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CN109570497A - Raw multiple dimensioned pottery aluminium composite material of multiphase and preparation method thereof in one kind - Google Patents

Raw multiple dimensioned pottery aluminium composite material of multiphase and preparation method thereof in one kind Download PDF

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Publication number
CN109570497A
CN109570497A CN201811607765.6A CN201811607765A CN109570497A CN 109570497 A CN109570497 A CN 109570497A CN 201811607765 A CN201811607765 A CN 201811607765A CN 109570497 A CN109570497 A CN 109570497A
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powder
composite material
pottery
aluminium composite
ticn
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邱丰
董柏欣
杨宏宇
姜启川
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Qingdao Automotive Research Institute Jilin University
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Qingdao Automotive Research Institute Jilin University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • B22F2003/208—Warm or hot extruding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Products (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention discloses the raw multiple dimensioned pottery aluminium composite material of multiphase in one kind, the chemical composition and its mass percent of the interior raw multiple dimensioned pottery aluminium composite material of multiphase are as follows: Al:40~80wt.%；Cu:0~5wt.%；Mg:0~5wt.%；TiCN, AlN and TiB2: 20~50wt.%.The present invention also provides the preparation methods of the multiple dimensioned pottery aluminium composite material of multiphase raw in one kind, by Al powder, Ti powder, Cu powder, Mg powder and B4C and BN mixed-powder is sintered in-situ endogenic preparation and contains the multiple dimensioned TiCN-AlN-TiB of multiphase2The pottery aluminium composite material of particle, and optimize TiCN-AlN-TiB2The percentage composition of particle realizes TiCN-AlN-TiB in pottery aluminium composite material2The multiple dimensioned distribution of the multiphase of particle.

Description

Raw multiple dimensioned pottery aluminium composite material of multiphase and preparation method thereof in one kind
Technical field
The present invention relates to Ceramic Composite processing and preparation fields, and more particularly, the present invention relates to multiphase raw in one kind is more Scale pottery aluminium composite material and preparation method thereof.
Background technique
In recent years, ceramic particle reinforced metal base composites are with its excellent physics, chemical property, gradually instead of tradition Alloy is widely used as engineering material and functional material.Wherein, transition metal carbide, nitride, boride, it is with higher Specific strength, higher hardness and modulus, higher fusing point, chemical stability is good, thermal expansion coefficient is lower and good conductance The features such as rate, can be used as reinforced phase reinforced aluminium alloy, or as the heterogeneous forming core core of alloy, increase nucleation rate, and refinement is closed The solidified structure of gold.The crystal face that many experiments show different sizes, the ceramic particle of pattern is exposed in α-Al melt is not Together.Interface energy, interfacial structure and the mismatch of crystal face and α-Al melt exposed at ceramic particle and melt interface etc. Factor and the size of ceramic particle, pattern have important relation.Mismatch is low between ceramic particle and melt, and interface cohesion is steady Fixed, lower mismatch is conducive to improve the wetability of particle in the base, so particle is easy to realize coherence between matrix, That is the ceramic particle core that can be used as heterogeneous forming core promotes the heterogeneous forming core of α-Al.In addition, particle strengthens base as reinforced phase When body, size also has a significant impact to the comprehensive mechanical property of final composite material.The size of ceramic particle also will affect Its strengthening effect and thinning microstructure effect.Larger-size micrometer-sized particles, which can induce, generates stress concentration around particle, but It is the forming core that larger-size ceramics can be conducive to alloy, is conducive to thinning microstructure.The lesser ceramics of size, with matrix When interfacial wettability is preferable, be conducive to by dendrite capture enter it is transgranular, thus it is transgranular distribution play second-phase strength make With the small sized particles by dendrite capture can also be adsorbed at solid liquid interface, so that the diffusion of solute is prevented, to prevent The growth of dendrite, to realize the effect of control dendritic growth, and small sized particles often all glomeration, be conducive to reduce stress It concentrates.Therefore, the reinforcing that mixes of multiple dimensioned interior raw ceramic particle is conducive to improve the comprehensive mechanical property of composite material, and makees When use for hardening agent, it is also beneficial to the raising of the comprehensive performance of reinforced alloys.
Summary of the invention
It is an object of the invention to design and develop a kind of interior raw multiple dimensioned pottery aluminium composite material of multiphase, pass through original position Interior raw preparation contains the multiple dimensioned TiCN-AlN-TiB of multiphase2The pottery aluminium composite material of particle, and optimize TiCN-AlN-TiB2Particle Percentage composition, realize pottery aluminium composite material in TiCN-AlN-TiB2The multiple dimensioned distribution of the multiphase of particle.
Another object of the present invention is to have designed and developed a kind of preparation side of interior raw multiple dimensioned pottery aluminium composite material of multiphase Method, by Al powder, Ti powder, Cu powder, Mg powder and B4It is multiple dimensioned containing multiphase that C and BN mixed-powder is sintered in-situ endogenic preparation TiCN-AlN-TiB2The pottery aluminium composite material of particle, and optimize TiCN-AlN-TiB2The percentage composition of particle realizes that pottery aluminium is compound TiCN-AlN-TiB in material2The multiple dimensioned distribution of the multiphase of particle.
It is of the present invention the utility model has the advantages that
(1) the interior raw multiple dimensioned pottery aluminium composite material of multiphase provided by the invention contains multiphase by in-situ endogenic preparation Multiple dimensioned TiCN-AlN-TiB2The pottery aluminium composite material of particle, wherein ceramic particle is that nano/submicron/micron mixes scale, And optimize TiCN-AlN-TiB2The percentage composition of particle, multiphase ceramic particle are stabilized in aluminum substrate, and interface cohesion is good It is good, it is uniformly dispersed, realizes TiCN-AlN-TiB in pottery aluminium composite material2The multiple dimensioned distribution of the multiphase of particle.
(2) preparation method of the multiple dimensioned pottery aluminium composite material of interior raw multiphase provided by the invention, by Al powder, Ti powder, Cu powder, Mg powder and B4C and BN mixed-powder is sintered in-situ endogenic preparation and contains the multiple dimensioned TiCN-AlN-TiB of multiphase2The pottery aluminium of particle is multiple Condensation material, and optimize TiCN-AlN-TiB2The percentage composition of particle, multiphase ceramic particle are stabilized in aluminum substrate, interface It is well combined, is uniformly dispersed, realize TiCN-AlN-TiB in pottery aluminium composite material2The multiple dimensioned distribution of the multiphase of particle, and multiphase Interfacial reaction will not occur for multiple dimensioned particle stabilized presence, interior raw ceramic particle and alloy matrix aluminum, and particle size is nanometer, Asia Micron, micron mix, and will not reduce the plasticity of composite material, have important application value.Integrated operation is simple, save at This, has important economic benefit.
Detailed description of the invention
Fig. 1 is TiCN-AlN-TiB prepared by comparative example 12The X-ray diffraction analysis figure of/Al pottery aluminium composite material.
Fig. 2 is TiCN-AlN-TiB prepared by comparative example 12TiCN, TiB2 granule-morphology figure in/Al pottery aluminium composite material.
Fig. 3 is TiCN-AlN-TiB prepared by comparative example 12The size distribution plot of TiCN in/Al pottery aluminium composite material.
Fig. 4 is TiCN-AlN-TiB prepared by comparative example 12The size distribution plot of TiB2 in/Al pottery aluminium composite material.
Fig. 5 is TiCN-AlN-TiB prepared by embodiment 12The X-ray diffraction analysis figure of/Al pottery aluminium composite material.
Fig. 6 is TiCN-AlN-TiB prepared by embodiment 12TiCN, TiB2 granule-morphology figure in/Al pottery aluminium composite material.
Fig. 7 is TiCN-AlN-TiB prepared by embodiment 12The size distribution plot of TiCN in/Al pottery aluminium composite material.
Fig. 8 is TiCN-AlN-TiB prepared by embodiment 12The size distribution plot of TiB2 in/Al pottery aluminium composite material.
Fig. 9 is TiCN-AlN-TiB prepared by embodiment 22The X-ray diffraction analysis figure of/Al pottery aluminium composite material.
Figure 10 is TiCN-AlN-TiB prepared by embodiment 22TiCN, TiB2 granule-morphology figure in/Al pottery aluminium composite material.
Figure 11 is TiCN-AlN-TiB prepared by embodiment 22The size distribution plot of TiCN in/Al pottery aluminium composite material.
Figure 12 is TiCN-AlN-TiB prepared by embodiment 22The size distribution plot of TiB2 in/Al pottery aluminium composite material.
Figure 13 is TiCN-AlN-TiB prepared by embodiment 32The X-ray diffraction analysis figure of/Al pottery aluminium composite material.
Figure 14 is TiCN-AlN-TiB prepared by embodiment 32TiCN, TiB2 granule-morphology figure in/Al pottery aluminium composite material.
Figure 15 is TiCN-AlN-TiB prepared by embodiment 32The size distribution plot of TiCN in/Al pottery aluminium composite material.
Figure 16 is TiCN-AlN-TiB prepared by embodiment 32The size distribution plot of TiB2 in/Al pottery aluminium composite material.
Figure 17 is TiCN-AlN-TiB prepared by embodiment 42The X-ray diffraction analysis figure of/Al pottery aluminium composite material.
Figure 18 is TiCN-AlN-TiB prepared by embodiment 42TiCN, TiB2 granule-morphology figure in/Al pottery aluminium composite material.
Figure 19 is TiCN-AlN-TiB prepared by embodiment 42The size distribution plot of TiCN in/Al pottery aluminium composite material.
Figure 20 is TiCN-AlN-TiB prepared by embodiment 42The size distribution plot of TiB2 in/Al pottery aluminium composite material.
Figure 21 is TiCN-AlN-TiB prepared by embodiment 52The X-ray diffraction analysis figure of/Al pottery aluminium composite material.
Figure 22 is TiCN-AlN-TiB prepared by embodiment 52TiCN, TiB2 granule-morphology figure in/Al pottery aluminium composite material.
Figure 23 is TiCN-AlN-TiB prepared by embodiment 52The size distribution plot of TiCN in/Al pottery aluminium composite material.
Figure 24 is TiCN-AlN-TiB prepared by embodiment 52The size distribution plot of TiB2 in/Al pottery aluminium composite material.
Figure 25 is TiCN-AlN-TiB prepared by embodiment 62The X-ray diffraction analysis figure of/Al pottery aluminium composite material.
Figure 26 is TiCN-AlN-TiB prepared by embodiment 62TiCN, TiB2 granule-morphology figure in/Al pottery aluminium composite material.
Figure 27 is TiCN-AlN-TiB prepared by embodiment 62The size distribution plot of TiCN in/Al pottery aluminium composite material.
Figure 28 is TiCN-AlN-TiB prepared by embodiment 62The size distribution plot of TiB2 in/Al pottery aluminium composite material.
Figure 29 is TiCN-AlN-TiB prepared by comparative example 22The X-ray diffraction analysis figure of/Al pottery aluminium composite material.
Figure 30 is TiCN-AlN-TiB prepared by comparative example 22TiCN, TiB2 granule-morphology figure in/Al pottery aluminium composite material.
Figure 31 is TiCN-AlN-TiB prepared by comparative example 22The size distribution plot of TiCN in/Al pottery aluminium composite material.
Figure 32 is TiCN-AlN-TiB prepared by comparative example 22The size distribution plot of TiB2 in/Al pottery aluminium composite material.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art referring to specification text Word can be implemented accordingly.
The present invention provides the raw multiple dimensioned pottery aluminium composite material of multiphase, the interior raw multiple dimensioned pottery aluminium composite wood of multiphase in one kind The chemical composition and its mass percent of material are as follows: Al:40~80wt.%；Cu:0~5wt.%；Mg:0~5wt.%；TiCN, AlN and TiB2: 20~50wt.%.
The interior raw multiple dimensioned pottery aluminium composite material of multiphase provided by the invention contains the more rulers of multiphase by in-situ endogenic preparation Spend TiCN-AlN-TiB2The pottery aluminium composite material of particle, wherein ceramic particle mixes scale for nano/submicron/micron, and excellent Change TiCN-AlN-TiB2The percentage composition of particle, multiphase ceramic particle are stabilized in aluminum substrate, and interface cohesion is good, point It dissipates uniformly, realizes TiCN-AlN-TiB in pottery aluminium composite material2The multiple dimensioned distribution of the multiphase of particle.
The present invention also provides the preparation methods of the multiple dimensioned pottery aluminium composite material of multiphase raw in one kind, comprising:
Step 1: a certain amount of BN powder (granularity of BN powder is 0.5~1.3 μm) is taken, with the speed of 200~300r/min High speed ball milling is activated 1.5~3h；
Step 2: taking a certain amount of B4C powder (B4The granularity of C powder is 0.5~6.5 μm) BN after ball milling is activated is added (the B in powder4The molar ratio of C and BN is 1:1), 1.5 are activated with the speed high speed ball milling of 200~300r/min~ 3h obtains B4C and BN mixed-powder；
Step 3: weighing that Al powder (granularity of aluminium powder is 13~48 μm), (granularity of titanium valve is 13~45 μ to Ti powder in proportion M), Cu powder (granularity of copper powder is 45 μm), Mg powder (granularity of magnesium powder is 45 μm) and B4C and BN mixed-powder, using ZrO2Mill 8~48h of ball mixing and ball milling；
Wherein, the mass percentage of each component meets: Al:50~80wt.%, Ti:13.16~32.88wt.%, B4C:4.72~11.81wt.%, BN:2.12~5.31wt.%, Cu:0~5wt.%, Mg:0~5wt.%；Described Ti, B4C and The molar ratio of BN is 9:2.8:2.8；
Wherein, the ZrO2Abrading-ball and Al powder, Ti powder, Cu powder, Mg powder and B4C, the mass ratio of BN mixed-powder is 8:1；
Step 4: by Al powder, Ti powder, Cu powder, Mg powder and B4C and BN mixed-powder is wrapped up with aluminium foil, and encapsulation process is set In mold, 0.5~3min of pressure maintaining obtains the cold pressing cylinder pressure that consistency is 60~75% under the pressure of 60~100MPa Base.
Step 5: by Al powder, Ti powder, Cu powder, Mg powder and B4Cylindrical green compact is made in C and BN mixed-powder, wraps graphite Paper is placed in progress vacuum-sintering in graphite jig, and (graphite jig is the intermediate cylinder for having through-hole, and intracavity diameter is 32mm), 573K is warming up to the rate of heat addition of 25~60K/min, and carries out 10~20min of vacuum degassing；It is continuously heating to When 773K, 15~25min is kept the temperature；
Step 6: 1173K~1200K being continuously heating to the rate of heat addition of 30~60K/min, when the gas that pressure gauge is shown After being pressed with significant changes, stop heating after keeping the temperature 10~30min；
Step 7: when temperature is down to 1053K, applying the pressure of axial 45~75MPa, pressure maintaining to the cylindrical green compact 30~90s is cooled to room temperature in a vacuum, obtains multiple dimensioned TiCN, AlN and TiB in situ2The pottery aluminium composite material of particle；
Wherein, TiCN, AlN and TiB in the pottery aluminium composite material2The mass fraction of particle is 20~50wt.%.
Step 8: the pottery aluminium composite material being subjected to homogenization heat treatment, heat treatment temperature is 673~773K, heat treatment Time is 18~60h；
Step 9: extrusion lubricant, the extruding lubrication will be uniformly smeared on the outside of the pottery aluminium composite material after the heat treatment Agent is molybdenum disulfide and high temperature lubricating oil mixture, and being placed in hot die steel, (hot die steel is H13 hot-work die Steel, intracavity diameter 30mm) in carry out hot extrusion, be heated to 773K~833K, keep the temperature 30~60min；
Step 10: after heat preservation, axial compressive force being applied to the pottery aluminium composite material and carries out extrusion forming, extrusion ratio is 16:1~38:1.
Comparative example 1
The preparation method of this comparative example the following steps are included:
(1) powder ball milling activating pretreatment, specific as follows:
Step 1.1: pressing B4The molar ratio of C and BN is that 1:1 weighs a certain amount of B respectively4C and BN powder is spare, wherein B4C The granularity of powder is 0.5 μm, purity >=92.0wt.%；The granularity of BN powder is 0.5 μm, purity >=99.0wt.%.
Step 1.2: BN powder being put into ball grinder, with planetary ball mill by BN powder with the speed high speed of 300r/min Ball milling is activated 2.5h.
Step 1.3: B4C powder is added, and into the BN powder of ball milling activating pretreatment with the ball-milling treatment 2h of 200r/min, Obtain the mixed-powder of B4C and BN.The ratio of grinding media to material that high speed ball milling is activated twice is 8:1, using zirconium dioxide abrading-ball, is mixed The volume for closing powder is no more than the 1/2 of ball milling tank volume；
(2) preparation reaction green compact, specific as follows:
Step 2.1: weighing the B after Al powder, Ti powder, ball milling are activated by a certain percentage4C powder and BN powder are spare, wherein The granularity of aluminium powder is 13 μm, purity >=99.9wt.%；The granularity of titanium valve is 13 μm, purity >=99.9wt.%；
Step 2.2: the mixing B after aluminium powder, titanium valve, ball milling are activated4C and BN powder is configured to 100g according to the following ratio Mixed-powder obtains Al-Ti-B4C-BN green compact；Wherein Ti:B4The molar ratio of C:BN is 9:2.8:2.8；Each component reactant powder Weight is as follows: Al powder: 85g, Ti powder: 10.32g, B4C powder: 3.54g, BN powder: 1.59g.
Step 2.3: the powder of the above prepared different component being put into ball grinder, fills diameter in advance in this outer tank For the ZrO2 ball of 5mm~22mm, totally 6 kinds, 10 every kind, diameter is respectively 5mm, 7mm, 11mm, 15mm, 20mm, 22mm, ZrO2 The total 800g of ball quality；Ball grinder is installed in planetary batch mixer, and the revolving speed of batch mixer is set as 50r/min, mixed uniformly Time is 30h；Wherein the mass ratio of zirconium oxide balls and mixed-powder is 8:1, and the overall volume of powder and zirconium oxide balls is not More than the 3/4 of tank body volume；
Step 2.4: superscribing the powder stated and mixed in step with aluminium foil, and do encapsulation process appropriate, be subsequently placed into With in the stainless steel mould of the inner cavity Φ 30mm, die top is equipped with stainless steel column for centre, and hydraulic press applies with list at room temperature Pressure in the axial direction, then pressure maintaining 1min obtains cold pressing cylindrical green compact at 85MPa, and green compact diameter is Φ 30, high 36mm, densification Degree is 70%；
(3) Al-Ti-B4C-BN system green compact in-situ sintering reacts, specific as follows:
Step 3.1: obtained cylindrical green compact being wrapped with graphite paper, is integrally put into the intermediate cylindrical stone for having through-hole In black mold (the cylindrical graphite mold inner-cavity diameter is Φ 32mm).A high-strength graphite compression bar is placed at the top of green compact, The position of fixed green compact in a mold.Finally will integrally it be put into the graphite jig and graphite compression bar that are fixed with cylindrical green compact In vacuum sintering funace；Fire door is closed, is subsequently vacuumed out to furnace pressure lower than 100Pa.
Step 3.2: beginning to warm up, heating speed is set as 45K/min；When temperature is increased to 573K, vacuum degassing is carried out 10min；
Step 3.3: when temperature is increased to 783K, keeping the temperature 20min, keep graphite jig temperature and cylindrical green compact temperature Unanimously.
Step 3.4: when temperature continuation is increased to 1185K with 45K/min, observing the pressure gauge in vacuum sintering funace After having significant change, 15min is kept the temperature, heating is then stopped.
Step 3.5: when temperature is down to 1053K, axial direction 70MPa pressure, subsequent pressure maintaining 50s being applied to cylindrical green compact； The cylinder densified after reaction and through axial compressive force contains the interior multiple dimensioned TiCN-AlN-TiB of raw multiphase2The pottery aluminium of ceramic particle Composite material is cooled to room temperature in a vacuum with furnace.
(4) the hot extrusion dispersion of TiCN-AlN-TiB2 particle and pottery aluminium compound plastic forming:
Step 4.1: obtained pottery aluminium composite material being subjected to homogenization heat treatment, heat treatment temperature is set as 700K, heat The processing time is 45h.
Arrangement 4.2: the cylindrical pottery compound outside of aluminium after extrusion lubricant to be equably applied to Homogenization Treatments.Its In, the group of extrusion lubricant becomes molybdenum disulfide and high temperature lubricating oil mixture；To then make pottery, aluminium is compound to be put into hot die steel In mold (for H13 hot die steel, the size of hot-work die steel mold is Φ 30mm)；
Step 4.3: cylinder is made pottery, and aluminium is compound and hot-work die steel mold is put into thermal-squeezing device, is heated to 803K keeps the temperature 20min；
Step 4.4: after heat preservation, to the cylinder pottery compound application axial compressive force of aluminium, carrying out extrusion forming；Extrusion ratio is 24:1。
By in Al-Ti-B4TiCN-AlN-TiB is prepared in the reaction of C-BN system in-situ endogenic2The mass fraction of particle is Raw multiphase micron/nano mixes scale pottery aluminium composite material in 15wt.%, and Fig. 1 is pottery aluminium composite material prepared by comparative example 1 X-ray diffraction analysis, as shown in Figure 1, the pottery aluminium composite material is by α-Al phase, Al3Ti、TiB2, AlN and TiCN ceramic phase Composition.Fig. 2-4 is TiCN, TiB in the pottery aluminium composite material of comparative example 12Granule-morphology and size distribution plot.Pass through particle size Statistical chart, TiCN ceramic particle average-size are 49.29nm, TiB2Particle mean size is 100.2nm.It is said by the comparative example Bright Al content of working as is 85wt.%, and generates TiCN-AlN-TiB2The mass fraction of particle is the interior raw multiphase micron of 15wt.% Particle mean size in nano hybrid scale pottery aluminium composite material is nanoscale, and there is no realize the mixed of particle scale It is miscellaneous.
Embodiment 1:
This example preparation method the following steps are included:
(1) powder ball milling activating pretreatment, specific as follows:
Step 1.1: pressing B4The molar ratio of C and BN is that 1:1 weighs a certain amount of B respectively4C and BN powder is spare, wherein B4C The granularity of powder is 0.5 μm, purity >=92.0wt.%；The granularity of BN powder is 0.5 μm, purity >=99.0wt.%.
Step 1.2: BN powder being put into ball grinder, with planetary ball mill by BN powder with the speed high speed of 200r/min Ball milling is activated 2h.
Step 1.2: B is added into the BN powder of ball milling activating pretreatment4C powder, and with the ball-milling treatment 2h of 300r/min, Obtain B4The mixed-powder of C and BN.The ratio of grinding media to material that high speed ball milling is activated twice is 8:1, using zirconium dioxide abrading-ball, is mixed The volume for closing powder is no more than the 1/2 of ball milling tank volume；
(2) preparation reaction green compact, specific as follows:
Step 2.1: weighing the B after Al powder, Ti powder, ball milling are activated by a certain percentage4C powder and BN powder are spare, wherein The granularity of aluminium powder is 13 μm, purity >=99.9wt.%；The granularity of titanium valve is 13 μm, purity >=99.9wt.%；
Step 2.2: mixing B4C and the BN powder after aluminium powder, titanium valve, ball milling activation processing is configured to 100g according to the following ratio Mixed-powder obtains Al-Ti-B4C-BN green compact；Wherein Ti:B4The molar ratio of C:BN is 9:2.8:2.8；Each component reactant powder Weight is as follows, Al powder: 80g, Ti powder: 13.16g, B4C powder: 4.72g, BN powder: 2.12g.
Step 2.3: the powder of the above prepared different component being put into ball grinder, fills diameter in advance in this outer tank For the ZrO of 5mm~22mm2Ball, totally 6 kinds, 10 every kind, diameter is respectively 5mm, 7mm, 11mm, 15mm, 20mm, 22mm, ZrO2 The total 800g of ball quality；Ball grinder is installed in planetary batch mixer, and the revolving speed of batch mixer is set as 60r/min, mixed uniformly Time is for 24 hours；Wherein the mass ratio of zirconium oxide balls and mixed-powder is 8:1, and the overall volume of powder and zirconium oxide balls is not More than the 3/4 of tank body volume；
Step 2.4 superscribes the powder stated and mixed in step with aluminium foil, and do encapsulation process appropriate, is subsequently placed into Between with the inner cavity Φ 30mm stainless steel mould in, die top is equipped with stainless steel column, at room temperature hydraulic press apply with unidirectional Axial compressive force, then pressure maintaining 3min obtains cold pressing cylindrical green compact at 60MPa, and green compact diameter is Φ 30, high 40mm, consistency It is 65%；
(3) Al-Ti-B4C-BN system green compact in-situ sintering reacts, specific as follows:
Step 3.1: obtained cylindrical green compact being wrapped with graphite paper, is integrally put into the intermediate cylindrical stone for having through-hole In black mold (the cylindrical graphite mold inner-cavity diameter is Φ 32mm).A high-strength graphite compression bar is placed at the top of green compact, The position of fixed green compact in a mold.Finally will integrally it be put into the graphite jig and graphite compression bar that are fixed with cylindrical green compact In vacuum sintering funace；Fire door is closed, is subsequently vacuumed out to furnace pressure lower than 100Pa.
Step 3.2: beginning to warm up, heating speed is set as 40K/min；When temperature is increased to 573K, vacuum degassing is carried out 10min；
Step 3.3: when temperature is increased to 773K, keeping the temperature 20min, keep graphite jig temperature and cylindrical green compact temperature Unanimously.
Step 3.4: when temperature continuation is increased to 1173K with 40K/min, observing the pressure gauge in vacuum sintering funace After having significant change, 10min is kept the temperature, heating is then stopped.
Step 3.5: when temperature is down to 1053K, axial direction 55MPa pressure, subsequent pressure maintaining 40s being applied to cylindrical green compact； The pottery aluminium that the cylinder densified after reaction and through axial compressive force contains the multiple dimensioned TiCN-AlN-TiB2 ceramic particle of interior raw multiphase Composite material is cooled to room temperature in a vacuum with furnace.
(4) TiCN-AlN-TiB2The hot extrusion of particle disperses and pottery aluminium compound plastic forming:
Step 4.1: carrying out homogenization heat treatment for obtained pottery aluminium is compound, heat treatment temperature is set as 673K, heat treatment Time is 60h.
Step 4.2: the cylindrical pottery compound outside of aluminium after extrusion lubricant to be equably applied to Homogenization Treatments.Its In, the group of extrusion lubricant becomes molybdenum disulfide and high temperature lubricating oil mixture；To then make pottery, aluminium is compound to be put into hot die steel In mold (for H13 hot die steel, the size of hot-work die steel mold is Φ 30mm)；
Step 4.3: cylinder is made pottery, and aluminium is compound and hot-work die steel mold is put into thermal-squeezing device, is heated to 823K keeps the temperature 35min；
Step 4.4: after heat preservation, to the cylinder pottery compound application axial compressive force of aluminium, carrying out extrusion forming；Extrusion ratio is 32:1。
By in Al-Ti-B4TiCN-AlN-TiB is prepared in the reaction of C-BN system in-situ endogenic2The mass fraction of particle is The interior raw multiphase micron/nano of 20wt.% mixes scale pottery aluminium composite material, and Fig. 5 is pottery aluminium composite wood prepared by embodiment 1 The X-ray diffraction analysis of material, as shown in Figure 5, the pottery aluminium composite material is by α-Al phase, Al3Ti、TiB2, TiCN ceramic phase group At.Fig. 6-8 is Al-Ti-B4Reaction generates TiCN-AlN-TiB in C-BN system2The mass fraction of particle is the pottery aluminium of 20wt.% TiCN, TiB in composite material2Granule-morphology and size distribution plot.By particle size statistical chart, TiCN ceramic particle is averaged ruler Very little is 62.49nm, TiB2Particle mean size is 176.44nm.
Embodiment 2:
The preparation method of this example the following steps are included:
(1) powder ball milling activating pretreatment, specific as follows:
Step 1.1: pressing B4The molar ratio of C and BN is that 1:1 weighs a certain amount of B respectively4C and BN powder is spare, wherein B4C The granularity of powder is 3.5 μm, purity >=92.0wt.%；The granularity of BN powder is 0.5 μm, purity >=99.0wt.%.
Step 1.2: BN powder being put into ball grinder, with planetary ball mill by BN powder with the speed high speed of 300r/min Ball milling is activated 1.5h.
Step 1.3: B is added into the BN powder of ball milling activating pretreatment4C powder, and with the ball-milling treatment 3h of 200r/min, Obtain B4The mixed-powder of C and BN.The ratio of grinding media to material that high speed ball milling is activated twice is 8:1, using zirconium dioxide abrading-ball, is mixed The volume for closing powder is no more than the 1/2 of ball milling tank volume；
(2) preparation reaction green compact, specific as follows:
Step 2.1: weighing the B after Al powder, Ti powder, ball milling are activated by a certain percentage4C powder and BN powder are spare, wherein The granularity of aluminium powder is 23 μm, purity >=99.9wt.%；The granularity of titanium valve is 18 μm, purity >=99.9wt.%；
Step 2.2: the mixing B after aluminium powder, titanium valve, ball milling are activated4C and BN powder several is configured to as following 100g mixed-powder obtains Al-Ti-B4C-BN green compact；Wherein Ti:B4The molar ratio of C:BN is 9:2.8:2.8；Each component reaction Powder quality is as follows, Al powder: 70g, Ti powder: 19.73g, B4C powder: 7.09g, BN powder: 3.18g.
Step 2.3: the powder of the above prepared different component being put into ball grinder, fills diameter in advance in this outer tank For the ZrO of 5mm~22mm2Ball, totally 6 kinds, 10 every kind, diameter is respectively 5mm, 7mm, 11mm, 15mm, 20mm, 22mm, ZrO2 The total 800g of ball quality；Ball grinder is installed in planetary batch mixer, and the revolving speed of batch mixer is set as 30r/min, mixed uniformly Time is 36h；Wherein the mass ratio of zirconium oxide balls and mixed-powder is 8:1, and the overall volume of powder and zirconium oxide balls is not More than the 3/4 of tank body volume；
Step 2.4: superscribing the powder stated and mixed in step with aluminium foil, and do encapsulation process appropriate, be subsequently placed into With in the stainless steel mould of the inner cavity Φ 30mm, die top is equipped with stainless steel column for centre, and hydraulic press applies with list at room temperature Pressure in the axial direction, then pressure maintaining 1.5min obtains cold pressing cylindrical green compact at 80MPa, and green compact diameter is Φ 30, high 35mm, causes Density is 75%；
(3) Al-Ti-B4The reaction of C-BN system green compact in-situ sintering, specific as follows:
Step 3.1: obtained cylindrical green compact being wrapped with graphite paper, is integrally put into the intermediate cylindrical stone for having through-hole In black mold (the cylindrical graphite mold inner-cavity diameter is Φ 32mm).A high-strength graphite compression bar is placed at the top of green compact, The position of fixed green compact in a mold.Finally will integrally it be put into the graphite jig and graphite compression bar that are fixed with cylindrical green compact In vacuum sintering funace；Fire door is closed, is subsequently vacuumed out to furnace pressure lower than 100Pa.
Step 3.2: beginning to warm up, heating speed is set as 25K/min；When temperature is increased to 573K, vacuum degassing is carried out 20min；
Step 3.3: when temperature is increased to 773K, keeping the temperature 15min, keep graphite jig temperature and cylindrical green compact temperature Unanimously.
Step 3.4: when temperature continuation is increased to 1180K with 30K/min, observing the pressure gauge in vacuum sintering funace After having significant change, 15min is kept the temperature, heating is then stopped.
Step 3.5: when temperature is down to 1053K, axial direction 60MPa pressure, subsequent pressure maintaining 50s being applied to cylindrical green compact； The cylinder densified after reaction and through axial compressive force contains the interior multiple dimensioned TiCN-AlN-TiB of raw multiphase2The pottery aluminium of ceramic particle Composite material is cooled to room temperature in a vacuum with furnace.
(4) the hot extrusion dispersion of TiCN-AlN-TiB2 particle and pottery aluminium compound plastic forming:
Step 4.1: obtained pottery aluminium composite material being subjected to homogenization heat treatment, heat treatment temperature is set as 723K, heat The processing time is 36h.
Step 4.2: the cylindrical pottery compound outside of aluminium after extrusion lubricant to be equably applied to Homogenization Treatments.Its In, the group of extrusion lubricant becomes molybdenum disulfide and high temperature lubricating oil mixture；To then make pottery, aluminium is compound to be put into hot die steel In mold (for H13 hot die steel, the size of hot-work die steel mold is Φ 30mm)；
Step 4.3: cylinder is made pottery, and aluminium is compound and hot-work die steel mold is put into thermal-squeezing device, is heated to 773KK keeps the temperature 60min；
Step 4.4: after heat preservation, to the cylinder pottery compound application axial compressive force of aluminium, carrying out extrusion forming；Extrusion ratio is 16:1；
By in Al-Ti-B4TiCN-AlN-TiB is prepared in the reaction of C-BN system in-situ endogenic2The mass fraction of particle is The interior raw multiphase micron/nano of 30wt.% mixes scale pottery aluminium composite material, and Fig. 9 is pottery aluminium composite wood prepared by embodiment 2 The X-ray diffraction analysis of material, as shown in Figure 9, the pottery aluminium composite material is by α-Al phase, Al3Ti、TiB2, AlN and TiCN are ceramic Phase composition.Figure 10-12 is Al-Ti-B4Reaction generates TiCN-AlN-TiB in C-BN system2The mass fraction of particle is 30wt.% Pottery aluminium composite material in TiCN, TiB2Granule-morphology and size distribution plot.Pass through particle size statistical chart, TiCN ceramic particle Average-size is 77.52nm, TiB2Particle mean size is 248.9nm.
Embodiment 3
The preparation method of this example the following steps are included:
(1) powder ball milling activating pretreatment, specific as follows:
Step 1.1: pressing B4The molar ratio of C and BN is that 1:1 weighs a certain amount of B respectively4C and BN powder is spare, wherein B4C The granularity of powder is 6.5 μm, purity >=92.0wt.%；The granularity of BN powder is 1.3 μm, purity >=99.0wt.%.
Step 1.2: BN powder being put into ball grinder, with planetary ball mill by BN powder with the speed high speed of 300r/min Ball milling is activated 2.5h.
Step 1.3: B is added into the BN powder of ball milling activating pretreatment4C powder, and with the ball-milling treatment 2h of 200r/min, Obtain B4The mixed-powder of C and BN.The ratio of grinding media to material that high speed ball milling is activated twice is 8:1, using zirconium dioxide abrading-ball, is mixed The volume for closing powder is no more than the 1/2 of ball milling tank volume；
(2) preparation reaction green compact, specific as follows:
Step 2.1: weighing the B after Al powder, Ti powder, ball milling are activated by a certain percentage4C powder and BN powder are spare, wherein The granularity of aluminium powder is 38 μm, purity >=99.9wt.%；The granularity of titanium valve is 25 μm, purity >=99.9wt.%；
Step 2.2: the mixing B after aluminium powder, titanium valve, ball milling are activated4C and BN powder is configured to 100g according to the following ratio Mixed-powder obtains Al-Ti-B4C-BN；Wherein Ti:B4The molar ratio of C:BN is 9:2.8:2.8；Each component reacts powder matter Measure as follows, Al powder: 60g, Ti powder: 26.31g, B4C powder: 9.45g, BN powder: 4.24g.
Step 2.3: the powder of the above prepared different component being put into ball grinder, fills diameter in advance in this outer tank For the ZrO of 5mm~22mm2Ball, totally 6 kinds, 10 every kind, diameter is respectively 5mm, 7mm, 11mm, 15mm, 20mm, 22mm, ZrO2 The total 800g of ball quality；Ball grinder is installed in planetary batch mixer, and the revolving speed of batch mixer is set as 20r/min, mixed uniformly Time is 48h；Wherein the mass ratio of zirconium oxide balls and mixed-powder is 8:1, and the overall volume of powder and zirconium oxide balls is not More than the 3/4 of tank body volume；
Step 2.4: superscribing the powder stated and mixed in step with aluminium foil, and do encapsulation process appropriate, be subsequently placed into With in the stainless steel mould of the inner cavity Φ 30mm, die top is equipped with stainless steel column for centre, and hydraulic press applies with list at room temperature Pressure in the axial direction, then at 100MPa pressure maintaining 0.5min obtain cold pressing cylindrical green compact, green compact diameter be Φ 30, high 35mm, Consistency is 75%；
(3) Al-Ti-B4The reaction of C-BN system green compact in-situ sintering, specific as follows:
Step 3.1: obtained cylindrical green compact being wrapped with graphite paper, is integrally put into the intermediate cylindrical stone for having through-hole In black mold (the cylindrical graphite mold inner-cavity diameter is Φ 32mm).A high-strength graphite compression bar is placed at the top of green compact, The position of fixed green compact in a mold.Finally will integrally it be put into the graphite jig and graphite compression bar that are fixed with cylindrical green compact In vacuum sintering funace；Fire door is closed, is subsequently vacuumed out to furnace pressure lower than 100Pa.
Step 3.2: beginning to warm up, heating speed is set as 25~60K/min；When temperature is increased to 573K, vacuum is carried out Degasification 10-20min；
Step 3.3: when temperature is increased to 773K, keeping the temperature 15~25min, make graphite jig temperature and cylindrical green compact temperature It is consistent.
Step 3.4: when temperature continuation is increased to 1173K~1200K with 30~60K/min, observing vacuum heating-press sintering After pressure gauge in furnace has significant change, 10-30min is kept the temperature, heating is then stopped.
Step 3.5: when temperature is down to 1053K, axial 45~75MPa pressure, subsequent pressure maintaining being applied to cylindrical green compact 50s；The cylinder densified after reaction and through axial compressive force contains the interior multiple dimensioned TiCN-AlN-TiB of raw multiphase2Ceramic particle Pottery aluminium composite material is cooled to room temperature in a vacuum with furnace.
(4) the hot extrusion dispersion of TiCN-AlN-TiB2 particle and pottery aluminium compound plastic forming:
Step 4.1: by pottery aluminium composite material carry out homogenization heat treatment, heat treatment temperature be set as 673K~ 773K, heat treatment time are 18~60h.
Step 4.2: the cylindrical pottery compound outside of aluminium after extrusion lubricant to be equably applied to Homogenization Treatments.Its In, the group of extrusion lubricant becomes molybdenum disulfide and high temperature lubricating oil mixture；To then make pottery, aluminium is compound to be put into hot die steel In mold (for H13 hot die steel, the size of hot-work die steel mold is Φ 30mm)；
Step 4.3: cylinder is made pottery, and aluminium is compound and hot-work die steel mold is put into thermal-squeezing device, is heated to 773K ~833K keeps the temperature 30~60min；
Step 4.4: after heat preservation, to the cylinder pottery compound application axial compressive force of aluminium, carrying out extrusion forming；Extrusion ratio is 16:1~38:1；
By in Al-Ti-B4TiCN-AlN-TiB is prepared in the reaction of C-BN system in-situ endogenic2The mass fraction of particle is The interior raw multiphase micron/nano of 40wt.% mixes scale pottery aluminium composite material, and Figure 13 is pottery aluminium composite wood prepared by embodiment 3 The X-ray diffraction analysis of material, as shown in Figure 13, the pottery aluminium composite material is by α-Al phase, Al3Ti、TiB2, AlN and TiCN are ceramic Phase composition.Figure 14-16 is Al-Ti-B4Reaction generates TiCN-AlN-TiB in C-BN system2The mass fraction of particle is 30wt.% Pottery aluminium composite material in TiCN, TiB2Granule-morphology and size distribution plot.Pass through particle size statistical chart, TiCN ceramic particle Average-size is 230nm, TiB2Particle mean size is 630nm.
Embodiment 4:
The preparation method of this example the following steps are included:
(1) powder ball milling activating pretreatment, specific as follows:
Step 1.1: pressing B4The molar ratio of C and BN is that 1:1 weighs a certain amount of B respectively4C and BN powder is spare, wherein B4C The granularity of powder is 6.5 μm, purity >=92.0wt.%；The granularity of BN powder is 1.3 μm, purity >=99.0wt.%.
Step 1.2: BN powder being put into ball grinder, with planetary ball mill by BN powder with the speed high speed of 300r/min Ball milling is activated 1.5h.
Step 1.3: B is added into the BN powder of ball milling activating pretreatment4C powder, and with the ball-milling treatment 2h of 250r/min, Obtain B4The mixed-powder of C and BN.The ratio of grinding media to material that high speed ball milling is activated twice is 8:1, using zirconium dioxide abrading-ball, is mixed The volume for closing powder is no more than the 1/2 of ball milling tank volume；
(2) preparation reaction green compact, specific as follows:
Step 2.1: weighing the B after Al powder, Ti powder, ball milling are activated by a certain percentage4C powder and BN powder are spare, wherein The granularity of aluminium powder is 45 μm, purity >=99.9wt.%；The granularity of titanium valve is 45 μm, purity >=99.9wt.%；
Step 2.2: the mixing B after aluminium powder, titanium valve, ball milling are activated4C and BN powder is configured to 100g according to the following ratio Mixed-powder obtains Al-Ti-B4C-BN；Wherein Ti:B4The molar ratio of C:BN is 9:2.8:2.8；Each component reacts powder matter Measure as follows, Al powder: 50g, Ti powder: 32.88g, B4C powder: 11.81g, BN powder: 5.31g.
Step 2.3: the powder of the above prepared different component being put into ball grinder, fills diameter in advance in this outer tank For the ZrO of 5mm~22mm2Ball, totally 6 kinds, 10 every kind, diameter is respectively 5mm, 7mm, 11mm, 15mm, 20mm, 22mm, ZrO2 The total 800g of ball quality；Ball grinder is installed in planetary batch mixer, and the revolving speed of batch mixer is set as 80r/min, mixed uniformly Time is 8h；Wherein the mass ratio of zirconium oxide balls and mixed-powder is 8:1, and the overall volume of powder and zirconium oxide balls does not surpass Cross the 3/4 of tank body volume；
Step 2.4: superscribing the powder stated and mixed in step with aluminium foil, and do encapsulation process appropriate, be subsequently placed into With in the stainless steel mould of the inner cavity Φ 30mm, die top is equipped with stainless steel column for centre, and hydraulic press applies with list at room temperature Pressure in the axial direction, then at 100MPa pressure maintaining 0.5min obtain cold pressing cylindrical green compact, green compact diameter be Φ 30, high 45mm, Consistency is 60%；
(3) Al-Ti-B4The reaction of C-BN system green compact in-situ sintering, specific as follows:
Step 3.1: obtained cylindrical green compact being wrapped with graphite paper, is integrally put into the intermediate cylindrical stone for having through-hole In black mold.A high-strength graphite compression bar, the position of fixed green compact in a mold are placed at the top of green compact.It will finally have and be fixed with The graphite jig and graphite compression bar of cylindrical green compact are integrally put into vacuum sintering funace；Close fire door, be subsequently vacuumed out to Furnace pressure is lower than 100Pa.
Step 3.2: beginning to warm up, heating speed is set as 60K/min；When temperature is increased to 573K, vacuum degassing is carried out 10min；
Step 3.3: when temperature is increased to 773K, keeping the temperature 25min, keep graphite jig temperature and cylindrical green compact temperature Unanimously.
Step 3.4: when temperature continuation is increased to 1173K with 60K/min, observing the pressure gauge in vacuum sintering funace After having significant change, 10min is kept the temperature, heating is then stopped.
Step 3.5: when temperature is down to 1053K, axial direction 75MPa pressure, subsequent pressure maintaining 30s being applied to cylindrical green compact； The cylinder densified after reaction and through axial compressive force contains the interior multiple dimensioned TiCN-AlN-TiB of raw multiphase2The pottery aluminium of ceramic particle Composite material is cooled to room temperature in a vacuum with furnace.
(4) the hot extrusion dispersion of TiCN-AlN-TiB2 particle and pottery aluminium compound plastic forming:
Step 4.1: carrying out homogenization heat treatment for obtained pottery aluminium is compound, heat treatment temperature is set as 773K, heat treatment Time is 18h.
Step 4.2: the cylindrical pottery compound outside of aluminium after extrusion lubricant to be equably applied to Homogenization Treatments.Its In, the group of extrusion lubricant becomes molybdenum disulfide and high temperature lubricating oil mixture；To then make pottery, aluminium is compound to be put into hot die steel In mold；
Step 4.3: cylinder is made pottery, and aluminium is compound and hot-work die steel mold is put into thermal-squeezing device, is heated to 803K keeps the temperature 45min；
Step 4.4: after heat preservation, to the cylinder pottery compound application axial compressive force of aluminium, carrying out extrusion forming；Extrusion ratio is 38:1；
By in Al-Ti-B4TiCN-AlN-TiB is prepared in the reaction of C-BN system in-situ endogenic2The mass fraction of particle is The interior raw multiphase micron/nano of 50wt.% mixes scale pottery aluminium composite material, and Figure 17 is pottery aluminium composite wood prepared by embodiment 4 The X-ray diffraction analysis of material, as shown in Figure 17, the pottery aluminium composite material is by α-Al phase, Al3Ti、TiB2, AlN and TiCN are ceramic Phase composition.Figure 18-20 is Al-Ti-B4Reaction generates TiCN-AlN-TiB in C-BN system2The mass fraction of particle is 30wt.% Pottery aluminium composite material in TiCN, TiB2Granule-morphology and size distribution plot.Pass through particle size statistical chart, TiCN ceramic particle Average-size is 682.9nm, TiB2Particle mean size is 1130nm.
Embodiment 5:
The preparation method of this example the following steps are included:
(1) powder ball milling activating pretreatment, specific as follows:
Step 1.1: pressing B4The molar ratio of C and BN is that 1:1 weighs a certain amount of B respectively4C and BN powder is spare, wherein B4C The granularity of powder is 2.6 μm, purity >=92.0wt.%；The granularity of BN powder is 0.5 μm, purity >=99.0wt.%.
Step 1.2: BN powder being put into ball grinder, with planetary ball mill by BN powder with the speed high speed of 300r/min Ball milling is activated 2.5h.
Step 1.3: B is added into the BN powder of ball milling activating pretreatment4C powder, and with the ball-milling treatment of 300r/min 1.5h obtains B4The mixed-powder of C and BN.The ratio of grinding media to material that high speed ball milling is activated twice is 8:1, is ground using zirconium dioxide Ball, the volume of mixed powder are no more than the 1/2 of ball milling tank volume；
(2) preparation reaction green compact, specific as follows:
Step 2.1: weighing the B after Al powder, Ti powder, ball milling are activated by a certain percentage4C powder and BN powder are spare, wherein The granularity of aluminium powder is 48 μm, purity >=99.9wt.%；The granularity of titanium valve is 45 μm, purity >=99.9wt.%；The granularity of copper powder It is 45 μm, purity >=99.5wt.%；
Step 2.2: the mixing B after aluminium powder, titanium valve, ball milling are activated4C and BN powder and Cu powder several are matched as following Than being configured to 100g mixed-powder, Al-Ti-B is obtained4C-BN-Cu green compact；Wherein Ti:B4The molar ratio of C:BN is 9:2.8:2.8； Each component reactant powder quality is as follows, Al powder: 65g, Ti powder: 19.73g, B4C powder: 7.09g, BN powder: 3.18g, Cu powder: 5g.
Step 2.3: the powder of the above prepared different component being put into ball grinder, fills diameter in advance in this outer tank For the ZrO of 5mm~22mm2Ball, totally 6 kinds, 10 every kind, diameter is respectively 5mm, 7mm, 11mm, 15mm, 20mm, 22mm, ZrO2 The total 800g of ball quality；Ball grinder is installed in planetary batch mixer, and the revolving speed of batch mixer is set as 50r/min, mixed uniformly Time is 22h；Wherein the mass ratio of zirconium oxide balls and mixed-powder is 8:1, and the overall volume of powder and zirconium oxide balls is not More than the 3/4 of tank body volume；
Step 2.4: superscribing the powder stated and mixed in step with aluminium foil, and do encapsulation process appropriate, be subsequently placed into With in the stainless steel mould of the inner cavity Φ 30mm, die top is equipped with stainless steel column for centre, and hydraulic press applies with list at room temperature Pressure in the axial direction, then pressure maintaining 2min obtains cold pressing cylindrical green compact at 70MPa, and green compact diameter is Φ 30, high 40mm, densification Degree is 70%；
(3) Al-Ti-B4The reaction of C-BN-Cu system green compact in-situ sintering, specific as follows:
Step 3.1: obtained cylindrical green compact being wrapped with graphite paper, is integrally put into the intermediate cylindrical stone for having through-hole In black mold.A high-strength graphite compression bar, the position of fixed green compact in a mold are placed at the top of green compact.It will finally have and be fixed with The graphite jig and graphite compression bar of cylindrical green compact are integrally put into vacuum sintering funace；Close fire door, be subsequently vacuumed out to Furnace pressure is lower than 100Pa.
Step 3.2: beginning to warm up, heating speed is set as 30K/min；When temperature is increased to 573K, vacuum degassing is carried out 20min；
Step 3.3: when temperature is increased to 773K, keeping the temperature 15min, keep graphite jig temperature and cylindrical green compact temperature Unanimously.
Step 3.4: when temperature continuation is increased to 1183K with 30K/min, observing the pressure gauge in vacuum sintering funace After having significant change, 10min is kept the temperature, heating is then stopped.
Step 3.5: when temperature is down to 1053K, axial direction 45MPa pressure, subsequent pressure maintaining 90s being applied to cylindrical green compact； The cylinder densified after reaction and through axial compressive force contains the interior multiple dimensioned TiCN-AlN-TiB of raw multiphase2The pottery aluminium of ceramic particle Composite material is cooled to room temperature in a vacuum with furnace.
(4) TiCN-AlN-TiB2The hot extrusion of particle disperses and pottery aluminium compound plastic forming:
Step 4.1: obtained pottery aluminium composite material being subjected to homogenization heat treatment, heat treatment temperature is set as 773K, heat The processing time is 18h.
Step 4.2: the cylindrical pottery compound outside of aluminium after extrusion lubricant to be equably applied to Homogenization Treatments.Its In, the group of extrusion lubricant becomes molybdenum disulfide and high temperature lubricating oil mixture；To then make pottery, aluminium is compound to be put into hot die steel In mold；
Step 4.3: cylinder is made pottery, and aluminium is compound and hot-work die steel mold is put into thermal-squeezing device, is heated to 773K ~833K keeps the temperature 30~60min；
Step 4.4: after heat preservation, to the cylinder pottery compound application axial compressive force of aluminium, carrying out extrusion forming；Extrusion ratio is 30:1。
By in Al-Ti-B4TiCN-AlN-TiB is prepared in the reaction of C-BN-Cu system in-situ endogenic2The mass fraction of particle Mix the pottery aluminium composite material of scale for the interior raw multiphase micron/nano of 30wt.%, Figure 21 is that pottery aluminium prepared by embodiment 5 is multiple The X-ray diffraction analysis of condensation material, by Figure 21 it is found that the pottery aluminium composite material is by α-Al phase, Al3Ti、Al2Cu、TiB2, AlN With TiCN ceramics phase composition.Figure 22-24 is Al-Ti-B4Reaction generates TiCN-AlN-TiB in C-BN system2The quality of particle point Number is TiCN, TiB in the pottery aluminium composite material of 30wt.%2Granule-morphology and size distribution plot.By particle size statistical chart, TiCN ceramic particle average-size is 103.67nm, TiB2Particle mean size is 334.26nm.
Embodiment 6
The preparation method of this example the following steps are included:
(1) powder ball milling activating pretreatment, specific as follows:
(1a) is that 1:1 weighs a certain amount of B respectively by the molar ratio of B4C and BN4C and BN powder is spare, wherein B4C powder Granularity is 1.3 μm, purity >=92.0wt.%；The granularity of BN powder is 1.3 μm, purity >=99.0wt.%.
BN powder is put into ball grinder by (1b), with planetary ball mill by BN powder with the speed high speed ball milling of 250r/min It is activated 2h.
(1c) B4C powder is added into the BN powder of ball milling activating pretreatment, and with the ball-milling treatment 2h of 250r/min, obtains The mixed-powder of B4C and BN.The ratio of grinding media to material that high speed ball milling is activated twice is 8:1, using zirconium dioxide abrading-ball, mixed powder The volume of body is no more than the 1/2 of ball milling tank volume；
(2) preparation reaction green compact, specific as follows:
(2a) weighs the B4C powder after Al powder, Ti powder, ball milling are activated by a certain percentage and BN powder is spare, wherein aluminium powder Granularity be 38 μm, purity >=99.9wt.%；The granularity of titanium valve is 25 μm, purity >=99.9wt.%；The granularity of magnesium powder is 45 μ M, purity >=99.5wt.%.
(2b) aluminium powder, titanium valve, ball milling are activated after mixing B4C and BN powder and Mg powder several match by following 100g mixed-powder is made, obtains Al-Ti-B4C-BN-Mg green compact；Wherein the molar ratio of Ti:B4C:BN is 9:2.8:2.8；Respectively Component reactant powder quality is as follows, Al powder: 65g, Ti powder: 19.73g, B4C powder: 7.09g, BN powder: 3.18g, Mg powder: 5g.
The powder of the above prepared different component is put into ball grinder by (2c), and filling diameter in this outer tank in advance is The ZrO2 ball of 5mm~22mm, totally 6 kinds, 10 every kind, diameter is respectively 5mm, 7mm, 11mm, 15mm, 20mm, 22mm, ZrO2 ball The total 800g of quality；Ball grinder is installed in planetary batch mixer, and the revolving speed of batch mixer is set as 40r/min, when mixed uniformly Between be 18h；Wherein the mass ratio of zirconium oxide balls and mixed-powder is 8:1, and the overall volume of powder and zirconium oxide balls does not surpass Cross the 3/4 of tank body volume；
(2d) superscribes the powder stated and mixed in step with aluminium foil, and does encapsulation process appropriate, is subsequently placed into centre In stainless steel mould with the inner cavity Φ 30mm, die top is equipped with stainless steel column, and hydraulic press applies with one-way shaft at room temperature To pressure, then pressure maintaining 3min obtains cold pressing cylindrical green compact at 60MPa, and green compact diameter is Φ 30, high 45mm, and consistency is 60%；
(3) Al-Ti-B4C-BN-Mg system green compact in-situ sintering reacts, specific as follows:
(3a) wraps cylindrical green compact obtained in step (2) with graphite paper, is integrally put into the intermediate circle for having through-hole In cylindricality graphite jig.A high-strength graphite compression bar, the position of fixed green compact in a mold are placed at the top of green compact.It will finally have The graphite jig and graphite compression bar for being fixed with cylindrical green compact are integrally put into vacuum sintering funace；Fire door is closed, is then taken out Vacuum to furnace pressure is lower than 100Pa.
(3b) is begun to warm up, and heating speed is set as 50K/min；When temperature is increased to 573K, vacuum degassing is carried out 15min；
When (3c) temperature is increased to 773K, 15min is kept the temperature, graphite jig temperature and cylindrical green compact temperature is made to keep one It causes.
When the continuation of (3d) temperature is increased to 1183K with 40K/min, observe the pressure in vacuum sintering funace in respect of aobvious After writing variation, 10min is kept the temperature, heating is then stopped.
(3e) applies axial direction 55MPa pressure, subsequent pressure maintaining 65s when temperature is down to 1053K, to cylindrical green compact；Reaction The pottery that the cylinder densified afterwards and through axial compressive force contains multiple dimensioned (the TiCN-AlN-TiB2)/Al ceramic particle of interior raw multiphase Aluminium is compound to be cooled to room temperature in a vacuum with furnace.
(4) the hot extrusion dispersion of TiCN-AlN-TiB2 particle and pottery aluminium compound plastic forming:
(4a) carries out homogenization heat treatment for the resulting pottery aluminium of step (3) is compound, and heat treatment temperature is set as 693KK, heat The processing time is 48h.
Extrusion lubricant is equably applied to the cylindrical pottery compound outside of aluminium after Homogenization Treatments by (4b).Wherein, it squeezes The group of pressure lubricating agent becomes molybdenum disulfide and high temperature lubricating oil mixture；To then make pottery, aluminium is compound to be put into hot-work die steel mold In；
(4c) is compound by cylinder pottery aluminium and hot-work die steel mold is put into thermal-squeezing device, is heated to 813K, protects Warm 45min；
After (4d) is kept the temperature, to the cylinder pottery compound application axial compressive force of aluminium, extrusion forming is carried out；Extrusion ratio is 38: 1；
Wherein, in step (2b), in Al-Ti-B4C-BN-Mg system in the preparation of mixed-powder, mole of Ti:B4C:BN Than being 9:2.8:2.8；
Wherein, in step (3), the cylindrical graphite mold inner-cavity diameter is Φ 32mm；；
Wherein, the material of hot-work die steel mold used in step (4) are as follows: H13 hot die steel, hot-work die punching block The size of tool is Φ 30mm；
The interior raw multiphase for being 30wt.% by the content prepared in the reaction of Al-Ti-B4C-BN-Mg system in-situ endogenic The TiCN-AlN-TiB2/Al pottery aluminium that micron/nano mixes scale ceramic particle is compound, and Figure 25 is that pottery aluminium prepared by example 6 is multiple The X-ray diffraction analysis of conjunction, by Figure 25 it is found that the TiCN-AlN-TiB2/Al pottery aluminium it is compound by α-Al phase, Al3Ti, Al12Mg17, TiB2, AlN and TiCN ceramics phase composition.Figure 26-28 is that reaction generates mass fraction in Al-Ti-B4C-BN system For 30wt.%TiCN-AlN-TiB2/ Al pottery aluminium compound TiCN, TiB2 granule-morphology and size distribution plot.Pass through particle size Statistical chart, TiCN ceramic particle average-size are 50.48nm, and TiB2 particle mean size is 170.9nm.
Comparative example 2
Raw multiple dimensioned (the TiCN-AlN-TiB2)/Al pottery aluminium of multiphase is compound in one kind and preparation method, which is characterized in that packet Include following steps:
(1) powder ball milling activating pretreatment, specific as follows:
(1a) be that 1:1 weighs that a certain amount of B4C and BN powder is spare respectively by the molar ratio of B4C and BN, wherein B4C powder Granularity is 6.5 μm, purity >=92.0wt.%；The granularity of BN powder is 1.3 μm, purity >=99.0wt.%.
BN powder is put into ball grinder by (1b), with planetary ball mill by BN powder with the speed high speed ball milling of 300r/min It is activated 3h.
(1c) B4C powder is added into the BN powder of ball milling activating pretreatment, and with the ball-milling treatment 1.5h of 250r/min, obtains To the mixed-powder of B4C and BN.The ratio of grinding media to material that high speed ball milling is activated twice is 8:1, using zirconium dioxide abrading-ball, mixing The volume of powder is no more than the 1/2 of ball milling tank volume；
(2) preparation reaction green compact, specific as follows:
(2a) weighs the B4C powder after Al powder, Ti powder, ball milling are activated by a certain percentage and BN powder is spare, wherein aluminium powder Granularity be 48 μm, purity >=99.9wt.%；The granularity of titanium valve is 38 μm, purity >=99.9wt.%；
Mixing B4C and BN powder after aluminium powder, titanium valve, ball milling are activated by (2b) several is configured to 100g by following Mixed-powder obtains Al-Ti-B4C-BN green compact；Wherein the molar ratio of Ti:B4C:BN is 9:2.8:2.8；Each component reactant powder Weight is as follows: Al:35g, Ti:42.75g, B4C:15.35g, BN:6.90g；Described Ti, B4The molar ratio of C and BN is 9:2.8: 2.8；
The powder of the above prepared different component is put into ball grinder by (2c), and filling diameter in this outer tank in advance is The ZrO2 ball of 5mm~22mm, totally 6 kinds, 10 every kind, diameter is respectively 5mm, 7mm, 11mm, 15mm, 20mm, 22mm, ZrO2 ball The total 800g of quality；Ball grinder is installed in planetary batch mixer, and the revolving speed of batch mixer is set as 75r/min, when mixed uniformly Between be 10h；Wherein the mass ratio of zirconium oxide balls and mixed-powder is 8:1, and the overall volume of powder and zirconium oxide balls does not surpass Cross the 3/4 of tank body volume；
(2d) superscribes the powder stated and mixed in step with aluminium foil, and does encapsulation process appropriate, is subsequently placed into centre In stainless steel mould with the inner cavity Φ 30mm, die top is equipped with stainless steel column, and hydraulic press applies with one-way shaft at room temperature To pressure, then pressure maintaining 2min obtains cold pressing cylindrical green compact at 80MPa, and green compact diameter is Φ 30, high 38mm, and consistency is 71.5%；
(3) Al-Ti-B4C-BN system green compact in-situ sintering reacts, specific as follows:
(3a) wraps cylindrical green compact obtained in step (2) with graphite paper, is integrally put into the intermediate circle for having through-hole In cylindricality graphite jig.A high-strength graphite compression bar, the position of fixed green compact in a mold are placed at the top of green compact.It will finally have The graphite jig and graphite compression bar for being fixed with cylindrical green compact are integrally put into vacuum sintering funace；Fire door is closed, is then taken out Vacuum to furnace pressure is lower than 100Pa.
(3b) is begun to warm up, and heating speed is set as 40K/min；When temperature is increased to 573K, vacuum degassing is carried out 15min；
When (3c) temperature is increased to 773K, 10min is kept the temperature, graphite jig temperature and cylindrical green compact temperature is made to keep one It causes.
When the continuation of (3d) temperature is increased to 1205K with 40K/min, observe the pressure in vacuum sintering funace in respect of aobvious After writing variation, 15min is kept the temperature, heating is then stopped.
(3e) applies axial direction 50MPa pressure, subsequent pressure maintaining 40s when temperature is down to 1053K, to cylindrical green compact；Reaction The pottery that the cylinder densified afterwards and through axial compressive force contains multiple dimensioned (the TiCN-AlN-TiB2)/Al ceramic particle of interior raw multiphase Aluminium is compound to be cooled to room temperature in a vacuum with furnace.
(4) the hot extrusion dispersion of TiCN-AlN-TiB2 particle and pottery aluminium compound plastic forming:
(4a) carries out homogenization heat treatment for the resulting pottery aluminium of step (3) is compound, and heat treatment temperature is set as 713K, at heat The reason time is 40h.
Extrusion lubricant is equably applied to the cylindrical pottery compound outside of aluminium after Homogenization Treatments by (4b).Wherein, it squeezes The group of pressure lubricating agent becomes molybdenum disulfide and high temperature lubricating oil mixture；To then make pottery, aluminium is compound to be put into hot-work die steel mold In；
(4c) is compound by cylinder pottery aluminium and hot-work die steel mold is put into thermal-squeezing device, is heated to 823K, protects Warm 45min；
After (4d) is kept the temperature, to the cylinder pottery compound application axial compressive force of aluminium, extrusion forming is carried out；Extrusion ratio is 18: 1；
Wherein, in step (2b), in Al-Ti-B4C-BN system in the preparation of mixed-powder, the molar ratio of Ti:B4C:BN It is 9:2.8:2.8；
Wherein, in step (3), the cylindrical graphite mold inner-cavity diameter is Φ 32mm；；
Wherein, the material of hot-work die steel mold used in step (4) are as follows: H13 hot die steel, hot-work die punching block The size of tool is Φ 30mm；
The interior raw multiphase for being 65wt.% by the content prepared in the reaction of Al-Ti-B4C-BN-Mg system in-situ endogenic The TiCN-AlN-TiB2/Al pottery aluminium that micron/nano mixes scale ceramic particle is compound, and Figure 29 is that pottery aluminium prepared by example 6 is multiple The X-ray diffraction analysis of conjunction, by Figure 29 it is found that the TiCN-AlN-TiB2/Al pottery aluminium it is compound by α-Al phase, Al3Ti, Al12Mg17, TiB2, AlN and TiCN ceramics phase composition.Figure 30-32 is that reaction generates mass fraction in Al-Ti-B4C-BN system For 65wt.%TiCN-AlN-TiB2/Al pottery aluminium compound TiCN, TiB2 granule-morphology and size distribution plot.Pass through particle size Statistical chart, TiCN ceramic particle average-size are 0.75 μm, and TiB2 particle mean size is 1.38 μm.It can be with by comparative example 2 Find out, when the ceramic particle content of generation is 65wt.%, multiphase ceramic particle almost all is micrometer-sized particles, only few It measures nanometer size particles to exist, therefore is unsatisfactory for the requirement that preparation mixes size granule.
The preparation method of the interior raw multiple dimensioned pottery aluminium composite material of multiphase provided by the invention, by Al powder, Ti powder, Cu powder, Mg Powder and B4C and BN mixed-powder is sintered in-situ endogenic preparation and contains the multiple dimensioned TiCN-AlN-TiB of multiphase2The pottery aluminium of particle is compound Material, and optimize TiCN-AlN-TiB2The percentage composition of particle, multiphase ceramic particle are stabilized in aluminum substrate, interface knot It closes well, is uniformly dispersed, realize TiCN-AlN-TiB in pottery aluminium composite material2The multiple dimensioned distribution of the multiphase of particle, and multiphase is more Size granule is stabilized, and interfacial reaction will not occur for interior raw ceramic particle and alloy matrix aluminum, and particle size is nanometer, sub-micro Rice, micron mix, and will not reduce the plasticity of composite material, have important application value.Integrated operation is simple, save the cost, With important economic benefit.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited In specific details and legend shown and described herein.

Claims (9)

1. the raw multiple dimensioned pottery aluminium composite material of multiphase in one kind, which is characterized in that the interior raw multiple dimensioned pottery aluminium composite wood of multiphase The chemical composition and its mass percent of material are as follows: Al:40~80wt.%；Cu:0~5wt.%；Mg:0~5wt.%；TiCN, AlN and TiB2: 20~50wt.%.
2. the preparation method of the raw multiple dimensioned pottery aluminium composite material of multiphase in one kind characterized by comprising
Step 1: by Al powder, Ti powder, Cu powder, Mg powder and B4Cylindrical green compact is made in C and BN mixed-powder, wraps graphite paper and sets Carry out vacuum-sintering in graphite jig, 573K be warming up to the rate of heat addition of 25~60K/min, and carry out vacuum degassing 10~ 20min；When being continuously heating to 773K, 15~25min is kept the temperature；
Wherein, the chemical composition and its mass percent of the cylindrical green compact are as follows: Al:50~80wt.%, Ti:13.16~ 32.88wt.%, B4C:4.72~11.81wt.%, BN:2.12~5.31wt.%, Cu:0~5wt.%, Mg:0~5wt.%； Described Ti, B4The molar ratio of C and BN is 9:2.8:2.8；
Step 2: 1173K~1200K being continuously heating to the rate of heat addition of 30~60K/min, stops adding after keeping the temperature 10~30min Heat；
Step 3: when temperature is down to 1053K, the pressure of 45~75MPa axial to cylindrical green compact application, pressure maintaining 30~ 90s is cooled to room temperature in a vacuum, obtains multiple dimensioned TiCN, AlN and TiB in situ2The pottery aluminium composite material of particle；
Wherein, TiCN, AlN and TiB in the pottery aluminium composite material2The mass fraction of particle is 20~50wt.%.
3. the preparation method of the raw multiple dimensioned pottery aluminium composite material of multiphase in as claimed in claim 2, which is characterized in that also wrap It includes:
Step 4: the pottery aluminium composite material being subjected to homogenization heat treatment, heat treatment temperature is 673~773K, heat treatment time For 18~60h；
Step 5: will uniformly smear extrusion lubricant on the outside of the pottery aluminium composite material after the heat treatment, be placed in hot die steel Middle carry out hot extrusion is heated to 773K~833K, keeps the temperature 30~60min；
Step 6: after heat preservation, axial compressive force being applied to the pottery aluminium composite material and carries out extrusion forming, extrusion ratio 16:1 ~38:1.
4. the preparation method of the raw multiple dimensioned pottery aluminium composite material of multiphase in as claimed in claim 2 or claim 3, which is characterized in that institute It states Al powder, Ti powder, Cu powder, Mg powder and B4Cylindrical green compact is made in C and BN mixed-powder
Step 1: weighing Al powder, Ti powder, Cu powder, Mg powder and B in proportion4C and BN mixed-powder, using ZrO2Abrading-ball mixing ball Grind 8~48h；
Wherein, the ZrO2Abrading-ball and Al powder, Ti powder, Cu powder, Mg powder and B4C, the mass ratio of BN mixed-powder is 8:1；
Step 2: by Al powder, Ti powder, Cu powder, Mg powder and B4C and BN mixed-powder is wrapped up with aluminium foil, and encapsulation process is placed in mould In tool, 0.5~3min of pressure maintaining obtains the cold pressing cylindrical green compact that consistency is 60~75% under the pressure of 60~100MPa.
5. the preparation method of the raw multiple dimensioned pottery aluminium composite material of multiphase in as claimed in claim 4, which is characterized in that the B4C Preparation with BN mixed-powder includes:
Step 1: taking a certain amount of BN powder, 1.5~3h is activated with the speed high speed ball milling of 200~300r/min；
Step 2: taking a certain amount of B4C powder is added in the BN powder after ball milling is activated, with the speed of 200~300r/min High speed ball milling is activated 1.5~3h, obtains B4C and BN mixed-powder；
Wherein, the B4The molar ratio of C and BN is 1:1.
6. the preparation method of the raw multiple dimensioned pottery aluminium composite material of multiphase in as claimed in claim 5, which is characterized in that the B4C The granularity of powder is 0.5~6.5 μm, and the granularity of BN powder is 0.5~1.3 μm, and the granularity of aluminium powder is 13~48 μm, and the granularity of titanium valve is 13~45 μm, the granularity of copper powder is that the granularity of 45 μm of magnesium powders is 45 μm.
7. the preparation method of the raw multiple dimensioned pottery aluminium composite material of multiphase in as claimed in claim 3, which is characterized in that described to squeeze Pressure lubricating agent is molybdenum disulfide and high temperature lubricating oil mixture.
8. such as the preparation method of the interior raw multiple dimensioned pottery aluminium composite material of multiphase described in claim 5 or 6, which is characterized in that institute Stating graphite jig is the intermediate cylinder for having through-hole, intracavity diameter 32mm.
9. the preparation method of the interior raw multiple dimensioned pottery aluminium composite material of multiphase as described in claim 3 or 7, which is characterized in that institute Stating hot die steel is H13 hot die steel, intracavity diameter 30mm.
CN201811607765.6A 2018-12-27 2018-12-27 Raw multiple dimensioned pottery aluminium composite material of multiphase and preparation method thereof in one kind Pending CN109570497A (en)

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