CN1203898A - Low temp. sintering of aluminum nitride ceramics - Google Patents
Low temp. sintering of aluminum nitride ceramics Download PDFInfo
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- CN1203898A CN1203898A CN 98110938 CN98110938A CN1203898A CN 1203898 A CN1203898 A CN 1203898A CN 98110938 CN98110938 CN 98110938 CN 98110938 A CN98110938 A CN 98110938A CN 1203898 A CN1203898 A CN 1203898A
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- 238000005245 sintering Methods 0.000 title claims abstract description 48
- 239000000919 ceramic Substances 0.000 title claims abstract description 23
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title description 11
- 239000000843 powder Substances 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000000654 additive Substances 0.000 claims abstract description 29
- 230000000996 additive effect Effects 0.000 claims abstract description 23
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 6
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 5
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 5
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 59
- 229910017083 AlN Inorganic materials 0.000 claims description 58
- 238000009766 low-temperature sintering Methods 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 16
- 239000012298 atmosphere Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 238000003892 spreading Methods 0.000 claims description 9
- 230000007480 spreading Effects 0.000 claims description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 8
- 239000011575 calcium Substances 0.000 claims description 8
- 229910052744 lithium Inorganic materials 0.000 claims description 8
- 229910052727 yttrium Inorganic materials 0.000 claims description 8
- 229910052791 calcium Inorganic materials 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- 238000001272 pressureless sintering Methods 0.000 claims description 6
- 239000010953 base metal Substances 0.000 claims description 4
- 238000001308 synthesis method Methods 0.000 claims description 4
- 229910052702 rhenium Inorganic materials 0.000 claims description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 229910014813 CaC2 Inorganic materials 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 8
- 235000015895 biscuits Nutrition 0.000 description 8
- 239000010439 graphite Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000011800 void material Substances 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 238000003825 pressing Methods 0.000 description 6
- 230000000630 rising effect Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- 241000209456 Plumbago Species 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000000462 isostatic pressing Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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Abstract
The low-temp. sintering method of AlN ceramic is characterized by that (1): the initial AlN powder material adopted by said invention is the powder material obtained by general carbontherma reduction method or high-temp. self-extending method; (2) the selected additive material is technical-grade CaC2 and monovalent metal oxide and rare earth oxide; (3).sintering temp. is less than 1600 deg.C. The AlN ceramic prepared by said invented method has good performance price ratio, heat conductivity is 130-230 W.m(-1).K(-1), dielectric loss is 1 X 10 to the power 16 ohm.cm.
Description
The present invention relates to the low-temperature sintering of aluminium nitride (AlN) pottery, or rather, be lower than under 1600 ℃ of conditions, adopt polynary cheap additive, make the aluminium nitride ceramics densified sintering product and have high thermal conductivity and excellent resistivity in temperature.Belong to the nitride ceramics field.
Aluminium nitride ceramics has the excellent comprehensive performance, is the advanced ceramics of new generation that is subjected to extensive concern over past ten years.Especially its good heat conductivity, hot expansibility and silicon chip are approaching, nontoxic, the volume resistance height, the intensity height, its over-all properties is better than aluminum oxide, beryllium oxide, is the ideal material of LSI and VLSI substrate and encapsulation, also can be used for high power transistor, switch power supply substrate, electrical device, application prospect is very wide.
The research of high thermal-conductivity aluminum nitride ceramics has obtained bigger progress over past ten years, but its application presents relative stagnant condition, and its reason is that the aluminium nitride ceramics product price is high.Current important tendency is to be devoted to improve the ratio of performance to price of high-thermal conductivity A 1 N product, and its low temperature sintering is most important trend.With before carry out agglomerating technology and compare at 1800～1900 ℃, will reduce the sintering cost greatly near sintering temperature is reduced to 1600 ℃, for example as can adopt continuous fritting furnace, significantly cut down the consumption of energy etc., thereby significantly improve the AlN competitiveness of product; Its favourable influence to product properties then has been to slow down in the sintering process AlN powder top layer oxygen to the diffusion of AlN crystal grain inside, is beneficial to the heat conductivility that improves the AlN pottery, and can promote the deoxygenation effect of follow-up heat treatment process.
Because AlN belongs to dystectic strong covalent bond compound, be difficult to densified sintering product when additive-free, investigators mainly take following two kinds of operational paths to reach low sintering purpose: (1) adopts higher submicron order and the nano level AlN material powder of sintering activity; (2) add a fairly large number of sinter additives, form liquid phase at a lower temperature, finish the densification of AlN pottery by liquid phase sintering mechanism.But the shortcoming of last method is the powder cost further to be increased; The latter then often forms lower thermal conductivity second phase of parcel AlN crystal grain, and the heat conductivility of aluminium nitride ceramics is descended.
The present invention aims to provide a kind of low-temperature sintering method of high heat conductance AlN pottery, makes product have the good ratio of performance to price.
Specifically, the present invention adopts common aluminium nitride powder and conventional cheap additives to carry out the low-temperature sintering of aluminium nitride ceramics, and temperature is 1500～1600 ℃, and for achieving the above object, low-temperature sintering method provided by the invention is characterized in that:
(1) aluminium nitride powder with the preparation of carbothermic method and self-propagating high-temperature synthesis method is a starting raw material, the former median size 2 μ m, and oxygen level is 0.6wt%; Latter's median size 3～4 μ m, oxygen level is 0.4wt%;
(2) the sintering additive main component of selecting for use is cheap technical grade carbide of calcium (CaC
2), utilize itself and the easy reaction properties of water electrode, be expected to reduce significantly in auxiliary material and the environment moisture to the detrimentally affect of AlN, effective control oxygen level in whole process of preparation.In addition, other additives that use are monovalent base metal oxide and Y
2O
3Deng rare earth oxide, add-on is 2～4wt%CaC
2Or x%CaC
2+ y%R
2O (x is 2～4, and y is 1～3); Or x%CaC
2+ y%R
2O+z%Re
2O
3(x is 2～4, and y is 1～3, and z is 1～3, is weight ratio), R
2O is K
2O, Li
2Monovalent base metal oxides such as O, Re
2O
3Be Y
2O
3, La
2O
3, Pr
2O
3, Nd
2O
3, 5m
2O
3, Gd
2O
3, Tb
2O
3, Dy
2O
3, Ho
2O
3, Er
2O
3, Er
2O
3, Yb
2O
3Or Lu
2O
3Among any.The quantity of other additives can maintain lower level behind the adding carbide of calcium, helps the eliminating of sintered compact oxygen impurities, and keeps the closely contact mutually of aluminum nitride grain; It is 4～10wt% that additive adds total amount;
(3) sintering process parameter is the N that flows
2Or N
2+ H
2Under the atmosphere, in 1500～1600 ℃
Hot pressed sintering, (pressure is 20～40MPa, is incubated 4～8 hours) or
1550～1600 ℃ of following pressureless sinterings (being incubated 4～10 hours).Pressure divides two during hot pressing
Inferior applying applies 10～15MPa earlier when temperature reaches 1300～1400 ℃.
The thermal conductivity of the AlN goods of low-temperature sintering method preparation provided by the invention is between 120～200Wm
-1K
-1Between, sample rate is all greater than 99% theoretical density.Three-point bending strength is greater than 450MPa, and specific inductivity is 7.3, dielectric loss 1 * 10
-4, resistivity is 1 * 10
13Ω m, sample overall dimension is diameter 120mm disk.
This shows that the advantage that the present invention has is fairly obvious:
(1) initial AlN material powder is not had particular requirement, adopt common commercially available particle diameter 2.0 μ m the carbothermic method preparation or be that the powder of 3～4 μ m get final product its low price and easy acquisition with the particle diameter that the self-propagating high-temperature synthesis method is produced;
(2) main component of sintering additive is cheap technical grade carbide of calcium, because of it very easily reacts with water, deoxidation effect is obvious, can not only in the whole preparation process flow process, control oxygen level effectively, and the add-on of other additives reduces behind the use carbide of calcium, when reducing cost, also help the removal of oxygen impurities in the preparation process and the purification of AlN crystal boundary, thereby make prepared AlN pottery have high heat-conducting property;
(3) adopt conventional ceramic preparation technology, under 1500～1600 ℃ sintering temperature, can make the aluminium nitride ceramics goods of high-compactness (theoretical density is more than 99%), make it to be very suitable for large-scale industrial production.
Below in conjunction with embodiment, further specify substantive distinguishing features of the present invention and obvious improvement.Embodiment 1
Additive therefor is CaC
2, Y
2O
3Mixture with alkalimetal oxide.Concrete component is 3.0%CaC
2, 1.0%Li
2O is (with Li
2CO
3Form adds) and 2.0%Y
2O
3(being weight ratio) is with the aluminium nitride powder uniform mixing.Aluminum nitride powder is prepared by carbothermic method, and median size is 2.0 μ m.Initial powder is dry-pressing formed with single shaft, and forming pressure is 4MPa.Biscuit is inserted in the graphite jig that applies BN, in mobile N2 atmosphere in 1500 ℃ of hot pressed sinterings.Sintering schedule is 20 ℃/min of heat-up rate, and temperature begins pressurization when rising to 1350 ℃, and pressure is 12MPa, and temperature rises to 30MPa with pressure after arriving preset temperature again, is incubated 6 hours.The sample furnace cooling.
Low sintering aluminium nitride ceramics performance is as follows:
Density (gcm
-3) 3.260
Crystalline phase (X light analysis) AlN
Void content (%)＜0.2
Intensity (MPa) 510
Thermal conductivity (Wm
-1K
-1) 150 embodiment 2
Additive therefor is CaC
2, Y
2O
3Mixture with alkalimetal oxide.Concrete component is 3.0%CaC
2, 1.0%K
2O is (with K
2CO
3Form adds) and 2.0%Y
2O
3(being weight ratio) is with the aluminium nitride powder uniform mixing.Aluminum nitride powder is prepared by carbothermic method, and median size is 2.0 μ m.Initial powder is dry-pressing formed with single shaft, and forming pressure is 4MPa.Biscuit is inserted in the graphite jig that applies BN, at mobile N
2+ H
2In the atmosphere in 1550 ℃ of hot pressed sinterings.Sintering schedule is 20 ℃/min of heat-up rate, and temperature begins pressurization when rising to 1300 ℃, and pressure is 15MPa, and temperature rises to 40MPa with pressure after arriving preset temperature again, is incubated 8 hours.The sample furnace cooling.
Low sintering aluminium nitride ceramics performance is as follows:
Density (gcm
-3) 3.258
Crystalline phase (X light analysis) AlN
Void content (%)＜0.3
Intensity (MPa) 500
Thermal conductivity (Wm-1K-1) 130 embodiment 3
Additive therefor is the mixture of technical grade carbide of calcium and alkalimetal oxide, and concrete composition is 1.0%Li
2O is (with Li
2CO
3Form adds) and 4.0%CaC
2(being weight ratio) is with the aluminium nitride powder uniform mixing.Aluminum nitride powder is by spreading the method preparation certainly, and median size is 4.0 μ m.Initial powder isostatic pressing, forming pressure are 200MPa.Biscuit is inserted in the plumbago crucible or boron nitride crucible that applies BN, at mobile N
2In the atmosphere in 1600 ℃ of pressureless sinterings.10 ℃/min of heat-up rate is incubated 12 hours.The sample furnace cooling.
Low sintering aluminium nitride ceramics performance is as follows:
Density (gcm
-3) 3.260
Crystalline phase (X light analysis) AlN
Void content (%)＜0.2
Intensity (MPa) 520
Thermal conductivity (Wm
-1K
-1) 140 embodiment 4
Additive therefor is 4% (weight ratio) technical grade carbide of calcium, with the aluminium nitride powder uniform mixing.Aluminum nitride powder is by spreading the method preparation certainly, and median size is 3.0 μ m.Initial powder is dry-pressing formed with single shaft, and forming pressure is 4MPa.Biscuit is inserted in the graphite jig that applies BN, at mobile N
2+ H
2In the atmosphere in 1600 ℃ of hot pressed sinterings.Sintering schedule is 20 ℃/min of heat-up rate, and temperature begins pressurization when rising to 1350 ℃, and pressure is 10MPa, and temperature rises to 30MPa with pressure after arriving preset temperature again, is incubated 6 hours.The sample furnace cooling.
Low sintering aluminium nitride ceramics performance is as follows:
Density (gcm
-3) 3.260
Crystalline phase (X light analysis) AlN
Void content (%)＜0.2
Intensity (MPa)＞500
Thermal conductivity (Wm
-1K
-1) 130 embodiment 5
Additive therefor is CaC
2, Y
2O
3Mixture with alkalimetal oxide.Concrete component is 3.0%CaC
2, 1.0%Li
2O is (with Li
2CO
3Form adds) and 2.0%Y
2O
3(being weight ratio) is with the aluminium nitride powder uniform mixing.Aluminum nitride powder is by spreading the method preparation certainly, and median size is 4.0 μ m.Initial powder is dry-pressing formed with single shaft, and forming pressure is 4MPa.Biscuit is inserted in the graphite jig that applies BN, at mobile N
2In the atmosphere in 1600 ℃ of hot pressed sinterings.Sintering schedule is 20 ℃/min of heat-up rate, and temperature begins pressurization when rising to 1400 ℃, and pressure is 10MPa, and temperature rises to 30MPa with pressure after arriving preset temperature again, is incubated 6 hours.The sample furnace cooling.
Low sintering aluminium nitride ceramics performance is as follows:
Density (gcm-3) 3.264
Crystalline phase (X light analysis) AlN
Void content (%)＜0.5
Intensity (MPa) 490
Thermal conductivity (Wm
-1K
-1)＞200 embodiment 6
Additive therefor is CaC
2, Y
2O
3Mixture with alkalimetal oxide.Concrete component is 3.0%CaC
2, 1.0%K
2O is (with K
2CO
3Form adds) and 2.0%Y
2O
3(being weight ratio) is with the aluminium nitride powder uniform mixing.Aluminum nitride powder is by spreading the method preparation certainly, and median size is 4.0 μ m.Initial powder is dry-pressing formed with single shaft, and forming pressure is 4MPa.Biscuit is inserted in the graphite jig that applies BN, at mobile N
2In the atmosphere in 1500 ℃ of hot pressed sinterings.Sintering schedule is 20 ℃/min of heat-up rate, and temperature begins pressurization when rising to 1300 ℃, and pressure is 15MPa, and temperature rises to 40MPa with pressure after arriving preset temperature again, is incubated 8 hours.The sample furnace cooling.
Low sintering aluminium nitride ceramics performance is as follows:
Density (gcm
-3) 3.258
Crystalline phase (X light analysis) AlN
Void content (%)＜0.4
Intensity (MPa) 500
Thermal conductivity (Wm
-1K
-1) 140 embodiment 7
Additive therefor is the mixture of carbide of calcium, alkaline earth metal oxide and rare earth oxide.Concrete component is 2.0%CaC
2, 2.0%Li
2O is (with Li
2CO
3The form adding), 3.0%Dy
2O
3(being weight ratio) is with the aluminium nitride powder uniform mixing.Aluminum nitride powder is by spreading the method preparation certainly, and median size is 3.0 μ m.Initial powder isostatic pressing, forming pressure are 200MPa.Biscuit is inserted in the plumbago crucible or boron nitride crucible that applies BN, at mobile N
2In the atmosphere in 1550 ℃ of pressureless sinterings.10 ℃/min of heat-up rate is incubated 10 hours.The sample furnace cooling.
Low sintering aluminium nitride ceramics performance is as follows:
Density (gcm
-3) 3.265
Crystalline phase (X light analysis) AlN
Void content (%)＜0.3
Intensity (MPa) 470
Thermal conductivity (Wm
-1K
-1) 160 embodiment 8
Additive therefor is CaC
2, rare-earth oxide and alkalimetal oxide mixture.Concrete component is 2.0%CaC
2, 2.0%K
2O is (with K
2CO
3Form adds) and 2.0%Sm
2O
3(being weight ratio) is with the aluminium nitride powder uniform mixing.Aluminum nitride powder is prepared by carbothermic method, and median size is 2.0 μ m.Initial powder is dry-pressing formed with single shaft, and forming pressure is 4MPa.Biscuit is inserted in the graphite jig that applies BN, at mobile N
2In the atmosphere in 1500 ℃ of hot pressed sinterings.Sintering schedule is 20 ℃/min of heat-up rate, and temperature begins pressurization when rising to 1300 ℃, and pressure is 15MPa, and temperature rises to 40MPa with pressure after arriving preset temperature again, is incubated 4 hours.The sample furnace cooling.
Low sintering aluminium nitride ceramics performance is as follows:
Density (gcm
-3) 3.255
Crystalline phase (X light analysis) AlN
Void content (%)＜0.4
Intensity (MPa) 540
Thermal conductivity (Wm
-1K
-1) 125
Claims (11)
1. the low-temperature sintering of an aluminium nitride ceramics comprises the initial powder selection of aluminium nitride, the selection of additive and the selection of sintering process parameter.It is characterized in that:
(1) the AlN powder with the preparation of carbothermic method and self-propagating high-temperature synthesis method is a starting raw material, the former median size 2 μ m, latter's median size 3～4 μ m;
(2) sinter additives of selecting for use is cheap technical grade carbide of calcium (CaC
2), monovalent base metal oxide (R
2O) and rare earth oxide (Re
2O
3).Add-on is 2～4wt%CaC
2Or x%CaC
2+ y%R
2O (x is 2～4, and y is 1～3); Or x%CaC
2+ y%R
2O+z%Re
2O
3(x is 2～4, and y is 1～3, and z is 1～3, is weight ratio), it is 4～10wt% that additive adds total amount;
(3) sintering process parameter is the N that flows
2Or N
2+ H
2Under the atmosphere, in 1500～1600 ℃ of hot pressed sinterings, pressure is 20～40MPa, is incubated 4～8 hours or 1550～1600 ℃ of following pressureless sinterings, is incubated 4～10 hours.
2. by the described low-temperature sintering of claim 1, it is characterized in that described monovalent base metal oxide is K
2O, Li
2O; Rare earth oxide is Y
2O
3, La
2O
3, Pr
2O
3, Nd
2O
3, Sm
2O
3, Gd
2O
3, Tb
2O
3, Dy
2O
3, Ho
2O
3, Er
2O
3, Er
2O
3, Yb
2O
3Or Lu
2O
3Among any.
3. by the described low-temperature sintering of claim 1, it is characterized in that described hot pressed sintering pressure applies at twice, in the time of 1300～1400 ℃, apply 10～15MPa earlier, after temperature reaches 1500～1600 ℃, be applied to 20～40MPa again.
4. by claim 1,2 described low-temperature sinterings, it is characterized in that:
(1) the AlN powder is prepared by carbothermic method, median size 2.0 μ m;
(2) additive is 3.0%CaC
2+ 1.0%Li
2O+2.0%Y
2O
3(being weight ratio);
(3) sintering schedule is 20 ℃/min of temperature rise rate, and temperature rises to 1350 ℃, begins pressurization, and pressure is 12MPa, and temperature rises to 30MPa with pressure after reaching 1500 ℃ again, is incubated 6 hours, furnace cooling.
5. by claim 1,2 described low-temperature sinterings, it is characterized in that:
(1) the AlN powder is prepared by carbothermic method, median size 2.0 μ m;
(2) additive is 3.0%CaC
2+ 1.0%K
2O+2.0%Y
2O
3(being weight ratio);
(3) sintering schedule is 20 ℃/min of temperature rise rate, and temperature rises to 1300 ℃, begins pressurization, and pressure is 15MPa, and temperature rises to 40MPa with pressure after reaching 1500 ℃ again, is incubated 8 hours, furnace cooling.
6. by claim 1,2 described low-temperature sinterings, it is characterized in that:
(1) the AlN powder is by the preparation of self-propagating high-temperature synthesis method, median size 4.0 μ m;
(2) additive is 4.0%CaC
2+ 1.0%Li
2O (being weight ratio);
(3) sintering schedule is at mobile N
2In 1600 ℃ of pressureless sinterings, 10 ℃/min of heat-up rate is incubated 12 hours, furnace cooling in the atmosphere.
7. by claim 1,2 described low-temperature sinterings, it is characterized in that:
(1) the AlN powder is by spreading the method preparation certainly, and median size is 3.0 μ m;
(2) additive is 4.0% (weight ratio) CaC
2
(3) sintering schedule is 20 ℃/min of temperature rise rate, and temperature rises to 1350 ℃, begins pressurization, and pressure is 10MPa, and temperature rises to 30MPa with pressure after reaching 1600 ℃ again, is incubated 6 hours, furnace cooling.
8. by claim 1,2 described low-temperature sinterings, it is characterized in that:
(1) the AlN powder is by spreading the method preparation certainly, and median size is 4.0 μ m;
(2) additive is 3.0%CaC
2+ 1.0%Li
2O+2.0%Y
2O
3(being weight ratio);
(3) sintering schedule is 20 ℃/min of temperature rise rate, and temperature rises to 1400 ℃, beginning
Pressurization, pressure is 10MPa, temperature rises to pressure after reaching 1600 ℃ again
30MPa is incubated 6 hours, furnace cooling.
9. by claim 1,2 described low-temperature sinterings, it is characterized in that:
(1) the AlN powder is by spreading the method preparation certainly, and median size is 4.0 μ m;
(2) additive is 3.0%CaC
2+ 1.0%K
2O+2.0%Y
2O
3(being weight ratio);
(3) sintering schedule is 20 ℃/min of temperature rise rate, and temperature rises to 1300 ℃, begins pressurization, and pressure is 15MPa, and temperature rises to 40MPa with pressure after reaching 1500 ℃ again, is incubated 8 hours, furnace cooling.
10. by claim 1,2 described low-temperature sinterings, it is characterized in that:
(1) the AlN powder is by spreading the method preparation certainly, and median size is 4.0 m;
(2) additive is 2.0%CaC
2+ 2.0%Li
2O+3.0%Dy
2O
3(being weight ratio);
(3) sintering schedule is at mobile N
2In 1550 ℃ of pressureless sinterings, 10 ℃/min of heat-up rate is incubated 10 hours, furnace cooling in the atmosphere.
11., it is characterized in that by claim 1,2 described low-temperature sinterings:
(1) the AlN powder is prepared by carbothermic method, and median size is 2.0 μ m;
(2) additive is 2.0%CaC
2+ 2.0%K
2O+2.0%Sm
2O
3(being weight ratio);
(3) sintering schedule is 20 ℃/min of temperature rise rate, and temperature rises to 1300 ℃, beginning
Pressurization, pressure is 15MPa, temperature rises to pressure after reaching 1500 ℃ again
40MPa is incubated 4 hours, furnace cooling.
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| CN98110938A CN1092165C (en) | 1998-07-08 | 1998-07-08 | Low temp. sintering of aluminum nitride ceramics |
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| CN98110938A CN1092165C (en) | 1998-07-08 | 1998-07-08 | Low temp. sintering of aluminum nitride ceramics |
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| CN1092165C CN1092165C (en) | 2002-10-09 |
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Cited By (7)
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| CN1301935C (en) * | 2005-07-29 | 2007-02-28 | 四川艺精长运超硬材料有限公司 | Process for preparing AIN ceramic material |
| CN102344281A (en) * | 2010-07-30 | 2012-02-08 | 比亚迪股份有限公司 | Aluminium nitride ceramic wafer and preparation method thereof |
| CN105801127A (en) * | 2016-03-03 | 2016-07-27 | 上海大学 | Method for preparing high-thermal-conductivity aluminum nitride ceramic substrate for integrated circuit package |
| CN105837224A (en) * | 2016-05-31 | 2016-08-10 | 武汉理工大学 | Method for preparing aluminum nitride ceramics by aid of ammonium fluoride which is used as additive |
| CN104402480B (en) * | 2014-10-30 | 2016-09-07 | 青岛橡胶谷知识产权有限公司 | A kind of aluminium nitride ceramics composite and preparation method thereof |
| CN116332653A (en) * | 2022-12-19 | 2023-06-27 | 湖南聚能陶瓷材料有限公司 | High-performance aluminum nitride ceramic material and preparation method thereof |
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Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61261270A (en) * | 1985-05-15 | 1986-11-19 | 日本電気株式会社 | Manufacture of aluminum nitride sintered body |
| JPS6418977A (en) * | 1987-07-13 | 1989-01-23 | Nec Corp | Production of aluminum nitride powder and aluminum nitride sintered product |
| JPH01188472A (en) * | 1988-01-22 | 1989-07-27 | Nec Corp | Production of aluminum nitride sintered body |
| US5322824A (en) * | 1993-05-27 | 1994-06-21 | Chia Kai Y | Electrically conductive high strength dense ceramic |
| US5424261A (en) * | 1993-12-22 | 1995-06-13 | The Carborundum Company | Low temperature sintering route for aluminum nitride ceramics |
| CN1130607A (en) * | 1995-11-17 | 1996-09-11 | 清华大学 | Manufacturing method of high thermal conductivity aluminum nitride ceramics |
| JPH1188472A (en) * | 1997-09-10 | 1999-03-30 | Nec Corp | Line data sampling device, network system containing the same, line data sampling method and recording medium recording line data sampling program |
| CN1076012C (en) * | 1998-04-24 | 2001-12-12 | 中国科学院上海硅酸盐研究所 | Process for preparation of transparent aluminium nitride ceramic |
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- 1998-07-08 CN CN98110938A patent/CN1092165C/en not_active Expired - Fee Related
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| CN105801127A (en) * | 2016-03-03 | 2016-07-27 | 上海大学 | Method for preparing high-thermal-conductivity aluminum nitride ceramic substrate for integrated circuit package |
| CN105837224A (en) * | 2016-05-31 | 2016-08-10 | 武汉理工大学 | Method for preparing aluminum nitride ceramics by aid of ammonium fluoride which is used as additive |
| CN105837224B (en) * | 2016-05-31 | 2019-01-01 | 武汉理工大学 | It is a kind of using ammonium fluoride as the preparation method of the aluminium nitride ceramics of additive |
| CN116332653A (en) * | 2022-12-19 | 2023-06-27 | 湖南聚能陶瓷材料有限公司 | High-performance aluminum nitride ceramic material and preparation method thereof |
| CN116332653B (en) * | 2022-12-19 | 2024-03-15 | 湖南聚能陶瓷材料有限公司 | High-performance aluminum nitride ceramic material and preparation method thereof |
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