CN1078257C - Melting-casting process of preparing metal-base composite material through in-situ reaction and spray formation - Google Patents
Melting-casting process of preparing metal-base composite material through in-situ reaction and spray formation Download PDFInfo
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Abstract
The present invention provides a preparing technology for forming metal based composite materials through atomization and spraying by fusion casting-in-situ reactions, which solves the problems of particle loss and the nonuniform distribution of particles in alloy basal bodies existing in the present preparing technologies for forming metal based composite materials through spraying by in-situ reactions. Basal body alloy is smelted while the generation of wild phases and the preparation of blanks of metal based composite materials formed through atomization and spraying are realized, a technological process for preparing composite materials is obviously shortened, and the manufacturing cost of metal based composite materials is greatly reduced. The present invention can be used for preparing various particle reinforced metal based composite materials including aluminium based alloy, copper based alloy, zinc based alloy, titanium based alloy and ferrous based alloy.
Description
The present invention is applicable to the metal-base composites field.Relate to founding-reaction in atomised jet form metal based composites preparation technology.
The atomised jet forming technique is a kind of novel mmaterial synthetic technology, its outstanding advantage is to have the nearly ability that is shaped of rapid solidification, the blank with definite shape that can directly have rapid solidification tissue and performance characteristic by liquid metal atomizing and formation of deposits is to reduce or to remove various expensive manufacturings and process middle-chain.Utilize spray forming technology to prepare the important directions that particles reiforced metal-base composition is this technology development in recent years.But existing domestic and international reaction-injection moulding particles reiforced metal-base composition technology of preparing is in the reaction-injection moulding process a certain amount of wild phase particle to be sprayed in the atomizing cone mostly, deposits on depositor to obtain the matrix material blank with metal drop Forced Mixing (or reaction in) back.The disadvantage of these class methods is that the enhanced granule utilization ratio is low (according to estimates, to be had the enhanced granule more than 50% to fail to enter atomizing cone approximately, but is taken away by air-flow, cause very big waste.Someone in addition think that this is the deadly defect that existing codeposition reaction-injection moulding prepares metal-base composites), material preparation cost height.
In recent years, reaction in (in-situ reaction) particles reiforced metal-base composition new preparation technology has obtained development rapidly, and reaction in atomised jet forming technique be wherein up-to-date also be one of important techniques very, its tempo is subjected to the common concern of domestic and international research unit and industrial community.So far, the reaction that may carry out in the reaction in reaction-injection moulding process comprises:
1. gas-liquid reaction: promptly in the atomised jet forming process, (or all) reactant gas is (as N to sneak into certain proportion in atomizing gas
2, O
2Or CH
4Deng), impel the second particulate original position generation mutually by the composition of adjusting atomizing gas and molten metal.
Metal liquid stream is atomized into the very little drop of particle diameter in Models of Spray Deposition, and its drop size depends on the size of nozzle and the flow velocity of metal and atomization air flow.Lubanska (JOM, 22 (1970) 45) has derived the radius relationship formula of estimating metal drop size:
η is a dynamic viscosity in the formula, and j is a mass flow rate, N
WeBe the Weber number, its value is (T.W.Clyne and P.J.Withers, An Introduction to Metal Matrix Composites, Cambridge University Press, London (1993)):
U is a liquid drop speed in the formula, and λ is the surface tension of drop.During with the hydrogen atomized aluminum, know about 100～200 μ m of the mean diameter of drop by (1) and (2) formula.These drops had both had very high temperature, had very big body surface area again simultaneously, and this just provides motivating force for the chemical reaction in the Models of Spray Deposition.By means of in the drop flight course and the chemical reaction between the atomizing gas and on matrix in the deposition process of setting and the chemical reaction that adds between the reaction particles can generate the tiny wild phase ceramic particle of granularity.
The people such as Lavernia of California university (Scr.Metall.Mater., 29 (1993) 1341) adopt N
2-O
2Mixed gas atomised jet shaping Ni
3Al alloy (containing Y and B) has obtained the Al that small and dispersed distributes
2O
3And Y
2O
3Particle enhanced Ni
3The Al based composites.By the oxygen partial pressure in the control mixed gas, content and distribution of sizes thereof that can the controlled oxidation composition granule, as increase the oxygen level in the mixed gas or increase the dispersity (promptly reducing droplet size) of aluminium liquid, can improve the degree of oxidation of molten drop, promptly increase the formation amount of oxide compound.Microstructure and mechanics property analysis result show, the thermostability of reaction synthetic composite material obviously improves, as in 1200 ℃ of insulating processes, crystal grain in the nitrogen atomization jet deposition formation material is constantly grown up with holding time prolonging, and adopts the crystal grain that contains oxygen reaction spray atomization and deposition shaped material that any variation takes place hardly.
People such as Perez (Ser.Metall.Mater., 31 (1994) 231) adopt N
2-O
2Mixed gas spray atomization and deposition shaping Cu-1at%Al alloy.When oxygen level was 8%, original position had formed the Al of about 1vol%
2O
3CuO/Cu with about 2～4vol%
2O.
People such as Peng Xiaodong (material Leader, (2) (1993) 72B) are dispersed into a large amount of tiny molten drops with aluminium liquid in oxidizing atmosphere, make its surface oxidation generate Al
2O
3Film.These Al
2O
3Film can finally just form the Al that disperse distributes because of colliding broken in the deposition process between the molten drop mutually and spreading out
2O
3Reinforced aluminum matrix composites.
2. liquid-liquid reaction: in atomization process, two kinds of liquid metals are mixed, can form refractory grain by reaction.People such as Lee (Proc.MRS, 132 (1989) 87) have reported and have utilized liquid-liquid prepared in reaction TiB
2The experimental result of granule reinforced copper base composite material.But utilize liquid-liquid reaction to tend to emit a large amount of reaction heat when forming refractory grain, cause melt to heat rapidly, bring very big difficulty for the control of spray atomization and deposition forming process, so the application of this method is restricted.
Gu 3. liquid-reaction: in the spray atomization and deposition forming process, Gu there are some possible liquid-reactions.The particle that sprays into dissolves in atomization process and generates stable disperse phase with one or more element reactions in the matrix.By the rate of cooling of control spraying and subsequently the rate of cooling of blank can control the size of disperse phase.Quote the unexposed experimental result of delivering of Britain AEA company according to people such as Lawley (Powder Metall., 37 (1994) 123), in nitrogen atomization jet deposition formation process, in 316L that contains Ti and 304 stainless steel molten drops, spray into Cr
xThe N particle can form the tiny TiN disperse phase of the about 20nm of diameter in blank, its result will make the mechanical property of material be significantly improved.
As everyone knows, the performance of particles reiforced metal-base composition depends on that to a great extent can particle distribute in disperse in matrix.Because gas-liquid reaction mainly is that outside surface at molten drop carries out, and therefore causes wild phase to assemble easily and is distributed in the crystal boundary area, has weakened the strengthening effect of wild phase.Liquid-liquid reaction often reaction is too fierce, is difficult to control, has also limited the application of this method.Gu the technology of passing through liquid-required wild phase of reaction acquisition that proposes has recently been widened the preparation approach of reaction in reaction-injection moulding metal-base composites, but preceding topic is to find a kind of labile supersaturation metastable (or hyperergy) solid granulates, and this brings numerous difficulties for this class solid granulates of test and Selection.And as mentioned above, Gu the wild phase in the existing domestic and international reaction in atomised jet shaping generates by gas-liquid and liquid-reaction in spray chamber without exception, the wild phase particle utilization ratio that generates by these class methods is still lower.
The object of the present invention is to provide a kind of simple and practical, relative low price, reaction in atomised jet form metal based composites preparation method easy to utilize.This method places the melting chamber alloy melt to finish (being called founding-reaction in) generation of wild phase, and then carries out follow-up atomised jet forming step, to obtain the particles reiforced metal-base composition that even dispersion distributes.
Formation of the present invention: founding-when reaction in reaction-injection moulding method prepared metal-base composites, technological process mainly comprised the preparation of prefabricated section, the melting and the atomised jet shaping three phases of mother alloy: the preparation of (3) prefabricated section in employing
The selection of reactant species: according to the requirement of compound system, determine to participate in the reactant that reaction forms the hard particles phase, comprise two classes to particle wild phase kind:
The first kind:
(3) in the formula, M represents matrix element Al, Cu and alloy thereof; X represents metallic element or non-metallic element Ti, Zr, V, Mo, C, B, Si; Y represents non-metallic element, as C, and B, Si.When X was non-metallic element, XY was the combination of C and B or C and two kinds of non-metallic elements of Si.
Second class:
(4) in the formula, M represents matrix element Al, and alloy; N represents magnesium-yttrium-transition metal Cu, Zn, Cr.Said metallic element, non-metallic element and transition group metallic oxide are Powdered in above-mentioned first and second class, and size range is 10～250 μ m.
When two kinds of reactants were Ti and C combination, its ratio range (weight ratio) was 1: 0.1～0.7; If Ti and B combination, its ratio range (weight ratio) is 1: 0.1～0.8; If Al and CuO combination, its ratio range (weight ratio) is 1: 0.2～0.7.
Can add a certain amount of catalyzer or stopping agent according to the complexity of system reaction in the preparation prefabricated section process.Said catalyzer is Al, Ni, Cu.Said stopping agent comprises two classes: a class is Si, SiO
2, Al
2O
3, they do not participate in the chemical reaction between the reactant, only play the effect of thinner; Another kind of is villaumite and villiaumite, and they participate in the chemical reaction between the reactant.The weight ratio of catalyzer and two kinds of reactants is (0～0.8): 1.When having added the stopping agent of thinner effect, the weight ratio of stopping agent and two kinds of reactants is (0.05～0.5): 1; When adding the stopping agent that participates in chemical reaction between the reactant, the weight ratio of villaumite and villiaumite and two kinds of reactants is (0.03～0.20): 1.
Mix: above-mentioned various raw materials are put into mixer by certain stoichiometric ratio mix.In order to improve the plasticity of prefabricated section, can in the raw material that mixes, add the organic volatile binding agent, the organic volatile binding agent is (0.02～0.15) with the raw material weight ratio that mixes: 1; These binding agents can volatilize or decompose at a certain temperature fully.
Compression moulding: with the raw material compression moulding at room temperature that mixes, pressure range is 50～500MPa.(4) melting of matrix material mother alloy
The melting of matrix alloy: with an amount of matrix alloy Al, Cu puts into medium-frequency induction furnace and heats, and Heating temperature is above 150～300 ℃ of this alloy melting point.
Add prefabricated section: the prefabricated section that will account for weight alloy 1～20% is pressed in the alloy melt with the graphite bell jar, insulation: 1～30 minute.(3) preparation of atomised jet form metal based composites blank
Because tiny, thermodynamically stable enhanced granule generates in the melting chamber alloy melt entirely, so follow-up atomised jet forming step can be continued to use every processing parameter that existing reaction-injection moulding prepares the metallic substance blank among the present invention:
| Atomizing gas | High pure nitrogen |
| Atomizing pressure | (0.5-0.9)MPa |
| The superheating temperature of melt | (150-300)℃ |
| The catheter diameter | (3.0-3.6)mm |
| The deposition distance | (350-450)mm |
The present invention proposes to introduce the method that founding-reaction in generates the particle wild phase in reaction-injection moulding metal-base composites preparation process, is reaction in reaction-injection moulding metal-base composites Development of Preparation Technology.
The invention has the advantages that: (1) enhanced granule utilization ratio height, particle is evenly distributed in alloy substrate.The present invention places the melting chamber alloy melt to finish the generation of enhanced granule, has solved the problem of particle loss in the domestic and foreign current reaction in reaction-injection moulding metal-base composites technology of preparing at all.And, utilize wild phase particle size that the present invention generates mostly below 1 μ m, sinking velocity is very little.These enhanced granule are through the stirring of melt electromagnetic force and the effect of molten drop spray atomization and deposition, and disperse is distributed among the matrix very equably.(2) technology is easy, and cost is cheap relatively, is easy to realize industrialization.Reaction in reaction-injection moulding metal-base composites technology of preparing before will spray into certain reaction gas or hyperergy particle without exception in spray chamber, to obtain required wild phase particle.The present invention moves into the generation of enhanced granule in the melting chamber alloy melt from spray chamber and finishes.Generate the particulate whole process and all under atmospheric condition, carry out, simple to operation.And melting, the particulate of matrix alloy are generated in the present invention and the preparation of reaction-injection moulding metal-base composites is carried out synchronously, thereby can obviously shorten preparation technology's flow process of matrix material, the preparation cost of reduction material, is easy to realize industrialization.(3) can continue to use refining and Modification Treatment Technique in the casting alloy repeatedly, improve the over-all properties of matrix material.The wild phase particle size of utilizing the present invention to generate is little, fine with the wettability of matrix alloy, particle can not bring to molten surface with the bubble floating in the matrix alloy, thereby matrix material mother alloy melt can continue to use the refining in the casting alloy and Modification Treatment Technique is carried out repeatedly refining and the processing of going bad, to improve the over-all properties of matrix material.(4) can continue to use every processing parameter that existing reaction-injection moulding prepares the metallic substance blank, equipment need not to do any change.The process all fours that follow-up reaction-injection moulding process and existing reaction-injection moulding prepare metallic substance among the present invention, equipment need not to do any change.
Embodiment 1
Preparation reaction-injection moulding 3% (weight) TiC/ commercial-purity aluminium matrix material.In Al: Ti: C=2: 70: 28 ratio takes by weighing an amount of purity and is respectively 98%, 99.8% and 99.5%, and granularity is respectively Al powder, Ti powder and the C powder of 75 μ m, 45 μ m and 10 μ m, and it is mixed.On 50 tons of press, be pressed into the cylindrical prefabricated section of φ 20 * 30mm.2 kilograms of commercial-purity aluminiums are put into medium-frequency induction furnace melt, and be heated to 850 ℃.Be pressed in the aluminium liquid with the prefabricated section of graphite bell jar, be incubated 10 minutes 0.06 kilogram.When treating that temperature is reduced to 750 ℃ of left and right sides, add the hexachloroethane refining that accounts for liquation weight 0.4%.At atomizing gas is that nitrogen, atomizing pressure are that 0.6MPa, catheter diameter are reaction-injection moulding under the 3.0mm, obtains 3% (weight) TiC particle and strengthens the commercial-purity aluminium matrix material.Matrix material σ
bBe not less than 140MPa, δ is not less than 10%.
Embodiment 2
Preparation 3% (weight) TiB
2/ commercial-purity aluminium matrix material.In Al: Ti: B=30: 40: 30 ratio takes by weighing an amount of purity and is respectively 98%, 99.8% and 99.9%, and granularity is respectively Al powder, Ti powder and B powder and an amount of refining agent of 75 μ m, 45 μ m and 10 μ m, and it is mixed.On 50 tons of press, be pressed into the cylindrical prefabricated section of φ 20 * 30mm.2 kilograms of commercial-purity aluminiums are put into medium-frequency induction furnace melt, and be heated to 900 ℃.Be pressed in the aluminium liquid with the prefabricated section of graphite bell jar, be incubated 10 minutes 0.06 kilogram.Add the hexachloroethane refining that accounts for liquation weight 0.3%.At atomizing gas is that nitrogen, atomizing pressure are that 0.6MPa, catheter diameter are reaction-injection moulding under 3.0～3.2mm, obtains 3% (weight) TiB
2/ commercial-purity aluminium matrix material.Extruding back matrix material σ
bBe not less than 180MPa.
Embodiment 3
Preparation reaction-injection moulding 5% (weight) TiC/Al-21Si-2.5Cu matrix material.In Al: Ti: C=3: 72: 25 ratio takes by weighing an amount of purity and is respectively 98%, 99.8% and 99.5%, and granularity is respectively Al powder, Ti powder and C powder and an amount of refining agent of 75 μ m, 45 μ m and 10 μ m, and it is mixed.On 50 tons of press, be pressed into the cylindrical prefabricated section of φ 20 * 30mm.4 kilograms of Al-21Si-2.5Cu alloys are put into medium-frequency induction furnace melt, and be heated to 950 ℃.Be pressed in the aluminium liquid with the prefabricated section of graphite bell jar, be incubated 10 minutes 0.20 kilogram.Add the hexachloroethane refining that accounts for liquation weight 0.3%.At atomizing gas is that nitrogen, atomizing pressure are that 0.6～0.8MPa, catheter diameter are reaction-injection moulding under 3.0～3.6mm, obtains 5% (weight) TiC/Al-21Si-2.5Cu matrix material.Matrix material σ
bBe not less than 400MPa.
Embodiment 4
Preparation 8% (weight) TiC/7075 matrix material.In Al: Ti: C=2: 71: 27 ratio takes by weighing an amount of purity and is respectively 98%, 99.8% and 99.5%, and granularity is respectively Al powder, Ti powder and the C powder of 75 μ m, 45 μ m and 10 μ m, and it is mixed.On 50 tons of press, be pressed into the cylindrical prefabricated section of φ 20 * 30mm.5 kilogram of 7075 alloy put into medium-frequency induction furnace melt, and be heated to 900 ℃.Be pressed in the aluminium liquid with the prefabricated section of graphite bell jar, be incubated 10 minutes 0.40 kilogram.Add the hexachloroethane refining that accounts for liquation weight 0.3%.At atomizing gas is that nitrogen, atomizing pressure are that 0.6～0.7MPa, catheter diameter are reaction-injection moulding under 3.0～3.6mm, obtains the 8wt.%TiC/7075 matrix material.Matrix material σ
bBe not less than 550MPa.
Embodiment 5
Preparation 5% (weight) TiC/7075 matrix material.In Al: Ti: C=2: 71: 27 ratio takes by weighing an amount of purity and is respectively 98%, 99.8% and 99.5%, and granularity is respectively Al powder, Ti powder and the C powder of 75 μ m, 45 μ m and 10 μ m, and it is mixed.On 50 tons of press, be pressed into the cylindrical prefabricated section of φ 20 * 30mm.4 kilogram of 7075 alloy put into medium-frequency induction furnace melt, and be heated to 900 ℃.Be pressed in the aluminium liquid with the prefabricated section of graphite bell jar, be incubated 10 minutes 0.20 kilogram.Add the hexachloroethane refining that accounts for liquation weight 0.3%.At atomizing gas is that nitrogen, atomizing pressure are that 0.6～0.7MPa, catheter diameter are reaction-injection moulding under 3.0～3.5mm, obtains 5% (weight) TiC/7075 matrix material.Extruding back matrix material σ
bBe not less than 650MPa.
Claims (1)
1, a kind of method of founding-preparing metal-base composite material through in-situ reaction and spray formation is characterized in that: technological process comprises preparation prefabricated section, master alloy melting and atomised jet shaping three phases:
A. prepare prefabricated section: the selective reaction thing, can select two classes: the first kind:
In the formula, M represents matrix element Al, and Cu and alloy thereof: X represents metallic element or non-metallic element Ti, Zr, V, Mo, C, B, Si; Y represents non-metallic element C, B, Si.When X was non-metallic element, XY was the combination of C and B or C and two kinds of non-metallic elements of Si; Second class:
In the formula, M represents matrix element Al and alloy thereof; N represents magnesium-yttrium-transition metal Cu, Zn, Cr; Said metallic element, non-metallic element and transition group metallic oxide are Powdered in above-mentioned first and second class, and size range is 10～250 μ m;
When two kinds of reactants were Ti and C combination, its ratio range (weight ratio) was 1: 0.1～0.7; If Ti and B combination, its ratio range (weight ratio) is 1: 0.1～0.8; If Al and CuO combination, its ratio range (weight ratio) is 1: 0.2～0.7;
During the preparation prefabricated section, can add a certain amount of catalyzer or stopping agent, said catalyzer is Al, Ni, Cu; Said stopping agent one class is Si, SiO
2, Al
2O
3, they do not participate in the chemical reaction between the reactant; Another kind of is villaumite and villiaumite, and they participate in the chemical reaction between the reactant.The weight ratio of catalyzer and two kinds of reactants is (0～0.8): 1; When having added the stopping agent of thinner effect, the weight ratio of stopping agent and two kinds of reactants is (0.05～0.5): 1; When adding the stopping agent that participates in chemical reaction between the reactant, the weight ratio of villaumite and villiaumite and two kinds of reactants is (0.03～0.20): 1; When two kinds of reactants were Ti and C combination, its range of choice (weight ratio) was 1: 0.3～0.5; If Ti and B combination, its range of choice (weight ratio) is 1: 0.3～0.6; If Al and CuO combination, its range of choice (weight ratio) is 1: 0.4～0.5;
During the preparation prefabricated section, can add the organic volatile binding agent in the raw material that mixes, the organic volatile binding agent is (0.02～0.15) with the raw material weight ratio that mixes: 1;
Above-mentioned various raw materials are put into mixer by certain stoichiometric ratio mix, with the raw material compression moulding at room temperature that mixes, pressure range is 50～500MPa again;
B. the melting of matrix material mother alloy: with an amount of matrix alloy Al, Cu and alloy thereof are put into medium-frequency induction furnace and are heated, and Heating temperature is above 150～300 ℃ of this alloy melting point; 1～20% the prefabricated section that will account for the weight alloy ratio again is pressed in the alloy melt with the graphite bell jar, insulation: 1～30 minute;
C. atomised jet is shaped every processing parameter of available existing reaction-injection moulding metallic substance blank with preparation metal-base composites blank.
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| CN1323179C (en) * | 2003-09-01 | 2007-06-27 | 昆明贵金属研究所 | High-strength, High-conductivity copper-base alloy material and preparing method thereof |
| CN100534673C (en) * | 2004-01-29 | 2009-09-02 | 北京科技大学 | Method for preparing Si-Al alloy using spray deposition forming process |
| CN1297682C (en) * | 2004-02-02 | 2007-01-31 | 北京科技大学 | Preparation method for reinforced aluminum base composite material composed by in situ alpha-Al2O3 crystal whisker and TiC grain |
| CN103882251B (en) * | 2014-02-25 | 2016-06-22 | 山东科技大学 | The apparatus and method of dispersed and strengthened copper-based composite material are prepared in molten drop deposition reaction |
| CN103831421A (en) * | 2014-03-26 | 2014-06-04 | 铜仁学院 | Method for preparing local enhancement aluminum matrix composite |
| CN107586984B (en) * | 2017-09-07 | 2019-11-26 | 哈尔滨理工大学 | Al-Ti-C alloy and preparation method thereof |
| CN112593111B (en) * | 2020-12-11 | 2022-01-28 | 迈特李新材料(深圳)有限公司 | Carbide nanoparticle modified aluminum-based nanocomposite and preparation method thereof |
| RU2753630C1 (en) * | 2021-03-04 | 2021-08-18 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Method for alloying aluminum with tantalum |
| CN113699398B (en) * | 2021-08-24 | 2022-04-22 | 湘潭大学 | Short-process preparation method of high-strength high-toughness corrosion-resistant deformation ZnCuTi plate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN2258500Y (en) * | 1995-11-23 | 1997-07-30 | 中南工业大学 | Jet sedimentation device for preparing metal base composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2258500Y (en) * | 1995-11-23 | 1997-07-30 | 中南工业大学 | Jet sedimentation device for preparing metal base composite material |
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