CN104098336A - Method for preparing high-thermal-conductivity high-strength silicon nitride ceramic - Google Patents

Method for preparing high-thermal-conductivity high-strength silicon nitride ceramic Download PDF

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Publication number
CN104098336A
CN104098336A CN201310129987.2A CN201310129987A CN104098336A CN 104098336 A CN104098336 A CN 104098336A CN 201310129987 A CN201310129987 A CN 201310129987A CN 104098336 A CN104098336 A CN 104098336A
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silicon nitride
sintering aid
heat conductance
high strength
strength silicon
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林森
曾宇平
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

A disclosed method for preparing high-thermal-conductivity high-strength silicon nitride ceramic comprises: uniformly mixing alpha-Si3N4 powder and a sinter aid according to a ratio, and then successively performing dry-pressing forming and isostatic pressing processing, so as to prepare a blank, wherein the sintering aid is a mixture employing Yb2O3 as a main sintering aid and employing at least one of Y2O3, Lu2O3, Nd2O3, Er2O3 and MgO as an auxiliary sintering aid; and embedding the prepared blank in Si3N4 powder, and performing gas pressure sintering at 1650-1850 DEG C in inert atmosphere, and then cooling to room temperature along with a furnace. The silicon nitride ceramic material prepared by using the method has high thermal conductivity and high strength, and is capable of satisfying application requirements of silicon nitride ceramic to fields such as high-speed circuits and large-power devices. The preparation method is simple in technology and low in cost, is suitable of large-scale production, and has practical value.

Description

A kind of method of preparing high heat conductance, high strength silicon nitride pottery
Technical field
The preparation method who the present invention relates to a kind of high heat conductance, high strength silicon nitride pottery, belongs to non-oxide ceramics preparing technical field.
Background technology
Along with developing rapidly and the miniaturization of electronic component of large-scale integrated circuit, to having higher requirement as the ceramic substrate of unicircuit mainstay.At the applied environment of some special harshness, not only require this ceramic substrate to there is good heat conductivility, and should there is outstanding mechanical strength.The Ceramic Substrate Material extensively adopting is at present mainly Al 2o 3, but Al 2o 3lower (the 20Wm of pottery thermal conductivity -1k -1), large, the linear expansivity of specific inductivity and with the shortcoming such as the linear expansivity of silicon cell differs greatly, more and more cannot meet more accurate industry and commercial use, therefore positive R and D in recent years replace other stupalith of alumina substrate, as AlN, BeO, SiC, Si 3n 4pottery etc.
Wherein, BeO pottery, AlN are ceramic, SiC is ceramic all has a very high thermal conductivity, and their thermal conductivity is respectively 300Wm -1k -1, 260Wm -1k -1, 270Wm -1k -1, but when practical application equal defectiveness, as: BeO has severe toxicity, and long-term suction can cause that chronic berylliosis of lung is sick, and the sintering cost of pure BeO pottery is also higher; The mechanical property of AlN pottery is poor, is unfavorable for water base processing, and the differing greatly of its linear expansivity and silicon cell; SiC ceramic electrical insulation degree is low, and dielectric loss is large, and high frequency characteristics is poor.Therefore, these three kinds of potteries have all been subject to certain limitation in application.
Nineteen ninety-five, the people such as Haggerty just predict Si 3n 4pottery thermal conductivity can reach 200-320Wm -1k -1, and Si 3n 4pottery is one of advanced ceramics material that intensity is the highest, in the situation that heat dissipation capacity is identical, and Si 3n 4even if ceramic substrate very thin thickness also can meet the requirement of intensity and heat radiation, so Si 3n 4the thermal property of pottery is also more and more paid attention to by people.In addition as substrate material, compare Si with AlN material 3n 4pottery also has good oxidation-resistance, is convenient under aqueous conditions preparation and processes, and so not only can reduce manufacturing cost but also can avoid the environmental pollution of using organic reagent to bring; In addition, Si 3n 4pottery thermal expansivity is low, is only 3.2 * 10 -6/ ℃, be about Al 2o 31/3, and approach with single crystalline Si, can form that good heat is mated with components and parts and electrical insulating property good, nontoxic etc.The thermal conductivity of high potentiality and excellent mechanical property make Si 3n 4pottery is considered to heat radiation and the packaged material of a kind of very promising high speed circuit and high power device.
Si 3n 4the thermal conductivity of pottery is mainly subject to the impact of phon scattering mean free path, and its major influence factors is β-Si 3n 4defect, grain-size and oxygen level etc., wherein topmost influence factor or the oxygen level of lattice in phase content, Grain-Boundary Phase composition and content thereof, lattice.Silicon nitride is that the compound of strong covalent bond and the self-diffusion coefficient of silicon nitride are low, thereby solid state sintering difficulty, must add sintering aid and reach liquid phase sintering and realize densification.
Scientist is attempting using different types of sintering aid and sintering method to prepare high heat conductance, high-intensity silicon nitride ceramics both at home and abroad, and the researchist of Japan is by adding 5mol%Y 2o 3as sintering aid reaction sintering 4h under 0.1MPa nitrogen atmosphere, 1400 ℃ of conditions, then under 1MPa nitrogen atmosphere, 1900 ℃ of conditions, be incubated 60h with 2mol%MgO, finally, with the annealing of 0.2 ℃/min speed, obtain thermal conductivity up to 177Wm -1k -1, the silicon nitride ceramics that three-point bending strength is 460MPa, referring to [Adv.Mater., 23 (2011), 4563-4567].Although silicon nitride ceramics thermal conductivity prepared by this method is very high, prepare consuming time, highly to annealing rate requirement, and the silicon nitride ceramics intensity of preparing is less.Domestic researchist is by adding nitrogen magnesium silicide and yttrium oxide under the hot pressing condition of 20MPa, and 1750 ℃ of insulation 1h obtain thermal conductivity up to 129Wm -1k -1silicon nitride ceramics, referring to [Adv Eng.Ceram.Compos., 18 (2011), 202017].But in this method, nitrogen magnesium silicide used needs self-control, and cost is higher.
Summary of the invention
The problems referred to above and the defect that for prior art, exist, the object of this invention is to provide a kind of method of preparing high heat conductance, high strength silicon nitride pottery, to meet silicon nitride ceramics at the application requiring in high speed circuit and high power device field.
For achieving the above object, the technical solution used in the present invention is as follows:
A method of preparing high heat conductance, high strength silicon nitride pottery, comprises the steps:
A) by α-Si 3n 4powder and sintering aid mix in proportion, and then carry out successively dry-pressing formed and wait static pressure to process, and make base substrate; Described sintering aid is with Yb 2o 3be main sintering aid, with Y 2o 3, Lu 2o 3, Nd 2o 3, Er 2o 3, at least one mixture that is auxiliary sintering aid in MgO;
B) base substrate step a) being made is imbedded Si 3n 4in powder, under inert atmosphere, carry out gas pressure sintering in 1650 ℃～1850 ℃, then cool to room temperature with the furnace.
As a kind of preferred version, α-Si 3n 4the ratio of powder and sintering aid is 86mol%:14mol%～99mol%:1mol%, more preferably 90mol%:10mol%.
As a kind of preferred version, the mol ratio of main sintering aid and auxiliary sintering aid is 1:1～3:1, more preferably 1:1.
As a kind of preferred version, described sintering aid is Yb 2o 3with the MgO mixture that 1:1 forms in molar ratio.
As a kind of preferred version, described α-Si 3n 4the median size of powder is 0.5 μ m, and wherein the content of α phase is greater than 95wt%.
As a kind of preferred version, described Yb 2o 3the purity of (ytterbium oxide) is greater than 99%, and median size is 5 μ m.
As a kind of preferred version, carrying out dry-pressing formed pressure is 10～25MPa.
As a kind of preferred version, the pressure that waits static pressure to process is 100～300MPa.
As further preferred version, the described static pressure processing selecting isostatic cool pressing mode that waits.
As a kind of preferred version, the nitrogen atmosphere that described inert atmosphere is 0.4～2Mpa.
The present invention is by selecting Yb 2o 3as main sintering aid, Y 2o 3, Lu 2o 3, Nd 2o 3, Er 2o 3, at least one in MgO be as auxiliary sintering aid, and adopts gas pressure sintering method to prepare silicon nitride ceramics simultaneously, than with prior art, there is following significance effect:
1) Yb 2o 3as heavy rare earth element, can effectively absorb the lattice oxygen in silicon nitride ceramics, be conducive to improve thermal conductivity, and form high containing Yb Grain-Boundary Phase fusing point, have stable high-temperature performance;
2) prepared silicon nitride ceramic material has high heat conductance and high strength, and thermal conductivity can reach 84Wm -1k -1, three-point bending resistance intensity can reach 966MPa, and fracture toughness property can reach 6.29Mpam 1/2, can meet silicon nitride ceramics at the application requiring in high speed circuit and high power device field;
3) preparation technology of the present invention is simple, and cost is low, is applicable to large-scale production, has practical value.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the embodiment of the present invention 1～3 prepared silicon nitride ceramics;
Fig. 2 is the cross-section morphology figure of the embodiment of the present invention 1～6 prepared silicon nitride ceramics.
Embodiment
Below in conjunction with specific embodiments and the drawings, further set forth the present invention.
Embodiment 1
With 5mol%Yb 2o 3and 5mol%MgO is as sintering aid, with α-Si of 90mol% 3n 4powder makes to mix through ball milling; Then dry-pressing formed under 20Mpa pressure, then under 200MPa pressure, wait static pressure to process; Reinstall plumbago crucible, imbed Si 3n 4in powder, under 0.6MPa nitrogen atmosphere, carry out gas pressure sintering 4 hours in 1850 ℃; After sintering finishes, make sample cool to room temperature with the furnace.
The thermal conductivity of the silicon nitride ceramics being made by the present embodiment is 82W/ (mK), and three-point bending resistance intensity is 966MPa, and fracture toughness property is 6.29MPam 1/2.The XRD figure of this stupalith is as shown in Fig. 1 (a), and its fracture apperance figure is as shown in Fig. 2 (a).
Embodiment 2
With 5mol%Yb 2o 3and 5mol%MgO is as sintering aid, with α-Si of 90mol% 3n 4powder makes to mix through ball milling; Then dry-pressing formed under 20Mpa pressure, then under 200MPa pressure, wait static pressure to process; Reinstall plumbago crucible, imbed Si 3n 4in powder, under 0.6MPa nitrogen atmosphere, carry out gas pressure sintering 4 hours in 1800 ℃; After sintering finishes, make sample cool to room temperature with the furnace.
The thermal conductivity of the silicon nitride ceramics being made by the present embodiment is 64W/ (mK), and three-point bending resistance intensity is 810MPa, and fracture toughness property is 5.93MPam 1/2.The XRD figure of this stupalith is as shown in Fig. 1 (b), and its fracture apperance figure is as shown in Fig. 2 (b).
Embodiment 3
With 5mol%Yb 2o 3and 5mol%MgO is as sintering aid, with α-Si of 90mol% 3n 4powder makes to mix through ball milling; Then dry-pressing formed under 20Mpa pressure, then under 200MPa pressure, wait static pressure to process; Reinstall plumbago crucible, imbed Si 3n 4in powder, under 0.6MPa nitrogen atmosphere, carry out gas pressure sintering 4 hours in 1750 ℃; After sintering finishes, make sample cool to room temperature with the furnace.
The thermal conductivity of the silicon nitride ceramics being made by the present embodiment is 57W/ (mK), and three-point bending resistance intensity is 752MPa, and fracture toughness property is 4.91MPam 1/2.The XRD figure of this stupalith is as shown in Fig. 1 (c), and its fracture apperance figure is as shown in Fig. 2 (c).
Embodiment 4
With 3mol%Yb 2o 3and 3mol%MgO is as sintering aid, with α-Si of 94mol% 3n 4powder makes to mix through ball milling; Then dry-pressing formed under 20Mpa pressure, then under 200MPa pressure, wait static pressure to process; Reinstall plumbago crucible, imbed Si 3n 4in powder, under 0.6MPa nitrogen atmosphere, carry out gas pressure sintering 4 hours in 1850 ℃; After sintering finishes, make sample cool to room temperature with the furnace.
The thermal conductivity of the silicon nitride ceramics being made by the present embodiment is 65W/ (mK), and three-point bending resistance intensity is 911MPa, and fracture toughness property is 5.76MPam 1/2.The fracture apperance figure of this stupalith is as shown in Fig. 2 (d).
Embodiment 5
With 4mol%Yb 2o 3and 4mol%MgO is as sintering aid, with α-Si of 92mol% 3n 4powder makes to mix through ball milling; Then dry-pressing formed under 20Mpa pressure, then under 200MPa pressure, wait static pressure to process; Reinstall plumbago crucible, imbed Si 3n 4in powder, under 0.6MPa nitrogen atmosphere, carry out gas pressure sintering 4 hours in 1850 ℃; After sintering finishes, make sample cool to room temperature with the furnace.
The thermal conductivity of the silicon nitride ceramics being made by the present embodiment is 79W/ (mK), and three-point bending resistance intensity is 906MPa, and fracture toughness property is 5.94MPam 1/2.The fracture apperance figure of this stupalith is as shown in Fig. 2 (e).
Embodiment 6
With 7mol%Yb 2o 3and 7mol%MgO is as sintering aid, with α-Si of 86mol% 3n 4powder makes to mix through ball milling; Then dry-pressing formed under 20Mpa pressure, then under 200MPa pressure, wait static pressure to process; Reinstall plumbago crucible, imbed Si 3n 4in powder, under 0.6MPa nitrogen atmosphere, carry out gas pressure sintering 4 hours in 1850 ℃; After sintering finishes, make sample cool to room temperature with the furnace.
The thermal conductivity of the silicon nitride ceramics being made by the present embodiment is 84W/ (mK), and three-point bending resistance intensity is 947MPa, and fracture toughness property is 6.27MPam 1/2.The fracture apperance figure of this stupalith is as shown in Fig. 2 (f).
Visible in sum: the present invention is by selecting Yb 2o 3as main sintering aid, Y 2o 3, Lu 2o 3, Nd 2o 3, Er 2o 3, at least one in MgO be as auxiliary sintering aid, and adopts gas pressure sintering method simultaneously, can make and have high heat conductance and high-intensity silicon nitride ceramic material, thermal conductivity can reach 84Wm -1k -1, three-point bending resistance intensity can reach 966MP a, fracture toughness property can reach 6.29Mpam 1/2, can meet silicon nitride ceramics at the application requiring in high speed circuit and high power device field; And preparation technology of the present invention is simple, cost is low, is applicable to large-scale production; There is practical value.
Finally be necessary described herein: above embodiment is only for being described in more detail technical scheme of the present invention; 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.

Claims (10)

1. a method of preparing high heat conductance, high strength silicon nitride pottery, is characterized in that, comprises the steps:
A) by α-Si 3n 4powder and sintering aid mix in proportion, and then carry out successively dry-pressing formed and wait static pressure to process, and make base substrate; Described sintering aid is with Yb 2o 3be main sintering aid, with Y 2o 3, Lu 2o 3, Nd 2o 3, Er 2o 3, at least one mixture that is auxiliary sintering aid in MgO;
B) base substrate step a) being made is imbedded Si 3n 4in powder, under inert atmosphere, carry out gas pressure sintering in 1650 ℃～1850 ℃, then cool to room temperature with the furnace.
2. the method for preparing high heat conductance, high strength silicon nitride pottery according to claim 1, is characterized in that: α-Si 3n 4the ratio of powder and sintering aid is 86mol%:14mol%～99mol%:1mol%.
3. the method for preparing high heat conductance, high strength silicon nitride pottery according to claim 1, is characterized in that: in described sintering aid, the mol ratio of main sintering aid and auxiliary sintering aid is 1:1～3:1.
4. the method for preparing high heat conductance, high strength silicon nitride pottery according to claim 3, is characterized in that: described sintering aid is Yb 2o 3with the MgO mixture that 1:1 forms in molar ratio.
5. the method for preparing high heat conductance, high strength silicon nitride pottery according to claim 1, is characterized in that: described α-Si 3n 4the median size of powder is 0.5 μ m, and wherein the content of α phase is greater than 95wt%.
6. the method for preparing high heat conductance, high strength silicon nitride pottery according to claim 1, is characterized in that: described Yb 2o 3purity be greater than 99%, median size is 5 μ m.
7. the method for preparing high heat conductance, high strength silicon nitride pottery according to claim 1, is characterized in that: carrying out dry-pressing formed pressure is 10～25MPa.
8. the method for preparing high heat conductance, high strength silicon nitride pottery according to claim 1, is characterized in that: the pressure that waits static pressure to process is 100～300MPa.
9. the method for preparing high heat conductance, high strength silicon nitride pottery according to claim 1, is characterized in that: the described static pressure processing selecting isostatic cool pressing mode that waits.
10. the method for preparing high heat conductance, high strength silicon nitride pottery according to claim 1, is characterized in that: the nitrogen atmosphere that described inert atmosphere is 0.4～2Mpa.
CN201310129987.2A 2013-04-15 2013-04-15 Method for preparing high-thermal-conductivity high-strength silicon nitride ceramic Pending CN104098336A (en)

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CN106631041A (en) * 2017-01-06 2017-05-10 张海波 Production and manufacturing technology of silicon nitride ceramic tiny component
CN106747469A (en) * 2016-12-27 2017-05-31 郑州源冉生物技术有限公司 A kind of high-performance silicon nitride ceramic material and preparation method thereof
CN108585881A (en) * 2018-06-14 2018-09-28 哈尔滨工业大学 A kind of high heat conductivity silicon nitride ceramics and preparation method thereof
CN108666233A (en) * 2017-03-31 2018-10-16 上海新昇半导体科技有限公司 A kind of chip preparation method and chip can be used as catch or control wafer
CN108727035A (en) * 2017-04-24 2018-11-02 京瓷株式会社 Ceramic wafer and electronic device
CN108863397A (en) * 2018-07-13 2018-11-23 威海圆环先进陶瓷股份有限公司 A kind of technique preparing SiN ceramic with high heat conductivity crucible
CN109694253A (en) * 2017-10-24 2019-04-30 中国科学院上海硅酸盐研究所 A method of normal pressure-sintered silicon nitride ceramics thermal conductivity is improved by carbon doping
CN109890550A (en) * 2016-08-09 2019-06-14 国立大学法人大阪大学 Silicon nitride sinter friction stir welding tools component and the friction stir weld device for using the tool component
CN110423122A (en) * 2019-08-06 2019-11-08 中国科学院上海硅酸盐研究所 A kind of low-loss, high thermal conductivity silicon nitride ceramics preparation method
CN110948711A (en) * 2019-08-01 2020-04-03 常熟华融太阳能新型材料有限公司 Preparation method of IGBT ceramic substrate
CN111362704A (en) * 2020-03-19 2020-07-03 西安澳秦新材料有限公司 High-thermal-conductivity silicon nitride ceramic and preparation method thereof
CN113929468A (en) * 2021-05-20 2022-01-14 中国科学院上海硅酸盐研究所 Pink silicon nitride ceramic and preparation method and application thereof

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Cited By (17)

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CN106187216A (en) * 2016-07-13 2016-12-07 南通中兴多元复合钢管有限公司 The tri compound sintering aid of highly heat-conductive carbon/ceramic ceramic chip is prepared for production
CN109890550A (en) * 2016-08-09 2019-06-14 国立大学法人大阪大学 Silicon nitride sinter friction stir welding tools component and the friction stir weld device for using the tool component
CN109890550B (en) * 2016-08-09 2022-01-04 国立大学法人大阪大学 Friction stir welding tool member made of silicon nitride sintered body and friction stir welding device using same
CN106747469A (en) * 2016-12-27 2017-05-31 郑州源冉生物技术有限公司 A kind of high-performance silicon nitride ceramic material and preparation method thereof
CN106631041A (en) * 2017-01-06 2017-05-10 张海波 Production and manufacturing technology of silicon nitride ceramic tiny component
CN108666233A (en) * 2017-03-31 2018-10-16 上海新昇半导体科技有限公司 A kind of chip preparation method and chip can be used as catch or control wafer
CN108666233B (en) * 2017-03-31 2021-02-05 上海新昇半导体科技有限公司 Wafer preparation method capable of being used as separation blade or control blade and wafer
CN108727035A (en) * 2017-04-24 2018-11-02 京瓷株式会社 Ceramic wafer and electronic device
CN109694253A (en) * 2017-10-24 2019-04-30 中国科学院上海硅酸盐研究所 A method of normal pressure-sintered silicon nitride ceramics thermal conductivity is improved by carbon doping
CN109694253B (en) * 2017-10-24 2020-08-18 中国科学院上海硅酸盐研究所 Method for improving thermal conductivity of normal pressure sintered silicon nitride ceramic by carbon doping
CN108585881A (en) * 2018-06-14 2018-09-28 哈尔滨工业大学 A kind of high heat conductivity silicon nitride ceramics and preparation method thereof
CN108863397A (en) * 2018-07-13 2018-11-23 威海圆环先进陶瓷股份有限公司 A kind of technique preparing SiN ceramic with high heat conductivity crucible
CN110948711A (en) * 2019-08-01 2020-04-03 常熟华融太阳能新型材料有限公司 Preparation method of IGBT ceramic substrate
CN110423122A (en) * 2019-08-06 2019-11-08 中国科学院上海硅酸盐研究所 A kind of low-loss, high thermal conductivity silicon nitride ceramics preparation method
CN110423122B (en) * 2019-08-06 2021-08-06 中国科学院上海硅酸盐研究所 Preparation method of low-loss and high-thermal-conductivity silicon nitride ceramic
CN111362704A (en) * 2020-03-19 2020-07-03 西安澳秦新材料有限公司 High-thermal-conductivity silicon nitride ceramic and preparation method thereof
CN113929468A (en) * 2021-05-20 2022-01-14 中国科学院上海硅酸盐研究所 Pink silicon nitride ceramic and preparation method and application thereof

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Application publication date: 20141015