CN102828060B - Titanium nitride ceramic reinforced copper-based composite material and preparation method thereof - Google Patents
Titanium nitride ceramic reinforced copper-based composite material and preparation method thereof Download PDFInfo
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- CN102828060B CN102828060B CN201210274498.1A CN201210274498A CN102828060B CN 102828060 B CN102828060 B CN 102828060B CN 201210274498 A CN201210274498 A CN 201210274498A CN 102828060 B CN102828060 B CN 102828060B
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Abstract
The invention discloses a titanium nitride ceramic reinforced copper-based composite material and a preparation method thereof. Raw materials for the composite material comprise, by weight, titanium nitride, titanium oxide, a sintering aid and carbon black, wherein copper alloy is added into a perform. The preparation method comprises the following steps: carrying out heating, insulation, sintering and introduction of flowing nitrogen so as to obtain a porous titanium nitride perform with a porosity of 45 to 75%; preheating a die casting machine and heating the copper alloy until the copper alloy is molten; and dumping molten copper alloy liquid into a mold cavity in which the perform is disposed, pressing the molten copper alloy liquid into the porous titanium nitride perform by using a press, separating an ingot from a die after the ingot is cooled and carrying out heat treatment on the ingot so as to obtain the titanium nitride ceramic reinforced copper-based composite material. Particles in the titanium nitride ceramic reinforced copper-based composite material are mutually connected, and the composite material has the advantages of low density, high specific strength and specific stiffness, good wear resistance, excellent thermal conductivity and electroconductivity and a stable size and is extensively used in the industries like frictional wear structural members of mechanical and electrical special equipment, high temperature and corrosion resistant structural members of bearing special equipment, the aerospace industry and automobile manufacturing.
Description
Technical field
The present invention relates to a kind of Ceramic Reinforced MMCs and preparation method thereof, particularly a kind of titanium nitride ceramic strengthens Cu-base composites and preparation method thereof.
Background technology
Particles reiforced metal-base composition is by additional ceramic particle reinforced phase or the spontaneous matrix material that obtains having concurrently metal advantage (toughness and plasticity) and enhanced granule advantage (high rigidity and high-modulus) in metallic matrix that enters.This kind of material has higher specific tenacity, specific rigidity and mechanical behavior under high temperature, low thermal expansivity, good wear resistance and heat conductivility, in addition also have reinforcement cost low, microtexture is even, material isotropy, can adopt the conventional metals such as hot pressing, hot rolling complete processing the advantage such as to process, thereby receive much attention compared with fiber reinforcement, whisker reinforced metal matrix composites.Particles reiforced metal-base composition has application prospect quite widely at industrial circles such as space flight, aviation, automobile, electronics, optics.The volume of the hard wild phase of the disperse in matrix material exceedes 20%, can embody the excellent properties of hard wild phase, and manufacture method mainly contains stirring casting method, squeeze casting method, powder metallurgic method etc.
(1), stirring casting method
Stirring casting method is that metal melt is carried out to violent stirring, drops into enhanced granule, it is uniformly distributed in metal melt, then direct pouring moulding.This method technique is simple, and facility investment is few, is convenient to large-scale production.But have enhanced granule volume fraction restricted (being generally no more than 20%), the distribution of enhanced granule is difficult to realize homogenizing, has the defects such as pore, can only make ingot casting, needs secondary processing.Referring to Zhou Yao and etc., " solidification technology ", China Machine Press, 1998:389～399.
(2), powder metallurgic method
Powder metallurgy technology claims again solid metal diffusion technique, and this method is that solid metal powder and enhanced granule mechanical uniform are mixed, and under certain temperature and pressure condition, suppresses sinter molding.Powder metallurgy technology has advantages of that some are unique, as lower in manufactured temperature, has alleviated the surface reaction between matrix and enhanced granule, has reduced the generation of hard compounds on interface; The volume fraction of enhanced granule is higher; Enhanced granule is evenly distributed, and is not prone to segregation and segregation.But powder metallurgy technology also exists some drawbacks, as the size and shape of product is subject to certain limitation; Processing sequence is many, and preparation cycle is long, and cost is high, and the possibility reducing costs is little, and especially expensive preparation cost has restricted the defects such as the application and development of powder metallurgy technology.Referring to Chinese patent CN1487109 " powder metallurgy self-generating ceramic particle reinforced aluminium base composite material and preparation method thereof ".
(3), squeeze casting method
This legal system is a kind of very ripe method for metal-base composites.First squeeze casting method is that reinforcement is made to prefabricated section, puts into mould, then pours into matrix alloy liquation, and pressurization subsequently makes matrix liquation infiltrate prefabricated section and becomes ingot.Extrusion casting has following advantage: with short production cycle, be easy to produce in enormous quantities; Can prepare the same or analogous product of shape of shape and end article; The time of liquid metal infiltration is short, and speed of cooling is fast, can reduce and even eliminate granular boundary reaction; The volume fraction variable range of wild phase is large.But extrusion casting is difficult for the complex-shaped product of preparation, in the time that infiltration pressure is very large, the integrity of mould and institute's product is had a great impact.Referring to Peng L M. Mechanical properties of ceramic – metal composites by pressure infiltration of metal into porous ceramics, Materials Science and Engineering A, 2004,374:1-9.
At present aspect the preparation of particles reiforced metal-base composition, also there are some problems: the volume fraction of (1) particulates reinforcements has very important impact to the mechanical property of matrix material.But the volume fraction of existing technology controlling and process wild phase is more difficult.(2) in most of matrix material, wild phase is discontinuous.Current research shows, in the time that the wild phase in matrix material and matrix are interpenetrating(polymer)networks distributed architecture, can show more excellent mechanical property.(3) ceramic performs and molten metal bath wettability are poor.There is no impressed pressure, molten metal bath is difficult to infiltrate completely in ceramic performs.
Summary of the invention
The present invention seeks to improve the existing defect of existing metal-base composites preparation method, provide one to there is high strength, high rigidity, production technique is simple, preparation cost is low, in conjunction with the advantage of carbothermic method and casting die, a kind of titanium nitride ceramic of excellent product performance strengthens Cu-base composites.
Another object of the present invention is to provide the preparation method of titanium nitride ceramic enhancing Cu-base composites.
In order to overcome the deficiencies in the prior art, technical scheme of the present invention is to solve like this: the special character that a kind of titanium nitride ceramic strengthens Cu-base composites is the front raw materials by weight portion ratio of titanium nitride ceramic precast body sintering, formed by 5 parts～95 parts titanium nitrides, 0.1 part～69 parts titanium oxide, 5 component sintering additives, 0.1 part～21 parts carbon blacks, 59 parts～79 parts copper alloys that wherein add precast body gross weight in titanium nitride ceramic precast body, described sintering aid is yttrium oxide.
Described copper alloy is the cast copper alloy of various models.
Described titanium nitride ceramic strengthens a preparation method for Cu-base composites, carries out in the steps below:
(1), by ratio of weight and the number of copies, take titanium nitride, titanium oxide, sintering aid, carbon black;
(2), by the above-mentioned each material mixing taking, be prepared into mixed powder with wet ball grinding, sieve after mixed powder is dry; Above-mentioned material is packed in mold cavity, and compression molding is precast body;
(3), under 6 normal atmosphere nitrogen atmospheres, be warmed up to gradually at 1650 ℃ and be incubated 2 hours with the heat-up rate of 4 ℃/min, obtain sintered porous titanium nitride precast body, in sintering process, pass into all the time flowing nitrogen 3L/min;
(4), the part that directly contacts with liquid metal of pressure die-casting machine coats releasing agent, with conveniently stripped;
(5), porous titanium nitride precast body and pressure die-casting machine are preheated to 500 ℃～700 ℃, copper alloy are heated to temperature and reach 1100 ℃ of molten states;
(6), after pressure die-casting machine internal temperature and molten copper aluminium alloy all reach predetermined temperature, molten copper aluminium alloy is poured in the cavity of placing porous titanium nitride precast body;
(7), then rely on pressing machine that molten copper aluminium alloy is pressed in porous titanium nitride precast body, in the time that pressure reaches 20～40MPa pressure, stop pressurization, and keep pressure 10 minutes, finally after ingot bar is cooling, separate with mould;
(8), unnecessary copper alloy will be removed after ingot bar again melting.
(9), carry out obtaining matrix material after T6 thermal treatment process to removing the titanium nitride precast body of unnecessary copper alloy, described T6 thermal treatment process: in half an hour, furnace temperature is risen to 500 ℃ from room temperature after product is put into retort furnace, and be incubated 6 hours, then sample is taken out to shrend, then within 6 hours, eliminate internal stress 180 ℃ of insulations.
Compared with prior art, porous titanium nitride stupalith prepared by use carbothermic method is as the prefabricated component of wild phase in the present invention, and the titanium nitride ceramic that utilizes compression casting technology to prepare mechanical property excellence strengthens Cu-base composites.With respect to existing particles reiforced metal-base composition, have the following advantages:
(1) the porous titanium nitride precast body relative density that prepared by carbothermic method is 45-75%, can adjust by controlling the relative density of porous titanium nitride precast body the volume fraction of titanium nitride wild phase.
(2) in the application of Ceramic Reinforced MMCs, ceramic network skeleton carries most weight, matrix material prepared by present method is IPN pore network tissue, the crystal grain of the porous titanium nitride of preparing due to carbothermic method is in addition tiny, even air hole distribution, so titanium nitride wild phase and copper alloy matrix are evenly distributed.The microtexture of the matrix material that therefore, prepared by present method is better than particle enhanced copper alloy composite materials prepared by other technique.
(3) because of the non-constant of wettability of molten copper aluminium alloy and titanium nitride ceramic, squeeze casting method makes molten copper aluminium alloy make a forcible entry into porous titanium nitride precast body inner air vent by mechanical pressure, and pressure remains to always and solidifies end.This method not only can overcome porous titanium nitride precast body and the poor deficiency of molten copper aluminium alloy wettability, simultaneously because the infiltration time is short, setting rate fast and avoid titanium nitride in the process of preparing matrix material with molten copper aluminium alloy generation untoward reaction, the mechanical pressure applying not only can overcome the various resistances in precast body, and can also make the hot gas flow in molten copper aluminium alloy forward position discharge die cavity, improve the filling capacity of molten copper aluminium alloy to the small pore of porous titanium nitride precast body, the matrix material density after die casting is significantly raise.So by the advantage in conjunction with carbothermic method and casting die, it is high that the titanium nitride ceramic enhancing Cu-base composites of preparation has density, the feature of mechanical property excellence.Be widely used in the industries such as electrical category special equipment frictional wear structural part, pressure-bearing class special equipment corrosion-and high-temp-resistant structural part, aerospace and automobile making.
Accompanying drawing explanation
Fig. 1 is the porous titanium nitride precast body microstructure photo before embodiment 1 die casting;
Fig. 2 is that embodiment 1 titanium nitride strengthens Cu-base composites microstructure photo.
Embodiment
Below in conjunction with specific embodiment, content of the present invention is described in further detail:
embodiment 1
A kind of titanium nitride ceramic strengthens the front raw materials by weight portion ratio of titanium nitride ceramic precast body sintering of Cu-base composites, formed by 5 parts～95 parts titanium nitrides, 0.1 part～69 parts titanium oxide, 5 component sintering additives, 0.1 part～21 parts carbon blacks, 59 parts～79 parts copper alloys that wherein add matrix material gross weight in titanium nitride ceramic precast body, described sintering aid is yttrium oxide.
Described copper alloy is the cast copper alloy of various models.
Described titanium nitride ceramic strengthens a preparation method for Cu-base composites, carries out in the steps below:
(1), by ratio of weight and the number of copies, take titanium nitride, titanium oxide, sintering aid, carbon black;
(2), by the above-mentioned each material mixing taking, be prepared into mixed powder with wet ball grinding, sieve after mixed powder is dry; Above-mentioned material is packed in mold cavity, and compression molding is precast body;
(3), under 6 normal atmosphere nitrogen atmospheres, be warmed up to gradually at 1650 ℃ and be incubated 2 hours with the heat-up rate of 4 ℃/min, obtain sintered porous titanium nitride precast body, in sintering process, pass into all the time flowing nitrogen 3L/min;
(4), the part that directly contacts with liquid metal of pressure die-casting machine coats releasing agent, with conveniently stripped;
(5), porous titanium nitride precast body and pressure die-casting machine are preheated to 500 ℃～700 ℃, copper alloy are heated to temperature and reach 1100 ℃ of molten states;
(6), after pressure die-casting machine internal temperature and molten copper aluminium alloy all reach predetermined temperature, molten copper aluminium alloy is poured in the cavity of placing porous titanium nitride precast body;
(7), then rely on pressing machine that molten copper aluminium alloy is pressed in porous titanium nitride precast body, in the time that pressure reaches 20～40MPa pressure, stop pressurization, and keep pressure 10 minutes, finally after ingot bar is cooling, separate with mould;
(8), unnecessary copper alloy will be removed after ingot bar again melting.
(9), carry out obtaining matrix material after T6 thermal treatment process to removing the titanium nitride precast body of unnecessary copper alloy, described T6 thermal treatment process: in half an hour, furnace temperature is risen to 500 ℃ from room temperature after product is put into retort furnace, and be incubated 6 hours, then sample is taken out to shrend, then within 6 hours, eliminate internal stress 180 ℃ of insulations.
In sum, table 1 is the void content that the titanium nitride ceramic of embodiments of the invention 2～9 compositions strengthens the composition of Cu-base composites and the porous titanium nitride precast body of preparation, measures the ventilate rate of porous titanium nitride precast body with Archimedes's drainage.Scanning electronic microscope is observed microstructure on sample section.The embodiment 2-9 titanium nitride that obtained by aforesaid method strengthens Cu-base composites and measures three-point bending strength and the fracture toughness property under room temperature, carries out microhardness testing with Vickers' hardness instrument.The results of property of these void content and mechanical property is as table 1, shown in 2.
The preparation method of embodiment 2～9 is with embodiment 1.
Composition and void content that table 1 is titanium nitride porous preform of the present invention
table 2 titanium nitride ceramic of the present invention strengthens Cu-base composites Die Casting Condition and performance
Be 500～700 ℃ in the temperature of pressure die-casting machine as can be seen from Table 2, copper alloy Heating temperature is 1100 ℃, die casting in the scope that die casting pressure is 20～40MPa, and matrix material has shown very high flexural strength, fracture toughness property and microhardness.Reach as high as respectively 594MPa,
, 347 HV.
Figure 1 shows that the porous titanium nitride precast body microstructure photo before embodiment 2 die casting.
The crystal grain of this porous titanium nitride precast body microstructure photo explanation precast body is evenly distributed, and void content is more flourishing.
Figure 2 shows that embodiment 2 titanium nitrides strengthen Cu-base composites microstructure photo.
The crystal grain in precast body is connected into sheet by the copper alloy that this titanium nitride strengthens in Cu-base composites microstructure photo explanation ingot bar, strengthened the intensity of ingot bar.
Claims (2)
1. a titanium nitride ceramic strengthens Cu-base composites, it is characterized in that the front raw materials by weight portion ratio of titanium nitride ceramic precast body sintering, formed by 5 parts～95 parts titanium nitrides, 0.1 part～69 parts titanium oxide, 5 component sintering additives, 0.1 part～21 parts carbon blacks, wherein in titanium nitride ceramic precast body, add 59 parts～79 parts copper alloys of matrix material gross weight, described sintering aid is yttrium oxide, the preparation method of described Cu-base composites, carries out in the steps below:
(1), by ratio of weight and the number of copies, take titanium nitride, titanium oxide, sintering aid, carbon black;
(2), by the above-mentioned each material mixing taking, be prepared into mixed powder with wet ball grinding, sieve after mixed powder is dry; Above-mentioned material is packed in mold cavity, and compression molding is precast body;
(3), under 6 normal atmosphere nitrogen atmospheres, be warmed up to gradually at 1650 ℃ and be incubated 2 hours with the heat-up rate of 4 ℃/min, obtain sintered porous titanium nitride precast body, in sintering process, pass into all the time flowing nitrogen 3L/min;
(4), the part that directly contacts with liquid metal of pressure die-casting machine coats releasing agent, with conveniently stripped;
(5), porous titanium nitride precast body and pressure die-casting machine are preheated to 500 ℃～700 ℃, copper alloy are heated to temperature and reach 1100 ℃ of molten states;
(6), after pressure die-casting machine internal temperature and molten copper aluminium alloy all reach predetermined temperature, molten copper aluminium alloy is poured in the cavity of placing porous titanium nitride precast body;
(7), then rely on pressing machine that molten copper aluminium alloy is pressed in porous titanium nitride precast body, in the time that pressure reaches 20～40MPa pressure, stop pressurization, and keep pressure 10 minutes, finally after ingot bar is cooling, separate with mould;
(8), will after ingot bar again melting, remove unnecessary copper alloy,
(9), carry out obtaining matrix material after T6 thermal treatment process to removing the titanium nitride precast body of unnecessary copper alloy, described T6 thermal treatment process: in half an hour, furnace temperature is risen to 500 ℃ from room temperature after product is put into retort furnace, and be incubated 6 hours, then sample is taken out to shrend, then within 6 hours, eliminate internal stress 180 ℃ of insulations.
2. a kind of titanium nitride ceramic according to claim 1 strengthens Cu-base composites, it is characterized in that described copper alloy is the cast copper alloy of various models.
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| CN1701052A (en) * | 2003-10-27 | 2005-11-23 | 罗伯特·博世有限公司 | Method for producing a composite part and metal/ceramic part |
| CN101734920A (en) * | 2009-12-04 | 2010-06-16 | 西安交通大学 | Titanium nitride porous ceramics and preparation method thereof |
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| CN1701052A (en) * | 2003-10-27 | 2005-11-23 | 罗伯特·博世有限公司 | Method for producing a composite part and metal/ceramic part |
| CN101734920A (en) * | 2009-12-04 | 2010-06-16 | 西安交通大学 | Titanium nitride porous ceramics and preparation method thereof |
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