CN112545066B - Graphene porous ceramic capable of heating, atomization core and preparation method thereof - Google Patents
Graphene porous ceramic capable of heating, atomization core and preparation method thereof Download PDFInfo
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- CN112545066B CN112545066B CN202011561876.5A CN202011561876A CN112545066B CN 112545066 B CN112545066 B CN 112545066B CN 202011561876 A CN202011561876 A CN 202011561876A CN 112545066 B CN112545066 B CN 112545066B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000000919 ceramic Substances 0.000 title claims abstract description 91
- 238000010438 heat treatment Methods 0.000 title claims abstract description 87
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000000889 atomisation Methods 0.000 title abstract description 12
- 239000012188 paraffin wax Substances 0.000 claims abstract description 57
- 238000005245 sintering Methods 0.000 claims abstract description 47
- 239000001993 wax Substances 0.000 claims abstract description 37
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 238000000498 ball milling Methods 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 239000011812 mixed powder Substances 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 20
- 239000002002 slurry Substances 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 238000002844 melting Methods 0.000 claims abstract description 13
- 230000008018 melting Effects 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 239000011159 matrix material Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 58
- 239000007788 liquid Substances 0.000 claims description 27
- 239000005543 nano-size silicon particle Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 23
- 229910002804 graphite Inorganic materials 0.000 claims description 19
- 239000010439 graphite Substances 0.000 claims description 19
- 235000012239 silicon dioxide Nutrition 0.000 claims description 18
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 13
- 239000010433 feldspar Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 238000001694 spray drying Methods 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 229920002472 Starch Polymers 0.000 claims description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 7
- 239000004327 boric acid Substances 0.000 claims description 7
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 7
- 239000000292 calcium oxide Substances 0.000 claims description 7
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 7
- 239000008107 starch Substances 0.000 claims description 7
- 235000019698 starch Nutrition 0.000 claims description 7
- 235000013312 flour Nutrition 0.000 claims description 6
- 239000004005 microsphere Substances 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 229910010293 ceramic material Inorganic materials 0.000 claims description 5
- PNYYBUOBTVHFDN-UHFFFAOYSA-N sodium bismuthate Chemical compound [Na+].[O-][Bi](=O)=O PNYYBUOBTVHFDN-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- YIJBJMMXMAYULT-UHFFFAOYSA-K Cl(=O)(=O)[O-].[Bi+3].Cl(=O)(=O)[O-].Cl(=O)(=O)[O-] Chemical compound Cl(=O)(=O)[O-].[Bi+3].Cl(=O)(=O)[O-].Cl(=O)(=O)[O-] YIJBJMMXMAYULT-UHFFFAOYSA-K 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims description 3
- 244000046052 Phaseolus vulgaris Species 0.000 claims description 3
- 239000004793 Polystyrene Substances 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000006004 Quartz sand Substances 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 150000003863 ammonium salts Chemical class 0.000 claims description 3
- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
- 229910052810 boron oxide Inorganic materials 0.000 claims description 3
- 239000004927 clay Substances 0.000 claims description 3
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 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
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 3
- 229920002223 polystyrene Polymers 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 239000004576 sand Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 239000005909 Kieselgur Substances 0.000 claims 1
- 239000000463 material Substances 0.000 description 10
- 229910001385 heavy metal Inorganic materials 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000012535 impurity Substances 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical group O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 239000012856 weighed raw material Substances 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000003287 bathing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000003571 electronic cigarette Substances 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
Classifications
-
- 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
- A24F40/46—Shape or structure of electric heating means
-
- 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
- A24F40/70—Manufacture
Abstract
The invention relates to a graphene porous ceramic capable of heating, an atomization core and a preparation method thereof, wherein the ceramic is prepared from a matrix material and comprises the following components in parts by weight: 1-60 parts of graphene oxide powder, 10-80 parts of ceramic powder, 1-50 parts of pore-forming agent and 1-40 parts of sintering aid. The atomizing core comprises a heating body and positive and negative electrodes arranged at two ends of the heating body, and the heating body is made of graphene porous ceramic capable of heating. The preparation method comprises the following steps: weighing graphene oxide powder, ceramic powder, pore-forming agent and sintering aid raw materials, mixing and ball milling; baking and drying the mixture to obtain mixed powder; heating paraffin to a melting state, adding mixed powder while stirring, and continuously stirring for 1-8 h to obtain paraffin slurry; injecting paraffin slurry into a mould prepared in advance, cooling and forming, and demoulding to obtain a paraffin mould; fifthly, placing the wax mould into a furnace for preheating to remove wax, and obtaining a wax removing sample; and (3) placing the paraffin removal sample into a furnace for sintering, and heating, preserving heat and cooling to obtain the graphene porous ceramic.
Description
Technical Field
The invention belongs to the technical field of heatable ceramics and atomization cores manufactured by the heatable ceramics, and particularly relates to a heatable graphene porous ceramic, an atomization core and a preparation method thereof.
Background
The electronic atomizer comprises an atomization core, wherein the atomization core is used for heating and atomizing liquid to be atomized into aerosol, steam or vapor so as to be convenient for a user to inhale, and the liquid to be atomized can be smoke liquid or solution containing medicines for health medical treatment. The atomizing core is a key component of the electronic atomizer, and the atomizing effect, the heating efficiency and the use experience of the electronic atomizer are directly determined by the performance advantages and disadvantages of the electronic atomizer.
The atomizing core in the market at present is generally by liquid-guiding cotton with heating resistance wire, or ceramic liquid-guiding body and heating resistance wire are constituteed, and the combination mode of resistance wire and ceramic liquid-guiding body has implantation type, printing type, paster type etc. and different combination modes have brought the promotion of certain degree in heat transfer efficiency. The invention patent CN111671163 discloses a preparation method of a graphene thermal conductive ceramic heating element of an electronic cigarette atomizer, which utilizes the rapid thermal reaction efficiency of a graphene material, good thermal stability and thermal conductivity, and coats and fixes a graphene modified thermal conductive coating on ceramic, namely prints or sprays the graphene modified thermal conductive coating on the surface of the ceramic heating element, wherein compared with a resistance wire, the heating surface is further increased by the graphene modified thermal conductive coating, so that the heat transfer efficiency is improved, but the graphene modified thermal conductive coating is a heating element on the surface of the ceramic, in essence, a process of transferring heat from the heating element to the ceramic heating element is realized, a larger temperature gradient is inevitably generated in the heating process, meanwhile, fatigue is generated due to the difference of thermal stress in the repeated heating and cooling process, the reliability of a porous ceramic structure is reduced, impurities and heavy metals in the ceramic are easily separated out and mixed into liquid to be atomized under the condition of unstable structure, and the heavy metal exceeding standard brings potential harm to human bodies.
Disclosure of Invention
The invention aims to solve the technical problems that the prior heating mode has poor structural stability due to larger temperature gradient and thermal fatigue in the heating process, and the problems that impurities and heavy metals in ceramics are easy to separate out and mix into liquid to be atomized to cause exceeding standards under the condition of unstable structure, and provides a graphene porous ceramic capable of heating, an atomizing core and a preparation method thereof.
The technical scheme is that the graphene porous ceramic capable of heating is prepared from a matrix material, wherein the matrix material comprises the following raw material components in parts by weight: 1-60 parts of graphene oxide powder, 10-80 parts of ceramic powder, 1-50 parts of pore-forming agent and 1-40 parts of sintering aid.
Preferably, the matrix material comprises the following raw material components in parts by weight: 10-40 parts of graphene oxide powder, 20-80 parts of ceramic powder, 1-30 parts of pore-forming agent and 1-20 parts of sintering aid.
Preferably, the graphene oxide powder is obtained by chemical oxidation, ultrasonic treatment, spraying and drying treatment of graphite under the condition of strong acid through bismuthate.
Preferably, the ceramic powder comprises at least one of kaolin, diatomite, alumina, silicon nitride, silicon carbide, quartz sand, glass sand, clay and feldspar powder;
preferably, the pore-forming agent is at least one of graphite, starch, flour, bean flour, polystyrene microsphere, polymethyl methacrylate microsphere, carbonate, ammonium salt, sucrose and fiber, and the particle size of the pore-forming agent is 1-200 microns;
preferably, the sintering aid is at least one of boron oxide, boric acid, oleic acid, stearic acid, sodium silicate, calcium oxide, ferric oxide and titanium oxide.
Preferably, the matrix material further comprises the following raw material components in parts by weight: 1-40 parts of nano silicon oxide.
Preferably, the nano silicon oxide is nano silicon dioxide, and the nano silicon dioxide is colloidal nano silicon dioxide or powdery nano silicon dioxide.
Preferably, the porosity of the exothermic graphene porous ceramic is 35-70%.
The invention further provides an atomization core, which comprises a heating body for conducting and heating liquid to be atomized and positive and negative electrodes arranged at two ends of the heating body, wherein the heating body is made of graphene porous ceramic capable of heating.
Preferably, the heating element further comprises a liquid guide layer connected with the heating element, wherein the liquid guide layer is made of porous ceramic materials.
The invention also provides a preparation method of the graphene porous ceramic capable of generating heat, which is characterized by comprising the following steps:
weighing graphene oxide powder, ceramic powder, pore-forming agent and sintering aid raw materials according to a formula, and placing the raw materials into a ball milling device for mixing and ball milling;
roasting and drying the ball-milled mixture to obtain mixed powder;
heating paraffin to a melting state, adding the mixed powder while stirring, and continuing stirring for 1-8 hours after the adding to obtain paraffin slurry;
fourthly, injecting the paraffin slurry into a mould prepared in advance, cooling and forming, and demoulding to obtain a paraffin mould;
fifthly, placing the wax pattern into a furnace for preheating to remove wax, and obtaining a wax removing sample;
and (3) placing the paraffin removal sample into a furnace for sintering, wherein the sintering process comprises heating, heat preservation and cooling to obtain the graphene porous ceramic.
The invention also provides a preparation method of the graphene porous ceramic capable of generating heat, which is characterized by comprising the following steps:
weighing graphene oxide powder, nano silicon oxide, ceramic powder, pore-forming agent and sintering aid raw materials according to a formula, and placing the raw materials into a ball milling device for mixing and ball milling;
roasting and drying the ball-milled mixture to obtain mixed powder;
heating paraffin to a melting state, adding the mixed powder while stirring, and continuing stirring for 1-8 hours after the adding to obtain paraffin slurry;
fourthly, injecting the paraffin slurry into a mould prepared in advance, cooling and forming, and demoulding to obtain a paraffin mould;
fifthly, placing the wax pattern into a furnace for preheating to remove wax, and obtaining a wax removing sample;
and (3) placing the paraffin removal sample into a furnace for sintering, wherein the sintering process comprises heating, heat preservation and cooling to obtain the graphene porous ceramic.
Preferably, the graphene oxide powder is prepared by the following steps: taking graphite, carrying out chemical oxidation by using a strong oxidant under the condition of concentrated sulfuric acid, washing with water until the pH value is slightly acidic, obtaining graphene oxide dispersion liquid by ultrasonic treatment, and carrying out spray drying on the graphene oxide dispersion liquid to obtain graphene oxide powder.
Preferably, the graphite is flake graphite with granularity of 500-5000 meshes, the strong oxidant comprises one or more of sodium bismuthate, potassium bismuthate, bismuth chlorate, bismuth nitrate and bismuth oxynitrate, the pH value after water washing is 5-7, and the spray drying temperature is 80-200 ℃.
Preferably, in the step, the rotating speed of the ball milling device is set to be 150-350 rpm, the ball milling time is 1-10 h, and the diameter of the grinding material is 1-20 mm.
Preferably, in the step (ii), the baking and drying temperature is 60-120 ℃, and the baking and drying time is 2-12 h.
Preferably, in the step, the melting point of the paraffin is 60-110 ℃, and the weight of the paraffin is 10-60% of the weight of the mixed powder.
Preferably, in the step of bathing, the temperature of the wax removal is 400-800 ℃ and the time of the wax removal is 2-12 h.
Preferably, in the step (II), the sintering temperature is 700-1500 ℃, the heating speed is 1-5 ℃/min, and the sintering heat preservation time is 2-12 h; the sintering protective atmosphere is a reducing atmosphere, and the reducing atmosphere comprises hydrogen or mixed gas of hydrogen and inert gas.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, by utilizing the excellent electrothermal property of the graphene material, the graphene thermal conductive material is added in the process of preparing the porous ceramic, so that the ceramic heating body and the heating resistor material are integrally formed, and the problem of poor structural stability caused by larger temperature gradient and thermal fatigue in the heating process is solved;
the graphene porous ceramic is integrally formed into a ceramic resistor, so that atomized liquid can be conducted, and the graphene porous ceramic can generate heat integrally inside, and has the advantages of high electric heating conversion efficiency, uniform heating, wide tolerance temperature range of-50 ℃ to 500 ℃ and good atomization effect of the liquid to be atomized;
according to the invention, the graphene oxide and the ceramic material are integrally sintered, so that the graphene oxide ceramic composite material has reliable structural stability, and the problems that the ceramic is easy to crack and easily separate out impurities and heavy metals in the use process, and the heavy metals exceed standards to bring potential harm to human bodies are solved.
Drawings
FIG. 1 is a schematic structural view of an atomizing core of the present invention;
fig. 2 is a bottom view of the atomizing core of the present invention.
Detailed Description
The invention relates to a graphene porous ceramic capable of heating, which is prepared from the following raw materials in parts by weight: 1-60 parts of graphene oxide powder, 10-80 parts of ceramic powder, 1-50 parts of pore-forming agent and 1-40 parts of sintering aid. Preferably, the matrix material comprises the following raw material components in parts by weight: 10-40 parts of graphene oxide powder, 20-80 parts of ceramic powder, 1-30 parts of pore-forming agent and 1-20 parts of sintering aid.
The graphene oxide powder is obtained by chemical oxidation of graphite through bismuthate under the condition of strong acid, ultrasonic treatment, spraying and drying treatment. The ceramic powder comprises at least one of kaolin, diatomite, alumina, silicon nitride, silicon carbide, quartz sand, glass sand, clay and feldspar powder. The pore-forming agent is at least one of graphite, starch, flour, bean flour, polystyrene microsphere, polymethyl methacrylate microsphere, carbonate, ammonium salt, sucrose and fiber, and the particle size of the pore-forming agent is 1-200 microns. The sintering aid is at least one of boron oxide, boric acid, oleic acid, stearic acid, sodium silicate, calcium oxide, ferric oxide and titanium oxide.
According to the invention, graphene oxide is added into a porous ceramic matrix material to serve as a heating material, the surface of the graphene oxide comprises hydroxyl, carboxyl and other functional groups, the oxygen-containing functional groups on the surface of ceramic particles and the hydroxyl, carboxyl and other functional groups on the surface of the graphene, a stable combination is formed between the ceramic powder material and the graphene in a reducing atmosphere sintering process, so that the graphene porous ceramic capable of heating is obtained, and the graphene has conductivity, so that the graphene porous ceramic can be integrally a resistor and can generate heat when being electrified. The resistance value can be adjusted through the proportion of the graphene and the ceramic powder, the electrothermal conversion efficiency is high, the electrothermal conversion efficiency is good, the thermal conductivity is good, the tolerance temperature range is up to-50 ℃ to 500 ℃, the heating is uniform, the tobacco tar atomization effect is good, and the graphene material is integrally sintered, so that the structural stability is excellent, the graphene material cannot be broken in the use process, and the problem of heavy metal exceeding standard caused by separating impurities and heavy metals is avoided.
The matrix material also comprises the following raw material components in parts by weight: 1-40 parts of nano silicon oxide. The nanometer silicon oxide is nanometer silicon dioxide, and the nanometer silicon dioxide is colloid nanometer silicon dioxide or powder nanometer silicon dioxide. After the components of the nano silicon oxide are added, a micro-nano composite structure is formed through a curing reaction in the calcining process, the nano silicon oxide has an ultrahigh specific surface area, and the surface of the nano silicon oxide contains a large number of hydroxyl groups, so that the sintering temperature can be effectively reduced when the nano silicon oxide reacts with a ceramic powder solid phase, and the nano silicon oxide can enable a product to simultaneously maintain high porosity and realize high strength. Under the conditions of high strength and stable internal structure, the graphene porous ceramic is not easy to crack, impurities are not easy to separate out and heavy metals are not easy to separate out in the use process, and the excessive heavy metals can be avoided to the greatest extent.
The porosity of the graphene porous ceramic capable of heating is 35-70%.
The invention discloses an atomization core, which comprises a heating body for conducting and heating liquid to be atomized, positive and negative electrodes arranged at two ends of the heating body, wherein the heating body is made of graphene porous ceramic capable of heating, and a liquid guide layer connected with the heating body, and the liquid guide layer is made of porous ceramic materials.
The invention discloses a preparation method of a graphene porous ceramic capable of heating, which comprises the following steps:
weighing graphene oxide powder, ceramic powder, pore-forming agent and sintering aid raw materials according to a formula, and placing the raw materials into a ball milling device for mixing and ball milling; wherein the rotating speed of the ball milling device is set to be 150-350 rpm, the ball milling time is 1-10 h, and the diameter of the grinding material is 1-20 mm;
roasting and drying the ball-milled mixture to obtain mixed powder; wherein the baking and drying temperature is 60-120 ℃, and the baking and drying time is 2-12 h;
heating paraffin to a melting state, adding mixed powder while stirring, and continuing stirring for 1-8 hours after the adding to obtain paraffin slurry; wherein, the melting point of the paraffin is 60-110 ℃, and the weight of the paraffin is 10-60% of the weight of the mixed powder.
Injecting paraffin slurry into a mould prepared in advance, cooling and forming, and demoulding to obtain a paraffin mould;
fifthly, placing the wax mould into a furnace for preheating to remove wax, and obtaining a wax removing sample; wherein the temperature of the wax removal is 400-800 ℃, and the time of the wax removal is 2-12 h.
Sixthly, placing the paraffin removal sample into a furnace for sintering, wherein the sintering process comprises heating, heat preservation and cooling to obtain graphene porous ceramic; wherein the sintering temperature is 700-1500 ℃, the heating speed is 1-5 ℃/min, and the sintering heat preservation time is 2-12 h; the sintering protective atmosphere is a reducing atmosphere, and the reducing atmosphere comprises hydrogen or mixed gas of hydrogen and inert gas.
The preparation method of the graphene porous ceramic capable of generating heat comprises the following steps:
weighing graphene oxide powder, nano silicon dioxide, ceramic powder, pore-forming agent and sintering aid raw materials according to a formula, and placing the raw materials into a ball milling device for mixing and ball milling; wherein the rotating speed of the ball milling device is set to be 150-350 rpm, the ball milling time is 1-10 h, and the diameter of the grinding material is 1-20 mm;
roasting and drying the ball-milled mixture to obtain mixed powder; wherein the baking and drying temperature is 60-120 ℃, and the baking and drying time is 2-12 h;
heating paraffin to a melting state, adding mixed powder while stirring, and continuing stirring for 1-8 hours after the adding to obtain paraffin slurry; wherein, the melting point of the paraffin is 60-110 ℃, and the weight of the paraffin is 10-60% of the weight of the mixed powder.
Injecting paraffin slurry into a mould prepared in advance, cooling and forming, and demoulding to obtain a paraffin mould;
fifthly, placing the wax mould into a furnace for preheating to remove wax, and obtaining a wax removing sample; wherein the temperature of the wax removal is 400-800 ℃, and the time of the wax removal is 2-12 h.
Sixthly, placing the paraffin removal sample into a furnace for sintering, wherein the sintering process comprises heating, heat preservation and cooling to obtain graphene porous ceramic; wherein the sintering temperature is 700-1500 ℃, the heating speed is 1-5 ℃/min, and the sintering heat preservation time is 2-12 h; the sintering protective atmosphere is a reducing atmosphere, and the reducing atmosphere comprises hydrogen or mixed gas of hydrogen and inert gas.
The graphene oxide powder is prepared by the following steps:
taking graphite, carrying out chemical oxidation by using a strong oxidant under the condition of concentrated sulfuric acid, washing with water until the pH value is slightly acidic, obtaining graphene oxide dispersion liquid by ultrasonic treatment, and carrying out spray drying on the graphene oxide dispersion liquid to obtain graphene oxide powder. Wherein the graphite is flake graphite, the granularity is 500-5000 meshes, the strong oxidant comprises one or more of sodium bismuthate, potassium bismuthate, bismuth chlorate, bismuth nitrate and bismuth oxynitrate, the pH value after water washing is 5-7, and the spray drying temperature is 80-200 ℃.
The invention will be further described in detail with reference to examples below:
example 1
The graphene porous ceramic capable of heating is prepared from the following raw material components in percentage by weight: 20% of graphene oxide powder, 60% of feldspar powder, 15% of pore-forming agent, 4% of calcium oxide and 1% of boric acid. Wherein the mesh number of the feldspar powder is 400 meshes, and the pore-forming agent is starch with the particle size of 1 micron. The graphene oxide powder is obtained by carrying out ultrasonic treatment spray drying on graphite after chemical oxidation of bismuthate under the condition of strong acid.
Example two
The graphene porous ceramic capable of heating is prepared from the following raw material components in percentage by weight: 20% of graphene oxide powder, 20% of nano silicon dioxide, 40% of feldspar powder, 15% of pore-forming agent, 4% of calcium oxide and 1% of boric acid. Wherein the mesh number of the feldspar powder is 400 meshes, and the pore-forming agent is starch with the particle size of 1 micron. The graphene oxide powder is obtained by carrying out ultrasonic treatment spray drying on graphite after chemical oxidation of bismuthate under the condition of strong acid. The nano silicon dioxide is silica sol with the particle size of 150nm, and the amount of the nano silicon dioxide of the silica sol is calculated by the solid silicon dioxide.
Example III
The atomizing core of the embodiment of the invention, as shown in fig. 1 and 2, comprises a heating body 1 and positive and negative electrodes 3 arranged at two ends of the heating body 1, wherein the heating body 1 is used for conducting and heating liquid to be atomized, the heating body is made of the graphene porous ceramic capable of heating, which is described in the previous embodiment, the upper surface of the heating body is also connected with a liquid guide layer 2 made of a porous ceramic material, the liquid to be atomized flows to the liquid guide layer 2 from top to bottom, the liquid guide layer 2 can conduct downwards and permeate the liquid to be atomized, the liquid to be atomized continues to permeate the heating body 1, and the heating body 1 is made of the graphene porous ceramic capable of heating, so that the heating body 1 can integrally heat, heat is uniform, and an atomization effect is good. The electrode 3 shown in fig. 1 is an electrode with a charged lead, and the electrode 3 shown in fig. 2 is a circular electrode sheet which can be sintered together with the heating element 1. The electrode plate can be connected with the spring electrode in a conflicting mode for electrifying.
Example IV
The preparation method of the graphene porous ceramic capable of generating heat comprises the following steps:
adding 10g of flake graphite with granularity of 1500 meshes into 250mL of concentrated sulfuric acid, stirring for 60min, adding 40g of sodium bismuthate, continuously stirring at high speed for 3h, pouring the reaction solution into 300mL of deionized water, filtering by using ceramic membrane filtering equipment, cleaning the obtained solid to pH 6-7, adding into 1000mL of deionized water, performing ultrasonic treatment for 2h to obtain graphene oxide aqueous dispersion, and performing spray drying at 150 ℃ to obtain graphene oxide powder;
weighing 20% of graphene oxide powder, 60% of feldspar powder, 15% of pore-forming agent, 4% of calcium oxide and 1% of boric acid according to the weight percentage; wherein, the mesh number of the feldspar powder is 400 meshes, and the pore-forming agent is starch with the particle size of 1 micron; placing the weighed raw materials into a ball mill for mixed ball milling, wherein the rotation speed of the ball mill is 300rpm, the ball milling time is 10 hours, and the diameter of abrasive particles is 20mm;
placing the ball-milled mixture in a 60 ℃ oven for baking and drying, and baking for 12 hours to obtain dried mixed powder;
weighing paraffin accounting for 40% of the total weight of raw materials in the steps, wherein the melting point of the paraffin is 60 ℃, heating the paraffin to 65 ℃, adding the mixed powder while stirring in a melted state, and continuing stirring for 6 hours after the adding is finished to obtain paraffin slurry;
fifthly, injecting paraffin slurry into a mould prepared in advance, cooling and forming, and demoulding to obtain a paraffin mould;
the wax film is placed into a wax removing furnace, heated to 400 ℃ in air atmosphere and subjected to wax removal for 6 hours to obtain a wax removed sample;
and (3) putting the paraffin removal sample into a sintering furnace, and sintering in a hydrogen atmosphere at 1150 ℃ at a heating rate of 3 ℃/min for 4 hours.
Example five
The preparation method of the graphene porous ceramic capable of generating heat comprises the following steps:
adding 10g of flake graphite with granularity of 1500 meshes into 250mL of concentrated sulfuric acid, stirring for 60min, adding 40g of sodium bismuthate, continuously stirring at high speed for 3h, pouring the reaction solution into 300mL of deionized water, filtering by using ceramic membrane filtering equipment, cleaning the obtained solid to pH 6-7, adding into 1000mL of deionized water, performing ultrasonic treatment for 2h to obtain graphene oxide aqueous dispersion, and performing spray drying at 150 ℃ to obtain graphene oxide powder;
weighing 20% of graphene oxide powder, 20% of colloidal nano silicon dioxide, 40% of feldspar powder, 15% of pore-forming agent, 4% of calcium oxide and 1% of boric acid according to the weight percentage; wherein, the mesh number of the feldspar powder is 400 meshes, and the pore-forming agent is starch with the particle size of 1 micron; placing the weighed raw materials into a ball mill for mixed ball milling, wherein the rotation speed of the ball mill is 300rpm, the ball milling time is 10 hours, and the diameter of abrasive particles is 20mm;
placing the ball-milled mixture in a 60 ℃ oven for baking and drying, and baking for 12 hours to obtain dried mixed powder;
weighing paraffin accounting for 40% of the total weight of raw materials in the steps, wherein the melting point of the paraffin is 60 ℃, heating the paraffin to 65 ℃, adding the mixed powder while stirring in a melted state, and continuing stirring for 6 hours after the adding is finished to obtain paraffin slurry;
fifthly, injecting paraffin slurry into a mould prepared in advance, cooling and forming, and demoulding to obtain a paraffin mould;
the wax film is placed into a wax removing furnace, heated to 400 ℃ in air atmosphere and subjected to wax removal for 6 hours to obtain a wax removed sample;
and (3) putting the paraffin removal sample into a sintering furnace, and sintering in a hydrogen atmosphere at 1150 ℃ at a heating rate of 3 ℃/min for 4 hours.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (17)
1. The graphene porous ceramic capable of generating heat is characterized by being prepared from a matrix material, wherein the matrix material comprises the following components in parts by weight: 10-40 parts of graphene oxide powder, 20-80 parts of ceramic powder, 1-40 parts of nano silicon oxide, 1-30 parts of pore-forming agent and 1-20 parts of sintering aid; the nano silicon oxide is nano silicon dioxide, and the nano silicon dioxide is colloidal nano silicon dioxide or powdery nano silicon dioxide.
2. The heatable graphene porous ceramic according to claim 1, wherein the graphene oxide powder is obtained by chemical oxidation of graphite with bismuthate under strong acid conditions, ultrasonic treatment, spraying and drying treatment.
3. The heatable graphene porous ceramic according to claim 1, wherein the ceramic powder comprises at least one of kaolin, diatomaceous earth, alumina, silicon nitride, silicon carbide, quartz sand, glass sand, clay, feldspar powder.
4. The heatable graphene porous ceramic according to claim 1, wherein the pore-forming agent is at least one of graphite, starch, flour, bean flour, polystyrene microspheres, polymethyl methacrylate microspheres, carbonate, ammonium salt, sucrose, and fibers, and the pore-forming agent has a particle size of 1-200 microns.
5. The heatable graphene porous ceramic according to claim 1, wherein the sintering aid is at least one of boron oxide, boric acid, oleic acid, stearic acid, sodium silicate, calcium oxide, iron oxide, titanium oxide.
6. The heatable graphene porous ceramic according to claim 1, wherein the porosity of the heatable graphene porous ceramic is 35-70%.
7. An atomizing core, characterized by comprising a heating body for conducting and heating liquid to be atomized and positive and negative electrodes arranged at two ends of the heating body, wherein the heating body is made of the graphene porous ceramic capable of heating according to any one of claims 1-6.
8. The atomizing core of claim 7, further comprising a liquid-conducting layer coupled to the heat generator, the liquid-conducting layer being made of a porous ceramic material.
9. A method for preparing the heatable graphene porous ceramic according to claim 1, comprising the steps of:
weighing graphene oxide powder, ceramic powder, pore-forming agent and sintering aid raw materials according to a formula, and placing the raw materials into a ball milling device for mixing and ball milling;
roasting and drying the ball-milled mixture to obtain mixed powder;
heating paraffin to a melting state, adding the mixed powder while stirring, and continuing stirring for 1-8 hours after the adding to obtain paraffin slurry;
fourthly, injecting the paraffin slurry into a mould prepared in advance, cooling and forming, and demoulding to obtain a paraffin mould;
fifthly, placing the wax pattern into a furnace for preheating to remove wax, and obtaining a wax removing sample;
and (3) placing the paraffin removal sample into a furnace for sintering, wherein the sintering process comprises heating, heat preservation and cooling to obtain the graphene porous ceramic.
10. A method for preparing the heatable graphene porous ceramic according to claim 1, comprising the steps of:
weighing graphene oxide powder, nano silicon oxide, ceramic powder, pore-forming agent and sintering aid raw materials according to a formula, and placing the raw materials into a ball milling device for mixing and ball milling;
roasting and drying the ball-milled mixture to obtain mixed powder;
heating paraffin to a melting state, adding the mixed powder while stirring, and continuing stirring for 1-8 hours after the adding to obtain paraffin slurry;
fourthly, injecting the paraffin slurry into a mould prepared in advance, cooling and forming, and demoulding to obtain a paraffin mould;
fifthly, placing the wax pattern into a furnace for preheating to remove wax, and obtaining a wax removing sample;
and (3) placing the paraffin removal sample into a furnace for sintering, wherein the sintering process comprises heating, heat preservation and cooling to obtain the graphene porous ceramic.
11. The method for preparing a heat-generating graphene porous ceramic according to claim 9 or 10, wherein the graphene oxide powder is prepared by:
taking graphite, carrying out chemical oxidation by using a strong oxidant under the condition of concentrated sulfuric acid, washing with water until the pH value is slightly acidic, obtaining graphene oxide dispersion liquid by ultrasonic treatment, and carrying out spray drying on the graphene oxide dispersion liquid to obtain graphene oxide powder.
12. The method for preparing a heat-generating graphene porous ceramic according to claim 11, wherein the graphite is flake graphite, the granularity is 500-5000 meshes, the strong oxidant comprises one or more of sodium bismuthate, potassium bismuthate, bismuth chlorate, bismuth nitrate and bismuth oxynitrate, the pH value after water washing is 5-7, and the spray drying temperature is 80-200 ℃.
13. The method for preparing the heatable graphene porous ceramic according to claim 9 or 10, characterized in that in the step, the rotation speed of a ball milling device is set to 150-350 rpm, the ball milling time is 1-10 h, and the abrasive diameter is 1-20 mm.
14. The method for preparing a heat-generating graphene porous ceramic according to claim 9 or 10, wherein in the step (ii), the baking and drying temperature is 60-120 ℃ and the baking and drying time is 2-12 h.
15. The method for preparing a heatable graphene porous ceramic according to claim 9 or 10, wherein in the step (iii), the melting point of the paraffin is 60-110 ℃, and the weight of the paraffin is 10-60% of the weight of the mixed powder.
16. The method for preparing a heat-generating graphene porous ceramic according to claim 9 or 10, wherein, in the step, the temperature of the wax removal is 400-800 ℃, and the time of the wax removal is 2-12 h.
17. The method for preparing a heat-generating graphene porous ceramic according to claim 9 or 10, wherein, in the step III, the sintering temperature is 700-1500 ℃, the heating speed is 1-5 ℃/min, and the sintering heat preservation time is 2-12 h; the sintering protective atmosphere is a reducing atmosphere, and the reducing atmosphere comprises hydrogen or mixed gas of hydrogen and inert gas.
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| CN114190602A (en) * | 2021-11-11 | 2022-03-18 | 立讯精密工业股份有限公司 | Atomizing core and atomizer |
| CN114538953A (en) * | 2022-03-28 | 2022-05-27 | 深圳市立场科技有限公司 | Manufacturing process of heating ceramic atomizing core and heating ceramic atomizing core |
| CN115159991B (en) * | 2022-07-18 | 2023-12-12 | 深圳市赛尔美电子科技有限公司 | Porous ceramic heating structure and preparation method thereof |
| CN115286423B (en) * | 2022-08-03 | 2023-07-14 | 东莞市国研电热材料有限公司 | Patch type hydrogen protection high-temperature integrated sintered microporous ceramic atomization core, preparation method thereof and microporous ceramic atomization core |
| CN115819070B (en) * | 2022-11-16 | 2023-12-19 | 深圳市爱斯强科技有限公司 | Ceramic slurry and ceramic matrix |
| CN116144964B (en) * | 2023-02-22 | 2023-08-18 | 无锡盛旭复合材料有限公司 | Preparation method of multilayer graphene reinforced aluminum matrix composite |
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