CN115012223B - Gold chrysanthemum petal-shaped PEDOT cladding Co (OH) 2 Ni/CC material and preparation method thereof - Google Patents

Gold chrysanthemum petal-shaped PEDOT cladding Co (OH) 2 Ni/CC material and preparation method thereof Download PDF

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CN115012223B
CN115012223B CN202210401648.4A CN202210401648A CN115012223B CN 115012223 B CN115012223 B CN 115012223B CN 202210401648 A CN202210401648 A CN 202210401648A CN 115012223 B CN115012223 B CN 115012223B
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张新孟
毛子轩
张鹏程
白明玥
葛万银
伍媛婷
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a gold-wire chrysanthemum petal-shaped PEDOT coated Co (OH) 2 -Ni/CC material and method for its preparation comprising the steps of: step 1, 0.1454 to 0.2908g CoCl 2 ·6H 2 O and 0.0589-0.1178 g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A; step 2, immersing the carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining into an autoclave, reacting for 3-15 hours at 150-200 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material; step 3, 0.0865 to 0.8651gC is firstly carried out 12 H 25 SO 4 Na and 0.3192-1.5960 g LiClO 4 And 0.0426-0.2130 g PEDOT monomer are uniformly mixed to obtain a mixed solution B, and then Co (OH) 2 Placing Ni/CC material into the mixed solution B, electroplating by an electrochemical workstation to coat a layer of PEDOT on the surface of the mixed solution to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material. The material has short detection response time, high sensitivity and excellent electrochemical performance.

Description

Gold chrysanthemum petal-shaped PEDOT cladding Co (OH) 2 Ni/CC material and preparation method thereof
Technical Field
The invention relates to preparation of micro-nano materials, in particular to a gold-wire chrysanthemum petal-shaped PEDOT coated Co (OH) 2 Ni/CC material and a method for preparing the same.
Background
In recent years, transition metals and metal hydroxides have been widely studied. The transition metal has good conductivity, environmental friendliness, poisoning resistance and adjustable chemical valence and high electrochemical activity. In particular, nano-scale Co and Ni are of great interest due to their electrocatalytic activity, high electrochemically active surface area and conductivity. Transition metal hydroxide (Co (OH) 2 ，Ni(OH) 2 ) The layered structure with large spacing, large specific surface area and good electrochemical oxidation-reduction activity is easy to form in natural environment. However, the transition metal hydroxide has fewer active sites, and electrochemical properties are different from those of other materials, so that the effect of improving the active sites can be achieved by doping and modifying the transition metal hydroxide. Ni-Co (OH) 2 The complex may produce a synergistic effect, increase active sites, intra-ionic displacement, but still have small amounts of agglomeration, resulting in reduced electrocatalytic activity and conductivity. Thus, ni-Co (OH) is utilized 2 Composite construction of sensors with wear resistance, flexibility, high conductivity and durability remains a challenge.
Carbon cloth is certainly a nano material anchoring substrate which is worthy of attention because of its excellent flexibility, electrical conductivity, three-dimensional (3D) macroporous structure, good corrosion resistance to strong acid and alkaline medium and mechanical stability. Thus, CC has been used to solve the problem of nanocomposite agglomeration and to improve the electrochemical properties of the material over the past few years. Unfortunately, the conductivity of CC is still insufficient and needs to be further improved. Therefore, we have attempted to solve the above-mentioned problems. In recent years, poly 3, 4-ethylenedioxythiophene (PEDOT) has been attracting attention in the electrochemical field. PEDOT is a conductive polymer first synthesized by Bayer in germany in 1988. The PEDOT is different from the common polymer material, and has the advantages of simple molecular structure, high conductivity, good environmental stability, easy film manufacture, good transparency and the like. Due to the characteristics, the PEDOT has important application in the fields of antistatic packaging, preparation of organic photoelectric materials, electrochemical capacitors and electrochemical sensors. In the reported literature, the sensing performance and stability of the sensing material can be improved through compounding of PEDOT.
Lei Zhi et al (Chinese patent CN202010512850.5, publication No. CN111627717A, publication date 2020.09.04) disclose a carbon fiber cloth/PEDOT nanotube composite material having high specific capacitance, good rate capability and excellent cycle stability, and a method for preparing the same; the growth of the PEDOT nanotubes not only improves the conductivity and the flexibility of the carbon fiber cloth, but also improves the electrochemical performance of the carbon fiber cloth by taking the PEDOT as a pseudo-capacitance material, and the mutual interweaving among the PEDOT nanotubes is beneficial to the conduction of ions, so that the wide application of the material in the field of energy storage is widened. Li Zhenjiang et al (Chinese patent CN201610644860.8, publication No. CN106290498B, publication date 2019.11.05) disclose a catalyst based on PEDOT-rGO-Ni (OH) 2 A preparation method of an enzyme-free glucose sensor electrode of a composite nano material. Has good application prospect in the fields of clinical diagnosis, food industry analysis and the like.
The method of compounding/wrapping the sensing material with the conductive polymer like PEDOT provides possibility for exploring the electrochemical sensor with lower detection limit, wider detection range, higher sensitivity, strong selectivity, scientific research and perfect industrialization compatibility. It is anticipated that the method of encapsulating the matrix material with the conductive polymer will be a research hotspot in the field of electrochemical sensors. However, it is worth noting that there is no report in the literature that the PEDOT is used for wrapping the carbon cloth composite material so as to improve the electrochemical sensing performance of the composite material.
Disclosure of Invention
The invention aims to provide a golden chrysanthemum petal-shaped PEDOT coated Co (OH) 2 Ni/CC material and preparation method thereof, and prepared golden chrysanthemum petal-shaped Co (OH) 2 The detection response time of the Ni/CC@PEDOT material is short, the sensitivity is high, and the electrochemical performance is excellent.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
gold chrysanthemum petal-shaped PEDOT cladding Co (OH) 2 -a method for preparing a Ni/CC material comprising the steps of:
Step 1, 0.1454 to 0.2908gCoCl 2 ·6H 2 O and 0.0589-0.1178 g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing the carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining into an autoclave, reacting for 3-15 hours at 150-200 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.0865 to 0.8651g C is firstly carried out 12 H 25 SO 4 Na and 0.3192-1.5960 g LiClO 4 And 0.0426-0.2130 g PEDOT monomer are uniformly mixed to obtain a mixed solution B, and then Co (OH) 2 Placing Ni/CC material into the mixed solution B, electroplating by an electrochemical workstation to coat a layer of PEDOT on the surface of the mixed solution to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Further, the size of the carbon cloth in the step 2 is 1.5x1.5 cm.
Further, the CoCl used in step 2 2 ·6H 2 O and NiCl 2 ·6H 2 O is AR grade and the purity is 99.0%.
Further, the electric potential of the electroplating in the step 3 is 0.5-1.5V, and the time is 1-15 min.
Golden chrysanthemum petal-shaped Co (OH) 2 Ni/CC@PEDOT material, the surface of which is grown with golden chrysanthemum petal-shaped fibers.
Further, the width of the golden chrysanthemum petal-shaped fiber is 400nm.
The invention has the following beneficial effects:
1. the invention uses EDOT monomer and CoCl 2 ·6H 2 O and NiCl 2 ·6H 2 O is used as raw material, carbon Cloth (CC) is used as supporting material, deionized water is used as solvent, C 12 H 25 SO 4 Na is a surface wetting agent, liClO 4 Preparing the chrysanthemum petal-shaped Co (OH) with gold wires as an initiator through electroplating 2 The composite material growing the morphology has short detection response time, high sensitivity and long-term stabilityGood and the like.
2. In the unique three-dimensional structure formed by the morphology, the PEDOT tightly coats the composite material, so that the interface conduction mechanism of the composite material can be improved, and the transmission path of nuclear mass is increased. Firstly, the petal-shaped morphology of the golden chrysanthemum can increase the conductive channel for detecting the composite material, and improve the electron transmission efficiency. Secondly, the golden chrysanthemum petal-shaped three-dimensional nano-belt can contact more molecules to be detected, and the three-dimensional network is formed by the conductive fibers, so that the molecules of the objects to be detected can reach the surface of the carbon fibers. Meanwhile, the PEDOT with the surface coated is used as a conductive material, so that the stability of the surface structure of the composite material can be improved, and the Ni-Co (OH) on the surface of the CC can be reduced 2 The loss of the particles in the testing process increases the service life of the material. Therefore, the golden chrysanthemum petal-shaped Co (OH) prepared by the invention 2 The Ni/CC@PEDOT material can improve the adsorption performance and the mass transfer rate in the test process, further improves the electrochemical sensing performance, and has a certain reference function for constructing a high-performance sensing material design.
3. The golden chrysanthemum petal-shaped Co (OH) prepared by the invention 2 The morphology structure of the Ni/CC@PEDOT material provides a new thought for the surface morphology design of materials such as a sensing material, a battery cathode material, a catalyst, a magnetic material and the like, and the preparation method is simple, low in preparation cost and wide in application prospect.
Drawings
Fig. 1: co (OH) of the present invention 2 -Ni/CC@PEDOT vs. H 2 O 2 I-t plot for electrochemical sensing of (a).
Fig. 2: co (OH) of the present invention 2 SEM images of Ni/CC material;
fig. 3: co (OH) of the present invention 2 SEM image of Ni/cc@pedot material one;
fig. 4: co (OH) of the present invention 2 SEM image of Ni/cc@pedot material two;
fig. 5: co (OH) of the present invention 2 EDS energy spectrum of Ni/CC@PEDOT material.
Detailed Description
The following examples are given to illustrate the present invention in further detail, but are not to be construed as limiting the invention thereto.
Example 1
Step 1, 0.1454g CoCl 2 ·6H 2 O and 0.0589g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
Step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 6 hours at 150 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.0865gC is firstly added 12 H 25 SO 4 Na and 0.9576g LiClO 4 And 0.0426g PEDOT monomer are mixed uniformly to obtain a mixed solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with electric potential of 1.5V and electroplating time of 1min by electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 2
Step 1, 0.1454g CoCl 2 ·6H 2 O and 0.0736g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 4 hours at 160 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, first, 0.2595g C 12 H 25 SO 4 Na and 0.9576g LiClO 4 And 0.0852g PEDOT monomer are mixed uniformly to obtain a mixed solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.5V and an electroplating time of 5min at an electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 3
Step 1, 0.1454g CoCl 2 ·6H 2 O and 0.0882g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 5 hours at 170 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.4325gC is firstly added 12 H 25 SO 4 Na and 0.9576g LiClO 4 And 0.2130g PEDOT monomer are mixed uniformly to obtain a mixed solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.5V at 15min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 4
Step 1, 0.1454g of CoCl 2 ·6H 2 O and 0.1030g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
Step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3 hours at 180 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, firstly, 0.8651gC is added 12 H 25 SO 4 Na and 0.9576g LiClO 4 And 0.1704g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.5V at 10min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 5
Step 1, step 0.1454gCoCl 2 ·6H 2 O and 0.1178g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 7 hours at 190 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.6055gC is firstly added 12 H 25 SO 4 Na and 0.9576g LiClO 4 And 0.1278g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.5V at an electrochemical workstation for 3min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 6
Step 1, 0.1454g CoCl 2 ·6H 2 O and 0.0589g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3 hours at 200 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.0865gC is firstly added 12 H 25 SO 4 Na and 0.3192g LiClO 4 And 0.0426g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with electric potential of 0.7V and electroplating time of 1min by electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 7
Step 1, 0.1454g of CoCl 2 ·6H 2 O and 0.0736g NiCl 2 ·6H 2 O addingPutting into 30mL deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
Step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 6 hours at 160 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.2595gC is firstly added 12 H 25 SO 4 Na and 0.3192g LiClO 4 And 0.0852g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 0.7V at an electrochemical workstation for 3min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 8
Step 1, 0.1454g of CoCl 2 ·6H 2 O and 0.0882g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 6 hours at 170 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.4325gC is firstly added 12 H 25 SO 4 Na and 0.3192g LiClO 4 And 0.1278g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with electric potential of 0.7V and electroplating time of 5min by electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 9
Step 1, 0.1454g CoCl 2 ·6H 2 O and 0.1030g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 6 hours at 180 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.6055gC is firstly added 12 H 25 SO 4 Na and 0.3192g LiClO 4 And 0.1704g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 0.7V at 10min by electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 10
Step 1, 0.1454g CoCl 2 ·6H 2 O and 0.1178g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
Step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 6 hours at 190 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.7785gC is firstly added 12 H 25 SO 4 Na and 0.3192g LiClO 4 And 0.2130g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with electric potential of 0.7V and electroplating time of 15min by electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 11
Step 1, 0.1454g of CoCl 2 ·6H 2 O and 0.1178g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, firstly immersing the carbon cloth with the length of 1.5 multiplied by 1.5cm into the solution A,then the solution A immersed with the carbon cloth is filled into a polytetrafluoroethylene lining and placed in an autoclave, the carbon cloth is taken out after reaction for 6 hours at 200 ℃ under the sealing condition, and is washed and dried in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, firstly, 0.8651gC is added 12 H 25 SO 4 Na and 0.3192g LiClO 4 And 0.2130g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with electric potential of 0.7V and electroplating time of 15min by electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 12
Step 1, 0.1875g CoCl is added first 2 ·6H 2 O and 0.0589g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3 hours at 150 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.0865gC is firstly added 12 H 25 SO 4 Na and 0.6384g LiClO 4 And 0.0426g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electrochemical workstation at a plating potential of 1.0V for 1min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 13
Step 1, 0.1875g CoCl is added first 2 ·6H 2 O and 0.0736g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
Step 2, firstly immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining and placing the polytetrafluoroethylene lining into an autoclaveIn the process, the carbon cloth is taken out after the reaction for 3 hours at 160 ℃ under the sealing condition, washed and dried in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.2595gC is firstly added 12 H 25 SO 4 Na and 0.6384g LiClO 4 And 0.0852g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at an electrochemical workstation for 3min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 14
Step 1, 0.1875g CoCl is added first 2 ·6H 2 O and 0.0882g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3 hours at 170 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.4325gC is firstly added 12 H 25 SO 4 Na and 0.6384g LiClO 4 And 0.1278g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at 5min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 15
Step 1, 0.1875g CoCl 2 ·6H 2 O and 0.1030g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3 hours at 180 ℃ under a sealed condition, taking out the carbon cloth, and washingWashing and vacuum drying to obtain Co (OH) 2 -Ni/CC material;
step 3, first, 0.6055g C 12 H 25 SO 4 Na and 0.6384g LiClO 4 And 0.1704g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electrochemical workstation at a plating potential of 1.0V for 10min to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 16
Step 1, 0.1875g CoCl 2 ·6H 2 O and 0.1178g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3 hours at 190 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.7785gC is firstly added 12 H 25 SO 4 Na and 0.6384g LiClO 4 And 0.2130g PEDOT are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at 15min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 17
Step 1, 0.1875g CoCl 2 ·6H 2 O and 0.0589g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3 hours at 200 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, firstly, 0.8651gC is added 12 H 25 SO 4 Na and 0.6384g LiClO 4 And 0.1278g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at 5min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 18
Step 1, 0.1875g CoCl 2 ·6H 2 O and 0.0589g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3 hours at 150 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.0865gC is firstly added 12 H 25 SO 4 Na and 1.2768g LiClO 4 And 0.0426g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electrochemical workstation at a plating potential of 1.2V for 1min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 19
Step 1, 0.1875g CoCl 2 ·6H 2 O and 0.0736g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3 hours at 160 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.2595gC is firstly added 12 H 25 SO 4 Na and 1.2768g LiClO 4 Uniformly mixing 0.0852g PEDOT to obtain a solutionLiquid B, then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.2V at an electrochemical workstation for 3min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 20
Step 1, 0.1875g CoCl 2 ·6H 2 O and 0.0882g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3 hours at 170 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.4325gC is firstly added 12 H 25 SO 4 Na and 1.2768g LiClO 4 And 0.1278g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.2V at 5min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 21
Step 1, 0.1875g CoCl 2 ·6H 2 O and 0.1030g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3 hours at 180 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.6055gC is firstly added 12 H 25 SO 4 Na and 1.2768g LiClO 4 And 0.1704g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 The Ni/CC material is put into solution B and worked by electrochemistryElectroplating at a station with an electroplating potential of 1.2V for 10min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 22
Step 1, 0.1875g CoCl 2 ·6H 2 O and 0.1178g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3 hours at 190 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.7785gC is firstly added 12 H 25 SO 4 Na and 1.2768g LiClO 4 And 0.2130g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.2V at 15min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 23
Step 1, 0.1875g CoCl 2 ·6H 2 O and 0.0736g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3 hours at 200 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, firstly, 0.8651gC is added 12 H 25 SO 4 Na and 1.2768g LiClO 4 And 0.1704g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.2V at an electrochemical workstation for 3min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 24
Step 1, 0.2181g CoCl 2 ·6H 2 O and 0.0589g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 9 hours at 150 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.0865gC is firstly added 12 H 25 SO 4 Na and 1.5960g LiClO 4 And 0.0426g PEDOT monomer are electroplated by an electrochemical workstation at a plating potential of 0.5V for 1min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 25
Step 1, 0.2181g CoCl 2 ·6H 2 O and 0.0736g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 9 hours at 160 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, first 0.2595gC 12 H 25 SO 4 Na and 1.5960g LiClO 4 And 0.0852g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 0.5V at an electrochemical workstation for 3min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 26
Step 1, 0.2181g CoCl 2 ·6H 2 O and 0.0882g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 9 hours at 170 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.4325gC is firstly added 12 H 25 SO 4 Na and 1.5960g LiClO 4 And 0.1278g PEDOT monomer to give solution B, and then mixing Co (OH) 2 Placing Ni/CC material into solution B, electroplating with electric potential of 0.5V and electroplating time of 5min by electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 27
Step 1, 0.2181g CoCl 2 ·6H 2 O and 0.1030g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 9 hours at 180 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, first, 0.6055g C 12 H 25 SO 4 Na and 1.5960g LiClO 4 And 0.1704g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 0.5V at 10min by electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 28
Step 1, 0.2181g CoCl 2 ·6H 2 O and 0.1178gNiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 9 hours at 190 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.7785gC is firstly added 12 H 25 SO 4 Na and 1.5960g LiClO 4 And 0.2130g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with electric potential of 0.5V and electroplating time of 15min by electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 29
Step 1, 0.2181g CoCl 2 ·6H 2 O and 0.1030g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 9 hours at 200 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, firstly, 0.8651gC is added 12 H 25 SO 4 Na and 1.5960g LiClO 4 And 0.2130g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with electric potential of 0.5V and electroplating time of 15min by electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 30
Step 1, 0.2181g CoCl 2 ·6H 2 O and 0.0589g NiCl 2 ·6H 2 Adding O into 30mL deionized water, and performing ultrasonic dispersionUniformly obtaining a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 9 hours at 150 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.0865gC is firstly added 12 H 25 SO 4 Na and 0.3192g LiClO 4 And 0.0426g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electrochemical workstation at a plating potential of 1.0V for 1min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 31
Step 1, 0.2181g CoCl 2 ·6H 2 O and 0.0736g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 9 hours at 160 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
Step 3, 0.2595gC is firstly added 12 H 25 SO 4 Na and 0.3192g LiClO 4 And 0.0852g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at an electrochemical workstation for 3min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 32
Step 1, 0.2181g CoCl 2 ·6H 2 O and 0.0882g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, firstly, 1.5X1 is carried out.Immersing 5cm carbon cloth in the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 9 hours at 170 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.4325gC is firstly added 12 H 25 SO 4 Na and 0.3192g LiClO 4 And 0.1278g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at 5min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 33
Step 1, 0.2181g CoCl 2 ·6H 2 O and 0.1030g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 9 hours at 180 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.6055gC is firstly added 12 H 25 SO 4 Na and 0.3192g LiClO 4 And 0.1704g PEDOT monomer to give solution B, and then mixing Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at 10min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 34
Step 1, 0.2181g CoCl 2 ·6H 2 O and 0.1178g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, firstly immersing 1.5 multiplied by 1.5cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining andplacing the mixture in an autoclave, reacting for 9 hours at 190 ℃ under a sealed condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, first, 0.7785g C 12 H 25 SO 4 Na and 0.3192g LiClO 4 And 0.2130g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at 15min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 35
Step 1, 0.2181g CoCl 2 ·6H 2 O and 0.1030g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 9 hours at 200 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, firstly, 0.8651g C 12 H 25 SO 4 Na and 0.3192g LiClO 4 And 0.1278g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at an electrochemical workstation for 3min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 36
Step 1, 0.2544g CoCl 2 ·6H 2 O and 0.0589g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 12 hours at 150 ℃ under a sealed condition, and taking out the carbonCloth, washing, vacuum drying to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.0865gC is firstly added 12 H 25 SO 4 Na and 0.6384g LiClO 4 And 0.0426g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electrochemical workstation at a plating potential of 1.0V for 1min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 37
Step 1, 0.2544g CoCl 2 ·6H 2 O and 0.0736g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 12 hours at 160 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.2595gC is firstly added 12 H 25 SO 4 Na and 0.6384g LiClO 4 And 0.0852g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at an electrochemical workstation for 3min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 38
Step 1, 0.2544g CoCl 2 ·6H 2 O and 0.0882g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 12 hours at 170 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.4325gC is firstly added 12 H 25 SO 4 Na and 0.6384g LiClO 4 And 0.1278g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at 5min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 39
Step 1, 0.2544g CoCl 2 ·6H 2 O and 0.1030g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 12 hours at 180 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.6055gC is firstly added 12 H 25 SO 4 Na and 0.6384g LiClO 4 And 0.1704g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at 10min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 40
Step 1, 0.2544g CoCl 2 ·6H 2 O and 0.1178g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 12 hours at 190 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.7785gC is firstly added 12 H 25 SO 4 Na and 0.6384g LiClO 4 And 0.2130g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at 15min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 41
Step 1, 0.2544g CoCl 2 ·6H 2 O and 0.0882g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 12 hours at 200 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, firstly, 0.865gC is added 12 H 25 SO 4 Na and 0.6384g LiClO 4 And 0.2130g PEDOT monomer to give solution B, and then mixing Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 1.0V at 10min at electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 42
Step 1, 0.2908g CoCl 2 ·6H 2 O and 0.0589g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 15 hours at 150 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.0865gC is firstly added 12 H 25 SO 4 Na and 0.3192g LiClO 4 0.0426g PEDOT monomer is uniformly mixed to obtainSolution B, then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with electric potential of 0.5V and electroplating time of 1min by electrochemical workstation to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 43
Step 1, 0.2908g CoCl 2 ·6H 2 O and 0.0736g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 15 hours at 160 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.2595gC is firstly added 12 H 25 SO 4 Na and 0.6384g LiClO 4 And 0.0852g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B, electroplating with an electroplating potential of 0.7V at an electrochemical workstation for 3min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 44
Step 1, 0.2908g CoCl 2 ·6H 2 O and 0.0882g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 15 hours at 170 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, 0.4325gC is firstly added 12 H 25 SO 4 Na and 0.9576g LiClO 4 And 0.1278g PEDOT monomer are mixed uniformly to obtain solution B, and then Co (OH) 2 Placing Ni/CC material into solution B by electrochemical methodElectroplating in a workstation with electroplating potential of 1.0V and electroplating time of 5min to obtain Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Example 45
Step 1, 0.2908g CoCl 2 ·6H 2 O and 0.1030g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing 1.5X1.5 cm carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 15 hours at 180 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, first 0.6055gC 12 H 25 SO 4 Na and 1.2768g LiClO 4 And 0.1704g PEDOT monomer are uniformly mixed to obtain a solution B, and electroplating is carried out by an electrochemical workstation, wherein the electroplating potential is 1.2V, and the electroplating time is 10min, so that Co (OH) 2 Coating a layer of PEDOT on the surface of the Ni/CC material to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material.
Referring to FIG. 1, H is added continuously to 0.1M potassium hydroxide at a potential of-0.67V 2 O 2 ，CC、Co(OH) 2 Ni/CC and Co (OH) 2 Amperometric response curve of the Ni/cc@pedot electrode. As can be seen from the graph, the response time of the modified electrode is less than 3s, and Co (OH) 2 The response of the Ni/CC@PEDOT electrode to the current signal is higher than Co (OH) 2 Ni/CC, since PEDOT is uniformly coated on Co (OH) 2 The Ni/CC surface improves the electrical mobility of the composite material, so that the sensitivity of the composite material is obviously improved.
Referring to FIG. 2, co (OH) is prepared in the examples 2 SEM of Ni/CC electrode material, from which it can be seen that Co (OH) is present in the sample 2 The Ni nanospheres are uniformly distributed on the surface of the carbon fiber, the diameter of the Ni nanospheres is about 300-500 nm, the shape and the size of the nanosphere particles are the same, and no obvious agglomeration phenomenon exists.
Referring to FIG. 3, co (OH) prepared in example 1 2 -Ni/SEM image of CC@PEDOT material, it can be seen that PEDOT is uniformly coated on Co (OH) 2 Ni/CC surface, and fine golden chrysanthemum petal-shaped fibers uniformly grown on the surface, co (OH) cannot be visually seen through SEM image 2 Morphology of Ni nanosphere particles, it can be seen that PEDOT completely covers Co (OH) 2 -Ni/CC。
Referring to fig. 4, which is a partial enlarged view of fig. 3, it can be seen that PEDOT is not only wrapped on the surface of carbon fiber, but also gold chrysanthemum petal-shaped fibers are grown on the surface of the composite layer, the width of the fibers is about 400nm, and the swing of the fibers can be clearly seen under a scanning electron microscope.
Referring to FIG. 5, co (OH) 2 EDS energy spectrum of golden chrysanthemum petal-shaped nano-belt structure of Ni/CC@PEDOT composite material. Through EDS element analysis of the composite material, the chrysanthemum petal-shaped nano-belt part of the golden thread contains C, O, S, co elements, ni elements and the like. Wherein the S element is contained in a large amount, and the S element is derived from the S element in PEDOT.

Claims (5)

1. Gold chrysanthemum petal-shaped PEDOT cladding Co (OH) 2 -a method for preparing a Ni/CC material, characterized in that it comprises the following steps:
step 1, 0.1454 to 0.2908g CoCl 2 ·6H 2 O and 0.0589-0.1178 g NiCl 2 ·6H 2 Adding O into 30mL of deionized water, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 2, immersing the carbon cloth into the solution A, then filling the solution A immersed with the carbon cloth into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an autoclave, reacting for 3-15 hours at the temperature of 150-200 ℃ under a sealing condition, taking out the carbon cloth, washing, and drying in vacuum to obtain Co (OH) 2 -Ni/CC material;
step 3, firstly, 0.0865 to 0.8651gC 12 H 25 SO 4 Na and 0.3192-1.5960 g LiClO 4 And 0.0426-0.2130 g PEDOT monomer are uniformly mixed to obtain a mixed solution B, and then Co (OH) 2 Placing Ni/CC material into the mixed solution B, electroplating by an electrochemical workstation to coat a layer of PEDOT on the surface of the mixed solution to obtain golden chrysanthemum petal-shaped Co (OH) 2 -Ni/cc@pedot material;
the electric potential of the electroplating is 0.5-1.5V, and the time is 1-15 min.
2. The golden chrysanthemum petal-shaped PEDOT coated Co (OH) of claim 1 2 A process for the preparation of Ni/CC material, characterized in that the CoCl used in step 1 2 ·6H 2 O and NiCl 2 ·6H 2 O is AR grade and the purity is 99.0%.
3. The golden chrysanthemum petal-shaped PEDOT coated Co (OH) of claim 1 2 -a method for preparing a Ni/CC material, characterized in that the carbon cloth in step 2 has a size of 1.5 x 1.5cm.
4. A golden chrysanthemum petal-shaped Co (OH) prepared by the method of claim 1 2 -Ni/cc@pedot material characterized by Co (OH) 2 And the surface of the Ni/CC@PEDOT material is grown with golden chrysanthemum petal-shaped fibers.
5. A golden chrysanthemum petal-shaped Co (OH) according to claim 4 2 -Ni/cc@pedot material, characterized in that the gold chrysanthemum petal-shaped fibers have a width of 400nm.
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