CN109821539B - Ni @ NiFe L DH three-dimensional shell-core structure material and application and preparation method thereof - Google Patents
Ni @ NiFe L DH three-dimensional shell-core structure material and application and preparation method thereof Download PDFInfo
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Abstract
The invention provides a Ni @ NiFe L DH three-dimensional shell-core structure material and an application and a preparation method thereof, the Ni @ NiFe L DH three-dimensional shell-core structure material has good electrical conductivity of a Ni nano bead chain core, the Ni nano bead chain core and a NiFe L DH composite shell wrapped outside the Ni nano bead chain core can be used as an electrocatalyst, the Ni @ NiFe L DH three-dimensional shell-core structure material has high water decomposition catalytic capability, high stability and high industrial value.
Description
Technical Field
The invention relates to the technical field of nano composite structures, in particular to a Ni @ NiFe L DH three-dimensional shell-core structure material and an application and a preparation method thereof.
Background
Electrochemical water decomposition is a clean and sustainable method for converting renewable energy, namely hydrogen, so that hydrogen is generated instead of reforming or thermally cracking traditional hydrocarbons such as fossil fuel or biomass, and the like, and people attract extensive attention. However, since the electrochemical processes of cathodic Hydrogen Evolution (HER) and anodic Oxygen Evolution (OER) are slow, very high overpotentials are required to decompose water, and especially the oxygen evolution process involves four electron transfer, the energy barrier to overcome is very high. At present, the most advanced electrocatalysts are Pt-based materials for HER and Ru, Ir-based materials for OER, respectively, which have smaller initial potentials, but they are to achieve higher current densities (100mA · cm)-2) High overpotentials are still required and, in addition, they belong to rare elements, the extremely high cost limits their widespread use.
Researchers have invested considerable effort to develop effective and low cost bifunctional electrocatalysts to replace the above-mentioned noble metal catalysts, such as Co-, Ni-, and Fe-based and their compounds transition metal-based layered double hydroxide nanosheets (L DHs) have been intensively studied in the field of total water electrolysis due to their unique two-dimensional layered structure, i.e., more sufficient exposure of catalytically active sites than zero-and one-dimensional structures, and facilitating diffusion of water molecules and rapid release of gaseous products, furthermore, they are inexpensive and abundant in storage to show the great potential for large-scale electrolysis of water, in 2014, Song and Hu have stripped off bulk CoCo, NiCo, and NiFe L DHs to expose active sites more sufficiently, enhancing OER activity, however, L DH is very poor in conductivity, when L DH is combined with electrodes using conductive adhesives (such as Nafion polymer adhesives), they produce very large electrical resistance, furthermore, the stripping method is complex and costly, is for large-scale practical applications, 2106. feo et al can promote high conductivity of the electrically conductive nickel-supported nano-tubes, and thus, the feo-conductive layer can reliably promote high conductivity of the feo-supported nano-Co-electrode, and the feo-Co-supported electrically conductive layer, which can promote high conductivity of the feo-supported nano-Co-nano-electrode.
Disclosure of Invention
The invention aims to provide a Ni @ NiFe L DH three-dimensional shell-core structure material, and an application and a preparation method thereof, so as to obtain the Ni @ NiFe L DH three-dimensional shell-core structure material with high decomposition catalytic capability and high material stability.
In order to achieve the purpose, the invention provides a Ni @ NiFe L DH three-dimensional shell-core structure material which comprises foamed nickel, a Ni nano bead chain core and a NiOH-FeOH composite shell, wherein the Ni nano bead chain core grows on the foamed nickel in situ, and the NiOH-FeOH composite shell is wrapped outside the Ni nano bead chain core.
Preferably, the Ni nano bead chain core grows uniformly at the network node part of the foamed nickel.
Preferably, the network node part grown by the foam nickel is flat.
Preferably, the NiOH-FeOH composite shell is amorphous.
Preferably, the NiOH-FeOH composite shell is composed of a plurality of NiOH-FeOH nanolayers.
The invention also provides a preparation method of the Ni @ NiFe L DH three-dimensional shell-core structure material, which comprises the following steps:
step 1: growing a Ni nano bead chain core on the foamed nickel in situ by adopting a magnetic field assisted chemical reduction method;
step 2: and forming a NiOH-FeOH composite shell outside the Ni nano bead chain core.
Preferably, the step 1 comprises the following steps:
step 1.1: cleaning the foamed nickel;
step 1.2: heating the nickel salt precursor aqueous solution;
step 1.3: adding the foamed nickel into the nickel salt precursor aqueous solution, and adding hydrazine hydrate;
step 1.4: adjusting the pH value of the nickel salt precursor aqueous solution;
step 1.5: placing the salt precursor aqueous solution in a magnetic field for heat preservation;
step 1.6: and taking out the foamed nickel and cleaning.
Preferably, in step 1.1, the nickel foam is washed and then rinsed.
Preferably, in step 1.3, the foamed nickel is washed by concentrated hydrochloric acid; and repeatedly washing the foamed nickel by using ethanol and deionized water for many times, wherein the concentration of the concentrated hydrochloric acid is 30-40 wt%, and the washing time is 20-30 minutes.
Preferably, in step 1.3, the aqueous solution of a nickel salt precursor comprises: containing NiCl2·6H2O and Na3C6H5O7·2H2An aqueous solution of O; wherein, it contains NiCl2·6H2O is 0.02-0.06M, Na3C6H5O7·2H2O is 18-19 mM, 45-55 m L aqueous solution, the heating temperature is 70-80 ℃, and the volume of the hydrazine hydrate is 1-2.5 m L.
Preferably, in step 1.4, alkali liquor is added into the nickel salt precursor aqueous solution, so as to adjust the pH of the nickel salt precursor aqueous solution to 13.
Preferably, in step 1.5, the direction of the magnetic field is perpendicular to the surface of the top of the nickel foam, and the salt precursor aqueous solution is placed in the magnetic field and kept for 70-100 min.
Preferably, in step 1.6, ethanol and deionized water are sequentially adopted to wash the foamed nickel; the washing time with ethanol and deionized water was the same.
Preferably, the NiOH-FeOH composite shell is prepared by adopting pulse electrodeposition, the Ni nano bead chain core is used as a working electrode, the foil is used as a counter electrode, and the silver chloride reference electrode forms a three-electrode system for pulse deposition.
Preferably, Ni (NO) is adopted in the pulse electrodeposition process3)2·6H2O and FeSO4·7H2Taking an aqueous solution with O as a precursor as an electrolyte; ni2+:Fe2+＝1:1～9:1。
Preferably, during the pulse electrodeposition, a pulse electric field is applied while nitrogen gas is introduced.
The invention also provides an application of the Ni @ NiFe L DH three-dimensional shell-core structure material, and the Ni @ NiFe L DH three-dimensional shell-core structure material is used as an electrocatalyst.
Compared with the prior art, the Ni @ NiFe L DH three-dimensional shell-core structure material has the advantages that the Ni nano bead chain core has good conductivity, the Ni nano bead chain core and the NiFe L DH composite shell wrapped outside the Ni nano bead chain core can be used as an electrocatalyst, the Ni @ NiFe L DH three-dimensional shell-core structure material has high water decomposition catalytic capability and high stability, and has particularly high industrial value.
Drawings
FIG. 1 is an SEM and XRD picture of a three-dimensional core-shell structured material in one embodiment of the invention; wherein, FIGS. 1(a), (b), and (c) are SEM images of Ni nanobead chains; FIGS. 1(d), (e) are SEM images of three-dimensional core-shell structures; FIG. 1(f) is an XRD pattern of a three-dimensional core-shell structure;
FIG. 2 is a TEM picture and a line scan energy spectrum and STEM-mapping graph of a three-dimensional shell-core structured material in an embodiment of the present invention; wherein, FIGS. 2(a) and (b) are TEM images; FIG. 2(c) is an HR-TEM image; FIG. 2(d) is a line scan energy spectrum; FIG. 2(e) is a STEM-mapping chart;
FIG. 3 is an XPS survey and Ni2p, Fe2p high resolution survey of a three-dimensional core-shell structured material in accordance with an embodiment of the present invention; wherein, FIG. 3(a) is an XPS survey; FIG. 3(b) shows a Ni2p high-resolution spectrum; FIG. 3(c) shows a high resolution spectrum of Fe2 p;
FIG. 4 is a test chart of the electrolytic water catalytic performance and stability of the three-dimensional core-shell structure material according to an embodiment of the present invention; wherein, FIG. 4(a) is a test chart of the catalytic performance of the electrolyzed water; FIG. 4(b) is a graph showing that the current density is 10mA cm -224 hour stability test pattern.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be further described below.
The invention provides a Ni @ NiFe L DH three-dimensional shell-core structure material which comprises foamed nickel, a Ni nano bead chain core and a NiOH-FeOH composite shell, wherein the Ni nano bead chain core grows on the foamed nickel in situ, and the NiOH-FeOH composite shell is wrapped outside the Ni nano bead chain core.
In the embodiment, the Ni nano bead chain core grows uniformly at the network node part of the foam nickel.
In this embodiment, the network node part grown by the nickel foam is flat.
In this example, the NiOH-FeOH composite shell is amorphous.
In this example, the NiOH-FeOH composite shell is composed of multiple NiOH-FeOH nanolayers.
The invention also provides a preparation method of the Ni @ NiFe L DH three-dimensional shell-core structure material, which comprises the following steps:
step 1: growing a Ni nano bead chain core on the foamed nickel in situ by adopting a magnetic field assisted chemical reduction method;
step 2: and forming a NiOH-FeOH composite shell outside the Ni nano bead chain core.
In this embodiment, step 1 includes the following steps:
step 1.1: cleaning the foamed nickel;
step 1.2: heating the nickel salt precursor aqueous solution;
step 1.3: adding foamed nickel into nickel salt precursor aqueous solution, and adding hydrazine hydrate;
step 1.4: adjusting the pH value of the nickel salt precursor aqueous solution;
step 1.5: placing the salt precursor aqueous solution in a magnetic field for heat preservation;
step 1.6: taking out the foamed nickel and cleaning.
In this example, in step 1.1, the nickel foam is first cleaned and then rinsed.
In this example, in step 1.3, the nickel foam is washed with concentrated hydrochloric acid; and repeatedly washing the foamed nickel by using ethanol and deionized water for many times, wherein the concentration of concentrated hydrochloric acid is 30-40 wt%, and the washing time is 20-30 minutes.
In this example, in step 1.3, the aqueous nickel salt precursor solution comprises: containing NiCl2·6H2O and Na3C6H5O7·2H2An aqueous solution of O; wherein, it contains NiCl2·6H2O is 0.02-0.06M, Na3C6H5O7·2H2O is 18 to 19mM and 45 to 55m L waterThe solution is heated at 70-80 ℃ and the volume of the hydrazine hydrate is 1-2.5 m L.
In this example, in step 1.4, the pH of the aqueous solution of nickel salt precursor is adjusted to 13 by adding an alkaline solution to the aqueous solution of nickel salt precursor.
In this example, in step 1.5, the magnetic field is oriented perpendicular to the surface of the top of the nickel foam, and the aqueous solution of the salt precursor is placed in the magnetic field and incubated for 70-100 min.
In this example, in step 1.6, the nickel foam is washed with ethanol and deionized water in sequence; the washing time with ethanol and deionized water was the same.
In this embodiment, a NiOH-FeOH composite shell is prepared by pulse electrodeposition, and a three-electrode system is formed by using a Ni nanoparticle chain core as a working electrode, a foil as a counter electrode, and a silver chloride reference electrode, and is subjected to pulse deposition.
In this example, Ni (NO) was used in the pulse electrodeposition process3)2·6H2O and FeSO4·7H2Taking an aqueous solution with O as a precursor as an electrolyte; ni2+:Fe2+＝1:1～9:1。
In this example, during pulsed electrodeposition, a pulsed electric field was applied while nitrogen gas was bubbled.
The invention also provides an application of the Ni @ NiFe L DH three-dimensional shell-core structure material, and the Ni @ NiFe L DH three-dimensional shell-core structure material is used as an electrocatalyst.
The invention will be further elucidated by means of specific examples and in combination with data:
in the embodiment, Ni @ NiFe L DH three-dimensional shell-core structure material is characterized in that Ni nano bead chains uniformly grow in a network node part of foamed nickel, the network node part is relatively flat, the three-dimensional shell-core structure material comprises Ni crystals and an amorphous NiOH-FeOH composite shell, the NiOH-FeOH composite shell is composed of a plurality of NiOH-FeOH nano layers, when the three-dimensional shell-core structure material is used as an electrocatalyst, in order to improve the water decomposition catalytic performance, the thickness of the composite shell can be preferably 84-100 nm, the thickness of each NiOH-FeOH nano layer is 10-10.5 nm, in the three-dimensional shell-core structure material, the proportion of Fe to Ni is 1 (6-8), preferably 1:7, and the three-dimensional shell-core structure material can show very high water decomposition catalytic performance and has good stability when being used as the electrocatalyst.
The following describes a preparation method of the Ni @ NiFe L DH three-dimensional core-shell structure material of this example, including:
step 1: growing the Ni nano bead chain core in situ on the foamed nickel by adopting a magnetic field assisted chemical reduction method;
specifically, the area of the nickel foam can be 3 × 3cm2(ii) a The step 1 specifically comprises the following steps:
step 1.1: cleaning the foamed nickel; here, the cleaning process in step 1, 1 specifically includes: firstly, cleaning the foamed nickel, and then washing; wherein, concentrated hydrochloric acid can be adopted in the cleaning process, the concentration of the concentrated hydrochloric acid can be 30-40 wt%, preferably 37 wt%, and the cleaning time is 20-30 minutes; the washing process is repeated washing for a plurality of times by sequentially adopting ethanol and deionized water.
Step 1.2: heating the Ni salt precursor water solution, then adding foamed nickel into the heated Ni salt precursor water solution, and adding hydrazine hydrate into the heated Ni salt precursor water solution; here, the Ni salt precursor aqueous solution includes: containing NiCl2·6H2O and Na3C6H5O7·2H2An aqueous solution of O. Wherein NiCl2·6H2The molar concentration of O may be 0.02-0.06, preferably 0.05M, Na3C6H5O7·2H2The molar concentration of O is 18-19 mM, preferably 18.75mM, 45-55 m L aqueous solution, preferably 50m L aqueous solution is added, the heating temperature is 70-80 ℃, preferably 75 ℃.
Step 1.3: adding alkali liquor into the aqueous solution obtained in the step 1.2 to adjust the pH value of the aqueous solution to be alkaline; here, the pH value is adjusted to 13 as an optimum choice. The concentration of the added alkali liquor is 0.5-2M, preferably 1M, and the components of the alkali liquor can be KOH, NaOH and the like. KOH is preferred.
Step 1.4: placing the aqueous solution subjected to the step 1.3 in a magnetic field for heat preservation, wherein the direction of the magnetic field is vertical to the top surface of the foamed nickel; here, the magnetic field may be applied using magnets placed in parallel, for example, a beaker containing an aqueous solution is placed between two flat ndfeb magnets placed in parallel up and down so that the magnetic field is perpendicular to the top surface of the nickel foam. Preferably, the holding time in the magnetic field is 70 to 100 minutes, for example, 90 minutes is the most preferable.
Step 1.5: taking out the foamed nickel and cleaning. Here, the foamed nickel may be washed with ethanol and deionized water in sequence. The time for washing with ethanol and deionized water can be the same, preferably within 5-10 minutes.
Step 2: and forming a NiOH-FeOH composite shell outside the Ni nano bead chain core.
Specifically, the NiOH-FeOH composite shell can be prepared by adopting a pulse electrodeposition method; the method specifically comprises the following steps: the Ni nano bead chain core is used as a working electrode, a platinum sheet is used as a counter electrode and a silver chloride reference electrode to form a three-electrode system, and pulse electrodeposition is carried out. In the pulse electrodeposition process, Ni (NO) is preferably used in a concentration of 0.14M3)2·6H2O and FeSO of 0.016M, 0.02M, 0.07M, 0.14M4·7H2Taking an aqueous solution with O as a precursor as an electrolyte; wherein Ni2+:Fe2+The ratio of the amount of the electrolyte is preferably 1:1 to 9:1, and the volume of the electrolyte is preferably 100 to 130m L to promote Ni2+And Fe2+The deposition of (2) is performed by using a pulse electric field with a certain period, for example, 10s is taken as one period, and the period number can be 1-12, for example, 1, 5, 9, 10 periods; in each period, the potential of-0.86V is kept for a first time and the potential of-1.1V is kept for a second time, and the ratio of the first time to the second time can be 0s:10 s-10 s:0 s. For example, 0s:10s, 3s:7s, 5s:5s, 9s:1s, etc. To prevent Fe2+Oxidized and nitrogen is introduced in the whole pulse electrodeposition process.
Finally, washing and naturally drying the obtained Ni @ NiFe L DH three-dimensional shell-core structure material.
Obtained by the above-mentioned preparation method of this exampleThe Ni @ NiFe L DH three-dimensional core-shell structure material is yellow green, Ni nano bead chains are uniformly grown on the network node parts of the nickel foam, the network node parts grown by the nickel foam are flat, as shown in (a) in FIG. 1, Ni nano particles on the nano bead chains are uniform in size as shown in (b) and (c) in FIGS. 1(d) and (e) show that the Ni @ NiFe L DH three-dimensional core-shell structure material has a multi-layer nano layer on the outer shell layer, and in combination with FIG. 2, it can be found that the Ni nano bead is wrapped by the outer shell, further in FIG. 2(e), Ni and Fe are distributed in the outer shell, the content is Fe: Ni ═ 1:7, in combination with the XRD spectrum of FIG. 1(f), three crystal faces of (006), (012) and (110) correspond to amorphous Ni (OH)2–Fe(OH)3Phase of Ni (OH) with an amorphous shell2–Fe(OH)3The composite shell is characterized in that a plurality of nano layers of the shell are NiOH-FeOH nano layers. Further referring to fig. 3(a), (b), and (c), it can be further confirmed that the prepared three-dimensional core-shell structure material contains Fe and Ni elements, Ni exists in positive divalent state, and Fe exists in positive trivalent state.
Referring to fig. 4, a linear voltammogram in fig. 4(a) shows that the Ni @ NiFe L DH three-dimensional core-shell structure material of the present embodiment completely achieves or even exceeds the water electrolysis catalytic performance of the current mainstream commercial noble metal electrode pair, and the stability test in fig. 4(b) shows that the Ni @ NiFe L DH three-dimensional core-shell structure material of the present embodiment has good 24h stability, the potential increase is less than 2.5%, and the material has good stability, is suitable for commercial large-scale production, and has high industrial value and commercial value.
The above description is only a preferred embodiment of the present invention, and does not limit the present invention in any way. It will be understood by those skilled in the art that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (17)
1. The Ni @ NiFe L DH three-dimensional shell-core structure material is characterized by comprising foamed nickel, a Ni nano bead chain core and a NiOOH-FeOOH composite shell, wherein the Ni nano bead chain core grows on the foamed nickel in situ, the Ni nano bead chain core grows on the foamed nickel in situ by adopting a magnetic field assisted chemical reduction method, Ni nano particles on the Ni nano bead chain core are uniform in size, and the NiOOH-FeOOH composite shell wraps the Ni nano bead chain core.
2. The Ni @ NiFe L DH three-dimensional putamen structural material of claim 1, wherein the Ni nanobead chain core is uniformly grown at the network node sites of the nickel foam.
3. The Ni @ NiFe L DH three-dimensional core-shell structural material of claim 1, wherein the network node sites on which the nickel foam grows are flat.
4. The Ni @ NiFe L DH three-dimensional core-shell structural material of claim 1, wherein the NiOOH-FeOOH composite shell is amorphous.
5. The Ni @ NiFe L DH three-dimensional core-shell structural material of claim 1, wherein the NiOOH-FeOOH composite shell is composed of multiple NiOOH-FeOOH nanolayers.
6. A method for preparing a Ni @ NiFe L DH three-dimensional core-shell structured material, for preparing a Ni @ NiFe L DH three-dimensional core-shell structured material according to any one of claims 1 to 5, comprising the following steps:
step 1: growing a Ni nano bead chain core on the foamed nickel in situ by adopting a magnetic field assisted chemical reduction method;
step 2: and forming a NiOOH-FeOOH composite shell outside the Ni nano bead chain core.
7. The method for preparing the Ni @ NiFe L DH three-dimensional core-shell structural material according to claim 6, wherein the step 1 comprises the steps of:
step 1.1: cleaning the foamed nickel;
step 1.2: heating the nickel salt precursor aqueous solution;
step 1.3: adding the foamed nickel into the nickel salt precursor aqueous solution, and adding hydrazine hydrate;
step 1.4: adjusting the pH value of the nickel salt precursor aqueous solution;
step 1.5: placing the salt precursor aqueous solution in a magnetic field for heat preservation;
step 1.6: and taking out the foamed nickel and cleaning.
8. The method of claim 7, wherein the foamed nickel is washed and then rinsed in step 1.1.
9. The method for preparing the Ni @ NiFe L DH three-dimensional shell-core structure material according to claim 8, wherein in step 1.1, the foamed nickel is washed by concentrated hydrochloric acid, and the foamed nickel is repeatedly washed by ethanol and deionized water for multiple times, wherein the concentration of the concentrated hydrochloric acid is 30-40 wt%, and the washing time is 20-30 minutes.
10. The method of claim 7, wherein in step 1.3, the aqueous solution of the nickel salt precursor comprises NiCl2·6H2O and Na3C6H5O7·2H2An aqueous solution of O; wherein, it contains NiCl2·6H2O is 0.02-0.06M, Na3C6H5O7·2H2O is 18-19 mM, and the water solution is 45-55 m L, the heating temperature is 70-80 ℃, and the volume of the hydrazine hydrate is 1-2.5 m L.
11. The method for preparing the Ni @ NiFe L DH three-dimensional shell-core structure material according to claim 7, wherein the pH of the aqueous solution of nickel salt precursor is adjusted to 13 by adding alkali solution to the aqueous solution of nickel salt precursor in step 1.4.
12. The method for preparing the Ni @ NiFe L DH three-dimensional core-shell structural material according to claim 7, wherein the magnetic field is perpendicular to the surface of the top of the nickel foam in step 1.5, and the salt precursor aqueous solution is placed in the magnetic field and kept for 70-100 min.
13. The method for preparing the Ni @ NiFe L DH three-dimensional core-shell structure material according to claim 7, wherein in the step 1.6, the foamed nickel is washed by ethanol and deionized water in sequence, and the washing time by ethanol and the washing time by deionized water are the same.
14. The method for preparing the Ni @ NiFe L DH three-dimensional core-shell structure material according to claim 6, wherein the NiOOH-FeOOH composite shell is prepared by pulse electrodeposition, the Ni nanobead chain core is used as a working electrode, and the foil is used as a counter electrode and a silver chloride reference electrode to form a three-electrode system for pulse deposition.
15. The method for preparing the Ni @ NiFe L DH three-dimensional core-shell structure material according to claim 14, wherein Ni (NO) is adopted in the pulse electrodeposition process3)2·6H2O and FeSO4·7H2Taking an aqueous solution with O as a precursor as an electrolyte; ni2+: Fe2+= 1:1 ~ 9:1。
16. The method for preparing the Ni @ NiFe L DH three-dimensional core-shell structure material according to claim 14, wherein during the pulsed electrodeposition, a pulsed electric field is applied while nitrogen gas is introduced.
17. Use of a Ni @ NiFe L DH three-dimensional core-shell structured material, using a Ni @ NiFe L DH three-dimensional core-shell structured material according to any of claims 1 to 5, characterized in that a Ni @ NiFe L DH three-dimensional core-shell structured material is used as electrocatalyst.
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