CN116752250A - Method for preparing flexible mullite nanofiber by electrostatic spinning - Google Patents
Method for preparing flexible mullite nanofiber by electrostatic spinning Download PDFInfo
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- CN116752250A CN116752250A CN202310906775.4A CN202310906775A CN116752250A CN 116752250 A CN116752250 A CN 116752250A CN 202310906775 A CN202310906775 A CN 202310906775A CN 116752250 A CN116752250 A CN 116752250A
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- mullite
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- nanofiber
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- 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 title claims abstract description 70
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 69
- 239000002121 nanofiber Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000010041 electrostatic spinning Methods 0.000 title claims abstract description 17
- 239000000835 fiber Substances 0.000 claims abstract description 37
- 239000002243 precursor Substances 0.000 claims abstract description 36
- 238000009987 spinning Methods 0.000 claims abstract description 28
- 238000001354 calcination Methods 0.000 claims abstract description 19
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 7
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 5
- 229920001296 polysiloxane Polymers 0.000 claims description 5
- 229920002545 silicone oil Polymers 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000004321 preservation Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- -1 aluminum carboxylate Chemical class 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000000578 dry spinning Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009704 powder extrusion Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000004580 weight loss Effects 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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Inorganic Fibers (AREA)
Abstract
A method for preparing flexible mullite nanofibers by electrostatic spinning. The method comprises the following steps: 1) Aluminum nitrate nonahydrate, ethyl orthosilicate and aluminum isopropoxide are used as raw materials, deionized water is used as a solvent, and oxalic acid is used as a catalyst to prepare a precursor solution. Polyethylene oxide and polyvinyl alcohol are dissolved in deionized water according to a certain proportion to be used as spinning auxiliary agents. 2) And preparing the mullite precursor nanofiber by adopting an electrostatic spinning method. 3) Drying the precursor nanofiber, calcining in a muffle furnace by adopting a stepped heating program, and cooling to room temperature. The flexible mullite fiber obtained by the method has the advantages of continuous and uniform fiber structure, good flexibility, low heat conductivity coefficient and high temperature resistance, and meets the requirements of heat preservation and heat insulation fields such as building heat preservation, aerospace, wearable protection systems and the like.
Description
Technical Field
The invention belongs to the technical field of heat preservation and heat insulation, and particularly provides a method for preparing flexible mullite nanofibers by electrostatic spinning.
Background
In the face of the constant consumption of energy and the increase in carbon emissions worldwide, there is an increasing need for materials with thermal insulation and fire resistance properties. Mullite (3 Al) 2 O 3 ·2SiO 2 ) Is a polycrystalline ceramic material with the use temperature as high as 1600 ℃, and has good thermal stability, dielectric property, chemical stability and creep resistance. The mullite fiber has the structural characteristics that the fiber can be inserted and staggered to form air holes, and still air is reserved, so that the heat insulation capability of the material is enhanced. However, the inherent brittleness of mullite fibers as ceramic materials limits their use and development. The existing methods for preparing mullite fibers such as a sol-gel method, a melting method and an ultrafine powder extrusion method can prepare mullite continuous fibers, but the methods have certain defects that the prepared fibers are mostly micron-sized fibers. The electrostatic spinning method can prepare nano mullite fiber, so that the nano mullite fiber has smaller pores and lower thermal conductivity.
CN110117841B discloses a method for preparing mullite nanofiber by electrospinning biphase precursor, wherein the raw materials used in the method are high in price, and the solvents used in the method contain toxicity of isopropyl alcohol and DMF, so that the method is not suitable for sustainable industrial production. CN113860862a discloses a preparation method of a mullite fiber with low cost, which comprises the steps of respectively preparing an aluminum carboxylate solution and a silicon additive, mixing the aluminum carboxylate solution with the silicon additive, reacting to obtain a precursor sol, concentrating, aging, spinning, heat treating and the like to obtain the mullite fiber. The method has the advantages of multiple manufacturing steps, long time consumption, high technical difficulty of the dry spinning method and relatively high production cost. In view of the above problems, it is necessary to develop a simple and economical method for preparing mullite fiber, and to overcome the brittleness of mullite fiber, so that the application range of mullite nanofiber in the field of high-temperature heat insulation is expanded.
Disclosure of Invention
Aiming at the phenomena, the invention provides the method for preparing the flexible mullite nanofiber by electrostatic spinning, which has the advantages of simple process, low-cost and easily available raw materials, safe and environment-friendly preparation process, and can improve the inherent brittleness of the mullite fiber and expand the application field of the mullite fiber.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
(1) And (3) preparing a spinning solution. With aluminum nitrate nonahydrate (AlNO) 3 ·9H 2 O), tetraethoxysilane (TEOS), aluminum Isopropoxide (AIP) as raw materials, deionized water (H) 2 O) as solvent, oxalic acid (C) 2 H 2 O 4 ) As a catalyst, a precursor solution was prepared. Polyethylene oxide (PEO) and polyvinyl alcohol (PVA) are dissolved in deionized water according to a certain proportionH 2 In O), stirring is carried out at 80 ℃ until the spinning auxiliary agent is in a clear and transparent state. And adding the dissolved spinning auxiliary agent into the precursor solution according to a certain proportion, and uniformly stirring to obtain a spinning solution.
(2) And preparing the mullite precursor nanofiber by adopting an electrostatic spinning technology. The spinning solution was first loaded into a 10ml medical syringe using an 18 gauge stainless steel spinning needle. The spinning needle head is connected with the positive pole of the high-voltage power supply, the receiving roller is connected with the negative pole of the high-voltage power supply, a high-voltage electrostatic field is formed between the positive pole and the negative pole, the spinning solution is stretched into filaments under the action of the electric field force after being ejected from the needle head, and then the mullite precursor fiber falls on the silicone paper wrapped on the receiving roller. Wherein, parameters of the electrostatic spinning process are as follows: the positive pressure is 16kV, the negative pressure is-8 kV, the propelling speed is 1.5ml/h, the receiving distance is 15cm, the ambient temperature is 20-30 ℃, the ambient humidity is 20-30%, and the rotating speed of the receiving roller is 150rpm.
(3) And (5) heat treatment of the mullite precursor nanofiber. The precursor nanofibers together with the silicone oil paper were dried in a 60 ℃ dry box for 24 hours. And separating the silicone paper from the precursor fiber after the drying is finished, and calcining the precursor nanofiber in a muffle furnace. The step heating program is adopted: heating at a heating rate of 1 ℃/min within a temperature range of 20-600 ℃; and heating at a heating rate of 2 ℃/min within the temperature range of 600-1300 ℃. The highest calcination temperatures were set at 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃, 1300 ℃, respectively. And (3) raising the temperature to the highest calcination temperature according to the temperature raising program, and preserving the heat for 1 hour to remove bound water and organic matters in the fiber. And cooling to room temperature after the calcination is finished, and obtaining the flexible mullite nanofiber calcined at different temperatures.
The invention provides a method for preparing flexible mullite nanofibers by electrostatic spinning. The diameter of the prepared flexible mullite nanofiber is 282-363 nm, and the structure is kept continuously and uniformly after calcination at 900-1300 ℃, so that the phenomena of fracture and pulverization are avoided.
The invention provides a method for preparing flexible mullite nanofibers by electrostatic spinning, which has the following advantages and outstanding effects:
(1) Aiming at the current situation of lack of materials in the field of high-temperature heat insulation, the invention provides a method for preparing flexible mullite nanofibers by utilizing an electrostatic spinning technology. The prepared fiber structure is continuous and uniform, has small pores, low heat conductivity and good flexibility, and has no phenomena of fragmentation, pulverization and the like. The mullite nanofiber can be used in the fields of building heat preservation and insulation, aerospace, wearable protection systems and the like, so that the application range of the mullite nanofiber is expanded.
(2) The invention provides a method for preparing flexible mullite nanofibers by electrostatic spinning, wherein the addition amount of a spinning auxiliary agent is small, the phenomenon of fiber weight loss after calcination can be effectively improved, the fiber structure and spinning performance are further improved, and mullite nanofibers with excellent morphology and performance are obtained.
(3) The invention provides a method for preparing flexible mullite nanofibers by electrostatic spinning, which has the advantages of raw material mixing uniformity, safety, energy consumption, operation difficulty and the like, wherein the raw materials are cheap and easily available, the process is simple and economical, and water is used as a solvent, so that the method is safe and environment-friendly.
Description of the drawings:
in order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is an SEM image of a mullite precursor nanofiber of a flexible mullite nanofiber after calcination at different temperatures (a) mullite precursor nanofiber; (b) 900 ℃; (c) 1000 ℃; (d) 1100 ℃; (e) 1200 ℃; (f) 1300 ℃.
FIG. 2 is average diameter statistics of mullite precursor nanofibers and flexible mullite nanofibers after calcination at different temperatures (a) mullite precursor nanofibers; (b) 900 ℃; (c) 1000 ℃; (d) 1100 ℃; (e) 1200 ℃; (f) 1300 ℃.
FIG. 3 is an XRD pattern of mullite precursor nanofibers and flexible mullite nanofibers after calcination at different temperatures
FIG. 4 is an SEM image of a 1200℃calcined flexible mullite nanofiber in a bent state
FIG. 5 is a photograph of 1200℃calcined flexible mullite nanofibers in a bent state
Detailed Description
Example 1:
(1) And (3) preparing a spinning solution. Into a 50ml round bottom flask was charged 10g deionized water and 3.2g aluminum nitrate nonahydrate (AlNO) was added with stirring at 35 ℃ 3 ·9H 2 O) after it has been completely dissolved, 1.8g of tetraethyl orthosilicate (TEOS) and after 1min 3.6g of Aluminum Isopropoxide (AIP) and 0.1g of oxalic acid (C) 2 H 2 O 4 ) Stirring at 300rpm for 18h gave a clear and transparent precursor solution. Polyethylene oxide (PEO) and polyvinyl alcohol (PVA) are mixed according to the mass ratio of 2:3 are dissolved in deionized water, stirred for 24 hours at 80 ℃ until the solution is completely dissolved, and the solution is in a clear and transparent state and is used as a spinning auxiliary agent. 1.9g of the dissolved spinning auxiliary agent is added into 5g of the precursor solution, and the mixture is stirred for 19h to obtain a uniform and transparent spinning solution.
(2) And preparing the mullite precursor nanofiber by adopting an electrostatic spinning technology. The spinning solution obtained in the step (1) is sucked into a 10ml medical injector, and an 18-gauge stainless steel spinning needle is adopted. The spinning needle head is connected with the positive electrode of the high-voltage power supply, and the receiving roller is connected with the negative electrode of the high-voltage power supply. And wrapping the silicone paper on a receiving roller to be used as a receiving device of the mullite precursor fiber. The following parameters were set: the push injection speed is 1.5ml/h, the spinning positive pressure is 16kV, the negative pressure is 8kV, the receiving distance is 15cm, the rotating speed of the receiving roller is 150rpm, the spinning environment temperature is 20-30 ℃, and the air humidity is 20-30%.
(3) And (5) heat treatment of the mullite precursor nanofiber. And (3) putting the precursor nanofiber collected in the step (2) and silicone oil paper into a drying oven at 60 ℃ for drying for 24 hours, and separating the silicone oil paper from the precursor nanofiber. Calcining the dried precursor nanofiber in a muffle furnace, and adopting a step-type heating program: heating at a heating rate of 1 ℃/min within a temperature range of 20-600 ℃; and heating at a heating rate of 2 ℃/min within the temperature range of 600-1300 ℃. The highest calcination temperatures were set at 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃, 1300 ℃, respectively. And (3) raising the temperature to the highest calcination temperature according to the temperature raising program, and preserving the heat for 1 hour to remove bound water and organic matters in the fiber. And cooling to room temperature after the calcination is finished, and finally obtaining the stable flexible mullite nanofiber. The room temperature thermal conductivity of the obtained flexible mullite nanofiber material product is 0.035W/(m.K). And storing the obtained flexible mullite fibers calcined at different temperatures in a sealing bag.
SEM test is carried out on the mullite precursor nanofiber prepared in the embodiment 1 and the flexible mullite nanofiber calcined at different temperatures, and the result is shown in figure 1, wherein the fiber structure is continuous and uniform, the fiber surface is smooth, the fiber diameter is uniform, and the phenomena of fracture and pulverization are avoided.
The average diameter statistics of the mullite precursor nanofiber prepared in the example 1 and the flexible mullite nanofiber calcined at different temperatures are shown in fig. 2. The diameter of the prepared flexible mullite nanofiber is 282-363 nm, the average diameter of the fiber is gradually reduced along with the increase of the calcination temperature, the fiber is mainly caused by pyrolysis of organic matters and densification of mullite, and the fiber diameter is increased when the temperature reaches 1300 ℃, and the fiber diameter is related to the generation and growth of mullite grains.
The XRD patterns of the mullite precursor nanofiber prepared in the above example 1 and the fiber films calcined at different temperatures are shown in FIG. 3. At 1000 ℃, a characteristic peak of mullite (ICDD#15-0776) is detected, which indicates that the mullite nanofiber starts to crystallize at about 1000 ℃ to 1300 ℃, and the characteristic peak of mullite is more obvious and sharp.
SEM images of the 1200 ℃ calcined flexible mullite nanofibers prepared in example 1 in a bent state are shown in fig. 4. A photograph of the 1200 ℃ calcined flexible mullite nanofiber prepared in example 1 in a bent state is shown in fig. 5. It can be seen that the sample remained a continuous fibrous structure in the bent state, with good flexibility.
The invention is not a matter of the known technology.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (1)
1. The method for preparing the flexible mullite nanofiber by electrostatic spinning is characterized by comprising the following specific steps of:
(1) Preparing a spinning solution: into a 50ml round bottom flask was charged 10g deionized water and 3.2g aluminum nitrate nonahydrate (AlNO) was added with stirring at 35 ℃ 3 ·9H 2 O) after it has been completely dissolved, 1.8g of tetraethyl orthosilicate (TEOS) and after 1min 3.6g of Aluminum Isopropoxide (AIP) and 0.1g of oxalic acid (C) 2 H 2 O 4 ) Stirring at 300rpm for 18h gave a clear and transparent precursor solution. Polyethylene oxide (PEO) and polyvinyl alcohol (PVA) are mixed according to the mass ratio of 2:3 are dissolved in deionized water, stirred for 24 hours at 80 ℃ until the solution is completely dissolved, and the solution is in a clear and transparent state and is used as a spinning auxiliary agent; adding 1.9g of dissolved spinning auxiliary agent into 5g of precursor solution, and stirring for 19h to obtain uniform and transparent spinning solution;
(2) Preparing mullite precursor nanofiber by adopting an electrostatic spinning technology: sucking the spinning solution obtained in the step (1) into a medical injector of 10m1, and adopting an 18-gauge stainless steel spinning needle, wherein the spinning needle is connected with the positive electrode of a high-voltage power supply, and a receiving roller is connected with the negative electrode of the high-voltage power supply; wrapping the silicone paper on a receiving roller to be used as a receiving device of mullite precursor fibers: the following parameters were set: the positive pressure is 16kV, the negative pressure is-8 kV, the propelling speed is 1.5ml/h, the receiving distance is 15cm, the ambient temperature is 20-30 ℃, the ambient humidity is 20-30%, and the rotating speed of the receiving roller is 150rpm:
(3) Heat treatment of mullite precursor nanofibers: putting the precursor nanofiber obtained in the step (2) and silicone oil paper into a drying oven at 60 ℃ for drying for 24 hours; the dried precursor fiber is torn off from the silicone paper, is put into a muffle furnace for calcination, and adopts a step heating program: heating at a heating rate of 1 ℃/min within a temperature range of 20-600 ℃; heating at a heating rate of 2 ℃/min within the temperature range of 600-1300 ℃; setting the highest calcination temperature at 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃ and 1300 ℃ respectively; raising the temperature to the highest calcination temperature according to the heating program, and preserving the heat for 1 hour to remove bound water and organic matters in the fiber; and cooling to room temperature after the calcination is finished, and obtaining the stable flexible mullite nanofiber calcined at different temperatures.
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| CN202310906775.4A CN116752250A (en) | 2023-07-21 | 2023-07-21 | Method for preparing flexible mullite nanofiber by electrostatic spinning |
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