CN103121854A - Porous silicon nitride ceramic and production method thereof - Google Patents
Porous silicon nitride ceramic and production method thereof Download PDFInfo
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- CN103121854A CN103121854A CN2011103663402A CN201110366340A CN103121854A CN 103121854 A CN103121854 A CN 103121854A CN 2011103663402 A CN2011103663402 A CN 2011103663402A CN 201110366340 A CN201110366340 A CN 201110366340A CN 103121854 A CN103121854 A CN 103121854A
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Abstract
The invention relates to porous silicon nitride ceramic and a production method thereof. A product of the porous silicon nitride ceramic has silicon nitride in beta-phase silicon nitride crystal form in cylinder or rod shape. The product is 20-65% in total porosity and 450-50MPa in bending strength. The silicon nitride in the product of porous silicon nitride ceramic is in the beta-phase crystal form in the cylinder or rod shape, and strength and toughness of the product can be improved further.
Description
Technical field
The invention belongs to the porous silicon nitride ceramic field, relate to a kind of porous silicon nitride ceramic and utilize from the method that spreads the standby porous silicon nitride ceramic of legal system, relate more specifically to take silica flour and silicon nitride powder as raw material, by certainly spreading the preparation method of the standby porous silicon nitride ceramic of legal system.
Background technology
Porous silicon-nitride ceramic material is owing to having lightweight, the characteristics such as high temperature resistant, corrosion-resistant, have wide practical use in fields such as high temperature air filtration, sensor, support of the catalyst, separatory membranes, therefore the preparation method about porous silicon nitride ceramic becomes one of focus of present research.But present research is raw material mainly with the silicon nitride powder of costliness, prepares porous silicon-nitride ceramic material by with no pressure or gas pressure sintering.From cost consideration, prepare porous silicon-nitride ceramic material take silica flour as raw material and will more be conducive to realize its industrialization promotion.
To provide necessary energy by the outside from the method for spreading, bring out the local chemical reaction that occurs of high heat-producing chemical reaction system, then with the carrying out of the automatic holding reaction of fast automatic ripple burning, show as combustion wave and spread in whole reaction system, last synthetic materials.Particularly the method that certainly spreads of nitrogen-silicon system is synthetic, and reaction is undertaken by the nitrogen of gas phase and the pasc reaction of solid phase under condition of high voltage, but not enough the carrying out that can affect reaction of the hole gas between silica flour makes final reacting product have remaining silicon to exist.Therefore generally all adopt the silicon nitride powder that adds certain content as weighting agent/thinner, sufficient hole is provided, thereby promotes to react completely.
Chinese patent literature CN1657496 discloses a kind of working method of micro-component of silicon nitride ceramics, it uses the Si powder as raw material, and Si powder is inserted in graphite jig, use hot-press arrangement or plasma discharge sinter machine to carry out presintering, again with silica flour pre-burning body mechanical workout flakiness, workpiece after processing is placed in graphite or silicon nitride crucible, put into the electric furnace chamber that is connected with nitrogen and carry out nitriding treatment, and at crucible bottom place mat boron nitride particle, workpiece is placed on boron nitride particle, carry out nitriding treatment in 1300～1450 ℃ of temperature ranges.The disclosed method of CN1657496 is only applicable to prepare laminar parts, has certain density after the pre-burning of silica flour formed body and intensity can realize little processing, if but the thickness of workpiece is enough not thin, the silicon that can't guarantee to have in the nitriding treatment process in the silica flour forming and sintering body of certain density all is nitrided into silicon nitride, therefore can not utilize described method to make the silicon nitride ceramic parts with higher-strength and toughness.
The preparation technology of porous ceramics has foaming, adds pore-forming material method, gel injection method, hydro-thermal reaction method etc. at present.There is the low problem of porous ceramics intensity that technique is more complicated and prepare in existing method more.Chinese patent literature CN1433959A, CN1569742A disclose by self-propagating reaction and have prepared beta-silicon nitride powder, and the beta-silicon nitride whisker of preparing has very high intensity and toughness, can be used for realizing crystal whisker reinforced and toughened.But utilize from spreading the standby block body ceramic material of legal system report is not but arranged.
Summary of the invention
The inventor recognizes that the generation that realizes the column beta phase silicon nitride in block porous silicon-nitride ceramic material can obtain high-intensity bulk ceramic material.
The invention provides a kind of porous silicon nitride ceramic goods, in described porous silicon nitride ceramic goods, the form of silicon nitride is column or the crystallization of bar-shaped β phase; The goods total porosity is 20 ~ 65%, and bending strength is 450 ~ 50MPa.
Porous silicon nitride ceramic goods provided by the invention, comprising silicon nitride present column or bar-shaped β phase crystal habit, can further improve intensity and the toughness of product.
Porous silicon nitride ceramic goods provided by the invention be by the silica flour that will have certain fineness, silicon nitride powder, with the mixture compression molding of sintering aid be the formed body with definite shape, then formed body is placed in that via nitride in the self-propagating reaction cavity is processed and the porous silicon nitride ceramic goods with definite shape that make, wherein said formed body be embedded in help lend some impetus in the buried powder that formed body carries out self-propagating reaction and in the self-propagating reaction cavity via nitride process.
In starting material, the ratio of silica flour and silicon nitride powder can be 9～5:1～5.Again, the ratio of silica flour and silicon nitride powder is preferably 7～5:3～5.
Buried powder of the present invention can be the mixture of pure silicon powder or silica flour and silicon nitride powder.Again, in buried powder the ratio of silica flour and silicon nitride powder can select to have with formed body in the silica flour ratio identical with silicon nitride powder.
The present invention is by mixing it silica flour, silicon nitride powder and sintering aid ball milling in ball grinder and crossing the mixture that the 80-200 mesh sieve has certain fineness with acquisition.
It is that 1-50 μ m, purity are the silica flour of 80-99.99% that the present invention preferably adopts particle diameter.
The sintering aid that the present invention preferably adopts is Y
2O
3, Yb
2O
3, Lu
2O
3, Nd
2O
3, Er
2O
3, in one or more.
Disclosing the particle that makes wherein by self-overgrowth reaction process in prior art is the beta-silicon nitride powder of beta-silicon nitride crystal formation, does not but have report to utilize from spreading method and prepares the block body ceramic material with definite shape.The present invention realizes the nitrogenize of silica flour in starting material by certainly spreading method, and realizes the generation of column beta phase silicon nitride in having the ceramic bad body of definite shape, thereby obtains high-intensity porous silicon-nitride ceramic material.
Another aspect of the present invention provides a kind of preparation method of porous silicon nitride ceramic, comprise the silica flour that will have certain fineness, silicon nitride powder, with the mixture compression molding of sintering aid be the formed body with definite shape; Formed body is embedded in to help lend some impetus in the buried powder that formed body carries out self-propagating reaction inserts together in the self-propagating reaction cavity, via nitride is processed and is made the porous silicon nitride ceramic goods with definite shape.
Preparation method of the present invention, compression molding pressure is preferably 5-100MPa.Compression molding pressure is more preferably 5-50MPa.
In preparation method of the present invention, will have the silica flour of regulation ratio and silicon nitride powder in ball mill together with sintering aid ball milling, drying, cross the 80-200 mesh sieve to reach the mixture with certain fineness.Wherein, described Ball-milling Time can be 1～24 hour.In addition, the nitriding treatment time of the present invention is preferably 1～10 minute.
Again, utilizing the porous silicon nitride ceramic total porosity that preparation method of the present invention makes is 20 ~ 65%, and bending strength is 450 ~ 50MPa.
The present invention is take silica flour as reaction raw materials, take silicon nitride powder as filler, with respect to the pressureless sintering take pure silicon nitride powder as raw material or gas pressure sintering, cost obviously reduces, the technique power consumption is low, the time is short, be fit to the advantage of suitability for industrialized production in conjunction with certainly spreading simultaneously, thereby is conducive to realize the industrial-scale production of porous silicon-nitride ceramic material.The present invention realizes the nitrogenize of silicon by certainly spreading method, and can realize the generation of column beta phase silicon nitride, thereby obtains to have high-intensity porous silicon-nitride ceramic material.
Description of drawings
Fig. 1 illustrates the XRD figure of the porous silicon-nitride ceramic material in example embodiment of the present invention (embodiment 1); Wherein sample changes beta phase silicon nitride fully into;
Fig. 2 illustrates the stereoscan photograph of the porous silicon-nitride ceramic material of Fig. 1 of the present invention;
Fig. 3 illustrates the stereoscan photograph of the porous silicon-nitride ceramic material in another example embodiment of the present invention (embodiment 2);
Fig. 4 illustrates the stereoscan photograph of the porous silicon-nitride ceramic material in another example embodiment of the present invention (embodiment 4).
Embodiment
With reference to Figure of description, and further illustrate with the following embodiments the present invention, should be understood that Figure of description and following embodiment only are used for explanation the present invention, and unrestricted the present invention.
The invention provides a kind of porous silicon nitride ceramic goods, in goods, the form of silicon nitride is column or bar-shaped beta phase silicon nitride crystal habit; The goods total porosity is 20 ~ 65%, and bending strength is 450 ~ 50MPa.Make its main composition silicon nitride present column or bar-shaped β phase crystal habit in the porous silicon nitride ceramic goods, can further improve intensity and the toughness of product.
At this, the present invention also provides a kind of preparation method of porous silicon nitride ceramic, the silica flour by will have certain fineness, silicon nitride powder, with the mixture compression molding of sintering aid be the formed body with definite shape; Then formed body is embedded in to help lend some impetus in the buried powder that formed body carries out self-propagating reaction and inserts together in the self-propagating reaction cavity, via nitride is processed and is made the porous silicon nitride ceramic goods with definite shape.
In the preparation method of porous silicon nitride ceramic provided by the invention, by it being mixed silica flour, silicon nitride powder and sintering aid ball milling in ball grinder, and drying and cross the 80-200 mesh sieve with the silica flour that obtains to have certain fineness, silicon nitride powder, with the mixture of sintering aid.Wherein, Ball-milling Time can be 1～24 hour.In addition, silica flour, silicon nitride powder, with the mixture of sintering aid in the ratio of silica flour and silicon nitride powder can be 9～5:1～5; Described ratio is preferably 7～5:3～5.Again, wherein sintering aid can be Y
2O
3, Yb
2O
3, Lu
2O
3, Nd
2O
3, Er
2O
3In one or more.
In the preparation method of porous silicon nitride ceramic provided by the invention, when the formed body that has definite shape after compression molding is carried out nitriding treatment, for promoting to carry out smoothly self-propagating reaction through the formed body that the certain pressure moulding makes in the self-propagating reaction cavity, formed body can be embedded in then to insert together again in buried powder and carry out nitriding treatment in the self-propagating reaction cavity.Buried powder wherein can be the mixture of pure silicon powder or silica flour and silicon nitride powder.Again, when selecting buried powder to be the mixture of silica flour and silicon nitride powder, in buried powder, the ratio of silica flour and silicon nitride powder can have identical with the ratio of middle silica flour and silicon nitride powder in formed body.In addition, the time of nitriding treatment can be 1～10 minute, and the time is short, efficient is high.
Preparation method of the present invention is take silica flour as reaction raw materials, take silicon nitride powder as filler, with respect to the pressureless sintering take pure silicon nitride powder as raw material or gas pressure sintering, cost obviously reduces, the technique power consumption is low, the time is short, be fit to the advantage of suitability for industrialized production in conjunction with certainly spreading simultaneously, thereby is conducive to realize the industrial-scale production of porous silicon nitride.
In addition, by the porous silicon nitride ceramic of preparation method's preparation of the present invention, the total porosity of goods can reach 20 ~ 65%, and bending strength reaches 450 ~ 50MPa.In goods, the form of silicon nitride can be for example to be column or bar-shaped beta phase silicon nitride crystal habit; In addition, the length of described beta phase silicon nitride crystallization can be 7 ~ 20 μ m, and diameter is 0.5 ~ 3 μ m, and length-to-diameter ratio is 5 ~ 10.Again, in one embodiment, described column or bar-shaped beta phase silicon nitride crystallization are β-Si
3N
4
As mentioned above, have and openly utilize the self propagating high temperature synthetic method to prepare whisker to be the beta-silicon nitride powder of beta-silicon nitride crystal formation.But powder just can need to be produced the silicon nitride ceramics with definite shape through down-stream.Preparation method of the present invention utilize from spread method directly preparation realize the generation of column beta phase silicon nitride, can make have high porosity, low density, high-intensity block body ceramic material.
Below list some exemplary embodiments so that the present invention to be described better.Wherein the void content numerical value in each embodiment is to adopt the test of Archimedes's drainage to draw (GB/T 3810.3-2006); Bending strength test carries out on American I nstron company 5566 material universal testing machines, and loading rate is 0.5 mm/min, and span is 30mm, and sample size is 3mm * 4mm * 36mm.
Embodiment 1:
Take ethanol as solvent, silicon nitride ball is ball-milling medium, with mass ratio 70:30:6 with silica flour, silicon nitride powder and yttrium oxide ball milling 24 hours in ball grinder.With the slurry 60 ℃ of dryings in baking oven that mix, then cross 100 mesh sieves.Powder after sieving is pressed into porous body with stainless steel mould 10MPa.Base substrate is embedded in the silicon of same proportioning/silicon nitride buried powder, puts into the self-propagating reaction cavity, passes into nitrogen, and synthetic through ignition, the reaction times is 4 minutes, synthetic after naturally cooling in stove; Learn after testing: the void content of the porous silicon-nitride ceramic material that the present embodiment makes is 54%, and bending strength is 120MPa; Fig. 1 is the XRD figure of porous silicon-nitride ceramic material after self-propagating reaction in embodiment 1; Be β-Si through XRD determining
3N
4Fig. 2 is the stereoscan photograph of porous silicon-nitride ceramic material after self-propagating reaction in embodiment 1.And certainly to spread rear microscopic appearance be column or bar-shaped beta phase silicon nitride; The brilliant length of described beta phase silicon nitride rod is 7 ~ 20 μ m, and diameter is 0.5 ~ 3 μ m, and average aspect ratio is about 5 ~ 10.
Embodiment 2:
Take ethanol as solvent, silicon nitride ball is ball-milling medium, with mass ratio 50:50:6 with silica flour, silicon nitride powder and ytterbium oxide ball milling 24 hours in ball grinder.With the slurry 60 ℃ of dryings in baking oven that mix, then cross 100 mesh sieves.Powder after sieving is pressed into porous body with stainless steel mould 5MPa.Porous body is embedded in the silicon of same proportioning/silicon nitride buried powder, puts into the self-propagating reaction cavity, passes into nitrogen, and synthetic through ignition, the reaction times is 3 minutes, synthetic after naturally cooling in stove;
Learn after testing: the void content of the porous silicon-nitride ceramic material that the present embodiment makes is 59%, and bending strength is 110MPa;
Referring to Fig. 3, it shows in the present embodiment the stereoscan photograph of porous silicon-nitride ceramic material after self-propagating reaction.And certainly to spread rear microscopic appearance be column or bar-shaped beta phase silicon nitride.The brilliant length of described beta phase silicon nitride rod is 7 ~ 20 μ m, and diameter is 0.5 ~ 3 μ m, and average aspect ratio is about 5 ~ 10.
Embodiment 3:
Take ethanol as solvent, silicon nitride ball is ball-milling medium, with mass ratio 70:30:6 with silica flour, silicon nitride powder and yttrium oxide ball milling 24 hours in ball grinder.With the slurry 60 ℃ of dryings in baking oven that mix, then cross 100 mesh sieves.Powder after sieving is pressed into porous body with stainless steel mould 30MPa.Porous body is embedded in the silicon of same proportioning/silicon nitride buried powder, puts into the self-propagating reaction cavity, passes into nitrogen, and synthetic through ignition, the reaction times is 5 minutes, synthetic after naturally cooling in stove; Learn after testing: the microscopic appearance of the porous silicon nitride ceramic that the present embodiment makes is column or bar-shaped beta phase silicon nitride; The brilliant length of described beta phase silicon nitride rod is about 7 ~ 20 μ m, and diameter is about 0.5 ~ 3 μ m, and average aspect ratio is about 5 ~ 10; Further test the porous silicon nitride ceramic of the present embodiment preparation, its void content is 45%, and bending strength is 200MPa.
Embodiment 4:
Take ethanol as solvent, silicon nitride ball is ball-milling medium, with mass ratio 70:30:6 with silica flour, silicon nitride powder and lutecium oxide ball milling 24 hours in ball grinder.With the slurry 60 ℃ of dryings in baking oven that mix, then cross 100 mesh sieves.Powder after sieving is pressed into porous body with stainless steel mould 10MPa.Porous body is embedded in the silicon of same proportioning/silicon nitride buried powder, puts into the self-propagating reaction cavity, passes into nitrogen, and synthetic through ignition, the reaction times is 4 minutes, synthetic after naturally cooling in stove; Learn after testing: the void content of the porous silicon-nitride ceramic material that the present embodiment makes is 53%, and bending strength is 150MPa; Fig. 4 is the stereoscan photograph of porous silicon-nitride ceramic material after self-propagating reaction in the present embodiment.And certainly to spread rear microscopic appearance be column or bar-shaped beta phase silicon nitride.The brilliant length of described beta phase silicon nitride rod is about 7 ~ 20 μ m, and diameter is about 0.5 ~ 3 μ m, and average aspect ratio is about 5 ~ 10.
Embodiment 5:
Take ethanol as solvent, silicon nitride ball is ball-milling medium, with mass ratio 50:50:6 with silica flour, silicon nitride powder and Neodymium trioxide ball milling 24 hours in ball grinder.With the slurry 60 ℃ of dryings in baking oven that mix, then cross 100 mesh sieves.Powder after sieving is pressed into porous body with stainless steel mould 100MPa.Porous body is embedded in the buried powder of pure silicon powder, puts into the self-propagating reaction cavity, passes into nitrogen, and synthetic through ignition, the reaction times is 9 minutes, naturally cooling in synthetic rear stove; Learn after testing: the microscopic appearance of the porous silicon nitride ceramic that the present embodiment makes is column or bar-shaped beta phase silicon nitride; The brilliant length of described beta phase silicon nitride rod is about 2 ~ 10 μ m, and diameter is about 0.5 ~ 3 μ m, and average aspect ratio is about 3 ~ 5; Further test the porous silicon nitride ceramic of the present embodiment preparation, its void content is 23%, and bending strength is 410MPa.
Embodiment 6:
Take ethanol as solvent, silicon nitride ball is ball-milling medium, with mass ratio 70:30:6 with silica flour, silicon nitride powder and Erbium trioxide ball milling 24 hours in ball grinder.With the slurry 60 ℃ of dryings in baking oven that mix, then cross 200 mesh sieves.Powder after sieving is pressed into porous body with stainless steel mould 80MPa.Porous body is embedded in silica flour that mass ratio is 90:10, silicon nitride powder buried powder, puts into the self-propagating reaction cavity, passes into nitrogen, and synthetic through ignition, the reaction times is 8 minutes, synthetic after naturally cooling in stove; Learn after testing: the microscopic appearance of the porous silicon nitride ceramic that the present embodiment makes is column or bar-shaped beta phase silicon nitride; The brilliant length of described beta phase silicon nitride rod is about 2 ~ 10 μ m, and diameter is about 0.5 ~ 3 μ m, and average aspect ratio is about 3 ~ 5; Further test the porous silicon nitride ceramic of the present embodiment preparation, its void content is 31%, and bending strength is 350MPa.
Embodiment 7:
Take ethanol as solvent, silicon nitride ball is ball-milling medium, with mass ratio 50:50:6 with silica flour, silicon nitride powder and yttrium oxide ball milling 24 hours in ball grinder.With the slurry 60 ℃ of dryings in baking oven that mix, then cross 100 mesh sieves.Powder after sieving is pressed into porous body with stainless steel mould 5MPa.Porous body is embedded in the silicon of same proportioning/silicon nitride buried powder, puts into the self-propagating reaction cavity, passes into nitrogen, and synthetic through ignition, the reaction times is 3 minutes, synthetic after naturally cooling in stove;
Learn after testing: the microscopic appearance of the porous silicon nitride ceramic that the present embodiment makes is column or bar-shaped beta phase silicon nitride; The brilliant length of described beta phase silicon nitride rod is about 7 ~ 20 μ m, and diameter is about 0.5 ~ 3 μ m, and average aspect ratio is about 5 ~ 10; Further test the porous silicon nitride ceramic of the present embodiment preparation, its void content is 64%, and bending strength is 75MPa.
Claims (14)
1. porous silicon nitride ceramic goods, is characterized in that, in described porous silicon nitride ceramic goods, the form of silicon nitride is column or bar-shaped beta phase silicon nitride crystal habit; The goods total porosity is 20 ~ 65%, and bending strength is 450～50MPa.
2. porous silicon nitride ceramic goods according to claim 1, is characterized in that, described column or bar-shaped beta phase silicon nitride crystallization are β-Si
3N
4
3. porous silicon nitride ceramic goods according to claim 1, is characterized in that, the length of described beta phase silicon nitride crystallization is 7～20 μ m, and diameter is 0.5～3 μ m, and length-to-diameter ratio is 5～10:1.
According to claim 1 to 3 one of any described porous silicon nitride ceramic goods, it is characterized in that, described porous silicon nitride ceramic goods be by the silica flour that will have certain fineness, silicon nitride powder, with the mixture compression molding of sintering aid be the formed body with definite shape, then formed body is placed in that via nitride in the self-propagating reaction cavity is processed and the porous silicon nitride ceramic goods with definite shape that make, wherein said formed body be embedded in help lend some impetus in the buried powder that formed body carries out self-propagating reaction and in the self-propagating reaction cavity via nitride process.
According to claim 1 to 3 one of any described porous silicon nitride ceramic goods, it is characterized in that, in described formed body, the ratio of silica flour and silicon nitride powder is 9～5:1～5.
6. porous silicon nitride ceramic goods according to claim 5, is characterized in that, in described formed body, the ratio of silica flour and silicon nitride powder is 7～5:3～5.
7. porous silicon nitride ceramic goods according to claim 4, is characterized in that, described buried powder is the mixture of pure silicon powder or silica flour and silicon nitride powder.
8. porous silicon nitride ceramic goods according to claim 7, is characterized in that, in described buried powder the ratio of silica flour and silicon nitride powder have with described formed body in the silica flour ratio identical with silicon nitride powder.
9. porous silicon nitride ceramic goods according to claim 4, it is characterized in that, by it is mixed silica flour, silicon nitride powder and sintering aid ball milling in ball grinder and cross the 80-200 mesh sieve with the silica flour that obtains to have certain fineness, silicon nitride powder, with the mixture of sintering aid.
10. porous silicon nitride ceramic goods according to claim 4, is characterized in that, the particle diameter of described silica flour is that 1～50 μ m, purity are 80～99.99%.
11. porous silicon nitride ceramic goods according to claim 4 is characterized in that, described sintering aid is Y
2O
3, Yb
2O
3, Lu
2O
3, Nd
2O
3, Er
2O
3In one or more.
12. the preparation method of a porous silicon nitride ceramic is characterized in that comprising: will have certain fineness silica flour, silicon nitride powder, with the mixture compression molding of sintering aid be the formed body with definite shape; Formed body is embedded in to help lend some impetus in the buried powder that formed body carries out self-propagating reaction inserts together in the self-propagating reaction cavity, via nitride is processed and is made the porous silicon nitride ceramic goods with definite shape.
13. preparation method according to claim 12 is characterized in that, compression molding pressure is 5-100MPa.
14. according to claim 12 or 13 described preparation methods is characterized in that, the described nitriding treatment time is 1～10 minute.
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| CN109734456A (en) * | 2019-03-11 | 2019-05-10 | 中国科学院理化技术研究所 | A kind of preparation method of porous silicon nitride ceramic |
| CN111099919A (en) * | 2020-01-14 | 2020-05-05 | 中国人民解放军国防科技大学 | Silicon nitride ceramic with hierarchical pore structure and preparation method thereof |
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| CN112624769A (en) * | 2020-12-22 | 2021-04-09 | 中国科学院上海硅酸盐研究所 | Porous SiBCN/Si3N4Composite ceramic and preparation method thereof |
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| CN108707771A (en) * | 2018-05-08 | 2018-10-26 | 中国人民解放军国防科技大学 | Silicon nitride foamed ceramic reinforced aluminum-based composite material and preparation method and application thereof |
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| CN111196729A (en) * | 2020-01-09 | 2020-05-26 | 中国科学院上海硅酸盐研究所 | Method for preparing porous silicon nitride ceramic by using ultralow-content sintering aid |
| CN111196729B (en) * | 2020-01-09 | 2021-08-06 | 中国科学院上海硅酸盐研究所 | Method for preparing porous silicon nitride ceramic by using ultralow-content sintering aid |
| CN111099919A (en) * | 2020-01-14 | 2020-05-05 | 中国人民解放军国防科技大学 | Silicon nitride ceramic with hierarchical pore structure 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 |
| CN111423247A (en) * | 2020-03-31 | 2020-07-17 | 深圳麦克韦尔科技有限公司 | Porous ceramic, preparation method and heating element thereof |
| CN112624769A (en) * | 2020-12-22 | 2021-04-09 | 中国科学院上海硅酸盐研究所 | Porous SiBCN/Si3N4Composite ceramic and preparation method thereof |
| CN114225718A (en) * | 2021-12-24 | 2022-03-25 | 中国科学院上海硅酸盐研究所 | NaA molecular sieve membrane on surface of porous silicon nitride ceramic and preparation method thereof |
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