CN103073300A - Method for realizing low-temperature sintering of transition metal nitride ceramics - Google Patents
Method for realizing low-temperature sintering of transition metal nitride ceramics Download PDFInfo
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Abstract
The invention relates to a method for realizing the low-temperature sintering of transition metal nitride ceramics. According to the method, transition metal nitride MeN is used as raw materials, transition metal Me' is used as sintering agents, and the sintering is carried out through hot pressing sintering or discharge plasma sintering, wherein the hot pressing sintering or the discharge plasma sintering is characterized in that the heat insulation is carried out at the first temperature so that the transition metal nitride and the transition metal directly react to form solid solution, then, a certain pressure is exerted, and in addition, the temperature is raised to the second temperature for carrying out sintering. In the sintering process, through the solid solution effect at a certain temperature, Me' enters MeN crystal lattices, the non-stoichiometry (Me, Me')N<1-x> phases with the controlled nitrogen vacancy concentration are formed, and the mass transfer process in the sintering process is promoted through the nitrogen vacancy concentration increase, so the low-temperature sintering compaction of the transition metal nitride ceramics is realized.
Description
Technical field
The present invention relates to a kind of method that realizes transition metal nitride ceramic low-temp sintering, thereby be specifically related to a kind ofly improve the method that nitrogen vacancy concentration acceleration of sintering prepares the transition metal nitride stupalith at a lower temperature based on the solid solution effect, belong to non-oxidized substance diphase ceramic material preparing technical field.
Background technology
In the 4th generation nuclear energy fission system, investigators propose to use actinium series nitride (be called for short AnN, wherein, An is the radioelement such as Am, Cm) as nuclear fuel.The 4th generation nuclear energy fission system places reactor core or the employed inertial base material of parcel nuclear fuel (being called for short the IMF material) has proposed harsh service requirements.The IMF material need to have the characteristics such as high-melting-point or decomposition temperature, high heat conductance, high-fracture toughness, highly anti-radiation, high resistance pyrochemistry corrodibility, low irradiation rate of expansion and neutron-absorption cross-section be little usually.Under the condition of not considering material fracture toughness, only have transition metal carbide (to be called for short MeC, such as TiC, ZrC, HfC etc.) or transition metal nitride (be called for short MeN, such as TiN, ZrN, HfN etc.) can satisfy the fission selection requirement of the IMF of system material system of nuclear energy of the 4th generation.MeC and MeN pottery have good neutron performance, heat physical properties, stability at elevated temperature usually; In addition, it also has and the single Nitride Phase of other a lot of actinide elementss crystal configuration (NaCl type) together, can also form with it sosoloid as the lapping of AnN nuclear fuel, this just can reduce the possibility that in use causes mishap with AnN because thermal expansivity does not mate largely.
In the nuclear fuel that uses, part actinium series nitride has very high saturated vapor pressure, such as ThN, AmN etc., is volatilizing above just being easy under about 1500 ℃ the temperature.Tamman empirical law according to ceramic post sintering knows that the sintering temperature of pottery is generally its fusing point (T
m) 70 ~ 80%, i.e. (0.7 ~ 0.8) T
mAnd the fusing point of MeC and MeN pottery is all between 2950 ~ 3450 ℃, and this just means that for MeC and MeN pottery, the required temperature of sintering densification will be at least more than 2065 ℃.AnN nuclear fuel itself needs the contradiction of excessive temperature ability sintering densification to bring great difficulty to the preparation of nucleus fuel element because high saturated vapor pressure volatilizees easily with its MeC and MeN body material (IMF material) at a lower temperature.
And relevant MeN(Me=Ti, Zr, Hf) report of ceramic low-temp sintering, adopted is to introduce low melting point metal (Ni, Cr) as additive more, forms at a lower temperature the liquid phase acceleration of sintering, but weak point is to introduce impurity, amorphous liquid phase can remain in grain boundaries, affects the performance of material, especially high-temperature behavior.The preparation method of the inventor's disclosed a kind of zirconium boride 99.5004323A8ure or zirconium carbide ceramics in Chinese patent CN102190495A for example, it is with Zr powder and C powder or Zr powder and B
4The C powder is as complex sintering aids.In addition, the method is to promote the densification of material and suppress the grain growth of crystal by generated in-situ zirconium carbide with higher sintering activity or zirconium boride 99.5004323A8ure second phase particles, and its sintering temperature is higher, is 1800～2000 ℃.Therefore, the low-temperature sintering densification of high-performance transition metal nitride stupalith becomes a brand-new research direction.
Summary of the invention
For above-mentioned problems of the prior art, the object of the present invention is to provide the method that realizes transition metal nitride ceramic low-temp sintering in a kind of situation not introducing impurity phase.Different from inventor preparation method of disclosed a kind of zirconium boride 99.5004323A8ure or zirconium carbide ceramics in Chinese patent CN102190495A, the present invention has utilized the reaction solid solution effect of transition metal nitride and transition metal, form sosoloid by ceramic matrix raw material and sintering aid direct reaction, thereby further reduced sintering temperature, be low to moderate under 1300 ℃ the temperature minimum, can realize the sintering densification of material.
At this, the invention provides a kind of method that realizes transition metal nitride ceramic low-temp sintering, described method be take transition metal nitride MeN as raw material, transition metal M e ' carries out sintering by hot pressed sintering or discharge plasma sintering as sintering aid, wherein said hot pressed sintering or discharge plasma sintering (SPS) are to be incubated first to make transition metal nitride and transition metal reaction form sosoloid under the first temperature, apply certain pressure again and are warming up to the second temperature and carry out sintering.
In the present invention, described transition metal nitride MeN can be TiN, ZrN or HfN, and Me is Ti, Zr or Hf), then Me ' is Ti, Zr or Hf.Transition metal nitride described in the present invention and transition metal direct reaction refer to that Me ' enters and form the controlled sosoloid of nitrogen vacancy concentration in the lattice of MeN.Described sosoloid can be used non-stoichiometric formula (Me, Me ') N
1-xExpression, wherein 0＜x≤0.23, and this x are the (impacts of 1mol%～30mol%) of the addition that is subjected to transition metal sintering aid Me '.Particularly, this x span is according to reaction equation: (1-x) MeN+xMe ' → (Me, Me ') N
1-xCalculate acquisition, and further verified by test.
Preferably, the purity of described transition metal nitride MeN raw material greater than 98%, particle diameter is 1～20 μ m; More preferably particle diameter is 1～5 μ m.Again, described transition metal sintering aid be preferably purity greater than 98%, particle diameter is the powder of 1～100 μ m; More preferably particle diameter is 5～50 μ m.
Again, preferably described transition metal nitride raw material is to be in molar ratio 1:(0.01～0.3 with described transition metal sintering aid) mix, and then carry out sintering by hot pressed sintering or discharge plasma sintering.More preferably this mol ratio is 1:(0.1～0.3).
Hot pressing of the present invention or SPS process are carried out hot pressed sintering or SPS sintering for mixed powder is placed mould in vacuum or inert atmosphere, obtain the final product of densification under lower temperature.The preferred inner wall surface of the mould of described hot pressed sintering or discharge plasma sintering applies the graphite jig of boron nitride.
In described hot pressed sintering, described the first temperature is preferably 1000～1400 ℃, and soaking time is preferably 10～60 minutes; Described exerting pressure is preferably 20～100MPa, and described the second temperature is preferably 1400～1800 ℃, and soaking time is preferably 0.5～5 hour.
Again, temperature rise rate is preferably 5～50 ℃/minute in described hot pressed sintering.
In described discharge plasma sintering, described the first temperature is preferably 1000～1300 ℃, and soaking time is preferably 1～30 minute; Described exerting pressure is preferably 20～100MPa, and described the second temperature is preferably 1300～1600 ℃, and soaking time is preferably 1～30 minute.
Again, temperature rise rate is preferably 50～200 ℃/minute in described discharge plasma sintering.
Preferably, described hot pressed sintering or discharge plasma sintering carry out under vacuum or inert atmosphere.Described inert atmosphere is preferably argon gas atmosphere.
The mixing process of transition metal nitride raw material of the present invention and described transition metal sintering aid can comprise ball milling and dry two steps.
The preferred planetary ball mill of described ball milling, ball-milling medium can be acetone or alcohol, and abrading-ball can be silicon nitride or silicon carbide, and rotating speed can be 100～600 rev/mins, and Ball-milling Time can be 1～20 hour.
Described drying can adopt make compound elder generation rotary evaporation again the mode of oven for drying carry out, wherein the rotary evaporation temperature can be 40～80 ℃, the oven for drying temperature can be 50～150 ℃.
In sintering process of the present invention, by the solid solution effect under certain temperature (1000～1400 ℃), Me ' enters in the lattice of MeN, forms controlled non-stoichiometric (Me, the Me ') N of nitrogen vacancy concentration
1-xPhase, the increase of nitrogen vacancy concentration have promoted the mass transfer process in the sintering process, thereby have realized the low-temperature sintering densification of transition metal nitride pottery.The relative density of the transition metal nitride pottery that the present invention is prepared is 95%～99%, and lattice parameter is (to ZrN
1-x)
Compared with prior art, the present invention is in the situation of not introducing impurity phase, and sintering temperature is lower than 1800 ℃, even is low to moderate 1300 ℃, greatly reduces sintering temperature.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the transition metal nitride pottery of preparation among the embodiment 1;
Fig. 2 is scanning electron microscope (SEM) photo of the transition metal nitride pottery fracture of preparation among the embodiment 1.
Embodiment
Further specify 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.
Relevant MeN(Me=Ti in the prior art, Zr, Hf) low-temperature sintering of pottery, adopted is to introduce low melting point metal (Ni, Cr) as additive more, forms at a lower temperature the liquid phase acceleration of sintering, this will introduce impurity, and amorphous liquid phase can remain in grain boundaries, affects the performance of material, especially high-temperature behavior.Compared with prior art, the present invention realizes the method for transition metal nitride ceramic low-temp sintering, is to adopt transition metal nitride (MeN, Me=Ti, Zr, Hf) ceramic powder is raw material, and transition metal (Me ', Me '=Ti, Zr, Hf) be sintering aid, with raw material with after sintering aid mixes, by the low-temperature sintering of hot pressing or discharge plasma sintering process implementation transition metal nitride pottery.In the sintering process, by solid solution effect at a certain temperature, Me ' enters in the lattice of MeN, forms controlled non-stoichiometric (Me, the Me ') N of nitrogen vacancy concentration
1-xPhase, the increase of nitrogen vacancy concentration have promoted the mass transfer process in the sintering process, thereby have realized the low-temperature sintering densification of transition metal nitride pottery.
In one embodiment, described transition metal nitride select purity greater than 98%, particle diameter is the powder of 1～20 μ m; Described transition metal select purity greater than 98%, particle diameter is the powder of 1～100 μ m.
In another embodiment, described raw material mixes with sintering aid, is to be in molar ratio 1:(0.01 ~ 0.3 by described transition metal nitride and described transition metal) mix.
In yet another embodiment, described raw material and sintering aid mixing process comprise ball milling and dry two steps.
In yet another embodiment, 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; Described drying is again oven for drying of first rotary evaporation, and the rotary evaporation temperature is 40～80 ℃, and the oven for drying temperature is 50～150 ℃.
In yet another embodiment, described hot pressing or discharge plasma sintering process are carried out hot pressing or discharge plasma sintering for mixed powder is placed mould in vacuum or inert atmosphere, obtain the final product of densification under lower temperature.
In yet another embodiment, described mould is the graphite jig that inner wall surface applies BN.
In yet another embodiment, described inert atmosphere is argon gas atmosphere.
In yet another embodiment, described hot pressed sintering is first to be warming up to 1000～1400 ℃ and be incubated 10～60 minutes with 5～50 ℃/minute temperature rise rate; Then apply 20～100MPa pressure, be warming up to 1400～1800 ℃ and be incubated 0.5～5 hour with 5～50 ℃/minute temperature rise rate again; After insulation finishes, cool to room temperature.
In yet another embodiment, described discharge plasma sintering is first to be warming up to 1000～1300 ℃ and be incubated 1～30 minute with 50～200 ℃/minute temperature rise rate; Then apply 20～100MPa pressure, be warming up to 1300～1600 ℃ and be incubated 1～30 minute with 50～200 ℃/minute temperature rise rate again; After insulation finishes, cool to room temperature.
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 specified; 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 also only are examples in the OK range, namely, those skilled in the art can do by the explanation of this paper and select in the suitable scope, and not really want to be defined in the hereinafter concrete numerical value of example.
Weighing ZrN powder 10 grams, Zr powder 1.734 grams mix: take acetone as solvent, with 560 rev/mins speed, use Si
3N
4Ball is abrading-ball planetary ball mill 8 hours, the powder that the gained slurry obtains mixing after 60 ℃ of lower oven dry by rotary evaporation; Place inner wall surface to apply the graphite jig of BN the powder that mixes, again mould is placed hot pressing furnace to carry out hot pressed sintering: under vacuum, be warming up to 1200 ℃ and be incubated 30 minutes with 10 ℃/minute temperature rise rate first; When insulation finishes, pass into argon gas; When continuing to be warming up to 1300 ℃, apply 30MPa pressure; Be warming up to 1500 ℃ and be incubated 1 hour with 10 ℃/minute temperature rise rate again; After insulation finished, cool to room temperature took out product and gets final product;
In embodiment 1～18, adopt the relative density of Archimedes's drainage test material.In addition, utilize X-ray diffractometer (XRD, D/Max2550V, Japan), adopt CuK
α 1(wavelength
Ray also adopts the silicon single crystal standard specimen to detect product and lattice parameter thereof.Detection is learnt: through prepared transition metal nitride pottery ZrN behind 1500 ℃ the sintering densification
1-xThe precise chemical structure formula be ZrN
0.83, its relative density is 98.9%, lattice parameter slightly increases,
(the ZrN lattice parameter of stoichiometric ratio is
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the ZrN pottery of preparation among the embodiment 1, and as seen from Figure 1, final product is pure ZrN mutually
1-xPhase.Fig. 2 is the stereoscan photograph of the ZrN pottery fracture of preparation among the embodiment 1, as seen from Figure 2, adopts method provided by the invention, has realized at low temperatures final product phase ZrN
1-xSintering densification.
Embodiment 2
Weighing ZrN powder 10 grams, Zr powder 0.087 gram mixes.All the other contents are all with described in the embodiment 1, but the ceramic densifying temperature is elected 1800 ℃ as;
Detection is learnt: the relative density through prepared transition metal nitride pottery behind 1800 ℃ the sintering densification is 95.5%, and lattice parameter slightly increases,
Embodiment 3
Weighing ZrN powder 10 grams, Zr powder 0.433 gram mixes.All the other contents are all with described in the embodiment 1, but the ceramic densifying temperature is elected 1700 ℃ as;
Detection is learnt: the relative density through prepared transition metal nitride pottery behind 1700 ℃ the sintering densification is 96.2%, and lattice parameter slightly increases,
Embodiment 4
Weighing ZrN powder 10 grams, Zr powder 0.867 gram mixes.All the other contents are all with described in the embodiment 1, but the ceramic densifying temperature is elected 1600 ℃ as;
Detection is learnt: the relative density through prepared transition metal nitride pottery behind 1600 ℃ the sintering densification is 96.8%, and lattice parameter slightly increases,
Embodiment 5
Weighing ZrN powder 10 grams, Zr powder 2.601 grams mix.All the other contents are all with described in the embodiment 1, but the ceramic densifying temperature is elected 1400 ℃ as;
Detection is learnt: the relative density through prepared transition metal nitride pottery behind 1400 ℃ the sintering densification is 98.2%, and lattice parameter slightly increases,
Embodiment 6
Weighing ZrN powder 10 grams, Ti powder 0.455 gram mixes.All the other contents are all with described in the embodiment 1, but the ceramic densifying temperature is elected 1600 ℃ as;
Detection is learnt: the relative density through prepared transition metal nitride pottery behind 1600 ℃ the sintering densification is 97.6%, and lattice parameter decreases,
Embodiment 7
Weighing ZrN powder 10 grams, Ti powder 0.910 gram mixes.All the other contents are all with described in the embodiment 1;
Detection is learnt: the relative density through prepared transition metal nitride pottery behind 1500 ℃ the sintering densification is 98.8%, and lattice parameter decreases,
Embodiment 8
Weighing ZrN powder 10 grams, Ti powder 1.365 grams mix.All the other contents are all with described in the embodiment 1, but the ceramic densifying temperature is elected 1400 ℃ as;
Detection is learnt: the relative density through prepared transition metal nitride pottery behind 1400 ℃ the sintering densification is 97.6%, and lattice parameter decreases,
Embodiment 9
Weighing TiN powder 10 grams, Ti powder 0.774 gram mixes.All the other contents are all with described in the embodiment 1, but the ceramic densifying temperature is elected 1600 ℃ as;
Detection is learnt: the relative density through prepared transition metal nitride pottery behind 1600 ℃ the sintering densification is 98.1%.
Embodiment 10
Weighing TiN powder 10 grams, Ti powder 1.547 grams mix.All the other contents are all with described in the embodiment 1;
Detection is learnt: the relative density through prepared transition metal nitride pottery behind 1500 ℃ the sintering densification is 99.0%.
Embodiment 11
Weighing TiN powder 10 grams, Ti powder 2.321 grams mix.All the other contents are all with described in the embodiment 1, but the ceramic densifying temperature is elected 1400 ℃ as;
Detection is learnt: the relative density through prepared transition metal nitride pottery behind 1400 ℃ the sintering densification is 98.2%.
Embodiment 12
Weighing HfN powder 10 grams, Hf powder 0.927 gram mixes.All the other contents are all with described in the embodiment 1, but the ceramic densifying temperature is elected 1700 ℃ as;
Detection is learnt: the relative density of making pottery through prepared transition metal nitride behind 1700 ℃ the sintering densification is 97.6%.
Embodiment 13
Weighing HfN powder 10 grams, Hf powder 1.854 grams mix.All the other contents are all with described in the embodiment 1, but the ceramic densifying temperature is elected 1600 ℃ as;
Detection is learnt: the relative density of making pottery through prepared transition metal nitride behind 1600 ℃ the sintering densification is 98.3%.
Embodiment 14
Weighing HfN powder 10 grams, Hf powder 2.782 grams mix.All the other contents are all with described in the embodiment 1;
Detection is learnt: the relative density of making pottery through prepared transition metal nitride behind 1500 ℃ the sintering densification is 97.8%.
Embodiment 15
Weighing ZrN powder 10 grams, Zr powder 1.734 grams mix: take acetone as solvent, with 560 rev/mins speed, use Si
3N
4Ball is abrading-ball planetary ball mill 8 hours, the powder that the gained slurry obtains mixing after 60 ℃ of lower oven dry by rotary evaporation; Place inner wall surface to apply the graphite jig of BN the powder that mixes, again mould is placed the discharge plasma sintering stove to carry out discharge plasma sintering: under vacuum, be warming up to 1200 ℃ and be incubated 1 minute with 150 ℃/minute temperature rise rate first; When insulation finishes, apply 30MPa pressure; Be warming up to 1400 ℃ and be incubated 5 minutes with 100 ℃/minute temperature rise rate again; After insulation finished, cool to room temperature took out product and gets final product;
Detection is learnt: through prepared transition metal nitride pottery ZrN behind 1400 ℃ the sintering densification
1-xRelative density be 98.3%, lattice parameter slightly increases,
Embodiment 16
Weighing ZrN powder 10 grams, Ti powder 0.455 gram mixes.All the other contents are all with described in the embodiment 15;
Detection is learnt: the relative density through prepared transition metal nitride pottery behind 1400 ℃ the sintering densification is 97.4%, and lattice parameter decreases,
Embodiment 17
Weighing ZrN powder 10 grams, Zr powder 2.601 grams mix.All the other contents are all with described in the embodiment 15, but the ceramic densifying temperature is elected 1300 ℃ as;
Detection is learnt: the relative density through prepared transition metal nitride pottery behind 1300 ℃ the sintering densification is 98.1%.
Embodiment 18
Weighing ZrN powder 10 grams, Ti powder 0.910 gram mixes.All the other contents are all with described in the embodiment 15, but the ceramic densifying temperature is elected 1300 ℃ as;
Detection is learnt: the relative density through prepared transition metal nitride pottery behind 1300 ℃ the sintering densification is 97.7%.
In sum as seen, the present invention adopts transition metal nitride (MeN, Me=Ti, Zr, Hf) ceramic powder is raw material, transition metal (Me ', Me '=Ti, Zr, Hf) be sintering aid, with raw material with after sintering aid mixes, by the low-temperature sintering of hot pressing or discharge plasma sintering process implementation transition metal nitride pottery.In the sintering process, by solid solution effect at a certain temperature, Me ' enters in the lattice of MeN, forms controlled non-stoichiometric (Me, the Me ') N of nitrogen vacancy concentration
1-xPhase, the increase of nitrogen vacancy concentration have promoted the mass transfer process in the sintering process, thereby have realized the low-temperature sintering densification of transition metal nitride pottery.
Industrial applicability: the method for realization transition metal nitride ceramic low-temp sintering of the present invention, prepare at a lower temperature the transition metal nitride stupalith thereby improve nitrogen vacancy concentration acceleration of sintering based on the solid solution effect, 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. method that realizes transition metal nitride ceramic low-temp sintering, it is characterized in that, take transition metal nitride MeN as raw material, transition metal M e ' carries out sintering by hot pressed sintering or discharge plasma sintering as sintering aid, wherein said hot pressed sintering or discharge plasma sintering are to be incubated first to make transition metal nitride and transition metal direct reaction form sosoloid under the first temperature, apply certain pressure again and are warming up to the second temperature and carry out sintering.
2. method according to claim 1 is characterized in that, Me is Ti, Zr or Hf; Me ' is Ti, Zr or Hf.
3. method according to claim 1 and 2 is characterized in that, described transition metal nitride is purity greater than 98%, particle diameter is the powder of 1～20 μ m; Described transition metal is purity greater than 98%, particle diameter is the powder of 1～100 μ m.
4. each described method is characterized in that according to claim 1～3, and the mol ratio of described transition metal nitride and described transition metal is 1:(0.01～0.3).
5. each described method is characterized in that according to claim 1～4, and in described hot pressed sintering, described the first temperature is 1000～1400 ℃, and soaking time is 10～60 minutes; Described exerting pressure is 20～100MPa, and described the second temperature is 1400～1800 ℃, and soaking time is 0.5～5 hour.
6. method according to claim 5 is characterized in that, temperature rise rate is 5～50 ℃/minute in described hot pressed sintering.
7. each described method is characterized in that according to claim 1～4, and in described discharge plasma sintering, described the first temperature is 1000～1300 ℃, and soaking time is 1～30 minute; Described exerting pressure is 20～100MPa, and described the second temperature is 1300～1600 ℃, and soaking time is 1～30 minute.
8. method according to claim 7 is characterized in that, in described discharge plasma sintering, temperature rise rate is 50～200 ℃/minute.
9. each described method is characterized in that according to claim 1～8, and described hot pressed sintering or discharge plasma sintering carry out under vacuum or inert atmosphere.
10. method according to claim 9 is characterized in that, described inert atmosphere is argon gas atmosphere.
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| CN105439562A (en) * | 2015-12-09 | 2016-03-30 | 燕山大学 | Preparation method of multi-component transition metal covalent bond compound of single-phase simple crystal structure |
| CN107021761A (en) * | 2017-04-26 | 2017-08-08 | 燕山大学 | A kind of silicon nitride based self lubricated composite material |
| CN109626974A (en) * | 2018-12-12 | 2019-04-16 | 温州市星峰新材料有限公司 | A kind of low-temperature co-burning ceramic material and preparation method thereof |
| CN112679211A (en) * | 2021-01-29 | 2021-04-20 | 北方民族大学 | ZrN-lanthanum oxide complex phase ceramic and pressureless reaction sintering preparation method thereof |
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| CN104446499A (en) * | 2014-11-26 | 2015-03-25 | 燕山大学 | Method for preparing TiN-A1N-TiB2 ceramic composite material at low temperature |
| CN104446499B (en) * | 2014-11-26 | 2016-05-04 | 燕山大学 | A kind of low temperature is prepared TiN-AlN-TiB2The method of ceramic composite |
| CN105439562A (en) * | 2015-12-09 | 2016-03-30 | 燕山大学 | Preparation method of multi-component transition metal covalent bond compound of single-phase simple crystal structure |
| CN107021761A (en) * | 2017-04-26 | 2017-08-08 | 燕山大学 | A kind of silicon nitride based self lubricated composite material |
| CN109626974A (en) * | 2018-12-12 | 2019-04-16 | 温州市星峰新材料有限公司 | A kind of low-temperature co-burning ceramic material and preparation method thereof |
| CN109626974B (en) * | 2018-12-12 | 2021-08-27 | 苏州研资工业技术有限公司 | Low-temperature co-fired ceramic material and preparation method thereof |
| CN112679211A (en) * | 2021-01-29 | 2021-04-20 | 北方民族大学 | ZrN-lanthanum oxide complex phase ceramic and pressureless reaction sintering preparation method thereof |
| CN112679211B (en) * | 2021-01-29 | 2022-05-06 | 北方民族大学 | ZrN-lanthanum oxide complex phase ceramic and pressureless reaction sintering preparation method thereof |
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