CN114381758A - Nickel-doped boehmite and reduced graphene oxide composite electrocatalyst and preparation and application thereof - Google Patents
Nickel-doped boehmite and reduced graphene oxide composite electrocatalyst and preparation and application thereof Download PDFInfo
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Abstract
The invention discloses a nickel-doped boehmite and reduced graphene oxide composite electrocatalyst, and preparation and application thereof3@ RGO electrocatalysts useful for the conversion of CO2Electrocatalytic reduction to CO. The preparation method is simple, and the obtained catalyst has high catalytic activity.
Description
Technical Field
The invention belongs to the field of electrocatalysis, and particularly relates to a nickel-doped boehmite and reduced graphene oxide composite electrocatalyst, and preparation and application thereof.
Background
Greenhouse gas carbon dioxide (CO)2) Electrochemical conversion to energy fuels and value-added chemicals is one of the most valuable methods of collecting pollutants and producing renewable energy. Electrocatalytic CO2Reduction to carbon monoxide (CO) is a major concern of researchers due to its economic and environmental advantages. However, CO2The stable molecular structure and slow reaction kinetics allow reduction (CO)2RR) are poor in reaction rate and selectivity, thereby limiting its industrial application.
In recent years, nanoscale inorganic layered materials have been widely used in the fields of novel nanocomposites, ion exchange materials, photochemistry, catalysis, and the like. The Zhang Ping team proposes that ferronickel bimetal hydroxide is stripped into single pieces by a solid phase stripping technology, the single pieces and carbon nano tubes are subjected to electrostatic self-assembly, and then a (CNT-N-NiFe) electrocatalyst is prepared by high-temperature calcination and used for carbon dioxide electrocatalytic reduction to carbon monoxide, namely, carbon monoxide FaradayThe efficiency reaches 82.6 percent, but the method destroys the structure of the Double metal Hydroxide, and the material preparation process is complicated (CHEN H, ZHANG P, XIE R, et al, high-Temperature simulation Induced Carbon Nanotubes @ NiFe-layer-Double-Hydroxide nanodielectrics Taking as an Oxygen Evolution Reaction for CO)2 Electroreduction[J].AdvancedMaterials Interfaces,2021,8(19).)
Boehmite is a compound assembled by interaction of positively charged host layers and interlayer anions through non-covalent bonds, and has low electron transfer efficiency in an electrocatalytic process. The combination of boehmite and a conductive material (such as graphene, carbon nanotubes, carbon quantum dots, etc.) is one of effective methods for improving the conductivity thereof, but graphene seriously affects the ion transmission rate and conductivity due to its aggregation effect.
Disclosure of Invention
Based on the problems in the prior art, the invention provides a nickel-doped boehmite and reduced graphene oxide composite electrocatalyst, and preparation and application thereof, and aims to efficiently electrocatalytically reduce carbon dioxide into carbon monoxide.
The invention adopts the following technical scheme for realizing the purpose:
a preparation method of a nickel-doped boehmite and reduced graphene oxide composite electrocatalyst is characterized by comprising the following steps: adding urea into a mixed solution of formamide and water for dissolving, then adding graphene oxide for ultrasonic dispersion, then sequentially adding nickel nitrate hexahydrate and aluminum nitrate nonahydrate, stirring uniformly, adjusting the pH to 8-10, and then continuously carrying out hydrothermal reaction for 6-8 h at 160-200 ℃; after the reaction is finished, cooling to room temperature, washing and drying the obtained product to obtain the nickel-doped boehmite and reduced graphene oxide composite electrocatalyst which is marked as Ni-AlO (OH)3@RGO。
Further: the dosage ratio of formamide, water, urea, graphene oxide to nickel nitrate hexahydrate is 20-25 mL: 55-60 mL: 2.4 g: 80 mg: 0.870g, wherein the molar ratio of the nickel nitrate hexahydrate to the aluminum nitrate nonahydrate is 1-5: 1.
the nickel-doped boehmite and reduced graphene oxide composite electrocatalyst disclosed by the invention can be used for electrocatalysis of carbon dioxide to carbon monoxide.
The invention has the beneficial effects that:
1. according to the invention, partial graphene oxide is reduced by a one-step hydrothermal synthesis method, and the double-metal hydroxide is used as a substrate and grows and assembles in situ on the single-layer reduced graphene oxide to form a composite catalytic material which is a CO composite catalytic material with multiple active sites, large specific surface area and good conductivity2Provides a new strategy for the conversion application of the catalyst, and can also realize the electrocatalysis of CO2Large-scale commercialization of reduction provides both theoretical and technical support.
2. According to the preparation method, Graphene Oxide (GO) is used, oxygen-containing functional groups among graphene oxide layers can break large pi bonds to weaken Van der Waals force and expand interlayer spacing, the graphene oxide layers are peeled into single-layer graphene oxide by an ultrasonic method, and the single-layer graphene oxide is used as a conductive carrier to grow the layered double metal hydroxide composite electrocatalyst. On one hand, due to the unique six-membered ring network structure with carbon atoms, graphene oxide has a large specific surface area and a large pi conjugated structure, and two surfaces of a sheet layer can be combined with metal hydroxide together through covalent bonds to form a stable composite material. On the other hand, the growth of the metal hydroxide on the graphene oxide can increase the specific surface area of the graphene oxide monomer and the metal hydroxide monomer, and the increase of the pore duct is beneficial to the transmission of substances.
3. The catalyst based on the double metal hydroxide has higher catalytic activity of electrocatalytic reduction of carbon dioxide into carbon monoxide compared with single metal hydroxide.
Drawings
FIG. 1 is an XRD pattern of each sample in example 1, wherein (a) corresponds to Ni-AlO (OH)3(b) corresponds to AlO (OH) @ RGO, (c) corresponds to Ni-AlO (OH)3@ RGO, (d) corresponding to Ni (OH)2@ RGO, (e) corresponds to GO.
FIG. 2 is a SEM photograph of each sample in example 1, wherein (a) is a SEM photograph of GO, and (b) is a photograph of Ni-AlO (OH)3SEM picture of (b), (c) is Ni (OH)2SEM photograph of @ RGO, (d) is Ni-AlO (OH)3SEM spectra of @ RGO.
FIG. 3 shows Ni-AlO (OH) in example 13The mapping and EDX diagrams of @ RGO, wherein (a) is Ni-AlO (OH)3Mapping spectrum of @ RGO, (b) is Ni-AlO (OH)3EDX profile of @ RGO.
FIG. 4 is a TEM image of each sample in example 1, wherein (a) corresponds to Ni-AO (OH)3(b) corresponds to AlO (OH) @ RGO, (c) corresponds to Ni (OH)2@ RGO, (d) corresponding to Ni-AlO (OH)3@RGO。
FIG. 5 shows N of each sample in example 12Adsorption and desorption isotherms (inset) and pore size distribution curves, wherein (a) corresponds to GO, (b) corresponds to Ni-AlO (OH)3(c) corresponds to AlO (OH) @ RGO, (d) corresponds to Ni (OH)2@ RGO, (e) corresponding to Ni-AlO (OH)3@RGO。
FIG. 6 is an XPS spectrum for each sample of example 1, wherein (a) is the full spectrum, (b) is the Ni 2p fine spectrum, (C) is the Al 2p fine spectrum, (d) is the C1s fine spectrum, and (e) is the N1s fine spectrum.
FIG. 7 shows AlO (OH) @ RGO and Ni (OH) in example 12@ RGO and Ni-AlO (OH)3The electrochemical performance characterization result graph of @ RGO comprises (a) LSV curve corresponding to each sample, carbon monoxide Faraday efficiency (CO FE) curve corresponding to each sample, and carbon monoxide bias current density j corresponding to each sampleCOCurve, (d) Tafel curve corresponding to each sample, (e) slope curve corresponding to current density difference (delta j) and different scanning rates of each sample, (f) slope curve corresponding to Ni-AlO (OH)3Catalytic stability of @ RGO at-0.9 Vvs.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
This example prepares the electrocatalyst as follows:
adding 2.4g of urea into a mixed solution of 24mL of formamide and 56mL of water for dissolving, then adding 80mg of graphene oxide for uniform ultrasonic dispersion, and then sequentially adding 0.870g of nitre hexahydrateNickel acid and 0.375g of aluminum nitrate nonahydrate are evenly stirred, the pH value is adjusted to 10 by using 1M NaOH solution, and then the mixture is moved to a stainless steel high-pressure reaction kettle to carry out hydrothermal reaction for 8 hours at 180 ℃; after the reaction is finished, cooling to room temperature, washing the obtained product for multiple times by using deionized water and ethanol, and drying at 60 ℃ to obtain the nickel-doped boehmite and reduced graphene oxide composite electrocatalyst which is recorded as Ni-AlO (OH)3@RGO。
For comparison, this example also prepared a single metal electrocatalyst, Ni (OH)2@ RGO, AlO (OH) @ RGO and Ni-AlO (OH) without graphene, the preparation method is the same as the above method, and the difference is that: preparation of Ni (OH)2No aluminum nitrate nonahydrate was added at @ RGO, no nickel nitrate hexahydrate was added at AlO (OH) @ RGO, and no GO was added at Ni-AlO (OH) preparation.
FIG. 1 is an XRD pattern of each sample, wherein (a) corresponds to Ni-AlO (OH)3(b) corresponds to AlO (OH) @ RGO, (c) corresponds to Ni-AlO (OH)3@ RGO, (d) corresponding to Ni (OH)2@ RGO, (e) corresponds to GO. The XRD pattern reflects Ni-AlO (OH)3AlO (OH) @ RGO and Ni-AlO (OH)3The layered structure of @ RGO shows that the baseline is basically stable and no obvious miscellaneous peak appears by observing the whole atlas, which indicates that the layered structure formed by water and alumina is good and the crystal phase is single. After all the GO is subjected to hydrothermal reaction, the (001) characteristic diffraction peak of the GO at 10.59 degrees disappears, and a graphene (002) characteristic peak appears, which indicates that after hydrothermal synthesis, oxygen-containing groups among graphene oxide layers are reduced, and Reduced Graphene Oxide (RGO) is formed.
FIG. 2 is an SEM image of each sample, wherein (a) is the SEM image of GO, and (b) is Ni-AlO (OH)3SEM picture of (b), (c) is Ni (OH)2SEM photograph of @ RGO, (d) is Ni-AlO (OH)3SEM spectra of @ RGO. From 2(a) it can be observed that GO without any treatment is in a layered structure and overlaps. As can be seen from FIG. 2(b), Ni-AlO (OH) prepared by hydrothermal synthesis3In a stacked lamellar structure. As can be seen from FIG. 2(c), Ni (OH) was produced by hydrothermal synthesis2The Ni compound in @ RGO forms a small number of extremely thin small fragments to be attached to the reduced graphene oxide, and most of the reduced graphene oxide is exposed. FIG. 2(d) shows that Ni-AlO (OH)3@ RGO Ni-AlO (OH)3The graphene oxide (RGO) is closely and uniformly adhered to an RGO layered structure in a sheet layer shape, has good appearance, improves the specific surface area of the catalyst, is beneficial to the adsorption of reactant molecules by materials, and also presents obvious irregular wrinkle appearance in the sheet layer shape.
FIG. 3(a) shows Ni-AlO (OH)3The mapping spectrum of @ RGO shows that Ni, Al, O and C exist in the compound, and elements in the catalyst prepared by the hydrothermal synthesis method are uniformly dispersed without forming agglomeration of metal particles. FIG. 3(b) shows Ni-AlO (OH)3EDX spectra of the corresponding region of @ RGO showed a Ni to Al content ratio of 1:16.2, indicating that a small amount of nickel was successfully doped into AlO (OH).
FIG. 4 is a TEM image of each sample, wherein (a) corresponds to Ni-AlO (OH)3(b) corresponds to AlO (OH) @ RGO, (c) corresponds to Ni (OH)2@ RGO, (d) corresponding to Ni-AlO (OH)3@ RGO. In FIG. 4(a), a large number of irregular lamellar structures with edges composed of fibrous structural units are observed, and the interior exhibits an agglomerated structure which is not favorable for the exposure of active sites; RGO and AlO (OH) close packing is observed in FIG. 4(b), with no apparent monolithic layer structure present; FIG. 4(c) because the phase of nickel-related hydroxide formation is minimal, only a tightly packed RGO structure is observed; fig. 4(d) shows that Ni — alo (oh) is attached to the gauze-like monolithic layer of reduced graphene oxide in a monolithic layer structure, and this is stacked as a structural unit to form a lamellar structure.
FIG. 5 shows N of each sample2Adsorption and desorption isotherms (inset) and pore size distribution curves, wherein (a) corresponds to GO, (b) corresponds to Ni-AO (OH)3(c) corresponds to AlO (OH) @ RGO, (d) corresponds to Ni (OH)2@ RGO, (e) corresponding to Ni-AlO (OH)3@ RGO. As can be seen from FIG. 5, GO and Ni-AlO (OH)3All belong to III type isotherms, and H3 type hysteresis loops appear in a medium specific pressure region, which indicates that the catalyst has mesopores. Table 1 summarizes the BET specific surface area, pore volume and pore size of each catalyst.
TABLE 1 physical adsorption Performance parameters of the samples
FIG. 6 shows Ni-AlO (OH)3、AlO(OH)@RGO、Ni(OH)2@ RGO and Ni-AlO (OH)3The XPS spectra of @ RGO, where (a) is the full spectrum of each sample, (b) is the Ni 2p fine spectrum, (C) is the Al 2p fine spectrum, (d) is the C1s fine spectrum, and (e) is the N1s fine spectrum. In the presence of Ni-AlO (OH)3The peaks for C, O, Al, N and Ni are readily observed in @ RGO, which is consistent with the EDX results. FIG. 6(b) shows Ni (OH)2@ RGO and Ni-AlO (OH)3Fine spectra of Ni 2p of @ RGO, the results in the figure indicate that Ni-AlO (OH)3Binding energy of Ni 2p of @ RGO to Ni (OH)2@ RGO has a binding energy of 0.05eV higher. FIG. 6(c) is AlO (OH) @ RGO and Ni-AlO (OH)3The results of Al 2p fine Spectroscopy of @ RGO showed that Al 2p has a binding energy of 74.10eV in AlO (OH) @ RGO and Ni-AlO (OH)3The binding energy in @ RGO is 74.03eV, indicating that doping with a small amount of nickel shifts the binding energy of Al 2p by 0.07eV in the direction of lower binding energy. It can therefore be concluded that the cause of this change is likely to be associated with Ni2+Ion doping of AlO (OH). As a result, Ni-AlO (OH)3@ RGO of Al3+The electron balance structure becomes an electron-rich junction, which is beneficial to improving the electrocatalytic performance.
Weigh 5mg of the prepared catalyst and 2mg of carbon black in a test tube; according to the volume ratio of 100: 1 preparing a mixed solution of absolute ethyl alcohol and Nafion, adding 0.5mL of the mixed solution into a test tube, and carrying out ultrasonic treatment for 30min to form black ink. Spreading 40 μ L of the extract on 1cm of the substrate with a pipette2Drying the carbon paper electrode at 60 ℃ for later use. The electrochemical workstation of Shanghai Chenghua CHI660E was used as a three-electrode system to study Ni-AlO (OH)3@ RGO) for electrocatalytic carbon dioxide reduction (CO)2RR) electrocatalytic properties. The reference electrode is a silver/silver chloride electrode, the counter electrode is a platinum mesh electrode, and the catalyst is coated on carbon paper to serve as a working electrode. All catalysts were tested for electrochemical performance in a type H two-compartment cell. Electrocatalytic reduction of carbon dioxide takes place in the cathode reaction tank, and the electrolyte in the cathode reaction tank and the anode reaction tank is 20mL0.1M potassium bicarbonate (KHCO)3) Aqueous solution, pH 6.8. Gas mass flow meter for carbon dioxide (CO) control2) Flow rate 20 mL/min-1Gas outlet of cathode reaction tank andgas chromatography was used for communication, and the whole reaction was carried out at room temperature and atmospheric pressure. Recording the linear sweep voltammetry, carbon monoxide faradaic efficiency, partial current density, Tafel slope, electrochemical active area and stability of the three catalysts.
By Linear Sweep Voltammetry (LSV) vs. Ni-AlO (OH)3@ RGO, Ni @ RGO and AlO (OH) @ RGO for CO2And the electrochemical performance of reduction is evaluated, and the change relation of the catalytic current of the sample along with the voltage can be preliminarily obtained. As shown in FIG. 7(a), in the same potential region, Ni-AlO (OH)3@ RGO, indicating the maximum current density of Ni-AlO (OH)3@ RGO has a high activity for electrocatalytic reduction of carbon dioxide. FIG. 7(c) shows the partial current density of electrocatalytic reduction of carbon dioxide to carbon monoxide for each catalyst, Ni-AlO (OH)3@ RGO has the highest bias current density. From the Faraday efficiency (CO FE) curve of carbon monoxide in FIG. 7(b), it can be seen that the Faraday efficiency of carbon monoxide reached up to 44.9% at AlO (OH) @ RGO, Ni (OH)2@ RGO has a carbon monoxide Faraday efficiency of up to 88.2%, while Ni-AlO (OH)3The maximum Faraday efficiency of carbon monoxide of @ RGO can reach 92.2 percent, which is in accordance with Ni2+、Al3+And the synergistic effect of reducing graphene oxide. And, in contrast, the results of FIG. 7(d) show Ni-AlO (OH)3@ RGO has the smallest Tafel slope, indicating that Ni-AlO (OH)3The @ RGO has larger current gain when the applied potential is lower, which is favorable for promoting the catalytic reaction, and further proves the excellent catalytic activity of the @ RGO. CO for further exploration of catalyst materials2RR catalytic mechanism, determine the reaction active surface area, AlO (OH)) @ RGO, Ni @ RGO and Ni-AlO (OH)) @ RGO were subjected to cyclic voltammogram analysis. As shown in FIG. 7(e), the voltage window is set to-0.6-0.7 Vvs RHE, and the scan speed is set to 1-10 mV s-1And setting the current density point as-0.65V, and obtaining the double electric layer capacitance (Cdl) of the material by fitting the slope, thereby comparing electrochemical active areas. The results indicate that Cdl of Ni-AlO (OH) @ RGO has a maximum value, meaning the largest electrochemically active area (ECSA), and thus more active sites participate in the reaction.
According to the above experimental results, it is shown that the nickel-doped boehmite and the reduced aluminaCompared with a single metal hydroxide and graphene composite catalyst, the electrochemical performance of the graphene composite electrocatalyst is obviously improved. The doping of a small amount of nickel shifts the binding energy of Al 2p toward a lower binding energy, and it is inferred that this result is Ni-AlO (OH)3@ RGO of Al3+The electron balance structure becomes an electron-rich structure, which is beneficial to improving the electrocatalytic performance. In addition, the lamellar double metal hydroxide grows on the reduced graphene oxide, so that the formation of non-uniform slits is facilitated, the transfer of reactants and products is accelerated, and the exposure of active sites is facilitated.
The above illustration is only an exemplary embodiment of the present invention and is not intended to limit the present invention.
Claims (4)
1. A preparation method of a nickel-doped boehmite and reduced graphene oxide composite electrocatalyst is characterized by comprising the following steps: adding urea into a mixed solution of formamide and water for dissolving, then adding graphene oxide for ultrasonic dispersion, then sequentially adding nickel nitrate hexahydrate and aluminum nitrate nonahydrate, stirring uniformly, adjusting the pH to 8-10, and then continuously carrying out hydrothermal reaction for 6-8 h at 160-200 ℃; after the reaction is finished, cooling to room temperature, washing and drying the obtained product to obtain the nickel-doped boehmite and reduced graphene oxide composite electrocatalyst which is marked as Ni-AlO (OH)3@RGO。
2. The method of claim 1, wherein: the dosage ratio of formamide, water, urea, graphene oxide to nickel nitrate hexahydrate is 20-25 mL: 55-60 mL: 2.4 g: 80 mg: 0.870g, wherein the molar ratio of the nickel nitrate hexahydrate to the aluminum nitrate nonahydrate is 1-5: 1.
3. a nickel-doped boehmite and reduced graphene oxide composite electrocatalyst prepared according to the preparation method of claim 1 or 2.
4. Use of a nickel-doped boehmite and reduced graphene oxide composite electrocatalyst according to claim 3, characterised in that: used for electrocatalytic reduction of carbon dioxide to carbon monoxide.
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| CN105719850A (en) * | 2016-01-25 | 2016-06-29 | 中国石油大学(华东) | Grapheme@polypyrrole/layer double hydroxide nanowire ternary composite and preparation method and application thereof |
| US20190048482A1 (en) * | 2017-08-10 | 2019-02-14 | Board Of Trustees Of The University Of Arkansas | 3d reduced graphene oxide foams embedded with nanocatalysts, synthesizing methods and applications of same |
| CN113546628A (en) * | 2021-06-22 | 2021-10-26 | 南京工业大学 | Preparation method of bimetallic hydroxide-graphene aerogel electrocatalyst |
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| CN105719850A (en) * | 2016-01-25 | 2016-06-29 | 中国石油大学(华东) | Grapheme@polypyrrole/layer double hydroxide nanowire ternary composite and preparation method and application thereof |
| US20190048482A1 (en) * | 2017-08-10 | 2019-02-14 | Board Of Trustees Of The University Of Arkansas | 3d reduced graphene oxide foams embedded with nanocatalysts, synthesizing methods and applications of same |
| CN113546628A (en) * | 2021-06-22 | 2021-10-26 | 南京工业大学 | Preparation method of bimetallic hydroxide-graphene aerogel electrocatalyst |
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| CN115814754A (en) * | 2022-12-14 | 2023-03-21 | 南昌宝弘新材料技术有限公司 | Boehmite modified adsorbent and preparation method and application thereof |
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