction α -Al2O3The principle of the preparation technology of the whisker and TiC particle composite reinforced aluminum matrix composite material is as follows: according to the requirement of material design, proper reactants are selected, and a reinforcing phase with fine size and uniform distribution is generated in situ at proper temperature by means of the base metal or alloy and the chemical reaction between the base metal or alloy and the reinforcing phase. 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 ofthe 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.
Disclosure of Invention
The invention aims to provide in-situ α -Al2O3The preparation method of the whisker and TiC particle composite reinforced aluminum matrix composite material is used for occasions requiring light high-strength composite materials.
The invention comprises a fusion casting-in-situ reaction α -Al2O3The preparation method of the whisker and TiC particle composite reinforced aluminum matrix 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 prefabricated block of α -Al generated by fusion casting-in-situ reaction method2O3The whisker, wherein the oxygen mainly comes from the oxygen in the air, the impurity oxygen brought by the in-situ reactant, the oxygen adsorbed on the surface of the powder, the oxygen adsorbed on the surface of the precast block and the oxygen brought by the in-situ reactant, in order to increase α -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 can be selected:
the first type:
the second type:
in the third category:
ti, C and TiO mentioned in the above first, second and third classes2The 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 C is 1: 0.1-0.8; when combined as a second type of reactant, TiO2The proportion range (weight ratio) of C to C is 2: 0.2-0.5; when combined as a third type of reactant, Ti, C and TiO2The ratio (weight ratio) of the components is 4: 15-30.
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 0.5-5 kg 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 1-20 wt% of the alloy is put into a furnacePressing into an alloy melt, keeping the temperature for 1-30 minutes, refining, degassing, pouring into a metal mold or a sand mold or molding by using methods such as extrusion, die casting and the like to obtain an in-situ reaction α -Al2O3The crystal whisker and the TiC particles are compounded and reinforced with the aluminum matrix composite.
Because of α -Al in the aluminum matrix composite material2O3The number of whiskers is often less than 5% by weight and is not easily detected by X-ray diffraction, and therefore, the phase analysis is performed on the reacted reaction mass.
The invention has the advantages that:
(1)α-Al2O3the crystal whisker and the TiC particles are 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 uniformly distributed in the alloy matrix.
(2) Simple process, low cost and easy realization of industrialization.
(3) Al produced by the invention2O3The crystal whisker and TiC have small particle size and are not easy to be brought to the surface of the molten liquid along with the floating of bubbles in the matrix alloy, so that the composite material melt can continue to be used for refining and deteriorating in the cast alloyThe treatment technology carries out refining and modification for many times so as to improve the comprehensive performance of the composite material.
Drawings
FIG. 1 is an X-ray diffraction pattern of a Ti-C-Al reaction mass of the present invention, showing that the reaction mass is formed of TiC, α -Al2O3And C, the generated α -Al is verified by the observation of scanning electron microscope tissue and energy spectrum analysis2O3Whiskers rather than particles. The C diffraction peak appears in the figure in order to eliminate the brittle intermetallic compound Al3The Ti is caused by the intentionally excessive graphite in the ratio of the Ti-C-Al precast block. Because the common ratio of Ti to C is 1 to 1 (mol percent) and Al which is easy to generate brittle phase is selected from the Ti-C-Al precast block3And (3) Ti. The reason is as follows: the aluminum powder in the precast block is firstly melted after the precast block is heated. The molten Al is quickly adsorbed by Ti and C powder in the precast block. On the one hand, Ti on the surface layer of Ti powder is dissolved in molten Al, and when the molten Ti concentration is equal to or greater than 0.15 wt.% (cell composition), a cell reaction occurs to form Al3Ti diffuses into Al liquid. On the other hand, Al distant from Ti particles3Because the temperature of Ti is very high, the concentration of Ti is low, and Ti is easy to decompose into Al and Ti. The decomposed Ti diffuses to the C particles through the Al liquid to form a Ti-rich layer, and the C and the Ti react on an interface to generate TiC. As the reaction proceeds, Ti in the Al liquid is gradually reduced, so that Al which is formed3Ti is gradually decomposed into Ti and Al. When the amount of Ti is relatively excessive, on the one hand, Al3The amount of Ti will increase significantly. On the other hand, Al3The Ti concentration around Ti is high so that Al is formed3Ti is not easily decomposed into Ti and Al, and Al is finally caused3The amount of Ti increases. When the Ti content is excessive, the C content in the prefabricated block is increased to ensure that the prefabricated block and the Ti react completely to generate the required TiC as much as possible, which is helpful for eliminating Al in the composite material3A Ti phase.
FIG. 2 is in situ α -Al in the present invention2O3And scanning the structure of the whisker and TiC particle composite reinforced aluminum matrix composite material.
FIG. 3 is in situ α -Al in the present invention2O3Transmission electron micrograph of whisker, α -Al2O3The shape of the whisker is a straight plate. The diameter of the whisker is less than 100 nm. The Selected Area Diffraction Pattern (SADP) of any single whisker confirms that it is a single crystal with the direction of growth perpendicular to the direction of the crystal plane (0002).
Detailed Description
Example 1
Preparation of 0.3% α -Al2O3Weighing Al powder, Ti powder and C powder with the purity of 98%, 99.8% and 99.5% and the particle size of 75 microns, 45 microns and 10 microns according to the proportion of Al, Ti and C being 2: 70: 28, uniformly mixing, pressing into cylindrical prefabricated block with the diameter of 20 x 30mm on a 50 ton press, melting 2 kg of industrial pure aluminum in an intermediate frequency induction furnace, heating to 850 ℃, pressing 0.06 kg of the prefabricated block into molten aluminum by using a graphite bell jar, preserving heat for 10 minutes, adding hexachloroethane accounting for 0.4 wt% of the molten liquid when the temperature is reduced to 750 ℃, refining, pouring into a metal mold when the temperature of the molten liquid is 720 ℃, and obtaining α -Al with the weight of 0.3 percent2O3Whiskers and 3 wt% TiC/technical pure aluminum composite. Composite material sigmab147MPa and delta of 14 percent.
Example 2
Preparation of 0.45% α -Al2O3Whiskers (calculated. wt.%) and 5 wt.% of a TiC/Al-21Si-2.5Cu composite. In the ratio of Al to TiO2Weighing appropriate amount of Al powder and TiO powder with purity of 98%, 99.8% and 99.5% and particle size of 75 μm, 75 μm and 10 μm respectively in a ratio of C to C of 1: 2.22: 0.332Mixing the powder with the powder C, 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 0.20 kg of prefabricated block into the aluminum liquid by using a graphite bell jar, and keeping the temperature for 15 minutes. And adding hexachloroethane accounting for 0.3 weight percent of the molten liquid for refining. 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 0.45Weight% α -Al2O3Whisker and 5 wt% TiC/Al-21Si-2.5Cu composite. Composite material sigmabIs 450 MPa.
Example 3
Preparation of 0.5% α -Al2O3Whiskers (calculated. wt%) and 5 wt% of a TiC/7075 composite. In the ratio of Al to TiO2Weighing appropriate amount of Al powder and TiO powder with purity of 98%, 99.8% and 99.5% and particle size of 75 μm, 45 μm and 10 μm respectively in a ratio of Ti to C of 1: 2.6: 0.442Powder, Ti powder and CMixing the above powders, pressing into cylindrical prefabricated blocks with diameter of 20 × 30mm on a 50 t press, melting 4 kg of 7075 alloy in a medium frequency induction furnace, heating to 900 deg.C, pressing 0.20 kg of prefabricated blocks into molten aluminum with a graphite bell jar, keeping the temperature for 10 min, adding hexachloroethane 0.3 wt% of the molten liquid, refining, pouring into a metal mold at 730 deg.C to obtain α -Al 0.5 wt%2O3Whiskers and 5 wt% TiC/7075 composite. Composite material sigma after extrusionb675 MPa.

Claims (4)

1. Fusion casting-in-situ reaction α -Al2O3The preparation method of the whisker and TiC particle composite reinforced aluminum matrix 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: three classes of reactants can be selected:
the first type:
the second type:
in the third category:
ti, C and TiO mentioned in the above first, second and third classes2The powder is powder, the particle size range is 10-250 mu m, and the purity is more than 96.0 weight percent;
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 composite material, namely putting 0.5-5 kg of matrix alloy Al and alloy thereof into a medium-frequency induction furnace for heating at a temperature of 150-250 ℃ above the melting point of the alloy, pressing a prefabricated block accounting for 1-20 wt% of the alloy into an alloy melt, preserving heat for 1-30 minutes, refining, degassing, pouring into a metal mold or an extrusion mold for extrusion to obtain in-situ reaction α -Al2O3The crystal whisker and the TiC particles are compounded and reinforced with the aluminum matrix composite.
2. The method of claim 1, wherein: when the first type of reactants are combined, the weight ratio of the Ti to the C is 1: 0.1-0.8.
3. The method of claim 1, wherein: when combined as a second type of reactant, TiO2The weight ratio of the C to the C is 2: 0.2-0.5.
4. The method of claim 1, wherein: when combined as a third type of reactant, Ti, C and TiO2The weight ratio of the components is 4: 15-30.
CNB2004100011587A 2004-02-02 2004-02-02 Preparation method for reinforced aluminum base composite material composed by in situ alpha-Al2O3 crystal whisker and TiC grain Expired - Fee Related CN1297682C (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
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CN103203446A (en) * 2013-03-23 2013-07-17 广州有色金属研究院 Preparation method for local ceramic reinforced aluminum matrix composite wear-resistant part
CN104087878A (en) * 2014-06-30 2014-10-08 北京科技大学 Method for preparing composite material for engine cylinder piston
CN106544531A (en) * 2015-09-22 2017-03-29 中国矿业大学 A kind of process of In-situ Synthesis TiC Particle refining aluminum alloy solidified structure
CN106566938A (en) * 2016-10-30 2017-04-19 山西汾西重工有限责任公司 Aluminum-based composite material melt purification method
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

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1089118C (en) * 1997-04-01 2002-08-14 中国科学院金属研究所 Telchnique for preparing in-situ authigenic metal-base composite material
CN1078257C (en) * 1999-02-03 2002-01-23 北京科技大学 Melting-casting process of preparing metal-base composite material through in-situ reaction and spray formation
CN1108389C (en) * 2000-06-27 2003-05-14 北京科技大学 Process for in-situ alloying and reaction particles reiforced metal-base composition
CN1122114C (en) * 2001-03-23 2003-09-24 中国科学院金属研究所 High-strnegth Ti-base composition reinforced by in-situ combination of crystal whiskers with particles

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103203446A (en) * 2013-03-23 2013-07-17 广州有色金属研究院 Preparation method for local ceramic reinforced aluminum matrix composite wear-resistant part
CN103203446B (en) * 2013-03-23 2015-10-07 广州有色金属研究院 A kind of local pottery strengthens the preparation method of aluminum-base composite wearing piece
CN104087878A (en) * 2014-06-30 2014-10-08 北京科技大学 Method for preparing composite material for engine cylinder piston
CN104087878B (en) * 2014-06-30 2015-12-09 北京科技大学 A kind of preparation method of engine cylinder piston matrix material
CN106544531A (en) * 2015-09-22 2017-03-29 中国矿业大学 A kind of process of In-situ Synthesis TiC Particle refining aluminum alloy solidified structure
CN106566938A (en) * 2016-10-30 2017-04-19 山西汾西重工有限责任公司 Aluminum-based composite material melt purification method
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

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