CN102173852A - Method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique - Google Patents
Method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique Download PDFInfo
- Publication number
- CN102173852A CN102173852A CN2011100353048A CN201110035304A CN102173852A CN 102173852 A CN102173852 A CN 102173852A CN 2011100353048 A CN2011100353048 A CN 2011100353048A CN 201110035304 A CN201110035304 A CN 201110035304A CN 102173852 A CN102173852 A CN 102173852A
- Authority
- CN
- China
- Prior art keywords
- milk sap
- alumina porous
- porous ceramic
- molding process
- gel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Abstract
The invention relates to a method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique, which comprises the following steps: (1) by using alkane or ester containing more than four carbon atoms as a disperse phase and using surfactant with an HLB (hydrophile-lipophile balance) value of 8-20 as an emulsifier, stirring to obtain an oil-in-water emulsion; (2) preparing a stable suspension containing organic monomers, a crosslinking agent, a catalyst, a dispersant and ceramic powder; (3) mixing the emulsion and suspension to obtain a slurry, adding a proper amount of initiator, and evenly stirring; (4) casting the slurry into a die, carrying out crosslinking curing, stripping, drying the blank, and discharging adhesive from the blank; and (5) sintering the blank by using a certain firing procedure, thereby finally obtaining the alumina porous ceramics. The number and size of pores of the porous ceramics can be effectively regulated and controlled, the required device and technological process are simple, and the porous ceramics have high mechanical strength.
Description
Technical field
The present invention relates to the method that a kind of milk sap attached gel molding process prepares alumina porous ceramic, relate to a kind of or rather with the approach of the oil droplet in the oil-in-water emulsion as the introducing pore, and the preparation light porous heat-insulating material that combines with aqueous gel casting technology, belong to the porous ceramics field.
Background technology
Porous ceramics has advantages such as porosity height, density be low, high temperature resistant, corrosion-resistant, all has broad application prospects in fields such as metallurgy, catalysis, chemical industry, environmental protection, the energy.At present, the preparation method of porous ceramics mainly contains and adds solid pore-forming material method, foaming, organic precursor pickling process etc.Solid pore-forming material method is by adding solid pore-forming material (as graphite, starch, sawdust etc.) when the ceramic batch, occupy certain space in ceramic body, in sintering process pore-forming material is burnt and forms pore.The porous ceramics air hole structure of this method preparation is different, and void content is lower and gas cell distribution is inhomogeneous.Foaming is to add organic or inorganic foaming agent in ceramic size, produces foam in whipping process, and drying and sintering make porous ceramics.The porous ceramics aperture of this method preparation is less and mostly be the hole of holding one's breath, but foaming is to the having relatively high expectations of raw material, and processing condition are wayward.Organic precursor pickling process is mainly used in preparation perforate porous ceramics, and the tridimensional network that utilizes organic foam body (as polyurethane sponge etc.) to be had evenly is coated in slurry on the organic foam body, obtains netted porous ceramics after burning foams.The porous ceramics void content of this prepared is higher, and the aperture is big, is mainly used in the metal melt filtering device.
Milk sap is meant that a kind of liquid is dispersed in another kind of and its not miscible liquid and the dispersion system that forms with the form of drop.Drop is called disperse phase, and the liquid of another kind of continuous distribution is called dispersion medium.Milk sap can be divided into usually oil-in-water (oil-in-water, O/W) and water-in-oil (water-in-oil, W/O) two types.The preparation of true emulsion need add certain tensio-active agent, i.e. emulsifying agent usually.Adjust the ratio of water, oil and emulsifying agent, the size that can make disperse phase is less than 100nm, and at this moment milk sap becomes transparent, and more stable, is called microemulsion.At present, Water in Oil emulsion has been widely used in the especially preparation of nanometer grade powder of inorganic materials superfine powder, and oil-in-water emulsion then is mainly used in pharmaceutical carrier and pesticide field.Oil phase in the oil-in-water emulsion as pore-forming material, is expected to be used for the preparation of porous ceramic film material, its precondition be with dispersive oil droplet anchored in place in ceramic body.
In the invention nineties in 20th century, it combines traditional slip-casting shaping process and organic chemistry macromolecular polymerization reaction gel injection molding and forming technology dexterously, can be used for the material preparation of different shape complexity by U.S. Oak Ridge National Key Laboratory.The ultimate principle of this technology is by preparation high solid loading, low viscous ceramic size, again by adding a small amount of initiator and catalyzer or making organic monomer and linking agent polymerization reaction take place in the slurry make the slurry in-situ solidifying by the mode that heats, obtain the base substrate of high strength, good uniformity, through operations such as super-dry, binder removal and sintering, prepare the ceramic component of near net-shape then.This forming technique has received various countries scientific worker's concern since invention, especially have bigger advantage when the ceramic part of moulding complicated shape.
Adopt water system gel injection technology, just can be in the solidified base substrate with the oil phase drop anchored in place in the oil-in-water emulsion, and ceramic powder and gelling system still are distributed in aqueous phase.This is equivalent to add the drop pore-forming material in ceramic size, successfully introduces pore thereby in sintering process the oil phase drop burnt.By a large amount of literature searches, do not find that the method that adopts milk sap to combine with gel injection molding and forming technology prepares the report of porous ceramics.
Summary of the invention
The objective of the invention is to propose the method that a kind of milk sap attached gel molding process prepares alumina porous ceramic, oil-in-water emulsion is combined with gel injection technology, realize the adjustable of the pore quantity of porous ceramic film material and size, the porous ceramics that makes simultaneously possesses higher physical strength.
The technical scheme that the present invention proposes is: a kind of milk sap attached gel molding process prepares the method for alumina porous ceramic, and described preparation method comprises drying, binder removal and the sintering of base substrate behind the mixed gel casting forming of preparation, milk sap and suspension, moulding of the ceramic powder stable suspension of the preparation of oil-in-water emulsion, certain solid load.Its concrete processing step is:
1) preparation of oil-in-water emulsion:
With water is dispersion medium, is disperse phase with the organism of 0.5～10 times of volume of dispersion medium, and add HLB value at 8～20 tensio-active agent as emulsifying agent, prepare the oil-in-water-type true emulsion through stirring.Wherein, described organism is to contain four carbon atom above alkane or ester class, described tensio-active agent is a kind of in anion surfactant, cats product, the nonionogenic tenside, and its consumption is the disperse phase quality
2) have the preparation of the ceramic powder stable suspension of certain solid load:
With water, organic monomer, linking agent, catalyzer, dispersion agent and alumina powder jointed the batching, and carry out ball milling and mix, obtain solid load at 20～80% stable suspension.Wherein, described organic monomer is a kind of in acrylamide AM, Methacrylamide MAM, propyl group acrylamide, vinyl pyrrolidone NVP, Jia Jibingxisuanyizhi, the vinylbenzene; Described linking agent is a kind of in methylene-bisacrylamide MBAM, diallyl tartrate diamide DATDA, the propenyl methyl acrylate; Described catalyzer is N, N, N ', N '-Tetramethyl Ethylene Diamine TEMED; Described dispersion agent is a kind of in tripolyphosphate ammonium, Hexamethylphosphoric acid triamide, the ammonium polyacrylate; Dispersion agent, organic monomer, linking agent, catalyst consumption are respectively 0.1～3.0%, 3～10%, 0.1～2.0%, 0.01～0.3% of alumina powder jointed quality; Described ball milling hybrid technique, ball milling speed are 20～300r/min, and the ball milling time is 0.5～12h;
3) the mixed gel casting forming of milk sap and suspension:
Milk sap and suspension mixed stir and add initiator, be stirred well to evenly, then mixed slurry is injected the mould of smearing releasing agent and make it that crosslinking reaction take place, carry out the demoulding after leaving standstill for some time.Wherein, the volume ratio of milk sap and suspension is 1: 4～8: 1; Described initiator is a persulphate, and consumption is 10～80% of a monomer mass, and described crosslinking time is 1～30min;
4) drying of base substrate, binder removal and sintering:
Base substrate after the demoulding is successively carried out drying in climatic chamber and common loft drier; In air atmosphere, carry out binder removal and sintering then.Described climatic chamber drying, temperature and humidity are respectively at 35～80 ℃, 30～90%, and the time length is 4～12h; Described common loft drier drying, temperature are at 80～110 ℃, and the time length is 6～36h; Described binder removal technology, temperature rise rate are 0.3～1 ℃/min, and in 300～600 ℃ of insulation 0.5～5h; Described sintering process, temperature rise rate are 0.5～3 ℃/min, and in 1400～1700 ℃ of insulation 1～3h.
Organism as disperse phase can be: a kind of in pentamethylene, hexanaphthene, normal heptane, octane, isopropyl laurate, ethyl palmitate, the n-capric acid methyl esters.
Tensio-active agent as emulsifying agent can be: a kind of in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, cetyl trimethylammonium bromide, the tween series of surfactants.
Persulphate as initiator can be: a kind of in Sodium Persulfate, Potassium Persulphate, the ammonium persulphate.
Advantage of the present invention:
Oil-in-water emulsion is combined with gel injection technology, can realize the pore quantity of porous ceramic film material and the regulation and control of size by adjusting to the milk sap proportion of composing, required equipment and technical process are fairly simple, the ceramic systems that is suitable for is wide, and prepared finished product has higher physical strength simultaneously.
Description of drawings
Fig. 1 is the electron scanning micrograph of the embodiment of the invention 1 prepared sample section.
Embodiment
Embodiment 1
Being dispersion medium with water at first, is disperse phase with the pentamethylene, is emulsifying agent with the cetyl trimethylammonium bromide, preparation milk sap, and wherein the disperse phase volume is 3 times of water, the emulsifying agent consumption is going of disperse phase quality.With the Hexamethylphosphoric acid triamide is dispersion agent, acrylamide is a monomer, methylene-bisacrylamide is a linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is a catalyzer, with the rotating speed planetary ball mill 12h of 20r/min, the preparation solid load is 70% alumina stable suspension, and wherein dispersion agent, monomer, linking agent, catalyst consumption are respectively 1.0%, 8.0%, 2.0%, 0.05% of aluminum oxide quality.Milk sap and suspension are mixed with volume ratio at 1: 1 and add ammonium persulphate as initiator, consumption is 10% of a monomer mass, and mould is injected in the back that stirs, and leaves standstill 30min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 40 ℃ and 40%, and insulation 6h changes over to then in 100 ℃ the common loft drier and is incubated 6h.Base substrate after the oven dry earlier in tube furnace the temperature rise rate with 0.5 ℃/min rise to 400 ℃ of insulation 3h, to remove organism wherein, rise to 1600 ℃ and be incubated 1h with the temperature rise rate of 1 ℃/min then, burn till porous ceramics.The porosity of gained porous ceramics is 58%, and ultimate compression strength is 25MPa.Fig. 1 has provided the microtexture of section hole behind the porous ceramics sintering.
Embodiment 2
Being dispersion medium with water at first, is disperse phase with the normal heptane, is emulsifying agent with the Sodium dodecylbenzene sulfonate, preparation milk sap, and wherein the disperse phase volume is 10 times of water, the emulsifying agent consumption is the disperse phase quality
With the ammonium polyacrylate is dispersion agent, Methacrylamide is a monomer, diallyl tartrate diamide is a linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is a catalyzer, with the rotating speed planetary ball mill 8h of 50r/min, the preparation solid load is 80% alumina stable suspension, and wherein dispersion agent, monomer, linking agent, catalyst consumption are respectively 3.0%, 4.0%, 0.8%, 0.01% of aluminum oxide quality.Milk sap and suspension are mixed with volume ratio at 8: 1 and add Sodium Persulfate as initiator, consumption is 30% of a monomer mass, and mould is injected in the back that stirs, and leaves standstill 10min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 60 ℃ and 50%, and insulation 8h changes over to then in 90 ℃ the common loft drier and is incubated 24h.Base substrate after the oven dry earlier in tube furnace the temperature rise rate with 0.3 ℃/min rise to 400 ℃ of insulation 4h, to remove organism wherein, rise to 1400 ℃ and be incubated 1h with the temperature rise rate of 0.5 ℃/min then, burn till porous ceramics.The porosity of gained porous ceramics is 85%, and ultimate compression strength is 15MPa.
Embodiment 3
Being dispersion medium with water at first, is disperse phase with the octane, is emulsifying agent with the sodium lauryl sulphate, preparation milk sap, and wherein the disperse phase volume is 5 times of water, the emulsifying agent consumption is the disperse phase quality
With the tripolyphosphate ammonium is dispersion agent, vinyl pyrrolidone is a monomer, methylene-bisacrylamide is a linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is a catalyzer, with the rotating speed planetary ball mill 4h of 100r/min, the preparation solid load is 60% alumina stable suspension, and wherein dispersion agent, monomer, linking agent, catalyst consumption are respectively 0.1%, 3%, 0.1%, 0.1% of aluminum oxide quality.Milk sap and suspension are mixed with volume ratio at 4: 1 and add Potassium Persulphate as initiator, consumption is 60% of a monomer mass, and mould is injected in the back that stirs, and leaves standstill 5min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 55 ℃ and 80%, and insulation 10h changes over to then in 110 ℃ the common loft drier and is incubated 10h.Base substrate after the oven dry earlier in tube furnace the temperature rise rate with 0.8 ℃/min rise to 300 ℃ of insulation 5h, to remove organism wherein, rise to 1500 ℃ and be incubated 3h with the temperature rise rate of 3 ℃/min then, burn till porous ceramics.The porosity of gained porous ceramics is 51%, and ultimate compression strength is 27MPa.
Embodiment 4
Being dispersion medium with water at first, is disperse phase with the isopropyl laurate, is emulsifying agent with the tween 80, preparation milk sap, and wherein the disperse phase volume is 7 times of water, the emulsifying agent consumption is the disperse phase quality
With the Hexamethylphosphoric acid triamide is dispersion agent, acrylamide is a monomer, the propenyl methyl acrylate is a linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is a catalyzer, with the rotating speed planetary ball mill 1h of 200r/min, the preparation solid load is 62% alumina stable suspension, and wherein dispersion agent, monomer, linking agent, catalyst consumption are respectively 0.5%, 10%, 1.2%, 0.2% of aluminum oxide quality.Milk sap and suspension are mixed with volume ratio at 2: 1 and add Sodium Persulfate as initiator, consumption is 30% of a monomer mass, and mould is injected in the back that stirs, and leaves standstill 15min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 35 ℃ and 90%, and insulation 12h changes over to then in 100 ℃ the common loft drier and is incubated 30h.Base substrate after the oven dry earlier in tube furnace the temperature rise rate with 1 ℃/min rise to 600 ℃ of insulation 0.5h, to remove organism wherein, rise to 1700 ℃ and be incubated 1h with the temperature rise rate of 2 ℃/min then, burn till porous ceramics.The porosity of gained porous ceramics is 70%, and ultimate compression strength is 18MPa.
Embodiment 5
Being dispersion medium with water at first, is disperse phase with the ethyl palmitate, is emulsifying agent with the polysorbate60, preparation milk sap, and wherein the disperse phase volume is 0.5 times of water, the emulsifying agent consumption is the disperse phase quality
With the ammonium polyacrylate is dispersion agent, Jia Jibingxisuanyizhi is a monomer, methylene-bisacrylamide is a linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is a catalyzer, with the rotating speed planetary ball mill 0.5h of 300r/min, the preparation solid load is 30% alumina stable suspension, and wherein dispersion agent, monomer, linking agent, catalyst consumption are respectively 1.5%, 7%, 1.5%, 0.12% of aluminum oxide quality.Milk sap and suspension are mixed with volume ratio at 1: 4 and add ammonium persulphate as initiator, consumption is 80% of a monomer mass, and mould is injected in the back that stirs, and leaves standstill 1min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 80 ℃ and 70%, and insulation 4h changes over to then in 110 ℃ the common loft drier and is incubated 6h.Base substrate after the oven dry earlier in tube furnace the temperature rise rate with 0.5 ℃/min rise to 300 ℃ of insulation 3h, to remove organism wherein, rise to 1650 ℃ and be incubated 2h with the temperature rise rate of 2 ℃/min then, burn till porous ceramics.The porosity of gained porous ceramics is 25%, and ultimate compression strength is 103MPa.
Embodiment 6
Being dispersion medium with water at first, is disperse phase with the n-capric acid methyl esters, is emulsifying agent with the cetyl trimethylammonium bromide, preparation milk sap, and wherein the disperse phase volume is 2 times of water, the emulsifying agent consumption is the disperse phase quality
With the tripolyphosphate ammonium is dispersion agent, acrylamide is a monomer, the propenyl methyl acrylate is a linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is a catalyzer, with the rotating speed planetary ball mill 6h of 150r/min, the preparation solid load is 20% alumina stable suspension, and wherein dispersion agent, monomer, linking agent, catalyst consumption are respectively 2.0%, 5%, 1.0%, 0.3% of aluminum oxide quality.Milk sap and suspension are mixed with volume ratio at 1: 2 and add ammonium persulphate as initiator, consumption is 50% of a monomer mass, and mould is injected in the back that stirs, and leaves standstill 20min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 70 ℃ and 60%, and insulation 7h changes over to then in 80 ℃ the common loft drier and is incubated 36h.Base substrate after the oven dry earlier in tube furnace the temperature rise rate with 0.7 ℃/min rise to 500 ℃ of insulation 4h, to remove organism wherein, rise to 1550 ℃ and be incubated 2h with the temperature rise rate of 1 ℃/min then, burn till porous ceramics.The porosity of gained porous ceramics is 45%, and ultimate compression strength is 82MPa.
Embodiment 7
Being dispersion medium with water at first, is disperse phase with the hexanaphthene, is emulsifying agent with the sodium lauryl sulphate, preparation milk sap, and wherein the disperse phase volume is 6 times of water, the emulsifying agent consumption is the disperse phase quality
With the ammonium polyacrylate is dispersion agent, the propyl group acrylamide is a monomer, methylene-bisacrylamide is a linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is a catalyzer, with the rotating speed planetary ball mill 2h of 80r/min, the preparation solid load is 50% alumina stable suspension, and wherein dispersion agent, monomer, linking agent, catalyst consumption are respectively 0.3%, 9%, 0.5%, 0.08% of aluminum oxide quality.Milk sap and suspension are mixed with volume ratio at 5: 1 and add Potassium Persulphate as initiator, consumption is 40% of a monomer mass, and mould is injected in the back that stirs, and leaves standstill 3min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 60 ℃ and 70%, and insulation 6h changes over to then in 100 ℃ the common loft drier and is incubated 20h.Base substrate after the oven dry earlier in tube furnace the temperature rise rate with 1 ℃/min rise to 400 ℃ of insulation 5h, to remove organism wherein, rise to 1450 ℃ and be incubated 1h with the temperature rise rate of 2 ℃/min then, burn till porous ceramics.The porosity of gained porous ceramics is 68%, and ultimate compression strength is 18MPa.
Embodiment 8
Being dispersion medium with water at first, is disperse phase with the ethyl palmitate, is emulsifying agent with the Sodium dodecylbenzene sulfonate, preparation milk sap, and wherein the disperse phase volume is 4 times of water, the emulsifying agent consumption is the disperse phase quality
With the tripolyphosphate ammonium is dispersion agent, vinylbenzene is monomer, diallyl tartrate diamide is a linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is a catalyzer, with the rotating speed planetary ball mill 2h of 100r/min, the preparation solid load is 55% alumina stable suspension, and wherein dispersion agent, monomer, linking agent, catalyst consumption are respectively 1.0%, 6%, 1.4%, 0.15% of aluminum oxide quality.Milk sap and suspension are mixed with volume ratio at 3: 1 and add ammonium persulphate as initiator, consumption is 20% of a monomer mass, and mould is injected in the back that stirs, and leaves standstill 10min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 75 ℃ and 80%, and insulation 8h changes over to then in 105 ℃ the common loft drier and is incubated 12h.Base substrate after the oven dry earlier in tube furnace the temperature rise rate with 0.5 ℃/min rise to 500 ℃ of insulation 2h, to remove organism wherein, rise to 1550 ℃ and be incubated 2h with the temperature rise rate of 1.5 ℃/min then, burn till porous ceramics.The porosity of gained porous ceramics is 55%, and ultimate compression strength is 26MPa.
Claims (12)
1. a milk sap attached gel molding process prepares the method for alumina porous ceramic, it is characterized in that: described preparation method comprises drying, binder removal and the sintering of base substrate behind the mixed gel casting forming of preparation, milk sap and suspension, moulding of the ceramic powder stable suspension of the preparation of oil-in-water emulsion, certain solid load;
1) preparation of oil-in-water emulsion:
With water is dispersion medium, is disperse phase with the organism of 0.5～10 times of volume of dispersion medium, and add the HLB value at 8～20 tensio-active agent as emulsifying agent, the volume of tensio-active agent is a disperse phase
Through stirring preparation oil-in-water-type true emulsion;
2) preparation of the ceramic powder stable suspension of certain solid load:
With water, organic monomer, linking agent, catalyzer, dispersion agent and alumina powder jointed the batching, and carry out ball milling and mix, obtain solid load and be 20～80% stable suspension;
3) the mixed gel casting forming of milk sap and suspension:
Milk sap and suspension are mixed and add initiator according to a certain volume, be stirred well to evenly, then mixed slurry is injected the mould of smearing releasing agent, carry out the demoulding after leaving standstill for some time;
4) drying of base substrate, binder removal and sintering:
Base substrate after the demoulding is successively carried out drying in climatic chamber and common loft drier; In air atmosphere, carry out binder removal and sintering then.
2. the method for preparing alumina porous ceramic by the described milk sap attached gel of claim 1 molding process is characterized in that described organism is to contain four carbon atom above alkane or ester class.
3. the method for preparing alumina porous ceramic by the described milk sap attached gel of claim 1 molding process is characterized in that described tensio-active agent is a kind of in anion surfactant, cats product, the nonionogenic tenside.
4. the method for preparing alumina porous ceramic by the described milk sap attached gel of claim 1 molding process is characterized in that dispersion agent, organic monomer, linking agent, catalyst levels are respectively 0.1～3.0%, 3～10%, 0.1～2.0%, 0.01～0.3% of alumina powder jointed quality.
5. the method for preparing alumina porous ceramic by claim 1 or 4 described milk sap attached gel molding process is characterized in that described organic monomer is a kind of in acrylamide AM, Methacrylamide MAM, propyl group acrylamide, vinyl pyrrolidone NVP, Jia Jibingxisuanyizhi, the vinylbenzene; Described linking agent is a kind of in methylene-bisacrylamide MBAM, diallyl tartrate diamide DATDA or the propenyl methyl acrylate; Described catalyzer is N, N, N ', N '-Tetramethyl Ethylene Diamine TEMED; Described dispersion agent is a kind of in tripolyphosphate ammonium or Hexamethylphosphoric acid triamide or the ammonium polyacrylate.
6. prepare the method for alumina porous ceramic by the described milk sap attached gel of claim 1 molding process, it is characterized in that described ball milling hybrid technique, ball milling speed is 20～300r/min, and the ball milling time is 0.5～12h.
7. the method for preparing alumina porous ceramic by the described milk sap attached gel of claim 1 molding process is characterized in that the volume ratio when described milk sap and suspension mix is 1: 4～8: 1; Described initiator is a persulphate, and consumption is 10～80% of a monomer mass; Described crosslinking time is 1～30min.
8. the method for preparing alumina porous ceramic by the described milk sap attached gel of claim 1 molding process is characterized in that carrying out exsiccant temperature, humidity at climatic chamber is controlled at 35～80 ℃, 30～90% respectively, and the time length is 4～12h; Carry out the exsiccant temperature at common loft drier and be controlled at 80～110 ℃, the time length is 6～36h.
9. prepare the method for alumina porous ceramic by the described milk sap attached gel of claim 1 molding process, when it is characterized in that the base substrate binder removal, temperature rise rate is 0.3～1 ℃/min, and in 300～600 ℃ of insulation 0.5～5h; Temperature rise rate is 0.5～3 ℃/min during sintering, and in 1400～1700 ℃ of insulation 1～3h.
10. prepare the method for alumina porous ceramic by claim 1 or 2 described milk sap attached gel molding process, it is characterized in that as the organism of disperse phase being: a kind of in pentamethylene, hexanaphthene, normal heptane, octane, isopropyl laurate, ethyl palmitate, the n-capric acid methyl esters.
11. prepare the method for alumina porous ceramic by claim 1 or 3 described milk sap attached gel molding process, it is characterized in that as the tensio-active agent of emulsifying agent being: a kind of in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, cetyl trimethylammonium bromide, the tween series of surfactants.
12. annotate the method that membrane process prepare alumina porous ceramic by claim 1 or 6 described milk sap attached gels, it is characterized in that as the persulphate of initiator being: a kind of in Sodium Persulfate, Potassium Persulphate, the ammonium persulphate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110035304 CN102173852B (en) | 2011-01-29 | 2011-01-29 | Method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110035304 CN102173852B (en) | 2011-01-29 | 2011-01-29 | Method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102173852A true CN102173852A (en) | 2011-09-07 |
| CN102173852B CN102173852B (en) | 2013-03-06 |
Family
ID=44517150
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110035304 Active CN102173852B (en) | 2011-01-29 | 2011-01-29 | Method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102173852B (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193394A (en) * | 2014-08-29 | 2014-12-10 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing lightweight alumina hollow sphere heat insulation product |
| CN105439565A (en) * | 2015-11-20 | 2016-03-30 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of lightweight silicon carbide ceramic friction-increasing material |
| CN107324833A (en) * | 2016-04-28 | 2017-11-07 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of porous silicon-nitride ceramic material |
| CN109627011A (en) * | 2018-12-12 | 2019-04-16 | 萍乡学院 | A kind of preparation method and porous ceramics of the porous ceramics with concentric holes |
| CN111712474A (en) * | 2017-12-19 | 2020-09-25 | 康宁股份有限公司 | Green ceramic mixture comprising stabilized emulsion and method of forming ceramic body |
| CN113172222A (en) * | 2021-04-30 | 2021-07-27 | 中南大学 | Gel-casting-process-based aluminum electrolysis metal ceramic inert anode preparation method |
| CN113185321A (en) * | 2021-05-27 | 2021-07-30 | 洛阳理工学院 | Preparation method of porous SiOC ceramic with composite pore structure |
| CN113233916A (en) * | 2021-05-20 | 2021-08-10 | 山东大学 | Preparation device and method of porous alumina microfiber based on microfluidic chip |
| CN113880551A (en) * | 2021-10-13 | 2022-01-04 | 福建省威尔陶瓷股份有限公司 | High-strength daily tableware reinforced porcelain and preparation method thereof |
| CN114105615A (en) * | 2021-09-15 | 2022-03-01 | 杭州大和江东新材料科技有限公司 | Preparation method of alumina porous ceramic |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1456535A (en) * | 2003-05-30 | 2003-11-19 | 武汉理工大学 | Process for preparing porous ceramic by water-based gel injection moulding method |
| CN1800101A (en) * | 2006-01-05 | 2006-07-12 | 南京工业大学 | Process for preparing porous ceramic materials |
-
2011
- 2011-01-29 CN CN 201110035304 patent/CN102173852B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1456535A (en) * | 2003-05-30 | 2003-11-19 | 武汉理工大学 | Process for preparing porous ceramic by water-based gel injection moulding method |
| CN1800101A (en) * | 2006-01-05 | 2006-07-12 | 南京工业大学 | Process for preparing porous ceramic materials |
Non-Patent Citations (2)
| Title |
|---|
| 刘雪丽 等: "凝胶注模制备氧化铝多孔陶瓷及性能研究", 《硅酸盐通报》, vol. 27, no. 6, 30 December 2008 (2008-12-30), pages 1162 - 1165 * |
| 谢安建 等: "微乳状液及其研究", 《阜阳师范学院学报》, no. 32, 30 December 1997 (1997-12-30), pages 38 - 41 * |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193394B (en) * | 2014-08-29 | 2016-04-20 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of preparation method of light aluminum oxide hollow ball insulating product |
| CN104193394A (en) * | 2014-08-29 | 2014-12-10 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing lightweight alumina hollow sphere heat insulation product |
| CN105439565A (en) * | 2015-11-20 | 2016-03-30 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of lightweight silicon carbide ceramic friction-increasing material |
| CN107324833B (en) * | 2016-04-28 | 2020-07-14 | 中国科学院上海硅酸盐研究所 | Preparation method of porous silicon nitride ceramic material |
| CN107324833A (en) * | 2016-04-28 | 2017-11-07 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of porous silicon-nitride ceramic material |
| CN111712474A (en) * | 2017-12-19 | 2020-09-25 | 康宁股份有限公司 | Green ceramic mixture comprising stabilized emulsion and method of forming ceramic body |
| US11505499B2 (en) | 2017-12-19 | 2022-11-22 | Corning Incorporated | Green ceramic mixtures comprising a stabilized emulsion and methods for forming a ceramic body |
| CN109627011A (en) * | 2018-12-12 | 2019-04-16 | 萍乡学院 | A kind of preparation method and porous ceramics of the porous ceramics with concentric holes |
| CN109627011B (en) * | 2018-12-12 | 2022-02-18 | 萍乡学院 | Preparation method of porous ceramic with concentric holes and porous ceramic |
| CN113172222A (en) * | 2021-04-30 | 2021-07-27 | 中南大学 | Gel-casting-process-based aluminum electrolysis metal ceramic inert anode preparation method |
| CN113233916A (en) * | 2021-05-20 | 2021-08-10 | 山东大学 | Preparation device and method of porous alumina microfiber based on microfluidic chip |
| CN113233916B (en) * | 2021-05-20 | 2022-03-11 | 山东大学 | Preparation device and method of porous alumina microfiber based on microfluidic chip |
| CN113185321A (en) * | 2021-05-27 | 2021-07-30 | 洛阳理工学院 | Preparation method of porous SiOC ceramic with composite pore structure |
| CN114105615A (en) * | 2021-09-15 | 2022-03-01 | 杭州大和江东新材料科技有限公司 | Preparation method of alumina porous ceramic |
| CN113880551A (en) * | 2021-10-13 | 2022-01-04 | 福建省威尔陶瓷股份有限公司 | High-strength daily tableware reinforced porcelain and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102173852B (en) | 2013-03-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102173852B (en) | Method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique | |
| Franks et al. | Colloidal processing: enabling complex shaped ceramics with unique multiscale structures | |
| CN102219543B (en) | Preparation method of silicon carbide porous ceramic capable of serving as high-temperature smoke dust filter | |
| US8043694B2 (en) | Impregnated ceramic foam made of recrystallized silicon carbide | |
| CN105645901B (en) | Light thermal-insulation sheet material prepared with construction refuse regenerated fine powder and preparation method thereof | |
| CN101054311B (en) | Process of preparing porous ceramic material by ''freezing-gel forming'' | |
| CN103011884B (en) | Preparation method of corundum/mullite light-weight heat insulating material | |
| CN101956091B (en) | Method for preparing titanium alloy material through gelcasting-selfpropagation high-temperature synthesis | |
| CN106965291A (en) | A kind of gel injection-moulding 3D printing preparation method of gradient ceramic | |
| CN102584329A (en) | High-porosity porous ceramic and preparation method thereof | |
| CN104129979A (en) | Calcium feldspar porous ceramics with controllable structure and adjustable performance and preparation method thereof | |
| US6171532B1 (en) | Method of stabilizing sintered foam and of producing open-cell sintered foam parts | |
| CN106518095B (en) | A kind of method that surfactant hydrophobic modifiers dispersants prepare foamed ceramics | |
| CN106830989A (en) | A kind of foam notes the method that shape low-temperature sintering of congealing into prepares iron tailings porous ceramics | |
| CN105777082B (en) | A kind of method that starch pregel consolidation in-situ forming prepares nano aluminium oxide ceramics | |
| CN104446625A (en) | High-porosity porous ceramic and preparation method thereof | |
| CN110294636A (en) | A kind of lightweight heat-proof metallurgy of nickel waste residue foamed ceramics and preparation method thereof | |
| CN109678478A (en) | A kind of light, high-intensitive and lower thermal conductivity anorthite porous ceramic film material and preparation method thereof | |
| Gülsoy et al. | Sintered foams from precipitation hardened stainless steel powder | |
| CN105036788A (en) | Preparation method of foamed ceramic | |
| CN102515819A (en) | Preparation method of porous zirconium dioxide ceramics | |
| CN102517469A (en) | Method for preparing porous material | |
| Lorignon et al. | From wastes to interconnected porous monolith: Upcycling of Al-based metal organic framework via pickering emulsion template | |
| CN107935628A (en) | A kind of properties of SiC foam ceramics and preparation method thereof | |
| CN102976758B (en) | Preparation method of macroporous interconnection SiC ceramics |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |