CN104163633A - Method for rapidly preparing high heat conduction Si3N4 ceramic with low cost - Google Patents

Method for rapidly preparing high heat conduction Si3N4 ceramic with low cost Download PDF

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CN104163633A
CN104163633A CN201410318834.7A CN201410318834A CN104163633A CN 104163633 A CN104163633 A CN 104163633A CN 201410318834 A CN201410318834 A CN 201410318834A CN 104163633 A CN104163633 A CN 104163633A
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mgo
zro
powder
heat conduction
pottery
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郭伟明
马提
游洋
伍尚华
林华泰
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Guangdong University of Technology
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Guangdong University of Technology
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Abstract

The invention discloses a method for rapidly preparing high heat conduction Si3N4 ceramic with low cost. The method is characterized in that Si powder is taken as a raw material, ZrO2 powder is taken as a nitridation catalyst, ZrO2-MgO-Re2O3 is taken as a sintering aid, wherein Re2O3 is taken as a rare earth oxide, Si, ZrO2 and MgO-Re2O3 are mixed according to mass fraction and then dried to obtain a Si-ZrO2-MgO-Re2O3 mixing powder; the mixing powder is subjected to a two-step insulation method and a pressureless sintering process to obtain the high heat conduction Si3N4 ceramic; According to the ceramic material, the relative density is higher than 95%, hardness is 8-20 GPa, fracture toughness is 3-8MPa.m<1/2>, bending strength is 200-1000Mpa, and the thermal conductivity is 20-100W.m<-1>,K<-1>. By introducing a ZrO2 catalyst, Si powder nitridation IS accelerated, the introduction of ZrO2-MgO-Re2O3 can improve the densification of Si3N4, and the high heat conduction Si3N4 ceramic can be rapidly prepared with low cost.

Description

A kind of low cost, prepare high heat conduction Si fast 3n 4the method of pottery
Technical field
The present invention relates to non-oxidized substance base ceramic material field, specifically disclose a kind of low cost, prepare high heat conduction Si fast 3n 4the method of pottery.
Background technology
Si 3n 4the excellent properties such as that pottery has is wear-resisting, high temperature resistant, high heat conduction, are widely used in LED heat-radiating substrate, high speed cutting tool and engine key components and parts etc.Common Si 3n 4pottery is with high-purity Si 3n 4powder is that raw material is prepared by hot pressed sintering, and cost is higher, and can not prepare the sample of complicated shape.
In order to reduce costs, prepare complicated shape, occurred take that Si powder, as raw material, prepares Si by reaction pressure sintering 3n 4pottery.On the one hand, powder preparation and ceramic dense are combined to a step, significantly reduce costs; On the other hand, by gas pressure sintering, can realize Si in enormous quantities, complicated shape 3n 4the preparation of pottery.Yet, because the velocity ratio of Si powder nitrogenize is slower, and the Si forming after nitrogenize 3n 4densification is more difficult.Therefore, in fact Si powder reaction pressure sintering is prepared Si 3n 4the processing condition of pottery are very harsh.For example, Zhu etc. be take Si powder as raw material, by reaction pressure sintering, prepare Si 3n 4pottery, first Si powder completes nitrogenize, the Si then forming at 1400 ℃ of insulation 8h 3n 4powder continues to be warmed up to 1900 ℃ and under 10atm nitrogen, is incubated 12h and just can completes densification (X.W.Zhu, Y.Zhou, K.Hirao, Z. . " ProcessingandThermalConductivityofSintered Reaction-BondedSiliconNitride.I:EffectofSiPowderCharacte ristics, " J.Am.Ceram.Soc., 2006,89:3331-3339).Si powder reaction pressure sintering is prepared Si 3n 4mainly there is two large problems in pottery: (1) Si powder nitridation time is longer, need to be at 1400 ℃ of insulation 8h; (2) Si 3n 4densification condition is too harsh, and nitrogen pressure higher (10atm), sintering temperature higher (1900 ℃), soaking time are grown (12h).So long period and harsh preparation technology's partial offset take the low-cost advantage that Si powder brings as raw material.
The present invention is by introducing ZrO 2catalyzer is accelerated the nitrogenize of Si powder and is introduced ZrO 2-MgO-Re 2o 3(Re 2o 3for rare earth oxide, wherein Re is Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or Lu) improve Si 3n 4densification, realized low-cost, prepare high heat conduction Si fast 3n 4pottery.In the present invention, at Si powder, at 1400 ℃ of nitridation times, from 8h, be significantly reduced to 1～2h, Si 3n 4densification condition also becomes and relaxes very much, only needs 1atm nitrogen pressure, 1700～1800 ℃ of insulation 1～2h.
Summary of the invention
The present invention is by introducing ZrO 2catalyzer is accelerated the nitrogenize of Si powder and is introduced ZrO 2-MgO-Re 2o 3improve Si 3n 4densification, realized low-cost, prepare high heat conduction Si fast 3n 4pottery.
The present invention is achieved by the following technical programs:
A kind of low cost provided by the invention, prepare high heat conduction Si fast 3n 4the method of pottery, comprises the steps:
(1) take Si powder as raw material, with ZrO 2powder is nitrided catalyst, with ZrO 2-MgO-Re 2o 3for sintering aid, Re wherein 2o 3for rare earth oxide, Re is Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or Lu; Press Si:ZrO 2: MgO-Re 2o 3massfraction than be 60～98%:1～20%:1～20% proportioning through batch mixing, dry after, obtain Si-ZrO 2-MgO-Re 2o 3mixed powder; Described MgO-Re 2o 3in MgO:Re 2o 3massfraction ratio is 1～99%:99～1%;
(2) by Si-ZrO 2-MgO-Re 2o 3mixed powder is put into mould, by cold isostatic compaction, obtains base substrate;
(3) by Si-ZrO 2-MgO-Re 2o 3base substrate is prepared high heat conduction Si by two step thermal-insulating method pressureless sinterings 3n 4pottery.
The described Si powder purity of step (1) is 95～100%, and particle diameter is <10 μ m; ZrO 2purity is 98～100%, and particle diameter is <10 μ m; MgO powder purity is 99.9%, Re 2o 3purity is 99.9%.
In step (1), by Si, ZrO 2and MgO-Re 2o 3by described massfraction ratio, prepare burden, take ethanol as solvent, with Si 3n 4ball is ball-milling medium, on roll-type ball mill, mixes 4～48h, after being dried, obtains Si-ZrO 2-MgO-Re 2o 3mixed powder.
Preferably, in step (1), on roll-type ball mill, mix 24h.
Preferably, the described Si:ZrO of step (1) 2: MgO-Re 2o 3massfraction than for 80%:10%:10%, described MgO-Re 2o 3in MgO:Re 2o 3massfraction is than being 55%:45%.
Preferably, described Re 2o 3in the preferred Y of Re.
Cold isostatic compaction pressure 100～300MPa that step (2) is described, the dwell time is 1～10min.
Preferably, the cold isostatic compaction pressure 200MPa that step (2) is described, the dwell time is 5min.
Step (3) is described that two step thermal-insulating methods are: by Si-ZrO 2-MgO-Re 2o 3base substrate is put into boron nitride crucible, with the temperature rise rate of 20 ℃/min, temperature is risen to 1300～1450 ℃ and be incubated 0.5～4h, then with the temperature rise rate of 10 ℃/min, temperature is risen to 1600～1900 ℃ and be incubated 0.5～4h, the nitrogen that whole process sintering atmosphere is 1atm, obtains high heat conduction Si by pressureless sintering 3n 4pottery.
Preferably, step (3) is described that two step thermal-insulating methods are: by Si-ZrO 2-MgO-Re 2o 3base substrate is put into boron nitride crucible, heat-up rate with 20 ℃/min is raised to 1400 ℃ of insulation 2h by temperature, then the heat-up rate with 10 ℃/min is raised to 1800 ℃ of insulation 2h by temperature, and the nitrogen that whole process sintering atmosphere is 1atm, obtains high heat conduction Si by pressureless sintering 3n 4pottery.
Low cost, high heat conduction Si that the present invention also provides aforesaid method to prepare 3n 4stupalith, its relative density is higher than 95%, and hardness is 8～20GPa, and fracture toughness property is 3～8MPam 1/2, bending strength is 200～1000Mpa, thermal conductivity is 20-100Wm -1k -1.
Preferably, above-mentioned Si 3n 4the relative density 98% of pottery, hardness is 15GPa, fracture toughness property is 6MPam 1/2, flexural strength is 800Mpa, thermal conductivity is 80Wm -1k -1.
Compared with prior art, beneficial effect of the present invention:
(1) with ZrO 2as the catalyzer of Si powder nitrogenize, significantly accelerated nitriding velocity, at 1400 ℃ of nitridation times, from 8h, be significantly reduced to 1～2h;
(2) Si forming after the nitrogenize of Si powder in prior art 3n 4powder densification needs harsh processing condition, atmosphere pressures high (10atm), sintering temperature high (1900 ℃), soaking time long (12h).And the present invention is with ZrO 2-MgO-Re 2o 3for sintering aid, the Si forming after nitrogenize 3n 4powder has been realized densification under mild conditions, only needs 1atm nitrogen pressure, 1800 ℃ of insulation 1～2h.
(3), by the present invention, really realized quick, low-cost preparation Si 3n 4pottery.
Accompanying drawing explanation
Fig. 1 is the Si of the embodiment of the present invention 1 preparation 3n 4the XRD figure of pottery.
Fig. 2 is the Si of the embodiment of the present invention 1 preparation 3n 4the SEM figure of pottery.
Embodiment
Below in conjunction with Figure of description and specific embodiment, the present invention is described in further detail and completely, but limit by no means the present invention, the present invention is also not only confined to the content of following embodiment, if following used experimental technique is without specified otherwise, be the method for the existing routine of the art, the batching of using or material, if no special instructions, be by the available batching of commercial sources or material.Provide case study on implementation below:
Embodiment 1
The high heat conduction Si of low-cost preparation fast, 3n 4pottery, concrete grammar is as follows:
(1) take Si powder (particle diameter <10 μ m) is matrix material, with ZrO 2powder (particle diameter is <10 μ m), MgO powder (purity is 99.9%) and Y 2o 3powder (purity is 99.9%) is additive, according to Si powder massfraction be 80%, ZrO 2massfraction is 10%, MgO-Y 2o 3the massfraction of powder is 10% to prepare burden, wherein MgO:Y 2o 3massfraction, than for 55%:45%, be take ethanol as solvent, with Si 3n 4ball is ball-milling medium, on roll-type ball mill, mixes 24h, through batch mixing, dry after, the Si-ZrO that obtains mixing 2-MgO-Y 2o 3mixed powder.
(2) by Si-ZrO 2-MgO-Y 2o 3mixed powder is put into mould and is carried out cold isostatic compaction, cold isostatic compaction pressure 200MPa, and the dwell time is 5min.
(3) by Si-ZrO 2-MgO-Y 2o 3base substrate is put into boron nitride crucible, with the heat-up rate of 20 ℃/min, temperature is raised to 1400 ℃ of insulation 2h, and then the heat-up rate with 10 ℃/min is raised to 1800 ℃ of insulation 2h by temperature, and the nitrogen that whole process atmosphere is 1atm, obtains Si by pressureless sintering 3n 4pottery.
The Si that the present embodiment prepares 3n 4the relative density of pottery reaches 98%.Its XRD figure spectrum and microstructure are as depicted in figs. 1 and 2.Hardness is 15GPa, and fracture toughness property is 6MPam 1/2, flexural strength is 800Mpa, thermal conductivity is 80Wm -1k -1.
Embodiment 2
According to Si powder massfraction be 60%, ZrO 2powder massfraction is 20%, MgO-Yb 2o 3powder massfraction is 20% to prepare burden, wherein MgO:Yb 2o 3massfraction, than for 60%:40%, is prepared Si according to embodiment 1 method 3n 4first pottery, be wherein warming up to 1375 ℃ of insulation 4h, is then warming up to 1700 ℃ of insulation 2h.The relative density of preparing gained stupalith is 99%, and the hardness of material is 16GPa, and fracture toughness property is 6.5MPam 1/2, flexural strength is 750Mpa, thermal conductivity is 50Wm -1k -1.
Embodiment 3
According to Si powder massfraction be 70%, ZrO 2powder massfraction is 20%, MgO-La 2o 3powder massfraction is 10% to prepare burden, wherein MgO:La 2o 3massfraction, than for 75%:25%, is prepared Si according to embodiment 1 method 3n 4first pottery, be wherein warming up to 1375 ℃ of insulation 4h, is then warming up to 1800 ℃ of insulation 2h.The relative density of preparing gained stupalith is 98%, and the hardness of material is 16GPa, and fracture toughness property is 7MPam 1/2, flexural strength is 600Mpa, thermal conductivity is 60Wm -1k -1.
Embodiment 4
According to Si powder massfraction be 70%, ZrO 2powder massfraction is 15%, MgO-Lu 2o 3powder massfraction is 15% to prepare burden, wherein MgO:Lu 2o 3massfraction, than for 55%:45%, is prepared Si according to embodiment 1 method 3n 4first pottery, be wherein warming up to 1400 ℃ of insulation 1h, is then warming up to 1750 ℃ of insulation 4h.The relative density of preparing gained stupalith is 99%, and the hardness of material is 18GPa, and fracture toughness property is 7.5MPam 1/2, flexural strength is 700Mpa, thermal conductivity is 75Wm -1k -1.
Embodiment 5
According to Si powder massfraction be 85%, ZrO 2powder massfraction is 10%, MgO-Y 2o 3powder massfraction is 5% to prepare burden, wherein MgO:Y 2o 3massfraction, than for 65%:35%, is prepared Si according to embodiment 1 method 3n 4first pottery, be wherein warming up to 1400 ℃ of insulation 2h, is then warming up to 1800 ℃ of insulation 4h.The relative density of preparing gained stupalith is 97%, and the hardness of material is 13GPa, and fracture toughness property is 5.5MPam 1/2, flexural strength is 680Mpa, thermal conductivity is 70Wm -1k -1.
Embodiment 6
According to Si powder massfraction be 85%, ZrO 2powder massfraction is 7.5%, MgO-Nd 2o 3powder massfraction is 7.5% to prepare burden, wherein MgO:Nd 2o 3massfraction, than for 50%:50%, is prepared Si according to embodiment 1 method 3n 4first pottery, be wherein warming up to 1400 ℃ of insulation 2h, is then warming up to 1800 ℃ of insulation 4h.The relative density of preparing gained stupalith is 98%, and the hardness of material is 15GPa, and fracture toughness property is 5.5MPam 1/2, flexural strength is 800Mpa, thermal conductivity is 75Wm -1k -1.
Embodiment 7
According to Si powder massfraction be 90%, ZrO 2powder massfraction is 5%, MgO-Gd 2o 3powder massfraction is 5% to prepare burden, wherein MgO:Gd 2o 3massfraction, than for 40%:60%, is prepared Si according to embodiment 1 method 3n 4first pottery, be wherein warming up to 1400 ℃ of insulation 4h, is then warming up to 1900 ℃ of insulation 2h.The relative density of preparing gained stupalith is 97%, and the hardness of material is 15GPa, and fracture toughness property is 6.8MPam 1/2, flexural strength is 780Mpa, thermal conductivity is 60Wm -1k -1.
Embodiment 8
According to Si powder massfraction be 98%, ZrO 2powder massfraction is 1%, MgO-Y 2o 3powder massfraction is 1% to prepare burden, wherein MgO:Y 2o 3massfraction, than for 90%:10%, is prepared Si according to embodiment 1 method 3n 4first pottery, be wherein warming up to 1450 ℃ of insulation 4h, is then warming up to 1900 ℃ of insulation 4h.The relative density of preparing gained stupalith is 95%, and the hardness of material is 12GPa, and fracture toughness property is 4.5MPam 1/2, flexural strength is 350Mpa, thermal conductivity is 40Wm -1k -1.

Claims (10)

  1. A low cost, prepare high heat conduction Si fast 3n 4the method of pottery, is characterized in that comprising the steps:
    (1) take Si powder as raw material, with ZrO 2powder is nitrided catalyst, with ZrO 2-MgO-Re 2o 3for sintering aid, Re wherein 2o 3for rare earth oxide, Re is Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or Lu; Press Si:ZrO 2: MgO-Re 2o 3massfraction than be 60～98%:1～20%:1～20% proportioning through batch mixing, dry after, obtain Si-ZrO 2-MgO-Re 2o 3mixed powder; Described MgO-Re 2o 3in MgO:Re 2o 3massfraction ratio is 1～99%:99～1%;
    (2) by Si-ZrO 2-MgO-Re 2o 3mixed powder is put into mould, by cold isostatic compaction, obtains base substrate;
    (3) by Si-ZrO 2-MgO-Re 2o 3base substrate is prepared high heat conduction Si by two step thermal-insulating method pressureless sinterings 3n 4pottery.
  2. 2. method according to claim 1, is characterized in that: the described Si powder purity of step (1) is 95～100%, and particle diameter is <10 μ m; ZrO 2purity is 98～100%, and particle diameter is <10 μ m; MgO powder purity is 99.9%, Re 2o 3purity is 99.9%.
  3. 3. method according to claim 1, is characterized in that: in step (1), by Si, ZrO 2and MgO-Re 2o 3by described massfraction ratio, prepare burden, take ethanol as solvent, with Si 3n 4ball is ball-milling medium, on roll-type ball mill, mixes 4～48h, after being dried, obtains Si-ZrO 2-MgO-Re 2o 3mixed powder.
  4. 4. method according to claim 3, is characterized in that: in step (1), on roll-type ball mill, mix 24h.
  5. 5. method according to claim 1, is characterized in that: the Si:ZrO that step (1) is described 2: MgO-Re 2o 3massfraction than for 80%:10%:10%, described MgO-Re 2o 3in MgO:Re 2o 3massfraction is than being 55%:45%.
  6. 6. method according to claim 1, is characterized in that: cold isostatic compaction pressure 100～300MPa that step (2) is described, the dwell time is 1～10min.
  7. 7. method according to claim 6, is characterized in that: the cold isostatic compaction pressure 200MPa that step (2) is described, the dwell time is 5min.
  8. 8. method according to claim 1, is characterized in that: step (3) is described that two step thermal-insulating methods are: by Si-ZrO 2-MgO-Re 2o 3base substrate is put into boron nitride crucible, with the temperature rise rate of 20 ℃/min, temperature is risen to 1300～1450 ℃ and be incubated 0.5～4h, then with the temperature rise rate of 10 ℃/min, temperature is risen to 1600～1900 ℃ and be incubated 0.5～4h, the nitrogen that whole process sintering atmosphere is 1atm, obtains high heat conduction Si by pressureless sintering 3n 4pottery.
  9. 9. method according to claim 8, is characterized in that: step (3) is described that two step thermal-insulating methods are: by Si-ZrO 2-MgO-Re 2o 3base substrate is put into boron nitride crucible, heat-up rate with 20 ℃/min is raised to 1400 ℃ of insulation 2h by temperature, then the heat-up rate with 10 ℃/min is raised to 1800 ℃ of insulation 2h by temperature, and the nitrogen that whole process sintering atmosphere is 1atm, obtains high heat conduction Si by pressureless sintering 3n 4pottery.
  10. 10. the high heat conduction Si preparing according to method described in claim 1 to 9 3n 4pottery, is characterized in that: described Si 3n 4the relative density of pottery is greater than 95%, and hardness is 8～20GPa, and fracture toughness property is 3～8MPam 1/2, bending strength is 200～1000Mpa, thermal conductivity is 20-100WmK -1.
CN201410318834.7A 2014-07-04 2014-07-04 Method for rapidly preparing high heat conduction Si3N4 ceramic with low cost Pending CN104163633A (en)

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CN104909765A (en) * 2015-06-01 2015-09-16 广东工业大学 Method for rapidly preparing high-performance Si3N4 ceramic ball at low cost
CN105819867A (en) * 2016-04-15 2016-08-03 广东工业大学 Electrosparking and mechanical processing Si3N4-ZrSi2-BN composite ceramic material and preparation method
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CN108863395A (en) * 2017-05-12 2018-11-23 中国科学院上海硅酸盐研究所 A kind of high heat conductance, high strength silicon nitride ceramic material and preparation method thereof
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CN104609865A (en) * 2015-02-09 2015-05-13 广东工业大学 Preparation method of silicon nitride-based conductive ceramic and molding method of silicon nitride-based conductive ceramic cutting tool
CN104909765A (en) * 2015-06-01 2015-09-16 广东工业大学 Method for rapidly preparing high-performance Si3N4 ceramic ball at low cost
CN105819867A (en) * 2016-04-15 2016-08-03 广东工业大学 Electrosparking and mechanical processing Si3N4-ZrSi2-BN composite ceramic material and preparation method
CN105819867B (en) * 2016-04-15 2018-10-02 广东工业大学 It is a kind of can electrical discharge machining and mechanical processing Si3N4-ZrSi2- BN diphase ceramic materials and preparation method
CN106904977A (en) * 2017-03-20 2017-06-30 广东工业大学 A kind of method that two-step sintering method prepares the tough Si3N4 ceramic materials of table hard-core
CN106904977B (en) * 2017-03-20 2020-09-25 广东工业大学 Preparation of surface hard and core tough Si by two-step sintering method3N4Method for producing ceramic material
CN108863395A (en) * 2017-05-12 2018-11-23 中国科学院上海硅酸盐研究所 A kind of high heat conductance, high strength silicon nitride ceramic material and preparation method thereof
CN108863395B (en) * 2017-05-12 2021-01-12 中国科学院上海硅酸盐研究所 High-thermal-conductivity and high-strength silicon nitride ceramic material and preparation method thereof
WO2019134354A1 (en) * 2018-01-05 2019-07-11 广东工业大学 Si3n4 gradient material and preparation method thereof
CN109400176A (en) * 2018-09-27 2019-03-01 广东工业大学 A kind of high-performance silicon nitride ceramics and its preparation method and application
CN111253162A (en) * 2019-02-22 2020-06-09 中国科学院上海硅酸盐研究所苏州研究院 Method for preparing high-strength high-toughness high-thermal-conductivity silicon nitride ceramic
CN110550957A (en) * 2019-08-21 2019-12-10 广东工业大学 In-situ synthesized silicon nitride/zirconium boride composite ceramic and preparation method and application thereof

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