CN103903880A - Method for in-situ preparation of graphene supercapacitor electrode based on nickel foam - Google Patents
Method for in-situ preparation of graphene supercapacitor electrode based on nickel foam Download PDFInfo
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- CN103903880A CN103903880A CN201410075654.0A CN201410075654A CN103903880A CN 103903880 A CN103903880 A CN 103903880A CN 201410075654 A CN201410075654 A CN 201410075654A CN 103903880 A CN103903880 A CN 103903880A
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Abstract
The invention discloses a method for in-situ preparation of a graphene supercapacitor electrode based on nickel foam. The method includes the steps that graphite oxide slurry is prepared with the Hummers method, and processed nickel foam is steeped into the graphite oxide slurry, so that the graphite oxide slurry enters a three-dimensional hole-shaped structure of the nickel foam; the graphite oxide slurry is directly put into a low-temperature vacuum environment after being dried, pyrolysis reduction is performed on graphite oxide, and therefore the graphene supercapacitor electrode obtained through in-situ preparation and based on the nickel foam is obtained. According to the method, the contact area between the functional graphene and the nickel foam is enlarged, the contact resistance between electrode materials and a current collector is reduced, and meanwhile the process of mixing and coating active substances, binders and conductive agents in a traditional electrode preparation technology is omitted. The supercapacitor electrode has the high specific capacity and the good circulation performance, the preparation method is fast and convenient to conduct, and the method can be applied to large-scale production of the supercapacitor electrode.
Description
Technical field
The present invention relates to a kind of method of preparing Graphene electrode of super capacitor based on nickel foam original position, belong to new forms of energy application.
Background technology
Along with developing rapidly of portable electronic consumer goods MP3, smart mobile phone, notebook computer, electric automobile, hybrid vehicle market, people are environmentally friendly, and high performance energy storage device has had increasing demand.Ultracapacitor, claims again electrochemical capacitor, double electric layer capacitor, has extraordinary energy storage capacity, and the cycle life of overlength and fast charging and discharging capabilities, more and more expressed great expectations by people.Ultracapacitor, operating temperature range is wide, and environmental friendliness is pollution-free, conventionally has very high power density and than electric capacity, the cycle life of overlength and hold facility have instantaneous large charging and discharging capabilities and high efficiency for charge-discharge simultaneously.
Ultracapacitor is by electrode, barrier film, and electrolyte forms.Wherein the electrode material of ultracapacitor is the key factor of restriction ultracapacitor development, directly affects the amount of capacity of ultracapacitor, power density, energy density, cycle life, temperature characterisitic, security feature etc.Commercial electrode material for super capacitor comprises carbon-based material, metal oxide and polymeric material at present.Wherein carbon-based material is most widely used electrode material, mainly comprises active carbon, carbon nano-tube, and graphite, porous carbon, carbon fiber, and be subject to recently the Graphene of everybody extensive concern.Graphene (Graphene) is by the tightly packed a kind of New Type of Carbon material forming of monolayer carbon atom, there is the cellular crystal structure of hexagonal, it is the basis that forms other different carbonaceous materials, it can be rolled into the fullerene of zero dimension, be rolled into two-dimentional carbon nano-tube, be layering into three-dimensional graphite.Single-layer graphene at room temperature has high heat conductance, shows quantum hall effect, high electron mobility etc. under room temperature; Graphene, due to its unique two-dimensional structure, has the specific area of super large simultaneously, and the theoretical specific area of single-layer graphene reaches 2630m
2/ g, therefore Graphene is desirable electrode material for super capacitor.
The preparation method of Graphene has developed into the multiple preparation method who meets different application needs from initial tear tape method at present, comprise epitaxial growth method, chemical vapour deposition technique, chemistry redox method, dilatometry etc., wherein chemistry redox method and dilatometry are applicable to the functional form Graphene that electrode material for super capacitor large-scale production, the especially dilatometry of Graphene prepare and have the needed high-specific surface area of electrode material and unique central hole structure.At present, traditional preparation method based on Graphene electrode of super capacitor mixes with binding agent, conductive agent the functional form Graphene of preparing by said method according to certain ratio, then add solvent to make slurry, be finally coated in again on the collectors such as nickel foam.Conventionally binding agent is insulator, causes the internal resistance of electrode material to increase, and stops the fast transport of electronics simultaneously, and batch mixing process tends to cause the structure of functional form Graphene to be destroyed, and available effective ratio area reduces.The Graphene ultracapacitor specific volume value that traditional handicraft is prepared not is very desirable, exist actual specific capacitance less, can only under low range, discharge and recharge and the problem such as cycle life is shorter, the performance such as ratio electric capacity, cyclical stability therefore how improving based on Graphene ultracapacitor becomes the task of top priority.
Summary of the invention
The object of this invention is to provide a kind of method of preparing Graphene electrode of super capacitor based on nickel foam original position, nickel foam is as the collector of ultracapacitor, simultaneously also as the support frame of functional form graphene three-dimensional structure., then nickel foam is immersed in graphite oxide slurry for graphite oxide slurry by Hummers legal system, graphite oxide slurry is entered in the 3 D stereo cavernous structure of nickel foam.Directly put into after drying and under cryogenic vacuum environment, make graphite oxide pyrolysis reduction, the graphite oxide after pyrolysis reduction is attached on the skeleton of nickel foam and forms 3 D stereo network configuration.Take full advantage of nickel foam three-dimensional net structure and high surface, improve the contact area of functional form Graphene and electrolyte, active material and the process of binding agent mixed pulp and the process of coating in traditional preparation technology are saved, reduce the internal resistance of capacitor simultaneously, improved specific capacity and cyclical stability.
A kind of method of preparing Graphene electrode of super capacitor based on nickel foam original position provided by the invention, it adopts collector is that hole count is the nickel foam of 15～110PPI, its thickness 0.5～10mm; First pass through Hummers legal system for graphite oxide slurry, then nickel foam is immersed in graphite oxide slurry, graphite oxide slurry is entered in the 3 D stereo cavernous structure of nickel foam; Directly putting into after drying under cryogenic vacuum environment reduces graphite oxide pyrolysis, graphite oxide after pyrolysis reduction is attached on the metallic framework of nickel foam and forms 3 D stereo network configuration, obtains preparing Graphene electrode of super capacitor based on nickel foam original position.
Described method comprises following concrete steps:
(1) ultrasonic cleaning in the KOH of 0.05mol/L solution of above-mentioned nickel foam with except degreasing, then is cleaned and removed surperficial oxide in rare HCl solution of 0.05mol/L, finally clean up with pure water and dry under vacuum environment;
(2) by the standby graphite oxide slurry of Hummers legal system, then directly nickel foam after treatment is immersed in to ultrasonic 1～3h in graphite oxide slurry, then take out, remove the unnecessary slurry in surface with scraper, and vacuumize at 30～50 ℃ of temperature;
(3) the dried nickel foam that is attached with graphite oxide is put into the heating furnace that is heated in advance 200～500 ℃;
(4) heating furnace is evacuated to rapidly to vacuum, after bleeding, the vacuum degree of heating furnace is 1～0.1Pa, and naturally cool to room temperature react 3～15min under this vacuum environment after, after stamping-out, obtain preparing Graphene electrode of super capacitor based on nickel foam original position.
In step (2), the concentration of described graphite oxide slurry is 0.2～0.5wt%.
In step (2), the described vacuum drying time is 24～48h.
Beneficial effect of the present invention is as follows:
(1) the present invention has utilized the 3 D stereo network configuration of nickel foam, and attached function type Graphene on the metallic framework of nickel foam takes full advantage of the specific area of nickel foam superelevation, makes electrode material have very large specific area.
(2) preparation method provided by the invention has saved the mixed pulp process of electrode active material and binding agent and conductive agent and slurry and has been coated to the process of collector, reduce the internal resistance of capacitor, improved capacitor large current density power and cyclical stability.
(3) what prepared by the present invention prepare Graphene electrode of super capacitor based on nickel foam original position has three-dimensional net structure, increase the contact area of functional form Graphene and electrolyte, improve migration and the diffusion velocity of ion, and made electrode there is high ratio electric capacity.
(4) provided by the inventionly prepare Graphene electrode of super capacitor based on nickel foam original position, preparation method's simple and fast, is suitable for the large-scale production of ultracapacitor, has larger market application foreground.
Embodiment
embodiment 1
(1) adopt Hummers legal system for graphite oxide slurry.First, in 500ml conical flask, add the 92ml concentrated sulfuric acid, and conical flask is put into cryostat, temperature is controlled to 0 ℃ of left and right.Add the natural flake graphite powder 4g processing with watery hydrochloric acid in advance, then add 2g NaNO
3, more slowly add 12g KMNO
4, after stirring reaction 2h.By in the constant water bath box of 35 ℃ of conical flask immigrations, continue stirring reaction 2 hours, now solution is purple green.Then slowly add 184 ml deionized waters, heating-up temperature is elevated to 75 ℃, continue to stir 1～3h.Slowly add appropriate hydrogen peroxide, now solution becomes golden yellow, filter while hot, and the hydrochloric acid that is 5% with mass fraction and deionized water cyclic washing is until sulfate radical-free ion in filtrate.Finally obtain certain density pure graphite oxide slurry, the concentration that regulates again graphite oxide slurry is 0.2wt%～0.5wt%, nickel foam clean surface washing is immersed in graphite oxide slurry and is taken out after ultrasonic 1～3h, and slurry unnecessary nickel foam surface is removed with scraper.
(2) nickel foam of the graphite oxide slurry that is attached with 0.2wt% of preparation in step (1) is placed in vacuum drying chamber to dry 48h in 30 ℃ of environment, then the dried nickel foam sample that is attached with graphite oxide is put into the heating furnace that is heated in advance 200 ℃, then rapidly heating furnace is evacuated to rapidly to vacuum, after bleeding, the vacuum degree of heating furnace is 1Pa, and it naturally cools to room temperature to react 3min relief under this vacuum environment, after becoming certain size, stamping-out obtains preparing Graphene electrode of super capacitor based on nickel foam original position.
(3) on electrochemical workstation and constant current charge-discharge instrument, carry out respectively electrochemical property test.Test result shows, the electrode of ultracapacitor in the time that charging and discharging currents density is 1A/g than electric capacity up to 268F/g; In the time that sweep speed is 1mV/s, than electric capacity up to 265F/g.
embodiment 2
(1) nickel foam that is attached with 0.3wt% graphite oxide slurry of preparation in example 1 is placed in vacuum drying chamber to dry 48h in 40 ℃ of environment, then the dried nickel foam sample that is attached with graphite oxide is put into the heating furnace that is heated in advance 250 ℃, then rapidly heating furnace is evacuated to rapidly to vacuum, after bleeding, the vacuum degree of heating furnace is 0.5Pa, and it naturally cools to room temperature to react 3min relief under this vacuum environment, after becoming certain size, stamping-out obtains preparing Graphene electrode of super capacitor based on nickel foam original position.
(2) on electrochemical workstation and constant current charge-discharge instrument, carry out respectively electrochemical property test.Test result shows, the electrode of ultracapacitor in the time that charging and discharging currents density is 1A/g than electric capacity up to 247F/g, in the time that sweep speed is 1mV/s, than electric capacity up to 243F/g.
embodiment 3
(1) nickel foam that is attached with 0.5wt% graphite oxide slurry of preparation in example 1 is placed in vacuum drying chamber to dry 48h in 50 ℃ of environment, then the dried nickel foam sample that is attached with graphite oxide is put into the heating furnace that is heated in advance 300 ℃, then rapidly heating furnace is evacuated to rapidly to vacuum, after bleeding, the vacuum degree of heating furnace is 0.1Pa, and it naturally cools to room temperature to react 3min relief under this vacuum environment, after becoming certain size, stamping-out obtains preparing Graphene electrode of super capacitor based on nickel foam original position.
(2) on electrochemical workstation and constant current charge-discharge instrument, do respectively electrochemical property test.Test result shows, the electrode of ultracapacitor in the time that charging and discharging currents density is 1A/g than electric capacity up to 256F/g, in the time that sweep speed is 1mV/s, than electric capacity up to 252F/g.
embodiment 4
(1) nickel foam that is attached with 0.4wt% graphite oxide slurry of preparation in example 1 is placed in vacuum drying chamber to dry 48h in 35 ℃ of environment, then the dried nickel foam sample that is attached with graphite oxide is put into the heating furnace that is heated in advance 400 ℃, then rapidly heating furnace is evacuated to rapidly to vacuum, after bleeding, the vacuum degree of heating furnace is 0.7Pa, and it naturally cools to room temperature to react 7min relief under this vacuum environment, after becoming certain size, stamping-out obtains preparing Graphene electrode of super capacitor based on nickel foam original position.
(2) on electrochemical workstation and constant current charge-discharge instrument, do respectively electrochemical property test.Test result shows, the electrode of ultracapacitor in the time that charging and discharging currents density is 1A/g than electric capacity up to 237F/g, in the time that sweep speed is 1mV/s, than electric capacity up to 232F/g.
embodiment 5
(1) nickel foam that is attached with 0.4wt% graphite oxide slurry of preparation in example 1 is placed in vacuum drying chamber to dry 48h in 45 ℃ of environment, then the dried nickel foam sample that is attached with graphite oxide is put into the heating furnace that is heated in advance 500 ℃, then rapidly heating furnace is evacuated to rapidly to vacuum, after bleeding, the vacuum degree of heating furnace is 0.3Pa, and it naturally cools to room temperature to react 12min relief under this vacuum environment, after becoming certain size, stamping-out obtains preparing Graphene electrode of super capacitor based on nickel foam original position.
(2) on electrochemical workstation and constant current charge-discharge instrument, do respectively electrochemical property test.Test result shows, the electrode of ultracapacitor in the time that charging and discharging currents density is 1A/g than electric capacity up to 224F/g, in the time that sweep speed is 1mV/s, than electric capacity up to 221F/g.
embodiment 6
(1) identical with step with embodiment 1 other conditions, vacuumize temperature is adjusted into 50 ℃, be then cooled to room temperature, after becoming certain size, stamping-out obtains preparing Graphene electrode of super capacitor based on nickel foam original position.
(2) on electrochemical workstation and constant current charge-discharge instrument, carry out respectively electrochemical property test.Test result shows, the electrode of ultracapacitor in the time that charging and discharging currents density is 1A/g than electric capacity up to 209F/g, in the time that sweep speed is 1mV/s, than electric capacity up to 201F/g.
embodiment 7
(1) identical with step with embodiment 1 other conditions, the lower reaction time of vacuum environment is adjusted into 10min, be then cooled to room temperature, after becoming certain size, stamping-out obtains preparing Graphene electrode of super capacitor based on nickel foam original position.
(2) on electrochemical workstation and constant current charge-discharge instrument, carry out respectively electrochemical property test.Test result shows, the electrode of ultracapacitor in the time that charging and discharging currents density is 1A/g than electric capacity up to 209F/g, in the time that sweep speed is 1mV/s, than electric capacity up to 201F/g.
embodiment 8
(1) identical with step with embodiment 1 other conditions, the lower reaction time of vacuum environment is adjusted into 15min, be then cooled to room temperature, after becoming certain size, stamping-out obtains preparing Graphene electrode of super capacitor based on nickel foam original position.
(2) on electrochemical workstation and constant current charge-discharge instrument, carry out respectively electrochemical property test.Test result shows, the electrode of ultracapacitor in the time that charging and discharging currents density is 1A/g than electric capacity up to 209F/g, in the time that sweep speed is 1mV/s, than electric capacity up to 201F/g.
embodiment 9
(1) identical with step with embodiment 1 other conditions, vacuum degree is adjusted into 0.1Pa, be then cooled to room temperature, after becoming certain size, stamping-out obtains preparing Graphene electrode of super capacitor based on nickel foam original position.
(2) after compressing tablet and cutting, can obtain electrode for super capacitor.On electrochemical workstation and constant current charge-discharge instrument, do respectively electrochemical property test.Test result shows, the electrode of ultracapacitor in the time that charging and discharging currents density is 1A/g than electric capacity up to 197F/g, in the time that sweep speed is 1mV/s, than electric capacity up to 190F/g.
embodiment 10
(1) identical with step with embodiment 3 other conditions, the lower reaction time of vacuum environment is adjusted into 10min, be then cooled to room temperature, after becoming certain size, stamping-out obtains preparing Graphene electrode of super capacitor based on nickel foam original position.
(2) after compressing tablet and cutting, can obtain electrode for super capacitor.On electrochemical workstation and constant current charge-discharge instrument, do respectively electrochemical property test.Test result shows, the electrode of ultracapacitor in the time that charging and discharging currents density is 1A/g than electric capacity up to 183F/g, in the time that sweep speed is 1mV/s, than electric capacity up to 178F/g.
embodiment 11
(1) identical with step with embodiment 3 other conditions, the lower reaction time of vacuum environment is adjusted into 15min, be then cooled to room temperature, after becoming certain size, stamping-out obtains preparing Graphene electrode of super capacitor based on nickel foam original position.
(2) after compressing tablet and cutting, can obtain electrode for super capacitor.On electrochemical workstation and constant current charge-discharge instrument, do respectively electrochemical property test.Test result shows, the electrode of ultracapacitor in the time that charging and discharging currents density is 1A/g than electric capacity up to 183F/g, in the time that sweep speed is 1mV/s, than electric capacity up to 178F/g.
Claims (4)
1. a method of preparing Graphene electrode of super capacitor based on nickel foam original position, is characterized in that: adopting collector is that hole count is the nickel foam of 15～110PPI, its thickness 0.5～10mm; First pass through Hummers legal system for graphite oxide slurry, then nickel foam is immersed in graphite oxide slurry, graphite oxide slurry is entered in the 3 D stereo cavernous structure of nickel foam; Directly putting into after drying under cryogenic vacuum environment reduces graphite oxide pyrolysis, graphite oxide after pyrolysis reduction is attached on the metallic framework of nickel foam and forms 3 D stereo network configuration, obtains preparing Graphene electrode of super capacitor based on nickel foam original position.
2. method according to claim 1, its feature comprises following concrete steps:
(1) ultrasonic cleaning in the KOH of 0.05mol/L solution of above-mentioned nickel foam with except degreasing, then is cleaned and removed surperficial oxide in rare HCl solution of 0.05mol/L, finally clean up with pure water and dry under vacuum environment;
(2) by the standby graphite oxide slurry of Hummers legal system, then directly nickel foam after treatment is immersed in to ultrasonic 1～3h in graphite oxide slurry, then take out, remove the unnecessary slurry in surface with scraper, and vacuumize at 30～50 ℃ of temperature;
(3) the dried nickel foam that is attached with graphite oxide is put into the heating furnace that is heated in advance 200～500 ℃;
(4) heating furnace is evacuated to rapidly to vacuum, after bleeding, the vacuum degree of heating furnace is 1～0.1Pa, and naturally cool to room temperature react 3～15min under this vacuum environment after, after stamping-out, can obtain preparing Graphene electrode of super capacitor based on nickel foam original position.
3. method according to claim 2, is characterized in that: in step (2), the concentration of described graphite oxide slurry is 0.2～0.5wt%.
4. method according to claim 2, is characterized in that: in step (2), the described vacuum drying time is 24～48h.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104291324A (en) * | 2014-09-09 | 2015-01-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of graphene foams |
| CN104576087A (en) * | 2015-02-03 | 2015-04-29 | 哈尔滨工业大学 | Production method of electrode of supercapacitor |
| CN104882297A (en) * | 2015-04-09 | 2015-09-02 | 山东师范大学 | Process for preparing stretchable supercapacitor based on highly conductive graphene/nickel particle mixed structure |
| CN105788877A (en) * | 2016-04-26 | 2016-07-20 | 北京航空航天大学 | Foamed three-dimensional graphene super capacitor electrode material and preparation method thereof |
| CN105836855A (en) * | 2016-06-13 | 2016-08-10 | 西安工业大学 | Preparation method and application of graphene gas diffusion electrode |
| CN105845461A (en) * | 2016-03-22 | 2016-08-10 | 重庆大学 | Carbon-filled foamed nickel, preparation method and application of carbon-filled foamed nickel |
| CN106206082A (en) * | 2016-08-20 | 2016-12-07 | 海南师范大学 | There is the preparation method and application of the nickel oxide/graphene combination electrode of electrochemical capacitance energy storage characteristic |
| CN106219521A (en) * | 2016-07-12 | 2016-12-14 | 昆明理工大学 | A kind of preparation method of three-dimensional foam Graphene |
| CN106803592A (en) * | 2015-11-26 | 2017-06-06 | 中国科学院金属研究所 | Graphene/redox graphene hydridization nesting porous network structure material and preparation and application |
| CN108364800A (en) * | 2018-01-22 | 2018-08-03 | 上海理工大学 | A kind of electrode material for super capacitor and preparation method thereof of nitrogen-doped graphene quantum dot/graphene |
| WO2019042206A1 (en) * | 2017-08-28 | 2019-03-07 | 刘铁林 | Water body mineralization device using nickel-based graphene field effect |
| WO2019047718A1 (en) * | 2017-09-11 | 2019-03-14 | 刘铁林 | Field effect space purification device |
| CN114044912A (en) * | 2021-10-19 | 2022-02-15 | 上海应用技术大学 | Ni-Co-ZIF composite material and preparation method and application thereof |
| CN114512352A (en) * | 2022-03-04 | 2022-05-17 | 广东工业大学 | Preparation method of flexible self-supporting electrode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104291324A (en) * | 2014-09-09 | 2015-01-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of graphene foams |
| CN104576087A (en) * | 2015-02-03 | 2015-04-29 | 哈尔滨工业大学 | Production method of electrode of supercapacitor |
| CN104882297B (en) * | 2015-04-09 | 2017-05-24 | 山东师范大学 | Process for preparing stretchable supercapacitor based on highly conductive graphene/nickel particle mixed structure |
| CN104882297A (en) * | 2015-04-09 | 2015-09-02 | 山东师范大学 | Process for preparing stretchable supercapacitor based on highly conductive graphene/nickel particle mixed structure |
| CN106803592B (en) * | 2015-11-26 | 2019-06-11 | 中国科学院金属研究所 | Graphene/redox graphene hydridization nesting porous network structure material and preparation and application |
| CN106803592A (en) * | 2015-11-26 | 2017-06-06 | 中国科学院金属研究所 | Graphene/redox graphene hydridization nesting porous network structure material and preparation and application |
| CN105845461A (en) * | 2016-03-22 | 2016-08-10 | 重庆大学 | Carbon-filled foamed nickel, preparation method and application of carbon-filled foamed nickel |
| CN105788877A (en) * | 2016-04-26 | 2016-07-20 | 北京航空航天大学 | Foamed three-dimensional graphene super capacitor electrode material and preparation method thereof |
| CN105836855A (en) * | 2016-06-13 | 2016-08-10 | 西安工业大学 | Preparation method and application of graphene gas diffusion electrode |
| CN105836855B (en) * | 2016-06-13 | 2019-02-15 | 西安工业大学 | A kind of preparation method and application of graphene gas-diffusion electrode |
| CN106219521A (en) * | 2016-07-12 | 2016-12-14 | 昆明理工大学 | A kind of preparation method of three-dimensional foam Graphene |
| CN106219521B (en) * | 2016-07-12 | 2018-08-31 | 昆明理工大学 | A kind of preparation method of three-dimensional foam graphene |
| CN106206082A (en) * | 2016-08-20 | 2016-12-07 | 海南师范大学 | There is the preparation method and application of the nickel oxide/graphene combination electrode of electrochemical capacitance energy storage characteristic |
| WO2019042206A1 (en) * | 2017-08-28 | 2019-03-07 | 刘铁林 | Water body mineralization device using nickel-based graphene field effect |
| WO2019047718A1 (en) * | 2017-09-11 | 2019-03-14 | 刘铁林 | Field effect space purification device |
| CN108364800A (en) * | 2018-01-22 | 2018-08-03 | 上海理工大学 | A kind of electrode material for super capacitor and preparation method thereof of nitrogen-doped graphene quantum dot/graphene |
| CN114044912A (en) * | 2021-10-19 | 2022-02-15 | 上海应用技术大学 | Ni-Co-ZIF composite material and preparation method and application thereof |
| CN114512352A (en) * | 2022-03-04 | 2022-05-17 | 广东工业大学 | Preparation method of flexible self-supporting electrode material |
| CN114512352B (en) * | 2022-03-04 | 2023-11-21 | 广东工业大学 | Preparation method of flexible self-supporting electrode material |
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