CN103588482A - Manufacture method of high porosity and high strength yttrium-silicon-oxygen porous ceramics - Google Patents

Manufacture method of high porosity and high strength yttrium-silicon-oxygen porous ceramics Download PDF

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CN103588482A
CN103588482A CN201310617437.5A CN201310617437A CN103588482A CN 103588482 A CN103588482 A CN 103588482A CN 201310617437 A CN201310617437 A CN 201310617437A CN 103588482 A CN103588482 A CN 103588482A
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porous ceramics
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yttrium
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CN103588482B (en
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王京阳
吴贞
孙鲁超
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Institute of Metal Research of CAS
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Abstract

The invention relates to the porous ceramics material field, and concretely relates to a method for manufacturing high porosity and high strength yttrium-silicon-oxygen porous ceramics material through a foaming injection coagution process. According to the method, yttrium oxide and silicon oxide mixed power can be taken as a raw material, water is taken as a disperse medium, polyethyleneimine or ammonium citrate is selected as a dispersant, acrylamide or N-methylolacrylamide is taken as a monomer, a cross-linking agent N,N'-methylene bisacrylamide is added, a foaming agent sodium dodecyl sulfate, a peeling inhibitor polyoxyethylene, a catalyst N, N, N',N'-tetramethyl ethylenediamine and an initiator ammonium persulfate are added after stirring, and then injection mold solidification is carried out, drying is carried out for 24-48 hours at room temperature after demoulding, and then drying is carried out for 24-36 hours under the temperature of 60-90 DEG C, high temperature reaction sintering is carried out for 1.5-2.5 hours under the temperature of 1500-1550 DEG C finally, and the gamma-Y2Si2O7 porous ceramics can be finally manufactured. The manufactured gamma-Y2Si2O7 porous ceramics material having a multi-layer pore structure has controllable porosity with high porosity (75-85%) and high strength (3-8MPa).

Description

The preparation method of a kind of high porosity and high strength yttrium silica porous ceramics
Technical field
The present invention relates to porous ceramic film material field, be specially a kind of by foaming gel-casting prepare high porosity and high strength yttrium silica (γ-Y 2si 2o 7) method of porous ceramic film material.
Background technology
Yttrium silica (γ-Y 2si 2o 7) pottery has the performance of many brilliances, its thermal conductivity extremely low (<3W/ (mK), >300 ℃), thermal expansivity are little by (～3.9 * 10 -6k -1, 25～1400 ℃), damage tolerance is good, heat/corrosion resistance is high, also has good chemistry and thermostability (J.Y.Wang, et al.Acta.Mater. (material journal) .2007 (55): 6019 – 26.).Rely on its excellent over-all properties to make γ-Y 2si 2o 7pottery has broad application prospects, such as: can be used as the ring barrier coating of high-temperature structural material, silicon based ceramic and good thermal insulation material etc.
At present, more about the research of yttrium silica ceramic block material and coating preparation and property aspect, and γ-Y 2si 2o 7the relevant report of the synthetic and performance of porous ceramics seldom.γ-Y 2si 2o 7porous ceramics will have γ-Y 2si 2o 7pottery and the common advantage of porous ceramics, high than table intensity, high porosity, lower thermal conductivity, low density and performance (A.R.Studart, et al.J.Am.Ceram.Soc. (the U.S. pottery association journal) .2006 (89): 1771-89.) such as good anti-oxidant and high temperature resistant.So, γ-Y 2si 2o 7porous ceramics can be used as thermal isolation good in Aeronautics and Astronautics field and thermally protective materials, possesses extremely tempting prospect.
Summary of the invention
The preparation method who the object of the present invention is to provide a kind of high porosity and high strength yttrium silica porous ceramics, makes γ-Y 2si 2o 7porous ceramics has high porosity and high-intensity feature.
Technical scheme of the present invention is as follows:
A preparation method for high porosity and high strength yttrium silica porous ceramics, yttrium silica stupalith is γ-Y 2si 2o 7porous ceramics, concrete steps are as follows:
1) preparation of slurry: according to the mass fraction, with Y 2o 3and SiO 280～120 parts of the mixed powders of mol ratio 1:2,30～50 parts of deionized waters, 4～8 parts of organic monomers, 0.5～1.5 part of dispersion agent, linking agent N, 0.3～0.9 part of N '-methylene-bisacrylamide is raw material, mix, then stir 1～4 hour, form slurry;
2) according to the mass fraction, in described slurry, add 0.5～1.5 part of whipping agent sodium lauryl sulphate, stirring is foamed 15～30 minutes, then add 0.5～1.5 part, peeling inhibitor, catalyst n, N, N ', 1～5 part of 2～6 parts of N '-Tetramethyl Ethylene Diamines and initiator ammonium persulfate, stir after 20～60 seconds injection molding at once, after the demoulding, form base substrate;
3) by base substrate at room temperature dry 24～48 hours, then in baking oven 60～90 ℃ dry 24～36 hours, finally in air, at 1500～1550 ℃, carry out pyroreaction sintering, burn off organism gel, just can obtain the γ-Y that has macroscopic pores and micron hole concurrently 2si 2o 7porous ceramic film material.
The preparation method of described high porosity and high strength yttrium silica porous ceramics, γ-Y 2si 2o 7the porosity ranges of porous ceramic film material is 75～85%, and macroscopic pores is uniformly distributed, and pore diameter range is 80～300 μ m, and the hole wall of macroscopic pores has a micron hole, and pore diameter range is 0.1～2 μ m.
The preparation method of described high porosity and high strength yttrium silica porous ceramics, Y 2o 3and SiO 2the size scope of mixed powder be 0.1～3.5 μ m.
The preparation method of described high porosity and high strength yttrium silica porous ceramics, organic monomer is acrylamide or N hydroxymethyl acrylamide, dispersion agent is polymine or ammonium citrate; Peeling inhibitor is polyacrylamide, polyoxyethylene, polyoxyethylene glycol or starch.
The preparation method of described high porosity and high strength yttrium silica porous ceramics, catalyst n, N, N ', N '-Tetramethyl Ethylene Diamine and initiator ammonium persulfate are the aqueous solution of massfraction 15～25%.
The preparation method of described high porosity and high strength yttrium silica porous ceramics, the temperature rise rate of pyroreaction sintering is 4～8 ℃/min, soaking time is 1.5～2.5 hours.
Advantage of the present invention and beneficial effect are:
1. the present invention proposes to prepare high porosity and high strength yttrium silica (γ-Y by foaming gel-casting 2si 2o 7) method of porous ceramic film material, the method can be prepared and have macroscopic pores and micron hole and controlled high porosity and the high-intensity γ-Y of porosity concurrently 2si 2o 7porous ceramics.
2. of the present invention easy to operate, only need that preparation, foaming, injection molding through slurry solidifies, the flow process such as the demoulding, dry and pyroreaction sintering, and preparation, injection molding solidifies all in air atmosphere, carries out with heat treatment process.
3. cost of the present invention is lower, without specific installation, is easy to scale operation.
4. the temperature that the present invention chooses can make sample generate the γ-Y of pure phase 2si 2o 7thereby material has excellent high-temperature behavior.
5. the present invention can prepare the γ-Y with higher porosity and higher-strength 2si 2o 7porous ceramic film material, moreover this porous ceramic skeleton has a micron hole, can greatly reduce thermal conductivity, is the light heat-insulating material of excellent property.
In a word, the inventive method is usingd yttrium oxide and silicon oxide mixed powder as raw material, and water is dispersion medium, and selecting polymine or ammonium citrate is dispersion agent, with acrylamide or N hydroxymethyl acrylamide C 4h 7nO 2for monomer, then add linking agent N, N '-methylene-bisacrylamide C 7h 10n 2o 2, after stirring, add whipping agent sodium lauryl sulphate, peeling inhibitor polyoxyethylene, catalyst n, N, N ', N '-Tetramethyl Ethylene Diamine C 10h 24n 2and initiator ammonium persulfate, then carry out injection molding and solidify.After the demoulding, be first at room temperature dried 24～48 hours, then at 60～90 ℃, be dried 24～36 hours, finally at 1500～1550 ℃, carry out the pyroreaction sintering of 1.5～2.5 hours, finally prepare γ-Y 2si 2o 7porous ceramics.The technique of the inventive method is simple, with low cost, workable, can prepare and have Hierarchical porosity structure and the controlled high porosity (75～85%) of porosity and the γ-Y of high strength (3～8MPa) 2si 2o 7porous ceramic film material.
Accompanying drawing explanation
Fig. 1 (a)-Fig. 1 (c) is γ-Y 2si 2o 7the stereoscan photograph of porous ceramic film material.Wherein, Fig. 1 (a) and Fig. 1 (b) are embodiment 1; Fig. 1 (c) is embodiment 2.
Fig. 2 is γ-Y 2si 2o 7the X-ray diffraction spectrogram of porous ceramic film material.
Embodiment
High porosity of the present invention and high strength yttrium silica (γ-Y 2si 2o 7) preparation method of porous ceramic film material, concrete steps are as follows:
1) preparation of slurry: according to the mass fraction, with Y 2o 3and SiO 280～120 parts of the mixed powders of mol ratio 1:2,30～50 parts of deionized waters, 4～8 parts of organic monomers, 0.5～1.5 part of dispersion agent, linking agent N, 0.3～0.9 part of N '-methylene-bisacrylamide is raw material, mix, then stir 1～4 hour, form slurry;
2) add 0.5～1.5 part of rapid stirring of whipping agent sodium lauryl sulphate (stirrer speed range is 1000～2000rpm) to foam 15～30 minutes, then add 0.5～1.5 part, peeling inhibitor, catalyst n, N, N ', 1～5 part of 2～6 parts of N '-Tetramethyl Ethylene Diamines and initiator ammonium persulfate, stir after 20～60 seconds injection molding at once, after the demoulding, form base substrate;
3) base substrate is at room temperature dried to 24～48 hours, then in baking oven 60～90 ℃ dry 24～36 hours, finally in air, at 1500～1550 ℃, carry out pyroreaction sintering, burn off organism gel, just can obtain and have macroscopic pores and micron hole and the controlled Y of porosity concurrently 2si 2o 7porous ceramic film material.γ-Y 2si 2o 7the porosity ranges of porous ceramic film material is 75～85%, and macroscopic pores is uniformly distributed, and pore diameter range is 80～300 μ m, and the hole wall of macroscopic pores has a micron hole, and pore diameter range is 0.1～2 μ m.
In the present invention, Y 2o 3and SiO 2the size scope of mixed powder be 0.1～3.5 μ m, organic monomer is acrylamide or N hydroxymethyl acrylamide, dispersion agent is polymine or ammonium citrate; Peeling inhibitor is polyacrylamide, polyoxyethylene, polyoxyethylene glycol or starch; Catalyst n, N, N ', N '-Tetramethyl Ethylene Diamine and initiator ammonium persulfate are that massfraction is 15～25% the aqueous solution; The temperature rise rate of pyroreaction sintering is 4～8 ℃/min, and soaking time is 1.5～2.5 hours.
Below by embodiment in detail the present invention is described in detail.
Embodiment 1
First take deionized water 50g, under constantly stirring, add successively polymine 1.5g, acrylamide 6g, N, N '-methylene-bisacrylamide 0.9g, and Y 2o 3and SiO 2the mixed powder 120g of mol ratio 1:2, mixes, and then stirs 4 hours, forms slurry;
Then in slurry, add sodium lauryl sulphate 1.5g, rapid stirring (stirrer rotating speed is 1500rpm) foams 30 minutes, then add polyoxyethylene 1.5g, N, N, N ', the aqueous solution 5g that the aqueous solution 6g that N '-Tetramethyl Ethylene Diamine massfraction is 15% and ammonium persulphate massfraction are 25%, stirs after 20 seconds injection molding at once and solidifies, and forms base substrate after the demoulding;
By base substrate at room temperature dry 48 hours, then in baking oven 90 ℃ dry 24 hours, finally in air, with 6 ℃/min of temperature rise rates, be heated to 1525 ℃ and carry out pyroreaction sintering and be incubated 2 hours obtaining γ-Y 2si 2o 7porous ceramics.In the present embodiment, the porosity of sample is 75.5%, and compressive strength is 7.73MPa.γ-Y 2si 2o 7the microscopic appearance of porous ceramics is by the SEM photo demonstration of Fig. 1 (a) and Fig. 1 (b), and the macroscopic pores pore size of sample is 80～200 μ m, and hole window size is 20～70 μ m.In the present embodiment, micron hole size is 0.2～1.6 μ m.
Embodiment 2
First take deionized water 30g, under constantly stirring, add successively ammonium citrate 0.5g, acrylamide 4g, N, N '-methylene-bisacrylamide 0.3g, and Y 2o 3and SiO 2the mixed powder 80g of mol ratio 1:2, mixes, and then stirs 1 hour, forms slurry;
Then in slurry, add sodium lauryl sulphate 0.5g, rapid stirring (stirrer rotating speed is 1800rpm) foams 15 minutes, then add polyoxyethylene glycol 0.5g, N, N, N ', the aqueous solution 4g that the aqueous solution 2g that N '-Tetramethyl Ethylene Diamine massfraction is 25% and ammonium persulphate massfraction are 20%, stirs after 60 seconds injection molding at once and solidifies, and forms base substrate after the demoulding;
By base substrate at room temperature dry 24 hours, then in baking oven 60 ℃ dry 36 hours, finally in air, with 4 ℃/min of temperature rise rates, be heated to 1500 ℃ and carry out pyroreaction sintering and be incubated 2.5 hours obtaining Y 2si 2o 7porous ceramics.In the present embodiment, the porosity of sample is 80.6%, and compressive strength is 5.10MPa.The microscopic appearance of porous ceramics is by the SEM photo demonstration of Fig. 1 (c), and a micron hole size for sample is 0.3～2 μ m, and grain size is 2～7 μ m.In the present embodiment, macroscopic pores pore size is 90～210 μ m.
Embodiment 3
First take deionized water 40g, under constantly stirring, add successively ammonium citrate 1g, N hydroxymethyl acrylamide 8g, N, N '-methylene-bisacrylamide 0.5g, and Y 2o 3and SiO 2the mixed powder 100g of mol ratio 1:2, mixes, and then stirs 2.5 hours, forms slurry;
Then in slurry, add sodium lauryl sulphate 1g, rapid stirring (stirrer rotating speed is 1300rpm) foams 25 minutes, then add starch 1g, N, N, N ', the aqueous solution 3g that the aqueous solution 5g that N '-Tetramethyl Ethylene Diamine massfraction is 20% and ammonium persulphate massfraction are 15%, stirs after 50 seconds injection molding at once and solidifies, and forms base substrate after the demoulding;
By base substrate at room temperature dry 36 hours, then in baking oven 75 ℃ dry 30 hours, finally in air, with 7.5 ℃/min of temperature rise rates, be heated to 1550 ℃ and carry out pyroreaction sintering and be incubated 1.5 hours obtaining γ-Y 2si 2o 7porous ceramics.In the present embodiment, the porosity of sample is 84.6%, and compressive strength is 3.09MPa.The macroscopic pores pore size of sample is 70～250 μ m, and micron hole size is 0.3～1.5 μ m.The XRD spectrum demonstration of corresponding phase composite in accompanying drawing 2, as can be seen from Figure 2, sample is comparatively pure γ-Y 2si 2o 7phase.
Embodiment result shows, adopting process of the present invention simply foams and notes solidifying method, can be by regulating the addition of whipping agent to control porosity, the porous ceramic articles that adopts the method to prepare has very high porosity and higher compressive strength, and can prepare the porous ceramics that has macroscopic pores and micron hole concurrently.

Claims (6)

1. a preparation method for high porosity and high strength yttrium silica porous ceramics, is characterized in that, yttrium silica stupalith is γ-Y 2si 2o 7porous ceramics, concrete steps are as follows:
1) preparation of slurry: according to the mass fraction, with Y 2o 3and SiO 280～120 parts of the mixed powders of mol ratio 1:2,30～50 parts of deionized waters, 4～8 parts of organic monomers, 0.5～1.5 part of dispersion agent, linking agent N, 0.3～0.9 part of N '-methylene-bisacrylamide is raw material, mix, then stir 1～4 hour, form slurry;
2) according to the mass fraction, in described slurry, add 0.5～1.5 part of whipping agent sodium lauryl sulphate, stirring is foamed 15～30 minutes, then add 0.5～1.5 part, peeling inhibitor, catalyst n, N, N ', 1～5 part of 2～6 parts of N '-Tetramethyl Ethylene Diamines and initiator ammonium persulfate, stir after 20～60 seconds injection molding at once, after the demoulding, form base substrate;
3) by base substrate at room temperature dry 24～48 hours, then in baking oven 60～90 ℃ dry 24～36 hours, finally in air, at 1500～1550 ℃, carry out pyroreaction sintering, burn off organism gel, just can obtain the γ-Y that has macroscopic pores and micron hole concurrently 2si 2o 7porous ceramic film material.
2. according to the preparation method of high porosity claimed in claim 1 and high strength yttrium silica porous ceramics, it is characterized in that γ-Y 2si 2o 7the porosity ranges of porous ceramic film material is 75～85%, and macroscopic pores is uniformly distributed, and pore diameter range is 80～300 μ m, and the hole wall of macroscopic pores has a micron hole, and pore diameter range is 0.1～2 μ m.
3. according to the preparation method of high porosity claimed in claim 1 and high strength yttrium silica porous ceramics, it is characterized in that Y 2o 3and SiO 2the size scope of mixed powder be 0.1～3.5 μ m.
4. according to the preparation method of high porosity claimed in claim 1 and high strength yttrium silica porous ceramics, it is characterized in that, organic monomer is acrylamide or N hydroxymethyl acrylamide, and dispersion agent is polymine or ammonium citrate; Peeling inhibitor is polyacrylamide, polyoxyethylene, polyoxyethylene glycol or starch.
5. according to the preparation method of high porosity claimed in claim 1 and high strength yttrium silica porous ceramics, it is characterized in that, catalyst n, N, N ', N '-Tetramethyl Ethylene Diamine and initiator ammonium persulfate are the aqueous solution of massfraction 15～25%.
6. according to the preparation method of high porosity claimed in claim 1 and high strength yttrium silica porous ceramics, it is characterized in that, the temperature rise rate of pyroreaction sintering is 4～8 ℃/min, and soaking time is 1.5～2.5 hours.
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CN103951462A (en) * 2014-04-28 2014-07-30 胡海波 Preparation method of high-strength light-weight ceramic plate
CN104387110A (en) * 2014-10-30 2015-03-04 中国科学院金属研究所 Green preparation method of light-weight low-thermal-conductivity gamma-Y2Si2O7 porous ceramic
CN104402522A (en) * 2014-10-31 2015-03-11 中航复合材料有限责任公司 Method and device for preparing porous ceramic by heavy gas-protective direct-foaming technology
CN105036788A (en) * 2015-09-01 2015-11-11 中国科学院重庆绿色智能技术研究院 Preparation method of foamed ceramic
CN105985131A (en) * 2015-02-12 2016-10-05 中国科学院金属研究所 Method for preparing Y2SiO5 porous material with high temperature resistance and low thermal conductivity
CN109251040A (en) * 2018-09-28 2019-01-22 航天特种材料及工艺技术研究所 A kind of porous aluminum carbon matrix precursor and preparation method thereof
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CN103011817A (en) * 2012-12-24 2013-04-03 中国科学院金属研究所 Preparation method of yttrium-silicon-oxygen porous high-temperature ceramic material

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CN102659398A (en) * 2012-04-25 2012-09-12 中钢集团洛阳耐火材料研究院有限公司 Method for manufacturing light magnesia-alumina spinel insulation materials
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CN103951462A (en) * 2014-04-28 2014-07-30 胡海波 Preparation method of high-strength light-weight ceramic plate
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CN104387110B (en) * 2014-10-30 2016-01-13 中国科学院金属研究所 The low thermal conductance γ of a kind of lightweight-Y 2si 2o 7the environment-friendly preparation method thereof of porous ceramics
CN104402522A (en) * 2014-10-31 2015-03-11 中航复合材料有限责任公司 Method and device for preparing porous ceramic by heavy gas-protective direct-foaming technology
CN104402522B (en) * 2014-10-31 2016-03-30 中航复合材料有限责任公司 The direct foaming of a kind of heavy gas shield prepares method and the device of porous ceramics
CN105985131A (en) * 2015-02-12 2016-10-05 中国科学院金属研究所 Method for preparing Y2SiO5 porous material with high temperature resistance and low thermal conductivity
CN105036788B (en) * 2015-09-01 2017-06-23 中国科学院重庆绿色智能技术研究院 The preparation method of foamed ceramics
CN105036788A (en) * 2015-09-01 2015-11-11 中国科学院重庆绿色智能技术研究院 Preparation method of foamed ceramic
CN109251040A (en) * 2018-09-28 2019-01-22 航天特种材料及工艺技术研究所 A kind of porous aluminum carbon matrix precursor and preparation method thereof
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CN113134893A (en) * 2020-01-20 2021-07-20 西部宝德科技股份有限公司 Preparation method of ceramic fiber filter tube for high-temperature flue gas purification
CN111747754A (en) * 2020-07-10 2020-10-09 中国人民解放军国防科技大学 Carbon fiber reinforced SiYOC composite material and preparation method thereof
CN115872732A (en) * 2023-02-23 2023-03-31 中国人民解放军国防科技大学 Porous yttrium silicate-aluminum oxide complex phase wave-transmitting ceramic and preparation method thereof
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