CN107602095A - A kind of high thermal conductivity ceramic substrate and preparation method thereof - Google Patents

A kind of high thermal conductivity ceramic substrate and preparation method thereof Download PDF

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CN107602095A
CN107602095A CN201710956913.4A CN201710956913A CN107602095A CN 107602095 A CN107602095 A CN 107602095A CN 201710956913 A CN201710956913 A CN 201710956913A CN 107602095 A CN107602095 A CN 107602095A
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ceramic substrate
thermal conductivity
powder
high thermal
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CN107602095B (en
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王若梅
徐颜峰
陈龙
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Guangdong Weishi New Materials Co ltd
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Abstract

The invention discloses a kind of high thermal conductivity ceramic substrate and preparation method thereof, belong to electronic package material technical field.Count in parts by weight, weigh 70~80 parts of alumina powders, 10~15 parts of brown iron oxides, 20~25 parts of cupric oxide powders, 20~25 parts of carbon dusts, 13~18 parts of boron oxide powders, 12~16 parts of modified glass-fibers, 8~14 parts of metallic oxide crystal whiskers and 3~5 parts of ice crystals successively;By carbon dust, boron oxide powder, after ice crystal and modified glass-fiber mixing and ball milling, sieving, obtains compound powder, by compound powder, alumina powder, after brown iron oxide, cupric oxide powder and metallic oxide crystal whisker mixing, add in mould, it is compressing in mould, blank is obtained, blank is moved into sintering furnace and sintered, obtains high thermal conductivity ceramic substrate.Ceramic substrate prepared by the present invention has excellent heat conductivility and mechanical strength.

Description

A kind of high thermal conductivity ceramic substrate and preparation method thereof
Technical field
The invention discloses a kind of high thermal conductivity ceramic substrate and preparation method thereof, belongs to electronic package material technology neck Domain.
Background technology
During Electronic Packaging, substrate mainly plays mechanical support protection and is electrically interconnected(Insulation)Effect.With electronic seal Dress technology gradually develops towards miniaturization, high density, multi-functional and high reliability direction, and the power density of electronic system increases therewith Add, heat dissipation problem is increasingly severe.Good general does not cause device performance degradation, structural failure, is layered or burns for radiating.Good device Part radiating depends on the heat radiation structure design of optimization, encapsulating material selection(Thermal interfacial material and heat-radiating substrate)And encapsulation manufacture work Skill etc..Wherein, the selection of baseplate material is key link, directly influences device cost, performance and reliability.
Electronic Packaging is as follows to baseplate material performance requirement:Thermal conductivity is high, and dielectric constant is low, the thermal expansion with chip material Coefficients match, mechanical strength is high, and processing characteristics is good, and cost is low etc..In fact, above-mentioned performance is difficult to meet simultaneously, sometimes even It is conflicting, it can only be selected in practical application according to specific encapsulated object.Conventional baseplate material mainly includes plastics base Plate, metal substrate, ceramic substrate and the major class of composite base plate four.At present, although ceramic substrate is not in leading position, but due to The continuous reduction of its good thermal conductivity, heat resistance, insulating properties, low thermal coefficient of expansion and cost, in Electronic Packaging particularly work( Rate electronic device such as IGBT(Igbt)、LD(Laser diode), great power LED(Light emitting diode)、CPV (Focus type photovoltaic)Application in encapsulation is more and more extensive.For a long time, most ceramic substrate materials continue to use oxidation always Aluminium and beryllium oxide ceramics, but the thermal conductivity of aluminum oxide substrate is low, and thermal coefficient of expansion and silicon less match;Although beryllium oxide has excellent Good combination property, but its higher production cost and it is hypertoxic the shortcomings that limit its application.Therefore from performance, cost Consider that the two can not fully meet the needs of modern electronic devices development with factors such as environmental protection.
Therefore, the shortcomings that how improving traditional ceramics substrate mechanical property and bad heat conductivility, to obtain higher synthesis The ceramic substrate of performance, it is that it is promoted and is applied to broader field, meets industrial production demand urgent problem to be solved.
The content of the invention
The present invention solves the technical problem of:Lacked for traditional ceramics substrate mechanical property and heat conductivility are bad A kind of point, there is provided high thermal conductivity ceramic substrate and preparation method thereof.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of high thermal conductivity ceramic substrate, is made up of the raw material of following parts by weight:
70~80 parts of alumina powder
10~15 parts of brown iron oxide
20~25 parts of cupric oxide powder
20~25 parts of carbon dust
13~18 parts of boron oxide powder
12~16 parts of modified glass-fiber
8~14 parts of metallic oxide crystal whisker
3~5 parts of ice crystal
The preparation method of the modified glass-fiber is:
By nano silicon and silane coupler in mass ratio 8:11~10:11 mixing, and add nano silicon quality 10~12 times of absolute ethyl alcohol, after being stirred, treatment fluid is obtained, by glass fibre and treatment fluid in mass ratio 1:6~1:8 is mixed Close, sonic oscillation, filter, dry, obtain modified glass-fiber;
The preparation method of the high thermal conductivity ceramic substrate is:
(1)Formed by raw material and weigh each component;
(2)By carbon dust, boron oxide powder, after ice crystal and modified glass-fiber mixing and ball milling, sieving, compound powder is obtained, will be mixed After conjunction feed powder end, alumina powder, brown iron oxide, cupric oxide powder and metallic oxide crystal whisker mixing, add in mould, in mould It is compressing, blank is obtained, blank is moved into sintering furnace and sintered, obtains high thermal conductivity ceramic substrate.
The metallic oxide crystal whisker is any one in magnesia crystal whisker or cupric oxide whisker.
The glass fibre is any one in alkali-free glass fibre or medium-alkali glass fibre.
The silane coupler is silane coupler KH-560, in silane resin acceptor kh-550 or Silane coupling reagent KH-570 Any one.
Step(2)The compressing condition be prior to pressure be 80~90MPa suppress 30~45s, be then at pressure 100~110MPa suppresses 100~110s.
The beneficial effects of the invention are as follows:
(1)The present invention adds brown iron oxide, cupric oxide powder and carbon dust, first, iron oxide when preparing high thermal conductivity ceramic substrate The addition of powder and cupric oxide powder can serve as fluxing agent, make the sintering temperature of ceramic substrate reduce, from the cause for making aluminium oxide ceramics Density improves, and then is improved the mechanical property of product, and secondly, in sintering process, the carbon in carbon dust can be with oxygen reduction Change iron powder and iron and copper in cupric oxide powder, and the density of iron and copper is both greater than the density of aluminum oxide, therefore in sintering process In the iron that is displaced and a copper part can be deposited on substrate bottom, subsequently with copper foil recombination process, be advantageous to substrate with The welding of copper foil, both compatibilities are improved, and effectively reduce thermal contact resistance, overall thermal conductivity energy is improved, in addition, part iron and copper Two layers uniform layers of copper and iron layer can be formed in alumina ceramic face, and firm mode combines, so that product surface Thermal conductivity improve, furthermore the addition of carbon dust can react with silica, generation carborundum be distributed in ceramic substrate In system, it is improved the heat conductivility of product;
(2)The present invention adds modified glass fibre peacekeeping metallic oxide crystal whisker when preparing high thermal conductivity ceramic substrate, on the one hand, Surface-active is improved glass fibre after modification, and contact site is increased, and after adding in ceramic substrate system, can be made in system Adhesion enhancing between each material, so that the mechanical property of product is improved, on the other hand, modified glass fibre peacekeeping metal The addition of oxide whisker, the hole left after carbon dust reaction can be filled, so that the consistency of ceramic substrate system is carried Height, and then it is improved the mechanical property of product.
Brief description of the drawings
Fig. 1 ceramic substrates heat conductivility and mechanics properties testing result.
Embodiment
By nano silicon and silane coupler in mass ratio 8:11~10:11 are mixed in beaker, and into beaker The absolute ethyl alcohol of 10~12 times of nano silicon quality is added, beaker immigration digital display is tested the speed constant temperature blender with magnetic force, Yu Wen Spend for 45~60 DEG C, under conditions of rotating speed is 300~360r/min, after being stirred, obtain treatment fluid, by glass fibre and processing Liquid in mass ratio 1:6~1:8 are mixed in flask, and flask is moved into sonic oscillation instrument, under conditions of frequency is 45~55kHz After 15~22min of sonic oscillation, filtering, filter cake is obtained, filter cake is moved into drying box, dried under conditions of being 75~90 DEG C in temperature 60~80min, obtain modified glass-fiber;Count in parts by weight, weigh 70~80 parts of alumina powders, 10~15 parts of iron oxide successively Powder, 20~25 parts of cupric oxide powders, 20~25 parts of carbon dusts, 13~18 parts of boron oxide powders, 12~16 parts of modified glass-fibers, 8~14 Part metallic oxide crystal whisker and 3~5 parts of ice crystals;By carbon dust, boron oxide powder, ice crystal and modified glass-fiber add mixer In be stirred, obtain compound, add mixture into ball mill, and into ball mill add 4~5 times of mixture quality oxygen Change zirconium ball milling pearl, after 2~3h of ball milling, cross 100~120 mesh sieves, obtain compound powder, by compound powder, alumina powder, oxidation Iron powder, cupric oxide powder and metallic oxide crystal whisker mixing after, add mould in, by mould move into forcing press in, in temperature be 70 It is compressing under conditions of~80 DEG C, blank is obtained, blank is moved into sintering furnace, is led to 80~120mL/min speed into stove Enter argon gas, under argon gas guard mode, under conditions of temperature is 1150~1300 DEG C, sinter molding, cool to room temperature with the furnace Afterwards, come out of the stove, obtain high thermal conductivity ceramic substrate.The metallic oxide crystal whisker is any one in magnesia crystal whisker or cupric oxide whisker Kind.The glass fibre is any one in alkali-free glass fibre or medium-alkali glass fibre.The silane coupler is that silane is even Join agent KH-560, any one in silane resin acceptor kh-550 or Silane coupling reagent KH-570.The compressing condition is It is that 80~90MPa suppresses 30~45s prior to pressure, is that 100~110MPa suppresses 100~110s then at pressure.
Example 1
By nano silicon and silane coupler in mass ratio 10:11 are mixed in beaker, and nanometer two is added into beaker The absolute ethyl alcohol that 12 times of siliconoxide mass, beaker immigration digital display is tested the speed constant temperature blender with magnetic force, is 60 DEG C in temperature, rotating speed is Under conditions of 360r/min, after being stirred, treatment fluid is obtained, by glass fibre and treatment fluid in mass ratio 1:8 are mixed in flask In, flask is moved into sonic oscillation instrument, after sonic oscillation 22min under conditions of frequency is 55kHz, filtering, filter cake is obtained, will filter Cake moves into drying box, dries 80min under conditions of being 90 DEG C in temperature, obtains modified glass-fiber;Count, claim successively in parts by weight Take 80 parts of alumina powders, 15 parts of brown iron oxides, 25 parts of cupric oxide powders, 25 parts of carbon dusts, 18 parts of boron oxide powders, 16 parts of modified glass fibres Dimension, 14 parts of metallic oxide crystal whiskers and 5 parts of ice crystals;By carbon dust, boron oxide powder, ice crystal and modified glass-fiber add stirring It is stirred in machine, obtains compound, added mixture into ball mill, and the oxygen of 5 times of mixture quality is added into ball mill Change zirconium ball milling pearl, after ball milling 3h, cross 120 mesh sieves, compound powder is obtained, by compound powder, alumina powder, brown iron oxide, oxygen After changing copper powder and metallic oxide crystal whisker mixing, add in mould, mould is moved into forcing press, in the condition that temperature is 80 DEG C Under it is compressing, obtain blank, by blank move into sintering furnace in, argon gas is passed through into stove with 120mL/min speed, argon gas protect Under state, under conditions of temperature is 1300 DEG C, sinter molding, after cooling to room temperature with the furnace, comes out of the stove, obtain high thermal conductivity ceramic base Plate.The metallic oxide crystal whisker is magnesia crystal whisker.The glass fibre is alkali-free glass fibre.The silane coupler is Silane coupler KH-560.The compressing condition is 110MPa then at pressure to be that 90MPa suppresses 45s prior to pressure Suppress 110s.
Example 2
By nano silicon and silane coupler in mass ratio 10:11 are mixed in beaker, and nanometer two is added into beaker The absolute ethyl alcohol that 12 times of siliconoxide mass, beaker immigration digital display is tested the speed constant temperature blender with magnetic force, is 60 DEG C in temperature, rotating speed is Under conditions of 360r/min, after being stirred, treatment fluid is obtained, by glass fibre and treatment fluid in mass ratio 1:8 are mixed in flask In, flask is moved into sonic oscillation instrument, after sonic oscillation 22min under conditions of frequency is 55kHz, filtering, filter cake is obtained, will filter Cake moves into drying box, dries 80min under conditions of being 90 DEG C in temperature, obtains modified glass-fiber;Count, claim successively in parts by weight Take 80 parts of alumina powders, 18 parts of boron oxide powders, 16 parts of modified glass-fibers, 14 parts of metallic oxide crystal whiskers and 5 parts of ice crystals;Will Boron oxide powder, ice crystal and modified glass-fiber are added in mixer and are stirred, and are obtained compound, are added mixture into ball mill In, and the zirconium oxide ball milling pearl of 5 times of mixture quality is added into ball mill, after ball milling 3h, 120 mesh sieves are crossed, obtain compound powder End, by compound powder, after alumina powder and metallic oxide crystal whisker mixing, add in mould, mould moved into forcing press, It is compressing under conditions of temperature is 80 DEG C, blank is obtained, blank is moved into sintering furnace, with 120mL/min speed into stove Argon gas is passed through, under argon gas guard mode, under conditions of temperature is 1300 DEG C, sinter molding, after cooling to room temperature with the furnace, is gone out Stove, obtain high thermal conductivity ceramic substrate.The metallic oxide crystal whisker is magnesia crystal whisker.The glass fibre is that alkali-free glass is fine Dimension.The silane coupler is silane coupler KH-560.The compressing condition be prior to pressure be 90MPa compacting 45s, it is that 110MPa suppresses 110s then at pressure.
Example 3
Count in parts by weight, weigh 80 parts of alumina powders successively, 15 parts of brown iron oxides, 25 parts of cupric oxide powders, 25 parts of carbon dusts, 18 parts Boron oxide powder, 16 parts of glass fibres, 14 parts of metallic oxide crystal whiskers and 5 parts of ice crystals;By carbon dust, boron oxide powder, ice crystal and Glass fibre is added in mixer and is stirred, and is obtained compound, is added mixture into ball mill, and is added and mixed into ball mill The zirconium oxide ball milling pearl of 5 times of quality of material is closed, after ball milling 3h, 120 mesh sieves is crossed, compound powder is obtained, by compound powder, aluminum oxide After powder, brown iron oxide, cupric oxide powder and metallic oxide crystal whisker mixing, add in mould, mould is moved into forcing press, Yu Wen Spend to be compressing under conditions of 80 DEG C, obtain blank, blank is moved into sintering furnace, is passed through with 120mL/min speed into stove Argon gas, under argon gas guard mode, under conditions of temperature is 1300 DEG C, sinter molding, after cooling to room temperature with the furnace, come out of the stove, Obtain high thermal conductivity ceramic substrate.The metallic oxide crystal whisker is magnesia crystal whisker.The glass fibre is alkali-free glass fibre. The silane coupler is silane coupler KH-560.The compressing condition be prior to pressure be 90MPa suppress 45s, It is that 110MPa suppresses 110s then at pressure.
Example 4
By nano silicon and silane coupler in mass ratio 10:11 are mixed in beaker, and nanometer two is added into beaker The absolute ethyl alcohol that 12 times of siliconoxide mass, beaker immigration digital display is tested the speed constant temperature blender with magnetic force, is 60 DEG C in temperature, rotating speed is Under conditions of 360r/min, after being stirred, treatment fluid is obtained, by glass fibre and treatment fluid in mass ratio 1:8 are mixed in flask In, flask is moved into sonic oscillation instrument, after sonic oscillation 22min under conditions of frequency is 55kHz, filtering, filter cake is obtained, will filter Cake moves into drying box, dries 80min under conditions of being 90 DEG C in temperature, obtains modified glass-fiber;Count, claim successively in parts by weight Take 80 parts of alumina powders, 15 parts of brown iron oxides, 25 parts of cupric oxide powders, 25 parts of carbon dusts, 18 parts of boron oxide powders, 16 parts of modified glass fibres 5 parts of ice crystals of peacekeeping;By carbon dust, boron oxide powder, ice crystal and modified glass-fiber are added in mixer and are stirred, and must be mixed Material, is added mixture into ball mill, and the zirconium oxide ball milling pearl of 5 times of mixture quality is added into ball mill, after ball milling 3h, 120 mesh sieves are crossed, obtain compound powder, by compound powder, alumina powder, brown iron oxide, after cupric oxide powder mixing, add mould In, mould is moved into forcing press, it is compressing under conditions of temperature is 80 DEG C, blank is obtained, blank is moved into sintering furnace, Argon gas is passed through into stove with 120mL/min speed, under argon gas guard mode, under conditions of temperature is 1300 DEG C, sintered into Type, after cooling to room temperature with the furnace, come out of the stove, obtain high thermal conductivity ceramic substrate.The silane coupler is silane coupler KH-560. The compressing condition is that 110MPa suppresses 110s then at pressure to be that 90MPa suppresses 45s prior to pressure.
Comparative example:The ceramic substrate of circuit board Co., Ltd of Shenzhen production.
The high thermal conductivity ceramic substrate of the gained of example 1 to 4 and comparative example product are subjected to performance detection, specific detection method It is as follows:
1. heat conductivility:Using thermal resistance tester(The body heat resistance of measurable multiple solutions system and interface resistance)To test specimen Thermal Synthetic Conductance is detected;
2. mechanical property:Test specimen tensile strength is detected according to GB/T14619.
Specific testing result is shown in brief description of the drawings, from brief description of the drawings Fig. 1 testing results, technical solution of the present invention preparation High thermal conductivity ceramic substrate its mechanical property while its heat conductivility is improved also significantly improves, in pottery electronic package material skill Had broad prospects in the development in art field.

Claims (5)

  1. A kind of 1. high thermal conductivity ceramic substrate, it is characterised in that:It is made up of the raw material of following parts by weight:
    70~80 parts of alumina powder
    10~15 parts of brown iron oxide
    20~25 parts of cupric oxide powder
    20~25 parts of carbon dust
    13~18 parts of boron oxide powder
    12~16 parts of modified glass-fiber
    8~14 parts of metallic oxide crystal whisker
    3~5 parts of ice crystal
    The preparation method of the modified glass-fiber is:
    By nano silicon and silane coupler in mass ratio 8:11~10:11 mixing, and add nano silicon quality 10~12 times of absolute ethyl alcohol, after being stirred, treatment fluid is obtained, by glass fibre and treatment fluid in mass ratio 1:6~1:8 is mixed Close, sonic oscillation, filter, dry, obtain modified glass-fiber;
    The preparation method of the high thermal conductivity ceramic substrate is:
    (1)Formed by raw material and weigh each component;
    (2)By carbon dust, boron oxide powder, after ice crystal and modified glass-fiber mixing and ball milling, sieving, compound powder is obtained, will be mixed After conjunction feed powder end, alumina powder, brown iron oxide, cupric oxide powder and metallic oxide crystal whisker mixing, add in mould, in mould It is compressing, blank is obtained, blank is moved into sintering furnace and sintered, obtains high thermal conductivity ceramic substrate.
  2. A kind of 2. high thermal conductivity ceramic substrate according to claim 1, it is characterised in that:The metallic oxide crystal whisker is Any one in magnesia crystal whisker or cupric oxide whisker.
  3. A kind of 3. high thermal conductivity ceramic substrate according to claim 1, it is characterised in that:The glass fibre is alkali-free glass Any one in glass fiber or medium-alkali glass fibre.
  4. A kind of 4. high thermal conductivity ceramic substrate according to claim 1, it is characterised in that:The silane coupler is silane Any one in coupling agent KH-560, silane resin acceptor kh-550 or Silane coupling reagent KH-570.
  5. A kind of 5. high thermal conductivity ceramic substrate according to claim 1, it is characterised in that:Step(2)It is described compressing Condition be prior to pressure be 80~90MPa suppress 30~45s, then at pressure be 100~110MPa suppress 100~110s.
CN201710956913.4A 2017-10-16 2017-10-16 High-thermal-conductivity ceramic substrate and preparation method thereof Active CN107602095B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108484182A (en) * 2018-04-08 2018-09-04 江苏中翼汽车新材料科技有限公司 Magnesium oxide-based ceramic foam filter of a kind of magnesia crystal whisker fabricated in situ magnesium aluminate spinel enhancing and preparation method thereof
CN112110718A (en) * 2020-11-18 2020-12-22 广东欧文莱陶瓷有限公司 Ceramic tile with natural touch and preparation method thereof
CN112723892A (en) * 2021-01-07 2021-04-30 林萍华 Preparation method of ceramic material with excellent thermal conductivity and ceramic material
CN115093203A (en) * 2022-07-07 2022-09-23 张欢湛 Preparation method of carbon-based aluminum oxide composite material

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105236942A (en) * 2015-11-11 2016-01-13 苏州宽温电子科技有限公司 High-heat-conduction ceramic substrate material and preparing method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105236942A (en) * 2015-11-11 2016-01-13 苏州宽温电子科技有限公司 High-heat-conduction ceramic substrate material and preparing method thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108484182A (en) * 2018-04-08 2018-09-04 江苏中翼汽车新材料科技有限公司 Magnesium oxide-based ceramic foam filter of a kind of magnesia crystal whisker fabricated in situ magnesium aluminate spinel enhancing and preparation method thereof
WO2019196178A1 (en) * 2018-04-08 2019-10-17 江苏中翼汽车新材料科技有限公司 Magnesium aluminate spinel reinforced magnesium oxide-based foam ceramic filter synthesized in situ from magnesium oxide whisker, and preparation method therefor
US20200316505A1 (en) * 2018-04-08 2020-10-08 Jiangsu Zhongyi Automobile New Material Technology Co., Ltd. Magnesium aluminate spinel reinforced magnesium oxide-based foam ceramic filter synthesized in situ from magnesium oxide whisker, and preparation method therefor
US11702366B2 (en) * 2018-04-08 2023-07-18 Jiangsu Zhongyi Automobile New Material Technology Co., Ltd. Magnesium aluminate spinel reinforced magnesium oxide-based foam ceramic filter synthesized in situ from magnesium oxide whisker, and preparation method therefor
CN112110718A (en) * 2020-11-18 2020-12-22 广东欧文莱陶瓷有限公司 Ceramic tile with natural touch and preparation method thereof
CN112723892A (en) * 2021-01-07 2021-04-30 林萍华 Preparation method of ceramic material with excellent thermal conductivity and ceramic material
CN112723892B (en) * 2021-01-07 2022-06-10 东莞市钧杰陶瓷科技有限公司 Preparation method of ceramic material with excellent thermal conductivity and ceramic material
CN115093203A (en) * 2022-07-07 2022-09-23 张欢湛 Preparation method of carbon-based aluminum oxide composite material

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