CN115354346A - P-induced doped CoFe-LDH/porous carbon electrolysis water hydrogen evolution electrode material and preparation and application thereof - Google Patents
P-induced doped CoFe-LDH/porous carbon electrolysis water hydrogen evolution electrode material and preparation and application thereof Download PDFInfo
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 80
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 47
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- QZRHHEURPZONJU-UHFFFAOYSA-N iron(2+) dinitrate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QZRHHEURPZONJU-UHFFFAOYSA-N 0.000 claims description 4
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- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical group O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims description 2
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/006—Compounds containing, besides cobalt, two or more other elements, with the exception of oxygen or hydrogen
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention belongs to the field of electrode materials, and discloses a P-induced doped CoFe-LDH/porous carbon electrolysis water hydrogen evolution electrode material, and preparation and application thereof. The electrolytic water hydrogen evolution electrode material comprises porous carbon and phosphorus-induced doped CoFe-LDH, wherein the phosphorus-induced doped CoFe-LDH randomly and uniformly grows on the porous carbon. The method takes pretreated carbonized wood as a carrier, takes ferric salt, cobalt salt and urea as raw materials, grows metal hydroxide on the surface of the carbonized wood through a hydrothermal method, and finally phosphorizes the metal hydroxide on the surface of the carbonized wood through a gas-solid reaction method by taking sodium hypophosphite monohydrate as a phosphorus source to prepare the P-induced doped CoFe-LDH/porous carbon electrode material. The surface of the electrode material for hydrogen evolution from electrolyzed water prepared by the invention has the characteristic of super-gas-phobicity, and simultaneously shows higher electrocatalysis performance, and the electrode material has the advantages of rich raw material storage, simple preparation process, economy and environmental protection.
Description
Technical Field
The invention belongs to the field of electrode materials, and particularly relates to a P-induced doped CoFe-LDH/porous carbon electrolysis water hydrogen evolution electrode material, and preparation and application thereof.
Background
To alleviate the global energy crisis and reduce environmental pollution, development of alternative and environmentally friendly new energy sources has been the focus of research today. Among the many alternative energy sources, hydrogen has been the focus of research by researchers because of its high energy density and zero pollution. Among the existing hydrogen production technologies, the electrolysis of hydrogen with a simple process and low cost has been considered as one of the most promising technologies. However, the process of electrolyzing water requires a higher overpotential. Therefore, a catalyst with higher activity is needed to reduce energy consumption and achieve good reaction effect. The best currently available catalysts are noble metal (platinum) based catalysts, but their further development in the industry is limited by their rarity and high cost. Then the development of alternatives to noble metal-based catalysts has become a focus of research. Transition metal based catalysts show excellent performance in all alternatives, with transition metal phosphides being of more central interest.
Through continuous research and development, the micro-morphology of the active material and the preparation process of the hydrogen evolution electrode are the key points for improving the hydrogen production efficiency of the electrolyzed water. Due to the high specific surface area of the nano material, active sites can be fully exposed, so that the performance of the material is greatly improved; meanwhile, due to reasonable development of the nano-structure material, the surface of the material shows excellent hydrophobic property in liquid, and a correct idea is provided for electrode materials related to gas in aqueous solution. On the other hand, since the conventional catalyst is mostly powdered, the glassy carbon electrode needs to be coated with a conductive paste. The mutual overlapping of the active materials inevitably occurs during the manufacturing process, and the electron transfer resistance is increased by the conductive paste, thereby failing to optimize the hydrogen evolution efficiency. To solve the above problems, most studies are now conducted to grow active materials in situ on conductive substrates with high specific surface area, such as metal substrates (nickel foam, copper foam, etc.), carbon materials (carbon cloth, carbon paper, biomass porous carbon) substrates, and the like. However, most of the above conductive substrates are not in line with the concept of complicated and costly processes and economical efficiency.
In the chinese patent application publication CN 110038613A, zhanglei et al, dip nickel foam into Tris-HCl buffer solution containing Fe-based metal salt, add dopamine, stir, wash, dry to obtain nickel foam-poly dopamine-iron-based metal hybrid material, and finally, obtain self-supporting iron-based metal phosphide/carbon composite material by high temperature phosphorization in a tubular furnace. However, the obtained material has large and uneven surface appearance size, so that the catalytic performance is poor, and the further development of the material is limited.
In the chinese patent application publication CN 109956458A, wandeli et al prepared hollow nano spherical phosphide from transition metal salt and polyol by solvothermal method, hydrothermal method and high-temperature solid-gas phosphorization method. However, since the prepared catalyst is powdered, a process is required during use, so that active sites are not sufficiently exposed, thereby having poor performance.
The Chinese patent application publication CN 109590002A prepares hydrogel containing a phosphorus source and a metal source, and then the prepared hydrogel is calcined at high temperature under protective gas to obtain the transition metal phosphide hydrogen evolution material. Although the raw materials are wide in source and low in price. However, the preparation process is complex, the steps are complicated, and the glassy carbon electrode is still needed for assistance in final use; meanwhile, in the hydrogen production process, the bubbles and the surface of the material have stronger binding force, and the hydrogen evolution performance is influenced. Therefore, there is a large gap from the ideal hydrogen evolution electrode material.
Chinese patent application publication CN 109772385A is to disperse transition metal or transition metal compound in distilled water, then mix with phytic acid and dry to colloid, then bake in microwave oven, calcine and reduce in tubular oven with H2 and stew in inert gas containing low concentration oxygen, finally obtain the carbon self-supported metal phosphide catalyst. The resulting samples, in which the carbon film encapsulates the catalyst from oxidation, are complicated and require various gases to be introduced into the tube furnace, which is dangerous, thus limiting further commercial applications.
Chinese patent application publication CN 104630822A is to perform a gas-solid reaction on foamed nickel or metal-modified foamed nickel in a tubular furnace atmosphere by using solid red phosphorus as a phosphorus source, and finally form a self-supporting three-dimensional porous mode transition metal phosphide hydrogen evolution electrode. The obtained electrode has good catalytic performance and acid, neutral and alkaline environments, but is not suitable for further commercial development due to the complex preparation process and high preparation cost of the foam metal.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a P-induced doped CoFe-LDH/porous carbon electrolysis water hydrogen evolution electrode material.
The invention also aims to provide a preparation method of the P-induced doped CoFe-LDH/porous carbon electrolytic water hydrogen evolution electrode material. The method relates to a pretreatment method for carbonized wood, and a P-induced doped CoFe-LDH/porous carbon electrode material is prepared by taking pretreated carbonized wood as a carrier, taking iron salt, cobalt salt and urea as raw materials, growing metal hydroxide on the surface of the carbonized wood by a hydrothermal method, and finally phosphorizing the metal hydroxide on the surface of the carbonized wood by a gas-solid reaction method by taking sodium hypophosphite monohydrate as a phosphorus source. The surface of the electrode material for hydrogen evolution by electrolysis water prepared by the invention has the characteristic of super-gas-dredging, and simultaneously shows higher electrocatalytic performance, and the electrode material has the advantages of rich raw material storage, simple preparation process, economy and environmental protection. The pretreated carbonized wood surface is clean and activated, so that the metal hydroxide nano structure can be uniformly loaded on the carbonized wood surface, and finally the P-induced doped CoFe-LDH with the nano structure is loaded on the carbonized wood; p-induced doped CoFe-LDH with a nano structure has a higher specific surface area, and active sites are fully exposed, so that the P-induced doped CoFe-LDH has higher catalytic activity; the contact area between the nano structure on the surface of the material and gas is smaller, and the super-hydrophobic performance is shown, so that a good route is provided for the preparation of the three-position self-supporting electrolysis water hydrogen evolution catalyst.
The invention further aims to provide application of the P-induced doped CoFe-LDH/porous carbon electrolyzed water hydrogen evolution electrode material in electrolyzed water hydrogen evolution.
The purpose of the invention is realized by the following scheme:
a preparation method of a phosphorus-induced doped CoFe-LDH/porous carbon electrolysis water hydrogen evolution electrode material with a nano structure comprises the following steps:
(1) Calcining natural wood serving as a raw material at high temperature under the condition of nitrogen or inert gas to obtain porous carbon, and finally cutting, washing and drying to obtain a required porous carbon sheet;
(2) Preparing a mixture containing cobalt salt, iron salt and urea CO (NH) 2 ) 2 The mixed aqueous solution is subjected to vacuum impregnation with the porous carbon sheet, then the mixed aqueous solution and the impregnated porous carbon sheet are placed in a high-pressure reaction kettle for closed reaction, and after the reaction is finished, the porous carbon sheet is washed and dried to obtain the porous carbon sheet with the hydrothermal synthesis product growing on the surface;
(3) Sodium hypophosphite monohydrate NaH 2 PO 2 ·H 2 And (3) placing the porous carbon sample obtained in the step (2) at the downstream of the tubular furnace at an upper air inlet of the tubular furnace, sealing the tubular furnace and keeping the inside of the tubular furnace oxygen-free, then introducing inert gas and heating for reaction to obtain the porous carbon sheet uniformly loaded with the nano-structure phosphorus-induced doped transition metal hydroxide.
The natural wood in the step (1) is at least one of basswood, poplar and eucalyptus, and is preferably basswood;
the high-temperature calcination in the step (1) refers to calcination at 500-1400 ℃ for 0.5-24h;
the cutting in the step (1) means cutting in a direction perpendicular to the growing direction of the wood.
The porous carbon sheet obtained in the step (1) can further comprise a cleaning and activating step before the step (2), and the cleaning and activating step comprises the following specific steps: firstly, cleaning for 0.5-5h by using concentrated acid (preferably 40-86 wt% concentrated nitric acid), so that the surface of the porous carbon is activated, the uniform growth of transition metal hydroxide on the surface is facilitated, and then, respectively cleaning for 5-30min by using deionized water and a low-boiling-point organic solvent, so that the surface of the porous carbon sheet is clean; wherein the low boiling point organic solvent is one or two of ethanol, acetone, diethyl ether and dichloromethane.
The cobalt salt in the step (2) is cobalt nitrate hexahydrate Co (NO) 2 ·6H 2 O、CoSO 4 ·7H 2 O、CoCl 2 Preferably cobalt nitrate hexahydrate Co (NO) 2 ·6H 2 O; the ferric salt in the step (2) is ferric nitrate nonahydrate Fe (NO) 3 ·9H 2 O、Fe 2 (SO 4 ) 3 ·7H 2 O、CoCl 3 Preferably, iron nitrate nonahydrate Fe (NO) 3 ·9H 2 O。
Cobalt nitrate hexahydrate Co (NO) in the mixed aqueous solution in the step (2) 2 ·6H 2 O and iron nitrate nonahydrate Fe (NO) 3 ·9H 2 The concentration of O and urea is 0-1mol/L, preferably 0.1-0.3mol/L;
the use amount of the porous carbon sheet and the mixed solution in the step (2) meets the following requirements, and when the specification of the carbon sheet is as follows: when the length is 0.1-5cm, width is 0.1-5cm and thickness is 0.5-10mm, the above-mentioned material is immersed in 5-100ml of mixed aqueous solution.
The vacuum impregnation time in the step (2) is 0-180 minutes;
the reaction in step (2) is carried out in a high-pressure reaction kettle in a closed manner at the temperature of 50-300 ℃ for 1-24h;
the washing in the step (2) is to repeatedly wash and rinse the carbon sheet by water to remove soluble ions and metal hydroxide with weak surface; the drying refers to vacuum drying at 50-100 ℃ for 1-24 hours.
The sodium hypophosphite monohydrate NaH in the step (3) 2 PO 2 ·H 2 The mass ratio of the O to the porous carbon sheet is (0.1-10): 1;
the specific operation of making the inside of the tube furnace oxygen-free in the step (3) is as follows: sealing the tube furnace, vacuumizing the furnace, introducing inert gas into the furnace, and repeating the operation for 1-10 times to ensure that the furnace is oxygen-free; the inert gas is continuously introduced at a flow rate of 10-500 ml/min.
The porous carbon sample in step (3) is preferably placed vertically.
The heating reaction in the step (3) refers to heating the temperature in the furnace to 100-500 ℃ at a heating rate of 1-10 ℃/min, and then preserving the heat for 0.5-10h.
According to the invention, porous carbon obtained from natural wood under inert gas is used as a substrate, and the carbon material obtained at high temperature has good conductivity, so that the conductivity of the active material is improved; and moreover, compared with a metal foam substrate, the metal foam substrate has good acid corrosion resistance, and the service life of the electrode is prolonged. Secondly, metal phosphide is continuously paid attention as a catalyst material with a very promising prospect, and the metal phosphide with a nano sheet structure is synthesized to be uniformly loaded on porous carbon by utilizing a hydrothermal method and a gas-solid reaction method in the design; meanwhile, the nano-square shape fully exposes the active sites, and the catalytic activity can be obviously improved.
The phosphorus-induced doped CoFe-LDH/porous carbon electrolytic water hydrogen evolution electrode material with the nano structure prepared by the method comprises porous carbon and phosphorus-induced doped CoFe-LDH, wherein the phosphorus-induced doped CoFe-LDH randomly and uniformly grows on the porous carbon, and the phosphorus-induced doped transition metal hydroxide is of a square-sheet structure or a block structure with the side length of 1-1000 mu m and the thickness of 10 nm-10 mu m.
The phosphorus-induced doped CoFe-LDH/porous carbon electrolyzed water hydrogen evolution electrode material with the square plate structure is used as a hydrogen evolution catalyst to be applied to electrolyzed water hydrogen evolution.
Compared with the prior art, the invention has the following advantages and beneficial effects:
in order to make up the defects of the powder electrode in the using process and enable the size of the active material to be in a nanometer level with high specific surface area, the invention uses porous carbon as a load matrix and carries nano flaky metal phosphide on the surface of the porous carbon in situ.
According to the invention, the active substance is uniformly loaded on the porous carbon through two steps, the obtained composite material is directly used as an electrolytic water hydrogen evolution electrode, the preparation process is simple, the raw material source is rich, and the defects of the traditional powder catalyst in the using process are well overcome.
The phosphorus-induced doped transition metal hydroxide prepared by the invention is uniformly loaded on the porous carbon sheet, and the nano structure of the phosphorus-induced doped transition metal hydroxide enables the gas generated in the hydrogen evolution process to have a smaller contact area, so that the gas and the surface of the material have smaller adhesive force, the gas can easily escape after being generated due to the smaller adhesive force, the subsequent hydrogen evolution process is prevented from being influenced, and finally the electrode shows excellent catalytic performance in the electrolytic water hydrogen evolution process.
According to the invention, the nano-flaky transition metal phosphide uniformly and disorderly grows on the surface of the porous carbon in situ, the specific surface area of the active substance is maximized due to the nano-flaky morphology, more active sites are exposed, the uniform and disorderly accumulation avoids mutual overlapping of the active substances, and the catalyst can exert the maximum catalytic effect. Therefore, the invention presents the active material in a nanometer-sized appearance and exerts the efficiency to the maximum extent.
The invention can accurately regulate and control the microscopic morphology of the transition metal hydroxide in the process of preparing the transition metal hydroxide, so that the thickness of the transition metal layered hydroxide can be regulated and controlled, the actual catalytic process of the transition metal layered hydroxide is finally influenced by the structural morphology, and a novel process method is provided for the reasonable preparation of the electrode in the process of electrolyzing water and generating hydrogen.
The surface of the electrode material for hydrogen evolution by electrolysis water prepared by the invention has the characteristic of super-gas-dredging, and simultaneously shows higher electrocatalytic performance, and the electrode material has the advantages of rich raw material storage, simple preparation process, economy and environmental protection. The pretreated carbonized wood surface is clean and activated, so that the metal hydroxide nano structure can be uniformly loaded on the carbonized wood surface, and finally the P-induced doped CoFe-LDH with the nano structure is loaded on the carbonized wood; the P-induced doped CoFe-LDH with the nano structure has a higher specific surface area, and active sites are fully exposed, so that the P-induced doped CoFe-LDH has higher catalytic activity; the contact area between the nano structure on the surface of the material and gas is smaller, and the super-hydrophobic performance is shown, so that a good route is provided for the preparation of the three-position self-supporting electrolysis water hydrogen evolution catalyst.
Drawings
FIG. 1 is a scanning electron micrograph (2000 times) of P-CoFe-LDH/CW after step (3) of example 1.
FIG. 2 is a scanning electron micrograph (2000 times) of P-CoFe-LDH/CW after step (3) of example 2. In comparison with fig. 1, fig. 2 shows the structure obtained at a higher solvent solubility, and a dense packing of the square platelet structure on the porous carbon can be observed.
FIG. 3 is a scanning electron micrograph (2000 times) of P-CoFe-LDH/CW after step (3) of example 3.
FIG. 4 is an X-ray diffraction pattern of CoFe-LDH/CW and P-CoFe-LDH/CW after steps (2) and (3) of example 2.
FIG. 5 is an X-ray photoelectron spectrum of CoFe-LDH/CW and P-CoFe-LDH/CW after steps (2) and (3) of example 2.
FIG. 6 is a linear sweep voltammogram of the electrode materials prepared in examples 1 to 3 of the present invention in 1.0mol/L KOH.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The reagents used in the examples are commercially available without specific reference.
Example 1
(1) The natural basswood is used as a raw material and is calcined in a tubular furnace for 6 hours at 1000 ℃. Then cutting into carbon sheets with the thickness of 1mm by a small table saw along the direction vertical to the growth direction of the wood, and then cleaning and drying for later use.
(2) The prepared carbonized wood chips are firstly treated by ultrasonic treatment with concentrated nitric acid (63 wt%) for 2 hours, then treated by ultrasonic treatment with deionized water, ethanol and acetone for 15 minutes respectively, and dried for later use. The preparation 20mL of the catalyst contained 0.01mol/L of Co (NO) 2 ·6H 2 O、0.01mol/L Fe(NO) 3 ·9H 2 O and 0.2mol/LA mixed aqueous solution of urea of (4). Mixing carbonized wood chips with the length of 2cm, the width of 1cm and the thickness of 1mm with the mixed solution, vacuumizing to realize vacuum impregnation for 10 minutes to ensure that the mixed solution fully enters the porous carbonized wood chips, then transferring the mixed solution and the carbonized wood chips into a high-pressure reaction kettle together, and keeping the temperature of the reaction kettle at 120 ℃ for 12 hours. And naturally cooling at room temperature, taking out the carbonized wood chips, fully washing with deionized water, and carrying out vacuum drying at 75 ℃ for 12 hours to obtain the composite material of the square-sheet structure CoFe-LDH loaded on the surfaces of the carbonized wood chips.
(3) 1g of NaH 2 PO 2 ·H 2 And (3) placing O at an upper air inlet of the tube furnace, placing 0.1g of the porous carbon sample obtained in the step (2) at the downstream of the tube furnace, sealing the tube furnace and keeping the tube furnace oxygen-free, then introducing inert gas, heating to 300 ℃ at a speed of 2 ℃/min, reacting and preserving heat for 2h, and obtaining the composite material loaded on the surface of the carbonized wood chips and uniformly loaded with P-CoFe-LDH.
Example 2
(1) The natural basswood is used as a raw material and is calcined in a tubular furnace for 6 hours at 1000 ℃. Then cutting into carbon sheets with the thickness of 1mm by a small table saw along the direction vertical to the growth direction of the wood, and then cleaning and drying for later use.
(2) The prepared carbonized wood chips are firstly treated by ultrasonic treatment for 2 hours by concentrated nitric acid (63 wt percent), then treated by ultrasonic treatment for 15 minutes by deionized water, ethanol and acetone respectively, and dried for standby. The preparation 20mL of Co (NO) containing 0.03mol/L 2 ·6H 2 O、0.03mol/L Fe(NO) 3 ·9H 2 A mixed aqueous solution of O and 0.2mol/L of urea. Mixing carbonized wood chips with the length of 2cm, the width of 1cm and the thickness of 1mm with the mixed solution, vacuumizing to realize vacuum impregnation for 10 minutes, fully introducing the mixed solution into the porous carbonized wood chips, transferring the mixed solution and the carbonized wood chips into a high-pressure reaction kettle, and keeping the temperature of the reaction kettle at 120 ℃ for 12 hours. And naturally cooling at room temperature, taking out the carbonized wood chips, fully washing with deionized water, and carrying out vacuum drying at 75 ℃ for 12 hours to obtain the composite material of the square-sheet structure CoFe-LDH loaded on the surfaces of the carbonized wood chips.
(3) 1g of NaH 2 PO 2 ·H 2 And (3) placing 0.11g of the porous carbon sample obtained in the step (2) at the downstream of the tube furnace at an upper air inlet of the tube furnace, sealing the tube furnace, keeping the interior of the tube furnace oxygen-free, introducing inert gas, raising the temperature to 300 ℃ at the speed of 2 ℃/min, reacting and preserving the temperature for 2h, and obtaining the composite material loaded on the surface of the carbonized wood chip and uniformly loaded with the P-CoFe-LDH.
Example 3
(1) The natural basswood is taken as a raw material and calcined in a tubular furnace for 6 hours at 1000 ℃. Then cutting into carbon sheets with the thickness of 1mm by a small table saw along the direction vertical to the growth direction of the wood, and then cleaning and drying for later use.
(2) The prepared carbonized wood chips are firstly treated by ultrasonic treatment for 2 hours by concentrated nitric acid (63 wt percent), then treated by ultrasonic treatment for 15 minutes by deionized water, ethanol and acetone respectively, and dried for standby. The amount of the catalyst was 20mL of Co (NO) containing 0.05mol/L 2 ·6H 2 O、0.05mol/L Fe(NO) 3 ·9H 2 A mixed aqueous solution of O and 0.2mol/L of urea. Mixing carbonized wood chips with the length of 2cm, the width of 1cm and the thickness of 1mm with the mixed solution, vacuumizing to realize vacuum impregnation for 10 minutes to ensure that the mixed solution fully enters the porous carbonized wood chips, then transferring the mixed solution and the carbonized wood chips into a high-pressure reaction kettle together, and keeping the temperature of the reaction kettle at 120 ℃ for 12 hours. Naturally cooling at room temperature, taking out the carbonized wood chips, fully washing with deionized water, and carrying out vacuum drying at 75 ℃ for 12 hours to obtain the composite material of the square-sheet structure CoFe-LDH loaded on the surfaces of the carbonized wood chips.
(3) 1g of NaH 2 PO 2 ·H 2 And (3) placing O at an upper air inlet of the tube furnace, placing 0.12g of the porous carbon sample obtained in the step (2) at the downstream of the tube furnace, sealing the tube furnace and keeping the tube furnace oxygen-free, then introducing inert gas, heating to 300 ℃ at the speed of 2 ℃/min, reacting and preserving heat for 2h, and obtaining the composite material loaded on the surface of the carbonized wood chips and uniformly loaded with P-CoFe-LDH.
FIG. 1 is a scanning electron micrograph (2000 times) of P-CoFe-LDH/CW after step (3) of example 1. A square platelet structure was observed to be spread over the porous carbon.
FIG. 2 is a scanning electron micrograph (2000 times) of P-CoFe-LDH/CW after step (3) of example 2. In comparison with fig. 1, fig. 2 is the structure obtained at higher solvent solubility, and close packing of the square platelet structure on the porous carbon can be observed.
FIG. 3 is a scanning electron micrograph (2000 times) of P-CoFe-LDH/CW after step (3) of example 3. In comparison with fig. 2, fig. 3 is a structure obtained by further increasing the solvent solubility, and it can be observed that a block-like structure is grown on the porous carbon, which is mainly caused by the continuous thickening of the block-like structure in the thickness direction.
A three-electrode (saturated calomel electrode is used as a reference electrode, a graphite rod is used as a counter electrode and a prepared sample is used as a working electrode) system is selected by utilizing an electrochemical workstation to represent linear sweep voltammograms of different samples. FIG. 6 is a linear sweep voltammogram of the electrode materials prepared in examples 1 to 3 of the present invention in 1.0mol/L KOH.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such modifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of a phosphorus-induced doped CoFe-LDH/porous carbon electrolysis water hydrogen evolution electrode material is characterized by comprising the following steps:
(1) Calcining natural wood serving as a raw material at high temperature under the condition of nitrogen or inert gas to obtain porous carbon, and finally cutting, washing and drying to obtain a required porous carbon sheet;
(2) Preparing a mixture containing cobalt salt, iron salt and urea CO (NH) 2 ) 2 The mixed aqueous solution is vacuum-impregnated with the porous carbon sheet, then the mixed aqueous solution and the impregnated porous carbon sheet are placed in a high-pressure reaction kettle for closed reaction, and after the reaction is finished, the porous carbon sheet is washed and dried to obtain the porous carbon sheet with the hydro-thermal synthesis product growing on the surface;
(3) Sodium hypophosphite monohydrate NaH 2 PO 2 ·H 2 And (3) placing the porous carbon sample obtained in the step (2) at the downstream of the tubular furnace at an upper tuyere of the tubular furnace, sealing the tubular furnace and enabling the inside of the tubular furnace to be free of oxygen, then introducing inert gas and heating for reaction to obtain the porous carbon sheet uniformly loaded with the nano-structure phosphorus-induced doped transition metal hydroxide, namely the phosphorus-induced doped CoFe-LDH/porous carbon electrolysis water hydrogen evolution electrode material.
2. The preparation method of the phosphorus-induced doped CoFe-LDH/porous carbon electrolytic water hydrogen evolution electrode material as claimed in claim 1, wherein:
the natural wood in the step (1) is at least one of basswood, poplar and eucalyptus;
the high-temperature calcination in the step (1) refers to calcination at 500-1400 ℃ for 0.5-24h;
the cutting in the step (1) refers to cutting along the direction perpendicular to the growth direction of the wood.
3. The preparation method of the phosphorus-induced doped CoFe-LDH/porous carbon electrolytic water hydrogen evolution electrode material as claimed in claim 1, wherein:
the porous carbon sheet obtained in the step (1) may further include an activation and cleaning step before the step (2), specifically as follows: cleaning with concentrated acid for 0.5-5h to activate the surface of the porous carbon, so that transition metal hydroxide can uniformly grow on the surface, and then cleaning with deionized water and low-boiling-point organic solvent for 5-30min to clean the surface of the porous carbon sheet; wherein the low boiling point organic solvent is one or two of ethanol, acetone, diethyl ether and dichloromethane.
4. The preparation method of the phosphorus-induced doped CoFe-LDH/porous carbon electrolytic water hydrogen evolution electrode material as claimed in claim 1, wherein:
the cobalt salt in the step (2) is cobalt nitrate hexahydrate Co (NO) 2 ·6H 2 O、CoSO 4 ·7H 2 O、CoCl 2 Preferably cobalt nitrate hexahydrate Co (NO) 2 ·6H 2 O; iron described in step (2)The salt is ferric nitrate nonahydrate Fe (NO) 3 ·9H 2 O、Fe 2 (SO 4 ) 3 ·7H 2 O、CoCl 3 Preferably, iron nitrate nonahydrate Fe (NO) 3 ·9H 2 O。
5. The preparation method of the phosphorus-induced doped CoFe-LDH/porous carbon electrolytic water hydrogen evolution electrode material as claimed in claim 1, wherein:
cobalt nitrate hexahydrate Co (NO) in the mixed aqueous solution in the step (2) 2 ·6H 2 O and iron nitrate nonahydrate Fe (NO) 3 ·9H 2 The concentration of O and urea is 0-1mol/L; preferably 0.01-0.03mol/L;
the use amount of the porous carbon sheet and the mixed solution in the step (2) meets the following requirements, and when the specification of the carbon sheet is as follows: when the length is 0.1-5cm, the width is 0.1-5cm and the thickness is 0.5-10mm, the water-soluble polymer is correspondingly immersed in 5-100ml of mixed aqueous solution.
6. The preparation method of the phosphorus-induced doped CoFe-LDH/porous carbon electrolysis water hydrogen evolution electrode material as claimed in claim 1, wherein:
the vacuum impregnation time in the step (2) is 0-180 minutes;
the reaction temperature in the step (2) is 50-300 ℃ and the reaction time is 1-24h.
7. The preparation method of the phosphorus-induced doped CoFe-LDH/porous carbon electrolytic water hydrogen evolution electrode material as claimed in claim 1, wherein:
the sodium hypophosphite monohydrate NaH in the step (3) 2 PO 2 ·H 2 The mass ratio of the O to the porous carbon sheet is (0.1-10): 1.
8. the preparation method of the phosphorus-induced doped CoFe-LDH/porous carbon electrolytic water hydrogen evolution electrode material as claimed in claim 1, wherein:
the heating reaction in the step (3) is to heat the temperature in the furnace to 100-500 ℃ at a heating rate of 1-10 ℃/min, and then to keep the temperature for 0.5-10h.
9. A phosphorus-induced doped CoFe-LDH/porous carbon electrohydroelectrolytic hydrogen evolution electrode material prepared by the method of any one of claims 1 to 8.
10. The use of the phosphorus-induced doped CoFe-LDH/porous carbon electrolyzed water hydrogen evolution electrode material of claim 9 in the electrolysis of water to evolve hydrogen.
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