CN106220186A - A kind of preparation method of ceramic base electronic substrate - Google Patents
A kind of preparation method of ceramic base electronic substrate Download PDFInfo
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- CN106220186A CN106220186A CN201610636561.XA CN201610636561A CN106220186A CN 106220186 A CN106220186 A CN 106220186A CN 201610636561 A CN201610636561 A CN 201610636561A CN 106220186 A CN106220186 A CN 106220186A
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Abstract
The invention discloses the preparation method of a kind of ceramic base electronic substrate, belong to ceramic substrate material preparing technical field.After the present invention takes the mixing ultrasonic disperse such as Yttrium trinitrate, calcium nitrate, it is dried to constant weight, sintering nitridation prepares nano aluminum nitride, samaric nitrate mixing and ball milling after milling with dehydration, is dried to constant weight, calcines after pulverizing and sieving, mix with paraffin again, extruder grain, dry-pressing prepares idiosome, prepares ceramic base electronic substrate through binder removal, sintering.The invention has the beneficial effects as follows: preparation process of the present invention is simple, and products obtained therefrom sintering character is good, during sintering, pore-free produces, and material bending strength is high；Surface soundness is good, occurs without phenomenons such as the moisture absorption and electrode slurry are endosmosis.
Description
Technical field
The present invention relates to the preparation method of a kind of ceramic base electronic substrate, belong to ceramic substrate material technology of preparing neck
Territory.
Background technology
Baseplate material primarily serves semiconductor chip in Electronic Packaging and supports, dispels the heat, protects, insulate and mutual with external circuit
Effect even.Along with Electronic Encapsulating Technology develops towards high-frequency high-speed, multi-functional, high-performance, small size and high reliability direction,
Electronic package substrate material plays the most important effect in a new generation's electronic package material.Science and industrial quarters are to electricity
Sub-base plate for packaging material is had higher requirement, and also promotes electronic package substrate material simultaneously and develops rapidly.Ceramic substrate
Refer to that Copper Foil is at high temperature bonded directly to aluminium oxide (Al2O3) or aluminium nitride (AlN) ceramic substrate surface (single or double)
On special process plate.Made ultra-thin composite base plate has good electrical insulation performance, high thermal conduction characteristic, excellent solder
Property and high adhesive strength, and can etch various figure as pcb board, there is the biggest current capacity.Therefore, pottery
Substrate has become high-power electric and electronic circuit structure technology and the basic material of interconnection technique.Can be widely used for high-power electric
Semiconductor module；Semiconductor cooler, electronic heater；Power control circuit, power hybrid circuit；Intelligent power assembly；High
Frequently Switching Power Supply, solid-state relay；Automotive electronics, space flight and aviation and military electronic assembly；Solar cell panel assembly；Telecommunication is special
With switch, receive system；The industrial electronics such as laser.But owing to ceramic sintered bodies sintering character is poor, generate when high temperature sintering
A large amount of pores, make the bending strength of material reduce, cause the appearance of the moisture absorption and the phenomenon such as electrode slurry is endosmosis, material surface densification
Property is poor, limits the range of application of ceramic substrate material.
Summary of the invention
The technical problem to be solved: poor for ceramic sintered bodies sintering character, easily generates when high temperature sintering
A large amount of pores, make the bending strength of material reduce, cause the appearance of the moisture absorption and the phenomenon such as electrode slurry is endosmosis, material surface densification
Property poor drawback, it is provided that after one takes the mixing ultrasonic disperse such as Yttrium trinitrate, calcium nitrate, be dried to constant weight, sintering nitridation system
Obtain nano aluminum nitride, samaric nitrate mixing and ball milling after milling with dehydration, be dried to constant weight, calcine after pulverizing and sieving, then mix with paraffin
Closing, extruder grain, dry-pressing prepares idiosome, through the method that binder removal, sintering prepare ceramic base electronic substrate.The present invention prepares step
Rapid simple, products obtained therefrom sintering character is good, and during sintering, pore-free produces, and material bending strength is high, and surface soundness is good, efficient solution
The moisture absorption of having determined and the phenomenon produced problem such as electrode slurry is endosmosis.
For solving above-mentioned technical problem, the present invention uses the technical scheme as described below to be:
(1) weigh 2～3g Yttrium trinitrates respectively, 1～2g calcium nitrate, 100～120g aluminum nitrates, 15～20g glucoses, add 80～
In 100mL deionized water, with 300W ultrasonic echography disperse 15～20min, obtain mixed solution, mixed solution is placed in 120～
Being dried in 130 DEG C of baking ovens to constant weight, loaded by dried powder body in tube furnace, controlling temperature is 600～700 DEG C, at an oxygen
Change under carbon atmosphere, after calcining 1～2h, proceed in vacuum sintering furnace, be passed through the volume ratio nitrogen hydrogen as 19:1 with 1～2L/min speed
Gaseous mixture, and it is heated to 1300～1600 DEG C of sintering nitridations 3～4h, it is cooled to room temperature, obtains nano aluminum nitride；
(2) weigh 2～3g six nitric hydrate samariums and add processed 30～40min in 280～290 DEG C of drying baker, at dehydration
Samaric nitrate after reason loads in ball grinder, after adding 30～50mL dehydrated alcohol, is placed in ball mill, with 300r/min ball milling 30
～40min, add 90～92g above-mentioned nano aluminum nitrides, continue ball milling 2～3h, obtain composite mortar；
(3) above-mentioned composite mortar is placed in 110～120 DEG C of drying baker it is dried to constant weight, and add in pulverizer and pulverize, mistake
200 mesh sieves, the powder after sieving is placed in Muffle furnace, calcines 2～3h, naturally cool to room temperature, take at 600～650 DEG C
Go out the powder after calcining, it is placed in 90～100 DEG C of waters bath with thermostatic control with 6～8g paraffin and mixs homogeneously, be cooled to room temperature, obtain mixed
Close ceramic material；
(4) proceeding in comminutor by above-mentioned hybrid ceramic material, cross 60 mesh sieve pelletizes, the powder body after pelletize loads in dry press dry
Molded, obtain idiosome, gained idiosome is placed in high temperature box furnace, with 1 DEG C/min ramp to 180～200 DEG C, keep temperature
Degree binder removal 2～3h, is placed in the idiosome after binder removal in vacuum tube furnace, under nitrogen atmosphere, is heated to 1700～1750 DEG C, burns
Knot 2～3h, is cooled to room temperature, obtains ceramic base electronic substrate.
The ceramic base electronic substrate heat conductivity that the present invention prepares reaches 112.5～132.7W/(m K), thermal expansion system
Number is 6.0 × 10-6/ DEG C～7.0 × 10-6/ DEG C, bending strength is 286～328MPa, and breakdown strength is 46～52kV/mm, is situated between
Electric intensity is 8.1～9.3kV/mm.
The present invention is compared with additive method, and Advantageous Effects is:
(1) preparation process of the present invention is simple, and products obtained therefrom sintering character is good, and during sintering, pore-free produces, and material bending strength is high；
(2) surface soundness is good, occurs without phenomenons such as the moisture absorption and electrode slurry are endosmosis.
Detailed description of the invention
Weigh 2～3g Yttrium trinitrates, 1～2g calcium nitrate, 100～120g aluminum nitrates, 15～20g glucoses the most respectively, add
Enter in 80～100mL deionized waters, disperse 15～20min with 300W ultrasonic echography, obtain mixed solution, mixed solution is placed in
Being dried in 120～130 DEG C of baking ovens to constant weight, loaded by dried powder body in tube furnace, controlling temperature is 600～700 DEG C,
Under carbon monoxide atmosphere, after calcining 1～2h, proceed in vacuum sintering furnace, be passed through volume ratio as 19:1 with 1～2L/min speed
Nitrogen and hydrogen mixture, and it is heated to 1300～1600 DEG C of sintering nitridations 3～4h, it is cooled to room temperature, obtains nano aluminum nitride；Then weigh
2～3g six nitric hydrate samariums add processed 30～40min in 280～290 DEG C of drying baker, by the samaric nitrate after processed
Load in ball grinder, after adding 30～50mL dehydrated alcohol, be placed in ball mill, with 300r/min ball milling 30～40min, then add
Enter 90～92g above-mentioned nano aluminum nitrides, continue ball milling 2～3h, obtain composite mortar；Again above-mentioned composite mortar is placed in 110～120
Being dried to constant weight in DEG C drying baker, and add in pulverizer and pulverize, cross 200 mesh sieves, the powder after sieving is placed in Muffle furnace,
At 600～650 DEG C, calcine 2～3h, naturally cool to room temperature, take out the powder after calcining, itself and 6～8g paraffin are placed in 90
～mix homogeneously in 100 DEG C of waters bath with thermostatic control, it is cooled to room temperature, obtains hybrid ceramic material；Finally above-mentioned hybrid ceramic material is turned
Entering in comminutor, cross 60 mesh sieve pelletizes, the powder body after pelletize loads in dry press dry-pressing formed, obtains idiosome, is put by gained idiosome
In high temperature box furnace, with 1 DEG C/min ramp to 180～200 DEG C, keep temperature binder removal 2～3h, by the idiosome after binder removal
It is placed in vacuum tube furnace, under nitrogen atmosphere, is heated to 1700～1750 DEG C, sinter 2～3h, be cooled to room temperature, obtain ceramic
Base electronic substrate.
Example 1
Weigh 2g Yttrium trinitrate, 1g calcium nitrate, 100g aluminum nitrate, 15g glucose the most respectively, add in 80mL deionized water, with
300W ultrasonic echography dispersion 15min, obtains mixed solution, is placed in by mixed solution in 120 DEG C of baking ovens and is dried to constant weight, will be dried
After powder body load in tube furnace, controlling temperature is 600 DEG C, under carbon monoxide atmosphere, after calcining 1h, proceeds to vacuum sintering furnace
In, it is passed through the volume ratio nitrogen and hydrogen mixture as 19:1 with 1L/min speed, and is heated to 1300 DEG C of sintering nitridation 3h, be cooled to room
Temperature, obtains nano aluminum nitride；Then weigh 2g six nitric hydrate samarium and add processed 30min in 280 DEG C of drying baker, at dehydration
Samaric nitrate after reason loads in ball grinder, after adding 30mL dehydrated alcohol, is placed in ball mill, with 300r/min ball milling 30min,
Add the above-mentioned nano aluminum nitride of 90g, continue ball milling 2h, obtain composite mortar；Above-mentioned composite mortar is placed in 110 DEG C of drying baker again
In be dried to constant weight, and add in pulverizer pulverize, cross 200 mesh sieves, the powder after sieving is placed in Muffle furnace, at 600 DEG C
Lower calcining 2h, naturally cools to room temperature, takes out the powder after calcining, it is placed in 6g paraffin in 90 DEG C of waters bath with thermostatic control and mixes all
Even, it is cooled to room temperature, obtains hybrid ceramic material；Finally above-mentioned hybrid ceramic material is proceeded in comminutor, crosses 60 mesh sieve pelletizes,
Powder body after pelletize loads in dry press dry-pressing formed, obtains idiosome, is placed in high temperature box furnace by gained idiosome, with 1 DEG C/min
Ramp, to 180 DEG C, keeps temperature binder removal 2h, is placed in vacuum tube furnace by the idiosome after binder removal, under nitrogen atmosphere, adds
Heat, to 1700 DEG C, sinters 2h, is cooled to room temperature, obtains ceramic base electronic substrate.
Preparation process of the present invention is simple, and products obtained therefrom sintering character is good, and during sintering, pore-free produces, material bending strength
High；Surface soundness is good, occurs without phenomenons such as the moisture absorption and electrode slurry are endosmosis；The ceramic base electronic substrate heat conduction system prepared
Number reaches 112.5 W/(m K), thermal coefficient of expansion is 6.0 × 10-6/ DEG C, bending strength is 286MPa, and breakdown strength is 46kV/
Mm, dielectric strength is 8.1kV/mm.
Example 2
Weigh 3g Yttrium trinitrate, 2g calcium nitrate, 110g aluminum nitrate, 18g glucose the most respectively, add in 90mL deionized water, with
300W ultrasonic echography dispersion 18min, obtains mixed solution, is placed in by mixed solution in 125 DEG C of baking ovens and is dried to constant weight, will be dried
After powder body load in tube furnace, controlling temperature is 650 DEG C, under carbon monoxide atmosphere, after calcining 2h, proceeds to vacuum sintering furnace
In, it is passed through the volume ratio nitrogen and hydrogen mixture as 19:1 with 2L/min speed, and is heated to 1450 DEG C of sintering nitridation 4h, be cooled to room
Temperature, obtains nano aluminum nitride；Then weigh 3g six nitric hydrate samarium and add processed 35min in 285 DEG C of drying baker, at dehydration
Samaric nitrate after reason loads in ball grinder, after adding 40mL dehydrated alcohol, is placed in ball mill, with 300r/min ball milling 35min,
Add the above-mentioned nano aluminum nitride of 91g, continue ball milling 3h, obtain composite mortar；Above-mentioned composite mortar is placed in 115 DEG C of drying baker again
In be dried to constant weight, and add in pulverizer pulverize, cross 200 mesh sieves, the powder after sieving is placed in Muffle furnace, at 625 DEG C
Lower calcining 3h, naturally cools to room temperature, takes out the powder after calcining, it is placed in 7g paraffin in 95 DEG C of waters bath with thermostatic control and mixes all
Even, it is cooled to room temperature, obtains hybrid ceramic material；Finally above-mentioned hybrid ceramic material is proceeded in comminutor, crosses 60 mesh sieve pelletizes,
Powder body after pelletize loads in dry press dry-pressing formed, obtains idiosome, is placed in high temperature box furnace by gained idiosome, with 1 DEG C/min
Ramp, to 190 DEG C, keeps temperature binder removal 3h, is placed in vacuum tube furnace by the idiosome after binder removal, under nitrogen atmosphere, adds
Heat, to 1725 DEG C, sinters 3h, is cooled to room temperature, obtains ceramic base electronic substrate.
Preparation process of the present invention is simple, and products obtained therefrom sintering character is good, and during sintering, pore-free produces, material bending strength
High；Surface soundness is good, occurs without phenomenons such as the moisture absorption and electrode slurry are endosmosis；The ceramic base electronic substrate heat conduction system prepared
Number reaches 122.6 W/(m K), thermal coefficient of expansion is 6.5 × 10-6/ DEG C, bending strength is 307MPa, and breakdown strength is 49kV/
Mm, dielectric strength is 8.7kV/mm.
Example 3
Weigh 3g Yttrium trinitrate, 2g calcium nitrate, 120g aluminum nitrate, 20g glucose the most respectively, add in 100mL deionized water, with
300W ultrasonic echography dispersion 20min, obtains mixed solution, is placed in by mixed solution in 130 DEG C of baking ovens and is dried to constant weight, will be dried
After powder body load in tube furnace, controlling temperature is 700 DEG C, under carbon monoxide atmosphere, after calcining 2h, proceeds to vacuum sintering furnace
In, it is passed through the volume ratio nitrogen and hydrogen mixture as 19:1 with 2L/min speed, and is heated to 1600 DEG C of sintering nitridation 4h, be cooled to room
Temperature, obtains nano aluminum nitride；Then weigh 3g six nitric hydrate samarium and add processed 40min in 290 DEG C of drying baker, at dehydration
Samaric nitrate after reason loads in ball grinder, after adding 50mL dehydrated alcohol, is placed in ball mill, with 300r/min ball milling 40min,
Add the above-mentioned nano aluminum nitride of 92g, continue ball milling 3h, obtain composite mortar；Above-mentioned composite mortar is placed in 120 DEG C of drying baker again
In be dried to constant weight, and add in pulverizer pulverize, cross 200 mesh sieves, the powder after sieving is placed in Muffle furnace, at 650 DEG C
Lower calcining 3h, naturally cools to room temperature, takes out the powder after calcining, it is placed in 100 DEG C of waters bath with thermostatic control with 8g paraffin and mixes
Uniformly, it is cooled to room temperature, obtains hybrid ceramic material；Finally above-mentioned hybrid ceramic material is proceeded in comminutor, cross 60 mesh sieves and make
Grain, powder body after pelletize loads in dry press dry-pressing formed, obtains idiosome, be placed in high temperature box furnace by gained idiosome, with 1 DEG C/
Min ramp, to 200 DEG C, keeps temperature binder removal 3h, is placed in vacuum tube furnace by the idiosome after binder removal, at nitrogen atmosphere
Under, it is heated to 1750 DEG C, sinters 3h, be cooled to room temperature, obtain ceramic base electronic substrate.
Preparation process of the present invention is simple, and products obtained therefrom sintering character is good, and during sintering, pore-free produces, material bending strength
High；Surface soundness is good, occurs without phenomenons such as the moisture absorption and electrode slurry are endosmosis；The ceramic base electronic substrate heat conduction system prepared
Number reaches 132.7 W/(m K), thermal coefficient of expansion is 7.0 × 10-6/ DEG C, bending strength is 328MPa, and breakdown strength is 52kV/
Mm, dielectric strength is 9.3kV/mm.
Claims (1)
1. the preparation method of a ceramic base electronic substrate, it is characterised in that concrete preparation process is:
(1) weigh 2～3g Yttrium trinitrates respectively, 1～2g calcium nitrate, 100～120g aluminum nitrates, 15～20g glucoses, add 80～
In 100mL deionized water, with 300W ultrasonic echography disperse 15～20min, obtain mixed solution, mixed solution is placed in 120～
Being dried in 130 DEG C of baking ovens to constant weight, loaded by dried powder body in tube furnace, controlling temperature is 600～700 DEG C, at an oxygen
Change under carbon atmosphere, after calcining 1～2h, proceed in vacuum sintering furnace, be passed through the volume ratio nitrogen hydrogen as 19:1 with 1～2L/min speed
Gaseous mixture, and it is heated to 1300～1600 DEG C of sintering nitridations 3～4h, it is cooled to room temperature, obtains nano aluminum nitride；
(2) weigh 2～3g six nitric hydrate samariums and add processed 30～40min in 280～290 DEG C of drying baker, at dehydration
Samaric nitrate after reason loads in ball grinder, after adding 30～50mL dehydrated alcohol, is placed in ball mill, with 300r/min ball milling 30
～40min, add 90～92g above-mentioned nano aluminum nitrides, continue ball milling 2～3h, obtain composite mortar；
(3) above-mentioned composite mortar is placed in 110～120 DEG C of drying baker it is dried to constant weight, and add in pulverizer and pulverize, mistake
200 mesh sieves, the powder after sieving is placed in Muffle furnace, calcines 2～3h, naturally cool to room temperature, take at 600～650 DEG C
Go out the powder after calcining, it is placed in 90～100 DEG C of waters bath with thermostatic control with 6～8g paraffin and mixs homogeneously, be cooled to room temperature, obtain mixed
Close ceramic material；
(4) proceeding in comminutor by above-mentioned hybrid ceramic material, cross 60 mesh sieve pelletizes, the powder body after pelletize loads in dry press dry
Molded, obtain idiosome, gained idiosome is placed in high temperature box furnace, with 1 DEG C/min ramp to 180～200 DEG C, keep temperature
Degree binder removal 2～3h, is placed in the idiosome after binder removal in vacuum tube furnace, under nitrogen atmosphere, is heated to 1700～1750 DEG C, burns
Knot 2～3h, is cooled to room temperature, obtains ceramic base electronic substrate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108516837A (en) * | 2018-04-24 | 2018-09-11 | 常州思宇知识产权运营有限公司 | A kind of microwave attenuative ceramics and preparation method thereof |
| CN108863393A (en) * | 2018-07-03 | 2018-11-23 | 北京科技大学 | A kind of preparation method of high thermal conductivity and high-intensitive aluminium nitride ceramics |
| CN110759750A (en) * | 2019-11-01 | 2020-02-07 | 吴俊楠 | Preparation method of high-thermal-conductivity ceramic material for LED |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108516837A (en) * | 2018-04-24 | 2018-09-11 | 常州思宇知识产权运营有限公司 | A kind of microwave attenuative ceramics and preparation method thereof |
| CN108863393A (en) * | 2018-07-03 | 2018-11-23 | 北京科技大学 | A kind of preparation method of high thermal conductivity and high-intensitive aluminium nitride ceramics |
| CN110759750A (en) * | 2019-11-01 | 2020-02-07 | 吴俊楠 | Preparation method of high-thermal-conductivity ceramic material for LED |
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