CN107620087A - A kind of FeOOH nickel-ferric spinel integration analysis oxygen electrode and preparation and application - Google Patents
A kind of FeOOH nickel-ferric spinel integration analysis oxygen electrode and preparation and application Download PDFInfo
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Abstract
The present invention relates to a kind of FeOOH nickel-ferric spinel integration analysis oxygen electrode being applied in alkaline medium and preparation and application；The application of electrode is in the oxygen evolution reaction being catalyzed under alkalescence condition during water electrolysis hydrogen production.Advantage：Nickel iron hydroxide integrated electrode morphology controllable；Preparation process is simple, mild condition；It can be used for water electrolytic cell hydrogen production by water decomposition under applying bias.There is preferable performance when FeOOH/nickel-ferric spinel integrated electrode prepared by the present invention is used as into alkaline solid polymer electrolyte (AEM) water electrolytic cell.The present invention has extensive value in regeneratable fuel cell (RFC), photoelectrocatalysis, electrolysis hydrogen generator device.
Description
Technical field
The present invention relates to a kind of electrolyzed alkaline water FeOOH/nickel-ferric spinel (FeOOH/NiFe LDHs) integration
Area load 2 is made by steps such as presoma mixing-hydro-thermal reaction-washing-vacuum drying in the preparation method of electrode, this method
~3 μm of height, the setting of 25~35nm thickness, crossing nanotube platy layer.The integrated electrode finally obtained under alkalescence condition as making
Analysis oxygen electrode, it can be applied in AEM water electrolysis, RFC or various electrolysis units.
Background technology
Water electrolysis provides the transformation routes of a cleaning from water to hydrogen.Such as used using production of renewable energy resources electric energy
With electrolysis water, CO can be veritably realized2Zero-emission.The hydrogen purity obtained in this way is very high, reachable
More than 99.9%, for requiring the manufacturing using the delicate electronic device of high-purity hydrogen, this is a kind of preferably former
Expect gas source.Water electrolysis hydrogen production technology ripe can be used before 50 years.But the hydrogen produced by this way is in the world
Proportion in hydrogen total output is still very small.Akaline liquid electrolytic cell water electrolysis is a kind of relatively ripe technology, 1902
The unit quantity run during year has just reached more than 400.The service life of alkaline water electrolytic cell can reach 15 years, alkalescence
Electrolytic cell water electrolysis technology turns into the most long commercialization water electrolysis hydrogen production technology of whole world run time.
Core in electrolytic process be electrochemical reaction carry out needed for elctro-catalyst, this directly influence electrolytic efficiency,
The life-span of electrolysis energy consumption, electrolysis cost and electrolytic cell.The base metal oxygen-separating catalyst used under alkalescence condition is directed in the recent period
The research of aspect has the trend gradually increased.
Patent CN201380011533.3 describes a kind of preparation method for preparing carbon load manganese oxide composite material.Should
Carbon load MnO described in methodxComposite oxygen evolution reaction electrode and carry out.Although the catalyst is in alkaline bar
There is good analysis oxygen electro catalytic activity, but the catalyst still has the shortcomings that it can not overcome under part.Carbon material is as load
The loaded catalyst of body support corrosion under the decomposition voltage of alkaline full electrolytic cell test is more serious, influences full electrolytic cell
The longtime running life-span.Liheng Wu et al. (ACS, 2015,137 (22), 7071-7074) describe one kind and use solvent heat-burning
The preparation method of single dispersing cobalt granule prepared by knot process.The a diameter of diameter of cobalt nano-particle prepared by this method exists
10nm or so spheric granules, its analysis oxygen electrocatalysis characteristic as oxygen-separating catalyst in 0.1M KOH solutions reach 0.39V@
10mA/cm2。
But current numerous results of study show, without using the integrated electrode of any binding agent or resin it is more traditional two
Member, or even the transition metal oxide of ternary have stronger applicability under alkaline medium condition, and can be in higher electrolysis electricity
Flow down (300~1000mA cm-2), long-term stable operation in strongly basic medium, be one of OER electrodes most potential at present.
Presoma, complexant are carried out a series of chemistry instead by this method using hydrothermal synthesis method under high temperature, alkalescence condition
Should, obtained FeOOH/nickel-ferric spinel (FeOOH/NiFe LDHs) then is made by steps such as washing-vacuum drying
Integration analysis oxygen electrode.Compared with the preparation method of traditional catalyst, hydrothermal synthesis method has that technique is simple, cost is cheap, just
In realizing the advantages such as industrialized production, compared with the pattern that synthetic catalyst is effectively controlled under temperate condition, there is preferably catalysis
Activity, and stability.
The content of the invention
It is an object of the invention to provide a kind of FeOOH used under alkalescence condition/nickel-ferric spinel (FeOOH/
NiFe LDHs) integration analysis oxygen electrode preparation method, ensure according to this method prepare integration analysis oxygen electrode can make
Electrolysis water reaction can efficiently be carried out under less applying bias.
To achieve the above object, the technical solution adopted by the present invention is：Using hydro-thermal reaction compared with being controlled under temperate condition
It is homogeneous to synthesize size, decentralization is good, the setting of the μ m-thick of thickness 2~3, crossing nanotube platy layer are carried on foam nickel base
On integrated electrode.
It need to prepare by precursor solution-hydro-thermal reaction-washing-vacuum drying after as integration analysis oxygen electrode；Take
Nickel inorganic salts and iron inorganic salts presoma, ammonium fluoride, urea, are dissolved them in aqueous solvent, to water under conditions of stirring
Middle addition surfactant, stirring is until obtain clear solution；Above-mentioned solution is transferred in hydrothermal reaction kettle, submergence is put in advance
Nickel foam in kettle, carries out hydro-thermal reaction under 100~180 DEG C of heating condition, and water heating kettle is cooled to room temperature；By what is obtained
Greenish-black foam nickel is washed；Electrode is transferred in vacuum drying chamber and dried, finally gives foamed nickel supported hydroxyl oxygen
Change iron-nickel-ferric spinel integrated electrode (FeOOH/NiFe LDHs@Ni foam) integrated electrode.
Specifically manufacturing process is：What is loaded in the integrated electrode nickel foam is included as nickel-ferric spinel, FeOOH；
The pattern feature that the catalyst layer of gained integrated electrode nickel foam upper epidermis load is final is 0.5~8 μm of height, 10
~100nm it is thick erect in nickel foam upper surface, crossing nanotube platy layer.
The preparation and mixing of precursor solution
I. the configuration of precursor solution is carried out from nickel inorganic salts, iron inorganic salts, controls the gross mass of precursor salt solution
In 0.1~1g or so；
Ii. solvent of the deionized water as hydro-thermal reaction is selected, dosage is controlled in 20~40mL；
Iii. from carry out speed of the fluorides such as ammonium fluoride as complexant control reaction, the usage amount of complexant is 1
~3g；
Iv. from urea as alkali source, the usage amount of urea is between 0.1~1g；The progress of hydro-thermal reaction：Hydro-thermal reaction
Institute's carry out condition should control 5~15h of hydro-thermal reaction under conditions of 100~180 DEG C；
Vacuum drying condition：Drying needs to be dried in vacuo 6~12h progress at 50~80 DEG C.
Stirring is to obtaining more than the time 30min of clear solution.
FeOOH-nickel-ferric spinel integration analysis oxygen electrode can water electrolysis hydrogen production process under applied catalysis alkalescence condition
In oxygen evolution reaction.
FeOOH-nickel-ferric spinel integration analysis oxygen electrode can be used as oxygen-separating catalyst to be urged applied to RFC, photoelectricity
During the electrolyzed alkaline water or alkaline medium electrolysis water of change, APE water electrolytic cells or alkaline water electrolytic hydrogen generator.
The integrated electrode prepared by this method has good analysis oxygen electrocatalysis characteristic and stability in the basic conditions.
Advantages of the present invention：
1st, hydrothermal synthesis method technique compared with template is simple, cost is cheap, is easy to implement industrialized production, gentleer
Under the conditions of effectively 0.5~8 μm of height of control synthesis, 10~50nm thick setting, crossing nanotube platy layer, the electrode, which has, well urges
Change Activity and stabill.
2nd, can be by controlling reaction condition and preparation parameter effectively to regulate and control the pattern of product.
3rd, compared with powder catalyst, FeOOH/nickel-ferric spinel (FeOOH/NiFe LDHs) of this law preparation
Integration analysis oxygen electrode has higher analysis oxygen catalytic activity, for the applying bias needed for water electrolytic cell hydrogen production by water decomposition more
It is small；Morphology controllable；Compared with carbon-supported analysis oxygen elctro-catalyst, there is more preferable stability.By the ferronickel integration electricity of preparation
Make that there is preferable performance during the oxygen evolution reaction of alkaline water electrolytic hydrogen-preparing in pole.Urged simultaneously in regeneratable fuel cell (RFC), photoelectricity
Change, have extensive value in electrolysis hydrogen generator device.
Brief description of the drawings
Fig. 1 are that precursor solution is using 0.261g nickel nitrates and 0.5g ferric nitrates as raw material；0.2g urea is as alkali source；
0.2g ammonium fluorides are as complexant；1.5g polyethylene glycol is as surfactant；Hydro-thermal reaction 5 hours；Reaction temperature is set to 120
℃.Control the FESEM images of the integrated electrode of synthesis.
Fig. 2 are FeOOH/nickel-ferric spinel (FeOOH/NiFe LDHs) integration obtained by step described in embodiment 1
Electrode；At normal temperatures, half-cell test is carried out in three-electrode system, using 1M KOH solutions as electrolyte, carries out linear volt-ampere
Scan obtained polarization curve.
Fig. 3 are nickel hydroxide integrated electrode obtained by step described in embodiment 1；At normal temperatures, enter in three-electrode system
Row half-cell is tested, and using 1M KOH solutions as electrolyte, carries out constant current test curve.
Fig. 4 are nickel hydroxide integrated electrode obtained by step described in embodiment 1；At normal temperatures, enter in three-electrode system
Row half-cell is tested, and using 1M KOH solutions as electrolyte, carries out the polarization curve that linear voltammetric scan obtains.
Fig. 5 are iron hydroxide integrated electrode obtained by step described in embodiment 1；At normal temperatures, enter in three-electrode system
Row half-cell is tested, and using 1M KOH solutions as electrolyte, carries out the polarization curve that linear voltammetric scan obtains.
Embodiment
Below in conjunction with the accompanying drawings, to FeOOH/nickel-ferric spinel (FeOOH/NiFe LDHs) integration analysis oxygen electrode
Preparation method, characteristic and application are described further：
Embodiment 1
Prepare：
(1) mixing of precursor solution：Using 0.261g nickel nitrates, 0.5g ferric nitrates as raw material, 0.2g urea is as alkali source；
1.5g polyethylene glycol is as surfactant；0.2g ammonium fluorides are as complexant；It is dissolved in 40mL deionized waters stirring 30min；
(2) hydro-thermal reaction：(1) solution is transferred in the 50mL hydrothermal reaction kettles of pre-set foam nickel substrate, done in air blast
The interior hydro-thermal reaction 5h under the conditions of 120 DEG C of dry case, water heating kettle furnace cooling, is made greenish-black foam nickel.Deionized water washing 3~
5 times, 60 DEG C of vacuum drying 8h, FeOOH/nickel-ferric spinel (FeOOH/NiFe LDHs) integration analysis oxygen electrode is made.
As seen from Figure 1, using hydro-thermal reaction compared with temperate condition control synthesis size it is homogeneous, decentralization is good
Good, 0.5~8 μm of height, 10~50nm thickness setting, crossing nanotube platy layer are carried on the integrated electrode in foam nickel base.
Half-cell is tested：Half-cell system is using the 1M KOH solutions of logical oxygen to saturation as electrolyte, integration electricity
Pole carries out LSV scannings, as shown in Figure 2,3.Using the integrated electrode that this method is prepared in 1M KOH electrolyte solutions
100mA/cm2Electrolytic current density under current potential be 1.565V (vs.RHE).In the 10mA/cm shown in Fig. 32Constant current survey
Examination, electrolytic potential remain unchanged substantially.The integrated electrode prepared by this method has good analysis oxygen electricity in the basic conditions
Catalytic performance and stability..
Embodiment 2
Iron hydroxide integrated electrode is prepared by 1 identical preparation process of embodiment, and the dosage of nickel nitrate is in presoma
0.7g, test condition is the same as embodiment 1.
Half-cell is tested：Half-cell system is using the 1M KOH solutions of logical oxygen to saturation as electrolyte, integration electricity
Pole carries out LSV scannings, as shown in Figure 2,3.Using the integrated electrode that this method is prepared in 1M KOH electrolyte solutions
100mA/cm2Electrolytic current density under current potential be 1.594V (vs.RHE).
Embodiment 3
Nickel hydroxide integrated electrode is prepared by 1 identical preparation process of embodiment, and the dosage of nickel nitrate is in presoma
0.8g, test condition is the same as embodiment 1.
Half-cell is tested：Half-cell system is using the 1M KOH solutions of logical oxygen to saturation as electrolyte, integration electricity
Pole carries out LSV scannings, as shown in Figure 2,3.Using the integrated electrode that this method is prepared in 1M KOH electrolyte solutions
100mA/cm2Electrolytic current density under current potential be 1.678V (vs.RHE).
Claims (7)
1. the preparation method of FeOOH-nickel-ferric spinel integrated electrode, it is characterised in that：
It need to prepare by precursor solution-hydro-thermal reaction-washing-vacuum drying after as integration analysis oxygen electrode；Take nickel without
Machine salt and iron inorganic salts presoma, ammonium fluoride, urea, are dissolved them in aqueous solvent, are added under conditions of stirring into water
Enter surfactant, stirring is until obtain clear solution；Above-mentioned solution is transferred in hydrothermal reaction kettle, submergence is previously placed in kettle
In nickel foam, hydro-thermal reaction is carried out under 100~180 DEG C of heating condition, water heating kettle is cooled to room temperature；It is blackish green by what is obtained
Color nickel foam is washed；By electrode be transferred in vacuum drying chamber dry, finally give foamed nickel supported FeOOH-
Nickel-ferric spinel integrated electrode (FeOOH/NiFe LDHs@Ni foam) integrated electrode.
2. according to the preparation method of the integrated electrode described in claim 1, it is characterised in that：
(1) what is loaded in the integrated electrode nickel foam is included as nickel-ferric spinel, FeOOH；
(2) the final pattern feature of the catalyst layer of gained integrated electrode nickel foam upper epidermis load is 0.5~8 μm of height, 10
~100nm it is thick erect in nickel foam upper surface, crossing nanotube platy layer.
3. according to the preparation method of the integrated electrode described in claim 1 or 2, it is characterised in that：
(1) preparation and mixing of precursor solution
I. the configuration of precursor solution is carried out from nickel inorganic salts, iron inorganic salts, controls the gross mass of precursor salt solution 0.1
~1g or so；
Ii. solvent of the deionized water as hydro-thermal reaction is selected, dosage is controlled in 20~40mL；
Iii. from carry out speed of the fluorides such as ammonium fluoride as complexant control reaction, the usage amount of complexant is in 1~3g；
Iv. from urea as alkali source, the usage amount of urea is between 0.1~1g；
(2) progress of hydro-thermal reaction
Hydro-thermal reaction, which carries out condition, should control 5~15h of hydro-thermal reaction under conditions of 100~180 DEG C；
(3) vacuum drying condition
Drying needs to be dried in vacuo 6~12h progress at 50~80 DEG C.
4. according to the preparation method of the integrated electrode described in claim 1,2 or 3, it is characterised in that：Stirring is transparent to obtaining
More than the time 30min of solution.
A kind of 5. integrated electrode of any preparations of claim 1-4.
A kind of 6. application of integration analysis oxygen electrode described in claim 5, it is characterised in that：FeOOH-nickel-ferric spinel
Integration analysis oxygen electrode can be under applied catalysis alkalescence condition during water electrolysis hydrogen production oxygen evolution reaction.
7. the application of oxygen electrode is analysed according to integration described in claim 6, it is characterised in that：FeOOH-nickel-ferric spinel
Integration analysis oxygen electrode can be applied to RFC, photoelectrocatalysis, APE water electrolytic cells or alkaline water electrolytic hydrogen as oxygen-separating catalyst
During the electrolyzed alkaline water or alkaline medium electrolysis water of generator.
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| CN108311151A (en) * | 2018-01-25 | 2018-07-24 | 北京化工大学 | A kind of analysis oxygen elctro-catalyst and preparation method thereof based on dilval/nickel cobalt oxide binary composite |
| CN108642516A (en) * | 2018-04-16 | 2018-10-12 | 青岛大学 | A method of large area prepares self-supporting high-performance and analyses oxygen electrode at room temperature |
| CN108660471A (en) * | 2018-02-11 | 2018-10-16 | 中国工程物理研究院材料研究所 | A kind of preparation method for the nickel-ferric spinel water oxygen polarizing electrode being supported on azepine graphite foam |
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