CN116283345A - Porous ceramic atomizing core and preparation method thereof - Google Patents
Porous ceramic atomizing core and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 169
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 100
- 238000010438 heat treatment Methods 0.000 claims abstract description 89
- 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 39
- 238000005245 sintering Methods 0.000 claims abstract description 38
- 239000002002 slurry Substances 0.000 claims abstract description 36
- 239000002994 raw material Substances 0.000 claims abstract description 30
- 238000004512 die casting Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000000465 moulding Methods 0.000 claims abstract description 17
- 239000004094 surface-active agent Substances 0.000 claims abstract description 17
- 239000011230 binding agent Substances 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000012298 atmosphere Substances 0.000 claims abstract description 13
- 238000005238 degreasing Methods 0.000 claims abstract description 13
- 238000000889 atomisation Methods 0.000 claims abstract description 12
- 238000004537 pulping Methods 0.000 claims abstract description 9
- 238000007873 sieving Methods 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 47
- 238000000034 method Methods 0.000 claims description 27
- 239000000377 silicon dioxide Substances 0.000 claims description 20
- 239000011148 porous material Substances 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 10
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000006004 Quartz sand Substances 0.000 claims description 6
- 235000013871 bee wax Nutrition 0.000 claims description 6
- 239000012166 beeswax Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000012188 paraffin wax Substances 0.000 claims description 6
- 239000001993 wax Substances 0.000 claims description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
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- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims description 2
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
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- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 235000021313 oleic acid Nutrition 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 238000005299 abrasion Methods 0.000 abstract description 4
- 238000005266 casting Methods 0.000 abstract description 3
- 239000003571 electronic cigarette Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 2
- WGACMNAUEGCUHG-VYBOCCTBSA-N (2s)-2-[[(2s)-2-[[(2s)-2-acetamidopropanoyl]amino]propanoyl]amino]-n-[(2s)-6-amino-1-[[(2s)-1-[(2s)-2-[[(2s)-1-[[(2s)-5-amino-1-[[(2s)-1-[[(2s)-1-[[(2s)-6-amino-1-[[(2s)-1-amino-3-(4-hydroxyphenyl)-1-oxopropan-2-yl]amino]-1-oxohexan-2-yl]amino]-3-hydroxy- Chemical compound CC(=O)N[C@@H](C)C(=O)N[C@@H](C)C(=O)N[C@@H](CCC(N)=O)C(=O)N[C@@H](CCCCN)C(=O)N[C@@H](CCCN=C(N)N)C(=O)N1CCC[C@H]1C(=O)N[C@@H](CO)C(=O)N[C@@H](CCC(N)=O)C(=O)N[C@@H](CCCN=C(N)N)C(=O)N[C@@H](CO)C(=O)N[C@@H](CCCCN)C(=O)N[C@H](C(N)=O)CC1=CC=C(O)C=C1 WGACMNAUEGCUHG-VYBOCCTBSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
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- 239000010433 feldspar Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
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- 108010074544 myelin peptide amide-12 Proteins 0.000 description 1
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- UFMBFIIJKCBBHN-MEKJRKEKSA-N myelin peptide amide-16 Chemical compound C([C@@H](C(=O)N[C@@H](CC(C)C)C(=O)N[C@@H](C)C(=O)N[C@@H](CO)C(=O)N[C@@H](C)C(N)=O)NC(=O)[C@H](CCCCN)NC(=O)[C@H](CO)NC(=O)[C@H](CCCNC(N)=N)NC(=O)[C@H](CCC(N)=O)NC(=O)[C@H](CO)NC(=O)[C@H]1N(CCC1)C(=O)[C@H](CCCNC(N)=N)NC(=O)[C@H](CCCCN)NC(=O)[C@H](CCC(N)=O)NC(=O)[C@H](C)NC(=O)[C@H](C)NC(C)=O)C1=CC=C(O)C=C1 UFMBFIIJKCBBHN-MEKJRKEKSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/068—Carbonaceous materials, e.g. coal, carbon, graphite, hydrocarbons
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/638—Removal thereof
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/64—Burning or sintering processes
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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Abstract
The invention relates to the technical field of atomization, and discloses a preparation method of a porous ceramic atomization core, which comprises the following steps: (1) material preparation: mixing and ball milling ceramic aggregate, grinding aid, sintering aid and pore-forming agent, and sieving to obtain raw material powder; drying the raw material powder; (2) proportioning and pulping: mixing, heating and stirring raw material powder, a binder and a surfactant to obtain ceramic slurry; (3) hot-press casting forming: performing hot die casting molding on the ceramic slurry to obtain a ceramic green body; (4) wax removal: burying and burning the ceramic green body in alumina powder calcined at high temperature, and degreasing under a set atmosphere; (5) sintering: and (3) carrying out secondary sintering on the degreased ceramic green body in an atmospheric environment according to a preset temperature curve to obtain the porous ceramic atomization core. The invention adopts hot die casting molding, is more suitable for small parts with complex appearance and high precision, uses less complex equipment, has small die abrasion, is convenient to operate, has higher production efficiency, and has adjustable ceramic strength, aperture and porosity.
Description
Technical Field
The invention relates to the technical field of atomization, in particular to a porous ceramic atomization core and a preparation method thereof.
Background
At present, the manufacturing modes of the porous ceramic atomizing core are divided into the following molding modes: injection molding, dry press molding, casting molding, hot die casting molding, and the like. The formula is also divided into a plurality of systems, and the systems are divided into clay raw materials, quartz raw materials, feldspar raw materials and the like according to the different ceramic aggregates; the choice of pore-forming agent and binder is also quite different from ceramic aggregate.
The existing hot-pressing casting forming process is complex, the cost is high, the strength of the prepared porous ceramic atomization core is low, the forming efficiency is low, and the automatic production is not facilitated, so that the industrial large-scale production and application are not facilitated.
Therefore, it is necessary to develop a porous ceramic atomizing core and a preparation method thereof, which adopt hot die casting molding, are more suitable for small-sized parts with complex appearance and high precision, and the used equipment is not complex, the die abrasion is small, the operation is convenient, the production efficiency is higher, and the ceramic strength, the aperture and the porosity are adjustable.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a porous ceramic atomizing core and a preparation method thereof. The invention adopts hot die casting molding, is more suitable for small parts with complex appearance and high precision, uses less complex equipment, has small die abrasion, is convenient to operate, has higher production efficiency, and has adjustable ceramic strength, aperture and porosity. The calcined high-purity oxide is adopted on the raw materials, so that the introduction of impurities can be reduced, and the ceramic performance is controlled more strictly and effectively. The porous ceramic atomizing core can be applied to the fields of electronic cigarettes, medical cosmetology and the like.
The invention adopts the following technical proposal to realize the aim:
a method for preparing a porous ceramic atomizing core, which comprises the following steps:
(1) Preparing materials:
mixing and ball milling ceramic aggregate, grinding aid, sintering aid and pore-forming agent, and sieving to obtain raw material powder; drying the raw material powder to make the water content of the raw material powder less than 0.2%;
(2) Preparing materials and pulping:
mixing, heating and stirring raw material powder, a binder and a surfactant to obtain ceramic slurry; the ceramic slurry comprises the following components in percentage by mass: 30-90% of ceramic aggregate, 0.4-0.8% of grinding aid, 5-15% of sintering aid, 20-35% of pore-forming agent, 18-30% of binder and 0.4-1.2% of surfactant; the ceramic aggregate is high-purity silica powder and high-purity alumina powder which are calcined at high temperature, and the purity is more than or equal to 99.9%; the alumina powder accounts for 10-30% of the total mass of the ceramic slurry, and the silica powder accounts for 20-60% of the total mass of the ceramic slurry;
(3) And (3) hot die casting and forming:
performing hot die casting molding on the ceramic slurry to obtain a ceramic green body;
(4) And (3) wax removal: burying and burning the ceramic green body in alumina powder calcined at high temperature, and degreasing under a set atmosphere;
(5) Sintering: and (3) carrying out secondary sintering on the degreased ceramic green body in an atmospheric environment according to a preset temperature curve to obtain the porous ceramic atomization core.
Preferably, the sieving of step (1) is specifically: the screen residue of the ten-thousand-hole screen is less than 5 percent or the screen passes through a screen with the aperture of 0.2 mm.
Preferably, the drying conditions in step (1) are: drying at 120-200 deg.c for 2-8 hr.
The ceramic aggregate used in the present invention must be clinker, i.e., calcined, material. Preferably, the high-purity silica powder and the high-purity alumina powder are obtained by calcining ceramic aggregate at 1300-1420 ℃ for 2-5 h.
Preferably, the particle size of the silica powder and the alumina powder in the ceramic aggregate is 10-40 μm.
Preferably, the grinding aid is one or a combination of quartz sand, glass powder and acrylic.
Preferably, the sintering aid is low-temperature glass powder or a mixture of high-purity magnesia powder and high-purity calcium oxide powder, the purity is more than or equal to 99.9%, and the mass ratio of the high-purity magnesia powder to the high-purity calcium oxide powder is 2/3-3/2. The sintering aid can reduce sintering temperature and promote densification of ceramic blanks.
Preferably, the pore-forming agent is graphite powder with the particle size of 20-40 mu m.
Preferably, the binder is paraffin wax.
Preferably, the surfactant is beeswax, oleic acid or stearic acid.
Preferably, in the step (2), the specific method of pulping is as follows: the adhesive and the surfactant are uniformly mixed, heated to 60-90 ℃ to be melted, then poured into the raw material powder, and stirred for 2-5 hours while being heated to prepare the ceramic slurry.
Preferably, in the step (3), the grouting temperature is 60-75 ℃ and the pressure is 0.3-0.6 MPa during hot die casting molding, and the pressure is maintained for 1-60 s.
Preferably, in the step (4), the particle size of the high-temperature calcined alumina powder is 20-50 μm, and the burial depth is 1-5 cm; the degreasing atmosphere is set as follows: heating from room temperature to 120 ℃ at a heating rate of 0.5 ℃/min, and preserving heat for 1h; then heating to 300 ℃ at a heating rate of 0.3 ℃/min, and preserving heat for 1h; then heating to 450 ℃ at a heating rate of 0.5 ℃/min, preserving heat for 2 hours, heating to 850 ℃ at a heating rate of 2.5 ℃/min, and preserving heat for 1 hour; then the temperature is increased to 1050 ℃ at the heating rate of 2.5 ℃/min, the heat is preserved for 1h, and finally the furnace is cooled.
Preferably, in step (5), the preset temperature profile is: heating from room temperature to 1050 ℃ at a heating rate of 5 ℃/min, and preserving heat for 1h; then heating to 1400-1450 ℃ at a heating rate of 3 ℃/min, preserving heat for 2h, and finally cooling along with the furnace.
Another object of the present invention is to disclose a porous ceramic atomizing core made by the above method.
Preferably, the pore diameter of the micropores of the porous ceramic atomizing core is 15-25 mu m, the porosity is 45-55%, and the density is 0.8-1.2 g/cm 3 。
The ceramic atomizing core obtained by the method has adjustable strength, aperture and porosity, and the strength, aperture and porosity of the atomizing core can be adjusted from the aspects of a formula and technological parameters (including single weight of a product and sintering temperature). Ceramic properties were adjusted in the formulation: the adjusting direction is the aluminum powder content (namely the aluminum oxide content) in the ceramic aggregate and the addition amount of graphite powder (pore-forming agent).
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts hot die casting molding, is more suitable for small parts with complex appearance and high precision, uses less complex equipment, has small die abrasion, is convenient to operate, has higher production efficiency, and has adjustable ceramic strength, aperture and porosity.
The invention adopts calcined high-purity oxide on the raw material, can reduce the introduction of impurities, and is more strictly and effectively controlled on the ceramic performance.
The porous ceramic atomizing core can be applied to the fields of electronic cigarettes, medical cosmetology and the like.
Detailed Description
The invention is further described below in connection with examples, which are not to be construed as limiting the scope of the invention as claimed.
Adjustment of the addition of high purity alumina powder in ceramic aggregate
Example 1:
a method for preparing a porous ceramic atomizing core, which comprises the following steps:
(1) Preparing materials:
mixing and ball milling ceramic aggregate, grinding aid, sintering aid and pore-forming agent, and sieving (the residue of a ten-thousand-hole sieve is less than 5%) to obtain raw material powder; drying the raw material powder (the drying condition is that the temperature is 120-200 ℃ and the drying time is 2-8 h) to ensure that the water content is less than 0.2 percent.
(2) Preparing materials and pulping:
mixing binder (paraffin) and surfactant (beeswax), heating to 60deg.C to melt, adding raw material powder, heating and stirring for 2 hr to obtain ceramic slurry. The ceramic slurry comprises the following components in percentage by mass: the ceramic aggregate is high-purity silica powder and high-purity alumina powder which are calcined at high temperature, the purity is more than or equal to 99.9%, and the grain diameter is 10-40 mu m; alumina powder accounts for 10% of the total mass of the ceramic slurry, silica powder accounts for 40% of the total mass of the ceramic slurry, grinding aid (quartz sand) 0.6%, sintering aid (low-temperature glass powder) 6%, pore-forming agent (graphite powder with particle size of 20-40 μm) 25%, binder 18% and surfactant 0.4%.
(3) And (3) hot die casting and forming:
performing hot die casting molding on the ceramic slurry (the grouting temperature is 60-75 ℃, the pressure is 0.3-0.6 MPa, and the pressure is maintained for 1-60 s) to obtain a ceramic green body (the single weight of the ceramic green body is 0.16 g);
(4) And (3) wax removal: burying and burning the ceramic green body in alumina powder calcined at high temperature, and degreasing under a set atmosphere; the grain diameter of the alumina powder calcined at high temperature is 20-50 mu m, and the embedding depth is 1-5 cm; the degreasing atmosphere is set as follows: heating from room temperature to 120 ℃ at a heating rate of 0.5 ℃/min, and preserving heat for 1h; then heating to 300 ℃ at a heating rate of 0.3 ℃/min, and preserving heat for 1h; then heating to 450 ℃ at a heating rate of 0.5 ℃/min, preserving heat for 2 hours, heating to 850 ℃ at a heating rate of 2.5 ℃/min, and preserving heat for 1 hour; then the temperature is increased to 1050 ℃ at the heating rate of 2.5 ℃/min, the heat is preserved for 1h, and finally the furnace is cooled.
(5) Sintering: and (3) carrying out secondary sintering on the degreased ceramic green body in an atmospheric environment according to a preset temperature curve to obtain the porous ceramic atomization core. The preset temperature curve is as follows: heating from room temperature to 1050 ℃ at a heating rate of 5 ℃/min, and preserving heat for 1h; then heating to 1400 ℃ at a heating rate of 3 ℃/min, preserving heat for 2 hours, and finally cooling along with the furnace.
The ceramic aggregate used in the present invention must be clinker, i.e., calcined, material. Preferably, the high purity silica powder and the high purity alumina powder are obtained by calcining ceramic aggregate at 1300 ℃ for 2 hours.
The porous ceramic atomizing cores of examples 2 to 6 were prepared in the same manner as in example 1, but the high-purity alumina powder content in the ceramic aggregate of examples 2 to 6 was 11%, 12%, 13%, 14% and 15% of the total mass of the ceramic slurry, respectively.
The properties of the porous ceramic atomized cores prepared in examples 1 to 6 are shown in Table 1:
table 1 performance tables of porous ceramic atomized cores produced in examples 1 to 6
| Examples | High purity alumina powder content% | Average pore size μm | Porosity% | Strength MPa |
| 1 | 10 | 15 | 46 | 7 |
| 2 | 11 | 15 | 48 | 7 |
| 3 | 12 | 16 | 52 | 7 |
| 4 | 13 | 17 | 52 | 7 |
| 5 | 14 | 17 | 54 | 7 |
| 6 | 15 | 16 | 53 | 7 |
In table 1, pore diameter was measured by a bubble pressure method, porosity was measured by a saturated water treatment by a vacuum pumping method, and compressive strength was measured by compression, as follows.
The control of the content of the high-purity alumina powder in the adjustment method of the present invention has been described above, but is not limited to the above embodiment. From the results of examples 1 to 6, it is apparent that the high-purity alumina powder content can effectively adjust the average pore diameter (porosity) of the porous ceramic, and as the proportion of the high-purity alumina powder content increases, the pore diameter (porosity) increases relatively, but decreases beyond a critical value.
Adjustment of the addition amount of graphite powder
Example 7:
a method for preparing a porous ceramic atomizing core, which comprises the following steps:
(1) Preparing materials:
mixing and ball milling ceramic aggregate, grinding aid, sintering aid and pore-forming agent, and sieving (the residue of a ten-thousand-hole sieve is less than 5%) to obtain raw material powder; drying the raw material powder (the drying condition is that the temperature is 120-200 ℃ and the drying time is 2-8 h) to ensure that the water content is less than 0.2 percent.
(2) Preparing materials and pulping:
mixing binder (paraffin) and surfactant (beeswax), heating to 70deg.C to melt, adding raw material powder, heating and stirring for 5 hr to obtain ceramic slurry. The ceramic slurry comprises the following components in percentage by mass: the ceramic aggregate is high-purity silica powder and high-purity alumina powder which are calcined at high temperature, the purity is more than or equal to 99.9%, and the grain diameter is 10-40 mu m; alumina powder accounts for 10% of the total mass of the ceramic slurry, silica powder accounts for 30% of the total mass of the ceramic slurry, grinding aid (quartz sand) is 0.4%, sintering aid (low-temperature glass powder) is 15%, pore-forming agent (graphite powder with particle size of 20-40 μm) is 20%, binder is 24%, and surfactant is 0.6%.
(3) And (3) hot die casting and forming:
performing hot die casting molding on the ceramic slurry (the grouting temperature is 60-75 ℃, the pressure is 0.3-0.6 MPa, and the pressure is maintained for 1-60 s) to obtain a ceramic green body (the single weight of the ceramic green body is 0.16 g);
(4) And (3) wax removal: burying and burning the ceramic green body in alumina powder calcined at high temperature, and degreasing under a set atmosphere; the grain diameter of the alumina powder calcined at high temperature is 20-50 mu m, and the embedding depth is 1-5 cm; the degreasing atmosphere is set as follows: heating from room temperature to 120 ℃ at a heating rate of 0.5 ℃/min, and preserving heat for 1h; then heating to 300 ℃ at a heating rate of 0.3 ℃/min, and preserving heat for 1h; then heating to 450 ℃ at a heating rate of 0.5 ℃/min, preserving heat for 2 hours, heating to 850 ℃ at a heating rate of 2.5 ℃/min, and preserving heat for 1 hour; then the temperature is increased to 1050 ℃ at the heating rate of 2.5 ℃/min, the heat is preserved for 1h, and finally the furnace is cooled.
(5) Sintering: and (3) carrying out secondary sintering on the degreased ceramic green body in an atmospheric environment according to a preset temperature curve to obtain the porous ceramic atomization core. The preset temperature curve is as follows: heating from room temperature to 1050 ℃ at a heating rate of 5 ℃/min, and preserving heat for 1h; then heating to 1400 ℃ at a heating rate of 3 ℃/min, preserving heat for 2 hours, and finally cooling along with the furnace.
The ceramic aggregate used in the present invention must be clinker, i.e., calcined, material. Preferably, the high purity silica powder and the high purity alumina powder are obtained by calcining ceramic aggregate at 1300 ℃ for 2 hours.
The porous ceramic atomized cores of examples 8 to 11 were prepared in the same manner as in example 7, but the graphite powder contents of examples 8 to 11 were 25%, 28%, 30% and 35% of the total mass of the ceramic slurry, respectively.
The properties of the porous ceramic atomized cores prepared in examples 7 to 11 are shown in Table 2:
table 2 performance tables of porous ceramic atomized cores produced in examples 7 to 11
| Examples | The addition amount of the graphite powder is% | Average pore size μm | Porosity% | Strength MPa |
| 7 | 20 | 13 | 44 | 6.5 |
| 8 | 25 | 18 | 50 | 7 |
| 9 | 28 | 20 | 54 | 6.5 |
| 10 | 30 | 22 | 58 | 6 |
| 11 | 35 | 25 | 58 | 5 |
The control of the amount of graphite powder added in the adjustment method of the present invention has been described above, but is not limited to the above embodiment. When graphite powder is used as a pore-forming agent, the pore diameter and the open porosity of the porous ceramic are correspondingly increased along with the increase of the content of the graphite powder, but the ceramic strength is obviously reduced after the content of the graphite powder exceeds 30 percent.
Single-load adjustment of ceramic green bodies
Example 12
A method for preparing a porous ceramic atomizing core, which comprises the following steps:
(1) Preparing materials:
mixing and ball milling ceramic aggregate, grinding aid, sintering aid and pore-forming agent, and sieving (the residue of a ten-thousand-hole sieve is less than 5%) to obtain raw material powder; drying the raw material powder (the drying condition is that the temperature is 120-200 ℃ and the drying time is 2-8 h) to ensure that the water content is less than 0.2 percent.
(2) Preparing materials and pulping:
mixing binder (paraffin) and surfactant (beeswax), heating to 90deg.C to melt, adding raw material powder, heating and stirring for 4 hr to obtain ceramic slurry. The ceramic slurry comprises the following components in percentage by mass: the ceramic aggregate is high-purity silica powder and high-purity alumina powder which are calcined at high temperature, the purity is more than or equal to 99.9%, and the grain diameter is 10-40 mu m; alumina powder accounts for 10% of the total mass of the ceramic slurry, silica powder accounts for 35% of the total mass of the ceramic slurry, grinding aid (quartz sand) 0.8%, sintering aid (low-temperature glass powder) 5%, pore-forming agent (graphite powder with particle size of 20-40 μm) 30%, binder 18% and surfactant 1.2%.
(3) And (3) hot die casting and forming:
performing hot die casting molding on the ceramic slurry (the grouting temperature is 60-75 ℃, the pressure is 0.3-0.6 MPa, and the pressure is maintained for 1-60 s) to obtain a ceramic green body (the single weight of the ceramic green body is 0.155 g);
(4) And (3) wax removal: burying and burning the ceramic green body in alumina powder calcined at high temperature, and degreasing under a set atmosphere; the grain diameter of the alumina powder calcined at high temperature is 20-50 mu m, and the embedding depth is 1-5 cm; the degreasing atmosphere is set as follows: heating from room temperature to 120 ℃ at a heating rate of 0.5 ℃/min, and preserving heat for 1h; then heating to 300 ℃ at a heating rate of 0.3 ℃/min, and preserving heat for 1h; then heating to 450 ℃ at a heating rate of 0.5 ℃/min, preserving heat for 2 hours, heating to 850 ℃ at a heating rate of 2.5 ℃/min, and preserving heat for 1 hour; then the temperature is increased to 1050 ℃ at the heating rate of 2.5 ℃/min, the heat is preserved for 1h, and finally the furnace is cooled.
(5) Sintering: and (3) carrying out secondary sintering on the degreased ceramic green body in an atmospheric environment according to a preset temperature curve to obtain the porous ceramic atomization core. The preset temperature curve is as follows: heating from room temperature to 1050 ℃ at a heating rate of 5 ℃/min, and preserving heat for 1h; then heating to 1400 ℃ at a heating rate of 3 ℃/min, preserving heat for 2 hours, and finally cooling along with the furnace.
The ceramic aggregate used in the present invention must be clinker, i.e., calcined, material. Preferably, the high purity silica powder and the high purity alumina powder are obtained by calcining ceramic aggregate at 1300 ℃ for 2 hours.
A porous ceramic atomized core of examples 13-15 was prepared in the same manner as in example 12, but the ceramic green bodies of examples 13-15 had a single weight of 0.16g, 0.165g, and 0.17g, respectively.
The properties of the porous ceramic atomized cores prepared in examples 12 to 15 are shown in Table 3:
TABLE 3 Performance Table of porous ceramic atomizing cores prepared in examples 12 to 15
| Examples | Single g of ceramic green body | Average pore size μm | Porosity% | Strength MPa |
| 12 | 0.155 | 19 | 52 | 7 |
| 13 | 0.16 | 18 | 50 | 7 |
| 14 | 0.165 | 18 | 52 | 7 |
| 15 | 0.17 | 16 | 46 | 7 |
In the above, the ceramic performance was adjusted in terms of the process parameter control, and the adjustment method of the present invention has been described with respect to the single control of the ceramic green body, but is not limited to the above embodiment. As can be seen from table 3: the single weight of the ceramic green body can obviously adjust the average pore diameter of the porous ceramic, and the pore diameter is obviously reduced and the open porosity is also reduced along with the increase of the single weight.
Ceramic sintering temperature adjustment
Example 16
A method for preparing a porous ceramic atomizing core, which comprises the following steps:
(1) Preparing materials:
mixing and ball milling ceramic aggregate, grinding aid, sintering aid and pore-forming agent, and sieving (the residue of a ten-thousand-hole sieve is less than 5%) to obtain raw material powder; drying the raw material powder (the drying condition is that the temperature is 120-200 ℃ and the drying time is 2-8 h) to ensure that the water content is less than 0.2 percent.
(2) Preparing materials and pulping:
mixing binder (paraffin) and surfactant (beeswax), heating to 60deg.C to melt, adding raw material powder, heating and stirring for 5 hr to obtain ceramic slurry. The ceramic slurry comprises the following components in percentage by mass: the ceramic aggregate is high-purity silica powder and high-purity alumina powder which are calcined at high temperature, the purity is more than or equal to 99.9%, and the grain diameter is 10-40 mu m; alumina powder accounts for 10% of the total mass of the ceramic slurry, silica powder accounts for 25% of the total mass of the ceramic slurry, grinding aid (quartz sand) 0.6%, sintering aid (low-temperature glass powder) 10%, pore-forming agent (graphite powder with particle size of 20-40 μm) 30%, binder 24% and surfactant 0.4%.
(3) And (3) hot die casting and forming:
performing hot die casting molding on the ceramic slurry (the grouting temperature is 60-75 ℃, the pressure is 0.3-0.6 MPa, and the pressure is maintained for 1-60 s) to obtain a ceramic green body (the single weight of the ceramic green body is 0.16 g);
(4) And (3) wax removal: burying and burning the ceramic green body in alumina powder calcined at high temperature, and degreasing under a set atmosphere; the grain diameter of the alumina powder calcined at high temperature is 20-50 mu m, and the embedding depth is 1-5 cm; the degreasing atmosphere is set as follows: heating from room temperature to 120 ℃ at a heating rate of 0.5 ℃/min, and preserving heat for 1h; then heating to 300 ℃ at a heating rate of 0.3 ℃/min, and preserving heat for 1h; then heating to 450 ℃ at a heating rate of 0.5 ℃/min, preserving heat for 2 hours, heating to 850 ℃ at a heating rate of 2.5 ℃/min, and preserving heat for 1 hour; then the temperature is increased to 1050 ℃ at the heating rate of 2.5 ℃/min, the heat is preserved for 1h, and finally the furnace is cooled.
(5) Sintering: and (3) carrying out secondary sintering on the degreased ceramic green body in an atmospheric environment according to a preset temperature curve to obtain the porous ceramic atomization core. The preset temperature curve is as follows: heating from room temperature to 1050 ℃ at a heating rate of 5 ℃/min, and preserving heat for 1h; then heating to 1400 ℃ at a heating rate of 3 ℃/min, preserving heat for 2 hours, and finally cooling along with the furnace.
The ceramic aggregate used in the present invention must be clinker, i.e., calcined, material. Preferably, the high purity silica powder and the high purity alumina powder are obtained by calcining ceramic aggregate at 1300 ℃ for 2 hours.
A porous ceramic atomized core of examples 17 to 21 was produced in the same manner as in example 16, but the ceramic sintering temperatures of examples 17 to 21 were 1410℃C, 1420℃C, 1430℃C, 1440℃C and 1450℃respectively.
The properties of the porous ceramic atomized cores prepared in examples 17 to 21 are shown in Table 4:
TABLE 4 Performance Table of porous ceramic atomizing cores prepared in examples 17 to 21
| Examples | Ceramic sintering temperature | Average pore size μm | Porosity% | Strength MPa |
| 16 | 1400 | 20 | 55 | 6.5 |
| 17 | 1410 | 19 | 54 | 6.5 |
| 18 | 1420 | 18 | 54 | 7 |
| 19 | 1430 | 18 | 52 | 7 |
| 20 | 1440 | 18 | 53 | 7.5 |
| 21 | 1450 | 17 | 54 | 7.5 |
In the above, the ceramic sintering temperature control was described in the adjustment method of the present invention, but the method is not limited to the above embodiment. From the above data it is demonstrated that ceramic sintering temperature has a significant effect on pore size and open porosity; the sintering temperature is higher than 1400 ℃, the higher the temperature is, the smaller the average pore diameter of the porous ceramic is, but the ceramic strength is obviously improved.
The porous ceramic atomizing core obtained by the method has high strength, porosity and adjustable aperture. By adjusting the parameters, the porous ceramic atomizing cores with different performances can be manufactured. The method can adjust the performance of the atomizing core to adapt to different electronic cigarette oils.
The pore diameter of the micropores of the porous ceramic atomizing core is 15-25 mu m, and the porosity is 45-55%.
The foregoing embodiments have been provided for the purpose of illustrating the principles and implementations of embodiments of the present invention, and are merely intended to facilitate an understanding of the principles of embodiments of the present invention; meanwhile, as for those skilled in the art, according to the embodiments of the present invention, there are variations in the specific embodiments and the application scope, and the present description should not be construed as limiting the present invention.
Claims (10)
1. A method for preparing a porous ceramic atomizing core, which is characterized by comprising the following steps:
(1) Preparing materials:
mixing and ball milling ceramic aggregate, grinding aid, sintering aid and pore-forming agent, and sieving to obtain raw material powder; drying the raw material powder to make the water content of the raw material powder less than 0.2%;
(2) Preparing materials and pulping:
mixing, heating and stirring raw material powder, a binder and a surfactant to obtain ceramic slurry; the ceramic slurry comprises the following components in percentage by mass: 30-90% of ceramic aggregate, 0.4-0.8% of grinding aid, 5-15% of sintering aid, 20-35% of pore-forming agent, 18-30% of binder and 0.4-1.2% of surfactant; the ceramic aggregate is high-purity silica powder and high-purity alumina powder which are calcined at high temperature, and the purity is more than or equal to 99.9%; the alumina powder accounts for 10-30% of the total mass of the ceramic slurry, and the silica powder accounts for 20-60% of the total mass of the ceramic slurry;
(3) And (3) hot die casting and forming:
performing hot die casting molding on the ceramic slurry to obtain a ceramic green body;
(4) And (3) wax removal: burying and burning the ceramic green body in alumina powder calcined at high temperature, and degreasing under a set atmosphere;
(5) Sintering: and (3) carrying out secondary sintering on the degreased ceramic green body in an atmospheric environment according to a preset temperature curve to obtain the porous ceramic atomization core.
2. The method for preparing a porous ceramic atomized core according to claim 1, wherein the sieving in the step (1) is specifically: the screen residue of the ten-thousand-hole screen is less than 5 percent or passes through a screen with the aperture of 0.2 mm; the drying conditions are as follows: drying at 120-200 deg.c for 2-8 hr.
3. The method for preparing a porous ceramic atomized core according to claim 1, wherein the high-purity silica powder and the high-purity alumina powder are obtained by calcining ceramic aggregate at 1300-1420 ℃ for 2-5 hours; the particle size of the silica powder and the alumina powder in the ceramic aggregate is 10-40 mu m.
4. The method for preparing the porous ceramic atomizing core according to claim 1, wherein the grinding aid is one or a combination of quartz sand, glass powder and acrylic; the sintering aid is low-temperature glass powder or a mixture of high-purity magnesia powder and high-purity calcium oxide powder, the purity is more than or equal to 99.9%, and the mass ratio of the high-purity magnesia powder to the high-purity calcium oxide powder is 2/3-3/2; the pore-forming agent is graphite powder with the particle size of 20-40 mu m; the binder is paraffin; the surfactant is beeswax, oleic acid or stearic acid.
5. The method for preparing a porous ceramic atomized core according to claim 1, wherein in the step (2), the concrete method for pulping is as follows: the adhesive and the surfactant are uniformly mixed, heated to 60-90 ℃ to be melted, then poured into the raw material powder, and stirred for 2-5 hours while being heated to prepare the ceramic slurry.
6. The method for producing a porous ceramic atomized core according to claim 1, wherein in the step (3), the injection temperature is 60 to 75 ℃ and the pressure is 0.3 to 0.6MPa during the hot-cast molding, and the pressure is maintained for 1 to 60 seconds.
7. The method for producing a porous ceramic atomized core according to claim 1, wherein in the step (4), the particle diameter of the high-temperature calcined alumina powder is 20 to 50 μm, and the burial depth is 1 to 5cm; the degreasing atmosphere is set as follows: heating from room temperature to 120 ℃ at a heating rate of 0.5 ℃/min, and preserving heat for 1h; then heating to 300 ℃ at a heating rate of 0.3 ℃/min, and preserving heat for 1h; then heating to 450 ℃ at a heating rate of 0.5 ℃/min, preserving heat for 2 hours, heating to 850 ℃ at a heating rate of 2.5 ℃/min, and preserving heat for 1 hour; then the temperature is increased to 1050 ℃ at the heating rate of 2.5 ℃/min, the heat is preserved for 1h, and finally the furnace is cooled.
8. The method of claim 1, wherein in step (5), the predetermined temperature profile is: heating from room temperature to 1050 ℃ at a heating rate of 5 ℃/min, and preserving heat for 1h; then heating to 1400-1450 ℃ at a heating rate of 3 ℃/min, preserving heat for 2h, and finally cooling along with the furnace.
9. A porous ceramic atomising core made according to the method of any one of claims 1 to 8.
10. The porous ceramic atomizing core of claim 9, wherein the porous ceramic atomizing core has a pore size of 15-25 μm, a porosity of 45-55%, and a density of 0.8-1.2 g/cm 3 。
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