CN115611520B - 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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- 238000010438 heat treatment Methods 0.000 title claims abstract description 72
- 239000005373 porous glass Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title abstract description 21
- 239000011521 glass Substances 0.000 claims abstract description 232
- 238000005191 phase separation Methods 0.000 claims abstract description 54
- 238000000889 atomisation Methods 0.000 claims abstract description 43
- 239000000843 powder Substances 0.000 claims abstract description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 34
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 33
- IURNOFSIYGTQFC-UHFFFAOYSA-N [Si].[B].[Na] Chemical compound [Si].[B].[Na] IURNOFSIYGTQFC-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 22
- 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 21
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 18
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 17
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 17
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 17
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 16
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004327 boric acid Substances 0.000 claims abstract description 13
- 238000000465 moulding Methods 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 10
- 230000008018 melting Effects 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000010791 quenching Methods 0.000 claims abstract description 9
- 230000000171 quenching effect Effects 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 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
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000005530 etching Methods 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000012071 phase Substances 0.000 description 24
- 239000000243 solution Substances 0.000 description 22
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 description 15
- 229960001866 silicon dioxide Drugs 0.000 description 14
- 239000000463 material Substances 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 11
- 238000000498 ball milling Methods 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 3
- 229910001947 lithium oxide Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 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 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 238000000222 aromatherapy Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- MOOAHMCRPCTRLV-UHFFFAOYSA-N boron sodium Chemical compound [B].[Na] MOOAHMCRPCTRLV-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003571 electronic cigarette Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- -1 oxygen ions Chemical class 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000004512 die casting Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Geochemistry & Mineralogy (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Glass Compositions (AREA)
Abstract
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; s2, heating and melting the glass raw material to obtain sodium-boron-silicon glass liquid; s3, carrying out phase separation treatment on sodium-boron-silicon glass liquid after processing and forming to obtain phase separation glass with different enrichment areas; s4, quenching and grinding the split phase glass to obtain glass powder; s5, molding glass powder into a certain shape, and then carrying out split-phase treatment to obtain a glass atomized core green body; s6, placing the glass atomized core green body in an acid solution, and forming a porous structure on the glass atomized core green body; and S7, cleaning and drying the glass atomized core green body to obtain the porous glass atomized core. The invention also provides a porous glass atomizing core and a heating 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 demands of the market for heating atomizing equipment such as a water supplementing instrument, an electronic cigarette, an aromatherapy device and the like, a user has higher requirements for the heating uniformity, the atomizing efficiency and the like of the atomizing equipment. The microporous ceramic is widely applied to various heating and atomizing equipment because of the characteristics of good heating uniformity, high heating and atomizing efficiency and the like.
The existing microporous ceramic is generally formed by forming micropores on the ceramic by adopting a method of adding a pore-forming agent, and is formed by adopting a die casting or injection molding mode and the like. The microporous ceramic prepared by the method has poor uniformity of micropores, and a large amount of paraffin and other organic matters are required to be added in the forming process, so that the problems of deformation, material shortage and the like are easy to occur in the sintering process. Meanwhile, the adoption of the powder burying sintering mode can lead to adhesion of a large amount of wax removing powder on the inner wall of the microporous ceramic, the powder adhered on 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 long-term use. In addition, the porous ceramic prepared by the method needs to consume a great deal 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 prepare the porous glass atomization core with uniform pore diameter and a three-dimensional network structure and can avoid the problems of powder sticking, 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; wherein, the mass fraction of each component in the glass raw material is as follows: 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 into 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-separated glass, and grinding the phase-separated glass to obtain glass powder;
S5, molding the glass powder into a certain shape, and then placing the glass powder into a heat treatment furnace for split-phase treatment to obtain a glass atomized core green body;
S6, placing the glass atomization core green body in an acid solution to remove soluble phases in the glass atomization core, so as 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.
In one realizable mode, the glass raw material comprises 0.5-8% of sodium carbonate, 0.5-3% of lithium carbonate, 0.5-5% of phosphorus pentoxide and 0.5-5% of titanium dioxide.
In one implementation, in the step S6, the glass atomized core green body is pretreated in a pretreatment solution to remove a thin glass layer on the surface of the glass atomized core green body before the glass atomized core green body is placed in the acid solution.
In one implementation, the pretreatment solution is a hydrofluoric acid solution with a volume concentration of 0-10%.
In one implementation manner, the step S2 specifically includes:
and (3) placing the glass raw material into a high-temperature furnace, heating at a speed of 5-10 ℃/min, and preserving heat for 2-4 hours after heating to 1400-1500 ℃ so as to obtain the molten sodium-boron-silicon glass liquid.
In one implementation manner, the step S3 specifically includes:
pouring the sodium-boron-silicon glass liquid into a mould for molding, then placing the mould into a heat treatment furnace for heating to 400-700 ℃, and preserving heat for 0-24 hours for phase separation treatment, thus obtaining the phase separation glass with different enrichment areas.
In one implementation manner, the step S4 specifically includes:
and placing the split-phase glass into deionized water or distilled water for quenching treatment, and grinding the split-phase glass to obtain the glass powder with the mesh number of 80-200 meshes.
In one implementation manner, the step S5 specifically includes:
molding the glass powder into a certain shape, then placing the glass powder into a heat treatment furnace, heating to 400-700 ℃, heating at a speed of 0-10 ℃/min, and preserving the heat for 0-24 hours for split-phase treatment; and after the phase separation treatment is finished, cooling to room temperature at a speed of 5-10 ℃ per minute, thereby obtaining the glass atomized core green body.
In one implementation manner, the step S6 specifically includes:
And placing the glass atomized core green body into 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.
The invention also provides a porous glass atomizing core which is manufactured by adopting the preparation method of the porous glass atomizing 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 atomization core, a glass system based on a sodium-boron-silicon system is adopted, and in the heat treatment process, the sodium-boron-silicon glass can have a liquid phase separation process, namely various phenomena that cations compete for oxygen ions can occur in an oxide melt, so that a part of sodium-boron-rich phase which can be dissolved in acid and a silicon-dioxide-rich phase which is slightly dissolved in acid are formed; the glass substrate after heat treatment is subjected to acid leaching to obtain the porous glass atomization core taking silicon dioxide, silicon-containing compounds, silicate and the like as frameworks. The porous glass atomization core with uniform pore diameter and three-dimensional network structure can be prepared by the preparation method, the problems of powder sticking, sintering deformation, material shortage and the like can be avoided, meanwhile, the preparation process is simple, the production efficiency can be improved, and the production cost can be reduced.
Drawings
Fig. 1 is a schematic structural view of a porous glass atomizing core according to an embodiment of the present invention.
FIG. 2 is an electron microscope image of the internal structure of the porous glass atomizing core in an embodiment of the present invention.
FIG. 3 is another electron microscope image of the internal structure of the porous glass atomizing core in an embodiment of the present invention.
Detailed Description
The following describes in further detail the embodiments of the present invention with reference to the drawings and examples. The following examples are illustrative of the invention and 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 objects and not necessarily for describing a particular sequential or chronological order.
The terms upper, lower, left, right, front, rear, top, bottom and the like (if any) in the description and in the claims are used for descriptive purposes and not necessarily for describing relative positions of structures in the figures and in describing relative positions of structures. It should be understood that the use of directional terms should not be construed to limit the scope of the invention as claimed.
The preparation method of the porous glass atomization core provided by the embodiment of the invention comprises the following steps:
s1, fully grinding and uniformly mixing sodium carbonate (Na 2CO3), boric acid (H 3BO3), silicon dioxide (SiO 2), lithium carbonate (Li 2CO3), phosphorus pentoxide (P 2O5) and titanium dioxide (TiO 2) to obtain a glass raw material; wherein, the mass fractions of each component in the glass raw material are respectively as follows: 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 into a high-temperature furnace, and heating and melting to obtain sodium-boron-silicon glass liquid;
s3, processing and forming 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 split-phase glass, and grinding the split-phase glass to obtain glass powder;
s5, molding glass powder into a certain shape by virtue of mold pressing, and then placing the glass powder into a heat treatment furnace for split-phase treatment to obtain a glass atomized core green body;
S6, placing the glass atomization core green body in an acid solution to remove soluble phases in the glass atomization core, so as to form a porous structure on the glass atomization core green body;
And S7, cleaning and drying the glass atomized core green body to obtain the porous glass atomized core.
Specifically, the preparation method of the porous glass atomization core provided by the embodiment adopts a glass system based on a sodium-boron-silicon system, and in the heat treatment process, the sodium-boron-silicon glass can have a liquid phase separation process, namely various positive ions compete for oxygen ions in an oxide melt, so that a part of sodium-boron-rich phase which can be dissolved in acid and a silicon-dioxide-rich phase which is slightly dissolved in acid are formed; the glass substrate after heat treatment is subjected to acid leaching to obtain the porous glass atomization core taking silicon dioxide, silicon-containing compounds, silicate and the like as frameworks. The porous glass atomization core with uniform pore diameter and three-dimensional network structure can be prepared by the preparation method, the problems of powder sticking, sintering deformation, material shortage and the like can be avoided, meanwhile, the preparation process 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 the element basis of the sodium borosilicate glass. By adding lithium carbonate, the lithium carbonate is decomposed into lithium oxide (Li 2 O) under a high-temperature environment, and the lithium oxide is used as a regulator in a glass structure, has the characteristic of secondary activation, can reduce the melting temperature and melt viscosity of a glass material (when the O/Si ratio in the glass material is small, the lithium oxide can break silicon oxygen bonds and reduce the melt viscosity, and 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, thereby reducing the temperature during melting and phase separation, saving energy and reducing the production difficulty. By adding phosphorus pentoxide and titanium dioxide, the titanium dioxide is mainly used as a crystal nucleus agent, and can promote the growth of crystal nuclei, so that the phase separation speed and the phase separation uniformity are improved; phosphorus pentoxide has smaller ionic radius (the phase separation strength is inversely proportional to the ionic radius, the smaller the ionic radius is, the stronger the phase separation effect is), so that the phosphorus pentoxide can further promote the generation of fine crystal nucleus in the phase separation process of glass, improve the phase separation speed and the phase separation uniformity, and enlarge the phase separation area.
Specifically, in the step S3-S5, the sodium boron silicon glass liquid is processed and molded and then subjected to phase separation treatment to obtain phase separation glass with different enrichment areas, the phase separation glass is ground to obtain glass powder, and then the glass powder is subjected to phase separation treatment after compression molding to obtain a glass atomized core green body, namely, the glass material is subjected to phase separation treatment twice in the process, so that each component in the glass material can be completely separated, the uniformity of phase separation is improved, and the uniformity of micropores formed on the porous glass atomized core is further improved.
Preferably, in the step S1, the mass fraction of sodium carbonate in the glass raw material is 0.5% -8%, the mass fraction of lithium carbonate is 0.5% -3%, the mass fraction of phosphorus pentoxide is 0.5% -5%, and the mass fraction of titanium dioxide is 0.5% -5%.
In one 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 for pretreatment to remove the glass thin layer on the surface of the glass atomized core green body. The pretreatment liquid can be hydrofluoric acid solution with volume concentration of 0-10%.
Specifically, after the glass is subjected to phase separation treatment, a glass thin layer with changed components is formed on the surface of the glass due to volatilization of Na 2 O and B 2O3, and the glass thin layer on the surface of the glass atomized core green body is removed by placing the glass atomized core green body in hydrofluoric acid solution for pretreatment, so that the process of acid corrosion of the glass thin layer is prevented from being slowed down, and the acid corrosion rate is improved.
As an embodiment, the step S2 specifically includes:
and (3) placing the glass raw material into a high-temperature furnace, heating at a speed of 5-10 ℃/min, and preserving heat for 2-4 hours after heating to 1400-1500 ℃ so as to obtain molten sodium-boron-silicon glass liquid.
As an embodiment, the step S3 specifically includes:
Pouring sodium-boron-silicon glass liquid into a mould (such as a graphite mould) for molding, then placing the mould into a heat treatment furnace for heating to 400-700 ℃, and preserving heat for 0-24 hours for phase separation treatment, thus obtaining the phase separation glass with different enrichment areas.
As an embodiment, the step S4 specifically includes:
The phase-separated glass is placed in deionized water or distilled water for quenching treatment, and then the phase-separated glass is ground for 12-24 hours, so that the glass powder with 80-200 meshes is obtained.
Specifically, in order to prevent the phase diffusion of the high-temperature phase-separated glass during natural cooling, the phase-separated glass is quenched by deionized water or distilled water, so that particles in the phase-separated glass are prevented from moving again in the cooling process to cause the phase-separated interface to be blurred.
As an embodiment, the step S5 specifically includes:
Molding glass powder into a certain shape, then placing the glass powder into a heat treatment furnace, heating to 400-700 ℃, heating at a speed of 0-10 ℃/min, and preserving heat for 0-24 hours to perform phase separation treatment; after the phase separation treatment is finished, cooling to room temperature at a speed of 5-10 ℃/min, and thus obtaining the glass atomized core green body.
As an embodiment, the step S6 specifically includes:
And placing the glass atomized core green body into 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.
As an embodiment, the step S7 specifically includes:
carrying out ultrasonic deionized water cleaning on the glass atomized core green body for 3-5 times to ensure that no acid solution remains on the glass atomized core green body; and then placing the glass atomized core green body into a baking oven, and drying at 100-200 ℃ for 2-4 hours to obtain the porous glass atomized core.
As shown in fig. 1, the embodiment of the invention further provides a porous glass atomization core 1, which is manufactured by adopting the preparation method of the porous glass atomization core.
As shown in fig. 1, as an embodiment, a heating film 2 is disposed on the surface of the porous glass atomization core 1, the heating film 2 may be made of a metal film or other conductive heating materials, and the heating film 2 may be formed by depositing a heating metal on the surface of the porous glass atomization 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 film 2, and the electrodes 3 on opposite sides are electrically connected to opposite ends of the heat generating film 2, respectively. The electrode 3 may be made of a material having good electrical 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, the electrode 3 is provided with a lead 4, the lead 4 is electrically connected with the electrode 3, the lead 4 can be fixed on the electrode 3 by welding, and the lead 4 is used for being electrically connected with a power supply (not shown).
As shown in fig. 1, as one 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 shape.
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 supplementing instrument, an aromatherapy device and the like.
The porous glass atomizing 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 by the embodiment has a three-dimensional network structure which is mutually communicated, and the three-dimensional communicated microporous structure increases the curvature of an interface, so that capillaries in the porous glass atomization core 1 are crisscrossed vertically and horizontally and can generate larger pressure jump, the capillary force is greatly enhanced, and a driving force is provided for liquid seepage; in addition, the three-dimensional intercommunication micropore structure can increase the contact of liquid and solid two-phase interface, shortens the transmission path of liquid to promote transmission efficiency. Meanwhile, the pore size of micropores on the porous glass atomization core 1 is uniform, and the distribution of the micropores is uniform, so that the porous glass atomization core 1 has the advantages of high liquid guiding capacity, good heating uniformity, high heating atomization efficiency and high structural strength.
2. The preparation process of the porous glass atomization core 1 does not need to add a large amount of paraffin and other organic matters for bonding, so that the problems of serious influence on yield caused by sintering deformation, powder sticking, large shrinkage, material shortage and the like are avoided, and meanwhile, the preparation 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 the 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%; fully grinding the raw materials by roller ball milling or planetary ball milling after weighing, and uniformly mixing to obtain glass raw materials;
S2, glass melting: placing the glass raw material into an alumina crucible, then placing the alumina crucible into a high-temperature muffle furnace, heating the alumina crucible to 1450 ℃ at a speed of 5 ℃/min, 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 mould for molding, then placing the glass liquid into a heat treatment furnace for heating to 660 ℃, and preserving heat for 4 hours for phase separation treatment, thus obtaining phase separation glass with different enrichment areas;
s4, carrying out phase separation post-treatment on glass: quenching the split-phase glass in deionized water or distilled water, and then ball-milling the split-phase glass in a planetary ball mill for 24 hours to obtain glass powder with 160 meshes;
S5, forming and phase separation treatment of the glass atomized core green body: pressing glass powder into a certain shape through a die, then placing the glass powder into a heat treatment furnace, heating to 620 ℃, keeping the temperature at a speed of 5 ℃/min, and carrying out split-phase treatment after keeping the temperature for 2 hours; after the phase separation treatment is finished, cooling to room temperature at a speed of 8 ℃/min, thereby obtaining a glass atomized core green body;
S6, pretreatment and acid corrosion treatment of the glass atomized core green body: firstly, placing the glass atomized core green body in hydrofluoric acid solution with the volume concentration of 5% for pretreatment so as to remove a glass thin layer on the surface of the glass atomized core green body; then placing the glass atomized core green body into hydrochloric acid solution with the molar concentration of 1.2mol/L for etching treatment, sealing a beaker mouth, and etching for 4 hours to form a porous structure on the glass atomized core green body;
S7, cleaning and drying the glass atomized core green body: carrying out ultrasonic deionized water cleaning on the glass atomized core green body for 5 times to ensure that no acid solution remains on the glass atomized core green body; and then placing the glass atomized core green body into a baking oven, and drying for 2 hours at the temperature of 150 ℃ to obtain the porous glass atomized core with the three-dimensional intercommunicating reticular 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 the 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%; fully grinding the raw materials by roller ball milling or planetary ball milling after weighing, and uniformly mixing to obtain glass raw materials;
s2, glass melting: placing the glass raw material into an alumina crucible, then placing the alumina crucible into a high-temperature muffle furnace, heating the alumina crucible at a speed of 5 ℃/min, and then preserving heat for 4 hours after heating the alumina crucible to 1400 ℃ so as to obtain molten sodium-boron-silicon glass liquid;
s3, glass phase separation treatment: pouring molten sodium-boron-silicon glass liquid into a preheated graphite mould for molding, then placing the glass liquid into a heat treatment furnace for heating to 640 ℃, and preserving heat for 4 hours for phase separation treatment, thus obtaining phase separation glass with different enrichment areas;
s4, carrying out phase separation post-treatment on glass: quenching the split-phase glass in deionized water or distilled water, and then ball-milling the split-phase glass in a planetary ball mill for 24 hours to obtain glass powder with 160 meshes;
s5, forming and phase separation treatment of the glass atomized core green body: pressing glass powder into a certain shape through a die, then placing the glass powder into a heat treatment furnace, heating to 600 ℃, heating at a speed of 5 ℃/min, and preserving heat for 2 hours to perform split-phase treatment; after the phase separation treatment is finished, cooling to room temperature at a speed of 8 ℃/min, thereby obtaining a glass atomized core green body;
S6, pretreatment and acid corrosion treatment of the glass atomized core green body: firstly, placing the glass atomized core green body in hydrofluoric acid solution with the volume concentration of 5% for pretreatment so as to remove a glass thin layer on the surface of the glass atomized core green body; then placing the glass atomized core green body into hydrochloric acid solution with the molar concentration of 1.5mol/L for etching treatment, sealing a beaker mouth, and etching for 4 hours to form a porous structure on the glass atomized core green body;
S7, cleaning and drying the glass atomized core green body: carrying out ultrasonic deionized water cleaning on the glass atomized core green body for 5 times to ensure that no acid solution remains on the glass atomized core green body; and then placing the glass atomized core green body into a baking oven, and drying for 2 hours at the temperature of 150 ℃ to obtain the porous glass atomized core with the three-dimensional intercommunicating reticular 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 the 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%; fully grinding the raw materials by roller ball milling or planetary ball milling after weighing, and uniformly mixing to obtain glass raw materials;
S2, glass melting: placing the glass raw material into an alumina crucible, then placing the alumina crucible into a high-temperature muffle furnace, heating the alumina crucible at a speed of 5 ℃/min, and then preserving heat for 2 hours after heating the alumina crucible to 1400 ℃ so as to obtain molten sodium-boron-silicon glass liquid;
s3, glass phase separation treatment: pouring molten sodium-boron-silicon glass liquid into a preheated graphite mould for molding, then placing the glass liquid into a heat treatment furnace for heating to 650 ℃, and preserving heat for 4 hours for phase separation treatment, thus obtaining phase separation glass with different enrichment areas;
s4, carrying out phase separation post-treatment on glass: quenching the split-phase glass in deionized water or distilled water, and then ball-milling the split-phase glass in a planetary ball mill for 24 hours to obtain glass powder with 160 meshes;
S5, forming and phase separation treatment of the glass atomized core green body: pressing glass powder into a certain shape through a die, then placing the glass powder into a heat treatment furnace, heating to 620 ℃, keeping the temperature at a speed of 5 ℃/min, and carrying out split-phase treatment after keeping the temperature for 2 hours; after the phase separation treatment is finished, cooling to room temperature at a speed of 8 ℃/min, thereby obtaining a glass atomized core green body;
S6, pretreatment and acid corrosion treatment of the glass atomized core green body: firstly, placing the glass atomized core green body in hydrofluoric acid solution with the volume concentration of 5% for pretreatment so as to remove a glass thin layer on the surface of the glass atomized core green body; then placing the glass atomized core green body into hydrochloric acid solution with the molar concentration of 1.5mol/L for etching treatment, sealing a beaker mouth, and etching for 4 hours to form a porous structure on the glass atomized core green body;
S7, cleaning and drying the glass atomized core green body: carrying out ultrasonic deionized water cleaning on the glass atomized core green body for 5 times to ensure that no acid solution remains on the glass atomized core green body; and then placing the glass atomized core green body into a baking oven, and drying for 2 hours at the temperature of 150 ℃ to obtain the porous glass atomized core with the three-dimensional intercommunicating reticular structure.
The prepared porous glass atomized cores were tested, and the parameters of the prepared porous glass atomized cores of the examples are shown in the following table:
| Examples | Porosity (%) | Compressive strength (MPa) | Pore size (micron) | Oil guiding time (seconds) |
| First embodiment | 56 | 15 | 5～20 | 23 |
| Second embodiment | 58 | 14 | 5～20 | 20 |
| Third embodiment | 58 | 14 | 5～20 | 20 |
From the above table, it can be seen that the porosity of the porous glass atomization core in each embodiment is between 50% and 60%, the pore size is suitable, the oil (tobacco tar) guiding capability is strong, the structural strength is high, and the use requirement can be met.
The internal structure of the porous glass atomized core prepared in the first example was subjected to electron microscopic scanning, and the results are shown in fig. 2 and 3 (wherein fig. 2 is an electron microscopic image at a magnification of 5000 times, and fig. 3 is an electron microscopic image at a magnification of 10000 times). As shown in the scanning results of fig. 2 and 3, the porous glass atomizing core prepared in the first embodiment has a three-dimensional inter-working network-like microporous structure, and the micropores are uniformly distributed (the porous glass atomizing cores prepared in the second embodiment and the third embodiment have substantially the same structure as the first embodiment).
The foregoing is merely illustrative 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 about variations or substitutions within the technical scope of the present invention, and the invention should be covered. Therefore, the protection scope of the invention is subject to the protection scope of the claims.
Claims (12)
1. A method for preparing a porous glass atomized core, which 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; wherein, the mass fraction of each component in the glass raw material is as follows: the mass fraction of sodium carbonate is 0.5-10%, the mass fraction of boric acid is 10-20%, the mass fraction of silicon dioxide is 60-80%, the mass fraction of lithium carbonate is 0.5-5%, the mass fraction of phosphorus pentoxide is 0.5-5%, and the mass fraction of titanium dioxide is 0.5-5%;
s2, placing the glass raw material into 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, placing the split-phase glass into deionized water or distilled water for quenching treatment, and grinding the split-phase glass to obtain glass powder;
S5, molding the glass powder into a certain shape, and then placing the glass powder into a heat treatment furnace for split-phase treatment to obtain a glass atomized core green body;
S6, placing the glass atomization core green body in an acid solution to remove soluble phases in the glass atomization core, so as 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.
2. The method for producing a porous glass atomized core according to claim 1, wherein the mass fraction of sodium carbonate in the glass raw material is 0.5% -8%, and the mass fraction of lithium carbonate is 0.5% -3%.
3. The method of producing a porous glass atomized core according to claim 1, wherein in step S6, the glass atomized core green body is pretreated in a pretreatment liquid to remove a glass thin layer on the surface of the glass atomized core green body, before the glass atomized core green body is placed in the acid solution.
4. The method for producing a porous glass atomized core as claimed in claim 3, wherein the pretreatment liquid is a hydrofluoric acid solution having a volume concentration of 5 to 10%.
5. The method for preparing a porous glass atomized core as claimed in claim 1, wherein the step S2 specifically comprises:
and (3) placing the glass raw material into a high-temperature furnace, heating at a speed of 5-10 ℃/min, and preserving heat for 2-4 hours after heating to 1400-1500 ℃ so as to obtain the molten sodium-boron-silicon glass liquid.
6. The method for preparing a porous glass atomized core as claimed in claim 1, wherein the step S3 specifically comprises:
Pouring the sodium-boron-silicon glass liquid into a mould for molding, then placing the mould into a heat treatment furnace for heating to 400-700 ℃, and preserving heat for 4-24 hours for phase separation treatment, thus obtaining the phase separation glass with different enrichment areas.
7. The method for producing a porous glass atomized core as claimed in claim 1, wherein in the step S4, the mesh number of the glass frit is 80 to 200 mesh.
8. The method for preparing a porous glass atomized core as claimed in claim 1, wherein the step S5 specifically comprises:
Molding the glass powder into a certain shape, then placing the glass powder into a heat treatment furnace, heating to 400-700 ℃, keeping the temperature at a speed of 5-10 ℃/min, and carrying out split-phase treatment after keeping the temperature for 2-24 hours; and after the phase separation treatment is finished, cooling to room temperature at a speed of 5-10 ℃ per minute, thereby obtaining the glass atomized core green body.
9. The method for preparing a porous glass atomized core as claimed in claim 1, wherein the step S6 specifically comprises:
And placing the glass atomized core green body into hydrochloric acid solution with the molar concentration of 0.5-2.0mol/L for etching treatment, wherein the etching treatment time is 4-12 hours, so that a porous structure is formed on the glass atomized core green body.
10. The method for preparing a porous glass atomized core as claimed in claim 1, wherein the step S7 specifically comprises:
And cleaning the glass atomized core green body by ultrasonic deionized water for 3-5 times, and then placing the glass atomized core green body into a baking oven, and drying at the temperature of 100-200 ℃ for 2-4 hours to obtain the porous glass atomized core.
11. A porous glass atomising core produced by the method of any one of claims 1 to 10.
12. A heated atomizer comprising the porous glass atomizer core of claim 11.
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