CN108468060A - A kind of preparation and its application of efficient, novel porous nitrogen oxides nanometer sheet catalyst electrode - Google Patents
A kind of preparation and its application of efficient, novel porous nitrogen oxides nanometer sheet catalyst electrode Download PDFInfo
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- CN108468060A CN108468060A CN201810218117.5A CN201810218117A CN108468060A CN 108468060 A CN108468060 A CN 108468060A CN 201810218117 A CN201810218117 A CN 201810218117A CN 108468060 A CN108468060 A CN 108468060A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
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- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
- C25B11/077—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the compound being a non-noble metal oxide
- C25B11/0771—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the compound being a non-noble metal oxide of the spinel type
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Abstract
The invention discloses a kind of efficient, novel porous nitrogen oxides nanometer sheet catalyst electrode (Co3O3.62N0.38) preparation and its application.Porous C o3O3.62N0.38The preparation of nanometer sheet catalyst, using the method for electrochemical deposition, prepares Co (OH) using cheap graphite flake as substrate2Presoma；Then the presoma is made annealing treatment 2 hours under 400 degrees Celsius in ammonia atmosphere.DFT theoretical calculations show porous C o3O3.62N0.38Nanometer sheet catalyst has good electric conductivity and the excellent adsorption free energy to intermediate, therefore porous C o3O3.62N0.38Nanometer sheet catalyst presents excellent electrochemical catalysis production oxygen performance, has ultralow electrolysis water overpotential and lower Tafel.Meanwhile the synthetic method of the combination electrode is simple and efficient, synthesis cost economy is cheap, is suitble to the commercial Application of electrochemical decomposition water, has extensive scientific meaning.
Description
Technical field
The present invention relates to electrocatalytic decomposition water technical fields, more particularly to a kind of preparation of porous nitrogen oxide catalyst
And its application in terms of electrochemical decomposition water.
Background technology
With the consumption of the non-renewable energy resources such as global fossil energy, the exhaustion of fossil energy is inevitable, the energy
Crisis is that the mankind must problems faced.Therefore, sustainable novel energy (such as solar energy, wind energy, nuclear energy, biomass energy)
Development and utilization, it is extremely urgent to improve its ratio in entire energy resource structure.But the storage of these novel energies and company
Continuous supply property is the problem that must be solved, wherein it is an important approach to convert it into chemical energy, such as electrochemical credit
Solve water hydrogen manufacturing and oxygen.
In electrochemical catalysis decomposes aquatic products oxygen system, the oxidation of water and reduction reaction need under certain electrode potential
It could occur, therefore develop efficient catalyst to reduce the overpotential in reaction process, to realize effective reduction of energy consumption
It is particularly important.So far, most effective production VPO catalysts are RuO2And IrO2, but due to the high cost of noble metal and
It is rare and limit its industrial applications in production.In recent years, the electrolysis aquatic products VPO catalysts based on transition metal base, by
In its cheap price and relatively high catalytic activity, the extensive concern of researcher is caused.Studies have shown that by reasonable
Regulate and control the component of catalyst and change the pattern of catalyst, can effectively improve the activity of catalyst, reduce the overpotential of reaction.
Even so, the catalytic activity of the catalyst of transition metal base is still up for further improving.Therefore, by design and rational,
The ability that material that is simple, cheap, stablizing produces oxygen to improve electrode catalyst, which is prepared, with a kind of simple method many work
It does.
Invention content
For existing problem, problem to be solved by this invention is exactly by design and rational, and it is a kind of efficient, novel to provide
Effective drop of reaction overpotential is realized in the preparation of nitrogen oxide catalyst electrode and its application in terms of electro-chemical water decomposition
It is low.
To achieve the goals above, the present invention mainly adopts the following technical scheme that,
A kind of preparation method of efficient, novel porous nitrogen oxides nanometer sheet catalyst electrode, includes the following steps：
1) presoma Co (OH)2The preparation of nanometer sheet：
Configure 5-10mM Co (NO3)2Solution as electrolyte, under room temperature, using Graphite as working electrode, stone
Frotton is to electrode, and mercury/mercuric oxide electrode is reference electrode, and under conditions of -1.42V, electrochemical deposition obtains Co (OH)2
Nanometer sheet, the Co (OH)2The thickness of nanometer sheet is 10-20nm；
2)Co3O3.62N0.38The preparation of/Graphite：
The presoma that will be obtained in step 1), in 380-420 degrees Celsius of NH30.5h or more is calcined under ambient conditions, with
Cooled to room temperature obtains Co afterwards3O3.62N0.38/ Graphite electrodes.
Preferably, the NH3Atmosphere is the NH that ammonia level is 103/N2Gaseous mixture.
Preferably, the calcination temperature is preferably 400 DEG C.
The invention also discloses efficient, the novel porous nitrogen oxides nanometer sheet catalyst that a kind of the method is prepared
Electrode；The electrode is Co3O3.62N0.38/ Graphite electrodes；Its current density is 10mA/cm2When, required overpotential
Only 0.23V, the catalyst have porous nano chip architecture, the Co3O3.62N0.38With spinel structure.
The invention discloses porous nitrogen oxides nanometer sheet catalyst electrode the answering in electrochemical decomposition aquatic products oxygen
With.Electro-chemical test shows in 1.0M KOH solutions, Co3O3.68N0.32Catalyst has low overpotential (0.23V, electric current
Density is 10.0mA/cm2), lower Tafel values are 48mV/decade, and therefore, binary catalyst presents good electricity and urges
Change activity, solve high cost well and exceeds potential problem.
Compared with the existing technology, the present invention has the following advantages：
1. synthesis technology is simple, catalyst is synthesized by the method for electro-deposition and calcining, simplifies technological process.
2. electrolysis water current potential is substantially better than the prior art, overpotential is only 0.23V, hence it is evident that other most transition metal
Base catalyst.
3. low overpotential causes to generate larger electric current under the voltage of reduction, to generate at lower voltages more
More oxygen and hydrogen.
4. electrochemical analysis means and theoretical calculation prove, catalyst has excellent electric conductivity and the suction to intermediate product
Attached ability, this is also the reason of catalyst shows excellent catalytic performance place.
Description of the drawings
Fig. 1-1 shows Co of the embodiment 1 by scanning electron microscopic observation3O4/ Graphite shape appearance figures；
Fig. 1-2 shows that embodiment 1 obtains Co by x-ray photoelectron spectroscopy3O4The XPS of/Graphite schemes；
Fig. 2-1 shows Co of the embodiment 2 by scanning electron microscopic observation3O3.68N0.32/ Graphite shape appearance figures；
Fig. 2-2 shows that embodiment 2 obtains Co by x-ray photoelectron spectroscopy3O3.68N0.32The XPS of/Graphite schemes；
Fig. 3-1 shows the shape appearance figure for the sample that embodiment 3 is 200 DEG C by scanning electron microscopic observation annealing temperature；
Fig. 3-2 shows the shape appearance figure for the sample that the annealing temperature that embodiment 3 passes through scanning electron microscopic observation is 300 DEG C
Fig. 3-3 shows the shape appearance figure for the sample that the annealing temperature that embodiment 3 passes through scanning electron microscopic observation is 500 DEG C
Fig. 4-1 shows the electrode polarization curve graph for the sample that the different annealing temperature of embodiment 4 obtain；
Fig. 4-2 shows the catalyst electrode Co in embodiment 43O4/ Graphite and Co3O3.68N0.32/ Graphite's
Tafel；
Fig. 4-3 shows the catalyst electrode Co in embodiment 43O4/ Graphite and Co3O3.68N0.32The electricity of/Graphite
Chemical impedance spectrogram；
Fig. 4-4 shows Co in embodiment 43O3.68N0.32The stability diagram of/Graphite electrodes；
Fig. 4-5 shows Co in embodiment 43O3.68N0.32The production oxygen efficiency curve graph of/Graphite electrodes；
Fig. 5-1 shows Co in embodiment 53O4/ Graphite and Co3O3.68N0.32The DOS of/Graphite electrodes schemes；
Fig. 5-2 shows Co in embodiment 53O4/ Graphite and Co3O3.68N0.32The electron spin of/Graphite electrodes is total
Shake spectrogram；
Fig. 5-3 shows Co in embodiment 53O4/ Graphite and Co3O3.68N0.32The adsorption free energy figure of/Graphite.
Specific implementation mode
Comparative example 1
It is 0.2826cm by geometric area2Graphite flake (diameter 0.6cm, thickness 0.1cm), successively use deionized water, nothing
Water-ethanol and acetone are cleaned by ultrasonic 30 minutes, remove the organic matter on surface.It places in an oven, 40 degree of dryings 12 hours are spare.
Dried graphite flake is fixed on to the bottom of electrode bar (polytetrafluoroethylene (PTFE) shell inside has conductive copper rod) with conductive silver glue, is made
For an electrode.
Using graphite flake (Graphite) electrode as working electrode, stone mill stick is to electrode, and Mercurous sulfate electrode is reference electricity
Pole.Electrodeposit liquid is the Co (OH) of 10mmol/L2Solution, volume are 60mL.Before electrodeposit reaction starts, electrolyte expose into
30min high pure nitrogens will also be continually fed into N in addition in reaction process2.Electro-deposition current potential is -1.42V (vs.Hg/Hg2SO4), it sinks
The product time is 15min.After deposition terminates, sample ultrapure water is clean, 60 degree of dryings 12 hours.
Co is obtained using the method for annealing3O4Catalyst electrode.By above-mentioned Co (OH)2/ Graphite is placed in tube furnace
In, reaction is passed through nitrogen half an hour in advance before starting, and with the oxygen in cleared tube furnace, reaction is continually fed into the gas after starting
Body, until being down to room temperature after reaction.Then with the heating rate of 5 DEG C/min, temperature is risen to 400 DEG C, the reaction time 2
Hour.After reaction, it is naturally cooling to room temperature, obtains Co3O4/ Graphite catalyst electrodes.It is obtained by scanning electron microscope
Co3O4The pattern picture of/Graphite is as Figure 1-1, if the XPS 1-2 obtained by x-ray photoelectron spectroscopy.
Embodiment 1
The pretreatment of graphite flake and presoma Co (OH)2Preparation method with embodiment 1.
Co is obtained using the method for annealing3O3.68N0.32Catalyst electrode.By above-mentioned Co (OH)2/ Graphite is placed in
In tube furnace, reaction is passed through the NH that ammonia level is 10 in advance before starting3/N2Gaseous mixture half an hour, with cleared tube furnace
In oxygen, reaction is continually fed into the gas after starting, until be down to room temperature after reaction.Then with the heating of 5 DEG C/min
Temperature is risen to 400 DEG C by rate, and the reaction time is 2 hours.After reaction, it is naturally cooling to room temperature, is obtained
Co3O3.68N0.32/ Graphite catalyst electrodes.The Co obtained by scanning electron microscope3O3.68N0.32The pattern picture of/Graphite
As shown in Fig. 2-1, illustrate that the pattern of catalyst is porous nano chip arrays.The formation of porous structure may be because of calcining atmosphere
For NH3, living radical, etching Co (OH) are generated at a high temperature of 400 degree2Nanometer sheet, so form porous structure.Pass through X-ray
If the XPS 2-2 that photoelectron spectroscopy obtains, illustrate that catalyst is made of Co, O, N, and element ratio is close to Co:O:N≈3：
3.62：0.38.The metering in composition formula of O and N and be 4, it may be possible to because of O in a part of N element substitution in reaction process
The position (forming Co-O keys) of element, the polymer-based group of a part of N and O formation-N-O-.
Embodiment 2
For experimentation with case study on implementation 2, variation is that the temperature of annealing is changed into 200 DEG C, 300 DEG C and 500 DEG C.It is logical
Pattern picture such as Fig. 3-1 (200 DEG C), 3-2 (300 DEG C) and 3-3 of sample under the different calcination temperatures that overscanning Electronic Speculum obtains
(500℃).At 200 DEG C, reaction temperature is low to be generated temperature without free radical, therefore the pattern of sample does not change.And temperature
When being increased to 300 DEG C, free radical starts to generate, but the amount of free radical is few, and etching reaction is slow, so the hole formed is compared
It is few.And as temperature is increased to 400 DEG C, the quantitative change of free radical is more, therefore will appear the porous structure such as figure.When temperature is increased to
When 500 DEG C, because temperature is excessively high, etching is violent, therefore fragmentation occurs in nanometer chip architecture.Therefore the catalyst obtained at 400 DEG C
Catalytic performance it is best, such as Fig. 4-1.
Embodiment 3
Using the electrochemical workstation of three-electrode system, 1M KOH solutions are electrolyte, are prepared under above-mentioned different condition
Sample is stone mill stick to electrode as working electrode, and reference electrode is Hg/HgO electrodes, measures the electrocatalysis characteristic of catalyst.
Before experiment, electrolyte is persistently exposed into 30 minutes N2Oxygen in exclusion system is continually fed into nitrogen in test process.Scanning speed
Rate is 10mV/s, and polarization of electrode curve graph is as shown in Fig. 4-1, the sample Co that is prepared under 400 DEG C of annealing temperatures3O3.68N0.32Tool
There are the catalytic efficiency most having, electric current 10mA-2When current potential be 0.23V.Therefore subsequent research is with Co3O3.68N0.32And Co3O4Make
For research object.As shown in the Fig. 4-2, Co3O3.68N0.32And Co3O4Tafel values be divided into 48 and 65mV/decade.As Fig. 4-3 institute
It is shown as Co3O3.68N0.32And Co3O4Electrochemical impedance figure, research shows that Co3O3.68N0.32Catalyst has smaller impedance.Surely
Qualitative test is tested using current versus time curve, test result such as Fig. 4-4, Co3O3.68N0.32The activity after testing 20 hours
It has no and is decreased obviously.Production oxygen efficiency curve such as Fig. 4-5 of electrode, the production oxygen efficiency of electrode is close to calculated value.
Embodiment 5
With Co3O3.68N0.32And Co3O4As research object, using the electronic structure of first principle Study of Catalyst.With
CP2K is calculation procedure, and the PBE functions of D3 corrections are describing the system.The number of U is 5.9eV in calculating process.Water decomposition is produced
The calculating of the Gibbs free energy of oxygen reaction usesFormula：Δ G=EDFT+ΔZPE–TΔS.Certainly using electronics simultaneously
The means for revolving resonance, further illustrate the change of the electronic structure of catalyst.As shown in Fig. 5-1 and 5-2, Co3O3.68N0.32It compares
In Co3O4, electric conductivity improves significantly.As shown in Fig. 5-3, Co3O3.68N0.32Have for reaction intermediate better
Adsorption energy.
Claims (5)
1. a kind of preparation method of efficient, novel porous nitrogen oxides nanometer sheet catalyst electrode, it is characterised in that including as follows
Step：
1) presoma Co (OH)2The preparation of nanometer sheet：
Configure 5-10mM Co (NO3)2Solution as electrolyte, under room temperature, using Graphite as working electrode, stone mill stick
For to electrode, mercury/mercuric oxide electrode is reference electrode, under conditions of -1.42V, electrochemical deposition obtains Co (OH)2Nanometer
Piece, the Co (OH)2The thickness of nanometer sheet is 10-20nm；
2)Co3O3.62N0.38The preparation of/Graphite：
The presoma that will be obtained in step 1), in 380-420 degrees Celsius of NH30.5h or more is calcined under ambient conditions, it is then natural
It is cooled to room temperature and obtains Co3O3.62N0.38/ Graphite electrodes.
2. preparation method according to claim 1, it is characterised in that the NH3Atmosphere is that ammonia level is 10
NH3/N2Gaseous mixture.
3. preparation method according to claim 1, it is characterised in that the calcination temperature is preferably 400 DEG C.
4. efficient, the novel porous nitrogen oxides nanometer sheet catalyst electrode that a kind of method as described in claim 1 is prepared,
It is characterized in that the electrode is Co3O3.62N0.38/ Graphite electrodes；Its current density is 10mA/cm2When, required mistake
Potential is only 0.23V, and the catalyst has porous nano chip architecture, the Co3O3.62N0.38With spinel structure.
5. a kind of porous nitrogen oxides nanometer sheet catalyst electrode answering in electrochemical decomposition aquatic products oxygen as claimed in claim 4
With.
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Cited By (1)
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| CN113106486A (en) * | 2021-02-26 | 2021-07-13 | 西安电子科技大学 | Preparation method of cobalt oxide rich in oxygen defects for electrocatalytic water decomposition oxygen analysis |
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