CN100537801C - A kind of preparation method of aluminum matrix composite - Google Patents
A kind of preparation method of aluminum matrix composite Download PDFInfo
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- CN100537801C CN100537801C CNB2006101379167A CN200610137916A CN100537801C CN 100537801 C CN100537801 C CN 100537801C CN B2006101379167 A CNB2006101379167 A CN B2006101379167A CN 200610137916 A CN200610137916 A CN 200610137916A CN 100537801 C CN100537801 C CN 100537801C
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Abstract
A kind of preparation method of aluminum matrix composite, wherein, this method comprises the aluminium of molten state and KBF
4, K
2TiF
6And TiO
2Mix, be cooled to 500-600 ℃ of reaction then, heat up again and make said mixture to molten state continue reaction, remove by product, obtain the aluminum matrix composite precursor, make described aluminum matrix composite precursor maintain molten state, and the aluminum matrix composite precursor of this molten state is mixed with magnesium, copper.Parameters such as tensile strength, yield strength, elongation at break and Young's modulus by the goods A-frame of the aluminum matrix composite die cast that adopts method provided by the invention to obtain all are significantly improved, the good mechanical properties of the goods that the aluminum matrix composite that adopts method of the present invention to obtain makes is described, especially more excellent in the mechanical property that adopts the goods that obtain after the Hpdc moulding.
Description
Technical field
The invention relates to a kind of preparation method of matrix material, more particularly, is the preparation method about a kind of aluminum matrix composite.
Background technology
Aluminum matrix composite has specific tenacity, specific modulus height, high temperature resistant, wear-resistant and thermal expansivity is little, dimensional stabilizing etc. is excellent physicals and mechanical properties have a wide range of applications in industries such as aerospace, military and national defense field and automobile, electronic instrument.According to the state difference of the two reactive components existence that participates in synthetic wild phase, Gu the preparation method of described aluminum matrix composite mainly comprises solution-air, solid-liquid, solid-three kinds of reaction patterns.
The gas-liquid reaction method also claims the VIS method.This technological principle is as carrier with rare gas element, the gas that will contain C or N feeds in the superalloy liquid, make C or N and the reaction of alloy liquid in the decomposing gas, in alloy substrate, form the carbide or the nitride of tiny, disperse, stable, high rigidity, high elastic coefficient, generate the thermodynamically stable metal-base composites that contains the ceramic particle wild phase after the cooled and solidified.
The solid-liquid reaction method, both form this method by metal direct oxidation method (DIMOXTM) and metal pressure-free impregnation method (PRIMEXTM).The DIMOXTM method is for oxidation under melting condition prepares the metal-base composites that contains the ceramic particle wild phase with metal and alloy thereof.
What the PRIMEXTM method was used is non-oxidizing gas, in this technology, two processes takes place simultaneously: the one, and liquid metal is the infiltration in ceramics preparative spare under the effect of ambiance; The 2nd, the reaction of liquid metal and surrounding gas and produce new enhancing particle.Discover that the quantity of the AlN that original position forms and size depend primarily on the wetting-out rate of Al liquid, and N in the wetting-out rate of Al liquid and the ambiance
2The temperature of dividing potential drop, melt is relevant with composition, and therefore, the tissue of matrix material and performance are easily by adjusting composition, the N of melt
2Dividing potential drop and treatment temp and being controlled effectively.
XDTM method, this method are by U.S.'s Martin Marietta laboratory invention.It is with two solid-state reactive element powder and metallic matrix powder mixes evenly and after the compacting degasification, and pressed compact is heated rapidly to temperature more than the metallic matrix fusing point, and heat-producing chemical reaction takes place in melt the reagent element, generates the wild phase ceramic particle.Prepare matrix material with this Technology, wild phase is wetting by liquid metal, and the interface is just becoming a focus of current matrix material research in conjunction with firmly.But too tiny particle can increase the viscosity of melt greatly, therefore, is difficult to the further casting of this material.
The solid-solid reaction method also claims mechanical alloying method (Mechanical Alloying), and this method is that powder deforms through extruding with different powder ball milling in high energy ball mill, diffusion or carry out solid state reaction and form alloy between atom.
CN1740354A discloses a kind of preparation method of in-situ grain reinforced high temperature aluminium base composite material, adopt the component and the weight percent of the in-situ grain reinforced high temperature aluminium base composite material that this method obtains to be: 11-13%Si, 0.5-1.5%Mg, 0.8-1.3%Cu, 0.8-1.5%Ni, 1-20%TiB
2, surplus is Al; This preparation method may further comprise the steps:
(1) add ZL 102 alloy and Al-Si master alloy or commercial-purity aluminium in crucible, heating up in the fusing back, covers with insulating covering agent, and insulating covering agent adopts the concise no sodium insulating covering agent of aluminium alloy;
(2) with KBF
4And KTiF
6Uniform mixing, the oven dry back adds in the melt, carries out mechanical stirring;
(3) after reaction finishes, take out by product, add technical pure Mg, Al-Ni and Al-Cu master alloy, take off removing dross, vacuumize and leave standstill;
(4) assembling median septum, riser pipe, mould, low pressure molding.
The aluminum matrix composite that adopts this method to obtain is undesirable in the mechanical property of low pressure shaping back goods, after this material is passed through the Hpdc moulding, and poor-performings such as the tensile strength of goods and Young's modulus.
Summary of the invention
The objective of the invention is to overcome the unfavorable defective of goods mechanical property that obtains behind the aluminum matrix composite die cast that to adopt existing preparation method to obtain, provide a kind of goods that die cast is obtained to have the preparation method of the aluminum matrix composite of excellent mechanical performances.
The invention provides a kind of preparation method of aluminum matrix composite, wherein, this method comprises the aluminium of molten state and KBF
4, K
2TiF
6And TiO
2Mix, be cooled to 500-600 ℃ of reaction then, heat up again and make said mixture to molten state continue reaction, remove by product, obtain the aluminum matrix composite precursor, make described aluminum matrix composite precursor maintain molten state, and the aluminum matrix composite precursor of this molten state is mixed with magnesium, copper.
The parameters such as tensile strength, yield strength, elongation at break and Young's modulus of the goods A-frame that the aluminum matrix composite die cast that is obtained by employing method provided by the invention obtains all are significantly improved, the good mechanical properties of the goods that the aluminum matrix composite that adopts method of the present invention to obtain makes is described, especially more excellent in the mechanical property that adopts the goods that obtain after the Hpdc moulding.
Embodiment
According to method provided by the invention, this method comprises the aluminium of molten state and KBF
4, K
2TiF
6And TiO
2Mix, be cooled to 500-600 ℃ of reaction then, heating up makes said mixture to molten state continue reaction again, remove by product, obtain the aluminum matrix composite precursor, make described aluminum matrix composite precursor maintain molten state, and the aluminum matrix composite precursor of this molten state is mixed with magnesium, copper.
Intensification makes aluminium and KBF
4, K
2TiF
6And TiO
2Mixture to molten state refer to aluminium, KBF
4, K
2TiF
6And TiO
2All be in molten state.The temperature of described molten state is 1200-1900 ℃, is preferably 1300-1700 ℃.
Under the preferable case, with the aluminium and the KBF of molten state
4, K
2TiF
6And TiO
2The blended method comprises, under agitation, and with KBF
4, K
2TiF
6And TiO
2Powder is jetted equably in molten state aluminium, by the shearing force that stirs with KBF
4, K
2TiF
6And TiO
2The aluminium thorough mixing of powder and molten state is even, to guarantee KBF
4, K
2TiF
6And TiO
2Can be evenly distributed in the aluminum matrix composite.
Described aluminium and KBF
4, K
2TiF
6And TiO
2Charge weight than for 1:0.03-1.2:0.03-1.2:0.1-0.4, be preferably 1:0.05-1:0.05-1:0.15-0.35.
According to method of the present invention, oxidized in order to prevent molten state aluminium, under the preferable case, described aluminium and KBF with molten state
4, K
2TiF
6And TiO
2Be blended in the rare gas element and carry out, described rare gas element refers to not any one gas or the gaseous mixture with reactant and product generation chemical reaction, as in nitrogen, the periodic table of elements zero group gas one or more, be preferably in argon gas, nitrogen and the helium one or more.
For by the shearing force that stirs with KBF
4, K
2TiF
6And TiO
2With the aluminium thorough mixing of molten state, described stirring is preferably carried out under high-speed stirring, and stirring velocity is preferably 500-800 rev/min.
Described aluminium is 1:0.01-0.08:0.02-0.1 with the charge weight ratio of magnesium, copper.
In order further to improve the mechanical property of aluminum matrix composite, under the preferable case, this method comprises that also the aluminum matrix composite precursor with molten state mixes with zinc and chromium, described aluminum matrix composite precursor with molten state and zinc and chromium mix can with the aluminum matrix composite precursor of molten state and magnesium, copper blended simultaneously, before or after carry out, preferably simultaneously, the aluminum matrix composite precursor of molten state is mixed with zinc and chromium the aluminum matrix composite precursor of molten state and magnesium, copper blended.Described aluminium is 1:0-0.2:0-0.2 with the charge weight ratio of zinc, chromium, is preferably 1:0.1-0.2:0.1-0.2.
According to the present invention, with the aluminium and the KBF of molten state
4, K
2TiF
6And TiO
2After mixing, with aluminium and KBF
4, K
2TiF
6And TiO
2Temperature of reaction to reduce to 500-600 ℃ purpose be to make the aluminum matrix composite that obtains have good mechanical property.Because the semi-solid temperature of base aluminum is 565 ℃, at 550-570 ℃, reacts under the semi-solid temperature near base aluminum, can make the aluminum matrix composite that obtains have better mechanical property; Can also be the time by this material die cast, reduce conventional die casting inherent subsurface porosity and defective such as loose, improve casting quality, increase die life, therefore, preferably make described aluminium and KBF
4, K
2TiF
6And TiO
2Temperature of reaction reduce to 550-570 ℃ of reaction.Described at 500-600 ℃, the time of reacting under preferred 550-570 ℃ can be for greater than 1 minute, reaction times surpasses after 60 minutes, the performance of the aluminum matrix composite that obtains has not had obvious variation, therefore at 500-600 ℃, the time of reacting under preferred 550-570 ℃ is preferably 5-60 minute.
Aluminium and KBF with molten state
4, K
2TiF
6And TiO
2Mixture place 500-600 ℃ of reaction to finish after, it is in order to make reaction more thorough that this mixture is warming up to the purpose that molten state continues reaction.The time of reacting under the molten state of reaction mixture can be for greater than 1 minute, reaction times surpasses after 10 minutes, the performance of the aluminum matrix composite that obtains has not had obvious variation, and therefore the time of reacting under the melt temperature of aluminium is preferably 5-10 minute.
In reaction process, the by product of generation comprises sylvite and the Al that generates in the reaction process
2O
3Oxide inclusion, the method for removing described by product is conventionally known to one of skill in the art, in general, the method for removing described by product is included in the aluminum matrix composite precursor with before magnesium, copper mix, at aluminium and KBF
4, K
2TiF
6And TiO
2The mixed melting thing in add scouring agent and/or feed rare gas element.
The kind of described scouring agent and add-on are conventionally known to one of skill in the art, as, described scouring agent can be selected from KCl, NaCl, NaSiF
6, Na
3AlF
6In one or more, the add-on of described scouring agent and aluminium, KBF
4, K
2TiF
6And TiO
2The weight ratio of total add-on be 0.01-0.05:1.
Add rare gas element and can make melts produce bubble, in floating-upward process, can adsorb Al by these bubbles
2O
3Inclusion makes it to float in the slag on mixture surface, has just removed by product when slag is salvaged out.In addition, the hydrogen that rare gas element can also absorption reaction generates in the process of come-up, and escape in the atmosphere, thereby reduced the concentration of hydrogen in the mixture.Described rare gas element can feed in the mixture by conduit, as graphite guide tube.The kind of described rare gas element and add-on are conventionally known to one of skill in the art, be selected from and both be insoluble to melts, again not with the gas of melts and hydrogen reaction, as in nitrogen, the periodic table of elements zero group gas one or more.
With the method for aluminum matrix composite die cast is conventionally known to one of skill in the art, as, described forming method can adopt low pressure molding or high-pressure molding, and the present invention preferably adopts the method for high-pressure molding that aluminum matrix composite is carried out die cast.The method of described high-pressure molding comprises transfer mold is preheated to 200-300 ℃, aluminum matrix composite with molten state pours in the chamber of transfer mold then, type is filled in the die casting of pressurizeing to aluminum matrix composite, described mold filling pressure is the 60-110 MPa, keep top pressure 5-15 second, finish this die casting operation after the goods that obtain are solidified fully, obtain the goods that obtain by after the described aluminum matrix composite compression moulding.
Below will the present invention will be further described by specific embodiment.
Embodiment 1
Present embodiment illustrates the preparation method of aluminum matrix composite provided by the invention and goods.
Under 720 ℃, in resistance furnace, add 80 gram commercial-purity aluminiums, make the aluminium fusion, then, under nitrogen protection, and under 600 rev/mins stirring velocity, with 4 gram KBF
4, 4 the gram K
2TiF
6With 12 gram TiO
2Powder is evenly jetted in molten aluminum; with fused aluminium thorough mixing; then; be cooled to 565 ℃; under nitrogen protection, and after reacting 30 minutes under 650 rev/mins the stirring velocity, stop to stir, heat up again said mixture to molten state (1300 ℃); react after 8 minutes, add 2 gram scouring agent NaSiF then
6And stir and to obtain the aluminum matrix composite precursor after removing by product, this aluminum matrix composite precursor is continued to maintain molten state (1300 ℃), and adding 1.2 gram technical pure Mg, 2.4 restrain Cu in the aluminum matrix composite precursor of this molten state, mix, remove removing dross, obtain aluminum matrix composite.
The A-frame transfer mold is preheating to 220 ℃, set die-casting technological parameter, described processing parameter comprises that two positions are made as 280 ± 30 millimeters, a position is made as 130 ± 30 millimeters, the die sinking time is 4.5 ± 2 seconds, ejecting time-delay is 4.0 ± 2 seconds, pumping rate is 4.0 ± 2 circles, close die cavity then, pour into the above-mentioned aluminum matrix composite melt that obtains, type is filled in pressurization die casting, reach the top pressure of 110 MPas until squeeze pressure, keep maximal pressure casting pressure 5 seconds, and treated that composite castings solidified fully, obtain goods A-frame A1 provided by the invention.Behind the die cast, A1 carries out T6 thermal treatment to these goods.
Embodiment 2
Present embodiment illustrates the preparation method of aluminum matrix composite provided by the invention and goods.
Under 720 ℃, in resistance furnace, add 80 gram commercial-purity aluminiums, make the aluminium fusion, then, under nitrogen protection, and under 650 rev/mins stirring velocity, with 14 gram KBF
4, 12 the gram K
2TiF
6With 16 gram TiO
2Powder is evenly jetted in molten aluminum; with the molten aluminum thorough mixing; then; be cooled to 565 ℃; under nitrogen protection; and after reacting 40 minutes under 650 rev/mins the stirring velocity, stop to stir; heat up again said mixture to molten state (1350 ℃); react after 5 minutes, add 1.7 gram KCl scouring agents then, and stir and obtain the aluminum matrix composite precursor after removing by product; this aluminum matrix composite precursor is continued to maintain molten state (1350 ℃); and adding 1.6 restrains technical pure Mg in the aluminum matrix composite precursor of this molten state; 3.2 gram copper mixes, and removes removing dross, obtains aluminum matrix composite.
The A-frame transfer mold is preheating to 250 ℃, configure die-casting technological parameter, described processing parameter comprises that two positions are made as 280 ± 30 millimeters, a position is made as 130 ± 30 millimeters, the die sinking time is 4.5 ± 2 seconds, ejecting time-delay is 4.0 ± 2 seconds, pumping rate is 4.0 ± 2 circles, close die cavity then, pour into the above-mentioned aluminum matrix composite melt that obtains, type is filled in pressurization die casting, reach the top pressure of 110 MPas until squeeze pressure, keep maximal pressure casting pressure 5 seconds, and treated that composite castings solidified fully, obtain goods A-frame A2.Behind the die cast, goods A2 is carried out T6 thermal treatment.
Embodiment 3
Present embodiment illustrates the preparation method of aluminum matrix composite provided by the invention and goods.
Under 720 ℃, in resistance furnace, add 80 gram commercial-purity aluminiums, make the aluminium fusion, then, under argon shield, and under 650 rev/mins stirring velocity, with 30 gram KBF
4, 35 the gram K
2TiF
6With 24 gram TiO
2Powder is evenly jetted in molten aluminum; with the molten aluminum thorough mixing; then; be cooled to 565 ℃; under the helium protection, and stop to stir after reacting 50 minutes under 650 rev/mins the stirring velocity, heating up is warming up to molten state (1550 ℃) with said mixture again; react after 7 minutes, add 3 gram NaSiF then
6With 2 gram KCl scouring agents, and in this mixed melting thing, feed continuously nitrogen, and stir and remove by product, obtain the aluminum matrix composite precursor, this aluminum matrix composite precursor is continued to maintain molten state (1550 ℃), and in the aluminum matrix composite precursor of this molten state, add 3.2 gram technical pure Mg, 4 gram technical pure Zn, 4 gram Cu and 6 gram Cr, mixed 6 minutes, remove removing dross, obtain aluminum matrix composite.
The A-frame transfer mold is preheating to 240 ℃, configure die-casting technological parameter, described processing parameter comprises that two positions are made as 280 ± 30 millimeters, a position is made as 130 ± 30 millimeters, the die sinking time is 4.5 ± 2 seconds, ejecting time-delay is 4.0 ± 2 seconds, pumping rate is 4.0 ± 2 circles, close die cavity then, pour into the above-mentioned aluminum matrix composite melt that obtains, type is filled in pressurization die casting, reach the top pressure of 110 MPas until squeeze pressure, keep maximal pressure casting pressure 10 seconds, and treated that composite castings solidified fully, obtain the goods A-frame A3 that obtains by aluminum matrix composite.Behind the die cast, goods A3 is carried out T6 thermal treatment.
Embodiment 4
Present embodiment illustrates the preparation method of aluminum matrix composite provided by the invention and goods.
Under 720 ℃, in resistance furnace, add 80 gram commercial-purity aluminiums, make the aluminium fusion, then, under argon shield, and under 650 rev/mins stirring velocity, with 60 gram KBF
4, 56 the gram K
2TiF
6With 28 gram TiO
2Powder is evenly jetted in molten aluminum; with the molten aluminum thorough mixing; then; be cooled to 565 ℃; under argon shield, and stop to stir after reacting 15 minutes under 650 rev/mins the stirring velocity, heating up is warming up to molten state (1700 ℃) with said mixture again; react after 10 minutes, add 6 gram Na then
3AlF
6Scouring agent, and in this mixed melting thing, feed continuously nitrogen, and stir and to remove by product and obtain the aluminum matrix composite precursor, this aluminum matrix composite precursor is continued to maintain molten state (1700 ℃), and adding 4.8 gram technical pure Mg, 7 gram Cu and 8 restrain Cr in the aluminum matrix composite precursor of this molten state, mixed 7 minutes, and removed removing dross, obtain aluminum matrix composite.
The A-frame transfer mold is preheating to 260 ℃, configure die-casting technological parameter, described processing parameter comprises that two positions are made as 280 ± 30 millimeters, a position is made as 130 ± 30 millimeters, the die sinking time is 4.5 ± 2 seconds, ejecting time-delay is 4.0 ± 2 seconds, pumping rate is 4.0 ± 2 circles, close die cavity then, pour into the above-mentioned aluminum matrix composite melt that obtains, type is filled in pressurization die casting, reach the top pressure of 110 MPas until squeeze pressure, keep maximal pressure casting pressure 15 seconds, and treated that composite castings solidified fully, obtain the goods A-frame A4 that obtains by aluminum matrix composite.Behind the die cast, goods A4 is carried out T6 thermal treatment.
Comparative Examples 1
The aluminum matrix composite of this Comparative Examples explanation prior art and the preparation method of goods.
Prepare aluminum matrix composite according to CN1740354A embodiment 1 disclosed method, and, obtain reference goods A-frame B1 according to the above-mentioned aluminum matrix composite of die casting parameter die casting in the embodiment of the invention 1 method.Behind the die cast, goods B1 is carried out T6 thermal treatment.
Embodiment 5-8
The following examples illustrate the performance of goods provided by the invention.
Goods A1-A4 to embodiment 1-4 preparation carries out every performance test, and testing method is as follows:
(new three thinks measurement technology company limited, CMT5205) goes up tensile strength, yield strength, elongation at break and the Young's modulus that testing standard is measured goods, and test result is as shown in table 1 below in the universal material experimental machine with GB GBT228 standard.
Comparative Examples 2
The performance of the goods that this Comparative Examples explanation prior art provides.
Goods B1 to Comparative Examples 1 preparation carries out every performance test, and testing method is as follows:
(new three thinks measurement technology company limited, CMT5205) goes up tensile strength, yield strength, elongation at break and the Young's modulus of measuring goods, and test result is shown in following table 1 in the universal material experimental machine with GB GBT228 standard.
Table 1
| The embodiment numbering | The goods numbering | Tensile strength (MPa) | Yield strength (MPa) | Elongation at break (%) | Young's modulus (gpa) |
| Embodiment 5 | A1 | 362 | 311 | 3.7 | 89 |
| Embodiment 6 | A2 | 421 | 373 | 5.1 | 102 |
| Embodiment 7 | A3 | 493 | 418 | 5.6 | 113 |
| Embodiment 8 | A4 | 495 | 413 | 5.5 | 115 |
| Comparative Examples 2 | B1 | 352 | 303 | 3.3 | 82 |
By last table 1 as can be seen, the goods B1 that obtains with respect to the aluminum matrix composite die cast of prior art, the tensile strength of the goods A1-A4 that aluminum matrix composite die cast of the present invention obtains has improved 2.8-40.6%, yield strength has improved 2.6-37.9%, elongation at break has increased 12.1-69.6%, and Young's modulus has improved 8.5-40.2%.The good mechanical properties of the goods that the aluminum matrix composite that as seen adopts method of the present invention to obtain makes and being significantly improved, especially more excellent in the mechanical property that adopts the goods that obtain after the Hpdc moulding.
Claims (8)
1, a kind of preparation method of aluminum matrix composite is characterized in that, this method comprises the aluminium of molten state and KBF
4, K
2TiF
6And TiO
2Mix and obtain mixture, be cooled to 500-600 ℃ of reaction then, heat up again and make said mixture to molten state continue reaction, remove by product, obtain the aluminum matrix composite precursor, make described aluminum matrix composite precursor maintain molten state, and the aluminum matrix composite precursor of this molten state is mixed with magnesium and copper.
2, method according to claim 1, wherein, described with aluminium and KBF
4, K
2TiF
6And TiO
2The blended method comprises under agitation, with KBF
4, K
2TiF
6And TiO
2Powder is jetted equably in molten state aluminium.
3, method according to claim 1, wherein, the aluminium of described molten state and KBF
4, K
2TiF
6And TiO
2Be blended in the rare gas element and carry out.
4, method according to claim 1, wherein, described aluminium and KBF
4, K
2TiF
6And TiO
2Charge weight than for 1:0.03-1.2:0.03-1.2:0.1-0.4.
5, method according to claim 1, wherein, described aluminium is 1:0.01-0.08:0.02-1 with the charge weight ratio of magnesium, copper.
6, method according to claim 1, wherein, this method comprises that also the aluminum matrix composite precursor with molten state mixes with zinc and chromium.
7, method according to claim 6, wherein, described aluminium is 1:0-0.2:0-0.2 with the charge weight ratio of zinc, chromium.
8, method according to claim 1, wherein, before described method of removing by product is included in the aluminum matrix composite precursor that will obtain and magnesium, copper mixes, to aluminium and KBF
4, K
2TiF
6And TiO
2The mixed melting thing in add scouring agent and/or feed rare gas element.
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|---|---|---|---|
| CNB2006101379167A CN100537801C (en) | 2006-10-30 | 2006-10-30 | A kind of preparation method of aluminum matrix composite |
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|---|---|---|---|
| CNB2006101379167A CN100537801C (en) | 2006-10-30 | 2006-10-30 | A kind of preparation method of aluminum matrix composite |
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|---|---|
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| CN100537801C true CN100537801C (en) | 2009-09-09 |
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Effective date of registration: 20201214 Address after: No.8 huozhan Road, Jingjiang Economic and Technological Development Zone, Taizhou City, Jiangsu Province, 214500 Patentee after: Jiangsu Dexiang Chemical Machinery Co.,Ltd. Address before: 518119 BYD Industrial Park, Yanan Road, Kwai Chung Town, Longgang District, Guangdong, Shenzhen Patentee before: BYD Co.,Ltd. |
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