CN110415989A - A kind of method that electrodeposition process prepares the super capacitor material of cobaltous selenide - Google Patents

A kind of method that electrodeposition process prepares the super capacitor material of cobaltous selenide Download PDF

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Publication number
CN110415989A
CN110415989A CN201910724158.6A CN201910724158A CN110415989A CN 110415989 A CN110415989 A CN 110415989A CN 201910724158 A CN201910724158 A CN 201910724158A CN 110415989 A CN110415989 A CN 110415989A
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China
Prior art keywords
graphene oxide
electrode
solution
cobaltous selenide
super capacitor
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CN201910724158.6A
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张明义
李璐
周雪娇
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Harbin Normal University
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Harbin Normal 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
    • H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

Abstract

The invention discloses a kind of methods that electrodeposition process prepares the super capacitor material of cobaltous selenide, comprising the following steps: step A, prepares graphene oxide foam nickel electrode；Step B, precursor solution is configured；Step C, with electrochemical deposition method by cobaltous selenide depositing nano-materials to graphene oxide foam nickel electrode surface；Step D, the super capacitor material to get cobaltous selenide is dried after after the reaction was completed, product being used respectively deionized water, ethyl alcohol rinse.When the cobaltous selenide nano material that this method obtains is used as the electrode material of supercapacitor, there is biggish promotion in specific capacitance, charge-discharge performance, is tested under the conditions of constant current density is 1A/g, specific capacitance can reach 1750F/g or more；And its charge-discharge performance is good, in the case where current density is 20A/g, by 5000 charge and discharge cycles, is still able to maintain 87% or more specific capacitance value.

Description

A kind of method that electrodeposition process prepares the super capacitor material of cobaltous selenide
Technical field
The present invention relates to the supercapacitors that technical field of nano material more particularly to a kind of electrodeposition process prepare cobaltous selenide The method of material.
Background technique
Selenides is a kind of potential super capacitor material, and people are used for electrode of super capacitor material to selenides at present The research and development of material is also very rare, is rarely reported.Cobaltous selenide all has advantage, high activity in capacitance and electric conductivity Surface be also beneficial to being obviously improved for chemical property, thus cobaltous selenide will be a kind of super capacitor with excellent properties Device electrode material will cause the extensive concern of people.Currently, researchers tentatively synthesize base by several limited modes In the nanometer sheet of cobaltous selenide and the nanostructure of nanotube, the specific capacitance for characterizing capacitance size is about 200F/g-300F/g. In the case where electrode material is formed and determined, reasonable structure design can effectively improve the chemical property of electrode, such as The contact area of electrode active material and electrolyte can be increased by obtaining higher specific surface area, and specific membrane structure is also advantageous In the electro-chemical activity for promoting material, to effectively improve the utilization rate of active material, many electricity such as specific capacitance are then improved Chemical property index.In addition, seeking low cost, the electrode material preparation method of methods simplification, the production for supercapacitor Industry is also very necessary.
Chinese invention patent CN106024405A discloses a kind of no template electric-sedimentation method and prepares cobaltous selenide supercapacitor The method of material, the material are nanometer flower structure.The nano-electrode material has excellent electrochemistry high rate performance and circulation steady Qualitative energy, has expanded the preparation method and application field of electrochemical capacitor material.
But the material specific capacitance, in terms of still have biggish room for promotion, therefore the present invention mentions A kind of method that electrodeposition process prepares the super capacitor material of cobaltous selenide is gone out.
Summary of the invention
Technical problems based on background technology, the invention proposes the super electricity that a kind of electrodeposition process prepares cobaltous selenide The method of container material.
Technical scheme is as follows:
A kind of method that electrodeposition process prepares the super capacitor material of cobaltous selenide, comprising the following steps:
A, cyclic voltammetry will be utilized in graphene oxide dispersion as working electrode after nickel foam cleaning, drying Graphene oxide foam nickel electrode is made after dry in scanning；
B, Na is configured2SeO3Solution and Co (CH3COO)2Solution adds CH3COOLi solution is uniformly mixed, and obtains forerunner Liquid solution；
C, the graphene oxide foam nickel electrode in step A is immersed in precursor solution, with electrochemical deposition method by selenium Change cobalt depositing nano-materials to graphene oxide foam nickel electrode surface, and during this, electrochemical deposition working electrode is institute State graphene oxide foam nickel electrode；
D, after the reaction was completed, product is used respectively deionized water, ethyl alcohol rinse after dry to get.
Preferably, in the step A, the cleaning is successively to use deionized water, dilute hydrochloric acid, dehydrated alcohol, third Ketone is cleaned by ultrasonic respectively；Each 25~50min of scavenging period, the mass fraction of the dilute hydrochloric acid are 1~5%.
Preferably, in the step A, in the graphene oxide dispersion mass concentration of graphene oxide be 2~ 4g/L。
Preferably, in the step A, the condition of the cyclic voltammetry be using saturated calomel electrode as reference electrode, Platinized platinum is to electrode, and voltage is -1.4~0.6V, and sweeping speed is to scan under 25~80mV/s.
Preferably, in the step B, Na2SeO3The concentration of solution is 0.005~0.02mol/L, Co (CH3COO)2It is molten Liquid concentration is 0.03~0.05mol/L, CH3The concentration of COOLi solution is 0.05~0.2mol/L.
Preferably, in the step C, the technological parameter of electrochemical deposition are as follows: depositing temperature is 45~75 DEG C, and voltage is Voltage is -1.2~0.35V, and sweeping speed is to scan under 40~60mV/s, and cycle-index is 10~20 times.
The invention has the beneficial effects that: the present invention is heavy without template electric disclosed in Chinese invention patent CN106024405A On the basis of area method prepares cobaltous selenide super capacitor material, by the way that working electrode is adjusted to graphene oxide nickel foam electricity Pole is still nano flower shape although the structure for obtaining cobaltous selenide nano material has no big variation；But obtained cobaltous selenide is received When rice material is used as the electrode material of supercapacitor, there is biggish promotion in specific capacitance, charge-discharge performance, in constant current Density is tested under the conditions of being 1A/g, and specific capacitance can reach 1750F/g or more；And its charge-discharge performance is good, in electric current Density is, by 5000 charge and discharge cycles, to be still able to maintain 87% or more specific capacitance value under 20A/g.
Specific embodiment
Embodiment 1:
A kind of method that electrodeposition process prepares the super capacitor material of cobaltous selenide, comprising the following steps:
A, cyclic voltammetry will be utilized in graphene oxide dispersion as working electrode after nickel foam cleaning, drying Graphene oxide foam nickel electrode is made after dry in scanning；The cleaning is successively using deionized water, dilute hydrochloric acid, anhydrous Ethyl alcohol, acetone are cleaned by ultrasonic respectively；Each 35min of scavenging period, the mass fraction of the dilute hydrochloric acid are 3.5%；The drying For 85 DEG C of dry 75min；The mass concentration of graphene oxide is 2.5g/L in the graphene oxide dispersion；The circulation volt The condition of peace method is using saturated calomel electrode as reference electrode, and platinized platinum is to electrode, and voltage is -1.4~0.6V, and sweeping speed is It is scanned under 55mV/s；
B, Na is configured2SeO3Solution and Co (CH3COO)2Solution adds CH3COOLi solution is uniformly mixed, and obtains forerunner Liquid solution；Na2SeO3The concentration of solution is 0.015mol/L, Co (CH3COO)2Solution concentration is 0.04mol/L, CH3COOLi is molten The concentration of liquid is 0.15mol/L；
C, the graphene oxide foam nickel electrode in step A is immersed in precursor solution, with electrochemical deposition method by selenium Change cobalt depositing nano-materials to graphene oxide foam nickel electrode surface, and during this, electrochemical deposition working electrode is institute State graphene oxide foam nickel electrode；The technological parameter of electrochemical deposition are as follows: depositing temperature is 60 DEG C, and voltage is that voltage is -1.2 ~0.35V, sweeping speed is to scan under 45mV/s, and cycle-index is 18 times；
D, after the reaction was completed, product is used respectively deionized water, ethyl alcohol rinse after 60 DEG C of dry 6h to get.
Embodiment 2:
A kind of method that electrodeposition process prepares the super capacitor material of cobaltous selenide, comprising the following steps:
A, cyclic voltammetry will be utilized in graphene oxide dispersion as working electrode after nickel foam cleaning, drying Graphene oxide foam nickel electrode is made after dry in scanning；The cleaning is successively using deionized water, dilute hydrochloric acid, anhydrous Ethyl alcohol, acetone are cleaned by ultrasonic respectively；Each 50min of scavenging period, the mass fraction of the dilute hydrochloric acid are 1%；The drying is 100 DEG C of dry 60min；The mass concentration of graphene oxide is 4g/L in the graphene oxide dispersion；The cyclic voltammetric The condition of method is using saturated calomel electrode as reference electrode, and platinized platinum is to electrode, and voltage is -1.4~0.6V, and sweeping speed is 25mV/s Lower scanning；
B, Na is configured2SeO3Solution and Co (CH3COO)2Solution adds CH3COOLi solution is uniformly mixed, and obtains forerunner Liquid solution；Na2SeO3The concentration of solution is 0.02mol/L, Co (CH3COO)2Solution concentration is 0.03mol/L, CH3COOLi solution Concentration be 0.2mol/L；
C, the graphene oxide foam nickel electrode in step A is immersed in precursor solution, with electrochemical deposition method by selenium Change cobalt depositing nano-materials to graphene oxide foam nickel electrode surface, and during this, electrochemical deposition working electrode is institute State graphene oxide foam nickel electrode；The technological parameter of electrochemical deposition are as follows: depositing temperature is 45 DEG C, and voltage is that voltage is -1.2 ~0.35V, sweeping speed is to scan under 60mV/s, and cycle-index is 10 times；
D, after the reaction was completed, product is used respectively deionized water, ethyl alcohol rinse after 60 DEG C of dry 8h to get.
Embodiment 3:
A kind of method that electrodeposition process prepares the super capacitor material of cobaltous selenide, comprising the following steps:
A, cyclic voltammetry will be utilized in graphene oxide dispersion as working electrode after nickel foam cleaning, drying Graphene oxide foam nickel electrode is made after dry in scanning；The cleaning is successively using deionized water, dilute hydrochloric acid, anhydrous Ethyl alcohol, acetone are cleaned by ultrasonic respectively；Each 25min of scavenging period, the mass fraction of the dilute hydrochloric acid are 5%；The drying is 80 DEG C of dry 80min；The mass concentration of graphene oxide is 2g/L in the graphene oxide dispersion；The cyclic voltammetry Condition be using saturated calomel electrode as reference electrode, platinized platinum is to electrode, and voltage is -1.4~0.6V, and sweeping speed is under 80mV/s Scanning；
B, Na is configured2SeO3Solution and Co (CH3COO)2Solution adds CH3COOLi solution is uniformly mixed, and obtains forerunner Liquid solution；Na2SeO3The concentration of solution is 0.005mol/L, Co (CH3COO)2Solution concentration is 0.05mol/L, CH3COOLi is molten The concentration of liquid is 0.05mol/L；
C, the graphene oxide foam nickel electrode in step A is immersed in precursor solution, with electrochemical deposition method by selenium Change cobalt depositing nano-materials to graphene oxide foam nickel electrode surface, and during this, electrochemical deposition working electrode is institute State graphene oxide foam nickel electrode；The technological parameter of electrochemical deposition are as follows: depositing temperature is 75 DEG C, and voltage is that voltage is -1.2 ~0.35V, sweeping speed is to scan under 40mV/s, and cycle-index is 20 times；
D, after the reaction was completed, product is used respectively deionized water, ethyl alcohol rinse after 60 DEG C of dry 5h to get.
Comparative example 1
Graphene oxide foam nickel electrode in embodiment 1 is replaced with into the grapheme foam nickel electrode after reduction, remaining Preparation method is constant.
Comparative example 2
Graphene oxide foam nickel electrode in embodiment 1 is replaced with into foam nickel screen, remaining preparation method is constant.
By the super capacitor material of the embodiment 1-3 and comparative example 1-2 cobaltous selenide prepared carries out specific capacitance, charge and discharge follow Ring performance detection obtains following detection data (each embodiment or comparative example detect 3 data, are averaged), specific data It is shown in Table 1.
Wherein, 1A/g specific capacitance value are as follows: the specific capacitance value tested under the conditions of constant current density is 1A/g；
20A/g specific capacitance value are as follows: in the case where current density is 20A/g, after 5000 charge and discharge cycles, detect again Specific capacitance value.
Table 1: the specific capacitance and charge and discharge of the super capacitor material of the cobaltous selenide of embodiment 1-3 and comparative example 1-2 preparation Cycle performance detection data；
Embodiment 1 Embodiment 2 Embodiment 3 Comparative example 1 Comparative example 2
1A/g specific capacitance value 1806 1758 1773 1135 896
20A/g specific capacitance value 1593 1547 1553 1003 739
By the above test data it is recognised that the super capacitor material of cobaltous selenide prepared by the present invention, not only specific capacitance Value is obviously improved, and charge-discharge performance also has more apparent improvement.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (7)

1. a kind of method that electrodeposition process prepares the super capacitor material of cobaltous selenide, which comprises the following steps:
A, it will be swept in graphene oxide dispersion using cyclic voltammetry after nickel foam cleaning, drying as working electrode It retouches, graphene oxide foam nickel electrode is made after dry；
B, Na is configured2SeO3Solution and Co (CH3COO)2Solution adds CH3COOLi solution is uniformly mixed, and it is molten to obtain presoma Liquid；
C, the graphene oxide foam nickel electrode in step A is immersed in precursor solution, with electrochemical deposition method by cobaltous selenide For depositing nano-materials to graphene oxide foam nickel electrode surface, and during this, electrochemical deposition working electrode is the oxygen Graphite alkene foam nickel electrode；
D, after the reaction was completed, product is used respectively deionized water, ethyl alcohol rinse after dry to get.
2. the method that electrodeposition process as described in claim 1 prepares the super capacitor material of cobaltous selenide, which is characterized in that institute In the step A stated, the cleaning is successively to be cleaned by ultrasonic respectively using deionized water, dilute hydrochloric acid, dehydrated alcohol, acetone；Clearly Time each 25~50min is washed, the mass fraction of the dilute hydrochloric acid is 1~5%.
3. the method that electrodeposition process as described in claim 1 prepares the super capacitor material of cobaltous selenide, which is characterized in that institute In the step A stated, the mass concentration of graphene oxide is 2~4g/L in the graphene oxide dispersion.
4. the method that electrodeposition process as described in claim 1 prepares the super capacitor material of cobaltous selenide, which is characterized in that institute In the step A stated, the condition of the cyclic voltammetry is using saturated calomel electrode as reference electrode, and platinized platinum is to electrode, voltage For -1.4~0.6V, sweeping speed is to scan under 25~80mV/s.
5. the method that electrodeposition process as described in claim 1 prepares the super capacitor material of cobaltous selenide, which is characterized in that institute In the step B stated, Na2SeO3The concentration of solution is 0.005~0.02mol/L, Co (CH3COO)2Solution concentration be 0.03~ 0.05mol/L, CH3The concentration of COOLi solution is 0.05~0.2mol/L.
6. the method that electrodeposition process as described in claim 1 prepares the super capacitor material of cobaltous selenide, which is characterized in that institute In the step C stated, the technological parameter of electrochemical deposition are as follows: depositing temperature be 45~75 DEG C, voltage be voltage be -1.2~ 0.35V, sweeping speed is to scan under 40~60mV/s, and cycle-index is 10~20 times.
7. the method that electrodeposition process as described in claim 1 prepares the super capacitor material of cobaltous selenide, which is characterized in that packet Include following steps:
A, it will be swept in graphene oxide dispersion using cyclic voltammetry after nickel foam cleaning, drying as working electrode It retouches, graphene oxide foam nickel electrode is made after dry；The cleaning is successively to use deionized water, dilute hydrochloric acid, anhydrous second Alcohol, acetone are cleaned by ultrasonic respectively；Each 35min of scavenging period, the mass fraction of the dilute hydrochloric acid are 3.5%；The drying is 85 DEG C of dry 75min；The mass concentration of graphene oxide is 2.5g/L in the graphene oxide dispersion；The cyclic voltammetric The condition of method is using saturated calomel electrode as reference electrode, and platinized platinum is to electrode, and voltage is -1.4~0.6V, and sweeping speed is 55mV/s Lower scanning；
B, Na is configured2SeO3Solution and Co (CH3COO)2Solution adds CH3COOLi solution is uniformly mixed, and it is molten to obtain presoma Liquid；Na2SeO3The concentration of solution is 0.015mol/L, Co (CH3COO)2Solution concentration is 0.04mol/L, CH3COOLi solution Concentration is 0.15mol/L；
C, the graphene oxide foam nickel electrode in step A is immersed in precursor solution, with electrochemical deposition method by cobaltous selenide For depositing nano-materials to graphene oxide foam nickel electrode surface, and during this, electrochemical deposition working electrode is the oxygen Graphite alkene foam nickel electrode；The technological parameter of electrochemical deposition are as follows: depositing temperature be 60 DEG C, voltage be voltage be -1.2~ 0.35V, sweeping speed is to scan under 45mV/s, and cycle-index is 18 times；
D, after the reaction was completed, product is used respectively deionized water, ethyl alcohol rinse after 60 DEG C of dry 6h to get.
CN201910724158.6A 2019-08-07 2019-08-07 A kind of method that electrodeposition process prepares the super capacitor material of cobaltous selenide Pending CN110415989A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112018361A (en) * 2020-08-31 2020-12-01 华中科技大学 Carbon cloth loaded carbon coated cobalt selenide nanosheet battery cathode material and preparation thereof
CN113675007A (en) * 2021-08-13 2021-11-19 益阳市安兴电子有限公司 Electrode with good cycle performance, preparation method thereof and super capacitor

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CN106128790A (en) * 2016-09-08 2016-11-16 上海理工大学 A kind of preparation method of Graphene electrode material for super capacitor
CN107967998A (en) * 2017-11-22 2018-04-27 东北大学 The preparation method of grapheme foam nickel electrode

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Publication number Priority date Publication date Assignee Title
CN106024405A (en) * 2016-05-31 2016-10-12 浙江大学 Method for preparing cobalt selenide super-capacitor material by non-template electrodeposition method
CN106128790A (en) * 2016-09-08 2016-11-16 上海理工大学 A kind of preparation method of Graphene electrode material for super capacitor
CN107967998A (en) * 2017-11-22 2018-04-27 东北大学 The preparation method of grapheme foam nickel electrode

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112018361A (en) * 2020-08-31 2020-12-01 华中科技大学 Carbon cloth loaded carbon coated cobalt selenide nanosheet battery cathode material and preparation thereof
CN113675007A (en) * 2021-08-13 2021-11-19 益阳市安兴电子有限公司 Electrode with good cycle performance, preparation method thereof and super capacitor

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Application publication date: 20191105