CN103641510A - Method for preparing O-Sialon porous ceramic by adding PMMA (polymethyl methacrylate) pore forming agent - Google Patents
Method for preparing O-Sialon porous ceramic by adding PMMA (polymethyl methacrylate) pore forming agent Download PDFInfo
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Abstract
The invention relates to a method for preparing an O-Sialon porous ceramic by adding a PMMA (polymethyl methacrylate) pore forming agent, and the method is used for preparing the O-Sialon porous ceramic through spray granulation and in situ sintering. The method comprises the following steps: by using absolute ethyl alcohol as a dispersion medium, PVB (polyvinyl butyral) as a dispersing agent and a binder, and PEG-400 and n-butanol as a plasticizer to uniformly disperse ceramic powder and PMMA, performing spray granulation, forming, tape-ranking and sintering to obtain the product. The density of the obtained product is 1.35-1.75g.cm<-3>, the porosity is between 40-60%, the room temperature flexure strength is between 50-120MPa, the heat conductivity coefficient is between 0.90-2.25W/mK, and the microstructure is uniform.
Description
Technical field
The invention belongs to porous ceramic film material technical field, be specifically related to be a kind of by add pore-forming material prepare O ?the method of Sialon porous ceramics.This material has low thermal conductivity, and lower volume density has higher bending strength, can be used as high temperature insulating material and uses.
Background technology
The features such as it is high that porous ceramics has porosity, and volume density is little, and specific surface area is large, the speciality of the vesicular structure that it is special and material itself combines, and has excellent over-all properties.In addition, porous material is high temperature resistant, and corrosion resistance is good, and chemical stability is high, and good stability of the dimension has excellent heat-proof quality, and as high temperature insulating material, application prospect is very wide.
O ?Sialon (Si
2 ?xa1
xo
1+xn
2 ?x; 0 < x≤0.3) be Al atomic substitutions Si
2n
2a part of Si atom in O and the continuous solid solution that forms, O ?Sialon retained Si
3n
4advantageous property, and compare Si
3n
4be easy to sintering, simultaneously because autologous density is low, the advantage such as resistance toheat and corrosion resistance is good, long service life makes it have very large application space.In addition, O ?Sialon pottery oxygen level relatively high, so antioxidant property is excellent.O ?Sialon porous material can be regarded as O ?the complex body of Sialon and pore, had both O ?the advantage of Sialon material and porous material, there is density low, high temperature resistant, the features such as high-temperature oxidation resistance excellence, the excellent candidate of high temperature insulating material, therefore to O ?the research of Sialon porous ceramics significant.
For preparation Sialon porous ceramics, there is at present multiple preparation technology, wherein pore-forming material method is to prepare a kind of important process of porous ceramics, the feature of this technique is by add the pore-forming material of easy volatile in ceramic batch, utilize pore-forming material in base substrate, to occupy certain space, then after sintering, pore-forming material leaves matrix and forms pore and prepare porous ceramics.Add pore-forming material and can form the hole of holding one's breath, make sintered article both there is high void content, there is again good intensity.
(the Liang little Ying such as Liang little Ying, Li Jianfeng. add pore-forming material legal system for porous silicon nitride ceramic [J]. Chinese science and technology information, 2008,12:083.) by adding gac, as pore-forming material, prepared porous silicon nitride ceramic, the ceramic void content preparing is greater than 70%, and average bending strength is greater than 8MPa.
Zhang Guo ?(the Yang J F such as Jun, Zhang G J, Ohji T.Fabrication of low shrinkage, porous silicon nitride ceramics by addition of a small amount of carbon.Journal of the American Ceramic Society, 2001,84 (7): 1639 ?1641) with Y
2o
3for sintering aid, add a small amount of powdered carbon (1 ?5vol%) and prepared the porous silicon nitride ceramic of low-shrinkage, and the impact of the powdered carbon of having studied different-grain diameter size (13nm and 5 μ m) on the performance of material.Result shows, the Si preparing
3n
4pottery porosity can reach 50% ?60%, and intensity is 100MPa.Adding carbon dust can significantly increase the void content of material and reduce its shrinking percentage.
Chinese patent 102351563(Chen Fei, Pan Haoliang, Shen Qiang etc., the preparation method with the high porosity porous SiN ceramic of multi-stage porous gauge structure) disclose a kind of take silicone resin as binding agent and aperture pore-forming material, naphthalene powder be macropore pore-forming material, preparation has the method for the porous SiN ceramic of multi-stage porous gauge structure, and the pottery preparing has the excellent properties such as pore size distribution is wide, even pore distribution, porosity is high, mechanical strength is better.
Chinese patent 102850084A(Peng Hong; Li Shaorong, a kind of preparation method of take the porous ceramics that organic resin foam microspheres is pore-forming material) a kind of preparation method who utilizes the porous ceramics that organic resin foam microspheres is pore-forming material is disclosed, by the granulation of sieving, shaped by fluid pressure, preparing Production of Ceramics, to go out aperture even, the porous ceramics that pore size is controlled, has improved the sintering qualified rate of product greatly.
PMMA microballoon is a kind of pore-forming material of excellent performance, by controlling its particle diameter and add-on, can obtain the controlled material of porosity and aperture.At interpolation PMMA microballoon, prepare in the technique of porous material as pore-forming material, the mixing of microballoon, dispersion technology are the key factors that affects its pore-creating performance.Adopt traditional dispersion dry technology to be difficult to it to scatter uniformly, especially, for the mixture of ceramic powder and organic microballoon, traditional methods such as pressurization granulation easily damage the structure of microballoon in addition, affect its pore-creating effect.The present invention by adding certain binding agent and softening agent to realize the dispersed of powder and microballoon in disperseing slip; and by spray granulation, protect the structure of microballoon; to realize the target of even pore-creating, guarantee the mechanical property of material, improve its heat-proof quality.
Summary of the invention
The object of the invention is to adopt the mode of adding pore-forming material PMMA microballoon, pass through spray granulation, reaction in－situ sintering provide a kind of O ?the preparation method of Sialon porous ceramics, under the condition of void content that improves porous ceramics, guarantee that material has higher mechanical property and heat-proof quality.
Because PMMA just can degrade 210 ℃ time, therefore, during mist projection granulating, the selection of slip solvent is just most important.The water of usining carries out mist projection granulating as slip solvent, and its drying temperature more than 200 ℃, easily damages PMMA conventionally.For water, ethanol has low surface tension, low boiling point and the high character such as vapour pressure, and ethanol is good to the wettability of powder, be conducive to the dispersion of powder in slurry, and it is low to have slurry viscosity, rate of drying is fast, the advantages such as hot-fluid is low are a kind of well behaved dispersion medium.The solvability of polyvinyl butyral acetal (PVB) in organic solvent is good, good with the compatibility of other organic additives, in addition, PVB is easily adsorbed on by the hydroxyl on molecule and ester group the dispersion stabilization that pottery and PMMA microsphere surface form sterically hindered enhanced granule.PEG ?400 and propyl carbinol as excellent performance softening agent, good with ethanol medium consistency, can effectively reduce the intermolecular frictional force of PVB binding agent, improve binding agent plasticity-at room temperature.Therefore select in the present invention dehydrated alcohol as dispersion medium, polyvinyl butyral acetal (PVB) is dispersion agent and binding agent, and poly(oxyethylene glycol) 400 (PEG ?400) and propyl carbinol are softening agent.
The present invention is achieved by the following technical programs:
Adopt and take PMMA microballoon as a pore-forming material, by spray granulation, reaction in－situ sintering prepare O ?the method of Sialon porous ceramics, its step is as follows:
(1) according to ratio of quality and the number of copies Si
3n
4(56 ?66 parts), SiO
2(20 ?26 parts), Al
2o
3(5 ?15 parts), sintering aid (3 ?7 parts) batching, then add 60 ?the dehydrated alcohol of 100 parts, a step ball milling;
(2) in the slip after a step ball milling, add the PMMA microballoon of 20 parts of 5 ?, and add the polyvinyl butyral acetal of 4 parts of 1 ?, the softening agent of 37 parts of ?, two step ball millings, obtain mist projection granulating slip
(3) by the slip mist projection granulating obtaining, powder compression moulding;
(4) by the binder removal in retort furnace of the base substrate after moulding, dump temperature be 500 ?800 ℃, soaking time be 1 ?2h;
(5) by the sample after binder removal in 1360 ?carry out sintering in 1450 ℃ of nitrogen atmosphere stoves and obtain product.
A described step ball milling grinds 4 ?6h for adopting roller ball mill ball milling 24 ?48h or adopting to stir to grind; Two step ball millings for adopt roller ball mill ball milling 12 ?24h.
Described PMMA microballoon is as pore-forming material, mean particle size D
502 μ m ?10 μ m.
Described sintering aid is Y
2o
3with the composition in MgO, its ratio is preferably (1 ?4): (1 ?3).
Described softening agent be PEG ?400 and the mixture of propyl carbinol, its ratio is (1 ?3): (1 ?4).
Described compression moulding is dry-pressing or isostatic pressing.
By introducing pore-forming material PMMA microballoon, the mode of mist projection granulating, has prepared and has had compared with high porosity, good mechanical properties, O ?Sialon porous material density 1.35 ?1.75gcm
?3, void content between 40% ?between 60%, room temperature bending strength 50 ?between 120MPa, thermal conductivity 0.90 ?between 2.25W/mK, uniform microstructure.
Accompanying drawing explanation
Fig. 1 is the micro-structure diagram of the porous material for preparing of embodiment 1.
Specific implementation method
According to concrete grammar, illustrate below:
Method steps is:
(1) batching: compare Si according to powder quality
3n
4(56 ?66 parts), SiO
2(20 ?26 parts), Al
2o
3(5 ?15 parts), sintering aid (3 ?7 parts) batching, then add 60 ?the dehydrated alcohol of 100 parts, a step ball milling;
(2) prepare slip: in the slip after a step ball milling, add the pore-forming material of 20 parts of 5 ?, and add PVB dispersion agent and the binding agent of 4 parts of 1 ?, the softening agent of 37 parts of ?, two step ball millings, obtain mist projection granulating slip.
(3) mist projection granulating: by the slip mist projection granulating obtaining.
(4) moulding: the pelletizing compression moulding obtaining.
(5) binder removal: by the binder removal in retort furnace of the base substrate after moulding, dump temperature be 500 ?800 ℃, soaking time be 1 ?2h.
(6) sintering: by the sample after binder removal in 1360 ?carry out sintering in 1450 ℃ of nitrogen atmosphere stoves and obtain product.
A described step ball milling grinds 4 ?6h for adopting roller ball mill ball milling 24 ?48h or adopting to stir to grind; Two step ball millings for adopt roller ball mill ball milling 12 ?24h.
Described pore-forming material is PMMA microballoon, mean particle size D
502 μ m ?10 μ m.
Described sintering aid is Y
2o
3with the composition in MgO, its ratio is preferably (1 ?4): (1 ?3).
Described softening agent be PEG ?400 and the mixture of propyl carbinol, its ratio is (1 ?3): (1 ?4).
Described compression moulding is dry-pressing or isostatic pressing.
The extrudate density that sintering obtains in described step (6) 1.35 ?1.75gcm
?3, void content between 40% ?between 60%, room temperature bending strength 50 ?between 120MPa, thermal conductivity 0.90 ?between 2.25W/mK, uniform microstructure.
Embodiment 1: Yi α ?Si
3n
4, SiO
2, Al
2o
3for raw material, with Y
2o
3as sintering aid, take PMMA microballoon as pore-forming material, wherein the D of PMMA with MgO
50be 6 μ m.
(1) batching: compare Si according to powder quality
3n
4: SiO
2: Al
2o
3=62 parts: 26 parts: 5 parts of batchings, add the Y of 4 parts
2o
3make knots auxiliary agent with the MgO of 3 parts, then add the dehydrated alcohol of 60 parts, adopt roller ball mill ball milling 24h.
(2) prepare slip: in the slip after ball milling, add 5 parts of pore-forming materials, and add 1 part of PVB, 400,1 parts of propyl carbinols of 2 parts of PEG ?, adopt roller ball mill ball milling 12h, obtain mist projection granulating slip.
(3) mist projection granulating: by the slip mist projection granulating obtaining.
(4) moulding: the pelletizing obtaining is dry-pressing formed.
(5) binder removal: by the binder removal in retort furnace of the base substrate after moulding, dump temperature is 500 ℃, and soaking time is 2h.
(6) sintering: sintering: the sample after binder removal is carried out to sintering in 1420 ℃ of nitrogen atmosphere stoves and obtain goods.
The extrudate density obtaining after sintering is 1.71cm
?3, void content is 42%, and room temperature bending strength is 111Mpa, and thermal conductivity is 2.17W/mK.
Embodiment 2: Yi α ?Si
3n
4, SiO
2, Al
2o
3for raw material, with Y
2o
3as sintering aid, take PMMA microballoon as pore-forming material, wherein the D of PMMA with MgO
50be 2 μ m.
(1) batching: compare Si according to powder quality
3n
4: SiO
2: Al
2o
3=66 parts: 20 parts: 10 parts of batchings, add the Y of 1 part
2o
3make knots auxiliary agent with the MgO of 3 parts, then add the dehydrated alcohol of 80 parts, adopt roller ball mill ball milling 48h.
(2) prepare slip: in the slip after ball milling, add the pore-forming material of 10 parts, and add 3 parts of PVB, 400,2 parts of propyl carbinols of 3 parts of PEG ?, adopt roller ball mill ball milling 16h, obtain mist projection granulating slip.
(3) mist projection granulating: by the slip mist projection granulating obtaining.
(4) moulding: by the pelletizing isostatic pressing obtaining.
(5) binder removal: by the binder removal in retort furnace of the base substrate after moulding, dump temperature is 600 ℃, and soaking time is 2h.
(6) sintering: sintering: the sample after binder removal is carried out to sintering in 1360 ℃ of nitrogen atmosphere stoves and obtain goods.
The extrudate density obtaining after sintering is 1.63cm
?3, void content is 45%, and room temperature bending strength is 85Mpa, and thermal conductivity is 1.26W/mK.
Embodiment 3: Yi α ?Si
3n
4, SiO
2, Al
2o
3for raw material, with Y
2o
3as sintering aid, take PMMA microballoon as pore-forming material, wherein the D of PMMA with MgO
50be 10 μ m.
(1) batching: compare Si according to powder quality
3n
4: SiO
2: Al
2o
3=56 parts: 25 parts: 15 parts of batchings, add the Y of 3 parts
2o
3make knots auxiliary agent with the MgO of 1 part, then add the dehydrated alcohol of 80 parts, adopt and stir mill grinding 4h.
(2) prepare slip: in the slip after grinding, add the pore-forming material of 15 parts, and add 2 parts of PVB, 400,4 parts of propyl carbinols of 3 parts of PEG ?, adopt roller ball mill ball milling 20h, obtain mist projection granulating slip.
(3) mist projection granulating: the slip mist projection granulating obtaining.
(4) moulding: the pelletizing obtaining is dry-pressing formed.
(5) binder removal: the binder removal in retort furnace of the base substrate after moulding, dump temperature is 700 ℃, soaking time is 1h.
(6) sintering: the sample after binder removal carries out sintering and obtains goods in 1450 ℃ of nitrogen atmosphere stoves.
The extrudate density obtaining after sintering is 1.57cm
?3, void content is 47%, and room temperature bending strength is 73Mpa, and thermal conductivity is 1.11W/mK.
Embodiment 4: Yi α ?Si
3n
4, SiO
2, Al
2o
3for raw material, with Y
2o
3as sintering aid, take PMMA microballoon as pore-forming material, wherein the D of PMMA with MgO
50be 6 μ m.
(1) batching: compare Si according to powder quality
3n
4: SiO
2: Al
2o
3=62 parts: 26 parts: 9 parts of batchings, add the Y of 1 part
2o
3make knots auxiliary agent with the MgO of 2 parts, then add the dehydrated alcohol of 100 parts, adopt and stir mill grinding 6h.
(2) prepare slip: in the slip after grinding, add the pore-forming material of 20 parts, and add 4 parts of PVB, 400,3 parts of propyl carbinols of 1 part of PEG ?, adopt roller ball mill ball milling 24h, obtain mist projection granulating slip.
(3) mist projection granulating: the slip mist projection granulating obtaining.
(4) moulding: the pelletizing isostatic pressing obtaining.
(5) binder removal: by the binder removal in retort furnace of the base substrate after moulding, dump temperature is 800 ℃, and soaking time is 1h.
Sintering: the sample after binder removal is carried out to sintering in 1390 ℃ of nitrogen atmosphere stoves and obtain goods.
The extrudate density obtaining after sintering is 1.37cm
?3, void content is 58%, and room temperature bending strength is 53Mpa, and thermal conductivity is 0.95W/mK.
Claims (4)
1. add PMMA pore-forming material and prepare a method for O ?Sialon porous ceramics, it is characterized in that step is as follows:
(1) according to ratio of quality and the number of copies Si
3n
4(56 ?66 parts), SiO
2(20 ?26 parts), Al
2o
3(5 ?15 parts), sintering aid (3 ?7 parts) batching, then add 60 ?the dehydrated alcohol of 100 parts, a step ball milling;
(2) in the slip after a step mill, add the PMMA microballoon of 20 parts of 5 ?, and add the polyvinyl butyral acetal of 4 parts of 1 ?, the softening agent of 37 parts of ?, two step ball millings, obtain mist projection granulating slip;
(3) by the slip mist projection granulating obtaining, powder compression moulding;
(4) by the binder removal in retort furnace of the base substrate after moulding, dump temperature be 500 ?800 ℃, soaking time be 1 ?2h;
(5) by the sample after binder removal in 1360 ?carry out sintering in 1450 ℃ of nitrogen atmosphere stoves and obtain product.
2. method as claimed in claim 1, is characterized in that a described step ball milling stirs mill and grinds 4 ?6h for adopting roller ball mill ball milling 24 ?48h or adopting; Two step ball millings for adopt roller ball mill ball milling 12 ?24h.
3. method as claimed in claim 1, it is characterized in that described softening agent be PEG ?400 and the mixture of propyl carbinol, its ratio of quality and the number of copies is (1 ?3): (1 ?4).
4. method as claimed in claim 1, is characterized in that described sintering aid is Y
2o
3with the composition in MgO, its ratio of quality and the number of copies is (1 ?4): (1 ?3).
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104326766A (en) * | 2014-10-13 | 2015-02-04 | 航天材料及工艺研究所 | Preparation method of porous silicon nitride ceramic material with spherical pore structure |
| CN107794393A (en) * | 2016-09-05 | 2018-03-13 | 中南大学 | A kind of preparation method of micron-sized low porosity porous Al alloy |
| CN110407584A (en) * | 2019-08-28 | 2019-11-05 | 武汉轻工大学 | A kind of porous Ti2AlN ceramic and preparation method thereof |
| CN115364852A (en) * | 2022-07-26 | 2022-11-22 | 浙江梦溪环保科技有限公司 | Porous ceramic loaded with nano noble metal oxide catalyst and preparation method and application thereof |
| CN115893980A (en) * | 2022-09-30 | 2023-04-04 | 安徽华仕新材有限公司 | Process for preparing porous support body ceramic by using nodulizer micro powder |
| CN115954131A (en) * | 2022-12-20 | 2023-04-11 | 瑞声科技（南京）有限公司 | Copper paste for printing capillary structure and preparation method thereof |
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|---|---|---|---|---|
| CN104326766A (en) * | 2014-10-13 | 2015-02-04 | 航天材料及工艺研究所 | Preparation method of porous silicon nitride ceramic material with spherical pore structure |
| CN104326766B (en) * | 2014-10-13 | 2016-05-04 | 航天材料及工艺研究所 | A kind of preparation method of the porous silicon-nitride ceramic material with spherical pore structure |
| CN107794393A (en) * | 2016-09-05 | 2018-03-13 | 中南大学 | A kind of preparation method of micron-sized low porosity porous Al alloy |
| CN110407584A (en) * | 2019-08-28 | 2019-11-05 | 武汉轻工大学 | A kind of porous Ti2AlN ceramic and preparation method thereof |
| CN115364852A (en) * | 2022-07-26 | 2022-11-22 | 浙江梦溪环保科技有限公司 | Porous ceramic loaded with nano noble metal oxide catalyst and preparation method and application thereof |
| CN115893980A (en) * | 2022-09-30 | 2023-04-04 | 安徽华仕新材有限公司 | Process for preparing porous support body ceramic by using nodulizer micro powder |
| CN115893980B (en) * | 2022-09-30 | 2023-08-11 | 安徽华仕新材有限公司 | Process for preparing porous support ceramic by using nodulizer micropowder |
| CN115954131A (en) * | 2022-12-20 | 2023-04-11 | 瑞声科技（南京）有限公司 | Copper paste for printing capillary structure and preparation method thereof |
| CN116922914A (en) * | 2023-07-24 | 2023-10-24 | 青岛伟东包装有限公司 | High-gloss low-haze plastic film and preparation method thereof |
| CN116922914B (en) * | 2023-07-24 | 2024-04-05 | 青岛伟东包装有限公司 | High-gloss low-haze plastic film and preparation method thereof |
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