CN109852992A - Water nano-chip arrays electrode and its preparation method and application is decomposed in a kind of efficient electro-catalysis entirely - Google Patents
Water nano-chip arrays electrode and its preparation method and application is decomposed in a kind of efficient electro-catalysis entirely Download PDFInfo
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- Y02E60/30—Hydrogen technology
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Abstract
The invention discloses a kind of efficient electro-catalysis to decompose water nano-chip arrays electrode and its preparation method and application entirely.This method, using the method for chloride ion corrosion, prepares the electrode material with ultrathin nanometer chip arrays pattern using nickel foam as substrate.It, can be with the component of different metal in the more hydroxide of Effective Regulation by controlling the concentration of chloride ion and species of metal ion being added.The present invention has the Ni of ultrathin nanometer chip arrays pattern5Co3Mo-OH electrode presents excellent electrochemical catalysis and decomposes water H2-producing capacity (η10=52mV) and production oxygen performance (η100=304mV).Meanwhile the material is in 100mAcm‑2Under the conditions of can with stable operation 100h, have excellent electrochemical stability.In addition Ni5Co3Mo-OH can carry out the full water that decomposes as cathode and anode simultaneously and react, in 10mAcm‑2Voltage is 1.43V under current density condition.It is believed that development of this patent to preparing more metal hydroxides nano-chip arrays and providing new thinking, while more metal hydroxides being promoted to apply in terms of catalysis and the energy.
Description
Technical field
The present invention relates to the systems that electrochemistry decomposes water technical field more particularly to more metal hydroxides nano-chip arrays entirely
Preparation Method and its high-efficiency electrochemical decompose water application entirely.
Background technique
It is considered as a kind of environmental-friendly energy storage and the skill utilized that electrochemistry, which decomposes water entirely and generates hydrogen and oxygen,
Art.The best material of the aqueous energy of electrochemical decomposition is Pt/C, IrO at present2And RuO2Equal noble metal catalysts.However noble metal its
The problems such as expensive price and weak stability, so that these electrodes higher cost in industrial application, to limit it
Large-scale application in practice.Non-noble metallic materials, such as transition metal nitride, transition metal oxide, transition metal
Hydroxide and perovskite oxide can effectively catalyze water and generate hydrogen and oxygen, be expected to replace in electrochemical decomposition water field
For precious metal material.However, the activity and margin of stability due to these materials are formed on certain work pH range, as two
Application of electrode has certain challenge in total moisture solution.In addition, using unifunctional catalyst respectively as anode and cathode
It requires corresponding different production technology and equipment, causes the increase of production cost.Therefore, it develops same under alkaline condition
When have the excellent double-function catalyzing electrode for producing hydrogen and producing oxygen performance there is important application value.
In numerous transition metal electrodes, the hydroxide nano chip arrays based on foam nickel electrode are due to more
Active site, biggish active area, do not use the advantages that adhesive at faster electron transport rate, it is considered to be Yi Zhongyou
Different full decomposition water material.Such as the third metal is introduced into bimetallic Ni-Co or Ni-Mo double-hydroxide and forms ternary
Ni-Co-M or Ni-Fe-M catalyst can improve its electrocatalysis characteristic.Although having more document to more metal hydroxides
It is studied, but for the excellent difunctional hydroxide nano chip arrays for decomposing aqueous energy and electrochemical stability entirely
Research remains unchanged deficient.
In addition, the method for preparing more metal hydroxides nanometer sheets at present is mostly co-electrodeposition method, hydrothermal synthesis method, ion friendship
Change method and Fe+3Corrosion engineering method etc..However, since most of synthetic method is by synthesis temperature, anionic type and conjunction
At the influence of pH.Therefore, can only be used to synthesize double-metal hydroxide or three metal hydroxides.Such as stratiform emerging at present
Double-hydroxide (LDH) must contain trivalent metal ion and bivalent metal ion, and synthesize by stringent metal ratio, because
This limits the diversity of more metal hydroxides, to limit the development of more metal hydroxides.In conclusion lacking at present
A kind of method for preparing multicomponent and adjustable more metal hydroxides nano-chip arrays of weary mild simplicity.
When metal surface forms electrolyte layer, it may occur that galvanic interaction corrodes.In corrosion process, chlorine
Ion plays important role.This is because chloride ion can be adsorbed on metal surface more easily, to destroy its inertia
Protective layer, so that electrolyte layer is promoted to be formed, accelerated corrosion reaction.Under humid conditions, the oxygen in air and water are in yin
Pole is reduced generation hydroxyl, and metal hydroxides is then generated in conjunction with the metal ion of anode.Numerous researchs cause at present
For power in how to prevent the metal reaction that is not corroded from being destroyed, this research then utilizes corrosion reaction, is transformed into a kind of mildly making
The method of standby more metal hydroxides nano-chip arrays electrodes.
Summary of the invention
Problem to be solved by this invention is just to provide the mild chloride ion quarter corrosion made of metal of one kind and divides entirely for efficient
The method for solving water nano-chip arrays electrode, realizes that more metal hydroxide components are controllable, and passes through the ternary of synthesis
Ni5Co3Mo-OH nano-chip arrays bifunctional electrodes material improves electro-catalysis and produces hydrogen and produce oxygen performance, realizes and decompose answering for water entirely
With.And a kind of good idea and method is provided for the preparation of other more metal hydroxides nano-chip arrays electrodes.
To achieve the goals above, the present invention mainly adopts the following technical scheme that,
A kind of preparation method that water nano-chip arrays electrode is decomposed in efficient electro-catalysis entirely includes the following steps: in high concentration cl
At least one metal salt and nickel foam are added in solion；Control pH≤6 of initial reaction liquid；It is carried out under aerobic conditions anti-
It answers, obtains efficient electro-catalysis total moisture solution electrode, the concentration of the halide ion in the high concentration halide ion solution is greater than
50 mMs every liter.
Preferably, the nickel foam further includes pre-treatment step before being reacted, the pre-treatment step are as follows:
Foam nickel base is pre-processed by acid and solvent, removes the oxide layer on surface, nickel foam that treated drying is spare.
Preferably, the metal salt added in Chloride Solution is preferably two or more.
Preferably, the metal salt is metal halide salt, metal nitrate, metal sulfate, metal acetate salt；It is described
Metal salt metal cation redox potential be less than nickel ion.
Preferably, the concentration range of metal ion is greater than 0.5 mM every liter.
Water electrode is decomposed entirely the invention also discloses the efficient electro-catalysis produces hydrogen, production oxygen or full decomposition in efficient electro-catalysis
Application in water.The electrode is applied to hydrogen producing as the cathode of three-electrode system, and anode is applied to produce oxygen, Huo Zhezuo
It is applied to full decomposition water for the working electrode of bipolar electrode system.
Preferably, the step 1) foam nickel base is having a size of 2 × 2cm2。
Preferably, the step 1) concentration of hydrochloric acid is 1M；Hydrochloric acid, acetone and ethyl alcohol difference ultrasound 15min.
Preferably, the reaction condition are as follows: water bath with thermostatic control shaking table temperature is 30 DEG C, revolving speed 150rpm, and when reaction is a length of
12h。
A kind of Ni has been prepared using the above method in the present invention5Co3Mo-OH/ foamed nickel electrode material.
Using the electrochemical workstation of three-electrode system, Ni5Co3For Mo-OH/ nickel foam as working electrode, graphite rod is pair
Electrode, saturation Ag/AgCl are reference electrode, and electrolyte is 1M KOH solution, and 50 milliliters of 1M KOH solutions are added in electrolytic cell,
Constant potential+10mAcm-2Oxygen is collected under current density；-10 mA·cm-2Hydrogen is collected under current density.
Bipolar electrode system, Ni are taken in full decomposition water reaction5Co3Mo-OH/ nickel foam carries out electricity respectively as anode and cathode
It is catalyzed total moisture solution.Electrolyte is 50 milliliters of 1M KOH solutions, Ni5Co3The work area of Mo-OH/ nickel foam is respectively 1cm2,
In constant potential+10mAcm-2Oxygen is collected under current density；-10mA·cm-2Hydrogen is collected under current density.
The present invention utilizes chloride ion corrosion nickel foam, and is reacted using the electrochemical corrosion in Process of Metallic Corrosion,
The Co added in the metal cation Ni and solution of generation on cathode, Mo ion are shifted and are produced to anode jointly
Raw OH-It reacts, generates NiCoMo-OH nano-chip arrays.Electro-chemical test shows in 1M KOH solution, without fixed
The trimetallic catalyst Ni of type5Co3Mo-OH shows superior Hydrogen Evolution Performance (in -10mAcm-2It is excessively electric under current density
Gesture is 52mV), meanwhile, analysis oxygen performance is also very good (in+10mAcm-2Overpotential under current density is 304mV).Also,
Ni5Co3Mo-OH is in+100 and -100mAcm-2It can stablize respectively 100 hours under current density.Based on Ni5Co3Mo-OH
Good liberation of hydrogen and analysis oxygen performance, we are by Ni5Co3Mo-OH is applied to bipolar electrode system, Ni5Co3Mo-OH is in+10mAcm-2Voltage under current density is only 1.43V.In 100mAcm-2It can continue to keep 100 hours good steady under current density
It is qualitative.The performance is electro-catalysis effect best in the hydroxide reported at present.
Compared with the existing technology, the invention has the following advantages that
1. synthesis technology is simple, reaction condition is mild, catalysis electrode by the method one-step synthesis by chloride ion corrosion,
Simplify process flow.
2. synthetic method can regulate and control nanometer sheet component.Pass through species of metal ion and dense in control reaction solution
Degree, can be generated more metal hydroxides nanometer sheets of different component, extends the type of more metal hydroxides nanometer sheets.
3. electrode prepared by has excellent H2-producing capacity ((η10=52mV) and production oxygen performance (η100=304mV).Together
When the material in 100mAcm-2Under the conditions of can be with stable operation 100h.
4. electrode prepared by has difunctional electro catalytic activity.It is anti-that full decomposition water is carried out as cathode and anode simultaneously
It answers, in 10mAcm-2Voltage is only 1.43V under density conditions.
Detailed description of the invention
Fig. 1 is nano-chip arrays electrode material formation mechenism figure in embodiment 1.
The pattern picture of the nickel foam for the blank that Fig. 2-1, which is embodiment 1, to be obtained by scanning electron microscope；
Obtained nano-chip arrays under the conditions of the different chlorine ion concentrations that Fig. 2-2, which is embodiment 1, to be obtained by scanning electron microscope
The pattern picture of electrode；
The pattern of obtained nano-chip arrays electrode under the condition of different pH that Fig. 3, which is embodiment 2, to be obtained by scanning electron microscope
Picture；
Fig. 4 is that embodiment 2 passes through X-ray photoelectron spectroscopic analysis Ni5Co3Mo-OH nano-chip arrays element valence and each
The interaction of element；
Fig. 5-1 is to obtain Ni by transmission electron microscope in embodiment 35Co3Mo-OH nano-chip arrays pattern and distribution diagram of element；
Fig. 5-2 is Ni in embodiment 35Co3Mo-OH nano-chip arrays application of electrode produces the polarization curve of oxygen in anode；
Fig. 5-3 is Ni in embodiment 35Co3Mo-OH nano-chip arrays application of electrode produces the polarization curve of hydrogen in cathode；
Fig. 5-4 is Ni in embodiment 35Co3The current versus time curve of Mo-OH nano-chip arrays electrode stability test；
Fig. 6-1 is Ni in embodiment 45Co3Mo-OH nano-chip arrays application of electrode is in the performance test figure for decomposing water entirely；
Fig. 6-2 is Ni in embodiment 45Co3Mo-OH nano-chip arrays application of electrode is in the stability test figure for decomposing water entirely；
Fig. 7 is that embodiment 5 is obtained by scanning electron microscope through nanometer sheet prepared by regulation metal ion component and type
The pattern picture of array electrode.
Specific embodiment
Embodiment 1
Nano-chip arrays formation mechenism is as follows: in primary battery anode region, high concentration Cl-Solution can strengthen corrosion, will
Nickel foam is oxidized to Ni2+, subsequent Cl-It can constantly migrate to anode region and constantly be enriched with, as shown in formula 1；Water and sky simultaneously
Oxygen reaction in gas, is reduced to hydroxyl (OH in cathode zone-), as shown in formula 2；Final metal ions Mx+With Ni2+
In conjunction in foam nickel surface and OH-Reaction generates more metal hydroxides nano-chip arrays, as shown in formula 3.Its mechanism figure is such as
Shown in Fig. 1.According to this mechanism, implement following experiment.
Cathode:O2+2H2O+4e-→4OH- (2)
Ni2++Mx++(2+x)OH-→Ni-M-OH2+x (3)
It will be having a size of 2 × 2cm2Foam nickel base (thickness 1mm), be successively 1M hydrochloric acid, acetone and anhydrous second with concentration
Alcohol is cleaned by ultrasonic 15 minutes, removes the oxide on surface.Electrode surface liquid is dried up with argon gas, is put into spare in hermetic bag.It is logical
The pattern picture of the nickel foam for the blank that overscanning Electronic Speculum obtains is as shown in Fig. 2-1.The nickel foam of blank has 3 D pore canal knot
Structure, smooth surface.
Prepare reaction solution, liquor capacity 50mL.Reaction solution NaCl, CoCl2·6H2O and MoCl5It forms, wherein NaCl
Concentration is respectively 5mM, 50mM, 500mM and 1000mM, CoCl2·6H2O concentration is 0.5mM, MoCl5Concentration is 0.5mM.Solution
Initial pH value is adjusted to 3.5 by 1M hydrochloric acid.It is to be added anti-in 100mL conical flask that the nickel foam handled well, which is put into volume,
Solution is answered, and is sealed with preservative film.Reactor is placed in water bath with thermostatic control shaking table and is reacted.Water bath with thermostatic control shaking table temperature is 30
DEG C, revolving speed 150rpm, when reaction a length of 12h.Prepared nano-chip arrays electrode uses deionization after taking out in reactor
After water and ethyl alcohol are respectively washed three times, are dried up and saved with argon gas.Electrode is made under the conditions of various concentration chloride ion can be obtained such as Fig. 2-2
Shape appearance figure.It can be obtained from the figure that not observing a nanometer chip architecture under low chlorine ion concentration conditions；With chlorine ion concentration by
Cumulative height is grown into out nanometer chip architecture.
Embodiment 2
Referring to the electrode preparation method of embodiment 1, more metal hydroxides nanometer sheets are prepared under the conditions of different initial pH
Electrode.Reaction solution initial pH value is adjusted by 1M hydrochloric acid, is adjusted to 2,3.5,5.5 respectively.NaCl concentration is in reaction solution
0.5M, remaining reaction condition are same as Example 1.Prepared electrode in reactor after taking out, with deionized water and ethyl alcohol
After being respectively washed three times, is dried up and saved with argon gas.As Fig. 3 can obtain obtained more metal hydroxides under the conditions of different initial pH
Shape appearance figure.It can be obtained by Fig. 3, occur nanometer chip architecture in acid condition, and pH value is lower, nanometer chip size is bigger,
Quantity is more.
Embodiment 3
Referring to 1 the method for embodiment, NaCl concentration is 0.5M in reaction solution, under conditions of initial pH is 3.5,
Ni is prepared5Co3Mo-OH nano-chip arrays electrode.Fig. 4 is to pass through X-ray photoelectron spectroscopic analysis Ni5Co3Mo-OH receives
The valence state of the rice each element of chip arrays electrode.Fig. 5-1 is the Ni as obtained by scanning electron microscope and transmission electron microscope5Co3Mo-OH electrode
Pattern and distribution diagram of element.It can be obtained from the figure that resulting materials have nano-chip arrays structure, and each element is evenly distributed on and receives
In rice chip architecture.Fig. 5-2 shows the material in 10mAcm-2Under density conditions, the overpotential for producing hydrogen is respectively 52mV.Fig. 5-3
Show the material in 100mAcm-2Under density conditions, the overpotential for producing oxygen is respectively 304mV.Fig. 5-4 shows that the material exists
100mA·cm-2Under density conditions, electrochemical stability with higher.
Embodiment 4
Ni will be prepared in example 35Co3Mo-OH nano-chip arrays use bipolar electrode body as electrode in 1M KOH solution
It is the full decomposition water performance test carried out and stability test.It can be obtained by Fig. 6-1, the material is in 10mAcm-2Density conditions
Lower voltage is only 1.43V；Meanwhile can be obtained by Fig. 6-2, in 10mAcm-2And 100mAcm-2It is continually and steadily transported under current density
Row 100 hours.
Embodiment 5
Referring to 1 the method for embodiment, change different metal ions type and concentration in reaction solution, to more metal hydrogen-oxygens
The component and pattern of compound are regulated and controled.For monometallic Ni (OH)2The preparation of nanometer sheet, reaction solution, which is changed to concentration, is
The NaCl and concentration of 0.5M is the NiCl of 0.5mM2·6H2O.Reaction solution is changed to dense by the preparation for double-metal hydroxide
The CoCl that degree is 0.5M NaCl and concentration is 0.5mM2·6H2O.Preparation for more metal hydroxides, in the double gold of preparation
(i.e. NaCl (0.5M) and CoCl on the basis of the reaction solution of category oxide2·6H2O (0.5/n mM)), it is separately added into FeCl3·
6H2O, CuCl2·2H2O,MoCl5,MnCl2·4H2O, and ZnCl2, concentration is 0.5/n mM, and n represents the type of metal.Such as
Fig. 7, which can be obtained, obtains the pattern and distribution diagram of element of different more metal hydroxides by scanning electron microscope and transmission electron microscope.It can by figure
, different metal salting liquid produces nanometer sheet, and element is evenly distributed in nanometer chip architecture.
Embodiment 6
Referring to 1 the method for embodiment, change the anionic type of different metal salt in reaction solution, to more metal hydrogen-oxygens
The component and pattern of compound are regulated and controled.Preparation for double-metal hydroxide, it is 0.5M that reaction solution, which is changed to concentration,
Co (the NO that NaCl and concentration are 0.5mM3)·6H2O.Preparation for more metal hydroxides nanometer sheets, is preparing bimetallic
(i.e. NaCl (0.5 M) and Co (NO on the basis of the reaction solution of oxide nano-slice3)·6H2O (0.5/n mM)), it is separately added into
Fe(NO3)3·9H2O,Mn(CH3COO)2·4H2O, and Zn (CH3COO)2·2H2O, concentration are 0.5/n mM, and n represents metal
Type.
Claims (9)
1. the preparation method that water nano-chip arrays electrode is decomposed in a kind of efficient electro-catalysis entirely, it is characterised in that include the following steps:
At least one metal salt and nickel foam are added in high-concentration chlorine ion solution；Control pH≤6 of initial reaction liquid；In aerobic item
It is reacted under part, obtains efficient electro-catalysis total moisture solution electrode, the halide ion in the high concentration halide ion solution
Concentration be greater than 50 mMs every liter.
2. preparation method according to claim 1, it is characterised in that the nickel foam further includes before being reacted
Pre-treatment step, the pre-treatment step are as follows: foam nickel base is pre-processed by acid and solvent, removes the oxygen on surface
Change layer, nickel foam that treated drying is spare.
3. preparation method according to claim 1, it is characterised in that the metal salt added in Chloride Solution is preferably two
Kind is two or more.
4. preparation method according to claim 1 or 3, it is characterised in that the metal salt is metal halide salt, metal
Nitrate, metal sulfate, metal acetate salt；The redox potential of the metal cation of the metal salt be less than nickel from
Son.
5. preparation method according to claim 1, it is characterised in that the concentration range of metal ion is greater than 0.5 mM often
It rises.
6. water nano-chip arrays electrode is decomposed in efficient electro-catalysis prepared by a kind of method as described in claim 1 entirely.
7. electrode according to claim 6, it is characterised in that water nano-chip arrays are decomposed in prepared efficient electro-catalysis entirely
Electrode, has nano-chip arrays pattern, and nanometer sheet thickness is 2~30nm.
8. efficient electro-catalysis described in a kind of claim 6 decomposes water electrode entirely and produces hydrogen in efficient electro-catalysis, produces oxygen or decompose water entirely
In application.
9. application as claimed in claim 8, it is characterised in that the electrode is applied to produce hydrogen as the cathode of three-electrode system
Gas, anode are applied to produce oxygen, or the working electrode as bipolar electrode system is applied to full decomposition water.
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| CN111822000A (en) * | 2020-06-11 | 2020-10-27 | 安徽师范大学 | Pt nanoparticle loaded molybdenum dioxide/nickel hydroxide nanosheet array structure material and preparation method and application thereof |
| CN112575348A (en) * | 2020-12-25 | 2021-03-30 | 中南大学 | NF-NiFeOx(OH)y-S electrode, its preparation and application as OER catalytic material |
| US11390958B2 (en) * | 2019-03-12 | 2022-07-19 | De Nora Permelec Ltd | Alkaline water electrolysis method and alkaline water electrolysis anode |
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| CN109852992B (en) | 2020-04-28 |
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