CN102344297A - Forming method for preparing Si3N4 porous ceramic through tertiary butyl alcohol (TBA)-based gel casting method - Google Patents
Forming method for preparing Si3N4 porous ceramic through tertiary butyl alcohol (TBA)-based gel casting method Download PDFInfo
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Abstract
The invention discloses a forming method for preparing Si3N4 porous ceramic through a tertiary butyl alcohol (TBA)-based gel casting method, belonging to the field of porous ceramic. In the method, TBA is used as a new solvent instead of the solvent water in the traditional water-based gel casting forming. The method comprises the following steps: dissolving acrylamide, N,N'-methylene bisacrylamide and polyvinyl pyrrolidone in the TBA, and preparing into a premixed liquid; then adding Si3N4, Al2O3 and Y2O3, and carrying out ball milling for 12 hours; and carrying out forming, drying, binder removal, sintering and other procedures to prepare high-porosity high-strength silicon nitride porous ceramic, wherein the porosity of the ultimately prepared Si3N4 porous ceramic ranges between 40% and 75%, and the strength is 40-140 Mpa. The method has the following advantages: (1) the problem of Si3N4 hydrolysis in the conventional water-based gel casting forming process is avoided; and (2) the problem of high cracking possibility during the forming and drying of water-based gel casting is solved, and the forming and drying process of gel casting is simplified.
Description
Technical field
The present invention relates to a kind of trimethyl carbinol base (TBA) gel injection legal system and be equipped with Si
3N
4The technology of porous ceramics belongs to the porous ceramics field.
Background technology
Porous ceramics is to be one type of stupalith of principal phase with the gas phase, has advantage high temperature resistant, corrosion-resistant and that thermal shock resistance is good than other porous material, has broad application prospects in fields such as metallurgy, chemical industry, biology, aerospace.Great amount of manpower and material resources has all been dropped in countries in the world, financial resources are used for the research of this type of material, and has obtained bigger progress.
Silicon nitride ceramics is one of over-all properties best material in the structural ceramics.Except having the general ceramic material high strength, high elastic coefficient, high temperature resistant, outside the advantage such as corrosion-resistant, have also that specific inductivity is low, dielectric loss is little, the high-frequency dielectric steady performance, become one of focus in space flight, the aeronautical material research field gradually.
The characteristics of porous ceramics are that a large amount of pores are arranged, so the key of its preparation and difficult point form vesicular structure exactly.The preparation technology of common porous ceramics has: extrusion moulding, add the pore-forming material method, sol-gel method, freeze-drying, reaction sintering, gel casting forming method etc.
The gel casting forming method is a kind of new ceramics moulding process of U.S.'s Oak Ridge laboratory development in 1992; The inner little additive (monomer and linking agent) of this technology utilization slurry thus the chemical reaction effect make the ceramic size original position solidify the formation base substrate; Acquisition has the biscuit of good microscopic uniformity, thus the reliability of material of significantly improving.This method has that cost is low, and equipment is simple, and pore is even, and biggest advantage is can the moulding complicated shape.Water-base gel casting technology is mature on the whole at present, but in the water-base gel casting process, because the surface tension of water is big, the contraction that base substrate produces in drying process is big, thereby easy of crack; Water saturation vapour pressure in addition is little, is not easy volatilization, so time of drying is very long, and the exsiccant environmental requirement is also relatively harsher, need be long-time dry in the low temperature and high relative humidity environment.
With the water ratio, the surface tension of the trimethyl carbinol (TBA) is little, and saturated vapor pressure is big, can effectively alleviate in the aqueous gel casting process, and body drying distortion, rimose problem, and can effectively shorten time of drying.Up to the present having only Tsing-Hua University's new ceramics and hand work National Key Laboratory to adopt TBA is that solvent prepares aluminum oxide and zirconium white.Document Ceramics With Ultra-Low Density Fabricated by Gel-casting:An Unconventional Vie (Ruifeng Chen; Yong Huang etc; J.Am.Ceram.Soc.90[11] 3424-3429 (2007)), having prepared volume fraction is the Al of 5-15%
2O
3Pottery, void content 60%-92% wherein, intensity is 10-50Mpa; Document Porous yttria stabilized zirconia ceramics with ultra-low thermal conductivity (Liang Fa Hu; Chang An Wang; Yong Huang; J Mater Sci (2010) 45:3242-3246) be solvent with TBA in; Prepared high porosity (52-76%) with the gel casting forming method, and the ZrO of even aperture distribution (0.7-1.8 μ m)
2Pottery, above-mentioned report all are to be equipped with oxide ceramics with TBA base gel injection legal system, and the processability of oxide ceramics is relatively good, but the strength ratio of oxide ceramics goods is lower.
At present, also not retrieving with TBA is solvent, adopts the gel injection legal system to be equipped with porous Si
3N
4The document and the open patent of invention of pottery.
Summary of the invention
The objective of the invention is to seek a kind of novel dissolvent and replace water, adopt the gel injection method to prepare high-performance high porosity (40-75%), high strength (40-140Mpa) porous SiN ceramic.The objective of the invention is to realize through following technological process:
(1) monomer acrylamide (AM), 1-6% linking agent nitrogen-nitrogen methylene-bisacrylamide (MBAM), 1-5% polyethylene of dispersing agent pyrrolidone (PVP) and the 40-80% trimethyl carbinol of pressing 5-30% mixes; The preparation premixed liquid adds 20-60% beta-silicon nitride powder and 3-10% sintering aid (Al in premixed liquid
2O
3Y
2O
3), make slurry behind the ball milling 8-24h.
(2) slurry adds the initiator (ammonium persulphate) of 2-10% then through vacuum stripping, behind the catalyzer of 1-5% (Tetramethyl Ethylene Diamine), and vacuum stripping 20s again, injection molding, moulding in 30-65 ℃ of water-bath.The demoulding behind the 60min, drying obtained dry base substrate in 24 hours under the room temperature ventilated environment.
(3) with dry base substrate slow binder removal in air furnace, the highest dump temperature is 560 ℃, and temperature rise rate is 0.2 ℃/min; Be lower than 1200 ℃ of employing vacuum sinterings at last; Be higher than 1200 ℃ and adopt gas pressure sintering, final sintering temperature is 1650-1800 ℃, and soaking time 0.5-3 hour, sintering atmosphere was a nitrogen.
(4) the invention is characterized in the little and high characteristic of saturated vapor pressure of the surface tension of utilizing TBA; Solved in the water-base gel casting technology shortcoming of length consuming time in the body drying process and easy of crack; Simplify drying process, improved efficient and success ratio.
The invention has the advantages that:
(1) adopts TBA to replace water, can shorten time of drying significantly, simplified drying process as solvent.
(2) because the saturated vapor pressure of TBA is big, and surface tension is little, make base substrate shrinking percentage in dry and binder removal process little, solved base substrate easy deformation and rimose shortcoming, improved yield rate.
(3) because drying distortion and the shrinking percentage of base substrate in dry and binder removal process is little, make α-Si
3N
4To β-Si
3N
4There is enough space to grow during transformation, thereby, improved the length-to-diameter ratio (length-to-diameter ratio＞10) of bar-shaped β-Si3N4 crystal grain greatly, intercrystalline is overlapped fully.Therefore, not only improve the void content (40-75%) of porous SiN ceramic, and improved intensity (40-140Mpa).
Description of drawings
Fig. 1 is that AM and MBAM total content are 15wt%, and ratio is 4: 1 o'clock, and sintering temperature is 1700 ℃, the XRD figure of sintered compact spectrum when being incubated 1 hour.Can know that by figure principal crystalline phase is β-Si
3N
4
Fig. 2 is that AM and MBAM total content are 15wt%, and ratio is 4: 1, and solid load is 30%, and sintering temperature is 1700 ℃, is incubated the SEM photo of 1 hour sintered compact fracture.
Fig. 3 be the sample of different solid loads at 1700 ℃ of sintering, the porous Si that obtains behind the insulation 1h
3N
4The void content and the bending strength of pottery.
Embodiment
(1) Si
3N
4Powder is 20wt%, and the TBA powder is 80wt%, and organic content is Si
3N
4Reach 15% of TBA gross weight, wherein the ratio of AM and MBAM is 4: 1
(2) Si
3N
4Powder is 30wt%, and the TBA powder is 70wt%, and organic content is Si
3N
4Reach 15% of TBA gross weight, wherein the ratio of AM and MBAM is 4: 1
(3) Si
3N
4Powder is 40wt%, and the TBA powder is 60wt%, and organic content is Si
3N
4Reach 15% of TBA gross weight, wherein the ratio of AM and MBAM is 4: 1
(4) Si
3N
4Powder is 50wt%, and the TBA powder is 50wt%, and organic content is Si
3N
4Reach 15% of TBA gross weight, wherein the ratio of AM and MBAM is 4: 1
(5) Si
3N
4Powder is 60wt%, and the TBA powder is 40wt%, and organic content is Si
3N
4Reach 15% of TBA gross weight, wherein the ratio of AM and MBAM is 4: 1
Embodiment 1
Processing step is following:
(1) ball milling: the Si that takes by weighing 20wt% according to the design component
3N
4Behind the TBA powder of powder and 80wt%, add 15% organism, wherein the ratio of AM and MBAM is 4: 1.Thorough mixing is even then, and as mill ball, the material powder: agate ball=1: 1 (mass ratio) places the nylon jar to utilize roll-type ball mill batch mixing 12h with agate ball;
(2) moulding: the slip that ball milling is good is poured in the mould of tetrafluoroethylene, is placed on 30-65 ℃ water-bath 35-60min moulding; The demoulding then
(3) drying: the base substrate that the demoulding is come out is placed on the sheet glass, dry 24h under the state of natural ventilation;
(4) binder removal: slow binder removal in air furnace, the highest dump temperature is 560 ℃, temperature rise rate is 0.2 ℃/min;
(5) high temperature sintering: sample places sintering under the high temperature after the nitrogenize, 1700 ℃ of sintering temperatures, soaking time 1.5h;
Product of the present invention is porous Si
3N
4Pottery, wherein void content is 75.6%, and bending strength is 36.5MPa, and crystal grain diameter is 0.5 μ m, and length-to-diameter ratio is 6-10.
Embodiment 2
(1) ball milling: the Si that takes by weighing 30wt% according to the design component
3N
4Behind the TBA powder of powder and 70wt%, add 15% organism, wherein the ratio of AM and MBAM is 4: 1.Thorough mixing is even then, and as mill ball, the material powder: agate ball=1: 1 (mass ratio) places the nylon jar to utilize roll-type ball mill batch mixing 12h with agate ball;
(2) moulding: the slip that ball milling is good is poured in the mould of tetrafluoroethylene, is placed on 30-65 ℃ water-bath 35-60min moulding; The demoulding then;
(3) drying: the base substrate that the demoulding is come out is placed on the sheet glass, dry 24h under the state of natural ventilation;
(4) binder removal: slow binder removal in the air road, the highest dump temperature is 560 ℃, temperature rise rate is 0.2 ℃/min;
(5) high temperature sintering: sample places sintering under the high temperature after the nitrogenize, 1700 ℃ of sintering temperatures, soaking time 1.5h;
Product of the present invention is porous Si
3N
4Pottery, wherein void content is 68.5%, bending strength is 62.5MPa.
Embodiment 3
(1) ball milling: the Si that takes by weighing 40wt% according to the design component
3N
4Behind the TBA powder of powder and 60wt%, add 15% organism, wherein the ratio of AM and MBAM is 4: 1.Thorough mixing is even then, and as mill ball, the material powder: agate ball=1: 1 (mass ratio) places the nylon jar to utilize roll-type ball mill batch mixing 12h with agate ball;
(2) moulding: the slip that ball milling is good is poured in the mould of tetrafluoroethylene, is placed on 30-65 ℃ water-bath 35-60min moulding; The demoulding then;
(3) drying: the base substrate that the demoulding is come out is placed on the sheet glass, dry 24h under the state of natural ventilation;
(4) binder removal: slow binder removal in the air road, the highest dump temperature is 560 ℃, temperature rise rate is 0.2 ℃/min
(5) high temperature sintering: sample places sintering under the high temperature after the nitrogenize, 1700 ℃ of sintering temperatures, soaking time 1.5h;
Product of the present invention is porous Si
3N
4Pottery, wherein void content is 62.5%, bending strength is 96.5MPa.
Embodiment 4
(1) ball milling: the Si that takes by weighing 50wt% according to the design component
3N
4Behind the TBA powder of powder and 50wt%, add 15% organism, wherein the ratio of AM and MBAM is 4: 1.Thorough mixing is even then, and as mill ball, the material powder: agate ball=1: 1 (mass ratio) places the nylon jar to utilize roll-type ball mill batch mixing 12h with agate ball;
(2) moulding: the slip that ball milling is good is poured in the mould of tetrafluoroethylene, is placed on 30-65 ℃ water-bath 35-60min moulding; The demoulding then;
(3) drying: the base substrate that the demoulding is come out is placed on the sheet glass, dry 24h under the state of natural ventilation;
(4) binder removal: slow binder removal in the air road, the highest dump temperature is 560 ℃, temperature rise rate is 0.2 ℃/min;
(5) high temperature sintering: sample places sintering under the high temperature after the nitrogenize, 1700 ℃ of sintering temperatures, soaking time 1.5h;
Product of the present invention is porous Si
3N
4Pottery, wherein void content is 50.8%, bending strength is 125.5MPa.
Embodiment 5
(1) ball milling: the Si that takes by weighing 60wt% according to the design component
3N
4Behind the TBA powder of powder and 40wt%, add 15% organism, wherein the ratio of AM and MBAM is 4: 1., thorough mixing is even then, and as mill ball, the material powder: agate ball=1: 1 (mass ratio) places the nylon jar to utilize roll-type ball mill batch mixing 12h with agate ball;
(2) moulding: the slip that ball milling is good is poured in the mould of tetrafluoroethylene, is placed on 30-65 ℃ water-bath 35-60min moulding; The demoulding then;
(3) drying: the base substrate that the demoulding is come out is placed on the sheet glass, dry 24h under the state of natural ventilation;
(4) binder removal: slow binder removal in the air road, the highest dump temperature is 560 ℃, temperature rise rate is 0.2 ℃/min;
(5) high temperature sintering: sample places sintering under the high temperature after the nitrogenize, 1700 ℃ of sintering temperatures, soaking time 1.5h;
Product of the present invention is porous Si
3N
4Pottery, wherein void content is 42.5%, bending strength is 140.5MPa.
Above content is to combine concrete preferred implementation to further explain that the present invention did; Can not assert that the specific embodiment of the present invention only limits to this; Those of ordinary skill for technical field under the present invention; Under the prerequisite that does not break away from the present invention's design; Can also make some simple deduction or replace, all should be considered as belonging to the present invention and confirm scope of patent protection by claims of being submitted to.
Claims (7)
1. a trimethyl carbinol base gel injection legal system is equipped with Si
3N
4The forming method of porous ceramics, this method comprises: slip preparation, moulding, drying, binder removal and sintering is characterized in that:
(1) slip preparation: monomer acrylamide, 1-6wt% linking agent nitrogen-nitrogen methylene-bisacrylamide, 1-5wt% polyethylene of dispersing agent pyrrolidone and the 40-80wt% trimethyl carbinol of 5-30wt% are mixed the preparation premixed liquid; In premixed liquid, add beta-silicon nitride powder that accounts for premixed liquid total amount 20-60wt% and the sintering aid that accounts for premixed liquid total amount 3-10wt%, make slurry behind the ball milling 8-24h;
(2) moulding: with the slip for preparing through vacuum stripping, after adding the initiator that accounts for slip 2-10wt% then and accounting for the catalyzer of slip 1-5wt%, injection molding behind the vacuum stripping 20s again, the demoulding behind the moulding 60min in 30-65 ℃ of water-bath;
(3) drying: with base substrate dry 24h under the room temperature ventilation condition of the demoulding;
(4) binder removal: slow binder removal in air furnace, the highest dump temperature is 560 ℃, temperature rise rate is 0.2 ℃/min;
(5) sintering: be lower than 1200 ℃ of employing vacuum sinterings; Be higher than 1200 ℃ and adopt gas pressure sintering, final sintering temperature is 1650-1800 ℃, and soaking time 0.5-3 hour, sintering atmosphere was a nitrogen.
2. by the described preparation method of claim 1, it is characterized in that: described monomer is an acrylamide, and linking agent is nitrogen-nitrogen methylene-bisacrylamide.
3. by the described preparation method of claim 1, it is characterized in that: described dispersion agent is the PVP polyvinylpyrrolidone.
4. by the described preparation method of claim 1, it is characterized in that: described sintering aid is aluminum oxide and yttrium oxide, and the adding total amount of sintering aid is the 3-10wt% that accounts for the premixed liquid total amount.
5. by the described preparation method of claim 1, it is characterized in that said sintering process is carried out stage by stage: adopt vacuum sintering below 1200 ℃, 10 ℃/minute of temperature rise rates; Adopt air pressure to burn more than 1200 ℃, 5 ℃/minute of temperature rise rates are incubated 0.5-3 hour, and atmosphere is nitrogen.
6. by the described preparation method of claim 1, it is characterized in that: the said trimethyl carbinol is a solvent.
7. by claim 1,2,3,4 or 5 described preparing methods, it is characterized in that: the porous SiN ceramic of said preparing method's preparation has high porosity 40-75% and high-flexural strength 40-140Mpa.
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Cited By (8)
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|---|---|---|---|---|
| CN102824784A (en) * | 2012-08-23 | 2012-12-19 | 武汉理工大学 | Porous ceramic filtration device for suction vehicle and double-pressure feeding vehicle |
| CN103232264A (en) * | 2013-04-18 | 2013-08-07 | 哈尔滨工业大学 | Preparation method of BN/Si3N4 composite ceramic with spherical porous structure |
| CN103406973A (en) * | 2013-07-25 | 2013-11-27 | 中南大学 | Formation technology for preparation of porous or compact material with gel-casting of alcohol-water basic material slurry |
| CN103664190A (en) * | 2013-11-26 | 2014-03-26 | 河海大学 | Method for preparing porous silicon nitride ceramic |
| CN107353036A (en) * | 2017-08-21 | 2017-11-17 | 广东工业大学 | A kind of porous silicon nitride ceramic based on increases material manufacturing technology, its preparation method and its application |
| CN108752008A (en) * | 2018-06-14 | 2018-11-06 | 哈尔滨工业大学 | A kind of porous Si2N2O high temperature resistant wave-permeable ceramics and preparation method thereof |
| CN111410540A (en) * | 2020-03-05 | 2020-07-14 | 中国科学院上海硅酸盐研究所 | Preparation method of porous silicon nitride ceramic with directional pore structure |
| CN114956820A (en) * | 2022-05-31 | 2022-08-30 | 西北工业大学 | Rare earth composite oxide porous high-entropy ceramic and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102824784A (en) * | 2012-08-23 | 2012-12-19 | 武汉理工大学 | Porous ceramic filtration device for suction vehicle and double-pressure feeding vehicle |
| CN103232264A (en) * | 2013-04-18 | 2013-08-07 | 哈尔滨工业大学 | Preparation method of BN/Si3N4 composite ceramic with spherical porous structure |
| CN103406973A (en) * | 2013-07-25 | 2013-11-27 | 中南大学 | Formation technology for preparation of porous or compact material with gel-casting of alcohol-water basic material slurry |
| CN103406973B (en) * | 2013-07-25 | 2015-08-05 | 中南大学 | A kind of alcohol aqueous gel-casting prepares the moulding process of porous or dense material |
| CN103664190A (en) * | 2013-11-26 | 2014-03-26 | 河海大学 | Method for preparing porous silicon nitride ceramic |
| CN103664190B (en) * | 2013-11-26 | 2016-02-10 | 河海大学 | A kind of preparation method of porous silicon nitride ceramic |
| CN107353036A (en) * | 2017-08-21 | 2017-11-17 | 广东工业大学 | A kind of porous silicon nitride ceramic based on increases material manufacturing technology, its preparation method and its application |
| CN107353036B (en) * | 2017-08-21 | 2020-10-23 | 广东工业大学 | Porous silicon nitride ceramic based on additive manufacturing technology, and preparation method and application thereof |
| CN108752008A (en) * | 2018-06-14 | 2018-11-06 | 哈尔滨工业大学 | A kind of porous Si2N2O high temperature resistant wave-permeable ceramics and preparation method thereof |
| CN108752008B (en) * | 2018-06-14 | 2020-07-21 | 哈尔滨工业大学 | Porous Si2N2O high-temperature-resistant wave-transparent ceramic and preparation method thereof |
| CN111410540A (en) * | 2020-03-05 | 2020-07-14 | 中国科学院上海硅酸盐研究所 | Preparation method of porous silicon nitride ceramic with directional pore structure |
| CN114956820A (en) * | 2022-05-31 | 2022-08-30 | 西北工业大学 | Rare earth composite oxide porous high-entropy ceramic and preparation method and application thereof |
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Application publication date: 20120208 |