CN113149616A - Hollow ceramic micro-nanofiber, preparation method thereof and heat insulation material - Google Patents
Hollow ceramic micro-nanofiber, preparation method thereof and heat insulation material Download PDFInfo
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- CN113149616A CN113149616A CN202110149945.XA CN202110149945A CN113149616A CN 113149616 A CN113149616 A CN 113149616A CN 202110149945 A CN202110149945 A CN 202110149945A CN 113149616 A CN113149616 A CN 113149616A
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- hollow ceramic
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- 239000002243 precursor Substances 0.000 claims abstract description 43
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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
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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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
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Abstract
The invention discloses a hollow ceramic micro-nanofiber, a preparation method thereof and a heat insulation material, wherein the preparation method comprises the following steps: dissolving a high polymer material in a solvent to prepare a high polymer solution; then uniformly mixing the ceramic precursor with the polymer solution to prepare a spinning precursor solution; and spinning the spinning precursor solution by adopting a solution jet spinning technology to prepare composite fibers, and then calcining to prepare the hollow ceramic micro-nano fibers. The preparation method of the hollow ceramic micro-nano fiber is characterized in that the spinning precursor solution is subjected to solution jet spinning and then calcined to prepare the hollow ceramic micro-nano fiber, the production process and equipment are simple, the hollow ceramic micro-nano fiber is non-toxic and environment-friendly, high voltage is not required, the hollow ceramic micro-nano fiber is safe and reliable, the three-dimensional fiber cotton can be prepared, the production efficiency is high, and the prepared hollow ceramic micro-nano fiber is good in quality and has high temperature resistance and chemical stability.
Description
Technical Field
The invention relates to the technical field of ceramic fiber materials, in particular to a hollow ceramic micro-nanofiber, a preparation method thereof and a heat insulation material.
Background
The ceramic fiber has lower thermal conductivity and stable chemical and thermal properties, and the micro-nano ceramic fiber has small diameter; compared with solid fibers, the hollow ceramic fibers have smaller density and larger surface area, have wide application in the fields of chemical synthesis, environmental protection dye adsorption, aerospace, high-temperature air filtration, high-temperature industrial kilns, building heat preservation, fire-proof clothes, catalyst carriers and the like, and are materials with great development prospects. At present, the preparation of hollow ceramic fibers mainly comprises the following three methods: single tube electrospinning, multi-capillary electrospinning and template atomic layer deposition. The electrostatic spinning method is low in liquid outlet speed and production efficiency, is suitable for preparing a two-dimensional fiber membrane, is difficult to produce three-dimensional fiber cotton, needs long time, needs high voltage and has potential safety hazards; the method for multi-capillary electrostatic spinning has complex equipment and multiple processes, and because of the action of an electric field, fibers with good quality are difficult to obtain, and the preparation process is unstable; the template atomic deposition method has the disadvantages of complex process, low efficiency, poor continuity of the prepared fiber and small length-diameter ratio, and needs to adopt a separation extractant to remove the template after the preparation is finished, thereby increasing the cost and causing environmental pollution. Therefore, the application of the hollow ceramic fiber is greatly limited by the existing preparation method, and the development of a simple, stable and efficient preparation method of the hollow ceramic fiber is urgently needed
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a hollow ceramic micro-nanofiber, a preparation method thereof and a heat insulation material.
The invention provides a preparation method of hollow ceramic micro-nano fibers, which comprises the following steps:
s1, dissolving the high polymer material in a solvent to prepare a high polymer solution;
s2, uniformly mixing the ceramic precursor with the polymer solution to prepare a spinning precursor solution;
s3, spinning the spinning precursor solution by adopting a solution jet spinning technology to prepare composite fibers;
and S4, calcining the composite fiber to obtain the hollow ceramic micro-nano fiber.
The preparation method is to prepare the hollow ceramic micro-nanofiber, wherein the forming mechanism of the hollow structure is shown in figure 1, in the calcining process, a ceramic precursor on the surface of the fiber reacts with oxygen to generate an oxide, the inside of the fiber is difficult to oxidize due to lack of oxygen, the concentration gradient of the ceramic precursor and the oxide is formed from the surface to the inside of the fiber, ceramic precursor particles are diffused from inside to outside, oxide particles are diffused from outside to inside, the diffusion speed of the ceramic precursor particles is high, so that vacancy diffusion is caused, and the hollow ceramic micro-nanofiber is formed.
The preparation method of the hollow ceramic micro-nanofiber provided by the embodiment of the invention at least has the following beneficial effects: according to the preparation method, the hollow ceramic micro-nanofiber can be prepared by carrying out solution jet spinning on the spinning precursor solution and then calcining, the production equipment and the production process are simple, needle cannula and a plurality of capillaries are not needed, large-scale production can be realized, and the preparation method is non-toxic and environment-friendly. The method adopts a solution jet spinning technology for spinning, does not need high voltage, is safe and reliable, can prepare three-dimensional cellucotton, and has small dependence on a spinning precursor solution and high production efficiency; the hollow ceramic micro-nano fiber prepared by the method has small diameter, high length-diameter ratio, large surface area, high purity, good continuity and uniformity and low density (about 6mg cm)-3) The high-temperature-resistant and chemical-resistant composite material has good flexibility, high temperature resistance and chemical stability, and has wide application prospects in the fields of chemical synthesis, environment-friendly adsorption of dyes, aerospace, high-temperature air filtration, high-temperature industrial kilns, building heat preservation, fire-proof clothes, catalyst carriers and the like.
According to some embodiments of the invention, in step S2, the ceramic precursor comprises an alumina precursor, and the alumina precursor accounts for 10% to 100% of the total mass of the ceramic precursor.
According to some embodiments of the invention, the alumina precursor is selected from at least one of aluminum chloride hexahydrate, aluminum nitrate nonahydrate, aluminum sulfate, aluminum isopropoxide, aluminum acetylacetonate, aluminum acetate, aluminum n-butoxide, aluminum tri-sec-butoxide.
According to some embodiments of the invention, in step S2, the ceramic precursor further includes at least one of a hafnium oxide precursor, a zirconium oxide precursor, and a yttrium oxide precursor; preferably, the hafnium oxide precursor is selected from at least one of hafnium tetrachloride, hafnium sulfate, hafnium n-butoxide, hafnium ethoxide, hafnium hydroxide, hafnium oxychloride octahydrate, and hafnium oxynitrate; the zirconia precursor is selected from at least one of zirconium oxychloride octahydrate, zirconium acetate, zirconium n-propoxide, zirconium hydroxide and zirconium carbonate; the yttrium oxide precursor is at least one of yttrium phosphate, yttrium nitrate hexahydrate, yttrium chloride, yttrium sulfate octahydrate and yttrium isopropoxide.
According to some embodiments of the invention, in step S2, the polymer solution has a mass concentration of 2% to 30%; the mass ratio of the ceramic precursor to the polymer solution is 0.1: 1-10: 1.
In step S1, the polymer material is added to the solvent, and stirred and dissolved at 50-1000 rpm for 0.1-10 hours at room temperature (25 ℃) to 100 ℃ to obtain a polymer solution.
According to some embodiments of the invention, in step S1, the polymer material is selected from at least one of polyvinyl alcohol, polyacrylonitrile, polyvinyl chloride, polystyrene, polyethylene glycol, polyurethane, polyacrylic acid, polyvinyl pyrrolidone, cellulose acetate, methyl cellulose, carboxymethyl cellulose, polyvinylidene fluoride, polymethyl methacrylate, polyacrylamide, polyethylene oxide, polylactic acid, polyamide, polycaprolactone, polyvinyl butyral, polyaniline, polyimide, and polycarbonate.
According to some embodiments of the invention, in step S1, the solvent is selected from at least one of water, formic acid, tetrahydrofuran, acetone, acetylacetone, butanone, N-hexane, cyclohexane, N-heptane, acetonitrile, N-methylpyrrolidone, 1, 2-propanediol, chloroform, dichloromethane, 1, 2-dichloroethane, methanol, ethanol, isopropanol, 1-methoxy-2-propanol, tert-butanol, N-butanol, toluene, xylene, ethylenediamine, dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide, and carbon tetrachloride.
In step S3, the solution jet spinning technique is to draw a thin stream of solution with a high-speed airflow and solidify the solution into nanofibers along with evaporation of the solvent. The method specifically comprises the steps of spraying a spinning precursor solution from a spinning nozzle of a spinning die head on a jet spinning device by utilizing the solution jet spinning device through compressed air, and depositing fibers sprayed from the spinning nozzle on a receiver to obtain the composite fibers. Wherein, the receiver can adopt a metal net, a plastic net or a non-woven fabric with holes. The distance between the spinneret orifice and the receiver is generally 20-100 cm; the air flow velocity of the compressed air is generally 5 to 50 m/s.
According to some embodiments of the invention, in step S3, the jet speed of the spinning (i.e., the jet speed of the spinneret) is 0.5 to 15 mL/h.
According to some embodiments of the invention, the temperature of the calcination is 800 to 1600 ℃; preferably, the calcination is continuous temperature rise calcination or stepped temperature rise calcination; further preferably, the continuous heating calcination is to heat the mixture to 800-1600 ℃ at a speed of 0.1-10 ℃/min and keep the temperature for 0-24 h; the temperature is raised to 300-600 ℃ at the speed of 0.1-5 ℃/min for the step-type temperature raising calcination, the temperature is kept for 0-10 h, then the temperature is raised to 800-1600 ℃ at the speed of 1-10 ℃/min, and the temperature is kept for 0-10 h.
In a second aspect of the present invention, a hollow ceramic micro-nanofiber is provided, which is prepared by any one of the methods for preparing a hollow ceramic micro-nanofiber provided in the first aspect of the present invention. The average diameter of the hollow ceramic micro-nanofiber is 50-3500 nm.
In a third aspect of the present invention, a thermal insulation material is provided, wherein the raw material of the thermal insulation material comprises any one of the hollow ceramic micro-nanofibers provided by the second aspect of the present invention.
Drawings
The invention is further described with reference to the following figures and examples, in which:
FIG. 1 is a schematic diagram of a mechanism for forming a hollow structure of the hollow ceramic micro-nanofiber of the present invention;
FIG. 2 is a diagram of a hollow ceramic micro-nanofiber prepared in example 1 of the present invention;
FIG. 3 is an SEM image of a hollow ceramic micro-nanofiber prepared in example 1 of the present invention;
FIG. 4 is a flexible display diagram of a hollow ceramic micro-nanofiber prepared in example 1 of the present invention;
FIG. 5 is an SEM image of the hollow ceramic micro-nanofiber prepared in example 2 of the present invention;
FIG. 6 is an SEM image of a hollow ceramic micro-nanofiber prepared in example 3 of the present invention;
FIG. 7 is an SEM image of a hollow ceramic micro-nanofiber prepared in example 4 of the present invention;
fig. 8 is an SEM image of the hollow ceramic micro-nanofiber prepared in example 5 of the present invention.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Example 1
A specific preparation method of the hollow ceramic micro-nanofiber comprises the following steps:
s1, preparation of polymer solution: adding 1g of polyvinyl alcohol into 10g of deionized water, stirring and dissolving at 90 ℃ at the rotating speed of 800rpm for 1.5h to obtain a polyvinyl alcohol solution;
s2, preparing a spinning precursor solution: adding 6g of aluminum chloride hexahydrate into the polyvinyl alcohol solution prepared in the step S1, and uniformly stirring to obtain a spinning precursor solution;
s3, solution jet spinning: spraying the spinning precursor solution obtained in the step S2 from a spinning nozzle of a spinning die head at a speed of 5mL/h by adopting a solution jet spinning technology and using compressed air with a flow speed of 15m/S, and depositing the obtained fibers on a metal mesh receiver which is 40cm away from the spinning nozzle to obtain composite fibers;
s4, calcining: and (5) raising the temperature of the composite fiber obtained in the step (S3) from room temperature to 1000 ℃ at the speed of 5 ℃/min, preserving the temperature for 1h, and cooling to room temperature to obtain the hollow ceramic micro-nanofiber.
A real object diagram of the hollow ceramic micro-nanofiber prepared in this embodiment is shown in fig. 2, and specifically is the hollow ceramic micro-nanofiber carried on a flower in fig. 2. The obtained hollow ceramic micro-nanofibers were observed with a Scanning Electron Microscope (SEM), and the results are shown in fig. 3. The average diameter is 620nm, the diameter is small, the length-diameter ratio is high, the surface area is large, the continuity and the uniformity are good, the density is low, the flexibility is good, and the concrete flexibility display of the hollow ceramic nanofiber of the prepared product is shown in figure 4.
Example 2
A specific preparation method of the hollow ceramic micro-nanofiber comprises the following steps:
s1, preparation of polymer solution: adding 0.75g of polyvinyl alcohol into 10g of deionized water, and stirring and dissolving at 90 ℃ at the rotating speed of 800rpm for 1h to obtain a polyvinyl alcohol solution;
s2, preparing a spinning precursor solution: adding 19.5g of zirconium acetate and 14.4g of aluminum chloride hexahydrate into the polyvinyl alcohol solution prepared in the step S1, and uniformly stirring to obtain a spinning precursor solution;
s3, solution jet spinning: spraying the spinning precursor solution obtained in the step S2 from a spinning nozzle of a spinning die head at a speed of 5mL/h by adopting a solution jet spinning technology and using compressed air with a flow speed of 15m/S, and depositing the obtained fibers on a non-woven fabric which is 50cm away from the spinning nozzle to obtain composite fibers;
s4, calcining: and (4) raising the temperature of the composite fiber obtained in the step (S3) from room temperature to 1000 ℃ at the speed of 2 ℃/min, preserving the temperature for 1h, and cooling to room temperature to obtain the hollow ceramic micro-nanofiber.
The hollow ceramic micro-nanofiber prepared in example 2 was observed by a Scanning Electron Microscope (SEM), and the obtained result is shown in fig. 5. The average diameter of the composite material is 2496nm, the diameter is small, the length-diameter ratio is high, the surface area is large, the continuity and the uniformity are good, the density is low, and the flexibility is good.
Example 3
A specific preparation method of the hollow ceramic micro-nanofiber comprises the following steps:
s1, preparation of polymer solution: adding 1g of polyvinylpyrrolidone into 10g of deionized water, stirring and dissolving for 2 hours at the rotating speed of 800rpm under the condition of room temperature to obtain polyvinylpyrrolidone solution;
s2, preparing a spinning precursor solution: adding 6g of aluminum chloride hexahydrate and 0.5g of hafnium tetrachloride into the polyvinylpyrrolidone solution prepared in the step S1, and uniformly stirring to obtain a spinning precursor solution;
s3, solution jet spinning: spraying the spinning precursor solution obtained in the step S2 from a spinning nozzle of a spinning die head at a speed of 5mL/h by adopting a solution jet spinning technology and using compressed air with a flow speed of 15m/S, and depositing the obtained fibers on non-woven fabrics 40cm away from the spinning nozzle to obtain composite fibers;
s4, calcining: and (4) increasing the temperature of the composite fiber obtained in the step (S3) from room temperature to 600 ℃ at the speed of 0.5 ℃/min, preserving the heat for 1h, increasing the temperature to 1000 ℃ at the speed of 2 ℃/min, preserving the heat for 1h, and cooling to room temperature to obtain the hollow ceramic micro-nanofiber.
The hollow ceramic micro-nanofiber prepared in example 3 was observed by a Scanning Electron Microscope (SEM), and the obtained result is shown in fig. 6. The average diameter is 725nm, the diameter is small, the length-diameter ratio is high, the surface area is large, the continuity and the uniformity are good, the density is low, and the flexibility is good.
Example 4
A specific preparation method of the hollow ceramic micro-nanofiber comprises the following steps:
s1, preparation of polymer solution: adding 0.75g of polyvinyl alcohol into 10g of deionized water, and stirring and dissolving at 90 ℃ at the rotating speed of 800rpm for 1h to obtain a polyvinyl alcohol solution;
s2, preparing a spinning precursor solution: adding 6g of aluminum chloride hexahydrate, 1g of hafnium tetrachloride and 3g of zirconium acetate into the polyvinyl alcohol solution prepared in the step S1, and uniformly stirring to obtain a spinning precursor solution;
s3, solution jet spinning: spraying the spinning precursor solution obtained in the step S2 from a spinning nozzle of a spinning die head at a speed of 5mL/h by adopting a solution jet spinning technology and using compressed air with a flow speed of 15m/S, and depositing the obtained fibers on non-woven fabrics 40cm away from the spinning nozzle to obtain composite fibers;
s4, calcining: and (4) increasing the temperature of the composite fiber obtained in the step (S3) from room temperature to 1100 ℃ at the speed of 5 ℃/min, preserving the temperature for 1h, and cooling to room temperature to obtain the hollow ceramic micro-nanofiber.
The hollow ceramic micro-nanofiber prepared in example 4 was observed by a Scanning Electron Microscope (SEM), and the obtained result is shown in fig. 7. The average diameter of the material is 233nm, the diameter is small, the length-diameter ratio is high, the surface area is large, the continuity and the uniformity are good, the density is low, and the flexibility is good.
Example 5
A specific preparation method of the hollow ceramic micro-nanofiber comprises the following steps:
s1, preparation of polymer solution: adding 0.75g of polyvinylpyrrolidone into 10g of deionized water, stirring and dissolving for 1.5h at the rotating speed of 800rpm at room temperature to obtain polyvinylpyrrolidone solution;
s2, preparing a spinning precursor solution: adding 6g of aluminum chloride hexahydrate and 5.7g of yttrium nitrate hexahydrate into the polyvinylpyrrolidone solution prepared in the step S1, and uniformly stirring to obtain a spinning precursor solution;
s3, solution jet spinning: spraying the spinning precursor solution obtained in the step S2 from a spinning nozzle of a spinning die head at a speed of 5mL/h by using a solution jet spinning technology and compressed air with a flow speed of 20m/S, and depositing the obtained fibers on a non-woven fabric which is 30cm away from the spinning nozzle to obtain composite fibers;
s4, calcining: and (4) increasing the temperature of the composite fiber obtained in the step (S3) from room temperature to 600 ℃ at the speed of 0.5 ℃/min, preserving the heat for 1h, increasing the temperature to 1000 ℃ at the speed of 2 ℃/min, preserving the heat for 1h, and cooling to room temperature to obtain the hollow ceramic micro-nanofiber.
The hollow ceramic micro-nanofiber prepared in example 5 was observed by a Scanning Electron Microscope (SEM), and the obtained result is shown in fig. 8. The average diameter is 3110nm, the diameter is small, the length-diameter ratio is high, the surface area is large, the continuity and the uniformity are good, the density is low, and the flexibility is good.
From the above, the production process and production equipment of the hollow ceramic micro-nanofiber are simple, non-toxic and environment-friendly, high voltage is not required, safety and reliability are achieved, three-dimensional cellucotton can be prepared, production efficiency is high, the quality of the hollow ceramic micro-nanofiber product is good, high temperature resistance and chemical stability are achieved, and the hollow ceramic micro-nanofiber can be used for preparing heat insulation materials or applied to the fields of chemical synthesis, environment-friendly adsorption dyes, aerospace, high-temperature air filtration, fire-proof clothes, catalyst carriers and the like.
Claims (10)
1. A preparation method of hollow ceramic micro-nano fibers is characterized by comprising the following steps:
s1, dissolving the high polymer material in a solvent to prepare a high polymer solution;
s2, uniformly mixing the ceramic precursor with the polymer solution to prepare a spinning precursor solution;
s3, spinning the spinning precursor solution by adopting a solution jet spinning technology to prepare composite fibers;
and S4, calcining the composite fiber to obtain the hollow ceramic micro-nano fiber.
2. The method for preparing the hollow ceramic micro-nanofiber according to claim 1, wherein in step S2, the ceramic precursor contains an alumina precursor, and the alumina precursor accounts for 10-100% of the total mass of the ceramic precursor.
3. The preparation method of the hollow ceramic micro-nanofiber according to claim 2, wherein the alumina precursor is selected from at least one of aluminum chloride hexahydrate, aluminum nitrate nonahydrate, aluminum sulfate, aluminum isopropoxide, aluminum acetylacetonate, aluminum acetate, aluminum n-butoxide, and aluminum tri-sec-butoxide.
4. The method for preparing hollow ceramic micro-nanofibers according to claim 2, wherein in step S2, the ceramic precursor further comprises at least one of a hafnium oxide precursor, a zirconium oxide precursor, and a yttrium oxide precursor; preferably, the hafnium oxide precursor is selected from at least one of hafnium tetrachloride, hafnium sulfate, hafnium n-butoxide, hafnium ethoxide, hafnium hydroxide, hafnium oxychloride octahydrate, and hafnium oxynitrate; the zirconia precursor is selected from at least one of zirconium oxychloride octahydrate, zirconium acetate, zirconium n-propoxide, zirconium hydroxide and zirconium carbonate; the yttrium oxide precursor is at least one of yttrium phosphate, yttrium nitrate hexahydrate, yttrium chloride, yttrium sulfate octahydrate and yttrium isopropoxide.
5. The method for preparing the hollow ceramic micro-nanofiber according to claim 1, wherein in step S2, the mass concentration of the polymer solution is 2-30%; the mass ratio of the ceramic precursor to the polymer solution is 0.1: 1-10: 1.
6. The method of claim 5, wherein in step S1, the polymer material is at least one selected from polyvinyl alcohol, polyacrylonitrile, polyvinyl chloride, polystyrene, polyethylene glycol, polyurethane, polyacrylic acid, polyvinylpyrrolidone, cellulose acetate, methyl cellulose, carboxymethyl cellulose, polyvinylidene fluoride, polymethyl methacrylate, polyacrylamide, polyethylene oxide, polylactic acid, polyamide, polycaprolactone, polyvinyl butyral, polyaniline, polyimide, and polycarbonate.
7. The method of claim 5, wherein in step S1, the solvent is at least one selected from water, formic acid, tetrahydrofuran, acetone, acetylacetone, methyl ethyl ketone, N-hexane, cyclohexane, N-heptane, acetonitrile, N-methylpyrrolidone, 1, 2-propanediol, chloroform, dichloromethane, 1, 2-dichloroethane, methanol, ethanol, isopropanol, 1-methoxy-2-propanol, tert-butanol, N-butanol, toluene, xylene, ethylenediamine, dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and carbon tetrachloride.
8. The preparation method of the hollow ceramic micro-nanofiber according to any one of claims 1 to 7, wherein the calcining temperature is 800-1600 ℃; preferably, the calcination is a continuous temperature rise calcination or a stepwise temperature rise calcination.
9. A hollow ceramic micro-nanofiber, which is prepared by the preparation method of the hollow ceramic micro-nanofiber according to any one of claims 1 to 8.
10. A thermal insulation material, characterized by comprising the hollow ceramic micro-nanofibers according to claim 9.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113773093A (en) * | 2021-08-06 | 2021-12-10 | 华南理工大学 | Ceramic fiber membrane and preparation method and application thereof |
| CN114656288A (en) * | 2022-03-15 | 2022-06-24 | 中国科学院过程工程研究所 | MXene/ceramic fiber photothermal conversion composite material and preparation method and application thereof |
| CN114687008A (en) * | 2022-04-02 | 2022-07-01 | 深圳大学 | Superfine denier functional nanofiber and preparation method thereof |
| CN114804860A (en) * | 2022-02-23 | 2022-07-29 | 东华大学 | Hafnium oxide ceramic nanofiber and preparation method thereof |
| CN114836850A (en) * | 2022-05-17 | 2022-08-02 | 哈尔滨工业大学 | Hollow zirconia fiber and template-free preparation method thereof |
| CN115446954A (en) * | 2022-08-25 | 2022-12-09 | 安徽中材新材料科技有限公司 | Production method of composite molybdenum plate fluid hole cover plate brick |
| CN115991017A (en) * | 2022-11-28 | 2023-04-21 | 苏州大学 | Double-layer heat-sensitive fireproof flame-retardant nonwoven material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110424067A (en) * | 2019-07-08 | 2019-11-08 | 清华大学 | A kind of flexibility silicon dioxide fibre aerogel material and preparation method thereof |
| CN110846741A (en) * | 2019-10-09 | 2020-02-28 | 清华大学 | Flexible mullite fiber aerogel material and preparation method thereof |
| CN111646816A (en) * | 2020-05-11 | 2020-09-11 | 昆山柔维环境科技有限公司 | Zirconia-alumina composite fiber aerogel material and preparation method thereof |
-
2021
- 2021-02-03 CN CN202110149945.XA patent/CN113149616A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110424067A (en) * | 2019-07-08 | 2019-11-08 | 清华大学 | A kind of flexibility silicon dioxide fibre aerogel material and preparation method thereof |
| CN110846741A (en) * | 2019-10-09 | 2020-02-28 | 清华大学 | Flexible mullite fiber aerogel material and preparation method thereof |
| CN111646816A (en) * | 2020-05-11 | 2020-09-11 | 昆山柔维环境科技有限公司 | Zirconia-alumina composite fiber aerogel material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| VINÍCIUS D. SILVA等: "1D hollow MFe2O4 (M = Cu, Co, Ni) fibers by Solution Blow Spinning for oxygen evolution reaction", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
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|---|---|---|---|---|
| CN113773093A (en) * | 2021-08-06 | 2021-12-10 | 华南理工大学 | Ceramic fiber membrane and preparation method and application thereof |
| CN114804860A (en) * | 2022-02-23 | 2022-07-29 | 东华大学 | Hafnium oxide ceramic nanofiber and preparation method thereof |
| CN114656288A (en) * | 2022-03-15 | 2022-06-24 | 中国科学院过程工程研究所 | MXene/ceramic fiber photothermal conversion composite material and preparation method and application thereof |
| CN114687008A (en) * | 2022-04-02 | 2022-07-01 | 深圳大学 | Superfine denier functional nanofiber and preparation method thereof |
| CN114687008B (en) * | 2022-04-02 | 2023-05-23 | 深圳大学 | Superfine denier functional nanofiber and preparation method thereof |
| CN114836850A (en) * | 2022-05-17 | 2022-08-02 | 哈尔滨工业大学 | Hollow zirconia fiber and template-free preparation method thereof |
| CN114836850B (en) * | 2022-05-17 | 2023-08-04 | 哈尔滨工业大学 | Hollow zirconia fiber and template-free preparation method thereof |
| CN115446954A (en) * | 2022-08-25 | 2022-12-09 | 安徽中材新材料科技有限公司 | Production method of composite molybdenum plate fluid hole cover plate brick |
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