CN103113125A - Lamellar compound platy crystal grain dispersed and enhanced transition metal carbide multiphase material and ultralow temperature preparation method thereof - Google Patents
Lamellar compound platy crystal grain dispersed and enhanced transition metal carbide multiphase material and ultralow temperature preparation method thereof Download PDFInfo
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- CN103113125A CN103113125A CN2013100462468A CN201310046246A CN103113125A CN 103113125 A CN103113125 A CN 103113125A CN 2013100462468 A CN2013100462468 A CN 2013100462468A CN 201310046246 A CN201310046246 A CN 201310046246A CN 103113125 A CN103113125 A CN 103113125A
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Abstract
The invention relates to a lamellar compound platy crystal grain dispersed and enhanced transition metal carbide multiphase material and an ultralow temperature preparation method thereof. The multiphase material comprises transition metal carbide MC taken as a main phase and a lamellar compound M(x+1)ACx which is taken as a dispersed phase, dispersed and distributed in platy crystal grains and closely combined with the transition metal carbide to realize bridging connection, wherein the M(x+1)ACx is obtained by in situ synthesis of the transition metal carbide MC as well as a transition metal M and a simple substance A of an element in a family IIIA or IVA, and x in the formula is equal to 1 or 2. The lamellar compound M(x+1)ACx can effectively refine the transition metal carbide crystal grains, and phases formed by an in situ synthesis reaction are closely combined, so that mechanical properties, thermal conductivity and other properties of the obtained multiphase material are improved.
Description
Technical field
The present invention relates to transition metal carbide composite diphase material and very low temperature preparation method thereof that a kind of lamellar compound plate-like grain disperse strengthens, be specifically related to a kind ofly based on there being in-situ synthesized reaction that liquid phase exists to prepare at a lower temperature the method for transition metal carbide-lamellar compound composite diphase material, belong to non-oxidized substance diphase ceramic material preparing technical field.
Background technology
Nuclear power source has obtained broad research both domestic and external and application as a kind of emerging energy in recent decades.U.S.'s core academic year that hold in June, 1999 can go up, the U.S., France, Britain, Japan and other countries proposed four generation nuclear power system imagination.Four generation nuclear energy technology refer to nuclear energy technology leaved for development, can solve economy, the security of nuclear energy, can improve also that nuclear waste is processed and the problem of atomic scatterring [Ma Xuquan, nuclear energy exploitation and application, Chemical Industry Press, 2005].Transition metal carbide MC(M=Ti, Zr, Hf, Ta) with its high-melting-point, solid-state phase changes do not occur, and have a series of excellent properties such as thermal shock resistance relatively preferably, higher hot strength and become four generations the inertial base fuel (IMF) that adopts of nuclear power system important candidate material [" Gen IV Nuclear Energy Systems ", FY-04Annual Report, 2004].And simultaneously, four generation nuclear power system also higher requirement has been proposed its IMF that adopts: the densification of the one, IMF under mild temperature, in general, the sintering densification temperature will be controlled at below 1600 ℃; The highly malleablized of the 2nd, IMF material.The development that exists for IMF of the problems referred to above has brought huge obstacle, causes substantially belonging to so far blank about the bibliographical information of the IMF material of low-temperature sintering, strong mechanical performance.
Rule graceful according to Thailand, the sintering temperature of stupalith is generally 70 ~ 80% of its fusing point, and the candidate material TiC of IMF, the fusing point of ZrC etc. all surpasses 3000 ℃.Utilize the business powder and be difficult to its sintering temperature is reduced to below 1600 ℃ in conjunction with conventional sintering process.But for extreme environments for use such as the high service temperature of IMF, strong irradiation and heat-flash impacts, only with TiC, ZrC is that a series of advanced structural ceramic materials of representative just can meet the demands, this is also the important breakthrough mouth that advanced structural ceramic is used at energy field according to the Strategic Demand of country simultaneously, and the development in the new millennium has important directive significance to structural ceramic material.Therefore, sintering densification transition metal carbide stupalith becomes a brand-new research direction at lower than the temperature of 1600 ℃.Usually, in stupalith compound disperse phase can promote its under mild temperature densification and make its highly malleablized, for example Chinese patent CN100355695C discloses a kind of chromium carbide and carbon titanium nitride particle dispersion consolidatedization alumina ceramic composite material, Chinese patent CN100336929C discloses a kind of preparation method of in-situ produced titanium carbide dispersion strengthening copper based composite material, but the transition metal carbide composite diphase material that strengthens about disperse also rarely has report.
Summary of the invention
For the existing the problems referred to above of prior art, the present invention is according to the design of material thought of introducing lamellar compound nano slabby crystal grain disperse enhancing in fragility, low intensive carbide ceramics, purpose is to provide transition metal carbide composite diphase material and the very low temperature preparation method thereof that a kind of lamellar compound plate-like grain disperse strengthens, to satisfy the application requiring of transition metal carbide composite diphase material in nuclear power system inertial base fuel.
At this, on the one hand, the invention provides the transition metal carbide composite diphase material that a kind of lamellar compound plate-like grain disperse strengthens, described composite diphase material comprises: as the transition metal carbide MC of principal phase; With distribute and closely be combined the lamellar compound M that realizes bridging with described transition metal carbide as disperse phase and with the plate-like grain disperse
(x+1)AC
x, M wherein
(x+1)AC
xBy described transition metal carbide MC and transition metal M and IIIA or the synthetic gained of the IVA element simple substance A of family original position, x=1 or 2 in formula.
In the present invention, transition metal M is any one in Ti, Zr, Hf and Ta; IIIA or the IVA element simple substance A of family are any one in Si, Al, Ga, Ge, In, Sn and Pb.
Layered compound M
(x+1)AC
xMolar percentage in described composite diphase material is preferably 1%～50%, and more preferably 10%～30%.
The lamellar compound M that described transition metal carbide MC and transition metal M and IIIA or the IVA element simple substance A of family reaction in－situ generate
(x+1)AC
xCombining closely between each phase that the effectively described transition metal carbide crystal grain of refinement, and in-situ synthesized reaction forms, thus mechanical property, thermal conductivity and other multinomial performance of the resulting composite diphase material of the present invention all are improved.The relative density of described composite diphase material of the present invention is more than 98%, and flexural strength is more than 600MPa.
On the other hand, the present invention also provides the preparation method of the transition metal carbide composite diphase material that layered compound plate-like grain disperse strengthens, and described method is to carry out ball milling to mix and make mixed powder take transition metal carbide, transition metal and IIIA or IVA family element simple substance as raw material; And described mixed powder is carried out reactive hot press sintering or react the discharge plasma sintering making described composite diphase material under certain sintering temperature, wherein said transition metal is the simple substance of the transition metal in described transition metal carbide.
In described reactive hot press sintering or reaction discharge plasma sintering process, described transition metal and IIIA or IVA family element simple substance form transition liquid-phase, effectively promote mass transfer process in the ceramic post sintering process, be conducive to the densification of pottery at lower temperature; Simultaneously described transition metal and IIIA or IVA family element simple substance also with described transition metal carbide generation in-situ synthesized reaction, consumed the described transition metal carbide of part, effectively reduced the grain-size of described transition metal carbide, and the tabular layered compound of reaction in－situ generation, can either effectively hinder the growth of described transition metal carbide crystal grain, also play tabular toughness reinforcing effect; In addition, layered compound crystal grain realizes bridging, has increased the thermal conductance path, has improved thermal conductance, and simultaneously, tabular layered compound crystal grain has also played the effect that improves the anti-irradiation tolerance of material.
The mol ratio of described transition metal carbide, described transition metal, described IIIA or IVA family simple substance is preferably (3～100): 1:1, more preferably (5～20): 1:1.
Preferably, described transition metal carbide is purity greater than 99%, particle diameter is the powder of 1～10 μ m, and more preferably particle diameter is 1～5 μ m; Described transition metal is purity greater than 99%, particle diameter is the powder of 1～100 μ m, and more preferably particle diameter is 1～20 μ m; Described IIIA or IVA family simple substance powder are purity greater than 99%, particle diameter is the powder of 1～100 μ m, and more preferably particle diameter is 1～20 μ m.
Described reaction hot-pressing is preferably first with the temperature rise rate of 5～50 ℃/minute and is warming up to 1000～1400 ℃ and be incubated 10～60 minutes; Then apply 20～100MPa pressure, then be warming up to 1200～1600 ℃ and be incubated 0.5～5 hour with the temperature rise rate of 5～50 ℃/minute.
Describedly answer the discharge plasma sintering to be preferably first with the temperature rise rate of 50～200 ℃/minute to be warming up to 1000～1400 ℃ and be incubated 1～30 minute; Then apply 20～100MPa pressure, then be warming up to 1200～1600 ℃ and be incubated 1～30 minute with the temperature rise rate of 50～200 ℃/minute.
The mould of described reactive hot press sintering or reaction discharge plasma sintering is preferably the graphite jig that inner wall surface applies BN.
Again, described reactive hot press sintering or reaction discharge plasma sintering preferably carry out in vacuum or inert atmosphere.Described inert atmosphere is preferably argon gas atmosphere.
Preferably, described ball milling is planetary ball mill, and ball-milling medium is acetone or alcohol, and abrading-ball is Si
3N
4Or SiC, rotating speed is 100～600 rev/mins, Ball-milling Time is 1～20 hour; Drying temperature is 50～150 ℃.
The present invention utilizes the in-situ synthesized reaction of material powder to realize the sintering densification of transition metal carbide stupalith under lower sintering temperature (1200～1600 ℃), and has obtained to have the transition metal carbide composite diphase material that the lamellar compound plate-like grain disperse of good mechanical property, thermal conductivity and other multinomial performance strengthens.
Description of drawings
Fig. 1 is microstructural alternative schematic diagram in transition metal carbide composite diphase material very low temperature preparation process in the present invention, raw materials usedly in figure selects raw material as example in embodiment 1;
Fig. 2 is the transition metal carbide composite diphase material fracture of very low temperature preparation in embodiment 1 and the stereoscan photograph of polished surface, and wherein Fig. 2 (a) is the fracture stereoscan photograph; Fig. 2 (b) is the polished surface stereoscan photograph.
Embodiment
Further illustrate the present invention below in conjunction with following embodiment, should be understood that following embodiment only is used for explanation the present invention, and unrestricted the present invention.
The preparation method of the transition metal carbide composite diphase material that lamellar compound plate-like grain disperse of the present invention strengthens is to carry out ball milling to mix and make mixed powder take transition metal carbide, transition metal and IIIA or IVA family element simple substance as raw material; And described mixed powder is carried out reactive hot press sintering or react the discharge plasma sintering making described composite diphase material under certain sintering temperature, wherein said transition metal is the simple substance of the transition metal in described transition metal carbide.The prepared composite diphase material of method of the present invention comprises the transition metal carbide MC as principal phase; With distribute and closely be combined the lamellar compound M that realizes bridging with described transition metal carbide as disperse phase and with the plate-like grain disperse
(x+1)AC
x, M wherein
(x+1)AC
xBy described transition metal carbide MC and transition metal M and IIIA or the synthetic gained of the IVA element simple substance A of family original position, x=1 or 2 in formula.
More specifically, as example, preparation method of the present invention can comprise the following steps:
A) transition metal carbide, transition metal, IIIA or IVA family element simple substance are mixed, ball milling, drying obtains mixed powder;
B) gained mixed powder of upper step is placed in mould, adopts reactive hot press sintering or reaction discharge plasma sintering process in vacuum or inert atmosphere, sintering and obtain final product under lower sintering temperature.
In one example, the described ball milling of described step in a) is planetary ball mill, and ball-milling medium is acetone or alcohol, and abrading-ball is Si
3N
4Or SiC, rotating speed is 100～600 rev/mins, Ball-milling Time is 1～20 hour; Drying temperature is 50～150 ℃.
In one example, the mould therefor described step b) selects inner wall surface to apply the graphite jig of BN.Be argon gas atmosphere at inert atmosphere described in another example.
In another example, at step b) in, described reactive hot press sintering is first to be warming up to 1000～1400 ℃ and be incubated 10～60 minutes with the temperature rise rate of 5～50 ℃/minute; Then apply 20～100MPa pressure, then be warming up to 1200～1600 ℃ and be incubated 0.5～5 hour with the temperature rise rate of 5～50 ℃/minute; After insulation finishes, cool to room temperature.
In another example, at step b) in, described reaction discharge plasma sintering is first to be warming up to 1000～1400 ℃ and be incubated 1～30 minute with the temperature rise rate of 50～200 ℃/minute; Then apply 20～100MPa pressure, then be warming up to 1200～1600 ℃ and be incubated 1～30 minute with the temperature rise rate of 50～200 ℃/minute; After insulation finishes, cool to room temperature.
In addition, lower sintering temperature of the present invention refers to 1200～1600 ℃.
Compared with prior art, it is raw material that the present invention adopts transition metal carbide, transition metal, IIIA or IVA family element simple substance, by reactive hot press sintering or reaction discharge plasma sintering process, utilize material powder generation in-situ synthesized reaction, thereby realized the sintering preparation of the transition metal carbide composite diphase material under very low temperature.The stupalith that obtains is a kind of transition metal carbide-lamellar compound composite diphase material, and its microstructure is that the disperse of lamellar compound plate-like grain distributes and closely is combined with the tiny transition metal carbide of crystal grain.Effect due to the effective refinement transition metal carbide of tabular lamellar compound crystal grain, and combining closely between each phase of in-situ synthesized reaction formation, thereby mechanical property, thermal conductivity and other multinomial performance of the resulting composite diphase material of the present invention all are improved.
The below further exemplifies embodiment to describe the present invention in detail.Should understand equally; following examples only are used for the present invention is further illustrated; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameters such as the temperature that following example is concrete, time are only also examples in OK range, namely, those skilled in the art can do by the explanation of this paper and select in suitable scope, and not really want to be defined in the hereinafter concrete numerical value of example.
Embodiment 1
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 2.470 grams and Si powder 1.449 grams mix; Take acetone as solvent, with the speed of 560 rev/mins, use Si
3N
4Ball is abrading-ball planetary ball mill 8 hours, the powder that the gained slurry obtains mixing after oven dry under 60 ℃ by rotary evaporation; The powder that mixes is placed in graphite jig, then mould is placed in hot pressing furnace carries out hot pressed sintering: first be warming up to 1300 ℃ and be incubated 30 minutes with the temperature rise rate of 10 ℃/minute; When insulation finishes, apply 30MPa pressure; Be warming up to 1500 ℃ and be incubated 1 hour with the temperature rise rate of 10 ℃/minute again; After insulation finished, cool to room temperature took out product and gets final product;
Fig. 1 is microstructural alternative schematic diagram in transition metal carbide composite diphase material very low temperature preparation process in the present invention.As seen from Figure 1: in temperature-rise period, Ti and Si form transition liquid-phase, have effectively promoted mass transfer process in the ceramic post sintering process, are conducive to the densification of pottery at lower temperature; Simultaneously, the reaction in－situ of TiC and Ti, Si has consumed part TiC, has effectively reduced the grain-size of TiC, and the tabular second-phase Ti of reaction in－situ generation
3SiC
2, can either effectively hinder the growth of TiC crystal grain, also played tabular toughness reinforcing effect; In addition, Ti
3SiC
2Crystal grain is realized bridging, has increased the thermal conductance path, has improved thermal conductance, simultaneously, and tabular Ti
3SiC
2Crystal grain has also played the effect that improves the anti-irradiation tolerance of material;
Fig. 2 is the transition metal carbide composite diphase material fracture of very low temperature preparation in embodiment 1 and the stereoscan photograph of polished surface, and wherein Fig. 2 (a) is the fracture stereoscan photograph; Fig. 2 (b) is the polished surface stereoscan photograph.As seen from Figure 2: the TiC particle has less and uniform grain-size, tabular second-phase Ti
3SiC
2Be evenly distributed on around principal phase TiC particle, can find out from the fracture stereoscan photograph, fracture shows as the brilliant fracture of transgranular fracture and edge mixed mode;
In addition, adopt the relative density of Archimedes's drainage test material in embodiment 1～18; Adopt the flexural strength of universal testing machine (INSTRON-5566 type, the U.S.) test material.Three-point bending method is adopted in the flexural strength test, and specimen size is that the span of 2.5mm * 2.0mm * 25mm, test is 20mm, and the rate travel of pressure head is 0.5mm/min.Detection is learnt: be 99.9% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1500 ℃; Its flexural strength is 1003MPa.
Embodiment 2
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 0.200 gram and Si powder 0.117 gram mix;
All the other contents are all with described in embodiment 1, but the ceramic densifying temperature is elected 1600 ℃ as;
Detection is learnt: be 98.9% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1600 ℃; Its flexural strength is 625MPa.
Embodiment 3
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 1.999 grams and Si powder 1.173 grams mix;
All the other contents are all with described in embodiment 1, but the ceramic densifying temperature is elected 1550 ℃ as;
Detection is learnt: be 99.2% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1550 ℃; Its flexural strength is 866MPa.
Embodiment 4
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 6.596 grams and Si powder 3.870 grams mix;
All the other contents are all with described in embodiment 1, but the ceramic densifying temperature is elected 1450 ℃ as;
Detection is learnt: be 99.9% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1450 ℃; Its flexural strength is 759MPa.
Embodiment 5
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 2.499 grams and Al powder 1.408 grams mix;
All the other contents are all with described in embodiment 1;
Detection is learnt: be 99.8% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1500 ℃; Its flexural strength is 945MPa.
Embodiment 6
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 2.499 grams and Ga powder 3.639 grams mix;
All the other contents are all with described in embodiment 1;
Detection is learnt: be 98.9% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1500 ℃; Its flexural strength is 891MPa.
Embodiment 7
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 2.499 grams and Ge powder 3.792 grams mix;
All the other contents are all with described in embodiment 1;
Detection is learnt: be 98.7% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1500 ℃; Its flexural strength is 820MPa.
Embodiment 8
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 2.499 grams and In powder 5.993 grams mix;
All the other contents are all with described in embodiment 1;
Detection is learnt: be 98.3% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1500 ℃; Its flexural strength is 835MPa.
Embodiment 9
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 2.499 grams and Sn powder 6.197 grams mix;
All the other contents are all with described in embodiment 1;
Detection is learnt: be 98.8% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1500 ℃; Its flexural strength is 872MPa.
Embodiment 10
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 2.499 grams and Pb powder 10.816 grams mix;
All the other contents are all with described in embodiment 1;
Detection is learnt: be 98.2% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1500 ℃; Its flexural strength is 826MPa.
Embodiment 11
Press the stoichiometric ratio weighing: ZrC powder 50 grams, Zr powder 2.762 grams and Si powder 0.850 gram mix;
All the other contents are all with described in embodiment 1;
Detection is learnt: be 99.0% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1500 ℃; Its flexural strength is 915MPa.
Embodiment 12
Press the stoichiometric ratio weighing: HfC powder 50 grams, Hf powder 2.932 grams and Si powder 0.461 gram mix;
All the other contents are all with described in embodiment 1;
Detection is learnt: be 98.8% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1500 ℃; Its flexural strength is 934MPa.
Embodiment 13
Press the stoichiometric ratio weighing: TaC powder 50 grams, Ta powder 2.931 grams and Si powder 0.455 gram mix;
All the other contents are all with described in embodiment 1;
Detection is learnt: be 98.4% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1500 ℃; Its flexural strength is 885MPa.
Embodiment 14
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 2.470 grams and Si powder 1.449 grams mix; Take acetone as solvent, with the speed of 560 rev/mins, use Si
3N
4Ball is abrading-ball planetary ball mill 8 hours, the powder that the gained slurry obtains mixing after oven dry under 60 ℃ by rotary evaporation; The powder that mixes is placed in graphite jig, then mould is placed in the discharge plasma sintering oven carries out sintering: first be warming up to 1200 ℃ and be incubated 30 minutes with the temperature rise rate of 100 ℃/minute; When insulation finishes, apply 30MPa pressure; Be warming up to 1400 ℃ and be incubated 5 minutes with the temperature rise rate of 100 ℃/minute again; After insulation finished, cool to room temperature took out product and gets final product;
Detection is learnt: be 99.8% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1400 ℃; Its flexural strength is 989MPa.
Embodiment 15
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 0.200 gram and Si powder 0.117 gram mix;
All the other contents are all with described in embodiment 14, but the ceramic densifying temperature is elected 1500 ℃ as;
Detection is learnt: be 98.6% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1500 ℃; Its flexural strength is 710MPa.
Embodiment 16
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 1.999 grams and Si powder 1.173 grams mix;
All the other contents are all with described in embodiment 14, but the ceramic densifying temperature is elected 1450 ℃ as;
Detection is learnt: be 98.9% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1450 ℃; Its flexural strength is 842MPa.
Embodiment 17
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 6.596 grams and Si powder 3.870 grams mix;
All the other contents are all with described in embodiment 14, but the ceramic densifying temperature is elected 1350 ℃ as;
Detection is learnt: be 99.9% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1350 ℃; Its flexural strength is 811MPa.
Embodiment 18
Press the stoichiometric ratio weighing: TiC powder 50 grams, Ti powder 2.499 grams and Al powder 1.408 grams mix;
All the other contents are all with described in embodiment 14;
Detection is learnt: be 99.6% through prepared its relative density of transition metal carbide composite diphase material after the sintering densification of 1400 ℃; Its flexural strength is 927MPa.
In sum as seen, it is raw material that the present invention adopts transition metal carbide, transition metal, IIIA and IVA family element simple substance, by reaction hot-pressing or reaction discharge plasma sintering process, utilize starting material powder generation in-situ synthesized reaction, thereby realized the sintering preparation of the transition metal carbide composite diphase material under very low temperature.The stupalith that obtains is a kind of transition metal carbide-lamellar compound composite diphase material, and its microstructure is that the disperse of lamellar compound plate-like grain distributes and closely is combined with the tiny transition metal carbide of crystal grain.Effect due to the effective refinement transition metal carbide of tabular lamellar compound crystal grain, and combining closely between each phase of in-situ synthesized reaction formation, thereby mechanical property, thermal conductivity and other multinomial performance of the resulting composite diphase material of the present invention all are improved.
Industrial applicability: the transition metal carbide composite diphase material that lamellar compound plate-like grain disperse of the present invention strengthens has good mechanical property, thermal conductivity and other multinomial performance, preparation method of the present invention has realized the sintering densification of transition metal carbide stupalith under lower sintering temperature, can be applicable to the fields such as inertial base fuel of the 4th generation of technology such as nuclear energy system (Gen-IV).
Claims (10)
1. the transition metal carbide composite diphase material that the disperse of lamellar compound plate-like grain strengthens, is characterized in that, described composite diphase material comprises: as the transition metal carbide MC of principal phase; With distribute and closely be combined the lamellar compound M that realizes bridging with described transition metal carbide as disperse phase and with the plate-like grain disperse
(x+1)AC
x,
M wherein
(x+1)AC
xBy described transition metal carbide MC and transition metal M and IIIA or the synthetic gained of the IVA element simple substance A of family original position, x=1 or 2 in formula.
2. the transition metal carbide composite diphase material of lamellar compound plate-like grain disperse enhancing according to claim 1, is characterized in that, transition metal M is any one in Ti, Zr, Hf and Ta; IIIA or the IVA element simple substance A of family are any one in Si, Al, Ga, Ge, In, Sn and Pb.
3. the transition metal carbide composite diphase material of lamellar compound plate-like grain disperse enhancing according to claim 1 and 2, is characterized in that layered compound M
(x+1)AC
xMolar percentage in described composite diphase material is 1%～50%.
4. the transition metal carbide composite diphase material of lamellar compound plate-like grain disperse enhancing according to claim 3, is characterized in that layered compound M
(x+1)AC
xMolar percentage in described composite diphase material is 10%～30%.
5. the transition metal carbide composite diphase material that the disperse of the described lamellar compound plate-like grain of any one strengthens according to claim 1～4 is characterized in that the relative density of described composite diphase material is more than 98%, and flexural strength is more than 600MPa.
6. the very low temperature preparation method of the transition metal carbide composite diphase material that in a claim 1～5, the disperse of the described lamellar compound plate-like grain of any one strengthens, it is characterized in that, carry out ball milling take transition metal carbide, transition metal and IIIA or IVA family element simple substance as raw material and mix and make mixed powder; And described mixed powder is carried out reactive hot press sintering or react the discharge plasma sintering making described composite diphase material under certain sintering temperature,
Wherein said transition metal is the simple substance of the transition metal in described transition metal carbide.
7. preparation method according to claim 6, is characterized in that, the mol ratio of described transition metal carbide, described transition metal, described IIIA or IVA family simple substance is (3～100): 1:1.
8. according to claim 6 or 7 described preparation methods, is characterized in that, described transition metal carbide is purity greater than 99%, particle diameter is the powder of 1～10 μ m; Described transition metal is purity greater than 99%, particle diameter is the powder of 1～100 μ m; Described IIIA or IVA family simple substance powder are purity greater than 99%, particle diameter is the powder of 1～100 μ m.
9. the described preparation method of any one according to claim 6～8, is characterized in that, described reaction hot-pressing is first to be warming up to 1000～1400 ℃ and be incubated 10～60 minutes with the temperature rise rate of 5～50 ℃/minute; Then apply 20～100MPa pressure, then be warming up to 1200～1600 ℃ and be incubated 0.5～5 hour with the temperature rise rate of 5～50 ℃/minute.
10. the described preparation method of any one according to claim 6～8, is characterized in that, the described discharge plasma sintering of answering is first to be warming up to 1000～1400 ℃ and be incubated 1～30 minute with the temperature rise rate of 50～200 ℃/minute; Then apply 20～100MPa pressure, then be warming up to 1200～1600 ℃ and be incubated 1～30 minute with the temperature rise rate of 50～200 ℃/minute.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106319628A (en) * | 2015-07-06 | 2017-01-11 | 中国科学院金属研究所 | High-quality ultrathin two-dimensional transition-group metal carbide crystal and preparation method thereof |
| CN107540376A (en) * | 2017-09-25 | 2018-01-05 | 常熟理工学院 | A kind of zirconium carbide carborundum composite-phase ceramic material and preparation method thereof |
| CN109053206A (en) * | 2018-08-31 | 2018-12-21 | 中国科学院金属研究所 | A kind of short fiber reinforced orientation MAX phase ceramics based composites and preparation method |
| CN110642609A (en) * | 2019-10-22 | 2020-01-03 | 济南大学 | High-density alumina/MAX phase composite material and in-situ synthesis method thereof |
| CN115340383A (en) * | 2022-08-26 | 2022-11-15 | 中南大学 | Method for improving fracture toughness of multi-component carbide and multi-component carbide |
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2013
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106319628A (en) * | 2015-07-06 | 2017-01-11 | 中国科学院金属研究所 | High-quality ultrathin two-dimensional transition-group metal carbide crystal and preparation method thereof |
| CN106319628B (en) * | 2015-07-06 | 2019-02-19 | 中国科学院金属研究所 | A kind of high-quality ultra-thin two dimension transition metal carbides crystal and preparation method thereof |
| CN107540376A (en) * | 2017-09-25 | 2018-01-05 | 常熟理工学院 | A kind of zirconium carbide carborundum composite-phase ceramic material and preparation method thereof |
| CN109053206A (en) * | 2018-08-31 | 2018-12-21 | 中国科学院金属研究所 | A kind of short fiber reinforced orientation MAX phase ceramics based composites and preparation method |
| CN110642609A (en) * | 2019-10-22 | 2020-01-03 | 济南大学 | High-density alumina/MAX phase composite material and in-situ synthesis method thereof |
| CN115340383A (en) * | 2022-08-26 | 2022-11-15 | 中南大学 | Method for improving fracture toughness of multi-component carbide and multi-component carbide |
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