CN110230073A - A kind of preparation method of metal-layered double hydroxide combination electrode material - Google Patents
A kind of preparation method of metal-layered double hydroxide combination electrode material Download PDFInfo
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- CN110230073A CN110230073A CN201910446942.5A CN201910446942A CN110230073A CN 110230073 A CN110230073 A CN 110230073A CN 201910446942 A CN201910446942 A CN 201910446942A CN 110230073 A CN110230073 A CN 110230073A
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Abstract
The present invention relates to a kind of metal-layered double hydroxide combination electrode material preparation methods, and metallic substrates is taken to be placed in hydrothermal reaction kettle, are added the nitrate and urea of two kinds of metals, and hydro-thermal reaction is to get arriving purpose product.Compared with prior art, the present invention prepares alloy/double hydroxide nano chip arrays self-support type electrode with boundary layer enhancing using hydro-thermal method, the material had both had the excellent conductivity of base metal material and the multifunctionality of surface vertical nanowires chip arrays structure, simultaneously again because its special boundary layer generates humidification, starting overpotential needed for greatly reducing reaction, so that the oxygen of sandwich generates electrocatalysis characteristic and increases substantially.
Description
Technical field
The invention belongs to combination electrode material preparation technical fields, and it is multiple to be related to a kind of metal-layered double hydroxide
The preparation method of composite electrode material.
Background technique
With the growing energy demand of the mankind, electrolysis water is as a kind of green sustainable technologies, increasingly by people
Concern.As the hydrogen evolution reaction (HER) of one of electrolysis water technology half-reaction, it is excellent that reaction possesses great thermodynamics
Gesture, and catalytic mechanism research is more mature perfect.In comparison, oxygen evolution reaction (OER) is due to being related to the more of complexity
Heavy particle coupling and multielectron transfer process, cause oxygen evolution dynamics more slow, and need higher overpotential
To accelerate reaction to carry out.Thus, higher water oxygen overpotential limits the efficiency of all-hydrolytic reaction, becomes all-hydrolytic technology
Bottleneck.Therefore, high activity is prepared, the OER catalyst of low reaction overpotential is the committed step for improving all-hydrolytic technical efficiency.
Although the research of the base metal elctro-catalyst about OER has been achieved with greater advance, designing and synthesizing can be lower
The OER catalyst of overpotential driving larger current density still has larger challenge.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of double gold of metal-stratiform
The preparation method for belonging to hydroxide combination electrode material prepares alloy/bis- hydrogen-oxygens with boundary layer enhancing using hydro-thermal method
The self-support type electrode of compound nano-chip arrays, which had both had the excellent conductivity of base metal material and surface is hung down
The multifunctionality of straight nano-chip arrays structure, while being greatly reduced anti-because its special boundary layer generates humidification again
Required starting overpotential is answered, so that the oxygen of sandwich generates electrocatalysis characteristic and increases substantially.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of metal-layered double hydroxide combination electrode material, takes metallic substrates to be placed in hydro-thermal
In reaction kettle, it is added the nitrate and urea of two kinds of metals, hydro-thermal reaction is to get arriving purpose product.
Further, the metallic substrates obtain after washing its oxide layer by metal material.Metallic substrates are made
For the skeleton of whole combination electrode material, play the role of physical support, while being provided again for hydroxide nano chip arrays
Growth site, vertical-growth in situ contacts so that there is compound rear electrode material excellent electrical conductance and oxygen to generate performance.
Further, the metallic substrates are elemental metals or alloy foil sheet.
Further, the metallic substrates are iron, nickel or iron-nickel alloy sheet.
Further, the nitrate of two kinds of metals is respectively ferric nitrate and nickel nitrate.
Further, the molar ratio of the nitrate of two kinds of metals and urea is 1:1:10, two of them metal nitrate
Molar ratio can regulate and control ratio according to demand, and metal salt keeps certain proportion with urea, therefore molar ratio range applicatory is
(1~4): (1~4): (10~40).
Further, the process of hydro-thermal reaction specifically: the first hydro-thermal reaction 12h at 120 DEG C is placed in 80 DEG C again after cleaning
6h is heated in vacuum drying oven.
Research finds mainly have for hydro-thermal method for the growth and control of layered double hydroxide pattern
Two o'clock influence factor.Firstly, the reaction condition of hydro-thermal include reaction temperature and time all can be to layered double hydroxide
Crystal structure and grain size impact.The study found that at the same temperature, with the increase of hydro-thermal time, or
Person is under the same reaction time, the increase of hydrothermal temperature, then the crystallinity of layered hydroxide improves, and partial size increases.Secondly, adding
Agent is added to play an important role in the synthesis process.In initial reaction stage, with reaction speed is formed from additive and metal ion
Object control.Then, the particular crystal plane of the additive and the product acts on, so that the growth of the crystal face is limited, finally, system
It is standby to obtain thermodynamically stable two-dimensional sheet structured product.
The present invention is by forming chemistry under hydrothermal reaction condition between metallic substrates and layered double hydroxide
Key, at the composite material of metal and hydroxide nano array with specific interface layer: being made using alloy and metal material
For substrate, since liquid phase Situ Hydrothermal method is grown, layered duplex metal hydroxide nanometer chip arrays can be equal in metal material surface
Even vertical-growth；During the reaction, urea decomposes ammonification and carbonate, as interlayer anion.Generation is decomposed by urea
Carbanion tends to be adsorbed on (001) surface, has been passivated this plane, and nanometer sheet is more likely to vertical-growth, finally
Form the array of rock-steady structure；Electrolyte supply and electronics are provided while metal and alloy materials are as support metallic substrates
Transmission channels better ensure that the efficient progress of oxygen generating process, promote electrolysis water process.Simultaneously as the alloy prepared
With hydroxide electrode, centre forms middle layer and greatly facilitates to oxygen generation reaction rate, greatly reduces anti-
Overpotential should be started；The intermediate product that the hydroxide boundary layer formed during the growth process simultaneously generates reaction to oxygen again has
Superior adsorption energy.
In the present invention, layered double hydroxide material in situ vertical-growth is this to hang down on alloy and metallic substrates
The long nano-chip arrays of growing straight are not only that reaction intermediate provides many Nanoscale channels, and enable reaction intermediate into
Enter two-dimensional slice surface texture, more active sites are provided, it is ensured that each nanometer sheet is directly contacted with metal substrate.In turn
It is greatly promoted electronics transfer in layer, the synergistic effect between hydroxide layer and substrate provides for absorption OH intermediate
Advantageous localized chemical environment and suitable electronic structure, so that improving oxygen generates reaction rate.
Layered double-hydroxide material is during being grown in metallic substrates, in metallic substrates and layered bi-metal hydrogen-oxygen
It will form the hydroxide layer of metallic substrates between compound, this hydroxide layer interface is to can during electrocatalytic reaction
To be stabilized, and oxygen can be effectively facilitated and generate reaction rate.
It is excellent that the metal of preparation and the composite construction electrode material of layered double hydroxide had both had metal material
Conductivity, while the analysis oxygen attribute for having layered double hydroxide multi-functional and excellent, and substrate and hydroxide
The coupling hydroxide boundary layer that centre is formed, generates the hydrogen of electrolysis water and oxygen generation reaction has promotion catalytic action,
Can under extremely low overpotential precipitated oxygen, and can be directly used as self-support type electrode.Metal prepared by this material
And the method for hydroxide composite material can be applied not only in electrolysis water reaction, for photocatalytic water, light degradation and hydrogen reduction
Reaction, also available popularization and effective use.
Compared with prior art, the present invention utilizes the metal semiconductor composite material of chemical vapor deposition growth, by electric energy
It is converted into Hydrogen Energy, by the selection to metal base material and semiconductor growing reaction raw materials, different-shape, difference can be synthesized
The material of characteristic, which not only has stable physical structure, during electrolysis water, is also able to maintain stable performance.
Specifically, have the following advantages that and the utility model has the advantages that
(1) present invention uses metal or alloy as the metallic substrates of chemical hydro-thermal method synthesis nano-chip arrays, vertical former
Position growth nano-chip arrays, can be improved the stability and electric conductivity of the composite material of generation.
(2) metal and layered double hydroxide composite material that the present invention synthesizes, prepare simple, cheap, steady
It is qualitative good, it can be directly as self-support type electrode material, without load.
(3) present invention can adjust the condition of reaction by presoma raw material in adjusting hydrothermal method, can be in different gold
Belong to original position vertical-growth in substrate and goes out different nano-array combination electrode materials.
(4) the oxygen cleanliness without any pollution that the present invention generates, there is energy-saving and emission-reduction effect.
(5) metal and hydroxide composite material that the present invention synthesizes have extremely low oxygen evolution reaction overpotential, mention significantly
High electrolysis water efficiency, has excellent analysis oxygen performance.
Detailed description of the invention
Fig. 1 is that hydro-thermal method original position vertical-growth iron nickel laminated double hydroxide nanometer chip arrays show in different metal substrate
It is intended to；
Fig. 2 is the composite material electron scanning micrograph that metallic substrates are different-alloy or metal；
Fig. 3 is the composite material transmission electron microscope photo that metallic substrates are different-alloy or metal；
Fig. 4 is close for the iron nickel layered double-hydroxide composite material electrolysis water oxygen generation kinetic current grown in different base
Spend the variation relation figure with voltage；
Fig. 5 is that the combination electrode material in different metal base is electrolysed the Tafel curve figure that water oxygen generates reaction.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.The present embodiment is with technical solution of the present invention
Premised on implemented, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to
Following embodiments.
Embodiment 1
(1) iron-nickel alloy-iron nickel layered double-hydroxide preparation
Iron-nickel alloy sheet (20 × 40 × 0.3mm) is washed oxide on surface with acetic acid (2M) by process shown in Figure 1
Layer, is then successively cleaned by ultrasonic ten minutes in ethyl alcohol and deionized water.By six water nickel nitrates (0.5mmol), nine water ferric nitrates
(0.5mmol) and urea (5mmol) are dissolved in 36 milliliters of deionized water, are evenly stirred until and are completely dissolved.It then will be molten
Liquid is transferred in steel high-pressure water heating kettle, and then ready iron-nickel alloy paillon is totally immersed in reaction liquid.It will be close
The polytetrafluoroethyllining lining stainless steel autoclave (50ml) of envelope, which is transferred in baking oven at 120 DEG C, reacts 12h, then natural cooling
To room temperature.Then the iron-nickel alloy paillon after reaction is taken out, is rinsed for several times with ethyl alcohol, deionized water, vacuum baking is finally putting into
It is taken out after being kept for 6 hours at 80 DEG C in case.It finally can be obtained iron-nickel alloy-iron nickel layered double-hydroxide compound electric
Pole material.
The above-mentioned iron-nickel alloy being prepared-iron nickel layered double-hydroxide is used for electrolysis water oxygen evolution reaction again, specifically
Process is as follows:
Electrochemical measurement is tested on the electrochemical workstation of three-electrode configuration (CHI760 instrument).Electrolyte is
The KOH electrolyte of 0.1M, reference electrode are reversible hydrogen electrode, and platinum filament is to electrode.The potassium hydroxide solution for preparing 0.1M is made
For electrolyte, high purity oxygen gas 30 minutes are led into electrolyte to being saturated, keeps oxygen saturation state in electrolyte.Again with three electrodes
System, wherein working electrode is iron-nickel alloy-iron nickel layered double-hydroxide material by clip type, cyclic voltammetry
With the speed of sweeping of 10mV/s, scanning range is 1.0V to 1.8V, tests 15 circulations, obtains the current density of material under different voltages
Cyclic voltammetry curve.Tafel curve is to sweep fast 1mV/s in test condition, and scanning range is by the linear volt under 1.0V to 1.8V
Peace scanning curve obtains.In test process, in order to exclude the middle generation bubble interference of reaction process, using stirring magneton in electrode
Underface stirring, mixing speed 600rpm.Due to the electric conductivity that iron-nickel alloy base material is excellent, and it is vertical in situ raw
The high-specific surface area of long iron nickel double-hydroxide layer structure, which generates in the hydrogen of electrolysis water and oxygen generates reaction
There is great catalytic action.
Embodiment 2
(1) iron-iron nickel layered double-hydroxide preparation
The preparation of iron-iron nickel layered double-hydroxide: other than iron-nickel alloy paillon is replaced with iron foil piece, remaining and reality
It is identical to apply example 1.
(2) iron-iron nickel layered double-hydroxide is used for electrolysis water oxygen evolution reaction
Iron-iron nickel layered double-hydroxide is used for electrolysis water oxygen evolution reaction: with embodiment 1, but reaction efficiency is not
Together, as shown in Figure 4.Iron-iron nickel layered double-hydroxide, in the KOH electrolyte of 0.1M, oxygen evolution reaction is opened with 210mV's
Dynamic overpotential, and be 10mA/cm in electric current2When reaction overpotential be 390mV.
Embodiment 3
(1) nickel-iron nickel layered double-hydroxide preparation
Nickel-iron nickel layered double-hydroxide preparation: with embodiment 1, it is only necessary to which iron-nickel alloy paillon is replaced with nickel foil
Piece.
(2) nickel-iron nickel layered double-hydroxide is used for electrolysis water oxygen evolution reaction
Nickel-iron nickel layered double-hydroxide is used for electrolysis water oxygen evolution reaction: with embodiment 1, but reaction efficiency is not
Together, as shown in Figure 4.Iron-iron nickel layered double-hydroxide, in the KOH electrolyte of 0.1M, oxygen evolution reaction is opened with 220mV's
Dynamic overpotential, and be 10mA/cm in electric current2When reaction overpotential be 410mV.
Fig. 2 and Fig. 3 is respectively the combination electrode material in the different metal base obtained into embodiment 3 of embodiment 1
Electron scanning micrograph and transmission electron microscope photo, from figure 2 it can be seen that after hydro-thermal reaction, in three differences
Substrate metal paillon on it can be observed that generate one layer of uniform nano-chip arrays.Obviously, the nanometer sheet of hexagon is vertically given birth to
It grows on each metal foil, and then forms the iron nickel laminated double hydroxide nanometer array layer of even porous.Different base
The iron nickel layered double-hydroxide pattern of upper growth is similar, but size slightly difference.The hexagon nanometer grown on different paillons
Piece, thickness are about 15-25 nanometers, and size range is 400-650 nanometers.The transmission electron microscope photo of Fig. 3, shows simultaneously
The two-dimensional nano chip architecture of iron nickel layered double-hydroxide.
Fig. 4 is that the combination electrode material in the different metal base obtained into embodiment 3 of embodiment 1 is electrolysed water oxygen generation
For kinetic current density with the variation relation figure of voltage, test condition is the potassium hydroxide electrolyte in the 0.1M of oxygen saturation.From
It can be seen that iron-nickel alloy-iron nickel layered double-hydroxide at 1.25V (vs.RHE) in Fig. 4 after resnstance transformer,
It can be observed that the redox peaks pair of two, trivalent nickel element, and oxidation current peak when 1.35V is caused by oxygen evolution reaction.
In contrast, the current potential that the redox couple on the cyclic voltammetry curve of the catalyst on iron and nickel substrate occurs is higher.
Fig. 4 can be seen that iron-nickel alloy-iron nickel layered double-hydroxide has optimal analysis oxygen compared to other two kinds of iron, nickel substrate
Reactivity worth.Iron-nickel alloy-iron nickel layered double-hydroxide has reports that minimum reaction starting overpotential is only 90mV at present,
And electric current be 10mA/cm2When reaction overpotential be only 130mV, it is anti-far below iron or Ni-Fe nickel layered double-hydroxide
Answer overpotential.Illustration can find out the oxygen evolution reaction starting overpotential of three Different electrodes respectively in Fig. 4 and electric current is 10mA/
cm2Overpotential, be followed successively by 90mV/130mV, 210mV/390mV and 220mV/410mV.
Fig. 5 is that the combination electrode material in the different metal base obtained into embodiment 3 of embodiment 1 is electrolysed water oxygen generation
The Tafel curve figure of reaction, wherein its polarization curve from process resnstance transformer correction of Tafel curve, sweep speed are
1mV/s.It can be to show layered double hydroxide in different metal or alloy deeper into ground by Tafel curve
Oxygen evolution reaction activity on paillon substrate.With the iron in example 2-iron nickel layered double-hydroxide Tafel slope
(54.8mVdec-1) is compared with nickel in example 3-iron nickel layered double-hydroxide Tafel slope (57.6mVdec-1),
It is only 39.8mVdec-1 that iron-nickel alloy-iron nickel layered double-hydroxide, which has minimum Tafel slope, in example 1, into one
Step shows that it has highest electrolysis water OER catalytic activity in three examples.
For Hydrothermal Growth and control layered double hydroxide pattern, mainly there is two o'clock influence factor.It is first
First, the reaction condition of hydro-thermal include reaction temperature and time all can crystal structure and crystal grain to layered double hydroxide
Size impacts.The study found that at the same temperature, with the increase of hydro-thermal time, or in the same reaction time
Under, the increase of hydrothermal temperature, then the crystallinity of layered hydroxide improves, and partial size increases.Secondly, additive is in the synthesis process
It plays an important role.In initial reaction stage, reaction speed is controlled by the complex that additive and metal ion are formed.Then, described
The particular crystal plane of additive and the product acts on, so that the growth of the crystal face is limited, finally, to which thermodynamics be prepared
Stable two-dimensional sheet structured product.This research under hydrothermal reaction condition, metallic substrates and layered double hydroxide it
Between form chemical bond, at the composite material of metal and hydroxide nano array with specific interface layer: using alloy and
Metal material is as substrate, and since liquid phase Situ Hydrothermal method is grown, layered duplex metal hydroxide nanometer chip arrays can be in metal
The growth of material surface uniform vertical；During the reaction, urea decomposes ammonification and carbonate, as interlayer anion.By urea
It decomposes the carbanion generated to tend to be adsorbed on (001) surface, has been passivated this plane, nanometer sheet is more likely to vertically
Growth, ultimately forms the array of rock-steady structure.Therefore, the molar ratio of the total metal salt and urea that use keeps the proportion of 1:5, and
Two kinds of metal nitrates can regulate and control ratio according to demand, and then available metallic element is than different layered bi-metal hydrogen-oxygens
Compound nano-chip arrays structure.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (7)
1. a kind of metal-layered double hydroxide combination electrode material preparation method, which is characterized in that take metallic substrates
It is placed in hydrothermal reaction kettle, is added the nitrate and urea of two kinds of metals, hydro-thermal reaction is to get arriving purpose product.
2. a kind of preparation method of metal-layered double hydroxide combination electrode material according to claim 1,
It is characterized in that, the metallic substrates obtain after washing its oxide layer by metal material.
3. a kind of preparation side of metal-layered double hydroxide combination electrode material according to claim 1 or 2
Method, which is characterized in that the metallic substrates are elemental metals or alloy foil sheet.
4. a kind of preparation method of metal-layered double hydroxide combination electrode material according to claim 3,
It is characterized in that, the metallic substrates are iron, nickel or iron-nickel alloy sheet.
5. a kind of preparation method of metal-layered double hydroxide combination electrode material according to claim 1,
It is characterized in that, the nitrate of two kinds of metals is respectively ferric nitrate and nickel nitrate.
6. a kind of metal-layered double hydroxide combination electrode material preparation side according to claim 1 or 5
Method, which is characterized in that the nitrate of two kinds of metals and the molar ratio of urea are (1-4): (1-4): (10-40).
7. a kind of preparation method of metal-layered double hydroxide combination electrode material according to claim 1,
It is characterized in that, the process of hydro-thermal reaction specifically: the first hydro-thermal reaction 12h at 120 DEG C is placed in again in 80 DEG C of vacuum drying ovens after cleaning
Heat 6h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111197170A (en) * | 2020-02-24 | 2020-05-26 | 苏州科技大学 | Metal organic framework material/nickel-iron alloy composite electro-catalytic electrode and preparation method and application thereof |
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| CN106011911A (en) * | 2016-05-26 | 2016-10-12 | 重庆大学 | Method of partial vulcanization to improve oxygen evolution electrode performance of metal hydroxide |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106011911A (en) * | 2016-05-26 | 2016-10-12 | 重庆大学 | Method of partial vulcanization to improve oxygen evolution electrode performance of metal hydroxide |
Non-Patent Citations (1)
| Title |
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| QIAN XIANG ET AL: "In Situ Vertical Growth of Fe−Ni Layered Double-Hydroxide Arrays on Fe−Ni Alloy Foil: Interfacial Layer Enhanced Electrocatalyst with Small Overpotential for Oxygen Evolution Reaction", 《ACS ENERGY LETTERS》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111197170A (en) * | 2020-02-24 | 2020-05-26 | 苏州科技大学 | Metal organic framework material/nickel-iron alloy composite electro-catalytic electrode and preparation method and application thereof |
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