CN107540381A - A kind of aluminium nitride ceramic substrate slurry - Google Patents
A kind of aluminium nitride ceramic substrate slurry Download PDFInfo
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- CN107540381A CN107540381A CN201710685168.4A CN201710685168A CN107540381A CN 107540381 A CN107540381 A CN 107540381A CN 201710685168 A CN201710685168 A CN 201710685168A CN 107540381 A CN107540381 A CN 107540381A
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Abstract
The present invention relates to a kind of aluminium nitride ceramic substrate slurry, the slurry is made up of the component of following parts by weight：800 900 parts of aluminum nitride ceramic powder, without 8 10 parts of 240 300 parts of benzene ternary solvent system, 15 25 parts of dispersant, 40 50 parts of composite sintering agent, 46 parts of toughened system and binding agent；Wherein, the aluminum nitride ceramic powder is 2.8m from surface area2/ g aluminum nitride ceramic powder, the no benzene ternary solvent system are the mixed solvent of ethanol, isopropanol and butanone, and one kind that the dispersant is selected in Sodium Polyacrylate, polysorbate and polyethylene glycol, the composite sintering agent is Li2O‑CaO‑YF3Composite sintering agent, the toughened system are Mo, W and NbC mixed metal particles, and the binding agent is polyvinyl butyral resin.The advantage of the invention is that：By the adjustment and optimization to each component raw material in slurry, and the content of strict control each component raw material, and then make the combination property of aluminium nitride ceramic substrate prepared more preferably.
Description
Technical field
The present invention relates to ceramic material field, relates generally to ceramic substrate preparing technical field, more particularly to a kind of nitridation
Aluminium ceramic substrate slurry.
Background technology
With the raising of high power module circuit level and the development of great power LED, to dielectric substrate material used
Higher requirement is proposed, aluminium nitride ceramics material is due to higher thermal conductivity, being widely used to various high-power electricity
The dielectric substrate material of sub- original paper.
Existing AlN ceramic prepare be usually only addition sintering aid and aluminum nitride powder be mixed together, then through into
Type technique is for example dry-pressing formed or flow casting molding, re-sinters and forms, the AlN ceramic prepared in this way has thermal conductance
Height, the characteristics of electric property is good, but its mechanical performance to be present poor, such as fracture toughness, bending strength is relatively low and thermal shock resistance compared with
Difference.With the development of high power electronic Packaging Industry, the application field of Electronic Packaging product is more and more extensive, its application environment
Become increasingly complex, therefore the also more and more higher of the requirement to its package substrate, then prepare a kind of substrate right and wrong of high comprehensive performance
Often it is necessary.
AlN ceramic prepares combination property of the slurry to AlN ceramic substrates of AlN ceramic due to its particularity
There is important influence；Therefore it is improved and optimizes on the basis of known AlN ceramic slurry, to obtain more preferable property
The AlN ceramic of energy parameter is the problem of current ceramic material area research.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of aluminium nitride ceramic substrate slurry, and it passes through to each group in slurry
The adjustment and optimization of point raw material, and the content of strict control each component raw material, and then the aluminium nitride ceramic substrate for making to prepare
Combination property is more preferably.
In order to solve the above technical problems, the technical scheme is that：A kind of aluminium nitride ceramic substrate slurry, its innovative point
It is：The slurry is made up of the component of following parts by weight：Aluminum nitride ceramic powder 800-900 parts, without benzene ternary solvent body
It is 240-300 parts, dispersant 15-25 parts, composite sintering agent 40-50 parts, toughened system 4-6 parts and binding agent 8-10 parts；Its
In, the aluminum nitride ceramic powder is 2.8m from surface area2/ g aluminum nitride ceramic powder, the no benzene ternary solvent system
For the mixed solvent of ethanol, isopropanol and butanone, the dispersant is selected in Sodium Polyacrylate, polysorbate and polyethylene glycol
One kind, the composite sintering agent are Li2O-CaO-YF3Composite sintering agent, the toughened system are Mo, W and NbC hybrid metal
Particle, the binding agent are polyvinyl butyral resin.
Further, the alumina ceramic powder includes the element of following content：Al 64.6%, N 34.4%, O
0.9%th, C 0.06%, Ca 3 × 10-4% and Fe 2 × 10-5%.
Further, the mass ratio of ethanol, isopropanol and butanone is 1 in the no benzene ternary solvent system:1:2~3.
Further, Li in the composite sintering agent2O, CaO and YF3Mass ratio be 25:8:100.
Further, Mo, W and NbC mass ratio are 2 in the toughened system:2:1.
The advantage of the invention is that：
(1) aluminium nitride ceramic substrate slurry of the present invention, in formula, aluminum nitride ceramic powder is smaller from grain graininess, grain
The powder being evenly distributed is spent, there is good powdery row material characteristic, good base has been laid for the excellent properties of aluminium nitride ceramic substrate
Plinth, in aluminium nitride ceramic substrate slurry of the present invention, the parts by weight content range of aluminum nitride ceramic powder is limited as 800-900
Part, while aluminium nitride ceramic substrate combination property is improved, it also ensure that it as core skeleton；
In formula, solvent is selected without benzene ternary solvent system, and successfully substitution tradition, which is cast, forms malicious solvent, reduces environment
Pollution, production cost is reduced, in aluminium nitride ceramic substrate slurry of the present invention, the parts by weight for limiting no benzene ternary solvent system contain
Amount scope is 240-300 parts, can effectively dissolve aluminum nitride ceramic powder and other additives；
In formula, composite sintering agent selects Li2O-CaO-YF3Composite sintering agent, it can effectively reduce the oxygen of AIN particle surfaces
Content, reduces the formation of oxygen defect in AIN lattices under high temperature, and then aluminium nitride ceramic substrate can be made to have higher thermal conductivity,
In aluminium nitride ceramic substrate slurry of the present invention, the parts by weight content range of composite sintering agent is limited as 40-50 parts, sintering aid
Content is strict controlled in 10% less than aluminum nitride ceramic powder, and sintering aid addition is excessive, on the contrary can be to aluminium nitride ceramics base
The performance of piece has the opposite effect；
Toughened system select with high-melting-point, high rigidity, high elastic modulus Mo, W and NbC mixed metal particles, have
Effect improves the fracture toughness of aluminium nitride ceramic substrate, and the toughened system and the chemical intermiscibility of aluminium nitride matrix that add are good,
High heat conductance and excellent electric property can be met simultaneously；And by the synergy of each component, aluminium nitride can be significantly improved
The combination property of ceramic substrate, also cause the stability of aluminium nitride ceramic substrate more preferably.
(2) aluminium nitride ceramic substrate slurry of the present invention, in formula, to alumina ceramic powder, without benzene ternary solvent system,
The selection of composite sintering agent and toughened system has been made further to limit, and then can obtain performance more under conditions of more excellent
Good aluminium nitride ceramic substrate.
With reference to embodiment, the present invention is further detailed explanation.
Embodiment
The following examples can make professional and technical personnel that the present invention be more fully understood, but therefore not send out this
It is bright to be limited among described scope of embodiments.
Aluminium nitride ceramic substrate slurry of the present invention, the slurry are made up of the component of following parts by weight：Aluminium nitride ceramics
Powder 800-900 parts, without benzene ternary solvent system 240-300 parts, dispersant 15-25 parts, composite sintering agent 40-50 parts, toughness reinforcing
System 4-6 parts and binding agent 8-10 parts；Wherein, the aluminum nitride ceramic powder is smaller from grain graininess, even particle size distribution
Powder, i.e. surface area is 2.8m2/ g aluminum nitride ceramic powder, the no benzene ternary solvent system be ethanol, isopropanol and
The mixed solvent of butanone, one kind that the dispersant is selected in Sodium Polyacrylate, polysorbate and polyethylene glycol are described compound to help
Burning agent is Li2O-CaO-YF3Composite sintering agent, the toughened system be Mo, W and NbC mixed metal particles, the binding agent
For polyvinyl butyral resin.
By multiple screening, and in view of the effect of each component collaboration, preferably, determining alumina ceramic powder choosing
With the element for including following content：Al 64.6%, N 34.4%, O 0.9%, C 0.06%, Ca 3 × 10-4% and Fe 2 ×
10-5%；Mass ratio without ethanol, isopropanol and butanone in benzene ternary solvent system is 1:1:2~3；Li in composite sintering agent2O、
CaO and YF3Mass ratio be 25:8:100；Mo, W and NbC mass ratio are 2 in toughened system:2:1；Obtained target product
Performance it is optimal.
Citing and explanation in detail are carried out to this kind of aluminium nitride ceramic substrate slurry by following examples below：
Embodiment 1
The present embodiment aluminium nitride ceramic substrate slurry, the slurry are made up of the component of following parts by weight：Aluminium nitride is made pottery
800 parts of porcelain powder, without 240 parts of benzene ternary solvent system, 15 parts of dispersant, 40 parts of composite sintering agent, 4 parts of toughened system and viscous
Tie 8 parts of agent；Wherein, the aluminum nitride ceramic powder is smaller from grain graininess, and the powder of even particle size distribution, i.e. surface area are
2.8m2/ g aluminum nitride ceramic powder, and the alumina ceramic powder includes the element of following content：Al 64.6%, N
34.4%th, O 0.9%, C 0.06%, Ca 3 × 10-4% and Fe 2 × 10-5%；The no benzene ternary solvent system is second
The mixed solvent of alcohol, isopropanol and butanone, and the mass ratio of ethanol, isopropanol and butanone is 1:1:2；The dispersant is from poly-
PAA, the composite sintering agent are Li2O-CaO-YF3Composite sintering agent, and Li2O, CaO and YF3Mass ratio be 25:8:
100；The toughened system is Mo, W and NbC mixed metal particles, and Mo, W and NbC mass ratio are 2:2:1；The bonding
Agent is polyvinyl butyral resin.
Embodiment 2
Compared with Example 1, each component content is constant, only will be without ethanol, isopropanol and butanone in benzene ternary solvent system
Mass ratio be changed to 1:1:3.
Embodiment 3
Compared with Example 1, each component content is constant, only will be without ethanol, isopropanol and butanone in benzene ternary solvent system
Mass ratio be changed to 1:1:2.5.
Table 1 below is that the quality without ethanol, isopropanol and butanone in benzene ternary solvent system compares contrast table in embodiment 1-3
Lattice：
In order to test the performance for the aluminium nitride ceramic substrate for using embodiment 1-3 aluminium nitride ceramic substrates slurry to prepare, each reality
The aluminium nitride ceramic substrate slurry of example is applied by the aluminium nitride ceramic substrate of flow casting molding, it is then each to aluminium nitride ceramic substrate
Sample is tested, and performance test results are shown in Table 2.
The performance test data of the aluminium nitride ceramic substrate of the embodiment 1-3 aluminium nitride ceramic substrate slurries of table 2
Conclusion：As can be seen from the above table, the aluminium nitride ceramic substrate of embodiment 1-3 aluminium nitride ceramic substrate slurry,
Chip density is in 3.391g/cm3~3.462g/cm3, relative density is more than 99.5%, substrate thermal conductivity >=180w/m.k, base
Piece bending strength >=402MPa, substrate dielectric constant≤8.98 (1MHz, room temperature)；And substrate fracture toughness is in 2.94MPa.m1/2
~3.08MPa.m1/2Between, substrate specific insulation is in 1.8*1012Ω .cm~2.1*1012Between Ω .cm；Thus, with this
The combination property of the aluminium nitride ceramic substrate of the aluminium nitride ceramic substrate slurry of invention greatly improves；In addition, embodiment 1-3 enters
Row is compared, it can be seen that every test performance of embodiment 3 is superior to other two embodiments, thus embodiment 3 is most
Good embodiment.
Embodiment 4
Compared with Example 3, each component content is constant, and dispersant only is changed into polysorbate by Sodium Polyacrylate.
Embodiment 5
Compared with Example 3, each component content is constant, and dispersant only is changed into polyethylene glycol by Sodium Polyacrylate.
In order to test the performance for the aluminium nitride ceramic substrate for using embodiment 3-5 aluminium nitride ceramic substrates slurry to prepare, each reality
The aluminium nitride ceramic substrate slurry of example is applied by the aluminium nitride ceramic substrate of flow casting molding, it is then each to aluminium nitride ceramic substrate
Sample is tested, and performance test results are shown in Table 3.
The performance test data of the aluminium nitride ceramic substrate of the embodiment 3-5 aluminium nitride ceramic substrate slurries of table 3
Conclusion：As can be seen from the above table, the aluminium nitride ceramic substrate of embodiment 3-5 aluminium nitride ceramic substrate slurry,
Chip density is in 3.462g/cm3~3.526g/cm3, for relative density more than 99.5%, substrate thermal conductivity is more than 180w/m.k,
Substrate bending strength is more than 410MPa, substrate dielectric constant≤8.85 (1MHz, room temperature)；And substrate fracture toughness exists
3.08MPa.m1/2~3.28MPa.m1/2Between, substrate specific insulation is in 1.98*1012Ω .cm~2.3*1012Ω .cm it
Between；Thus, greatly improved with the combination property of the aluminium nitride ceramic substrate of the aluminium nitride ceramic substrate slurry of the present invention；This
Outside, embodiment 3-5 is compared, it can be seen that and every test performance of embodiment 5 is superior to other two embodiments,
Thus embodiment 5 is most preferred embodiment, i.e. dispersant selects polyethylene glycol, and the performance of aluminium nitride ceramic substrate is optimal.
Embodiment 6
The present embodiment aluminium nitride ceramic substrate slurry, the slurry are made up of the component of following parts by weight：Aluminium nitride is made pottery
900 parts of porcelain powder, without 300 parts of benzene ternary solvent system, 25 parts of dispersant, 50 parts of composite sintering agent, 6 parts of toughened system and viscous
Tie 10 parts of agent；Wherein, the aluminum nitride ceramic powder is smaller from grain graininess, the powder of even particle size distribution, i.e. surface area
For 2.8m2/ g aluminum nitride ceramic powder, and the alumina ceramic powder includes the element of following content：Al 64.6%, N
34.4%th, O 0.9%, C 0.06%, Ca 3 × 10-4% and Fe 2 × 10-5%；The no benzene ternary solvent system is second
The mixed solvent of alcohol, isopropanol and butanone, and the mass ratio of ethanol, isopropanol and butanone is 1:1:2.5；The dispersant is selected
Polyethylene glycol, the composite sintering agent are Li2O-CaO-YF3Composite sintering agent, and Li2O, CaO and YF3Mass ratio be 25:8:
100；The toughened system is Mo, W and NbC mixed metal particles, and Mo, W and NbC mass ratio are 2:2:1；The bonding
Agent is polyvinyl butyral resin.
Embodiment 7
The present embodiment aluminium nitride ceramic substrate slurry, the slurry are made up of the component of following parts by weight：Aluminium nitride is made pottery
850 parts of porcelain powder, without 270 parts of benzene ternary solvent system, 20 parts of dispersant, 45 parts of composite sintering agent, 5 parts of toughened system and viscous
Tie 9 parts of agent；Wherein, the aluminum nitride ceramic powder is smaller from grain graininess, and the powder of even particle size distribution, i.e. surface area are
2.8m2/ g aluminum nitride ceramic powder, and the alumina ceramic powder includes the element of following content：Al 64.6%, N
34.4%th, O 0.9%, C 0.06%, Ca 3 × 10-4% and Fe 2 × 10-5%；The no benzene ternary solvent system is second
The mixed solvent of alcohol, isopropanol and butanone, and the mass ratio of ethanol, isopropanol and butanone is 1:1:2.5；The dispersant is selected
Polyethylene glycol, the composite sintering agent are Li2O-CaO-YF3Composite sintering agent, and Li2O, CaO and YF3Mass ratio be 25:8:
100；The toughened system is Mo, W and NbC mixed metal particles, and Mo, W and NbC mass ratio are 2:2:1；The bonding
Agent is polyvinyl butyral resin.
Table 4 below is embodiment 5-7 each group distribution ratio contrast table lattice：
The embodiment 5-7 of table 4 weight proportion
In order to test the performance for the aluminium nitride ceramic substrate for using embodiment 5-7 aluminium nitride ceramic substrates slurry to prepare, each reality
The aluminium nitride ceramic substrate slurry of example is applied by the aluminium nitride ceramic substrate of flow casting molding, it is then each to aluminium nitride ceramic substrate
Sample is tested, and performance test results are shown in Table 5.
The performance test data of the aluminium nitride ceramic substrate of the embodiment 5-7 aluminium nitride ceramic substrate slurries of table 5
Conclusion：As can be seen from the above table, the aluminium nitride ceramic substrate of embodiment 5-7 aluminium nitride ceramic substrate slurry,
Chip density is in 3.526g/cm3~3.62g/cm3, relative density >=99.9%, substrate thermal conductivity is more than 185w/m.k, substrate
Bending strength is more than 425MPa, substrate dielectric constant≤9.2 (1MHz, room temperature)；And substrate fracture toughness is in 3.26MPa.m1/2~
3.35MPa.m1/2Between, substrate specific insulation is in 2.3*1012Ω .cm~2.53*1012Between Ω .cm；Thus, sent out with this
The combination property of the aluminium nitride ceramic substrate of bright aluminium nitride ceramic substrate slurry greatly improves；In addition, embodiment 5-7 is carried out
It is compared, it can be seen that every test performance of embodiment 7 is superior to other two embodiments, thus embodiment 7 is optimal
Embodiment.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The skill of the industry
For art personnel it should be appreciated that the present invention is not limited to the above embodiments, described in above-described embodiment and specification is explanation
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (5)
- A kind of 1. aluminium nitride ceramic substrate slurry, it is characterised in that：The slurry is made up of the component of following parts by weight：Nitridation Aluminium ceramic powders 800-900 parts, without benzene ternary solvent system 240-300 parts, dispersant 15-25 parts, composite sintering agent 40-50 Part, toughened system 4-6 parts and binding agent 8-10 parts；Wherein, the aluminum nitride ceramic powder is 2.8m from surface area2/ g nitrogen Change aluminium ceramic powders, the no benzene ternary solvent system is the mixed solvent of ethanol, isopropanol and butanone, and the dispersant is selected One kind in Sodium Polyacrylate, polysorbate and polyethylene glycol, the composite sintering agent are Li2O-CaO-YF3Composite sintering agent, The toughened system is Mo, W and NbC mixed metal particles, and the binding agent is polyvinyl butyral resin.
- 2. aluminium nitride ceramic substrate slurry according to claim 1, it is characterised in that：The alumina ceramic powder includes The element of following content：Al 64.6%, N 34.4%, O 0.9%, C 0.06%, Ca 3 × 10-4% and Fe 2 × 10-5%.
- 3. aluminium nitride ceramic substrate slurry according to claim 1, it is characterised in that：In the no benzene ternary solvent system The mass ratio of ethanol, isopropanol and butanone is 1:1:2~3.
- 4. aluminium nitride ceramic substrate slurry according to claim 1, it is characterised in that：Li in the composite sintering agent2O、 CaO and YF3Mass ratio be 25:8:100.
- 5. aluminium nitride ceramic substrate slurry according to claim 1, it is characterised in that：In the toughened system Mo, W and NbC mass ratio is 2:2:1.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5437116A (en) * | 1977-08-30 | 1979-03-19 | Mitsubishi Metal Corp | Tough thermet containing oxygen |
| JPH01103961A (en) * | 1987-10-16 | 1989-04-21 | Tokuyama Soda Co Ltd | Aluminum nitride sintered compact and its production |
| CN101734922A (en) * | 2008-11-27 | 2010-06-16 | 北京有色金属研究总院 | Microwave attenuator material with high heat conductivity and preparation method thereof |
| CN101748319A (en) * | 2008-12-19 | 2010-06-23 | 北京有色金属研究总院 | Electron-irradiation resisting shielding material and method for preparing same |
| CN103553691A (en) * | 2013-11-01 | 2014-02-05 | 广东工业大学 | Particle dispersion toughening aluminum nitride ceramic substrate and preparation method thereof |
| CN103819196A (en) * | 2013-12-30 | 2014-05-28 | 莱鼎电子材料科技有限公司 | Modified aluminum nitride ceramic substrate and production method thereof |
-
2017
- 2017-08-11 CN CN201710685168.4A patent/CN107540381A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5437116A (en) * | 1977-08-30 | 1979-03-19 | Mitsubishi Metal Corp | Tough thermet containing oxygen |
| JPH01103961A (en) * | 1987-10-16 | 1989-04-21 | Tokuyama Soda Co Ltd | Aluminum nitride sintered compact and its production |
| CN101734922A (en) * | 2008-11-27 | 2010-06-16 | 北京有色金属研究总院 | Microwave attenuator material with high heat conductivity and preparation method thereof |
| CN101748319A (en) * | 2008-12-19 | 2010-06-23 | 北京有色金属研究总院 | Electron-irradiation resisting shielding material and method for preparing same |
| CN103553691A (en) * | 2013-11-01 | 2014-02-05 | 广东工业大学 | Particle dispersion toughening aluminum nitride ceramic substrate and preparation method thereof |
| CN103819196A (en) * | 2013-12-30 | 2014-05-28 | 莱鼎电子材料科技有限公司 | Modified aluminum nitride ceramic substrate and production method thereof |
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