CN106187285B - The preparation method and porous ceramic film material of porous ceramic film material and its application - Google Patents
The preparation method and porous ceramic film material of porous ceramic film material and its application Download PDFInfo
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- CN106187285B CN106187285B CN201510217823.4A CN201510217823A CN106187285B CN 106187285 B CN106187285 B CN 106187285B CN 201510217823 A CN201510217823 A CN 201510217823A CN 106187285 B CN106187285 B CN 106187285B
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Abstract
The present invention relates to a kind of preparation methods of porous ceramic film material, the following steps are included: silicate starting materials and pore creating material are mixed, premix is obtained, wherein the silicate starting materials include sodium metasilicate and other compounds, other compounds are at least one of oxide, nitride, carbide；Premix is dry, obtain silicate aggregate；Silicate aggregate is kneaded with binder, injection raw material is obtained, wherein by mass percentage, silicate aggregate is 50%~60%, binder is 40%~50%；It is injection moulded injection raw material to obtain biscuit；And biscuit is successively subjected to degumming process, calcination processing, obtain porous ceramic film material.The preparation method of above-mentioned porous ceramic film material; addition pore creating material method is combined with injection moulding; the porous ceramic film material porosity of preparation is high, aperture is controllable and has good mechanical property; due to using injection molding technique; compared to using dry pressuring forming process; production efficiency is improved significantly, and is suitble to large-scale production.
Description
Technical field
The present invention relates to field of ceramic material preparation, preparation method more particularly to a kind of porous ceramic film material and porous
Ceramic material and its application.
Background technique
Ceramic material is with natural or synthetic compound by one kind inorganic non-metallic material made of forming and high temperature sintering
Material, purposes are very extensive.
The preparation method of common porous ceramic film material industrial at present mainly has addition pore creating material method, foam impregnation
Method, foaming, injection moulding, granulation mass area method etc..But method made above has its limitation, such as addition pore creating material method
The pore size distribution uniformity of porous ceramic film material obtained is poor, poor mechanical property, and production efficiency is low；What Polymeric sponge method obtained
Article shape density is not easy to control；Foaming is higher to ingredient requirement, and process conditions are not easy to control；The acquisition of granulation mass area method
The product porosity is lower.Therefore, how to prepare that porosity is high, aperture is controllable, good mechanical properties porous ceramic film materials are anxious
Problem to be solved.
Electronic cigarette, for giving up smoking or the electronic product of cigarette substitute, has imitated conventional cigarette appearance, and wherein as a kind of
The tobacco juice of storage does not generate other harmful components such as tar, the suspended particulate in cigarette, will not bring two in heating atomization
Secondary harm of smoking or burning cigarette butt deal with the problem of easily causing fire improperly.Electronic smoke atomizer is that cigarette is stored in electronic cigarette
Liquid and the main component for generating smog.But electronic smoke atomizer common at present, using multiple assembly is constituted, structure is complicated,
Production technology is complicated and service life is low.
Summary of the invention
Based on this, it is necessary to provide and a kind of obtain that porosity is high, aperture is controllable, good mechanical properties porous ceramic film materials
Preparation method and porous ceramic film material.
It there is a need to provide that a kind of porosity is high, aperture is controllable, good mechanical properties porous ceramic film materials.
It there is a need to provide a kind of high production efficiency, the electronic smoke atomizer long using the time.
A kind of preparation method of porous ceramic film material, comprising the following steps:
Silicate starting materials and pore creating material are mixed, premix are obtained, wherein the silicate starting materials include sodium metasilicate and its
His compound, other compounds are at least one of oxide, nitride, carbide, and by mass percentage, sodium metasilicate is
20%~40%, other compounds are 45%~75%, and pore creating material is 3%~20%；
The premix is dry, obtain silicate aggregate；
The silicate aggregate is kneaded with the binder, obtains injection raw material, wherein by mass percentage
Meter, silicate aggregate is 50%~60%, binder is 40%~50%；
It is injection moulded the injection raw material to obtain biscuit；And
The biscuit is successively subjected to degumming process, calcination processing, obtains the porous ceramic film material.
The preparation method of above-mentioned porous ceramic film material combines with injection moulding addition pore creating material method, preparation it is more
Hole ceramic material porosity is high, aperture is controllable and has good mechanical property, due to using injection molding technique, compared to adopting
With dry pressuring forming process, production efficiency is improved significantly, and is suitble to large-scale production.
The pore creating material is at least one of sawdust, starch, graphite in one of the embodiments,.
The dry condition of the premix in one of the embodiments, are as follows: in 70 DEG C~110 DEG C dry 200min~
400min。
In one of the embodiments, by mass percentage, the binder include: 60%~80% paraffin, 5%
~15% polypropylene, 5%~15% stearic acid and 5%~15% dibutyl phthalate.
The condition that the silicate aggregate and the binder are kneaded in one of the embodiments, are as follows: in 180 DEG C
~220 DEG C of mixing 3h~5h.
The injection moulding condition of the injection raw material in one of the embodiments, are as follows: injection temperature is 100 DEG C~160
℃；Injection pressure is 50MPa~140MPa；Dwell pressure is 10MPa~30MPa.
The condition of the degumming process of the biscuit in one of the embodiments, are as follows: keep the temperature 3h at 200 DEG C~800 DEG C
~10h.
The condition of the calcination processing of the biscuit in one of the embodiments, are as follows: keep the temperature 1h at 800 DEG C~1600 DEG C
~4h.
A kind of porous ceramic film material is made using the preparation method of above-mentioned porous ceramic film material.
Application of the above-mentioned porous ceramic film material in electronic smoke atomizer.
Detailed description of the invention
Fig. 1 is the flow chart of the preparation method of the porous ceramic film material of an embodiment；
Fig. 2 is the decomposition texture schematic diagram of the electronic smoke atomizer of an embodiment；
Fig. 3 is the schematic diagram of the section structure of electronic smoke atomizer shown in Fig. 2.
Specific embodiment
To facilitate the understanding of the present invention, a more comprehensive description of the invention is given in the following sections with reference to the relevant attached drawings.In attached drawing
Give preferred embodiment of the invention.But the invention can be realized in many different forms, however it is not limited to herein
Described embodiment.On the contrary, purpose of providing these embodiments is keeps the understanding to the disclosure more saturating
It is thorough comprehensive.
Refering to fig. 1, the porous ceramics preparation method of an embodiment, comprising the following steps:
Step S100: raw material is provided.
Raw material includes silicate starting materials, pore creating material and binder, and silicate starting materials include sodium metasilicate and other compounds,
His compound is at least one of oxide, nitride, carbide.Using resourceful and free of contamination inorganic silicate material
Expect the aggregate as porous ceramic film material, the condition of sintering is more mild, it can be achieved that under lower temperature, air atmosphere and normal pressure
Sintering.
Particularly, oxide include aluminium oxide, zirconium oxide, silica, iron oxide, sodium oxide molybdena, potassium oxide, calcium oxide and
Magnesia etc..
Particularly, nitride includes silicon nitride etc..
Particularly, carbide includes silicon carbide, boron carbide etc..
Particularly, other compound powders are broken to partial size is 60 μm~250 μm.Preferably, other compounds are ground
Sieve.Specifically, by the ground standard screen for being sieved through 60 mesh, 200 mesh equal-specifications of other compounds.
Wherein, while sodium metasilicate is as raw material, also has the function of fluxing agent.Sodium metasilicate as raw material is used as simultaneously
Fluxing agent can effectively reduce sintering temperature, and the glass phase with cementation is generated in high temperature, improve porous ceramic matrix
The intensity of body.Particularly, sodium metasilicate can be by anhydrous sodium metasilicate, sodium silicate nanahydrate (Na2SiO3·9H2O) or modulus be 1.5~
3.5 sodium metasilicate provides.Wherein, modulus is the amount of the substance of silica and sodium oxide molybdena in waterglass (main component sodium metasilicate)
The ratio between.Preferably, sodium metasilicate is provided by modulus for 2.6~2.8 sodium metasilicate.
Step S200: silicate starting materials and pore creating material are mixed, premix is obtained.
The specific steps of step S200 are as follows: pore creating material is sequentially added in other compounds, fluxing agent is mixed to get premix
Material.Particularly, sodium metasilicate is added in form of an aqueous solutions, therefore obtained premix is wet feed.
Particularly, by mass percentage, by 20%~40% sodium metasilicate, 45%~75% other compounds, 3%
~20% pore creating material mixing, obtains premix.
Particularly, the time of silicate starting materials and pore creating material mixing is 0.5h~2h.
Preferably, dry-mixed using tumbling ball mill or planetary ball mill when silicate starting materials, pore creating material being mixed.It can manage
Other modes mixing also can be used in solution, as long as guaranteeing that different materials are uniformly mixed, is such as stirred using blender or kneader
It is dry-mixed.
Particularly, pore creating material is at least one of sawdust, starch, graphite.Using sawdust, starch, sucrose, wood-fibred and
This large-sized complicated organic matter of short carbon fiber or inorganic matter can control finally formed more according to demand as pore creating material
The aperture of hole ceramic material and porosity obtain being suitable for storing, conduct liquid and generate the intercommunicating pore structure of smog.
Particularly, the partial size of pore creating material is 10 μm~800 μm.
Preferably, using the pore creating material with different shape and structure, the connection hole shape of porous ceramic film material is obtained.Example
Such as: using when there is the sawdust of strip to do pore creating material, the pore structure of obtained porous ceramic film material has a large amount of threadiness
Structure；When doing pore creating material using spherical starch, the pore structure of obtained porous ceramic film material is mostly spheroid shape.
Preferably, the granularity for controlling pore creating material then can control the pore structure size of porous ceramic film material.
Preferably, the additional amount of pore creating material, the quantity and distribution density of the pore structure of controllable producing porous ceramic material are controlled.
Therefore by adjusting type, the granularity, incorporation of pore creating material, different porous ceramic film materials can be prepared, to meet different product
Demand.
Step S300: premix is dry, obtain silicate aggregate.
The dry condition of premix are as follows: in 70 DEG C~110 DEG C dry 200min~400min.
Preferably, the drying of premix carries out in drying box.
Step S400: silicate aggregate is kneaded with binder, obtains injection raw material.
Particularly, by mass percentage, by 50%~60% silicate aggregate and 40%~50% binder into
Row is kneaded, and obtains injection raw material.
Particularly, by mass percentage, binder includes: 60%~80% paraffin (PW), poly- the third of 5%~15%
Alkene (PP), 5%~15% stearic acid (SA) and 5%~15% dibutyl phthalate (DBP).Step S400 is specific
Are as follows: at 180 DEG C~220 DEG C, after PP is melted completely, 170 DEG C~190 DEG C are cooled to, silicate aggregate, paraffin is added, is mixed
0.5h~1h is closed, stearic acid, DBP are continuously added, mixes 1h~2h.
Particularly, the condition of mixing is in 180 DEG C~220 DEG C mixing 3h~5h.
Particularly, it is kneaded and is carried out using kneading machine.
Step S500: it is injection moulded injection raw material to obtain biscuit.
Preferably, before step S500, injection raw material is stand-by through cooling, pelletizing.
It is furthermore preferred that the cooling of injection raw material uses natural cooling.It is furthermore preferred that injection raw material pelletizing to partial size is less than
5mm。
Particularly, pelletizing is carried out using crushing plant.Preferably, pelletizing technique uses jaw crushing equipment, roll crushing
The machinery such as equipment or hammer crushing equipment are crushed.It is, of course, also possible to using other Mechanical Crushings, as long as guaranteeing broken rear former
The Particle size requirements of material, for example use impact type crushing plant, circular cone type crushing plant, rotary type crushing plant etc..
Preferably, the injection moulding condition of raw material is injected are as follows: injection temperature is 100 DEG C~160 DEG C；Injection pressure is
50MPa~140MPa；Dwell pressure is 10MPa~30MPa.It is appreciated that injection technological parameter can with the difference of raw material proportioning
It is adjusted.
Preferably, the injection moulding for injecting raw material is carried out in injection (mo(u)lding) machine, will inject raw material and injection (mo(u)lding) machine is added
In hopper, corresponding injection technological parameter is set, is injection moulded to obtain biscuit.
Porous ceramic film material is prepared using injection molding technique, can the multiple biscuits of one-pass molding, both can guarantee product shrink
Rate is smaller, and improves production efficiency, is suitble to large-scale industrial production.
Step S600: biscuit is successively subjected to degumming process, calcination processing, obtains porous ceramic film material.
Preferably, the condition of the degumming process of biscuit are as follows: 3h~10h is kept the temperature at 200 DEG C~800 DEG C.It is furthermore preferred that will
Biscuit is warming up to 200 DEG C~800 DEG C with 1 DEG C/min~10 DEG C/min heating rate.
Particularly, the degumming process of biscuit divides the different temperatures stage to carry out, and different physics occurs in the different temperatures stage
Chemical reaction.Specifically, the physical-chemical reaction that the different temperatures stage occurs include in conjunction with the sloughing of water, the sloughing of constitution water,
The sloughing of pore creating material, the degumming of binder.Particularly, the soaking time of each temperature stage is 0.5h~2h.
Preferably, the condition of the calcination processing of biscuit are as follows: 1h~4h is kept the temperature at 800 DEG C~1600 DEG C.It is furthermore preferred that will
Biscuit is warming up to 800 DEG C~1600 DEG C with 0.5 DEG C/min~5 DEG C/min heating rate.
Particularly, it after step S600, further comprises the steps of: porous ceramic film material natural cooling.
The preparation method of above-mentioned porous ceramic film material combines with injection moulding addition pore creating material method, preparation it is more
Hole ceramic material porosity is high, aperture is controllable and has good mechanical property, due to using injection molding technique, compared to adopting
With dry pressuring forming process, production efficiency is improved significantly, and is suitble to large-scale production.
The porous ceramic film material of one embodiment is prepared using the preparation method of above-mentioned porous ceramics.
Particularly, the porosity of porous ceramic film material is 35%~70%, and aperture is 200nm~2 μm.
Above-mentioned porous ceramic film material is in the application in electronic smoke atomizer.
It needs to store tobacco juice in electronic smoke atomizer and is atomized part tobacco juice every time, lead to the structure of electronic smoke atomizer
Complex, production technology is complicated.Component for electronic smoke atomizer rationally, with higher porosity and some strength
The preparation method of porous ceramic film material.
Particularly, tobacco juice is stored using porous ceramic film material in electronic smoke atomizer.Above-mentioned porous ceramic film material production
Simple process, sintering temperature are low, and porosity with higher and good mechanical strength can be fine for storing tobacco juice
Control smoke amount keep electronic smoke atomizer structure simple so simplifying the structure of electronic smoke atomizer, production technology letter
Just, functional.
Referring to Fig.2, the electronic smoke atomizer 200 of an embodiment, including liquid storing part 210, imbibition portion 220 and atomization portion
230, tobacco juice is stored in liquid storing part 210, above-mentioned porous ceramic film material is filled in imbibition portion 220, and liquid storing part 210 and imbibition portion 220 connect
It is logical, the porous ceramic film material contact in atomization portion 230 and imbibition portion 220, so that the tobacco juice in liquid storing part 210 be made to enter imbibition portion
220 are absorbed by porous ceramic film material, and the tobacco juice that atomization portion 230 absorbs porous ceramic film material is atomized.
Refering to Fig. 2 and Fig. 3, particularly, atomization portion 230 is equipped with the first venthole 231, and the tobacco juice after atomization is logical by first
Stomata 231 enters outside electronic smoke atomizer 200.
Particularly, liquid storing part 210 is equipped with the second venthole 211, the first ventilation of the second venthole 211 and atomization portion 230
Hole 231 is connected to.Particularly, electronic smoke atomizer 200 further includes cigarette holder 240, and cigarette holder 240 is connect with liquid storing part 210, and and liquid storage
Second venthole 211 in portion 210 is connected to.
Specifically, in the present embodiment, atomization portion 230 is heating wire, and 230 adstante febre of atomization portion inhales porous ceramic film material
The tobacco juice of receipts is atomized.
Further, above-mentioned electronic smoke atomizer 200 further includes electric connection 250, and electric connection 250 is connect with atomization portion 230,
By the connections such as electric connection 250 and power supply for driving atomization portion 230.
Further, above-mentioned electronic smoke atomizer 200 further includes shell 260, liquid storing part 210, imbibition portion 220, atomization portion
230, cigarette holder 240 and electric connection 250 are set in shell 260.
The imbibition portion 220 of electronic smoke atomizer 200 absorbs tobacco juice from liquid storing part 210 using above-mentioned porous ceramic film material, by
Good mechanical strength, higher porosity in above-mentioned porous ceramic film material make imbibition portion 220 that can reach storage tobacco juice
Purpose, and can be good at controlling smoke amount, so the structure of electronic smoke atomizer is simplified, above-mentioned electronic smoke atomizer 200
Structure is simple, and production technology is easy, functional, long service life.
The following are the specific embodiments of the preparation method of above-mentioned porous ceramic film material.
The method that the porous ceramic film material of following embodiment preparation of the present invention is tested for the property are as follows: Archimedes's drainage
Measure the porosity of porous ceramic film material；With electronic universal tester to bending strength (the GB/T 4741- of porous ceramic film material
1999) it is tested；Use the average pore size of BET specific surface instrument measurement porous ceramic film material.
Embodiment 1:
After ground 80 mesh of alumina powder, 400g alumina powder is taken, 80 mesh~100 mesh sawdust 60g is added, in
Ball grinding stirring mixing 30min in ball mill adds industrial waterglass (main component sodium metasilicate) 230g that modulus is 2.6, mixes
Stirring 30min is closed, premix is obtained.
Premix is put in 80 DEG C of dry 400min in drying box, obtains dry silicate aggregate.
Kneading machine is preheated to 220 DEG C, polypropylene 20g is added in kneading machine, until being cooled to after polypropylene melts completely
170 DEG C, add silicate aggregate 400g, paraffin 300g, mixing 1h；Continuously add stearic acid 40g, dibutyl phthalate
40g, mixing 2h obtain injection raw material.
Raw material cooling will be injected, using crocodile formula crushing plant pelletizing.Injection (mo(u)lding) machine is added in injection raw material after pelletizing
Hopper in, be injection moulded to obtain biscuit, injection temperature is 135 DEG C, injection pressure 140MPa, dwell pressure 10MPa.Element
Under the size of base is preferably supplemented.
Biscuit is put into high-temperature pressure resistance furnace, is warming up to 200 DEG C with the heating rate of 5 DEG C/min, keeps the temperature 2h, then with
Same rate is warming up to 300 DEG C, is warming up to 420 DEG C after keeping the temperature 1h, keeps the temperature 2h, then be warming up to 500 DEG C of guarantors with the rate of 2 DEG C/min
Warm 1h, abjection combine water, constitution water, pore creating material and binder.Sample is warming up to 1400 DEG C of burnings again with the rate of 2 DEG C/min
1h is tied, the porous ceramic film material is obtained after furnace cooling.
Porous ceramic film material is subjected to porosity, bending strength, average pore size measurement.With this condition, porous ceramics material
The porosity of material is 49.58%, bending strength 15.60Mpa, and average pore size is 1.250 μm.
Embodiment 2:
After zirconium oxide abrasive is crossed 60 meshes, 400g zirconium oxide is taken, 60 mesh~80 mesh sawdust 80g is added, in ball mill
Middle ball grinding stirring mixing 40min adds the industrial waterglass 160g that modulus is 2.8, and 20min is mixed, obtains premix.
Premix is put in 100 DEG C of dry 300min in drying box, obtains dry silicate aggregate.
Kneading machine is preheated to 220 DEG C, polypropylene 40g is added in kneading machine, until being cooled to after polypropylene melts completely
170 DEG C, add silicate aggregate 400g, paraffin 280g, mixing 1h；Continuously add stearic acid 40g, dibutyl phthalate
40g, mixing 2h obtain injection raw material.
It will the cooling of injection raw material, pelletizing.Injection raw material after pelletizing is added in hopper, is injection moulded to obtain element
Base, injection temperature are 140 DEG C, injection pressure 120MPa, dwell pressure 20MPa.
Biscuit is put into high-temperature pressure resistance furnace, is warming up to 200 DEG C with the heating rate of 2 DEG C/min, keeps the temperature 2h, then with
Same rate is warming up to 300 DEG C, is warming up to 420 DEG C after keeping the temperature 1h, keeps the temperature 2h, then be warming up to 500 DEG C of guarantors with the rate of 2 DEG C/min
Warm 1h, abjection combine water, constitution water, pore creating material and binder.Sample is warming up to 1200 DEG C of burnings again with the rate of 2 DEG C/min
1h is tied, the porous ceramic film material is obtained after furnace cooling.Porous ceramic film material is subjected to porosity, bending strength, average hole
Diameter measurement.With this condition, the porosity of porous ceramic film material is 64.71%, bending strength 10.70Mpa, and average pore size is
1.885μm。
Embodiment 3:
After silicon nitride powder grinding is sieved with 100 mesh sieve, 400g silicon nitride powder is taken, the graphite 133g of 200 mesh is added, in ball mill
Middle ball grinding stirring mixing 30min adds the industrial waterglass 355g that modulus is 1.5, and 30min is mixed, obtains premix.
Premix is put in 110 DEG C of dry 300min in drying box, obtains dry silicate aggregate.
Kneading machine is preheated to 220 DEG C, polypropylene 20g is added in kneading machine, until being cooled to after polypropylene melts completely
170 DEG C, add silicate aggregate 400g, paraffin 320g, mixing 1h；Continuously add stearic acid 20g, dibutyl phthalate
40g, mixing 2h obtain injection raw material.
It will the cooling of injection raw material, pelletizing.Injection raw material after pelletizing is added in hopper, is injection moulded to obtain element
Base, injection temperature are 160 DEG C, injection pressure 140MPa, dwell pressure 30MPa.
Biscuit is put into high-temperature pressure resistance furnace, is warming up to 200 DEG C with the heating rate of 4 DEG C/min, keeps the temperature 2h, then with
The heating rate of 2 DEG C/min is warming up to 420 DEG C, keeps the temperature 1h, then be warming up to 600 DEG C of heat preservation 1.5h with the rate of 2 DEG C/min, deviates from
In conjunction with water, constitution water, graphite and binder；Sample is warming up to 1600 DEG C of sintering 4h again with the rate of 2 DEG C/min, it is cold with furnace
But the porous ceramic film material is obtained afterwards.Porous ceramic film material is subjected to porosity, bending strength, average pore size measurement.Herein
Under the conditions of, the porosity of porous ceramic film material is 36.95%, bending strength 19.60Mpa, average pore size 270nm.
Embodiment 4:
By ground 150 mesh of diatomite ore raw material, wherein diatomite ore raw material based on mass fraction, contains titanium dioxide
Silicon 90%, aluminium oxide 6%, iron oxide 1%, sodium oxide molybdena 2.5%, other 0.5%.400g diatomite ore raw material is taken, is added 300
Purpose starch 40g, the ball grinding stirring mixing 30min in ball mill add the industrial waterglass 200g that modulus is 3.5, mixing
30min is stirred, premix is obtained.
Premix is put in 80 DEG C of dry 300min in drying box, obtains dry silicate aggregate.
Kneading machine is preheated to 200 DEG C, polypropylene 32 is added in kneading machine, until being cooled to after polypropylene melts completely
170 DEG C, add silicate aggregate 400g, paraffin 240g, mixing 1h；Continuously add stearic acid 26g, dibutyl phthalate
22g, mixing 2h obtain injection raw material.
It will the cooling of injection raw material, pelletizing.Injection raw material after pelletizing is added in hopper, is injection moulded to obtain element
Base, injection temperature are 120 DEG C, injection pressure 80MPa, dwell pressure 10MPa.
Biscuit is put into high-temperature pressure resistance furnace, is warming up to 200 DEG C with the heating rate of 2 DEG C/min, keeps the temperature 2h, then with
Same rate is warming up to 380 DEG C, is warming up to 420 DEG C after keeping the temperature 1h, keeps the temperature 1h, then be warming up to 500 DEG C of guarantors with the rate of 2 DEG C/min
Warm 1h, abjection combine water, constitution water, starch and binder；Sample is warming up to 950 DEG C of sintering again with the rate of 2 DEG C/min
1h obtains the porous ceramic film material after furnace cooling.Porous ceramic film material is subjected to porosity, bending strength, average pore size
Measurement.With this condition, the porosity of porous ceramic film material is 50.47%, bending strength 17.60Mpa, and average pore size is
475nm。
Embodiment 5:
By ground 250 mesh of feldspar-kaolin mixed mineral raw material, andesine-kaolin mixed mineral raw material with
Mass fraction meter contains silica 65%, aluminium oxide 28%, iron oxide 0.5%, sodium oxide molybdena 5%, other 1.5%.Take 400g long
The starch 12g of 300 mesh is added in stone-kaolin mixed mineral raw material, and ball grinding stirring mixing 30min, adds mould in ball mill
The industrial waterglass 85g that number is 2.5 is mixed 30min, obtains premix.
Premix is put in 80 DEG C of dry 300min in drying box, obtains dry silicate aggregate.
Kneading machine is preheated to 180 DEG C, polypropylene 40g is added in kneading machine, until being cooled to after polypropylene melts completely
170 DEG C, dry feedstock 400g, paraffin 160g are added, stearic acid 40g, dibutyl phthalate 27g is added in mixing 1h, mixes
Expect 2h, obtains injection raw material.
It will the cooling of injection raw material, pelletizing.Injection raw material after pelletizing is added in hopper, is injection moulded to obtain element
Base, injection temperature are 100 DEG C, injection pressure 50MPa, dwell pressure 10MPa.
Biscuit is put into high-temperature pressure resistance furnace, is warming up to 200 DEG C with the heating rate of 2 DEG C/min, keeps the temperature 2h, then with
Same rate is warming up to 380 DEG C, is warming up to 420 DEG C after keeping the temperature 40min, keeps the temperature 1h, then be warming up to 500 with the rate of 2 DEG C/min
DEG C heat preservation 40min, abjection combine water, constitution water, starch and binder；Sample is warming up to 800 again with the rate of 2 DEG C/min
DEG C sintering 2h, the porous ceramic film material is obtained after furnace cooling.Porous ceramic film material is subjected to porosity, bending strength, is put down
Equal inside diameter measurement.With this condition, the porosity of porous ceramic film material is 44.82%, bending strength 13.35Mpa, average hole
Diameter is 200nm.
Comparative example:
By ground 150 mesh of diatomite ore raw material, wherein diatomite ore raw material based on mass fraction, contains titanium dioxide
Silicon 90%, aluminium oxide 6%, iron oxide 1%, sodium oxide molybdena (potassium) 2.5%, other 0.5%.100g diatomite ore raw material is taken, is added
The starch 10g for entering 300 mesh, the ball grinding stirring mixing 30min in ball mill add the industrial waterglass 50g that modulus is 3.5,
30min is mixed, obtains wet feed, is fitted into cylindrical die, required green compact is pressed under 8MPa pressure.
Green compact is put into high-temperature pressure resistance furnace, 600 DEG C of heat preservation 2h are warming up to 2 DEG C/min rate, remove pore creating material
And moisture；Sample is warming up to 800 DEG C of sintering 2h again with the rate of 2 DEG C/min, required porous ceramics is obtained after furnace cooling.It will
The porous ceramics carries out porosity, bending strength, average pore size measurement.With this condition, the porosity of the porous ceramics is
72.12%, bending strength 9.60MPa, average pore size 621nm.
From Examples 1 to 5 it can be seen that porous ceramic film material prepared by the preparation method of porous ceramic film material of the invention
Porosity is higher and intensity is preferable, and the porosity of porous ceramic film material obtained is 35%~70%, and bending strength is 10.7~
20MPa, aperture are 200nm~2 μm.Meanwhile Examples 1 to 5, compared with comparative example, comparative example is using dry-pressing formed sample obtained
Though product porosity is high, compression strength is very low, and requirement is not achieved in intensity.
Compare comparative example and embodiment 4, comparative example is identical as 4 silicate aggregate proportion of embodiment, subsequent forming agglomerant
Skill is different.It can be seen that, due to containing moisture in raw material, demoulding is compared after molding when comparative example is formed using dry pressuring forming process
Difficulty, easily causes deformation or damage at phenomena such as be easy to causeing sizing, falling off and compact strength is inadequate in transportational process.And
Embodiment 4 is using injection moulding, and the sample of extrusion is due to binder rapid curing at low temperature, so that sample surfaces are smooth, no
With die bonds, easy mold release, and sample has certain intensity, and situations such as deformation is damaged is less prone in transportational process.
It follows that in the subsequent sintering process, unbalance stress is formed using dry pressuring forming process, in green compact sintering process
Easily there is phenomena such as cracking, destroy；As long as and being injection moulded injection temperature, the injection pressure kept in one injection forming process
Power, dwell pressure and time, these technological parameters were constant, and porous ceramic film material performance obtained is stable, structure is uniform, reduced
Cracking destruction phenomenon in sintering.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (8)
1. a kind of preparation method of porous ceramic film material, which comprises the following steps:
Silicate starting materials and pore creating material are mixed, premix is obtained, wherein the silicate starting materials include sodium metasilicate and other changes
Close object, other compounds be at least one of oxide, nitride, carbide, the premix by mass percentage by
Following components composition: sodium metasilicate 20%~40%, other compounds 45%~75% and pore creating material 3%~20%；The oxidation
Object is at least one of aluminium oxide, zirconium oxide, silica, iron oxide, sodium oxide molybdena, potassium oxide, calcium oxide and magnesia, institute
Stating nitride is silicon nitride, and the carbide is at least one of silicon carbide and boron carbide；The pore creating material is sawdust, forms sediment
At least one of powder, graphite；
The premix is dry, obtain silicate aggregate；
The silicate aggregate is kneaded with binder, obtains injection raw material, wherein by mass percentage, silicate
Aggregate is 50%~60%, binder is 40%~50%；By mass percentage, the binder includes 60%~80%
Paraffin, 5%~15% polypropylene, 5%~15% stearic acid and 5%~15% dibutyl phthalate；
It is injection moulded the injection raw material to obtain biscuit；And
The biscuit is successively subjected to degumming process, calcination processing, obtains the porous ceramic film material.
2. the preparation method of porous ceramic film material according to claim 1, which is characterized in that the dry item of the premix
Part are as follows: in 70 DEG C~110 DEG C dry 200min~400min.
3. the preparation method of porous ceramic film material according to claim 1, which is characterized in that the silicate aggregate and institute
State the condition that binder is kneaded are as follows: in 180 DEG C~220 DEG C mixing 3h~5h.
4. the preparation method of porous ceramic film material according to claim 1, which is characterized in that the injection of the injection raw material
Condition of molding are as follows: injection temperature is 100 DEG C~160 DEG C；Injection pressure is 50MPa~140MPa；Dwell pressure be 10MPa~
30MPa。
5. the preparation method of porous ceramic film material according to claim 1, which is characterized in that the degumming process of the biscuit
Condition are as follows: at 200 DEG C~800 DEG C keep the temperature 3h~10h.
6. the preparation method of porous ceramic film material according to claim 1, which is characterized in that the calcination processing of the biscuit
Condition are as follows: at 800 DEG C~1600 DEG C keep the temperature 1h~4h.
7. a kind of porous ceramic film material, which is characterized in that using the described in any item porous ceramic film materials of claim 1~6
Preparation method is made.
8. application of the porous ceramic film material as claimed in claim 7 in electronic smoke atomizer.
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