CN107162629A - A kind of preparation method of foamed ceramics - Google Patents
A kind of preparation method of foamed ceramics Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of foamed ceramics, belong to porous ceramic film material preparing technical field.Rice husk is first crushed and dries obtained powdered rice hulls by the present invention after autoclaving, organic matter in powdered rice hulls is set first to carbonize at low temperature again, coordinate the catalytic action of nanometer iron powder and sodium fluoride, form silicon carbide whisker, after unreacted charing organic matter is removed through aerobic calcining, unreacted silica is removed using hydrofluoric acid, enable silicon carbide whisker after purification, it is well mixed with poly-vinyl alcohol solution, self-control sintering aid, aluminum oxide etc., chilled again, thaw cycles make polyvinyl alcohol crosslinked solidification, most sintered afterwards after vacuum freeze drying and foamed ceramics is made.Foamed ceramics of the present invention shrinks small when base substrate is burnt till, and is difficult to collapse, and products machinery intensity is high, and density is small, and its density is only 0.25~0.32g/cm3, compression strength is up to 3.9~4.7MPa.
Description
Technical field
The invention discloses a kind of preparation method of foamed ceramics, belong to porous ceramic film material preparing technical field.
Background technology
Foamed ceramics is that it is after common porous ceramic, the porous pottery of honeycomb as the porous ceramics of foam-like in a kind of moulding
The third generation porous ceramic articles grown up after porcelain.This high-performance ceramics has three-dimensional communication duct, at the same because with
Special performance, such as high-specific surface area, high osmosis, low unit weight, lower thermal conductivity and the attention for increasingly causing each side.These
Excellent performance makes it in fields such as catalyst carrier, melted metal filtering, high temperature air filtration, refractory material, biomaterials
It is used widely.
Foamed ceramics material develops into high temperature resistant, corrosion-resistant, resistance to sudden heating material by initial unselected clay matter(Such as carbon
SiClx, aluminum oxide, cordierite, aluminium titanates, mullite, spodumene etc.).The preparation method of foam ceramic material is a lot, wherein should
With more successfully having:Add pore-creating agent method, foaming method, organic precursor infusion process and colloidal sol-gel method etc..
Addition pore-creating agent method is, by adding pore creating material in ceramic batch, to occupy certain in base substrate using pore creating material
Space, then through oversintering, pore creating material leaves matrix and forms stomata to prepare foamed ceramics, and profit can be made in this way
Obtain complex-shaped foamed ceramics product;Foaming method be mixed into the raw material for preparing the cruel foamed plastics of polyurethane second compared with
Many ceramic powders(It is well prepared in advance), foaming agent, catalyst and foam stabiliser etc. are added, is stirred, is allowed to
Generation foamable reaction and obtain foamed ceramics base substrate, this method can prepare complex-shaped foamed ceramics product, with meet
The application of some special occasions;Sol-gel processing be by foamed ceramics stock dispersion in a solvent, then by hydrolysis
Activated monomer is generated, activated monomer is polymerize, start to turn into colloidal sol, and then generate the gel with certain space structure, then
Foamed ceramics is made by drying and being heat-treated, this method is mainly used to prepare aperture in nano level micropore ceramics material;
Organic precursor proofing method refers to the organic precursor that will be handled well(Generally select polyurethane second vinegar foamed plastics)Soak people
It is repeated multiple times in ceramic slurry well prepared in advance, gas is excluded, slurry is fully infiltrated organic precursor, then will be unnecessary
Slurry is excluded, and is rolled repeatedly, so that slurry is uniformly attached on the twine in presoma network structure, then through drying and sintering system
Into foamed ceramics, this method optimizes inorganic binder system, strict control impregnating slurry technique mistake by controlling size performance
Journey, can prepare high performance foamed ceramics product.
Although the preparation technology of existing foamed ceramics is a lot, some foamed ceramicses of good performance are can be prepared by,
Be the foam ceramic material for preparing of existing these techniques there is also some problems, the foamed ceramics that mainly prepared by existing process
Universal density is high, intensity is relatively low, and base substrate is also easily collapsed in preparation process, causes foamed ceramics to use limited.Therefore,
How to prepare the foamed ceramics with low-density, high intensity and high yield rate is a problem rich in challenge meaning.
The content of the invention
The technical problems to be solved by the invention are:Relatively low for conventional foam ceramic material intensity, density is larger, and system
There is provided a kind of preparation method of foamed ceramics for the problem of base substrate is easily collapsed during standby.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
(1)300~500g rice husks are weighed, in autoclave, after insulation boiling, stands and drains away the water and naturally cool to room
Temperature, then size-reduced drying, obtain dry powdered rice hulls;
(2)Weigh after 100~150g dries powdered rice hulls, 0.6~0.8g nanometer iron powders, 10~15min of stirring mixing and be transferred to successively
Retort, the insulation reaction under argon gas guard mode treats that insulation reaction terminates, and stopping is passed through argon gas, under the conditions of air atmosphere
Oxidation reaction is incubated, reaction to be oxidized naturally cools to room temperature after terminating, and the material after oxidation reaction is poured into 300~
400mL mass fractions is in 3~5% hydrofluoric acid solutions, stirring are mixed after 10~15min, is filtered, washed and dried to constant weight, is obtained
Loose silicon carbide whisker;
(3)Weigh and sieved after 100~120g kaolin, 200~220g quartzs, 600~650g potassium feldspars, ball milling successively, obtained
Sintering aid powder;
(4)Count by weight, 100~150 parts of mass fractions sequentially added in batch mixer for 5~8% poly-vinyl alcohol solutions,
10~15 component sintering additive powder, 15~20 parts of loose silicon carbide whiskers, 80~120 parts of average grain diameters are 60~80 μm of oxidation
Aluminium powder, 3~5 parts of ammonium citrates, 2~4 parts of emulsifier op-10s, 3~5h of constant temperature stirring mixing;
(5)Treat that constant temperature stirring mixing terminates, material in batch mixer injected in mould, and by mould be placed in liquid nitrogen freezing 30~
40s, then the mould after freezing is taken out, in 4~6h of naturally to thaw under room temperature condition, such freezing, thaw cycles 3~5 times, and
Mould after final thaw is transferred in vacuum freezing drying oven, 2~4h of vacuum freeze drying, the demoulding obtains ceramic green, then pass through
Sintering, produces foamed ceramics.
Step(1)Described insulation conditions of cooking is:Boiling temperature is 120~140 DEG C, and digestion time is 45~60min.
Step(1)Before described insulation boiling, 10~15g sodium hydroxides can also be added into autoclave.
Step(2)0.3~0.5g sodium fluorides can also be added in described drying powdered rice hulls.
Step(2)The described insulation reaction condition under argon gas guard mode is:With 10~15mL/min speed into stove
Argon gas is passed through, under argon gas guard mode, 550~600 DEG C are warming up to 6~8 DEG C/min rate programs, insulation carbonizes 2~4h,
1400~1500 DEG C, 3~5h of insulation reaction are warming up to 10~15 DEG C/min rate programs again.
Step(2)The described oxidation reaction condition that is incubated in air atmosphere is:In-furnace temperature to be carbonized is naturally cooled to
700~750 DEG C, then be passed through with 10~15mL/min speed into above-mentioned retort after air, 2~4h of insulation oxidation reaction, from
So it is cooled to room temperature.
Step(3)Described sieving condition was 325~500 mesh sieves.
Step(4)Can also be added in described poly-vinyl alcohol solution poly-vinyl alcohol solution quality 6~8% chitosan and
The glutaraldehyde of poly-vinyl alcohol solution quality 0.3~0.5%.
The beneficial effects of the invention are as follows:
(1)The present invention is first using rice husk cheap and easy to get as silicon source, and autoclaving in the basic conditions makes rice hull cellulose tentatively solve
Fibre, makes rice husk short texture, is fully contacted beneficial to the catalyst with sodium fluoride and nanometer iron powder composition, with after under lower temperature
Organic matter in rice husk is carbonized, then coordinates the catalytic action of nanometer iron powder and sodium fluoride, carbonization is formed under higher temperature conditions
Silicon wafer palpus, enables the charing organic matter not reacted completely to remove using being calcined under the conditions of air atmosphere, coordinates hydrofluoric acid
Immersion, can remove unreacted silica, so that silicon carbide whisker is purified, in product foamed ceramics, because there is carbon
SiClx whisker is as the addition of reinforcement, the problem of base substrate collapses in preparation process so as to being prevented effectively from foamed ceramics;
(2)The present invention in high-speed agitating process, can make air equal in micro-bubble form by the addition of emulsifier op-10
Even to be distributed in material, in refrigerating process, part water forms tiny ice crystal, then makes ice crystal distillation row through vacuum freeze drying
Go out, the pore structure of oriented alignment is formed in ceramic body, reduces product density, while using freeze-thaw circulation, making
Polyvinyl alcohol, chitosan and glutaraldehyde crosslink solidification, and the three-dimensional net structure of formation further can avoid blank structure from collapsing
Fall into, improve the intensity of foamed ceramics product.
Embodiment
300~500g rice husks are weighed first, and 10~15g sodium hydroxides pour into the high pressure steaming for filling 1000~1200mL water
In pot, under the conditions of temperature is 120~140 DEG C, 45~60min of boiling is incubated, then by material filtering in autoclave, obtain boiling
Rice husk, standing drains away the water and naturally cools to room temperature, then the rice husk after cooling is transferred in freezing crusher crush 10~
20min, and the rice husk after crushing is transferred in baking oven, dried under the conditions of temperature is 105~110 DEG C to constant weight, obtain drying of rice
Shell powder, then weighs and powdered rice hulls is dried obtained by 100~150g successively, and 0.3~0.5g sodium fluorides, 0.6~0.8g nanometer iron powders fall
Enter in crucible, after 10~15min of glass bar stirring mixing, crucible is transferred to retort, with 10~15mL/min speed to stove
Argon gas is inside passed through, under argon gas guard mode, 550~600 DEG C are warming up to 6~8 DEG C/min rate programs, insulation charing 2~
4h, then 1400~1500 DEG C are warming up to 10~15 DEG C/min rate programs, 3~5h of insulation reaction treats that insulation reaction terminates, stopped
Argon gas is only passed through, and naturally cools to 700~750 DEG C, then air is passed through into retort with 10~15mL/min speed, is incubated
2~4h of oxidation reaction, after naturally cool to room temperature, the material after oxidation reaction is poured into and fills 300~400mL mass fractions and is
In the plastic beaker of 3~5% hydrofluoric acid solutions, after 10~15min of waddy stirring mixing, material filtering in plastic beaker is obtained
Filter cake, and filter cake is washed with deionized until the filter cake after washing then is transferred in baking oven by cleaning solution in neutrality, it is in temperature
Dried under the conditions of 105~110 DEG C to constant weight, obtain loose silicon carbide whisker, then weigh 100~120g kaolin successively, 200~
220g quartzs, 600~650g potassium feldspars, are poured into ball mill, are 10 by ball material mass ratio:1~20:1 adds zirconia ball
Grind and 325~500 mesh sieves are crossed after pearl, 24~36h of ball-milling treatment, ball milling, obtain sintering aid powder, then count by weight, mixed
100~150 parts of mass fractions are sequentially added in material machine for 5~8% poly-vinyl alcohol solutions, 10~15 parts of gained sintering aid powder,
15~20 parts of loose silicon carbide whiskers, 80~120 parts of average grain diameters are 60~80 μm of alumina powder, 3~5 parts of ammonium citrates, 2
~4 parts of emulsifier op-10s, the chitosan of poly-vinyl alcohol solution quality 6~8% and the penta of poly-vinyl alcohol solution quality 0.3~0.5%
Dialdehyde, is 45~55 DEG C in temperature, rotating speed is under the conditions of 600~800r/min, constant temperature stirring 3~5h of mixing treats that constant temperature is stirred
Mixing terminates, and material in batch mixer is injected in mould, and mould is placed in into 30~40s of freezing in liquid nitrogen, then by after freezing
Mould takes out, in 4~6h of naturally to thaw under room temperature condition, so freezing, thaw cycles 3~5 times, and by the mould after final thaw
Tool is transferred in vacuum freezing drying oven, 2~4h of vacuum freeze drying, the demoulding, obtains ceramic green, finally turns gained ceramic green
Enter sintering furnace, under the conditions of temperature is 1450~1500 DEG C, sinter 2~3h, cool to room temperature with the furnace, discharge, produce foam pottery
Porcelain.
Example 1
300g rice husks are weighed first, are poured into the autoclave for filling 1000mL water, and under the conditions of temperature is 120 DEG C, insulation is steamed
45min is boiled, then by material filtering in autoclave, obtains boiling rice husk, standing drains away the water and naturally cools to room temperature, then will be cold
But the rice husk after, which is transferred in freezing crusher, crushes 10min, and the rice husk after crushing is transferred in baking oven, in temperature be 105 DEG C
Under the conditions of dry to constant weight, obtain dry powdered rice hulls, then weigh successively and powdered rice hulls are dried obtained by 100g, 0.6g nanometer iron powders fall
Enter in crucible, after glass bar stirring mixing 10min, crucible is transferred to retort, argon is passed through into stove with 10mL/min speed
Gas, under argon gas guard mode, is warming up to 550 DEG C, insulation carbonizes 2h with 6 DEG C/min rate programs, then with 10 DEG C/min speed
Temperature programming is to 1400 DEG C, and insulation reaction 3h treats that insulation reaction terminates, and stopping is passed through argon gas, and naturally cools to 700 DEG C, then
Air is passed through into retort with 10mL/min speed, oxidation reaction 2h is incubated, after naturally cool to room temperature, after oxidation reaction
Material pour into fill 300mL mass fractions be 3% hydrofluoric acid solution plastic beaker in, with waddy stirring mixing 10min after,
By material filtering in plastic beaker, filter cake is obtained, and filter cake is washed with deionized until cleaning solution is in neutrality, then by after washing
Filter cake is transferred in baking oven, is dried under the conditions of temperature is 105 DEG C to constant weight, is obtained loose silicon carbide whisker, then weigh 100g successively
Kaolin, 200g quartzs, 600g potassium feldspars are poured into ball mill, are 10 by ball material mass ratio:1 adds zirconium oxide ball milling pearl,
325 mesh sieves are crossed after ball-milling treatment 24h, ball milling, sintering aid powder is obtained, then counted by weight, are sequentially added in batch mixer
100 parts of mass fractions are 5% poly-vinyl alcohol solution, 10 parts of gained sintering aid powder, 15 parts of loose silicon carbide whiskers, and 80 parts are put down
Equal particle diameter is 60 μm of alumina powder, 3 parts of ammonium citrates and 2 parts of emulsifier op-10s, is 45 DEG C in temperature, rotating speed is 600r/
Under the conditions of min, constant temperature stirring mixing 3h treats that constant temperature stirring mixing terminates, material in batch mixer is injected in mould, and by mould
It is placed in liquid nitrogen and freezes 30s, then the mould after freezing is taken out, in naturally to thaw 4h under room temperature condition, so freezing, defrosting is followed
Ring 3 times, and the mould after final thaw is transferred in vacuum freezing drying oven, vacuum freeze drying 2h, the demoulding obtains ceramic green
Base, is finally transferred to sintering furnace by gained ceramic green, under the conditions of temperature is 1450 DEG C, sinters 2h, cools to room temperature with the furnace, go out
Material, produces foamed ceramics.
Example 2
400g rice husks are weighed first, are poured into the autoclave for filling 1100mL water, and under the conditions of temperature is 130 DEG C, insulation is steamed
53min is boiled, then by material filtering in autoclave, obtains boiling rice husk, standing drains away the water and naturally cools to room temperature, then will be cold
But the rice husk after, which is transferred in freezing crusher, crushes 15min, and the rice husk after crushing is transferred in baking oven, in temperature be 108 DEG C
Under the conditions of dry to constant weight, obtain dry powdered rice hulls, then weigh successively and powdered rice hulls are dried obtained by 125g, 0.7g nanometer iron powders fall
Enter in crucible, after glass bar stirring mixing 13min, crucible is transferred to retort, argon is passed through into stove with 13mL/min speed
Gas, under argon gas guard mode, is warming up to 575 DEG C, insulation carbonizes 3h with 7 DEG C/min rate programs, then with 13 DEG C/min speed
Temperature programming is to 1450 DEG C, and insulation reaction 4h treats that insulation reaction terminates, and stopping is passed through argon gas, and naturally cools to 725 DEG C, then
Air is passed through into retort with 13mL/min speed, oxidation reaction 3h is incubated, after naturally cool to room temperature, after oxidation reaction
Material pour into fill 350mL mass fractions be 4% hydrofluoric acid solution plastic beaker in, with waddy stirring mixing 13min after,
By material filtering in plastic beaker, filter cake is obtained, and filter cake is washed with deionized until cleaning solution is in neutrality, then by after washing
Filter cake is transferred in baking oven, is dried under the conditions of temperature is 108 DEG C to constant weight, is obtained loose silicon carbide whisker, then weigh 110g successively
Kaolin, 210g quartzs, 625g potassium feldspars are poured into ball mill, are 15 by ball material mass ratio:1 adds zirconium oxide ball milling pearl,
410 mesh sieves are crossed after ball-milling treatment 30h, ball milling, sintering aid powder is obtained, then counted by weight, are sequentially added in batch mixer
125 parts of mass fractions are 7% poly-vinyl alcohol solution, 13 parts of gained sintering aid powder, 18 parts of loose silicon carbide whiskers, and 100 parts are put down
Equal particle diameter is 70 μm of alumina powder, 4 parts of ammonium citrates and 3 parts of emulsifier op-10s, is 50 DEG C in temperature, rotating speed is 700r/
Under the conditions of min, constant temperature stirring mixing 4h treats that constant temperature stirring mixing terminates, material in batch mixer is injected in mould, and by mould
It is placed in liquid nitrogen and freezes 35s, then the mould after freezing is taken out, in naturally to thaw 56h under room temperature condition, so freezing, defrosting
Circulation 4 times, and the mould after final thaw is transferred in vacuum freezing drying oven, vacuum freeze drying 3h, the demoulding obtains ceramic green
Base, is finally transferred to sintering furnace by gained ceramic green, under the conditions of temperature is 1475 DEG C, sinters 2h, cools to room temperature with the furnace, go out
Material, produces foamed ceramics.
Example 3
Weigh 500g rice husks first, 15g sodium hydroxides are poured into the autoclave for filling 1200mL water, in temperature be 140 DEG C of bars
Under part, boiling 60min is incubated, then by material filtering in autoclave, obtains boiling rice husk, standing drains away the water and naturally cooled to
Room temperature, then the rice husk after cooling is transferred in freezing crusher crushes 20min, and the rice husk after crushing is transferred in baking oven, in
Temperature obtains dry powdered rice hulls to be dried under the conditions of 110 DEG C to constant weight, then weighs successively and powdered rice hulls, 0.5g are dried obtained by 150g
Sodium fluoride, 0.8g nanometer iron powders, is poured into crucible, and after glass bar stirring mixing 15min, crucible is transferred into retort, with
15mL/min speed is passed through argon gas into stove, under argon gas guard mode, and 600 DEG C, insulation are warming up to 8 DEG C/min rate programs
4h is carbonized, then 1500 DEG C are warming up to 15 DEG C/min rate programs, insulation reaction 5h treats that insulation reaction terminates, stopping is passed through argon
Gas, and 750 DEG C are naturally cooled to, then air is passed through into retort with 15mL/min speed, oxidation reaction 4h is incubated, nature is treated
Room temperature is cooled to, the material after oxidation reaction is poured into and filled in the plastic beaker that 400mL mass fractions are 5% hydrofluoric acid solution,
After waddy stirring mixing 15min, by material filtering in plastic beaker, filter cake is obtained, and filter cake is washed with deionized until washing
Liquid is washed in neutrality, then the filter cake after washing is transferred in baking oven, is dried under the conditions of temperature is 110 DEG C to constant weight, obtains loose carbon
SiClx whisker, then 120g kaolin is weighed successively, 220g quartzs, 650g potassium feldspars are poured into ball mill, by ball material mass ratio
For 20:500 mesh sieves are crossed after 1 addition zirconium oxide ball milling pearl, ball-milling treatment 36h, ball milling, sintering aid powder is obtained, then by weight
Number meter, sequentially adds 150 parts of mass fractions for 8% poly-vinyl alcohol solution in batch mixer, 15 parts of gained sintering aid powder, 20
The loose silicon carbide whisker of part, 120 parts of average grain diameters are 80 μm of alumina powder, and 5 parts of ammonium citrates, 4 parts of emulsifier op-10s gather
The chitosan of glycohol solution quality 8% and the glutaraldehyde of poly-vinyl alcohol solution quality 0.5%, are 55 DEG C in temperature, rotating speed is
Under the conditions of 800r/min, constant temperature stirring mixing 5h treats that constant temperature stirring mixing terminates, material in batch mixer is injected in mould, and
Mould is placed in liquid nitrogen and freezes 40s, then the mould after freezing is taken out, in naturally to thaw 6h under room temperature condition, so freeze,
Thaw cycles 5 times, and the mould after final thaw is transferred in vacuum freezing drying oven, vacuum freeze drying 4h, the demoulding must make pottery
Porcelain green compact, are finally transferred to sintering furnace by gained ceramic green, under the conditions of temperature is 1500 DEG C, sinter 3h, cool to room with the furnace
Temperature, discharging, produces foamed ceramics.
To foamed ceramics made from example 1~3 and commercially available unlike material(Cordierite, aluminum oxide)Foamed ceramics carries out performance
Test, its testing result such as following table:
Above-described embodiment is not limited for the present invention preferably embodiment, but embodiments of the present invention by above-described embodiment
System, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of foamed ceramics, it is characterised in that specifically preparation process is:
(1)300~500g rice husks are weighed, in autoclave, after insulation boiling, stands and drains away the water and naturally cool to room
Temperature, then size-reduced drying, obtain dry powdered rice hulls;
(2)Weigh after 100~150g dries powdered rice hulls, 0.6~0.8g nanometer iron powders, 10~15min of stirring mixing and be transferred to successively
Retort, the insulation reaction under argon gas guard mode treats that insulation reaction terminates, and stopping is passed through argon gas, under the conditions of air atmosphere
Oxidation reaction is incubated, reaction to be oxidized naturally cools to room temperature after terminating, and the material after oxidation reaction is poured into 300~
400mL mass fractions is in 3~5% hydrofluoric acid solutions, stirring are mixed after 10~15min, is filtered, washed and dried to constant weight, is obtained
Loose silicon carbide whisker;
(3)Weigh and sieved after 100~120g kaolin, 200~220g quartzs, 600~650g potassium feldspars, ball milling successively, obtained
Sintering aid powder;
(4)Count by weight, 100~150 parts of mass fractions sequentially added in batch mixer for 5~8% poly-vinyl alcohol solutions,
10~15 component sintering additive powder, 15~20 parts of loose silicon carbide whiskers, 80~120 parts of average grain diameters are 60~80 μm of oxidation
Aluminium powder, 3~5 parts of ammonium citrates, 2~4 parts of emulsifier op-10s, 3~5h of constant temperature stirring mixing;
(5)Treat that constant temperature stirring mixing terminates, material in batch mixer injected in mould, and by mould be placed in liquid nitrogen freezing 30~
40s, then the mould after freezing is taken out, in 4~6h of naturally to thaw under room temperature condition, such freezing, thaw cycles 3~5 times, and
Mould after final thaw is transferred in vacuum freezing drying oven, 2~4h of vacuum freeze drying, the demoulding obtains ceramic green, then pass through
Sintering, produces foamed ceramics.
2. a kind of preparation method of foamed ceramics according to claim 1, it is characterised in that step(1)Described insulation is steamed
The condition of boiling is:Boiling temperature is 120~140 DEG C, and digestion time is 45~60min.
3. a kind of preparation method of foamed ceramics according to claim 1, it is characterised in that:Step(1)Described insulation
Before boiling, 10~15g sodium hydroxides can also be added into autoclave.
4. a kind of preparation method of foamed ceramics according to claim 1, it is characterised in that:Step(2)Described drying
0.3~0.5g sodium fluorides can also be added in powdered rice hulls.
5. a kind of preparation method of foamed ceramics according to claim 1, it is characterised in that:Step(2)It is described in argon
Insulation reaction condition is under gas shielded state:Argon gas is passed through into stove with 10~15mL/min speed, under argon gas guard mode,
550~600 DEG C are warming up to 6~8 DEG C/min rate programs, insulation carbonizes 2~4h, then with 10~15 DEG C/min rate program liters
Temperature is to 1400~1500 DEG C, 3~5h of insulation reaction.
6. a kind of preparation method of foamed ceramics according to claim 1, it is characterised in that:Step(2)It is described in sky
Oxidation reaction condition is incubated in gas atmosphere is:In-furnace temperature to be carbonized naturally cools to 700~750 DEG C, then with 10~15mL/
Min speed is passed through into above-mentioned retort after air, 2~4h of insulation oxidation reaction, naturally cools to room temperature.
7. a kind of preparation method of foamed ceramics according to claim 1, it is characterised in that:Step(3)Described sieving
Condition was 325~500 mesh sieves.
8. a kind of preparation method of foamed ceramics according to claim 1, it is characterised in that:Step(4)Described poly- second
The chitosan and poly-vinyl alcohol solution quality 0.3~0.5% of poly-vinyl alcohol solution quality 6~8% can also be added in enolate solution
Glutaraldehyde.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102010226A (en) * | 2010-12-09 | 2011-04-13 | 东北大学 | Macroporous SiC ceramic preparation method |
CN106007763A (en) * | 2016-05-27 | 2016-10-12 | 海南中航特玻科技有限公司 | Method for preparing mullite honeycomb ceramic carrier with all crystal whisker structure |
-
2017
- 2017-05-14 CN CN201710337097.9A patent/CN107162629A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102010226A (en) * | 2010-12-09 | 2011-04-13 | 东北大学 | Macroporous SiC ceramic preparation method |
CN106007763A (en) * | 2016-05-27 | 2016-10-12 | 海南中航特玻科技有限公司 | Method for preparing mullite honeycomb ceramic carrier with all crystal whisker structure |
Non-Patent Citations (1)
Title |
---|
谢定方: "N2气氛中稻壳碳与二氧化硅合成SiC晶须的研究", 《N2气氛中稻壳碳与二氧化硅合成SIC晶须的研究》 * |
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