CN104959045B - A kind of method for preparing polyvinylidene fluoride nanometer array pore membrane - Google Patents
A kind of method for preparing polyvinylidene fluoride nanometer array pore membrane Download PDFInfo
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Abstract
A kind of method for preparing polyvinylidene fluoride nanometer array pore membrane, preparation process is：1）Anodised aluminium nano hole column template is prepared by two-step electrochemical anodizing method by base material of rafifinal；2）In anodic oxidation aluminium formwork front, drop takes the DMF solution of 4 μ L～8 μ L Kynoar, brushes surface with nitrogen, allows Kynoar to fill alumina nanohole column template in right amount and surface Kynoar is excessive；3）Then in 50 DEG C～80 DEG C of baking oven, solvent flashing obtains composite material template；4）Configuration CuCl2, NaOH degrade liquid, aluminium substrate and anodic oxidation aluminium formwork are degraded in dissolving, obtain Kynoar array pore membrane.This to prepare the nano-pore that array pore membrane has homogeneity, process is simple is with low cost, and future will be widely used in nano-filtration membrane and cell nano deielectric-coating.
Description
Technical field
The invention belongs to the preparing technical field of high score subarray nano-pore membrane material, more particularly to one kind prepare poly- inclined fluorine
The method of ethylene nano-array pore membrane.
Background technology
Polymer nano material, has many existence forms, nano wire, nanometer rods, nanotube, Nano microsphere, nanometer
Grain etc., polymer nano material can be widely applied to the every field of national economy due to its nano effect.Polymer nano rice noodle,
Nanotube can be applicable to the fields such as biomedicine, nanometer microelectronics, catalysis material due to its unique property.It is currently acquired poly-
Compound nano wire, the preparation method of nanofiber mainly have three kinds of method of electrostatic spinning, template and self-assembly method.Kynoar
The preparation of nano wire is mainly method of electrostatic spinning, and method of electrostatic spinning almost prepares the only method of nanofiber at present, will be poly-
Polymer solution or melt are placed in thousand of to up to ten thousand volt high voltage electric fields, and powered polymer drop is under electric field force effect in capillary
The Taylor conical points of pipe are accelerated, and overcome surface tension to form injection thread, thread solvent evaporation in course of injection
Solidification, finally falls on the reception device, forms the fiber felt of similar nonwoven fabric shape.With fiber obtained in method of electrostatic spinning than passing
The spinning process of system is thin much, and diameter arrives thousands of nanometers tens.At present with the polymer of method of electrostatic spinning preparation up to tens
Kind.Such as polyethylene glycol oxide (PEO), polyvinyl alcohol (PVA), polystyrene (PS), polymethyl methacrylate (PMMA), poly-
Lactic acid (PLA) etc..Dopant is added in polymer or electrospinning is carried out in triple systems and can substantially reduce gained Nanowire
The diameter of dimension, and composite fibre can be obtained.The preparation method of PVDF perforated membranes is various, including:Phase inversion method, fusion drawn method, burning
Connection, nuclear track etching method etc., wherein phase inversion method production technology flexible simple, easy industrialization, low cost, so being current
Most method used in preparation research.Material of preparing uniform dissolution is exactly formed casting solution after solvent by phase inversion method,
Phase transformation being carried out under certain condition, making casting solution solid-state is converted to by liquid, most used in phase inversion method is dipper precipitation
Method, is secondly thermally induced phase separation.
Polymer nanostructures array mechanism can also be obtained using template, and template is referred to containing highdensity nano-pillar
Shape hole, thickness is tens to hundreds of micron thick film, and conventional template has two kinds, and one kind is ordered into pores array oxidation aluminum dipping form
Plate, another kind is the chelating polymer template containing hole disorder distribution, and the template of other materials also has nano aperture glass, mesoporous boiling
Stone, porous silicon template and metal form.Polymer nanometer array system makees template using nano-array hole film, by chemical method
The macromolecule of polymer solution and molten condition is passed through into heat cure membrane formation process by Kynoar and sun at high temperature under high pressure
Pole alumina formwork is combined, and falls template in dissolved corrosion and obtain polymer nanometer array after film-forming.
Electrostatic spinning prepares polyvinylidene fluoride nanometer structure and phase inversion method prepares the side of Kynoar microcellular structure film
Method, these operational approach are complicated, and the micro nano structure that obtains and microcellular structure are uncontrollable, little using scope.With reference to sun
Pole alumina formwork method prepares polyvinylidene fluoride nanometer hole array film, can effectively obtain the polyvinylidene fluoride in nanometer size effect hole
Alkene array pore membrane, can be widely used in nano-filtration membrane and cell nano deielectric-coating.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, it is an object of the invention to provide one kind prepares polyvinylidene fluoride nanometer battle array
The method of row pore membrane, the method features simple and practical process, with low cost, technical skill is efficiently innovated, and is to prepare polymer nanocomposite battle array
Row pore membrane provides technical support.
For achieving the above object, the technical solution used in the present invention is：One kind prepares polyvinylidene fluoride nanometer array pore membrane
Method, comprise the following steps：
1）Anodised aluminium nano hole column template is prepared by two-step electrochemical anodizing method by base material of rafifinal, in the template
The top aperture diameter of alumina nanohole is 180nm～220nm, and bottom diameter is 140nm～150nm, top wall thickness 38nm
～48nm, bottom wall thickness 140nm～150nm, 430 nm of hole depth～450nm；
2）In anodised aluminium nano hole column template front, drop takes the N of 4 μ L～8 μ L Kynoar, N-dimethylformamide
Solution, standing make Kynoar fill anodised aluminium nano hole column pattern hole enough, then brush surface with nitrogen, blow away table
The excessive Kynoar in face so that surface alumina oxide nano hole column template is exposed, obtains Kynoar alumina formwork multiple
Close base material；
3）In 50 DEG C～80 DEG C of baking oven, solvent flashing obtains composite material template, and composite material template is moved to 195
DEG C～205 DEG C of thermal station on, heating melting 10min eliminates Kynoar thermal history, is then transferred quickly to 150 DEG C～160
DEG C Thermostatic platform in anneal, it is complete that thermostatical crystallization 8h～36h crystallizes which；
4）Configuration mol ratio is 1:1 CuCl2Hydrochloric acid solution, is diluted to 500ml and obtains CuCl2Dilute hydrochloric acid solution, then prepare
Kynoar alumina formwork composite base material is first immersed in CuCl by 5%～10%NaOH solution210min in solution, replaces molten
Aluminium substrate is taken off, deionized water is taken out and is cleaned repeatedly, then the Kynoar alumina formwork after dissolving aluminium substrate is combined
Base material is immersed in 20～40min in 5%～10%NaOH solution, corrosion dissolution anodic oxidation aluminium formwork.Take out remaining undissolved portion
Point, deionized water is cleaned 3～5 times repeatedly, and nitrogen is dried up, and obtains Kynoar array pore membrane.
The invention has the beneficial effects as follows：
The present invention is intended to provide a kind of method for preparing polyvinylidene fluoride nanometer array pore membrane, with anodic oxidation aluminium formwork is
Array mould plate, the casting in template obtain Kynoar anodic oxidation aluminium formwork composite, and then corrosion dissolution removes sun
Pole alumina formwork obtains Kynoar array pore membrane.The perforated membrane has orderly array hole surface, Kynoar hole
Footpath size in the range of 40nm～75nm, in ordered arrangement.
The present invention is prepared for polyvinylidene fluoride nanometer array pore membrane, and the method theoretical basiss are ripe, and technical skill is efficiently created
Newly, technical support is provided to prepare polymer nanometer array pore membrane.It is beneficial to industrialized production, future can obtain extensively should
With.
Description of the drawings
Fig. 1 is the polyvinylidene fluoride nanometer array pore membrane electron-microscope scanning figure of the present invention.
Fig. 2 is the polyvinylidene fluoride nanometer array pore membrane section electron-microscope scanning figure of the present invention..
Fig. 3 is anodic oxidation aluminium formwork electron-microscope scanning figure prepared by the present invention.
Fig. 4 is anodic oxidation aluminium formwork side electron-microscope scanning figure prepared by the present invention.
Specific embodiment
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment one
A kind of method for preparing polyvinylidene fluoride nanometer array pore membrane, includes following steps：
1）Anodised aluminium nano hole column template is prepared by two-step electrochemical anodizing method by base material of rafifinal, in the template
The top aperture diameter of alumina nanohole is 180nm, and bottom diameter is 140nm, top wall thickness 38nm, bottom wall thickness 140nm,
Hole depth 430nm；
2）In anodic oxidation aluminium formwork front, drop takes the DMF solution of 4 μ L Kynoar, and standing makes to gather
Vinylidene fills alumina formwork hole enough, then brushes surface with nitrogen, blows away the excessive Kynoar in surface so that table
Face alumina nanohole column template exposes, and obtains Kynoar alumina formwork composite base material；
3）In 50 DEG C of baking oven, solvent flashing obtains composite material template, and composite material template is moved to 195 DEG C of heat
On platform, heating melting 10min eliminates Kynoar thermal history, anneals in being then transferred quickly to 150 DEG C of Thermostatic platform,
It is complete that thermostatical crystallization 8h crystallizes which；
4）42g copper chlorides, 42ml hydrochloric acid are weighed respectively, are made into the CuCl of 500ml2Dilute hydrochloric acid solution, then prepare 5%NaOH
Kynoar alumina formwork composite base material is first immersed in CuCl by solution210min in solution, displacement dissolve aluminium substrate,
Take out deionized water to clean repeatedly, then the Kynoar alumina formwork composite base material after dissolving aluminium substrate is immersed in into 5%
40min in NaOH solution, corrosion dissolution anodic oxidation aluminium formwork take out remaining undissolved part, and deionized water cleans 3 repeatedly
Secondary, nitrogen is dried up, and obtains Kynoar array pore membrane.
Embodiment two
1st, a kind of method for preparing polyvinylidene fluoride nanometer array pore membrane, it is characterised in that include following steps：
1）Anodised aluminium nano hole column template is prepared by two-step electrochemical anodizing method by base material of rafifinal, in the template
The top aperture diameter of alumina nanohole is 200nm, and bottom diameter is 145nm, top wall thickness 43nm, bottom wall thickness 145nm,
Hole depth 440nm；
2）In anodised aluminium nano hole column template front, drop takes the DMF solution of 6 μ L Kynoar,
Standing makes Kynoar fill anodised aluminium nano hole column pattern hole enough, then brushes surface with nitrogen, blows away surface mistake
The Kynoar of amount so that surface alumina oxide nano hole column template is exposed, obtains Kynoar alumina formwork composite base
Material；
3）In 60 DEG C of baking oven, solvent flashing obtains composite material template, and template is moved in 200 DEG C of thermal station, heating
Melting 10min, eliminates Kynoar thermal history, anneals in being then transferred quickly to 155 DEG C of Thermostatic platform, thermostatical crystallization
It is complete that 24h crystallizes which；
4）42g copper chlorides, 42ml hydrochloric acid are weighed respectively, are made into the CuCl of 500ml2Dilute hydrochloric acid solution, then prepare 8%NaOH
Kynoar alumina formwork composite base material is first immersed in CuCl by solution210min in solution, displacement dissolve aluminium substrate,
Take out deionized water to clean repeatedly, then the Kynoar alumina formwork composite base material after dissolving aluminium substrate is immersed in into 8%
30min in NaOH solution, corrosion dissolution anodic oxidation aluminium formwork take out remaining undissolved part, and deionized water cleans 4 repeatedly
Secondary, nitrogen is dried up, and obtains Kynoar array pore membrane.
Embodiment three
A kind of method for preparing polyvinylidene fluoride nanometer array pore membrane, includes following steps：
1）Anodised aluminium nano hole column template is prepared by two-step electrochemical anodizing method by base material of rafifinal, in the template
The top aperture diameter of alumina nanohole is 220nm, and bottom diameter is 150nm, top wall thickness 48nm, bottom wall thickness 150nm,
Hole depth 450nm；
2）In anodised aluminium nano hole column template front, drop takes the DMF solution of 8 μ L Kynoar,
Standing makes Kynoar fill anodised aluminium nano hole column pattern hole enough, then brushes surface with nitrogen, blows away surface mistake
The Kynoar of amount so that surface alumina oxide nano hole column template is exposed, obtains Kynoar alumina formwork composite base
Material；
3）In 80 DEG C of baking oven, solvent flashing obtains composite material template, and template is moved in 200 DEG C of thermal station, heating
Melting 10min, eliminates Kynoar thermal history, anneals in being then transferred quickly to 160 DEG C of Thermostatic platform, thermostatical crystallization
It is complete that 36h crystallizes which；
4）42g copper chlorides, 42ml hydrochloric acid are weighed respectively, are made into the CuCl of 500ml2Dilute hydrochloric acid solution, then prepare 10%
Kynoar alumina formwork composite base material is first immersed in CuCl by NaOH solution210min in solution, displacement dissolve aluminum
Substrate, takes out deionized water and cleans repeatedly, then the Kynoar alumina formwork composite base material after dissolving aluminium substrate is soaked
The 20min in 10% NaOH solution, corrosion dissolution anodic oxidation aluminium formwork, do not take out remaining undissolved part, deionized water
Clean 5 times repeatedly, nitrogen is dried up, and obtains Kynoar array pore membrane.
By field emission scanning electron microscope（SEM）The structure and pattern on surface and section to Kynoar array pore membrane
Characterized.
Referring to Fig. 1, it is the electron-microscope scanning figure on the surface of the Kynoar array pore membrane of the present invention, can be with by electron microscope
Finding out, the hole with nano-scale being occurred in that on polyvinylidene difluoride film surface, the hole is in array ordered arrangement.Measured hole
Footpath size range is 40nm～75nm.
Referring to Fig. 2, it is the electron-microscope scanning figure of the section of the Kynoar array pore membrane of the present invention, can be with by electron microscope
Find out the nanometer pore of collimation occur in section, it was demonstrated that such nanometer pore is continuous in Kynoar array pore membrane.
Referring to Fig. 3,4, be the present invention by anodizing preparation the front of alumina formwork and the Electronic Speculum of side sweep
Tracing.As can be seen from Fig., the anodic oxidation aluminium formwork with array pore structure has been prepared.The aperture size of the template
For：Top aperture diameter be 180nm～220nm, bottom diameter be 140nm～150nm, top wall thickness 38nm～48nm, bottom
Wall thickness 140nm～150nm, 430 nm of hole depth～450nm.
Claims (4)
1. a kind of method for preparing polyvinylidene fluoride nanometer array pore membrane, it is characterised in that comprise the following steps：
1）Anodised aluminium nano hole column template is prepared by two-step electrochemical anodizing method by base material of rafifinal, is aoxidized in the template
The top aperture diameter of aluminum nano-pore be 180nm～220nm, bottom diameter be 140nm～150nm, top wall thickness 38nm～
48nm, bottom wall thickness 140nm～150nm, 430 nm of hole depth～450nm；
2）Anodised aluminium nano hole column template front drop take 4 μ L～8 μ L Kynoar N,N-dimethylformamide it is molten
Liquid, standing make Kynoar fill anodised aluminium nano hole column pattern hole enough, then brush surface with nitrogen, blow away surface
Excessive Kynoar so that surface alumina oxide nano hole column template is exposed, then volatilizees in 50 DEG C～80 DEG C of baking oven
Solvent, obtains Kynoar alumina formwork composite membrane；
3）By step 2）In the Kynoar alumina formwork composite membrane that obtains, be transferred in 195 DEG C～205 DEG C of thermal station,
Heating melting 10min, eliminates Kynoar thermal history, moves back in being then transferred quickly to 150 DEG C～160 DEG C of Thermostatic platform
Fire, it is complete that thermostatical crystallization 8h～36h crystallizes which, the Kynoar alumina formwork composite membrane after being annealed；
4）Configuration mol ratio is 1:1 CuCl2Hydrochloric acid solution, is diluted to 500mL and obtains CuCl2Dilute hydrochloric acid solution, then prepare 5%～
10%NaOH solution, first by step 3）Kynoar alumina formwork composite membrane after middle annealing is immersed in CuCl2Dilute hydrochloric acid is molten
10min in liquid, displacement dissolve aluminium substrate, take out deionized water and clean repeatedly, then gathering the annealing after dissolving aluminium substrate
Vinylidene alumina formwork composite membrane is immersed in 20～40min in 5%～10%NaOH solution, corrosion dissolution anodic oxidation aluminum dipping form
Plate, takes out remaining undissolved part, and deionized water is cleaned 3～5 times repeatedly, and nitrogen is dried up, that is, obtain polyvinylidene fluoride nanometer
Array pore membrane.
2. a kind of method for preparing polyvinylidene fluoride nanometer array pore membrane according to claim 1, it is characterised in that include
Following steps：
1）Anodised aluminium nano hole column template is prepared by two-step electrochemical anodizing method by base material of rafifinal, is aoxidized in the template
The top aperture diameter of aluminum nano-pore is 180nm, and bottom diameter is 140nm, top wall thickness 38nm, bottom wall thickness 140nm, hole depth
430 nm；
2）In anodised aluminium nano hole column template front, drop takes the DMF solution of 4 μ L Kynoar,
Standing makes Kynoar fill anodised aluminium nano hole column pattern hole enough, then brushes surface with nitrogen, blows away surface mistake
The Kynoar of amount so that surface alumina oxide nano hole column template is exposed, then the solvent flashing in 50 DEG C of baking oven, obtains
Kynoar alumina formwork composite membrane；
3）By step 2）In the Kynoar alumina formwork composite membrane that obtains, be transferred in 195 DEG C of thermal station, heating melting
10min, eliminates Kynoar thermal history, anneals in being then transferred quickly to 150 DEG C of Thermostatic platform, and thermostatical crystallization 8h makes which
Crystallization is complete, the Kynoar alumina formwork composite membrane after being annealed；
4）Configuration mol ratio is 1:1 CuCl2Hydrochloric acid solution, is diluted to 500mL and obtains CuCl2Dilute hydrochloric acid solution, then prepare 5%
NaOH solution, first by step 3）Kynoar alumina formwork composite membrane after middle annealing is immersed in CuCl2Dilute hydrochloric acid solution
Middle 10min, displacement dissolve aluminium substrate, take out deionized water and clean repeatedly, then will dissolve the poly- inclined of the annealing after aluminium substrate
Fluorothene alumina formwork composite membrane is immersed in 40min in 5%NaOH solution, and corrosion dissolution anodic oxidation aluminium formwork takes out remaining
Undissolved part, deionized water are cleaned 3 times repeatedly, and nitrogen is dried up, that is, obtain polyvinylidene fluoride nanometer array pore membrane.
3. a kind of method for preparing polyvinylidene fluoride nanometer array pore membrane according to claim 1, it is characterised in that include
Following steps：
1）Anodised aluminium nano hole column template is prepared by two-step electrochemical anodizing method by base material of rafifinal, is aoxidized in the template
The top aperture diameter of aluminum nano-pore is 200nm, and bottom diameter is 145nm, top wall thickness 43nm, bottom wall thickness 145nm, hole depth
440nm；
2）In anodised aluminium nano hole column template front, drop takes the DMF solution of 6 μ L Kynoar, quiet
Putting makes Kynoar fill anodised aluminium nano hole column pattern hole enough, then brushes surface with nitrogen, blows away surface excess
Kynoar so that surface alumina oxide nano hole column template is exposed, and then the solvent flashing in 60 DEG C of baking oven, is gathered
Vinylidene alumina formwork composite membrane；
3）By step 2）In the Kynoar alumina formwork composite membrane that obtains, be transferred in 205 DEG C of thermal station, heating melting
10min, eliminates Kynoar thermal history, anneals in being then transferred quickly to 155 DEG C of Thermostatic platform, and thermostatical crystallization 24h makes
Its crystallization is complete, the Kynoar alumina formwork composite membrane after being annealed；
4）Configuration mol ratio is 1:1 CuCl2Hydrochloric acid solution, is diluted to 500mL and obtains CuCl2Dilute hydrochloric acid solution, then prepare 8%
NaOH solution, first by step 3）Kynoar alumina formwork composite membrane after middle annealing is immersed in CuCl2Dilute hydrochloric acid solution
Middle 10min, displacement dissolve aluminium substrate, take out deionized water and clean repeatedly, then will dissolve the poly- inclined of the annealing after aluminium substrate
Fluorothene alumina formwork composite membrane is immersed in 30min in 8%NaOH solution, and corrosion dissolution anodic oxidation aluminium formwork takes out remaining
Undissolved part, deionized water are cleaned 4 times repeatedly, and nitrogen is dried up, that is, obtain polyvinylidene fluoride nanometer array pore membrane.
4. a kind of method for preparing polyvinylidene fluoride nanometer array pore membrane according to claim 1, it is characterised in that include
Following steps：
1）Anodised aluminium nano hole column template is prepared by two-step electrochemical anodizing method by base material of rafifinal, is aoxidized in the template
The top aperture diameter of aluminum nano-pore is 220nm, and bottom diameter is 150nm, top wall thickness 48nm, bottom wall thickness 150nm, hole depth
450nm；
2）In anodised aluminium nano hole column template front, drop takes the DMF solution of 8 μ L Kynoar, quiet
Putting makes Kynoar fill anodised aluminium nano hole column pattern hole enough, then brushes surface with nitrogen, blows away surface excess
Kynoar so that surface alumina oxide nano hole column template is exposed, and then the solvent flashing in 80 DEG C of baking oven, is gathered
Vinylidene alumina formwork composite membrane；
3）By step 2）In the Kynoar alumina formwork composite membrane that obtains, be transferred in 200 DEG C DEG C of thermal station, heating is molten
Melt 10min, eliminate Kynoar thermal history, anneal in being then transferred quickly to 160 DEG C of Thermostatic platform, thermostatical crystallization 36h
Crystallize which complete, the Kynoar alumina formwork composite membrane after being annealed；
4）Configuration mol ratio is 1:1 CuCl2Hydrochloric acid solution, is diluted to 500mL and obtains CuCl2Dilute hydrochloric acid solution, then prepare 10%
NaOH solution, first by step 3）Kynoar alumina formwork composite membrane after middle annealing is immersed in CuCl2Dilute hydrochloric acid solution
Middle 10min, displacement dissolve aluminium substrate, take out deionized water and clean repeatedly, then will dissolve the poly- inclined of the annealing after aluminium substrate
Fluorothene alumina formwork composite membrane is immersed in 20min in 10%NaOH solution, and corrosion dissolution anodic oxidation aluminium formwork takes out surplus
Remaining undissolved part, deionized water are cleaned 5 times repeatedly, and nitrogen is dried up.
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| CN103531817A (en) * | 2013-10-17 | 2014-01-22 | 山东玉皇化工有限公司 | Three-dimensional copper nanowire array current collector for lithium ion battery and production method of three-dimensional copper nanowire array current collector |
| CN105540535B (en) * | 2015-12-29 | 2017-01-25 | 陕西科技大学 | Method for preparing multi-scale high-gamma-phase polyvinylidene fluoride hollow nanowires |
| CN105624919B (en) * | 2016-03-14 | 2017-10-17 | 南京邮电大学 | The preparation method of the polymer patterning film of polyvinyl-fluoride |
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| CN107217289A (en) * | 2017-05-09 | 2017-09-29 | 南昌航空大学 | It is a kind of to remove the method that titanium alloy differential arc oxidation film layer remains matrix |
| CN109721134A (en) * | 2019-03-06 | 2019-05-07 | 哈尔滨工业大学 | A kind of preparation method of the conductive sintering membrane electrode suitable for microbial film filtering battery |
| CN111686588B (en) * | 2020-07-02 | 2022-04-01 | 厦门理工学院 | Composite nanofiltration membrane with layered double hydroxide as modified template and preparation method thereof |
| KR20230048882A (en) * | 2021-10-05 | 2023-04-12 | 주식회사 영광와이케이엠씨 | Photonic crystal composites with variable structural color and Manufacturing method thereof |
| CN115869778B (en) * | 2023-03-02 | 2023-05-16 | 广东省科学院生态环境与土壤研究所 | PVDF nanoparticle array porous membrane and preparation method and application thereof |
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