CN108374179B - A kind of preparation method and application of the compound nitrogen-doped carbon material of two cobaltous selenide of Fe2O3 doping - Google Patents
A kind of preparation method and application of the compound nitrogen-doped carbon material of two cobaltous selenide of Fe2O3 doping Download PDFInfo
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Abstract
The invention discloses a kind of preparation method and applications of compound nitrogen-doped carbon material of two cobaltous selenide of Fe2O3 doping.This method is using metal organic framework ZIF-67 as presoma, it etches to obtain the Fe-ZIF-67 of iron modification using ferric ion, Fe-ZIF-67 is subjected to charing and selenizing with selenium steam at high temperature, obtains the two cobaltous selenide (Fe-CoSe of Fe2O3 doping of N doping porous carbon load2@NC) powdered electrode material.By Fe-CoSe2@NC powder is made slurry brushing and Fe-CoSe is made on conductive paper of carbon fiber2@NC/CFP electrode.Fe-CoSe2The electrochemical catalysis H2-producing capacity index of@NC/CFP electrode are as follows: Tafel slope is 40.9mV/decade；Reach 10mA/cm2The overpotential of current density is -0.143V (vs RHE).Meanwhile there is this group of loading electrode excellent electrochemical stability apparent voltage fluctuation do not occur in 48 hours constant current stability tests.The combination electrode synthetic method is simple and efficient, is environmentally protective, and raw material and synthesis cost are low, is suitble to the industrial application of electrochemical decomposition aquatic products hydrogen, has extensive scientific meaning.
Description
Technical field
The present invention relates to a kind of electrocatalytic decomposition water combination electrode more particularly to a kind of efficient electrocatalytic decomposition aquatic products hydrogen are multiple
The preparation method and application of composite electrode, belong to water electrolysis hydrogen production field.
Background technique
With growing, serious environmental pollution and the future source of energy danger of the fossil energy consumptions amount such as global coal, petroleum
Machine is that the mankind must problems faced.Efficient, reproducible clean energy resource is developed, such as solar energy, wind energy, water energy, biomass
Energy and thus derivative electric energy, it is extremely urgent to improve its ratio in entire energy resource structure.In numerous new energies,
How to realize new energy storage and it is without interruption be a very crucial problem, wherein being translated into chemical energy is one
Main approach, such as electrolysis water hydrogen manufacturing.Efficient electrolysis aquatic products hydrogen catalyst is developed for improving water electrolysis hydrogen production process
The utilization efficiency of the middle energy is most important, so far, most efficiently produce hydrogen catalyst be noble metal platinum, but its high cost and
Scarcity limits its large-scale application in water electrolysis hydrogen production reaction.And it is based on the chemical combination of transition metal (iron, cobalt, nickel etc.)
Object presents good potential in electrolysis aquatic products hydrogen field, and cheap price and relatively high catalytic activity cause research people
The extensive concern of member.Therefore, to prepare cheap, efficient, stable transistion metal compound with a kind of simple method expensive to substitute
Metal platinum produces hydrogen material as electrode catalyst, is a job with important research meaning at present.
Summary of the invention
Problem to be solved by this invention is just to provide a kind of using simple mild preparation method, synthesizing efficient, cost
The electrolysis water catalysis low, stability is good produces hydrogen electrode material.
Another object of the present invention is to provide the preparation methods of electrolysis aquatic products hydrogen composite catalyzing electrode material.
The present invention has one to be designed to provide application method of the powdery electrode material in acidic electrolysis aquatic products hydrogen again.
The present invention mainly adopts the following technical scheme that realization:
A kind of preparation method of the compound nitrogen-doped carbon material of two cobaltous selenide of Fe2O3 doping, includes the following steps:
1) prepared by ZIF-67: by Co (NO3)2·6H2O and 2-methylimidazole are dissolved in methanol solvate respectively, room temperature condition
Lower mixing reaction, raw empurpled precipitating, as product ZIF-67 wash ZIF-67 precipitating repeatedly until being clarified
Colourless supernatant, sediment is centrifugated, drying for standby；
2) prepared by Fe-ZIF-67: by Fe (NO3)3·9H2O is dissolved in ethyl alcohol or water that obtain the ethyl alcohol containing ferric nitrate molten
Liquid or aqueous solution containing ferric nitrate；It takes product ZIF-67 obtained in step 1) to be dispersed in ethyl alcohol or water, slowly adds
Enter the ethanol solution containing ferric nitrate or the aqueous solution containing ferric nitrate, and stir, utilizes Fe3+The Hydrogen Proton etching that hydrolysis generates
ZIF-67 releases Co2+, with the consumption of Hydrogen Proton, Fe3+And Co2+Co-precipitation occurs on ZIF-67 particle, obtains iron modification
Fe-ZIF-67；
3)Fe-CoSe2@NC preparation: by Fe-ZIF-67 powder obtained in step 2) using selenium steam at 350-500 DEG C
Under the conditions of carry out charing and selenizing, obtain black powder N doping porous carbon load two cobaltous selenide combination electrode of Fe2O3 doping
Material, i.e. Fe-CoSe2@NC electrode material.
Preferably, in the step 1), Co (NO3)2·6H2The molar ratio range of O and 2-methylimidazole is 1:1-1:16,
Reaction time is 6-24 hours.
Preferably, the ZIF-67 and Fe (NO3)3·9H2The mass ratio of O is 2:1-8:1.
Preferably, in the step 3), charing and selenizing carry out in tube furnace, and selenizing charing is to carry with inert gas
Gas, selenizing carbonization condition be 400 DEG C reaction 1-4 hours.
The invention also discloses a kind of Fe-CoSe2The preparation method of@NC/CFP electrode, by the Fe-CoSe of preparation2@NC electricity
Slurry is made in pole material hybrid conductive carbon black, Kynoar dispersion, and slurry is uniformly brushed on conductive paper of carbon fiber, dry
Obtain Fe-CoSe2@NC/CFP electrode.
Preferably, Fe-CoSe2@NC dusty material and conductive black, Kynoar are according to mass ratio 1:(0.125-1):
(0.125-0.5) mixing, the upper Fe-CoSe of CFP2@NC effective active composition load capacity is 0.2-1mg/cm2。
Preferably, the drying process carries out under the conditions of 50 DEG C, and drying time is 12 hours.
The invention also discloses Fe-CoSe2Application of the@NC/CFP electrode in electrolysis aquatic products hydrogen.In 0.5MH2SO4Electrolysis
The electrochemistry carried out in liquid produces hydrogen test result and shows Fe-CoSe2@NC/CFP composite catalyzing electrode has high production hydrogen activity,
It, which is catalyzed, generates 10mA/cm2Current density only need the overpotential of -0.143V (vs.RHE), and surveyed in 48 hours constant currents
Excellent stability is shown during examination.
Compared with the existing technology, the invention has the following advantages that
1.Fe-CoSe2@NC/CFP water electrolysis hydrogen production overpotential is low, 10mA/cm2Overpotential is only -143mV.
2.Fe-CoSe2@NC/CFP water electrolysis hydrogen production Tafel slope is low, only 40.9mV/dec, slightly above noble metal platinum
(30mV/dec), lower Tafel slope illustrates that material can generate bigger electric current to drive under lower overpotential, to produce
Raw more hydrogen, improve the utilization efficiency of the energy.
3. electrode material synthesis technology is simple, reaction condition is mild, catalyst Fe-CoSe2@NC can be by being made slurry
Electrode use is made in brushing in conductive substrates, and process flow is simply controllable, is conducive to industrial operation.
Detailed description of the invention
Fig. 1 shows the ZIF-67 shape appearance figure that embodiment 2 passes through scanning electron microscopic observation；
Fig. 2 shows the Fe-ZIF-67 shape appearance figures that embodiment 2 passes through scanning electron microscopic observation；
Fig. 3 shows Fe-CoSe of the embodiment 2 by scanning electron microscopic observation2@NC shape appearance figure；
Fig. 4 shows ZIF-67, Fe-CoSe in embodiment 22@NC and CoSe2The crystalline state and crystalline structure of@NC characterizes；
Fig. 5 shows the Fe-CoSe in embodiment 42@NC/CFP and CoSe2@NC/CFP electrode linear scan volt-ampere curve；
Fig. 6 shows the Fe-CoSe in embodiment 42@NC/CFP and CoSe2The Tafel curve of@NC/CFP electrode；
Fig. 7 shows the Fe-CoSe in embodiment 42The current versus time curve of@NC/CFP electrode stability test；
Fig. 8 shows hydrogen actual production and theoretical yield versus time curve in embodiment 5.
Specific embodiment
Embodiment 1
The carbon fiber paper for being 2 square centimeters by geometric area successively spends dilute hydrochloric acid, ethyl alcohol, deionized water ultrasonic cleaning
30 minutes, remove the impurity such as metal ion and the organic matter on surface.Place in an oven, 50 DEG C drying 12 hours, it is spare.
Embodiment 2
ZIF-67 is prepared using solution deposit first, by 8mmol 2-methylimidazole and 2mmol cabaltous nitrate hexahydrate point
It is not dissolved in dissolution in 50ml methanol solution and obtains clear solution, is then stirred to react two kinds of solution mixed room temperatures 24 hours.
Then by reaction product centrifugation, washing, drying, pattern picture such as Fig. 1 institute of solid purple powder ZIF-67, ZIF-67 are obtained
Show, shows the granatohedron structure of standard.It takes 40mg ZIF-67 powder to be dispersed in 20ml ethanol solution, adds
Enter 5ml ferric nitrate ethanol solution (2mg/ml), is stirred to react under room temperature two hours, ZIF-67 is in Fe3+Hydrolyze the hydrogen generated
The corrasion of ion releases Co2+, with the consumption of Hydrogen Proton, Fe3+And Co2+Co-precipitation obtains iron on ZIF-67 particle
Then reaction product is centrifuged, is washed, is dried to obtain the solid powder Fe-ZIF-67 of purple, pattern by the Fe-ZIF-67 of modification
For picture as shown in Fig. 2, Fe-ZIF-67 maintains granatohedron structure, particle surface becomes coarse after etching.Then will
Fe-ZIF-67 uniformly spreads and is dispersed in porcelain boat, is put into tube furnace, using 100sccm argon gas as carrier gas, using selenium steam as reaction gas,
Two hours of high temperature selenizing are carried out under the conditions of 400 DEG C, obtain Fe-CoSe2@NC electrode material, pattern picture is as shown in figure 3, list
A Fe-CoSe2@NC particle still maintains granatohedron structure, and surface becomes more coarse.As a comparison, will not have
There is etched ZIF-67 powder to carry out same selenization, directly two hours of high temperature selenizing under the conditions of 400 DEG C, obtains
CoSe2@NC electrode material is with Fe-CoSe2@NC has similar pattern.ZIF-67,Fe-CoSe2@NC and CoSe2The crystallization of@NC
State and crystalline structure are as shown in figure 4, wherein Fe-CoSe2@NC and CoSe2Contain the good oblique cubic phase of crystallinity in@NC
Two cobaltous selenide crystal.
Embodiment 3
The above-mentioned Fe-CoSe that will be prepared2@NC dusty material and conductive black, Kynoar are according to mass ratio 5:4:1
Mixing is made slurry brushing with ethyl alcohol reconciliation and Fe-CoSe is made on CFP2@NC/CFP electrode, dry 12 under the conditions of 50 DEG C
Hour.By CoSe2@NC electrode material loads on CFP according to same ratio and brushing method, prepares CoSe2@NC/CFP electricity
Pole.Wherein Fe-CoSe2@NC and CoSe2Load capacity of the@NC active constituent on CFP is 0.5mg/cm2。
Embodiment 4
Using the electrochemical workstation of three-electrode system, the Fe-CoSe that will be prepared as described in Example 32@NC/CFP electrode
And CoSe2@NC/CFP electrode is as working electrode, and graphite rod is to electrode, and Ag/AgCl electrode is reference electrode, and electrolyte is
0.5M H2SO4Solution.Polarization curve sweep interval arrives -0.6V (vs.Ag/AgCl) for 0, sweep speed 3mV/s, Different electrodes
Polarization result as shown in figure 5, the Tafel curve that is calculated by polarization curve as shown in fig. 6, production hydrogen test result in figure
Show Fe-CoSe2@NC/CFP electrode reaches 10mA/cm2Current density only need -0.143V (vs.RHE), and it is undoped
CoSe2@NC/CFP electrode reaches 10mA/cm2Current density needs -0.173V (vs.RHE), Fe-CoSe2@NC/CFP electrode
And CoSe2The production hydrogen Tafel slope of@NC/CFP electrode is respectively 40.9mV/dec and 69.2mV/dec, therefore, Fe-CoSe2@
The H2-producing capacity of NC/CFP electrode is compared to CoSe2@NC/CFP electrode is obviously improved.Fe-CoSe2@NC/CFP electrode exists
10mA/cm2Under the conditions of constant current stability test data as shown in fig. 7, in 48 hours constant current test process, Fe-CoSe2@
The overpotential of NC/CFP electrode does not fluctuate significantly, shows good electrochemical stability.According to DFT theoretical calculation point
Analysis, Fe-CoSe2Crystal and CoSe2The production hydrogen activity site of crystal is mainly Co atom, and Fe-CoSe2The site Co in crystal
Reactive hydrogen adsorption free energy ratio CoSe2The site Co in crystal can accelerate the mistake being electrolysed in aquatic products hydrogen closer to zero
Cross the adsorption desorption process of state hydrogen, therefore Fe-CoSe2With higher catalytic activity.Embodiment 5
As described in Example 4, using the electrochemical workstation of three-electrode system, Fe-CoSe2@NC/CFP electrode is as work
Make electrode, graphite rod is to electrode, and Ag/AgCl electrode is reference electrode, and electrolyte is 0.5M H2SO4Solution.Electrolyte continues
It exposes into 30 minutes N2Oxygen in exclusion system is continually fed into nitrogen in test process.Apply 10mA constant current, every 30 minutes
A gas is taken, with hydrogen output in gas-chromatography test enclosed system.The curve that the yield of hydrogen changes over time such as Fig. 8,
Its practical hydrogen output measured is essentially identical to theoretical calculation yield, illustrates to be electrolysed during aquatic products hydrogen substantially without other pairs
Reaction occurs, Fe-CoSe2The current efficiency of@NC/CFP electrolysis aquatic products hydrogen is close to 100%.
Claims (8)
1. a kind of preparation method of the compound nitrogen-doped carbon material of two cobaltous selenide of Fe2O3 doping, includes:
1) prepared by ZIF-67: by Co (NO3)2·6H2O and 2-methylimidazole are dissolved in methanol solvate respectively, under room temperature
Reaction, raw empurpled precipitating is mixed, as product ZIF-67 washs ZIF-67 precipitating repeatedly until obtaining clarification nothing
The supernatant of color, sediment is centrifugated, drying for standby；
Characterized by further comprising following steps:
2) prepared by Fe-ZIF-67: by Fe (NO3)3·9H2O be dissolved in ethyl alcohol or water obtain the ethanol solution containing ferric nitrate or
Aqueous solution containing ferric nitrate；It takes product ZIF-67 obtained in step 1) to be dispersed in ethyl alcohol or water, is slowly added to contain
There are the ethanol solution of ferric nitrate or the aqueous solution containing ferric nitrate, and stir, utilizes Fe3+The Hydrogen Proton that hydrolysis generates etches ZIF-
67 release Co2+, with the consumption of Hydrogen Proton, Fe3+And Co2+Co-precipitation occurs on ZIF-67 particle, obtains iron modification
Fe-ZIF-67；
3) Fe-CoSe2@NC preparation: by Fe-ZIF-67 powder obtained in step 2 using selenium steam under the conditions of 350-500 DEG C
Charing and selenizing are carried out, the two cobaltous selenide combination electrode material of Fe2O3 doping of the N doping porous carbon load of black powder is obtained,
That is Fe-CoSe2@NC electrode material.
2. the preparation method of the compound nitrogen-doped carbon material of two cobaltous selenide of Fe2O3 doping according to claim 1, it is characterised in that
In the step 1), Co (NO3)2·6H2The molar ratio range of O and 2-methylimidazole is 1:1-1:16, and the reaction time is that 6-24 is small
When.
3. the preparation method of the compound nitrogen-doped carbon material of two cobaltous selenide of Fe2O3 doping according to claim 1, it is characterised in that
The ZIF-67 and Fe (NO3)3·9H2The mass ratio of O is 2:1-8:1.
4. the preparation method of the compound nitrogen-doped carbon material of two cobaltous selenide of Fe2O3 doping according to claim 1, it is characterised in that
In the step 3), charing and selenizing carry out in tube furnace, and selenizing is carbonized using inert gas as carrier gas, and selenizing carbonization condition is
400 DEG C reaction 1-4 hours.
5. a kind of Fe-CoSe2The preparation method of@NC/CFP electrode, it is characterised in that: prepare any one of claim 1-4 method
Fe-CoSe2Slurry is made in@NC electrode material hybrid conductive carbon black, Kynoar dispersion, and slurry is uniformly brushed in conduction
On carbon fiber paper, it is dried to obtain Fe-CoSe2@NC/CFP electrode.
6. Fe-CoSe according to claim 52The preparation method of@NC/CFP electrode, it is characterised in that: Fe-CoSe2@NC
Dusty material is with conductive black, Kynoar according to mass ratio 1:(0.125-1): (0.125-0.5) is mixed, the upper Fe- of CFP
CoSe2@NC effective active composition load capacity is 0.2-1mg/cm2。
7. Fe-CoSe according to claim 52The preparation method of@NC/CFP electrode, it is characterised in that the drying process
It is carried out under the conditions of 50 DEG C, drying time is 12 hours.
8. a kind of Fe-CoSe being prepared such as any one of claim 5-7 method2@NC/CFP electrode is in electrolysis aquatic products hydrogen
Using.
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