CN107344855A - A kind of multistage hole foamed ceramics of the microballoon containing porous graphene and preparation method thereof - Google Patents

A kind of multistage hole foamed ceramics of the microballoon containing porous graphene and preparation method thereof Download PDF

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CN107344855A
CN107344855A CN201710612342.2A CN201710612342A CN107344855A CN 107344855 A CN107344855 A CN 107344855A CN 201710612342 A CN201710612342 A CN 201710612342A CN 107344855 A CN107344855 A CN 107344855A
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microballoon
foamed ceramics
porous graphene
graphene
multistage hole
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陈东进
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Dongguan Lianzhou Intellectual Property Operation and Management Co Ltd
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Dongguan Lianzhou Intellectual Property Operation and Management Co Ltd
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Abstract

The present invention provides a kind of multistage hole foamed ceramics of the microballoon containing porous graphene and preparation method thereof, the multistage hole foamed ceramics of the microballoon containing porous graphene is the hole that foamed ceramics is attached to containing micropore, mesoporous and macropore multistage hole graphene microballoon, and preparation method is:Ceramic powder hydrophobization dressing agent will be added in ceramic slurry and polyvinyl alcohol, high speed machine stir to obtain particle stabilized foam, particle stabilized foam are placed under low temperature environment at once and solidified, take out and thaw, the foamed ceramics base substrate solidified;Graphene oxide/polyvinyl alcohol solution is added dropwise in liquid nitrogen and solidified, crystallization microballoon is formed, takes out and thaw, the graphene oxide microballoon solidified;The foamed ceramics base substrate of solidification is impregnated into the cross-linking agent solution of the graphene oxide microballoon containing solidification, low-speed oscillation, take out, vacuum freeze drying, the multistage hole foamed ceramics of mechanical performance, absorption property and the high microballoon containing porous graphene of porosity is obtained after sintering cooling.

Description

A kind of multistage hole foamed ceramics of the microballoon containing porous graphene and preparation method thereof
Technical field
The invention belongs to foam technology field, and in particular to a kind of multistage celled foams of microballoon containing porous graphene Ceramics and preparation method thereof.
Background technology
Graphene is a kind of flat film of hexagonal honeycomb lattice, the two-dimensional material of only one carbon atom thickness, is Other zero dimension fullerenes, one-dimensional CNT, the base unit of three-dimensional graphite Qiu Alto carbonaceous materials are built, grapheme material has Peculiar electricity, optics, mechanics and thermal property.Foamed ceramics is that have three as the porous ceramics of foam-like in a kind of moulding Connected pore channel is tieed up, the porous material that shape, size, permeability, the surface area agent chemical property in duct can moderately regulate and control, there is weight Amount is light, intensity height, high temperature resistant, corrosion-resistant, regeneration simply, service life is long and the advantages that good filtering adsorptivity.Therefore, stone The composite property that black alkene material is combined preparation with foamed ceramics protrudes, and has researching value.
Graphene/porous ceramics composite conducting material and preparation method thereof disclosed in Chinese patent CN 103219061B, will The ceramic powder of silica, alundum (Al2O3), aluminium nitride, carborundum, zirconium oxide and boron nitride that particle size differs is with gathering The binding agents such as vinyl alcohol are blended and grinding, drying forming, high annealing, porous ceramic bases are obtained, finally by chemical gas Phase deposition process, in porous ceramic bases surface direct growth graphene, obtain graphene/porous ceramics composite conducting material Material, composite conducting material prepared by this method conduct electricity very well, and stable mechanical property, can be applied to photovoltaic, conductive material, radiating In device.Graphene-porous ceramics composite adsorbing material and preparation method thereof disclosed in Chinese patent CN 104475019B is with answering With porous ceramic matrices suitable is impregnated in citric acid, sucrose, fructose, glucose, honey or milk soln, then passes through height The mixture sintering of porous ceramic matrices suitable area load is converted to graphene by temperature sintering, and it is compound to obtain graphene-porous ceramics Sorbing material, the cost of composite adsorbing material prepared by this method is cheap, and preparation method is simple, is led after loading graphene in sewage There is good application in domain, it is not protected from environmental, it is recycled.From above-mentioned prior art, graphene and porous ceramics system Standby composite has itself exclusive advantage in conductive field and adsorbing domain, applicant of the present invention on this basis, Optimize the structure and combination of graphene and porous ceramics, make every effort to further improve its combination property.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of multistage hole foamed ceramics of microballoon containing porous graphene and Its preparation method, will add ceramic powder hydrophobization dressing agent and polyvinyl alcohol in ceramic slurry, high speed machine stirs to obtain Grain stable foam, is placed under low temperature environment and solidifies at once, takes out and thaws, the foamed ceramics base substrate solidified, by graphite oxide Alkene/poly-vinyl alcohol solution is placed under low temperature environment and solidified through being formed by curing crystallization microballoon in liquid nitrogen at once, takes out and thaws, obtains The graphene oxide microballoon of solidification;After both crosslinked dose of crosslinkings, vacuum freeze drying, obtain containing porous stone after sintering cooling The multistage hole foamed ceramics of black alkene microballoon.Foamed ceramics prepared by the present invention contains micropore, the multistage hole of mesoporous and macropore, Grain is attached to hole surface, and porosity is high, and mechanical property and electric conductivity are excellent, and suitable application area is extensive.
In order to solve the above technical problems, the technical scheme is that:
A kind of multistage hole foamed ceramics of microballoon containing porous graphene, the multistage hole of the microballoon containing porous graphene Foamed ceramics includes foamed ceramics and porous graphene microballoon, and the porous graphene microballoon is attached to the hole of foamed ceramics In, micropore, the multistage hole of mesoporous and macropore, the multistage of the microballoon containing porous graphene are contained in the porous graphene microballoon The pore space structure of celled foams ceramics is to form micro-crystallization using polyvinyl alcohol freeze-thaw to form.
The present invention also provides a kind of preparation method of the multistage hole foamed ceramics of microballoon containing porous graphene, including following Step:
(1) ceramic powder hydrophobization dressing agent and polyvinyl alcohol will be added in ceramic slurry, regulation pH value to faintly acid is high Fast mechanical agitation obtains particle stabilized foam, and particle stabilized foam is placed under low temperature environment at once and solidifies 12-24h, takes out, Thaw 3-12h in the range of 0-10 DEG C, the foamed ceramics base substrate solidified;
(2) graphene oxide solution is added in poly-vinyl alcohol solution, is well mixed, is added dropwise in liquid nitrogen and solidifies, shape Into crystallization microballoon, take out, thaw 3-12h in the range of 0-10 DEG C, the graphene oxide microballoon solidified;
(3) the graphene oxide microballoon of solidification is added in cross-linking agent solution and be well mixed, then prepare step (1) Solidification foamed ceramics base substrate dipping wherein, low-speed oscillation, take out, vacuum freeze drying, obtain microballoon containing graphene oxide Foamed ceramics base substrate;
(4) the foamed ceramics base substrate for the microballoon containing graphene oxide for preparing step (3) is 1400-1900 in sintering temperature Sintered at DEG C, the multistage hole foamed ceramics of the microballoon containing porous graphene is obtained after cooling.
As the preferred of above-mentioned technical proposal, in the step (1), the raw material of ceramic slurry is silicon nitride or carbonization Silicon, the mass fraction of ceramic powders is 15-60% in ceramic slurry.
As the preferred of above-mentioned technical proposal, in the step (1), ceramic powder hydrophobization dressing agent is dodecyl chloride Change ammonium or cetyl chloride ammonium.
As the preferred of above-mentioned technical proposal, in the step (1), ceramic powder hydrophobization dressing agent accounts for ceramic slurry Mass fraction is 0.01-0.5wt%, and the mass fraction that polyvinyl alcohol accounts for ceramic slurry is 0.01-0.5wt%.
As the preferred of above-mentioned technical proposal, in the step (2), the concentration of graphene oxide in graphene oxide solution For 10-30mg/g, the mass fraction of polyvinyl alcohol is 1-4wt% in poly-vinyl alcohol solution.
As the preferred of above-mentioned technical proposal, in the step (2), the method for dropwise addition instills for syringe needle, solidification Time is 5-10min.
As the preferred of above-mentioned technical proposal, in the step (3), cross-linking agent solution is 1-3wt% glutaraldehyde solution.
As the preferred of above-mentioned technical proposal, in the step (3), graphene oxide microballoon, crosslinking agent and foamed ceramics Green body quality ratio is 10:0.5-0.8:100-150.
As the preferred of above-mentioned technical proposal, in the step (3), the vacuum of vacuum freeze drying is 5-10Pa, temperature Spend for-10-50 DEG C, time 12-36h.
Compared with prior art, the invention has the advantages that:
(1) graphene, graphene are contained in the multistage hole foamed ceramics of the microballoon containing porous graphene prepared by the present invention Reduce to obtain by graphene oxide, graphene oxide is roughly the same with the molecular structure of graphene, better than the effect of oxidant, carbon Ined succession on atomic scale many oxygen-content active groups, such as carboxyl, hydroxyl, epoxy radicals and carbonyl, the ratio surface of graphene oxide Product is larger, has higher hydrophily, mechanicalness and stability, therefore polyvinyl alcohol polymer molecule is easy to inlay rear oxidation In graphene deck structure, linked together in the form of covalent bond, form composite, then do by low-temperature setting and vacuum It is dry, polyvinyl alcohol is crystallized, separated with graphene oxide, makes the graphene oxide ball of preparation have multi-stage pore structure.
(2) foamed ceramics is with ceramic powder in the multistage hole foamed ceramics of the microballoon containing porous graphene prepared by the present invention End is raw material, and using hydrophobic modification agent and polyvinyl alcohol as auxiliary material, both are mixed into hair by high shear agitation technique Bubble, the presence of auxiliary material have beneficial to the stability for improving frothing foam, then by low-temperature setting and vacuum drying, by polyethylene Alcohol crystallizes, and is separated with porous ceramics, makes the porous ceramics of preparation have multi-stage pore structure.
(3) in the multistage hole foamed ceramics of the microballoon containing porous graphene prepared by the present invention foamed ceramics by will oxidation After graphene/polymer microballoon and polymer/porous ceramics base substrate are by cross-linking agents, then vacuum freeze drying is carried out, gone Except polyvinyl alcohol polymer, the technique that freeze-drying respectively removes polymer is eliminated, and regulation and control graphene oxide can be unified The pore space structure of microballoon and foamed ceramics base substrate, then unify to sinter through Overheating Treatment, graphene oxide is reduced into graphene, will Foamed ceramics blank sintering is foamed ceramics, and both are handled simultaneously, has deepened the infiltration between both materials, graphene and ceramics Between foam combine it is even closer, make the composite property more stable uniform of preparation.
(4) preparation method of the invention will freeze solidification, Freeze Drying Technique is combined with heat treatment technics, utilize two kinds The performance intercommunity of material, preparation technology controllability is strong, and the composite of preparation has micropore, mesoporous and macropore multi-stage porous Hole, and part is arranged radially, and is advantageous to improve absorption property, electric property and the separating property of composite, it is applicable In multiple fields.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment, herein illustrative examples and explanation of the invention For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1:
(1) it is addition lauryl ammonium chloride ceramic powder hydrophobization in 15% silicon nitride ceramics slurry by mass fraction Dressing agent and polyvinyl alcohol, wherein, the mass fraction that ceramic powder hydrophobization dressing agent accounts for ceramic slurry is 0.01wt%, poly- second The mass fraction that enol accounts for ceramic slurry is 0.01wt%, and regulation pH value is stirred to 4.5 in 2000r/min speed high speed machine Mix to obtain particle stabilized foam, particle stabilized foam is placed under low temperature environment at once and solidifies 12h, take out, in the range of 0 DEG C Defrosting 3h, the foamed ceramics base substrate solidified.
(2) 10mg/g graphene oxide solution is added in 1wt% poly-vinyl alcohol solution, is well mixed to be formed and mixes Solution is closed, mixed solution is instilled in liquid nitrogen through syringe needle and solidifies 5min, crystallization microballoon is formed, takes out, in the range of 0 DEG C Defrosting 3h, the graphene oxide microballoon solidified.
(3) it is 10 according to graphene oxide microballoon, crosslinking agent and foamed ceramics green body quality ratio:0.5:100, by solidification Graphene oxide microballoon is added in 1wt% glutaraldehyde solution and is well mixed, and then impregnates the foamed ceramics base substrate of solidification Wherein, low-speed oscillation 20min, take out, the vacuum freeze drying 12h in the case where vacuum is 5Pa and -10 DEG C, obtain containing graphite oxide The foamed ceramics base substrate of alkene microballoon.
(4) the foamed ceramics base substrate of the microballoon containing graphene oxide is warming up to 1400 DEG C with 3 DEG C/min speed, sintering 6h, the multistage hole foamed ceramics of the microballoon containing porous graphene is obtained after cooling.
Embodiment 2:
(1) it is addition cetyl chloride ammonium ceramic powder hydrophobization in 60% silicon carbide ceramics slurry by mass fraction Dressing agent and polyvinyl alcohol, wherein, the mass fraction that ceramic powder hydrophobization dressing agent accounts for ceramic slurry is 0.5wt%, poly- second The mass fraction that enol accounts for ceramic slurry is 0.5wt%, regulation pH value to 6.5, is stirred in 2500r/min speed high speed machine Particle stabilized foam is obtained, particle stabilized foam is placed under low temperature environment at once and solidifies 24h, is taken out, in the range of 10 DEG C Defrosting 12h, the foamed ceramics base substrate solidified.
(2) 30mg/g graphene oxide solution is added in 4wt% poly-vinyl alcohol solution, is well mixed to be formed and mixes Solution is closed, mixed solution is instilled in liquid nitrogen through syringe needle and solidifies 10min, crystallization microballoon is formed, takes out, in 10 DEG C of scopes Interior defrosting 12h, the graphene oxide microballoon solidified.
(3) it is 10 according to graphene oxide microballoon, crosslinking agent and foamed ceramics green body quality ratio:0.8:150, by solidification Graphene oxide microballoon is added in 3wt% glutaraldehyde solution and is well mixed, and then impregnates the foamed ceramics base substrate of solidification Wherein, low-speed oscillation 30min, take out, the vacuum freeze drying 36h in the case where vacuum is 10Pa and -50 DEG C, obtain containing graphite oxide The foamed ceramics base substrate of alkene microballoon.
(4) the foamed ceramics base substrate of the microballoon containing graphene oxide is warming up to 1900 DEG C with 5 DEG C/min speed, sintering 12h, the multistage hole foamed ceramics of the microballoon containing porous graphene is obtained after cooling.
Embodiment 3:
(1) it is addition cetyl chloride ammonium ceramic powder hydrophobization in 45% silicon nitride ceramics slurry by mass fraction Dressing agent and polyvinyl alcohol, wherein, the mass fraction that ceramic powder hydrophobization dressing agent accounts for ceramic slurry is 0.05wt%, poly- second The mass fraction that enol accounts for ceramic slurry is 0.2wt%, and regulation pH value stirs to 5 in 2200r/min speed high speed machine To particle stabilized foam, particle stabilized foam is placed under low temperature environment at once and solidifies 16h, taken out, thawed in the range of 5 DEG C 6h, the foamed ceramics base substrate solidified.
(2) 20mg/g graphene oxide solution is added in 2wt% poly-vinyl alcohol solution, is well mixed to be formed and mixes Solution is closed, mixed solution is instilled in liquid nitrogen through syringe needle and solidifies 6min, crystallization microballoon is formed, takes out, in the range of 6 DEG C Defrosting 6h, the graphene oxide microballoon solidified.
(3) it is 10 according to graphene oxide microballoon, crosslinking agent and foamed ceramics green body quality ratio:0.6:120, by solidification Graphene oxide microballoon is added in 1.5wt% glutaraldehyde solution and is well mixed, and then soaks the foamed ceramics base substrate of solidification Stain wherein, low-speed oscillation 25min, is taken out, and the vacuum freeze drying 24h in the case where vacuum is 6Pa and -20 DEG C, obtains oxygen-containing fossil The foamed ceramics base substrate of black alkene microballoon.
(4) the foamed ceramics base substrate of the microballoon containing graphene oxide is warming up to 1500 DEG C with 4 DEG C/min speed, sintering 8h, the multistage hole foamed ceramics of the microballoon containing porous graphene is obtained after cooling.
Embodiment 4:
(1) it is addition cetyl chloride ammonium ceramic powder hydrophobization in 25% silicon carbide ceramics slurry by mass fraction Dressing agent and polyvinyl alcohol, wherein, the mass fraction that ceramic powder hydrophobization dressing agent accounts for ceramic slurry is 0.3wt%, poly- second The mass fraction that enol accounts for ceramic slurry is 0.4wt%, and regulation pH value stirs to 5 in 2000r/min speed high speed machine To particle stabilized foam, particle stabilized foam is placed under low temperature environment at once and solidifies 16h, taken out, thawed in the range of 5 DEG C 5h, the foamed ceramics base substrate solidified.
(2) 15mg/g graphene oxide solution is added in 2.5wt% poly-vinyl alcohol solution, is well mixed and is formed Mixed solution, mixed solution is instilled in liquid nitrogen through syringe needle and solidifies 8min, formed crystallization microballoon, take out, in 4 DEG C of scopes Interior defrosting 10h, the graphene oxide microballoon solidified.
(3) it is 10 according to graphene oxide microballoon, crosslinking agent and foamed ceramics green body quality ratio:0.7:140, by solidification Graphene oxide microballoon is added in 2.5wt% glutaraldehyde solution and is well mixed, and then soaks the foamed ceramics base substrate of solidification Stain wherein, low-speed oscillation 25min, is taken out, and the vacuum freeze drying 12h in the case where vacuum is 6Pa and -40 DEG C, obtains oxygen-containing fossil The foamed ceramics base substrate of black alkene microballoon.
(4) the foamed ceramics base substrate of the microballoon containing graphene oxide is warming up to 1600 DEG C with 3.5 DEG C/min speed, sintering 10h, the multistage hole foamed ceramics of the microballoon containing porous graphene is obtained after cooling.
Embodiment 5:
(1) it is addition cetyl chloride ammonium ceramic powder hydrophobization in 45% silicon nitride ceramics slurry by mass fraction Dressing agent and polyvinyl alcohol, wherein, the mass fraction that ceramic powder hydrophobization dressing agent accounts for ceramic slurry is 0.25wt%, poly- second The mass fraction that enol accounts for ceramic slurry is 0.25wt%, and regulation pH value is stirred to 5.5 in 2500r/min speed high speed machine Mix to obtain particle stabilized foam, particle stabilized foam is placed under low temperature environment at once and solidifies 20h, take out, in 10 DEG C of scopes Interior defrosting 6h, the foamed ceramics base substrate solidified.
(2) 25mg/g graphene oxide solution is added in 3.5wt% poly-vinyl alcohol solution, is well mixed and is formed Mixed solution, mixed solution is instilled in liquid nitrogen through syringe needle and solidifies 7min, formed crystallization microballoon, take out, in 5 DEG C of scopes Interior defrosting 7h, the graphene oxide microballoon solidified.
(3) it is 10 according to graphene oxide microballoon, crosslinking agent and foamed ceramics green body quality ratio:0.7:130, by solidification Graphene oxide microballoon is added in 2.5wt% glutaraldehyde solution and is well mixed, and then soaks the foamed ceramics base substrate of solidification Stain wherein, low-speed oscillation 25min, is taken out, and the vacuum freeze drying 24h in the case where vacuum is 7Pa and -30 DEG C, obtains oxygen-containing fossil The foamed ceramics base substrate of black alkene microballoon.
(4) the foamed ceramics base substrate of the microballoon containing graphene oxide is warming up to 1600 DEG C with 3.5 DEG C/min speed, sintering 8h, the multistage hole foamed ceramics of the microballoon containing porous graphene is obtained after cooling.
Embodiment 6:
(1) it is addition cetyl chloride ammonium ceramic powder hydrophobization in 45% silicon nitride ceramics slurry by mass fraction Dressing agent and polyvinyl alcohol, wherein, the mass fraction that ceramic powder hydrophobization dressing agent accounts for ceramic slurry is 0.5wt%, poly- second The mass fraction that enol accounts for ceramic slurry is 0.3wt%, and regulation pH value stirs to 5 in 2000r/min speed high speed machine To particle stabilized foam, particle stabilized foam is placed under low temperature environment at once and solidifies 24h, taken out, thawed in the range of 0 DEG C 12h, the foamed ceramics base substrate solidified.
(2) 10mg/g graphene oxide solution is added in 4wt% poly-vinyl alcohol solution, is well mixed to be formed and mixes Solution is closed, mixed solution is instilled in liquid nitrogen through syringe needle and solidifies 5min, crystallization microballoon is formed, takes out, in 10 DEG C of scopes Interior defrosting 3h, the graphene oxide microballoon solidified.
(3) it is 10 according to graphene oxide microballoon, crosslinking agent and foamed ceramics green body quality ratio:0.8:150, by solidification Graphene oxide microballoon is added in 3wt% glutaraldehyde solution and is well mixed, and then impregnates the foamed ceramics base substrate of solidification Wherein, low-speed oscillation 20min, take out, the vacuum freeze drying 12h in the case where vacuum is 10Pa and -50 DEG C, obtain containing graphite oxide The foamed ceramics base substrate of alkene microballoon.
(4) the foamed ceramics base substrate of the microballoon containing graphene oxide is warming up to 1400 DEG C with 5 DEG C/min speed, sintering 12h, the multistage hole foamed ceramics of the microballoon containing porous graphene is obtained after cooling.
After testing, the multistage hole foamed ceramics and prior art of the microballoon containing porous graphene prepared by embodiment 1-6 The porosity of graphene/porous ceramic composite, the result of electric property and absorption property it is as follows:
As seen from the above table, the porosity of the multistage hole foamed ceramics of the microballoon containing porous graphene prepared by the present invention is high, Mechanical strength is good, and absorption property and electric conductivity significantly improve.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as Into all equivalent modifications or change, should by the present invention claim be covered.

Claims (10)

  1. A kind of 1. multistage hole foamed ceramics of microballoon containing porous graphene, it is characterised in that:The microballoon containing porous graphene Multistage hole foamed ceramics include foamed ceramics and porous graphene microballoon, the porous graphene microballoon is attached to foam pottery It is described micro- containing porous graphene containing micropore, the multistage hole of mesoporous and macropore in the porous graphene microballoon in the hole of porcelain The pore space structure of the multistage hole foamed ceramics of ball is to form micro-crystallization using polyvinyl alcohol freeze-thaw to form.
  2. 2. the preparation method of the multistage hole foamed ceramics of a kind of microballoon containing porous graphene, it is characterised in that including following step Suddenly:
    (1) ceramic powder hydrophobization dressing agent and polyvinyl alcohol, regulation pH value to faintly acid, high speed machine will be added in ceramic slurry Tool is stirred to obtain particle stabilized foam, and particle stabilized foam is placed under low temperature environment at once and solidifies 12-24h, is taken out, in 0- Thaw 3-12h in the range of 10 DEG C, the foamed ceramics base substrate solidified;
    (2) graphene oxide solution is added in poly-vinyl alcohol solution, is well mixed, is added dropwise in liquid nitrogen and solidifies, form knot Brilliant microballoon, take out, thaw 3-12h in the range of 0-10 DEG C, the graphene oxide microballoon solidified;
    (3) the graphene oxide microballoon of solidification is added in cross-linking agent solution and be well mixed, then consolidated prepared by step (1) The foamed ceramics base substrate dipping of change wherein, low-speed oscillation, takes out, vacuum freeze drying, obtains the bubble of the microballoon containing graphene oxide Foam ceramic body;
    (4) the foamed ceramics base substrate for the microballoon containing graphene oxide for preparing step (3) is in the case where sintering temperature is 1400-1900 DEG C Sintering, the multistage hole foamed ceramics of the microballoon containing porous graphene is obtained after cooling.
  3. 3. a kind of preparation method of the multistage hole foamed ceramics of microballoon containing porous graphene according to claim 2, its It is characterised by:In the step (1), the raw material of ceramic slurry is silicon nitride or carborundum, ceramic powders in ceramic slurry Mass fraction is 15-60%.
  4. 4. a kind of preparation method of the multistage hole foamed ceramics of microballoon containing porous graphene according to claim 2, its It is characterised by:In the step (1), ceramic powder hydrophobization dressing agent is lauryl ammonium chloride or cetyl chloride Ammonium.
  5. 5. a kind of preparation method of the multistage hole foamed ceramics of microballoon containing porous graphene according to claim 2, its It is characterised by:In the step (1), the mass fraction that ceramic powder hydrophobization dressing agent accounts for ceramic slurry is 0.01- 0.5wt%, the mass fraction that polyvinyl alcohol accounts for ceramic slurry are 0.01-0.5wt%.
  6. 6. a kind of preparation method of the multistage hole foamed ceramics of microballoon containing porous graphene according to claim 2, its It is characterised by:In the step (2), the concentration of graphene oxide is 10-30mg/g in graphene oxide solution, and polyvinyl alcohol is molten The mass fraction of polyvinyl alcohol is 1-4wt% in liquid.
  7. 7. a kind of preparation method of the multistage hole foamed ceramics of microballoon containing porous graphene according to claim 2, its It is characterised by:In the step (2), the method for dropwise addition instills for syringe needle, hardening time 5-10min.
  8. 8. a kind of preparation method of the multistage hole foamed ceramics of microballoon containing porous graphene according to claim 2, its It is characterised by:In the step (3), cross-linking agent solution is 1-3wt% glutaraldehyde solution.
  9. 9. a kind of preparation method of the multistage hole foamed ceramics of microballoon containing porous graphene according to claim 2, its It is characterised by:In the step (3), graphene oxide microballoon, crosslinking agent and foamed ceramics green body quality ratio are 10:0.5-0.8: 100-150。
  10. 10. a kind of preparation method of the multistage hole foamed ceramics of microballoon containing porous graphene according to claim 2, its It is characterised by:In the step (3), the vacuum of vacuum freeze drying is 5-10Pa, and temperature is-10-50 DEG C, time 12- 36h。
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108373151A (en) * 2018-05-25 2018-08-07 清华-伯克利深圳学院筹备办公室 A kind of preparation method of more fold hollow graphene microballoons
CN111099917A (en) * 2018-10-29 2020-05-05 中国石油化工股份有限公司 Porous composite material for generating electric arc in microwave and preparation method thereof
CN112823441A (en) * 2018-10-29 2021-05-18 中国石油化工股份有限公司 Porous composite material capable of generating electric arc in microwave field and preparation method and application thereof
CN113773067A (en) * 2021-11-11 2021-12-10 长沙中瓷新材料科技有限公司 Sagger based on cordierite and production process thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108373151A (en) * 2018-05-25 2018-08-07 清华-伯克利深圳学院筹备办公室 A kind of preparation method of more fold hollow graphene microballoons
CN108373151B (en) * 2018-05-25 2019-12-31 清华-伯克利深圳学院筹备办公室 Preparation method of multi-fold hollow graphene oxide microspheres
CN111099917A (en) * 2018-10-29 2020-05-05 中国石油化工股份有限公司 Porous composite material for generating electric arc in microwave and preparation method thereof
CN112823441A (en) * 2018-10-29 2021-05-18 中国石油化工股份有限公司 Porous composite material capable of generating electric arc in microwave field and preparation method and application thereof
CN113773067A (en) * 2021-11-11 2021-12-10 长沙中瓷新材料科技有限公司 Sagger based on cordierite and production process thereof
CN113773067B (en) * 2021-11-11 2022-01-18 长沙中瓷新材料科技有限公司 Sagger based on cordierite and production process thereof

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