CN103641510B - Add the method that PMMA pore-forming material prepares O-Sialon porous ceramics - Google Patents
Add the method that PMMA pore-forming material prepares O-Sialon porous ceramics Download PDFInfo
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Abstract
The present invention relates to a kind of method that the PMMA of interpolation pore-forming material prepares O-Sialon porous ceramics, by mist projection granulating, in-situ sintering prepare O the method of Sialon porous ceramics.By using dehydrated alcohol as dispersion medium, PVB as dispersion agent and binding agent, PEG 400 and propyl carbinol as softening agent, realize the dispersed of ceramic powder and PMMA, then mist projection granulating, shaping, binder removal, sintering obtains goods.The extrudate density obtained 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.
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, 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 its special vesicular structure 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, good stability of the dimension, and have excellent heat-proof quality, 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 formed, O ?Sialon remain 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, therefore 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 is excellent, 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 multiple preparation technology at present, wherein pore-forming material method prepares a kind of important process of porous ceramics, the feature of this technique is the pore-forming material by adding easy volatile in ceramic batch, utilize pore-forming material in base substrate, occupy certain space, then, after sintering, pore-forming material leaves matrix and forms pore to prepare porous ceramics.Add pore-forming material and can form hole of holding one's breath, make sintered article both have 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.) prepare porous silicon nitride ceramic by adding gac as pore-forming material, the ceramic void content prepared is greater than 70%, and average bending strength is greater than 8MPa.
ZhangGuo ?the (YangJF such as Jun, ZhangGJ, OhjiT.Fabricationoflowshrinkage, poroussiliconnitrideceramicsbyadditionofasmallamountofca rbon.JournaloftheAmericanCeramicSociety, 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 powdered carbon that have studied different-grain diameter size (13nm and 5 μm) is on the impact of the performance of material.Result shows, the Si prepared
3n
4pottery porosity can reach 50% ?60%, and intensity is 100MPa.Add carbon dust significantly to increase the void content of material and reduce its shrinking percentage.
Chinese patent 102351563(Chen Fei, Pan Haoliang, Shen Qiang etc., there is the preparation method of the high porosity porous SiN ceramic of multilevel pore size structure) to disclose one be binding agent and aperture pore-forming material, naphthalene powder with silicone resin is macropore pore-forming material, preparation has the method for the porous SiN ceramic of multilevel pore size structure, and the pottery prepared has the excellent properties such as pore size distribution is wide, even pore distribution, porosity are high, mechanical strength is better.
Chinese patent 102850084A(Peng Hong; Li Shaorong, a kind of with the preparation method of the organic resin foam microspheres porous ceramics that is pore-forming material) disclose a kind of preparation method of the porous ceramics utilizing organic resin foam microspheres to be pore-forming material, by granulation of sieving, shaped by fluid pressure, prepare Production of Ceramics and go out uniform pore diameter, the porous ceramics that pore size is controlled, improves the sintering qualified rate of product greatly.
PMMA microsphere is a kind of pore-forming material of excellent performance, can obtain the controlled material of porosity and aperture by controlling its particle diameter and add-on.Prepare in the technique of porous material in interpolation PMMA microsphere as pore-forming material, the mixing of microballoon, dispersion technology are the key factors affecting 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 micro-spheres, the methods such as pressurization granulation traditional in addition easily damage the structure of microballoon, affect its pore-creating effect.The present invention realizes the dispersed of powder and microballoon by adding certain binding agent and softening agent in dispersion slip; and the structure of microballoon is protected by spray granulation; to realize the target of even pore-creating, ensure 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 microsphere, 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 improving porous ceramics, ensure that material has higher mechanical property and heat-proof quality.
Because PMMA just can degrade 210 DEG C time, therefore, during mist projection granulating, the selection of slip solvent is just most important.Carry out mist projection granulating using water as slip solvent, its drying temperature more than 200 DEG C, easily damages PMMA usually.For water, ethanol has the character such as low surface tension, low boiling point and high vapour pressure, and ethanol is good to the wettability of powder, be conducive to powder dispersion in the 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 dispersion medium of good performance.Polyvinyl butyral acetal (PVB) solvability is in organic solvent good, good with the compatibility of other organic additives, in addition, PVB is easily adsorbed on the dispersion stabilization of pottery and PMMA microsphere space forming surface steric hindrance enhanced granule by the hydroxyl on molecule and ester group.PEG ?400 and propyl carbinol as excellent performance softening agent, good with ethanol medium consistency, effectively can reduce the intermolecular frictional force of PVB binding agent, improve binding agent plasticity-at room temperature.Therefore select dehydrated alcohol as dispersion medium in the present invention, 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:
A kind of employing with PMMA microsphere is 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 microsphere of 5 ?20 parts, and add the polyvinyl butyral acetal of 1 ?4 parts, the softening agent of 3 ?7 parts, two step ball millings, obtain mist projection granulating slip
(3) the slip mist projection granulating will obtained, powder compression moulding;
(4) by the base substrate binder removal in retort furnace after shaping, dump temperature be 500 ?800 DEG C, soaking time be 1 ?2h;
(5) by the sample after binder removal in 1360 ?carry out sintering in 1450 DEG C of nitrogen atmosphere stoves and obtain product.
A described step ball milling for adopt roller ball mill ball milling 24 ?48h or adopt Ball-stirring mill grind 4 ?6h; Two step ball millings for adopt roller ball mill ball milling 12 ?24h.
Described PMMA microsphere as pore-forming material, mean particle size D
502 μ m ?10 μm.
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 microsphere, the mode of mist projection granulating, has prepared and has had comparatively 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 that embodiment 1 prepares.
Specific implementation method
Illustrate according to concrete grammar below:
Method steps is:
(1) prepare burden: 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) slip is prepared: the pore-forming material adding 5 ?20 parts in the slip after a step ball milling, and the PVB dispersion agent and the binding agent that add 1 ?4 parts, the softening agent of 3 ?7 parts, two step ball millings, obtain mist projection granulating slip.
(3) mist projection granulating: by the slip mist projection granulating obtained.
(4) shaping: the pelletizing compression moulding obtained.
(5) binder removal: by the base substrate binder removal in retort furnace after shaping, dump temperature be 500 ?800 DEG C, soaking time be 1 ?2h.
(6) sinter: by the sample after binder removal in 1360 ?carry out sintering in 1450 DEG C of nitrogen atmosphere stoves and obtain product.
A described step ball milling for adopt roller ball mill ball milling 24 ?48h or adopt Ball-stirring mill grind 4 ?6h; Two step ball millings for adopt roller ball mill ball milling 12 ?24h.
Described pore-forming material is PMMA microsphere, mean particle size D
502 μ m ?10 μm.
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.
Sinter in described step (6) extrudate density that obtains 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
3with MgO as sintering aid, take PMMA microsphere as pore-forming material, the wherein D of PMMA
50it is 6 μm.
(1) prepare burden: compare Si according to powder quality
3n
4: SiO
2: Al
2o
3=62 parts: 26 parts: 5 parts 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, 2 parts of PEG ?, 400,1 part of propyl carbinol, adopt roller ball mill ball milling 12h, obtain mist projection granulating slip.
(3) mist projection granulating: by the slip mist projection granulating obtained.
(4) shaping: by dry-pressing formed for the pelletizing obtained.
(5) binder removal: by the base substrate binder removal in retort furnace after shaping, dump temperature is 500 DEG C, and soaking time is 2h.
(6) sinter: sintering: the sample after binder removal is carried out sintering in 1420 DEG C of nitrogen atmosphere stoves and obtains goods.
The extrudate density obtained 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
3with MgO as sintering aid, take PMMA microsphere as pore-forming material, the wherein D of PMMA
50it is 2 μm.
(1) prepare burden: compare Si according to powder quality
3n
4: SiO
2: Al
2o
3=66 parts: 20 parts: 10 parts 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: the pore-forming material adding 10 parts in the slip after ball milling, and add 3 parts of PVB, 3 parts of PEG ?, 400,2 parts of propyl carbinols, adopt roller ball mill ball milling 16h, obtain mist projection granulating slip.
(3) mist projection granulating: by the slip mist projection granulating obtained.
(4) shaping: by the pelletizing isostatic pressing obtained.
(5) binder removal: by the base substrate binder removal in retort furnace after shaping, dump temperature is 600 DEG C, and soaking time is 2h.
(6) sinter: sintering: the sample after binder removal is carried out sintering in 1360 DEG C of nitrogen atmosphere stoves and obtains goods.
The extrudate density obtained 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
3with MgO as sintering aid, take PMMA microsphere as pore-forming material, the wherein D of PMMA
50it is 10 μm.
(1) prepare burden: compare Si according to powder quality
3n
4: SiO
2: Al
2o
3=56 parts: 25 parts: 15 parts 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 Ball-stirring mill grinding 4h.
(2) prepare slip: the pore-forming material adding 15 parts in the slip after grinding, and add 2 parts of PVB, 3 parts of PEG ?, 400,4 parts of propyl carbinols, adopt roller ball mill ball milling 20h, obtain mist projection granulating slip.
(3) mist projection granulating: the slip mist projection granulating obtained.
(4) shaping: the pelletizing obtained is dry-pressing formed.
(5) binder removal: the binder removal in retort furnace of the base substrate after shaping, dump temperature is 700 DEG C, and soaking time is 1h.
(6) sinter: the sample after binder removal carries out sintering and obtains goods in 1450 DEG C of nitrogen atmosphere stoves.
The extrudate density obtained 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
3with MgO as sintering aid, take PMMA microsphere as pore-forming material, the wherein D of PMMA
50it is 6 μm.
(1) prepare burden: compare Si according to powder quality
3n
4: SiO
2: Al
2o
3=62 parts: 26 parts: 9 parts 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 Ball-stirring mill grinding 6h.
(2) prepare slip: the pore-forming material adding 20 parts in the slip after grinding, and add 4 parts of PVB, 1 part of PEG ?, 400,3 parts of propyl carbinols, adopt roller ball mill ball milling 24h, obtain mist projection granulating slip.
(3) mist projection granulating: the slip mist projection granulating obtained.
(4) shaping: the pelletizing isostatic pressing obtained.
(5) binder removal: by the base substrate binder removal in retort furnace after shaping, dump temperature is 800 DEG C, and soaking time is 1h.
Sintering: the sample after binder removal is carried out sintering in 1390 DEG C of nitrogen atmosphere stoves and obtains goods.
The extrudate density obtained 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 (3)
1. add the method that PMMA pore-forming material prepares 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
456 ?66 parts, SiO
220 ?26 parts, Al
2o
35 ?15 parts, sintering aid 3 ?7 parts of batchings, then add 60 ?the dehydrated alcohol of 100 parts, a step ball milling;
(2) in the slip after a step mill, add the PMMA microsphere of 5 ?20 parts, and add the polyvinyl butyral acetal of 1 ?4 parts, the softening agent of 3 ?7 parts, two step ball millings, described two step ball millings adopt roller ball milling, obtain mist projection granulating slip;
(3) the slip mist projection granulating will obtained, powder compression moulding;
(4) by the base substrate binder removal in retort furnace after shaping, dump temperature be 500 ?800 DEG C, soaking time be 1 ?2h;
(5) by the sample after binder removal in 1360 ?carry out sintering in 1450 DEG C of nitrogen atmosphere stoves and obtain product; Described softening agent be PEG ?400 and the mixture of propyl carbinol, its ratio of quality and the number of copies be 1 ?3:1 ?4.
2. method as claimed in claim 1, it is characterized in that a described step ball milling for adopt roller ball mill ball milling 24 ?48h or adopt Ball-stirring mill ball milling 4 ?6h; Two step ball millings for adopt roller ball mill ball milling 12 ?24h.
3. method as claimed in claim 1, is characterized in that described sintering aid is Y
2o
3and MgO, its ratio of quality and the number of copies be 1 ?4:1 ?3.
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US5316988A (en) * | 1993-08-02 | 1994-05-31 | Eg&G Idaho, Inc. | Sialon ceramic compositions and methods of fabrication |
CN1273227A (en) * | 2000-05-22 | 2000-11-15 | 东北大学 | In-situ synthesis process for preparing complex-phase TiN/O'-sialon material |
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