CN109763139A - α-Co(OH)2/ PPy/GO nanometer sheet and OER electro-catalysis modified electrode based on it - Google Patents
α-Co(OH)2/ PPy/GO nanometer sheet and OER electro-catalysis modified electrode based on it Download PDFInfo
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Abstract
The present invention relates to α-Co (OH)2/ PPy/GO nanometer sheet and OER electro-catalysis modified electrode based on it.The electrode include using glass-carbon electrode as basal electrode, and be attached on glass-carbon electrode α-cobalt hydroxide modification polypyrrole/graphene oxide (PPy/GO) nanometer sheet.Due to the presence of α-cobalt hydroxide, the reaction rate of water decomposition is enhanced, it is only necessary to which lower overpotential makes this nanometer material modified electrode show higher electro-chemical activity and good stability in terms of water decomposition.
Description
Technical field
The invention belongs to electrochemical catalysis fields, and in particular to a kind of electro-catalysis modified electrode and preparation method thereof and answer
With.
Background technique
Combustion product based on hydrogen high specific energy content and neutral carbon has always been considered as being that fossil is replaced to fire for a long time
Expect, meet the alternative fuel of global energy consumption.And hydrogen mode is produced by the environmental protection of two kinds of half-reactions of power of renewable energy
It is explored extensively.
Being electrolysed aquatic products hydrogen is abundant raw material, and method is simple, and hydrogen has extremely wide application.And it is anti-with liberation of hydrogen
Answer (HER) to compare, with multi-step, four electronic processes oxygen evolution reaction (OER) due to its slow dynamics by limitation.It is logical
It crosses and catalyst is added so that improving OER activity then becomes the key of electrolysis water.Conventional Ir/Ru class catalyst is played the part of in OER
Key player.However the disadvantages of its content is rare, expensive and stability is poor, produces very big limit to its large-scale application
System.Therefore develop it is a kind of can electro-catalysis water decomposition can especially improve the active chemically modified electrode of OER for the electricity of water
The research important in inhibiting of catalytic pyrolysis.
Summary of the invention
An object of the present invention is to provide cheap, the high α-Co (OH) of catalytic performance of one kind2/ PPy/GO nanometers
Piece.
It is a kind of with α-Co (OH) the second object of the present invention is to provide2/ PPy/GO nanometer sheet prepares OER electro-catalysis modification electricity
Pole is used for electro-catalysis splitting water.
To achieve the above object, used technical solution is as follows by the present invention:
α-Co(OH)2/ PPy/GO nanometer sheet, preparation method include the following steps:
1) under conditions of ultrasonic radiation, pyrroles's (Py) in-situ chemical is polymerize in GO nanometer sheet, polypyrrole/oxidation is obtained
Graphene (PPy/GO) nanometer sheet；
2) PPy/GO nanometer sheet is dispersed in water, then CoCl is added into system2·6H2O and ammonium hydroxide, stir evenly, into
Row reaction, products therefrom are successively washed with distilled water and ethyl alcohol, are centrifuged, and vacuum drying obtains α-Co (OH)2/ PPy/GO receives
Rice piece.
Preferably, above-mentioned α-Co (OH)2/ PPy/GO nanometer sheet, in mass ratio, CoCl2·6H2O:PPy/GO=30:1.
Preferably, above-mentioned α-Co (OH)2/ PPy/GO nanometer sheet, in step 2), reaction condition are as follows: room temperature, pH=8-10
Under, react 10-14h.
Preferably, above-mentioned α-Co (OH)2/ PPy/GO nanometer sheet, in step 1), under conditions of ultrasonic radiation, by pyrrole
The polymerization of (Py) in-situ chemical is coughed up in GO nanometer sheet prepared by Hummers method, obtains PPy/GO nanometer sheet.
One kind being based on α-Co (OH)2The OER electro-catalysis modified electrode of/PPy/GO nanometer sheet, is using glass-carbon electrode as substrate
Electrode, by above-mentioned α-Co (OH)2/ PPy/GO nanometer sheet is attached to manufactured α-Co (OH) on glass-carbon electrode2/ PPy/GO modification
Glass-carbon electrode.
One kind being based on α-Co (OH)2The preparation method of the OER electro-catalysis modified electrode of/PPy/GO nanometer sheet, including it is as follows
Step:
1) by above-mentioned α-Co (OH)2/ PPy/GO nanometer sheet, ultrasonic disperse obtain finely dispersed multiple in dehydrated alcohol
Close dressing agent；
2) finely dispersed composite modified dose of drop coating is dried at room temperature in clean glassy carbon electrode surface, obtains α-Co
(OH)2The glass-carbon electrode of/PPy/GO modification.
Above-mentioned one kind is based on α-Co (OH)2The OER electro-catalysis modified electrode of/PPy/GO nanometer sheet is in electrocatalytic decomposition water
Analyse the application in oxygen.Method is as follows: by above-mentioned α-Co (OH)2The glass-carbon electrode of/PPy/GO modification is as working electrode, Hg/
HgO electrode is reference electrode, and platinum electrode is auxiliary electrode, forms three-electrode system, the realization pair in 1M potassium hydroxide aqueous solution
The electro-catalysis of water.
Compared with prior art, the present invention having the following obvious advantages:
1. modified electrode prepared by the present invention is allowed the water to due to the presence of α-cobalt hydroxide on nanometer sheet surface
Accelerate water to resolve into the speed of oxygen and hydrogen under the participation of bivalent Co, realizes the application to water power catalysis, enhancing
Water cartalytic decomposition effect efficiency, make this nanometer material modified electrode shown in terms of water power catalysis higher activity and
It is good linear.
2. modified electrode prepared by the present invention shows stronger chemical property, preferable stability, preferable line
The advantages that property.
3. modified electrode prepared by the present invention, so that electrocatalytic decomposition aquatic products hydrogen oxygen is achieved, it is practical application electricity
Catalytic decomposition water provides new idea and method.
4. in the present invention, cobalt is cheap, amount of storage is big, meanwhile, polypyrrole/graphene oxide (PPy/GO) is used as bottom
Cobalt compound-organic conductive compound of object synthesis, promotes conductive capability of the cobalt compound in electrochemical catalysis, further
Improve the catalytic performance of cobalt compound.
5. modified electrode prepared by the present invention, cheap, stability, easy to operate, reaction speed is fast.
Detailed description of the invention
Fig. 1 is α-Co (OH)2The electron microscope of/PPy/GO nanometer sheet；
Wherein, (a) α-Co (OH)2/ PPy/GO nanometer sheet scanning electron microscope (SEM) picture；(b)α-Co(OH)2/ PPy/GO receives
Rice piece transmission electron microscope (TEM) picture.
Fig. 2 is the XRD diagram of different modifying electrode.
Fig. 3 is the linear sweep voltammetry comparison diagram of different modifying electrode electrocatalytic decomposition water.
Fig. 4 is Tafel slope figure of the different modifying electrode in electrocatalytic decomposition water.
Fig. 5 is the cyclic voltammogram that difference sweeps modified electrode under speed.
Speed and current density linear relationship are swept when Fig. 6 is modified electrode electrolysis water.
Fig. 7 is modified electrode chronoamperogram.
Fig. 8 is Nyquist figure of the modified electrode under different overvoltage.
Specific embodiment
The present invention is described in further details below in conjunction with preferred embodiments and drawings, it should be understood that described herein
Preferred embodiment only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1 α-Co (OH) 2/PPy/GO nanometer sheet
(1) the preparation method is as follows:
1) preparation of GO nanometer sheet: being added the 67.5mL concentrated sulfuric acid in there-necked flask, and 2.0g high purity graphite and 1.6g is added
NaNO3, and stir evenly, it keeps system temperature less than 5 DEG C, 9g KMnO is added in one hour into mixed solution4, then set
In 36 DEG C of water-bath 0.5h.It after being stored at room temperature 14 days, is diluted with 560mL60 DEG C of water, H is added dropwise2O2Glassy yellow is presented to solution,
After being centrifuged (rmp=10000), washing to neutrality while hot, 50 DEG C of vacuum drying obtain GO nanometer sheet.
2) PPy/GO nanometer sheet: 0.2g GO nanometer sheet ultrasonic disperse is added in 100mL deionized water, adds 0.2g pyrrole
It coughs up (Py), 1.2g FeCl is added after ultrasonic disperse3·6H2O continues ultrasound 0.5h, and centrifuge washing is simultaneously dried in vacuo, and obtains PPy/GO
Nanometer sheet.
3)α-Co(OH)2The preparation of/PPy/GO nanometer sheet: dispersing 50mg PPy/GO in 50mL water, then adds into system
Enter 1.5g Co (OH)2·6H2O, 1mL ammonium hydroxide stirs evenly, and then, under room temperature, alkalescent (pH=9), persistently stirs 12h,
After reaction, products therefrom is successively washed with distilled water and ethyl alcohol, is centrifuged, and vacuum drying obtains α-Co (OH)2/PPy/
GO nanometer sheet.
(2) it detects
1、α-Co(OH)2The electron microscope of/PPy/GO nanometer sheet is as shown in Figure 1, (a) is scanning electron microscope (SEM) picture；(b)
For transmission electron microscope (TEM) picture, as seen from Figure 1, α-Co (OH) prepared by the present invention2Slice is presented in/PPy/GO, nanometer sheet surface
Shape texture.
2, Fig. 2 is each composition X-ray diffractogram, and a is GO X-ray diffractogram, and b is PPy/GO X-ray diffractogram, and c is
Co(OH)2X-ray diffractogram, d are α-Co (OH)2/ PPy/GO X-ray diffractogram, wherein ● it is Co (OH)2Diffraction maximum, by
Fig. 2 comparison is as can be seen that the present invention synthesizes α-Co (OH) well2/PPy/GO。
Embodiment 2 is based on α-Co (OH)2The OER electro-catalysis modified electrode of/PPy/GO nanometer sheet
(1) the preparation method is as follows:
1) α-Co (OH) for the drying for taking 2mg embodiment 1 to prepare21mL ethyl alcohol, ultrasonic disperse is added in/PPy/GO nanometer sheet
20min obtains the black suspension that concentration is 2mg/mL, as composite modified dose, spare.
2) glass-carbon electrode: first being used 0.3 μM of aluminum oxide suspension grinding process on polishing cloth by the processing of electrode,
Then it is cleaned by ultrasonic with deionized water, then is polished to mirror surface on polishing cloth with 0.05 μM of aluminum oxide suspension, finally
It is cleaned by ultrasonic with ethyl alcohol, deionized water, is dried up with high pure nitrogen, it is spare.
3) prepared by modified electrode: composite modified dose of drop coating for pipetting the preparation of 5 μ L steps 1) with microsyringe is dry to polishing
The surface of net glass-carbon electrode, spontaneously dries at room temperature, obtains α-Co (OH)2The glass-carbon electrode of/PPy/GO modification, it is spare.
(2) electrochemical property test
1, the linear sweep voltammetry comparison of different modifying electrode electrocatalytic oxidation evolution reaction
Method: in 1M KOH electrolytic cell, respectively with GO modified glassy carbon electrode, PPy/GO modified glassy carbon electrode, Co (OH)2
Modified electrode, α-Co (OH)2/ GO modified electrode and α-Co (OH)2/ PPy/GO modified electrode is as working electrode, Hg/HgO electrode
For reference electrode, platinum electrode is as auxiliary electrode；Test carries out on CHI660e electrochemical workstation, attached calculating
Machine software is made for the acquisition and processing of experimental data；Linear sweep voltammetry is carried out in 1.2V~1.8V (vs.RHE) potential range
Test, records stable linear sweep voltammetry figure.
As shown in figure 3, cracking the linear sweep voltammetry comparison diagram of elutriation oxygen for the electro-catalysis of different modifying electrode, wherein a is bent
Line is GO electrode, and b curve is PPy/GO modified glassy carbon electrode, and two modified electrodes are all existing without there is apparent current break
As.C curve is Co (OH)2Modified glassy carbon electrode, d curve are α-Co (OH)2/ GO modified glassy carbon electrode, e curve are α-Co
(OH)2/ PPy/GO modified electrode.Curve c~e current density is gradually increased and overpotential is gradually reduced.Illustrate pure Co (OH)2Material
Material and α-Co (OH)2Although/GO has analysis oxygen performance but electric conductivity is poor, and a larger current then can be observed on e curve
Density and extremely low overpotential compare to obtain α-Co (OH)2/ PPy/GO modified electrode has preferable electro-catalysis living when being electrolysed elutriation oxygen
Property.Meanwhile the Tafel curve (such as Fig. 4) obtained by linear sweep voltammetry curve compares it is also seen that α-Co (OH)2/PPy/
GO has extremely low Tafel slope.Illustrate the good oxygen evolution reaction catalytic activity of the catalyst.
2, the research of modified electrode surface kinetics
With α-Co (OH)2/ PPy/GO modified electrode is working electrode, and Hg/HgO electrode is reference electrode, supplemented by platinum electrode
Help electrode；Experiment carries out on CHI660e electrochemical workstation, acquisition and processing including experimental data；In 1M KOH solution
In, cyclic voltammetry scan is carried out in 1.12~1.28V (vs.RHE) potential range, scanning speed range is 2~20mV/s.
Fig. 5 is α-Co (OH)2/ PPy/GO modified electrode oxygen evolution reaction cyclic voltammogram under the conditions of different scanning speed.
It can be seen from the figure that the current density of cyclic voltammetry curve also linearly increases, i.e. water oxygen with the increase of sweep speed
Peak current increases with the increase of scanning speed.Influence by research sweep speed to oxidation peak current, can speculate electricity
The dynamics of pole reaction.
Fig. 6 is the linear relationship of current density and scanning speed.As shown in fig. 6, sweep speed is in 2~20mV/s range
Interior, the oxidation peak current and scanning speed of water are at good linear relationship, thus obtained slope, that is, double layer capacity (Cdl) be
15.1mF.cm-2.It follows that the oxidation process of water is carried out in a manner of granule surface contral under the experiment condition.
3, the stability measurement of catalyst
With α-Co (OH)2/ PPy/GO modified electrode is working electrode, and Hg/HgO electrode is reference electrode, supplemented by platinum electrode
Help electrode；Experiment carries out on CHI660e electrochemical workstation, acquisition and processing including experimental data；In the KOH solution of 1M
In, prolonged chrono-amperometric test is carried out under 1.58V (vs.RHE) current potential.Fig. 7, after up to the test of 20h, this is urged
The current density of agent only has dropped 9.4%, that is, illustrates α-Co (OH)2/ PPy/GO nano material has under strongly alkaline conditions
Good stability.
4, electrochemical impedance is tested
With α-Co (OH)2/ PPy/GO material modified glassy carbon electrode is working electrode, and Hg/HgO electrode is reference electrode, platinum
Electrode is auxiliary electrode, and bottom liquid is the KOH solution of 1M；Experiment carries out under different overpotentials on CHI660e electrochemical workstation
Testing impedance, acquisition and processing including experimental data.As a result as shown in figure 8, from curve a~e, with the increasing of overpotential
Add, electronics transfer resistance (first semicircle in Rct curve) is gradually reduced, i.e., electric conductivity enhances, again from kinetically explaining
α-Co (OH) is released2Satisfactory electrical conductivity of/the PPy/GO in electrolysis elutriation oxygen.
The above description is only a preferred embodiment of the present invention, is merely illustrative for the purpose of the present invention, and not restrictive；
Those of ordinary skill in the art understand, can carry out many to it in the spirit and scope defined by the claims in the present invention and change
Become, modification or even equivalent change, but falls in protection scope of the present invention.
Claims (7)
1.α-Co(OH)2/ PPy/GO nanometer sheet, which is characterized in that preparation method includes the following steps:
1) under conditions of ultrasonic radiation, pyrroles's in-situ chemical is polymerize in GO nanometer sheet, PPy/GO nanometer sheet is obtained；
2) PPy/GO nanometer sheet is dispersed in water, then CoCl is added into system2·6H2O and ammonium hydroxide, stir evenly, and carry out anti-
It answers, products therefrom is successively washed with distilled water and ethyl alcohol, is centrifuged, and vacuum drying obtains α-Co (OH)2/ PPy/GO nanometer sheet.
2. α-Co (OH) according to claim 12/ PPy/GO nanometer sheet, which is characterized in that in mass ratio, CoCl2·
6H2O:PPy/GO=30:1.
3. α-Co (OH) according to claim 12/ PPy/GO nanometer sheet, which is characterized in that in step 2), reaction condition
Are as follows: room temperature under pH=8-10, reacts 10-14h.
4. one kind is based on α-Co (OH)2The OER electro-catalysis modified electrode of/PPy/GO nanometer sheet, which is characterized in that be with glass carbon electricity
Extremely basal electrode, by the described in any item α-Co of claim 1-3 (OH)2/ PPy/GO nanometer sheet is attached on glass-carbon electrode
Manufactured α-Co (OH)2The glass-carbon electrode of/PPy/GO modification.
5. one kind is based on α-Co (OH)2The preparation method of the OER electro-catalysis modified electrode of/PPy/GO nanometer sheet, which is characterized in that
Preparation method includes the following steps:
1) by α-Co (OH) described in claim 12/ PPy/GO nanometer sheet, ultrasonic disperse must be uniformly dispersed in dehydrated alcohol
Composite modified dose；
2) finely dispersed composite modified dose of drop coating is dried at room temperature in clean glassy carbon electrode surface, obtains α-Co (OH)2/
The glass-carbon electrode of PPy/GO modification.
6. as claimed in claim 4 a kind of based on α-Co (OH)2The OER electro-catalysis modified electrode of/PPy/GO nanometer sheet is in electro-catalysis
Decompose the application in water.
7. application according to claim 6, which is characterized in that method is as follows: by α-Co (OH) as claimed in claim 42/
The glass-carbon electrode of PPy/GO modification is reference electrode as working electrode, Hg/HgO electrode, and platinum electrode is auxiliary electrode, composition three
Electrode system realizes the electro-catalysis to water in 1M potassium hydroxide aqueous solution.
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| CN110359060A (en) * | 2019-07-30 | 2019-10-22 | 辽宁大学 | FeCoNiBOx/ PPy/rGO nano material and OER electro-catalysis modified electrode based on it |
| CN111074289A (en) * | 2020-01-21 | 2020-04-28 | 西北师范大学 | Flaky nano β -Co (OH)2Preparation method of (1) |
| CN112359377A (en) * | 2020-10-28 | 2021-02-12 | 贵州大学 | Catalyst prepared from six-membered cucurbituril, reduced graphene and polypyrrole and application of catalyst |
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