CN101955665A - Method for preparing composite material of polypyrrole granules and titanium dioxide nanotube array - Google Patents
Method for preparing composite material of polypyrrole granules and titanium dioxide nanotube array Download PDFInfo
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- CN101955665A CN101955665A CN2010102558601A CN201010255860A CN101955665A CN 101955665 A CN101955665 A CN 101955665A CN 2010102558601 A CN2010102558601 A CN 2010102558601A CN 201010255860 A CN201010255860 A CN 201010255860A CN 101955665 A CN101955665 A CN 101955665A
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Abstract
The invention discloses a method for preparing a composite material of polypyrrole granules and a titanium dioxide nanotube array. The method comprises the following steps of: (1) synthesizing a titanium dioxide nanotube array and roasting to obtain an anatase type titanium dioxide nanotube array; and (2) electrochemically polymerizing the roasted titanium dioxide nanotube array as a working electrode and a platinum electrode as an auxiliary electrode for 15-120 min under the condition of controlling the voltage to be 0.8-1.0V in an aqueous solution consisting of sodium dodecyl benzene sulfonate and pyrrole monomers to obtain a finished product of the composite material of the polypyrrole granules and the titanium dioxide nanotube array. In the invention, the nano polypyrrole granules are loaded on the titanium dioxide nanotube array by utilizing a constant potential, an implementation method is simple and convenient with the characteristics of low cost and is easy for operation, and the prepared composite material has important application in many high-tech fields such as high-performance catalysts, solar batteries, photoelectrocatalysis, and the like.
Description
Technical field
The present invention relates to the type material preparation field, the composite material and preparation method thereof of particularly a kind of polypyrrole particle and titanium dioxide nanotube array.
Background technology
Conductive polymers, for example polypyrrole, Polythiophene, polyaniline etc. owing to have special structure and excellent physical and chemical performance, therefore become the focus of Materials science research.Wherein, polypyrrole shows good electrical conductivity and antioxidant property owing to it has the big π bond structure of typical conjugation, and be easy to synthetic and advantages such as doping, make its polymer materials as hot topic, all being widely used in fields such as electrode materials, transmitter, solar cell, ultracapacitors, is one of present conducting polymer research field research direction of greatest concern.
Polypyrrole nano structure (nano particle, rod, pipe, fiber etc.) can be obtained by microemulsion polymerization method, interfacial polymerization and electrochemical polymerization method, also can in the presence of template, tensio-active agent or ionic liquid, be polymerized, the synthetic polypyrrole nano structure has the advantage of low-dimension nano material and conductive polymers concurrently like this, and both synergistic effects make electrochemical signals amplification, the electro catalytic activity of electrode can improve 2～4 orders of magnitude.Detection limit is the highest to promote 50,000 times; The polypyrrole nano biological sensor shows wide application prospect in fields such as biomedical engineering, clinical diagnosis, environmental monitoring, food sanitation and science, is an important research focus.
TiO
2(titanium dioxide) is with respect to other semiconductor materials, have higher thermostability and photochemical stability, compare with the TiO2 material of other forms, it has stronger adsorptive power and bigger specific surface area, thereby has very wide application prospect in photocatalysis field.But TiO
2There are some defectives in actual applications in semiconductor light-catalyst, and as greater band gap (Eg=3.2V), light absorption wavelength mainly is confined to the ultraviolet region, and is low to the absorption rate of solar energy; The recombination rate height of semiconductor carriers, quantum yield is lower, so need be to TiO
2Material is modified, and improves its utilization ratio to sunlight.
Can't provide in the prior art a kind of need not sputtering technology, easy to operate utilize the polypyrrole particle to titanium dioxide nanotube array modify, with the preparation method of synthetic composite material.
Summary of the invention
In view of this, the invention provides the composite material and preparation method thereof of a kind of polypyrrole particle and titanium dioxide nanotube array, present method is polymerization face with the electrode, need not sputtering technology, method is easy, and is with low cost, and the matrix material that synthesizes is with a wide range of applications.
The objective of the invention is to be achieved through the following technical solutions:
The composite material and preparation method thereof of this polypyrrole particle and titanium dioxide nanotube array may further comprise the steps:
1) synthesis of titanium dioxide nanotube array, and obtain the anatase titanium dioxide nanotube array through roasting;
2) in the aqueous solution of forming by Sodium dodecylbenzene sulfonate and pyrrole monomer, with the titanium dioxide nanotube array after the roasting as working electrode, platinum electrode is as supporting electrode, control voltage electrochemical polymerization 15～120min under the condition of 0.8～1.0V, obtain the composite finished product of polypyrrole particle and titanium dioxide nanotube array, wherein, the concentration of Sodium dodecylbenzene sulfonate in the aqueous solution is 0.05～0.15mol/L, and the concentration of pyrrole monomer in the aqueous solution is 0.05～0.1mol/L.
Further, in step 1), the synthetic of described titanium dioxide nanotube array may further comprise the steps:
(a) titanium foil sheet being put into successively mass percent concentration is 15～30% hydrochloric acid, dehydrated alcohol, distilled water, carries out ultrasonic cleaning respectively, removes its oxide on surface;
(b) titanium foil sheet after cleaning is dried is as anode, platinized platinum places the HF solution of 0.16～0.20M as negative electrode, normal-temperature reaction 1～2h under the voltage of 20～25V, taking-up cleans up with distilled water immediately then, forms the amorphous titanium dioxide nanotube array by this step;
Further, in step 1), described roasting is meant the amorphous titanium dioxide nanotube array roasting 1～2h in nitrogen or air atmosphere that will obtain by synthesis step (b), maturing temperature is 400～600 ℃, optimizing temperature is 400～450 ℃, obtains the anatase titanium dioxide nanotube array;
Further, in roasting process, maturing temperature is 400～450 ℃;
Further, in step (a), the purity of titanium foil sheet is more than or equal to 99.6%.
The invention has the beneficial effects as follows:
1. the present invention proposes a kind of constant potential loaded with nano polypyrrole particulate method on titanium dioxide nanotube array of utilizing, its implementation method is easy, and is with low cost, easy handling;
2. the present invention uses the nanometer polypyrrole particle to come titanium dioxide nanotube array is modified, and gives full play to the advantage of two kinds of nano materials, utilizes synergy of the two and nanometer size effect effectively to improve photocatalysis performance; The matrix material that the present invention obtains possessed electrochemical response signal that the conductive polymers chemically modified electrode had big, easily observation, stable in properties, have advantage such as certain anti-interference capability, this product has important use in many high-tech areas such as transmitter, solar cell, photocatalysis technologies.
Other advantages of the present invention, target and feature will be set forth to a certain extent in the following description, and to a certain extent, based on being conspicuous to those skilled in the art, perhaps can obtain instruction from the practice of the present invention to investigating hereinafter.Target of the present invention and other advantages can realize and obtain by following specification sheets and claims.
Description of drawings
In order to make the purpose, technical solutions and advantages of the present invention clearer, the present invention is described in further detail below in conjunction with accompanying drawing, wherein:
The stereoscan photograph of the matrix material that Fig. 1 makes for embodiment 1 (the Electronic Speculum magnification is 200,000);
The stereoscan photograph of the matrix material that Fig. 2 makes for embodiment 2 (the Electronic Speculum magnification is 200,000);
The stereoscan photograph of the matrix material that Fig. 3 makes for embodiment 3 (the Electronic Speculum magnification is 100,000);
The stereoscan photograph of the matrix material that Fig. 4 makes for embodiment 4 (the Electronic Speculum magnification is 200,000);
The stereoscan photograph of the matrix material that Fig. 5 makes for embodiment 5 (the Electronic Speculum magnification is 100,000);
Fig. 6 is the infrared spectrogram of the matrix material of the present invention's preparation.
Embodiment
Hereinafter with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail.Should be appreciated that preferred embodiment only for the present invention is described, rather than in order to limit protection scope of the present invention.
Titania nanotube is a kind of existence form of nano titanium oxide, method at titanium or titanium alloy surface preparation nano-tube array has template and anonizing, in template, at first to prepare orderly alumina formwork of porous or polymer template, prepare titania nanotube by sol-gel method or electrochemical deposition method then, the main drawback of this method is that the titania nanotube form of complex process and preparation depends on template, anonizing is relatively simple, can directly form nano-tube array on the titanium surface.
In following examples of the present invention, all be, but do not get rid of the possibility of using other synthetic method synthetic titania nanotubes in the present invention, to use by anonizing synthesis of titanium dioxide nanotube array.The scanning electron microscope that adopts in the present embodiment is the thermal field pistol electron microscope that U.S. FEI Co. produces, and model is FEI Nova400FEG-SEM.
Embodiment one
1) adopt anonizing synthesis of titanium dioxide nanotube array, and obtain the anatase titanium dioxide nanotube array, specifically may further comprise the steps through roasting:
(a) select for use purity more than or equal to 99.6% titanium foil sheet, after the oxide compound on surface is removed in the abrasive paper for metallograph polishing, put into hydrochloric acid (mass percent concentration is 15～30%), dehydrated alcohol, distilled water successively, difference ultrasonic cleaning 10min is with further removal oxide on surface;
(b) titanium foil sheet after cleaning is dried is as anode, and platinized platinum places the HF solution of 0.17M as negative electrode, and normal-temperature reaction 1.5h under the voltage of 23V takes out then and cleans up with distilled water immediately, forms the amorphous titanium dioxide nanotube array by this step.
(c) amorphous titanium dioxide nanotube array roasting 1h in nitrogen atmosphere that will obtain by step (b), maturing temperature is 400 ℃, obtains the anatase titanium dioxide nanotube array.
2) be in the aqueous solution of Sodium dodecylbenzene sulfonate and pyrrole monomer in solution composition, with the titanium dioxide nanotube array after the roasting as working electrode, platinum electrode is as supporting electrode, control voltage electrochemical polymerization 25min under the condition of 1.0V, obtain the composite finished product of polypyrrole and titanium dioxide nanotube array, its concrete form as shown in Figure 1.In the present embodiment, the concentration of Sodium dodecylbenzene sulfonate in the aqueous solution is 0.10mol/L, and the concentration of pyrrole monomer in the aqueous solution is 0.10mol/L.
Embodiment two
(a) select for use purity more than or equal to 99.6% titanium foil sheet, after the oxide compound on surface is removed in the abrasive paper for metallograph polishing, put into hydrochloric acid (mass percent concentration is 15～30%), dehydrated alcohol, distilled water successively, difference ultrasonic cleaning 12min is with further removal oxide on surface;
(b) titanium foil sheet after cleaning is dried is as anode, and platinized platinum places the HF solution of 0.17M as negative electrode, and normal-temperature reaction 1h under the voltage of 25V takes out then and cleans up with distilled water immediately, forms the amorphous titanium dioxide nanotube array by this step.
(c) amorphous titanium dioxide nanotube array roasting 1.2h in nitrogen atmosphere that will obtain by step (b), maturing temperature is 450 ℃, obtains the anatase titanium dioxide nanotube array.
2) be in the aqueous solution of Sodium dodecylbenzene sulfonate and pyrrole monomer in solution composition, with the titanium dioxide nanotube array after the roasting as working electrode, platinum electrode is as supporting electrode, control voltage electrochemical polymerization 25min under the condition of 1.0V, obtain the composite finished product of polypyrrole and titanium dioxide nanotube array, its concrete form as shown in Figure 2.In the present embodiment, the concentration of Sodium dodecylbenzene sulfonate in the aqueous solution is 0.1mol/L, and the concentration of pyrrole monomer in the aqueous solution is 0.05mol/L.
Embodiment three
(a) select for use purity more than or equal to 99.6% titanium foil sheet, after the oxide compound on surface is removed in the abrasive paper for metallograph polishing, put into hydrochloric acid (mass percent concentration is 15～30%), dehydrated alcohol, distilled water successively, difference ultrasonic cleaning 15min is with further removal oxide on surface;
(b) titanium foil sheet after cleaning is dried is as anode, and platinized platinum places the HF solution of 0.17M as negative electrode, and normal-temperature reaction 1.5h under the voltage of 20V takes out then and cleans up with distilled water immediately, forms the amorphous titanium dioxide nanotube array by this step.
(c) amorphous titanium dioxide nanotube array roasting 1.5h in air atmosphere that will obtain by step (b), maturing temperature is 450 ℃, obtains the anatase titanium dioxide nanotube array.
2) be in the aqueous solution of Sodium dodecylbenzene sulfonate and pyrrole monomer in solution composition, with the titanium dioxide nanotube array after the roasting as working electrode, platinum electrode is as supporting electrode, control voltage electrochemical polymerization 15min under the condition of 1.0V, obtain the composite finished product of polypyrrole and titanium dioxide nanotube array, its concrete form as shown in Figure 3.In the present embodiment, the concentration of Sodium dodecylbenzene sulfonate in the aqueous solution is 0.05mol/L, and the concentration of pyrrole monomer in the aqueous solution is 0.05mol/L.
Embodiment four
(a) select for use purity more than or equal to 99.6% titanium foil sheet, after the oxide compound on surface is removed in the abrasive paper for metallograph polishing, put into hydrochloric acid (mass percent concentration is 15～30%), dehydrated alcohol, distilled water successively, difference ultrasonic cleaning 10min is with further removal oxide on surface;
(b) titanium foil sheet after cleaning is dried is as anode, and platinized platinum places the HF solution of 0.16M as negative electrode, and normal-temperature reaction 1.5h under the voltage of 20V takes out then and cleans up with distilled water immediately, forms the amorphous titanium dioxide nanotube array by this step.
(c) amorphous titanium dioxide nanotube array roasting 1h in air atmosphere that will obtain by step (b), maturing temperature is 500 ℃, obtains the anatase titanium dioxide nanotube array.
2) be in the aqueous solution of Sodium dodecylbenzene sulfonate and pyrrole monomer in solution composition, with the titanium dioxide nanotube array after the roasting as working electrode, platinum electrode is as supporting electrode, control voltage electrochemical polymerization 60min under the condition of 1.0V, obtain the composite finished product of polypyrrole and titanium dioxide nanotube array, its concrete form as shown in Figure 4.In the present embodiment, the concentration of Sodium dodecylbenzene sulfonate in the aqueous solution is 0.10mol/L, and the concentration of pyrrole monomer in the aqueous solution is 0.10mol/L.
Embodiment five
(a) select for use purity more than or equal to 99.6% titanium foil sheet, after the oxide compound on surface is removed in the abrasive paper for metallograph polishing, put into hydrochloric acid (mass percent concentration is 15～30%), dehydrated alcohol, distilled water successively, difference ultrasonic cleaning 10min is with further removal oxide on surface;
(b) titanium foil sheet after cleaning is dried is as anode, and platinized platinum places the HF solution of 0.20M as negative electrode, and normal-temperature reaction 2h under the voltage of 25V takes out then and cleans up with distilled water immediately, forms the amorphous titanium dioxide nanotube array by this step.
(c) amorphous titanium dioxide nanotube array roasting 2h in air atmosphere that will obtain by step (b), maturing temperature is 600 ℃, obtains the anatase titanium dioxide nanotube array.
2) be in the aqueous solution of Sodium dodecylbenzene sulfonate and pyrrole monomer in solution composition, with the titanium dioxide nanotube array after the roasting as working electrode, platinum electrode is as supporting electrode, control voltage electrochemical polymerization 120min under the condition of 0.8V, obtain the composite finished product of polypyrrole and titanium dioxide nanotube array, its concrete form as shown in Figure 5.In the present embodiment, the concentration of Sodium dodecylbenzene sulfonate in the aqueous solution is 0.15mol/L, and the concentration of pyrrole monomer in the aqueous solution is 0.05mol/L.
In above embodiment,, can find to have linear relationship between the concentration of the concentration of polypyrrole particulate size and basic benzene sulfonic acid sodium salt and pyrrole monomer according to the difference of concentration.
Fig. 6 for by embodiment (five) make the polypyrrole particle and the matrix material infrared spectrogram of titanium dioxide nanotube array.By on the figure as can be known, 1533.4,1456 and 1109cm
-1Near absorption peak has all appearred, they all are the eigen vibration absorption peaks of polypyrrole ring.Wherein, at 1533.4cm
-1Near absorption peak be that asymmetric stretching vibration by the polypyrrole ring causes, at 1456cm
-1Near absorption peak causes that by its symmetrical stretching vibration pyrrole ring was not damaged when polymerization was described. at 1109cm
-1What the place occurred is polypyrrole ring C-H characteristic peak, and near 3446cm-1 is the N-H stretching vibration peak, and 1653cm-1 is the stretching vibration of the two keys of pyrrole ring C=C, and 1635cm-1 may be the residual moisture in the KBr powder.
The polypyrrole particle of the present invention's preparation and the matrix material of titanium dioxide nanotube array have wide application in following at least field:
1) solar cell: the polypyrrole particle of the present invention's preparation and the matrix material of titanium dioxide nanotube array, contact area with bigger polypyrrole and titanium dioxide nanotube array, and polypyrrole has intensive to absorb in visible and near-infrared region, therefore make the hole mobile material of solid solar battery of polypyrrole, be hopeful to replace the optoelectronic pole of dyestuff decorated nanometer titanium dioxide with the preparation solar cell.Compare and generally acknowledge the best dyestuff RuL2 (SCN) 2 of effect, the preparation process of polypyrrole is fairly simple, and ruthenium is a rare metal, and price is expensive, and the source is relatively more difficult again;
2) transmitter manufacturing: the electroconductibility of polypyrrole depends on parameters such as molecular chain structure, polymerization methods, and polypyrrole has good biocompatibility, so can be used as electrochemistry type transmitter at this synthetic matrix material, detect the electrochemical behaviors on this kind composite electrode such as CO2, H+, Dopamine HCL.
3) catalysis technique aspect: in making the spectral response of matrix material widen visible region with polypyrrole modifying, can also improve the separation efficiency of photogenerated charge, thereby make matrix material show good opto-electronic conversion performance, make full use of sunlight photocatalysis degradation tropeolin-D, phenol, waste water from dyestuff etc.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from the aim and the scope of the technical program, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (5)
1. the composite material and preparation method thereof of polypyrrole particle and titanium dioxide nanotube array is characterized in that: may further comprise the steps:
1) synthesis of titanium dioxide nanotube array, and obtain the anatase titanium dioxide nanotube array through roasting;
2) in the aqueous solution of forming by Sodium dodecylbenzene sulfonate and pyrrole monomer, with the titanium dioxide nanotube array after the roasting as working electrode, platinum electrode is as supporting electrode, control voltage electrochemical polymerization 15～120min under the condition of 0.8～1.0V, obtain the composite finished product of polypyrrole particle and titanium dioxide nanotube array, wherein, the concentration of Sodium dodecylbenzene sulfonate in the aqueous solution is 0.05～0.15mol/L, and the concentration of pyrrole monomer in the aqueous solution is 0.05～0.1mol/L.
2. the composite material and preparation method thereof of polypyrrole particle according to claim 1 and titanium dioxide nanotube array is characterized in that: in step 1, the synthetic of described titanium dioxide nanotube array may further comprise the steps:
(a) titanium foil sheet being put into successively mass percent concentration is 15～30% hydrochloric acid, dehydrated alcohol, distilled water, carries out ultrasonic cleaning respectively, removes its oxide on surface;
(b) titanium foil sheet after cleaning is dried is as anode, platinized platinum places the HF solution of 0.16～0.20M as negative electrode, normal-temperature reaction 1～2h under the voltage of 20～25V takes out with distilled water then and cleans up, and forms the amorphous titanium dioxide nanotube array by this step.
3. the composite material and preparation method thereof of polypyrrole particle according to claim 1 and 2 and titanium dioxide nanotube array, it is characterized in that: in step 1), described roasting is meant the amorphous titanium dioxide nanotube array roasting 1～2h in nitrogen or air atmosphere that will obtain by synthesis step (b), maturing temperature is 400～600 ℃, obtains the anatase titanium dioxide nanotube array.
4. the composite material and preparation method thereof of polypyrrole particle according to claim 3 and titanium dioxide nanotube array is characterized in that: in roasting process, maturing temperature is 400～450 ℃.
5. the composite material and preparation method thereof of polypyrrole particle according to claim 2 and titanium dioxide nanotube array is characterized in that: in step (a), the purity of titanium foil sheet is more than or equal to 99.6%.
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| CN102350317A (en) * | 2011-07-04 | 2012-02-15 | 西安交通大学苏州研究院 | Polypyrrole/titanium dioxide composite adsorbent, its preparation, application and regeneration methods |
| CN102505124A (en) * | 2011-11-16 | 2012-06-20 | 东南大学 | Polypyrrole nanocolumn embedded nanoporous array material, preparation method thereof and energy storage application thereof |
| CN102941124A (en) * | 2012-11-21 | 2013-02-27 | 江南大学 | Visible-light reaction polypyrrole/Bi2WO6 composite catalyst and preparation method thereof |
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| CN102350317B (en) * | 2011-07-04 | 2013-07-31 | 西安交通大学苏州研究院 | Polypyrrole/titanium dioxide composite adsorbent, its preparation, application and regeneration methods |
| CN102350317A (en) * | 2011-07-04 | 2012-02-15 | 西安交通大学苏州研究院 | Polypyrrole/titanium dioxide composite adsorbent, its preparation, application and regeneration methods |
| CN102505124A (en) * | 2011-11-16 | 2012-06-20 | 东南大学 | Polypyrrole nanocolumn embedded nanoporous array material, preparation method thereof and energy storage application thereof |
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| CN105845904A (en) * | 2016-04-01 | 2016-08-10 | 中南大学 | Metal oxide/polypyrrole hollow nanotube negative electrode composite material for sodium ion battery and preparation method for composite material |
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| CN106283099A (en) * | 2016-08-25 | 2017-01-04 | 岭南师范学院 | A kind of surfactant assist in electrodeposition synthesizing anatase type titanium dioxide and the method for manganese dioxide nano-composite material and application thereof |
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Application publication date: 20110126 |