CN1212288C - Aluminium nitride ceramic with high heat conductivity - Google Patents
Aluminium nitride ceramic with high heat conductivity Download PDFInfo
- Publication number
- CN1212288C CN1212288C CN 03100287 CN03100287A CN1212288C CN 1212288 C CN1212288 C CN 1212288C CN 03100287 CN03100287 CN 03100287 CN 03100287 A CN03100287 A CN 03100287A CN 1212288 C CN1212288 C CN 1212288C
- Authority
- CN
- China
- Prior art keywords
- aln
- earth metal
- aluminium nitride
- sintering aids
- mixed sintering
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Links
- 229910017083 AlN Inorganic materials 0.000 title claims abstract description 63
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000000919 ceramic Substances 0.000 title claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 49
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims description 16
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 10
- 229910001618 alkaline earth metal fluoride Inorganic materials 0.000 claims description 8
- 150000002910 rare earth metals Chemical group 0.000 claims description 8
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 abstract description 11
- 229910001404 rare earth metal oxide Inorganic materials 0.000 abstract description 11
- -1 rare earth metal fluorides Chemical class 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000005452 bending Methods 0.000 abstract description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 abstract 2
- 150000002222 fluorine compounds Chemical class 0.000 abstract 2
- 239000011230 binding agent Substances 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 235000015895 biscuits Nutrition 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 238000005266 casting Methods 0.000 description 7
- 239000007791 liquid phase Substances 0.000 description 7
- 239000000758 substrate Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000007766 curtain coating Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 239000004902 Softening Agent Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 2
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000009766 low-temperature sintering Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012777 electrically insulating material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
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- Ceramic Products (AREA)
Abstract
The present invention relates to an aluminium nitride ceramic with high heat conductivity, which belongs to the technical field of ceramic materials. The ceramic is made from AlN powder and mixed sintering aids, wherein the mixed sintering aids are either alkali earth oxides or alkali earth metal fluorides and either rare earth oxides or rare earth metal fluorides, the proportion of the AlN to the mixed sintering aids is (91 to 97.5)wt%: (9 to 2.5)wt%, and the proportion of the two mixed sintering aids is (0.5 to 4)wt%: (2 to 5)wt%. The present invention has another formula that the mixed sintering aids are either alkali earth oxides or alkali earth metal fluorides, either rare earth oxides or rare earth metal fluorides, and III family oxides, the proportion of the AlN to the mixed sintering aids is (89.5 to 97)wt%: (10.5 to 3)wt%, and the proportion of the three mixed sintering aids is (0.5 to 4)wt%: (2 to 4)wt%: (0.5 to 2.5)wt%. The aluminium nitride ceramic provided by the present invention has the characteristics of low sintering temperature, easy cofiring with metal, heat conductivity of 140 to 200 W/m. K, bending strength of no less than 300MPa, dielectric constant of 8.5 to 9.5 and dielectric loss of 3-4*10<-4>.
Description
Technical field
The present invention relates to a kind of high-heat conductivity aluminium nitride ceramics, belong to technical field of ceramic material.
Background technology
Along with developing rapidly of microelectronics, require to have higher thermal conductivity and superior dielectric properties as the substrate of electrically insulating material.High thermal conductivity, thermal expansivity and Si are complementary because aluminium nitride has, low specific inductivity, low dielectric loss, advantage such as nontoxic, and potentiality have a wide range of applications in fields such as power electronics, electronic information.But AlN belongs to the covalent linkage crystal, is difficult to sintering, and, because Al and O have very strong avidity, often contain Al in the AlN powder
2O
3, therefore, oxa-mass-energy reduces the thermal conductivity of AlN pottery greatly in the sintering process to AlN lattice diffusion formation oxygen defect.For overcoming above-mentioned defective, general manufacturing process adopts mostly and adds a certain amount of CaO or Y
2O
3Make sintering agent in alkaline-earth metal or rare-earth oxide, burn till at the high temperature more than 1800 ℃.The shortcoming of this technology is the sintering temperature height, burns for metallization altogether and brings difficulty.Along with the development of low-temperature sintering technology, also explored many low sintering technologies, yet thermal conductivity improves always not quite.But China's invalidated patent 95117462.2 provides a kind of patent of correct prescription ratio range mistake, and it can't realize high-heat conductivity aluminium nitride ceramics.
Summary of the invention
The objective of the invention is in order to overcome the deficiencies in the prior art, provide a kind of and realize that sintering temperature is low, be easy to the high-heat conductivity aluminium nitride ceramics that burns altogether with metal, by adding of the behavior of sintering aid control liquid phase in sintering process, the temperature rise period of sintering process is controlled by different liquid phases with holding stage, be beneficial to the densification of aluminium nitride ceramics and eliminate the lattice oxygen defective, like this, the aluminium nitride ceramics goods that acquisition has higher heat-conductivity under lower sintering temperature.
A kind of high-heat conductivity aluminium nitride ceramics that the present invention proposes, this pottery comprises the AlN powder and mixes sintering aid, described mixing sintering aid is A and B, its proportioning is, AlN: (A+B)=(91-97.5) wt%: (9-2.5) wt%, A: B=(0.5-4) wt%: (2-5) wt%, wherein, A is any in alkaline earth metal oxide and the alkaline-earth metal fluoride, and B is any in rare-earth oxide and the rare earth metal fluorochemical.A is alkaline-earth metal fluoride CaF
2, B is rare earth metal fluorochemical YF
3
In above-mentioned prescription, described alkaline earth metal oxide is CaO; Described alkaline-earth metal fluoride is CaF
2Described rare-earth oxide is Dy
2O
3, Y
2O
3In any; Described rare earth metal fluorochemical is YF
3
The another kind of high-heat conductivity aluminium nitride ceramics that the present invention proposes, this pottery comprises the AlN powder and mixes sintering aid, described mixing sintering aid is A, B and C, its proportioning is, AlN: (A+B+C)=(89.5-97) wt%: (10.5-3) wt%, A: B: C=(0.5-4) wt%: (24) wt%: (0.5-2.5) wt%, wherein A is any in alkaline earth metal oxide and the fluorochemical, B is any in rare-earth oxide and the fluorochemical, and C is the III-th family oxide compound.
In above-mentioned prescription, described alkaline earth metal oxide is CaO; Described alkaline-earth metal fluoride is CaF
2Described rare-earth oxide is Dy
2O
3And Y
2O
3In any; Described rare earth metal fluorochemical is YF
3Described III-th family oxide compound is B
2O
3
Because the present invention has adopted the mixing sintering aid with above characteristics, is reduced to below 1800 ℃ in sintering temperature, still can obtain to have the aluminium nitride ceramics of high-compactness and high heat conductance.Simultaneously,, can also guarantee the planeness and the roughness of substrate, on the other hand, also be easy to realize common burning with metal because sintering temperature is low.The thermal conductivity of the aluminium nitride ceramics that is obtained among the present invention can reach 140-200W/mK, and bending strength 〉=300MPa, specific inductivity are 8.5-9.5, and dielectric loss is 3-4 * 10
-4
Embodiment
The present invention prepares high-heat conductivity aluminium nitride ceramics and may further comprise the steps:
(1) preparation AlN compound
Adopting median size is raw material at the AlN powder of 1-3 μ m, oxygen level≤1.2wt%, nitrogen content 〉=33wt%, carbon content≤0.06wt%, add and mix sintering aid, described mixing sintering aid is A, B, its proportioning is, AlN: (A+B)=(91-97.5) wt%: (9-2.5) wt%, A: B=(O.5-4) wt%: (2-5) wt%, wherein, A is any in alkaline earth metal oxide and the alkaline-earth metal fluoride, and B is any in rare-earth oxide and the rare earth metal fluorochemical.
In above-mentioned prescription, described alkaline earth metal oxide is CaO; Described alkaline-earth metal fluoride is CaF
2Described rare-earth oxide is Dy
2O
3, Y
2O
3In any; Described rare earth metal fluorochemical is YF
3
The another kind of high-heat conductivity aluminium nitride ceramics that the present invention proposes, this pottery is made by AlN powder and mixing sintering aid, described mixing sintering aid is A, B and C, its proportioning is, AlN: (A+B+C)=(89.5-97) wt%: (10.5-3) wt%, A: B: C=(0.5-4) wt%: (2-4) wt%: (0.5-2.5) wt%, wherein A is any in alkaline earth metal oxide and the fluorochemical, B is any in rare-earth oxide and the fluorochemical, and C is the III-th family oxide compound.
In above-mentioned prescription, described alkaline earth metal oxide is CaO; Described alkaline-earth metal fluoride is CaF
2Described rare-earth oxide is Dy
2O
3, Y
2O
3In any; Described rare earth metal fluorochemical is YF
3Described III-th family oxide compound is B
2O
3
(2) preparation AlN base substrate:
Prepare the AlN biscuit with dry pressing: in the AlN compound that the above-mentioned the first step is made, add binding agent polyvinyl alcohol (PVA) or polyvinyl butyral acetal (PVB), at the forming under the pressure of 90-100MPa, be the AlN biscuit after the granulation;
(3) the AlN base substrate to preparation carries out binder removal under 550-600 ℃, air atmosphere;
(4) the AlN base substrate behind the above-mentioned binder removal is placed graphite heater furnace, pass to flowing nitrogen, in 1600-1800 ℃ of temperature, carry out sintering, be incubated 4-8 hour, can obtain the aluminium nitride ceramics of high-compactness high heat conductance.
In above-mentioned preparation method, the also available doctor-blade casting process of step (2) prepares the AlN biscuit: in the AlN compound that above-mentioned steps (1) is made, add solvent, dispersion agent, softening agent and binding agent, make casting slurry, prepare banded AlN base substrate with casting method; All the other steps the same (3), (4).
Mixing sintering aid of the present invention has the following advantages:
(1) the mixing sintering aid that is adopted has low common molten liquidus point, liquidus point can be controlled in below 1500 ℃, therefore, the sintering densification of aluminium nitride ceramics and the process of growth of crystal grain are controlled by liquid phase mainly, mainly are that diffusion control is different in this and the aluminium nitride ceramics high temperature sintering mechanism;
(2) liquid phase that the mixing sintering aid that is adopted forms changes in whole sintering process, in temperature-rise period, the main effect of liquid phase is to help nodulizing, and in insulating process, the character of liquid phase changes to some extent, not only play and help nodulizing, and play a part to eliminate aluminium nitride lattice oxygen defective, this has basic different with normally used low-temperature sintering method;
(3) the mixing sintering aid that is adopted does not have the aitiogenic chemically reactive with AlN, and the crystal habit of aluminium nitride shows as polyhedron, perfect, the face contact each other of grain growing, and heat-transfer interface is big, helps improving the thermal conductivity of aluminium nitride ceramics;
(4) the formed liquid phase of mixing sintering aid that is adopted has good flowability, is subjected to the effect of AlN grain growth impellent to retract to triangle crystal boundary place in the agglomerating later stage, thereby has reduced intergranular second phase, helps improving the thermal conductivity of AlN pottery;
(5) some composition in the mixing sintering aid that is adopted, different according to prescription, in sintering process, or itself can volatilize, or the volatilization of carbothermic reduction reaction formation nitride takes place, these all play a part to purify crystal boundary, can improve the thermal conductivity of AlN pottery.
The present invention will be further described below in conjunction with embodiment:
Embodiment 1
Prescription, calcining system and the thermal conductivity of table 1 AlN pottery
| Test piece number (Test pc No.) | Prescription is formed (wt) | Calcining system | Thermal conductivity (W/mK) | |||||
| Y 2O 3 | YF 3 | CaF 2 | B 2O 3 | AlN | Sintering temperature (℃) | Soaking time (h) | ||
| 1 | 5 | 4 | 91 | 1750 | 6 | 208 | ||
| 2 | 3 | 2 | 95 | 1650 | 6 | 187 | ||
| 3 | 3 | 4 | 93 | 1750 | 6 | 182 | ||
| 4 | 5 | 0.5 | 94.5 | 1650 | 6 | 180 | ||
| 5 | 2 | 2 | 96 | 1650 | 8 | 148 | ||
| 6 | 2 | 0.5 | 2.5 | 95 | 1650 | 4 | 146 | |
Additive therefor is Y
2O
3, YF
3And CaF
2And B
2O
3In the powder for preparing, add dehydrated alcohol, after 48 hours ball millings mix, ceramic preparation technology's drying routinely, sieve, add a spot of polyvinyl alcohol (PVB) or polyvinyl butyral acetal (PVB) is made binding agent, after the granulation, utilize dry pressing to be pressed into the biscuit of desired shape and size.Biscuit is placed in the graphite furnace through binder removal, carries out sintering with the protection of works such as flowing nitrogen, sintering temperature and soaking time, and the thermal conductivity of product sees Table 1.
Embodiment 2
Additive therefor is Dy
2O
3, CaO and B
2O
3, it is as shown in table 2 to fill a prescription in detail, adds solvent, dispersion agent, binding agent and softening agent and make casting slurry in prepared mixture, slurry mixing time 24-48 hour.Utilize flow casting molding mechanism to be equipped with the slabbing biscuit, in air, be heated to 600 ℃ of binder removals then.Curtain coating AlN biscuit behind the binder removal is placed graphite furnace, and with works such as flowing nitrogen protection carrying out sintering, table 2 has shown at 1650 ℃, is incubated the thermal conductivity of the product of acquisition in 4 hours.
The prescription and the thermal conductivity of table 2 curtain coating AlN pottery
| Test piece number (Test pc No.) | Prescription is formed (wt%) | Thermal conductivity (W/mK) | |||
| Dy 2O 3 | CaO | B 2O 3 | AlN | ||
| 1 | 3.6 | 0.5 | 1.4 | 94.5 | 130 |
| 2 | 4 | 1 | 1.0 | 94 | 140 |
| 3 | 3.2 | 1 | 2.5 | 93.3 | 156 |
Embodiment 3
Additive therefor is CaF
2, YF
3And B
2O
3, it is as shown in table 3 to fill a prescription in detail, adds solvent, dispersion agent, binding agent and softening agent and make casting slurry in prepared mixture, slurry mixing time 24-48 hour.Utilize flow casting molding mechanism to be equipped with the slabbing biscuit, in air, be heated to 600 ℃ of binder removals then.Curtain coating AlN biscuit behind the binder removal is placed graphite furnace, carry out sintering with the protection of works such as flowing nitrogen, table 3 has shown the thermal conductivity that obtains under the different sintering schedules.
The prescription and the thermal conductivity of table 3 curtain coating AlN pottery
| Test piece number (Test pc No.) | Prescription is formed (wt%) | Calcining system | Thermal conductivity (W/mK) | ||||
| YF 3 | CaF 2 | B 2O 3 | AlN | Sintering temperature (℃) | Soaking time (h) | ||
| 1 | 3 | 2 | 95 | 1750 | 6 | 185 | |
| 2 | 4 | 4 | 0.5 | 9l.5 | 1650 | 6 | 162 |
Claims (1)
1, a kind of high-heat conductivity aluminium nitride ceramics, it is characterized in that: described aluminium nitride ceramics is made by AlN powder and mixing sintering aid, described mixing sintering aid is A and B, its proportioning is, AlN: (A+B)=(91-97.5) wt%: (9-2.5) wt%, A: B=(0.5-4) wt%: (2-5) wt%, wherein, A is alkaline-earth metal fluoride CaF
2, B is rare earth metal fluorochemical YF
3
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03100287 CN1212288C (en) | 2003-01-10 | 2003-01-10 | Aluminium nitride ceramic with high heat conductivity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03100287 CN1212288C (en) | 2003-01-10 | 2003-01-10 | Aluminium nitride ceramic with high heat conductivity |
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| Publication Number | Publication Date |
|---|---|
| CN1421418A CN1421418A (en) | 2003-06-04 |
| CN1212288C true CN1212288C (en) | 2005-07-27 |
Family
ID=4789800
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|---|---|---|---|
| CN 03100287 Expired - Fee Related CN1212288C (en) | 2003-01-10 | 2003-01-10 | Aluminium nitride ceramic with high heat conductivity |
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| CN (1) | CN1212288C (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100426480C (en) * | 2006-03-06 | 2008-10-15 | 宇富半导体材料科技股份有限公司 | Chip pressing base and its application device |
| CN102826853B (en) * | 2012-09-04 | 2014-12-17 | 福建华清电子材料科技有限公司 | High-strength aluminum nitride ceramic substrate and manufacturing method thereof |
| CN103755351B (en) * | 2013-12-30 | 2015-08-26 | 莱鼎电子材料科技有限公司 | The LED production method of low cost aluminium nitride ceramic substrate |
| CN106167408A (en) * | 2016-07-20 | 2016-11-30 | 合肥毅创钣金科技有限公司 | A kind of great power LED cooling aluminum nitride ceramic substrate of low-temperature sintering high-compactness |
| CN106542828A (en) * | 2016-10-18 | 2017-03-29 | 华中科技大学 | A kind of aluminium nitride ceramics of low-temperature sintering high heat conductance and preparation method thereof |
| CN107935600B (en) * | 2017-12-08 | 2020-10-16 | 南充三环电子有限公司 | Ceramic composition, preparation method and application of ceramic composition and ceramic substrate |
| CN111484333A (en) * | 2019-01-28 | 2020-08-04 | 华中科技大学 | Aluminum nitride ceramic with high thermal conductivity and high strength and preparation method thereof |
| CN117510212A (en) * | 2023-10-26 | 2024-02-06 | 中国科学院上海硅酸盐研究所 | High-heat-conductivity high-microwave-absorption aluminum nitride ceramic material and preparation method thereof |
-
2003
- 2003-01-10 CN CN 03100287 patent/CN1212288C/en not_active Expired - Fee Related
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