CN103923335A - PEDOT : PSS/kaolin nanotube composite materials and manufacturing method thereof - Google Patents
PEDOT : PSS/kaolin nanotube composite materials and manufacturing method thereof Download PDFInfo
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- CN103923335A CN103923335A CN201410192249.7A CN201410192249A CN103923335A CN 103923335 A CN103923335 A CN 103923335A CN 201410192249 A CN201410192249 A CN 201410192249A CN 103923335 A CN103923335 A CN 103923335A
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Abstract
The invention relates to the field of conducting type nanocomposite with holes and discloses conductive macromolecule/kaolin nanotube (HNTs) composite materials and a manufacturing method thereof. The composite materials are obtained by combination of conductive macromolecule PEDOT : PSS and non-conductive kaolin nanotubes, and the weight of the kaolin nanotubes is 43.5%-79.4% of the total weight of the composite materials. Raw materials are easy to obtain, operation is easy, the conductivity of the composite materials is high, the specific surface area is large, different advantages of organic materials and inorganic materials are achieved, the features of nano materials are achieved, and advantage complementing is fully achieved. The PEDOT : PSS/kaolin nanotube composite materials have great application prospect in fields such as thermoelectricity, capacitors and electromagnetic waves.
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, not only there is the optical characteristics of metal and semiconductor material but also had mechanical property that polymkeric substance is good and the macromolecule conducting material of workability has caused 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 unique mechanism of doping effect, makes it become the good conductive polymers of application prospect.
[nano composite material taking kaolin nanotube as representative has caused researchist's very big concern with its unique structure and performance.Kaolin is a kind of aluminium silicate salt mineral of natural formation, being mainly hollow laminate structure, being 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, high temperature resistant, acidproof, insulation, length is at 1-2 μ m, external diameter 50 nm left and right, internal diameter 20-30nm.Kaolin nanotube is doped in PEDOT:PSS dispersion liquid, PEDOT:PSSS and kaolin are carried out compound, preparation PEDOT:PSS/HNTs matrix material, for this area provides a kind of novel conductive material, exploitation to kaolin nanotube and the development of conducting polymer materials are significant, have no at present relevant report.
Summary of the invention
The present invention aims to provide the new PE DOT:PSS/ kaolin nanotube matrix material that a kind of electrical efficiency is high, makes the different advantages of its existing organic and inorganic materials, has again the characteristic of nano material, realizes and 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 the kaolin nanotube and compound the obtaining of PEDOT:PSS with high conductivity by tubular structure,
Wherein kaolin nanotube quality is the 43.5-79.4% of matrix material total mass.
Be PEDOT:PSS/HNTs matrix material hereinafter to be referred 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 mixes it;
(2) above-mentioned dispersant liquid drop is added on PET film, 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, and 140 DEG C of-150 DEG C of thermal treatments, obtain 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 μ m, external diameter 50-60 nm, internal diameter 20-30nm.
Innovative point of the present invention is: conducting polymer PEDOT:PSS and nonconducting kaolin nanotube are carried out compound, inquired in matrix material and added kaolin content to its specific conductivity impact.
The invention has the beneficial effects as follows: raw material is easy to get, component proportion is easily controlled, preparation technology is simple to operation, and the kaolin nanotube in matrix material has pore space structure, compound with PEDOT:PSS after, improve the specific conductivity of material, increase the specific surface area of matrix material, optimized the Electromagnetic performance of material, the different advantages of existing organic and inorganic materials, there is again the characteristic of nano material, fully realized mutual supplement with each other's advantages.Be expected at hertzian wave, suitability for industrialized production and widespread use are realized in the fields such as thermoelectricity, ultracapacitor.
Brief description of the drawings
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 of the present invention cross section under 20000 times.
Figure 11 is the scanning electron microscope (SEM) photograph of PEDOT:PSS/HNTs matrix material of the present invention cross section 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 mono-
By 1.42g kaolin nanotube (the long 1-2 μ of size-grade distribution m, external diameter 50 nm left and right, internal diameter 20-30nm) be doped in 1.1402g PEDOT:PSS dispersion liquid, rapid stirring 24h, obtain obtaining uniform dispersion A, dispersion liquid A is added drop-wise on 2cm × 2cm PET film to 50 DEG C of heating 1h, 120 DEG C of heating 15min.The electric conductivity that adopts four probe method to record this nano composite material is 0.23 S.cm
-1.Above-mentioned matrix material is soaked to 10 min in formic acid, then 140 DEG C of thermal treatment 5min, the specific conductivity that records the nano composite material of formic acid immersion is 256.7 S.cm
-1.Specific surface area is
81.05 m 2 / g.Kaolin nanotube quality is 43.5 % of matrix material total mass.
Starting material PEDOT:PSS specific conductivity is 0.17 S.cm
-1.
Embodiment bis-
By 1.1402g kaolin nanotube (size-grade distribution 1-2 μ m, external diameter 50 nm left and right, internal diameter 20-30nm) be doped in 1.1402g PEDOT:PSS dispersion liquid, rapid stirring 24h, obtain obtaining uniform dispersion A, dispersion liquid A is added drop-wise on 2cm × 2cm PET film to 60 DEG C of heating 1h, 130 DEG C of heating 15min.The electric conductivity that adopts four probe method to record this nano composite material is 0.34 S.cm
-1.Above-mentioned matrix material is soaked to 10 min in formic acid, then 140 DEG C of thermal treatment 5min, the specific conductivity that records the nano composite material of formic acid immersion is 211.4 S.cm
-1.Specific surface area is
81.05 m 2 / g.Kaolin nanotube quality is 60.1 % of matrix material total mass.
Starting material PEDOT:PSS specific conductivity is 0.17 S.cm
-1.
Embodiment tri-
0.5701g kaolin nanotube is doped in 1.1402g PEDOT:PSS dispersion liquid, and rapid stirring 24h, obtains obtaining uniform dispersion A, dispersion liquid A is added drop-wise on 2cm × 2cmPET film to 50 DEG C of heating 1h, 130 DEG C of heating 15min.The electric conductivity that adopts four probe method to record this nano composite material is 0.51 S.cm
-1.Above-mentioned matrix material is soaked to 10 min in formic acid, then 150 DEG C of thermal treatment 5min, the specific conductivity that records the nano composite material of formic acid immersion is 70.1 S.cm
-1.Specific surface area is
81.05 m 2 / g.Kaolin nanotube quality is 69.8% of matrix material total mass.
Starting material PEDOT:PSS specific conductivity is 0.17 S.cm
-1.
Embodiment tetra-
0.38g kaolin nanotube is doped in 1.1402g PEDOT:PSS dispersion liquid, and rapid stirring 24h, obtains obtaining uniform dispersion A, dispersion liquid A is added drop-wise on 2cm × 2cm PET film to 60 DEG C of heating 1h, 120 DEG C of heating 15min.The electric conductivity that adopts four probe method to record this nano composite material is 0.57 S.cm
-1.Above-mentioned matrix material is soaked to 10 min in formic acid, then 150 DEG C of thermal treatment 5min, the specific conductivity that records the nano composite material of formic acid immersion is 40.3 S.cm
-1.Specific surface area is
81.05 m 2 / g.Kaolin nanotube quality is 75.5% of matrix material total mass.
Starting material PEDOT:PSS specific conductivity is 0.17 S.cm
-1.
Embodiment five
0.3167g kaolin nanotube is doped in 1.1402g PEDOT:PSS dispersion liquid, and rapid stirring 24h, obtains obtaining uniform dispersion A, dispersion liquid A is added drop-wise on 2cm × 2cm PET film to 60 DEG C of heating 1h, 130 DEG C of heating 15min.The electric conductivity that adopts four probe method to record this nano composite material is 0.26 S.cm
-1.Above-mentioned matrix material is soaked to 10 min in formic acid, then 150 DEG C of thermal treatment 5min, the specific conductivity that records the nano composite material of formic acid immersion is 22.2 S.cm
-1.Specific surface area is
81.05 m 2 / g.Kaolin nanotube quality is 79.4 % of matrix material total mass.
Starting material PEDOT:PSS specific conductivity is 0.17 S.cm
-1.
Claims (5)
1.PEDOT:PSS/ kaolin nanotube matrix material, is characterized in that, this nano composite material is by kaolin nanotube and PEDOT:PSS compound obtaining by the following method:
(1) first kaolin nanotube is dispersed in PEDOT:PSS dispersion liquid, stirring at room temperature, mixes it;
(2) above-mentioned dispersant liquid drop is added to PET above, 50 DEG C of-60 DEG C of heating, 120 DEG C of-130 DEG C of thermal treatments, obtain PEDOT:PSS/ kaolin nanotube film;
(3) PEDOT:PSS/ kaolin nanotube film soaks in formic acid, and 140 DEG C of-150 DEG C of thermal treatments, obtain the acid-treated PEDOT:PSS/ kaolin nanotube of first 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 μ m, external diameter 50-60 nm, internal diameter 20-30nm.
3. the method for the PEDOT:PSS/ kaolin nanotube matrix material described in preparation claim 1 or 2, is characterized in that, realizes as follows:
(1) first kaolin nanotube is dispersed in PEDOT:PSS dispersion liquid, stirring at room temperature, mixes it;
(2) above-mentioned dispersant liquid drop is added to PET above, 50 DEG C of-60 DEG C of heating, 120 DEG C of-130 DEG C of thermal treatments, obtain PEDOT:PSS/ kaolin nanotube film;
(3) PEDOT:PSS/ kaolin nanotube film soaks in formic acid, and 140 DEG C of-150 DEG C of thermal treatments, obtain the acid-treated PEDOT:PSS/ kaolin nanotube of first matrix material.
4. the method for preparation PEDOT:PSS/ kaolin nanotube matrix material claimed in claim 3, is characterized in that, kaolin nanotube and PEDOT:PSS weight ratio are 1:0.77--1:3.85.
5. the method for the PEDOT:PSS/ kaolin nanotube matrix material described in preparation claim 3 or 4, is characterized in that kaolin nanotube size-grade distribution 1-2 μ m, external diameter 50-60nm, internal diameter 20-30nm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744895A (en) * | 2014-09-24 | 2015-07-01 | 郑州大学 | Conductive polymer and halloysite nanotube composite wave-absorbing material and preparation method thereof |
| CN109036850A (en) * | 2018-07-27 | 2018-12-18 | 湖南艾华集团股份有限公司 | solid electrolyte, solid electrolyte preparation method and solid capacitor |
| WO2021060322A1 (en) * | 2019-09-26 | 2021-04-01 | 日本製紙株式会社 | Non-aqueous electrolyte secondary cell binder, non-aqueous electrolyte secondary cell electrode composition, non-aqueous electrolyte secondary cell electrode, and non-aqueous electrolyte secondary cell |
| CN113045935A (en) * | 2019-12-26 | 2021-06-29 | 武汉理工大学 | High-thermal-stability conductive ink applied to flexible circuit and preparation method thereof |
| CN113277784A (en) * | 2020-07-14 | 2021-08-20 | 李焕醒 | Pumice concrete with electromagnetic wave absorption function |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011238871A (en) * | 2010-05-13 | 2011-11-24 | Oike Ind Co Ltd | Organic thin film electrode |
| CN102621206A (en) * | 2012-04-19 | 2012-08-01 | 江西科技师范学院 | Method for preparing poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) (PEDOT:PSS) composite modified electrode |
| CN102876040A (en) * | 2012-10-08 | 2013-01-16 | 合肥杰事杰新材料股份有限公司 | Polyphenylene sulfide composite material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011238871A (en) * | 2010-05-13 | 2011-11-24 | Oike Ind Co Ltd | Organic thin film electrode |
| CN102621206A (en) * | 2012-04-19 | 2012-08-01 | 江西科技师范学院 | Method for preparing poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) (PEDOT:PSS) composite modified electrode |
| CN102876040A (en) * | 2012-10-08 | 2013-01-16 | 合肥杰事杰新材料股份有限公司 | Polyphenylene sulfide composite material and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744895A (en) * | 2014-09-24 | 2015-07-01 | 郑州大学 | Conductive polymer and halloysite nanotube composite wave-absorbing material and preparation method thereof |
| CN109036850A (en) * | 2018-07-27 | 2018-12-18 | 湖南艾华集团股份有限公司 | solid electrolyte, solid electrolyte preparation method and solid capacitor |
| WO2021060322A1 (en) * | 2019-09-26 | 2021-04-01 | 日本製紙株式会社 | Non-aqueous electrolyte secondary cell binder, non-aqueous electrolyte secondary cell electrode composition, non-aqueous electrolyte secondary cell electrode, and non-aqueous electrolyte secondary cell |
| CN113045935A (en) * | 2019-12-26 | 2021-06-29 | 武汉理工大学 | High-thermal-stability conductive ink applied to flexible circuit and preparation method thereof |
| CN113277784A (en) * | 2020-07-14 | 2021-08-20 | 李焕醒 | Pumice concrete with electromagnetic wave absorption function |
| CN113277784B (en) * | 2020-07-14 | 2023-04-14 | 苏州鱼得水电气科技有限公司 | Pumice concrete with electromagnetic wave absorption function |
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