CN108315760A - A kind of metal organic frame/foamed nickel electrode material and its preparation method and application - Google Patents
A kind of metal organic frame/foamed nickel electrode material and its preparation method and application Download PDFInfo
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- CN108315760A CN108315760A CN201810272983.2A CN201810272983A CN108315760A CN 108315760 A CN108315760 A CN 108315760A CN 201810272983 A CN201810272983 A CN 201810272983A CN 108315760 A CN108315760 A CN 108315760A
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Abstract
The invention discloses a kind of metal organic frame/foamed nickel electrode materials and its preparation method and application, preparation method includes, using nickel foam thin slice as nickel source and base material, it is placed in reaction kettle, the mixed solution containing ferrous salt and terephthalic acid (TPA) ligand, sealing, heating reaction is added, thin slice is taken out after cooling, rinses rear drying metal organic frame/foamed nickel electrode material well；The chemical formula of obtained metal organic frame is Fe2Ni2(OH)2(C8H4O4), belong to anorthic system, P1 (1) space group.Design is scientific and reasonable for method provided by the present invention, simple for process controllable, and raw material is easy to get and inexpensive, and production cost is low, efficient, is suitble to large-scale production, commercial application prospect wide；Product has high electro catalytic activity in alkaline solution to water oxidation reaction, and catalytic effect is continual and steady, and theoretical and practical significance is great.
Description
Technical field
The present invention relates to electrocatalysis material technical fields, and in particular to a kind of metal organic frame/foamed nickel electrode material
And its preparation method and application.
Background technology
Since twentieth century, global economy is expanded rapidly, and demand of the human society to the energy also increasingly increases, so
And conventional fossil fuel is largely become increasingly conspicuous using environmental problems such as caused flue dust, acid rain and greenhouse effects, seriously
Hinder the green sustainable development of human society.Meanwhile fossil fuel it is non-renewable be also doomed it will be depleted, Wu Fachi
It is continuous to use.In this context, develop and more and more widely paid attention to by people using the new energy of sustainable development.Too
Positive energy, the new energy such as wind energy and Hydrogen Energy are due to having the characteristics that economic and cleaning, it has also become the common focus of attention in the whole world, because
This, rationally generates hydrogen and oxygen using the electrical cracking water that solar energy and wind power generation generate, can be by interval, uncontrollable
Solar energy and wind energy transformation are that controllable chemical energy stores, and are then when required by the burning of hydrogen release chemical energy
The mankind provide the energy.Whole process does not have the participation of carbon dioxide and release, be very cleaning, ideal energy conversion process.
Electrolysis water as conversion process among the energy reacts (1), can be divided into water oxygen (2) and liberation of hydrogen (3) two and half is anti-
It answers：
2H2O→O2+2H2 (1)
2H2O→O2+4H++4e- (2)
4H++4e-→2H2 (3)。
Water oxidation reaction and the rate of evolving hydrogen reaction codetermine the efficiency of electrolysis water process, compared with evolving hydrogen reaction,
Water oxidation reaction needs the transfer by four electronics and proton, and reaction is inherently more complicated, is thermodynamically more difficult to occur, because
This becomes the principal element of limitation electrolysis water reaction process.
Currently, RuO2And IrO2Belong to the generally acknowledged catalyst with good water oxygen catalytic effect, however since it belongs to
Noble metal, it is expensive, it is not suitable for mass producing；In addition, fine catalyst is modified in electrode surface meeting by binder
The active site of catalyst exposure is reduced, and a large amount of bubbles generated seriously affect the effect of catalytic process binder.Therefore, it seeks
It looks for efficient stable and water oxidation catalyst cheap and easy to get is of great significance.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of metal organic frame/foamed nickel electrode material and
Preparation method and application.
A kind of preparation method of metal organic frame/foamed nickel electrode material is provided according to an aspect of the present invention, with bubble
Foam nickel thin slice is nickel source and base material, is placed in reaction kettle, and the mixed solution containing ferrous salt and terephthalic acid (TPA) ligand is added,
Sealing, heating reaction, takes out thin slice after cooling, rinses rear drying metal organic frame/foamed nickel electrode material well.
Specifically, the reaction kettle is ptfe autoclave；The thin slice takes out after cooling, and using ethyl alcohol and
After deionized water is alternately rinsed well, then it is placed in drying in baking oven.
In the above-mentioned technical solutions, the ferrous salt is FeCl2·4H2O and/or FeSO4·7H2O, the mixed solution
Using n,N-Dimethylformamide, second alcohol and water as solvent.
In the above-mentioned technical solutions, the molar ratio of the ferrous salt and terephthalic acid (TPA) is 0.48mmol：0.43-
0.53mmol, preferably 0.48mmol：0.48mmol.
Preferably, in the above-mentioned technical solutions, with the length and width of nickel foam thin slice and it is thick be respectively 3cm, 0.8-2cm and
0.6-1.8mm, and the superficial density of nickel foam thin slice is 240-350g/m2, the ferrous salt, n,N-Dimethylformamide, second
The inventory of alcohol and water is respectively 0.48mmol, 10-11mL, 0.7-0.8mL and 0.7-0.8mL, preferably 0.48mmol,
10.5mL, 0.75mL and 0.75mL.
It is further preferred that in the above-mentioned technical solutions, the volume of the reaction kettle is 20-50mL, and heating is anti-when reacting
It is 110-130 DEG C to answer temperature in the kettle, reaction time 10-14h.
In the above-mentioned technical solutions, the preparation method further includes the pretreatment to nickel foam thin slice before the reaction, specifically
Including removal surface oxide layer, removal surface organic matter and drying process.
Specifically, the removal surface oxide layer and removal surface organic matter are respectively to be placed in ultrasound in dilute hydrochloric acid and acetone
It after 10-20min, then is rinsed with deionized water, the temperature and time of the drying process is respectively 50-70 DEG C and 2-5h.
Metal organic frame/foam nickel electrode material that above-mentioned preparation method obtains is provided according to a further aspect of the invention
Material；The chemical formula of the metal organic frame is Fe2Ni2(OH)2(C8H4O4), belong to anorthic system, P1 (1) space group, structure cell
Parameter is α=90 °, β=96.276 °, γ=90 °, structure cell body
Product is
Above-mentioned preparation method or above-mentioned metal organic frame/foamed nickel electrode material are provided according to another aspect of the invention
Application, the specific application as electrode in catalytic water aoxidizes.
Preferably, using the three-electrode system of standard, using the metal organic frame/foamed nickel electrode material as work
Electrode is put into alkaline solution, catalytic water oxidation reaction.
Advantages of the present invention：
(1) present invention is using nickel foam thin slice as nickel source and base material, using iron ion and nickel ion as metal center, with right
Phthalic acid is ligand, and by strong coordinate bond self assembly, a step solvent-thermal method exists metal-organic framework material growth in situ
Conductive foam nickel base surface, design is scientific and reasonable and simple and practicable for preparation method, and process controllability is high, raw materials used to be easy to get
And it is cheap, production cost is low, and production efficiency is high, is suitble to scale industrial production, commercial application prospect wide；
(2) the metal organic frame carrying capacity in metal organic frame/foamed nickel electrode material provided by the present invention is big, and
With porous network structure, the speed of water oxidation reaction is may advantageously facilitate, is had to water oxidation reaction in alkaline solution high
Electro catalytic activity, and catalytic effect is continual and steady, in addition, it can be used directly as working electrode, does not need traditional electricity
Pole is modified and the use of the binders such as Nafion, simplifies using process, saves the time, improves catalytic activity and stabilization
Property, theoretical and practical significance is great.
Description of the drawings
A kind of metal organic frame/foamed nickel electrode material that Fig. 1 is provided by the embodiment of the present invention 1 is in different times magnifications
Scanning electron microscope diagram under rate；
A kind of elemental analysis for metal organic frame/foamed nickel electrode material that Fig. 2 is provided by the embodiment of the present invention 1
Figure；
A kind of X-ray diffraction for metal organic frame/foamed nickel electrode material that Fig. 3 is provided by the embodiment of the present invention 1
Collection of illustrative plates, wherein a is the X ray diffracting spectrum obtained after metal organic frame is fitted, and b is the X-ray diffractogram of electrode material
Spectrum；
A kind of metal organic frame/foamed nickel electrode material that Fig. 4 is provided by the embodiment of the present invention 1 is in 1mol/L KOH
The linear sweep voltammetry curve obtained in solution；
A kind of metal organic frame/foamed nickel electrode material that Fig. 5 is provided by the embodiment of the present invention 1 is in 1mol/L KOH
Current density plot under the constant potential obtained in solution.
Specific implementation mode
With reference to the accompanying drawings and examples, the specific implementation mode of the present invention is described in further detail.Implement below
Example is not limited to protection scope of the present invention for illustrating the present invention, and protection scope of the present invention is with claims
It is accurate.
Unless otherwise specified, experiment reagent used in the embodiment of the present invention and material etc. are commercially available, if not having
Body indicates, the conventional means that technological means used in the embodiment of the present invention is well known to the skilled person.
Embodiment 1
An embodiment of the present invention provides a kind of preparation method of metal organic frame/foamed nickel electrode material, specific steps
It is as follows：
Nickel foam thin slice, is cut into the rectangle of 3cm × 1cm by S1, pretreatment nickel foam thin slice, is placed in dilute hydrochloric acid ultrasonic
15min removes surface oxide layer, is then rinsed with deionized water, be subsequently placed at ultrasound 15min in acetone, remove surface has
Machine object, is then rinsed with deionized water again, is finally placed in baking oven, and dry 3h, saves backup at 60 DEG C；
S2, the FeCl for weighing 0.48mmol2·4H2Then 10.5mL N, N- is added in the terephthalic acid (TPA) of O and 0.48mmol
Dimethylformamide, 0.75mL ethyl alcohol and 0.75mL deionized waters are uniformly mixed and are placed in 30mL ptfe autoclaves,
Then pretreated nickel foam thin slice in step S1 is added again, ptfe autoclave is sealed, is placed in baking oven,
Heating reaction 12h, subsequent cooled to room temperature take out thin slice at 125 DEG C, after alternately being rinsed with ethyl alcohol and deionized water,
Dry 12h is to get metal organic frame/foamed nickel electrode material in 60 DEG C of baking oven.
It is put as shown in Figure 1 in difference for metal organic frame/foamed nickel electrode material prepared in the embodiment of the present invention 1
Scanning electron microscope (SEM) photograph under big multiplying power, it can be seen from the figure that synthesized metal organic frame is two-dimensional sheet material, and it is intensive
Ground is stacked on foam nickel base surface；It is illustrated in figure 2 metal organic frame/nickel foam prepared in the embodiment of the present invention 1
The elemental analysis figure for the metal organic frame that electrode material ultrasound obtains, it can be seen from the figure that the metal organic frame of synthesis
Containing carbon, oxygen, iron, four kinds of elements of nickel, and its content close to theoretical value, furthermore it is noted that metal-organic framework material
The nickel contained mainly since nickel foam is etched in the acid solution containing terephthalic acid (TPA), has released nickel ion and has joined
With in the building-up process to material；Fig. 3 show metal organic frame/foam nickel electrode prepared in the embodiment of the present invention 1
The X ray diffracting spectrum of material, in figure, asterisk mark part is the diffraction maximum of foam nickel base, other peaks have corresponding to metal
The diffraction maximum of machine frame frame material；In addition, measuring the embodiment of the present invention using High frequency combustion infrared-adsorption method (ASTM E1019-11)
The carrying capacity of metal organic frame is 2.63mg/cm in obtained electrode material2。
In the KOH solution of a concentration of 1mol/L, metal organic frame/nickel foam obtained by the embodiment of the present invention is studied
The electro-catalysis water oxygen reactivity worth of electrode material, detailed process are as follows：
It is put into using metal organic frame/foamed nickel electrode material as working electrode using the three-electrode system of standard
In KOH solution, Ag/AgCl electrodes are used as reference electrode, use platinum plate electrode as to electrode, in 0-0.6V potential ranges,
Linear scan volt-ampere curve is tested to sweep fast 1mV/s；In addition, permanent by applying to metal organic frame/foamed nickel electrode material
Fixed current potential records the variation of its catalytic current density, tests the stability of its catalytic process.
Metal organic frame/foamed nickel electrode material prepared in the embodiment of the present invention 1 is illustrated in figure 4 in 1mol/L
KOH solution in the linear sweep voltammetry curve that obtains, it can be seen from the figure that there is nickelous conversion in 1.44V or so
For the oxidation peak of nickelic, water oxidation reaction takes place in 1.45V later, and with the increase of current potential, catalytic current density
It increases rapidly, when current density reaches 50mA/cm2When, required overpotential is only 233mV；It is illustrated in figure 5 the embodiment of the present invention
Electric current is close after prepared metal organic frame/foamed nickel electrode material applies constant potential in the KOH solution of 1mol/L in 1
It writes music line, it can be seen from the figure that electric current keeps stablizing in the catalytic process of 48000s, variation is very small, illustrates the present invention
Metal organic frame/foamed nickel electrode material obtained by embodiment has fabulous catalytic stability.
Embodiment 2
An embodiment of the present invention provides a kind of preparation method of metal organic frame/foamed nickel electrode material, specific steps
It is as follows：
Nickel foam thin slice, is cut into the rectangle of 3cm × 2cm by S1, pretreatment nickel foam thin slice, is placed in dilute hydrochloric acid ultrasonic
20min removes surface oxide layer, is then rinsed with deionized water, be subsequently placed at ultrasound 20min in acetone, remove surface has
Machine object, is then rinsed with deionized water again, is finally placed in baking oven, and dry 5h, saves backup at 60 DEG C；
S2, the FeCl for weighing 0.48mmol2·4H2Then 11mL N, N- bis- is added in the terephthalic acid (TPA) of O and 0.45mmol
Methylformamide, 0.8mL ethyl alcohol and 0.8mL deionized waters are uniformly mixed and are placed in 50mL ptfe autoclaves, then
Pretreated nickel foam thin slice in step S1 is added again, ptfe autoclave is sealed, is placed in baking oven, 130
Heating reaction 14h, subsequent cooled to room temperature take out thin slice at DEG C, after alternately being rinsed with ethyl alcohol and deionized water, at 60 DEG C
Baking oven in dry 14h to get metal organic frame/foamed nickel electrode material.
Electrode material obtained by the embodiment of the present invention is measured using High frequency combustion infrared-adsorption method (ASTM E1019-11)
The carrying capacity of middle metal organic frame is 2.68mg/cm2。
In the KOH solution of a concentration of 1mol/L, metal organic frame/nickel foam obtained by the embodiment of the present invention is studied
The electro-catalysis water oxygen reactivity worth of electrode material, electrochemical property test the result shows that, which is in current density
50mA/cm2When, required overpotential is 235mV.
Embodiment 3
An embodiment of the present invention provides a kind of preparation method of metal organic frame/foamed nickel electrode material, specific steps
It is as follows：
Nickel foam thin slice, is cut into the rectangle of 3cm × 0.8cm, is placed in dilute hydrochloric acid and surpasses by S1, pretreatment nickel foam thin slice
Sound 10min removes surface oxide layer, is then rinsed with deionized water, be subsequently placed at ultrasound 10min in acetone, remove surface
Then organic matter is rinsed with deionized water again, be finally placed in baking oven, and dry 2h, saves backup at 60 DEG C；
S2, the FeCl for weighing 0.48mmol2·4H2Then 10mL N, N- bis- is added in the terephthalic acid (TPA) of O and 0.45mmol
Methylformamide, 0.7mL ethyl alcohol and 0.7mL deionized waters are uniformly mixed and are placed in 25mL ptfe autoclaves, then
Pretreated nickel foam thin slice in step S1 is added again, ptfe autoclave is sealed, is placed in baking oven, 120
Heating reaction 10h, subsequent cooled to room temperature take out thin slice at DEG C, after alternately being rinsed with ethyl alcohol and deionized water, at 60 DEG C
Baking oven in dry 12h to get metal organic frame/foamed nickel electrode material.
Electrode material obtained by the embodiment of the present invention is measured using High frequency combustion infrared-adsorption method (ASTM E1019-11)
The carrying capacity of middle metal organic frame is 2.60mg/cm2。
In the KOH solution of a concentration of 1mol/L, metal organic frame/nickel foam obtained by the embodiment of the present invention is studied
The electro-catalysis water oxygen reactivity worth of electrode material, electrochemical property test the result shows that, which is in current density
50mA/cm2When, required overpotential is 236mV.
Finally, the preferred embodiment that these are only the present invention, is not intended to limit the scope of the present invention.It is all this
Within the spirit and principle of invention, any modification, equivalent replacement, improvement and so on should be included in the protection model of the present invention
Within enclosing.
Claims (10)
1. a kind of preparation method of metal organic frame/foamed nickel electrode material, which is characterized in that using nickel foam thin slice as nickel source
And base material, it being placed in reaction kettle, the mixed solution containing ferrous salt and terephthalic acid (TPA) ligand, sealing is added, heating is reacted,
Thin slice is taken out after cooling, rinses rear drying metal organic frame/foamed nickel electrode material well.
2. preparation method according to claim 1, which is characterized in that the ferrous salt is FeCl2·4H2O and/or
FeSO4·7H2O, the mixed solution is using n,N-Dimethylformamide, second alcohol and water as solvent.
3. preparation method according to claim 1, which is characterized in that the ferrous salt and terephthalic acid (TPA) feed intake mole
Than for 0.48mmol：0.43-0.53mmol, preferably 0.48mmol：0.48mmol.
4. preparation method according to claim 2, which is characterized in that be respectively with the length and width and thickness of nickel foam thin slice
3cm, 0.8-2cm and 0.6-1.8mm, and the superficial density of nickel foam thin slice is 240-350g/m2, the ferrous salt, N, N- bis-
Methylformamide, the inventory of second alcohol and water are respectively 0.48mmol, 10-11mL, 0.7-0.8mL and 0.7-0.8mL, preferably
0.48mmol, 10.5mL, 0.75mL and 0.75mL.
5. preparation method according to claim 4, which is characterized in that the volume of the reaction kettle is 20-50mL, and heating is anti-
Seasonable reactor temperature is 110-130 DEG C, reaction time 10-14h.
6. according to claim 1-5 any one of them preparation methods, which is characterized in that further include thin to nickel foam before the reaction
The pretreatment of piece specifically includes removal surface oxide layer, removal surface organic matter and drying process；Preferably, the removal table
Face oxide layer and removal surface organic matter are respectively to be placed in dilute hydrochloric acid and acetone after ultrasound 10-20min, then rushed with deionized water
It washes, the temperature and time of the drying process is respectively 50-70 DEG C and 2-5h.
7. metal organic frame/the foamed nickel electrode material obtained according to claim 1-6 any one of them preparation methods.
8. metal organic frame/foamed nickel electrode material according to claim 7, which is characterized in that the metal is organic
The chemical formula of frame is Fe2Ni2(OH)2(C8H4O4), belong to anorthic system, P1 (1) space group, cell parameter is α=90 °, β=96.276 °, γ=90 °, unit cell volume are
9. having machine frame according to claim 1-6 any one of them preparation method or claim 7-8 any one of them metals
Application of the frame/foamed nickel electrode material as electrode in catalytic water oxidation.
10. application according to claim 9, which is characterized in that the three-electrode system of standard is used, the metal is organic
Frame/foamed nickel electrode material is put into as working electrode in alkaline solution, catalytic water oxidation reaction.
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| CN112981429A (en) * | 2021-02-24 | 2021-06-18 | 江南大学 | Metal organic framework and hydroxide heterojunction electrocatalyst and in-situ preparation method and application thereof |
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