CN103923335B - PEDOT:PSS/ kaolin nanotube matrix material and preparation method thereof - Google Patents
PEDOT:PSS/ kaolin nanotube matrix material and preparation method thereof Download PDFInfo
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- CN103923335B CN103923335B CN201410192249.7A CN201410192249A CN103923335B CN 103923335 B CN103923335 B CN 103923335B CN 201410192249 A CN201410192249 A CN 201410192249A CN 103923335 B CN103923335 B CN 103923335B
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Abstract
The present invention relates to the conductivity type field of nanocomposite materials containing hole, disclose a kind of conducting polymer/kaolin nanotube (HNTs) matrix material and preparation method thereof.Gained matrix material of the present invention carries out compound by conducting polymer PEDOT:PSS and nonconducting kaolin nanotube and obtains, and wherein kaolin nanotube quality is the 43.5-79.4% of matrix material total mass.Raw material of the present invention is easy to get, simple to operate, and Electrical Conductivity of Composites is high, and specific surface area is large, and the different advantages of existing organic and inorganic materials, have again the characteristic of nano material, adequately achieve mutual supplement with each other's advantages.PEDOT:PSS/ kaolin nanotube matrix material has fabulous application prospect in thermoelectricity, electrical condenser, hertzian wave etc.
Description
Technical field
The present invention relates to conductive nano composite material field, especially PEDOT:PSS/ kaolin nanotube matrix material and preparation method thereof.
Background technology
In recent years, the macromolecule conducting material of the optical characteristics but also the mechanical property having polymkeric substance good and workability that had not only had metal and semiconductor material causes showing great attention to of scientific circles and industry member.In numerous conductive polymerss, because PEDOT:PSS has good water-soluble, stability and film-forming properties, specific conductivity is high, and transmittance is good, and the mechanism of doping effect of uniqueness, makes it become the good conductive polymers of application prospect.
[take kaolin nanotube as the nano composite material of representative, cause the very big concern of researchist with the stuctures and properties of its uniqueness.Kaolin is a kind of alumino-silicate minerals of natural formation, mainly hollow laminate structure, is connected to form a crystal layer unit by one deck silicon-oxy tetrahedron and one deck alumina octahedral, is 1:1 type layered silicate, its internal surface is with positive charge, and outside surface is with negative charge.Kaolin nanotube is kaolinic a kind of tubular nanometer material, hollow, and both ends open is high temperature resistant, acidproof, insulation, length at 1-2 μm, external diameter about 50nm, internal diameter 20-30nm.Kaolin nanotube is doped in PEDOT:PSS dispersion liquid, PEDOT:PSSS and kaolin is made to carry out compound, preparation PEDOT:PSS/HNTs matrix material, for this area provides a kind of novel conductive material, to the exploitation of kaolin nanotube and the development of conducting polymer materials significant, have no relevant report at present.
Summary of the invention
The present invention aims to provide the high new PE DOT:PSS/ kaolin nanotube matrix material of a kind of electrical efficiency, makes the different advantages of its existing organic and inorganic materials, has again the characteristic of nano material, realizes having complementary advantages; Another object is to provide its preparation method.
For realizing the object of the invention, technological method is as follows:
This nano composite material is obtained by the kaolin nanotube of tubular structure and the PEDOT:PSS compound with high conductivity,
Wherein kaolin nanotube quality is the 43.5-79.4% of matrix material total mass.
Be PEDOT:PSS/HNTs matrix material hereinafter referred to as it.
The preparation method of described PEDOT:PSS/ kaolin nanotube matrix material comprises the steps:
(1) kaolin nanotube joins in PEDOT:PSS dispersion liquid, and rapid stirring under room temperature makes it mix;
(2) be added in PET film by above-mentioned dispersant liquid drop, 50 DEG C-60 DEG C heating 1h, 120 DEG C of-130 DEG C of thermal treatments, obtain PEDOT:PSS/NTsH film.
(3) PEDOT:PSS/HNTs film soaks in formic acid, 140 DEG C of-150 DEG C of thermal treatments, obtains the acid-treated PEDOT:PSS/HNTs matrix material of first.
Kaolin nanotube and PEDOT:PSS weight ratio are 1:0.77-1:3.85.Kaolin nanotube size-grade distribution 1-2 μm, external diameter 50-60nm, internal diameter 20-30nm.
Innovative point of the present invention is: conducting polymer PEDOT:PSS and nonconducting kaolin nanotube are carried out compound, has inquired in matrix material to add kaolin content and affect its specific conductivity.
The invention has the beneficial effects as follows: raw material is easy to get, component proportion easily controls, preparation technology is simple to operation, and the kaolin nanotube in matrix material has pore space structure, after PEDOT:PSS compound, improve the specific conductivity of material, add the specific surface area of matrix material, optimize the Electromagnetic performance of material, the different advantages of existing organic and inorganic materials, there is again the characteristic of nano material, adequately achieve mutual supplement with each other's advantages.Be expected at hertzian wave, the field such as thermoelectricity, ultracapacitor realizes suitability for industrialized production and widespread use.
Accompanying drawing explanation
Fig. 1 is the specific conductivity of PEDOT:PSS/HNTs matrix material and the relation of different kaolin content.
Fig. 2 is that formic acid soaks the specific conductivity of PEDOT:PSS/HNTs matrix material and the relation of different kaolin content.
Fig. 3 is the BET absorption figure of PEDOT:PSS/HNTs matrix material of the present invention.
Fig. 4 is the UV-IR-Vis spectrogram of PEDOT:PSS/HNTs matrix material of the present invention.
Fig. 5 is the XRD spectra of kaolin nanotube.
Fig. 6 is the XRD spectra of PEDOT:PSS/HNTs matrix material of the present invention.
Fig. 7 is the scanning electron microscope (SEM) photograph of kaolin nanotube under 40000 times.
Fig. 8 is the scanning electron microscope (SEM) photograph of PEDOT:PSS/HNTs composite material surface of the present invention under 20000 times.
Fig. 9 is the scanning electron microscope (SEM) photograph of PEDOT:PSS/HNTs composite material surface of the present invention under 50000 times.
Figure 10 is the scanning electron microscope (SEM) photograph of PEDOT:PSS/HNTs matrix material cross section of the present invention under 20000 times.
Figure 11 is the scanning electron microscope (SEM) photograph of PEDOT:PSS/HNTs matrix material cross section of the present invention under 50000 times.
Specific implementation method
Below in conjunction with drawings and Examples, the present invention is further illustrated.
Kaolin nanotube (HNTs), formic acid is commercially available product.
Embodiment one
By 1.42g kaolin nanotube (the long 1-2 μm of size-grade distribution, external diameter about 50nm, internal diameter 20-30nm) be doped in 1.1402gPEDOT:PSS dispersion liquid, rapid stirring 24h, obtain obtaining uniform dispersion A, dispersion liquid A is added drop-wise on 2cm × 2cmPET film, 50 DEG C of heating 1h, 120 DEG C of heating 15min.The electric conductivity adopting four probe method to record this nano composite material is 0.23S.cm
-1.Above-mentioned matrix material is soaked 10min in formic acid, then 140 DEG C of thermal treatment 5min, the specific conductivity recording the nano composite material that formic acid soaks is 256.7S.cm
-1.Specific surface area is 81.05m
2/ g.Kaolin nanotube quality is 43.5% of matrix material total mass.
Starting material PEDOT:PSS specific conductivity is 0.17S.cm
-1.
Embodiment two
By 1.1402g kaolin nanotube (size-grade distribution 1-2 μm, external diameter about 50nm, internal diameter 20-30nm) be doped in 1.1402gPEDOT:PSS dispersion liquid, rapid stirring 24h, obtain obtaining uniform dispersion A, dispersion liquid A is added drop-wise on 2cm × 2cmPET film, 60 DEG C of heating 1h, 130 DEG C of heating 15min.The electric conductivity adopting four probe method to record this nano composite material is 0.34S.cm
-1.Above-mentioned matrix material is soaked 10min in formic acid, then 140 DEG C of thermal treatment 5min, the specific conductivity recording the nano composite material that formic acid soaks is 211.4S.cm
-1.Specific surface area is 81.05m
2/ g.Kaolin nanotube quality is 60.1% of matrix material total mass.
Starting material PEDOT:PSS specific conductivity is 0.17S.cm
-1.
Embodiment three
0.5701g kaolin nanotube is doped in 1.1402gPEDOT:PSS dispersion liquid, rapid stirring 24h, obtains obtaining uniform dispersion A, dispersion liquid A is added drop-wise on 2cm × 2cmPET film, 50 DEG C of heating 1h, 130 DEG C of heating 15min.The electric conductivity adopting four probe method to record this nano composite material is 0.51S.cm
-1.Above-mentioned matrix material is soaked 10min in formic acid, then 150 DEG C of thermal treatment 5min, the specific conductivity recording the nano composite material that formic acid soaks is 70.1S.cm
-1.Specific surface area is 81.05m
2/ g.Kaolin nanotube quality is 69.8% of matrix material total mass.
Starting material PEDOT:PSS specific conductivity is 0.17S.cm
-1.
Embodiment four
0.38g kaolin nanotube is doped in 1.1402gPEDOT:PSS dispersion liquid, rapid stirring 24h, obtains obtaining uniform dispersion A, dispersion liquid A is added drop-wise on 2cm × 2cmPET film, 60 DEG C of heating 1h, 120 DEG C of heating 15min.The electric conductivity adopting four probe method to record this nano composite material is 0.57S.cm
-1.Above-mentioned matrix material is soaked 10min in formic acid, then 150 DEG C of thermal treatment 5min, the specific conductivity recording the nano composite material that formic acid soaks is 40.3S.cm
-1.Specific surface area is 81.05m
2/ g.Kaolin nanotube quality is 75.5% of matrix material total mass.
Starting material PEDOT:PSS specific conductivity is 0.17S.cm
-1.
Embodiment five
0.3167g kaolin nanotube is doped in 1.1402gPEDOT:PSS dispersion liquid, rapid stirring 24h, obtains obtaining uniform dispersion A, dispersion liquid A is added drop-wise on 2cm × 2cmPET film, 60 DEG C of heating 1h, 130 DEG C of heating 15min.The electric conductivity adopting four probe method to record this nano composite material is 0.26S.cm
-1.Above-mentioned matrix material is soaked 10min in formic acid, then 150 DEG C of thermal treatment 5min, the specific conductivity recording the nano composite material that formic acid soaks is 22.2S.cm
-1.Specific surface area is 81.05m
2/ g.Kaolin nanotube quality is 79.4% of matrix material total mass.
Starting material PEDOT:PSS specific conductivity is 0.17S.cm
-1.
Claims (4)
1.PEDOT:PSS/ kaolin nanotube matrix material, is characterized in that, this nano composite material by kaolin nanotube and PEDOT:PSS by the following method compound obtain:
(1) be first dispersed in by kaolin nanotube in PEDOT:PSS dispersion liquid, stirring at room temperature, makes it mix;
(2) above-mentioned dispersant liquid drop is added on PET, 50 DEG C-60 DEG C heating, 120 DEG C of-130 DEG C of thermal treatments, obtains PEDOT:PSS/ kaolin nanotube film;
(3) PEDOT:PSS/ kaolin nanotube film soaks in formic acid, 140 DEG C of-150 DEG C of thermal treatments, obtains first acid-treated PEDOT:PSS/ kaolin nanotube matrix material;
Wherein the quality of kaolin nanotube is the 43.5-79.4% of matrix material total mass.
2. PEDOT:PSS/ kaolin nanotube matrix material as claimed in claim 1, is characterized in that, kaolin nanotube size-grade distribution 1-2 μm, external diameter 50-60nm, internal diameter 20-30nm.
3. the preparation method of PEDOT:PSS/ kaolin nanotube matrix material as claimed in claim 1 or 2, is characterized in that, realizes as follows:
(1) be first dispersed in by kaolin nanotube in PEDOT:PSS dispersion liquid, stirring at room temperature, makes it mix;
(2) above-mentioned dispersant liquid drop is added on PET, 50 DEG C-60 DEG C heating, 120 DEG C of-130 DEG C of thermal treatments, obtains PEDOT:PSS/ kaolin nanotube film;
(3) PEDOT:PSS/ kaolin nanotube film soaks in formic acid, 140 DEG C of-150 DEG C of thermal treatments, obtains first acid-treated PEDOT:PSS/ kaolin nanotube matrix material.
4. the preparation method of PEDOT:PSS/ kaolin nanotube matrix material as claimed in claim 3, is characterized in that, kaolin nanotube size-grade distribution 1-2 μm, external diameter 50-60nm, internal diameter 20-30nm.
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