CN107326392B - A kind of preparation method of liberation of hydrogen oxygen-separating catalyst - Google Patents
A kind of preparation method of liberation of hydrogen oxygen-separating catalyst Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of liberation of hydrogen oxygen-separating catalyst, comprising the following steps: (1) prepares nickel foam substrate, pre-process to nickel foam substrate；(2) in situ synthesis prepares NaOH solution, NaOH solution and nickel foam is mixed into reaction kettle and reacted, is rinsed after the reaction was completed to nickel foam, dry, obtains Ni (OH)2/ foam nickel electrode；(3) electrodeposition process, with KMnO4For manganese source, electrodeposit liquid is prepared, inertia graphite electrode is anode, Ni (OH)2/ foam nickel electrode is cathode, and additional constant current carries out electro-deposition, MnO is prepared2‑Ni(OH)2/ foam nickel electrode.The preparation method of liberation of hydrogen oxygen-separating catalyst of the present invention prepares MnO using growth in situ and electrodeposition process2‑Ni(OH)2/ nickel foam, MnO2、Ni(OH)2It is carried in nickel foam in micron shape, improves the surface area of former foamed nickel electrode material, promote the electro catalytic activity of electrode.By Ni (OH)2And MnO2Compound liberation of hydrogen oxygen-separating catalyst MnO2‑Ni(OH)2/ nickel foam can be used as the anode and cathode of electrolytic water device.
Description
Technical field
The present invention relates to electrolysis water technical field, in particular to a kind of preparation method of liberation of hydrogen oxygen-separating catalyst.
Background technique
The energy and environment are basis for the survival of mankind, the power of social sustainable development.Currently, world energy sources mainly come
Derived from fossil energies such as coal, oil and natural gas, the process formed is very very long, and with the surge of population in the world and warp
The development of Ji, the mankind are much larger than its cumulative speed to the exploitation rate of fossil energy.Meanwhile discharge is a large amount of when fossil energy burning
The pollutants such as carbon dioxide, nitrogen oxides and dust, bring the environmental problems such as haze, acid rain and greenhouse effects, it is serious
Threaten the health and existence of the mankind.In certain degree, the mankind have been further exacerbated by the energy crisis and environmental problem in the world.
But in order to solve current energy crisis and environmental problem, the sustainable development of Lai Shixian human society and environment, we are in addition to wanting
It boosts environmental awareness, focuses on ecological protection, more urgent is to find new alternative energy source and clean energy resource, especially renewable
The energy.
Now, existing renewable energy includes solar energy, wind energy, water energy, geothermal energy, tide energy etc., these energy are equal
From the sun, can repeat to generate utilization.And people to the development and utilization of renewable resource had very great development and
Progress, but since these energy are influenced by many factors such as weather, geography in transducing and energy storage mode, in practical life
Intermittent energy supply can only be carried out in work.And Hydrogen Energy as can store, efficiently, cleaning and reproducible new energy, become 21 century
Most potential clean energy resource, but how sustainable real estate hydrogen to be the following mankind step into that hydrogen economy first has to solve
Problem.
Hydrogen is prepared using solar energy electrolyzing water, it is considered to be most promising and sustainable production hydrogen approach, but current phase
The development of electrolytic hydrogen production technology is limited to expensive electrolysis water cost.The Gibbs free energy of hydrolysis is less than 0, from thermodynamics angle
It spontaneous can not be carried out for degree, it requires effective catalyst and improve reaction rate by reducing activation energy, reduce energy consumption.Water
Being electrolysed net reaction includes two half equations: the half-reaction of cathode half-reaction and anode.Pt race metal and Ru, Ir based compound
It is considered as the state-of-the-art catalyst of HER and OER activity, IrO2It is used for OER and HER with Pt, is applying external voltage
1.5V when just can reach 10mAcm-2Current density (is used for integrated solar water decomposition).But since Pt, Ir, Ru are expensive
Metal, high production cost are unfavorable for large batch of use, enrich on the urgent searching earth and high catalytic activity, stability are good
Base metal substitutes these precious metal catalyst electrolysis waters.Meanwhile in order to continue water-splitting reaction, it is necessary to make HER's and OER
Catalyst is placed in identical electrolyte, it is contemplated that the overpotential of general HER catalyst in an acidic solution is relatively low, catalysis is lived
Property height and stability of material are good, and OER catalyst just has higher catalytic activity and material usually only in alkaline solution
The features such as stability, therefore, from the complexity for simplifying water electrolysis system, the angle for reducing system cost is set out, and earth content is rich
Rich base metal liberation of hydrogen oxygen-separating catalyst becomes one of current international research hot spot.
The information disclosed in the background technology section is intended only to increase the understanding to general background of the invention, without answering
When being considered as recognizing or imply that the information constitutes the prior art already known to those of ordinary skill in the art in any form.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of liberation of hydrogen oxygen-separating catalyst, the catalyst being prepared is applicable in
Liberation of hydrogen and oxygen evolution reaction are carried out in same electrolyte, can be reduced the cost and liberation of hydrogen, the overpotential for analysing oxygen of catalyst, be improved
The catalytic performance of catalyst provides yin-yang electrode catalyst for electrolytic water device, guarantees that electrolysis aquatic products hydrogen quickly, efficiently carries out.
To achieve the above object, the present invention provides a kind of preparation methods of liberation of hydrogen oxygen-separating catalyst, comprising the following steps:
(1) prepare nickel foam substrate, nickel foam substrate is pre-processed；
(2) in situ synthesis prepares NaOH solution, NaOH solution and nickel foam is mixed into reaction kettle and reacted, instead
Nickel foam should be rinsed after the completion, it is dry, obtain Ni (OH)2/ foam nickel electrode；
(3) electrodeposition process, with KMnO4For manganese source, electrodeposit liquid is prepared, inertia graphite electrode is anode, the step (2)
The Ni (OH) being prepared2/ foam nickel electrode is cathode, and additional constant current carries out electro-deposition, MnO is prepared2-Ni(OH)2/
Foam nickel electrode.
Preferably, in above-mentioned technical proposal, the pretreatment in the step (1) is, as concentration is 1- by foam substrate
10-20min is handled in the HCl solution of 3mol/L, takes out the foam substrate successively ultrasound 10-20min in ethyl alcohol, deionized water.
Preferably, in above-mentioned technical proposal, the concentration of NaOH solution is 0.01mol/L in the step (2).
Preferably, in above-mentioned technical proposal, the reaction condition of reaction kettle is in the step (2), is 140-180 in temperature
At a temperature of DEG C, 12-24h is reacted.
Preferably, in above-mentioned technical proposal, dry in the step (2) is to carry out under conditions of temperature is 50-60 DEG C
It is dry.
Preferably, in above-mentioned technical proposal, reaction kettle is the reaction kettle of polytetrafluoroethyllining lining in the step (2).
Preferably, in above-mentioned technical proposal, KMnO in the step (3)4Solution, concentration 0.0125-0.1mol/L.
Preferably, in above-mentioned technical proposal, additional constant current in the step (3): current density 5-20mA.
Preferably, in above-mentioned technical proposal, the sedimentation time of electro-deposition is 15-60min in the step (3).
Compared with prior art, the invention has the following beneficial effects:
(1) preparation method of liberation of hydrogen oxygen-separating catalyst of the present invention prepares MnO using growth in situ and electrodeposition process2-Ni
(OH)2/ nickel foam, not only preparation condition is easily controllable, and MnO2、Ni(OH)2It is carried in nickel foam, mentions in micron shape
The high surface area of former foamed nickel electrode material, promotes the electro catalytic activity of electrode.
(2) use nickel foam for the base material of liberation of hydrogen oxygen-separating catalyst, on the one hand rigidity is strong, is in since nickel foam has
Netted design feature increases the surface area of combination electrode, then is conducive to mass transfer and improves the electro-chemical activity of electrode；Separately
The Ni (OH) of one side growth in situ on base material2, not only reduce costs but also make Ni (OH)2In conjunction with base material more
Securely, the stability of catalyst is improved.
(3) MnO with high capacitance and high oxygen separated performance is introduced2, for improving the catalytic of liberation of hydrogen oxygen-separating catalyst
Play the role of on energy and reduction overpotential for oxygen evolution great.
(4) by Ni (OH)2And MnO2Compound liberation of hydrogen oxygen-separating catalyst MnO2-Ni(OH)2/ nickel foam can be used as electrolysis
The anode and cathode of water installations provides the premise with larger practical application meaning to lasting water-splitting reaction.
Detailed description of the invention
Fig. 1-a is the foam nickel electrode for using nickel foam in the preparation method of liberation of hydrogen oxygen-separating catalyst according to the present invention
SEM figure.
Fig. 1-b is the Ni that step (2) is prepared in the preparation method of liberation of hydrogen oxygen-separating catalyst according to the present invention
(OH)2The SEM of/foam nickel electrode schemes.
Fig. 1-c is that MnO is prepared in embodiment 12The SEM of/NF electrode schemes.
Fig. 1-d is that MnO is prepared in the preparation method of liberation of hydrogen oxygen-separating catalyst according to the present invention2-Ni(OH)2/ NF electrode
SEM figure.
Fig. 2 is NF, Ni (OH)2/ NF electrode, MnO2/ NF electrode and MnO2-Ni(OH)2The XRD diagram of/NF electrode
Fig. 3-a is difference KMnO in the preparation method of the liberation of hydrogen oxygen-separating catalyst of embodiment 1-34It is made under the conditions of solution concentration
Standby obtained preparation MnO2-Ni(OH)2The LSV of/NF electrode evolving hydrogen reaction schemes.
Fig. 3-b is difference KMnO in the preparation method of the liberation of hydrogen oxygen-separating catalyst of embodiment 1-34It is made under the conditions of solution concentration
Standby obtained preparation MnO2-Ni(OH)2The LSV of/NF electrode oxygen evolution reaction schemes.
Fig. 4-a is that different electric currents are close in the preparation method of the liberation of hydrogen oxygen-separating catalyst of embodiment 1, embodiment 4 and embodiment 5
The preparation MnO being prepared under the conditions of degree2-Ni(OH)2The LSV of/NF electrode evolving hydrogen reaction schemes.
Fig. 4-b is that different electric currents are close in the preparation method of the liberation of hydrogen oxygen-separating catalyst of embodiment 1, embodiment 4 and embodiment 5
The preparation MnO being prepared under the conditions of degree2-Ni(OH)2/ NF electrode analyses the reaction LSV figure of oxygen.
Fig. 5-a is different electro-deposition in the preparation method of the liberation of hydrogen oxygen-separating catalyst of embodiment 1, embodiment 6 and embodiment 7
The preparation MnO being prepared under time conditions2-Ni(OH)2The LSV of/NF electrode evolving hydrogen reaction schemes.
Fig. 5-b is different electro-deposition in the preparation method of the liberation of hydrogen oxygen-separating catalyst of embodiment 1, embodiment 6 and embodiment 7
The preparation MnO being prepared under time conditions2-Ni(OH)2The LSV of/NF electrode oxygen evolution reaction schemes.
Specific embodiment
With reference to the accompanying drawing, specific embodiments of the present invention will be described in detail, it is to be understood that guarantor of the invention
Shield range is not limited by the specific implementation.
Unless otherwise explicitly stated, otherwise in entire disclosure and claims, term " includes " or its change
Changing such as "comprising" or " including " etc. will be understood to comprise stated element or component, and not exclude other members
Part or other component parts.
Embodiment 1
MnO2-Ni(OH)2The preparation process of/NF electrode material:
(1) substrate pre-processes: firstly, nickel foam substrate material is cut into 3cm × 5cm size, the nickel foam that will have been cut out
Basis material, which is placed in the HCl of 2mol/L, handles 15min, to remove the oxide layer on surface；Then, by the nickel foam through acid processing
The matrix successively ultrasound 15min in ethyl alcohol, deionized water, removes the organic matter on surface；The SEM figure of nickel foam substrate is detected, such as
Shown in Fig. 1-a；The XRD diagram of nickel foam substrate is detected, as shown in Figure 2.
(2) in situ synthesis: compound concentration is 0.1mol/L NaOH solution 60mL, well-mixed solution and pre- place
In the reaction kettle for the polytetrafluoroethyllining lining that the nickel foam (NF) managed is transferred to 100mL, 160 DEG C at a temperature of, react 16h
Afterwards, room temperature is naturally cooled to, then the sample for being cooled to room temperature is rinsed well with deionized water, the condition for being 55 DEG C in temperature
Under, it is dried, obtains Ni (OH)2/ NF electrode；Detect the Ni (OH) being prepared2/ NF (as Ni (OH)2/ nickel foam) electricity
The SEM of pole schemes, as shown in Fig. 1-b；It detects Ni (OH)2The XRD diagram of/NF electrode, as shown in Figure 2.
(3) electrodeposition process: 100mL electrodeposit liquid is prepared, with KMnO4For manganese source, concentration 0.025mol/L uses 3cm
× 5cm inertia graphite electrode is anode, Ni (OH)2/ NF electrode is cathode, and keeping the distance between cathode and anode is 4cm, in room
Under the conditions of temperature, additional constant current 10mA, electro-deposition 30min prepare MnO2-Ni(OH)2/ NF electrode.What detection was prepared
MnO2-Ni(OH)2The SEM of/NF electrode schemes, as shown in Fig. 1-d；Detect MnO2-Ni(OH)2The XRD diagram of/NF electrode, such as Fig. 2 institute
Show.
It is to electrode, Hg with platinum electrode under the conditions of 0.5mol/L KOH solution | HgO | OH-(1M KOH) is reference electricity
Pole and MnO2-Ni(OH)2/ NF electrode is measurement MnO in the case of the three-electrode system of working electrode2-Ni(OH)2/ NF is (as
MnO2-Ni(OH)2/ nickel foam) electrode electrocatalysis characteristic.Testing result is as shown in Fig. 3-a and Fig. 3-b.
Fig. 3-a is different KMnO in embodiment 1-34The preparation MnO being prepared under the conditions of solution concentration2-Ni(OH)2/
The LSV of NF electrode evolving hydrogen reaction schemes.
Fig. 3-b is different KMnO in embodiment 1-34The preparation MnO being prepared under the conditions of solution concentration2-Ni(OH)2/
The LSV of NF electrode oxygen evolution reaction schemes.
MnO2The preparation process of/NF electrode material:
(1) substrate pre-processes: firstly, nickel foam substrate material is cut into 3cm × 5cm size, the nickel foam that will have been cut out
Basis material, which is placed in the HCl of 2mol/L, handles 15min, to remove the oxide layer on surface；Then, by the nickel foam through acid processing
The matrix successively ultrasound 15min in ethyl alcohol, deionized water, removes the organic matter on surface；
(2) electrodeposition process: 100mL electrodeposit liquid is prepared, with KMnO4For manganese source, concentration 0.025mol/L uses 3cm
× 5cm inertia graphite electrode is anode, and nickel foam (NF) electrode is cathode, and keeping the distance between cathode and anode is 4cm, in room
Under the conditions of temperature, additional constant current 10mA, electro-deposition 30min prepare MnO2/ NF electrode.Detect the MnO being prepared2/ NF electrode
SEM figure, as shown in fig 1-c；The XRD diagram of MnO2/NF electrode is detected, as shown in Figure 2.
Embodiment 2
MnO2-Ni(OH)2The preparation process of/NF electrode material:
(1) substrate pre-processes: firstly, nickel foam substrate material is cut into 3cm × 5cm size, the nickel foam that will have been cut out
Basis material, which is placed in the HCl of 2mol/L, handles 15min, to remove the oxide layer on surface；Then, by the nickel foam through acid processing
The matrix successively ultrasound 15min in ethyl alcohol, deionized water, removes the organic matter on surface；
(2) in situ synthesis: compound concentration is 0.1mol/L NaOH solution 60mL, well-mixed solution and pre- place
In the reaction kettle for the polytetrafluoroethyllining lining that the nickel foam (NF) managed is transferred to 100mL, 160 DEG C at a temperature of, react 16h
Afterwards, room temperature is naturally cooled to, then the sample for being cooled to room temperature is rinsed well with deionized water, the condition for being 55 DEG C in temperature
Under, it is dried, obtains Ni (OH)2/ NF electrode；
(3) electrodeposition process: 100mL electrodeposit liquid is prepared, with KMnO4For manganese source, concentration 0.0125mol/L uses 3cm
× 5cm inertia graphite electrode is anode, Ni (OH)2/ NF electrode is cathode, and keeping the distance between cathode and anode is 4cm, in room
Under the conditions of temperature, additional constant current 10mA, electro-deposition 30min prepare MnO2-Ni(OH)2/ NF electrode.
It is to electrode, Hg with platinum electrode under the conditions of 0.5mol/L KOH solution | HgO | OH-(1M KOH) is reference electricity
Pole and MnO2-Ni(OH)2/ NF electrode is measurement MnO in the case of the three-electrode system of working electrode2-Ni(OH)2/ NF electrode
Electrocatalysis characteristic.Testing result is as shown in Fig. 3-a and Fig. 3-b.
Fig. 3-a is different KMnO in embodiment 1-34The preparation MnO being prepared under the conditions of solution concentration2-Ni(OH)2/
The LSV of NF electrode evolving hydrogen reaction schemes.
Fig. 3-b is different KMnO in embodiment 1-34The preparation MnO being prepared under the conditions of solution concentration2-Ni(OH)2/
The LSV of NF electrode oxygen evolution reaction schemes.
Embodiment 3
MnO2-Ni(OH)2The preparation process of/NF electrode material:
(1) substrate pre-processes: firstly, nickel foam substrate material is cut into 3cm × 5cm size, the nickel foam that will have been cut out
Basis material, which is placed in the HCl of 2mol/L, handles 15min, to remove the oxide layer on surface；Then, by the nickel foam through acid processing
The matrix successively ultrasound 15min in ethyl alcohol, deionized water, removes the organic matter on surface；
(2) in situ synthesis: compound concentration is 0.1mol/L NaOH solution 60mL, well-mixed solution and pre- place
In the reaction kettle for the polytetrafluoroethyllining lining that the nickel foam (NF) managed is transferred to 100mL, 160 DEG C at a temperature of, react 16h
Afterwards, room temperature is naturally cooled to, then the sample for being cooled to room temperature is rinsed well with deionized water, the condition for being 55 DEG C in temperature
Under, it is dried, obtains Ni (OH)2/ NF electrode；
(3) electrodeposition process: 100mL electrodeposit liquid is prepared, with KMnO4For manganese source, concentration 0.1mol/L, with 3cm ×
5cm inertia graphite electrode is anode, Ni (OH)2/ NF electrode is cathode, and keeping the distance between cathode and anode is 4cm, in room temperature
Under the conditions of, additional constant current 10mA, electro-deposition 30min prepare MnO2-Ni(OH)2/ NF electrode.
It is to electrode, Hg with platinum electrode under the conditions of 0.5mol/L KOH solution | HgO | OH-(1M KOH) is reference electricity
Pole and MnO2-Ni(OH)2/ NF electrode is measurement MnO in the case of the three-electrode system of working electrode2-Ni(OH)2/ NF electrode
Electrocatalysis characteristic.Testing result is as shown in Fig. 3-a and Fig. 3-b.
Fig. 3-a is different KMnO in embodiment 1-34The preparation MnO being prepared under the conditions of solution concentration2-Ni(OH)2/
The LSV of NF electrode evolving hydrogen reaction schemes.
Fig. 3-b is different KMnO in embodiment 1-34The preparation MnO being prepared under the conditions of solution concentration2-Ni(OH)2/
The LSV of NF electrode oxygen evolution reaction schemes.
Embodiment 4
MnO2-Ni(OH)2The preparation process of/NF electrode material:
(1) substrate pre-processes: firstly, nickel foam substrate material is cut into 3cm × 5cm size, the nickel foam that will have been cut out
Basis material, which is placed in the HCl of 2mol/L, handles 15min, to remove the oxide layer on surface；Then, by the nickel foam through acid processing
The matrix successively ultrasound 15min in ethyl alcohol, deionized water, removes the organic matter on surface；
(2) in situ synthesis: compound concentration is 0.1mol/L NaOH solution 60mL, well-mixed solution and pre- place
In the reaction kettle for the polytetrafluoroethyllining lining that the nickel foam (NF) managed is transferred to 100mL, 160 DEG C at a temperature of, react 16h
Afterwards, room temperature is naturally cooled to, then the sample for being cooled to room temperature is rinsed well with deionized water, the condition for being 55 DEG C in temperature
Under, it is dried, obtains Ni (OH)2/ NF electrode；
(3) electrodeposition process: 100mL electrodeposit liquid is prepared, with KMnO4For manganese source, concentration 0.025mol/L uses 3cm
× 5cm inertia graphite electrode is anode, Ni (OH)2/ NF electrode is cathode, and keeping the distance between cathode and anode is 4cm, in room
Under the conditions of temperature, additional constant current 5mA, electro-deposition 30min prepare MnO2-Ni(OH)2/ NF electrode.
It is to electrode, Hg with platinum electrode under the conditions of 0.5mol/L KOH solution | HgO | OH-(1M KOH) is reference electricity
Pole and MnO2-Ni(OH)2/ NF electrode is measurement MnO in the case of the three-electrode system of working electrode2-Ni(OH)2/ NF electrode
Electrocatalysis characteristic.Testing result is as shown in Fig. 4-a and Fig. 4-b.
Fig. 4-a is the preparation that is prepared under different current density conditions in embodiment 1, embodiment 4 and embodiment 5
MnO2-Ni(OH)2The LSV of/NF electrode evolving hydrogen reaction schemes.
Fig. 4-b is the preparation that is prepared under different current density conditions in embodiment 1, embodiment 4 and embodiment 5
MnO2-Ni(OH)2The LSV of/NF electrode oxygen evolution reaction schemes.
Embodiment 5
MnO2-Ni(OH)2The preparation process of/NF electrode material:
(1) substrate pre-processes: firstly, nickel foam substrate material is cut into 3cm × 5cm size, the nickel foam that will have been cut out
Basis material, which is placed in the HCl of 2mol/L, handles 15min, to remove the oxide layer on surface；Then, by the nickel foam through acid processing
The matrix successively ultrasound 15min in ethyl alcohol, deionized water, removes the organic matter on surface；
(2) in situ synthesis: compound concentration is 0.1mol/L NaOH solution 60mL, well-mixed solution and pre- place
In the reaction kettle for the polytetrafluoroethyllining lining that the nickel foam (NF) managed is transferred to 100mL, 160 DEG C at a temperature of, react 16h
Afterwards, room temperature is naturally cooled to, then the sample for being cooled to room temperature is rinsed well with deionized water, the condition for being 55 DEG C in temperature
Under, it is dried, obtains Ni (OH)2/ NF electrode；
(3) electrodeposition process: 100mL electrodeposit liquid is prepared, with KMnO4For manganese source, concentration 0.025mol/L uses 3cm
× 5cm inertia graphite electrode is anode, Ni (OH)2/ NF electrode is cathode, and keeping the distance between cathode and anode is 4cm, in room
Under the conditions of temperature, additional constant current 20mA, electro-deposition 30min prepare MnO2-Ni(OH)2/ NF electrode.
It is to electrode, Hg with platinum electrode under the conditions of 0.5mol/L KOH solution | HgO | OH-(1M KOH) is reference electricity
Pole and MnO2-Ni(OH)2/ NF electrode is measurement MnO in the case of the three-electrode system of working electrode2-Ni(OH)2/ NF electrode
Electrocatalysis characteristic.Testing result is as shown in Fig. 4-a and Fig. 4-b.
Fig. 4-a is the preparation that is prepared under different current density conditions in embodiment 1, embodiment 4 and embodiment 5
MnO2-Ni(OH)2The LSV of/NF electrode evolving hydrogen reaction schemes.
Fig. 4-b is the preparation that is prepared under different current density conditions in embodiment 1, embodiment 4 and embodiment 5
MnO2-Ni(OH)2The LSV of/NF electrode oxygen evolution reaction schemes.
Embodiment 6
MnO2-Ni(OH)2The preparation process of/NF electrode material:
(1) substrate pre-processes: firstly, nickel foam substrate material is cut into 3cm × 5cm size, the nickel foam that will have been cut out
Basis material, which is placed in the HCl of 2mol/L, handles 15min, to remove the oxide layer on surface；Then, by the nickel foam through acid processing
The matrix successively ultrasound 15min in ethyl alcohol, deionized water, removes the organic matter on surface；
(2) in situ synthesis: compound concentration is 0.1mol/L NaOH solution 60mL, well-mixed solution and pre- place
In the reaction kettle for the polytetrafluoroethyllining lining that the nickel foam (NF) managed is transferred to 100mL, 160 DEG C at a temperature of, react 16h
Afterwards, room temperature is naturally cooled to, then the sample for being cooled to room temperature is rinsed well with deionized water, the condition for being 55 DEG C in temperature
Under, it is dried, obtains Ni (OH)2/ NF electrode；
(3) electrodeposition process: 100mL electrodeposit liquid is prepared, with KMnO4For manganese source, concentration 0.025mol/L uses 3cm
× 5cm inertia graphite electrode is anode, Ni (OH)2/ NF electrode is cathode, and keeping the distance between cathode and anode is 4cm, in room
Under the conditions of temperature, additional constant current 10mA, electro-deposition 15min prepare MnO2-Ni(OH)2/ NF electrode.
It is to electrode, Hg with platinum electrode under the conditions of 0.5mol/L KOH solution | HgO | OH-(1M KOH) is reference electricity
Pole and MnO2-Ni(OH)2/ NF electrode is measurement MnO in the case of the three-electrode system of working electrode2-Ni(OH)2/ NF electrode
Electrocatalysis characteristic.Testing result is as shown in Fig. 5-a and Fig. 5-b.
Fig. 5-a is the preparation that is prepared under the conditions of different electrodeposition times in embodiment 1, embodiment 6 and embodiment 7
MnO2-Ni(OH)2The LSV of/NF electrode evolving hydrogen reaction schemes.
Fig. 5-b is the preparation that is prepared under the conditions of different electrodeposition times in embodiment 1, embodiment 6 and embodiment 7
MnO2-Ni(OH)2The LSV of/NF electrode oxygen evolution reaction schemes.
Embodiment 7
MnO2-Ni(OH)2The preparation process of/NF electrode material:
(1) substrate pre-processes: firstly, nickel foam substrate material is cut into 3cm × 5cm size, the nickel foam that will have been cut out
Basis material, which is placed in the HCl of 2mol/L, handles 15min, to remove the oxide layer on surface；Then, by the nickel foam through acid processing
The matrix successively ultrasound 15min in ethyl alcohol, deionized water, removes the organic matter on surface；
(2) in situ synthesis: compound concentration is 0.1mol/L NaOH solution 60mL, well-mixed solution and pre- place
In the reaction kettle for the polytetrafluoroethyllining lining that the nickel foam (NF) managed is transferred to 100mL, 160 DEG C at a temperature of, react 16h
Afterwards, room temperature is naturally cooled to, then the sample for being cooled to room temperature is rinsed well with deionized water, the condition for being 55 DEG C in temperature
Under, it is dried, obtains Ni (OH)2/ NF electrode；
(3) electrodeposition process: 100mL electrodeposit liquid is prepared, with KMnO4For manganese source, concentration 0.025mol/L uses 3cm
× 5cm inertia graphite electrode is anode, Ni (OH)2/ NF electrode is cathode, and keeping the distance between cathode and anode is 4cm, in room
Under the conditions of temperature, additional constant current 10mA, electro-deposition 60min prepare MnO2-Ni(OH)2/ NF electrode.
It is to electrode, Hg with platinum electrode under the conditions of 0.5mol/L KOH solution | HgO | OH-(1M KOH) is reference electricity
Pole and MnO2-Ni(OH)2/ NF electrode is measurement MnO in the case of the three-electrode system of working electrode2-Ni(OH)2/ NF electrode
Electrocatalysis characteristic.Testing result is as shown in Fig. 5-a and Fig. 5-b.
Fig. 5-a is the preparation that is prepared under the conditions of different electrodeposition times in embodiment 1, embodiment 6 and embodiment 7
MnO2-Ni(OH)2The LSV of/NF electrode evolving hydrogen reaction schemes.
Fig. 5-b is the preparation that is prepared under the conditions of different electrodeposition times in embodiment 1, embodiment 6 and embodiment 7
MnO2-Ni(OH)2The LSV of/NF electrode oxygen evolution reaction schemes.
The aforementioned description to specific exemplary embodiment of the invention is in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed
And variation.The purpose of selecting and describing the exemplary embodiment is that explaining specific principle of the invention and its actually answering
With so that those skilled in the art can be realized and utilize a variety of different exemplary implementation schemes of the invention and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (6)
1. a kind of preparation method of liberation of hydrogen oxygen-separating catalyst, which comprises the following steps:
(1) prepare nickel foam substrate, nickel foam substrate is pre-processed；
(2) in situ synthesis prepares NaOH solution, NaOH solution and nickel foam is mixed into reaction kettle and reacted, has been reacted
Nickel foam is rinsed at rear, it is dry, obtain Ni (OH)2/ foam nickel electrode；The reaction condition of reaction kettle is
At a temperature of 140-180 DEG C, 12-24h is reacted；
(3) electrodeposition process, with KMnO4For manganese source, electrodeposit liquid is prepared, inertia graphite electrode is anode, step (2) preparation
Obtained Ni (OH)2/ foam nickel electrode is cathode, and additional constant current carries out electro-deposition, MnO is prepared2-Ni(OH)2/ foam
Nickel electrode；KMnO in the step (3)4Solution, concentration 0.0125-0.1mol/L；Additional constant current: electric current 5-20mA.
2. the preparation method of liberation of hydrogen oxygen-separating catalyst according to claim 1, which is characterized in that in the step (1)
Pretreatment is, by foam substrate as 10-20min is handled in the HCl solution that concentration is 1-3mol/L, to take out foam substrate successively
The ultrasound 10-20min in ethyl alcohol, deionized water.
3. the preparation method of liberation of hydrogen oxygen-separating catalyst according to claim 1, which is characterized in that in the step (2)
The concentration of NaOH solution is 0.01mol/L.
4. the preparation method of liberation of hydrogen oxygen-separating catalyst according to claim 1, which is characterized in that done in the step (2)
Dry is to be dried under conditions of temperature is 50-60 DEG C.
5. the preparation method of liberation of hydrogen oxygen-separating catalyst according to claim 1, which is characterized in that anti-in the step (2)
Answering kettle is the reaction kettle of polytetrafluoroethyllining lining.
6. the preparation method of liberation of hydrogen oxygen-separating catalyst according to claim 1, which is characterized in that electric in the step (3)
The sedimentation time of deposition is 15-60min.
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| CN108425144B (en) * | 2018-03-23 | 2020-04-24 | 陕西师范大学 | Preparation method of karst foam nickel for producing oxygen by electrocatalytic total decomposition of hydrogen in water |
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| CN113060800A (en) * | 2021-03-19 | 2021-07-02 | 西安建筑科技大学 | Preparation method and application of bimetal oxide modified foamed nickel composite electrode |
| CN114892207A (en) * | 2022-04-29 | 2022-08-12 | 江苏大学 | NiFeCo-LDH/NF electrocatalyst and preparation method thereof |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102082268A (en) * | 2011-01-06 | 2011-06-01 | 哈尔滨工程大学 | In-situ preparation method for anode material of Ni(OH)2 nickel-metal hydride (NI-MH) battery through foamed nickel |
| CN102664107A (en) * | 2012-05-31 | 2012-09-12 | 北京科技大学 | Preparation method of nano-manganese dioxide electrode |
| CN102709058A (en) * | 2012-07-01 | 2012-10-03 | 吉林大学 | Method for preparing manganese dioxide-nickel hydroxide composite electrode materials of super capacitors |
| CN105304352A (en) * | 2015-10-12 | 2016-02-03 | 哈尔滨工业大学深圳研究生院 | Method for preparing manganese dioxide/nickel hydroxide composite nano sheet by using nickel foam self-reaction and application of manganese dioxide/nickel hydroxide composite nano sheet to supercapacitor |
| CN105469901A (en) * | 2015-11-20 | 2016-04-06 | 燕山大学 | In-situ-growth-based method for preparing nickel hydroxide-nickel oxide film electrode |
| CN105719851A (en) * | 2016-01-26 | 2016-06-29 | 华中科技大学 | Preparation method and product of MnO2/Ni composite material |
| CN106158394A (en) * | 2016-06-29 | 2016-11-23 | 西北师范大学 | A kind of preparation method of nickel foam based super capacitor electrode material |
-
2017
- 2017-05-24 CN CN201710373829.XA patent/CN107326392B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102082268A (en) * | 2011-01-06 | 2011-06-01 | 哈尔滨工程大学 | In-situ preparation method for anode material of Ni(OH)2 nickel-metal hydride (NI-MH) battery through foamed nickel |
| CN102664107A (en) * | 2012-05-31 | 2012-09-12 | 北京科技大学 | Preparation method of nano-manganese dioxide electrode |
| CN102709058A (en) * | 2012-07-01 | 2012-10-03 | 吉林大学 | Method for preparing manganese dioxide-nickel hydroxide composite electrode materials of super capacitors |
| CN105304352A (en) * | 2015-10-12 | 2016-02-03 | 哈尔滨工业大学深圳研究生院 | Method for preparing manganese dioxide/nickel hydroxide composite nano sheet by using nickel foam self-reaction and application of manganese dioxide/nickel hydroxide composite nano sheet to supercapacitor |
| CN105469901A (en) * | 2015-11-20 | 2016-04-06 | 燕山大学 | In-situ-growth-based method for preparing nickel hydroxide-nickel oxide film electrode |
| CN105719851A (en) * | 2016-01-26 | 2016-06-29 | 华中科技大学 | Preparation method and product of MnO2/Ni composite material |
| CN106158394A (en) * | 2016-06-29 | 2016-11-23 | 西北师范大学 | A kind of preparation method of nickel foam based super capacitor electrode material |
Non-Patent Citations (1)
| Title |
|---|
| Manganese oxide films for electrochemical supercapacitors;J. Wei等;《Journal of Materials Processing Technology》;20071231;第186卷;第356–361页 |
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