CN115108829A - Electrostatic spinning preparation method of ceramic nano composite fiber - Google Patents
Electrostatic spinning preparation method of ceramic nano composite fiber Download PDFInfo
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- 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
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
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Abstract
The invention relates to an electrostatic spinning preparation method of ceramic nano composite fibers, which belongs to the technical field of composite fibers and comprises the following steps: dispersing ceramic nano particles and a ceramic precursor in a mixed solvent to obtain a suspension; adding a high polymer spinning carrier into the obtained suspension to obtain electrostatic spinning slurry; and (3) carrying out electrostatic spinning on the obtained electrostatic spinning slurry, and sintering the ceramic nano particle/ceramic precursor/high polymer composite nano fiber to obtain the ceramic nano composite fiber. In the technical scheme of the invention, uniform fibers can be realized only by more than 4% of the components of the high polymer textile carrier, and the ceramic nano composite fibers with average diameter distribution, high length-diameter ratio and good flexibility are obtained by sintering the fibers prepared by 9% of the high polymer textile carrier and 2.5% of the ceramic nano particles at the temperature of 1400 ℃.
Description
Technical Field
The invention belongs to the technical field of composite fibers, and particularly relates to an electrostatic spinning preparation method of ceramic nano composite fibers.
Background
With the development of nanotechnology, electrospinning has received much attention since 1934 as a convenient, low-cost, and efficient method, because it can achieve uniform and continuous nanofibers. The method is widely applied to preparation of one-dimensional nanofibers and has wide application prospects in the medical fields of compound transmission, medical bandage materials, composite reinforcing materials, catalytic materials and the like.
Chinese patent publication No. CN101905974B discloses an electrostatic spinning preparation method of ceramic nanocomposite fibers, which is specifically implemented according to the following steps: step 1: weighing 3-10% of ceramic nanoparticles with the particle size of 10-300 nm, 3-20% of ceramic precursor, 5-30% of high polymer textile carrier and 40-89% of solvent according to volume percentage, wherein the total volume is 100%; step 2: adding the high polymer textile carrier into a solvent, heating in a water bath and magnetically stirring; and step 3: adding the ceramic precursor into the high polymer textile carrier solution obtained in the step 2, heating in a water bath, and magnetically stirring and aging; and 4, step 4: adding the ceramic nanoparticles into the spinnable solution of the ceramic precursor obtained in the step (3), keeping the temperature constant in a water bath, and performing ultrasonic dispersion and constant-temperature swelling to form a spinning solution; and 5: preparing the silk solution into composite nano fibers according to an electrostatic spinning technology; step 6: and sintering the composite nano-fiber to obtain the ceramic nano-composite fiber. Although the method has the advantages of wide raw material selection condition and wide selectable range, the range of 5-30% of the high polymer textile carrier is too wide, so that the viscosity of the electrostatic spinning slurry is difficult to control, and the fiber quality is reduced.
Disclosure of Invention
The invention aims to provide an electrostatic spinning preparation method of ceramic nano composite fibers, which can obtain electrostatic spinning slurry with sufficient viscosity by controlling the proportion of a high polymer spinning carrier, and prepare a high-quality composite fiber material.
The technical problems to be solved by the invention are as follows: in the prior art, the range of 5-30% of the high polymer spinning carrier is too wide, so that the viscosity of electrostatic spinning slurry is difficult to control, and the fiber quality is reduced.
The purpose of the invention can be realized by the following technical scheme:
an electrostatic spinning preparation method of ceramic nano composite fiber comprises the following steps:
s1, dispersing the ceramic nanoparticles and the ceramic precursor in a mixed solvent, uniformly mixing, adding a dispersing agent, stirring for 20-40min, standing for 2-4h, and filtering out dregs at the bottom to obtain a suspension;
s2, adding a high polymer spinning carrier into the obtained suspension, heating in a water bath, magnetically stirring, and aging for 2-12h to obtain electrostatic spinning slurry;
s3, carrying out electrostatic spinning on the obtained electrostatic spinning slurry, wherein the parameters are as follows: given at a flow rate of 1mL/Hr and providing a potential of 15kV, and maintaining the tip-to-collector distance at 10-15cm, ceramic nanoparticles/ceramic precursor/high polymer composite nanofibers were produced;
s4, placing the ceramic nano particle/ceramic precursor/high polymer composite nano fiber in a crucible, and sintering at the temperature of 500-1400 ℃ to obtain the ceramic nano composite fiber.
Further, the ceramic nanoparticles are two or more of zirconia, yttria, iron oxide, cobalt oxide, nickel oxide, alumina, manganese dioxide, tin dioxide, lead oxide, chromium oxide, and cadmium oxide.
Further, the ceramic precursor is one or more of nickel nitrate hexahydrate, butyl titanate, ethyl orthosilicate, zinc acetate and manganese chloride.
Further, the mixed solvent is deionized water and ethanol in a volume ratio of 4-6: 6.
Further, in step S2, the high polymer textile carrier is one or more of polyvinylpyrrolidone, polyvinyl alcohol and polyethylene oxide.
Further, in step S2, the temperature of the water bath is 60-70 ℃.
Furthermore, the grain diameter of the ceramic nano-particles is 40-50 nm.
Further, the ceramic nano composite fiber comprises the following raw materials in percentage by mass: 1-2.5% of ceramic nano particles, 3-7% of ceramic precursor, 5-9% of high polymer textile carrier and the balance of solvent.
The invention has the beneficial effects that:
in the technical scheme of the invention, the influence of viscosity determined by the contents of the high polymer textile carrier (5-9%) and the ceramic nano particles (1-2.5%) is disclosed, the content of the ceramic nano particles can increase the viscosity of the fiber and the diameter of the fiber, only more than 4% of the high polymer textile carrier can realize uniform fiber, and the fiber prepared by 9% of the high polymer textile carrier and 2.5% of the ceramic nano particles is sintered at 1400 ℃, so that the ceramic nano composite fiber with the advantages of average diameter distribution, high length-diameter ratio and good flexibility is obtained.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The using process of the dispersant is as follows: the fiber is first hydrophobically modified with hydrophobic modifier, then modified with surfactant, then loaded with anionic clay, and then mixed with the foam concrete.
Example 1
The ceramic nano composite fiber comprises the following raw materials in percentage by mass: 1% of ceramic nano particles, 3% of ceramic precursor, 5% of high polymer textile carrier and the balance of solvent.
An electrostatic spinning preparation method of ceramic nano composite fiber comprises the following steps:
s1, dispersing the ceramic nanoparticles and the ceramic precursor in a mixed solvent, uniformly mixing, adding a dispersing agent (polyethylene glycol 6000 with the mass fraction of 0.6%, wherein the added mass is 2 times of that of the ceramic nanoparticles), stirring for 20min, standing for 2h, and filtering out dregs at the bottom to obtain a suspension;
the ceramic nano particles are zirconia and yttria, and the particle size is 40 nm;
the ceramic precursor is nickel nitrate hexahydrate;
the mixed solvent is deionized water and ethanol with the volume ratio of 4: 6;
s2, adding a high polymer spinning carrier into the obtained suspension, heating in a water bath at 60 ℃, magnetically stirring, and aging for 2 hours to obtain electrostatic spinning slurry;
the high polymer textile carrier is polyvinylpyrrolidone.
S3, carrying out electrostatic spinning on the obtained electrostatic spinning slurry, wherein the parameters are as follows: given a flow rate of 1mL/Hr and providing a potential of 15kV, and maintaining the tip-to-collector distance at 10cm, ceramic nanoparticles/ceramic precursor/high polymer composite nanofibers were produced;
s4, placing the ceramic nano particle/ceramic precursor/high polymer composite nano fiber in a crucible, and sintering at 500 ℃ to obtain the ceramic nano composite fiber.
Example 2
The ceramic nano composite fiber comprises the following raw materials in percentage by mass: 1.5% of ceramic nano particles, 5% of ceramic precursor, 7% of high polymer textile carrier and the balance of solvent.
An electrostatic spinning preparation method of ceramic nano composite fibers comprises the following steps:
s1, dispersing the ceramic nanoparticles and the ceramic precursor in a mixed solvent, uniformly mixing, adding a dispersing agent (polyethylene glycol 6000 with the mass fraction of 0.6% and the added mass of the dispersing agent is 2 times that of the ceramic nanoparticles), stirring for 30min, standing for 3h, and filtering out dregs at the bottom to obtain a suspension;
the ceramic nano particles are zirconium oxide and nickel oxide, and the particle size is 45 nm;
the ceramic precursor is nickel nitrate hexahydrate or butyl titanate;
the mixed solvent is deionized water and ethanol with the volume ratio of 5: 6;
s2, adding a high polymer spinning carrier into the obtained suspension, heating in a water bath at 65 ℃, magnetically stirring, and aging for 6 hours to obtain electrostatic spinning slurry;
the high polymer textile carrier is polyvinylpyrrolidone and polyethylene oxide.
S3, carrying out electrostatic spinning on the obtained electrostatic spinning slurry, wherein the parameters are as follows: given a flow rate of 1mL/Hr and providing a potential of 15kV with the tip-to-collector distance maintained at 13cm, ceramic nanoparticles/ceramic precursor/high polymer composite nanofibers were made;
s4, placing the ceramic nano particle/ceramic precursor/high polymer composite nano fiber in a crucible, and sintering at 1200 ℃ to obtain the ceramic nano composite fiber.
Example 3
The ceramic nano composite fiber comprises the following raw materials in percentage by mass: 2.5% of ceramic nano particles, 7% of ceramic precursor, 9% of high polymer textile carrier and the balance of solvent.
An electrostatic spinning preparation method of ceramic nano composite fiber comprises the following steps:
s1, dispersing the ceramic nanoparticles and the ceramic precursor in a mixed solvent, uniformly mixing, adding a dispersing agent (0.6 mass percent of polyethylene glycol 6000, the added mass of which is 2 times that of the ceramic nanoparticles), stirring for 20-40min, standing for 2-4h, and filtering out dregs at the bottom to obtain a suspension;
the ceramic nano particles are nickel oxide and aluminum oxide, and the particle size is 50 nm;
the ceramic precursor is ethyl orthosilicate and zinc acetate;
the mixed solvent is deionized water and ethanol with the volume ratio of 6: 6;
s2, adding a high polymer spinning carrier into the obtained suspension, heating in a water bath at 70 ℃, magnetically stirring, and aging for 12 hours to obtain electrostatic spinning slurry;
the high polymer textile carrier is polyvinyl alcohol and polyethylene oxide.
S3, carrying out electrostatic spinning on the obtained electrostatic spinning slurry, wherein the parameters are as follows: given a flow rate of 1mL/Hr and providing a potential of 15kV with the tip-to-collector distance maintained at 15cm, ceramic nanoparticles/ceramic precursor/high polymer composite nanofibers were made;
s4, placing the ceramic nano particle/ceramic precursor/high polymer composite nano fiber in a crucible, and sintering at 1400 ℃ to obtain the ceramic nano composite fiber.
Comparative example
The comparative example differs from example 1 in that: the ceramic nano composite fiber comprises the following raw materials in percentage by mass: 1% of ceramic nano particles, 3% of ceramic precursor, 4% of high polymer textile carrier and the balance of solvent, and the rest steps and raw materials are synchronous to the embodiment 1.
The viscosities of the electrospinning pastes prepared in examples 1 to 3 and comparative example were now tested, and the test results are shown in table 1 below.
TABLE 1
| Item | Viscosity (mpa.s) |
| Example 1 | 104 |
| Example 2 | 490 |
| Example 3 | 683 |
| Comparative example | 79 |
The ceramic nanocomposite fibers prepared in examples 1 to 3 and comparative example were now tested, and the test results are shown in table 2 below.
TABLE 2
| Item | Diameter (nm) | Aspect ratio |
| Example 1 | 120-150 | ＞2000 |
| Example 2 | 150-200 | ＞5000 |
| Example 3 | 180-250 | ＞5000 |
| Comparative example | - | - |
"-" indicates failure to form a fiber
From the above table 1 and table 2, it can be seen that the diameter distribution of the synthesized fibers is uniform, the aspect ratio is high, and the flexibility is good by controlling the viscosity in the electrospinning slurry in the examples of the present invention within a suitable range, and it is revealed that the fibers cannot be formed when the high polymer spinning carrier is 4%.
In the description of the specification, reference to the description of "one embodiment," "an example," "a specific example" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. The electrostatic spinning preparation method of the ceramic nano composite fiber is characterized by comprising the following steps of:
s1, dispersing the ceramic nanoparticles and the ceramic precursor in a mixed solvent, uniformly mixing, adding a dispersing agent, stirring for 20-40min, standing for 2-4h, and filtering out dregs at the bottom to obtain a suspension;
s2, adding a high polymer spinning carrier into the obtained suspension, heating in a water bath, magnetically stirring, and aging for 2-12h to obtain electrostatic spinning slurry;
s3, carrying out electrostatic spinning on the obtained electrostatic spinning slurry, wherein the parameters are as follows: giving a flow rate of 1mL/Hr and providing a potential of 15kV, and keeping the distance from the tip to the collector at 10-15cm to prepare the ceramic nanoparticle/ceramic precursor/high polymer composite nanofiber;
s4, placing the ceramic nano particle/ceramic precursor/high polymer composite nano fiber in a crucible, and sintering at the temperature of 500-1400 ℃ to obtain the ceramic nano composite fiber.
2. The electrospinning preparation method of a ceramic nanocomposite fiber according to claim 1, wherein the ceramic nanoparticles are two or more of zirconia, yttria, iron oxide, cobalt oxide, nickel oxide, alumina, manganese dioxide, tin dioxide, lead oxide, chromium oxide, and cadmium oxide.
3. The electrospinning preparation method of a ceramic nanocomposite fiber according to claim 1, wherein the ceramic precursor is one or more of nickel nitrate hexahydrate, butyl titanate, ethyl orthosilicate, zinc acetate, and manganese chloride.
4. The method of claim 1, wherein the solvent mixture is deionized water and ethanol at a volume ratio of 4-6: 6.
5. The method of claim 1, wherein in step S2, the polymer carrier is one or more selected from polyvinylpyrrolidone, polyvinyl alcohol, and polyethylene oxide.
6. The electrospinning preparation method of ceramic nanocomposite fibers according to claim 1, wherein the temperature of the water bath in step S2 is 60-70 ℃.
7. The electrospinning preparation method of ceramic nanocomposite fibers according to claim 1, wherein the ceramic nanoparticles have a particle size of 40-50 nm.
8. The electrostatic spinning preparation method of the ceramic nanocomposite fiber according to claim 1, wherein the ceramic nanocomposite fiber comprises the following raw materials in percentage by mass: 1-2.5% of ceramic nano particles, 3-7% of ceramic precursor, 5-9% of high polymer textile carrier and the balance of solvent.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880917A (en) * | 2010-02-05 | 2010-11-10 | 西安理工大学 | Method for preparing nano ceramic fibers |
| CN101905974A (en) * | 2010-02-05 | 2010-12-08 | 西安理工大学 | Electrostatic spinning preparation method of ceramic nanometer composite fibers |
| CN102515716A (en) * | 2011-12-08 | 2012-06-27 | 东华大学 | Preparation method of NiO/gamma-Al2O3 composite ceramic nanofiber |
| CN107224883A (en) * | 2017-06-14 | 2017-10-03 | 江苏久朗高科技股份有限公司 | The technique that a kind of method of electrostatic spinning prepares ceramic separation film |
| CN110828870A (en) * | 2019-10-22 | 2020-02-21 | 山东东岳未来氢能材料有限公司 | Flexible ceramic fiber membrane reinforced perfluoro proton exchange membrane and preparation method thereof |
| US20210198815A1 (en) * | 2019-12-25 | 2021-07-01 | South University Of Science And Technology Of China | Sic/zrc composite fiber, preparation method and use thereof |
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2022
- 2022-07-15 CN CN202210831138.0A patent/CN115108829A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880917A (en) * | 2010-02-05 | 2010-11-10 | 西安理工大学 | Method for preparing nano ceramic fibers |
| CN101905974A (en) * | 2010-02-05 | 2010-12-08 | 西安理工大学 | Electrostatic spinning preparation method of ceramic nanometer composite fibers |
| CN102515716A (en) * | 2011-12-08 | 2012-06-27 | 东华大学 | Preparation method of NiO/gamma-Al2O3 composite ceramic nanofiber |
| CN107224883A (en) * | 2017-06-14 | 2017-10-03 | 江苏久朗高科技股份有限公司 | The technique that a kind of method of electrostatic spinning prepares ceramic separation film |
| CN110828870A (en) * | 2019-10-22 | 2020-02-21 | 山东东岳未来氢能材料有限公司 | Flexible ceramic fiber membrane reinforced perfluoro proton exchange membrane and preparation method thereof |
| US20210198815A1 (en) * | 2019-12-25 | 2021-07-01 | South University Of Science And Technology Of China | Sic/zrc composite fiber, preparation method and use thereof |
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