CN106957176A - A kind of preparation method of high thermal conductivity silicon nitride ceramics - Google Patents
A kind of preparation method of high thermal conductivity silicon nitride ceramics Download PDFInfo
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- CN106957176A CN106957176A CN201610017235.0A CN201610017235A CN106957176A CN 106957176 A CN106957176 A CN 106957176A CN 201610017235 A CN201610017235 A CN 201610017235A CN 106957176 A CN106957176 A CN 106957176A
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- thermal conductivity
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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
- C04B35/584—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 based on silicon nitride
- C04B35/593—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 based on silicon nitride obtained by pressure sintering
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/3865—Aluminium nitrides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Abstract
The present invention provides a kind of preparation method of high thermal conductivity silicon nitride ceramics.SiN ceramic with high heat conductivity in the present invention is with β-Si3N4Powder is mixed with the high-purity AlN powders of additional 10%-15% and additional 10%-20% fluxing agents mass ratio, is prepared using hot pressing and sintering technique.In preparation process, mixed powder is first placed on 4MPa forming under the pressure, is then placed in graphite jig, the hot pressed sintering under the conditions of 10-35MPa, 1650 DEG C -1850 DEG C, soaking time 1-10h.The thermal conductivity of silicon nitride ceramics prepared by the present invention can reach 100W/ (m.k), and 3 rupture strengths can reach 850 MPa.
Description
Technical field
The invention belongs to non-oxide ceramicses technical field.Specifically related to a kind of preparation method of high thermal conductivity silicon nitride ceramics.
Background technology
Since the nineties in last century, it is swift and violent by the hi-tech development of representative of microelectronics and information technology, modern electronic devices develop to the direction such as high density, multi-functional, highly reliable, lightweight, long-life, small volume, high-power, semiconductor chip quantity is more and more more, wiring and packaging density are more and more high, circuit operating temperature is caused constantly to rise, fuel factor, which seems, to be particularly acute.Fundamentally to solve these problems need to research and develop the material with high heat conductance, be radiated by substrate.The ceramic material of substrate base, which usually can be used as, mainly Al2O3, BeO, SiC and AlN etc..Al2O3The thermal conductivity of ceramics is relatively low, is not suitable for high density, powerful application；BeO ceramics are most representational high heat-conducting ceramics, and its chemical stability, electrical insulating property and heat resistance are all fabulous.But there is BeO ceramics very strong toxicity, human body can cause acute pneumonia after largely sucking, long-term suction can trigger chronic berylliosis of lung disease, now tapered off and used in the industrial production；SiC ceramic thermal conductivity is very high, but its dielectric strength is relatively low, easily it is breakdown, thus application be restricted；AlN ceramic is a kind of excellent highly heat-conductive material, just it is being widely used in the heat sink material and encapsulating material of large scale integrated circuit, semiconductor module circuit and high power device, but current ceramics have that cost of manufacture is high, easy, and these problems have had a strong impact on its large-scale popularization and application.Patent CN103787663A discloses the preparation of the good Silicon Nitride Ceramic Cutter material of multiphase high intensity, thermal conductivity and cutter, and the material microstructure is by β-Si3N4Needle-like length is brilliant, β '-Si3N4Column length is brilliant, α-Si3N4Column crystal and equiax crystal and intergranular phase composition, intergranular is by Si, N, O, the bright-coloured system thulium and secondary densification aid metallic element that two kinds of Y and above ionic radius are distributed into ladder are constituted, at room temperature bending strength 900-950MPa, and thermal conductivity is 62-69W/（m.k）.Patent CN1152299A discloses the preparation of highly heat-conductive silicon nitride sinter, its manufacture method and pressure-welded structure, have and be converted into oxide to be less than 17.5% rare earth element more than 7.5%, on demand containing at least one in the aluminium nitride or aluminum oxide less than 1%；At least one selected in below 0.1-3.0% as needed oxide, carbide, nitride, silicide, the colony of boride composition, containing less than 0.3% impurity cationic.The sintering bulk thermal conductivities are more than 20W/（m.k）, three-point bending resistance intensity is more than 650MPa.It can be seen that, the silicon nitride ceramics thermal conductivity that the above method can obtain good heat conductivity is generally less than normal, it is impossible to fully meet requirement of the Ceramic Substrate Material to thermal conductivity, so as to have impact on use of the silicon nitride ceramics in field of electronic devices.
The content of the invention
In order to overcome the problem of current silicon nitride ceramics thermal conductivity is small, the present invention proposes a kind of preparation method of high thermal conductivity silicon nitride ceramics, specifically：
（1）With β-Si3N4Powder is raw material with the high-purity AlN powders of additional 10%-15% and additional 10%-20% fluxing agents；
（2）After step (1) raw material uniformly mixing, 4Mpa forming under the pressure is placed on, is then placed in graphite jig, the hot pressed sintering under 10-35Mpa, 1650 DEG C -1850 DEG C, soaking time 1-10h, nitrogen atmosphere terminates rear sample furnace cooling to room temperature.
The preparation method of high thermal conductivity silicon nitride ceramics as described above, it is characterised in that described β-Si3N4Purity is more than or equal to 85%, and granularity is between 0.2-20 μm.
The preparation method of high thermal conductivity silicon nitride ceramics as described above, it is characterised in that high-purity AlN powder purities are more than or equal to 99%, and granularity is at 0.3-10 μm.
The preparation method of high thermal conductivity silicon nitride ceramics as described above, it is characterised in that fluxing agent is mainly SiO2、Y2O3、MgO、CeO2。
The preparation method of high thermal conductivity silicon nitride ceramics as described above, it is characterised in that the pressure of hot pressed sintering is 10-35MPa, and temperature is 1650 DEG C -1850 DEG C, and soaking time is 1-10h.
The preparation method of high thermal conductivity silicon nitride ceramics as described above, it is characterised in that the silicon nitride ceramics thermal conductivity of preparation is more than 100W/ (m.k).
The present invention, which provides a kind of preparation method of high thermal conductivity silicon nitride ceramics, has advantages below：
(1) the creative thermal conductivity that silicon nitride ceramics is improved using AlN powders;
(2) preparation method is simple, feasible, is adapted to industrialized production;
(3) silicon nitride ceramics prepared by has excellent calorifics, mechanical property, and wherein thermal conductivity can arrive 850MPa to 100 W/ (m.k), rupture strength.
Brief description of the drawings：
Fig. 1 is the preparation flow figure of high thermal conductivity silicon nitride.
Embodiment：
The characteristics of the present invention is furture elucidated below by example, but it is not limited to embodiment.
Embodiment 1
By β-Si3N4Powder and additional 10% high-purity AlN powders and additional 7%SiO2、6%Y2O3, after the raw material such as 2%MgO will mix uniformly, be put into 4MPa forming under the pressure, be then placed in graphite jig, the hot pressed sintering under 10MPa, 1650 DEG C, soaking time 5h, nitrogen atmosphere terminates rear sample furnace cooling to room temperature.880MPa can be arrived to 98 W/ (m.k), 3 rupture strengths by silicon nitride ceramics thermal conductivity made above.
Embodiment 2
By β-Si3N4Powder and additional 15% high-purity AlN powders and additional 10%SiO2、5%Y2O3、5%CeO2After uniformly being mixed Deng raw material, 4MPa forming under the pressure is put into, is then placed in graphite jig, the hot pressed sintering under 25MPa, 1750 DEG C, soaking time 2h, nitrogen atmosphere terminates rear sample furnace cooling to room temperature.965MPa can be arrived to 124 W/ (m.k), 3 rupture strengths by silicon nitride ceramics thermal conductivity made above.
Embodiment 3
By β-Si3N4Powder and additional 13% high-purity AlN powders and additional 6%SiO2、8%Y2O3、5%CeO2After uniformly being mixed Deng raw material, 4MPa forming under the pressure is put into, is then placed in graphite jig, the hot pressed sintering under 28MPa, 1800 DEG C, soaking time 7h, nitrogen atmosphere terminates rear sample furnace cooling to room temperature.922MPa can be arrived to 131 W/ (m.k), 3 rupture strengths by silicon nitride ceramics thermal conductivity made above.
Embodiment 4
By β-Si3N4Powder and additional 14% high-purity AlN powders and additional 5%SiO2、10%Y2O3, after the raw material such as 5%MgO will mix uniformly, be put into 4MPa forming under the pressure, be then placed in graphite jig, the hot pressed sintering under 30MPa, 1820 DEG C, soaking time 8h, nitrogen atmosphere terminates rear sample furnace cooling to room temperature.1026MPa can be arrived to 141 W/ (m.k), 3 rupture strengths by silicon nitride ceramics thermal conductivity made above.
Claims (6)
1. a kind of preparation method of high thermal conductivity silicon nitride ceramics, including dispensing, mixing, shaping and sintering, it is characterised in that：
With β-Si3N4Powder is raw material with the high-purity AlN powders of additional 10%-15% and additional 10%-20% fluxing agents；
After step (1) raw material uniformly mixing, 4MPa forming under the pressure is placed on, is then placed in graphite jig, the hot pressed sintering under 10-35MPa, 1650 DEG C -1850 DEG C, soaking time 1-10h, nitrogen atmosphere terminates rear sample furnace cooling to room temperature.
2. high thermal conductivity silicon nitride ceramics preparation method according to claim 1, it is characterised in that described β-Si3N4Purity is more than or equal to 85%, and granularity is between 0.2-20 μm.
3. high thermal conductivity silicon nitride ceramics preparation method according to claim 1, it is characterised in that high-purity AlN powder purities are more than or equal to 99%, and granularity is between 0.3-10 μm.
4. high thermal conductivity silicon nitride ceramics preparation method according to claim 1, it is characterised in that fluxing agent is mainly SiO2、Y2O3、MgO、CeO2。
5. high thermal conductivity silicon nitride ceramics preparation method according to claim 1, it is characterised in that the pressure of hot pressed sintering is 10-35MPa, temperature is 1650 DEG C -1850 DEG C, and soaking time is 1-10h.
6. high thermal conductivity silicon nitride ceramics preparation method according to claim 1, it is characterised in that the silicon nitride ceramics thermal conductivity of preparation is more than 100W/ (m.k).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107663093A (en) * | 2017-10-26 | 2018-02-06 | 广东工业大学 | A kind of Si3N4Base composite ceramic and preparation method thereof |
| CN113233903A (en) * | 2021-01-15 | 2021-08-10 | 辽宁伊菲科技股份有限公司 | Silicon nitride ceramic substrate and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103848630A (en) * | 2012-11-28 | 2014-06-11 | 大连大友高技术陶瓷有限公司 | High density composite ceramic balls |
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- 2016-01-12 CN CN201610017235.0A patent/CN106957176A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103848630A (en) * | 2012-11-28 | 2014-06-11 | 大连大友高技术陶瓷有限公司 | High density composite ceramic balls |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107663093A (en) * | 2017-10-26 | 2018-02-06 | 广东工业大学 | A kind of Si3N4Base composite ceramic and preparation method thereof |
| CN113233903A (en) * | 2021-01-15 | 2021-08-10 | 辽宁伊菲科技股份有限公司 | Silicon nitride ceramic substrate and preparation method thereof |
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Application publication date: 20170718 |