CN108863435A - A method of Alumina Foam Ceramics are prepared from gel forming by Aluminum sol - Google Patents
A method of Alumina Foam Ceramics are prepared from gel forming by Aluminum sol Download PDFInfo
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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Abstract
The present invention develops a kind of method for preparing Alumina Foam Ceramics from gel forming by Aluminum sol, and this method comprises the following steps：1) Aluminum sol that solid concentration is 15~35wt% is prepared；2) surfactant is added in the Aluminum sol obtained by step 1) to foam；3) coagulant is added in step 2) gains；4) step 3) gains are toppled over into injection molding, it is dry after demoulding；5) step 4) gains are sintered, obtain Al2O3Foamed ceramics.The green body and foamed ceramics of high porosity high intensity can be obtained in the method, and compression strength is 0.4~7.9MPa, α-Al when the green body porosity is 63.1~94.5%2O3Compression strength is 26.1~97.8MPa when the porosity of foamed ceramics is 66.0~92.6%, and the compression strength under the identical porosity is about 2 times of other methods, can satisfy foamed ceramics in the application demand in mechanics direction.In addition, molding mode is simple, can prepare the foamed ceramics of specific shape, have broad application prospects from gel solidification under the action of inorganic coagulant after Aluminum sol foams in the present invention.
Description
Technical field
The invention belongs to foamed ceramics technical fields, and in particular to one kind prepares alumina bubble from gel forming by Aluminum sol
The method of foam ceramics.
Background technique
Foamed ceramics combines the characteristics of foamed material and ceramic material, has low-density, high-specific surface area, Gao Biqiang
Degree, high temperature resistant, it is corrosion-resistant, wear-resistant the advantages that, can be widely used in filtering, absorption, catalysis, in heat-insulation and heat-preservation field.Foam
The preparation process of ceramics mainly has addition pore creating material method, Polymeric sponge method and direct foaming.Adding pore creating material method can be with
Regulate and control the size and shape of stomata, but the porosity is lower, generally 50% hereinafter, be mainly used in general filter.It is organic
Foam impregnation method can prepare the foamed ceramics of high porosity, aperture, but wherein the exclusion of organic matter pollutes the environment.And it is direct
Foaming can prepare high porosity, high-intensitive foamed ceramics, and preparation process is fairly simple.
Direct foaming is to be introduced directly into bubble by modes such as stirrings in the slurry, and the foamed slurry formed at this time is one
A thermodynamic unstable system can be added surfactant, high molecular polymer and solid particle and carry out stable foam slurry.However
The blank strength only obtained by stable foam slurry is lower, is unfavorable for subsequent processing and transport.It at this time can be in preparation process
Middle addition curing agent carrys out fixed foam structure, increases blank strength.Common curing method has organic matter solidification and inorganic matter solid
Change.Dumping is needed using organic matter solidification such as gel injection-moulding, and some Orqanics Monomers have toxicity, and utilizes inorganic matter solid
Change can introduce impurity if cement solidification, it is therefore desirable to develop the new preparation process of one kind to increase blank strength.
The foamed ceramics of high porosity has many excellent performances, but as the increase compression strength of the porosity can be
It reduces.In production application, the intensity for improving foamed ceramics and green body is conducive to further processing, transport and application, has real
Border meaning.
Summary of the invention
Above-mentioned background and there are aiming at the problem that, the present invention develops a kind of prepared by Aluminum sol from gel forming and aoxidizes
The method of aluminum foam ceramics combines direct foaming with collosol and gel, and operation is very simple, and injection molding is convenient, molten using aluminium
Glue is formed from gel solidification, is conducive to the foamed ceramics for preparing specific shape, and coagulant is inorganic matter, no dumping mistake
Journey, additive amount is considerably less, only plays a part of to accelerate gel, not as curing agent.The present invention can prepare high porosity, high intensity
Foamed ceramics, compression strength of the foamed ceramics under the identical porosity is about 2 times of other methods.
The present invention is as follows using technical solution.
A method of Alumina Foam Ceramics being prepared from gel forming by Aluminum sol, are included the following steps：
(1) Aluminum sol powder is dissolved in and prepares the Aluminum sol that solid concentration is 15~35wt% in deionized water.
(2) mechanical stirring that Aluminum sol is carried out to high speed, is added the surfactant sodium dodecyl base of 0.03~0.24wt%
Sodium sulphate foams.
(3) coagulant that concentration is 0.03~0.09mmol/g is added, continues high-speed stirred.
(4) topple over injection molding, the rapid gel solidification of foamed slurry, in 20~30 DEG C, 80~95% constant temperature and humidity after demoulding
It is dry under environment.
(5) sample after drying is sintered at 400~1500 DEG C.
Aluminum sol powder used is AlO (OH), and partial size is 10~20nm.Powder is dissolved in deionized water to obtain aluminium molten
Glue.
Coagulant used can be a variety of inorganic electrolytes such as ammonium chloride, potassium chloride, potassium hydroxide, calcium chloride.Addition promotees
Solidifying agent can increase the ionic strength of slurry, compress colloid electric double layer, reduce the repulsion between colloid, accelerate the gelation of colloidal sol.
400 DEG C in step 5), 600 DEG C, 800 DEG C of sintering obtain γ-Al2O3, 1000 DEG C of sintering obtain θ-Al2O3, 1200 DEG C
And temperatures above is sintered to obtain α-Al2O3。
The aperture of foamed ceramics is 10~60 μm, α-Al2O3There are second level meso-hole structure, crystallite dimension on foamed ceramics hole wall
For nanoscale.
The present invention can obtain the green body and Alumina Foam Ceramics of high porosity high intensity, and the green body porosity is 63.1~
Compression strength is 0.4~7.9MPa, α-Al when 94.5%2O3The compression strength when porosity of foamed ceramics is 66.0~92.6%
For 26.1~97.8MPa, the compression strength under the identical porosity is about 2 times of other methods, can satisfy foamed ceramics in power
Learn the application demand in direction.
The beneficial effects of the invention are as follows：(1) present invention combines direct foaming with collosol and gel, avoids only with straight
Connect the problem of foaming obtains low-intensity ceramic body.Raw material is Aluminum sol, from gel solidification under the action of coagulant
High-intensitive ceramic body is obtained, curing agent is not needed.(2) green body and foamed ceramics prepared has high porosity high intensity,
Compression strength under the identical porosity is about 2 times of other methods, is had a clear superiority, and further adding for foamed ceramics is conducive to
Work, transport and application.(3) coagulant can be a variety of inorganic electrolytes, not need dumping, and additive amount is considerably less, and it is solidifying only to play acceleration
The effect of glue, not as curing agent.(4) it can be effectively controlled gel time by adjusting coagulation agent contents, make that there is mobility
Aluminum sol foamed slurry is cured as rapidly frothy gel after injection molding, ensure that the uniform air hole structure of foamed ceramics, is conducive to
Compression strength is improved, and the foamed ceramics with specific shape can be obtained.(5) molten by adjusting surface-active contents, aluminium
Microstructure, the porosity and the compression strength of foamed ceramics can be effectively controlled in glue solid concentration.(6)α-Al2O3Foamed ceramics has
Second level meso-hole structure is expected to be applied to filtration art.(7) 1500 DEG C of industrial alumina powder needs or more of sintering temperature, and aluminium
α-Al can be obtained in 1200 DEG C of sintering in colloidal sol2O3, sintering temperature is reduced, energy consumption is reduced.(8) it prepares raw material and there was only Aluminum sol,
A small amount of surfactant and coagulant are added later, does not introduce impurity substantially, utilize simplifying from gel solidification for foaming Aluminum sol
Preparation flow.
Detailed description of the invention
Fig. 1 is the wet base photo of foam after the method for the present invention demoulding.
Fig. 2 is the photo after the different shape foam body drying of the method for the present invention preparation.
Fig. 3 is the α-Al of the method for the present invention preparation2O3The micrograph of foamed ceramics.
Fig. 4 is the α-Al of the method for the present invention preparation2O3The micrograph of foamed ceramics hole wall.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples.
Fig. 1 is the wet base photo of foam after the method for the present invention demoulding.It can be seen that toppling over the wet base of injection molding has non-ordinary light
Sliding surface, substantially without defect, wet base conformality is good, has specific shape.
Fig. 2 is the photo after the different shape foam body drying of the method for the present invention preparation.It can be seen that dry body can be protected
Complete shape is held, there is smooth surface.
Fig. 3 is the α-Al of the method for the present invention preparation2O3The micrograph of foamed ceramics.It can be seen that air hole structure is relatively uniform, it is
10~60 μm, be conducive to improve compression strength.
Fig. 4 is the α-Al of the method for the present invention preparation2O3The micrograph of foamed ceramics hole wall.It can be seen that crystal grain is tiny, and hole
There is second level meso-hole structure on wall.
Embodiment 1
(1) Aluminum sol powder is dissolved in and prepares the Aluminum sol that solid concentration is 30wt% in deionized water.
(2) Aluminum sol is stirred under 2000rpm revolving speed with machine mixer, the lauryl sodium sulfate of 0.09wt% is added
It foams.
(3) ammonium chloride that concentration is 0.03mmol/g is added, continues high-speed stirred.
(4) topple over injection molding, sample solidifies rapidly, dry under 20 DEG C, 80% constant-temperature constant-humidity environment after demoulding.
(5) sample after drying is sintered, and 33h is warming up to 500 DEG C, keeps the temperature 1h, and 3 DEG C/min is warming up to 1200 DEG C, is protected
Warm 2h.
The porosity of green body is 81.90% after drying, compression strength 3.34MPa.Alumina Foam pottery is obtained after sintering
The porosity of porcelain is 80.69%, compression strength 66.73MPa.
Embodiment 2
(1) Aluminum sol powder is dissolved in and prepares the Aluminum sol that solid concentration is 15wt% in deionized water.
(2) Aluminum sol is stirred under 2000rpm revolving speed with machine mixer, the lauryl sodium sulfate of 0.24wt% is added
It foams.
(3) ammonium chloride that concentration is 0.09mmol/g is added, continues high-speed stirred.
(4) topple over injection molding, sample solidifies rapidly, dry under 20 DEG C, 80% constant-temperature constant-humidity environment after demoulding.
(5) sample after drying is sintered, and 33h is warming up to 500 DEG C, keeps the temperature 1h, and 3 DEG C/min is warming up to 1200 DEG C, is protected
Warm 2h.
The porosity of green body is 94.5% after drying, compression strength 0.4MPa.Alumina Foam Ceramics are obtained after sintering
The porosity be 92.6%, compression strength 26.1MPa.
Embodiment 3
(1) Aluminum sol powder is dissolved in and prepares the Aluminum sol that solid concentration is 25wt% in deionized water.
(2) Aluminum sol is stirred under 2000rpm revolving speed with machine mixer, the lauryl sodium sulfate of 0.03wt% is added
It foams.
(3) ammonium chloride that concentration is 0.06mmol/g is added, continues high-speed stirred.
(4) topple over injection molding, sample solidifies rapidly, dry under 30 DEG C, 95% constant-temperature constant-humidity environment after demoulding.
(5) sample after drying is sintered, and 33h is warming up to 500 DEG C, keeps the temperature 1h, and 3 DEG C/min is warming up to 1200 DEG C, is protected
Warm 2h.
The porosity of green body is 63.1% after drying, compression strength 7.9MPa.Alumina Foam Ceramics are obtained after sintering
The porosity be 66.0%, compression strength 97.8MPa.
Embodiment 4
(1) Aluminum sol powder is dissolved in and prepares the Aluminum sol that solid concentration is 35wt% in deionized water.
(2) Aluminum sol is stirred under 2000rpm revolving speed with machine mixer, the lauryl sodium sulfate of 0.09wt% is added
It foams.
(3) potassium chloride that concentration is 0.03mmol/g is added, continues high-speed stirred.
(4) topple over injection molding, sample solidifies rapidly, dry under 30 DEG C, 95% constant-temperature constant-humidity environment after demoulding.
(5) sample after drying is sintered, and 33h is warming up to 500 DEG C, keeps the temperature 1h, and 3 DEG C/min is warming up to 1500 DEG C, is protected
Warm 2h.
The porosity of green body is 73.8% after drying, compression strength 4.5MPa.Alumina Foam Ceramics are obtained after sintering
The porosity be 72.0%, compression strength 72.5MPa.
Technical solution of the present invention is described in detail in above-described embodiment.It is apparent that the present invention is not limited being retouched
The embodiment stated.Based on the embodiments of the present invention, those skilled in the art can also make a variety of variations accordingly, but appoint
What is equal with the present invention or similar variation shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of method for preparing Alumina Foam Ceramics from gel forming by Aluminum sol, it is characterised in that：Include the following steps：
1) Aluminum sol that solid concentration is 15~35wt% is prepared；
2) surfactant is added in the Aluminum sol obtained by step 1) to foam；
3) coagulant is added in step 2) gains；
4) step 3) gains are toppled over into injection molding, it is dry after demoulding；
5) step 4) gains are sintered.
2. according to the method for claim 1, it is characterised in that：Aluminum sol described in step 1) is dissolved in by Aluminum sol powder
Obtained in deionized water, Aluminum sol powder is AlO (OH), and partial size is 10~20nm.
3. according to the method for claim 1, it is characterised in that：Surfactant described in step 2) is dodecyl sulphate
Sodium, additive amount are 0.03~0.24wt% of Aluminum sol.
4. according to the method for claim 1, it is characterised in that：Dodecyl sulphate is added in step 2) under high velocity agitation
Sodium.
5. according to the method for claim 1, it is characterised in that：Coagulant described in step 3) is inorganic electrolyte, concentration
For 0.03~0.09mmol/g.
6. according to the method for claim 1, it is characterised in that：Green body in step 4) after demoulding 20~30 DEG C, 80~
It is dry under 95% constant-temperature constant-humidity environment.
7. according to the method for claim 1, it is characterised in that：The green body porosity in step 4) after demoulding is 63.1~
Compression strength is 0.4~7.9MPa when 94.5%.
8. according to the method for claim 1, it is characterised in that：The temperature of sintering described in step 5) is 400~1500 DEG C.
9. according to the method for claim 1, it is characterised in that：400 DEG C in step 5), 600 DEG C, 800 DEG C of sintering obtain γ-
Al2O3, 1000 DEG C of sintering obtain θ-Al2O3, 1200 DEG C and temperatures above are sintered to obtain α-Al2O3；α-the Al2O3Foamed ceramics
The porosity when being 66.0~92.6% compression strength be 26.1~97.8MPa.
10. according to the method for claim 9, it is characterised in that：The aperture of the foamed ceramics is 10~60 μm, α-Al2O3
There is second level meso-hole structure on foamed ceramics hole wall, crystallite dimension is nanoscale.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111777427A (en) * | 2020-06-24 | 2020-10-16 | 清华大学 | Preparation method of nacre-like layered high-strength super-tough ceramic |
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| CN111777427A (en) * | 2020-06-24 | 2020-10-16 | 清华大学 | Preparation method of nacre-like layered high-strength super-tough ceramic |
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