CN107417282A - A kind of preparation method of low-temperature pressureless sintering aluminium nitride ceramics - Google Patents

A kind of preparation method of low-temperature pressureless sintering aluminium nitride ceramics Download PDF

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CN107417282A
CN107417282A CN201610344841.3A CN201610344841A CN107417282A CN 107417282 A CN107417282 A CN 107417282A CN 201610344841 A CN201610344841 A CN 201610344841A CN 107417282 A CN107417282 A CN 107417282A
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nitride ceramics
aluminium nitride
low
preparation
pressureless sintering
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吴诚
刘久明
高勇
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Hebei Corefra Silicon Nitride Material Co Ltd
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Hebei Corefra Silicon Nitride Material Co Ltd
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    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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Abstract

The present invention provides a kind of preparation method of low-temperature pressureless sintering aluminium nitride ceramics.Aluminium nitride ceramics in the present invention is using high purity silicon nitride aluminium powder body as raw material, diopside powder and yttrium fluoride powder are used as sintering aid, the addition of sintering aid is 5wt% 15wt%, aluminium nitride ceramics is formed using low-temperature pressureless sintering mode, the aluminium nitride ceramics thermal conductivity of gained is more than 200W/ (m.k), and 3 rupture strengths can reach more than 300MPa.The present invention has the characteristics of technique is simple, and cost is cheap, is adapted to industrialized production.

Description

A kind of preparation method of low-temperature pressureless sintering aluminium nitride ceramics
Technical field
The invention belongs to non-oxide ceramicses technical field.More particularly to a kind of preparation method of low-temperature pressureless sintering aluminium nitride ceramics.
Background technology
With high-power and super large-scale integration development, the highly dense of integrated circuit causes the caloric value of the electronic component of unit area to sharply increase, if not solving the heat dissipation problem of substrate, electronic component will be difficult to normal work.So require baseplate material that there is high thermal conductivity, while have higher resistivity concurrently.Traditional baseplate material has Al2O3Ceramics and BeO ceramics, but Al2O3Ceramic substrate thermal conductivity is low, and linear expansion coefficient less matches with Si；BeO ceramics of the consistency up to more than 99%, its thermal conductivity at room temperature can reach 310W.m-1.K-1, but production cost is high and has severe toxicity, thus limit its application and popularization.Aluminium nitride ceramics is a kind of new highly heat-conductive material, the W.m of theoretical conductivity 320-1.K-1.Aluminium nitride ceramics hardness is high simultaneously, and thermal coefficient of expansion approaches with silicon, and body resistivity is higher, in addition the material non-toxic, corrosion-and high-temp-resistant, and its combination property is better than aluminum oxide and beryllium oxide, is new generation of semiconductor substrate and the ideal material of electron device package.
Patent CN105084904A discloses the preparation method of aluminium nitride ceramics material, and its method is：First, activated aluminosilicate material is prepared；2nd, alkali-activated carbonatite solution is prepared；3rd, slurry is prepared；4th, blank is prepared；5th, high-temperature process, that is, the preparation method of aluminium nitride ceramics material is completed.Patent CN103204682A discloses a kind of high heat conduction aluminium nitride ceramics heat dispersion substrate and preparation method thereof, the high heat conduction aluminium nitride ceramics heat dispersion substrate is to use aluminium nitride as primary raw material, the heat dispersion substrate of ceramics that the thermal conductivity being prepared by vibrating hot pressed sintering is 200 ~ 260W/ (mK).The invention also discloses a kind of preparation method of high heat conduction aluminium nitride ceramics heat dispersion substrate, including：Blank Jing Guo preliminary treatment is dry-pressing formed；The blank is subjected to ungrease treatment by vacuum degreasing stove；The blank Jing Guo degreasing is burnt till by vibrating in hot-pressed sintering furnace, obtains just finished product；By just finished product thermal insulation pressurize 0.5 ~ 8 hour, furnace cooling obtains aluminium nitride ceramics heat dispersion substrate.It can be seen that the preparation technology of the getable aluminium nitride ceramics of the above method is complex, the aluminium nitride ceramics of high thermal conductivity is obtained using hot pressed sintering and high-temperature process.
The content of the invention
In order to overcome current aluminium nitride ceramics preparation technology complicated and using hot pressed sintering by the way of, a kind of preparation method of low-temperature pressureless sintering aluminium nitride ceramics of present invention proposition, specifically：
（1）Using high purity silicon nitride aluminium powder body and additional 5wt%-10wt% diopsides powder and additional 1wt%-5wt% yttrium fluorides as raw material；
（2）After step (1) raw material addition absolute ethyl alcohol is mixed, it is subsequently placed in 100 DEG C of baking ovens and dries, add the PVB ethanol solutions that 8wt%-18wt% mass fractions are 5wt%, it is well mixed to be granulated, 200-400MPa forming under the pressure is put into, aluminium nitride ceramics is obtained under the conditions of 1500 DEG C -1650 DEG C, insulation 1-5h.
Low-temperature pressureless sintering aluminium nitride ceramics preparation method as described above, it is characterised in that described high purity silicon nitride aluminium purity is more than or equal to 99%, and granularity is between 0.2-2 μm.
Low-temperature pressureless sintering aluminium nitride ceramics preparation method as described above, it is characterised in that diopside powder is prepared by calcium carbonate, magnesia and silica.
Low-temperature pressureless sintering aluminium nitride ceramics preparation method as described above, it is characterised in that PVB addition is in 8wt%-18wt%.
Low-temperature pressureless sintering aluminium nitride ceramics preparation method as described above, it is characterised in that briquetting pressure 200-400MPa.
Low-temperature pressureless sintering aluminium nitride ceramics preparation method as described above, it is characterised in that the temperature of pressureless sintering is 1500 DEG C -1650 DEG C, and soaking time is 1-5h.
Low-temperature pressureless sintering aluminium nitride ceramics preparation method as described above, it is characterised in that the aluminium nitride ceramics thermal conductivity of preparation is more than 200W/ (m.k), and 3 rupture strengths are more than 300MPa.
The present invention, which provides a kind of low-temperature pressureless sintering aluminium nitride ceramics, has advantages below：
(1) creative proposition low-temperature pressureless sintering prepares aluminium nitride ceramics;
(2) preparation method technique is simple, feasible, is adapted to industrialized production;
(3) the aluminium nitride ceramics function admirable prepared by, thermal conductivity are more than 200W/ (m.k), and 3 rupture strengths can reach more than 300MPa.
Brief description of the drawings
Fig. 1 is the preparation flow figure of high thermal conductivity silicon nitride ceramics in the present invention；
Fig. 2 is the aluminium nitride ceramics sample prepared in the present invention.
Embodiment：
The characteristics of the present invention is furture elucidated below by example, but it is not limited to embodiment.
Embodiment 1
After high purity silicon nitride aluminium powder body is uniformly mixed with the raw material such as additional 10% diopside powder and additional 1% yttrium fluoride addition absolute ethyl alcohol, it is placed in drying box drying, add the PVB ethanol solutions that 18wt% mass fractions are 5wt%, it is well mixed to be granulated, 400MPa forming under the pressure is put into, aluminium nitride ceramics is obtained in 1650 DEG C, insulation 2h.330MPa can be arrived to 245 W/ (m.k), 3 rupture strengths by aluminium nitride ceramics thermal conductivity made above.
Embodiment 2
After high purity silicon nitride aluminium powder body is uniformly mixed with the raw material such as additional 8% diopside powder and additional 4% yttrium fluoride addition absolute ethyl alcohol, it is placed in drying box drying, add the PVB ethanol solutions that 12wt% mass fractions are 5wt%, it is well mixed to be granulated, 320MPa forming under the pressure is put into, aluminium nitride ceramics is obtained in 1600 DEG C, insulation 4h.306MPa can be arrived to 212 W/ (m.k), 3 rupture strengths by aluminium nitride ceramics thermal conductivity made above.
Embodiment 3
After high purity silicon nitride aluminium powder body is uniformly mixed with the raw material such as additional 5% diopside powder and additional 4% yttrium fluoride addition absolute ethyl alcohol, it is placed in drying box drying, add the PVB ethanol solutions that 14wt% mass fractions are 5wt%, it is well mixed to be granulated, 280MPa forming under the pressure is put into, aluminium nitride ceramics is obtained in 1580 DEG C, insulation 3h.301MPa can be arrived to 210 W/ (m.k), 3 rupture strengths by aluminium nitride ceramics thermal conductivity made above.
Embodiment 4
After high purity silicon nitride aluminium powder body is uniformly mixed with the raw material such as additional 7% diopside powder and additional 3% yttrium fluoride addition absolute ethyl alcohol, it is placed in drying box drying, add the PVB ethanol solutions that 15wt% mass fractions are 5wt%, it is well mixed to be granulated, 364MPa forming under the pressure is put into, aluminium nitride ceramics is obtained in 1620 DEG C, insulation 2h.335MPa can be arrived to 234 W/ (m.k), 3 rupture strengths by aluminium nitride ceramics thermal conductivity made above.

Claims (7)

1. a kind of preparation method of low-temperature pressureless sintering aluminium nitride ceramics, including dispensing, mixing, granulation, shaping and sintering, it is characterised in that：
（1）Using high purity silicon nitride aluminium powder body and additional 5wt%-10wt% diopsides powder and additional 1wt%-5wt% yttrium fluorides as raw material；
（2）The raw material that step (1) is got ready is added into absolute ethyl alcohol to be mixed, it is subsequently placed in 100 DEG C of baking ovens and dries, add the PVB ethanol solutions that 8wt%-18wt% mass fractions are 5wt%, it is well mixed to be granulated, 200-400MPa forming under the pressure is put into, aluminium nitride ceramics is obtained under the conditions of 1500 DEG C -1650 DEG C, insulation 1-5h.
2. low-temperature pressureless sintering aluminium nitride ceramics preparation method according to claim 1, it is characterised in that described high purity silicon nitride aluminium purity is more than or equal to 99%, and granularity is between 0.2-2 μm.
3. low-temperature pressureless sintering aluminium nitride ceramics preparation method according to claim 1, it is characterised in that diopside powder is prepared by calcium carbonate, magnesia and silica.
4. low-temperature pressureless sintering aluminium nitride ceramics preparation method according to claim 1, it is characterised in that the addition of PVB ethanol solutions is in 8wt%-18wt%.
5. low-temperature pressureless sintering aluminium nitride ceramics preparation method according to claim 1, it is characterised in that briquetting pressure 200-400MPa.
6. low-temperature pressureless sintering aluminium nitride ceramics preparation method according to claim 1, it is characterised in that the temperature of pressureless sintering is 1500 DEG C -1650 DEG C, and soaking time is 1-5h.
7. low-temperature pressureless sintering aluminium nitride ceramics preparation method according to claim 1, it is characterised in that the aluminium nitride ceramics thermal conductivity of preparation is more than 200W/ (m.k), and 3 rupture strengths are more than 300MPa.
CN201610344841.3A 2016-05-24 2016-05-24 A kind of preparation method of low-temperature pressureless sintering aluminium nitride ceramics Pending CN107417282A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107935601A (en) * 2017-12-23 2018-04-20 洛阳名力科技开发有限公司 A kind of aluminium nitride ceramics

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107935601A (en) * 2017-12-23 2018-04-20 洛阳名力科技开发有限公司 A kind of aluminium nitride ceramics

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Application publication date: 20171201