CN103074641B - The preparation method of the Pt/ITO electrode of efficient electric catalytic oxidation ammonia - Google Patents
The preparation method of the Pt/ITO electrode of efficient electric catalytic oxidation ammonia Download PDFInfo
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- CN103074641B CN103074641B CN201210586566.8A CN201210586566A CN103074641B CN 103074641 B CN103074641 B CN 103074641B CN 201210586566 A CN201210586566 A CN 201210586566A CN 103074641 B CN103074641 B CN 103074641B
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Abstract
The present invention discloses the preparation method of the Pt/ITO electrode of a kind of efficient electric catalytic oxidation ammonia; Described method comprises the steps: step one: preparation work electrode, and (a) is first by ITO clean; B wire is connected with the conducting surface through the cleaned ITO of step (a) and encapsulates by (), obtain working electrode; Step 2: electrode, saturated calomel reference electrode, working electrode and electrolytic solution are connected to form by Pt loop and form three-electrode system; Described electrolytic solution is by H2PtCl6Solution and HCl solution mix; Step 3: three-electrode system is accessed electrochemical workstation, carries out electrodeposition process. The present invention can effectively reduce the particle diameter of the Pt metallic particles that galvanic deposit obtains after introducing chlorion in electroplate liquid, obtains nano-sheet particle, improves the dispersion of metallic particles on ITO surface, the catalytic efficiency of platinum, the utilization ratio of Pt simultaneously. Step of the present invention is simple, it is easy to operation, with low cost, environmental protection, and effect is remarkable, and compared with current commercial catalyst electrode, performance is better.
Description
Technical field
The present invention relates to a kind of is the electrode preparation method of electrocatalysis technical field, is specifically related to the preparation method of the Pt/ITO electrode of a kind of efficient electric catalytic oxidation ammonia.
Background technology
The conductive base of load dispersion precious metal micro-/ nano particle stops material has important application prospect in fields such as electrocatalysis, the energy, biology, optics and electron devices. In recent years, tin indium oxide (ITO) transparent conductive film with superior electrical and optical property is adopted to cause rapid concern as conductive carrier. More traditional conducting base, ITO, except the advantage with low cost, also has good electroconductibility, high visible light transmissivity, the wide advantage such as electrochemical window and stable physical and chemical performance. But little at the content of nature Pt, Pt is expensive, causes the manufacturing cost of Pt/ITO electrode high. In order to reduce the manufacturing cost of Pt/ITO electrode, it is necessary to improving the utilization ratio of Pt, that add in electroplate liquid during Pt nano particle prepared by forefathers is H2SO4, the particle diameter of the particle obtained is 300-500nm, and causing the Pt in nano particle cannot utilize, and causes the utilization ratio of Pt very low.
Summary of the invention
For defect of the prior art, it is an object of the invention to provide the preparation method of the Pt/ITO electrode of a kind of efficient electric catalytic oxidation ammonia.
The present invention provides the preparation method of the Pt/ITO electrode of a kind of efficient electric catalytic oxidation ammonia, comprises the steps:
Step one: preparation work electrode,
A () is first by ITO clean;
B wire is connected and encapsulation process by () with the conducting surface through the cleaned ITO of step (a), obtain working electrode;
Step 2: assembling three-electrode system,
Electrode, saturated calomel reference electrode, working electrode and electrolytic solution are connected to form by Pt loop and form three-electrode system; Described electrolytic solution is by H2PtCl6Solution and HCl solution mix;
Step 3: three-electrode system is accessed electrochemical workstation, carries out electrodeposition process, obtains and finally obtains Pt/ITO electrode.
Preferably, described cleaning comprises the steps: with, after acetone soln cleaning, supersound process, ultrasonic time is 10min.
Preferably, in step one (b), described in be encapsulated as and seal with paraffin.
Preferably, described H2PtCl6The concentration of solution is 5mmol/L, and the concentration of described HCl solution is 0.5mol/L.
Preferably, described galvanic deposit is potentiostatic method, and deposition voltage is-1.5V��1.0V, and depositing time is 350��450s, and depositing temperature is 20��25 DEG C.
Compared with prior art, the present invention has following useful effect:
(1) the present invention adds HCl solution, due to Cl-The effect of ion so that the particle diameter of the Pt nano particle that deposition obtains is less than 10nm, substantially improves its dispersion property simultaneously, effectively improves the utilization ratio of Pt;
(2) the Pt/ITO electrode activity height that prepared by this inventive method, can be applicable to catalytic oxidation ammonia field, and polluting at processing environment and manufacture clean energy field has good application prospect;
(3) step of the present invention is simple, it is easy to operation, with low cost, environmental protection, and effect is remarkable, and compared with current commercial catalyst electrode, performance is better.
Accompanying drawing explanation
By reading with reference to the detailed description that non-limiting example is done by the following drawings, the other features, objects and advantages of the present invention will become more obvious:
Fig. 1 adds H in electroplate liquid2SO4The shape appearance figure that the Pt/ITO electrode prepared is observed under scanning electron microscope (SEM);
Fig. 2 adds the shape appearance figure that the Pt/ITO electrode that HCl prepares observes under scanning electron microscope (SEM) in electroplate liquid;
Fig. 3 adds H in electroplate liquid2SO4The sulfuric acid cyclic voltammetry curve figure of the Pt/ITO electrode prepared;
Fig. 4 is the sulfuric acid cyclic voltammetry curve figure adding the Pt/ITO electrode that HCl prepares in electroplate liquid;
Fig. 5 adds H in electroplate liquid2SO4The ammonia cyclic voltammetry curve figure of the Pt/ITO electrode prepared;
Fig. 6 is the ammonia cyclic voltammetry curve figure adding the Pt/ITO electrode that HCl prepares in electroplate liquid.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail. The technician contributing to this area is understood the present invention by following examples further, but does not limit the present invention in any form. It should be appreciated that to those skilled in the art, without departing from the inventive concept of the premise, it is also possible to make some distortion and improvement. These all belong to protection scope of the present invention.
Embodiment 1
The present embodiment relates to the preparation method of a kind of Pt/ITO electrode with high catalytic activity, comprises the steps:
Step one: preparation work electrode,
A first ITO is put into acetone by (), and carry out ultrasonic cleaning 10min;
B the conducting surface of wire and the ITO processed through step (a) is connected with wax and carries out encapsulation process by (), obtain working electrode;
Step 2: assembling three-electrode system,
The ITO working electrode and the concentration that electrode, saturated calomel reference electrode, step one are obtained Pt are 5mmol/LH2PtCl6With concentration be the electrolytic solution that 0.5mol/HCl two kinds of solution mix be connected to form loop form three-electrode system;
Step 3: the three-electrode system in step 2 is linked into electrochemical workstation, galvanic deposit mode is potentiostatic method, and deposition voltage is-1.5V, and depositing time is 350s, and depositing temperature is 20 DEG C. Obtain final product Pt/ITO electrode.
Implementation result: final product Pt/ITO electrode is observed in the secure execution mode (sem and obtained shape appearance figure as shown in Figure 2; The three-electrode system that the Pt/ITO electrode that the present embodiment is obtained puts into assembling is carried out sulfuric acid cyclic voltammetry, and potential region is-0.2��1.0V, and scanning speed is 50mV/s, and cycle index is 14, and obtains sulfuric acid volt-ampere curve, as shown in Figure 4; The three-electrode system that the Pt/ITO electrode that the present embodiment is obtained puts into assembling is carried out ammonia cyclic voltammetry, and potential region is-1.0��0.1V, and scanning speed is 10mV/s, and cycle index is 6, and obtains ammonia volt-ampere curve, as shown in Figure 6.
Embodiment 2
The present embodiment relates to the preparation method of a kind of Pt/ITO electrode with high catalytic activity, comprises the steps:
Step one: preparation work electrode,
A first ITO is put into acetone by (), and carry out ultrasonic cleaning 10min;
B the conducting surface of wire and the ITO processed through step (a) is connected with wax and carries out encapsulation process by (), obtain working electrode;
Step 2: assembling three-electrode system,
The ITO working electrode and the concentration that electrode, saturated calomel reference electrode, step one are obtained Pt are 5mmol/LH2PtCl6With concentration be the electrolytic solution that 0.5mol/HCl two kinds of solution mix be connected to form loop form three-electrode system;
Step 3: the three-electrode system in step 2 is linked into electrochemical workstation, galvanic deposit mode is potentiostatic method, and deposition voltage is-1.0V, and depositing time is 450s, and depositing temperature is 25 DEG C. Obtain final product Pt/ITO electrode.
Implementation result: final product Pt/ITO electrode is observed in the secure execution mode (sem and obtained shape appearance figure as shown in Figure 2; The three-electrode system that the Pt/ITO electrode that the present embodiment is obtained puts into assembling is carried out sulfuric acid cyclic voltammetry, and potential region is-0.2��1.0V, and scanning speed is 50mV/s, and cycle index is 14, and obtains sulfuric acid volt-ampere curve, as shown in Figure 4; The three-electrode system that the Pt/ITO electrode that the present embodiment is obtained puts into assembling is carried out ammonia cyclic voltammetry, and potential region is-1.0��0.1V, and scanning speed is 10mV/s, and cycle index is 6, and obtains ammonia volt-ampere curve, as shown in Figure 6.
Embodiment 3
The present embodiment relates to the preparation method of a kind of Pt/ITO electrode with high catalytic activity, comprises the steps:
Step one: preparation work electrode,
A first ITO is put into acetone by (), and carry out ultrasonic cleaning 10min;
B the conducting surface of wire and the ITO processed through step (a) is connected with wax and carries out encapsulation process by (), obtain working electrode;
Step 2: assembling three-electrode system,
The ITO working electrode and the concentration that electrode, saturated calomel reference electrode, step one are obtained Pt are 5mmol/LH2PtCl6With concentration be the electrolytic solution that 0.5mol/HCl two kinds of solution mix be connected to form loop form three-electrode system;
Step 3: the three-electrode system in step 2 is linked into electrochemical workstation, galvanic deposit mode is potentiostatic method, and deposition voltage is-1.2V, and depositing time is 400s, and depositing temperature is 23 DEG C. Obtain final product Pt/ITO electrode.
Implementation result: final product Pt/ITO electrode is observed in the secure execution mode (sem and obtained shape looks as shown in Figure 2, the three-electrode system that the Pt/ITO electrode that the present embodiment is obtained puts into assembling is carried out sulfuric acid cyclic voltammetry, potential region is-0.2��1.0V, scanning speed is 50mV/s, cycle index is 14, and obtain sulfuric acid volt-ampere curve, as shown in Figure 4; The three-electrode system that the Pt/ITO electrode that the present embodiment is obtained puts into assembling is carried out ammonia cyclic voltammetry, and potential region is-1.0��0.1V, and scanning speed is 10mV/s, and cycle index is 6, and obtains ammonia volt-ampere curve, as shown in Figure 6.
Comparative example 1
This comparative example relates to the preparation method of a kind of conventional Pt/ITO electrode, comprises the steps:
Step one: preparation work electrode,
A first ITO is put into acetone by (), and carry out ultrasonic cleaning;
B wire is connected with the ITO conducting surface processed through step (a) and carries out hermetically sealed with paraffin by (), obtain working electrode;
Step 2: assembling three-electrode system,
The ITO working electrode and the concentration that electrode, saturated calomel reference electrode, step one are obtained Pt are 5mmol/LH2PtCl6It is 0.5mol/H with concentration2SO4The electrolytic solution that two kinds of solution mixes is connected to form loop and forms three-electrode system;
Step 3: the three-electrode system in step 2 is linked into electrochemical workstation, galvanic deposit mode is potentiostatic method, and deposition voltage is-0.3V, and depositing time is 100s, and depositing temperature is 25 DEG C. Obtain final product Pt/ITO electrode.
Implementation result: as shown in Figure 1; The three-electrode system that the Pt/ITO electrode that comparative example is obtained puts into assembling is carried out sulfuric acid cyclic voltammetry, potential region is-0.2��1.0V, scanning speed is 50mV/s, and cycle index is 14, and obtains sulfuric acid volt-ampere curve, the three-electrode system that the Pt/ITO electrode that comparative example is obtained is put into assembling as shown in Figure 3 carries out ammonia cyclic voltammetry, potential region is-1.0��0.1V, and scanning speed is 10mV/s, and cycle index is 6, and obtain ammonia volt-ampere curve, as shown in Figure 5.
In sum, by the stereoscan photograph of embodiment 1��3 and comparative example 1 it may be seen that the Pt nanoparticle size in embodiment 1��3 has obvious reduction, simultaneously its dispersion property relatively comparative example 1 also increase substantially. And the experimental result that the hydrogen De contamination peak current density of the sulfuric acid curve of embodiment 1��3 is also greater than in comparative example 1. When catalytic oxidation ammonia, the peak current of embodiment 1��3 is 0.073mA/ug, the peak current of comparative example 1 is 0.036mA/ug, the activity of embodiment 1 is 2 times of comparative example 1, and namely the utilization ratio of Pt improves 100%, is original 200%, thus after proving that the present invention adds HCl solution, the particle diameter depositing the Pt nano particle obtained significantly is reduced, substantially improves its dispersion property simultaneously, effectively improve the utilization ratio of Pt;
Above specific embodiments of the invention are described. It is understood that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect the flesh and blood of the present invention.
Claims (1)
1. the preparation method of the Pt/ITO electrode of an efficient electric catalytic oxidation ammonia, it is characterised in that, comprise the steps:
Step one: preparation work electrode,
A () is first by ITO clean;
B wire is connected and encapsulation process by () with the conducting surface through the cleaned ITO of step (a), obtain working electrode;
Step 2: assembling three-electrode system,
Electrode, saturated calomel reference electrode, working electrode and electrolytic solution are connected to form by Pt loop and form three-electrode system; Described electrolytic solution is by H2PtCl6Solution and HCl solution mix;
Step 3: three-electrode system is accessed electrochemical workstation, carries out galvanic deposit, obtains and finally obtains Pt/ITO electrode;
In step one (a), described cleaning comprise the steps: with acetone soln clean after, supersound process, ultrasonic time is 10min;
In step one (b), described in be encapsulated as use paraffin seal;
In step 2, described H2PtCl6The concentration of solution is 5mmol/L, and the concentration of described HCl solution is 0.5mol/L;
In step 3, described galvanic deposit is potentiostatic method, and deposition voltage is-1.5V��1.0V, and depositing time is 350��450s, and depositing temperature is 20��25 DEG C.
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| CN109065900B (en) * | 2018-09-10 | 2021-06-08 | 华南理工大学 | Multilevel structure composite material and preparation and application thereof |
| CN113130916B (en) * | 2019-12-30 | 2022-06-14 | 大连大学 | Method for constructing lactose fuel cell based on PdNPs/NiNPs/ITO electrode |
| CN113668029B (en) * | 2021-08-27 | 2023-03-10 | 安徽大学 | Film formed by rough gold nanoparticles and preparation method and application thereof |
| CN114397344A (en) * | 2022-01-07 | 2022-04-26 | 湖北大学 | Single-wall carbon nanotube-based flexible electrode array, wearable sensor and sweat in-situ monitoring method thereof |
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| US7156962B2 (en) * | 2001-06-21 | 2007-01-02 | Sanyo Electric Co., Ltd. | Electrolyzing electrode and production method therefor and electrolysis method using electrolyzing electrode and electrolysis solution producing device |
| CN101024174A (en) * | 2007-03-23 | 2007-08-29 | 厦门大学 | Platinum icosahedron nano crystal catalyst, its preparing method and use |
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Patent Citations (3)
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| US7156962B2 (en) * | 2001-06-21 | 2007-01-02 | Sanyo Electric Co., Ltd. | Electrolyzing electrode and production method therefor and electrolysis method using electrolyzing electrode and electrolysis solution producing device |
| CN101024174A (en) * | 2007-03-23 | 2007-08-29 | 厦门大学 | Platinum icosahedron nano crystal catalyst, its preparing method and use |
| CN101914783A (en) * | 2010-08-13 | 2010-12-15 | 上海交通大学 | Electrochemical deposition-based method for preparing electro-catalysis ammonia oxide electrode |
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