CN111403184A - Nano carbon doped MnO2Preparation method of heterojunction flexible electrode - Google Patents

Nano carbon doped MnO2Preparation method of heterojunction flexible electrode Download PDF

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Publication number
CN111403184A
CN111403184A CN202010316327.5A CN202010316327A CN111403184A CN 111403184 A CN111403184 A CN 111403184A CN 202010316327 A CN202010316327 A CN 202010316327A CN 111403184 A CN111403184 A CN 111403184A
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carbon
nano
flexible electrode
mno
heterojunction
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叶志国
吴科奇
李多生
彭新元
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Nanchang Hangkong University
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Nanchang Hangkong University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/46—Metal oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes

Abstract

The invention discloses a nano-carbon doped MnO2The preparation method of the heterojunction flexible electrode comprises the steps of taking a mixed solution of a nano-carbon dispersed aqueous solution and a manganese sulfate solution added with sodium dodecyl sulfate and a dispersant TNWDIS as an electrolyte, and depositing nano-carbon and MnO on the surface of flexible carbon cloth or carbon paper serving as an anode substrate in a cooperative constant-current electrodeposition mode2The nano carbon doped manganese dioxide heterojunction flexible electrode with the internal three-dimensional conductive network interconnection is prepared. The method has the advantages of simple and convenient process, environmental protection, short production period, high bonding strength of the deposition material on the surface of the flexible electrode, good mechanical property, good flexibility, light weight, high energy density, low internal resistance and high specific capacitance, and is suitable for the fields of wearable sensors, folding equipment, aerospace and the like.

Description

Nano carbon doped MnO2Preparation method of heterojunction flexible electrode
Technical Field
The invention relates to nano-carbon doped MnO2A preparation method of a heterojunction flexible electrode relates to a method for modifying manganese dioxide doping of a supercapacitor electrode material by using high-conductivity nano carbon, and particularly belongs to the technical field of capacitor flexible electrode materials。
Background
The super capacitor is a novel energy storage device between a battery and a traditional capacitor, has the characteristics of high specific power, large specific capacitance, high specific energy, long service life, almost no maintenance, large-current charge and discharge, environmental protection, safety, high thermal stability and the like, and has wide application prospect in the fields of new energy automobiles, portable electronic equipment, emergency energy, aerospace and the like. And as electronic equipment tends to be more and more miniaturized, portable, light-weighted and wearable, the existing traditional battery system has heavy volume and low mass-to-capacitance ratio and is difficult to meet the objective life needs, so that the development of the flexible electrode material is very important on the basis of the development of novel energy storage equipment.
MnO2Is an electrode material with wide potential window and higher theoretical capacitive performance, but has more covalent bonds and d2sp3Valence electron hybridization of (1), resulting in MnO2The whole body presents hard brittleness and low carrier mobility, which makes MnO2Is easy to be broken, has low actual utilization rate and is not beneficial to practical application. The high-conductivity nano carbon (CNT, graphene and the like) is a good conductive material and has the characteristics of excellent mechanical property, large specific surface area and light weight, so that the high-conductivity nano carbon can be used for making up MnO2Hard-brittle and low carrier mobility. Commercial flexible carbon cloth and carbon paper in the market are mature in process, can be produced in large scale, and are low in cost, light in weight, thin in thickness, excellent in flexibility and good in conductivity. Therefore, the commercial carbon cloth or carbon paper is used as a basic electrode, and the nano carbon and MnO are made by adopting a coordinated constant current electrodeposition method2The nano sheets are naturally doped in the deposition process, and the characteristics of high conductivity and high flexibility of the carbon nano tubes or graphene are utilized to prepare the wearable positive electrode of the supercapacitor, which has high volume specific capacitance, high flexibility and light weight and flexibility.
Disclosure of Invention
The invention aims to provide nano-carbon doped MnO2The preparation method of the heterojunction flexible electrode enables the CNT, graphene and other nano carbon doped manganese dioxide flexible electrodes to haveHas excellent stability, high specific capacity, high active matter quality and high flexibility.
The invention relates to nano-carbon doped MnO2The preparation method of the heterojunction flexible electrode adopts the mixed solution of nano-carbon dispersed aqueous solution and manganese sulfate solution added with sodium dodecyl sulfate and dispersant TNWDIS as electrolyte, and adopts a synergistic constant-current electrodeposition mode to deposit nano-carbon and MnO on the surface of flexible carbon cloth or carbon paper as an anode substrate2The mixed phase is used as an active substance of an electrode to prepare the nano carbon doped MnO with three-dimensional conductive network interconnection inside2A heterojunction flexible electrode; the method comprises the following specific steps:
step 1: adding the nano-carbon into a mixed solution of sodium dodecyl sulfate and a dispersant TNWDIS, performing ultrasonic dispersion for 20-40 min, and mixing the obtained nano-carbon dispersion solution with MnSO4Mixing the solutions to prepare an electrolyte, wherein the content of the nano carbon is 0.1-2.0 mg m L-1，MnSO4The concentration is 0.1-0.5 mol L-1；
Step 2: taking a titanium plate as a cathode and flexible carbon cloth or carbon paper as an anode substrate, and carrying out synergistic constant-current electrodeposition in the electrolyte obtained in the step (1), wherein the temperature of the electrolyte is controlled to be 60-80 ℃, and the stirring speed is 600-900 r min-1The electrodeposition time is 180-480 s; after the electrodeposition is finished, repeatedly cleaning the anode electrode for 3-5 min by using deionized water;
and step 3: placing the cleaned anode electrode in a constant-temperature vacuum drying oven, and drying at 60 ℃ for 12 h to obtain nano-carbon doped MnO with the whole thickness of 0.2-0.3 mm2The heterojunction flexible electrode of (1).
The current density of the cooperative constant-current electrodeposition is maintained at 1-36 mA cm-2。
The nano carbon is carbon nano tube CNT or graphene.
The nano carbon is doped with MnO2In the active substance of the heterojunction flexible electrode, the atomic percentage content of carbon element is 25% -40%.
The invention has the beneficial effects that:
1. the invention will add sodium dodecyl sulfate andthe mixed solution of nano-carbon dispersed aqueous solution and manganese sulfate solution of the dispersant TNWDIS is used as electrolyte, and nano-carbon and MnO are deposited on the surface of flexible carbon cloth or carbon paper used as an anode substrate in a cooperative constant-current electrodeposition mode2The nano carbon doped manganese dioxide heterojunction flexible electrode with three-dimensional conductive network interconnection inside is prepared. The preparation process is simple and environment-friendly, the electrolyte is free of acid and alkali addition, strong-reducibility and strong-oxidizing-property substances are not added, any constant-current power supply is adopted, the process applicability is good, the production period is short, and the equipment investment cost is low.
2. In order to ensure the flexibility and the commercial applicability of the nano-carbon doped manganese dioxide heterojunction flexible electrode, the commercial flexible carbon cloth and the carbon paper are used as matrixes, and nano-carbon and MnO are used2The cooperative deposition mode has high material bonding strength and good mechanical property of the deposit on the surface of the flexible electrode, and reduces MnO2Possibility of brittle fracture, good flexibility and light weight.
3. The invention discloses a nano carbon doped manganese dioxide heterojunction flexible electrode L i2SO4、K2SO4、Na2SO40.25A g in an aqueous electrolyte environment-1Has a scanning rate of 390F g-1High mass specific capacitance and 29F cm-3At 0.5mol L-1Na of (2)2SO4In the solution, the concentration of the solution is 15mA cm under a strong current-2The capacitor is charged and discharged for 1000 times in a circulating way, has the capacitance retention rate of 99.9 percent, has high specific capacity and stable working window, is used as a flexible electrode with high energy density, low internal resistance and high specific capacitance, and is very suitable for the fields of wearable sensors, folding equipment, aerospace and the like.
Drawings
FIG. 1 shows an embodiment of the present invention 1 Nano-carbon doped MnO2Scanning an electron microscope image of the heterojunction flexible electrode;
FIG. 2 shows an embodiment of the present invention 1 with MnO doped with nanocarbon2A transmission electron microscope image of the heterojunction flexible electrode;
FIG. 3 shows an embodiment of the present invention 1 with MnO doped with nanocarbon2A heterojunction flexible electrode cyclic voltammetry curve;
FIG. 4 shows an embodiment of the present invention 1 nanocarbon doped MnO2A heterojunction flexible electrode charge-discharge curve;
FIG. 5 shows an embodiment of the present invention 1 nanocarbon doped MnO2A cycle stability curve of the heterojunction flexible electrode charge-discharge test;
FIG. 6 shows an embodiment of the present invention 1 nanocarbon doped MnO2A heterojunction flexible electrode schematic;
wherein: 1. MnO2(ii) a 2. A carbon nanotube; 3. carbon fibers;
FIG. 7 shows an embodiment of the present invention 1 nanocarbon doped MnO2And (3) a heterojunction flexible electrode object diagram.
Detailed description of the preferred embodiment
Example 1
0.1g CNT was placed in sodium dodecyl sulfate (C)12H25SO4Na) and a commercial carbon nanotube water dispersant (product number TNWDIS, purchased from Chengdu organic chemistry Co., Ltd., China academy of sciences) for 20 min, and mixing with MnSO4Mixing the solutions to prepare a mixed solution of 250m L serving as an electrolyte, wherein the MnSO4Is 0.1 mol L-1The concentration of the carbon nano tube is 0.4 mol L-1. The titanium plate is used as a cathode, the flexible carbon paper is used as an anode substrate, and the thickness of the anode substrate is 9 mA cm-2Performing constant-current electrodeposition for 600s in electrolyte at the current density of the flexible electrode to obtain the flexible electrode, and repeatedly cleaning for 2 min by using deionized water. Placing the obtained flexible electrode in a constant-temperature vacuum drying oven, drying at 60 deg.C for 12 hr to obtain carbon nanotube doped MnO2A flexible electrode.
Doping electrodeposited CNT with MnO2The flexible electrode of the super capacitor is 0.5mol L-1Na2SO4The electrolyte of (2) is subjected to electrochemical testing. The flexible electrode is a working electrode, the platinum sheet electrode is used as an auxiliary electrode, and the saturated calomel electrode is used as a reference electrode. The scanning speed of cyclic voltammetry test is 5-100 mV/s, and the scanning speed of constant current charging and discharging test is 0.25-10.0 Ag-1At 0.25A g-1Mass specific capacitance at test speed 390F g-1Volume ofThe specific capacitance reaches 29.0F cm-3The test voltage range is 0-0.8V.
CNT doped MnO prepared in this example2The scanning electron microscope image of the flexible electrode is shown in fig. 1, the transmission electron microscope image is shown in fig. 2, the cyclic voltammetry test curve is shown in fig. 3, and the constant current charging and discharging test curve is shown in fig. 4.
The microstructure of the surface of the flexible electrode (figure 1) is observed by a scanning electron microscope, and MnO is found2The electrode mainly comprises nano sheets, wherein the nano sheets are mutually overlapped to form nano holes, so that the electrode has a large specific surface area and more electrolyte ion transport channels.
The observation of the flexible electrode by transmission electron microscopy (FIG. 2) revealed that CNT and MnO2The resulting powder is tightly bound in the field of view of the transmissive electrode, presumably MnO2The surface of the CNT is a crystal epitaxial growth structure.
The observation results of two electron microscopes show that the three-dimensional conductive network is formed by mutually lapping the nano carbon material in a three-dimensional space, so that electrons can be rapidly transmitted in the carbon material, and MnO is reduced2An electron blocking effect.
Example 2
Ultrasonic dispersing 0.1g CNT in surfactant aqueous solution for 20 min, and mixing with MnSO4Mixing the solutions to prepare a mixed solution of 250m L serving as an electrolyte, wherein the MnSO4Is 0.1 mol L-1The concentration of the carbon nano tube is 0.4 mol L-1. Respectively taking a titanium plate as a cathode and flexible carbon paper as an anode substrate at 3.0 mA cm-2Performing constant-current electrodeposition in electrolyte under the current density to obtain a flexible electrode, cleaning the obtained flexible electrode in deionized water for 3 min, placing the flexible electrode in a constant-temperature vacuum drying oven, and drying at 60 ℃ for 12 h to obtain the carbon nano tube doped MnO2A flexible electrode.
Example 3
Ultrasonically dispersing 0.25 g of graphene in a surfactant aqueous solution for 20 min, and then mixing with MnSO4Mixing the solutions to prepare a mixed solution of 250m L serving as an electrolyte, wherein the MnSO4Is 0.1 mol L-1The concentration of graphene is 1.0 mg m L-1. . Respectively taking a titanium plate as a cathode and flexible carbon paper as an anode substrate at 3.0 mA cm-2Carrying out constant-current electrodeposition in electrolyte under the current density to obtain a flexible electrode, cleaning the flexible electrode obtained by electrodeposition in deionized water for 3 min, placing the flexible electrode in a constant-temperature vacuum drying oven, and drying at 60 ℃ for 12 h to obtain the graphene doped MnO2A flexible electrode.

Claims (4)

1. Nano carbon doped MnO2The preparation method of the heterojunction flexible electrode is characterized by comprising the following steps: the method comprises the steps of taking a mixed solution of a nano-carbon dispersed aqueous solution and a manganese sulfate solution added with sodium dodecyl sulfate and a dispersant TNWDIS as an electrolyte, and depositing nano-carbon and MnO on the surface of flexible carbon cloth or carbon paper serving as an anode substrate by adopting a synergistic constant-current electrodeposition mode2The mixed phase is used as an active substance of an electrode to prepare the nano carbon doped MnO with three-dimensional conductive network interconnection inside2A heterojunction flexible electrode; the method comprises the following specific steps:
step 1: adding the nano-carbon into a mixed solution of sodium dodecyl sulfate and a dispersant TNWDIS, performing ultrasonic dispersion for 20-40 min, and mixing the obtained nano-carbon dispersion solution with MnSO4Mixing the solutions to prepare an electrolyte, wherein the content of the nano carbon is 0.1-2.0 mg m L-1，MnSO4The concentration is 0.1-0.5 mol L-1；
Step 2: taking a titanium plate as a cathode and flexible carbon cloth or carbon paper as an anode substrate, and carrying out synergistic constant-current electrodeposition in the electrolyte obtained in the step (1), wherein the temperature of the electrolyte is controlled to be 60-80 ℃, and the stirring speed is 600-900 r min-1The electrodeposition time is 180-480 s; after the electrodeposition is finished, repeatedly cleaning the anode electrode for 3-5 min by using deionized water;
and step 3: placing the cleaned anode electrode in a constant-temperature vacuum drying oven, and drying at 60 ℃ for 12 h to obtain nano-carbon doped MnO with the whole thickness of 0.2-0.3 mm2The heterojunction flexible electrode of (1).
2. The nanocarbon doped MnO of claim 12The preparation method of the heterojunction flexible electrode is characterized by comprising the following steps: the current density of the cooperative constant-current electrodeposition is maintained at 1-36 mA cm-2。
3. The nanocarbon doped MnO of claim 12The preparation method of the heterojunction flexible electrode is characterized by comprising the following steps: the nano carbon is carbon nano tube CNT or graphene.
4. The nanocarbon doped MnO of claim 12The preparation method of the heterojunction flexible electrode is characterized by comprising the following steps: the nano carbon is doped with MnO2In the active substance of the heterojunction flexible electrode, the atomic percentage content of carbon element is 25% -40%.
CN202010316327.5A 2020-04-21 2020-04-21 Nano carbon doped MnO2Preparation method of heterojunction flexible electrode Pending CN111403184A (en)

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Cited By (5)

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CN111627728A (en) * 2020-07-20 2020-09-04 南昌航空大学 MnO doped with graphene2Preparation method of carbon cloth-based flexible composite electrode
CN113104882A (en) * 2021-03-11 2021-07-13 南昌大学 Method for doping variable valence transition metal oxide by electrochemical carbon
CN113745476A (en) * 2021-08-24 2021-12-03 西安交通大学 Manganese-based zinc ion battery positive electrode material and preparation method and application thereof
CN115465924A (en) * 2022-09-19 2022-12-13 西安泰金工业电化学技术有限公司 PPy/GO/MnO 2 Nano composite electrode, preparation method and application
CN117026248A (en) * 2023-05-19 2023-11-10 重庆大学 MnO with mesoporous structure 2 Composite material/C and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111627728A (en) * 2020-07-20 2020-09-04 南昌航空大学 MnO doped with graphene2Preparation method of carbon cloth-based flexible composite electrode
CN113104882A (en) * 2021-03-11 2021-07-13 南昌大学 Method for doping variable valence transition metal oxide by electrochemical carbon
CN113745476A (en) * 2021-08-24 2021-12-03 西安交通大学 Manganese-based zinc ion battery positive electrode material and preparation method and application thereof
CN115465924A (en) * 2022-09-19 2022-12-13 西安泰金工业电化学技术有限公司 PPy/GO/MnO 2 Nano composite electrode, preparation method and application
CN115465924B (en) * 2022-09-19 2024-03-26 西安泰金新能科技股份有限公司 PPy/GO/MnO 2 Nano composite electrode, preparation method and application
CN117026248A (en) * 2023-05-19 2023-11-10 重庆大学 MnO with mesoporous structure 2 Composite material/C and preparation method thereof

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