CN103319740A - Fast assembly method of Ag/PPy nanocomposite films - Google Patents

Fast assembly method of Ag/PPy nanocomposite films Download PDF

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Publication number
CN103319740A
CN103319740A CN201310303151XA CN201310303151A CN103319740A CN 103319740 A CN103319740 A CN 103319740A CN 201310303151X A CN201310303151X A CN 201310303151XA CN 201310303151 A CN201310303151 A CN 201310303151A CN 103319740 A CN103319740 A CN 103319740A
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substrate
ppy
assembling
film
ultrasonic
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CN103319740B (en
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缪晓莉
陈新
赵崇军
曹红亮
钱秀珍
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East China University of Science and Technology
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East China University of Science and Technology
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Abstract

The invention discloses a fast assembly method of Ag/PPy nanocomposite films on different substrates by the utilization of ultrasound and centrifugal force. The fast assembly method comprises the following steps: carrying out ultrasonic treatment on a reaction solution containing AgNO3 and pyrroles, standing in a dark place, and centrifuging by transferring the reaction solution into a centrifuge tube which is provided with a substrate beforehand. Thus, Ag/PPy nanocomposite particles undergo fast assembly for film forming. The method provided by the invention has advantages of simple process, easy operation and low cost. The prepared Ag/PPy nanocomposite film is uniform and complete and has good binding force with the substrate.

Description

A kind of method of rapid-assembling Ag/PPy nano compound film
Technical field
The present invention relates to a kind of method of rapid-assembling Ag/PPy nano compound film, be specifically related to utilize ultrasonic simplification reaction system and assemble the speed of film forming and the method for efficient at the auxiliary lower Ag/PPy of the raising Nano composite granules of centrifugal force at substrate.
Background technology
Polypyrrole (PPy) has good electroconductibility, oxidation-reduction quality, biocompatibility and environmental stability.And the Ag of nanoscale has the special optics and the catalytic performance that are determined by its shape and size.Both compound Ag/PPy nano composite materials that obtain, because synergy, physics, chemical property all make moderate progress, and huge potential using value is all being arranged aspect catalysis, biosensor, microelectronic device, the sensor.
Up to the present, had several different methods to prepare the Ag/PPy nano composite material, but large many body system is complicated, tend to add various oxygenants, reductive agent, and polyvinylpyrrolidone commonly used (PVP) is as stablizer.And ultrasonic water or some organic additives decomposition generation free radical of making can be directly as reductive agent, and product there is certain dissemination [Jin Ho Bang, Kenneth S. Suslick, Applications of Ultrasound to the Synthesis of Nanostructured Materials, Adv. Mater. 22 (2010) 1039-1059].Yet, not yet have and utilize the ultrasonic report that reaction system obtains Ag/PPy nano composite material this respect of simplifying.
The formation film is the prerequisite in the material devices process, the Ag/PPy film that utilizes the volatilization of solvent to obtain self-supporting is a kind of simple method, but, solvent evaporates is very consuming time, and the Ag/PPy film of self-supporting is frangible, bad mechanical property, and directly adding substrate, the Ag/PPy film is combined not tight with substrate.
Summary of the invention
Purpose of the present invention is intended to propose a kind of simply and effectively method of rapid-assembling Ag/PPy nano compound film, in order to effectively simplify reaction system, solve that the Ag/PPy self-supporting film is frangible, bad mechanical property, be combined the problem such as not tight with substrate and directly add substrate Ag/PPy film.The ultimate principle that the present invention is based on is: ultrasonicly make solvent (water or dimethyl formamide (DMF)) in the reaction system resolve into free radical can directly to promote AgNO as reductive agent 3And the reaction between the pyrroles, and product there is certain dissemination; Exist certain electrostatic attraction effect between Ag/PPy Nano composite granules and the substrate; can make particle assemble film forming at substrate; the booster action of centrifugal force is, particle can move along its direction has increased chance with substrate contact, thereby has improved speed and the efficient of self assembling process.
Preparation method of the present invention comprises the steps:
(1) with a certain amount of AgNO 3Be dissolved in the solvent of appropriate amount with the pyrroles;
(2) mixing solutions of (1) carried out supersound process;
(3) can place the dark place to leave standstill mentioned solution, can control dwell temperature and time of repose;
(4) step (2) or (3) gained solution are moved in the centrifuge tube, be placed with substrate in the centrifuge tube, carry out centrifugal (can control centrifuge speed, centrifugation time, centrifuging temperature), make Ag/PPy Nano composite granules rapid-assembling film forming on substrate;
(5) step (4) gained film is cleaned, then dry.
Description of drawings
Fig. 1 presses this patent embodiment 1 described method, the digital photograph of the Ag/PPy film for preparing at the ito glass substrate.
Fig. 2 presses this patent embodiment 2 described methods, (a) SEM figure (illustration: digital photograph) of the Ag/PPy film for preparing at the ito glass substrate; (b) CV data.
Fig. 3 presses this patent embodiment 3 described methods, the SEM figure of the Ag/PPy film for preparing at the ito glass substrate.
Fig. 4 presses this patent embodiment 4 described methods, the SEM figure (illustration: digital photograph) of the Ag/PPy film for preparing in silicon chip substrate.
Fig. 5 presses this patent embodiment 5 described methods, the SEM figure of the Ag/PPy film for preparing at the ito glass substrate.
Embodiment
Embodiment 1
Such as above-mentioned step, to 5 ml mixing solutionss (0.5 M AgNO 3+ 3.6 M pyrroles, DMF are as solvent) carry out supersound process, each ultrasonic 2 s, interval 6 s carry out 60 times altogether, and upper temperature limit is 40 ℃.Then, without leaving standstill, directly auxiliary lower so that the Ag/PPy Nano composite granules is assembled film forming (centrifuge speed is 16000 rpm, and centrifugation time is 5 min, and centrifuging temperature is 25 ℃) at the ITO substrate at centrifugal force.At last, water and ethanol clean respectively, drying.The digital photograph of gained film as shown in Figure 1.The Ag/PPy film is evenly complete and good with the substrate bonding force.
Embodiment 2
Such as above-mentioned step, to 5 ml mixing solutionss (0.5 M AgNO 3+ 3.6 M pyrroles, DMF are as solvent) carry out supersound process, each ultrasonic 2 s, interval 6 s carry out 60 times altogether, and upper temperature limit is 40 ℃.Then, move to the dark place, under 5 ℃, leave standstill 24 h.Then, auxiliary lower so that the Ag/PPy Nano composite granules is assembled film forming (centrifuge speed is 16000 rpm, and centrifugation time is 5 min, and centrifuging temperature is 25 ℃) at the ITO substrate at centrifugal force.At last, water and ethanol clean respectively, drying.The digital photograph of gained film, SEM figure and CV data are as shown in Figure 2.Though the products therefrom amount is few, can after substrate assembling film forming, can repeatedly or repeat structural characterization and performance measurement, and the gained film has good chemical property.
Embodiment 3
Such as above-mentioned step, to 5 ml mixing solutionss (0.5 M AgNO 3+ 3.6 M pyrroles, DMF are as solvent) carry out supersound process, each ultrasonic 2 s, interval 6 s carry out 60 times altogether, and upper temperature limit is 40 ℃.Then, move to the dark place, (be about 25 ℃) under the envrionment temperature, leave standstill 12 h.Then, auxiliary lower so that the Ag/PPy Nano composite granules is assembled film forming (centrifuge speed is 16000 rpm, and centrifugation time is 5 min, and centrifuging temperature is 25 ℃) at the ITO substrate at centrifugal force.At last, water and ethanol clean respectively, drying.The SEM figure of gained film as shown in Figure 3.Centrifugal force plays the selection effect to the Ag/PPy Nano composite granules, so that the film forming particle size is less, shape is homogeneous comparatively.
Embodiment 4
Such as above-mentioned step, to 5 ml mixing solutionss (0.5 M AgNO 3+ 3.6 M pyrroles, DMF are as solvent) carry out supersound process, each ultrasonic 2 s, interval 6 s carry out 60 times altogether, and upper temperature limit is 40 ℃.Then, move to the dark place, under 25 ℃, leave standstill 24 h.Then, auxiliary lower so that the Ag/PPy Nano composite granules is assembled film forming (centrifuge speed is 16000 rpm, and centrifugation time is 5 min, and centrifuging temperature is 25 ℃) in silicon chip substrate at centrifugal force.At last, water and ethanol clean respectively, drying.The digital photograph of gained film and SEM figure are as shown in Figure 4.The Ag/PPy Nano composite granules also can evenly distribute on silicon chip substrate and be good with the substrate bonding force.
Embodiment 5
Such as above-mentioned step, to 5 ml mixing solutionss (0.5 M AgNO 3+ 3.6 M pyrroles, DMF are as solvent) carry out supersound process, each ultrasonic 2 s, interval 6 s carry out 300 times altogether, and upper temperature limit is 40 ℃.Without leaving standstill, directly auxiliary lower so that the Ag/PPy Nano composite granules is assembled film forming (centrifuge speed is 16000 rpm, and centrifugation time is 5 min, and centrifuging temperature is 25 ℃) at the ITO substrate at centrifugal force.At last, water and ethanol clean respectively, drying.The SEM figure of gained film becomes membrane granule evenly to distribute on substrate as shown in Figure 5.

Claims (7)

1. one kind is utilized method ultrasonic and centrifugal action rapid-assembling Ag/PPy nano compound film on substrate, comprises the steps:
With a certain amount of AgNO 3Be dissolved in the solvent of appropriate amount with the pyrroles;
Mixing solutions to (1) carries out supersound process;
Can place the dark place to leave standstill mentioned solution, can control dwell temperature and time of repose;
Step (2) or (3) gained solution are moved in the centrifuge tube, be placed with substrate in the centrifuge tube, carry out centrifugal (can control centrifuge speed, centrifugation time, centrifuging temperature), make Ag/PPy Nano composite granules rapid-assembling film forming on substrate;
Step (4) gained film is cleaned, then dry.
2. according to claim 1ly utilize method ultrasonic and centrifugal action rapid-assembling Ag/PPy nano compound film on substrate, selected solvent is water or DMF.
3. ultrasonic device according to claim 1 can comprise ultrasonic cell disruptor, Ultrasonic Cleaners etc., and the ultrasound emission source can place solution inner, also can be used on the outside of containing the solution vessel, and ultrasound mode can be with step, also available continuous mode.
4. according to claim 1ly utilize method ultrasonic and centrifugal action rapid-assembling Ag/PPy nano compound film on substrate, leave standstill in the process, the dwell temperature optimization range is 5 ℃-65 ℃, and the time of repose optimization range is 0 h-24 h.
5. according to claim 1ly utilize method ultrasonic and centrifugal action rapid-assembling Ag/PPy nano compound film on substrate, selected substrate is ito glass or silicon chip.
6. according to claim 1ly utilize method ultrasonic and centrifugal action rapid-assembling Ag/PPy nano compound film on substrate, in the centrifugal process, the centrifuge speed optimization range is 10000-16500 rpm, the centrifugation time optimization range is 5-30 min, and the centrifuging temperature optimization range is 5-25 ℃.
7. according to claim 1ly utilize method ultrasonic and centrifugal action rapid-assembling Ag/PPy nano compound film on substrate, what use when film cleaning is water or methyl alcohol, ethanol, propyl alcohol.
CN201310303151.XA 2013-07-18 2013-07-18 A kind of method of rapid-assembling Ag/PPy nano compound film Expired - Fee Related CN103319740B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110057875A (en) * 2018-01-19 2019-07-26 天津大学 Polypyrrole-tungsten oxide nucleocapsid heterogeneous structural nano stick and its preparation method and application of Argent grain modification
CN110105569A (en) * 2019-04-23 2019-08-09 太仓萃励新能源科技有限公司 A kind of silver loads the synthetic method of poly- 3,4- ethyl dioxypyrrole
CN116334948A (en) * 2023-03-03 2023-06-27 金陵科技学院 Polypyrrole/silver/cellulose composite paper-based material, and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101328314A (en) * 2007-11-21 2008-12-24 华东理工大学 Method for rapidly preparing Ag/PPy composite material
CN102120824A (en) * 2010-12-23 2011-07-13 华东理工大学 Method for preparing transparent silver halide/high-molecular composite film
CN102140249A (en) * 2010-12-23 2011-08-03 华东理工大学 Method for quickly preparing silver/polypyrrole composite sol by adopting microwave method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101328314A (en) * 2007-11-21 2008-12-24 华东理工大学 Method for rapidly preparing Ag/PPy composite material
CN102120824A (en) * 2010-12-23 2011-07-13 华东理工大学 Method for preparing transparent silver halide/high-molecular composite film
CN102140249A (en) * 2010-12-23 2011-08-03 华东理工大学 Method for quickly preparing silver/polypyrrole composite sol by adopting microwave method

Non-Patent Citations (1)

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Title
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110057875A (en) * 2018-01-19 2019-07-26 天津大学 Polypyrrole-tungsten oxide nucleocapsid heterogeneous structural nano stick and its preparation method and application of Argent grain modification
CN110105569A (en) * 2019-04-23 2019-08-09 太仓萃励新能源科技有限公司 A kind of silver loads the synthetic method of poly- 3,4- ethyl dioxypyrrole
CN116334948A (en) * 2023-03-03 2023-06-27 金陵科技学院 Polypyrrole/silver/cellulose composite paper-based material, and preparation method and application thereof
CN116334948B (en) * 2023-03-03 2024-04-19 金陵科技学院 Polypyrrole/silver/cellulose composite paper-based material, and preparation method and application thereof

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