CN115262032B - Alumina flexible fiber and preparation method thereof - Google Patents
Alumina flexible fiber and preparation method thereof Download PDFInfo
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- CN115262032B CN115262032B CN202211005924.1A CN202211005924A CN115262032B CN 115262032 B CN115262032 B CN 115262032B CN 202211005924 A CN202211005924 A CN 202211005924A CN 115262032 B CN115262032 B CN 115262032B
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000013305 flexible fiber Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000009987 spinning Methods 0.000 claims abstract description 47
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 65
- 239000002243 precursor Substances 0.000 claims description 24
- 238000001354 calcination Methods 0.000 claims description 14
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 10
- 239000012266 salt solution Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 claims description 6
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 229920003169 water-soluble polymer Polymers 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 5
- 229920006240 drawn fiber Polymers 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 44
- 238000009413 insulation Methods 0.000 abstract description 8
- 238000003837 high-temperature calcination Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 239000000919 ceramic Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract 1
- 238000000071 blow moulding Methods 0.000 abstract 1
- 229920006158 high molecular weight polymer Polymers 0.000 abstract 1
- 229920000728 polyester Polymers 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000004964 aerogel Substances 0.000 description 3
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- 239000002121 nanofiber Substances 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000000349 field-emission scanning electron micrograph Methods 0.000 description 2
- 239000012784 inorganic fiber Substances 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses an alumina flexible fiber and a preparation method thereof, which relate to the field of inorganic ceramic materials, wherein the alumina flexible fiber is pure phase alumina flexible fiber, the high-molecular-weight polyester fiber is obtained by using a high-molecular-weight polymer and aluminum salt as raw materials and through a blow-molding spinning method and high-temperature calcination treatment. The invention prepares the pure-phase alumina flexible fiber for the first time, has the characteristics of ultra light and flexibility, solves the problem of high brittleness of alumina ceramics, has excellent heat insulation performance and good flexibility, and can be applied to aerospace heat insulation layers and heat insulation clothes in the field of military industry and high-temperature catalytic materials in the field of automobile industry; the invention uses green and environment-friendly polymer and aluminum salt as raw materials, has no other catalyst and auxiliary salt additive, has simple production process, low raw material cost and no environmental pollution, and is easy for industrialized mass production.
Description
Technical Field
The invention relates to the field of inorganic ceramic materials, in particular to an alumina flexible fiber and a preparation method thereof.
Background
The inorganic ceramic fiber is a fibrous light material integrating excellent properties such as heat insulation, fire resistance, high toughness and the like, and the high-end ceramic fiber product becomes a first-choice heat insulation material of a high-speed aerospace craft heat protection system. However, the inorganic nonmetallic salt nanofiber species are not a lot reported due to the difficulty in preparation, and mainly comprise SiO 2、ZrO2, mullite fibers and the like. For example, university of east China Ding Bin, 2014 teaches the preparation of flexible silica nanofiber aerogels (SCIENCE ADVANCES,2018,7 (1): 4: eaasa8925) using electrospinning and freeze-drying processes starting from silica and boroaluminosilicates. In 2017 Wang et al produced a lightweight high-elastic ZrO 2 nanofiber sponge by blow spinning (SCIENCE ADVANCES,2017,3 (6): 1603170). At present, there has been reports that silica, zirconia and the like and alumina are used for preparing composite inorganic fibers, for example, wu Hui subject group prepares and applies for a flexible mullite fiber aerogel material and a preparation method thereof in 2019, namely, a patent (patent application number 201910954101.5), wherein a mullite phase of the alumina and silica composite has certain acid resistance and can resist high temperature to 1500 ℃, but the alumina is used as a secondary inorganic phase, the silica is used as a main phase, and the alkali resistance and the high temperature resistance of the fibers are greatly reduced due to the existence of the silica. The group of the problem Wu Hui in 2020 applies again for a patent (patent application No. 202010394349.3) of "a zirconia-alumina composite fiber aerogel material and a method for producing the same". The zirconia-alumina composite fiber material has excellent high temperature resistance, wherein alumina is used as a secondary inorganic phase, zirconia is used as a main phase, and the existence of the zirconia greatly increases the cost of the fiber. In theory, the alumina fiber has wide sources and low price, has lower specific heat capacity, better acid-base corrosion resistance and Wen Jibian resistance, can be used in a high-temperature environment for a long time, has the highest use temperature of 1700-1800 ℃, and has extremely important application value in the fields of high-temperature thermal equipment, nuclear reactors, aerospace and the like. However, to date, there has been no report on pure phase alumina inorganic fibers, especially ultralight alumina fibers of hollow structure.
Therefore, the technical personnel in the art aim to overcome the difficulty that pure alumina is difficult to form fibers, and provide a preparation method of alumina flexible long fibers, so as to solve the problem that the application of ceramic inorganic materials in the fields of aerospace, heat insulation and heat preservation refractory materials, catalyst carriers and the like is limited due to the high cost, poor corrosion resistance and high temperature resistance.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention is to solve the technical problem of overcoming the difficulty of forming fiber by pure alumina.
In order to achieve the above object, the present invention provides an alumina flexible fiber, which is a pure phase alumina flexible fiber.
Further, the alumina flexible fiber is of a hollow or solid structure, the alumina flexible fiber is a long fiber, and the diameter is between 100nm and 10 um.
A method for preparing alumina flexible fiber, comprising the following steps:
Step 1, dissolving a water-soluble polymer in water to prepare a spinning aid solution;
Step 2, dissolving water-soluble aluminum salt in deionized water to prepare a salt solution;
Step 3, slowly adding the salt solution into the spinning aid solution, and placing the solution on a magnetic stirrer for stirring and mixing to prepare a spinning precursor solution;
Step 4, adding the spinning precursor solution into an injector, extruding the spinning solution through a coaxial inner needle under the pushing of a mechanical pump, introducing gas through a coaxial outer needle, forming drawn fibers by the spinning solution under the action of air flow, and collecting the fibers in a collector, wherein the problems that pure alumina fiber precursor is easy to hydrolyze and cause fiber adhesion embrittlement are overcome through the process;
And 5, calcining the fiber filaments in a muffle furnace at a high temperature to obtain the pure-phase alumina flexible fiber.
Further, the water-soluble polymer is one or more of polyethylene oxide PEO, polyvinylpyrrolidone PVP and polyvinyl alcohol PVA.
Further, the water-soluble aluminum salt in the step 1 is one or more of aluminum chloride hexahydrate or aluminum nitrate.
Further, the mass of the water-soluble aluminum salt in the spinning precursor solution in the step 2 is 1 to 50 times of the mass of the water-soluble polymer.
Further, the stirring time in the step 3 is half an hour to 10 days.
Further, the gas in step 4 is compressed air or inert gas.
Further, the inert gas is one of nitrogen or argon.
Further, the calcination condition in the step 5 is that after the temperature is raised to 180-400 ℃ at the speed of 1-20 ℃/min for 1-8 hours, the temperature is raised to 600-1600 ℃ at the speed of 1-20 ℃/min for 2-8 hours.
The invention has the following technical effects:
(1) The invention solves the problems of easy hydrolysis and fiber adhesion embrittlement of pure alumina fiber precursors through the design of the technological process, prepares the pure alumina flexible fiber for the first time, shows the characteristics of ultra-light and flexibility, solves the problem of large brittleness of alumina ceramics, and the prepared alumina flexible fiber not only has excellent heat insulation and heat preservation performance, but also has good flexibility, can be processed according to actual production requirements, and can be applied to aerospace heat insulation and preservation layers, heat insulation and heat preservation clothes in the field of military industry and high-temperature catalytic materials in the field of automobile industry;
(2) The invention can make the inside of the fiber be hollow structure by adjusting the process, and particularly the alumina fiber with hollow structure has great advantages in the application of light heat insulation material and high temperature catalytic material;
(3) The invention takes the green and environment-friendly polymer and aluminum salt as raw materials, has no other catalysts or other auxiliary salt additives in the preparation process of the spinning precursor liquid, has simple production process, low raw material cost and no environmental pollution, and is easy for industrialized mass production.
The conception, specific structure, and technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, features, and effects of the present invention.
Drawings
FIG. 1 is a flexible representation of a hollow structured pure alumina flexible fiber of a preferred embodiment of the present invention;
FIG. 2 is a FESEM image of a solid structured pure alumina flexible fiber of a preferred embodiment of the present invention;
FIG. 3 is a FESEM image of a hollow structured pure alumina flexible fiber of a preferred embodiment of the present invention;
fig. 4 is an XRD pattern of a pure alumina flexible fiber of hollow structure according to a preferred embodiment of the present invention.
Detailed Description
The following description of the preferred embodiments of the present invention refers to the accompanying drawings, which make the technical contents thereof more clear and easy to understand. The present invention may be embodied in many different forms of embodiments and the scope of the present invention is not limited to only the embodiments described herein.
Example 1
(1) Preparing a spinning aid solution: 0.75g of polyvinyl alcohol PVA (molecular weight 80000) was dissolved in 10mL of aqueous solution at ordinary temperature, designated as solution A;
(2) Salt solution preparation: 6g of aluminum chloride hexahydrate was dissolved in deionized water and noted as solution B;
(3) Preparing a spinning precursor solution: slowly adding the solution B into the solution A, and placing the solution A on a magnetic stirrer to stir for 3 days;
(4) Spinning: adding the spinning precursor solution obtained in the step (3) into a 10mL syringe, extruding the spinning solution at a speed of 0.02mL/min through a coaxial inner needle under the pushing of a mechanical pump, introducing compressed air into a coaxial outer needle, forming a wiredrawing fiber by the spinning solution under the action of air flow, adjusting the coaxial needle to be aligned with an inlet of a collector, and collecting the spun precursor fiber;
(5) High-temperature calcination: and (3) calcining the fiber filaments collected in the step (4) in a muffle furnace at a high temperature, wherein the calcining condition is that the temperature is raised to 200 ℃ at 20 ℃/min for 1 hour, and then the temperature is raised to 1000 ℃ at 5 ℃/min for 2 hours, so that the pure alumina flexible fiber with the solid structure is obtained.
As shown in FIG. 2, the fibers are uniformly distributed, the average length is more than 200um, the diameter is about 2um, the middle is of a solid structure, and the outer wall of the fiber is smooth and compact.
Example 2
(1) Preparing a spinning aid solution: 1g of polyethylene oxide PEO (60, 0000) was dissolved in 10mL of aqueous solution at room temperature, designated as solution A;
(2) Salt solution preparation: 8g of aluminum chloride hexahydrate was dissolved in deionized water and noted as solution B;
(3) Preparing a spinning precursor solution: slowly adding the solution B into the solution A, and placing the solution A on a magnetic stirrer to stir for 3 days;
(4) Spinning: adding the spinning precursor solution obtained in the step (3) into a 10mL syringe, extruding the spinning solution at a speed of 0.02mL/min through a coaxial inner needle under the pushing of a mechanical pump, introducing air into the coaxial outer needle, forming the spinning fiber by the spinning solution under the action of air flow, adjusting the coaxial needle to be aligned with an inlet of a collector, and collecting the spun precursor fiber;
(5) High-temperature calcination: and (3) calcining the fiber filaments collected in the step (4) in a muffle furnace at a high temperature, wherein the calcining condition is that the temperature is raised to 300 ℃ at 20 ℃/min for 1 hour, and then the temperature is raised to 1000 ℃ at 5 ℃/min for 2 hours, so that the pure alumina flexible fiber with the hollow structure is obtained.
As shown in FIG. 1, the alumina fiber looks like cotton, has excellent flexibility and can be folded at will.
As shown in figure 3, the fibers are uniformly distributed, the average length is more than 200um, the diameter is about 4.5um, the middle is of a hollow structure, the outer wall of the fiber is smooth and compact, and the inner wall of the fiber is porous and loose.
As shown in FIG. 4, the prepared hollow alumina fiber diffraction peak position is completely matched with the alumina standard card PDF#29-0063, and shows good crystallinity.
Example 3
(1) Preparing a spinning aid solution: 0.5g polyethylene oxide PEO (60, 0000) was dissolved in 10mL of aqueous solution at room temperature, designated as solution A;
(2) Salt solution preparation: 25g of aluminum chloride hexahydrate was dissolved in deionized water and designated as solution B;
(3) Preparing a spinning precursor solution: slowly adding the solution B into the solution A, and placing the solution A on a magnetic stirrer to stir for 5 days;
(4) Spinning: adding the spinning precursor solution obtained in the step (3) into a 10mL syringe, extruding the spinning solution at a speed of 0.01mL/min through a coaxial inner needle under the pushing of a mechanical pump, introducing argon into a coaxial outer needle, forming a fiber under the action of air flow, adjusting the coaxial needle to be aligned with an inlet of a collector, and collecting the spun precursor fiber;
(5) High-temperature calcination: and (3) calcining the fiber filaments collected in the step (4) in a muffle furnace at a high temperature, wherein the calcining condition is that the temperature is raised to 400 ℃ at 20 ℃/min, the heat is preserved for 8 hours, and then the temperature is raised to 1600 ℃ at 1 ℃/min, and the heat is preserved for 2 hours, so that the pure alumina flexible fiber with the hollow structure is obtained.
Example 4
(1) Preparing a spinning aid solution: 1g of polyethylene oxide PEO (60, 0000) was dissolved in 10mL of aqueous solution at room temperature, designated as solution A;
(2) Salt solution preparation: 1g of aluminum chloride hexahydrate was dissolved in deionized water and noted as solution B;
(3) Preparing a spinning precursor solution: slowly adding the solution B into the solution A, and placing the solution A on a magnetic stirrer to stir for half an hour;
(4) Spinning: adding the spinning precursor solution obtained in the step (3) into a 10mL syringe, extruding the spinning solution at a speed of 0.02mL/min through a coaxial inner needle under the pushing of a mechanical pump, introducing nitrogen into a coaxial outer needle, forming a fiber under the action of air flow, adjusting the coaxial needle to be aligned with an inlet of a collector, and collecting the spun precursor fiber;
(5) High-temperature calcination: and (3) calcining the fiber filaments collected in the step (4) in a muffle furnace at a high temperature, wherein the calcining condition is that the temperature is raised to 180 ℃ at 1 ℃/min for 1 hour, and then the temperature is raised to 600 ℃ at 1 ℃/min for 8 hours, so that the pure alumina flexible fiber with the hollow structure is obtained.
Example 5
(1) Preparing a spinning aid solution: 1g of polyvinylpyrrolidone PVP is dissolved in 10mL of aqueous solution at normal temperature and is marked as solution A;
(2) Salt solution preparation: 16g of aluminum nitrate was dissolved in deionized water and noted as solution B;
(3) Preparing a spinning precursor solution: slowly adding the solution B into the solution A, and placing the solution A on a magnetic stirrer to stir for 10 days;
(4) Spinning: adding the spinning precursor solution obtained in the step (3) into a 10mL syringe, extruding the spinning solution at a speed of 0.02mL/min through a coaxial inner needle under the pushing of a mechanical pump, introducing inert gas into the coaxial outer needle, forming the spinning fiber by the spinning solution under the action of air flow, adjusting the coaxial needle to be aligned with an inlet of a collector, and collecting the spun precursor fiber;
(5) High-temperature calcination: and (3) calcining the fiber filaments collected in the step (4) in a muffle furnace at a high temperature, wherein the calcining condition is that the temperature is raised to 300 ℃ at 20 ℃/min for 1 hour, and then the temperature is raised to 1100 ℃ at 5 ℃/min for 2 hours, so that the pure alumina flexible fiber with the hollow structure is obtained.
The foregoing describes in detail preferred embodiments of the present invention. It should be understood that numerous modifications and variations can be made in accordance with the concepts of the invention without requiring creative effort by one of ordinary skill in the art. Therefore, all technical solutions which can be obtained by logic analysis, reasoning or limited experiments based on the prior art by the person skilled in the art according to the inventive concept shall be within the scope of protection defined by the claims.
Claims (4)
1. The alumina flexible fiber is characterized in that the alumina flexible fiber is a pure-phase alumina flexible fiber, the alumina flexible fiber is of a hollow structure, and the preparation method of the alumina flexible fiber comprises the following steps:
Step 1, dissolving a water-soluble polymer in water to prepare a spinning aid solution;
Step 2, dissolving water-soluble aluminum salt in deionized water to prepare a salt solution;
Step 3, slowly adding the salt solution into the spinning aid solution, and placing the solution on a magnetic stirrer for stirring and mixing to prepare a spinning precursor solution;
The water-soluble polymer is polyethylene oxide PEO and polyvinylpyrrolidone PVP;
the water-soluble aluminum salt is one or more of aluminum chloride hexahydrate or aluminum nitrate;
The mass of the water-soluble aluminum salt in the spinning precursor solution is 1-50 times of that of the water-soluble polymer;
Step 4, adding the spinning precursor solution into an injector, extruding the spinning solution through a coaxial inner needle under the pushing of a mechanical pump, introducing gas through a coaxial outer needle, forming drawn fibers from the spinning solution under the action of air flow, and collecting the drawn fibers in a collector, wherein the gas is inert gas;
and 5, calcining the drawn fiber in a muffle furnace at a high temperature to obtain the pure-phase aluminum oxide flexible fiber, wherein the calcining condition is that the temperature is raised to 180-400 ℃ at a speed of 1-20 ℃/min, and then the temperature is raised to 600-1600 ℃ at a speed of 1-20 ℃/min and is kept for 2-8 hours.
2. The alumina flexible fiber of claim 1, wherein said alumina flexible fiber has a diameter between 100nm and 10 um.
3. The alumina flexible fiber of claim 1, wherein the agitation time in step 3 is from half an hour to 10 days.
4. The alumina flexible fiber of claim 1, wherein the inert gas of step4 is one of nitrogen or argon.
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| CN101185817A (en) * | 2007-12-12 | 2008-05-28 | 天津工业大学 | Method for preparing nano alumina fiber film material |
| CN110170282A (en) * | 2019-05-07 | 2019-08-27 | 清华大学 | A kind of anisotropy stratiform inorfil aerogel material and preparation method thereof |
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| CN102776603A (en) * | 2012-07-10 | 2012-11-14 | 东华大学 | Method for preparing porous hollow nano-alumina fiber by static spinning |
| CN106637446B (en) * | 2016-12-14 | 2019-05-31 | 清华大学 | Ceramic nanofibers and preparation method thereof and equipment |
| CN113149655B (en) * | 2021-04-01 | 2021-09-21 | 哈尔滨工业大学 | Method for preparing three-dimensional nanofiber ceramic aerogel through eddy current field assisted-electrostatic spinning |
| CN113151933A (en) * | 2021-05-21 | 2021-07-23 | 北京邮电大学 | Method for preparing alumina nano-fiber by utilizing electrostatic spinning |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101185817A (en) * | 2007-12-12 | 2008-05-28 | 天津工业大学 | Method for preparing nano alumina fiber film material |
| CN110170282A (en) * | 2019-05-07 | 2019-08-27 | 清华大学 | A kind of anisotropy stratiform inorfil aerogel material and preparation method thereof |
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