CN103881119B - A kind of preparation method of PVDF base Organic Iron electric polymer nanotube - Google Patents
A kind of preparation method of PVDF base Organic Iron electric polymer nanotube Download PDFInfo
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- CN103881119B CN103881119B CN201410020982.0A CN201410020982A CN103881119B CN 103881119 B CN103881119 B CN 103881119B CN 201410020982 A CN201410020982 A CN 201410020982A CN 103881119 B CN103881119 B CN 103881119B
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Abstract
The present invention discloses the preparation method of a kind of PVDF base Organic Iron electric polymer nanotube.It is characterized in that, by using anodised aluminium nanometer masterplate, Kynoar based polymer solution is dropped to anodised aluminium nano-form upper surface, by annealing, its solvent is made to volatilize, to making remained on surface Organic Iron electric polymer, it melts post-heating, utilize capillary tube and the molten state polyvinylidene fluoride ferroelectric polymers self gravitation effect of nanometer masterplate, Kynoar based polyalcohol infiltration masterplate, after thing to be polymerized condensation, polyvinylidene fluoride polymer nanotube is formed, sodium hydroxide solution is finally used to erode anodised aluminium nano-form, obtain polyvinylidene fluoride ferroelectric polymers nanotube.Template of the present invention prepares PVDF base Organic Iron electric polymer nanotube, and method and technique are simple, it is easy to control nanotube radial dimension, and unusual physical characteristic and related device for research PVDF base Organic Iron electric polymer nanotube provide possibility.
Description
Technical field
The present invention relates to the technology of preparing of organic polymer nanotube, refer specifically to a kind of based on polyvinylidene fluoride
The preparation method of Organic Iron electric polymer nanotube.
Background introduction
Nearly ten years, along with sensor and micro electro mechanical device are towards miniaturization, the development of miniaturization, the most
Through there being the proposition of nano mechanical device.Low-dimensional nano structure has attracted science due to its small size and bigger serface
In boundary and engineering circles, i.e. can be widely applied to nano electron device, nanocomposite optical device and nano-electromechanical device.
Wherein, 1-dimention nano pipe and nano wire property produced by size confinement effect are considered to receiving
Rice device is used widely.The at present research to one-dimensional nano structure focus primarily upon metal, alloy,
The preparation of oxide ceramics, semiconductor nanowires or nano tube structure and aspect of performance, for polymer
One-dimensional nano structure research is the fewest.
Ferroelectric material, i.e. has spontaneous polarization in some temperature range, and spontaneous polarization strength year external electric field become
The class material changed and change is a class focus material of Recent study.Research about ferroelectric material is main
Concentrate on nano film material, but the oxide nano of ferroelectric material shows and is much different from block
Material and the Strange properties of thin film.Inorganic iron electric material such as Barium metatitanate. based on oxide, lead zirconate titanate, strontium
Bismuth tantalum oxygen (sees: Rev.Adv.Mater.Sci.4 (2003) 114-122), is the most also related to ferroelectricity and receives
The report of mitron theoretical research, such as lead titanates (Phys.Rev.Lett.108,067601 (2012)).In recent years,
Copolymer p based on polyvinylidene fluoride PVDF, polyvinylidene fluoride and trifluoro-ethylene (VDF-TrFE) is
The ferroelectric polymer material of a kind of function admirable, can be widely used in energy conduction, information storage and
The functional material of infrared acquisition.It has relatively low dielectric constant, low elastic coefficient and low-density simultaneously, also
It it is the ideal material preparing sensor.
In the past few decades, ferroelectric thin film has obtained studying widely.One-dimensional nanostructures by
In its unusual characteristic the most increasingly by the extensive concern of scientific circles.Among these, ferroelectric nano-wire and nanometer
Pipe is extensively proved to can apply to the aspects such as nano-sensor, non-volatility memorizer and nano generator.
Nanotube stores owing to its bigger specific surface area can apply to high density energy simultaneously.The present invention is by base
Material based on PVDF base ferroelectric polymers, invents and a kind of prepares polymer nanotube based on template
Technical process.It is simple that template prepares polymer nanotube technique, and preparation temperature is low.Simultaneously can be by changing
Become template size and prepare various sizes of ferroelectric polymers nanotube, it is thus possible to widen the application neck of nanotube
Territory.
Summary of the invention
The present invention proposes the preparation method of a kind of PVDF base Organic Iron electric polymer nanotube, it is achieved that organic
The preparation of ferroelectric polymers nanotube.
The present invention discloses the preparation method of a kind of PVDF base Organic Iron electric polymer nanotube.Its feature exists
In, by using aluminum oxide template, Kynoar based polymer solution is dropped to anodised aluminium nanometer mould
Plate upper surface, by annealing so that it is solvent volatilizees, and post-heating is to making remained on surface Organic Iron electropolymerization
Thing its melt, utilize the capillarity of nano aperture in anodised aluminium nano-form and molten state to gather inclined fluorine
Vinyl ferroelectric polymers self gravitation effect, Kynoar based polyalcohol is filled out in infiltration template in nano-pore
Surface, after thing to be polymerized condensation, polyvinylidene fluoride polymer nanotube is formed, and finally uses sodium hydroxide
Solution corrosion falls anodised aluminium nano-form, obtains polyvinylidene fluoride ferroelectric polymers nanotube.This
Bright template prepares PVDF base Organic Iron electric polymer nanotube, and method and technique are simple, it is easy to control to receive
Mitron radial dimension, for studying the unusual physical characteristic of PVDF base Organic Iron electric polymer nanotube and being correlated with
Device provides possibility.
The concrete preparation method of PVDF base Organic Iron electric polymer nanotube is as follows:
(1) by nanoporous size scope 40-150nm, template thickness is the anodised aluminium nanometer of 60 μm
Template each ultrasonic cleaning 3 minutes in pure water, acetone, ethanol successively, by anodised aluminium nano-form
Surface clean is clean, then anneals 4 hours under 380-400 degree, removes anodised aluminium nano-form system
Remain in the Organic substance in aperture during Bei, make aperture inner surface smooth simultaneously, it is simple to form polymer
Nanotube；
(2) PVDF base Organic Iron electric polymer solution is dropped to anodised aluminium nano-form surface, and
Solvent is made to volatilize as annealing；
(3) the anodised aluminium nano-form of annealing is heated to 240-260 degree, makes anodised aluminium
On nano-form, PVDF base Organic Iron electric polymer fuses in template；
(4) cooling template is to room temperature, removes remained on surface PVDF base Organic Iron electric polymer, wherein said
Removing remained on surface PVDF base Organic Iron electric polymer method is that acetone soln wipes method；
(5) use sodium hydroxide solution to dissolve template, complete PVDF base Organic Iron electric polymer nanotube
Preparation, wherein said utilization sodium hydroxide solution dissolve template, concentration of sodium hydroxide solution is 2-4mol/L.
PVDF base Organic Iron electric polymer described in step (3) is Kynoar list polymers, poly-
Vinylidene-trifluoro-ethylene copolymer or Kynoar-trifluoro-ethylene-chlorine fluorothene trimer, its quality hundred
Dividing content 8-10%, solvent is butanone.
The invention has the advantages that the nanotube preparing a kind of PVDF base ferroelectric polymer material, technique is simple,
Low cost, it is easy to prepare the Organic Iron electric polymer nanotube of different scale.
Accompanying drawing illustrates:
Fig. 1 is that PVDF based polyalcohol nanotube prepares schematic diagram；Wherein: (a) PVDF based polyalcohol is received
Mitron preparation process schematic cross-section, (b) PVDF based polyalcohol nanotube has prepared rear anodised aluminium
Template surface schematic diagram.In figure: 1. anodised aluminium nano-form, 2. nano aperture, 3.PVDF base is polymerized
Thing, 4.PVDF based polyalcohol nanotube.
Fig. 2 is PVDF based polyalcohol nanotube preparation process figure.
Fig. 3 is PVDF based polyalcohol nanotube scanning electron microscope (SEM) photograph.
Detailed description of the invention:
Embodiment 1: combining accompanying drawing 1, the specific implementation method of the statement present invention, concrete steps are followed successively by:
Each ultrasonic cleaning 3 minutes in pure water, acetone, ethanol successively by anodised aluminium nano-form 1,
By clean for anodised aluminium nano-form surface clean.Then anneal 4 hours under 380 degree, be mainly
Remove in anodised aluminium nano-form preparation process and remain in the Organic substance in nano aperture 2, make simultaneously
Obtain aperture inner surface smooth, it is simple to form polymer nanotube；Template 1 is anodic oxidation aluminium formwork, and it is received
Metre hole footpath 2 size range 150nm, template thickness is 60 microns.
PVDF base Organic Iron electric polymer solution is dropped to anodised aluminium nano-form 1 surface；
P (VDF-TrFE) Organic Iron electric polymer solution, its solvent is butanone, and its solution concentration is that percent mass contains
Amount is 8%.
To drip and have the anodised aluminium nano-form 1 of P (VDF-TrFE) Organic Iron electric polymer 3 solution 60
The lower insulation of degree 30 minutes, under 135 degree, annealing 4 hours, make solvent volatilize；
The anodised aluminium nano-form 1 of annealing is heated to 240 degree, continues 30 minutes, make sun
On pole aluminium oxide nano-form 1, P (VDF-TrFE) Organic Iron electric polymer 3 fuses in template；
Cooling template, to room temperature, removes remained on surface P (VDF-TrFE) Organic Iron electric polymer 3；Remove table
Face residual PVDF base Organic Iron electric polymer 3 method also can use oxygen plasma by acetone soln erasing method
Etching method.
Using sodium hydroxide solution to dissolve template, concentration of sodium hydroxide solution is 2mol/L, completes
The preparation of P (VDF-TrFE) Organic Iron electric polymer nanotube 4, tube diameters 200 nanometer (see Fig. 3).
Embodiment 2:
In conjunction with accompanying drawing 1, the specific implementation method of the statement present invention, concrete steps are followed successively by:
Each ultrasonic cleaning 3 minutes in pure water, acetone, ethanol successively by anodised aluminium nano-form 1,
By clean for anodised aluminium nano-form surface clean.Then anneal 4 hours under 390 degree, be mainly
Remove in anodised aluminium nano-form preparation process and remain in the Organic substance in nano aperture 2, make simultaneously
Obtain aperture inner surface smooth, it is simple to form polymer nanotube；Template 1 is anodic oxidation aluminium formwork, and it is received
Metre hole footpath 2 size range 100nm, template thickness is 60 microns.
PVDF base Organic Iron electric polymer solution is dropped to anodised aluminium nano-form 1 surface；
P (VDF-TrFE) Organic Iron electric polymer solution, its solvent is butanone, and its solution concentration is that percent mass contains
Amount is 9%.
To drip and have the anodised aluminium nano-form 1 of P (VDF-TrFE) Organic Iron electric polymer 3 solution 60
The lower insulation of degree 30 minutes, under 135 degree, annealing 4 hours, make solvent volatilize；
The anodised aluminium nano-form 1 of annealing is heated to 250 degree, continues 30 minutes, make sun
On pole aluminium oxide nano-form 1, P (VDF-TrFE) Organic Iron electric polymer 3 fuses in template；
Cooling template, to room temperature, removes remained on surface P (VDF-TrFE) Organic Iron electric polymer 3；Remove table
Face residual PVDF base Organic Iron electric polymer 3 method also can use oxygen plasma by acetone soln erasing method
Etching method.
Using sodium hydroxide solution to dissolve template, concentration of sodium hydroxide solution is 3mol/L, completes
The preparation of P (VDF-TrFE) Organic Iron electric polymer nanotube 4, tube diameters 150 nanometer.
Embodiment 3: will be to combine accompanying drawing 1 below, the specific implementation method of the statement present invention, concrete steps
It is followed successively by:
Each ultrasonic cleaning 3 minutes in pure water, acetone, ethanol successively by anodised aluminium nano-form 1,
By clean for anodised aluminium nano-form surface clean.Then anneal 4 hours under 400 degree, be mainly
Remove in anodised aluminium nano-form preparation process and remain in the Organic substance in nano aperture 2, make simultaneously
Obtain aperture inner surface smooth, it is simple to form polymer nanotube；Template 1 is anodic oxidation aluminium formwork, and it is received
Metre hole footpath 2 size range 40nm, template thickness is 60 microns.
PVDF base Organic Iron electric polymer solution is dropped to anodised aluminium nano-form 1 surface；
P (VDF-TrFE) Organic Iron electric polymer solution, its solvent is butanone, and its solution concentration is that percent mass contains
Amount is 10%.
To drip and have the anodised aluminium nano-form 1 of P (VDF-TrFE) Organic Iron electric polymer 3 solution 60
The lower insulation of degree 30 minutes, under 135 degree, annealing 4 hours, make solvent volatilize；
The anodised aluminium nano-form 1 of annealing is heated to 260 degree, continues 30 minutes, make sun
On pole aluminium oxide nano-form 1, P (VDF-TrFE) Organic Iron electric polymer 3 fuses in template；
Cooling template, to room temperature, removes remained on surface P (VDF-TrFE) Organic Iron electric polymer 3；Remove table
Face residual PVDF base Organic Iron electric polymer 3 method also can use oxygen plasma by acetone soln erasing method
Etching method.
Using sodium hydroxide solution to dissolve template, concentration of sodium hydroxide solution is 4mol/L, completes
The preparation of P (VDF-TrFE) Organic Iron electric polymer nanotube 4, tube diameters 60 nanometer.
Claims (1)
1. the preparation method of a PVDF base Organic Iron electric polymer nanotube, it is characterised in that preparation side
Method comprises the following steps:
(1) by nanoporous size scope 40-150nm, template thickness is the anodised aluminium nanometer of 60 μm
Template each ultrasonic cleaning 3 minutes in pure water, acetone, ethanol successively, by anodised aluminium nano-form
Surface clean is clean, then anneals 4 hours under 380-400 degree, removes anodised aluminium nano-form system
Remain in the Organic substance in aperture during Bei, make aperture inner surface smooth simultaneously, it is simple to form polymer
Nanotube；
(2) PVDF base Organic Iron electric polymer solution is dropped to anodised aluminium nano-form surface, and
Solvent is made to volatilize as annealing；
(3) the anodised aluminium nano-form of annealing is heated to 240-260 degree, makes anodised aluminium
On nano-form, PVDF base Organic Iron electric polymer fuses in template；Described PVDF base Organic Iron voltolisation
Compound is Kynoar list polymers, Kynoar-trifluoro-ethylene copolymer or Kynoar-trifluoro second
Alkene-chlorine fluorothene trimer, its weight/mass percentage composition 8-10%, solvent is butanone；
(4) cooling template is to room temperature, removes remained on surface PVDF base Organic Iron electric polymer, wherein said
Removing remained on surface PVDF base Organic Iron electric polymer method is that acetone soln wipes method；
(5) use sodium hydroxide solution to dissolve template, complete PVDF base Organic Iron electric polymer nanotube
Preparation, wherein said utilization sodium hydroxide solution dissolve template, concentration of sodium hydroxide solution is 2-4mol/L.
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| WO2018156079A1 (en) * | 2017-02-21 | 2018-08-30 | Agency For Science, Technology And Research | Ultrasonic transducers and methods for producing an ultrasonic transducer |
| CN108192247B (en) * | 2018-02-09 | 2019-06-11 | 华中科技大学 | A kind of ferroelectric polymers electric card material and preparation method thereof |
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