CN105541306A - Alumina fiber reinforced alumina closed-cell foamed ceramic and preparation method thereof - Google Patents
Alumina fiber reinforced alumina closed-cell foamed ceramic and preparation method thereof Download PDFInfo
- Publication number
- CN105541306A CN105541306A CN201510990632.1A CN201510990632A CN105541306A CN 105541306 A CN105541306 A CN 105541306A CN 201510990632 A CN201510990632 A CN 201510990632A CN 105541306 A CN105541306 A CN 105541306A
- Authority
- CN
- China
- Prior art keywords
- foamed ceramics
- alumina
- cell foamed
- aluminum oxide
- closed cell
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/10—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 based on aluminium oxide
-
- C04B35/803—
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/522—Oxidic
- C04B2235/5224—Alumina or aluminates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5276—Whiskers, spindles, needles or pins
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
Abstract
The invention discloses alumina fiber reinforced alumina closed-cell foamed ceramic and a preparation method thereof. Service temperature of the alumina fiber reinforced alumina closed-cell foamed ceramic is lower than 1700 DEG C, compressive strength is 7 MPa to 10 MPa, heating permanent linear shrinkage under 1600 DEG C is less than 1.5 percent multiplied by 24 hours, a heat conductivity coefficient of a hot surface of 1000 DEG C is 0.40 to 0.60 W/m.K, volume density is 0.7 to 1.0 g/cm<3>, and porosity is 75 to 83 percent; content of Al2O3 of chemical compositions is not less than 95 wt%; a principal crystalline phase of the foamed ceramic is alpha-Al2O3; a micro phase also comprises mullite produced by high-temperature reaction between silica sol and alpha-Al2O3. According to the alumina fiber reinforced alumina closed-cell foamed ceramic and the preparation method thereof disclosed by the invention, in a manner of combining pore-forming agent adding with a foaming method, the prepared foamed ceramic is of a closed-cell structure, and is high in porosity and has good mechanical property; the alumina fiber reinforced alumina closed-cell foamed ceramic can be used as a fire-proof insulating material, and is applied to the fields of high-temperature electric furnace linings, building materials and the like.
Description
Technical field
The invention belongs to foamed ceramics technical field, be specifically related to aluminum oxide closed cell foamed ceramics of a kind of sapphire whisker enhancing and preparation method thereof.
Background technology
Foamed ceramics can be divided into closed cell foamed ceramics and open celled foam pottery by relation between hole.Alumina Foam Ceramics is owing to having high specific surface area, complicated pore distribution, pore size is controlled, there is good chemical stability simultaneously, the advantages such as thermostability and higher physical strength, are applied to the fields such as melted metal filtering, support of the catalyst, heat preserving and insulating material and material of construction.According to the difference of its application, also there is corresponding preparation method.
The slurry utilizing polyurethane sponge oxide impregnation aluminium powder form and aluminium dihydrogen phosphate to make in the paper " urethane template low-temperature growth Alumina Foam Ceramics strainer " delivered, obtain hanging biscuit, prepare Alumina Foam Ceramics strainer through 800 DEG C of pyrolysis.The volume density of foamed ceramics is 1.21g/cm
3, its folding strength reaches as high as 4.55MPa.The hole dimension of the porous ceramic film material adopting Polymeric sponge method to obtain and structure depend on hole dimension and the structure of the organic foam selected completely, also relevant with the slurry thickness be coated in eyed structure.It is higher and be the foamed ceramics of perforate that this method can prepare porosity, but the mechanical property of goods is poor, and organism loss on ignition is very large.
Adding pore-forming material method is before the preparation of preform blank, adds the pore-forming material occupying certain space volume.In follow-up sintering process, the pore-forming material of low ignition point is sintered vaporization and leaves matrix, thus in base substrate, go into certain hole, realizes the preparation of foamed ceramics.In foamed ceramics, shape and the distribution of pore-forming material are depended in the shape of pore and distribution, and advantage to obtain complex-shaped, that pore is different foam materials, and weak point is that the distributing homogeneity of pore is bad.The patent No. is that CN103787691A to disclose with the blend of water and pentamethylene as pore-forming material, is solidified by the polyreaction of polyethers, then through perforate process, obtained Alumina Foam Ceramics after high temperature sintering.Shortcoming needs extra perforate process, and in oxy-acetylene environment, will add operation easier.
When foamed ceramics is as heat preserving and insulating material, in order to make its thermal conductivity lower, foamed ceramics is needed to have higher porosity of holding one's breath.Foaming is suitable for height and holds one's breath the preparation of porosity stupalith, and the foamed ceramics void content prepared is large, intensity is high.Patent No. CN104311118A discloses and add polyose organic blowing agent and sintering aid etc. in ceramic powder, after 120 ~ 180 DEG C of foamed solidifications, burns till obtained ultralight Alumina Foam Ceramics, and shortcoming is that interpolation polysaccharide content is high, blowing temperature is high.In addition, foaming is prepared in porous ceramics process and is also easily occurred efflorescence peeling phenomenon.
Summary of the invention
The object of this invention is to provide aluminum oxide closed cell foamed ceramics of a kind of sapphire whisker enhancing and preparation method thereof, the foamed ceramics stable performance prepared, density is little, intensity is high.
To achieve these goals, the technical solution adopted in the present invention is: the aluminum oxide closed cell foamed ceramics that a kind of sapphire whisker strengthens, its use temperature <1700 DEG C, ultimate compression strength is 7MPa ~ 10MPa, heating permanent line shrinks (1600 DEG C × 24h) <1.5%, 1000 DEG C of hot side thermal conductivitys are 0.40 ~ 0.60W/mK, and volume density is 0.7 ~ 1.0g/cm
3, void content is 75 ~ 83%; Al in chemical constitution
2o
3content>=95wt%, the principal crystalline phase of foamed ceramics is the α-Al of matrix and reinforcement
2o
3, Micro Phases also comprises the mullite etc. that silicon sol and matrix and reinforcement pyroreaction produce.
Aluminum oxide closed cell foamed ceramics that a kind of sapphire whisker strengthens and preparation method thereof, comprises the following steps:
(1) ceramic size is prepared
By weight ratio, get alumina short fibre 10 ~ 30wt%, α-Al
2o
3powder 55 ~ 75wt%, pore-forming material 1 ~ 2%, rheological agent 0 ~ 1wt%, binding agent 5 ~ 15wt%, sintering aid 2 ~ 3wt%, abundant mix and blend, obtains the slurry with certain rheological properties energy;
(2) ceramic green is made
After adding the whipping agent of 2 ~ 5wt% in slurry after thorough mix-ing, heated and stirred 20 ~ 40s at 70 ~ 80 DEG C, until slurry foaming, before slurry does not produce and caves in, inject premolding non-porous mold, obtain wet base, and maintenance 0.5 ~ 1h at 70 ~ 75 DEG C is transferred in climatic chamber together with mould, treat base substrate curing and demolding, then be placed in blast dry oven dry 4 ~ 5h at 80 ~ 90 DEG C, obtain green compact;
(3) high temperature sintering is shaped
Green compact are placed in retort furnace, are warming up to 900 ± 50 DEG C with the temperature rise rate of 3 DEG C/min from 100 ± 10 DEG C, insulation 50 ~ 70min; Be warming up to 1600 ~ 1650 DEG C with 5 DEG C/min from 900 ± 50 DEG C again, and be incubated 100 ~ 120min, through mechanical process after furnace cooling, obtain aluminum oxide closed cell foamed ceramics.
In step (1), described pore-forming material is one in calcium sulfate or Graphite Powder 99 or its mixture, rheological agent is carboxymethyl cellulose, in binding agent, low temperature bonding agent is polyacrylamide, high-temperature agglomerant is one in silicon sol or Alumina gel or its mixture, and sintering aid is one in kaolin or wilkinite or its mixture.
Further, the preparation technology of Alumina gel is as follows: by anhydrous AlCl
3water-soluble with Al micro mist according to mol ratio 1:5, be placed in reactor, at 90 ~ 100 DEG C after back flow reaction 2 ~ 3h, filter obtain Alumina gel.
Further, the preparation technology of silicon sol is as follows: get tetraethoxy (TEOS) and dehydrated alcohol (EtOH) mixing as A liquid; Concentrated nitric acid (HNO is added in distilled water
3) and Glacial acetic acid (HAc) as B liquid; A liquid is slowly injected B liquid while stirring, and after leaving standstill 0.5 ~ 1h, be silicon sol, wherein, the volume ratio of each reactant is TEOS:ETOH:HNO
3: HAc=2.5:1:0.3:0.3.
In step (1), the preparation technology of alumina short fibre is as follows: alumina gel fiber is placed in retort furnace, is warming up to 500 DEG C, and is incubated 0.5 ~ 1h with 2 DEG C/min from 100 DEG C, the broken staple fibre forming 3 ~ 5mm after furnace cooling.
In step (2), whipping agent is one or its mixture of hydrogen peroxide or calcium carbonate.
Compared with prior art, advantage of the present invention is:
(1) adopt sapphire whisker as reinforcement, utilize the extracting of fiber, bridging, the enhanced mechanism such as crack deflection, improve the fracture toughness property of foamed ceramics matrix.
(2) material such as silicon sol and matrix at high temperature On In-situ Synthesis of Mullite Whisker etc., improves the intensity of foamed ceramics, plays effect toughness reinforcing further, and what some glassy phases that high temperature is formed simultaneously can reduce foamed ceramics effectively falls slag and efflorescence.
(3) mode adopting foaming to combine with pore-forming material method, obtained Minute pores is evenly distributed, and when not reducing ceramic ultimate compression strength, improves its void content further, and then improves the thermal and insulating performance of foamed ceramics.
Accompanying drawing explanation
Fig. 1 is the pictorial diagram of the aluminum oxide closed cell foamed ceramics that sapphire whisker of the present invention strengthens.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further described.
Embodiment 1:
Ethanol (EtOH) mixing of the tetraethoxy (TEOS) and 20ml of getting 50ml is as A liquid; Concentrated nitric acid (the HNO of 6ml is added in the water of 50ml
3) and the Glacial acetic acid (HAc) of 6ml as B liquid; A liquid is slowly injected B liquid while stirring, and after leaving standstill 0.5 ~ 1h, be silicon sol, the silicon sol particle size analysis prepared is little, diameter Distribution is narrow, stable performance, can preserve more than 20h.
Alumina gel fiber is put into retort furnace, is warming up to 500 DEG C with the temperature rise rate of 2 DEG C/min from 100 DEG C, and is incubated 0.5 ~ 1h, make gelled fibre carbonization, after furnace cooling, be broken into the staple fibre of 3 ~ 5mm.
Get the α-Al of 30wt% alumina short fibre and 55wt%
2o
3powder, adds Graphite Powder 99 2.0wt%, carboxymethyl cellulose 1.0wt%, polyacrylamide 1.0wt%, kaolin 2.0wt%, silicon sol 6.0% and appropriate distilled water, abundant mix and blend, obtains the slurry with certain rheological properties energy.After adding the calcium carbonate of 3.0wt% again, 70 DEG C of heated and stirred 30s, acidic silicasol and calcium carbonate reaction, slurry foaming, volumetric expansion.
Before foam collapse, above-mentioned slurry is injected premolding non-porous mold, obtains wet base, and it is complete to be transferred in climatic chamber maintenance 0.5h post-foaming at 70 DEG C together with mould.Treat base substrate curing and demolding, then put into blast dry oven 85 DEG C of dry 5h, obtain green compact.Green compact are warming up to 900 DEG C with 3 DEG C/min from 100 DEG C, insulation 60min, then are warming up to 1600 DEG C with 5 DEG C/min, and are incubated 120min, then with stove naturally cooling.Object is that the volatile gases produced at cold stage organism is slowly overflowed from ceramic matrix, forms pumiceous texture.Make ceramic matrix can not produce the defects such as tiny crack because internal stress is excessive simultaneously, ensure that the intensity of foamed ceramics.After mechanical process, obtain aluminum oxide closed cell foamed ceramics, as shown in Figure 1.
The alkaline reagents hydrolysis method such as ammoniacal liquor are added in the many employings of silicon sol of current preparation.Shortcoming is that ammoniacal liquor volatilization can produce very strong pungency, and the particle size analysis of secondly preparation is reunited greatly, easily, and the shelf time is short.If the too high meeting of the temperature rise rate of sintering process causes cracking, the distortion of material, if too low meeting slows down the densification process between crystal grain, reduce the performance of goods, and current consumption increases.Through test of many times, adopt the sintering process in the present embodiment more reasonable.
The aluminum oxide closed cell foamed ceramics principal crystalline phase that the sapphire whisker adopting above-mentioned method for making to obtain strengthens is the α-Al of sapphire whisker and matrix
2o
3, organism etc. volatilize completely when high temperature, and main in sample is aluminium, oxygen, silicon and some other trace element containing element.The volume density of this Alumina Foam Ceramics is about 0.75g/cm
3, void content is about 83%.1000 DEG C of hot side thermal conductivitys are about 0.42W/mK, and heating permanent line shrinks (1600 DEG C × 24h) and is about 1.3%, and ultimate compression strength is about 7.6MPa.
Embodiment 2:
30g Aluminum chloride anhydrous is dissolved in 500ml water, then puts into reactor with 30.3g aluminium micro mist, 90 ~ 100 DEG C of reflux 2 ~ 3h, filter and obtain Alumina gel (Al
2o
3massfraction be about 12.1%).Its zeta-potential value is about 35mV, and Absorbable organic halogens is saved to more than 3d.
Get the α-Al of 20wt% alumina short fibre and 60wt%
2o
3powder, adds calcium sulphate dihydrate 2.0wt%, carboxymethyl cellulose 1.0wt%, polyacrylamide 1.0wt%, Alumina gel 8wt%, wilkinite 3.0wt%.Abundant mix and blend after adding appropriate distilled water, obtains the slurry with certain rheological properties energy.After adding the superoxol of 5.0wt% again, 70 DEG C of heated and stirred 40s, until slurry foaming.
Before foam collapse, above-mentioned slurry is injected premolding non-porous mold, obtains wet base, and it is complete to be transferred in climatic chamber maintenance 1.0h post-foaming at 75 DEG C together with mould.Treat base substrate curing and demolding, then put into blast dry oven 90 DEG C of dry 4h, obtain green compact.Green compact are warming up to 850 DEG C with 3 DEG C/min from 100 DEG C, insulation 70min, then are warming up to 1650 DEG C with the temperature rise rate of 5 DEG C/min from 850 DEG C, and are incubated 100min, then with stove naturally cooling.After mechanical process, obtain aluminum oxide closed cell foamed ceramics.
Adopt the inorganic salt of aluminium to replace hydrolysis of alkoxide to prepare Alumina gel, preparation time is short, method is simple, raw material is cheap.By controlling stoichiometric ratio, Heating temperature and heat-up time, the Alumina gel that availability can be stable.
The volume density of the Alumina Foam Ceramics that the sapphire whisker adopting above-mentioned method for making to obtain strengthens is about 0.80g/cm
3, void content is about 80%, and 1000 DEG C of hot side thermal conductivitys are about 0.48W/mk, and heating permanent line shrinks (1600 DEG C × 24h) and is about 1.2%, and ultimate compression strength is about 8.1MPa.
Embodiment 3:
Get the α-Al of 15wt% alumina short fibre and 65wt%
2o
3powder, and add calcium sulphate dihydrate 2.0wt%, polyacrylamide 1.0wt%, Alumina gel 5.0wt%, silicon sol 6.0%, abundant mix and blend after wilkinite 3.0wt% and appropriate distilled water, obtain having certain rheological properties can slurry.After adding the calcium carbonate of 3.0% again, 70 DEG C of heated and stirred 20s, acidic silicasol and calcium carbonate reaction, slurry foaming, generation volumetric expansion.
Before foam collapse, above-mentioned slurry is injected premolding non-porous mold, obtains wet base, and it is complete to be transferred in climatic chamber maintenance 0.5h post-foaming at 75 DEG C together with mould.Treat base substrate curing and demolding, then put into blast dry oven 80 DEG C of dry 4.5h, obtain green compact.Green compact are warming up to 950 DEG C with 3 DEG C/min from 100 DEG C, insulation 50min, then with 5 DEG C/min to 1600 DEG C, and be incubated 120min, then with stove naturally cooling.After processing treatment, obtain aluminum oxide closed cell foamed ceramics.
The volume density of the Alumina Foam Ceramics that the sapphire whisker adopting above-mentioned method for making to obtain strengthens is about 0.90g/cm
3, void content is about 78%.1000 DEG C of hot side thermal conductivitys are about 0.54W/mK, and heating permanent line shrinks (1600 DEG C × 24h) and is about 1.1%, and ultimate compression strength is about 8.9MPa.
Embodiment 4:
Get the α-Al of 10wt% alumina short fibre and 75wt%
2o
3powder, adds Graphite Powder 99 2.0wt%, carboxymethyl cellulose 1.0wt%, polyacrylamide 0.5wt%, Alumina gel 4.5wt%, kaolin 2.0wt% and appropriate distilled water, abundant mix and blend, obtains the slurry with certain rheological properties energy.Add the superoxol (H of 5wt% again
2o
2content is 30%) after, 80 DEG C of heated and stirred 20s, slurry foaming, volumetric expansion.
Before foam collapse, above-mentioned slurry is injected premolding non-porous mold, obtains wet base, and it is complete to be transferred in climatic chamber maintenance 1.0h post-foaming at 75 DEG C together with mould.Treat base substrate curing and demolding, then put into blast dry oven 85 DEG C of dry 4.5h, obtain green compact.Green compact are warming up to 900 DEG C with the temperature rise rate of 3 DEG C/min from 100 DEG C, insulation 50min, then are warming up to 1600 DEG C with 5 DEG C/min, and are incubated 120min, with stove naturally cooling.After mechanical process, obtain aluminum oxide closed cell foamed ceramics.
The volume density of the Alumina Foam Ceramics that the sapphire whisker adopting above-mentioned method for making to obtain strengthens is about 1.0g/cm
3, void content is about 75%.1000 DEG C of hot side thermal conductivitys are about 0.59W/mK, and heating permanent line shrinks (1600 DEG C × 24h) and is about 1.0%, and ultimate compression strength is about 9.9MPa.
Comparative example 1:
Do not add alumina short fibre in comparative example 1, other implementation processes are with embodiment 1.The volume density of the Alumina Foam Ceramics obtained is about 1.3g/cm
3, void content is about 67%.1000 DEG C of hot side thermal conductivitys are about 0.67W/mK, and heating permanent line shrinks (1600 DEG C × 24h) and is about 0.73%, and ultimate compression strength is about 6.1MPa.
Comparative example 2:
Add the alumina short fibre in the replacement of the commercial alumina staple fibre after burning till through 1200 DEG C embodiment 1 in comparative example 2, other implementation processes are with embodiment 1.The volume density of the Alumina Foam Ceramics obtained is about 1.1g/cm
3, void content is about 70%.1000 DEG C of hot side thermal conductivitys are about 0.63W/mK, and heating permanent line shrinks (1600 DEG C × 24h) and is about 0.88%, and ultimate compression strength is about 7.2MPa.
Comparative example 3:
Do not add whipping agent in comparative example 3, other implementation processes are with embodiment 2.The volume density of the Alumina Foam Ceramics obtained is about 2.1g/cm
3, void content is about 53%.1000 DEG C of hot side thermal conductivitys are about 0.74W/mK, and heating permanent line shrinks (1600 DEG C × 24h) and is about 0.69%, and ultimate compression strength is about 8.4MPa.
Comparative example 4:
Do not add sintering aid and high-temperature agglomerant in comparative example 4, other implementation processes are with embodiment 1.The volume density of the Alumina Foam Ceramics obtained is about 0.66g/cm
3, void content is about 86%.1000 DEG C of hot side thermal conductivitys are about 0.38W/mK, and heating permanent line shrinks (1600 DEG C × 24h) and is about 0.9%, and ultimate compression strength is about 3.5MPa.
By relatively finding, adopt carbonization sapphire whisker not only can improve the void content of foamed ceramics, the mechanism such as the extracting of fiber, unsticking, bridging also can be utilized matrix to be played to the effect of reinforcement.Compare and adopt single pore-forming material method, adopt foaming to combine with pore-forming material method, can further improve its void content.Add sintering aid and high-temperature agglomerant and can reduce sintering temperature, what what reaction in－situ generated simultaneously can reduce foamed ceramics under room temperature as mullite crystal whisker etc. falls slag and efflorescence.
Claims (8)
1. the aluminum oxide closed cell foamed ceramics of a sapphire whisker enhancing, it is characterized in that, its use temperature <1700 DEG C, ultimate compression strength is 7MPa ~ 10MPa, heating permanent line under 1600 DEG C × 24h shrinks <1.5%, 1000 DEG C of hot side thermal conductivitys are 0.40 ~ 0.60W/mK, and volume density is 0.7 ~ 1.0g/cm
3, void content is 75 ~ 83%; Al in chemical constitution
2o
3content>=95wt%, the principal crystalline phase of foamed ceramics is α-Al
2o
3, Micro Phases also comprises silicon sol and α-Al
2o
3the mullite that pyroreaction produces.
2. an aluminum oxide closed cell foamed ceramics for sapphire whisker enhancing as claimed in claim 1, it is characterized in that, described foamed ceramics is prepared by following steps:
(1) ceramic size is prepared
By weight ratio, get alumina short fibre 10 ~ 30wt%, α-Al
2o
3powder 55 ~ 75wt%, pore-forming material 1 ~ 2%, rheological agent 0 ~ 1wt%, binding agent 5 ~ 15wt%, sintering aid 2 ~ 3wt%, abundant mix and blend, obtains the slurry with certain rheological properties energy;
(2) ceramic green is made
After adding the whipping agent of 2 ~ 5wt% in slurry after thorough mix-ing, heated and stirred 20 ~ 40s at 70 ~ 80 DEG C, until slurry foaming, before slurry does not produce and caves in, inject premolding non-porous mold, obtain wet base, and maintenance 0.5 ~ 1h at 70 ~ 75 DEG C is transferred in climatic chamber together with mould, treat base substrate curing and demolding, then be placed in blast dry oven dry 4 ~ 5h at 80 ~ 90 DEG C, obtain green compact;
(3) high temperature sintering is shaped
Green compact are placed in retort furnace, are warming up to 900 ± 50 DEG C with the temperature rise rate of 3 DEG C/min from 100 ± 10 DEG C, insulation 50 ~ 70min; Be warming up to 1600 ~ 1650 DEG C with 5 DEG C/min from 900 ± 50 DEG C again, and be incubated 100 ~ 120min, through mechanical process after furnace cooling, obtain described foamed ceramics.
3. the aluminum oxide closed cell foamed ceramics of sapphire whisker enhancing as claimed in claim 2, it is characterized in that, in step (1), described pore-forming material is one in calcium sulfate or Graphite Powder 99 or its mixture, rheological agent is carboxymethyl cellulose, and in binding agent, low temperature bonding agent is polyacrylamide, high-temperature agglomerant is one in silicon sol or Alumina gel or its mixture, and sintering aid is one in kaolin or wilkinite or its mixture.
4. the aluminum oxide closed cell foamed ceramics of sapphire whisker enhancing as claimed in claim 3, it is characterized in that, the preparation technology of Alumina gel is as follows: by anhydrous AlCl
3water-soluble with Al micro mist according to mol ratio 1:5, be placed in reactor, at 90 ~ 100 DEG C after back flow reaction 2 ~ 3h, filter obtain Alumina gel.
5. the aluminum oxide closed cell foamed ceramics that strengthens of sapphire whisker as claimed in claim 3, it is characterized in that, the preparation technology of silicon sol is as follows: get tetraethoxy and dehydrated alcohol mixing as A liquid; Dense HNO is added in distilled water
3with Glacial acetic acid as B liquid; A liquid is slowly injected B liquid while stirring, and after leaving standstill 0.5 ~ 1h, be silicon sol, wherein, the volume ratio of each reactant is tetraethoxy: dehydrated alcohol: HNO
3: Glacial acetic acid=2.5:1:0.3:0.3.
6. the aluminum oxide closed cell foamed ceramics of sapphire whisker enhancing as claimed in claim 2, it is characterized in that, in step (1), the preparation technology of alumina short fibre is as follows: alumina gel fiber is placed in retort furnace, 500 DEG C are warming up to from 100 DEG C with 2 DEG C/min, and be incubated 0.5 ~ 1h, the broken staple fibre forming 3 ~ 5mm after furnace cooling.
7. the aluminum oxide closed cell foamed ceramics of sapphire whisker enhancing as claimed in claim 2, it is characterized in that, in step (2), whipping agent is one or its mixture of hydrogen peroxide or calcium carbonate.
8. the preparation method of the aluminum oxide closed cell foamed ceramics of sapphire whisker enhancing as claimed in claim 1 or 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510990632.1A CN105541306B (en) | 2015-12-25 | 2015-12-25 | A kind of aluminium oxide closed cell foamed ceramics and preparation method thereof of alumina fibre enhancing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510990632.1A CN105541306B (en) | 2015-12-25 | 2015-12-25 | A kind of aluminium oxide closed cell foamed ceramics and preparation method thereof of alumina fibre enhancing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105541306A true CN105541306A (en) | 2016-05-04 |
| CN105541306B CN105541306B (en) | 2018-09-25 |
Family
ID=55820931
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510990632.1A Active CN105541306B (en) | 2015-12-25 | 2015-12-25 | A kind of aluminium oxide closed cell foamed ceramics and preparation method thereof of alumina fibre enhancing |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105541306B (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187117A (en) * | 2016-07-12 | 2016-12-07 | 南京理工宇龙新材料科技股份有限公司 | A kind of heat-barrier material based on branch construct aluminium oxide and preparation method thereof |
| CN106278341A (en) * | 2016-08-17 | 2017-01-04 | 柳州市亿廷贸易有限责任公司 | Anticracking floor tile |
| CN106673703A (en) * | 2016-11-29 | 2017-05-17 | 清华大学 | Preparation method of light-weight and high-strength zirconium oxide-reinforced porous aluminum oxide ceramic |
| CN107417288A (en) * | 2017-09-07 | 2017-12-01 | 济宁学院 | Alumina fibre enhancing nano aluminium oxide foamed ceramics and preparation method thereof |
| CN108484006A (en) * | 2018-03-09 | 2018-09-04 | 清华大学 | A kind of preparation method of the multi-stage porous Alumina Foam Ceramics to match in excellence or beauty with aeroge |
| CN109081688A (en) * | 2018-08-27 | 2018-12-25 | 芜湖市元奎新材料科技有限公司 | A kind of method that alumina fibre enhancing opoka prepares mullite porous ceramic |
| CN109180141A (en) * | 2018-08-31 | 2019-01-11 | 南通江山农药化工股份有限公司 | Alumina aerogels are insulated soft felt and its moulding process |
| CN110002855A (en) * | 2018-12-20 | 2019-07-12 | 江苏和腾热工装备科技有限公司 | A kind of high temperature resistant foamed ceramics and preparation method thereof prepared by FCC dead catalyst |
| CN110156446A (en) * | 2019-04-08 | 2019-08-23 | 启东市聚旺铸造有限公司 | The production method of ceramic mold for casting hollow turbo blade |
| CN110924588A (en) * | 2019-11-22 | 2020-03-27 | 山东理工大学 | Multifunctional light high-strength microcrystal foaming wall material suitable for assembly type building |
| CN111792944A (en) * | 2020-06-04 | 2020-10-20 | 上海利物盛企业集团有限公司 | Method for preparing foamed ceramic material by using foamed silica gel and inorganic powder compound as precursor |
| CN112500183A (en) * | 2021-02-01 | 2021-03-16 | 中南大学 | Preparation method of alumina fiber reinforced high-temperature-resistant anti-scouring heat-insulating material |
| CN113563101A (en) * | 2021-08-20 | 2021-10-29 | 山东鲁阳浩特高技术纤维有限公司 | Inorganic fiber foamed ceramic and preparation method thereof |
| CN115448748A (en) * | 2022-08-24 | 2022-12-09 | 佛山市陶本科技有限公司 | High-fire-resistance, extreme-high-strength foamed ceramic and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446635A (en) * | 2014-11-10 | 2015-03-25 | 西北工业大学 | Method for preparing closed-pore porous heat-insulating alumina ceramic |
| CN104496522A (en) * | 2014-12-02 | 2015-04-08 | 航天特种材料及工艺技术研究所 | Method for preparing aluminum oxide/mullite foamed ceramic |
| CN104876637A (en) * | 2015-05-25 | 2015-09-02 | 中航复合材料有限责任公司 | Fiber-reinforced pure inorganic flame retardant foam composite and preparation method thereof |
| CN105175001A (en) * | 2015-09-01 | 2015-12-23 | 中国科学院重庆绿色智能技术研究院 | Ultralight closed cell foam ceramic preparation |
-
2015
- 2015-12-25 CN CN201510990632.1A patent/CN105541306B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446635A (en) * | 2014-11-10 | 2015-03-25 | 西北工业大学 | Method for preparing closed-pore porous heat-insulating alumina ceramic |
| CN104496522A (en) * | 2014-12-02 | 2015-04-08 | 航天特种材料及工艺技术研究所 | Method for preparing aluminum oxide/mullite foamed ceramic |
| CN104876637A (en) * | 2015-05-25 | 2015-09-02 | 中航复合材料有限责任公司 | Fiber-reinforced pure inorganic flame retardant foam composite and preparation method thereof |
| CN105175001A (en) * | 2015-09-01 | 2015-12-23 | 中国科学院重庆绿色智能技术研究院 | Ultralight closed cell foam ceramic preparation |
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187117A (en) * | 2016-07-12 | 2016-12-07 | 南京理工宇龙新材料科技股份有限公司 | A kind of heat-barrier material based on branch construct aluminium oxide and preparation method thereof |
| CN106187117B (en) * | 2016-07-12 | 2019-05-24 | 南京理工宇龙新材料科技股份有限公司 | A kind of heat-barrier material and preparation method thereof based on branch construct aluminium oxide |
| CN106278341A (en) * | 2016-08-17 | 2017-01-04 | 柳州市亿廷贸易有限责任公司 | Anticracking floor tile |
| CN106673703A (en) * | 2016-11-29 | 2017-05-17 | 清华大学 | Preparation method of light-weight and high-strength zirconium oxide-reinforced porous aluminum oxide ceramic |
| CN107417288A (en) * | 2017-09-07 | 2017-12-01 | 济宁学院 | Alumina fibre enhancing nano aluminium oxide foamed ceramics and preparation method thereof |
| CN108484006A (en) * | 2018-03-09 | 2018-09-04 | 清华大学 | A kind of preparation method of the multi-stage porous Alumina Foam Ceramics to match in excellence or beauty with aeroge |
| CN109081688A (en) * | 2018-08-27 | 2018-12-25 | 芜湖市元奎新材料科技有限公司 | A kind of method that alumina fibre enhancing opoka prepares mullite porous ceramic |
| CN109180141A (en) * | 2018-08-31 | 2019-01-11 | 南通江山农药化工股份有限公司 | Alumina aerogels are insulated soft felt and its moulding process |
| CN110002855B (en) * | 2018-12-20 | 2021-12-28 | 江苏和腾热工装备科技有限公司 | High-temperature-resistant foamed ceramic prepared from FCC (fluid catalytic cracking) waste catalyst and preparation method thereof |
| CN110002855A (en) * | 2018-12-20 | 2019-07-12 | 江苏和腾热工装备科技有限公司 | A kind of high temperature resistant foamed ceramics and preparation method thereof prepared by FCC dead catalyst |
| CN110156446A (en) * | 2019-04-08 | 2019-08-23 | 启东市聚旺铸造有限公司 | The production method of ceramic mold for casting hollow turbo blade |
| CN110924588A (en) * | 2019-11-22 | 2020-03-27 | 山东理工大学 | Multifunctional light high-strength microcrystal foaming wall material suitable for assembly type building |
| CN110924588B (en) * | 2019-11-22 | 2022-02-22 | 山东理工大学 | Multifunctional light high-strength microcrystal foaming wall material suitable for assembly type building |
| CN111792944A (en) * | 2020-06-04 | 2020-10-20 | 上海利物盛企业集团有限公司 | Method for preparing foamed ceramic material by using foamed silica gel and inorganic powder compound as precursor |
| CN111792944B (en) * | 2020-06-04 | 2022-07-12 | 上海利物盛企业集团有限公司 | Method for preparing foamed ceramic material by using foamed silica gel and inorganic powder compound as precursor |
| CN112500183A (en) * | 2021-02-01 | 2021-03-16 | 中南大学 | Preparation method of alumina fiber reinforced high-temperature-resistant anti-scouring heat-insulating material |
| CN112500183B (en) * | 2021-02-01 | 2021-05-04 | 中南大学 | Preparation method of alumina fiber reinforced high-temperature-resistant anti-scouring heat-insulating material |
| CN113563101A (en) * | 2021-08-20 | 2021-10-29 | 山东鲁阳浩特高技术纤维有限公司 | Inorganic fiber foamed ceramic and preparation method thereof |
| CN113563101B (en) * | 2021-08-20 | 2023-01-24 | 山东鲁阳浩特高技术纤维有限公司 | Inorganic fiber foamed ceramic and preparation method thereof |
| CN115448748A (en) * | 2022-08-24 | 2022-12-09 | 佛山市陶本科技有限公司 | High-fire-resistance, extreme-high-strength foamed ceramic and preparation method thereof |
| CN115448748B (en) * | 2022-08-24 | 2023-09-22 | 佛山市陶本科技有限公司 | Foamed ceramic with high fire resistance and high limit strength and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105541306B (en) | 2018-09-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105541306A (en) | Alumina fiber reinforced alumina closed-cell foamed ceramic and preparation method thereof | |
| CN103011884B (en) | Preparation method of corundum/mullite light-weight heat insulating material | |
| CN105481355A (en) | Zirconia fiber-reinforced alumina closed-cell foam ceramic and preparation method thereof | |
| CN102010222B (en) | Silicon carbide porous ceramic and preparation method thereof | |
| CN103145444B (en) | Method for preparing heat-insulation lightweight porous mullite ceramic at low cost | |
| CN104987124B (en) | Cubic-phase zirconia fiber reinforced zirconia foamed ceramics and preparation method therefor | |
| CN101955371B (en) | Method for preparing closed pore foam ceramic | |
| CN106220218A (en) | A kind of ceramic foam filter and manufacture method thereof | |
| CN101967064A (en) | Protein foaming method for preparing porous ceramics composite material | |
| CN102643111A (en) | Preparation method for porous ceramics | |
| CN110294636B (en) | Light heat-insulating nickel metallurgy waste residue foamed ceramic and preparation method thereof | |
| CN102617180A (en) | Porous foamed ceramic and preparation method thereof | |
| CN108484194A (en) | A kind of Al2O3-SiO2Based composites and its fast preparation method | |
| CN106478077A (en) | A kind of porous thermal insulating ceramic material for building and preparation method thereof | |
| CN108863421A (en) | A kind of preparation method of fiber reinforcement anti-thermal shock foamed ceramics | |
| CN106396731A (en) | Refractory material with heat insulation and heat preservation as well as preparation method thereof | |
| CN104003755A (en) | Process for preparing ventilating brick by using polishing waste residue | |
| CN103467072A (en) | Preparation method for light microporous corundum ceramic | |
| CN104987115A (en) | Method for preparing heat-insulation heat-preservation ceramic by utilizing potassium hexatitanate whiskers | |
| CN107043224A (en) | Foam glass-SiO2Method for producing aerogels | |
| CN103058701A (en) | Preparation method for porous silicon nitride composite ceramic | |
| CN106431434B (en) | A kind of obturator-type alumina base mullite material and preparation method thereof | |
| CN100582059C (en) | Method for preparing foam silicon nitride ceramics | |
| CN107353027A (en) | Zirconium oxide closed cell foamed ceramics of Zirconium oxide fibre enhancing and preparation method thereof | |
| CN106396726A (en) | Porous refractory material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |