CN100412033C - Preparing process of great size energy-storing dielectric ceramic - Google Patents
Preparing process of great size energy-storing dielectric ceramic Download PDFInfo
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- CN100412033C CN100412033C CNB2006101254833A CN200610125483A CN100412033C CN 100412033 C CN100412033 C CN 100412033C CN B2006101254833 A CNB2006101254833 A CN B2006101254833A CN 200610125483 A CN200610125483 A CN 200610125483A CN 100412033 C CN100412033 C CN 100412033C
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Abstract
The great size energy-storing dielectric ceramic is prepared with ceramic material and borosilicate glass powder, through the steps of: dry stirring to compound mixed powder material for preparing borosilicate glass powder; high temperature smelting the mixed powder material and water quenching to prepare borosilicate glass powder; wet ball milling to obtain water-base slurry comprising ceramic material CaTiO3, BaTiO3, SrTiO3, SrZrO3, PZT, PbTiO3 and/or TiO2 and borosilicate glass powder accounting for 0.5-10 wt% of the solid material; spray pelletizing to prepare spherical grains; cold isostatic pressure forming great size ceramic biscuit; machining and singtering at 1150-1400 deg.c to obtain great size energy-storing dielectric ceramic. The great size energy-storing dielectric ceramic has high density, dielectric constant of 80-2000, voltage withstand higher than 30 kV/cm, and may be used as the energy-storing of pulse forming line and other high voltage system.
Description
Technical field
The present invention relates to a kind of preparation method of large size function ceramics, particularly a kind of preparation method who is used for the great size energy-storing dielectric ceramic of solid-state high-voltage pulse formation line technology belongs to the stupalith field.
Background technology
In the research of high-voltage pulse power technology, the pulse formation technology is a very important research project, and in more than the 40 year time of this technical development, the energy-accumulating medium that the high pressure short pulse forms line has experienced by the evolution of insulating transformer oil to deionized water.This development makes the linear induction high-current accelerator realize the target of low-resistance high current, has satisfied application requiring, and has promoted the progress and the application and development of related-art technology.At present, the pulse power part of linear induction high-current accelerator is except that the performance requriements that should satisfy accelerator itself, also require it to realize miniaturization, but it is relatively low as the pulse-forming line energy storage density of energy-accumulating medium with deionized water, to the supplemental equipment requirement height, make system huge, and " bridge joint " phenomenon can take place in the ion in the deionized water under action of high voltage, make maintenance cost very high, can not adapt to the technical requirements of the compact type pulse power.Therefore the research of carrying out novel solid-state high-density energy-accumulating medium material is extremely urgent.Because it is little that stupalith is revealed, the energy storage density height, if adopt and have the function ceramics of high-k and high-electric breakdown strength as energy-accumulating medium, can greatly reduce the physical length of pulse-forming line, greatly reduce requirement, thereby realize the miniaturization and the superpowerization of pulse power system subsystem.
The energy-storing dielectric ceramic that is applied to high-voltage pulse formation line need satisfy following requirement: the energy storage density that (1) is high; (2) low dielectric loss tg η; (3) specific structure and bigger physical size.At present, the research with high energy storage density ceramic systems has been obtained bigger progress, these systems comprise TiO
2System, PbTiO
3System, BaTiO
3System, SrTiO
3System, and their compound system.But, but there is very big difficulty in the preparation of the function ceramics of the large-size high-quality that satisfies its specified shape requirement, this has greatly limited the further popularization of function ceramics on Pulse Power Techniques are used.At present, report is also seldom seen in preparation method's the research that has a large size function ceramics of high energy storage density for this class.
Summary of the invention
The present invention is directed to the problem that exists in the current Pulse Power Techniques, a kind of preparation method of great size energy-storing dielectric ceramic is provided, make the great size energy-storing dielectric ceramic of preparing have high energy storage density, low dielectric loss, bigger physical size and specific contour structures, stable and reliable for performance, can directly apply to high-voltage pulse and form line.
The present invention is achieved through the following technical solutions,
The preparation method of great size energy-storing dielectric ceramic of the present invention, this Chu can be made by ceramic raw material and borosilicate glass powder by media ceramic, and its preparation process is as follows successively:
(1) the dry mixing preparation is used to prepare the mixed powder of borosilicate glass powder;
(2) mixed powder high melt and the shrend with step (1) prepares the borosilicate glass powder;
(3) mix the aqueous slurries of forming by the wet ball grinding preparation by ceramic raw material and borosilicate glass powder;
(4) the aqueous slurries mist projection granulating that step (3) is obtained obtains spheroidal particle;
(5) the spheroidal particle cold isostatic compaction that step (4) is obtained obtains forming great size ceramic biscuit;
(6) biscuit of ceramics that step (5) is obtained is machined into needed shape and size;
(7) will promptly obtain large-sized energy-storing dielectric ceramic through step (6) processed ceramics biscuit at 1150 ℃～1400 ℃ sintering temperatures;
Wherein said ceramic raw material is that purity is higher than 99% BaTiO
3, SrTiO
3, SrZrO
3, PbTiO
3, PZT (Pb-based lanthanumdoped zirconate titanates), TiO
2In the powder one or more, the initial particle of powder is 0.1～2 micron, the add-on of borosilicate glass powder is 0.5%～10% of a solid material quality in the aqueous slurries.
Below the inventive method is further described, particular content is as follows:
(1) the dry mixing preparation is used to prepare the mixed powder technology of borosilicate glass powder:
With purity greater than 99% PbO, H
3BO
3, SiO
2, CaO, Al
2O
3And Bi
2O
3Powder feeds intake according to proportioning, and dry mixing mixes it, and wherein the content of PbO is 0～30% of mixed powder quality, H
3BO
3Content be 10%～30% of mixed powder quality, SiO
2Content be 30%～60% of mixed powder quality, the content of CaO is 0～25% of mixed powder quality, Al
2O
3Content be 0～25% of mixed powder quality, Bi
2O
3Content be 0～20% of mixed powder quality, the quality percentage composition sum of each component of mixed powder is 100%, and PbO, CaO, Al
2O
3And Bi
2O
3Four kinds of raw materials are not zero simultaneously.
(2) above-mentioned mixed powder high melt and shrend prepare the borosilicate glass powder craft
The mixed powder that mixes is dropped in corundum or the platinum crucible, carried out high melt in 2 hours 1400 ℃～1500 ℃ insulations, then the fused frit is poured into immediately and carried out shrend in the deionized water, form the glass slag, with drying behind the broken ball milling of glass ground-slag, promptly obtain the borosilicate glass powder again.
(3) mix the aqueous slurries technology of forming by the wet ball grinding preparation by ceramic raw material and borosilicate glass powder
Ceramic raw material is mixed by the design proportioning with above-mentioned borosilicate glass powder, be prepared into wet ball grinding solid material, adopt rotary mill or agitating ball mill to carry out wet ball grinding, with Triammonium citrate as dispersion agent, with polyvinyl alcohol (PVA) as binding agent, with propyl carbinol or n-Octanol as defoamer, deionized water is as solvent, select for use agate ball or zirconia ball as ball-milling medium, wherein the diameter of ball is between 5 millimeters-12 millimeters, the add-on of borosilicate glass powder is 0.5%～10% of a solid material quality in the wet ball grinding solid material, dispersant is 0.2～1% of a solid material content quality, the content of binding agent is 0.2～2% of solid material content quality, propyl carbinol or n-Octanol content are the 0.2-0.8% of solid material content quality, the mass ratio of solid material and deionized water is 1: 0.4～2, and the mass ratio of solid material and ball-milling medium is 1: 1～4.The borosilicate glass powder directly is 0.1～2 micron.
During ball milling, the deionized water that at first will be dissolved with dispersion agent joins in the ball mill, drop into the solid material (ceramic raw material and above-mentioned borosilicate glass powder compound) that mixes then, behind the wet ball grinding 4～8 hours, in slip, add binding agent and defoamer again, then continued ball milling 2～4 hours, thereby make good dispersity, system is stable, is suitable for the aqueous slurries of mist projection granulating.
(4) the aqueous slurries mist projection granulating is centrifugal spraying or press atomization granulation, and the processing parameter of mist projection granulating is: inlet temperature is between 160～200 ℃, and air outlet temperature is between 110～120 ℃; Above method can be prepared size distribution between 20～200 microns and the spheroidal particle of good fluidity.
(5) spheroidal particle behind the mist projection granulating obtains forming great size ceramic biscuit technology by cold isostatic compaction
Spheroidal particle is inserted in the compressible resilient mould, and swing die limit, limit filler is piled up it naturally, sealing is put into the isostatic cool pressing Oil cylinder and is pressurizeed then, and pressure is between 100～300 MPas, forming great size ceramic biscuit is taken out in pressurize 5～30 minutes from elastic mould after the release.In actual production, can design difform elastic mould, and then make the forming great size ceramic biscuit of specified shape.
(6) biscuit of ceramics is machined into needed shape and size
Adopt anchor clamps that biscuit of ceramics is fixed on the lathe, be processed into needed shape and size.These machining process comprise: saw, mill, operation such as car, mill.
(7) biscuit of ceramics after the mechanical workout sinters the technology of great size energy-storing dielectric ceramic into
The processed ceramics biscuit is placed the corundum saggar with suspention, mode edge-on or that stand upside down, and the ZrO of high-temperature calcination is adopted in the space between alms bowl body and the biscuit of ceramics
2Powder, Al
2O
3Powder or ceramic raw material landfill, place gas kiln or electric furnace to carry out sintering in saggar, sintering temperature is between 1150～1400 ℃, and soaking time is between 1～4 hour, temperature rise rate is between 0.5～3 ℃/minute, and rate of temperature fall is between 1～5 ℃/minute.After temperature in the stove is lower than 200 ℃, can take out saggar, thereby finish the preparation process of great size energy-storing dielectric ceramic.
In the preparation of great size energy-storing dielectric ceramic, our research work is found: by the component of change borosilicate glass frit and the percentage composition ratio between each component, can adjust the fusing point and the wetting property of borosilicate glass powder, make it satisfy the processing requirement of different ceramic raw materials.An amount of borosilicate glass powder mixes in ceramic raw material, can significantly reduce the sintering temperature of energy-storing dielectric ceramic, suppress the misgrowth of ceramic crystalline grain, improve the porcelain body density, and then improve its withstand voltage properties, simultaneously, the doping broadening of borosilicate glass frit the sintering range of energy-storing dielectric ceramic, suppressed the stress cracking that causes because of density gradient in the densification process; But excessive doping can cause the porcelain body strain cracking, also can worsen its dielectric properties.The blending process of aqueous slurries has considerable influence to viscosity, dispersiveness and the stability of slip, and then influences the quality of mist projection granulating.Tackiness agent adds very little, and biscuit of ceramics intensity is not high, can influence its processing characteristics; Tackiness agent adds too much, can reduce forming of green body density and porcelain body sintered density.Atomizing granulating technology has considerable influence to the spheroidal particle quality of preparing, and suitable atomizing granulating technology helps to prepare the specific particle size range and the full particle of good fluidity.The cold isostatic compaction hypotony can reduce the density of biscuit of ceramics; Hypertonia can cause the biscuit cracking on the contrary.If ceramic sintering temperature is low excessively, can reduce its density; If sintering temperature is too high, porcelain body can produce gross blow hole.
Preparation method's simple and reliable process of the present invention, cost is low, can prepare coaxial shape, disc, cylindrical, plate shaped and other erose great size energy-storing dielectric ceramic, ceramic body density height is out of shape little, its specific inductivity is between 80～2000, withstand voltage between 30～90 kv/cm, product can have better market prospect and commercial value directly as the energy-accumulating medium of pulse-forming line and other high-pressure system.
Description of drawings
The spheroidal particle that obtains by mist projection granulating among Fig. 1: the embodiment 2.
The coaxial shape biscuit of ceramics that obtains by isostatic cool pressing and mechanical workout among Fig. 2: the embodiment 2.
The plate shaped biscuit of ceramics that obtains by isostatic cool pressing and mechanical workout among Fig. 3: the embodiment 3.
The plate shaped energy-storing dielectric ceramic sample of large size of preparation among Fig. 4: the embodiment 4.
Embodiment
Content below in conjunction with method provides specific embodiment:
The per-cent of material (%) unless otherwise indicated, means mass percent among the following embodiment.
Embodiment 1:
With 18%Al
2O
3Add 30t%H
3BO
3Add 52%SiO
2Powder mixes, and 1500 ℃ of insulations 2 hours, ball milling obtained glass powder after the shrend, then according to 99.5%TiO
2The ratio preparation aqueous slurries solid material that adds 0.5% borosilicate glass powder, solid material and deionized water quality ratio are 1: 1, Triammonium citrate content is 1% of solid material quality, the content of polyvinyl alcohol (PVA) is 0.5% of solid material quality, propyl carbinol is about 0.5% of solid material quality, and the mass ratio of solid material and ball-milling medium is 1: 2.Carried out wet ball grinding 4 hours by said ratio; The aqueous slurries of ball milling preparation is carried out centrifugal spray granulation, and inlet temperature is 165 ± 5 ℃, and air outlet temperature is 115 ± 5 ℃, and flow is 3 kilograms/hour; Utilize cold isostatic compaction, forming pressure 150 MPas, pressurize 5 minutes; Be machined into plate shaped after, 1400 ℃ of sintering 3 hours, make the large size function ceramics, ceramic body relative density 95.5%, specific inductivity is 90～100, dielectric loss is 8 * 10
-4, withstand voltage is 80～85kV/cm.
Embodiment 2:
With 25%Al
2O
3Add 30%H
3BO
3Add 45%SiO
2Powder mixes, and 1500 ℃ of insulations 2 hours, ball milling obtained the borosilicate glass powder after the shrend, then according to 98%TiO
2The ratio preparation aqueous slurries solid material that adds 2% borosilicate glass powder, solid material and deionized water quality ratio are 1: 2, Triammonium citrate content is about 0.5% of solid material quality, the content of PVA is 0.5% of solid material quality, n-Octanol is 0.5% of a solid material quality, and the mass ratio of solid material and ball-milling medium is 1: 4.Carried out wet ball grinding 4 hours by said ratio; The aqueous slurries of ball milling preparation is carried out centrifugal spray granulation, and inlet temperature is 165 ± 5 ℃, and air outlet temperature is 115 ± 5 ℃, and flow is 3 kilograms/hour; Utilize cold isostatic compaction, forming pressure 150 MPas, pressurize 5 minutes; Be machined into plate shaped after, 1380 ℃ of sintering 1 hour, make the large size function ceramics, ceramic body relative density 95.5%, specific inductivity is 80～100, dielectric loss is 8 * 10
-4, withstand voltage is 80～85 kv/cm.
Embodiment 3:
15%CaO is added 20%H
3BO
3Add 45%SiO
2 add20%Bi
2O
3Powder mixes, and 1450 ℃ of insulations 2 hours, ball milling obtained the borosilicate glass powder after the shrend, then according to 8.2%SrZrO
3Add 87.8%SrTiO
3The ratio preparation aqueous slurries solid material that adds 4% borosilicate glass powder, solid material and deionized water quality ratio are 1: 0.8., Triammonium citrate content is 0.7% of solid material quality, the content of PVA is 0.8% of solid material quality, propyl carbinol is about 0.4% of solid material quality, and the mass ratio of solid material and ball-milling medium is 1: 1.Carried out wet ball grinding 6 hours by said ratio; The aqueous slurries of ball milling preparation is carried out centrifugal spray granulation, and inlet temperature is 165 ± 5 ℃, and air outlet temperature is 110 ± 5 ℃, and flow is 5 kilograms/hour, utilizes cold isostatic compaction, forming pressure 200 MPas, pressurize 5 minutes; After being machined into coaxial shape,, make the large size function ceramics 1300 ℃ of sintering 3 hours, ceramic body relative density 96.2%, specific inductivity is 280～300, dielectric loss is 2 * 10
-3, withstand voltage is 60～65 kv/cm.
Embodiment 4:
21%CaO is added 25%H
3BO
3Add 42%SiO
2Add 12%Bi
2O
3Powder mixes, and 1450 ℃ of insulations 2 hours, ball milling obtained glass powder after the shrend, then according to 8.2%SrZrO
3Add 87.8t%SrTiO
3The ratio preparation aqueous slurries solid material that adds 4% borosilicate glass powder, solid material and deionized water quality ratio are 1: 0.8., Triammonium citrate content is 0.7% of solid material quality, the content of PVA is 0.8% of solid material quality, propyl carbinol is 0.4% of a solid material quality, and the mass ratio of solid material and ball-milling medium is 1: 2.Carried out wet ball grinding 6 hours by said ratio; The aqueous slurries of ball milling preparation is carried out centrifugal spray granulation, and inlet temperature is about 165 ℃, and air outlet temperature is 110 ℃, and flow is 5 kilograms/hour, utilizes cold isostatic compaction, forming pressure 200 MPas, pressurize 5 minutes; After being machined into coaxial shape,, make the large size function ceramics 1250 ℃ of sintering 3 hours, ceramic body relative density 96.2%, specific inductivity is 280～300, dielectric loss is 2 * 10
-3, withstand voltage is 60～65kV/cm.
Embodiment 5:
16%PbO is added 24%H
3BO
3Add 60%SiO
2Powder mixes, and 1400 ℃ of insulations 2 hours, ball milling obtained the borosilicate glass powder after the shrend, then according to 34.56%BaTiO
3+ 63.44%SrTiO
3The ratio preparation aqueous slurries solid material of+2% borosilicate glass powder, solid material and deionized water quality ratio are: 1: 0.6, Triammonium citrate content is 0.5% of solid material quality, the content of PVA is 1% of solid material quality, propyl carbinol is about 0.6% of solid material quality, and the mass ratio of solid material and ball-milling medium is about 1: 2.Carried out wet ball grinding 8 hours by said ratio; The aqueous slurries of ball milling preparation is carried out centrifugal spray granulation, and inlet temperature is 170 ± 5 ℃, and air outlet temperature is 115 ± 5 ℃, and flow is 5 kilograms/hour, utilizes cold isostatic compaction, forming pressure 250 MPas, pressurize 5 minutes; Be machined into plate shaped after, 1250 ℃ of sintering 2 hours, make the large size function ceramics, ceramic body relative density 96.4%, specific inductivity is 500-550, dielectric loss is 2 * 10
-2, withstand voltage is 40～45 kv/cm.
Embodiment 6:
25%CaO is added 15%Al
2O
3Add 10%H
3BO
3Add 35%SiO
2Add 15%Bi
2O
3Powder mixes, and 1400 ℃ of insulations 2 hours, ball milling obtained the borosilicate glass powder after the shrend, then according to 45.28%BaTiO
3+ 48.72%SrTiO
3The ratio preparation aqueous slurries solid material of+6% borosilicate glass powder, solid material and deionized water quality ratio are 1: 0.5, Triammonium citrate content is 0.7% of solid material quality, the content of PVA is 2% of solid material quality, propyl carbinol is 0.8% of a solid material quality, and the mass ratio of solid material and ball-milling medium is 1: 2.Carried out wet ball grinding 10 hours by said ratio; The aqueous slurries of ball milling preparation is carried out centrifugal spray granulation, and inlet temperature is 180 ± 5 ℃, and air outlet temperature is 115 ± 5 ℃, and flow is 5 kilograms/hour, utilizes cold isostatic compaction, forming pressure 150 MPas, pressurize 15 minutes; Be machined into plate shaped after, 1225 ℃ of sintering 2 hours, make the large size function ceramics, ceramic body relative density 95.3%, specific inductivity is 700-750, dielectric loss is 4 * 10
-2, withstand voltage is 38～40 kv/cm.
Embodiment 7:
30%PbO is added 15%CaO add 25%H
3BO
3Add 30%SiO
2Powder mixes, 1400 ℃ of insulations 2 hours, ball milling obtains the borosilicate glass powder after the shrend, the ratio preparation aqueous slurries solid material that adds 10% borosilicate glass powder then according to 90%PZT, solid material and deionized water quality ratio are 1: 0.6, and Triammonium citrate content is 0.6% of solid material quality, and the content of PVA is 0.2% of solid material quality, propyl carbinol is 0.2% of a solid material quality, and the mass ratio of solid material and ball-milling medium is 1: 2.Carried out wet ball grinding 6 hours by said ratio; The aqueous slurries of ball milling preparation is carried out centrifugal spray granulation, and inlet temperature is 170 ± 5 ℃, and air outlet temperature is 115 ± 5 ℃, and flow is 2 kilograms/hour, utilizes cold isostatic compaction, forming pressure 200 MPas, pressurize 5 minutes; Be machined into plate shaped after, 1150 ℃ of sintering 4 hours, make the large size function ceramics, ceramic body relative density 95.6%, specific inductivity is 1400-1500, dielectric loss is 6 * 10
-2, withstand voltage is 32～36 kv/cm.
Embodiment 8:
15%PbO is added 8%CaO add 12%Al
2O
3Add 20%H
3BO
3Add 35%SiO
2Add 10%Bi
2O
3Powder mixes, and 1400 ℃ of insulations 2 hours, ball milling obtained the borosilicate glass powder after the shrend, then according to 86.44%BaTiO
3Add 5.56%SrZrO
3The ratio preparation aqueous slurries solid material that adds 8% borosilicate glass powder, solid material and deionized water quality ratio are 1: 1. Triammonium citrate content is 0.2% of solid material quality, the content of PVA is 0.4% of solid material quality, propyl carbinol is 0.4% of a solid material quality, and the mass ratio of solid material and ball-milling medium is 1: 2.Carried out wet ball grinding 12 hours by said ratio; The aqueous slurries of ball milling preparation is carried out centrifugal spray granulation, and inlet temperature is 195 ± 5 ℃, and air outlet temperature is 120 ℃, and flow is 5 kilograms/hour, utilizes cold isostatic compaction, forming pressure 200 MPas, pressurize 20 minutes; 1250 ℃ of sintering 3 hours, make the large size function ceramics after the mechanical workout, ceramic body relative density 95.2%, specific inductivity is 1800-2000, dielectric loss is 8 * 10
-2, withstand voltage is 30～32 kv/cm.
Claims (8)
1. the preparation method of a great size energy-storing dielectric ceramic is characterized in that, this energy-storing dielectric ceramic is made by ceramic raw material and borosilicate glass powder, and its preparation process is as follows successively:
(1) the dry mixing preparation is used to prepare the mixed powder of borosilicate glass powder;
(2) mixed powder with step (1) prepares the borosilicate glass powder by high melt and shrend;
(3) mix the aqueous slurries of forming by the wet ball grinding preparation by ceramic raw material and borosilicate glass powder;
(4) the aqueous slurries mist projection granulating that step (3) is obtained obtains spheroidal particle;
(5) the spheroidal particle cold isostatic compaction that step (4) is obtained obtains forming great size ceramic biscuit;
(6) biscuit of ceramics that step (5) is obtained is machined into needed shape and size;
(7) will promptly obtain large-sized energy-storing dielectric ceramic through step (6) processed ceramics biscuit at 1150 ℃～1400 ℃ sintering temperatures;
Wherein said ceramic raw material is that purity is higher than 99% BaTiO
3, SrTiO
3, SrZrO
3, PbTiO
3, Pb-based lanthanumdoped zirconate titanates, TiO
2In the powder one or more, the initial particle of powder is 0.1～2 micron, the add-on of borosilicate glass powder is 0.5%～10% of a solid material quality in the aqueous slurries.
2. the preparation method of great size energy-storing dielectric ceramic as claimed in claim 1 is characterized in that described dry mixing preparation is used to prepare the mixed powder of borosilicate glass powder, is greater than 99% PbO, H with purity
3BO
3, SiO
2, CaO, Al
2O
3And Bi
2O
3Powder feeds intake according to proportioning, and dry mixing mixes it, and wherein the content of PbO is 0～30% of mixed powder quality, H
3BO
3Content be 10%～30% of mixed powder quality, SiO
2Content be 30%～60% of mixed powder quality, the content of CaO is 0～25% of mixed powder quality, Al
2O
3Content be 0～25% of mixed powder quality, Bi
2O
3Content be 0～20% of mixed powder quality, the quality percentage composition sum of each component of mixed powder is 100%, and PbO, CaO, Al
2O
3And Bi
2O
3Four kinds of raw materials are not zero simultaneously.
3. the preparation method of great size energy-storing dielectric ceramic as claimed in claim 1 is characterized in that the technology that described mixed powder high melt and shrend prepare the borosilicate glass powder is:
The mixed powder of dry mixing preparation is dropped in corundum or the platinum crucible, carried out high melt in 2 hours 1400 ℃～1500 ℃ insulations, then the frit of fusing is poured into immediately and carried out shrend in the deionized water, form the glass slag, again glass slag ball is galled the oven dry of broken back, promptly obtain the borosilicate glass powder, its particle diameter is 0.1～2 micron.
4. the preparation method of great size energy-storing dielectric ceramic as claimed in claim 1 is characterized in that described wet ball grinding preparation by the technology that ceramic raw material and borosilicate glass powder mix the aqueous slurries of forming is:
The deionized water that at first will be dissolved with dispersion agent joins in the ball mill, drop into then by ceramic raw material and borosilicate glass powder and mix the solid material of forming, behind the wet ball grinding 4～8 hours, in slip, add binding agent and defoamer again, then continue ball milling 2～4 hours, thereby make the aqueous slurries that is suitable for mist projection granulating.
5. the preparation method of great size energy-storing dielectric ceramic as claimed in claim 4, it is characterized in that described ceramic raw material mixes the solid material of forming with the borosilicate glass powder, adopt rotary mill or agitating ball mill to carry out wet ball grinding, with Triammonium citrate as dispersion agent, with polyvinyl alcohol as binding agent, with propyl carbinol or n-Octanol as defoamer, deionized water is as solvent, with agate ball or zirconia ball as ball-milling medium, wherein the diameter of ball is between 5 millimeters～12 millimeters, the add-on of borosilicate glass powder is 0.5%～10% of a solid material quality in the wet ball grinding solid material, dispersant is 0.2%～1% of a solid material content quality, the content of binding agent is 0.2%～2% of solid material content quality, propyl carbinol or n-Octanol content are 0.2%～0.8% of solid material content quality, the mass ratio of solid material and deionized water is 1: 0.4～2, and the mass ratio of solid material and ball-milling medium is 1: 1～4.
6. the preparation method of great size energy-storing dielectric ceramic as claimed in claim 1, the method that it is characterized in that described aqueous slurries mist projection granulating is centrifugal spraying or press atomization, the processing parameter of mist projection granulating is: inlet temperature is between 160～200 ℃, air outlet temperature is between 110～120 ℃, and the particle of being made is 20～200 microns a spheroidal particle.
7. the preparation method of great size energy-storing dielectric ceramic as claimed in claim 1 is characterized in that the technology that described spheroidal particle cold isostatic compaction obtains forming great size ceramic biscuit is:
Spheroidal particle is inserted in the compressible resilient mould swing die limit, limit filler, sealing then, putting into the isostatic cool pressing Oil cylinder pressurizes, pressure is between 100～300 MPas, and pressurize 5～30 minutes is taken out from elastic mould after the release and had forming great size ceramic biscuit.
8. the preparation method of great size energy-storing dielectric ceramic as claimed in claim 1 is characterized in that, the sintering process of the forming great size ceramic biscuit after the described mechanical workout is:
Biscuit of ceramics is placed the corundum saggar with suspention, mode edge-on or that stand upside down, adopt the Al of high-temperature calcination in the saggar around the biscuit
2O
3Powder, ZrO
2Powder or ceramic raw material powder are filled, place gas kiln or electric furnace to carry out sintering, sintering temperature is between 1150 ℃～1400 ℃, and soaking time is between 1～4 hour, temperature rise rate is between 0.5～3 ℃/minute, and rate of temperature fall is between 1～5 ℃/minute.
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| CN104211407B (en) * | 2014-09-05 | 2017-03-01 | 中国钢研科技集团有限公司 | A kind of moulding process of big-size complicated shape ceramics biscuits of carbonized bricks |
| CN104986955B (en) * | 2015-06-23 | 2018-01-12 | 电子科技大学 | A kind of nano-TiO2With insulating glass composite and preparation method thereof |
| CN109694247B (en) * | 2019-01-08 | 2021-08-20 | 陕西科技大学 | High-efficiency energy-storage linear dielectric ceramic material and preparation method thereof |
| CN112573831A (en) * | 2020-12-08 | 2021-03-30 | 赣州中瓷科技有限公司 | Glass bead for fixing filament of incandescent lamp and preparation process thereof |
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| CN1826299A (en) * | 2004-03-01 | 2006-08-30 | 株式会社村田制作所 | Insulating ceramic composition, insulating ceramic sintered body, and multilayer ceramic electronic component |
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| US6585951B1 (en) * | 2000-10-30 | 2003-07-01 | Idaho Research Foundation, Inc. | Methods for manufacturing dielectric powders |
| CN1606897A (en) * | 2001-12-21 | 2005-04-13 | 伊菲雷技术有限公司 | Low firing temperature thick film dielectric layer for electroluminescent display |
| CN1826299A (en) * | 2004-03-01 | 2006-08-30 | 株式会社村田制作所 | Insulating ceramic composition, insulating ceramic sintered body, and multilayer ceramic electronic component |
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