CN115262032A - Alumina flexible fiber and preparation method thereof - Google Patents
Alumina flexible fiber and preparation method thereof Download PDFInfo
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- CN115262032A CN115262032A CN202211005924.1A CN202211005924A CN115262032A CN 115262032 A CN115262032 A CN 115262032A CN 202211005924 A CN202211005924 A CN 202211005924A CN 115262032 A CN115262032 A CN 115262032A
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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 50
- 239000013305 flexible fiber Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 9
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 64
- 238000009987 spinning Methods 0.000 claims description 46
- 239000000835 fiber Substances 0.000 claims description 44
- 239000002243 precursor Substances 0.000 claims description 24
- 238000001354 calcination Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000012266 salt solution Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 230000009471 action Effects 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 229920006240 drawn fiber Polymers 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
- 239000004372 Polyvinyl alcohol Substances 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
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 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
- 239000007787 solid Substances 0.000 claims description 5
- 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
- 238000002156 mixing Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 2
- 238000009413 insulation Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000000919 ceramic 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
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 238000003837 high-temperature calcination Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution 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
- 238000004321 preservation Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000000349 field-emission scanning electron micrograph Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000071 blow moulding Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010041 electrostatic spinning 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
- 239000012784 inorganic fiber Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
Images
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
Abstract
The invention discloses an alumina flexible fiber and a preparation method thereof, and relates to the field of inorganic ceramic materials. The pure-phase alumina flexible fiber prepared by the invention has the characteristics of ultra-light weight and flexibility for the first time, solves the problem of large brittleness of alumina ceramics, has excellent heat insulation performance and good flexibility, and can be applied to aerospace heat insulation layers and heat insulation garments in the military field and high-temperature catalytic materials in the automobile industry field; the invention takes environment-friendly polymer and aluminum salt as raw materials, has no other catalysts or auxiliary salt additives, has simple production process, low raw material cost and no environmental pollution, and is easy for industrialized large-scale production.
Description
Technical Field
The invention relates to the field of inorganic ceramic materials, in particular to an aluminum oxide flexible fiber and a preparation method thereof.
Background
The inorganic ceramic fiber is a fibrous light material integrating excellent performances of heat insulation, fire resistance, high toughness and the like, and a high-end ceramic fiber product becomes a preferred heat insulation material of a high-speed aerospace craft heat protection system. However, few inorganic non-metal salt nanofibers have been reported due to the difficulty in preparation, and mainly include SiO 2 、ZrO 2 Mullite fiber, and the like. For example, the task group of the university of east china Ding Bin in 2014 uses silica and boroaluminosilicate as raw materials to prepare the flexible silica nanofiber aerogel by electrostatic spinning and freeze drying processes (Science Advances,2018,7 (1): 4 eaas8925. In 2017, wang et al prepared light high-elastic ZrO by blow molding spinning method 2 Nanofiber sponges (Science Advances,2017,3 (6): 1603170). For example, wu Hui, which is prepared in 2019, 10 and applied for a patent of "flexible mullite fiber aerogel material and a preparation method thereof" (patent application No. 201910954101.5), a mullite phase compounded by alumina and silica has certain acid resistance and can resist high temperature of 1500 ℃, but alumina is used as a secondary inorganic phase and silica is used as a main phase, and the alkali resistance and high temperature resistance of the fiber are greatly reduced due to the existence of silica. The patent of 'zirconia-alumina composite fiber aerogel material and a preparation method thereof' is applied again to the Wu Hui subject group in 5 months of 2020 (patent application No. 202010394349.3). The zirconia-alumina composite fiber material has excellent high temperature resistance, wherein alumina is used as a secondary inorganic phase, and zirconia is used as a main phase, and the cost of the fiber is greatly increased due to the existence of the zirconia. In theory, it is possible to use,the alumina fiber has the advantages of wide raw material source, low price, low specific heat capacity, good acid and alkali corrosion resistance and temperature and rapid change resistance, can be used in a high-temperature environment for a long time, has the maximum 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 have been no reports of pure phase alumina inorganic fibers, particularly ultra-light alumina fibers of hollow structure.
Therefore, the technical personnel in the field aim to overcome the difficulty that pure alumina is difficult to form fibers, and provide a preparation method of alumina flexible long fibers to solve the problem that the ceramic inorganic materials in the fields of aerospace, heat-insulating refractory materials, catalyst carriers and the like are limited in application due to high cost and poor corrosion resistance and high temperature resistance.
Disclosure of Invention
In view of the above defects of the prior art, the technical problem to be solved by the present invention is to overcome the difficulty that pure alumina is difficult to form into fibers.
In order to achieve the purpose, the invention provides an alumina flexible fiber which is a pure-phase alumina flexible fiber.
Further, the flexible alumina fiber is of a hollow or solid structure, is a long fiber and has a diameter of 100nm-10 um.
A preparation method of alumina flexible fibers 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, placing the solution on a magnetic stirrer, and stirring and mixing to prepare a spinning precursor solution;
step 4, adding the spinning precursor solution into an injector, extruding spinning liquid 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 liquid under the action of gas flow, and collecting the fibers in a collector, wherein the problems that a pure alumina fiber precursor is easy to hydrolyze and causes fiber adhesion and embrittlement are solved through the technical process;
and 5, calcining the fiber filaments in a muffle furnace at 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 and 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 calcining condition in the step 5 is that the temperature is raised to 180-400 ℃ at the speed of 1-20 ℃/min and is preserved for 1-8 hours, and then the temperature is raised to 600-1600 ℃ at the speed of 1-20 ℃/min and is preserved for 2-8 hours.
The invention has the following technical effects:
(1) The invention overcomes the problems that the precursor of the pure alumina fiber is very easy to hydrolyze and causes fiber adhesion and embrittlement through the design of the process, prepares the pure alumina flexible fiber for the first time, shows the characteristics of ultralight and flexibility, solves the problem of large brittleness of alumina ceramics, has excellent heat insulation and heat preservation performance and good flexibility, can be processed according to the actual production requirement, and can be applied to aerospace heat insulation and heat preservation layers and heat insulation and heat preservation clothes in the military field and high-temperature catalytic materials in the automobile industry field;
(2) The invention can make the inside of the fiber be a hollow structure by adjusting the process, and particularly the alumina fiber with the hollow structure has great advantages in the application of light heat-insulating materials and high-temperature catalytic materials;
(3) The invention takes environment-friendly polymer and aluminum salt as raw materials, has no other catalyst and auxiliary salt additive in the process of preparing the spinning precursor solution, has simple production process, low cost of the raw materials and no environmental pollution, and is easy for industrialized large-scale production.
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
Drawings
FIG. 1 is a flexible display of a hollow structure of pure alumina flexible fibers according to a preferred embodiment of the present invention;
FIG. 2 is a FESEM image of a solid structure pure alumina flex 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 a hollow structure according to a preferred embodiment of the present invention.
Detailed Description
The technical contents of the preferred embodiments of the present invention will be more clearly and easily understood by referring to the drawings attached to the specification. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
Example 1
(1) Preparing a spinning aid solution: at normal temperature, 0.75g of polyvinyl alcohol PVA (molecular weight 80000) is dissolved in 10mL of aqueous solution and is marked as solution A;
(2) Preparing a salt solution: 6g of aluminum chloride hexahydrate is dissolved in deionized water and is marked as a solution B;
(3) Preparing a spinning precursor solution: slowly adding the solution B into the solution A, and stirring for 3 days on a magnetic stirrer;
(4) The spinning process comprises the following steps: adding the spinning precursor solution obtained in the step (3) into a 10mL injector, extruding spinning solution at the speed of 0.02mL/min through a coaxial inner needle under the driving of a mechanical pump, introducing compressed air into a coaxial outer needle, forming drawn fibers 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 spun precursor fiber filaments;
(5) High-temperature calcination: and (4) 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 a speed of 20 ℃/min, the temperature is kept for 1 hour, then the temperature is raised to 1000 ℃ at a speed of 5 ℃/min, and the temperature is kept for 2 hours, so that the pure alumina flexible fiber with the solid structure is obtained.
As shown in figure 2, the fibers are uniformly distributed, the average length exceeds 200um, the diameter is about 2um, the middle part is of a solid structure, and the outer wall of the fiber is smooth and dense.
Example 2
(1) Preparing a spinning aid solution: at normal temperature, 1g of polyethylene oxide PEO (60, 0000) is dissolved in 10mL of aqueous solution and is marked as A solution;
(2) Preparing a salt solution: dissolving 8g of aluminum chloride hexahydrate in deionized water, and marking as a solution B;
(3) Preparing a spinning precursor solution: slowly adding the solution B into the solution A, and stirring for 3 days on a magnetic stirrer;
(4) The spinning process comprises the following steps: adding the spinning precursor solution obtained in the step (3) into a 10mL injector, extruding the spinning solution at the speed of 0.02mL/min through a coaxial inner needle under the driving of a mechanical pump, introducing air into a coaxial outer needle, forming a drawn 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 (4) 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 a speed of 20 ℃/min, the temperature is kept for 1 hour, then the temperature is raised to 1000 ℃ at a speed of 5 ℃/min, and the temperature is kept for 2 hours, so that the pure alumina flexible fiber with the hollow structure is obtained.
As shown in FIG. 1, the alumina fiber has a cotton-like appearance, excellent flexibility, and is freely foldable.
As shown in figure 3, the fibers are uniformly distributed, the average length exceeds 200um, the diameter is about 4.5um, the middle part of the fiber 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 diffraction peak position of the prepared hollow alumina fiber is completely consistent with that of the alumina standard card PDF #29-0063, and good crystallinity is shown.
Example 3
(1) Preparing a spinning aid solution: at normal temperature, 0.5g polyethylene oxide PEO (60, 0000) is dissolved in 10mL of aqueous solution, and is marked as A solution;
(2) Preparing a salt solution: dissolving 25g of aluminum chloride hexahydrate in deionized water, and marking as a solution B;
(3) Preparing a spinning precursor solution: slowly adding the solution B into the solution A, and stirring for 5 days on a magnetic stirrer;
(4) The spinning process comprises the following steps: adding the spinning precursor solution obtained in the step (3) into a 10mL injector, extruding the spinning solution at the speed of 0.01mL/min through a coaxial inner needle under the driving of a mechanical pump, introducing argon gas into a coaxial outer needle, forming a drawn fiber by the spinning solution under the action of airflow, adjusting the coaxial needle to be aligned with an inlet of a collector, and collecting the spun precursor fiber;
(5) High-temperature calcination: and (5) 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 a speed of 20 ℃/min, the temperature is kept for 8 hours, then the temperature is raised to 1600 ℃ at a speed of 1 ℃/min, and the temperature is kept for 2 hours, so that the pure alumina flexible fiber with the hollow structure is obtained.
Example 4
(1) Preparing a spinning aid solution: at normal temperature, 1g of polyethylene oxide PEO (60, 0000) was dissolved in 10mL of aqueous solution, and the solution was recorded as solution A;
(2) Preparing a salt solution: dissolving 1g of aluminum chloride hexahydrate in deionized water, and marking as a solution B;
(3) Preparing a spinning precursor solution: slowly adding the solution B into the solution A, and stirring for half an hour on a magnetic stirrer;
(4) The spinning process comprises the following steps: adding the spinning precursor solution obtained in the step (3) into a 10mL injector, extruding spinning solution at the speed of 0.02mL/min through a coaxial inner needle under the driving of a mechanical pump, introducing nitrogen into a coaxial outer needle, forming drawn fibers 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 spun precursor fibers;
(5) High-temperature calcination: and (4) 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 a speed of 1 ℃/min, the temperature is kept for 1 hour, then the temperature is raised to 600 ℃ at a speed of 1 ℃/min, and the temperature is kept for 8 hours, so that the pure alumina flexible fiber with the hollow structure is obtained.
Example 5
(1) Preparing a spinning aid solution: at normal temperature, 1g of polyvinylpyrrolidone PVP is dissolved in 10mL of water solution, and the solution is marked as A solution;
(2) Preparing a salt solution: dissolving 16g of aluminum nitrate in deionized water, and marking as a solution B;
(3) Preparing a spinning precursor solution: slowly adding the solution B into the solution A, and stirring for 10 days on a magnetic stirrer;
(4) The spinning process comprises the following steps: adding the spinning precursor solution obtained in the step (3) into a 10mL injector, extruding spinning solution at the speed of 0.02mL/min through a coaxial inner needle under the driving of a mechanical pump, introducing inert gas into a coaxial outer needle, forming drawn fibers by the spinning solution under the action of gas flow, adjusting the coaxial needle to be aligned with an inlet of a collector, and collecting spun precursor fibers;
(5) High-temperature calcination: and (4) 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 a speed of 20 ℃/min, the temperature is kept for 1 hour, then the temperature is raised to 1100 ℃ at a speed of 5 ℃/min, and the temperature is kept for 2 hours, so that the pure alumina flexible fiber with the hollow structure is obtained.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concept. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. The alumina flexible fiber is characterized in that the alumina flexible fiber is a pure-phase alumina flexible fiber.
2. The alumina flexible fiber according to claim 1, wherein the alumina flexible fiber is a hollow or solid structure, and the alumina flexible fiber is a long fiber with a diameter of 100nm-10 um.
3. A method of making the alumina flexible fiber of claim 1, comprising the steps of:
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 stirring and mixing the solution on a magnetic stirrer to prepare a spinning precursor solution;
step 4, adding the spinning precursor solution into an injector, extruding a spinning solution through a coaxial inner needle under the pushing of a mechanical pump, introducing gas through a coaxial outer needle, forming a drawn fiber by the spinning solution under the action of gas flow, and collecting the fiber in a collector;
and 5, calcining the fiber filaments in a muffle furnace at high temperature to obtain the pure-phase alumina flexible fiber.
4. The method for preparing the alumina flexible fiber according to claim 3, wherein the water-soluble polymer is one or more of polyethylene oxide (PEO), polyvinylpyrrolidone (PVP) and polyvinyl alcohol (PVA).
5. The method for preparing the alumina flexible fiber according to claim 3, wherein the water-soluble aluminum salt in the step 1 is one or more of aluminum chloride hexahydrate and aluminum nitrate.
6. The method of claim 3, wherein the mass of the water-soluble aluminum salt in the spinning precursor solution in the step 2 is 1 to 50 times the mass of the water-soluble polymer.
7. The method of preparing alumina flexible fibers according to claim 3 wherein the stirring time in step 3 is from half an hour to 10 days.
8. The method of claim 3, wherein the gas in step 4 is compressed air or an inert gas.
9. The method of claim 3, wherein the inert gas is one of nitrogen or argon.
10. The method for preparing the alumina flexible fiber according to claim 3, wherein the calcining condition in the step 5 is heating up to 180-400 ℃ at a rate of 1-20 ℃/min for 1-8 hours, and then heating up to 600-1600 ℃ at a rate of 1-20 ℃/min for 2-8 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115925319A (en) * | 2022-12-28 | 2023-04-07 | 安翼陶基复合材料(上海)有限公司 | Heat-absorbing fireproof coiled material containing hollow alumina fibers and manufacturing method thereof |
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