CN105565812B - A kind of preparation method of Sialon combination SiC porous material - Google Patents

A kind of preparation method of Sialon combination SiC porous material Download PDF

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CN105565812B
CN105565812B CN201510945685.1A CN201510945685A CN105565812B CN 105565812 B CN105565812 B CN 105565812B CN 201510945685 A CN201510945685 A CN 201510945685A CN 105565812 B CN105565812 B CN 105565812B
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porous material
powder
sic
sialon
preparation
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CN105565812A (en
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张欣
何建
李华臣
陈建章
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Hunan University of Science and Technology
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Abstract

A kind of preparation method of Sialon combination SiC porous material, comprising: weigh 60~80 parts by weight SiC powder, 10~20 parts by weight of activated alumina powders and 5~15 part by weight of metal silicon powders, enter ball mill grinding 3h and material powder is made；40~60 parts by weight green body reinforcing agents are weighed, 0.1~1.0 mass parts disperse adjustable solidification agent, and 0.1~1.0 mass parts silane coupling agent and material powder stir evenly obtained raw material slurry；It weighs 25 parts by weight 1wt% triterpenoid saponin plant foaming agent solution high-speed stirreds and foam is made；Foam and raw material slurry are stirred evenly into obtained foamed slurry；Foamed slurry casting, drying nitrogenize at 1400 DEG C Sialon combination SiC porous material are made.Wherein, 325 mesh of SiC Powder Particle Size and hereinafter, 200 mesh of metal Si Powder Particle Size and hereinafter, active oxidation aluminium powder be ρ-Al2O3, green body reinforcing agent is one of polyvinyl alcohol, calcium lignosulfonate and starch or its compound aqueous solution, and dispersion adjustable solidification agent is one of sodium carbonate, calgon, sodium tripolyphosphate, lithium carbonate or its is compound.

Description

A kind of preparation method of Sialon combination SiC porous material
Technical field
The invention belongs to porous material technical fields, and in particular to a kind of preparation side of Sialon combination SiC porous material Method.
Background technique
SiC material mechanical performance is excellent, and chemical stability is good, corrosion-resistant, anti-erosion, good thermal shock stability, is extremely heavy The high-temperature structural material wanted.The Si-C key of SiC is the extremely strong covalent bond of bonding force, the extremely difficult sintering of conventional method, usually addition sintering Auxiliary agent prepares SiC material using reaction sintering method, obtains silicate combination SiC, oxide combination SiC, mullite therefrom In conjunction with the various SiC products such as SiC, Si3N4 combination SiC, wherein Sialon combination SiC performance is best, and elevated temperature strength is high, heat resistanceheat resistant punching Hitting property is good, and inoxidizability, resistance to melt and soda acid aggressivity are strong etc..
The SiC porous material porosity is high, and good penetrability, sound isolating and heat insulating performance is good, has extensively in industry with high-tech area General application, throughout multiple fields such as metallurgy, chemical industry, electronics, the energy, aviation, environmental protection, biologies.For example, it is net to can be used as high-temperature gas Change the catalysis of device, solid particle and filter for molten metal, heat exchanger, sensor, heat preserving and insulating material and vehicle exhaust Agent carrier etc..
The preparation method of porous material has addition pore creating material method, Polymeric sponge method (replica method) and foaming etc..It closes Have some research papers and patent in the preparation of SiC porous material, such as:
Periodical " silicate journal " page 107 to page 112 of the 2nd phase of volume 34 in 2004 discloses what Liu Yan etc. write The article of " preparations of metallic filter high-performance SiC foam ceramics ", using Al2O3, bentonite and silica solution as sintering aid, Polyurethane foam is template, and D50 is respectively that 15.8 μm and 7.4 μm of SiC powder is raw material, and bending strength is made through 2 hangings Up to 2.87MPa, average pore size about 3mm, the good SiC foam ceramics of thermal shock resistance.
Periodical " Chinese pottery industry " page 9 to page 11 of the 1st phase of volume 20 in 2013 discloses what Guo Xingzhong etc. write The paper of " starch is that pore creating material prepares SiC porous material ", it was recently reported that using micron SiC as matrix, aluminium oxide and yttrium oxide are to burn Auxiliary agent is tied, starch is pore creating material, prepares SiC porous material using pressureless sintering technology.
" high-temperature dust removal is prepared with composite SiC porous material and performance study " (Bai Chengying, University Of Hainan's master's degree opinion Text, 2014), prepare and grind the silica that made internal disorder or usurp, mullite, cordierite combination SiC respectively using reaction in-situ combination technology Porous composite ceramics.
Patent (publication number: CN103058708A) reports a kind of system of lower thermal conductivity silicon nitride bonded silicon SiC porous material Preparation Method, preparation process are: 1) by SiC fine powder, water, dispersing agent and being used for the monomer of gel casting forming, crosslinking agent ball milling It is mixed to get uniform slurry；2) appropriate foaming agent is added in the slurry, slurry mechanical stirring is obtained into foamed slurry, to foam Appropriate initiator and catalyst are sequentially added in slurry, and Quick pouring is in mold；3) after slurry curing, demoulding obtains base Body, green body are successively dry in climatic chamber and a conventional oven；4) green body after drying is first arranged in air atmosphere stove Then glue is sintered in nitrogen atmosphere stove, finally obtain Si3N4 combination SiC porous material, can be used for aluminium cell periphery Thermal insulation material.
But so far there is not yet the research about Sialon combination SiC porous material is reported.
Summary of the invention
The present invention is a kind of preparation method of Sialon combination SiC porous material, and simple process is easy to operate, obtained Sialon combination SiC porous material bulk density it is small (be not more than 0.5g/cm3), low (1000 DEG C of the thermal coefficient of thermal coefficient No more than 0.25w/ (mk)), stomata is spherical in shape, and independent, closing state is evenly distributed, size about 0.5~1mm is mainly used for height The insulation of temperature and aggressive atmosphere.
To achieve the above object, the technical scheme adopted by the invention is that: with the SiC powder of 65~85 mass parts, 5~15 matter The active oxidation aluminium powder of the metal Si powder and 10~20 mass parts of measuring part is raw material, and corundum ball is 1~5h of abrasive media ball milling, is mixed It closes uniformly, material powder is made, the green body reinforcing agent of 40~60 mass parts is then added, the dispersion tune of 0.1~1.0 mass parts is solidifying Agent, the silane coupling agent of 0.1~1.0 mass parts, stirs evenly, and is made the moderate raw material slurry of viscosity, then with triterpenoid saponin Foams mix made from plant foaming agent is uniform, and sic foam slurry is made, through in casting, drying, industrial nitriding furnace 1400 DEG C of nitridations, are made Sialon combination SiC porous material.
In above-mentioned technical proposal: the carborundum content of SiC powder is greater than 97%, and granularity is 325 mesh and hereinafter, metal Si powder Degree is 200 mesh and hereinafter, active oxidation aluminium powder is ρ-Al2O3, green body reinforcing agent is polyvinyl alcohol, the wood of mass concentration 1~5% One of quality sulfoacid calcium and starch or its compound aqueous solution, dispersion adjustable solidification agent are sodium carbonate, calgon, trimerization phosphorus One of sour sodium, lithium carbonate or its is compound.
By adopting the above technical scheme, active oxidation aluminium powder (ρ-Al2O3) hydrate is formed after aquation, it is thickened foamed slurry And solid bubble effect being played, and assign porous body certain dry tenacity, 500 DEG C or so decomposition of hydrate generate extremely fine Aluminium oxide particles；Metallic silicon power nitrogenizes in nitrogen atmosphere generates extremely fine silicon nitride particles, atomic thin nitridation silicon grain Son reacts at high temperature with aluminium oxide particles generates Sialon, and silicon-carbide particle is combined, and Sialon is thus made and combines SiC porous material.Addition dispersion adjustable solidification agent dispersion carborundum particle simultaneously adjusts ρ-Al2O3Heat evolution velocity, add silane coupling agent Improve the interfacial combined function of foam and SiC particulate.For the baked strength for enhancing porous body, use mass concentration for 1~5% One of polyvinyl alcohol, calcium lignosulfonate and starch or its compound aqueous solution as green body reinforcing agent.Adjust foam Bulk density can be made down to 0.4g/cm in amount3Sialon combination SiC porous material.
After measured, bulk density prepared by the present invention is 0.5g/cm3Sialon combination SiC porous material, room temperature pressure resistance Intensity 1.5MPa, 1000 DEG C of thermal coefficients are 0.243w/ (m.k), and XRD interpretation of result shows that principal crystalline phase is α-SiC and β- Sialon。
Specific embodiment
Below with reference to specific example, the present invention is described in further detail.
The present invention is not limited by the following examples, can determine according to the technique and scheme of the present invention with actual conditions specific Embodiment.
Embodiment 1:
A kind of preparation method of Sialon combination SiC porous material.With
A, 80 parts by weight, 325 mesh SiC powder, 12.5 parts by weight ρ-Al are weighed2O3With 7.5 parts by weight, 200 mesh metal Si powder, add Enter and grind 3h into the ball mill that corundum ball is abrasive media, material powder is made, it is spare.
B, the green body reinforcing agent that 45~50 parts by weight mass concentrations are 2% is weighed, 0.1~0.4 parts by weight disperse adjustable solidification agent, 0.2~0.5 parts by weight silane resin acceptor kh-550 is added to step A through being sufficiently stirred obtained in mixed uniformly material powder The moderate raw material slurry of viscosity.
C, the foaming agent solution that 25 parts by weight mass concentrations are 1% is weighed, using high-speed mixer with 2500r.p.m machinery Foaming agent solution 3min is stirred, foam is made；
D, appropriate foam is added in raw material slurry, stirs, keeps slurry uniform with foams mix, foamed slurry is made.
E, by foamed slurry injection molding, one day is stood under air environment, makes foamed slurry curing molding, wet base is made.
F, wet base being placed in oven and dried, room temperature is slowly dry to 60 DEG C, and heating rate is not more than 2.5 DEG C/h, and 60 DEG C Drying demoulds afterwards for 24 hours, then rises to 110 DEG C with the speed of 5 DEG C/h, for 24 hours, dry body is made in heat preservation.
G, dry body nitrogenizes in industrial nitriding furnace at 1400 DEG C, and bulk density about 0.6g/cm is thus made3Sialon knot Close SiC porous material.
Embodiment 2:
A kind of preparation method of Sialon combination SiC porous material.With
A, the ρ-Al of 75 parts by weight, 325 mesh SiC powder, 15 parts by weight is weighed2O3With 10 parts by weight, 200 mesh metal Si powder, it is added 3h is ground into the ball mill that corundum ball is abrasive media, material powder is made, it is spare.
B, the green body reinforcing agent that 50~55 parts by weight mass concentrations are 2% is weighed, 0.1~0.4 parts by weight disperse adjustable solidification agent, 0.2~0.5 parts by weight silane resin acceptor kh-550 is added to step A through preparation is sufficiently stirred in mixed uniformly material powder The moderate raw material slurry of viscosity.
C, the foaming agent solution that 25 parts by weight mass concentrations are 1% is weighed, high-speed mixer turning with 2500r.p.m is used Foam is made in fast mechanical stirring foaming agent solution 3min.
D, appropriate foam is added in raw material slurry, stirs, keeps slurry uniform with foams mix, foamed slurry is made.
E, by foamed slurry injection molding, one day is stood under air environment, makes foamed slurry curing molding, wet base is made.
F, wet base being placed in oven and dried, room temperature is slowly dry to 60 DEG C, and heating rate is not more than 2.5 DEG C/h, and 60 DEG C Drying demoulds afterwards for 24 hours, then rises to 110 DEG C with the speed of 5 DEG C/h, for 24 hours, dry body is made in heat preservation.
G, dry body nitrogenizes in industrial nitriding furnace at 1400 DEG C, and bulk density about 0.5g/cm is thus made3Sialon knot Close SiC porous material.
Embodiment 3:
A kind of preparation method of Sialon combination SiC porous material.With
A, 70 parts by weight d are weighed50ρ-the Al of=1.5 μm of SiC powder, 20 parts by weight2O3With 10 parts by weight, 325 mesh metal Si Powder is added in the ball mill that corundum ball is abrasive media and grinds 3h, and material powder is made, spare.
B, the green body reinforcing agent that 55~60 parts by weight mass concentrations are 2% is weighed, 0.2~0.5 parts by weight disperse adjustable solidification agent, 0.2~0.5 parts by weight silane resin acceptor kh-550 is added to step A through preparation is sufficiently stirred in mixed uniformly material powder The moderate raw material slurry of viscosity.
C, the foaming agent solution that 25 parts by weight mass concentrations are 1% is weighed, high-speed mixer turning with 2500r.p.m is used Foam is made in fast mechanical stirring foaming agent solution 3min.
D, appropriate foam is added in raw material slurry, stirs, keeps slurry uniform with foams mix, foamed slurry is made.
E, by foamed slurry injection molding, one day is stood under air environment, makes foamed slurry curing molding, wet base is made.
F, wet base being placed in oven and dried, room temperature is slowly dry to 60 DEG C, and heating rate is not more than 2.5 DEG C/h, and 60 DEG C Drying demoulds afterwards for 24 hours, then rises to 110 DEG C with the speed of 5 DEG C/h, for 24 hours, dry body is made in heat preservation.
G, dry body nitrogenizes in industrial nitriding furnace at 1400 DEG C, and bulk density about 0.4g/cm is thus made3Sialon knot Close SiC porous material.
Above-described embodiment has stronger adaptability and preferable implementation result, can increase according to actual needs in specific implementation Subtract non-essential technical characteristic, to meet the needs of different situations.
The comparison of above-described embodiment and the prior art is as follows:
The present invention uses high pure raw material, does not introduce harmful components, the high-temperature behavior of material is guaranteed.ρ-Al2O3With very High activity, easily aquation form the adhesive bond of some strength, solidify foamed slurry using this characteristic.
ρ-Al in the present invention2O3500 DEG C of hydrated product or so decomposition generate atomic thin aluminium oxide particles, with silicon powder nitrogen Change the atomic thin silicon nitride particles formed and react generation Sialon at high temperature, silicon-carbide particle is combined, is thus made Sialon combination SiC porous material.
The present invention uses foam that can more accurately adjust the volume of product by changing foam additional amount as stomata source Density, the porosity and aperture.
Entire technical process of the invention not can cause environmental pollution, and be a kind of environmental-friendly technique, and operate letter It is single.
The above, preferable specific embodiment only of the invention, but scope of protection of the present invention is not limited thereto, Within the technical scope of the present disclosure, any changes or substitutions that can be easily thought of by anyone skilled in the art, It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims Subject to enclosing.

Claims (7)

1. a kind of preparation method of Sialon combination SiC porous material, it is characterised in that: with the SiC powder of 65~85 mass parts, 5 The metal Si powder of~15 mass parts and the active oxidation aluminium powder of 10~20 mass parts are raw material, and corundum ball is abrasive media ball milling 1 ~5h is uniformly mixed obtained material powder, and 40~60 mass parts green body reinforcing agents are then added, and the dispersion of 0.1~1.0 mass parts is adjusted Solidifying agent, 0.1~1.0 mass parts silane coupling agent stir evenly the moderate raw material slurry of obtained viscosity, then plant with triterpenoid saponin Sic foam slurry is uniformly made in foams mix made from object foaming agent, through in casting, drying, industrial nitriding furnace 1400 DEG C nitrogenize be made Sialon combination SiC porous material, the active oxidation aluminium powder be ρ-Al2O3。
2. the preparation method of Sialon combination SiC porous material according to claim 1, it is characterised in that: the SiC Powder carborundum content is greater than 97%, and granularity is 325 mesh and following.
3. the preparation method of Sialon combination SiC porous material according to claim 1, it is characterised in that: the gold Belonging to Si Powder Particle Size is 200 mesh and following.
4. the preparation method of Sialon combination SiC porous material according to claim 1, it is characterised in that: the green body Reinforcing agent is one of polyvinyl alcohol, calcium lignosulfonate and starch of mass concentration 1~5% or its compound aqueous solution.
5. the preparation method of Sialon combination SiC porous material according to claim 1, it is characterised in that: point Scattered adjustable solidification agent is one of sodium carbonate, calgon, sodium tripolyphosphate, lithium carbonate or its is compound.
6. the preparation method of Sialon combination SiC porous material according to claim 1, it is characterised in that: the silicon Alkane coupling agent is KH-550.
7. a kind of Sialon combination SiC porous material, combined as the Sialon described in any one of according to claim 1~6 It is obtained prepared by the preparation method of SiC porous material.
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