CN102093077A - Silicon nitride ceramic material with low dielectric constant and preparation method thereof - Google Patents
Silicon nitride ceramic material with low dielectric constant and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a silicon nitride ceramic material with low dielectric constant, and belongs to the technical field of functional ceramics. The silicon nitride ceramic material consists of the following materials in percentage by weight: 75 to 95 percent of silicon nitride, 0 to 10 percent of yttrium oxide, 0 to 10 percent of aluminum oxide and 1 to 5 percent of silicon oxide; and the materials are prepared into slurry, soft organic foam plastic is used as a carrier, a blank is prepared by slurry impregnation and extrusion, and the blank is sintered into the ceramic material, wherein the aperture of the soft organic foam plastic is 60 to 120PPI. The silicon nitride ceramic material with low dielectric constant has small dielectric constant and good wave penetrating performance; and a preparation method is scientific, reasonable, simple and feasible.
Description
Technical field
The present invention relates to a kind of preparation method of low-k silicon nitride ceramic material, belong to technical field of functional ceramics.
Background technology
High temperature resistant wave-permeable material, need low-k, low-loss, high temperature resistant, characteristics such as heat resistanceheat resistant is shaken and intensity is good, silicon nitride ceramics not only has good high low temperature over-all properties, also has outstanding electric property, be one of research focus of high temperature wave-transparent material, be widely used in fields such as space flight and aviation, car engine, machinery, chemical industry, oil.But existing silicon nitride ceramics density is higher, and specific inductivity is bigger, and Chinese scholars is devoted to the mode by the preparation porous silicon nitride ceramic, improves the dielectric properties of silicon nitride ceramics.
Porous ceramics is meant the new ceramic material with certain size and quantity pore texture, and porous ceramics has evenly-distributed air holes (void content is up to 50～90%), volume density is little, specific surface area is big, and has unique physical surface feature.Application number is the preparation method of a kind of porous silicon nitride of technology introduction of 02802876.7, metal Si powder mixes with sinter additives, with postheat treatment, carry out two step thermal treatments by microwave heating under 1000 ℃ or more temperature, carry out nitrogenizing reaction from its surface then, metal Si is diffused into the nitride that forms subsequently on the shell of metal Si, can obtain having evenly the porous silicon nitride ceramic of thin closed pore like this.200710144953.5 composite nitride silica flour and cenosphere are mixed, and isostatic cool pressing behind dry pressing then with the sintering under protective atmosphere of gained base substrate after the isostatic cool pressing, can prepare the big closed pore and the pottery of regular shape pore.The preparation specific inductivity less than 1.3, the good silicon nitride ceramics of the wave penetrate capability difficult point of investigation of materials still.
Summary of the invention
The object of the present invention is to provide a kind of low-k silicon nitride ceramic material, specific inductivity is little, and wave penetrate capability is good.
The present invention provides scientific and reasonable preparation method simultaneously, and is simple.
Low-k silicon nitride ceramic material of the present invention, the ingredients by weight percentage composition is:
Silicon nitride 75～95%
Yttrium oxide 0～10%
Aluminum oxide 0～10%
Silica 1～5%;
Batching is made slip, is carrier with soft organic foam plastic, and sintering is made after flooding slip, being crushed to base substrate, and the aperture of soft organic foam plastic is 60～120PPI.
Silicon nitride is that a kind of typical covalent linkage stable compound spread coefficient is low, be difficult to make its densification with the normal sintering method, the present invention utilizes sintering aids such as aluminum oxide and yttrium oxide, utilizes the mode of pressureless sintering or gas pressure sintering to make the silicon nitride foamed ceramics under nitrogen atmosphere.
Preparation method of the present invention is scientific and reasonable, and is simple, wherein:
Plastic removal carries out under oxidizing atmosphere, and temperature schedule is:
Room temperature to 500 ℃, 10～60 ℃/h;
500～800℃，80～200℃/h；
800 to 900 ℃, insulation 1～2h.
Sintering carries out under nitrogen atmosphere, sintering temperature: 1630～1750 ℃, and insulation 2～4h.
The best sintering after drying of base substrate after the moulding, 100～120 ℃ of bake out temperatures.
It is 0.5～4% solution that slip is mixed with concentration by macromolecule organic and solvent, adds 0.5～1% polymethacrylic acid dispersion agent, adds 20～40vol%(example again in weight ratio in solution) batching make.
Wherein, macromolecule organic is methylcellulose gum, carboxymethyl cellulose, polystyrene or polyvinyl alcohol.
Solvent is the mixture of a kind of or its arbitrary proportion in water, dehydrated alcohol or the trimethyl carbinol.
Soft organic foam plastic is to have elasticity and the flammable perforate organic foam plastic that can recover original form, the aperture is 60～120PPI, can be flexible urethane foam, polyvinyl chloride foam or polyethylene foams, wherein, flexible urethane foam is to be to soak about 20～30min in 9～11 the alkaline solution in the pH of 50～60 ℃ of temperature value, makes with seasoning behind the distilled water rinsing removal alkaline solution.
Low-k silicon nitride ceramic material density of the present invention is less than 0.2g/cm
3, specific inductivity is little, less than 1.3, and the flexural strength height, greater than 5MPa, wave penetrate capability is good, can satisfy application requiring.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
According to the weight ratio of 88:6:4:2, silicon nitride, aluminum oxide, yttrium oxide and silicon-dioxide are formed ceramic raw material.With ceramic raw material, carboxymethyl cellulose, dispersion agent D305, dispersion agent and water mix according to the weight ratio of 100:0.5:1:50, regulate pH value to 9.5, mix in ball mill then, make slip.
Select the flexible urethane foam of 80PPI for use, adopt roll-in to be stained with sizing process, on the porous plastics carrier, add ceramic slurry, with pushing in the carrier input roller press, extrude unnecessary slip again, make the foamed ceramics base substrate.
Base substrate is put into drying baker, dry down at 110 ℃, under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals with the speed of 20 ℃/h then from room temperature, porous plastics is volatilized fully, and the heat-up rate with 100 ℃/h is warming up to 800 ℃ of insulation 1h down then, makes biscuit have certain intensity, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1680 ℃ of insulation 2h, cold naturally going to room temperature can obtain to hang down the silicon nitride porous ceramics of dielectric.
Embodiment 2
According to the weight ratio of 85:6:4:5, silicon nitride, aluminum oxide, yttrium oxide and silicon-dioxide are formed ceramic raw material.Ceramic raw material, polyvinyl alcohol, dispersion agent D305 and water are mixed according to the weight ratio of 100:0.5:1:40, regulate pH value to 10, in ball mill, mix then, make slip.
Select the soft PVC porous plastics of 100PPI for use, adopt roll-in to be stained with sizing process, on the porous plastics carrier, add ceramic slurry, with pushing in the carrier input roller press, extrude unnecessary slip again, make the foamed ceramics base substrate.
Base substrate is put into drying baker; dry down at 110 ℃; under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals with the speed of 10 ℃/h then from room temperature; porous plastics is volatilized fully, and the heat-up rate with 150 ℃/h is warming up to 800 ℃ of insulation 1h down then, makes biscuit have certain intensity; biscuit is transferred in the gas pressure sintering stove then; be warming up to 1720 ℃ of insulation 2h under nitrogen protection, cold naturally going to room temperature can obtain to hang down the silicon nitride porous ceramics of dielectric.
Embodiment 3
According to the weight ratio of 75:10:10:5, silicon nitride, aluminum oxide, yttrium oxide and silicon-dioxide are formed ceramic raw material.Ceramic raw material, polystyrene, dispersion agent DA and distilled water are mixed according to the weight ratio of 100:1:1:60, regulate pH value to 9, in ball mill, mix then, make slip.
Select the soft polyethylene porous plastics of 120PPI for use, adopt the soaking paste rolling process, on the porous plastics carrier, add ceramic slurry, with pushing in the carrier input roller press, extrude superfluous slip again, make the foamed ceramics base substrate.
Base substrate is put into drying baker, dry down at 110 ℃, under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals with the speed of 40 ℃/h then from room temperature, porous plastics is volatilized fully, and the heat-up rate with 150 ℃/h is warming up to 800 ℃ of insulation 1h down then, makes biscuit have certain intensity, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1650 ℃ of insulation 3h, cold naturally going to room temperature can obtain to hang down the silicon nitride porous ceramics of dielectric.
Embodiment 4
According to the weight ratio of 88.5:6:4:1.5, silicon nitride, aluminum oxide, yttrium oxide and silicon-dioxide are formed ceramic raw material.Ceramic raw material, polystyrene, dehydrated alcohol are mixed according to the weight ratio of 100:0.5:100, in ball mill, mix then, make slip.
Select the flexible urethane foam of 100PPI for use, adopt roll-in to be stained with sizing process, on the porous plastics carrier, add ceramic slurry, with pushing in the carrier input roller press, extrude unnecessary slip again, make the foamed ceramics base substrate.
Base substrate is put into drying baker, dry down at 110 ℃, under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals with the speed of 40 ℃/h then from room temperature, porous plastics is volatilized fully, and the heat-up rate with 150 ℃/h is warming up to 800 ℃ of insulation 1h down then, makes biscuit have certain intensity, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1650 ℃ of insulation 2h, cold naturally going to room temperature, can obtain density is 0.13g/cm
3, specific inductivity is 1.15 silicon nitride porous ceramics.
Embodiment 5
According to the weight ratio of 90:5:4:1, silicon nitride, aluminum oxide, yttrium oxide and silicon-dioxide are formed ceramic raw material.Ceramic raw material, polystyrene and the trimethyl carbinol are mixed according to the weight ratio of 100:2:50, regulate pH value to 9.5, in ball mill, mix then, make slip.
Select the flexible urethane foam of 60PPI for use, adopt roll-in to be stained with sizing process, on the porous plastics carrier, add ceramic slurry, with pushing in the carrier input roller press, extrude unnecessary slip again, make the foamed ceramics base substrate.
Base substrate is put into drying baker, dry down at 110 ℃, under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals with the speed of 30 ℃/h then from room temperature, porous plastics is volatilized fully, and the heat-up rate with 100 ℃/h is warming up to 900 ℃ of insulation 1h down then, makes biscuit have certain intensity, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1660 ℃ of insulation 3h, cold naturally going to room temperature, can obtain density is 0.20g/cm
3, specific inductivity is 1.29 silicon nitride porous ceramics.
Embodiment 6
According to the weight ratio of 92:5:2:1, silicon nitride, aluminum oxide, yttrium oxide and silicon-dioxide are formed ceramic raw material.Ceramic raw material, polystyrene, dispersion agent D735 and water are mixed according to the weight ratio of 100:0.5:1:90, regulate pH value to 10, in ball mill, mix then, make slip.
Select the soft polyethylene porous plastics of 120PPI for use, adopt roll-in to be stained with sizing process, on the porous plastics carrier, add ceramic slurry, with pushing in the carrier input roller press, extrude unnecessary slip again, make the foamed ceramics base substrate.
Base substrate is put into drying baker, dry down at 110 ℃, under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals with the speed of 30 ℃/h then from room temperature, porous plastics is volatilized fully, and the heat-up rate with 200 ℃/h is warming up to 900 ℃ of insulation 1.5h down then, makes biscuit have certain intensity, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1700 ℃ of insulation 2h, cold naturally going to room temperature, can obtain density is 0.18g/cm
3, specific inductivity is 1.25 silicon nitride porous ceramics.
Embodiment 7
According to the weight ratio of 90:5:3:2, silicon nitride, aluminum oxide, yttrium oxide and silicon-dioxide are formed ceramic raw material.Ceramic raw material, polyvinyl alcohol, dispersion agent D305, dehydrated alcohol and water are mixed according to the weight ratio of 100:2.5:1:50:50, regulate pH value to 9.5, in ball mill, mix then, make slip.
Select the flexible urethane foam of 80PPI for use, adopt roll-in to be stained with sizing process, on the porous plastics carrier, add ceramic slurry, with pushing in the carrier input roller press, extrude unnecessary slip again, make the foamed ceramics base substrate.
Base substrate is put into drying baker, dry down at 110 ℃, under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals with the speed of 30 ℃/h then from room temperature, porous plastics is volatilized fully, and the heat-up rate with 180 ℃/h is warming up to 850 ℃ of insulation 1h down then, makes biscuit have certain intensity, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1720 ℃ of insulation 2h, cold naturally going to room temperature can obtain specific inductivity less than 1.3 silicon nitride porous ceramics.
Claims (9)
1. low-k silicon nitride ceramic material is characterized in that the ingredients by weight percentage composition is:
Silicon nitride 75～95%
Yttrium oxide 0～10%
Aluminum oxide 0～10%
Silica 1～5%;
Batching is made slip, is carrier with soft organic foam plastic, and sintering is made after flooding slip, being crushed to base substrate, and the aperture of soft organic foam plastic is 60～120PPI.
2. the preparation method of low-k silicon nitride ceramic material according to claim 1 is characterized in that sintering under nitrogen atmosphere, 1630～1750 ℃ of temperature, insulation 2～4h sintering.
3. the preparation method of low-k silicon nitride ceramic material according to claim 2 is characterized in that plastic removal under the oxidizing atmosphere, and temperature schedule is:
Room temperature to 500 ℃, 10～60 ℃/h;
500～800℃，80～200℃/h；
800 to 900 ℃, insulation 1～2h.
4. the preparation method of low-k silicon nitride ceramic material according to claim 3 is characterized in that after the moulding base substrate sintering after drying, 100～120 ℃ of bake out temperatures.
5. the preparation method of low-k silicon nitride ceramic material according to claim 4, it is characterized in that it is 0.5～4% solution that slip is mixed with concentration by macromolecule organic and solvent, add an amount of polymethacrylic acid dispersion agent, the batching that adds 20～40vol% again in solution makes.
6. the preparation method of low-k silicon nitride ceramic material according to claim 5 is characterized in that macromolecule organic is methylcellulose gum, carboxymethyl cellulose, polystyrene or polyvinyl alcohol.
7. the preparation method of low-k silicon nitride ceramic material according to claim 5 is characterized in that solvent is the mixture of a kind of or its arbitrary proportion in water, dehydrated alcohol or the trimethyl carbinol.
8. the preparation method of low-k silicon nitride ceramic material according to claim 7 is characterized in that soft organic foam plastic is flexible urethane foam, polyvinyl chloride foam or polyethylene foams.
9. the preparation method of low-k silicon nitride ceramic material according to claim 8, it is characterized in that flexible urethane foam is is to soak about 20～30min in 9～11 the alkaline solution in the pH of 50～60 ℃ of temperature value, makes with seasoning behind the distilled water rinsing removal alkaline solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105336556A (en) * | 2015-08-21 | 2016-02-17 | 国网山东省电力公司临沂供电公司 | Arc-extinguishing type drop-out fuse employing silicone rubber porcelain insulator |
| CN106431420A (en) * | 2016-09-14 | 2017-02-22 | 郑州峰泰纳米材料有限公司 | Method for preparing low-dielectric-constant foamed ceramic |
| CN107602092A (en) * | 2017-09-30 | 2018-01-19 | 佛山市飞时达新材料科技有限公司 | A kind of preparation method of porous nano ceramic material |
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| CN1552670A (en) * | 2003-12-12 | 2004-12-08 | 中国科学院上海硅酸盐研究所 | Mesh porous ceramic preparing method |
| US20060119018A1 (en) * | 2002-10-04 | 2006-06-08 | E-Tec Co., Ltd. | Cold-curing binder and process ror producing molding with the same |
| CN101555156A (en) * | 2009-05-15 | 2009-10-14 | 山东大学 | Boron nitride crystal whisker/silicon nitride ceramic composite material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060119018A1 (en) * | 2002-10-04 | 2006-06-08 | E-Tec Co., Ltd. | Cold-curing binder and process ror producing molding with the same |
| CN1552670A (en) * | 2003-12-12 | 2004-12-08 | 中国科学院上海硅酸盐研究所 | Mesh porous ceramic preparing method |
| CN101555156A (en) * | 2009-05-15 | 2009-10-14 | 山东大学 | Boron nitride crystal whisker/silicon nitride ceramic composite material and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105336556A (en) * | 2015-08-21 | 2016-02-17 | 国网山东省电力公司临沂供电公司 | Arc-extinguishing type drop-out fuse employing silicone rubber porcelain insulator |
| CN105336556B (en) * | 2015-08-21 | 2018-02-16 | 国网山东省电力公司临沂供电公司 | A kind of Arc-extinguishing-tydrop-out drop-out fuse using silicon rubber porcelain insulator |
| CN106431420A (en) * | 2016-09-14 | 2017-02-22 | 郑州峰泰纳米材料有限公司 | Method for preparing low-dielectric-constant foamed ceramic |
| CN107602092A (en) * | 2017-09-30 | 2018-01-19 | 佛山市飞时达新材料科技有限公司 | A kind of preparation method of porous nano ceramic material |
| CN107602092B (en) * | 2017-09-30 | 2020-12-04 | 永州明睿陶瓷科技有限公司 | Preparation method of porous nano ceramic material |
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