CN115819070B - Ceramic slurry and ceramic matrix - Google Patents
Ceramic slurry and ceramic matrix Download PDFInfo
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- CN115819070B CN115819070B CN202211435853.9A CN202211435853A CN115819070B CN 115819070 B CN115819070 B CN 115819070B CN 202211435853 A CN202211435853 A CN 202211435853A CN 115819070 B CN115819070 B CN 115819070B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 174
- 239000002002 slurry Substances 0.000 title claims abstract description 60
- 239000011159 matrix material Substances 0.000 title claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 87
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052709 silver Inorganic materials 0.000 claims abstract description 28
- 239000004332 silver Substances 0.000 claims abstract description 28
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 17
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- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 15
- 239000010439 graphite Substances 0.000 claims abstract description 15
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910000484 niobium oxide Inorganic materials 0.000 claims abstract description 14
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 229910000449 hafnium oxide Inorganic materials 0.000 claims abstract description 13
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- 239000002904 solvent Substances 0.000 claims abstract description 13
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 12
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- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 12
- 239000011521 glass Substances 0.000 claims abstract description 12
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 12
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- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 5
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- 238000001914 filtration Methods 0.000 claims description 4
- 229910001867 inorganic solvent Inorganic materials 0.000 claims description 4
- 239000003049 inorganic solvent Substances 0.000 claims description 4
- 229920000609 methyl cellulose Polymers 0.000 claims description 4
- 239000001923 methylcellulose Substances 0.000 claims description 4
- 239000004584 polyacrylic acid Substances 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
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- QBUKAFSEUHGMMX-MTJSOVHGSA-N (5z)-5-[[3-(1-hydroxyethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical compound C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1C(C)O QBUKAFSEUHGMMX-MTJSOVHGSA-N 0.000 description 1
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Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses ceramic slurry, and relates to the technical fields of ceramic slurry and ceramic production. A ceramic slurry comprising the following components in mass percent: 40-69% of ceramic skeleton powder, 5-20% of conductive powder, 20-40% of pore-forming agent, 0.15-0.75% of performance auxiliary agent, 2-8% of adhesive, 0.5-2.0% of dispersing agent and 2-10% of solvent; the ceramic skeleton powder is at least one of diatomite, kaolin and sodium silicate; the conductive powder is at least one of flake graphite, carbon nano tubes, nickel powder, silver-coated copper powder and silver-coated glass powder; the performance auxiliary agent is a mixture of niobium oxide, hafnium oxide and nano zirconium dioxide. The ceramic slurry can be used for preparing a ceramic matrix, and the obtained ceramic matrix has high average porosity, good thermal shock resistance, high-temperature oxidation resistance, bending strength and excellent conductivity; the ceramic matrix prepared from the ceramic slurry has conductivity, and the surface of the ceramic matrix is not required to be coated with the conductive slurry.
Description
Technical Field
The invention relates to the technical field of ceramic slurry and ceramic production, in particular to ceramic slurry and a ceramic matrix.
Background
The heating element used on the atomizer mainly comprises a metal heating element and a ceramic heating element, wherein the metal heating element is divided into a metal heating sheet or a heating wire, is the simplest and most common heating source, and has the advantages of high heating speed, long service life, low price and the like, so that the heating element is widely used. However, the metal heating element has the defect of active chemical property and cannot be used in corrosive environments such as acid or alkali; meanwhile, if the metal heating element is dry-burned (when the gas-soluble substance in the atomizer is insufficient or absent, the heating element is electrically conductive), an odor is generated.
The ceramic heater uses high purity ceramic as matrix and surface printing resistor slurry as heat source. The ceramic has stable chemical property, is not easy to react with other substances, and has stable heating and constant temperature, so the ceramic is often applied to the field of accurate temperature control. However, the traditional ceramic heating element has low strength and is easy to crack in the transportation and atomization processes; the conductive paste is not conductive, and the conductive paste is coated on the surface of the conductive paste to be applied to an aerosol atomization device, so that the conductive paste can be used as an atomization core to realize matrix atomization or preheating, and the phenomenon of core pasting is prevented; meanwhile, the process of coating the conductive paste on the surface is complex and has poor stability.
Therefore, research on ceramic powder is urgently needed, and the ceramic powder can be used for preparing porous and conductive ceramic, so that the ceramic has high strength, high-temperature oxidation resistance, high ageing resistance and other high performances, and multi-gradient sheet resistance can be realized by adjusting the proportion of the added conductive powder and the conductive powder.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides ceramic slurry which comprises ceramic framework powder, conductive powder, pore-forming agent, performance auxiliary agent, adhesive, dispersing agent and solvent, wherein the components cooperate with each other to enable the ceramic slurry to be used for preparing conductive ceramic. The ceramic prepared by the slurry has high average porosity, good thermal shock resistance, high-temperature oxidation resistance, bending strength and excellent conductivity, can realize multi-gradient sheet resistance by adjusting the proportion of the added conductive powder and the conductive powder, has excellent conductivity of an atomization core and can stably atomize when the sheet resistance is 150-300mΩ/≡, so that the ceramic can be applied to an aerosol atomization device for preparing the atomization core, realizes multistage heating atomization and prevents the occurrence of the phenomenon of core pasting.
Meanwhile, the invention also provides a preparation method of the ceramic slurry and a preparation method for preparing the conductive ceramic by using the ceramic slurry, which are simple, have few parameters and are beneficial to realizing large-scale mass production.
In particular, in one aspect, the invention discloses a ceramic slurry, which comprises the following components in percentage by mass: 40-69% of ceramic skeleton powder, 5-20% of conductive powder, 20-40% of pore-forming agent, 0.15-0.75% of performance auxiliary agent, 2-8% of adhesive, 0.5-2.0% of dispersing agent and 2-10% of solvent;
the ceramic skeleton powder is at least one of diatomite, kaolin and sodium silicate;
the conductive powder is at least one of flake graphite, carbon nano tubes, nickel powder, silver-coated copper powder and silver-coated glass powder;
the performance auxiliary agent is a mixture of niobium oxide, hafnium oxide and nano zirconium dioxide.
Preferably, in the performance auxiliary agent, niobium oxide accounts for 0.05-0.5% of the total mass of the ceramic slurry, hafnium oxide accounts for 0.05-0.5% of the total mass of the ceramic slurry, and nano zirconium dioxide accounts for 0.05-0.5% of the total mass of the ceramic slurry.
Preferably, the pore-forming agent is at least one of sawdust, starch, polyvinyl alcohol and polyvinyl chloride.
Preferably, the binder is at least one of paraffin, methylcellulose, ethylcellulose and polyethylene.
Preferably, the dispersing agent is at least one of stearic acid, polyvinylpyrrolidone and polyacrylic acid.
Preferably, the solvent is at least one of polyethylene glycol and terpineol.
The invention also discloses a preparation method of the ceramic slurry, which comprises the steps of premixing and grinding conductive powder, ceramic skeleton powder, pore-forming agent and performance auxiliary agent, and adding adhesive, dispersing agent and solvent for kneading for 4-12 hours to obtain the required ceramic slurry.
Preferably, the conductive powder needs to be pretreated; when the conductive powder is flake graphite or carbon nano tube, the pretreatment method is that the conductive powder is presintered for 3-6 hours at 250-500 ℃; when the conductive powder is nickel powder, silver-coated copper powder or silver-coated glass powder, the pretreatment method comprises the steps of soaking the conductive powder in an inorganic solvent, filtering and drying.
On the other hand, the invention also discloses a ceramic matrix capable of conducting electricity, which is obtained by using the ceramic slurry through granulation, injection molding and degreasing sintering.
Preferably, the degreasing is to keep the temperature for 2-4 hours in a reducing atmosphere at 400-650 ℃; the sintering is carried out in a reducing atmosphere at 1100-1300 ℃ for 1.5-3 hours.
The beneficial effects are that:
(1) The ceramic slurry comprises ceramic skeleton powder, conductive powder, pore-forming agent, performance auxiliary agent, adhesive, dispersing agent and solvent, wherein the components cooperate with each other to enable the ceramic slurry to be used for preparing a conductive ceramic matrix. The ceramic prepared from the ceramic slurry has high average porosity, good thermal shock resistance, high-temperature oxidation resistance, bending strength and excellent conductivity, and can realize multi-gradient sheet resistance by adjusting the proportion of the conductive powder, so that the ceramic can be applied to an aerosol atomization device for preparing an atomization core, multistage heating atomization is realized, and the phenomenon of pasting the core is prevented; specifically, the average porosity of the ceramic is 50-80%, the average pore diameter is 15-30 mu m, the compressive strength is 25-45MPa, the thermal shock resistance is good under a water quenching method, and the aging resistance is good under a high-temperature high-humidity reliability test.
(1) The preparation method of the ceramic slurry is simple, has few parameters, and is beneficial to realizing large-scale mass production; meanwhile, when the ceramic slurry is used for preparing the ceramic matrix, the prepared ceramic matrix has conductivity without coating the conductive slurry on the surface of the ceramic, and the ceramic matrix is simple to operate, has few parameters and is beneficial to large-scale mass production.
Drawings
In order to more clearly illustrate the technical solutions of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a microscopic view of the ceramic matrix prepared in example 1;
FIG. 2 is a microscopic view of the ceramic substrate prepared in comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be understood that the terms "comprises" and "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
It should be further understood that the term "and/or" as used in the present specification and the appended claims refers to any and all possible combinations of one or more of the associated listed items, and includes such combinations.
It should be further understood that, as used in the present specification and appended claims, the term "concentration" refers to mass concentration, and "%" refers to mass percent; unless otherwise indicated.
Ceramic slurry
The composite material comprises the following components in percentage by mass: 40-69% of ceramic skeleton powder, 5-20% of conductive powder, 20-40% of pore-forming agent, 0.15-0.75% of performance auxiliary agent, 2-8% of adhesive, 0.5-2.0% of dispersing agent and 2-10% of solvent;
the ceramic skeleton powder is at least one of diatomite, kaolin and sodium silicate;
the conductive powder is at least one of flake graphite, carbon nano tube, nickel powder, silver-coated copper powder and silver-coated glass powder; wherein the nickel powder can be silver-coated nickel powder or spherical nickel powder (D90 is less than 15 mu m);
the performance auxiliary agent is a mixture of niobium oxide, hafnium oxide and nano zirconium dioxide; wherein, in the performance auxiliary agent, niobium oxide accounts for 0.05 to 0.5 percent of the total mass of the ceramic slurry, hafnium oxide accounts for 0.05 to 0.5 percent of the total mass of the ceramic slurry, and nano zirconium dioxide accounts for 0.05 to 0.5 percent of the total mass of the ceramic slurry;
the pore-forming agent is at least one of saw dust, starch, polyvinyl alcohol and polyvinyl chloride;
the adhesive is at least one of paraffin, methyl cellulose, ethyl cellulose and polyethylene;
the dispersing agent is at least one of stearic acid, polyvinylpyrrolidone and polyacrylic acid;
the solvent is at least one of polyethylene glycol and terpineol.
The conductive powder preferably comprises the following components: at least one of flake graphite or carbon nano tube, the content is 1-20%; and at least one of nickel powder, silver coated copper powder or silver coated glass powder, wherein the content is 80-100%. Wherein, the flake graphite has a similar lamellar structure or carbon nanotube structure, and conductive powder such as nickel powder, silver-coated copper powder or silver-coated glass powder is added into the flake graphite, so that a good and stable one-dimensional structure can be constructed, the flake graphite has adhesiveness, and in the subsequent preparation process, the conductive structure of the ceramic matrix can be constructed, thereby providing conductivity for the ceramic matrix.
The performance auxiliary agent improves the performances of thermal shock resistance, high-temperature oxidation resistance, bending strength and the like of the ceramic through the mutual synergistic effect of niobium oxide, hafnium oxide and nano zirconium dioxide.
A method for preparing a ceramic slurry comprising the steps of:
s1, pretreatment is carried out on conductive powder, ceramic framework powder and pore-forming agent.
Specifically, the ceramic skeleton powder and the pore-forming agent are placed in a drying furnace at 90-110 ℃ for drying for 3-6 hours, and then are taken out for standby.
When the conductive powder is flake graphite or carbon nano tube, the conductive powder is pre-sintered for 3-6 hours at 250-500 ℃; when the conductive powder is nickel powder, silver-coated copper powder or silver-coated glass powder, the pretreatment method comprises the steps of soaking the conductive powder in an inorganic solvent, filtering and drying, wherein the organic solvent is preferably 50% alcohol.
The purpose of the pretreatment of the conductive powder is to remove oil stains, impurities and organic matters on the surface, and the conductive powder is cooled to room temperature for standby after the pretreatment.
S2, kneading, namely premixing and grinding the pretreated conductive powder, ceramic skeleton powder, pore-forming agent and performance auxiliary agent, and adding an adhesive, a dispersing agent and a solvent for kneading for 4-12 hours to obtain ceramic slurry.
Specifically, firstly, a three-dimensional mixer is used for carrying out premix mixing on ceramic skeleton powder, conductive powder, pore-forming agent and performance auxiliary agent, then a grinder is used for fully and uniformly mixing, the ground powder is added into a kneader, then an adhesive, a dispersing agent and an organic solvent are sequentially added, and the mixture is kneaded for 4-12 hours, so that ceramic slurry is obtained.
Ceramic matrix capable of conducting electricity
Granulating, injection molding, degreasing and sintering the ceramic slurry to obtain the ceramic slurry;
degreasing, namely, preserving heat for 2-4 hours in a reducing atmosphere at 400-650 ℃; the sintering is carried out in a reducing atmosphere at 1100-1300 ℃ for 1.5-3 hours. The reducing atmosphere is preferably a nitrogen atmosphere.
Specifically, the granulation is granulation injection molding, and after standing and cooling ceramic slurry, the ceramic slurry is put into a granulator for granulation to form granules; then injection molding is carried out on the pelletization material by a molding machine to obtain a molded green body; degreasing and sintering, namely burying powder into the formed green body, placing, performing catalytic degreasing by using a nitrogen atmosphere catalytic furnace, and sintering to obtain ceramic; specifically, the catalytic degreasing is to keep the temperature for 2-4 hours in a reducing atmosphere at 400-650 ℃; sintering, namely, preserving heat for 1.5-3 hours in a reducing atmosphere at 1100-1300 ℃.
Example 1:
the preparation method of the ceramic matrix capable of conducting electricity in the embodiment is as follows:
(1) Weighing 20% of flake graphite (D90=1000 meshes, purity 99%) by mass percent, putting into a muffle furnace, calcining at 400 ℃ for 3 hours, and taking out and cooling for standby; 5% of silver-coated nickel powder, 75% of spherical nickel powder (D90 is less than 15 mu m) is ultrasonically treated in 50% alcohol for 0.5 hour, and after suction filtration, the mixture is dried in a drying furnace at 80 ℃ for 2 hours and then mixed with graphite for standby; the diatomite, the kaolin, the sodium silicate and the starch are respectively put into a 100 ℃ drying furnace in advance for drying for 4 hours and then taken out for standby.
(2) According to mass percent, 20 percent of conductive powder, 16 percent of diatomite, 21 percent of kaolin, 5 percent of sodium silicate, 25 percent of starch, 0.2 percent of niobium oxide, 0.15 percent of hafnium oxide and 0.15 percent of nano zirconium dioxide are fully mixed by a three-roll mill and a grinder, 2 percent of polyethylene, 6 percent of paraffin, 2 percent of stearic acid and 2.5 percent of polyethylene glycol are added into a kneader, banburying and kneading are carried out for 6 hours at 95 ℃, ceramic slurry is obtained after kneading and cooling, and then the ceramic slurry is put into a ceramic granulator for granulation, thus obtaining granular ceramic feed with uniform size.
(3) The ceramic raw body is obtained by feeding ceramic through an injection molding process, and the process parameters are as follows: the molding pressure was 25bar and the speed was 25cm 3 And/s, wherein the injection temperature is 95 ℃, and the mold temperature is 26 ℃, so as to obtain the ceramic green body.
(4) Placing the ceramic green compact in a sagger, covering with alumina powder, degreasing in a nitrogen atmosphere catalytic furnace, degreasing according to a specific degreasing curve, wherein the maximum temperature is 580 ℃, and the heat preservation time is 1.5 hours;
(5) And after degreasing, placing the ceramic substrate into a reducing atmosphere sintering furnace for sintering, heating and sintering according to a specific curve, wherein the maximum temperature is 1160 ℃, preserving heat for 2 hours, and cooling to room temperature along with the furnace to obtain the ceramic substrate.
The ceramic matrix is detected, the thermal shock resistance is good under a water quenching method, and the ageing resistance is good under a high-temperature high-humidity reliability test.
Example 2:
the preparation method of the ceramic matrix capable of conducting electricity in the embodiment is as follows:
(1) Weighing 3% of the multiwall carbon nanotubes by mass percent, putting the multiwall carbon nanotubes into a muffle furnace, calcining the multiwall carbon nanotubes for 3 hours at 300 ℃, and taking out the multiwall carbon nanotubes for cooling for standby; 15% of silver-coated nickel powder, 82% of spherical nickel powder (D90 is less than 10 mu m) is ultrasonically treated in 50% alcohol for 0.5 hour, and after suction filtration, the silver-coated nickel powder is dried in a drying furnace at 80 ℃ for 2 hours and mixed for later use; the diatomite, the kaolin, the sodium silicate and the starch are respectively put into a 100 ℃ drying furnace in advance for drying for 4 hours and then taken out for standby.
(2) According to mass percent, 20 percent of conductive powder, 16 percent of diatomite, 21 percent of kaolin, 5 percent of sodium silicate, 25 percent of starch, 0.2 percent of niobium oxide, 0.15 percent of hafnium oxide and 0.15 percent of nano zirconium dioxide are fully mixed by a three-roll mill and a grinder, 2 percent of polyethylene, 6 percent of paraffin, 2 percent of stearic acid and 2.5 percent of polyethylene glycol are added into a kneader, banburying and kneading are carried out for 6 hours at 95 ℃, ceramic slurry is obtained after kneading and cooling, and then the ceramic slurry is put into a ceramic granulator for granulation, thus obtaining granular ceramic feed with uniform size.
(3) The ceramic raw body is obtained by feeding ceramic through an injection molding process, and the process parameters are as follows: the molding pressure was 25bar and the speed was 25cm 3 And/s, wherein the injection temperature is 95 ℃, and the mold temperature is 26 ℃, so as to obtain the ceramic green body.
(4) Placing the ceramic green compact in a sagger, covering with alumina powder, degreasing in a nitrogen atmosphere catalytic furnace, degreasing according to a specific degreasing curve, wherein the maximum temperature is 580 ℃, and the heat preservation time is 1.5 hours;
(5) And after degreasing, placing the ceramic substrate into a reducing atmosphere sintering furnace for sintering, heating and sintering according to a specific curve, wherein the maximum temperature is 1160 ℃, preserving heat for 2 hours, and cooling to room temperature along with the furnace to obtain the ceramic substrate.
The ceramic matrix obtained is detected, and the ceramic matrix has better thermal shock resistance and aging resistance under a high-temperature high-humidity reliability test by a water quenching method.
Example 3:
the preparation method of the ceramic matrix capable of conducting electricity in the embodiment is as follows:
(1) Weighing 3% of the multiwall carbon nanotubes by mass percent, putting the multiwall carbon nanotubes into a muffle furnace, calcining the multiwall carbon nanotubes for 3 hours at 300 ℃, and taking out the multiwall carbon nanotubes for cooling for standby; 15% of silver-coated copper powder, 82% of spherical nickel powder, ultrasonic treatment for 0.5 hour in 50% alcohol, suction filtration, drying in a drying oven at 80 ℃ for 2 hours, and mixing for later use; the diatomite, the kaolin, the sodium silicate and the sawdust are respectively put into a 100 ℃ drying furnace in advance for drying for 4 hours and then taken out for standby.
(2) According to mass percent, 10 percent of conductive powder, 20 percent of diatomite, 28 percent of kaolin, 16 percent of sodium silicate, 20 percent of sawdust, 0.25 percent of niobium oxide, 0.20 percent of hafnium oxide and 0.05 percent of nano zirconium dioxide are fully mixed by a three-roll mill, and then 1 percent of methyl cellulose, 1 percent of ethyl cellulose, 1 percent of paraffin, 0.5 percent of polyacrylic acid and 2.0 percent of terpineol are added into a kneader for banburying and kneading for 6 hours at 95 ℃, ceramic slurry is obtained after kneading and cooling, and then the ceramic slurry is put into a ceramic granulator for granulation, so that granular ceramic feed with uniform size is obtained.
(3) The ceramic raw body is obtained by feeding ceramic through an injection molding process, and the process parameters are as follows: the molding pressure was 25bar and the speed was 25cm 3 And/s, wherein the injection temperature is 95 ℃, and the mold temperature is 26 ℃, so as to obtain the ceramic green body.
(4) Placing the ceramic green compact in a sagger, covering with alumina powder, degreasing in a nitrogen atmosphere catalytic furnace, degreasing according to a specific degreasing curve, wherein the maximum temperature is 580 ℃, and the heat preservation time is 1.5 hours;
(5) And after degreasing, placing the ceramic substrate into a reducing atmosphere sintering furnace for sintering, heating and sintering according to a specific curve, wherein the maximum temperature is 1160 ℃, preserving heat for 2 hours, and cooling to room temperature along with the furnace to obtain the ceramic substrate.
The ceramic matrix obtained is detected, and the ceramic matrix has better thermal shock resistance and aging resistance under a high-temperature high-humidity reliability test by a water quenching method.
Example 4:
the preparation method of the ceramic matrix capable of conducting electricity in the embodiment is as follows:
(1) Weighing 3% of the multiwall carbon nanotubes by mass percent, putting the multiwall carbon nanotubes into a muffle furnace, calcining the multiwall carbon nanotubes for 3 hours at 300 ℃, and taking out the multiwall carbon nanotubes for cooling for standby; 15% of silver-coated glass powder, 82% of spherical nickel powder (D90 is less than 10 mu m) in 50% alcohol for 0.5 hour by ultrasonic treatment, drying in a drying furnace at 80 ℃ for 2 hours after suction filtration, and mixing for later use; the diatomite, the kaolin, the sodium silicate, the polyvinyl alcohol and the polyvinyl chloride are respectively put into a 100 ℃ drying furnace in advance for drying for 4 hours, and then taken out for standby.
(2) According to mass percent, 7% of conductive powder, 10% of diatomite, 20% of kaolin, 10% of sodium silicate, 20% of polyvinyl alcohol, 20% of polyvinyl chloride, 0.05% of niobium oxide, 0.25% of hafnium oxide and 0.25% of nano zirconium dioxide are fully mixed by a three-roll mill and a grinder, 2% of ethyl cellulose, 1% of paraffin, 1.0% of polyvinylpyrrolidone and 8.05% of terpineol are added into a kneader, banburying and kneading are carried out for 6 hours at 95 ℃, ceramic slurry is obtained after kneading and cooling, and then the ceramic slurry is put into a ceramic granulator for granulation, and granular ceramic feed with uniform size is obtained.
(3) The ceramic raw body is obtained by feeding ceramic through an injection molding process, and the process parameters are as follows: the molding pressure was 25bar and the speed was 25cm 3 And/s, wherein the injection temperature is 95 ℃, and the mold temperature is 26 ℃, so as to obtain the ceramic green body.
(4) Placing the ceramic green compact in a sagger, covering with alumina powder, degreasing in a nitrogen atmosphere catalytic furnace, degreasing according to a specific degreasing curve, wherein the maximum temperature is 580 ℃, and the heat preservation time is 1.5 hours;
(5) And after degreasing, placing the ceramic substrate into a reducing atmosphere sintering furnace for sintering, heating and sintering according to a specific curve, wherein the maximum temperature is 1160 ℃, preserving heat for 2 hours, and cooling to room temperature along with the furnace to obtain the ceramic substrate.
The ceramic matrix obtained is detected, and the ceramic matrix has better thermal shock resistance and aging resistance under a high-temperature high-humidity reliability test by a water quenching method.
Meanwhile, the following comparative examples were set according to example 1, as shown in table 1.
Table 1 comparative example and example 1 difference table
In comparative examples 3 to 6, less than 100% of the solvent was used up to 100%.
The porosity, the aperture, the compressive strength and the sheet resistance of the ceramic matrix are respectively measured by a porous density intelligent analyzer, an aperture analyzer, a flat pressure tester and a four-probe resistance tester;
the ceramic substrates prepared in examples and comparative examples were tested for performance by the above test methods, and the results of the performance parameters obtained are shown in table 2.
Table 2 performance tables of the ceramic matrices of examples and comparative examples
Meanwhile, the ceramic matrixes of the examples and the comparative examples are tested for thermal shock resistance by a water quenching method, and the ageing resistance is tested by a high-temperature high-humidity reliability test; the results of the obtained performance parameters are shown in Table 3.
Wherein, the ceramic matrix prepared in example 1 is shown in FIG. 1; a microscopic view of the ceramic matrix prepared in comparative example 1 is shown in FIG. 2.
Table 3 performance tables of ceramic substrates of examples and comparative examples
As is clear from tables 2-3, the ceramic substrates prepared in examples 1-4 have an average porosity of 50-80%, an average pore diameter of 15-30 μm, a compressive strength of 25-45MPa, and good thermal shock resistance and aging resistance under high temperature and high humidity reliability test. The ceramic matrix prepared by the method has high average porosity, good thermal shock resistance, high-temperature oxidation resistance, bending strength and excellent conductivity, and can realize multi-gradient sheet resistance by adjusting the proportion of the conductive powder, so that the ceramic matrix can be applied to an aerosol atomization device for preparing an atomization core, multistage heating atomization is realized, and the phenomenon of pasting the core is prevented.
In the comparative example, under the condition that the comparative example 1 is not dried, the conductive powder is agglomerated in the organic solvent, the subsequent grinding and dispersing effects are general, as can be seen from a microscopic image 2, so that the conductive network cannot be connected efficiently, and the sheet resistance of the final matrix is relatively high; in comparative example 2, the conductive powder is not pretreated, organic matters and other impurities exist on the surface of the conductive powder, the purity of the conductive powder is affected, and residues and large sheet resistance exist in a reducing atmosphere; in comparative example 3, the influence of graphite and carbon nano tubes on the performance of the ceramic matrix is not great, but the purpose of controlling the cost can be achieved under the condition of not influencing the conductivity by properly adding the graphite and carbon nano tubes.
In comparative examples 4 to 9, niobium oxide can effectively form a three-dimensional structure in porous ceramics, and due to the characteristics thereof, the electron diffusion capacity is reduced in the electromigration process, the conductivity is indirectly improved, meanwhile, the oxidation resistance and acid resistance of the porous ceramics at high temperature are better, and the lack of niobium oxide is not beneficial to improving the conductivity of a ceramic matrix and the oxidation resistance at high temperature; hafnium oxide has certain fire resistance, and can form silicon-hafnium bond with silicon dioxide under a certain temperature in a reducing atmosphere, so that the strength of the whole ceramic matrix is improved, but the square resistance is easily increased due to the wide band gap and high dielectric constant of the ceramic matrix and excessive addition; the nano zirconium dioxide has stable chemical property, and proper amount of the nano zirconium dioxide is added, so that the thermal shock resistance of the ceramic matrix is improved due to the good phase change toughening property of the nano zirconium dioxide, and the hardness of the ceramic matrix can be improved.
In the foregoing embodiments, the descriptions of the embodiments are focused on, and for those portions of one embodiment that are not described in detail, reference may be made to the related descriptions of other embodiments.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related technical fields are included in the scope of the present invention.
Claims (9)
1. A ceramic slurry characterized by comprising the following components in percentage by mass: 40-69% of ceramic skeleton powder, 5-20% of conductive powder, 20-40% of pore-forming agent, 0.15-0.75% of performance auxiliary agent, 2-8% of adhesive, 0.5-2.0% of dispersing agent and 2-10% of solvent;
the ceramic skeleton powder is at least one of diatomite, kaolin and sodium silicate;
the conductive powder comprises the following components: at least one of flake graphite or carbon nano tube, the content of which is 1-20% of the conductive powder; and at least one of nickel powder, silver-coated copper powder or silver-coated glass powder, wherein the content of the nickel powder, the silver-coated copper powder or the silver-coated glass powder accounts for 80-100% of the conductive powder;
when the nickel powder, the silver-coated copper powder or the silver-coated glass powder is used as the conductive powder, the pretreatment method comprises the steps of soaking the conductive powder in an inorganic solvent, filtering and drying;
the performance auxiliary agent is a mixture of niobium oxide, hafnium oxide and nano zirconium dioxide;
in the performance auxiliary agent, niobium oxide accounts for 0.05-0.5% of the total mass of the ceramic slurry, hafnium oxide accounts for 0.05-0.5% of the total mass of the ceramic slurry, and nano zirconium dioxide accounts for 0.05-0.5% of the total mass of the ceramic slurry.
2. The ceramic slurry of claim 1, wherein the pore-forming agent is at least one of sawdust, starch, polyvinyl alcohol, polyvinyl chloride.
3. The ceramic slurry of claim 2, wherein the binder is at least one of paraffin, methylcellulose, ethylcellulose, polyethylene.
4. The ceramic slurry of claim 3, wherein the dispersant is at least one of stearic acid, polyvinylpyrrolidone, and polyacrylic acid.
5. The ceramic slurry of claim 4, wherein the solvent is at least one of polyethylene glycol and terpineol.
6. A method for preparing the ceramic slurry according to any one of claims 1 to 5, wherein the conductive powder, the ceramic skeleton powder, the pore-forming agent and the performance aid are premixed and ground, and the binder, the dispersant and the solvent are added and kneaded for 4 to 12 hours to obtain the ceramic slurry.
7. The method for preparing ceramic slurry according to claim 6, wherein the conductive powder is subjected to pretreatment; when the conductive powder is flake graphite or carbon nano tube, the pretreatment method is that the conductive powder is presintered for 3-6 hours at 250-500 ℃; when the conductive powder is nickel powder, silver-coated copper powder or silver-coated glass powder, the pretreatment method comprises the steps of soaking the conductive powder in an inorganic solvent, filtering and drying.
8. A ceramic matrix obtained by sequentially granulating, injection molding, degreasing and sintering the ceramic slurry according to any one of claims 1 to 5.
9. The ceramic substrate of claim 7, wherein the degreasing means comprises: preserving heat for 2-4 hours in a reducing atmosphere at 400-650 ℃; the sintering mode comprises the following steps: preserving the temperature for 1.5 to 3 hours in the reducing atmosphere at the temperature of 1100 to 1300 ℃.
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