CN103360078A - Preparation method of silicon nitride composite material and substrate prepared from silicon nitride composite material - Google Patents
Preparation method of silicon nitride composite material and substrate prepared from silicon nitride composite material Download PDFInfo
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- CN103360078A CN103360078A CN2012100970511A CN201210097051A CN103360078A CN 103360078 A CN103360078 A CN 103360078A CN 2012100970511 A CN2012100970511 A CN 2012100970511A CN 201210097051 A CN201210097051 A CN 201210097051A CN 103360078 A CN103360078 A CN 103360078A
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Abstract
The invention discloses a preparation method of a silicon nitride composite material. The preparation method comprises the following steps of: mixing P2O5, ZnO, NaF and B2O3 so as to prepare glass powder; mixing the glass powder and silicon nitride powder so as to prepare mixed powder; carrying out dry-pressing molding on the mixed powder to prepare a presintering body; and removing glue from the presintering body and sintering so as to prepare the silicon nitride composite material. The invention also discloses a substrate prepared from the silicon nitride composite material. NaF-ZnO-P2O5-B2O3 series glass with low dielectric constant and silicon nitride are compounded and sintered at a low temperature so as to prepare the compact silicon nitride composite material. The silicon nitride composite material is used for preparing the substrate. The dielectric constant of the substrate can reach about 4, and the dielectric loss of the substrate can reach about 0.0008.
Description
Technical field
The present invention relates to the stupalith field, more particularly, relate to based on the composite manufacture method of silicon nitride ceramics and the substrate that utilizes this matrix material preparation.
Background technology
Silicon nitride ceramic material has the advantages such as specific inductivity is low, dielectric loss is little, thermal expansivity is little, high temperature resistant, and its intensity can maintain 900 ℃ high temperature always and do not descend, and is the ideal material of the high temperature resistant substrate of preparation.
Because silicon nitride is the strong covalent bond compound, only have the decomposition temperature that reaches silicon nitride when sintering temperature that enough ion migration speed just can be arranged, therefore solid state sintering is difficult to obtain fine and close silicon nitride ceramic material, usually adopt two kinds of methods to prepare silicon nitride ceramic material, a kind of is to help sintering by adding oxide compound, another kind is to adopt hot pressed sintering, the former can affect with silicon nitride reaction the electric and mechanical property of silicon nitride ceramics owing to oxide compound in preparation process, the latter is because the power consumption of this technique is large, cost is high, and can only make the simple product of shape matching, be difficult to realize industrialization, the Application Areas of silicon nitride ceramic material is restricted.
Summary of the invention
Technical problem to be solved by this invention is, consumes energy greatly for the preparation technology of existing silicon nitride composite material, and the defective that cost is high provides a kind of preparation method of silicon nitride composite material, this silicon nitride composite material processing simply, low cost of manufacture.
The present invention also provides a kind of substrate that adopts this silicon nitride composite material preparation.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of silicon nitride composite material said method comprising the steps of:
A, with P
2O
5, ZnO, NaF, B
2O
3Be mixed with into glass powder;
B, described glass powder is mixed with into mixed powder with beta-silicon nitride powder;
C, with the dry-pressing formed preparation presintering of described mixed powder body;
D, described presintering body is carried out binder removal and sintering is prepared into described silicon nitride composite material.
Further, based on P
2O
5, ZnO, NaF, B
2O
3Total mole number, described P
2O
5Account for 20～35%, ZnO accounts for 35～45%, NaF accounts for 20～25%, B
2O
35～10%.
Further, based on the total mass number of described glass powder and beta-silicon nitride powder, described glass powder accounts for 5wt%～30wt%.
Further, described step c is under the pressure of 80～120MPa, and is dry-pressing formed.
A kind of substrate is comprised of silicon nitride composite material.
The present invention selects low-k NaF-ZnO-P
2O
5-B
2O
3Be that glass and silicon nitride are compound by the fine and close silicon nitride composite material of low-temperature sintering preparation, the energy and sintering cost have been saved greatly, and this silicon nitride composite material prepared substrate, and the specific inductivity of this substrate can reach about 4, and dielectric loss can reach about 0.0008.
Description of drawings
Fig. 1 is a kind of silicon nitride composite material preparation method's of the present invention process flow sheet.
Embodiment
As shown in Figure 1, be a kind of silicon nitride composite material preparation method's of the present invention process flow sheet.Based on P
2O
5, ZnO, NaF, B
2O
3Total mole number, with P
2O
520～35%, ZnO 35～45%, NaF 20～25%, B
2O
35～10% batchings are mixed, and add ethanol and carry out ball milling, oven dry, and put into corundum crucible, and in high-temperature electric resistance furnace, be heated to 1400 ℃, and be incubated two hours, make glass melt clarification homogenizing; After glass melt is poured into water quenching, add the ethanol ball milling after, dry 200 mesh sieves of crossing are prepared into glass powder; With glass powder according to 5wt%～30wt% with after beta-silicon nitride powder mixes, add ethanol, binding agent carries out ball milling, and dry, cross 60 mesh sieves and be prepared into mixed powder; With mixed powder under the pressure of 80～120MPa, the dry-pressing formed presintering body of making; The presintering body is carried out binder removal and sintering:
(1) binder removal: the speed with 1 ℃/min slowly is warming up to 500 ℃, and insulation 1h, and thoroughly eliminating is clean to guarantee binding agent;
(2) sintering: in atmosphere furnace, pass into nitrogen and be warming up to maximum sintering temperature (1200～1500 ℃) with 10 ℃/min, and be incubated 2～4 hours, then the rate of temperature fall with 20 ℃/min is cooled to 400 ℃, cools at last room temperature with the furnace, is prepared into silicon nitride composite material.
The preparation method of this silicon nitride composite material adopts by the fine and close silicon nitride composite material of low-temperature sintering preparation, the energy and sintering cost have been saved greatly, and can make complicated product, realize extensive industrialization, and this silicon nitride composite material is used for preparing substrate, and the specific inductivity of this substrate can reach about 4, and dielectric loss can reach about 0.0008.
Embodiment 1
The method of the low dielectric, low-loss silicon nitride composite material of the present invention's preparation is as follows: by mole% taking by weighing P
2O
520%, ZnO 45%, NaF 25%, B
2O
310% also mixes, and adds ethanol, uses alumina balls as ball milling, in planetary ball mill behind the ball milling 4h, at 80 ℃ of lower dry 6h, dried powder is put into corundum crucible, and be warming up to 1400 ℃ with the speed of 5 ℃/min again, and be incubated two hours, after making glass melt clarification homogenizing, be poured into water quenching, the glass particle in the water is taken out, and add ethanol and carry out ball milling, cross 200 mesh sieves after dry to make glass powder.
Glass powder is prepared burden according to 5wt% and beta-silicon nitride powder, and adding ethanol, after binding agent PVB ball milling mixes, drying obtains mixed powder after crossing 60 mesh sieve granulations, pressure lower sheeting moulding at 120MPa obtains the presintering body, sintered compact is passed into nitrogen carry out sintering in atmosphere furnace, make the low dielectric, low-loss silicon nitride composite material of the present invention, concrete sintering schedule is as follows:
1, binder removal: the speed with 1 ℃/min slowly is warming up to 500 ℃, and insulation 1h, and thoroughly eliminating is clean to guarantee binding agent;
2, sintering: the product behind the binder removal is passed into nitrogen be warming up to 1500 ℃ of maximum sintering temperatures with 10 ℃/min, and be incubated 3 hours, then the rate of temperature fall with 20 ℃/min is cooled to 400 ℃, cools at last room temperature with the furnace.
The preparation method of this silicon nitride composite material adopts by the fine and close silicon nitride composite material of low-temperature sintering preparation, the energy and sintering cost have been saved greatly, and can make complicated product, realize extensive industrialization, and this silicon nitride composite material is used for preparing substrate, and the specific inductivity of this substrate can reach 3.8, and dielectric loss can reach 0.0007.
Embodiment 2
The method of the low dielectric, low-loss silicon nitride composite material of the present invention's preparation is as follows: by mole% taking by weighing P
2O
535%, ZnO 35%, NaF 25%, B
2O
35% also mixes, and adds ethanol, uses alumina balls as ball milling, in planetary ball mill behind the ball milling 4h, at 80 ℃ of lower dry 6h, dried powder is put into corundum crucible, and be warming up to 1400 ℃ with the speed of 5 ℃/min again, and be incubated two hours, after making glass melt clarification homogenizing, be poured into water quenching, the glass particle in the water is taken out, and add ethanol and carry out ball milling, cross 200 mesh sieves after dry to make glass powder.
Glass powder is prepared burden according to 15wt% and beta-silicon nitride powder, and adding ethanol, after binding agent PVB ball milling mixes, drying obtains mixed powder after crossing 60 mesh sieve granulations, pressure lower sheeting moulding at 80MPa obtains the presintering body, sintered compact is passed into nitrogen carry out sintering in atmosphere furnace, make the low dielectric, low-loss silicon nitride composite material of the present invention, concrete sintering schedule is as follows:
1, binder removal: the speed with 1 ℃/min slowly is warming up to 500 ℃, and insulation 1h, and thoroughly eliminating is clean to guarantee binding agent;
2, sintering: the product behind the binder removal is passed into nitrogen be warming up to 1350 ℃ of maximum sintering temperatures with 10 ℃/min, and be incubated 3 hours, then the rate of temperature fall with 20 ℃/min is cooled to 400 ℃, cools at last room temperature with the furnace.
The preparation method of this silicon nitride composite material adopts by the fine and close silicon nitride composite material of low-temperature sintering preparation, the energy and sintering cost have been saved greatly, and can make complicated product, realize extensive industrialization, and this silicon nitride composite material is used for preparing substrate, and the specific inductivity of this substrate can reach 4.2, and dielectric loss can reach 0.00075.
Embodiment 3
The method of the low dielectric, low-loss silicon nitride composite material of the present invention's preparation is as follows: by mole% taking by weighing P
2O
530%, ZnO 40%, NaF 23%, B
2O
37% also mixes, and adds ethanol, uses alumina balls as ball milling, in planetary ball mill behind the ball milling 4h, at 80 ℃ of lower dry 6h, dried powder is put into corundum crucible, and be warming up to 1400 ℃ with the speed of 5 ℃/min again, and be incubated two hours, after making glass melt clarification homogenizing, be poured into water quenching, the glass particle in the water is taken out, and add ethanol and carry out ball milling, cross 200 mesh sieves after dry to make glass powder.
Glass powder is prepared burden according to 30wt% and beta-silicon nitride powder, and adding ethanol, after binding agent PVB ball milling mixes, drying obtains mixed powder after crossing 60 mesh sieve granulations, pressure lower sheeting moulding at 100MPa obtains the presintering body, sintered compact is passed into nitrogen carry out sintering in atmosphere furnace, make the low dielectric, low-loss silicon nitride composite material of the present invention, concrete sintering schedule is as follows:
1, binder removal: the speed with 1 ℃/min slowly is warming up to 500 ℃, and insulation 1h, and thoroughly eliminating is clean to guarantee binding agent;
2, sintering: the product behind the binder removal is passed into nitrogen be warming up to 1200 ℃ of maximum sintering temperatures with 10 ℃/min, and be incubated 3 hours, then the rate of temperature fall with 20 ℃/min is cooled to 400 ℃, cools at last room temperature with the furnace.
The preparation method of this silicon nitride composite material adopts by the fine and close silicon nitride composite material of low-temperature sintering preparation, the energy and sintering cost have been saved greatly, and can make complicated product, realize extensive industrialization, and this silicon nitride composite material is used for preparing substrate, and the specific inductivity of this substrate can reach 4, and dielectric loss can reach 0.0008.
The above is described embodiments of the invention by reference to the accompanying drawings; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment only is schematic; rather than restrictive; those of ordinary skill in the art is under enlightenment of the present invention; not breaking away from the scope situation that aim of the present invention and claim protect, also can make a lot of forms, these all belong within the protection of the present invention.
Claims (5)
1. the preparation method of a silicon nitride composite material is characterized in that, said method comprising the steps of:
A, with P
2O
5, ZnO, NaF, B
2O
3Be mixed with into glass powder;
B, described glass powder is mixed with into mixed powder with beta-silicon nitride powder;
C, with the dry-pressing formed preparation presintering of described mixed powder body;
D, described presintering body is carried out binder removal and sintering is prepared into described silicon nitride composite material.
2. the preparation method of described a kind of silicon nitride composite material according to claim 1 is characterized in that, based on P
2O
5, ZnO, NaF, B
2O
3Total mole number, described P
2O
5Account for 20～35%, ZnO accounts for 35～45%, NaF accounts for 20～25%, B
2O
35～10%.
3. the preparation method of described a kind of silicon nitride composite material according to claim 1 is characterized in that based on the total mass number of described glass powder and beta-silicon nitride powder, described glass powder accounts for 5wt%～30wt%.
4. the preparation method of described a kind of silicon nitride composite material according to claim 1 is characterized in that described step c is under the pressure of 80～120MPa, and is dry-pressing formed.
5. a substrate is characterized in that, the silicon nitride composite material that is prepared by the described method of claim 1 forms.
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|---|---|---|---|
| CN2012100970511A CN103360078A (en) | 2012-04-05 | 2012-04-05 | Preparation method of silicon nitride composite material and substrate prepared from silicon nitride composite material |
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|---|---|---|---|
| CN2012100970511A CN103360078A (en) | 2012-04-05 | 2012-04-05 | Preparation method of silicon nitride composite material and substrate prepared from silicon nitride composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103833379A (en) * | 2014-01-10 | 2014-06-04 | 深圳市麦捷微电子科技股份有限公司 | Sintering process of low dielectric ceramic material and application thereof |
| CN113429212A (en) * | 2020-09-15 | 2021-09-24 | 深圳前海发维新材料科技有限公司 | Application of silicon nitride glass composite material with low thermal diffusivity, low friction coefficient, low thermal conductivity and low thermal expansion in engine |
-
2012
- 2012-04-05 CN CN2012100970511A patent/CN103360078A/en active Pending
Non-Patent Citations (4)
| Title |
|---|
| 周曦亚等: "氮化硅和微晶玻璃复合材料的研究", 《中国陶瓷》 * |
| 李志进等: "低介电常数NaF-ZnO-P2O5-B2O3玻璃的研究", 《玻璃与搪瓷》 * |
| 杨娟等: "低温共烧基板材料研究进展", 《材料导报》 * |
| 陈兴宇等: "玻璃/陶瓷体系低温共烧陶瓷的研究进展", 《佛山陶瓷》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103833379A (en) * | 2014-01-10 | 2014-06-04 | 深圳市麦捷微电子科技股份有限公司 | Sintering process of low dielectric ceramic material and application thereof |
| CN113429212A (en) * | 2020-09-15 | 2021-09-24 | 深圳前海发维新材料科技有限公司 | Application of silicon nitride glass composite material with low thermal diffusivity, low friction coefficient, low thermal conductivity and low thermal expansion in engine |
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Application publication date: 20131023 |