CN105753507B - A kind of preparation method of silicon carbide-calcium hexaluminate complex phase porous ceramics - Google Patents
A kind of preparation method of silicon carbide-calcium hexaluminate complex phase porous ceramics Download PDFInfo
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Abstract
The invention belongs to porous ceramics preparing technical fields, and in particular to a kind of preparation method of silicon carbide calcium hexaluminate complex phase porous ceramics.A kind of preparation method of the silicon carbide calcium hexaluminate complex phase porous ceramics proposed is combined as calcium source, and using foaming with aluminous cement solidification using aluminous cement, realizes that the fast curing-formed of foamed slurry obtains porous body；Then aluminous cement is utilized to generate calcium hexaluminate combined silicon carbide material, the final preparation for realizing silicon carbide calcium hexaluminate complex phase porous ceramics with alumina powder precursor reactant at high temperature.The present invention has the characteristics that low-density, high intensity, alkali resistant aggressivity be strong, good thermal shock stability.
Description
Technical field
The invention belongs to porous ceramics preparing technical fields, and in particular to a kind of silicon carbide-porous pottery of calcium hexaluminate complex phase
The preparation method of porcelain.
Background technology
With being constantly progressive for material preparation technology, porous ceramic film material has been obtained for significant progress；But arrive mesh
Before until, there is a problem of when oxide porous ceramic uses at high temperature elevated temperature strength and thermal shock resistance difference；And nitride is more
Although hole ceramics mechanical behavior under high temperature is excellent, its antioxygenic property is relatively poor；And carborundum porous ceramics then have heat
The coefficient of expansion is small, intensity is high, heat-resistant knocking stability is good, high temperature resistant, corrosion-resistant, service life is long and relatively good anti-oxidant
Property etc. series of advantages, therefore, carborundum porous ceramics caused people it is extensive concern and in-depth study；And
And carborundum porous ceramics have been widely applied to many fields, such as catalyst carrier, thermal current or molten metal mistake
Filter, high temperature membrane reactor, heat-insulating material and sensor etc..
Silicon carbide is due to being that strong covalent bond combines, and particle diffusion rate is very low when sintering, the ratio between crystal boundary energy and surface energy
It is very high, it is not easy to obtain enough energy formation crystal boundaries, the oxidation film on surface also plays diffusion barrier；Therefore be difficult take from
The normal pressure-sintered approach of sub-key bond material institute generally use produces high densification material, it is necessary to use some special process hands
Section is helped by the second phase substance, promotes its sintering；Main preparation method includes at present：Silicon carbide reaction-sintered, again
Crystalline silicon carbide, hot pressed sintering silicon carbide, constant pressure sintering silicon carbide, when being prepared using these four methods, sintering temperature is 1800
DEG C~2450 DEG C, energy expenditure is big.
The method for preparing porous ceramics at present has very much, and the most commonly used is addition pore creating material method and foamings, add pore-creating
Agent method is to lose agent, such as graphite, starch, sawdust added with machine burning during body preparation；Foaming is in body preparation
The mode of Cheng Liyong surfactant mechanical foamings, bubble are the unstable phase of thermodynamics, will appear in ceramic slurry and grow up, on
It is floating, phenomena such as rupture；Aluminous cement is common forming agent, and hydration reaction can occurs after meeting water in it, and then generates the hydraulicity,
It is widely used in ambiguity material.
Calcium hexaluminate has a series of excellent performances, and the range that solid solution is formed with the slag containing iron oxide is big, in alkalinity
There is sufficiently strong chemical resistance of concrete ability in environment, highly stable in a reducing atmosphere, the coefficient of expansion is main to tie close to aluminium oxide
Crystalline region is big, there is lower dissolubility in several polynary systems, and it is very extensive that these characteristics make calcium hexaluminate have in high temperature industry
Application prospect.
Invention content
In order to solve the above technical problems, the purpose of the present invention is to propose to a kind of silicon carbide-calcium hexaluminate complex phase porous ceramics
Preparation method.
The present invention is to complete above-mentioned purpose to adopt the following technical scheme that：
A kind of preparation method of silicon carbide-calcium hexaluminate complex phase porous ceramics, the preparation method use calcium aluminate water
Mud is combined as calcium source, and using foaming with aluminous cement solidification, realizes that the fast curing-formed of foamed slurry obtains
Porous body；Then aluminous cement is utilized to generate calcium hexaluminate silicon carbide material with alumina powder precursor reactant at high temperature
Material finally realizes the preparation of silicon carbide-calcium hexaluminate complex phase porous ceramics；Its specific method is：
（1）Silicon carbide powder, alumina powder, water, dispersant, aluminous cement are added in ball grinder by a certain percentage
Ball milling mixing is carried out, stable suspended nitride is obtained；
（2）Suspended nitride is moved to and carries out mechanical agitation in agitator, a certain amount of surface-active is added in stirring while
Agent continues to stir to get foamed slurry；Slurry is injected into mold after foam stabilization, foamed slurry rapid curing obtains having certain
The porous body of porosity；
（3）Porous body after molding, which moves in baking oven, dries, drying temperature be 80~120 DEG C, the duration be 5~
100h；Dry be placed in the kiln for be connected with particular atmosphere is warming up to 1400 DEG C~1600 DEG C with the heating rate of 5 DEG C/min, protects
Temperature obtains porous silicon carbide-calcium hexaluminate complex phase porous ceramics for 1~50 hour.
The alumina powder, water, dispersant, aluminium oxide abrading-ball, aluminous cement, foaming agent addition be respectively
5%~200%, 50%~300%, 0.3%~5%, 50%~300%, 6%~120%, the 4%~25% of carborundum powder weight.
The average grain diameter of the silicon carbide powder is 0.5~85 μm；The average grain diameter of alumina powder is 0.5~50 μm.
The dispersant be tripolyphosphate ammonium, sodium tripolyphosphate, Hexamethylphosphoric acid triamide, calgon, ammonium polyacrylate,
The mixture of the two or more arbitrary mass ratioes of one or both of tetramethylammonium hydroxide.
The foaming agent is lauryl sodium sulfate, dodecyl triethanolamine, ammonium lauryl sulfate, dodecyl
The mixture of the arbitrary mass ratio of one or more of benzene sulfonic acid sodium salt.
The content of aluminium oxide is 50~85% in the aluminous cement.
The atmosphere of the kiln is one kind in vacuum, argon gas and nitrogen.
A kind of preparation method of silicon carbide proposed by the present invention-calcium hexaluminate complex phase porous ceramics utilizes hair at normal temperatures
Bubble method is combined with cement solidification, realizes the fast curing-formed of foamed slurry；Six that reaction in-situ generates are utilized at high temperature
Calcium aluminate silicon carbide makes material that there is higher mechanical strength, the material of preparation to have both the spy of silicon carbide and calcium hexaluminate
Property；Have the characteristics that low-density, high intensity, alkali resistant aggressivity be strong, good thermal shock stability.
Specific implementation mode
Embodiment 1
Choose the carborundum powder ceramic powder and to account for carborundum powder weight 80% and meso-position radius be 1.5 that meso-position radius is 4.2 μm
μm alumina powder, to account for the water of carborundum powder weight 110% as decentralized medium, to account for carborundum powder weight 1.3%
Sodium tripolyphosphate is dispersant, to account for aluminous cement that carborundum powder weight 35% and alumina content are 65% as bonding agent
And ball milling in ball grinder is poured into, the rotating speed of ball mill is 38r/min, runs 10h；Slurry after ball milling is placed in agitator and is stirred
It mixes, is added while stirring and accounts for the dodecyl triethanolamine that carborundum powder weight is 10%, slurry injects mould after fully foaming
Tool, slurry is fast curing-formed, demoulds afterwards for 24 hours, and the green body after demoulding is placed in 100 DEG C of heat preservation 20h in electric drying oven with forced convection；It is dry
Green body after dry is warming up to 1500 DEG C in argon gas stove with the heating rate of 5 DEG C/min, keeps the temperature 10h, obtains-six aluminic acid of silicon carbide
Calcium complex phase porous ceramics.
Embodiment 2
Choose the carborundum powder ceramic powder and account for carborundum powder weight 60% and meso-position radius is that meso-position radius is 16.4 μm
4.5 μm of alumina powder, to account for the water of carborundum powder weight 80% as decentralized medium, to account for carborundum powder weight 0.8%
Tripolyphosphate ammonium be dispersant, to account for aluminous cement that carborundum powder weight 30% and alumina content are 58% as combination
Agent simultaneously pours into ball milling in ball grinder, and the rotating speed of ball mill is 38r/min, runs 10h.Slurry after ball milling is placed in agitator
Stirring, is added while stirring and accounts for the ammonium lauryl sulfate that carborundum powder weight is 8%, and slurry injects mould after fully foaming
Tool, slurry is fast curing-formed, demoulds afterwards for 24 hours, and the green body after demoulding is placed in 100 DEG C of heat preservation 20h in electric drying oven with forced convection.It is dry
Green body after dry is warming up to 1400 DEG C with the heating rate of 5 DEG C/min in a vacuum furnace, keeps the temperature 20h, obtains-six aluminic acid of silicon carbide
Calcium complex phase porous ceramics.
Embodiment 3
Choose the carborundum powder ceramic powder and account for carborundum powder weight 50% and meso-position radius is that meso-position radius is 38.2 μm
15.2 μm of alumina powder, to account for the water of carborundum powder weight 100% as decentralized medium, to account for carborundum powder weight
1.8% tetramethylammonium hydroxide is dispersant, to account for the calcium aluminate water that carborundum powder weight 20% and alumina content are 70%
Mud is bonding agent and pours into ball milling in ball grinder, and the rotating speed of ball mill is 38r/min, runs 10h.Slurry after ball milling is placed in
It is stirred in agitator, is added while stirring and accounts for the lauryl sodium sulfate that carborundum powder weight is 6%, slurry fully foams
After inject mold, slurry is fast curing-formed, demoulds afterwards for 24 hours, and the green body after demoulding is placed in electric drying oven with forced convection 80 DEG C of guarantors
Warm 20h.Green body after drying is warming up to 1550 DEG C in nitrogen furnace with the heating rate of 5 DEG C/min, keeps the temperature 8h, is carbonized
Silicon-calcium hexaluminate complex phase porous ceramics.
Embodiment 4
Choose the carborundum powder ceramic powder and account for carborundum powder weight 100% and meso-position radius is that meso-position radius is 52 μm
19.5 μm of alumina powder, to account for the water of carborundum powder weight 140% as decentralized medium, to account for carborundum powder weight
2.5% Hexamethylphosphoric acid triamide is dispersant, is to account for the aluminous cement that carborundum powder weight 50% and alumina content are 62%
Bonding agent simultaneously pours into ball milling in ball grinder, and the rotating speed of ball mill is 38r/min, runs 10h.Slurry after ball milling is placed in stirring
It is stirred in bucket, is added while stirring and accounts for the ammonium lauryl sulfate that carborundum powder weight is 10%, slurry is noted after fully foaming
Enter mold, slurry is fast curing-formed, demoulds afterwards for 24 hours, and the green body after demoulding is placed in 80 DEG C of heat preservations in electric drying oven with forced convection
20h.Green body after drying is warming up to 1500 DEG C with the heating rate of 5 DEG C/min in a vacuum furnace, keeps the temperature 20h, obtains silicon carbide-
Calcium hexaluminate complex phase porous ceramics.
Embodiment 5
Choose the carborundum powder ceramic powder and account for carborundum powder weight 120% and meso-position radius is that meso-position radius is 77 μm
25.5 μm of alumina powder, to account for the water of carborundum powder weight 160% as decentralized medium, to account for carborundum powder weight 3%
Sodium tripolyphosphate be dispersant, to account for aluminous cement that carborundum powder weight 80% and alumina content are 60% as combination
Agent simultaneously pours into ball milling in ball grinder, and the rotating speed of ball mill is 38r/min, runs 10h.Slurry after ball milling is placed in agitator
Stirring, is added while stirring and accounts for the ammonium lauryl sulfate that carborundum powder weight is 20%, and slurry injects mould after fully foaming
Tool, slurry is fast curing-formed, demoulds afterwards for 24 hours, and the green body after demoulding is placed in 110 DEG C of heat preservation 12h in electric drying oven with forced convection.It is dry
Green body after dry is warming up to 1450 DEG C in argon gas stove with the heating rate of 5 DEG C/min, keeps the temperature 30h, obtains-six aluminic acid of silicon carbide
Calcium complex phase porous ceramics.
Claims (5)
1. a kind of preparation method of silicon carbide-calcium hexaluminate complex phase porous ceramics, it is characterised in that：The preparation method uses
Aluminous cement is combined as calcium source, and using foaming with aluminous cement solidification, realizes the rapid curing of foamed slurry
Molding obtains porous body；Then aluminous cement is utilized to generate calcium hexaluminate combination carbon with alumina powder precursor reactant at high temperature
Silicon nitride material finally realizes the preparation of silicon carbide-calcium hexaluminate complex phase porous ceramics；Its specific method is：
（1）Silicon carbide powder, alumina powder, water, dispersant, aluminous cement, which are added in ball grinder, carries out ball milling mixing,
Obtain stable suspended nitride；Alumina powder, water, dispersant, aluminium oxide abrading-ball, aluminous cement addition be respectively carbon
5%~200%, 50%~300%, 0.3%~5%, 50%~300%, the 6%~120% of SiClx powder quality；
（2）Suspended nitride is moved to and carries out mechanical agitation in agitator, stirring while be incorporated as carborundum powder weight 4%~
25% foaming agent continues to stir to get foamed slurry；Slurry is injected into mold after foam stabilization, foamed slurry rapid curing obtains
To the porous body with certain porosity；
（3）Porous body after molding, which moves in baking oven, dries, and drying temperature is 80~120 DEG C, and the duration is 5~100h；
Dry be placed in the kiln for be connected with particular atmosphere is warming up to 1400 DEG C~1600 DEG C with the heating rate of 5 DEG C/min, and heat preservation 1~
Obtain within 50 hours porous silicon carbide-calcium hexaluminate complex phase porous ceramics；The particular atmosphere is in vacuum, argon gas and nitrogen
It is a kind of.
2. a kind of preparation method of silicon carbide-calcium hexaluminate complex phase porous ceramics as described in claim 1, it is characterised in that：
The average grain diameter of the silicon carbide powder is 0.5~85 μm；The average grain diameter of alumina powder is 0.5~50 μm.
3. a kind of preparation method of silicon carbide-calcium hexaluminate complex phase porous ceramics as described in claim 1, it is characterised in that：
The dispersant is tripolyphosphate ammonium, sodium tripolyphosphate, Hexamethylphosphoric acid triamide, calgon, ammonium polyacrylate, tetramethyl hydrogen
The mixture of the arbitrary mass ratio of one or more of amine-oxides.
4. a kind of preparation method of silicon carbide-calcium hexaluminate complex phase porous ceramics as described in claim 1, it is characterised in that：
The foaming agent is lauryl sodium sulfate, dodecyl triethanolamine, ammonium lauryl sulfate, neopelex
One or more of arbitrary mass ratio mixture.
5. a kind of preparation method of silicon carbide-calcium hexaluminate complex phase porous ceramics as described in claim 1, it is characterised in that：
The content of aluminium oxide is 50~85% in the aluminous cement.
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| CN106966740B (en) * | 2017-05-16 | 2019-09-10 | 武汉科技大学 | Waste incinerator calcium hexaluminate/silicon carbide castable and preparation method thereof |
| CN107892575B (en) * | 2017-11-24 | 2021-06-29 | 中钢集团洛阳耐火材料研究院有限公司 | Silicon carbide-calcium hexaluminate composite refractory material |
| CN112679224B (en) * | 2021-01-27 | 2022-09-16 | 辽宁罕王绿色建材有限公司 | Micro-crystallized porous ceramic plate and preparation method thereof |
| CN112898009B (en) * | 2021-02-20 | 2022-04-15 | 中冶武汉冶金建筑研究院有限公司 | Preparation method of calcium hexaluminate foamed ceramic with multilayer structure |
| CN114750081B (en) * | 2022-04-06 | 2024-04-02 | 郑州跃川超硬材料有限公司 | Ceramic bond with air holes and preparation method thereof |
| CN115231925A (en) * | 2022-07-20 | 2022-10-25 | 洛阳理工学院 | Method for preparing calcium hexaluminate combined silicon carbide ceramic by microwave |
| CN115521520A (en) * | 2022-10-21 | 2022-12-27 | 安徽电缆股份有限公司 | Termite-proof cable outer sheath material and preparation method thereof |
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