CN109559901A - Polypyrrole/molybdenum/titania nanotube ternary composite electrode preparation method - Google Patents
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Abstract
The invention discloses a kind of preparation methods of polypyrrole/molybdenum/titania nanotube ternary composite electrode, are to electrode using pretreated titanium sheet as working electrode, platinum electrode；By the working electrode and electrode is placed in containing NH4Second of electrochemicial oxidation is carried out in F and the ethylene glycol solution of deionized water, obtains titania nanotube；The titania nanotube is immersed in ammonium molybdate solution, high-temperature calcination is carried out after taking out drying, obtains molybdenum doping titania nanotube；It is to electrode, silver/silver chlorate for reference electrode by working electrode, platinum electrode of the molybdenum doping titania nanotube, electropolymerization is carried out in the aqueous solution containing pyrrole monomer and lithium perchlorate, it is after electropolymerization that electrode clean is dry, obtain polypyrrole/molybdenum/titania nanotube ternary composite electrode.The present invention can be made that electric conductivity is more excellent, the higher ternary composite electrode of specific capacitance.
Description
Technical field
The invention belongs to electrode material technical fields, and in particular to a kind of polypyrrole/molybdenum/titania nanotube ternary is multiple
The preparation method of composite electrode.
Background technique
In recent years, with the development of economy, people's lives level is greatly increased, but at the same time, energy
Source problem and environmental problem, which have become, restricts the new problem that human kind sustainable development is faced, and finds new energy and improves energy benefit
The subject under discussion to attract attention now is had become with rate.Supercapacitor has both chemical cell high energy as a kind of novel energy storage apparatus
The characteristics of metric density and ordinary capacitor high power density, and safety and environmental protection, charging rate are fast, have extended cycle life, and answer extensively
For fields such as automobile, aerospace, science and techniques of defence, information technology, electronics；However, the development and its application of supercapacitor
It is limited by electrode material energy density is relatively low, therefore the electrode material that exploitation is had excellent performance has become supercapacitor
Research emphasis in fields such as energy storages.
In recent years, the titania nanotube of one-dimensional high-sequential is logical by its biggish specific surface area and unique tubulose
Road characteristic is laid a good foundation for its electrode material for being used as supercapacitor；However, due to the electric conductivity of titania nanotube
Poor, electro-chemical activity is not high, is restricted its application in supercapacitor；Therefore titania nanotube is improved
Electric conductivity is particularly important；Studies have shown that using it is transient metal doped be a kind of effective approach, in all transition metal
In, Mo6+With its unique electron configuration and and Ti4+The ionic radius that matches and be concerned.
Summary of the invention
In view of this, the main purpose of the present invention is to provide a kind of polypyrrole/molybdenum/titania nanotube tri compounds
The preparation method of electrode.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
The embodiment of the present invention provides a kind of preparation method of polypyrrole/molybdenum/titania nanotube ternary composite electrode, should
Preparation method is realized by following steps:
Step (1), anodizing prepares titania nanotube: using pretreated titanium sheet as working electrode, platinum
Electrode is to electrode；By the working electrode and electrode is placed in containing NH4Is carried out in F and the ethylene glycol solution of deionized water
Making active materials for use in secondary electrochemical oxidation processes obtain titania nanotube；
Step (2) impregnates calcination method and prepares molybdenum doping titania nanotube: the titanium dioxide that the step (1) is obtained
Titanium nanotube is immersed in ammonium molybdate solution, is carried out high-temperature calcination after taking out drying, is obtained molybdenum doping titania nanotube；
Step (3), cyclic voltammetry prepare polypyrrole/molybdenum/titania nanotube ternary composite electrode: with the step
(2) the molybdenum doping titania nanotube obtained is working electrode, platinum electrode be to electrode, silver/silver chlorate is reference electrode,
Electropolymerization is carried out in aqueous solution containing pyrrole monomer and lithium perchlorate, dries electrode clean after electropolymerization, acquisition polypyrrole/
Molybdenum/titania nanotube ternary composite electrode.
By the working electrode and electrode is placed in containing NH in above scheme, in the step (1)4F and deionized water
Ethylene glycol solution in carry out electrochemicial oxidation before, further include, by the working electrode and to electrode be placed in containing
NH4First time electrochemicial oxidation is carried out in F and the ethylene glycol solution of deionized water, and then passes through ultrasound removal oxidation
Film.
In above scheme, pretreatment in the step (1), specifically: titanium sheet is used respectively 600 mesh and 1500 mesh sand paper into
Then row mechanical grinding passes through 1wt%HF and 3wt%HNO3Aqueous solution carry out chemical polishing.
It is described to contain NH in the step (1) in above scheme4In F and the ethylene glycol solution of deionized water, the NH4F
Concentration be 0.5~5wt%, the concentration of the deionized water is 2~8vol%；The mistake of the first time electrochemicial oxidation
Oxidation voltage is 60~80V in journey, and oxidization time is 2~4h.
By the working electrode and electrode is placed in containing NH in above scheme, in the step (1)4F and deionized water
Ethylene glycol solution in carry out oxidization time during second of electrochemicial oxidation be 0.5~2h.
In above scheme, in the step (2), the titania nanotube impregnates 12 in ammonium molybdate solution molybdic acid~
For 24 hours, the concentration of the aqueous ammonium is 0.1~1.0M.
In above scheme, in the step (2), the temperature of the high-temperature calcination is 350~550 DEG C, and the time is 1~3h.
In above scheme, in the step (3), the concentration of the pyrrole monomer is 0.05mol/L~0.4mol/L, described
The concentration of lithium perchlorate is 0.1mol/L~0.5mol/L.
In above scheme, in the electropolymerization of the step (3), surface sweeping rate is 20mV/s~100mV/s, and surface sweeping circle number is
10~50 circles.
It is described that electrode clean is dry in above scheme, specially use ethyl alcohol and deionized water clear respectively working electrode
Wash simultaneously natural air drying.
Compared with prior art, the present invention carries out two step anodizings and nano titania is made using titanium sheet as substrate
Then pipe prepares molybdenum doping titania nanotube using immersion calcination method, then carries out the composite modified of polypyrrole, finally obtain
Electric conductivity is more excellent, the higher ternary composite electrode of specific capacitance.
Detailed description of the invention
Fig. 1 is the constant current charge-discharge curve graph of the embodiment of the present invention 1 and comparative example 1 in the case where current density is 2.0A/g.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The embodiment of the present invention provides a kind of preparation method of polypyrrole/molybdenum/titania nanotube ternary composite electrode, should
Preparation method is realized by following steps:
Step (1), anodizing prepares titania nanotube: using pretreated titanium sheet as working electrode, platinum
Electrode is to electrode；By the working electrode and electrode is placed in containing NH4Is carried out in F and the ethylene glycol solution of deionized water
Making active materials for use in secondary electrochemical oxidation processes obtain titania nanotube；
Further, by the working electrode and electrode is placed in containing NH4In F and the ethylene glycol solution of deionized water into
It before row electrochemicial oxidation, further include by the working electrode and being placed in electrode containing NH4The second of F and deionized water
First time electrochemicial oxidation is carried out in glycol solution, and then oxide film dissolving is gone by ultrasound.
Specifically, the pretreatment are as follows: titanium sheet is subjected to mechanical grinding with 600 mesh and 1500 mesh sand paper respectively, is then led to
Cross 1wt%HF and 3wt%HNO3Aqueous solution carry out chemical polishing.
It is described to contain NH4In F and the ethylene glycol solution of deionized water, the NH4The concentration of F is 0.5~5wt%, described to go
The concentration of ionized water is 2~8vol%；
The oxidation voltage during the electrochemicial oxidation is 60~80V, first time electrochemicial oxidation twice
Oxidization time in the process is 2~4h, and the oxidization time during second of electrochemicial oxidation is 0.5~2h.
Step (2) impregnates calcination method and prepares molybdenum doping titania nanotube: the titanium dioxide that the step (1) is obtained
Titanium nanotube is immersed in ammonium molybdate solution, is carried out high-temperature calcination after taking out drying, is obtained molybdenum doping titania nanotube；
Specifically, the titania nanotube impregnate 12 in ammonium molybdate solution molybdic acid~for 24 hours, the aqueous ammonium
Concentration is 0.1~1.0M.
The temperature of the high-temperature calcination is 350~550 DEG C, and the time is 1~3h.
The high-temperature calcination can carry out in Muffle furnace, can also carry out high-temperature calcination using other equipment.
Step (3), cyclic voltammetry prepare polypyrrole/molybdenum/titania nanotube ternary composite electrode: with the step
(2) the molybdenum doping titania nanotube obtained is working electrode, platinum electrode be to electrode, silver/silver chlorate is reference electrode,
Electropolymerization is carried out in aqueous solution containing pyrrole monomer and lithium perchlorate, dries electrode clean after electropolymerization, acquisition polypyrrole/
Molybdenum/titania nanotube ternary composite electrode.
Specifically, the concentration of the pyrrole monomer is 0.05mol/L~0.4mol/L, and the concentration of the lithium perchlorate is
0.1mol/L~0.5mol/L.
In the electropolymerization, surface sweeping rate is 20mV/s~100mV/s, and surface sweeping circle number is 10~50 circles.
It is to clean working electrode with ethyl alcohol and deionized water respectively for electrode clean drying after the electropolymerization, and it is natural
It air-dries.
Embodiment 1
(1) anodizing prepares titania nanotube:
Using titanium sheet as substrate, firstly, titanium sheet is polished smooth, specific method be successively with 600 mesh and 1500 mesh sand paper into
Row mechanical grinding；Then, it is dipped in strong acid mixed solution and carries out chemical polishing, specific solution is 1wt%HF and 3wt%
HNO3Aqueous solution；Finally, platinum electrode is to electrode, first in 0.5wt%NH using the titanium sheet after polishing as working electrode4F and
In the ethylene glycol solution of 2vol% deionized water, in the oxidation at voltages 2h of 60V, ultrasound removes oxide film dissolving；It then will be after ultrasound
Titanium sheet put in the electrolytic solution progress second step anodic oxidation, oxidation voltage 60V, oxidization time 0.5h, obtain titanium dioxide
Titanium nanotube.
(2) it impregnates calcination method and prepares molybdenum doping titania nanotube:
The titania nanotube is immersed in the beaker equipped with 1.0M ammonium molybdate solution, places 12h, then put Muffle
In 450 DEG C of progress high-temperature calcinations in furnace, calcination time 2h obtains molybdenum doping titania nanotube.
(3) cyclic voltammetry prepares polypyrrole/molybdenum/titania nanotube trielement composite material:
Electropolymerization, using the molybdenum doping titania nanotube as working electrode, platinum electrode are carried out using cyclic voltammetry
It the use of instrument is electrochemical workstation for electrode, silver/silver chlorate is reference electrode, the electrolyte of electropolymerization is to contain 0.15M
Pyrrole monomer and 0.2M LiClO4Aqueous solution, the voltage range of cyclic voltammetric polymerization is -0.7~1.1V, and sweep speed is
50mV/s, scanning circle number are 20 circles.After preparation is completed, working electrode is cleaned with ethyl alcohol and deionized water respectively, and natural wind
It is dry, obtain polypyrrole/molybdenum/titania nanotube trielement composite material.
Embodiment 2
The preparation method of a kind of polypyrrole/molybdenum/titania nanotube ternary composite electrode of the present embodiment, with embodiment
1 compares, the difference is that the sweep speed in step (3) is 20mV/s, rest part is identical.
Embodiment 3
The preparation method of a kind of polypyrrole/molybdenum/titania nanotube ternary composite electrode of the present embodiment, with embodiment
1 compares, the difference is that the sweep speed of step (3) is 100mV/s, rest part is identical.
Embodiment 4
The preparation method of a kind of polypyrrole/molybdenum/titania nanotube ternary composite electrode of the present embodiment, with embodiment
1 compares, the difference is that the scanning circle number of step (3) is 10 circles, rest part is identical.
Embodiment 5
The preparation method of a kind of polypyrrole/molybdenum/titania nanotube ternary composite electrode of the present embodiment, with embodiment
1 compares, the difference is that the scanning circle number of step (3) is 50 circles, rest part is identical.
Embodiment 6
The preparation method of a kind of polypyrrole/molybdenum/titania nanotube ternary composite electrode of the present embodiment, with embodiment
1 compares, the difference is that the pyrrole monomer concentration of step (3) is 0.05mol/L, rest part is identical.
Embodiment 7
A kind of preparation method of the titania nanotube/polyaniline composite electrode of the present embodiment, compared with Example 1,
The difference is that pyrrole monomer concentration is 0.4mol/L in the electrolyte of step (3), rest part is identical.
Embodiment 8
The preparation method of a kind of polypyrrole/molybdenum/titania nanotube ternary composite electrode of the present embodiment, with embodiment
1 compares, the difference is that LiClO in the electrolyte of step (3)4Concentration is 0.1mol/L, and rest part is identical.
Embodiment 9
The preparation method of a kind of polypyrrole/molybdenum/titania nanotube ternary composite electrode of the present embodiment, with embodiment
1 compares, the difference is that LiClO in the electrolyte of step (3)4Concentration is 0.5mol/L, and rest part is identical.
Embodiment 10
The preparation method of a kind of polypyrrole/molybdenum/titania nanotube ternary composite electrode of the present embodiment, with embodiment
1 compares, the difference is that calcination temperature is 350 DEG C, calcination time 3h in step (2), rest part is identical.
Embodiment 11
The preparation method of a kind of polypyrrole/molybdenum/titania nanotube ternary composite electrode of the present embodiment, with embodiment
1 compares, the difference is that calcination temperature is 550 DEG C, calcination time 1h in step (2), rest part is identical.
Comparative example 1
The preparation method of a kind of titanium dioxide nanotube electrode of this comparative example, using high-purity titanium sheet as substrate, by titanium sheet
It polishes smooth；Using the titanium sheet after polishing as working electrode, platinum electrode is to be placed in calcining in high temperature furnace to electrode and obtain titanium dioxide
Nanotube.
Polypyrrole/molybdenum/titania nanotube ternary composite electrode that 1-11 of the embodiment of the present invention is obtained, comparative example 1
The carry out charge-discharge test of molybdenum doping titanium dioxide nanotube electrode is obtained, charge-discharge test is electrochemical workstation using instrument
(Autolab, MetrohmPGSTAT100, Switzerland ten thousand are logical), is carried out using constant current mode, and test electrolyte is 1.0mol/L's
Aqueous sulfuric acid, current density 1.0A/g, is tested using three-electrode system, the poly- pyrrole that wherein the present embodiment 1-11 is obtained
Cough up/molybdenum/titania nanotube ternary composite electrode, comparative example 1 obtain molybdenum doping titanium dioxide nanotube electrode respectively as
Working electrode, platinum electrode are to electrode, and silver/silver chlorate is reference electrode；It is calculated according to charging and discharging curve and active material weight
The capacitance of electrode out, the result is shown in shown in table 1.
Table 1
| Specific capacitance | |
| Embodiment 1 | 1280F/g |
| Embodiment 2 | 1080F/g |
| Embodiment 3 | 960F/g |
| Embodiment 4 | 1040F/g |
| Embodiment 5 | 980F/g |
| Embodiment 6 | 1160F/g |
| Embodiment 7 | 1120F/g |
| Embodiment 8 | 1130F/g |
| Embodiment 9 | 1170F/g |
| Embodiment 10 | 820F/g |
| Embodiment 11 | 880F/g |
| Comparative example 1 | 3.2F/g |
As shown in Table 1, by the post-depositional molybdenum doping titania nanotube of polypyrrole (poly- pyrrole i.e. produced by the present invention
Cough up/molybdenum/titania nanotube ternary composite electrode) specific capacitance to be far longer than the specific capacitance of titania nanotube.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the scope of the present invention.
Claims (10)
1. a kind of preparation method of polypyrrole/molybdenum/titania nanotube ternary composite electrode, which is characterized in that the preparation side
Method is realized by following steps:
Step (1), anodizing prepares titania nanotube: using pretreated titanium sheet as working electrode, platinum electrode
For to electrode；By the working electrode and electrode is placed in containing NH4It is carried out second in F and the ethylene glycol solution of deionized water
Electrochemicial oxidation obtains titania nanotube；
Step (2) impregnates calcination method and prepares molybdenum doping titania nanotube: the titanium dioxide that the step (1) obtains is received
Mitron is immersed in ammonium molybdate solution, is carried out high-temperature calcination after taking out drying, is obtained molybdenum doping titania nanotube；
Step (3), cyclic voltammetry prepare polypyrrole/molybdenum/titania nanotube ternary composite electrode: with the step (2)
The molybdenum doping titania nanotube of acquisition is working electrode, platinum electrode be to electrode, silver/silver chlorate is reference electrode, is being contained
Have and carries out electropolymerization in the aqueous solution of pyrrole monomer and lithium perchlorate, it is after electropolymerization that electrode clean is dry, acquisition polypyrrole/
Molybdenum/titania nanotube ternary composite electrode.
2. the preparation method of polypyrrole/molybdenum/titania nanotube ternary composite electrode according to claim 1, special
Sign is, by the working electrode and is placed in electrode containing NH in the step (1)4The ethylene glycol solution of F and deionized water
Before middle carry out electrochemicial oxidation, further include, by the working electrode and electrode is placed in containing NH4F and deionized water
Ethylene glycol solution in carry out first time electrochemicial oxidation, and then oxide film dissolving is gone by ultrasound.
3. the preparation method of polypyrrole/molybdenum/titania nanotube ternary composite electrode according to claim 1 or 2,
It is characterized in that, pretreatment in the step (1), specifically: titanium sheet is subjected to mechanical beat with 600 mesh and 1500 mesh sand paper respectively
Then mill passes through 1wt%HF and 3wt%HNO3Aqueous solution carry out chemical polishing.
4. the preparation method of polypyrrole/molybdenum/titania nanotube ternary composite electrode according to claim 3, special
Sign is, described to contain NH in the step (1)4In F and the ethylene glycol solution of deionized water, the NH4The concentration of F is 0.5
~5wt%, the concentration of the deionized water are 2~8vol%；Electricity is aoxidized during the first time electrochemicial oxidation
Pressure is 60~80V, and oxidization time is 2~4h.
5. the preparation method of polypyrrole/molybdenum/titania nanotube ternary composite electrode according to claim 4, special
Sign is, by the working electrode and is placed in electrode containing NH in the step (1)4The ethylene glycol solution of F and deionized water
Oxidization time is during second of electrochemicial oxidation of middle progress
0.5~2h.
6. the preparation method of polypyrrole/molybdenum/titania nanotube ternary composite electrode according to claim 5, special
Sign is, in the step (2), the titania nanotube impregnates 12 in ammonium molybdate solution molybdic acid~for 24 hours, the ammonium water
The concentration of solution is 0.1~1.0M.
7. the preparation method of polypyrrole/molybdenum/titania nanotube ternary composite electrode according to claim 6, special
Sign is, in the step (2), the temperature of the high-temperature calcination is 350~550 DEG C, and the time is 1~3h.
8. the preparation method of polypyrrole/molybdenum/titania nanotube ternary composite electrode according to claim 7, special
Sign is, in the step (3), the concentration of the pyrrole monomer is 0.05mol/L~0.4mol/L, the lithium perchlorate it is dense
Degree is 0.1mol/L~0.5mol/L.
9. the preparation method of polypyrrole/molybdenum/titania nanotube ternary composite electrode according to claim 8, special
Sign is, in the electropolymerization of the step (3), surface sweeping rate is 20mV/s~100mV/s, and surface sweeping circle number is 10~50 circles.
10. the preparation method of polypyrrole/molybdenum/titania nanotube ternary composite electrode according to claim 9, special
Sign is, described that electrode clean is dry, and working electrode is specially cleaned simultaneously natural air drying with ethyl alcohol and deionized water respectively.
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| CN110112012A (en) * | 2019-04-08 | 2019-08-09 | 华南理工大学 | A kind of polyaniline-titanium dioxide nanotube composite electrode and preparation method thereof |
| CN112713011A (en) * | 2020-12-23 | 2021-04-27 | 杭州电子科技大学 | Method for preparing super capacitor with double-conducting network |
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