CN115974579A - Ceramic powder, preparation method thereof and porous ceramic matrix - Google Patents
Ceramic powder, preparation method thereof and porous ceramic matrix Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 210
- 239000000843 powder Substances 0.000 title claims abstract description 170
- 239000011159 matrix material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 53
- 238000005245 sintering Methods 0.000 claims abstract description 39
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000203 mixture Substances 0.000 claims abstract description 31
- 238000005303 weighing Methods 0.000 claims abstract description 23
- 239000011787 zinc oxide Substances 0.000 claims abstract description 19
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005469 granulation Methods 0.000 claims abstract description 16
- 230000003179 granulation Effects 0.000 claims abstract description 16
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011230 binding agent Substances 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 239000002270 dispersing agent Substances 0.000 claims abstract description 15
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 238000005238 degreasing Methods 0.000 claims abstract description 12
- 239000007921 spray Substances 0.000 claims abstract description 8
- 238000003825 pressing Methods 0.000 claims abstract description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000498 ball milling Methods 0.000 claims description 31
- 238000001035 drying Methods 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 20
- 239000000126 substance Substances 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 9
- 239000004005 microsphere Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 4
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 4
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 239000004793 Polystyrene Substances 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 238000000889 atomisation Methods 0.000 claims description 3
- 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 description 3
- 229920002223 polystyrene Polymers 0.000 claims description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 16
- 239000011148 porous material Substances 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 15
- 230000009471 action Effects 0.000 description 10
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 8
- 238000009826 distribution Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 239000000443 aerosol Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000000713 high-energy ball milling Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 3
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
Classifications
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- 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
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Abstract
The invention discloses ceramic powder, a preparation method thereof and a porous ceramic matrix, wherein the preparation method comprises the steps of weighing 70-90 parts by weight of aluminum oxide, 5-20 parts by weight of zinc oxide whisker, 2-7 parts by weight of magnesium oxide and 1-3 parts by weight of rare earth oxide, and mixing to prepare a mixture; adding a sintering aid, a pore-forming agent, a binder, a dispersant and a solvent into the mixture to prepare ceramic slurry; and carrying out spray granulation on the ceramic slurry to obtain ceramic powder. The ceramic powder is prepared by the method. The porous ceramic matrix is prepared from the ceramic powder through particle size grading, dry pressing and degreasing sintering. The invention improves the pressure resistance of the alumina porous ceramic matrix, improves the aperture uniformity and reduces the degreasing sintering temperature.
Description
Technical Field
The invention relates to the field of ceramics and preparation processes thereof, in particular to a porous ceramic matrix, ceramic powder for preparing the porous ceramic matrix and a preparation method of the ceramic powder.
Background
The ceramic atomizing core is an important component of the electronic atomizer, the aerosol generating substrate is conducted by virtue of the capillary action of the porous ceramic substrate during atomization, and the aerosol generating substrate is heated and atomized by heat generated by the heating body when passing through the heating body on the porous ceramic substrate to form aerosol. The alumina porous ceramic matrix is a porous ceramic matrix commonly used for ceramic atomizing cores.
The existing alumina porous ceramic matrix has low compressive strength and pore diameter uniformity, and high degreasing and sintering temperatures, and needs to be improved.
Disclosure of Invention
The invention aims to provide a ceramic powder, a preparation method thereof and a porous ceramic matrix, so that the compressive strength of the alumina porous ceramic matrix is improved, the pore diameter uniformity is improved, and the degreasing sintering temperature is reduced.
The invention provides a preparation method of ceramic powder, which comprises the following steps:
weighing 70-90 parts by weight of alumina, 5-20 parts by weight of zinc oxide whisker, 2-7 parts by weight of magnesium oxide and 1-3 parts by weight of rare earth oxide, and mixing to prepare a mixture;
adding a sintering aid, a pore-forming agent, a binder, a dispersant and a solvent into the mixture to prepare ceramic slurry;
and carrying out spray granulation on the ceramic slurry to obtain ceramic powder.
Preferably, the step of weighing 70-90 parts by weight of alumina, 5-20 parts by weight of zinc oxide whisker, 2-7 parts by weight of magnesium oxide and 1-3 parts by weight of rare earth oxide, mixing and preparing the mixture comprises the following steps:
mixing aluminum oxide, zinc oxide whiskers, magnesium oxide and rare earth oxide, performing wet ball milling, drying and calcining to obtain the mixture.
The zinc oxide whisker is preferably in a four-pin shape, and the rare earth oxide is preferably at least one of the group consisting of lanthanum oxide and yttrium oxide.
Preferably, the step of weighing 70-90 parts by weight of alumina, 5-20 parts by weight of zinc oxide whisker, 2-7 parts by weight of magnesium oxide and 1-3 parts by weight of rare earth oxide, mixing to prepare a mixture, wherein,
the rotation speed of ball milling is 260-340r/min, and the ball milling time is 10-20h;
the calcining temperature is 600-800 ℃, and the calcining time is 3-6h.
Preferably, the step of adding a sintering aid, a pore-forming agent, a binder, a dispersant and a solvent to the mixture to prepare the ceramic slurry comprises:
and weighing the mixture, the sintering aid, the pore-forming agent, the binder, the dispersant and the solvent according to the proportion, adding the mixture, the sintering aid, the pore-forming agent, the binder, the dispersant and the solvent into a ball milling container, adjusting the pH of slurry to 6-7, and performing wet ball milling to obtain the ceramic slurry.
Preferably, the step of adding a sintering aid, a pore-forming agent, a binder, a dispersant and a solvent to the mixture to prepare ceramic slurry, wherein,
the sintering aid is at least one substance in a substance group consisting of talcum powder and kaolin, and the content of the sintering aid is 1-5 parts (by weight);
the pore-forming agent is at least one substance in a substance group consisting of activated carbon microspheres, polystyrene microspheres and methyl methacrylate microspheres, and the content of the pore-forming agent is 5-20 parts (by weight);
the binder is at least one substance in the substance group consisting of polyvinyl alcohol and polyethylene glycol, and the content of the binder is 2-7 parts by weight;
the dispersant is at least one substance in the substance group consisting of sodium hexametaphosphate, sodium metasilicate and sodium tripolyphosphate, and the content of the dispersant is 0.1 to 3 parts by weight;
the content of the mixture is 10-30 parts by weight;
the content of the solvent is 40-75 parts by weight.
Preferably, the step of spray granulating the ceramic slurry to obtain the ceramic powder comprises:
and (3) feeding the ceramic slurry into a centrifugal atomizer at the speed of 40-80g/min, feeding liquid drops formed after atomization into a drying chamber, spraying dried powder through a granulation nozzle, and sieving to obtain ceramic powder.
Preferably, the step of spray granulating the ceramic slurry to obtain ceramic powder, wherein,
the rotation speed of the centrifugal atomizer is 3000-10000r/min, the temperature of the drying chamber is 230-300 ℃, and the outlet temperature of the granulating nozzle is 90-130 ℃.
The ceramic powder provided by the invention is prepared by any one of the preparation methods of the ceramic powder.
The porous ceramic matrix provided by the invention is prepared from the ceramic powder through grain size distribution, dry pressing and degreasing sintering.
Preferably, the particle size grading comprises:
mixing 5-12 parts by weight of the ceramic powder with the grain diameter of 70-110 μm, 40-70 parts by weight of the ceramic powder with the grain diameter of 25-60 μm and 15-40 parts by weight of the ceramic powder with the grain diameter of less than 20 μm;
the sintering temperature of the degreasing sintering is 1100-1250 ℃.
Compared with the prior art, the invention has at least the following beneficial effects:
the preparation method of the ceramic powder optimizes the mechanical property and shows the appearance of the ceramic powder by adding materials such as zinc oxide whisker, magnesium oxide, rare earth oxide and the like into aluminum oxideThe microstructure is prepared by preparing spherical secondary particles with regular shapes by a spray granulation process, and experiments show that the repose angle of the prepared ceramic powder reaches 21-23 degrees and the apparent density reaches 0.93-1.09g/cm 3 。
The porous ceramic matrix is prepared from the ceramic powder prepared by the method through particle size grading, dry pressing and degreasing sintering, and has the characteristics of simple preparation method and contribution to industrial production. And the particle size distribution further ensures that the pore diameter range of the porous ceramic matrix is narrow and the pore diameter uniformity is improved. Experiments show that in 80% of the area, the difference value between the maximum aperture and the minimum aperture is between 30 and 40, the aperture sizes are concentrated, the porosity of the porous ceramic matrix is between 50 and 60 percent, and the bending strength of the porous ceramic matrix is between 9 and 15 MPa; the introduction of the zinc oxide whiskers improves the compressive strength of the porous ceramic matrix, the introduction of the magnesium oxide is beneficial to the formation of a uniform pore structure, and the introduction of the rare earth oxide reduces the sintering temperature.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
step 1, preparing ceramic powder
The concrete steps for preparing the ceramic powder are as follows:
step 1.1, weighing 70 parts of alumina, 20 parts of zinc oxide whiskers, 7 parts of magnesium oxide and 3 parts of lanthanum oxide by weight. And putting the weighed powder into a ball milling tank for high-energy ball milling, wherein the ball milling media are tungsten carbide balls and absolute ethyl alcohol, the rotating speed is 300r/min, and the ball milling time is 12h. Drying the powder subjected to ball milling, calcining for 4 hours at 600 ℃ to obtain a mixture, and collecting the mixture for later use;
step 1.2, weighing 20 parts by weight of the mixture prepared in the step 1.1, 3 parts by weight of talcum powder, 2 parts by weight of kaolin, 10 parts by weight of activated carbon microspheres and 60 parts by weight of deionized water, adding 1 part by weight of sodium hexametaphosphate after ball milling for half an hour, and weighing 4 parts by weight of polyvinyl alcohol after continuing ball milling for 1 hour. Adjusting the pH value of the slurry to 6-7 by using dilute hydrochloric acid, and continuing ball milling for 16h to obtain stably dispersed ceramic slurry;
step 1.3, feeding the ceramic slurry prepared in the step 1.2 into a centrifugal atomizer rotating at a high speed at a speed of 65g/min through a slurry pump, wherein the rotation speed of the atomizer is 5000r/min, the slurry is atomized into liquid drops under the action of centrifugal force, the liquid drops are contacted with hot air in a drying chamber, moisture is rapidly evaporated, the temperature in the drying chamber is 260 ℃, dried powder is sprayed out through a granulation nozzle, the outlet temperature is 105 ℃, ceramic powder with a regular shape is obtained, the ceramic powder is sieved by a 150-mesh sieve, undersize powder is taken out, sieved by a 300-mesh sieve, and oversize powder is taken out, so that ceramic powder A is obtained, and the performance of the powder A is shown in table 1;
step 1.4, sending the ceramic slurry prepared in the step 1.2 into a centrifugal atomizer rotating at a high speed at a speed of 55g/min through a slurry pump, wherein the rotating speed of the atomizer is 7000r/min, the slurry is atomized into liquid drops under the action of centrifugal force, the liquid drops are contacted with hot air in a drying chamber, moisture is rapidly evaporated, the temperature of the drying chamber is 265 ℃, dried powder is sprayed out through a granulation nozzle, the outlet temperature is 110 ℃, and ceramic powder with a regular shape is obtained, the ceramic powder is sieved through a 300-mesh sieve, undersize powder is taken, sieved through a 600-mesh sieve, and oversize powder is taken, so that ceramic powder B is obtained, and the performance of the powder B is shown in table 1;
step 1.5, sending the ceramic slurry prepared in the step 1.2 into a centrifugal atomizer rotating at a high speed at a speed of 50g/min through a slurry pump, wherein the rotating speed of the atomizer is 8000r/min, the slurry is atomized into liquid drops under the action of centrifugal force, the liquid drops are contacted with hot air in a drying chamber, moisture is rapidly evaporated, the temperature of the drying chamber is 280 ℃, dried powder is sprayed out through a granulation nozzle, the outlet temperature is 100 ℃, ceramic powder with a regular shape is obtained, the ceramic powder is sieved by a 800-mesh sieve, and undersize powder is taken out, so that ceramic powder C is obtained, and the performance of the powder C is shown in table 1;
step 2, preparing a porous ceramic matrix
The specific steps for preparing the porous ceramic matrix are as follows:
step 2.1, weighing 10 parts of ceramic powder A,60 parts of ceramic powder B and 30 parts of ceramic powder C by weight, and mixing in a mixer for 2 hours;
and 2.2, carrying out dry pressing molding on the ceramic powder mixed in the step 2.1, and carrying out a degreasing sintering process to obtain the porous ceramic matrix.
And (3) testing the performance of the prepared ceramic powder A and the ceramic powder B and the ceramic powder C:
specifically, the particle size of the ceramic powder was measured using a laser particle size analyzer, the angle of repose of the ceramic powder was measured using an angle of repose measuring instrument, the bulk density of the ceramic powder was measured using a general bulk density measuring instrument, and the properties of the ceramic powder in example 1 were measured by the above-described measuring methods, and the results of the obtained performance parameters are shown in table 1.
TABLE 1 ceramic powder Property parameter Table
| D50/(μm) | Angle of repose/(°) | Apparent density/(g/cm 3) | |
| Ceramic powder A | 83 | 22 | 0.93 |
| Ceramic powder B | 46 | 23 | 0.98 |
| Ceramic powder C | 14 | 23 | 1.03 |
Example 2:
step 1, preparing ceramic powder
The specific steps for preparing the ceramic powder are as follows:
step 1.1, weighing 85 parts of aluminum oxide, 10 parts of zinc oxide whiskers, 3 parts of magnesium oxide, 1 part of lanthanum oxide and 1 part of yttrium oxide by weight. And putting the weighed powder into a ball milling tank for high-energy ball milling, wherein the ball milling media are tungsten carbide balls and absolute ethyl alcohol, the rotating speed is 320r/min, and the ball milling time is 10 hours. Drying the powder subjected to ball milling, calcining for 5 hours at 700 ℃ to obtain a mixture, and collecting the mixture for later use;
step 1.2, weighing 13 parts by weight of the mixture prepared in the step 1.1, 2 parts by weight of talcum powder, 6 parts by weight of polystyrene microspheres and 75 parts by weight of deionized water, ball-milling for half an hour, then weighing 0.5 part by weight of sodium tripolyphosphate, adding the sodium tripolyphosphate, and continuing ball-milling for 1 hour, and then weighing 3.5 parts by weight of polyethylene glycol, adding the polyethylene glycol. Adjusting the pH value of the slurry to 6-7 by using dilute hydrochloric acid, and continuing ball milling for 20 hours to obtain stably dispersed ceramic slurry;
step 1.3, feeding the ceramic slurry prepared in the step 1.2 into a centrifugal atomizer rotating at a high speed at a speed of 70g/min through a slurry pump, wherein the rotation speed of the atomizer is 5000r/min, the slurry is atomized into liquid drops under the action of centrifugal force, the liquid drops are contacted with hot air in a drying chamber, moisture is rapidly evaporated, the temperature in the drying chamber is 280 ℃, dried powder is sprayed out through a granulation nozzle, the outlet temperature is 100 ℃, ceramic powder with a regular shape is obtained, the ceramic powder is sieved by a 150-mesh sieve, undersize powder is taken out, the undersize powder is sieved by a 300-mesh sieve, and oversize powder is taken out, so that ceramic powder D is obtained, and the performance of the powder D is shown in table 2;
step 1.4, feeding the ceramic slurry prepared in the step 1.2 into a centrifugal atomizer rotating at a high speed at a speed of 60g/min through a slurry pump, wherein the rotating speed of the atomizer is 7500r/min, the slurry is atomized into liquid drops under the action of centrifugal force, the liquid drops are contacted with hot air in a drying chamber, moisture is rapidly evaporated, the temperature in the drying chamber is 250 ℃, dried powder is sprayed out through a granulation nozzle, the outlet temperature is 110 ℃, and ceramic powder with a regular shape is obtained, the ceramic powder is sieved through a 300-mesh sieve, undersize powder is taken, sieved through a 600-mesh sieve, and oversize powder is taken, so that ceramic powder E is obtained, and the performance of the powder E is shown in table 2;
step 1.5, feeding the ceramic slurry prepared in the step 1.2 into a centrifugal atomizer rotating at a high speed at a speed of 50g/min through a slurry pump, wherein the rotation speed of the atomizer is 10000r/min, the slurry is atomized into liquid drops under the action of centrifugal force, the liquid drops are contacted with hot air in a drying chamber, moisture is rapidly evaporated, the temperature in the drying chamber is 290 ℃, dried powder is sprayed out through a granulation nozzle, the outlet temperature is 110 ℃, and ceramic powder with a regular shape is obtained, the ceramic powder is sieved through a 800-mesh sieve, and undersize powder is taken out to obtain ceramic powder F, and the performance of the ceramic powder F is shown in table 2;
step 2, preparing a porous ceramic matrix
The specific steps for preparing the porous ceramic matrix are as follows:
step 2.1, weighing 8.6 parts by weight of ceramic powder D,67.5 parts by weight of ceramic powder E and 22.9 parts by weight of ceramic powder F, and putting the materials into a mixer to mix for 2 hours;
and 2.2, carrying out dry pressing molding on the ceramic powder mixed in the step 2.1, and carrying out a degreasing sintering process to obtain the porous ceramic matrix.
Testing the performance of the prepared ceramic powder D and the ceramic powder E and the ceramic powder F:
specifically, the particle size of the powder was measured using a laser particle size analyzer, the angle of repose of the powder was measured using an angle of repose measuring instrument, the apparent density of the powder was measured using a general apparent density measuring instrument, and the properties of the ceramic powder in example 2 were measured by the above measurement methods, with the results of the obtained performance parameters shown in table 2.
TABLE 2 ceramic powder Property parameter Table
| D50/(μm) | Angle of repose/(°) | Apparent density/(g/cm 3) | |
| Ceramic powder D | 77 | 21 | 0.95 |
| Ceramic powder E | 43 | 22 | 0.97 |
| Ceramic powder F | 18 | 21 | 1.01 |
Example 3:
step 1, preparing ceramic powder
The concrete steps for preparing the ceramic powder are as follows:
step 1.1, weighing 80 parts of alumina, 10 parts of zinc oxide whiskers, 7 parts of magnesium oxide, 2 parts of lanthanum oxide and 1 part of yttrium oxide by weight. And putting the weighed powder into a ball milling tank for high-energy ball milling, wherein the ball milling media are tungsten carbide balls and absolute ethyl alcohol, the rotating speed is 260r/min, and the ball milling time is 8h. Drying the powder subjected to ball milling, calcining for 3 hours at 650 ℃ to obtain a mixture, and collecting the mixture for later use;
step 1.2, weighing 22 parts by weight of the mixture prepared in the step 1.1, 5 parts by weight of talcum powder, 15 parts by weight of activated carbon microspheres and 50 parts by weight of deionized water, after ball milling for half an hour, weighing 1 part by weight of sodium hexametaphosphate, and after continuing ball milling for 1 hour, weighing 7 parts by weight of polyvinyl alcohol, and adding the polyvinyl alcohol. Adjusting the pH value of the slurry to 6-7 by using dilute hydrochloric acid, and continuing ball milling for 24 hours to obtain stably dispersed ceramic slurry;
step 1.3, feeding the ceramic slurry prepared in the step 1.2 into a centrifugal atomizer rotating at a high speed at a speed of 68G/min through a slurry pump, wherein the rotation speed of the atomizer is 5500r/min, the slurry is atomized into liquid drops under the action of centrifugal force, the liquid drops are contacted with hot air in a drying chamber, water is evaporated rapidly, the temperature in the drying chamber is 270 ℃, dried powder is sprayed out through a granulation nozzle, the outlet temperature is 120 ℃, ceramic powder with a regular shape is obtained, the ceramic powder is sieved by a 150-mesh sieve, undersize powder is taken, sieved by a 300-mesh sieve, and oversize powder is taken, so that ceramic powder G is obtained, and the performance of the powder G is shown in table 3;
step 1.4, feeding the ceramic slurry prepared in the step 1.2 into a centrifugal atomizer rotating at a high speed at a speed of 60g/min through a slurry pump, wherein the rotating speed of the atomizer is 6500r/min, the slurry is atomized into liquid drops under the action of centrifugal force, the liquid drops are contacted with hot air in a drying chamber, moisture is rapidly evaporated, the temperature in the drying chamber is 275 ℃, dried powder is sprayed out through a granulation nozzle, the outlet temperature is 115 ℃, and ceramic powder with a regular shape is obtained, the ceramic powder is sieved through a 300-mesh sieve, undersize powder is taken out, sieved through a 600-mesh sieve, and oversize powder is taken out, so that ceramic powder H is obtained, and the performance of the powder H is shown in Table 3;
step 1.5, feeding the ceramic slurry prepared in the step 1.2 into a centrifugal atomizer rotating at a high speed at a speed of 45g/min through a slurry pump, wherein the rotating speed of the atomizer is 9000r/min, the slurry is atomized into liquid drops under the action of centrifugal force, the liquid drops are contacted with hot air in a drying chamber, moisture is rapidly evaporated, the temperature in the drying chamber is 280 ℃, dried powder is sprayed out through a granulation nozzle, the outlet temperature is 110 ℃, ceramic powder with a regular shape is obtained, the ceramic powder is sieved through a 800-mesh sieve, and undersize powder is taken, so that ceramic powder I is obtained, and the performance of the powder I is shown in table 3;
step 2, preparing a porous ceramic matrix
The specific steps for preparing the porous ceramic matrix are as follows:
step 2.1, weighing 5.8 parts by weight of ceramic powder F,55.6 parts by weight of ceramic powder G and 38.6 parts by weight of ceramic powder I, and mixing in a mixer for 2 hours;
and 2.2, carrying out dry pressing molding on the ceramic powder mixed in the step 2.1, and obtaining the porous ceramic matrix through a degreasing sintering process.
Testing the performance of the ceramic powder G and the ceramic powder H:
specifically, the particle size of the ceramic powder was measured using a laser particle size analyzer, the angle of repose of the ceramic powder was measured using an angle of repose measuring instrument, the bulk density of the ceramic powder was measured using a general bulk density measuring instrument, and the properties of the ceramic powder in example 3 were measured by the above-described measuring methods, and the results of the obtained performance parameters are shown in table 3.
TABLE 3 ceramic powder Property parameter Table
| D50/(μm) | Angle of repose/(°) | Apparent density/(g/cm 3) | |
| Ceramic powder G | 72 | 23 | 0.95 |
| Ceramic powder H | 49 | 22 | 0.99 |
| Ceramic powder I | 11 | 23 | 1.04 |
Comparative examples 1 to 9 were set according to example 1, and the differences between comparative examples 1 to 9 and example 1 are shown in table 4.
TABLE 4 Table for differences between comparative examples and example 1
The porous ceramic substrates prepared in examples 1 to 3 and comparative examples 1 to 9 were subjected to the following property tests:
in examples 1 to 3 and comparative examples 1 to 9, the sintering was carried out in a muffle furnace in step 2.2, the sintering temperature is shown in table 5, and the porous ceramics obtained after sintering were tested according to the following test items: the porosity of the porous ceramic matrix was measured using a porosity tester, the bending strength of the porous ceramic matrix was measured using an electronic universal tester, and the pore diameter of the porous ceramic matrix was measured using a pore diameter analyzer, the test results being shown in table 5.
TABLE 5 Performance Table of porous ceramics prepared in examples and comparative examples
From examples 1 to 3, it can be seen that the porous ceramic substrates with different pore diameters are obtained by adjusting the conditions of the spray granulation process and then obtaining the ceramic powders with different particle sizes through the particle size distribution of the ceramic powders, thereby achieving the purpose of controlling the pore structure.
As can be seen from Table 5, the porous ceramic substrates prepared in examples 1 to 3 had sintering temperatures of 1150 ℃ to 1200 ℃ and average pore diameters determined by the grain size distribution of the ceramic powders, and had normally distributed pore diameters, a difference between the maximum pore diameter and the minimum pore diameter of 80% of the area was 30 to 40, relatively concentrated pore diameters, a porosity of 50% to 60% of the porous ceramic substrates, and a flexural strength of 9 to 15MPa of the porous ceramic substrates.
In the comparative example 1, the zinc oxide whisker is replaced by spherical zinc oxide, particles are simply stacked, the improvement on the compressive strength of the porous ceramic matrix is limited, and the pore diameter is slightly reduced and the compressive strength is obviously reduced in a performance test. In comparative example 2, no zinc oxide whisker was added, resulting in a further decrease in the compressive strength of the ceramic and a slight increase in the sintering temperature. Analysis suggests that, because the zinc oxide whiskers adhere to the alumina substrate, the engagement between the crystal grains is enhanced, and the compressive strength is improved.
In comparative example 3, no magnesium oxide was added, the grains grew irregularly, the sintering temperature of the porous ceramic matrix was slightly increased, the pore diameter range reached 65, the pore diameter concentration was small, and the compressive strength was slightly decreased. Analysis shows that magnesia and alumina form magnesia-alumina spinel in the crystal boundary to inhibit the irregular growth of crystal grains and to form homogeneous pore structure.
In comparative example 4, no rare earth oxide was added, and in order to achieve the best sintering state, the sintering temperature was greatly increased and the energy consumption was increased. Analysis shows that the rare earth oxide can reduce sintering temperature and refine crystal grains.
In comparative example 5, the porous ceramic matrix was prepared only from the ceramic powder a without performing the grain size distribution of the ceramic powder, and the pore size of the porous ceramic matrix was significantly increased, the shrinkage of the ceramic was irregular, and the compressive strength was significantly reduced. In comparative example 6, the porous ceramic base was prepared by using only the ceramic powder B without performing the particle size distribution of the ceramic powder, and the pore diameter and compressive strength of the porous ceramic base were reduced. In comparative example 7, the porous ceramic base was prepared only from the ceramic powder C without performing the grain size distribution of the ceramic powder, and the pore size of the porous ceramic base was greatly reduced with less reduction in porosity and compressive strength.
In comparative example 8, the particle size ratio of the ceramic powder was changed, the ratio of the large particle size powder was increased, the pore size of the porous ceramic matrix was increased, and the compressive strength was reduced. In the comparative example 9, the grain size ratio of the ceramic powder is changed, the proportion of the small-grain-size powder is increased, the pore diameter of the porous ceramic matrix is reduced, the porosity is reduced, and the compressive strength is reduced.
The present invention has been described in detail with reference to the specific embodiments, and the detailed description is only for the purpose of helping those skilled in the art understand the present invention, and is not to be construed as limiting the scope of the present invention. Various modifications, equivalent changes, etc. made by those skilled in the art under the spirit of the present invention shall be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the ceramic powder is characterized by comprising the following steps:
weighing 70-90 parts by weight of alumina, 5-20 parts by weight of zinc oxide whisker, 2-7 parts by weight of magnesium oxide and 1-3 parts by weight of rare earth oxide, and mixing to prepare a mixture;
adding a sintering aid, a pore-forming agent, a binder, a dispersant and a solvent into the mixture to prepare ceramic slurry;
and carrying out spray granulation on the ceramic slurry to obtain ceramic powder.
2. The method for preparing ceramic powder according to claim 1, wherein the step of weighing 70-90 parts by weight of alumina, 5-20 parts by weight of zinc oxide whisker, 2-7 parts by weight of magnesium oxide and 1-3 parts by weight of rare earth oxide, mixing to prepare a mixture comprises
Mixing aluminum oxide, zinc oxide whiskers, magnesium oxide and rare earth oxide, performing wet ball milling, drying and calcining to obtain the mixture.
3. The method for preparing ceramic powder according to claim 2, wherein the step of weighing 70-90 parts by weight of alumina, 5-20 parts by weight of zinc oxide whisker, 2-7 parts by weight of magnesium oxide and 1-3 parts by weight of rare earth oxide, mixing to prepare a mixture, wherein,
the rotation speed of ball milling is 260-340r/min, and the ball milling time is 10-20h;
the calcining temperature is 600-800 ℃, and the calcining time is 3-6h.
4. The method for preparing ceramic powder according to claim 1, wherein the step of adding a sintering aid, a pore-forming agent, a binder, a dispersant and a solvent to the mixture to prepare a ceramic slurry comprises
And weighing the mixture, the sintering aid, the pore-forming agent, the binder, the dispersant and the solvent according to the proportion, adding the mixture, the sintering aid, the pore-forming agent, the binder, the dispersant and the solvent into a ball milling container, adjusting the pH of slurry to 6-7, and performing wet ball milling to obtain the ceramic slurry.
5. The method according to claim 4, wherein a sintering aid, a pore-forming agent, a binder, a dispersant and a solvent are added to the mixture to prepare a ceramic slurry, wherein,
the sintering aid is at least one substance in a substance group consisting of talcum powder and kaolin, and the content of the sintering aid is 1-5 parts (by weight);
the pore-forming agent is at least one substance in a substance group consisting of activated carbon microspheres, polystyrene microspheres and methyl methacrylate microspheres, and the content of the pore-forming agent is 5-20 parts (by weight);
the binder is at least one substance in the substance group consisting of polyvinyl alcohol and polyethylene glycol, and the content of the binder is 2-7 parts by weight;
the dispersant is at least one substance in the substance group consisting of sodium hexametaphosphate, sodium metasilicate and sodium tripolyphosphate, and the content of the dispersant is 0.1 to 3 parts by weight;
the content of the mixture is 10-30 parts by weight;
the content of the solvent is 40-75 parts by weight.
6. The method according to claim 1, wherein the step of spray granulating the ceramic slurry to obtain the ceramic powder comprises
And (3) feeding the ceramic slurry into a centrifugal atomizer at the speed of 40-80g/min, feeding liquid drops formed after atomization into a drying chamber, spraying dried powder through a granulation nozzle, and sieving to obtain ceramic powder.
7. The method according to claim 6, wherein the step of spray-granulating the ceramic slurry to obtain a ceramic powder comprises,
the rotation speed of the centrifugal atomizer is 3000-10000r/min, the temperature of the drying chamber is 230-300 ℃, and the outlet temperature of the granulating nozzle is 90-130 ℃.
8. A ceramic powder produced by the method for producing a ceramic powder according to any one of claims 1 to 7.
9. A porous ceramic substrate obtained from the ceramic powder according to claim 8 by size grading, dry pressing, degreasing and sintering.
10. Porous ceramic matrix according to claim 9,
the grain size grading comprises:
mixing 5-12 parts by weight of the ceramic powder with the grain diameter of 70-110 μm, 40-70 parts by weight of the ceramic powder with the grain diameter of 25-60 μm and 15-40 parts by weight of the ceramic powder with the grain diameter of less than 20 μm;
the sintering temperature of the degreasing sintering is 1100-1250 ℃.
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