CN106431420A - Method for preparing low-dielectric-constant foamed ceramic - Google Patents
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Abstract
The invention provides a method for preparing low-dielectric-constant foamed ceramic. The method comprises the following steps that 1, ceramic powder and a dispersant are ball-milled and mixed, the mass of the dispersant accounts for 0.5%-1.5% that of the ceramic powder, and ceramic slurry with the viscosity being 500 mPa's to 1,800 mPa's and the solid content mass fraction being 50%-70% is prepared; 2, the ceramic slurry is hung on pretreated polyurethane foam, drying is carried out after slurry hanging, then second slurry hanging is carried out, and sintering is carried out for 2 h to 4 h at the temperature of 160 DEG C to 1,600 DEG C after drying. The ceramic powder is prepared from 30-40 wt% of silicon nitride, 40-60 wt% of kaolin, 5-10 wt% of aluminum oxide and 1-5 wt% of silicon dioxide. The foamed ceramic prepared through the method is low in dielectric constant and good in wave transmission performance.
Description
Technical field
The invention belongs to function ceramics preparing technical field is and in particular to a kind of preparation side of low-k foamed ceramics
Method.
Background technology
High temperature resistant wave-permeable material, needs low-k, low-loss, high temperature resistant, heat resistanceheat resistant to shake and the features such as intensity is good, nitrogen
SiClx pottery not only has good high/low temperature combination property, also has outstanding electric property, is grinding of high temperature wave-transparent material
Study carefully one of focus, be widely used in the fields such as space flight and aviation, car engine, machinery, chemical industry, oil.But it is existing
Silicon nitride ceramics density is higher, and dielectric constant is larger, and Chinese scholars are devoted to by way of preparing porous silicon nitride ceramic,
Improve the dielectric properties of silicon nitride ceramics.
Porous ceramics refers to the new ceramic material with certain size sum metering-orifice gap structure, and porous ceramics has uniformly
The pore (porosity up to 50～90%) of distribution, volume density are little, specific surface area is big, and have the physical surface feature of uniqueness.
A kind of preparation method of porous silicon nitride of technology introduction of Application No. 02802876.7, metal Si powder is mixed with sinter additives
Close, be subsequently heat-treated, two step heat treatments are carried out by heating using microwave under 1000 DEG C or more temperature, then from its surface
Carry out nitridation reaction, metal Si is subsequently diffused into the nitride being formed on the shell of metal Si, so can obtain having uniformly,
The porous silicon nitride ceramic of thin closed pore.200710144953.5 by composite nitride silica flour and cenosphere mixing, through dry pressing
Then gained base substrate after isostatic cool pressing is sintered under protective atmosphere by isostatic cool pressing afterwards, can prepare big closure pore and rule
The pottery of shape pore.Prepare the difficult point that dielectric constant is less than the good silicon nitride ceramics still investigation of materials of 1.3, wave transparent performance.
Content of the invention
The present invention proposes a kind of preparation method of low-k foamed ceramics, and the foamed ceramics that the method prepares is situated between
Electric constant is little, and wave transparent performance is good.
The technical scheme is that and be achieved in that：
A kind of preparation method of low-k foamed ceramics, comprises the following steps：
1) by ceramic powder and dispersant ball milling mixing, dispersant is the 0.5～1.5% of ceramic powder quality, is obtained viscous
Spending for 500～1800mPa s, solid content mass fraction is 50%～70% ceramic slurry；
2) ceramic slurry is carried out hanging in the polyurethane foam through pretreatment, be dried after hanging, with laggard
Second hanging of row, drying is sintered 2～4h after 160 DEG C～1600 DEG C；
Wherein, ceramic powder is by silicon nitride 30～40wt%, kaolin 40～60wt%, aluminum oxide 5～10wt% and two
Silica 1～5wt% forms.
Further, dispersant is Triammonium citrate.
Further, the preprocess method of polyurethane foam：Clean surface, then the alkali being 8.5～10 in pH value with washing agent
20～30min is soaked, the carboxymethylcellulose calcium being finally 0.5% with mass fraction and 5% silicon sol solution make table in solution
Face activity is processed.
Further, the pore size of polyurethane foam is 30PPI～80PPI.
Further, step 2) drying means be placed in 80～120 DEG C of drying boxes be dried 12～24h.
Beneficial effect of the present invention：
1st, silicon nitride be a kind of typical covalent bond stable compound diffusion coefficient low it is difficult to make it with conventional sintering process
Densified, the present invention utilizes the sintering aid such as kaolin and aluminum oxide, and the mode using pressureless sintering or gas pressure sintering makes nitrogen
SiClx foamed ceramics, substantially increases the intensity of ceramic muscle, distinguished in the field advantage of melt filtration, Material reinforcement phase.
2nd, silicon nitride ceramic material with low dielectric constant dielectric constant of the present invention is little, and less than 1.1, bending strength is high, is more than
5.6MPa, wave transparent performance is good, disclosure satisfy that application requirement.
Specific embodiment
Embodiment 1
Ceramic powder is made up of silicon nitride 40wt%, kaolin 50wt%, aluminum oxide 9wt% and silica 1 wt%.
The preprocess method of polyurethane foam：Clean surface with washing agent, then pH value be 8.5 aqueous slkali in soak
30min, the carboxymethylcellulose calcium being finally 0.5% with mass fraction and 5% silicon sol solution do surface-active-treatment.
The preparation method of low-k foamed ceramics, comprises the following steps：
1) by ceramic powder and Triammonium citrate ball milling mixing, dispersant is the 0.5% of ceramic powder quality, prepared viscosity
It is 50% ceramic slurry for 600mPa s, solid content mass fraction；
2) by ceramic slurry through pretreatment specification be 30PPI polyurethane foam on carry out hanging, hanging is laggard
Row is dried in 120 DEG C of drying boxes and 12h is dried, and subsequently carries out second hanging, and 12h be dried in 80 DEG C of drying boxes, be dried after
Under air atmosphere, 160 DEG C of 240 DEG C of heating rates are 2 DEG C/min, are 0.4 0.9 in 240 DEG C 800 DEG C of heating rates
DEG C/min, it is 3.5 5 DEG C/min in 800 DEG C 1600 DEG C of heating rates, and be incubated 4h at 1600 DEG C.
It is used the foam for 30PPI for the specification as carrier, the pore size of the foamed ceramics of preparation is uniformly, almost all of
Hole is apparent pore, and hole hypertrophy of tendon and muscle is carefully more uniform, and preferably, its compression strength is 16MPa to intensity.
Embodiment 2
Ceramic powder is made up of silicon nitride 30wt%, kaolin 60wt%, aluminum oxide 5wt% and silica 5wt%.
The preprocess method of polyurethane foam：Clean surface with washing agent, then pH value be 9.5 aqueous slkali in soak
25min, the carboxymethylcellulose calcium being finally 0.5% with mass fraction and 5% silicon sol solution do surface-active-treatment.
The preparation method of low-k foamed ceramics, comprises the following steps：
1) by ceramic powder and Triammonium citrate ball milling mixing, dispersant is the 0.8% of ceramic powder quality, prepared viscosity
It is 60% ceramic slurry for 1000mPa s, solid content mass fraction；
2) by ceramic slurry through pretreatment specification be 50PPI polyurethane foam on carry out hanging, hanging is laggard
Row is dried in 80 DEG C of drying boxes and 24h is dried, and subsequently carries out second hanging, and 12h be dried in 120 DEG C of drying boxes, be dried after
Under air atmosphere, 160 DEG C of 240 DEG C of heating rates are 2 DEG C/min, are 0.4 0.9 in 240 DEG C 800 DEG C of heating rates
DEG C/min, it is 3.5 5 DEG C/min in 800 DEG C 1600 DEG C of heating rates, and be incubated 4h at 1600 DEG C.
It is used the foam for 50PPI for the specification as carrier, the pore size of the foamed ceramics of preparation is uniformly, almost all of
Hole is apparent pore, and hole hypertrophy of tendon and muscle is carefully more uniform, and preferably, its compression strength is 14MPa to intensity.
Embodiment 3
Ceramic powder is made up of silicon nitride 35wt%, kaolin 55wt%, aluminum oxide 6wt% and silica 4wt%.
The preprocess method of polyurethane foam：Clean surface with washing agent, then pH value be 10 aqueous slkali in soak
20min, the carboxymethylcellulose calcium being finally 0.5% with mass fraction and 5% silicon sol solution do surface-active-treatment.
The preparation method of low-k foamed ceramics, comprises the following steps：
1) by ceramic powder and Triammonium citrate ball milling mixing, dispersant is the 1.2% of ceramic powder quality, prepared viscosity
It is 65% ceramic slurry for 1200mPa s, solid content mass fraction；
2) by ceramic slurry through pretreatment specification be 70PPI polyurethane foam on carry out hanging, hanging is laggard
Row is dried in 80 DEG C of drying boxes and 24h is dried, and subsequently carries out second hanging, and 12h be dried in 120 DEG C of drying boxes, be dried after
Under air atmosphere, 160 DEG C of 260 DEG C of heating rates are 2 DEG C/min, are 0.4 0.9 in 260 DEG C 1000 DEG C of heating rates
DEG C/min, it is 3.5 5 DEG C/min in 1000 DEG C 1600 DEG C of heating rates, and be incubated 4h at 1600 DEG C.
It is used the foam for 70PPI for the specification as carrier, the pore size of the foamed ceramics of preparation is uniformly, almost all of
Hole is apparent pore, and hole hypertrophy of tendon and muscle is carefully more uniform, and preferably, its compression strength is 10MPa to intensity.
Embodiment 4
Ceramic powder is made up of silicon nitride 40wt%, kaolin 45wt%, aluminum oxide 10wt% and silica 5wt%.
The preprocess method of polyurethane foam：Clean surface with washing agent, then pH value be 10 aqueous slkali in soak
20min, the carboxymethylcellulose calcium being finally 0.5% with mass fraction and 5% silicon sol solution do surface-active-treatment.
The preparation method of low-k foamed ceramics, comprises the following steps：
1) by ceramic powder and Triammonium citrate ball milling mixing, dispersant is the 1.5% of ceramic powder quality, prepared viscosity
It is 70% ceramic slurry for 1800mPa s, solid content mass fraction；
2) by ceramic slurry through pretreatment specification be 80PPI polyurethane foam on carry out hanging, hanging is laggard
Row is dried in 80 DEG C of drying boxes and 24h is dried, and subsequently carries out second hanging, and 12h be dried in 120 DEG C of drying boxes, be dried after
Under air atmosphere, 160 DEG C of 260 DEG C of heating rates are 2 DEG C/min, are 0.4 0.9 in 260 DEG C 1000 DEG C of heating rates
DEG C/min, it is 3.5 5 DEG C/min in 1000 DEG C 1600 DEG C of heating rates, and be incubated 4h at 1600 DEG C.
It is used the foam for 80PPI for the specification as carrier, the pore size of the foamed ceramics of preparation is uniformly, almost all of
Hole is apparent pore, and hole hypertrophy of tendon and muscle is carefully more uniform, and preferably, its compression strength is 8MPa to intensity.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvement made etc., should be included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of low-k foamed ceramics is it is characterised in that comprise the following steps：
1) by ceramic powder and dispersant ball milling mixing, dispersant is the 0.5～1.5% of ceramic powder quality, and prepared viscosity is
500～1800mPa s, solid content mass fraction are 50%～70% ceramic slurry；
2) ceramic slurry is carried out hanging in the polyurethane foam through pretreatment, be dried after hanging, subsequently carry out the
Secondary hanging, drying is sintered 2～4h after 160 DEG C～1600 DEG C；
Wherein, ceramic powder is by silicon nitride 30～40wt%, kaolin 40～60wt%, aluminum oxide 5～10wt% and titanium dioxide
Silicon 1～5wt% forms.
2. the preparation method of low-k foamed ceramics according to claim 1 is it is characterised in that dispersant is lemon
Sour three ammoniums.
3. the preparation method of low-k foamed ceramics according to claim 1 is it is characterised in that polyurethane foam
Preprocess method：Clean surface with washing agent, then pH value be 8.5～10 aqueous slkali in soak 20～30min, finally use matter
Amount fraction is 0.5% carboxymethylcellulose calcium and 5% silicon sol solution does surface-active-treatment.
4. the preparation method of low-k foamed ceramics according to claim 3 is it is characterised in that polyurethane foam
Pore size is 30PPI～80PPI.
5. the preparation method of low-k foamed ceramics according to claim 1 is it is characterised in that step 2) drying side
Method is to be placed in 80～120 DEG C of drying boxes 12～24h is dried.
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| CN201610824573.5A CN106431420A (en) | 2016-09-14 | 2016-09-14 | Method for preparing low-dielectric-constant foamed ceramic |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111925229A (en) * | 2020-07-12 | 2020-11-13 | 西北工业大学 | Method for preparing high-performance foamed ceramic by combining template method with chemical vapor infiltration method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093077A (en) * | 2011-01-12 | 2011-06-15 | 中材高新材料股份有限公司 | Silicon nitride ceramic material with low dielectric constant and preparation method thereof |
| CN102417367A (en) * | 2011-09-07 | 2012-04-18 | 南昌大学 | Preparation method of high porosity sinking bead foam ceramic with controllable aperture |
| CN103253981A (en) * | 2013-04-25 | 2013-08-21 | 南昌大学 | Preparation method of mullite/silicon carbide complex-phase foamed ceramic |
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2016
- 2016-09-14 CN CN201610824573.5A patent/CN106431420A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093077A (en) * | 2011-01-12 | 2011-06-15 | 中材高新材料股份有限公司 | Silicon nitride ceramic material with low dielectric constant and preparation method thereof |
| CN102417367A (en) * | 2011-09-07 | 2012-04-18 | 南昌大学 | Preparation method of high porosity sinking bead foam ceramic with controllable aperture |
| CN103253981A (en) * | 2013-04-25 | 2013-08-21 | 南昌大学 | Preparation method of mullite/silicon carbide complex-phase foamed ceramic |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111925229A (en) * | 2020-07-12 | 2020-11-13 | 西北工业大学 | Method for preparing high-performance foamed ceramic by combining template method with chemical vapor infiltration method |
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Application publication date: 20170222 |