CN115611520A - Porous glass atomizing core, preparation method thereof and heating atomizing device - Google Patents
Porous glass atomizing core, preparation method thereof and heating atomizing device Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
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- 238000000889 atomisation Methods 0.000 claims abstract description 81
- 238000011282 treatment Methods 0.000 claims abstract description 57
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 38
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000843 powder Substances 0.000 claims abstract description 38
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 34
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- IURNOFSIYGTQFC-UHFFFAOYSA-N [Si].[B].[Na] Chemical compound [Si].[B].[Na] IURNOFSIYGTQFC-UHFFFAOYSA-N 0.000 claims abstract description 23
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002253 acid Substances 0.000 claims abstract description 22
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 19
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 18
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 17
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 15
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 14
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- 238000002844 melting Methods 0.000 claims abstract description 10
- 230000008018 melting Effects 0.000 claims abstract description 10
- 238000005191 phase separation Methods 0.000 claims description 51
- 238000000034 method Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000005530 etching Methods 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 238000000465 moulding Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
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- 238000003825 pressing Methods 0.000 claims description 7
- 238000007723 die pressing method Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 24
- 239000012071 phase Substances 0.000 description 23
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 description 15
- 239000000463 material Substances 0.000 description 14
- 230000008569 process Effects 0.000 description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 10
- 238000000498 ball milling Methods 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 8
- 239000011734 sodium Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 6
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 4
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- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 4
- 229910001947 lithium oxide Inorganic materials 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- 239000005388 borosilicate glass Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
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- 238000007789 sealing Methods 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
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- 239000002210 silicon-based material Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
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- 241000222519 Agaricus bisporus Species 0.000 description 1
- 235000001674 Agaricus brunnescens Nutrition 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B15/00—Details of spraying plant or spraying apparatus not otherwise provided for; Accessories
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
Abstract
The invention provides a preparation method of a porous glass atomization core, which comprises the following steps: s1, sufficiently grinding and uniformly mixing sodium carbonate, boric acid, silicon dioxide, lithium carbonate, phosphorus pentoxide and titanium dioxide to obtain a glass raw material; s2, heating and melting the glass raw material to obtain sodium-boron-silicon glass liquid; s3, carrying out phase splitting treatment after the sodium-boron-silicon glass liquid is processed and molded to obtain phase-splitting glass with different enrichment areas; s4, quenching and grinding the phase-split glass to obtain glass powder; s5, carrying out phase splitting treatment after the glass powder is molded into a certain shape to obtain a glass atomization core green body; s6, placing the glass atomization core green body in an acid solution to form a porous structure on the glass atomization core green body; and S7, cleaning and drying the glass atomization core green body to obtain the porous glass atomization core. The invention also provides a porous glass atomizing core and a heating and atomizing device.
Description
Technical Field
The invention relates to the technical field of heating atomization, in particular to a porous glass atomization core, a preparation method thereof and a heating atomization device.
Background
Along with the increasing demand of market to heating atomizing equipment such as moisturizing appearance, electron cigarette, champignon ware, the user has also higher requirement to performance such as heating homogeneity, atomizing efficiency of atomizing equipment. The microporous ceramic is widely applied to various heating and atomizing devices due to the characteristics of good heating uniformity, high heating and atomizing efficiency and the like.
The existing microporous ceramics generally adopt a method of adding pore-forming agent to form micropores on the ceramics, and are formed by a mode of die casting or injection molding, etc. The micropore uniformity of the micropore ceramic prepared by the method is poor, and a large amount of organic matters such as paraffin and the like are required to be added in the forming process, so that the problems of deformation, material shortage and the like are easily caused in the sintering process. Meanwhile, the mode of powder embedding and sintering can lead to a large amount of wax removing powder adhered to the inner wall of the microporous ceramic, the powder adhered to the inner wall is easy to fall off when the microporous ceramic is used, the powder falling phenomenon occurs, and the health of a user can be influenced after the microporous ceramic is used for a long time. In addition, the porous ceramic prepared by the method needs to consume a large amount of time and energy in the glue discharging process, so that the production efficiency is reduced, and the production cost is increased.
Disclosure of Invention
The invention aims to provide a preparation method of a porous glass atomization core, which can be used for preparing the porous glass atomization core with uniform pore diameter and a three-dimensional net structure and can avoid the problems of powder adhesion, sintering deformation, material shortage and the like.
The invention provides a preparation method of a porous glass atomization core, which comprises the following steps:
s1, fully grinding and uniformly mixing sodium carbonate, boric acid, silicon dioxide, lithium carbonate, phosphorus pentoxide and titanium dioxide to obtain a glass raw material; the glass raw material comprises the following components in percentage by mass: 0-10% of sodium carbonate, 10-20% of boric acid, 60-80% of silicon dioxide, 0-5% of lithium carbonate, 0-5% of phosphorus pentoxide and 0-5% of titanium dioxide;
s2, placing the glass raw material in a high-temperature furnace, and heating and melting to obtain a sodium-boron-silicon glass liquid;
s3, processing and forming the sodium-boron-silicon glass liquid, and then placing the sodium-boron-silicon glass liquid in a heat treatment furnace for phase separation treatment to obtain phase separation glass with different enrichment areas;
s4, quenching the phase separation glass, and then grinding the phase separation glass to obtain glass powder;
s5, molding the glass powder into a certain shape through die pressing, and then placing the glass powder into a heat treatment furnace for phase separation treatment to obtain a glass atomization core green body;
s6, placing the glass atomized core green body in an acid solution to remove a soluble phase in the glass atomized core, so that a porous structure is formed on the glass atomized core green body;
and S7, cleaning and drying the glass atomization core green body to obtain the porous glass atomization core.
In an achievable manner, the glass raw material has a mass fraction of 0.5% to 8% of sodium carbonate, a mass fraction of 0.5% to 3% of lithium carbonate, a mass fraction of 0.5% to 5% of phosphorus pentoxide and a mass fraction of 0.5% to 5% of titanium dioxide.
In an achievable manner, in the S6 step, the glass atomized core green compact is pretreated in a pretreatment solution to remove the thin glass layer on the surface of the glass atomized core green compact before the glass atomized core green compact is placed in the acid solution.
In one achievable form, the pretreatment solution is a hydrofluoric acid solution having a concentration of 0-10% by volume.
In an implementable manner, the S2 step specifically includes:
and (3) putting the glass raw material into a high-temperature furnace, heating at the speed of 5-10 ℃/min, heating to 1400-1500 ℃, and then preserving heat for 2-4 hours to obtain the molten sodium-boron-silicon glass liquid.
In an implementable manner, the S3 step specifically includes:
and pouring the sodium-boron-silicon glass liquid into a mold for molding, then placing the mold into a heat treatment furnace for heating to 400-700 ℃, and preserving heat for 0-24 hours for phase separation treatment, thereby obtaining the phase separation glass with different enrichment areas.
In an implementable manner, the S4 step specifically includes:
and putting the phase separation glass into deionized water or distilled water for quenching treatment, and then grinding the phase separation glass to obtain the glass powder with the mesh number of 80-200 meshes.
In an implementable manner, the step S5 specifically comprises:
the glass powder is made into a certain shape by mould pressing, then is placed in a heat treatment furnace to be heated to 400-700 ℃, the heating rate is 0-10 ℃/min, and the temperature is kept for 0-24 hours for phase splitting treatment; and after the phase separation treatment is finished, cooling to room temperature at the speed of 5-10 ℃/min to obtain the glass atomized core green body.
In an implementable manner, the S6 step specifically includes:
and (3) placing the glass atomization core green body in a hydrochloric acid solution with the molar concentration of 0.5-2.0mol/L for etching treatment, wherein the etching treatment time is 0-12 hours, so that a porous structure is formed on the glass atomization core green body.
The invention also provides a porous glass atomization core which is manufactured by the preparation method of the porous glass atomization core.
The invention also provides a heating atomization device which comprises the porous glass atomization core.
According to the preparation method of the porous glass atomizing core, a glass system based on a sodium borosilicate system is adopted, and during a heat treatment process, the sodium borosilicate glass can generate a liquid phase separation process, namely, various cations can generate a phenomenon of competing for oxygen ions in an oxide melt, so that a part of sodium-rich boron phase which can be dissolved in acid and a silicon dioxide-rich phase which is slightly dissolved in acid are formed; the porous glass atomizing core with silica, silicon-containing compound, silicate and the like as the framework can be obtained by performing the acid leaching process on the glass substrate after the heat treatment. The porous glass atomization core with uniform pore diameter and a three-dimensional reticular structure can be prepared by the preparation method, the problems of powder adhesion, sintering deformation, material shortage and the like can be avoided, and meanwhile, the preparation method is simple, the production efficiency can be improved, and the production cost can be reduced.
Drawings
FIG. 1 is a schematic structural diagram of a porous glass atomizing core in an embodiment of the present invention.
FIG. 2 is an electron microscope image of the internal structure of the porous glass atomizing core in the example of the present invention.
FIG. 3 is another electron micrograph of the internal structure of the porous glass atomizing core in the example of the present invention.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention.
The terms "first," "second," "third," "fourth," and the like in the description and in the claims, if any, are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order.
The terms of orientation, up, down, left, right, front, back, top, bottom, and the like (if any) referred to in the specification and claims of the present invention are defined by the positions of structures in the drawings and the positions of the structures relative to each other, only for the sake of clarity and convenience in describing the technical solutions. It is to be understood that the use of directional terms should not be taken to limit the scope of the claimed invention.
The preparation method of the porous glass atomization core provided by the embodiment of the invention comprises the following steps:
s1, mixing sodium carbonate (Na) 2 CO 3 ) Boric acid(H 3 BO 3 ) Silicon dioxide (SiO) 2 ) Lithium carbonate (Li) 2 CO 3 ) Phosphorus pentoxide (P) 2 O 5 ) And titanium dioxide (TiO) 2 ) Fully grinding and uniformly mixing to obtain a glass raw material; the glass raw material comprises the following components in percentage by mass: 0-10% of sodium carbonate, 10-20% of boric acid, 60-80% of silicon dioxide, 0-5% of lithium carbonate, 0-5% of phosphorus pentoxide and 0-5% of titanium dioxide;
s2, placing the glass raw material in a high-temperature furnace, and heating and melting to obtain sodium-boron-silicon glass liquid;
s3, processing and forming the sodium-boron-silicon glass liquid, and then placing the formed glass liquid in a heat treatment furnace for phase separation treatment to obtain phase separation glass with different enrichment areas;
s4, quenching the split-phase glass, and then grinding the split-phase glass to obtain glass powder;
s5, molding the glass powder into a certain shape through mold pressing, and then placing the glass powder into a heat treatment furnace for phase splitting treatment to obtain a glass atomization core green body;
s6, placing the glass atomized core green body in an acid solution to remove a soluble phase in the glass atomized core, so that a porous structure is formed on the glass atomized core green body;
and S7, cleaning and drying the glass atomization core green body to obtain the porous glass atomization core.
Specifically, in the preparation method of the porous glass atomizing core provided in this embodiment, a glass system based on a soda-borosilicate system is adopted, and during a heat treatment process, a liquid phase separation process occurs in the soda-borosilicate glass, that is, various cations compete for oxygen ions in an oxide melt, so that a part of a sodium-rich boron phase which can be dissolved in acid and a silica-rich phase which is slightly dissolved in acid are formed; the porous glass atomizing core with silica, silicon-containing compound, silicate and the like as the framework can be obtained by performing the acid leaching process on the glass substrate after the heat treatment. The porous glass atomization core with uniform pore diameter and a three-dimensional reticular structure can be prepared by the preparation method, the problems of powder adhesion, sintering deformation, material shortage and the like can be avoided, and meanwhile, the preparation method is simple, the production efficiency can be improved, and the production cost can be reduced.
Specifically, in the step S1, sodium carbonate, boric acid, and sodium element, boron element, and silicon element in silica in the glass raw material form an element basis of the soda-borosilicate glass. By adding lithium carbonate, lithium carbonate is decomposed into lithium oxide (Li) in a high-temperature environment 2 O), lithium oxide as a modifier in the glass structure, which has a secondary activation property capable of lowering the melting temperature and melt viscosity of the glass material (when the O/Si ratio in the glass material is small, lithium oxide can break silicon-oxygen bonds, lowering the melt viscosity; meanwhile, when 0.1-0.2% of lithium oxide is added into the glass material, the melting temperature can be reduced by 20-40 ℃, so that the glass material is easier to melt, the temperature during melting and phase splitting is reduced, the energy is saved, and the production difficulty is reduced. By adding phosphorus pentoxide and titanium dioxide, the titanium dioxide is mainly used as a crystal nucleus agent, which can promote the growth of crystal nuclei, thereby improving the phase separation rate and the uniformity of phase separation; the phosphorus pentoxide has small ionic radius (the split phase strength is inversely proportional to the ionic radius, and the smaller the ionic radius, the stronger the split phase effect), so that the phosphorus pentoxide can further promote the glass to generate fine crystal nuclei in the split phase process, improve the split phase rate and the split phase uniformity, and enlarge the split phase area.
Specifically, in the steps S3 to S5, phase-separated glass with different enrichment regions is obtained by performing phase-separating treatment after sodium-boron-silicon glass liquid is processed and molded, then phase-separated glass is ground to obtain glass powder, and then phase-separating treatment is performed after the glass powder is molded to obtain a glass atomization core green body, that is, in the process, two phase-separating treatments are performed on the glass material, so that each component in the glass material can be subjected to complete phase separation, and thus the uniformity of phase separation is improved, and further the uniformity of micropores formed on the porous glass atomization core is improved.
Preferably, in the step S1, the mass fraction of the sodium carbonate in the glass raw material is 0.5% to 8%, the mass fraction of the lithium carbonate is 0.5% to 3%, the mass fraction of the phosphorus pentoxide is 0.5% to 5%, and the mass fraction of the titanium dioxide is 0.5% to 5%.
As an embodiment, in the step S6, before the glass atomized core green body is placed in the acid solution, the glass atomized core green body is placed in a pretreatment solution to be pretreated, so as to remove the thin glass layer on the surface of the glass atomized core green body. The pretreatment solution can be hydrofluoric acid solution with volume concentration of 0-10%.
Specifically, after the glass is subjected to the phase separation treatment, the glass is separated from the solvent due to Na 2 O and B 2 O 3 The volatilization of the glass can form a glass thin layer with changed components on the surface of the glass, and the glass thin layer on the surface of the glass atomization core green body is removed by placing the glass atomization core green body in hydrofluoric acid solution for pretreatment, so that the process of acid corrosion is prevented from being slowed down by the glass thin layer, and the acid corrosion rate is improved.
As an embodiment, the step S2 specifically includes:
putting the glass raw material into a high-temperature furnace, heating at the speed of 5-10 ℃/min, heating to 1400-1500 ℃, and then preserving heat for 2-4 hours, thereby obtaining the molten sodium-boron-silicon glass liquid.
As an embodiment, the step S3 specifically includes:
pouring the sodium-boron-silicon glass liquid into a mold (such as a graphite mold) for molding, then placing the mold in a heat treatment furnace for heating to 400-700 ℃, and preserving heat for 0-24 hours for phase separation treatment, thereby obtaining the phase separation glass with different enrichment regions.
As an embodiment, the step S4 specifically includes:
putting the phase-separated glass into deionized water or distilled water for quenching treatment, and then grinding the phase-separated glass for 12-24 hours to obtain glass powder with 80-200 meshes.
Specifically, in order to prevent phase diffusion of high-temperature phase-separated glass during natural temperature reduction, deionized water or distilled water is used for quenching the phase-separated glass, so that the phenomenon that particles in the phase-separated glass move again in the cooling process to cause phase-separated interface blurring is prevented.
As an embodiment, the step S5 specifically includes:
the glass powder is made into a certain shape by mould pressing, then the glass powder is placed in a heat treatment furnace to be heated to 400-700 ℃, the heating rate is 0-10 ℃/min, and the temperature is kept for 0-24 hours for phase separation treatment; and after the phase separation treatment is finished, cooling to room temperature at the speed of 5-10 ℃/min to obtain the glass atomized core green body.
As an embodiment, the step S6 specifically includes:
and (3) placing the glass atomization core green body in a hydrochloric acid solution with the molar concentration of 0.5-2.0mol/L for etching treatment, wherein the etching treatment time is 0-12 hours, so that a porous structure is formed on the glass atomization core green body.
As an embodiment, the step S7 specifically includes:
carrying out ultrasonic deionized water cleaning on the glass atomization core green body for 3-5 times to ensure that no acid solution is left on the glass atomization core green body; and then putting the glass atomized core green body into an oven, and drying for 2-4 hours at the temperature of 100-200 ℃ to obtain the porous glass atomized core.
As shown in fig. 1, the embodiment of the present invention further provides a porous glass atomizing core 1, which is manufactured by the above preparation method of the porous glass atomizing core.
As shown in fig. 1, as an embodiment, a heating film 2 is disposed on a surface of a porous glass atomizing core 1, the material of the heating film 2 may be a metal film or other conductive heating material, and the heating film 2 may be formed by depositing a heating metal on the surface of the porous glass atomizing core 1 by printing, magnetron sputtering, vacuum evaporation, spraying, or the like.
As shown in fig. 1, as an embodiment, electrodes 3 are provided on opposite sides of the heat generating thin film 2, and the electrodes 3 on the opposite sides are electrically connected to opposite ends of the heat generating thin film 2, respectively. The electrode 3 may be made of a material having good conductivity, such as metal, and the electrode 3 may be fixed to the porous glass atomizing core 1 by means of adhesion, embedding, or the like. Meanwhile, a lead 4 is provided on the electrode 3, the lead 4 is electrically connected to the electrode 3, the lead 4 can be fixed on the electrode 3 by welding, and the lead 4 is used for electrically connecting to a power supply (not shown).
As shown in fig. 1, as an embodiment, the porous glass atomizing core 1 has a cylindrical structure. Of course, in other embodiments, the porous glass atomizing core 1 may have other shapes, such as a rectangular parallelepiped structure, etc.
The embodiment of the invention also provides a heating and atomizing device which comprises the porous glass atomizing core 1, wherein the heating and atomizing device can be an electronic cigarette, a water replenishing instrument, an aromatherapy device and the like.
The porous glass atomization core 1 and the preparation method thereof provided by the embodiment of the invention have the advantages that:
1. the porous glass atomization core 1 prepared in the embodiment is of a three-dimensional network structure which is communicated with each other, and the three-dimensional communicated microporous structure increases the curvature of an interface, so that capillaries in the porous glass atomization core 1 are criss-cross and all-around, larger pressure jump can be generated, the capillary force is greatly enhanced, and a driving force is provided for liquid seepage; in addition, the three-dimensional intercommunicated micropore structure can increase the contact between the two-phase interfaces of liquid and solid and shorten the transmission path of the liquid, thereby improving the transmission efficiency. Meanwhile, the pore sizes of the micropores on the porous glass atomization core 1 are uniform, and the micropores are uniformly distributed, so that the porous glass atomization core 1 is strong in liquid guiding capacity, good in heating uniformity, high in heating atomization efficiency and high in structural strength.
2. The porous glass atomizing core 1 is prepared without adding a large amount of organic matters such as paraffin for bonding, so that the problem that sintering deformation, powder adhesion, large shrinkage, material shortage and the like seriously affect the yield is avoided, and meanwhile, the manufacturing process is simple, the production efficiency can be improved, and the production cost is reduced.
First embodiment
The preparation method of the porous glass atomization core provided by the embodiment comprises the following steps:
s1, selecting, weighing and mixing glass raw materials: the glass raw materials are analytically pure sodium carbonate, boric acid, silicon dioxide, lithium carbonate, phosphorus pentoxide and titanium dioxide, and are weighed on an electronic balance according to a formula proportion, wherein the mass fraction of the sodium carbonate is 2%, the mass fraction of the boric acid is 12%, the mass fraction of the silicon dioxide is 80%, the mass fraction of the lithium carbonate is 2%, the mass fraction of the phosphorus pentoxide is 2%, and the mass fraction of the titanium dioxide is 2%; after weighing, fully grinding the raw materials by roller ball milling or planetary ball milling, and uniformly mixing to obtain a glass raw material;
s2, glass melting: putting a glass raw material into an alumina crucible, then placing the alumina crucible in a high-temperature muffle furnace, heating the glass raw material at the speed of 5 ℃/min to 1450 ℃, and then preserving the heat for 4 hours to obtain molten sodium-boron-silicon glass liquid;
s3, glass phase separation treatment: pouring molten sodium-boron-silicon glass liquid into a preheated graphite mold for molding, then placing the molded glass liquid into a heat treatment furnace for heating to 660 ℃, and preserving heat for 4 hours for phase separation treatment, thereby obtaining phase separation glass with different enrichment areas;
s4, glass phase separation post-treatment: putting the phase-separated glass into deionized water or distilled water for quenching treatment, and then putting the phase-separated glass into a planetary ball mill for ball milling for 24 hours to obtain glass powder with the mesh number of 160 meshes;
s5, forming a glass atomization core green body and performing phase splitting treatment: pressing the glass powder into a certain shape through a mould, then placing the glass powder in a heat treatment furnace to heat to 620 ℃, wherein the heating rate is 5 ℃/min, and preserving heat for 2 hours to carry out phase separation treatment; after the phase separation treatment is finished, cooling to room temperature at the speed of 8 ℃/min to obtain a glass atomized core green body;
s6, pretreatment and acid erosion treatment of the glass atomization core green body: firstly, placing the glass atomization core green body in hydrofluoric acid solution with volume concentration of 5% for pretreatment so as to remove a glass thin layer on the surface of the glass atomization core green body; then placing the glass atomization core green body in a hydrochloric acid solution with the molar concentration of 1.2mol/L for etching treatment, sealing the beaker, and etching for 4 hours, thereby forming a porous structure on the glass atomization core green body;
s7, cleaning and drying the glass atomization core green body: carrying out ultrasonic deionized water cleaning on the glass atomization core green body for 5 times to ensure that no acid solution residue exists on the glass atomization core green body; and then putting the glass atomization core green body into an oven, and drying for 2 hours at the temperature of 150 ℃ to obtain the porous glass atomization core with the three-dimensional intercommunicated net structure.
Second embodiment
The preparation method of the porous glass atomization core provided by the embodiment comprises the following steps:
s1, selecting, weighing and mixing glass raw materials: the glass raw materials are analytically pure sodium carbonate, boric acid, silicon dioxide, lithium carbonate, phosphorus pentoxide and titanium dioxide, and are weighed on an electronic balance according to a formula proportion, wherein the mass fraction of the sodium carbonate is 4%, the mass fraction of the boric acid is 16%, the mass fraction of the silicon dioxide is 70%, the mass fraction of the lithium carbonate is 4%, the mass fraction of the phosphorus pentoxide is 3%, and the mass fraction of the titanium dioxide is 3%; after weighing, fully grinding the raw materials by roller ball milling or planetary ball milling, and uniformly mixing to obtain a glass raw material;
s2, glass melting: putting a glass raw material into an alumina crucible, then placing the alumina crucible into a high-temperature muffle furnace, heating the alumina crucible at the speed of 5 ℃/min, heating the alumina crucible to 1400 ℃, and then preserving the heat for 4 hours to obtain molten sodium-boron-silicon glass liquid;
s3, glass phase separation treatment: pouring molten sodium-boron-silicon glass liquid into a preheated graphite mold for molding, then placing the molded glass liquid into a heat treatment furnace for heating to 640 ℃, and preserving heat for 4 hours for phase separation treatment, thereby obtaining phase separation glass with different enrichment areas;
s4, glass phase separation post-treatment: putting the phase-separated glass into deionized water or distilled water for quenching treatment, and then putting the phase-separated glass into a planetary ball mill for ball milling for 24 hours to obtain glass powder with the mesh number of 160 meshes;
s5, forming a glass atomization core green body and performing phase splitting treatment: pressing the glass powder into a certain shape through a mould, then placing the glass powder in a heat treatment furnace to be heated to 600 ℃, heating up at the speed of 5 ℃/min, and preserving heat for 2 hours to carry out phase separation treatment; after the phase separation treatment is finished, cooling to room temperature at the speed of 8 ℃/min, thereby obtaining a glass atomized core green body;
s6, pretreatment and acid corrosion treatment of the glass atomization core green body: firstly, placing the glass atomization core green body in hydrofluoric acid solution with volume concentration of 5% for pretreatment so as to remove a glass thin layer on the surface of the glass atomization core green body; then placing the glass atomization core green body in hydrochloric acid solution with the molar concentration of 1.5mol/L for etching treatment, sealing the beaker, and etching for 4 hours, thereby forming a porous structure on the glass atomization core green body;
s7, cleaning and drying the glass atomization core green body: carrying out ultrasonic deionized water cleaning on the glass atomization core green body for 5 times to ensure that no acid solution residue exists on the glass atomization core green body; and then putting the glass atomization core green body into an oven, and drying for 2 hours at the temperature of 150 ℃ to obtain the porous glass atomization core with the three-dimensional intercommunicated net structure.
Third embodiment
The preparation method of the porous glass atomization core provided by the embodiment comprises the following steps:
s1, selecting, weighing and mixing glass raw materials: the glass raw materials are analytically pure sodium carbonate, boric acid, silicon dioxide, lithium carbonate, phosphorus pentoxide and titanium dioxide, and are weighed on an electronic balance according to a formula proportion, wherein the mass fraction of the sodium carbonate is 6%, the mass fraction of the boric acid is 20%, the mass fraction of the silicon dioxide is 70%, the mass fraction of the lithium carbonate is 2%, the mass fraction of the phosphorus pentoxide is 0.5%, and the mass fraction of the titanium dioxide is 1.5%; after weighing, fully grinding the raw materials by roller ball milling or planetary ball milling, and uniformly mixing to obtain a glass raw material;
s2, glass melting: putting a glass raw material into an alumina crucible, then placing the alumina crucible into a high-temperature muffle furnace, heating the alumina crucible at the speed of 5 ℃/min, heating the alumina crucible to 1400 ℃, and then preserving the heat for 2 hours to obtain molten sodium-boron-silicon glass liquid;
s3, glass phase separation treatment: pouring molten sodium-boron-silicon glass liquid into a preheated graphite mold for molding, then placing the molded glass liquid into a heat treatment furnace for heating to 650 ℃, and preserving heat for 4 hours for phase separation treatment, thereby obtaining phase separation glass with different enrichment areas;
s4, glass phase separation post-treatment: putting the phase-separated glass into deionized water or distilled water for quenching treatment, and then putting the phase-separated glass into a planetary ball mill for ball milling for 24 hours to obtain glass powder with the mesh number of 160 meshes;
s5, forming a glass atomization core green body and performing phase splitting treatment: pressing the glass powder into a certain shape through a mold, then placing the glass powder into a heat treatment furnace to be heated to 620 ℃, wherein the heating speed is 5 ℃/min, and preserving heat for 2 hours to carry out phase splitting treatment; after the phase separation treatment is finished, cooling to room temperature at the speed of 8 ℃/min, thereby obtaining a glass atomized core green body;
s6, pretreatment and acid corrosion treatment of the glass atomization core green body: firstly, placing the glass atomization core green body in hydrofluoric acid solution with volume concentration of 5% for pretreatment so as to remove a glass thin layer on the surface of the glass atomization core green body; then placing the glass atomization core green body in hydrochloric acid solution with the molar concentration of 1.5mol/L for etching treatment, sealing the beaker, and etching for 4 hours, thereby forming a porous structure on the glass atomization core green body;
s7, cleaning and drying the glass atomization core green body: carrying out ultrasonic deionized water cleaning on the glass atomization core green body for 5 times to ensure that no acid solution residue exists on the glass atomization core green body; and then putting the glass atomization core green body into an oven, and drying for 2 hours at the temperature of 150 ℃ to obtain the porous glass atomization core with the three-dimensional intercommunicated net structure.
The porous glass atomizing cores obtained were tested, and the parameters of the porous glass atomizing cores obtained in each example are shown in the following table:
| examples | Porosity (%) | Compressive strength (MPa) | Pore size (micron) | Oil guiding time (second) |
| First embodiment | 56 | 15 | 5～20 | 23 |
| Second embodiment | 58 | 14 | 5～20 | 20 |
| Third embodiment | 58 | 14 | 5～20 | 20 |
As can be seen from the table above, the porosity of the porous glass atomizing core in each embodiment is between 50% and 60%, the pore size is appropriate, the oil (smoke) guiding capability is strong, the structural strength is high, and the use requirement can be met.
The internal structure of the porous glass atomizing core prepared in the first example was subjected to electron microscope scanning, and the results are shown in fig. 2 and fig. 3 (wherein fig. 2 is an electron microscope image at a magnification of 5000 times, and fig. 3 is an electron microscope image at a magnification of 10000 times). As shown in the scanning results of fig. 2 and fig. 3, the porous glass atomizing core prepared in the first example has a three-dimensional interconnected network micropore structure, and the micropores are uniformly distributed (the porous glass atomizing cores prepared in the second and third examples have substantially the same structure as that of the first example).
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily think of the changes or substitutions within the technical scope of the present invention, and shall cover the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (11)
1. The preparation method of the porous glass atomization core is characterized by comprising the following steps:
s1, fully grinding and uniformly mixing sodium carbonate, boric acid, silicon dioxide, lithium carbonate, phosphorus pentoxide and titanium dioxide to obtain a glass raw material; the glass raw material comprises the following components in percentage by mass: 0-10% of sodium carbonate, 10-20% of boric acid, 60-80% of silicon dioxide, 0-5% of lithium carbonate, 0-5% of phosphorus pentoxide and 0-5% of titanium dioxide;
s2, placing the glass raw material in a high-temperature furnace, and heating and melting to obtain sodium-boron-silicon glass liquid;
s3, processing and forming the sodium-boron-silicon glass liquid, and then placing the sodium-boron-silicon glass liquid in a heat treatment furnace for phase separation treatment to obtain phase separation glass with different enrichment areas;
s4, quenching the phase separation glass, and then grinding the phase separation glass to obtain glass powder;
s5, molding the glass powder into a certain shape through die pressing, and then placing the glass powder into a heat treatment furnace for phase separation treatment to obtain a glass atomization core green body;
s6, placing the glass atomized core green body in an acid solution to remove a soluble phase in the glass atomized core, so that a porous structure is formed on the glass atomized core green body;
and S7, cleaning and drying the glass atomization core green body to obtain the porous glass atomization core.
2. The method of preparing a porous glass atomizing core according to claim 1, wherein the glass raw material contains 0.5 to 8 mass% of sodium carbonate, 0.5 to 3 mass% of lithium carbonate, 0.5 to 5 mass% of phosphorus pentoxide, and 0.5 to 5 mass% of titanium dioxide.
3. The method of making a porous atomized glass core according to claim 1, wherein in step S6, the green glass atomized core is pretreated in a pretreatment solution to remove the thin glass layer on the surface of the green glass atomized core before the green glass atomized core is placed in the acid solution.
4. The method for preparing the porous glass atomizing core according to claim 3, wherein the pretreatment liquid is a hydrofluoric acid solution having a volume concentration of 0 to 10%.
5. The method for preparing a porous glass atomizing core according to claim 1, wherein the step S2 specifically comprises:
and (3) putting the glass raw material into a high-temperature furnace, heating at the speed of 5-10 ℃/min, heating to 1400-1500 ℃, and then preserving heat for 2-4 hours to obtain the molten sodium-boron-silicon glass liquid.
6. The method for preparing a porous glass atomizing core according to claim 1, wherein the step S3 specifically includes:
and pouring the sodium-boron-silicon glass liquid into a mold for molding, then placing the mold into a heat treatment furnace for heating to 400-700 ℃, and preserving heat for 0-24 hours for phase separation treatment, thereby obtaining the phase separation glass with different enrichment areas.
7. The method for preparing a porous glass atomizing core according to claim 1, wherein the step S4 specifically includes:
and putting the phase separation glass into deionized water or distilled water for quenching treatment, and then grinding the phase separation glass to obtain the glass powder with the mesh number of 80-200 meshes.
8. The method for preparing a porous glass atomizing core according to claim 1, wherein the step S5 specifically includes:
the glass powder is made into a certain shape by mould pressing, then the glass powder is placed in a heat treatment furnace to be heated to 400-700 ℃, the heating rate is 0-10 ℃/min, and the temperature is kept for 0-24 hours for phase separation treatment; and after the phase separation treatment is finished, cooling to room temperature at the speed of 5-10 ℃/min to obtain the glass atomized core green body.
9. The method for preparing a porous glass atomizing core according to claim 1, wherein the step S6 specifically includes:
and (3) placing the glass atomized core green body in a hydrochloric acid solution with the molar concentration of 0.5-2.0mol/L for etching treatment, wherein the etching treatment time is 0-12 hours, so that a porous structure is formed on the glass atomized core green body.
10. A porous glass atomizing core characterized by being produced by the method for producing a porous glass atomizing core according to any one of claims 1 to 9.
11. A heating atomizing device characterized by comprising the porous glass atomizing core according to claim 10.
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