CN108716007A - The method for improving hydroxide electrocatalytic hydrogen evolution reactivity worth by Lacking oxygen engineering - Google Patents
The method for improving hydroxide electrocatalytic hydrogen evolution reactivity worth by Lacking oxygen engineering Download PDFInfo
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Abstract
The present invention relates to a kind of methods improving hydroxide electrocatalytic hydrogen evolution reactivity worth by Lacking oxygen engineering, include the following steps：Prepare Ni (NO3)2·6H2O or Fe (NO3)3·9H2O or Co (NO3)2·6H2The homogeneous solution of one kind and urea in O；Homogeneous solution is transferred to reaction kettle, nickel foam NF substrates is erect in reaction kettle, and then reaction kettle is put into drying box, 12-15h is kept the temperature at 100-150 DEG C, reaction kettle is then naturally cooled into room temperature；3) NF substrates are taken out to be cleaned and dried；With Ce (NO3)3·6H2O and NaCl is electrolyte, prepares electrolyte；To wait for NF@NiFe LDH or NF the@Ni (OH) of electro-deposition2Or NF@NiCo LDH are working electrode, in 0.25-0.5mAcm‑2Under current density, electro-deposition 10min obtains the preferable hydroxide electrode material of HER performances.
Description
Technical field
The invention belongs to electrochemical catalysis electrolysis water fields, and in particular to and it is a kind of by Supporting cerium oxide nano particle,
Lacking oxygen is introduced in hydroxide composite material, the method to improve hydroxide HER performances under alkaline environment.
Background technology
With the exhaustion of fossil energy and the getting worse of environmental pollution, a kind of cleaning of searching, sustainable energy become assistant officer
It need to solve the problems, such as.Currently, the clean energy resourcies such as wind energy, solar energy, Hydrogen Energy obtain very big concern, but solar energy and wind energy are by environment
Factor influences.Hydrogen Energy becomes the shortcut for solving environmental problem as a kind of clean energy resource laid in.It is reacted by cathode hydrogen evolution
(HER) and Oxygen anodic evolution reaction (OER) combination driving made of electrolysis water reaction be widely used as it is most promising, can hold
The technology of supervention exhibition for future society provides clean energy resource.
Up to now, due to low overpotential and quick kinetics, noble metal and its oxide be it is most effective and
The electrolysis water catalyst of most stability.However, high cost, low reserves limit the wider practical application of noble metal catalyst.
Therefore, there is an urgent need to design a kind of novel low cost, the elctro-catalysts of high reserves replaces noble metal catalyst.It is several recently
Year, transistion metal compound, including oxide, hydroxide, sulfide, phosphide, nitride, stannide and its alloy exist
Excellent electrolysis water performance is achieved under alkaline environment.
In alkaline environment, the OER overpotentials of hydroxide are relatively low, and kinetics is fast, but due to phonon in solution
Lack, causes its HER performance poor.However the direct half-reaction that HER produces hydrogen as electro-catalysis is even more important.To improve hydroxide
The HER performances of object under alkaline condition, researchers have done many work.Such as：Sheet hydroxide is removed into list
Layer, with the more active sites of exposure；It is combined with conductive substrate, promotes the electron-transport of material；Doped precious metal atom
To accelerate HER kineticses.However, the experiment condition of these methods and its harsh, the doping site of atom has uncertain
Property, the factors such as experimental method is complex limit its extensive use.Therefore, one kind is simple, more effectively improves hydroxide
HER performances method it is most important.
Lacking oxygen engineering is to improve the most important method of HER performances.Lacking oxygen not only contributes to the quick transmission of electronics,
H2The decomposition of O, OH-The absorption of group can also optimize hydrogen adsorption free energy.In addition, the missing of oxygen atom, produces more
Dangling bonds can change Electronic Structure, make semiconductor transition at highly conductive metalloid conductor.In pure metal oxides,
Lacking oxygen is readily available.The NiO for by ion-exchange obtaining that there is Lacking oxygen, CoO；Had by liquid phase stripping method
The WO of Lacking oxygen3-r；δ-MnO are obtained by hydro-thermal method2Deng.However, the lamella due to hydroxide is thicker, exposure atom is less
The features such as, cause the introducing Lacking oxygen in hydroxide still to face prodigious problem.
Ceria have good oxygen storage capacity, Ce ions+between trivalent and+4 valences be easy conversion, Surface Oxygen from
Transport factor is very high, therefore cerium oxide can promote the electronics transfer at hydroxide/oxide interface, is conducive to interface Lacking oxygen
Generation, and then be conducive to HER performances.Further, since the selective penetrated property of cerium oxide, will not hinder the OER performances of material, it is full
Our needs of foot.
Invention content
In view of the deficiencies of the prior art, the technical issues of present invention intends to solve be：There is provided it is a kind of by Lacking oxygen engineering come
The method for improving hydroxide HER performances under alkaline condition.The method that the present invention uses hydro-thermal, prepares hydroxide, then
By the method Supporting cerium oxide nano particle of a step electro-deposition, operating method is simple, of low cost, by regulating and controlling electro-deposition
Time can adjust the load capacity and oxygen vacancy concentration of cerium oxide, and then regulate and control the performance of composite material.Technical solution is as follows：
A method of hydroxide electrocatalytic hydrogen evolution reactivity worth is improved by Lacking oxygen engineering, is included the following steps：
1) it is 0.5-2mmol according to the amount of substance and volume：0.5-5mmol：The proportioning of 30-40ml, prepares Ni respectively
(NO3)2·6H2O or Fe (NO3)3·9H2O or Co (NO3)2·6H2One kind, deionized water in O and urea are made uniformly molten
Liquid；
2) above-mentioned homogeneous solution is transferred to reaction kettle, nickel foam NF substrates is erect in reaction kettle, and then by reaction kettle
It is put into drying box, 12-15h is kept the temperature at 100-150 DEG C, reaction kettle is then naturally cooled into room temperature；
3) the NF substrates in taking out 2), it is dry at 60 DEG C again after cleaning, obtain NF@NiFe LDH or NF@Ni (OH)2Or
NF@NiCo LDH；
4) with Ce (NO3)3·6H2O and NaCl is electrolyte, prepares electrolyte；
5) under three-electrode system, to wait for NF@NiFe LDH or NF the@Ni (OH) of electro-deposition2Or NF@NiCo LDH are work
Make electrode, Ag/AgCl is reference electrode, and platinized platinum is to electrode in 0.25-0.5mAcm-2Under current density, electro-deposition 10min is obtained
To the preferable hydroxide electrode material of HER performances.
Preferably, it is 2mM according to the amount of substance and volume：The proportioning of 10mM and 200mL prepares Ce (NO3)3·6H2O and
Electrolyte is made in NaCl electrolyte and deionized water.
The invention successfully introduces Lacking oxygen in hydroxide system, improves hydroxide under alkaline condition whereby
HER performances.Compared with the existing technology for improving hydroxide HER performances, present invention environmental protection, operating method is simple, cost
Cheap, repeatability is strong.By adjusting the time of electro-deposition, the concentration of Lacking oxygen can be regulated and controled, reach regulation and control composite wood whereby
Expect the purpose of HER performances.
Description of the drawings
The X-ray diffraction analysis figure spectrum that Fig. 1 is the NiFe LDH prepared by the embodiment of the present invention 1, can be seen that from collection of illustrative plates,
Prepared product is NiFe LDH；
Fig. 2 (a) is the scanning electron microscope image of the NiFe LDH prepared by the embodiment of the present invention 1, can therefrom be seen
It is sheet to go out NiFe LDH, and its piece thickness is about 15-20nm；Fig. 2 (b) is the NF@NiFe prepared by the embodiment of the present invention 1
LDH/CeOxTransmission electron microscope image, can be seen that from collection of illustrative plates, CeOxNanoparticle size is about 5nm, is distribution
On the lamella of hydroxide；
Fig. 3 is in the embodiment of the present invention 1, to describe NF@NiFe LDH/CeOxIn Lacking oxygen done EPR characterization.From
Find out in collection of illustrative plates, load C eOxLater, the oxygen vacancy concentration of material has obtained greatly being promoted；
Fig. 4 is the NF@NiFe LDH/CeO prepared by the embodiment of the present invention 1x, NF@NiFe LDH, NF and comparison Pt/C
Electrocatalytic hydrogen evolution reacts LSV curves, it is seen that load C eOxLater, the HER performances of material have obtained greatly carrying
It rises；
Fig. 5 is the NF@NiFe LDH/CeO prepared by the embodiment of the present invention 1x, NF@NiFe LDH, NF and comparison Pt/C
Electrocatalytic hydrogen evolution reacts Tafel curves, it is seen that CeOxAccelerate the HER kineticses of NiFe LDH；
Fig. 6 is the NF@NiCo LDH/CeO prepared by the embodiment of the present invention 2x, NF@NiCo LDH, electrocatalytic hydrogen evolution reaction
LSV curves, it is seen that CeOxImprove the HER performances of NiCo LDH；
Fig. 7 is the NF@Ni (OH) prepared by the embodiment of the present invention 32/CeOx, NF@Ni (OH)2, electrocatalytic hydrogen evolution reaction LSV
Curve, it is seen that CeOxImprove Ni (OH)2HER performances.
Specific implementation mode
The specific embodiment of preparation method of the present invention is given below.These embodiments are only used for that the present invention will be described in detail and prepare
Method is not intended to limit the application scope of the claims.
Embodiment 1
Prepare NF@NiFe LDH/CeOxComposite material, and improve NF@NiFe LDH HER performances under alkaline condition.
(1) by 0.5mmol Ni (NO3)2·6H2O and 0.5mmol Fe (NO3)3·9H2O is dissolved in the deionized water of 35mL
In, 5mmol urea is then added, magnetic agitation 30min obtains homogeneous solution；
(2) above-mentioned homogeneous solution is transferred in 50mL polytetrafluoroethyllining linings, then by NF (1*2cm2) it is perpendicular stand upright on it is poly-
It in tetrafluoroethene inner liner wall, is packed into reaction kettle, and then reaction kettle is put into the air dry oven of resistance control, at 100 DEG C
Lower heat preservation 12h, then naturally cools to room temperature by reaction kettle.；
(3) NF in (2) is taken out, it is three times with deionized water and alcohol rinse, dry at 60 DEG C in an oven, obtain NF
NiFe LDH；
(4) in the 2mM Ce (NO of 200mL3)3·6H2In O and 10mM NaCl electrolyte, using CHI660E electrochemistry works
It stands, under three-electrode system, using NF@NiFe LDH as working electrode, Ag/AgCl is reference electrode, and platinized platinum is to exist to electrode
0.25mAcm-2Under current density, electro-deposition 10min obtains the hydroxide electrode material of Supporting cerium oxide (i.e. with Lacking oxygen)
Material, and under the conditions of this current density and electrodeposition time, oxygen vacancy concentration is higher, electrode material HER performances are best.
Embodiment 2
Prepare NF@NiCo LDH/CeOxComposite material, and improve NF@NiCo LDH HER performances under alkaline condition.
(1) by 0.5mmolNi (NO3)2·6H2O and 1.0mmol Co (NO3)2·6H2O is dissolved in the deionized water of 35mL
In, 3mmol urea is then added, magnetic agitation 30min obtains homogeneous solution；
(2) above-mentioned homogeneous solution is transferred in 50mL polytetrafluoroethyllining linings, then by NF (1*2cm2) it is perpendicular stand upright on it is poly-
It in tetrafluoroethene inner liner wall, is packed into reaction kettle, and then reaction kettle is put into the air dry oven of resistance control, at 100 DEG C
Lower heat preservation 12h, then naturally cools to room temperature by reaction kettle.；
(3) NF in (2) is taken out, it is three times with deionized water and alcohol rinse, dry at 60 DEG C in an oven, obtain NF
NiCo LDH；
(4) in the 2mM Ce (NO of 200mL3)3·6H2In O and 10mM NaCl electrolyte, using CHI660E electrochemistry works
It stands, under three-electrode system, using NF@NiCo LDH as working electrode, Ag/AgCl is reference electrode, and platinized platinum is to exist to electrode
0.25mAcm-2Under current density, electro-deposition 10min obtains the hydroxide electrode material of Supporting cerium oxide (i.e. with Lacking oxygen)
Material, and under the conditions of this current density and electrodeposition time, oxygen vacancy concentration is higher, electrode material HER performances are best.
Embodiment 3
Prepare NF@Ni (OH)2/CeOxComposite material, and improve NF@Ni (OH)2HER performances under alkaline condition.
(1) by 1.25mmol Ni (NO3)2·6H2O is dissolved in the deionized water of 35mL, and 2.5mmol urine is then added
Element, magnetic agitation 30min, obtains homogeneous solution；
(2) above-mentioned homogeneous solution is transferred in 50mL polytetrafluoroethyllining linings, then by NF (1*2cm2) it is perpendicular stand upright on it is poly-
It in tetrafluoroethene inner liner wall, is packed into reaction kettle, and then reaction kettle is put into the air dry oven of resistance control, at 100 DEG C
Lower heat preservation 12h, then naturally cools to room temperature by reaction kettle.；
(3) NF in (2) is taken out, it is three times with deionized water and alcohol rinse, dry at 60 DEG C in an oven, obtain NF
Ni(OH)2；
In the 2mM Ce (NO of 200mL3)3·6H2In O and 10mMNaCl electrolyte, using CHI660E electrochemical workstations,
Under three-electrode system, with NF@Ni (OH)2For working electrode, Ag/AgCl is reference electrode, and platinized platinum is to exist to electrode
0.25mAcm-2Under current density, electro-deposition 10min obtains the hydroxide electrode material of Supporting cerium oxide (i.e. with Lacking oxygen)
Material, and under the conditions of this current density and electrodeposition time, oxygen vacancy concentration is higher, electrode material HER performances are best.
Claims (2)
1. a method of hydroxide electrocatalytic hydrogen evolution reactivity worth is improved by Lacking oxygen engineering, is included the following steps：
1) it is 0.5-2mmol according to the amount of substance and volume：0.5-5mmol：The proportioning of 30-40ml prepares Ni (NO respectively3)2·
6H2O or Fe (NO3)3·9H2O or Co (NO3)2·6H2One kind, deionized water in O and urea, are made homogeneous solution；
2) above-mentioned homogeneous solution is transferred to reaction kettle, nickel foam NF substrates is erect in reaction kettle, and then reaction kettle is put into
Drying box keeps the temperature 12-15h at 100-150 DEG C, reaction kettle is then naturally cooled to room temperature；
3) the NF substrates in taking out 2), it is dry at 60 DEG C again after cleaning, obtain NF@NiFe LDH or NF@Ni (OH)2Or NF@
NiCo LDH；
4) with Ce (NO3)3·6H2O and NaCl is electrolyte, prepares electrolyte；
5) under three-electrode system, to wait for NF@NiFe LDH or NF the@Ni (OH) of electro-deposition2Or NF@NiCo LDH are work electricity
Pole, Ag/AgCl are reference electrode, and platinized platinum is to electrode in 0.25-0.5mA cm-2Under current density, electro-deposition 10min is obtained
The preferable hydroxide electrode material of HER performances.
2. according to the method described in claim 1, it is characterized in that, amount and volume according to substance are 2mM：10mM and 200mL
Proportioning prepare Ce (NO3)3·6H2Electrolyte is made in O and NaCl electrolyte and deionized water.
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| CN110026208A (en) * | 2019-05-10 | 2019-07-19 | 安徽师范大学 | Ni-based three nickel composite array elctro-catalyst of layered double-hydroxide@curing of the iron of heterojunction structure and its preparation method and application |
| CN110129815A (en) * | 2019-04-24 | 2019-08-16 | 北京大学深圳研究生院 | Modified TM-LDH nano material, preparation method and application |
| CN110565113A (en) * | 2019-08-21 | 2019-12-13 | 井冈山大学 | Preparation method of composite electrocatalytic material for alkaline electrocatalytic hydrogen evolution |
| CN110975869A (en) * | 2019-11-01 | 2020-04-10 | 华侨大学 | Preparation method and application of magnetic oxygen vacancy iron-cobalt layered double hydroxide catalyst |
| CN111013607A (en) * | 2019-12-26 | 2020-04-17 | 福州大学 | Iron nickel sulfide with in-situ conversion sulfur vacancy as well as preparation method and application thereof |
| CN111229232A (en) * | 2020-03-20 | 2020-06-05 | 苏州大学 | Foam nickel-based porous NiFe hydrotalcite nanosheet and preparation and application thereof |
| CN111992219A (en) * | 2020-09-22 | 2020-11-27 | 北京大学深圳研究生院 | Novel nickel-iron electrolyzed water oxygen production catalyst and preparation method thereof |
| CN112002913A (en) * | 2020-08-20 | 2020-11-27 | 常州大学 | Oxygen-enriched vacancy tungsten oxide supported catalyst and preparation method thereof |
| CN114561655A (en) * | 2022-03-28 | 2022-05-31 | 河北工业大学 | Preparation method and application of rare earth cerium doped nickel sulfide/iron sulfide heterojunction material |
| CN115094456A (en) * | 2022-06-02 | 2022-09-23 | 吉林大学 | Preparation method and application of cerium dioxide nano particle/nickel-iron bimetal phosphide/foamed nickel composite electrode |
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| CN110129815B (en) * | 2019-04-24 | 2020-10-16 | 北京大学深圳研究生院 | Modified TM-LDH nano material, preparation method and application thereof |
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| CN110026208B (en) * | 2019-05-10 | 2022-07-08 | 安徽师范大学 | Heterostructure iron-nickel-based layered double hydroxide @ nickel disulfide compound array electrocatalyst and preparation method and application thereof |
| CN110026208A (en) * | 2019-05-10 | 2019-07-19 | 安徽师范大学 | Ni-based three nickel composite array elctro-catalyst of layered double-hydroxide@curing of the iron of heterojunction structure and its preparation method and application |
| CN110565113B (en) * | 2019-08-21 | 2021-03-26 | 井冈山大学 | Preparation method of composite electrocatalytic material for alkaline electrocatalytic hydrogen evolution |
| CN110565113A (en) * | 2019-08-21 | 2019-12-13 | 井冈山大学 | Preparation method of composite electrocatalytic material for alkaline electrocatalytic hydrogen evolution |
| CN110975869A (en) * | 2019-11-01 | 2020-04-10 | 华侨大学 | Preparation method and application of magnetic oxygen vacancy iron-cobalt layered double hydroxide catalyst |
| CN111013607A (en) * | 2019-12-26 | 2020-04-17 | 福州大学 | Iron nickel sulfide with in-situ conversion sulfur vacancy as well as preparation method and application thereof |
| CN111229232A (en) * | 2020-03-20 | 2020-06-05 | 苏州大学 | Foam nickel-based porous NiFe hydrotalcite nanosheet and preparation and application thereof |
| CN111229232B (en) * | 2020-03-20 | 2023-10-31 | 苏州大学 | Foam nickel-based porous NiFe hydrotalcite nano-sheet and preparation and application thereof |
| CN112002913A (en) * | 2020-08-20 | 2020-11-27 | 常州大学 | Oxygen-enriched vacancy tungsten oxide supported catalyst and preparation method thereof |
| CN111992219A (en) * | 2020-09-22 | 2020-11-27 | 北京大学深圳研究生院 | Novel nickel-iron electrolyzed water oxygen production catalyst and preparation method thereof |
| CN111992219B (en) * | 2020-09-22 | 2022-12-20 | 北京大学深圳研究生院 | Novel nickel-iron electrolyzed water oxygen production catalyst and preparation method thereof |
| CN114561655A (en) * | 2022-03-28 | 2022-05-31 | 河北工业大学 | Preparation method and application of rare earth cerium doped nickel sulfide/iron sulfide heterojunction material |
| CN115094456A (en) * | 2022-06-02 | 2022-09-23 | 吉林大学 | Preparation method and application of cerium dioxide nano particle/nickel-iron bimetal phosphide/foamed nickel composite electrode |
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Application publication date: 20181030 |