CN113529405A - Cauliflower-shaped Co (OH) growing on surface of carbon cloth2Method for producing (E) -Ni - Google Patents

Cauliflower-shaped Co (OH) growing on surface of carbon cloth2Method for producing (E) -Ni Download PDF

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CN113529405A
CN113529405A CN202110771538.2A CN202110771538A CN113529405A CN 113529405 A CN113529405 A CN 113529405A CN 202110771538 A CN202110771538 A CN 202110771538A CN 113529405 A CN113529405 A CN 113529405A
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carbon cloth
cauliflower
uniform solution
ultrasonic dispersion
grade
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张新孟
毛子轩
赵元肖
欧阳海波
伍媛婷
许占位
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/49—Oxides or hydroxides of elements of Groups 8, 9, 10 or 18 of the Periodic System; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
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    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/40—Fibres of carbon

Abstract

The invention discloses a method for growing cauliflower-shaped Co (OH) on the surface of carbon cloth2The preparation method of the Ni specifically comprises the following steps of 1: adding graphene oxide into deionized water containing carbon cloth, and performing ultrasonic dispersion to obtain a uniform solution; step 2: adding CoCl into the homogeneous solution in the step 1 respectively2·6H2O and NiCl2·6H2O, obtaining a uniform solution through ultrasonic dispersion; and step 3: putting the solution obtained in the step 2 into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining into an autoclave, reacting for 4-12 h at 150-180 ℃ under a sealed condition, taking out carbon cloth CC, washing and drying to obtain Co (OH)2-Ni/rGO/CC material; the invention uses CoCl2·6H2O and NiCl2·6H2The preparation method is low in cost and simple and feasible; preparation of the resulting Co (OH)2the-Ni/rGO/CC material has short detection response time, high sensitivity and excellent electrochemical performance, and can be used as a sensing material, a battery cathode material, a catalyst, a gas sensitive material, a magnetic material and an electrochemical sensor electrode material.

Description

Cauliflower-shaped Co (OH) growing on surface of carbon cloth2Method for producing (E) -Ni
Technical Field
The invention belongs to the technical field of micro-nano material preparation, and particularly relates to a method for growing cauliflower-shaped Co (OH) on the surface of carbon cloth2-a method for the preparation of Ni.
Background
Transition metal-based sensing materials, such as sulfides, hydroxides, and selenides, have been extensively studied as alternatives to noble metal sensing materials. Among various transition metals, Co has long been found to be an excellent sensing material, has good adaptability, and can be prepared into various nanometer forms, such as nanorods, nanometer petals, nanometer microspheres, nanometer needles and the like, and the excellent performances of the nanometer forms in the aspects of response range, detection limit, stability, anti-interference performance and the like. But Co (OH)2Has few active sites, has certain difference in electrochemical performance compared with other materials, and can generally pass through the pair of Co (OH)2The doping modification is carried out to achieve the effect of improving the active sites. Wherein Ni atom is introduced into Co (OH)2Composite into Co (OH)2Ni, which provides it with more catalytically active sites, while providing many efficient electrolyte-accessible channels for deionization transport.
Hydrothermal method is considered as a promising method for synthesizing nano-structures, because it is environmentally friendly and has controllable morphology, and can produce various nano-structures including nanowires, nanosheets, nanoflowers, and the like. Xiao Hua et al (The Journal of Physical Chemistry C,2011,115(45): 22662-22668) in NiCl2·6H2O is nickel source, Co (NO)3)2·6H2O is a cobalt source and is electrodeposited in a standard three-electrode glass cell. At 1.0mA cm-2Under the constant current condition, carrying out electrodeposition by using an electrochemical workstation to obtain the industrial foam nickel loaded Co (OH)2A film.
Carbon Cloth (CC) as a common material in electrochemistryThe material is seen primarily because of its very good electrical conductivity and mechanical properties. The CC is used as a flexible self-supporting substrate, so that the specific surface area of the composite material can be greatly improved, and a firm substrate is provided for the growth of subsequent materials. Lvweixin et al (Chinese patent 201810510211.8, publication No. CN108425134A, published date 2018.08.21) proposed a nano NiCo2O4Preparation method of/CC electrode by combining hydrothermal method and electroplating method to prepare NiCo2O4Loading the nano-sheet to CC to prepare NiCo with a nano-sheet layered structure2O4a/CC electrode. The CC is used as a flexible self-supporting substrate, has good mechanical property and conductivity, and can greatly improve the specific surface area of the composite material. The electrochemical performance of the carbon nanotube can be kept unchanged under the condition of shape change, and the CC is low in price. However, it is worth noting that CoCl is not currently employed2·6H2O and NiCl2·6H2Hydrothermal reaction system with O as raw material to prepare Co (OH) with cauliflower shape growing on CC2-literature reports of Ni multilevel micro-nano structure materials.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a hydrothermal synthesis method for preparing Co (OH)2-a cauliflower-like material formed by self-assembling Ni micro-nano particles.
In order to achieve the purpose, the invention adopts the following technical scheme:
cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: adding 0.0075-0.0225 g of graphene oxide into 30mL of deionized water containing carbon cloth, and performing ultrasonic dispersion to obtain a uniform solution;
step 2: respectively adding 0.1454-0.2908 g of CoCl into the uniform solution obtained in the step 12·6H2O and 0.0589-0.1178 g NiCl2·6H2O, obtaining a uniform solution through ultrasonic dispersion;
and step 3: putting the solution obtained in the step 2 into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining into an autoclave, and sealing the autoclave at 150 to EReacting for 4-12 h at 180 ℃, taking out the carbon cloth CC, washing and drying to obtain Co (OH)2-Ni/rGO/CC materials.
Further, the ultrasonic dispersion time in the step 1 and the ultrasonic dispersion time in the step 2 are both 20-40 min.
Further, the carbon cloth CC has a sheet structure of 1.5cm by 1.5 cm.
Further, CoCl used in the step 22·6H2O and NiCl2·6H2O is AR grade, 99.0%.
Further, the autoclave in the step 3 was made of stainless steel and had a volume of 34.8 mL.
Further, the drying manner in the step 3 is vacuum drying.
Compared with the prior art, the invention has the following technical effects:
the invention uses CoCl2·6H2O and NiCl2·6H2The preparation method is characterized in that O is used as a raw material, carbon cloth CC is used as a supporting material, deionized water is used as a solvent, and graphene is added as a conductive carrier, so that the preparation cost is low, and the preparation method is simple and feasible; co (OH) prepared by hydrothermal synthesis2the-Ni/rGO/CC material has short detection response time, high sensitivity and excellent electrochemical performance, and can be used as a sensing material, a battery cathode material, a catalyst, a gas sensitive material, a magnetic material and an electrochemical sensor electrode material.
Drawings
FIG. 1 shows Co (OH) according to the present invention2/CC, Ni/CC and Co (OH)2-XRD pattern of Ni/rGO/CC;
FIG. 2 shows the present invention Co (OH)2-SEM picture of Ni/rGO/CC material;
FIG. 3 is an enlarged view of a portion of FIG. 1;
FIG. 4 shows the present invention Co (OH)2-Ni/rGO/CC Material Pair H2O2CV curve of electrochemical sensing of (1);
FIG. 5 shows the present invention Co (OH)2-Ni/rGO/CC Material Pair H2O2I-t plot of electrochemical sensing.
Detailed Description
The present invention will be explained in further detail with reference to examples.
Example 1
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 4h, taking out the carbon cloth CC, washing, and drying in vacuum for 6h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 2
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 8h, taking out the carbon cloth CC, washing, and drying in vacuum for 6h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 3
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 6h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 4
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 150 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 6h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 5
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 160 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 6h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 6
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 170 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 6h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 7
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 6h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 8
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 6h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 9
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 30min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 30min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 8h, taking out the carbon cloth CC, washing, and drying in vacuum for 9h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 10
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 30min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 30min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 9h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 11
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 30min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 30min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 150 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 9h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 12
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 30min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 30min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 160 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 9h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 13
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 30min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 30min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 170 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 9h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 14
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 30min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 30min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 9h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 15
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 4h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 16
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 8h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 17
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 18
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 150 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co: (A), (B), (C) and aOH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 19
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 160 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 20
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 170 ℃ for 12h, taking out the carbon cloth CC, washing, and vacuum drying for 12h to obtain the carbon cloth CCCo(OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 21
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.1454g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0589g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 22
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 4h, taking out the carbon cloth CC, washing, and vacuum drying for 6h to obtain the carbon cloth CCCo(OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 23
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 8h, taking out the carbon cloth CC, washing, and drying in vacuum for 6h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 24
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and vacuum drying for 6h to obtain the carbon cloth CCCo(OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 25
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 150 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 6h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 26
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining, sealing, reacting at 160 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 6h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 27
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 170 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 6h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 28
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0075g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 20min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 20min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 6h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 29
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 30min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 30min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 4h, taking out the carbon cloth CC, washing, and drying in vacuum for 9h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 30
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 30min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 30min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 8h, taking out the carbon cloth CC, washing, and drying in vacuum for 9h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 31
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 30min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 30min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 9h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 32
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 30min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 30min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 150 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 9h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 33
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 30min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 30min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 160 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 9h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 34
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 30min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 30min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 170 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 9h to obtain Co (OH))2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 35
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0150g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm multiplied by 1.5cm carbon cloth CC is added for ultrasonic dispersion for 30min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 30min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 9h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 36
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 4h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co: (A), (B), (C) and aOH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 37
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 8h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 38
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and vacuum drying for 12h to obtain the carbon cloth CCCo(OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 39
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 150 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 40
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining, sealing, reacting at 160 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
EXAMPLE 41
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 170 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 42
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: weigh 0.2908g of AR grade, 99.0% CoCl2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1178g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 43
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: 0.1768g of AR grade, 99.0% CoCl were weighed out2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.0896g of AR grade, 99.0% NiCl were weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co (OH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
Example 44
Cauliflower-shaped Co (OH) growing on surface of carbon cloth2A method for producing Ni, comprising the following steps;
step 1: 0.0225g of graphene oxide GO is weighed and added into 30mL of deionized water, and then 1.5cm × 1.5cm carbon cloth CC is added for ultrasonic dispersion for 40min to form a uniform solution.
Step 2: 0.2578g of AR grade, 99.0% CoCl were weighed out2·6H2O, adding the mixture into the uniform solution obtained in the step 1, and uniformly stirring; subsequently, 0.1000g of AR grade, 99.0% NiCl was weighed2·6H2And adding O into the solution, and performing ultrasonic dispersion for 40min to obtain a uniform solution.
And step 3: transferring the solution obtained in the step 2 into a stainless steel autoclave with a polytetrafluoroethylene lining and a volume of 34.8mL, sealing, reacting at 180 ℃ for 12h, taking out the carbon cloth CC, washing, and drying in vacuum for 12h to obtain Co: (A), (B), (C) and aOH)2-Ni micro-nano particles piled up cauliflower-like Co (OH) grown on carbon cloth CC2-Ni/rGO/CC materials.
As can be seen from FIG. 1, the synthesized Co (OH)2The XRD pattern of the-Ni/rGO/CC composite material shows characteristic diffraction peaks at 2 theta, 19.12 degrees, 26.60 degrees, 44.49 degrees, 51.85 degrees and 76.38 degrees, wherein the diffraction peaks are Co (OH)2The (001) plane of graphite, the (003) plane of graphite and the (111) (220) (311) plane of Ni.
From FIG. 2, it can be seen that Co (OH)2Ni grows on the surface of the carbon fiber, and the particle density is large and uniform. In addition, a large amount of lamellar materials are attached to the surface of the carbon fiber and enter the gaps of the carbon fiber to play a role in connecting two adjacent carbon fibers. The material is rGO and is formed by reducing the added graphite oxide solution on the surface of carbon fiber through hydrothermal reaction.
As can be seen from FIG. 3, as can be seen from FIG. 3, Co (OH)2The growth morphology of the-Ni composite material is similar to that of cauliflower-shaped micro-spheres, and the formation of the cauliflower morphology is mainly caused by Co (OH)2The lamellar structure of (2) has lamellar Co (OH) in the middle part and around the cauliflower2. The middle part of the Chinese cabbage heart has the exception of Co (OH)2And is also doped with metallic Ni. As can be seen from the figure, the cauliflower-like microspheres were accompanied by a short tail, also consisting of Co (OH)2. By measuring the maximum Co (OH)2Ni microspheres with a diameter size of 516.4nm, a minimum diameter size of 330.0nm, and an average platelet size of 426.4nm (20 Co (OH))2Average diameter of Ni microspheres).
From FIG. 4, GCE, CC, Ni-Co (OH)2/GCE and Co (OH)2-Ni/rGO/CC electrode at 50mv s in 0.1M potassium hydroxide-1Cyclic voltammogram of scan rate (c). As can be seen from CVs, the current response of the GCE is lowest, with the CC electrode being slightly higher. Co (OH)2The current signal of-Ni/rGO/CC is higher than that of Co (OH)2-Ni/GCE. We speculate that this is because of Co (OH)2the-Ni compound is loaded on the carbon cloth to improve the electron transfer rate and improve Co (OH)2Specific surface of-Ni/GCE electrodeAnd (4) accumulating. In addition, the addition of rGO can improve Co (OH)2The conductivity of Ni, accelerating the electron transfer rate. Meanwhile, the carbon cloth can be used as a supporting material, Co (OH)2The Ni composite material is distributed in the gaps and on the surface of the carbon fiber. Thus, Co (OH) can be reduced2-agglomeration of the Ni composite.
As can be seen from FIG. 5, by continuously adding H to 0.1M potassium hydroxide at a potential of-0.67V2O2，Co(OH)2-Ni/GCE, CC and Co (OH)2Amperometric response of Ni/rGO/CC electrodes. The response time of the modified electrode is less than 3 s. Co (OH)2The response of the-Ni/rGO/CC electrode to the current signal is higher than that of Co (OH)2-Ni/GCE. This is because of CC and Co (OH)2The carbon cloth after the-Ni is compounded can improve Co (OH)2Electromigration in Ni, the sensitivity of the composite is significantly improved.

Claims (6)

1. Cauliflower-shaped Co (OH) growing on surface of carbon cloth2-a method for the production of Ni, characterized in that: the method specifically comprises the following steps;
step 1: adding 0.0075-0.0225 g of graphene oxide into 30mL of deionized water containing carbon cloth, and performing ultrasonic dispersion to obtain a uniform solution;
step 2: respectively adding 0.1454-0.2908 g of CoCl into the uniform solution obtained in the step 12·6H2O and 0.0589-0.1178 g NiCl2·6H2O, obtaining a uniform solution through ultrasonic dispersion;
and step 3: putting the solution obtained in the step 2 into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining into an autoclave, reacting for 4-12 h at 150-180 ℃ under a sealed condition, taking out carbon cloth, washing and drying to obtain Co (OH)2-Ni/rGO/CC materials.
2. The method of claim 1, wherein the cauliflower-like Co (OH) grows on the surface of the carbon cloth2The preparation method of the Ni is characterized in that the ultrasonic dispersion time in the step 1 and the ultrasonic dispersion time in the step 2 are both 20-40 min.
3. As claimed in claim 1The cauliflower-shaped Co (OH) grows on the surface of the carbon cloth2-a method for producing Ni, characterized in that the carbon cloth has a sheet-like structure of 1.5cm × 1.5 cm.
4. The method of claim 1, wherein the cauliflower-like Co (OH) grows on the surface of the carbon cloth2-Ni, characterized in that CoCl used in the step 22·6H2O and NiCl2·6H2O is AR grade, 99.0%.
5. The method of claim 1, wherein the cauliflower-like Co (OH) grows on the surface of the carbon cloth2-Ni production method, characterized in that the autoclave in step 3 is made of stainless steel and has a volume of 34.8 mL.
6. The method of claim 1, wherein the cauliflower-like Co (OH) grows on the surface of the carbon cloth2-Ni production method, characterized in that the drying means in step 3 is vacuum drying.
CN202110771538.2A 2021-07-08 2021-07-08 Cauliflower-shaped Co (OH) growing on surface of carbon cloth2Method for producing (E) -Ni Pending CN113529405A (en)

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Application publication date: 20211022