CN107010990B - A kind of preparation method of low thermal conductivity cordierite porous ceramics - Google Patents
A kind of preparation method of low thermal conductivity cordierite porous ceramics Download PDFInfo
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- CN107010990B CN107010990B CN201710302366.8A CN201710302366A CN107010990B CN 107010990 B CN107010990 B CN 107010990B CN 201710302366 A CN201710302366 A CN 201710302366A CN 107010990 B CN107010990 B CN 107010990B
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- 229910052878 cordierite Inorganic materials 0.000 title claims abstract description 49
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000000919 ceramic Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 27
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000004321 preservation Methods 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 238000005245 sintering Methods 0.000 claims description 13
- 239000000853 adhesive Substances 0.000 claims description 7
- 230000001070 adhesive effect Effects 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000011164 primary particle Substances 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims 2
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims 2
- 229910011255 B2O3 Inorganic materials 0.000 abstract description 18
- 238000002156 mixing Methods 0.000 abstract description 5
- 239000011230 binding agent Substances 0.000 abstract description 4
- 238000009413 insulation Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 description 10
- 238000007599 discharging Methods 0.000 description 7
- 239000011148 porous material Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 229920002472 Starch Polymers 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 239000008107 starch Substances 0.000 description 3
- 235000019698 starch Nutrition 0.000 description 3
- 239000012856 weighed raw material Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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- 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
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/067—Macromolecular compounds
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- 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
- C04B35/16—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
- 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
- C04B35/185—Mullite 3Al2O3-2SiO2
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- 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
- C04B35/16—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
- 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
- C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/6303—Inorganic additives
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The invention relates to a preparation method of low-thermal-conductivity cordierite porous ceramic. The preparation method comprises the following steps: mixing cordierite, mullite and B2O3And a pore-forming agent PMMA, and putting the mixture into a ball mill according to a proportion for ball milling and mixing uniformly, wherein: the mass ratio of cordierite to mullite is between 5:5 and 7:3, B2O3The mass of the cordierite porous ceramic is 3% -10% of the mass sum of cordierite and mullite, the obtained powder is dried, granulated and tabletted, the obtained blank body is subjected to binder removal, and a sample subjected to binder removal is subjected to heat preservation and calcination for 0.5-4 h at 1175-1250 ℃ to obtain the low-thermal-conductivity cordierite porous ceramic. The low-thermal-conductivity cordierite porous ceramic prepared by the method has the characteristics of high apparent porosity, low thermal conductivity and good thermal insulation performance.
Description
Technical Field
The invention belongs to the field of preparation of heat-insulating ceramic materials, and particularly relates to a preparation method of heat-insulating porous ceramic with both apparent porosity and thermal conductivity.
Background
The heat insulation ceramic has wide application in industry, generally, the heat insulation ceramic reduces the thermal conductivity of the material through a large number of closed pores inside, but under some special conditions, the heat insulation porous ceramic must have certain open pores to meet other use requirements. Or, in other words, some porous ceramics mainly having open pores also require certain heat insulating properties, and the present patent is not directed to pursuing extremely high porosity or extremely low thermal conductivity, but to simultaneously have both of these properties.
The invention patent with the patent number of 201410627847.2 discloses a preparation method of closed-cell porous ceramic alumina heat-insulating ceramic, which mainly emphasizes that the open pores are lower than 5%, the heat conductivity can reach 0.1W/(mk), and the use temperature can exceed 1400 ℃.
The porous ceramic has a gas phase and a solid phase, the heat transfer of the porous ceramic comprises two parts of the gas phase and the solid phase, and the heat transfer has three forms: heat conduction, heat convection and heat radiation, wherein the heat convection can be ignored when the size of the air hole is less than 10mm, and the influence of the heat radiation is extremely small when the temperature is not very high. Heat conduction is thus the primary means of heat transfer in the present article. The heat conduction is microscopically realized by the vibration of crystal lattices, the energy of the crystal lattice vibration is quantized, generally phonons are used for expressing the energy photons of simple phonons in the crystal lattice vibration, the heat transfer can be described as the transmission of the phonons, air holes and hole walls in the porous ceramics can cause phonon scattering, and the thermal conductivity of the air holes is low, so that the existence of the air holes can reduce the heat transfer.
Disclosure of Invention
The invention aims to provide a preparation method of cordierite porous ceramic with low thermal conductivity, and the cordierite porous ceramic prepared by the method has the characteristics of low sintering temperature, high apparent porosity, low thermal conductivity and good heat preservation performance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
provides a preparation method of cordierite porous ceramic with low thermal conductivity, which comprises the steps of mixing cordierite, mullite and B2O3And a pore-forming agent PMMA (polymethyl methacrylate), and putting the mixture into a ball mill according to a certain proportion for ball milling and mixing uniformly, wherein: the mass ratio of cordierite to mullite is between 5:5 and 7:3, B2O3The mass of the cordierite porous ceramic is 3% -10% of the mass sum of cordierite and mullite, the obtained powder is dried, granulated and tabletted, the obtained blank body is subjected to binder removal, and a sample subjected to binder removal is subjected to heat preservation and calcination for 0.5-4 h at 1175-1250 ℃ to obtain the low-thermal-conductivity cordierite porous ceramic.
According to the scheme, the cordierite, the mullite and the B2O3Original pore formerThe particle size is 50 +/-40 mu m.
According to the scheme, the ball milling time is 6 hours, the drying temperature is 100 ℃, and the time is 24 hours.
According to the scheme, 10% of adhesive is added during granulation, the pressure is 10MPa during tabletting, and the pressure is maintained for 1 min.
According to the scheme, the adhesive is polyvinyl alcohol.
According to the scheme, the glue discharging temperature is 350 ℃, 400 ℃, 450 ℃ and 2 hours of heat preservation at 600 ℃. The invention preferably adopts the progressive heating system to discharge the glue (keeping the temperature at 350 ℃, 400 ℃ and 450 ℃ for 1 hour), can reduce the removal speed of gas generated by PMMA decomposition and oxidation, and obtains better PMMA removal effect. If PMMA reacts violently at a higher temperature and a large amount of gas is exhausted in a short time, the ceramic structure is easily damaged to generate a large amount of microcracks, and in extreme cases, the samples have macrocracks and other authorities. The polyvinyl alcohol is added at the temperature of 600 ℃ correspondingly to remove the temperature, the polyvinyl alcohol is used as a bonding agent adding system, the ceramic powder is mainly bonded by the polyvinyl alcohol before sintering, if the polyvinyl alcohol is removed quickly in a short time, large stress can be generated among ceramic particles, the size of the ceramic can be changed greatly, and the subsequent high-temperature sintering can be influenced by the arrangement change of the ceramic particles.
According to the scheme, the temperature rise rate of the heat preservation calcination is 0.5-2 ℃/min. Adding B2O3As a sintering aid, B is above 1000 DEG C2O3In the form of a liquid phase, liquid phase B2O3The method has the function of greatly promoting particle rearrangement and mass transfer. In addition, the sintering temperature is too slow, the ceramic particles are easy to fill the air holes to reduce the porosity, and the sintering temperature is too fast, so that the ceramic body containing the air holes has the defects of cracking and the like caused by the accumulation of larger thermal stress.
According to the scheme, the sintering temperature is preferably 1175-1225 ℃.
According to the scheme, the dosage of the pore-forming agent PMMA is cordierite, mullite and B2O310 to 30wt%, preferably 20 to 30wt%, and more preferably 25wt% of the sum of the three.
The invention has the beneficial effects that:
the invention uses cordierite and mullite as main raw materials and is matched with B2O3The sintering temperature of the preparation method of the low-thermal-conductivity cordierite porous ceramic material provided by the selection of the conditions such as the auxiliary agent, the pore-forming agent PMMA, the sintering temperature and the like is low, the apparent porosity of the prepared low-thermal-conductivity cordierite porous ceramic can reach about 60 percent, the thermal conductivity can reach about 0.11W/mk, and the lowest thermal diffusion coefficient can reach 0.28mm2About/s, simple process. The porosity is continuously adjustable within a certain range.
Drawings
FIG. 1 is a sample prepared by adding carbon powder as a pore-forming agent, and a, b and c are graphs respectively showing the relationship between the porosity, the thermal conductivity and the thermal diffusion coefficient and the content of the pore-forming agent;
FIG. 2 is a sample prepared by adding starch as a pore-forming agent, and a, b and c are graphs respectively showing the relationship between the porosity, the thermal conductivity and the thermal diffusion coefficient and the content of the pore-forming agent;
FIG. 3 is a sample prepared by adding PMMA as a pore-forming agent, and a, b and c are graphs of the relationship between the porosity, the thermal conductivity and the thermal diffusivity and the content of the pore-forming agent respectively;
FIG. 4 is a sample prepared by adding PMMA as a pore-forming agent, and a, b and c are graphs of the relationship between the porosity, the thermal conductivity and the thermal diffusivity and the sintering temperature respectively;
Detailed Description
For a better understanding of the present invention, the following examples are included to further illustrate the present invention, but the present invention is not limited to the following examples.
Example 1:
1) the raw materials used comprise cordierite, mullite and B2O3PMMA, the average value of the primary particle size of the raw materials is respectively 50 μm, 30 μm and 30 μm, and the raw material proportion is designed as follows: the mass ratio of cordierite to mullite is 5:5, B2O3The mass of the pore-forming agent is 3 percent of the sum of the mass of cordierite and mullite, and the mass of the pore-forming agent is cordierite, mullite and B2O310%, 15%, 20%, 25%, 30% of the sum of the mass of the three. Putting the weighed raw materials into a ball mill in proportion, and uniformly mixing the raw materials in the ball mill for 6 hours to obtain the productAnd (3) drying the powder at the drying temperature of 100 ℃ for 24 hours.
2) And (2) granulating the dried powder, sieving the powder by a 100-mesh sieve to obtain ceramic powder, tabletting, adding 10% of adhesive into the granules, keeping the pressure for 1min at 10MPa during tabletting, and carrying out gel discharging on the obtained blank in a resistance furnace at the gel discharging temperature of 350 ℃, 400 ℃, 450 ℃ for 1h and 600 ℃ for 2 h. And heating the sample subjected to rubber removal to 1200 ℃ at the speed of 1 ℃/min, and preserving the heat for 1.5h to obtain 5 parts of porous ceramic sample.
Carbon powder and starch are adopted to replace a pore-forming agent PMMA respectively to prepare the ceramic material.
The apparent porosity of the ceramic sample obtained by sintering the above carbon powder, starch and PMMA as pore formers was measured using Archimedes' principle, as shown in FIGS. 1-3. As can be seen from the figure, the thermal conductivity and the thermal conductivity coefficient of the sample can reach more than 60% by using PMMA as the pore-forming agent, and the data also shows that the thermal conductivity can reach 0.1104W/mk and the thermal conductivity coefficient can reach 0.2820mm by using PMMA as the pore-forming agent2And/s, significantly lower than the other two.
Example 2:
1) the raw materials used comprise cordierite, mullite and B2O3PMMA, the average value of the primary particle size of the raw materials is 70 μm, 50 μm and 40 μm respectively, and the raw material proportion is designed as follows: the mass ratio of cordierite to mullite is 5:5, B2O3The mass of the material is 3 percent of the sum of the mass of cordierite and mullite, and the mass of PMMA is cordierite, mullite and B2O3The mass sum of the three is 25 percent. Putting the weighed raw materials into a ball mill in proportion, performing ball milling for 6 hours, and drying the obtained powder at 100 ℃ for 24 hours.
2) And (2) granulating the dried powder, sieving the powder by a 100-mesh sieve to obtain ceramic powder, tabletting, adding 10% of adhesive into the granules, keeping the pressure for 1min at 10MPa during tabletting, and carrying out gel discharging on the obtained blank in a resistance furnace at the gel discharging temperature of 350 ℃, 400 ℃, 450 ℃ for 1h and 600 ℃ for 2 h. The sample after the glue discharging is heated to 1150 ℃, 1175 ℃, 1200 ℃, 1225 ℃, 1250 ℃ and 1275 ℃ at the speed of 1 ℃/min, and the temperature is kept for 1h, thus obtaining 6 parts of porous ceramic sample.
The ceramic sample obtained in example 2 was subjected to porosity measurement using the archimedes principle; the thermal conductivity and the thermal diffusivity were measured by a thermal constant analyzer, and the results are shown in FIG. 4. From the figure, it can be found that the apparent porosity is reduced along with the temperature rise, the apparent porosity is obviously reduced when the temperature exceeds 1225 ℃, the thermal conductivity and the thermal conductivity are slowly increased between 1150 ℃ and 1200 ℃, and the thermal conductivity are reduced between 1200 ℃ and 1275 ℃.
Example 3:
1) the raw materials used comprise cordierite, mullite and B2O3The primary particle size of PMMA is 50 +/-40 mu m, and the raw material proportion is designed as follows: the mass ratio of cordierite to mullite is 5:5, B2O3The mass of the carbon powder is 3 percent of the sum of the mass of cordierite and mullite, and the mass of the carbon powder is cordierite, mullite and B2O3The mass sum of the three is 25 percent. Putting the weighed raw materials into a ball mill in proportion, performing ball milling for 6 hours, and drying the obtained powder at 100 ℃ for 24 hours.
2) And (2) granulating the dried powder, sieving the powder by a 100-mesh sieve to obtain ceramic powder, tabletting, adding 10% of adhesive into the granules, keeping the pressure for 1min at 10MPa during tabletting, and carrying out gel discharge on the obtained blank in a resistance furnace at the gel discharge temperature of 300 ℃ for 1h and at the temperature of 600 ℃ for 2 h. And heating the sample after the glue discharging to 1225 ℃ at the speed of 1 ℃/min, and preserving the heat for 1h, 2h, 3h and 4h to obtain 4 parts of porous ceramic samples.
The test result of the sample shows that the difference of the heat preservation time has little influence on the porosity of the sample, the porosity is reduced from 63% to 61% along with the heat preservation time from 0.5h to 4h, the thermal conductivity and the thermal diffusion coefficient are not changed greatly, and the heat preservation temperature can be determined according to the actual production period from the perspective of industrial production economy.
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| CN109851337A (en) * | 2019-01-08 | 2019-06-07 | 广东山摩新材料科技有限公司 | A kind of high temperature dichroite-mullite refractory slab and preparation method thereof |
| CN110272260B (en) * | 2019-05-13 | 2021-09-21 | 山东国瓷功能材料股份有限公司 | Narrow-pore-diameter-distribution cordierite ceramic honeycomb body and preparation method thereof |
| CN110229000A (en) * | 2019-05-13 | 2019-09-13 | 山东国瓷功能材料股份有限公司 | A kind of high strength cordierite ceramic honeycomb body and preparation method thereof |
| CN113045328B (en) * | 2021-05-06 | 2023-02-17 | 中铭富驰（苏州）纳米高新材料有限公司 | Preparation method of porous ceramic plate and high-precision ceramic porous platform |
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