CN102093077B - 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 silicon nitride ceramic material with low dielectric constant, belong to technical field of functional ceramics.
Background technology
High temperature resistant wave-permeable material, need low-k, low-loss, high temperature resistant, the 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 study hotspot of high temperature wave-transparent material, be widely used in the 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 larger, 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 refers to have the new ceramic material of certain size and quantity pore texture, and porous ceramics has equally distributed pore (void content is up to 50～90%), volume density is little, specific surface area is large, 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, then carry out nitrogenizing reaction from its surface, metal Si is diffused into the nitride that the shell at metal Si forms subsequently, can obtain like this having evenly the porous silicon nitride ceramic of thin closed pore.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 large 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 silicon nitride ceramic material with low dielectric constant, specific inductivity is little, and wave penetrate capability is good.
The present invention provides scientific and reasonable preparation method simultaneously, and is simple.
Silicon nitride ceramic material with low dielectric constant 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, and take soft organic foam plastic as carrier, 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 the 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 in weight ratio again 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.
Silicon nitride ceramic material with low dielectric constant density of the present invention is less than 0.2g/cm
3, specific inductivity is little, and less than 1.3, flexural strength is high, and 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, then mix in ball mill, make slip.
Select the flexible urethane foam of 80PPI, 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, lower dry at 110 ℃, then under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals from room temperature with the speed of 20 ℃/h, porous plastics is volatilized fully, and then the heat-up rate with 100 ℃/h is warming up to 800 ℃ of lower insulation 1h, makes biscuit have some strength, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1680 ℃ of insulation 2h, naturally cold 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, then in ball mill, mix, make slip.
Select the soft PVC porous plastics of 100PPI, 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; lower dry at 110 ℃; then under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals from room temperature with the speed of 10 ℃/h; porous plastics is volatilized fully, and then the heat-up rate with 150 ℃/h is warming up to 800 ℃ of lower insulation 1h, makes biscuit have some strength; then biscuit is transferred in the gas pressure sintering stove; be warming up to 1720 ℃ of insulation 2h under nitrogen protection, naturally cold 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, then in ball mill, mix, make slip.
Select the soft polyethylene porous plastics of 120PPI, 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, lower dry at 110 ℃, then under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals from room temperature with the speed of 40 ℃/h, porous plastics is volatilized fully, and then the heat-up rate with 150 ℃/h is warming up to 800 ℃ of lower insulation 1h, makes biscuit have some strength, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1650 ℃ of insulation 3h, naturally cold 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, then in ball mill, mix, make slip.
Select the flexible urethane foam of 100PPI, 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, lower dry at 110 ℃, then under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals from room temperature with the speed of 40 ℃/h, porous plastics is volatilized fully, and then the heat-up rate with 150 ℃/h is warming up to 800 ℃ of lower insulation 1h, makes biscuit have some strength, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1650 ℃ of insulation 2h, naturally cold 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, then in ball mill, mix, make slip.
Select the flexible urethane foam of 60PPI, 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, lower dry at 110 ℃, then under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals from room temperature with the speed of 30 ℃/h, porous plastics is volatilized fully, and then the heat-up rate with 100 ℃/h is warming up to 900 ℃ of lower insulation 1h, makes biscuit have some strength, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1660 ℃ of insulation 3h, naturally cold 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, then in ball mill, mix, make slip.
Select the soft polyethylene porous plastics of 120PPI, 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, lower dry at 110 ℃, then under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals from room temperature with the speed of 30 ℃/h, porous plastics is volatilized fully, and then the heat-up rate with 200 ℃/h is warming up to 900 ℃ of lower insulation 1.5h, makes biscuit have some strength, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1700 ℃ of insulation 2h, naturally cold 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, then in ball mill, mix, make slip.
Select the flexible urethane foam of 80PPI, 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, lower dry at 110 ℃, then under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals from room temperature with the speed of 30 ℃/h, porous plastics is volatilized fully, and then the heat-up rate with 180 ℃/h is warming up to 850 ℃ of lower insulation 1h, makes biscuit have some strength, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1720 ℃ of insulation 2h, naturally cold going to room temperature can obtain specific inductivity less than 1.3 silicon nitride porous ceramics.
Claims (3)
1. silicon nitride ceramic material with low dielectric constant is characterized in that being prepared as follows:
According to the weight ratio of 88:6:4:2, silicon nitride, aluminum oxide, yttrium oxide and silicon-dioxide are formed ceramic raw material; Ceramic raw material, carboxymethyl cellulose, dispersion agent D305 and water are mixed according to the weight ratio of 100:0.5:1:50, regulate pH value to 9.5, then in ball mill, mix, make ceramic slurry;
Select the flexible urethane foam of 80PPI, 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, lower dry at 110 ℃, then under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals from room temperature with the speed of 20 ℃/h, porous plastics is volatilized fully, and then the heat-up rate with 100 ℃/h is warming up to 800 ℃ of lower insulation 1h, makes biscuit have some strength, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1680 ℃ of insulation 2h, naturally cold going to room temperature can obtain silicon nitride ceramic material with low dielectric constant.
2. silicon nitride ceramic material with low dielectric constant is characterized in that being prepared as follows:
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, then in ball mill, mix, make ceramic slurry;
Select the soft PVC porous plastics of 100PPI, 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; lower dry at 110 ℃; then under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals from room temperature with the speed of 10 ℃/h; porous plastics is volatilized fully, and then the heat-up rate with 150 ℃/h is warming up to 800 ℃ of lower insulation 1h, makes biscuit have some strength; then biscuit is transferred in the gas pressure sintering stove; be warming up to 1720 ℃ of insulation 2h under nitrogen protection, naturally cold going to room temperature can obtain silicon nitride ceramic material with low dielectric constant.
3. silicon nitride ceramic material with low dielectric constant is characterized in that being prepared as follows:
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, then in ball mill, mix, make ceramic slurry;
Select the soft polyethylene porous plastics of 120PPI, 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, lower dry at 110 ℃, then under oxidizing atmosphere, slowly be warming up to 500 ℃ of plastic removals from room temperature with the speed of 40 ℃/h, porous plastics is volatilized fully, and then the heat-up rate with 150 ℃/h is warming up to 800 ℃ of lower insulation 1h, makes biscuit have some strength, then biscuit is transferred in the vacuum sintering furnace, be warming up to 1650 ℃ of insulation 3h, naturally cold going to room temperature can obtain silicon nitride ceramic material with low dielectric constant.
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