CN108716008A - Three-dimensional ferronickel layered double-hydroxide array and its room temperature preparation method and application - Google Patents
Three-dimensional ferronickel layered double-hydroxide array and its room temperature preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of three-dimensional ferronickel layered double-hydroxide array and its room temperature preparation method and applications.The preparation method includes：The mixed solution for including molysite and polar neutral solvent is provided, nickel foam is set to be contacted with the mixed solution, and it is reacted in being stored at room temperature, acquisition is mainly assembled the three-dimensional ferronickel layered double-hydroxide array formed by ferronickel laminated double hydroxide nanometer piece, and the three-dimensional ferronickel layered double-hydroxide is array-supported in nickel foam.The three-dimensional ferronickel layered double-hydroxide array, which is mainly assembled by ferronickel laminated double hydroxide nanometer piece, to be formed, and has three-dimensional multistage structure.The present invention prepares three-dimensional ferronickel layered double-hydroxide array by simply reacting at room temperature, it is simple for process, raw material sources are extensive, room temperature synthesis does not need additional energy, and yield is higher, is suitable for large-scale production, while obtained product is three-dimensional sheet array structure, with high activity and superior stability, have wide application prospects in electro-catalysis oxygen evolution reaction.
Description
Technical field
The present invention relates to a kind of layered double-hydroxide array being carried in nickel foam and its room temperature preparation methods, especially
It is related to a kind of three-dimensional ferronickel layered double-hydroxide array being carried in nickel foam and its room temperature preparation method and application, belongs to
Materials science field.
Background technology
The energy crisis and environmental pollution brought with fossil energy are increasingly sharpened, and people are a kind of clear there is an urgent need to find
Clean, efficient, rich reserves the new sources of the physical efficiency containing energy.Hydrogen is exactly a kind of ideal new source of the physical efficiency containing energy.Water electrolysis hydrogen production
It is one of silicol process of greatest concern at present since the Oxygen anodic evolution reaction of electrolysis water is a four complicated electronic processes to make
It is the major reason for restricting electrolysis water development with prodigious overpotential.Known optimal catalyst be iridium dioxide and
Ruthenic oxide, however since its reserves is low and expensive, so that its application is extremely restricted.
Currently, the material of many base metal bases all shows good electro-catalysis oxygen evolution reaction performance, such as transition
Metal oxide, hydroxide, phosphate cpd and carbon-based material, wherein the most prominent with the performance of nickel iron compound.Mesh
The preceding method for synthesizing these materials is mainly hydrothermal/solvent heat, high temperature co-precipitation and electrochemical deposition, but these synthesize plans
Slightly all it is to need to be additionally provided a large amount of energy, greatly improves the cost of catalyst, does not meet the energy-efficient theme of our times,
And seriously constrain the process of its industrialized production.
Invention content
The main purpose of the present invention is to provide a kind of three-dimensional ferronickel layered double-hydroxide array and its room temperature preparation sides
Method, to overcome deficiency in the prior art.
Another object of the present invention, which also resides in, provides the three-dimensional ferronickel layered double-hydroxide array in electro-catalysis field
Purposes.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes：
An embodiment of the present invention provides a kind of room temperature preparation method of three-dimensional ferronickel layered double-hydroxide array, packets
It includes：
The mixed solution for including molysite and polar neutral solvent is provided；
So that nickel foam is contacted with the mixed solution, and in being stored at room temperature reaction, obtains mainly by the double hydrogen-oxygens of ferronickel stratiform
Compound nanometer sheet assembles the three-dimensional ferronickel layered double-hydroxide array to be formed, the three-dimensional ferronickel layered double-hydroxide array
It is carried in nickel foam.
The embodiment of the present invention additionally provides the three-dimensional ferronickel layered double-hydroxide array prepared by the method.
The embodiment of the present invention additionally provides a kind of three-dimensional ferronickel layered double-hydroxide array, mainly double by ferronickel stratiform
Hydroxide nano piece assembles to be formed, and has three-dimensional multistage structure.
The embodiment of the present invention additionally provides three-dimensional ferronickel layered double-hydroxide array above-mentioned in electro-catalysis field
Purposes.
The embodiment of the present invention additionally provides three-dimensional ferronickel layered double-hydroxide array above-mentioned in electro-catalysis oxygen evolution reaction
In purposes.
The embodiment of the present invention additionally provides a kind of electrocatalysis material or device, and it includes the three-dimensional double hydrogen of ferronickel stratiform above-mentioned
Oxide array.
Compared with prior art, beneficial effects of the present invention at least that：
1) present invention prepares three-dimensional ferronickel layered double-hydroxide array by simply reacting at room temperature, all to react
Cheng Jun is carried out at room temperature, and room temperature synthesis does not need additional energy, and processing step is extremely simple, and experiment condition is controllable, institute
Simple and easy to get using reagent, raw material sources are extensive, of low cost, and yield is higher, are suitable for large-scale production；
2) the three-dimensional ferronickel layered double-hydroxide array being carried in nickel foam prepared by the present invention has multistage tie
Structure is to be formed by array structure by three-dimensional sheet, and active site reservation is more, has high activity and superior stability,
Have wide application prospects in electro-catalysis oxygen evolution reaction；
3) preparation process of the invention can also be extended to the preparation process of other three-layer laminated double-hydroxide arrays, and produce
Rate is higher, is easy to iodine scale.
Description of the drawings
It, below will be to required in embodiment or description of the prior art in order to illustrate more clearly of technical scheme of the present invention
The attached drawing used is simply introduced, it should be apparent that, drawings discussed below is implemented as just some invented herein
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other accompanying drawings.
Fig. 1 a- Fig. 1 b are the three-dimensional ferronickel layered double-hydroxide being carried in the embodiment of the present invention 1 in nickel foam respectively
The electron scanning micrograph and transmission electron microscope photo of array, illustration is the scanning electron microscope of amplification in Fig. 1 a
Photo.
Fig. 2 is the three-dimensional ferronickel layered double-hydroxide array powder being carried in the embodiment of the present invention 1 in nickel foam
X-ray diffracting spectrum.
Fig. 3 is the energy for the three-dimensional ferronickel layered double-hydroxide array being carried in the embodiment of the present invention 1 in nickel foam
Dispersion X-ray collection of illustrative plates.
Fig. 4 is that the three-dimensional ferronickel layered double-hydroxide array being carried in the embodiment of the present invention 1 in nickel foam is used as electricity
Pole material carries out the polarization curve of electro-catalysis analysis oxygen.
Specific implementation mode
As previously mentioned, in view of it is existing synthesis oxygen evolution reaction catalysts method, if hydrothermal/solvent heat, high temperature pyrolysis with
And electrochemical deposition, all it is to need to be additionally provided a large amount of energy, inventor has found after studying for a long period of time and largely putting into practice：
The hydrolysis of ferric ion makes the aobvious acidity of solution, promotes the dissolving of nickel foam in this way, then, sour consumption further pushes three
This synergistic effect of the hydrolysis of valence iron, such ferronickel ion promotes it to generate ferronickel double-hydroxide in nickel foam surface in situ
Array, shown in forming process such as following formula (1)-(3).Based on this discovery, inventor is able to propose technical scheme of the present invention,
It will be as it was noted above, will make it more to explain in detail below.
(1)Fe3++(x+y)H2O→[Fe(OH)x(H2O)y]3-x++xH+
(2)3Ni+8H++2NO3 -→3Ni2++2NO+4H2O
(3)Ni2++[Fe(OH)x(H2O)y]3-x++NO3 -+H2O→NiFe LDH
As the one side of technical solution of the present invention, involved by be a kind of three-dimensional ferronickel layered double-hydroxide battle array
The room temperature preparation method of row comprising：
The mixed solution for including molysite and polar neutral solvent is provided；
So that nickel foam is contacted with the mixed solution, and in being stored at room temperature reaction, obtains mainly by the double hydrogen-oxygens of ferronickel stratiform
Compound nanometer sheet assembles the three-dimensional ferronickel layered double-hydroxide array to be formed, the three-dimensional ferronickel layered double-hydroxide array
It is carried in nickel foam.
In some embodiments, the preparation method may particularly include：
Nickel foam is immersed dissolved with the molten polar neutral solvent of molysite, and carries out being stored at room temperature reaction, is made by nanometer sheet
Assemble the three-dimensional ferronickel layered double-hydroxide array being carried in nickel foam formed.
In some embodiments, the mass ratio of the nickel foam and molysite is 2~6：1~5.
In some embodiments, the molysite includes Iron(III) chloride hexahydrate, Fe(NO3)39H2O, four chloride hydrates Asia
Any one in iron, green vitriol, ferric sulfate (III) and ferric acetyl acetonade (III) etc. or two or more combinations, but
It is without being limited thereto.
In some embodiments, the polar neutral solvent includes water, methanol, ethyl alcohol, propyl alcohol, butanol, ethylene glycol and N,
Any one in dinethylformamide etc. or two or more combinations, but not limited to this.
Aforementioned molysite and polar neutral solvent etc. can be selected from but be not limited only to type listed above.
Further, among an exemplary embodiments, the preparation method may include：First by ferric nitrate be dissolved in water and
In the mixed solution of ethyl alcohol, nickel foam is added and is stored at room temperature 12~72h of reaction, takes out the nickel foam after room temperature reaction later, and
Cleaning, drying at room temperature obtain target product.
Further, among an exemplary embodiments, the preparation method can specifically include：Take molysite and polar neutral
Solvent ultrasound after mixed at room temperature is evenly dispersed, so that molysite is dissolved in polar neutral solvent, forms the mixed solution.
Further, the mass volume ratio of the molysite and polar neutral solvent is 0.02~0.1g：5~30mL.
Among some more preferred embodiment, the preparation method may include：It is 0.02~0.1g to take quality
Molysite be dissolved in 5~30mL polar neutral solvents.
Further, the preparation method specifically includes：Nickel foam is totally submerged in the mixed solution, Zhi Houyu
It is stored at room temperature 12~72h of reaction, obtains the three-dimensional ferronickel layered double-hydroxide array.
Further, the preparation method further includes：After completion of the reaction, to obtained three-dimensional ferronickel layered double-hydroxide
Array is cleaned, and in drying at room temperature.
Wherein, as one, more specifically one of embodiment, the preparation method may comprise steps of：
I, ultrasound is evenly dispersed after taking molysite to be mixed with polar neutral solvent；
II, to step I, finally nickel foam is added in obtained mixed solution, and nickel foam is made to be totally submerged, then at room temperature
Stand 12~72h of reaction；
III, the nickel foam after being reacted at room temperature by step II is taken out, and is cleaned, drying at room temperature, obtains and described is carried on bubble
Three-dimensional ferronickel layered double-hydroxide array on foam nickel.
The present invention prepares three-dimensional ferronickel layered double-hydroxide array, all reaction process by simply reacting at room temperature
It carries out at room temperature, room temperature synthesis does not need additional energy, and processing step is extremely simple, and experiment condition is controllable, is made
Simple and easy to get with reagent, raw material sources are extensive, of low cost, and yield is higher, are suitable for large-scale production.
The preparation process of the present invention can also be extended to the preparation process of other three-layer laminated double-hydroxide arrays, and yield
It is higher, it is easy to iodine scale.
As the other side of technical solution of the present invention, it is double to further relate to the three-dimensional ferronickel stratiform prepared by preceding method
Hydroxide array.
As the other side of technical solution of the present invention, the present invention also provides a kind of three-dimensional double hydroxides of ferronickel stratiform
Object array is mainly assembled by ferronickel laminated double hydroxide nanometer piece and is formed, and appearance and size is uniform, and has three-dimensional multistage
Structure.
Preferably, the three-dimensional ferronickel layered double-hydroxide is array-supported in nickel foam.The three-dimensional multistage knot
Structure includes the array that ferronickel laminated double hydroxide nanometer piece is formed and the three-dimensional structure that nickel foam provides, and effectively remains work
Property site, makes it maintain material superior performance during electro-catalysis.
Further, the three-dimensional ferronickel layered double-hydroxide array appearance and size is uniform, and can largely prepare,
Three-dimensional multistage structure keeps superior chemical property to provide necessary condition for it.
The three-dimensional ferronickel layered double-hydroxide array being carried in nickel foam prepared by the present invention has multilevel hierarchy,
It is that array structure is formed by by three-dimensional sheet, active site reservation is more, has high activity and superior stability, is urged in electricity
Change and has wide application prospects in oxygen evolution reaction.
The other side of the embodiment of the present invention additionally provides three-dimensional ferronickel layered double-hydroxide array above-mentioned in electricity
Purposes in catalytic field.
The other side of the embodiment of the present invention additionally provides three-dimensional ferronickel layered double-hydroxide array above-mentioned in electricity
The purposes being catalyzed in oxygen evolution reaction.
For example, providing a kind of electrocatalysis material or device among some embodiments, it includes the three-dimensional ferronickels
Layered double-hydroxide array.
Further, the electrocatalysis material or device can be electro-catalysis analysis oxygen material or device, electrocatalytic hydrogen evolution
Material or device, electrocatalytic oxidation reducing material or device etc., and it is without being limited thereto.
To make the object, technical solutions and advantages of the present invention clearer, with reference to several preferred embodiments to this hair
Bright technical solution is further specifically described, but the present invention is not limited only to following embodiments, field technology people
The non-intrinsically safe modifications and adaptations that member makes under core guiding theory of the present invention, still fall within protection scope of the present invention.
Embodiment 1
It is 3 that the Fe(NO3)39H2O of 0.06g (0.15mmol), which is dissolved in 20mL water and ethyl alcohol volume ratio,:1 mixed solution
In, ultrasonic disperse is uniform, and the nickel foam 0.16g of 1.5cm × 3cm is then added, is stored at room temperature for 24 hours, you can obtain being carried on bubble
Three-dimensional ferronickel layered double-hydroxide array on foam nickel.
As can be seen that the three-dimensional ferronickel layered double-hydroxide array product shape that the present embodiment is obtained from Fig. 1 a- Fig. 1 b
Looks size uniformity, and there is three-dimensional multistage structure, this multilevel hierarchy includes the array of ferronickel laminated double hydroxide nanometer piece
With the three-dimensional structure provided by nickel foam.Fig. 2 and Fig. 3 are please referred to again, pass through powder x-ray diffraction and energy dispersion X-ray figure
Spectrum is it is found that the flaky material is ferronickel layered double-hydroxide.
Take the three-dimensional ferronickel layered double-hydroxide array of 1cm × 1cm being carried in nickel foam as working electrode.Electricity
Catalysis oxygen evolution reaction performance is measured using traditional three-electrode system, and silver/silver chloride electrode is as reference electrode, platinized platinum electricity
Pole is used as the linear sweep voltammetry curve measured with 5 millivolts of sweep speeds per second to electrode to characterize its electrocatalysis characteristic.Figure
Current potential has carried out ohm compensation and has been converted into the current potential relative to reversible hydrogen electrode in 4.
Embodiment 2
It is 3 that the Fe(NO3)39H2O of 0.02g (0.05mmol), which is dissolved in 30mL water and ethyl alcohol volume ratio,:1 mixed solution
In, ultrasonic disperse is uniform, and the nickel foam 0.12g of 1.5cm × 2.3cm is then added, is stored at room temperature 48h, you can be carried on
Three-dimensional ferronickel layered double-hydroxide array in nickel foam.
Embodiment 3
It is 3 that the Fe(NO3)39H2O of 0.1g (0.25mmol), which is dissolved in 30mL water and ethyl alcohol volume ratio,:1 mixed solution
In, ultrasonic disperse is uniform, and the nickel foam 0.04g of 1cm × 1.1cm is then added, is stored at room temperature 48h, you can obtain being carried on bubble
Three-dimensional ferronickel layered double-hydroxide array on foam nickel
Embodiment 4
The Iron(III) chloride hexahydrate of 0.04g (0.15mmol) is dissolved in 20mL water, ultrasonic disperse is uniform, then, is added
The nickel foam 0.16g of 1.5cm × 3cm, is stored at room temperature 72h, you can obtains being carried on the double hydrogen of three-dimensional ferronickel stratiform in nickel foam
Oxide array.
Embodiment 5
By the ferric sulfate solution of 0.06g (0.15mmol) in 20mL water, ultrasonic disperse is uniform, then, addition 1.5cm ×
The nickel foam 0.16g of 3cm, is stored at room temperature 72h, you can obtains being carried on the three-dimensional ferronickel layered double-hydroxide battle array in nickel foam
Row.
Embodiment 6
It is 5 that the green vitriol of 0.055g (0.2mmol), which is dissolved in 20mL water and methanol volume ratio,:1 mixing is molten
In liquid, ultrasonic disperse is uniform, and the nickel foam 0.16g of 1.5cm × 3cm is then added, is stored at room temperature 72h, you can be carried on
Three-dimensional ferronickel layered double-hydroxide array in nickel foam.
Embodiment 7
It is 6 that the Iron dichloride tetrahydrate of 0.04g (0.2mmol), which is dissolved in 5mL water and methanol volume ratio,:1 mixed solution
In, ultrasonic disperse is uniform, and the nickel foam 0.16g of 1.5cm × 3cm is then added, is stored at room temperature 12h, you can obtain being carried on bubble
Three-dimensional ferronickel layered double-hydroxide array on foam nickel.
In addition, inventor also utilizes the alternate embodiments such as listed other raw materials and other process conditions above
Various raw materials and corresponding process conditions in 1-7 have carried out corresponding experiment, obtain three-dimensional ferronickel layered double-hydroxide array
Pattern, performance etc. are also ideal, substantially similar to embodiment 1-7 products.
The present invention prepares the three-dimensional ferronickel layered double-hydroxide battle array being carried in nickel foam by simple room temperature method
Row, not only Non-energy-consumption, of low cost, and simple for process controllable, and raw material sources are extensive, and yield is higher, are suitable for large-scale production, together
When obtained product appearance and size it is uniform, have three-dimensional multistage structure, active site retain it is more, have high activity and it is superior surely
It is qualitative, have wide application prospects in electro-catalysis analysis oxygen field.
Technical scheme of the present invention is described in detail in embodiment described above, it should be understood that the above is only
For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in the spirit of the present invention,
Supplement or similar fashion replacement etc., should all be included in the protection scope of the present invention.
Claims (15)
1. a kind of room temperature preparation method of three-dimensional ferronickel layered double-hydroxide array, it is characterised in that including：
The mixed solution for including molysite and polar neutral solvent is provided；
So that nickel foam is contacted with the mixed solution, and in being stored at room temperature reaction, obtains mainly by ferronickel layered double-hydroxide
Nanometer sheet assembles the three-dimensional ferronickel layered double-hydroxide array to be formed, and the three-dimensional ferronickel layered double-hydroxide is array-supported
In in nickel foam.
2. preparation method according to claim 1, it is characterised in that：The mass ratio of the nickel foam and molysite is 2~6：1
~5.
3. preparation method according to claim 1, it is characterised in that：The molysite includes Iron(III) chloride hexahydrate, nine water
Close any one or two kinds in ferric nitrate, Iron dichloride tetrahydrate, green vitriol, ferric sulfate and ferric acetyl acetonade with
On combination.
4. preparation method according to claim 1, it is characterised in that：The polar neutral solvent includes water, methanol, second
Any one in alcohol, propyl alcohol, butanol, ethylene glycol and n,N-Dimethylformamide or two or more combinations.
5. preparation method according to claim 1, it is characterised in that specifically include：Take molysite with polar neutral solvent in room
Ultrasound is evenly dispersed after temperature mixing, so that molysite is dissolved in polar neutral solvent, forms the mixed solution.
6. preparation method according to claim 5, it is characterised in that：The quality volume of the molysite and polar neutral solvent
Than for 0.02~0.1g：5~30mL.
7. preparation method according to claim 1, it is characterised in that specifically include：Nickel foam is totally submerged in described mixed
It closes in solution, later in being stored at room temperature 12~72h of reaction, obtains the three-dimensional ferronickel layered double-hydroxide array.
8. according to the preparation method described in any one of claim 1-7, it is characterised in that further include：After completion of the reaction, right
It obtains three-dimensional ferronickel layered double-hydroxide array to be cleaned, and in drying at room temperature.
9. the three-dimensional ferronickel layered double-hydroxide array prepared by any one of claim 1-8 the methods.
10. a kind of three-dimensional ferronickel layered double-hydroxide array, mainly assembles shape by ferronickel laminated double hydroxide nanometer piece
At, and there is three-dimensional multistage structure.
11. three-dimensional ferronickel layered double-hydroxide array as claimed in claim 10, it is characterised in that：It is supported on nickel foam
On, the three-dimensional multistage structure includes the array that ferronickel laminated double hydroxide nanometer piece is formed and the three-dimensional knot that nickel foam provides
Structure.
12. use of the three-dimensional ferronickel layered double-hydroxide array in electro-catalysis field described in any one of claim 9-11
On the way.
13. the three-dimensional ferronickel layered double-hydroxide array described in any one of claim 9-11 is in electro-catalysis oxygen evolution reaction
Purposes.
14. a kind of electrocatalysis material or device, it is characterised in that include the three-dimensional ferronickel described in any one of claim 9-11
Layered double-hydroxide array.
15. electrocatalysis material according to claim 14 or device, it is characterised in that：The electrocatalysis material or device packet
Include electro-catalysis analysis oxygen material or device, electrocatalytic hydrogen evolution material or device, electrocatalytic oxidation reducing material or device in it is any one
Kind or two or more combinations.
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