CN107129307A - A kind of preparation method of composite conductive ceramic material - Google Patents
A kind of preparation method of composite conductive ceramic material Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of composite conductive ceramic material, the preparation method mainly dry, calcine and crush four steps by the preparation including mixed solution, the preparation of composite particles slurry, separation.The preparation method technique of the composite conductive ceramic material of the present invention is simple, production cycle is shorter, the materials safety used is nontoxic, the conducting ceramic material prepared is difficult the moisture absorption and reunion, dispersive property is good, in fine particle shape, electric conductivity is excellent, is adapted to large-scale industrial production and is used as electrostatic ceramic film and solid fuel cell, motor material.
Description
Technical field
The present invention relates to conductive material technical field, and in particular to a kind of preparation method of composite conductive ceramic material.
Background technology
Conducting ceramic material refers to possess ionic conduction, electronics, a kind of new function material of hole conduction in ceramic material
Material.Conductivity ceramics integrates metal electric property and ceramic structure characteristic, with electric properties such as metalloid electric conductivity,
It is architectural feature again with ceramics simultaneously, such as chemical property stabilization, high temperature resistant, long lifespan, radioresistance, corrosion-resistant, anti-oxidant,
It can be widely applied to the fields such as electrode, gas sensor, ferroelectric material, superconductor.At present, the preparation method of conductivity ceramics is main
There are sintering process, wet chemistry method, gaseous penetration method, microwave sintering method etc..The preparation method of above-mentioned conductivity ceramics, except purposes respectively has not
With outer, also there are problems that numerous and diverse process, process cycle length, complex process, cost of material, it is difficult to large-scale industry metaplasia
Production.
The content of the invention
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, there is provided a kind of preparation of composite conductive ceramic material
Method, the preparation technology is simple, and the cycle is shorter, and the materials safety used is nontoxic, and the conducting ceramic material prepared is difficult the moisture absorption
And reunion, electric conductivity is excellent, is adapted to large-scale industrial production.
The present invention solves technical problem and adopted the following technical scheme that：
A kind of preparation method of composite conductive ceramic material, comprises the following steps：
（1）The preparation of mixed solution：Diatomite is crossed after 80~100 mesh sieves and added in reaction vessel, deionized water is added, delayed
Slow to add beta-silicon nitride powder, the hydrochloric acid solution for being added dropwise 10~20% adjusts system pH to 3~5,10~20min of mechanical agitation,
Obtain dispersion liquid；By Zinc oxide powder, silicon carbide powder, Zirconium oxide powder, thorium oxide powder according to mass ratio 3~5：1~2：2
~3：Added after 1~2 mixing in dispersion liquid, the hydrochloric acid solution for adding 10~30% adjusts pH to 4~5, is obtained after stirring
Mixed solution；
（2）The preparation of composite particles slurry：By mixed solution under the conditions of 60~80 DEG C insulated and stirred 3~4 hours, then be warming up to
120~150 DEG C of insulated and stirreds 1~2 hour, pour into glass jar and stand 20~24 hours, obtain composite particles slurry；
（3）Separate drying：Composite particles 5~10min of pulp centrifuged separation is taken, is poured into separatory funnel, will using deionized water
Solid phase is washed 3~5 times, until being not detected by chlorion substantially；It is put into after solid phase washing in microwave drying oven, in 80~100 DEG C
Dry to water content and be less than 5%, obtain composite conductive powder；
（4）Calcining, crushing：Composite conductive powder is placed in roaster and is calcined 2~3 hours, then naturally cools to room temperature, is sent into
Air-flow micronizer, ultramicro grinding obtains the composite conductive ceramic material of the mesh of particle diameter 300~600.
Preferably, the step（1）The consumption of deionized water is 10~20 times of diatomite quality, and the consumption of silicon nitride is
1.5~2.5 times of diatomite quality.
Preferably, the Zinc oxide powder, silicon carbide powder, Zirconium oxide powder, thorium oxide powder are according to mass ratio 4：1：
3：Added after 2 mixing in dispersion liquid.
Preferably, the step（2）Mixed liquor is poured slowly into glass jar using separatory funnel.
Preferably, the step（3）Centrifuge and use common centrifugal separator, rotating speed is 4000~6000r/min.
Preferably, the step（3）Microwave drying oven select particle microwave vacuum dryer, its microwave power be 20~
40KW, vacuum pressure is 0.05~0.08MPa.
Preferably, the step（4）Roasting furnace temperature elevation is heated up using three hierarchical process, and the specially first stage is warming up to
400~500 DEG C, 5~10min is incubated, second stage is warming up to 650~750 DEG C, is incubated 10~20min, and the phase III is warming up to
850~950 DEG C, it is incubated 30~40min；The summation of heating and soaking time was ensured at 2~3 hours.
Preferably, the step（4）Air-flow ultramicro grinding carries out air-flow powder using the mixed gas of nitrogen and carbon dioxide
Broken, operating temperature is 10~20 DEG C.
Compared with prior art, the present invention has following beneficial effect：
（1）The preparation method of the composite conductive ceramic material of the present invention, the main preparation including mixed solution, composite particles slurry
Preparation, separation is dried, four steps are crushed in calcining, the preparation method technique is simple, and the production cycle is shorter, the raw material peace used
Atoxic, the conducting ceramic material prepared is difficult the moisture absorption and reunion, and dispersive property is good, and in fine particle shape, electric conductivity is excellent
It is good, it is adapted to large-scale industrial production and is used as electrostatic ceramic film and solid fuel cell, motor material.
（2）The mixed solution of the present invention, using the excellent diatomite of loose porous, adhesive property as matrix composition, with nitridation
Silicon formation dispersion, recycle ion-exchange reactions by zinc oxide, carborundum, zirconium oxide, the hydrochloric acid solution of thorium oxide with it is molten
Composite diatomite after swollen, control ph causes combined efficiency higher, and most of sodium ion in diatomite is replaced.
（3）The mixed solution of the present invention is stirred by heating up, standing obtains composite particles slurry, then by centrifuging,
Microwave drying obtains composite conducting conductor, and conducting ceramic material is obtained finally by temperature programming, air-flow crushing, by accurately controlling
The parameters such as temperature and time processed, it is ensured that the size and specification of each link product so that the conducting ceramic material collection metal electricity
Performance and the corrosion-resistant of ceramics, waterproof, resistance to compression, antioxygenic property are.
Embodiment
Invention is described in further detail below in conjunction with specific embodiment.
Embodiment 1
A kind of preparation method of composite conductive ceramic material, comprises the following steps：
（1）The preparation of mixed solution：100g diatomite is crossed after 80~100 mesh sieves and added in reaction vessel, 1500g is added
Ionized water, is slowly added to 210g beta-silicon nitride powders, and the hydrochloric acid solution for being added dropwise 15% adjusts system pH to 3~5, mechanical agitation
16min, obtains dispersion liquid；Zinc oxide powder 20g, silicon carbide powder 5g, Zirconium oxide powder 15g, thorium oxide powder 10g are mixed
Add afterwards in dispersion liquid, the hydrochloric acid solution for adding 20% adjusts pH to 4~5, and mixed solution is obtained after stirring.
（2）The preparation of composite particles slurry：By mixed solution under the conditions of 66 DEG C insulated and stirred 3.5 hours, then be warming up to
130 DEG C of insulated and stirreds 1.2 hours, are then poured slowly into glass jar using separatory funnel, are stood 22 hours, are obtained composite particles
Slurry.
（3）Separate drying：The pulp centrifuged separation 6min of composite particles is taken, is poured into separatory funnel, will using deionized water
Solid phase is washed 3~5 times, until being not detected by chlorion substantially；It is put into microwave drying oven, is dried extremely in 90 DEG C after solid phase washing
Water content is less than 5%, obtains composite conductive powder.Wherein, centrifuge use common centrifugal separator, rotating speed be 4000~
6000r/min；Microwave drying oven selects particle microwave vacuum dryer, and its microwave power is 20~40KW, and vacuum pressure is
0.05~0.08MPa.
（4）Calcining, crushing：Composite conductive powder is placed in roaster and is calcined 2~3 hours, heating uses three stage journeys
Sequence heats up, and the specially first stage is warming up to 400~500 DEG C, is incubated 5~10min, and second stage is warming up to 650~750 DEG C,
10~20min is incubated, the phase III is warming up to 850~950 DEG C, is incubated 30~40min；The summation of heating and soaking time ensures
At 2~3 hours；Room temperature is naturally cooled to again, air-flow micronizer is sent into, and ultramicro grinding obtains the purpose of particle diameter 300~600 and answered
Close conducting ceramic material.Wherein, air-flow ultramicro grinding carries out air-flow crushing, work using the mixed gas of nitrogen and carbon dioxide
Temperature is 10~20 DEG C.
Embodiment 2
A kind of preparation method of composite conductive ceramic material, comprises the following steps：
（1）The preparation of mixed solution：100g diatomite is crossed after 80~100 mesh sieves and added in reaction vessel, 1600g is added and goes
Ionized water, is slowly added to beta-silicon nitride powder 180g, and the hydrochloric acid solution for being added dropwise 10~20% adjusts system pH to 3~5, machinery
10~20min is stirred, dispersion liquid is obtained；By Zinc oxide powder 16g, silicon carbide powder 4g, Zirconium oxide powder 12g, thorium oxide powder
Added after last 8g mixing in dispersion liquid, the hydrochloric acid solution for adding 10~30% adjusts pH to 4~5, is mixed after stirring
Solution.
（2）The preparation of composite particles slurry：By mixed solution under the conditions of 75 DEG C insulated and stirred 3.6 hours, then be warming up to
140 DEG C of insulated and stirreds 1.8 hours, are then poured slowly into glass jar using separatory funnel, are stood 24 hours, are obtained composite particles
Slurry.
（3）Separate drying：The pulp centrifuged separation 8min of composite particles is taken, is poured into separatory funnel, will using deionized water
Solid phase is washed 3~5 times, until being not detected by chlorion substantially；It is put into microwave drying oven, is dried extremely in 92 DEG C after solid phase washing
Water content is less than 5%, obtains composite conductive powder.Wherein, centrifuge use common centrifugal separator, rotating speed be 4000~
6000r/min；Microwave drying oven selects particle microwave vacuum dryer, and its microwave power is 20~40KW, and vacuum pressure is
0.05~0.08MPa.
（4）Calcining, crushing：Composite conductive powder is placed in roaster and is calcined 2~3 hours, heating uses three stage journeys
Sequence heats up, and the specially first stage is warming up to 400~500 DEG C, is incubated 5~10min, and second stage is warming up to 650~750 DEG C,
10~20min is incubated, the phase III is warming up to 850~950 DEG C, is incubated 30~40min；The summation of heating and soaking time ensures
At 2~3 hours；Room temperature is naturally cooled to again, air-flow micronizer is sent into, and ultramicro grinding obtains the purpose of particle diameter 300~600 and answered
Close conducting ceramic material.Wherein, air-flow ultramicro grinding carries out air-flow crushing, work using the mixed gas of nitrogen and carbon dioxide
Temperature is 10~20 DEG C.
Embodiment 3
A kind of preparation method of composite conductive ceramic material, comprises the following steps：
（1）The preparation of mixed solution：100g diatomite is crossed after 80~100 mesh sieves and added in reaction vessel, deionization is added
Water 2200g, is slowly added to beta-silicon nitride powder 200g, and the hydrochloric acid solution for being added dropwise 10~20% adjusts system pH to 3~5, machinery
20min is stirred, dispersion liquid is obtained；By Zinc oxide powder 24g, silicon carbide powder 10g, Zirconium oxide powder 10g, thorium oxide powder 6g
Added after mixing in dispersion liquid, the hydrochloric acid solution for adding 10~30% adjusts pH to 4~5, mixing is obtained after stirring molten
Liquid.
（2）The preparation of composite particles slurry：By mixed solution under the conditions of 75 DEG C insulated and stirred 3.8 hours, then be warming up to
140 DEG C of insulated and stirreds 1.6 hours, are then poured slowly into glass jar using separatory funnel, are stood 24 hours, are obtained composite particles
Slurry.
（3）Separate drying：The pulp centrifuged separation 10min of composite particles is taken, is poured into separatory funnel, will using deionized water
Solid phase is washed 3~5 times, until being not detected by chlorion substantially；It is put into microwave drying oven, is dried extremely in 95 DEG C after solid phase washing
Water content is less than 5%, obtains composite conductive powder.Wherein, centrifuge use common centrifugal separator, rotating speed be 4000~
6000r/min；Microwave drying oven selects particle microwave vacuum dryer, and its microwave power is 20~40KW, and vacuum pressure is
0.05~0.08MPa.
（4）Calcining, crushing：Composite conductive powder is placed in roaster and is calcined 2~3 hours, heating uses three stage journeys
Sequence heats up, and the specially first stage is warming up to 400~500 DEG C, is incubated 5~10min, and second stage is warming up to 650~750 DEG C,
10~20min is incubated, the phase III is warming up to 850~950 DEG C, is incubated 30~40min；The summation of heating and soaking time ensures
At 2~3 hours；Room temperature is naturally cooled to again, air-flow micronizer is sent into, and ultramicro grinding obtains the purpose of particle diameter 300~600 and answered
Close conducting ceramic material.Wherein, air-flow ultramicro grinding carries out air-flow crushing, work using the mixed gas of nitrogen and carbon dioxide
Temperature is 10~20 DEG C.
Embodiment 4
A kind of preparation method of composite conductive ceramic material, comprises the following steps：
（1）The preparation of mixed solution：100g diatomite is crossed after 80~100 mesh sieves and added in reaction vessel, deionization is added
Water 1800g, is slowly added to beta-silicon nitride powder 250g, and the hydrochloric acid solution for being added dropwise 10~20% adjusts system pH to 3~5, machinery
10~20min is stirred, dispersion liquid is obtained；By Zinc oxide powder 20g, silicon carbide powder 5g, Zirconium oxide powder 8g, thorium oxide powder
Added after 6g mixing in dispersion liquid, the hydrochloric acid solution for adding 10~30% adjusts pH to 4~5, mixing is obtained after stirring molten
Liquid.
（2）The preparation of composite particles slurry：By mixed solution under the conditions of 60~80 DEG C insulated and stirred 3~4 hours, then rise
Then temperature is poured slowly into glass jar using separatory funnel to 120~150 DEG C of insulated and stirreds 1~2 hour, stands 20~24 small
When, obtain composite particles slurry.
（3）Separate drying：Composite particles 5~10min of pulp centrifuged separation is taken, pours into separatory funnel, uses deionization
Water washs solid phase 3~5 times, until being not detected by chlorion substantially；It is put into after solid phase washing in microwave drying oven, in 80~
100 DEG C of dryings to water content is less than 5%, obtains composite conductive powder.Wherein, centrifuge and use common centrifugal separator, rotating speed
For 4000~6000r/min；Microwave drying oven selects particle microwave vacuum dryer, and its microwave power is 20~40KW, vacuum
Pressure is 0.05~0.08MPa.
（4）Calcining, crushing：Composite conductive powder is placed in roaster and is calcined 2~3 hours, heating uses three stage journeys
Sequence heats up, and the specially first stage is warming up to 400~500 DEG C, is incubated 5~10min, and second stage is warming up to 650~750 DEG C,
10~20min is incubated, the phase III is warming up to 850~950 DEG C, is incubated 30~40min；The summation of heating and soaking time ensures
At 2~3 hours；Room temperature is naturally cooled to again, air-flow micronizer is sent into, and ultramicro grinding obtains the purpose of particle diameter 300~600 and answered
Close conducting ceramic material.Wherein, air-flow ultramicro grinding carries out air-flow crushing, work using the mixed gas of nitrogen and carbon dioxide
Temperature is 10~20 DEG C.
Described above is only the preferred embodiment of the present invention, and protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical schemes belonged under thinking of the present invention belong to protection scope of the present invention.It should be pointed out that for the art
Those of ordinary skill for, some improvements and modifications without departing from the principles of the present invention, also should be regarded as the present invention
Protection domain.
Claims (8)
1. a kind of preparation method of composite conductive ceramic material, it is characterised in that comprise the following steps：
（1）The preparation of mixed solution：Diatomite is crossed after 80~100 mesh sieves and added in reaction vessel, deionized water is added, delayed
Slow to add beta-silicon nitride powder, the hydrochloric acid solution for being added dropwise 10~20% adjusts system pH to 3~5,10~20min of mechanical agitation,
Obtain dispersion liquid；By Zinc oxide powder, silicon carbide powder, Zirconium oxide powder, thorium oxide powder according to mass ratio 3~5：1~2：2
~3：Added after 1~2 mixing in dispersion liquid, the hydrochloric acid solution for adding 10~30% adjusts pH to 4~5, is obtained after stirring
Mixed solution；
（2）The preparation of composite particles slurry：By mixed solution under the conditions of 60~80 DEG C insulated and stirred 3~4 hours, then be warming up to
120~150 DEG C of insulated and stirreds 1~2 hour, pour into glass jar and stand 20~24 hours, obtain composite particles slurry；
（3）Separate drying：Composite particles 5~10min of pulp centrifuged separation is taken, is poured into separatory funnel, will using deionized water
Solid phase is washed 3~5 times, until being not detected by chlorion substantially；It is put into after solid phase washing in microwave drying oven, in 80~100 DEG C
Dry to water content and be less than 5%, obtain composite conductive powder；
（4）Calcining, crushing：Composite conductive powder is placed in roaster and is calcined 2~3 hours, then naturally cools to room temperature, is sent into
Air-flow micronizer, ultramicro grinding obtains the composite conductive ceramic material of the mesh of particle diameter 300~600.
2. the preparation method of composite conductive ceramic material according to claim 1, it is characterised in that the step（1）Go
The consumption of ionized water is 10~20 times of diatomite quality, and the consumption of silicon nitride is 1.5~2.5 times of diatomite quality.
3. the preparation method of composite conductive ceramic material according to claim 1, it is characterised in that the oxide powder and zinc
End, silicon carbide powder, Zirconium oxide powder, thorium oxide powder are according to mass ratio 4：1：3：Added after 2 mixing in dispersion liquid.
4. the preparation method of composite conductive ceramic material according to claim 1, it is characterised in that the step（2）It is mixed
Liquid is closed to be poured slowly into glass jar using separatory funnel.
5. the preparation method of composite conductive ceramic material according to claim 1, it is characterised in that the step（3）From
Heart separation uses common centrifugal separator, and rotating speed is 4000~6000r/min.
6. the preparation method of composite conductive ceramic material according to claim 1, it is characterised in that the step（3）It is micro-
Ripple drying box selects particle microwave vacuum dryer, and its microwave power is 20~40KW, and vacuum pressure is 0.05~0.08MPa.
7. the preparation method of composite conductive ceramic material according to claim 1, it is characterised in that the step（4）Roasting
Stove heating is burnt using the heating of three hierarchical process, and the specially first stage is warming up to 400~500 DEG C, is incubated 5~10min, second-order
Section is warming up to 650~750 DEG C, is incubated 10~20min, and the phase III is warming up to 850~950 DEG C, is incubated 30~40min；Heating
Ensure with the summation of soaking time at 2~3 hours.
8. the preparation method of composite conductive ceramic material according to claim 1, it is characterised in that the step（4）Gas
Flow ultramicro grinding and air-flow crushing is carried out using the mixed gas of nitrogen and carbon dioxide, operating temperature is 10~20 DEG C.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1962544A (en) * | 2005-11-11 | 2007-05-16 | 中国科学院金属研究所 | Resistivity-controllable conductive silicon carbide foam ceramic material and its preparing process |
| CN103819190A (en) * | 2013-12-23 | 2014-05-28 | 青岛润鑫伟业科贸有限公司 | Preparation method of thoria conducting ceramic material |
| CN105174945A (en) * | 2015-08-03 | 2015-12-23 | 苏州云舒新材料科技有限公司 | Conductive ceramic material and preparation method thereof |
| CN105541309A (en) * | 2016-01-26 | 2016-05-04 | 苏州羽帆新材料科技有限公司 | Temperature-sensitive conductive ceramic material and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962544A (en) * | 2005-11-11 | 2007-05-16 | 中国科学院金属研究所 | Resistivity-controllable conductive silicon carbide foam ceramic material and its preparing process |
| CN103819190A (en) * | 2013-12-23 | 2014-05-28 | 青岛润鑫伟业科贸有限公司 | Preparation method of thoria conducting ceramic material |
| CN105174945A (en) * | 2015-08-03 | 2015-12-23 | 苏州云舒新材料科技有限公司 | Conductive ceramic material and preparation method thereof |
| CN105541309A (en) * | 2016-01-26 | 2016-05-04 | 苏州羽帆新材料科技有限公司 | Temperature-sensitive conductive ceramic material and preparation method thereof |
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