CN107721448A - A kind of preparation method of the mullite porous ceramic rich in whisker structure - Google Patents
A kind of preparation method of the mullite porous ceramic rich in whisker structure Download PDFInfo
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- CN107721448A CN107721448A CN201711036117.5A CN201711036117A CN107721448A CN 107721448 A CN107721448 A CN 107721448A CN 201711036117 A CN201711036117 A CN 201711036117A CN 107721448 A CN107721448 A CN 107721448A
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- C04B35/18—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 silicates other than clay rich in aluminium oxide
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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Abstract
The invention belongs to the preparation field of porous ceramic film material, and in particular to a kind of preparation method of the mullite porous ceramic rich in whisker structure.Its preparation process can be realized as follows:Ball milling mixing is carried out as initiation material dispensing using deionized water, dispersant, ceramic powder, mineralizer, monomer, crosslinking agent, obtains the slurry of stably dispersing;Foaming agent is added in the stable slurry of gained, mechanical agitation obtains foamed slurry, and initiator and catalyst are then sequentially added into foamed slurry, and is cast in gel solidification in mould and is molded;Base substrate after the demoulding is dried, obtains foam base substrate;Dried foam base substrate is placed in aluminum oxide saggar, and is placed in air atmosphere stove is sintered together, obtains the mullite porous ceramic rich in whisker structure.The present invention physically well develops with whisker structure, and draw ratio is big, and the strength of materials is high, and thermal conductivity is low, the characteristics of good thermal shock.
Description
Technical field
The invention belongs to the preparation field of porous ceramic film material, and in particular to a kind of mullite rich in whisker structure
The preparation method of ceramics.
Background technology
Porous ceramic film material has the advantages that low-density, lower thermal conductivity, high-specific surface area, high transmittance, high temperature insulating,
The fields such as catalyst carrier, filtrating smoke dust all have wide practical use;Mullite ceramic material has lower thermal conductivity and low-heat
The coefficient of expansion, applied in thermal-energy equipment field;Mullite porous ceramic material has the two advantage concurrently, is that high temperature kiln is heat-insulated
One of important candidate material of furnace lining.
The conventional preparation method of mullite porous ceramic mainly has following several at present:Granulation mass area method, addition pore creating material
Method, foaming etc.;Wherein, granulation mass area method is the preparation that loose structure is realized in the space formed using particle packing, addition
Pore creating material method is to add pore creating material in dispensing, and loose structure is ultimately formed by being ablated off pore creating material in sintering process.This
The porous ceramic film material porosity prepared by two methods is relatively low, and thermal conductivity is higher, it is impossible to plays good heat-blocking action;Foaming
Method is to add surfactant in ceramic slurry to make slurry foam, and so as to introduce stomata inside ceramics, forms loose structure;
The mullite porous ceramic porosity prepared by this method is high, and thermal conductivity is low, but asks there is also low intensity, thermal shock resistance are poor etc.
Topic.
The content of the invention
In order to solve the above technical problems, the purpose of the present invention is to propose to a kind of mullite porous ceramic rich in whisker structure
Preparation method.
The present invention adopts the following technical scheme that to complete above-mentioned purpose:
A kind of preparation method of the mullite porous ceramic rich in whisker structure, described preparation method include foam base substrate
Prepare the sintering with base substrate;Its concrete technology step is:
1)The preparation of foam base substrate:
Using deionized water, dispersant, ceramic powder, mineralizer, monomer, crosslinking agent as initiation material dispensing, and carry out ball milling and mix
Close, obtain the slurry of stably dispersing;Described ceramic powder includes the powder as silicon source and the powder as silicon source;The work
The 70~74% of ceramic powder quality is accounted for for the addition of the powder of silicon source;The addition of the powder as silicon source accounts for ceramics
The 26~30% of powder quality;The addition of the deionized water is 0.5~1 times of ceramic powder quality;The dispersant adds
Enter 0.5~0.8% that amount is ceramic powder quality;The addition of the mineralizer is the 5~10% of ceramic powder quality;The list
The addition of body is the 5~15% of ceramic powder quality;The addition of the crosslinking agent is the 0.5~1.5% of ceramic powder quality;
Foaming agent is added in the stable slurry of gained, mechanical agitation obtains foamed slurry, then sequentially adds and draws into foamed slurry
Agent and catalyst are sent out, and Quick pouring gel solidification in mould is molded;Base substrate after the demoulding is dried, obtains foam base
Body;
2)The sintering of base substrate:
Dried foam base substrate is placed in aluminum oxide saggar, and is placed in air atmosphere stove is sintered together, obtains richness
Mullite porous ceramic containing whisker structure.
The powder as silicon source is α-Al2O3Micro mist, γ-Al2O3One kind in micro mist, described α-Al2O3Micro mist
Purity>99%, average grain diameter is 3~6 μm;Described γ-Al2O3The purity of micro mist>99%, average grain diameter is 1~3 μm.
The powder as silicon source is fused quartz powder, one kind in Cab-O-sil, the purity of described fused quartz powder>
99%, average grain diameter is 5~10 μm;The purity of described Cab-O-sil>99%, average grain diameter is 5~10 μm.
Described mineralizer is one kind in aluminum fluoride, sodium fluoride.
Described monomer is one kind in acrylamide, Methacrylamide.
Described crosslinking agent is methylene-bisacrylamide.
Described dispersant is one kind in sodium tripolyphosphate, Hexamethylphosphoric acid triamide, polyacrylamide.
Described foaming agent is one kind in dodecyl sulphate amine, dodecyltriethanolamine sulfate, and addition is pottery
The 4~8% of porcelain powder quality.
Described initiator is ammonium persulfate, and addition is the 0.8~4% of ceramic powder quality;Described catalyst is N,
N, N ', N '-tetramethylethylenediamine, addition is the 0.05~0.2% of ceramic powder quality;
Described ball milling mixing, ball milling speed are 30~100r/min, and Ball-milling Time is 1~8h;Described mechanical agitation speed
For 80~200r/min, mixing time is 0.5~1.5h.
Described base substrate after the demoulding is dried, and is first to be protected in climatic chamber under 60 DEG C and 70% relative humidity
Hold 10~14h, then 100 DEG C of insulation 5h in air dry oven;Described sintering process refer to 1300~1600 DEG C be incubated 2~
5h。
The preparation method of a kind of mullite porous ceramic rich in whisker structure proposed by the present invention, first with foaming
Attached gel casting prepares the porous ceramics base substrate comprising silicon source and silicon source, and inside has substantial amounts of pore structure, to burn
Mullite vapor phase growth during knot provides the space of abundance;The mullite rich in whisker structure prepared using this method
Porous ceramic structure is uniform, and whisker structure physically well develops, and draw ratio is big, and the strength of materials is high, and thermal conductivity is low, good thermal shock.
Brief description of the drawings
Fig. 1 show the fracture apperance photo of the mullite porous ceramic rich in whisker structure prepared by embodiment 1.
Embodiment
The present invention is illustrated with reference to following embodiments and accompanying drawing:
Embodiment 1:
Deionized water 100g, polyacrylamide 0.6g are weighed, average grain diameter is 6 μm of α-Al2O3Micro mist 72g, average grain diameter are
10 μm of Cab-O-sil 28g, sodium fluoride 10g, acrylamide 10g, methylene-bisacrylamide 1.0g, it is situated between by ball milling of alumina balls
Matter, with 50r/min rotating speed mixing 5h.Dodecyltriethanolamine sulfate 8g is added in gained slurry, is existed with mixer
Mechanical agitation 0.5h under 200r/min rotating speeds, add ammonium persulfate 1.5g, N, N, N ', N '-tetramethylethylenediamine 0.1g, by it
It is poured into mould, stands curing and demolding.Base substrate after the demoulding is first protected in climatic chamber under 60 DEG C and 70% relative humidity
Hold 14h, then 100 DEG C of insulation 5h in air dry oven.Dried base substrate is placed in aluminum oxide saggar and burnt together in high temperature
In freezing of a furnace 2h is incubated in 1600 DEG C.The porosity of prepared mullite porous ceramic is 85%, compressive resistance 16MPa, its fracture
Pattern photo is as shown in Figure 1.
Embodiment 2:
Deionized water 75g, Hexamethylphosphoric acid triamide 0.5g are weighed, average grain diameter is 3 μm of γ-Al2O3Micro mist 74g, average grain diameter 5
μm fused quartz powder 26g, aluminum fluoride 10g, Methacrylamide 15g, methylene-bisacrylamide 1.5g, using alumina balls as
Ball-milling medium, with 80r/min rotating speed mixing 4h.Dodecyl sulphate amine 4g is added in gained slurry, is existed with mixer
Mechanical agitation 1h under 160r/min rotating speeds, add ammonium persulfate 1g, N, N, N ', N '-tetramethylethylenediamine 0.1g, poured into a mould
Into mould, curing and demolding is stood.Base substrate after the demoulding is first kept in climatic chamber under 60 DEG C and 70% relative humidity
10h, then 100 DEG C of insulation 5h in air dry oven.Dried base substrate is placed in aluminum oxide saggar together in high temperature sintering
In stove 4h is incubated in 1400 DEG C.The porosity of prepared mullite porous ceramic is 72%, compressive resistance 20MPa.
Embodiment 3:
Deionized water 100g, polyacrylamide 0.7g are weighed, average grain diameter is 1 μm of γ-Al2O3Micro mist 70g, average grain diameter are
10 μm of Cab-O-sil 30g, sodium fluoride 5g, acrylamide 15g, methylene-bisacrylamide 1.5g, it is situated between by ball milling of alumina balls
Matter, with 50r/min rotating speed mixing 6h.Dodecyltriethanolamine sulfate 6g is added in gained slurry, is existed with mixer
Mechanical agitation 1h under 120r/min rotating speeds, add ammonium persulfate 2g, N, N, N ', N '-tetramethylethylenediamine 0.1g, poured into a mould
Into mould, curing and demolding is stood.Base substrate after the demoulding is first kept in climatic chamber under 60 DEG C and 70% relative humidity
12h, then 100 DEG C of insulation 5h in air dry oven.Dried base substrate is placed in aluminum oxide saggar together in high temperature sintering
In stove 2h is incubated in 1600 DEG C.The porosity of prepared mullite porous ceramic is 81%, compressive resistance 17MPa.
Embodiment 4:
Deionized water 75g, sodium tripolyphosphate 0.8g are weighed, average grain diameter is 6 μm of α-Al2O3Micro mist 74g, average grain diameter are 5 μ
M Cab-O-sil 26g, aluminum fluoride 5g, Methacrylamide 10g, methylene-bisacrylamide 1.0g, it is situated between by ball milling of alumina balls
Matter, with 100r/min rotating speed mixing 1h.Dodecyl sulphate amine 8g is added in gained slurry, with mixer in 200r/min
Mechanical agitation 0.5h under rotating speed, add ammonium persulfate 4g, N, N, N ', N '-tetramethylethylenediamine 0.05g, it is poured into mould
In tool, curing and demolding is stood.Base substrate after the demoulding first keeps 14h in climatic chamber under 60 DEG C and 70% relative humidity, then
100 DEG C of insulation 5h in air dry oven.By dried base substrate be placed in aluminum oxide saggar together in high temperature sintering furnace in
1500 DEG C of insulation 3h.The porosity of prepared mullite porous ceramic is 82%, compressive resistance 17MPa.
Embodiment 5:
Deionized water 50g, Hexamethylphosphoric acid triamide 0.6g are weighed, average grain diameter is 3 μm of α-Al2O3Micro mist 70g, average grain diameter 10
μm fused quartz powder 30g, sodium fluoride 10g, acrylamide 5g, methylene-bisacrylamide 0.5g, using alumina balls as ball milling
Medium, with 30r/min rotating speed mixing 8h.Dodecyltriethanolamine sulfate 4g is added in gained slurry, is existed with mixer
Mechanical agitation 1.5h under 80r/min rotating speeds, add ammonium persulfate 0.8g, N, N, N ', N '-tetramethylethylenediamine 0.2g, by it
It is poured into mould, stands curing and demolding.Base substrate after the demoulding is first protected in climatic chamber under 60 DEG C and 70% relative humidity
Hold 10h, then 100 DEG C of insulation 5h in air dry oven.Dried base substrate is placed in aluminum oxide saggar and burnt together in high temperature
In freezing of a furnace 5h is incubated in 1300 DEG C.The porosity of prepared mullite porous ceramic is 74%, compressive resistance 20MPa.
Claims (10)
- A kind of 1. preparation method of the mullite porous ceramic rich in whisker structure, it is characterised in that:Described preparation method bag Include the preparation of foam base substrate and the sintering of base substrate;Its concrete technology step is:1)The preparation of foam base substrate:Using deionized water, dispersant, ceramic powder, mineralizer, monomer, crosslinking agent as initiation material dispensing, and carry out ball milling and mix Close, obtain the slurry of stably dispersing;Described ceramic powder includes the powder as silicon source and the powder as silicon source;The work The 70~74% of ceramic powder quality is accounted for for the addition of the powder of silicon source;The addition of the powder as silicon source accounts for ceramics The 26~30% of powder quality;The addition of the deionized water is 0.5~1 times of ceramic powder quality;The dispersant adds Enter 0.5~0.8% that amount is ceramic powder quality;The addition of the mineralizer is the 5~10% of ceramic powder quality;The list The addition of body is the 5~15% of ceramic powder quality;The addition of the crosslinking agent is the 0.5~1.5% of ceramic powder quality; Foaming agent is added in the stable slurry of gained, mechanical agitation obtains foamed slurry, then sequentially adds and draws into foamed slurry Agent and catalyst are sent out, and Quick pouring gel solidification in mould is molded;Base substrate after the demoulding is dried, obtains foam base Body;2)The sintering of base substrate:Dried foam base substrate is placed in aluminum oxide saggar, and is placed in air atmosphere stove is sintered together, obtains richness Mullite porous ceramic containing whisker structure.
- A kind of 2. preparation method of the mullite porous ceramic rich in whisker structure as claimed in claim 1, it is characterised in that: The powder as silicon source is α-Al2O3Micro mist, γ-Al2O3One kind in micro mist, described α-Al2O3The purity of micro mist> 99%, average grain diameter is 3~6 μm;Described γ-Al2O3The purity of micro mist>99%, average grain diameter is 1~3 μm.
- A kind of 3. preparation method of the mullite porous ceramic rich in whisker structure as claimed in claim 1, it is characterised in that: The powder as silicon source is fused quartz powder, one kind in Cab-O-sil, the purity of described fused quartz powder>99%, it is average Particle diameter is 5~10 μm;The purity of described Cab-O-sil>99%, average grain diameter is 5~10 μm.
- A kind of 4. preparation method of the mullite porous ceramic rich in whisker structure as claimed in claim 1, it is characterised in that: Described mineralizer is one kind in aluminum fluoride, sodium fluoride.
- A kind of 5. preparation method of the mullite porous ceramic rich in whisker structure as claimed in claim 1, it is characterised in that: Described monomer is one kind in acrylamide, Methacrylamide.
- A kind of 6. preparation method of the mullite porous ceramic rich in whisker structure as claimed in claim 1, it is characterised in that: Described crosslinking agent is methylene-bisacrylamide;Described dispersant is sodium tripolyphosphate, Hexamethylphosphoric acid triamide, polyacrylamide In one kind.
- A kind of 7. preparation method of the mullite porous ceramic rich in whisker structure as claimed in claim 1, it is characterised in that: Described foaming agent is one kind in dodecyl sulphate amine, dodecyltriethanolamine sulfate, and addition is ceramic powder constitution The 4~8% of amount.
- A kind of 8. preparation method of the mullite porous ceramic rich in whisker structure as claimed in claim 1, it is characterised in that: Described initiator is ammonium persulfate, and addition is the 0.8~4% of ceramic powder quality;Described catalyst is N, N, N ', N '- Tetramethylethylenediamine, addition are the 0.05~0.2% of ceramic powder quality.
- A kind of 9. preparation method of the mullite porous ceramic rich in whisker structure as claimed in claim 1, it is characterised in that: Described ball milling mixing, ball milling speed are 30~100r/min, and Ball-milling Time is 1~8h;Described mechanical agitation speed is 80 ~200r/min, mixing time are 0.5~1.5h.
- 10. a kind of preparation method of the mullite porous ceramic rich in whisker structure as claimed in claim 1, its feature exist In:Described base substrate after the demoulding is dried, be first in climatic chamber holding 10 under 60 DEG C and 70% relative humidity~ 14h, then 100 DEG C of insulation 5h in air dry oven;Described sintering process refers to be incubated 2~5h at 1300~1600 DEG C.
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CN111056834A (en) * | 2019-12-17 | 2020-04-24 | 洛阳索莱特材料科技有限公司 | Preparation method of spinel-mullite ceramic sagger |
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CN108975948A (en) * | 2018-08-27 | 2018-12-11 | 芜湖市元奎新材料科技有限公司 | A kind of preparation method of foam mullite porous ceramic |
CN110590349A (en) * | 2019-10-15 | 2019-12-20 | 北京中环鑫汇科技有限公司 | Low-heat-conduction high-temperature furnace lining material and preparation method thereof |
CN111056834A (en) * | 2019-12-17 | 2020-04-24 | 洛阳索莱特材料科技有限公司 | Preparation method of spinel-mullite ceramic sagger |
CN111056834B (en) * | 2019-12-17 | 2022-02-18 | 洛阳索莱特材料科技有限公司 | Preparation method of spinel-mullite ceramic sagger |
CN111533571A (en) * | 2020-05-26 | 2020-08-14 | 长安大学 | High-toughness mullite ceramic with whisker frame and preparation method thereof |
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