CN113215606A - Flaky N-FeV electrocatalyst and preparation and application thereof - Google Patents
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Abstract
The invention relates to preparation and application of a flaky N-FeV electrocatalyst. The preparation of the electrocatalyst adopts the following specific steps: firstly dissolving ammonium metavanadate and ferric nitrate nonahydrate into deionized water, stirring and dissolving, and then carrying out water bath for 1h at the water bath temperature of 90 ℃ to prepare the red brown powder FeV. And cooling, drying, and then putting the FeV into a tube furnace for N doping in an ammonia atmosphere to obtain the target product N-FeV. The invention has the advantages that: the preparation condition is mild, the process is simple, the cost is low, and the catalyst can be applied to the fields of electrocatalysis, photoelectrocatalysis hydrogen production or electrocatalysis full water decomposition.
Description
Technical Field
The invention relates to preparation and application of a flaky N-FeV electrocatalyst. The cocatalyst is applied to hydrogen production/oxygen production by water decomposition through electrocatalysis, shows high-efficiency and stable electrocatalysis hydrogen production/oxygen production performance, and is expected to be applied to the fields of lithium ion batteries, catalyst carriers or catalytic hydrogenation dehydrogenation.
Background
Transition metals are widely available in earth minerals and have been shown to have excellent hydrogen production (HER)/oxygen production (OER) activity in the current research, so that transition metal electrocatalysts have become a hot spot in the current research. From previous studies, it was found that Hydrogen (HER)/Oxygen (OER) production activity was higher for both the bimetallic oxide and the bimetallic hydroxide than for the single metal catalyst. Electrons of the V3 d orbit in vanadate are easy to be excited, and the transfer of electrons is facilitated, so that the research of an electrocatalyst is facilitated. Whether a simpler method can be utilized to synthesize the nano-FeV nanosheet under a milder condition and then the activity of the catalyst is improved through doping, interface engineering and defect engineering is still a challenging temperature.
The material doped with anions has the maximum atom utilization rate and excellent catalytic performance in catalytic reaction. The introduction of anions can change the morphology and electronic structure of the material, expose more surface active sites, improve the conductivity, optimize the binding energy of Gibbs free energy and water, and reduce the overpotential of water during decomposition. As an effective modification strategy, the surface anion modification also has the capability of adjusting the electronic structure, is beneficial to optimizing the adsorption energy of active species and improving the electrocatalytic activity. The anion doping is firstly proposed to improve the activity of FeV, so that the electron structure and the catalytic activity of a hydrogen production (HER)/oxygen production (OER) electrocatalyst are modified by doping N anions on the surface of the catalyst to induce FeV phase transition, and the result shows that the hydrogen production (HER)/oxygen production (OER) are improved, so that the N doping is an effective method for improving the performance of FeV.
The invention aims to prepare N-FeV and provides a method for preparing an N-FeV nanosheet, which has the advantages of high yield, simple process flow and mild conditions.
Technical scheme of the invention
A preparation method of an N-FeV nanosheet comprises the following specific steps:
(1) 0.47g of ammonium metavanadate (NH)4VO3) Dissolving in 100mL deionized water, stirring for 30min until the solid is completely dissolved to obtain saturated solutionThe solution was heated to 90 ℃ in a water bath.
(2) 0.4g of ferric nitrate nonahydrate (Fe (NO) was added dropwise to the saturated solution at 90 ℃ in step (1)3)3·9H2O), yellow precipitate begins to appear in the solution, and the yellow precipitate becomes reddish brown precipitate after water bath for 60 min;
cooling the reddish brown precipitate in the round-bottom flask to 25 ℃, removing supernatant, respectively and sequentially centrifugally washing the reddish brown precipitate for 3-5 times by using absolute ethyl alcohol and deionized water, and drying the reddish brown precipitate in vacuum at the drying temperature of 60-100 ℃, preferably 80 ℃; the drying temperature is 10-15 h, preferably 12 h; obtaining FeV.
(4) Grinding the reddish brown FeV obtained after drying for 0.5-2 h, transferring the ground reddish brown FeV into a tubular furnace, calcining the FeV at 400 ℃ for 2h in an ammonia atmosphere with the flow rate of 250mL/min, and cooling to obtain the N-FeV, wherein the temperature rise rate is 5 ℃/min.
The invention has the advantages that: the preparation method has the advantages of simple process flow, mild conditions, low cost and high yield, and is suitable for large-scale production, and the prepared FeV has a nanosheet structure. The catalyst promoter can be applied to the field of hydrogen production and oxygen production through electrocatalysis, and is also expected to be applied to the field of lithium ion batteries, catalyst carriers or catalytic hydrogenation dehydrogenation.
Drawings
FIG. 1 XRD patterns for FeV, N-FeV, P-FeV and A-FeV correspond to examples 1, 3 and 6-7.
FIG. 2 Mapping characterization of N-FeV corresponding to examples 2-5
FIG. 3 examples 3, 6 and 7 correspond to Scanning Electron Microscopes (SEM) of N-FeV, P-FeV and A-FeV.
FIG. 4 is a LSV diagram corresponding to examples 1 to 5, showing the hydrogen/oxygen production of catalysts at N-FeV-200 deg.C, N-FeV-400 deg.C, N-FeV-600 deg.C and N-FeV-800 deg.C.
FIG. 5 corresponds to the LSV plots for hydrogen/oxygen production for N-FeV, P-FeV and A-FeV catalysts in examples 3, 6 and 7.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1:
preparing FeV: will be 0.47g ammonium metavanadate (NH)4VO3) Dissolving in 100mL deionized water, stirring for 30min until the solid is completely dissolved to obtain clear and transparent solution, and heating to 90 deg.C in water bath; 0.4g nitric acid nonahydrate (Fe (NO) was added dropwise to the clear transparent solution at 90 ℃3)3·9H2O), yellow precipitate begins to appear in the solution, and the yellow precipitate becomes reddish brown precipitate after water bath for 60 min; and (3) cooling the reddish brown precipitate in the round-bottom flask to 25 ℃, removing supernatant, respectively and sequentially centrifugally washing the reddish brown precipitate for 4 times by using absolute ethyl alcohol and deionized water, then putting the washed reddish brown precipitate into a vacuum drying oven for drying at 80 ℃ for 12 hours, taking out and grinding the dried reddish brown precipitate.
From XRD in FIG. 1, it can be seen that the diffraction peak of FeV is completely matched with standard card (PDF #00-046-1334), indicating the successful preparation of FeV.
Example 2:
preparing FeV: 0.47g of ammonium metavanadate (NH)4VO3) Dissolving in 100mL deionized water, stirring for 30min until the solid is completely dissolved to obtain clear and transparent solution, and heating to 90 deg.C in water bath; 0.4g nitric acid nonahydrate (Fe (NO) was added dropwise to the clear transparent solution at 90 ℃3)3·9H2O), yellow precipitate begins to appear in the solution, and the yellow precipitate becomes reddish brown precipitate after water bath for 60 min; and (3) cooling the reddish brown precipitate in the round-bottom flask to 25 ℃, removing supernatant, respectively and sequentially centrifugally washing the reddish brown precipitate for 4 times by using absolute ethyl alcohol and deionized water, then putting the washed reddish brown precipitate into a vacuum drying oven for drying at 80 ℃ for 12 hours, taking out and grinding the dried reddish brown precipitate.
Grinding the reddish brown FeV obtained after drying for 1h, transferring the ground reddish brown FeV into a tubular furnace, calcining the FeV for 2h at 200 ℃ in an ammonia atmosphere with the flow rate of 250mL/min, and cooling to obtain N-FeV-200 ℃.
After N doping, we can prove the successful doping of N anions by Mapping of fig. 2. It can be seen from the SEM of FIG. 3 that the synthesized N-FeV appears as a sheet, and has the same morphology as the previously synthesized FeV, without a large change. The thickness of the nano-sheet is 15-30nm, and the specific surface area is 80-100m2/g。
Example 3:
preparing FeV: 0.47g of ammonium metavanadate (NH)4VO3) Dissolving in 100mL deionized water, stirring for 30min until the solid is completely dissolved to obtain clear and transparent solution, and heating to 90 deg.C in water bath; 0.4g nitric acid nonahydrate (Fe (NO) was added dropwise to the clear transparent solution at 90 ℃3)3·9H2O), yellow precipitate begins to appear in the solution, and the yellow precipitate becomes reddish brown precipitate after water bath for 60 min; and (3) cooling the reddish brown precipitate in the round-bottom flask to 25 ℃, removing supernatant, respectively and sequentially centrifugally washing the reddish brown precipitate for 4 times by using absolute ethyl alcohol and deionized water, then putting the washed reddish brown precipitate into a vacuum drying oven for drying at 80 ℃ for 12 hours, taking out and grinding the dried reddish brown precipitate.
Grinding the reddish brown FeV obtained after drying for 1h, transferring the ground reddish brown FeV into a tubular furnace, calcining the FeV for 2h at 400 ℃ in an ammonia atmosphere with the flow rate of 250mL/min, and cooling to obtain N-FeV-400 ℃.
After N doping, the prepared N-FeV-400 ℃ catalyst can prove the successful doping of N anions by Mapping in figure 2. It can be seen from the SEM of fig. 3 that the synthesized FeV appeared flaky, and the morphology was the same as that of the previously synthesized FeV, without much change. The thickness of the nano-sheet is 15-30nm, and the specific surface area is 80-100m2/g。
Example 4:
preparing FeV: 0.47g of ammonium metavanadate (NH)4VO3) Dissolving in 100mL deionized water, stirring for 30min until the solid is completely dissolved to obtain clear and transparent solution, and heating to 90 deg.C in water bath; 0.4g nitric acid nonahydrate (Fe (NO) was added dropwise to the clear transparent solution at 90 ℃3)3·9H2O), yellow precipitate begins to appear in the solution, and the yellow precipitate becomes reddish brown precipitate after water bath for 60 min; and (3) cooling the reddish brown precipitate in the round-bottom flask to 25 ℃, removing supernatant, respectively and sequentially centrifugally washing the reddish brown precipitate for 4 times by using absolute ethyl alcohol and deionized water, then putting the washed reddish brown precipitate into a vacuum drying oven for drying at 80 ℃ for 12 hours, taking out and grinding the dried reddish brown precipitate.
Grinding the reddish brown FeV obtained after drying for 1h, transferring the ground reddish brown FeV into a tubular furnace, calcining the FeV for 2h at 600 ℃ in an ammonia atmosphere with the flow rate of 250mL/min, and cooling to obtain the N-FeV-600 ℃.
After N doping, the prepared N-FeV is catalyzed at the temperature of 600 DEG CAgent, we can demonstrate the successful doping of the N anion by Mapping of fig. 2. It can be seen from the SEM of fig. 3 that the synthesized FeV appeared flaky, and the morphology was the same as that of the previously synthesized FeV, without much change. The thickness of the nano-sheet is 15-30nm, and the specific surface area is 80-100m2/g。
Example 5:
preparing FeV: 0.47g of ammonium metavanadate (NH)4VO3) Dissolving in 100mL deionized water, stirring for 30min until the solid is completely dissolved to obtain clear and transparent solution, and heating to 90 deg.C in water bath; 0.4g nitric acid nonahydrate (Fe (NO) was added dropwise to the clear transparent solution at 90 ℃3)3·9H2O), yellow precipitate begins to appear in the solution, and the yellow precipitate becomes reddish brown precipitate after water bath for 60 min; and (3) cooling the reddish brown precipitate in the round-bottom flask to 25 ℃, removing supernatant, respectively and sequentially centrifugally washing the reddish brown precipitate for 4 times by using absolute ethyl alcohol and deionized water, then putting the washed reddish brown precipitate into a vacuum drying oven for drying at 80 ℃ for 12 hours, taking out and grinding the dried reddish brown precipitate.
Grinding the reddish brown FeV obtained after drying for 1h, transferring the ground reddish brown FeV into a tubular furnace, calcining the FeV for 2h at 800 ℃ in an ammonia atmosphere with the flow rate of 250mL/min, and cooling to obtain N-FeV-800 ℃.
After N doping, the prepared N-FeV-800 ℃ catalyst can prove the successful doping of N anions by Mapping of figure 2. It can be seen from the SEM of fig. 3 that the synthesized FeV appeared flaky, and the morphology was the same as that of the previously synthesized FeV, without much change. The thickness of the nano-sheet is 15-30nm, and the specific surface area is 80-100m2/g。
Example 6:
preparing FeV: 0.47g of ammonium metavanadate (NH)4VO3) Dissolving in 100mL deionized water, stirring for 30min until the solid is completely dissolved to obtain clear and transparent solution, and heating to 90 deg.C in water bath; 0.4g nitric acid nonahydrate (Fe (NO) was added dropwise to the clear transparent solution at 90 ℃3)3·9H2O), yellow precipitate begins to appear in the solution, and the yellow precipitate becomes reddish brown precipitate after water bath for 60 min; the reddish brown precipitate in the round-bottom flask is cooled to 25 ℃, and then the supernatant is removed, and the solution is respectively extracted by absolute ethyl alcohol and removedSequentially centrifugally washing with ionized water for 4 times, then placing in a vacuum drying oven at 80 ℃, drying for 12h, taking out and grinding.
The FeV nanosheets and the FeV nanosheets are charged at a weight ratio of 0.1g and 500mg of NaH2PO2·H2Ceramic boat of O open in tube furnace, NaH2PO2·H2O upstream and FeV nanoplates downstream. Heating the sample at a rated temperature for 2h in Ar atmosphere under the condition that the heating rate is 5 ℃/min, naturally cooling to room temperature after the reaction is finished, and collecting the product to obtain the target product P-FeV.
After P doping, no P-FeV compound was found by XRD characterization, which is caused by the small amount of P doping. From the SEM of fig. 3, it can be seen that the synthesized FeV appeared flaky, the same morphology as the previously synthesized FeV, but the thickness of the nanosheets varied. The thickness of the nano-sheet is 10-25nm, and the specific surface area is 60-80m2/g。
Example 7:
preparing FeV: 0.47g of ammonium metavanadate (NH)4VO3) Dissolving in 100mL deionized water, stirring for 30min until the solid is completely dissolved to obtain clear and transparent solution, and heating to 90 deg.C in water bath; 0.4g nitric acid nonahydrate (Fe (NO) was added dropwise to the clear transparent solution at 90 ℃3)3·9H2O), yellow precipitate begins to appear in the solution, and the yellow precipitate becomes reddish brown precipitate after water bath for 60 min; and (3) cooling the reddish brown precipitate in the round-bottom flask to 25 ℃, removing supernatant, respectively and sequentially centrifugally washing the reddish brown precipitate for 4 times by using absolute ethyl alcohol and deionized water, then putting the washed reddish brown precipitate into a vacuum drying oven for drying at 80 ℃ for 12 hours, taking out and grinding the dried reddish brown precipitate.
And (3) putting the FeV nanosheet containing 0.1g of FeV nanosheet into a middle constant-temperature area of a tubular resistance furnace, starting to heat to 400 ℃, and naturally cooling to room temperature after the reaction is finished to obtain the target product A-FeV.
After a doping, no compound of a-FeV was found by XRD characterization, which is caused by the small amount of a doping. From the SEM of fig. 3, it can be seen that the synthesized FeV appeared flaky, the same morphology as the previously synthesized FeV, but the thickness of the nanosheets varied. The thickness of the nano-sheet is 5-20nm, and the specific surface areaThe product is 20-60m2/g。
FIG. 1 is an XRD pattern of N-FeV synthesized by N anion doping. The diffraction peaks of FeV are perfectly matched with the standard card (PDF #00-046-1334), which indicates the successful preparation of FeV. With the anion doping, it was found that the diffraction peak at 2 θ ═ 8.25 ° shifted, and the diffraction peak at (002) crystal plane was gradually decreased with the N anion doping, indicating that the phase transition occurred due to the anion doping induction. A significant shift of (001) at 8.25 ° 2 θ to the high angle side was observed, and this anion-doping-induced structural change was likely caused by the generation of numerous O holes.
FIG. 2(a) is a TEM image of N-FeV, and (b) (d) (e) is an elemental analysis image of Fe, V and O elements respectively, from which it can be seen that the three elements Fe, V and O are uniformly distributed on the surface of the nanosheet, from (c) it can be seen that the N element is successfully doped on the FeV nanosheet, and the doping on the surface is relatively uniform, no agglomeration phenomenon occurs, indicating that the N-FeV is successfully prepared.
FIG. 3 is an SEM image of N-anion doped synthetic N-FeV. The structure of the nanosheet after N doping is not changed greatly on the whole, but a high power electron microscope image shows that a porous structure appears on the nanosheet, a vacancy structure is possibly formed, active sites are increased, and the catalytic activity is improved.
FIG. 4 is a graph of the Linear Sweep Voltammetry (LSV) of N-anion doped synthetic N-FeV at different temperatures, with parameters typically set at a sweep rate of 5mV/s, to obtain hydrogen/oxygen production LSV plots. From the above figure, it can be seen that N-FeV is at 20mA/cm at 400 deg.C2The hydrogen production overpotential is 273mV at minimum, the Tafel slope is 109.72mV/dec at minimum, and the voltage is 20mA/cm2The minimum oxygen generation potential was 1.45V and the minimum Tafel slope was 55.72mV/dec, indicating that HER and its OER perform optimally at 400 ℃. From the LSV and Tafel slopes, 400 ℃ is considered the optimal temperature for N doping, since at 400 ℃ more N ions can attach to the surface of FeV nanoplates, so the performance is optimal. Above 400 ℃ and below 400 ℃, N ions cannot be doped to the maximum at the surface, so the performance is not as good as 400 ℃.
FIG. 5 is a plot of the hydrogen/oxygen production LSV obtained from the Linear Sweep Voltammetry (LSV) measurements performed on the various catalysts of examples 1-3, with parameters typically set at a sweep rate of 5 mV/s. FIG. a is an LSV diagram of hydrogen production of different catalysts, wherein the potentials of N-FeV, P-FeV, A-FeV and FeV are 273mV, 283mV, 300mV and 321mV respectively; FIG. b is a LSV graph of oxygen production for different catalysts, with potentials of 1.45V, 1.47V, 1.48V and 1.50mV for N-FeV, P-FeV, A-FeV and FeV, respectively. This shows that the N doping has better effect and better catalytic performance than the other two anions.
Claims (7)
1. A preparation method of a flaky N-FeV electrocatalyst is characterized by comprising the following steps: ferric nitrate nonahydrate and ammonium metavanadate are used as raw materials, a precursor FeV is synthesized through water bath, and then N-FeV with large specific surface area is obtained through N doping in an ammonia atmosphere.
2. The method for preparing a flower-like flaky N-FeV electrocatalyst according to claim 1, wherein: specifically, 0.1 to 1.0g (preferably, 0.2 to 0.8g, more preferably, 0.4 to 0.7g) of ammonium metavanadate (NH)4VO3) Add 80-150mL (preferred range: dissolving 90-140g, more preferably 95-120g deionized water in round bottom flask, heating to 90-150 deg.C in water bath to obtain transparent clear solution, adding ferric nitrate nonahydrate (Fe (NO)3)3·9H2O)0.2 to 1.5g (preferred range: 0.2 to 1.4g, more preferably 0.3 to 0.7g, is dissolved in 10 to 50mL (preferred range: 10-30g, more preferably 10-20g) deionized water, water bath for 1h-5h (preferred range: 1-4h, more preferably 1-3h), followed by washing the precipitate, drying, and then N-doping in an ammonia atmosphere to obtain N-FeV.
3. The method of claim 2, wherein: after 1-5 h of water bath, the reddish brown precipitate in the round-bottom flask is cooled to 20-40 ℃, the supernatant is removed, the reddish brown precipitate is respectively centrifugally washed for 3-5 times by absolute ethyl alcohol and deionized water in sequence, and the reddish brown precipitate is dried in vacuum at the drying temperature of 60-100 ℃, preferably 70-90 ℃, and more preferably 80 ℃; the drying temperature is 10-15 h, preferably 10-13 h; more preferably 12h, to obtain FeV.
4. The method of claim 2, wherein: preparation of N-FeV: grinding FeV for 0.5-2 h, preferably 0.5-1.5 h; more preferably 1h, then transferring the mixture to a tube furnace for N doping, wherein the flow rate is 100-400 mL/min, preferably 100-300 mL/min; more preferably 200mL/min of ammonia gas atmosphere, the temperature of N doping is 200-.
5. N-FeV obtained by the preparation method according to any one of claims 1 to 4.
6. The N-FeV of claim 5 as an active ingredient or carrier of a catalyst for use in electrocatalysis, photoelectrocatalysis hydrogen production or electrocatalysis water decomposition.
7. The use of claim 6, wherein:
the N-FeV serving as the electrocatalyst can be applied to electrocatalytic decomposition of water.
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| CN114540872A (en) * | 2022-03-23 | 2022-05-27 | 宁夏大学 | Ru/N-FeVO electrocatalyst and preparation application thereof |
| CN114540872B (en) * | 2022-03-23 | 2023-12-22 | 宁夏大学 | Ru/N-FeVO electrocatalyst and preparation and application thereof |
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