CN109576820A - A kind of preparation method of high-strength and high-toughness zirconium oxide nanofiber - Google Patents
A kind of preparation method of high-strength and high-toughness zirconium oxide nanofiber Download PDFInfo
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- CN109576820A CN109576820A CN201811542123.2A CN201811542123A CN109576820A CN 109576820 A CN109576820 A CN 109576820A CN 201811542123 A CN201811542123 A CN 201811542123A CN 109576820 A CN109576820 A CN 109576820A
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- zirconium oxide
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- 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
Abstract
The invention belongs to high-strength light technical field of nanometer material preparation, are related to a kind of preparation method of high-strength and high-toughness zirconium oxide nano-fiber material.This method utilizes ultrasonic wave added liquid phase reactor method, uses zirconium oxychloride octahydrate and polyvinylpyrrolidone etc. for raw material, controllable preparation high-strength and high-toughness zirconium oxide nano-fiber material.Specific method is that (1) prepares alcohol-water solution at room temperature, and suitable polyvinylpyrrolidone and zirconium oxychloride octahydrate is added, is stirred until homogeneous dispersion；(2) by mixed solution ultrasound 30min, then 20-60 DEG C of constant temperature, continues to react 2-6 hours under stirring condition, Temperature fall and centrifuge washing, freeze-drying obtain powdery product；(3) powdery product is placed in Muffle furnace, under air atmosphere, 100-700 DEG C of calcining 2h finally obtains high-strength and high-toughness zirconium oxide nano-fiber material.
Description
Technical field
The invention belongs to high-strength light technical field of nanometer material preparation, are related to a kind of high-strength and high-toughness zirconium oxide nanofiber
Preparation method.
Background technique
With the fast development of aerospace field, the requirement for novel aerospace material is higher and higher.It is controllable
Standby high-strength light, high-ductility, heat-resisting material establish the theory of related Controllable assembly, realize that magnanimity preparation process becomes aviation
The key technology of space material.The material for meeting novel spacecraft demand is prepared, to break through related international block and art wall
It builds, meets the great demand of national defense construction and national economy.
Currently, the emphasis of aerospace material research is mainly reflected in metal material, high molecular material and inorganic non-metallic
Material Field.Inorganic non-metallic material has many excellent performances, such as high temperature resistant, high rigidity, anticorrosive and excellent Jie
Electricity, piezoelectricity, optics, electromagnetic performance and its power and energy characteristic etc..Inorganic non-metallic material has become various structures, information and function
The main source of energy material, such as zirconia ceramics fiber.Zirconium oxide fibre is a kind of ceramic fibre of function admirable, in resistance to height
The fields such as warm heat-barrier material, structural reinforcement material and chemical resistant material have a wide range of applications.However, as ceramic material
Material Zirconium oxide fibre is fragile material, and tensile strength is not high, strongly limits it in the application in the fields such as aerospace.
Nano material is with its unique small-size effect, the features such as almost without defect and dislocation, is promoted in the strength of materials
Aspect has unique advantage, therefore becomes investigation of materials field pole by the Zirconium oxide fibre that nanosizing prepares high-strength and high ductility
Big challenge.
Summary of the invention
It is an object of the invention to be directed to the deficiency of existing technology of preparing, using ultrasonic wave added liquid phase reactor method, using eight
Water basic zirconium chloride and polyvinylpyrrolidone etc. are raw material, provide a kind of easy to operate, and controllable preparation high-strength and high-toughness zirconium oxide is received
The preparation method of rice fibrous material.It includes the following steps:
The first step prepares alcohol-water solution (water: ethyl alcohol=1:59-5:55) at room temperature, stirs 10-30min, obtains 60-
600mL uniformly mixed colourless transparent solution；
Second step takes solution obtained in the 6-60mL first step, 0.5-10g polyvinylpyrrolidone is added, at room temperature
10min is stirred, uniform colorless clear solution is obtained；
Third step takes 10-100mg zirconium oxychloride octahydrate that the colourless transparent solution that second step obtains, ultrasonic disperse is added
30min obtains white suspension solution；
20-60 DEG C of constant temperature of white suspension solution obtained in third step is persistently stirred 2-6h by the 4th step, is dropped to solution
For room temperature, centrifuge washing obtains white gels shape precipitating；
The precipitating of white gels shape obtained in 4th step is transferred in freeze drier by the 5th step, and dry 24-48h is obtained
To white powder；
Dry white powder obtained in 5th step is transferred in Muffle furnace by the 6th step, under air environment, 100-700
DEG C calcining 2-4h, obtain high-strength and high-toughness zirconium oxide nano-fiber material.
In the present invention, if be not particularly described, used solution is all prepared under normal conditions, such as
At room temperature substance is dissolved in and to be prepared in alcohol-water solution.
In the present invention, if be not particularly described, used device, instrument, equipment, material, technique, method,
Step, preparation condition etc. are all that this field routinely uses or those of ordinary skill in the art routinely use according to this field
What technology can be readily available.
In the present invention, available surfactant is polyvinylpyrrolidone, and available zirconium source is zirconium oxychloride octahydrate,
But it is not only limited to this.
In the present invention, its ratio be water for available alcohol-water solution: ethyl alcohol=1:59-5:55, but is not only limited to this.
In the present invention, available ultrasound assisting dispersion technology, but it is not only limited to this.
Relative to the preparation of existing Zirconium oxide fibre material, the present invention has the advantage that
1, the raw material used in preparation process of the present invention is simple and easy to get, and cost is relatively low, and there are no pollution to the environment, technique letter
It is single, it is easy to operate；
2, the fibrous material that the present invention is prepared has the characteristics that nanoscale；
3, amorphous zirconia nanofiber, crystalline state zirconia nanopowder fiber and nanocrystalline and amorphous may be implemented in the present invention
The preparation of the nanocrystalline enhancing amorphous zirconia nanofiber of ratio controllable adjustment.
Detailed description of the invention
Fig. 1 is liquid phase reactor schematic diagram of the present invention；
Fig. 2 is that nanocrystalline enhancing amorphous zirconia nanofiber, the amorphous zirconia that 1-3 of the embodiment of the present invention is obtained are received
The Mechanical test results of rice fiber and crystalline state zirconia nanopowder fiber；
Fig. 3 is that the nanocrystalline enhancing amorphous zirconia nanofiber transmission electron microscope that the embodiment of the present invention 1 obtains is low
Times and high power photo and selective electron diffraction photo；
Fig. 4 is the amorphous zirconia nanofiber transmission electron microscope low power and high power that the embodiment of the present invention 2 obtains
Photo and selective electron diffraction photo；
Fig. 5 is that the crystalline state zirconia nanopowder fiber transmission electron microscope low power that the embodiment of the present invention 3 obtains and high power are shone
Piece and selective electron diffraction photo.
Specific embodiment
Illustrate the preparation method of high-strength and high-toughness zirconium oxide nano-fiber material with reference to the accompanying drawings and examples.But
It should be appreciated that these embodiments are only intended to illustrate the present invention, and and it is not in any way limit the scope of the present invention.
Embodiment 1
The preparation method of nanocrystalline enhancing amorphous zirconia nanofiber
The first step prepares alcohol-water solution (water: ethyl alcohol=1:59) at room temperature, stirs 10-30min, and it is mixed to obtain 60-600mL
Close uniform colourless transparent solution；
Second step takes solution obtained in the 6-60mL first step, and 0.7g polyvinylpyrrolidone is added, is stirred at room temperature
10min obtains uniform colorless clear solution；
Third step takes 10-100mg zirconium oxychloride octahydrate that the colourless transparent solution that second step obtains, ultrasonic disperse is added
30min obtains white suspension solution；
30 DEG C of white suspension solution constant temperature obtained in third step is persistently stirred 2-6h, is reduced to room to solution by the 4th step
Temperature, centrifuge washing obtain white gels shape precipitating；
The precipitating of white gels shape obtained in 4th step is transferred in freeze drier by the 5th step, and dry 24-48h is obtained
To white powder；
Dry white powder obtained in 5th step is transferred in Muffle furnace by the 6th step, and under air environment, 400 DEG C are forged
2h is burnt, obtains nanocrystalline enhancing amorphous zirconia nano-fiber material (Fig. 3), the nanocrystalline enhancing amorphous zirconia nanofiber
Material has excellent mechanical property (Fig. 2).
Embodiment 2
The preparation method of amorphous zirconia nanofiber
The first step prepares alcohol-water solution (water: ethyl alcohol=2:58) at room temperature, stirs 10-30min, and it is mixed to obtain 60-600mL
Close uniform colourless transparent solution；
Second step takes solution obtained in the 6-60mL first step, 0.5-10g polyvinylpyrrolidone is added, at room temperature
10min is stirred, uniform colorless clear solution is obtained；
Third step takes 10-100mg zirconium oxychloride octahydrate that the colourless transparent solution that second step obtains, ultrasonic disperse is added
30min obtains white suspension solution；
20 DEG C of white suspension solution constant temperature obtained in third step is persistently stirred 2-6h, is reduced to room to solution by the 4th step
Temperature, centrifuge washing obtain white gels shape precipitating；
The precipitating of white gels shape obtained in 4th step is transferred in freeze drier by the 5th step, and dry 24-48h is obtained
To white powder；
Dry white powder obtained in 5th step is transferred in Muffle furnace by the 6th step, and under air environment, 300 DEG C are forged
2h is burnt, amorphous zirconia nano-fiber material (Fig. 4) is obtained, which has excellent power
It learns performance (Fig. 2).
Embodiment 3
The preparation method of crystalline state zirconia nanopowder fiber
The first step prepares alcohol-water solution (water: ethyl alcohol=3:57) at room temperature, stirs 10-30min, and it is mixed to obtain 60-600mL
Close uniform colourless transparent solution；
Second step takes solution obtained in the 6-60mL solution first step, 0.5-10g polyvinylpyrrolidone is added, in room
Temperature is lower to stir 10min, obtains uniform colorless clear solution；
Third step takes 10-100mg zirconium oxychloride octahydrate that the colourless transparent solution that second step obtains, ultrasonic disperse is added
30min obtains white suspension solution；
40 DEG C of white suspension solution constant temperature obtained in third step is persistently stirred 2-6h, is reduced to room to solution by the 4th step
Temperature, centrifuge washing obtain white gels shape precipitating；
The precipitating of white gels shape obtained in 4th step is transferred in freeze drier by the 5th step, and dry 24-48h is obtained
To white powder；
Dry white powder obtained in 5th step is transferred in Muffle furnace by the 6th step, and under air environment, 700 DEG C are forged
2h is burnt, crystalline state zirconia nanopowder fibrous material (Fig. 5) is obtained, which has good mechanical property
Energy (Fig. 2).
Claims (6)
1. a kind of preparation method of high-strength and high-toughness zirconium oxide nanofiber, it is characterised in that include the following steps:
The first step prepares alcohol-water solution (water: ethyl alcohol=1:59-5:55) at room temperature, stirs 10-30min, obtains 60-600mL
Uniformly mixed colourless transparent solution；
Second step takes solution obtained in the 6-60mL first step, and 0.5-10g polyvinylpyrrolidone is added, is stirred at room temperature
10min obtains uniform colorless clear solution；
Third step, the colourless transparent solution for taking 10-100mg zirconium oxychloride octahydrate addition second step to obtain, ultrasonic disperse 30min,
Obtain white suspension solution；
20-60 DEG C of constant temperature of white suspension solution obtained in third step is persistently stirred 2-6h by the 4th step, is reduced to room to solution
Temperature, centrifuge washing obtain white gels shape precipitating；
The precipitating of white gels shape obtained in 4th step is transferred in freeze drier by the 5th step, and dry 24-48h is obtained white
Color powder；
Dry white powder obtained in 5th step is transferred in Muffle furnace by the 6th step, and under air environment, 100-700 DEG C is forged
2-4h is burnt, high-strength and high-toughness zirconium oxide nano-fiber material is obtained.
2. a kind of preparation method of high-strength and high-toughness zirconium oxide nanofiber according to claim 1, it is characterised in that: institute
It is second alcohol and water with alcohol-water system, and there is certain proportion requirement.
3. a kind of preparation method of high-strength and high-toughness zirconium oxide nanofiber according to claim 1, it is characterised in that:
Zirconium oxychloride octahydrate is added after polyvinylpyrrolidone is first added in alcohol-water system, the sequence that the two is added must be consistent.
4. a kind of preparation method of high-strength and high-toughness zirconium oxide nanofiber according to claim 1, it is characterised in that: heat
When the temperature of processing is lower than 350 DEG C, amorphous state is presented in nanofiber, that is, forms amorphous zirconia nanofiber；Heat treatment temperature
For degree at 350-500 DEG C, nanocrystalline and noncrystal simultaneous state, and nanometer in controllable adjustment fiber is presented in nanofiber
The brilliant ratio with amorphous, that is, form nanocrystalline enhancing amorphous zirconia nanofiber；Heat treatment temperature is received at 500-700 DEG C
Tetragonal phase is presented in rice fiber, that is, forms crystalline state zirconia nanopowder fiber.
5. a kind of preparation method of high-strength and high-toughness zirconium oxide nanofiber according to claim 1, it is characterised in that: can
Standby nanofiber is controlled, fibre length is 5-50 μm, diameter 100-1000nm.
6. a kind of preparation method of high-strength and high-toughness zirconium oxide nanofiber according to claim 1, it is characterised in that: system
Standby three kinds of obtained form nanofibers all have higher intensity and toughness, wherein nanocrystalline enhancing amorphous zirconia Nanowire
Peacekeeping amorphous zirconia nanofiber intensity and toughness are apparently higher than crystalline state zirconia nanopowder fiber.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110396731A (en) * | 2019-04-25 | 2019-11-01 | 北京航空航天大学 | A kind of preparation method of bionical high-strength and high ductility nano-composite fiber |
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| CN1559915A (en) * | 2004-02-16 | 2005-01-05 | 华南理工大学 | Process of preparing zirconium oxide nano powder by supersonic sol-gel process |
| CN1861700A (en) * | 2006-05-26 | 2006-11-15 | 上海大学 | Preparation process of zirconium oxide base composite nano powder |
| CN101049965A (en) * | 2007-04-03 | 2007-10-10 | 浙江大学 | Method for preparing powder of zirconium oxide in high purity |
| CN101172856A (en) * | 2007-11-27 | 2008-05-07 | 中国建筑材料科学研究总院 | Method for producing zirconium oxide fibre |
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| CN104876265A (en) * | 2015-05-13 | 2015-09-02 | 南方科技大学 | Preparation method of mixed crystal type zirconium oxide nanoparticle |
| CN107500761A (en) * | 2017-09-29 | 2017-12-22 | 无锡特科精细陶瓷有限公司 | A kind of preparation method of dark-blue zirconia ceramic |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1559915A (en) * | 2004-02-16 | 2005-01-05 | 华南理工大学 | Process of preparing zirconium oxide nano powder by supersonic sol-gel process |
| CN1861700A (en) * | 2006-05-26 | 2006-11-15 | 上海大学 | Preparation process of zirconium oxide base composite nano powder |
| CN101049965A (en) * | 2007-04-03 | 2007-10-10 | 浙江大学 | Method for preparing powder of zirconium oxide in high purity |
| CN101172856A (en) * | 2007-11-27 | 2008-05-07 | 中国建筑材料科学研究总院 | Method for producing zirconium oxide fibre |
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| CN104876265A (en) * | 2015-05-13 | 2015-09-02 | 南方科技大学 | Preparation method of mixed crystal type zirconium oxide nanoparticle |
| CN107500761A (en) * | 2017-09-29 | 2017-12-22 | 无锡特科精细陶瓷有限公司 | A kind of preparation method of dark-blue zirconia ceramic |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110396731A (en) * | 2019-04-25 | 2019-11-01 | 北京航空航天大学 | A kind of preparation method of bionical high-strength and high ductility nano-composite fiber |
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