CN109942813A - The preparation method of ordered carbon nanotube array electrode and polyaniline nano linear array - Google Patents
The preparation method of ordered carbon nanotube array electrode and polyaniline nano linear array Download PDFInfo
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- CN109942813A CN109942813A CN201910228717.4A CN201910228717A CN109942813A CN 109942813 A CN109942813 A CN 109942813A CN 201910228717 A CN201910228717 A CN 201910228717A CN 109942813 A CN109942813 A CN 109942813A
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Abstract
The present invention relates to the preparation method technical fields of orderly polyaniline nano linear array, refer in particular to the preparation method of ordered carbon nanotube array electrode and polyaniline nano linear array；The following steps are included: ordered carbon nanotube array is vertically in polytetrafluoroethylene (PTFE) circular groove, ordered carbon nanotube array is totally submerged the preparation of ordered carbon nanotube array electrode by injection epoxy resin；It vacuumizes and removes bubble and heat；Circular groove is removed, the two-sided of ordered carbon nanotube array epoxy resin of polishing exposes the pipe end on carbon pipe two sides；By the one side of disk it is gold-plated after sticked on stainless steel substrates with conductive silver glue；It is encapsulated completely along the circumference coating epoxy resin of disk and is fixed on stainless steel substrates；It is made after standing and drying；Carbon nano pipe array electrode is successively polished with after ultrasonic cleaning, in aniline monomer/perchloric acid solution, using galvanostatic method, prepares polyaniline nano linear array.
Description
Technical field
The present invention relates to the preparation method technical fields of orderly polyaniline nano linear array, refer in particular to ordered carbon nanotube array
The preparation method of electrode and polyaniline nano linear array.
Background technique
Polyaniline has synthesis simple, chemistry and thermal stability are good as a kind of typical intrinsic conducting polymers material
Feature, be widely used in the fields such as supercapacitor, gas sensor, energy stores and conversion, water process.Orderly is poly-
Aniline nano linear array can effectively reduce the adverse effects such as ion diffusion, greatly compared to unordered nano wire from structure
Improve the performance of electrode.Polyaniline nano-line prepared by chemical method, interfacial polymerization is usually interleaved with each other, and forms unordered multidimensional
Structure；Although template can prepare orderly polyaniline nano linear array, when removing removing template, polyaniline knot will cause
The destruction of structure and performance.
Summary of the invention
The purpose of the present invention is to solve the shortcomings of the prior art offer ordered carbon nanotube array electrode and polyaniline are received
The preparation method of nanowire arrays solves present in existing preparation method: forming unordered multidimensional structure, will cause structure
The defects of with the destruction of performance.
To achieve the above object, the present invention is achieved by the following technical solutions: ordered carbon nanotube array electrode
Preparation method, comprising the following steps: ordered carbon nanotube array is vertically in polytetrafluoroethylene (PTFE) circular groove, epoxy resin is injected,
Ordered carbon nanotube array is totally submerged；It vacuumizes and removes bubble and heat；Circular groove is removed, ordered carbon nanotube array of polishing
Epoxy resin it is two-sided, expose the pipe end on carbon pipe two sides；By the one side of disk it is gold-plated after with conductive silver glue stick at stainless steel substrates
On；It is encapsulated completely along the circumference coating epoxy resin of disk and is fixed on stainless steel substrates；After standing and drying, orderly carbon is made
Nanometer pipe array electrode.
The preparation method of orderly polyaniline nano linear array, comprising the following steps: 1) prepare ordered carbon nanotube array electricity
Pole；2) carbon nano pipe array electrode is successively polished with after ultrasonic cleaning, using carbon nano pipe array electrode as Electrode, is saturated
Calomel electrode is reference electrode, and platinum electrode is auxiliary electrode, the cyclic activation in sulfuric acid；3) in aniline monomer/perchloric acid solution
In, using galvanostatic method, prepare polyaniline nano linear array.
In step 2, in 0.5mol/L sulfuric acid, in -0.3V in+2.0V potential region, with 0.1V/s cyclic activation 5
Circle.
In step 3, the concentration of aniline monomer solution is 0.3-0.6mol/L, and the concentration of corresponding perchloric acid solution is 0.6-
1.2mol/L。
In step 3, the constant current time is 20-60 minutes, constant current 0.016mA.
The height of ordered carbon nanotube array is 1-10 millimeters.
The replaceable epoxy resin of phenolic resin.
Before use, being both needed to use sand paper and aluminium oxide mud grinding process, elder generation is cleaned by ultrasonic carbon nanotube electrode in ethanol,
Then it is cleaned by ultrasonic in high purity water.
It is sticked on stainless steel substrates after the one side of carbon nanotube electrode is gold-plated with conductive silver glue, and is wrapped completely with epoxy resin
Envelope.
Aniline monomer/perchloric acid solution molar concentration rate is 1:2.
The beneficial effects of the present invention are: the step of by above-mentioned preparation, orderly one-dimensional polyaniline nano can be made
Linear array.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the orderly polyaniline nano linear array of 1 gained of embodiment.
Fig. 2 is the scanning electron microscope (SEM) photograph of the orderly polyaniline nano linear array of 2 gained of embodiment.
Fig. 3 is the scanning electron microscope (SEM) photograph of the orderly polyaniline nano linear array of 3 gained of embodiment.
Specific embodiment
The present invention will be further described below with reference to the drawings.
It should be noted that experimental method described in following embodiments is unless otherwise specified conventional method, institute
Reagent and material are stated, unless otherwise specified, is commercially obtained.
Using electrochemistry step current polymerization, polyaniline can be controlled by the nucleating point distribution density of reduction polyaniline
Orderly polyaniline nano linear array is grown along one-dimensional square.
Embodiment 1:
Ordered carbon nanotube array is vertically in polytetrafluoroethylene (PTFE) circular groove, high osmosis epoxy resin (SPI- is injected
812), ordered carbon nanotube array is totally submerged；Removing bubble is vacuumized, is heated 24 hours at 60 c；Remove circle
Slot is successively polished the two-sided of ordered carbon nanotube array epoxy resin with sand paper and 0.3 micron of aluminium oxide mud respectively, exposure
The pipe end on carbon pipe two sides out；By the one side of disk it is gold-plated after sticked on stainless steel substrates with conductive silver glue；Circumference along disk applies
By it, encapsulating is fixed on stainless steel substrates epoxy resin completely；After standing and drying, ordered carbon nanotube array electrode is made.
By ordered carbon nanotube array electrode successively it is polished and ultrasonic cleaning after, with carbon nano pipe array electrode be research
Electrode, saturated calomel electrode are reference electrode, and 213 type platinum electrodes are auxiliary electrode.In 0.5mol/L sulfuric acid, in -0.3V to+
In 2.0V potential region, with the circle of 0.1V/s cyclic activation 5.Using galvanostatic method, wherein the concentration of aniline monomer solution is
0.5mol/L, the concentration of corresponding perchloric acid solution are 1mol/L, and the constant current time is 30 minutes, constant current 0.016mA.System
It is standby to obtain orderly polyaniline nano linear array, scanning electron microscope (SEM) photograph as shown in Figure 1.
Embodiment 2:
Ordered carbon nanotube array is vertically in polytetrafluoroethylene (PTFE) circular groove, high osmosis epoxy resin (SPI- is injected
812), ordered carbon nanotube array is totally submerged；Removing bubble is vacuumized, is heated 24 hours at 60 c；Remove circle
Slot is successively polished the two-sided of ordered carbon nanotube array epoxy resin with sand paper and 0.3 micron of aluminium oxide mud respectively, exposure
The pipe end on carbon pipe two sides out；By the one side of disk it is gold-plated after sticked on stainless steel substrates with conductive silver glue；Circumference along disk applies
By it, encapsulating is fixed on stainless steel substrates epoxy resin completely；After standing and drying, ordered carbon nanotube array electrode is made.
By ordered carbon nanotube array electrode successively it is polished and ultrasonic cleaning after, with carbon nano pipe array electrode be research
Electrode, saturated calomel electrode are reference electrode, and 213 type platinum electrodes are auxiliary electrode.In 0.5mol/L sulfuric acid, in -0.3V to+
In 2.0V potential region, with the circle of 0.1V/s cyclic activation 5.Using galvanostatic method, wherein the concentration of aniline monomer solution is
0.3mol/L, the concentration of corresponding perchloric acid solution are 0.6mol/L, and the constant current time is 50 minutes, constant current 0.016mA.
Orderly polyaniline nano linear array, scanning electron microscope (SEM) photograph as shown in Figure 2 is prepared.
Embodiment 3:
Ordered carbon nanotube array is vertically in polytetrafluoroethylene (PTFE) circular groove, high osmosis epoxy resin (SPI- is injected
812), ordered carbon nanotube array is totally submerged；Removing bubble is vacuumized, is heated 24 hours at 60 c；Remove circle
Slot is successively polished the two-sided of ordered carbon nanotube array epoxy resin with sand paper and 0.3 micron of aluminium oxide mud respectively, exposure
The pipe end on carbon pipe two sides out；By the one side of disk it is gold-plated after sticked on stainless steel substrates with conductive silver glue；Circumference along disk applies
By it, encapsulating is fixed on stainless steel substrates epoxy resin completely；After standing and drying, ordered carbon nanotube array electrode is made.
By ordered carbon nanotube array electrode successively it is polished and ultrasonic cleaning after, with carbon nano pipe array electrode be research
Electrode, saturated calomel electrode are reference electrode, and 213 type platinum electrodes are auxiliary electrode.In 0.5mol/L sulfuric acid, in -0.3V to+
In 2.0V potential region, with the circle of 0.1V/s cyclic activation 5.Using galvanostatic method, wherein the concentration of aniline monomer solution is
0.6mol/L, the concentration of corresponding perchloric acid solution are 1.2mol/L, and the constant current time is 20 minutes, constant current 0.016mA.
Orderly polyaniline nano linear array, scanning electron microscope (SEM) photograph as shown in Figure 3 is prepared.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (5)
1. the preparation method of ordered carbon nanotube array electrode, it is characterised in that: the following steps are included: by ordered carbon nanotube battle array
Column are vertically in polytetrafluoroethylene (PTFE) circular groove, inject epoxy resin, ordered carbon nanotube array is totally submerged；It vacuumizes except degassing
It steeps and heats；Circular groove is removed, the two-sided of ordered carbon nanotube array epoxy resin of polishing exposes the pipe end on carbon pipe two sides；It will
It is sticked on stainless steel substrates after the one side of disk is gold-plated with conductive silver glue；Circumference coating epoxy resin along disk encapsulates it completely
It is fixed on stainless steel substrates；After standing and drying, ordered carbon nanotube array electrode is made.
2. the preparation method of orderly polyaniline nano linear array, it is characterised in that: the following steps are included: 1) preparing organized carbon nano
Pipe array electrode；2) carbon nano pipe array electrode successively it is polished and ultrasonic cleaning after, with carbon nano pipe array electrode be research
Electrode, saturated calomel electrode are reference electrode, and platinum electrode is auxiliary electrode, the cyclic activation in sulfuric acid；3) in aniline monomer/height
In solution chlorate, using galvanostatic method, polyaniline nano linear array is prepared.
3. the preparation method of orderly polyaniline nano linear array according to claim 2, it is characterised in that: in step 2,
In 0.5mol/L sulfuric acid, in -0.3V to+2.0V potential region, enclosed with 0.1V/s cyclic activation 5.
4. the preparation method of orderly polyaniline nano linear array according to claim 2, it is characterised in that: in step 3, benzene
The concentration of amine monomers solution is 0.3-0.6mol/L, and the concentration of corresponding perchloric acid solution is 0.6-1.2mol/L.
5. the preparation method of orderly polyaniline nano linear array according to claim 2, it is characterised in that: permanent in step 3
Current time is 20-60 minutes, constant current 0.016mA.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102737851A (en) * | 2011-04-15 | 2012-10-17 | 国家纳米科学中心 | Flexible supercapacitor and preparation method thereof |
| CN104616905A (en) * | 2015-01-09 | 2015-05-13 | 东南大学 | Polyaniline-carbon layer-titanium nitride nanowire array composite material and preparation method and application thereof |
| CN106183316A (en) * | 2016-07-08 | 2016-12-07 | 东华大学 | A kind of compliant conductive compound fabric and preparation thereof and application |
| CN108766616A (en) * | 2018-06-07 | 2018-11-06 | 深圳市梅莎新能源科技有限公司 | A kind of preparation method of carbon nanotube electrode |
-
2019
- 2019-03-25 CN CN201910228717.4A patent/CN109942813A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102737851A (en) * | 2011-04-15 | 2012-10-17 | 国家纳米科学中心 | Flexible supercapacitor and preparation method thereof |
| CN104616905A (en) * | 2015-01-09 | 2015-05-13 | 东南大学 | Polyaniline-carbon layer-titanium nitride nanowire array composite material and preparation method and application thereof |
| CN106183316A (en) * | 2016-07-08 | 2016-12-07 | 东华大学 | A kind of compliant conductive compound fabric and preparation thereof and application |
| CN108766616A (en) * | 2018-06-07 | 2018-11-06 | 深圳市梅莎新能源科技有限公司 | A kind of preparation method of carbon nanotube electrode |
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| 高新艳等: "电化学制备有序聚苯胺纳米线阵列", 《电化学》 * |
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Application publication date: 20190628 |