CN106098396B - It is a kind of for upright opening carbon compound film of ultracapacitor and preparation method thereof - Google Patents
It is a kind of for upright opening carbon compound film of ultracapacitor and preparation method thereof Download PDFInfo
- Publication number
- CN106098396B CN106098396B CN201610564328.5A CN201610564328A CN106098396B CN 106098396 B CN106098396 B CN 106098396B CN 201610564328 A CN201610564328 A CN 201610564328A CN 106098396 B CN106098396 B CN 106098396B
- Authority
- CN
- China
- Prior art keywords
- compound film
- performed polymer
- carbon
- carbon compound
- substrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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 belongs to the preparation methods of technical field of nanometer material preparation, more particularly to a kind of vertical mesoporous carbon compound film for ultracapacitor.The laminated film uses oligomeric water-soluble phenolic resin as carbon source, block copolymer is template, by the way that precursor solution in a variety of substrates such as nickel foam, carbon fiber is repeatedly added dropwise, heats volatilization self assembly, under the conditions of 100 DEG C~150 DEG C after 6 48h of hydro-thermal reaction, and it in an inert atmosphere, is carbonized to obtain with 400 DEG C~700 DEG C of temperature.The laminated film is the C film for having vertical channel structure, and vertical channel structure provides high specific surface area, and provides passage well into electrode material for electrolyte ion, while porous carbon promotes the electric conductivity of carbon composite.Vertical mesoporous carbon compound film prepared by the present invention obtains big specific capacitance and excellent stability as electrode of super capacitor.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, more particularly to a kind of preparation side of vertical mesoporous carbon compound film
Method and its application in ultracapacitor field.
Background technology
Increasingly failure with the non-renewable minerals energy such as traditional coal, oil, natural gas and the utilization at them
The environmental pollution generated in the process so that energy and environment become two faced in human kind sustainable development course and mainly ask greatly
Topic.At present, the development and utilization of the renewable and clean energy resources such as new energy solar energy, wind energy, thermal energy shows good hair
The impetus is opened up, huge potential is shown in terms of large-scale use from now on.But due to the supply of these regenerative resources
Intermittence is only stored when it can be generated, and could ensure the stable operation of energy consumption element；In addition, for clear
The application of the clean energy such as movable equipment (such as mobile phone, electric vehicle), sufficient power storage are also that it is normal
The premise of work.Accordingly, it is capable to the storage of amount, which becomes renewable and clean energy resource, realizes that one needs the pass solved in the process applied
Key problem.
Electric energy storage device widely studied in recent years mainly includes battery and ultracapacitor.Battery has larger energy
Metric density, can meet the application demand of most of electronic devices, but its less cycle charge-discharge number and relatively low fill
Discharge rate constrain its in demand high power density occasion application (Science, 1994,264:1115-1118,
Nature,2001,414:359–367).Compared with battery, ultracapacitor has higher cycle life and high charge-discharge speed
Rate, while possess the characteristic that simple in structure, property is stablized, it is allowed to supply in high-power energy conversion, portable electronic device, micro-current
Have in electric equipment it is good with (Science, 2008,321:651–652).
In recent years, scientist has put into substantial amounts of energy in the specific capacitance for increasing material specific surface area and material
(Nanoscale, 2013,5,8799-8820, Angew Chem Int Ed, 2011,50:1683-1687, ACS
Nano.2012,6(7):6400-6406).The research of flexible super capacitor at present be concentrated mainly on carbon fiber (micrometer fibers and
Nanofiber), carbon nanotubes, graphene and their composite construction.As supported based on flexible substrates (such as paper, sponge)
The flexible electrode of CNTs/Graphene coatings, the flexible electrode based on carbon fiber substrate, the paper-like based on CNTs/Graphene
Flexible electrode, the flexible electrode based on 3D macrostructures.
Although it is made some progress at present in terms of the synthesis of carbon-based electrode material, although Carbon-based supercapacitor is
Through being successfully commercialized, but in order to adapt to high integration electronics miniaturization, lightening and flexible needs, existing super electricity
Also there are many problems, charge transmission problem, the specific capacitance of material and stability problem, the utilization rate problems of active material for container
And device is ultra-thin and flexibility problem also has the space improved.Therefore, by electroactive material (electrode material) direct growth
On collector or directly constructing self-supporting high-specific surface area skeleton becomes optimization electrode structure, promotes charge transfer efficiency, carries
The effective measures of high active substance utilization rate.
It is inevitable development trend to adapt to this technological development direction to develop relevant new technology, the present invention is exactly
Therefore raw new technology.The present invention provides a kind of for upright opening carbon compound film of ultracapacitor and preparation method thereof.
The carbon compound film has the multilayer macropore structure perpendicular to substrate, has high specific surface area and excellent stabilization
Property；Macroporous structure is used to improve the efficiency of transmission of ion, increases electric conductivity；Meso-hole structure is used for increasing specific surface area, and raising is deposited
Storing up electricity is held.Meanwhile the carbon compound film has that preparation process is simple, the technologies such as at low cost, with obvious effects, applied widely are excellent
Gesture.
The content of the invention
Technical problem：In view of above-mentioned technical problem exists in the prior art, it is an object of the invention to provide one kind to be used for
Vertical mesoporous carbon compound film of ultracapacitor and preparation method thereof.The vertical mesoporous existing carbon fiber of carbon compound film
The macroporous structure of cloth/nickel foam in itself, while the mesopore orbit structure perpendicular to substrate is also equipped with,；Macroporous structure is used to improve
The efficiency of transmission of ion increases electric conductivity；Meso-hole structure is used for increasing specific surface area, improves storage capacitance.The laminated film
Using oligomeric water-soluble phenolic resin, block copolymer is template for carbon source, by by precursor solution in nickel foam, carbon fiber
Etc. being repeatedly added dropwise in a variety of substrates, heat volatilization self assembly, finally carbonization obtains；With preparation process is simple, at low cost, effect
Substantially, the technical advantages such as applied widely.The technical solution adopted in the present invention is as described below.
Technical solution：The present invention provides a kind of vertical mesoporous carbon compound film for ultracapacitor, and the carbon is compound
Film has the pore passage structure perpendicular to substrate, which is multilevel hierarchy, has macropore and meso pore characteristics, the hole of macropore
Footpath is about 30~500 μm, and mesoporous aperture is about 3~7nm；The carbon film material main component is carbon；The C film material
Material is supported on nickel foam or carbon cloth surface.
The carbon compound film is to use oligomeric water-soluble phenolic resin block copolymer is template for carbon source, pass through by
Precursor solution is repeatedly added dropwise in a variety of substrates such as nickel foam, carbon fiber, heats volatilization self assembly, in 100~150 DEG C of conditions
After when lower hydro-thermal reaction 6~48 is small, and in an inert atmosphere, it is carbonized to obtain with 400 DEG C~700 DEG C of temperature.
The carbon compound film has macroporous structure and meso-hole structure simultaneously, and macroporous structure is used to improve the transmission of ion
Efficiency increases electric conductivity；Meso-hole structure is used for increasing specific surface area, improves storage capacitance.The laminated film is that have to hang down
The C film of straight pore passage structure, vertical channel structure provide high specific surface area, and are electrolyte ion well into electricity
Pole material provides passage, while porous carbon promotes the electric conductivity of carbon composite.
The present invention also provides the preparation method of the vertical mesoporous carbon compound film for ultracapacitor, the preparations
Method concretely comprises the following steps：
(1) the synthesis of performed polymer synthesizes the phenolic resin performed polymer of low molecular weight and the single-stranded micella of Spherical Carbon：
By phenol, the aqueous solution of formalin and NaOH are mixed, and are stirred to react at 50~90 DEG C, obtain low molecule
The phenolic resin prepolymer reaction solution of amount.Then, polyether block copolymer is dissolved in water, and the prepolymer before addition
In reaction solution, after stirring 1~5h.Solution is diluted again, and is futher stirred at 50~90 DEG C to observing deposition.
Polyether block copolymer described in step (1) is F127, and molecular characterization is：MW=12600,
PEO106PPO70PEO106。
After the completion of step (1), the granular size for the performed polymer that DLS real-time testings are formed, step can be used after precipitation dissolving
Suddenly the formation mesoporous to later stage rule of the test effect of the micelle complex particle of performed polymer plays a crucial role in (1), and micella is multiple
Construction unit of the polymer beads as follow-up mesopore film can cause film uneven if micelle complex particle is uneven,
And micella is the template in duct in film, if micella is uneven, later stage duct is also uneven.
(2) base treatment and absorption performed polymer：
Substrate is ultrasonically treated, after cleaning and drying, substrate is immersed in performed polymer made from step (1) simultaneously
Performed polymer is adsorbed in fully infiltration.
Step (2) described substrate can be carbon cloth, nickel foam or silicon chip.
, it is necessary to which the performed polymer that appropriate step (1) is prepared is taken fully to soak when making substrate using carbon cloth or nickel foam
Moisten the carbon cloth handled well or nickel foam, put 40~80 DEG C of 3~10min of heating of baking oven, this infiltration, heating process repeat 3~5
It is secondary to adsorb performed polymer.
It during using silicon chip as substrate, will be ultrasonically treated, after cleaning and drying, the silicon chip that ultrasound is crossed be immersed in
Volume ratio is 3:1 H2SO4And H2O2Mixed solution in, impregnate 10min at normal temperatures, finally cleaned and dried with ultra-pure water；
Then silicon chip is immersed in performed polymer made from step (1) and fully infiltrated, make performed polymer in the abundant self assembly of silicon chip surface.
The formation mesoporous to later stage rule of the process of absorption performed polymer plays a crucial role in step (2), and thermal evaporation is conducive to
The further regular self assembly of micella performed polymer composite particles.If without this step, will obtain particle packing film rather than
Vertical porous membrane
(3) water-heat process
Substrate after step (2) adsorbs performed polymer is put into reaction kettle, is put into after adding in ultra-pure water and static soak
Baking oven carries out 6~48h of hydro-thermal reaction at 100 DEG C~150 DEG C.After its cooling, taking out load has the substrate of product, fully
After cleaning, baking oven is put into℃It is dry, obtain substrate/macromolecule laminated film.
(4) carbonisation
Substrate/macromolecule laminated film that step (3) drying is obtained further carbon in 400 DEG C~700 DEG C of argon gas
Change 1~3h to obtain vertical mesoporous carbon compound film.
In order to test the chemical property of vertical mesoporous carbon compound film, surveyed using cyclic voltammetry by three-electrode system
Try the chemical property of laminated film.Three electrodes are working electrode (vertical mesoporous carbon compound film) respectively, to electrode (metal platinum
Piece) and reference electrode (Ag/AgCl electrodes).The Na of 1mol/L2SO4Electrolyte is done, and as electrode of super capacitor, is surveyed
Try its ultracapacitor correlated performance.By test, vertical mesoporous carbon compound film has excellent chemical property, especially
It is that have big specific capacitance.In addition, vertical mesoporous multilayer pore passage structure causes the carbon compound film to have stable structure spy
Point.In summary, the upright opening carbon compound film prepared by the present invention obtains big specific capacitance as electrode of super capacitor
And excellent stability.
Carbon compound film of the present invention, the excellent chemical property and design feature having can be used to surpass
Grade electrode for capacitors.
The present invention has the advantages that：
1st, upright opening carbon compound film of the invention has the pore passage structure perpendicular to substrate, which ties to be multistage
Structure, has macropore and meso pore characteristics, and structural stability is good；
2nd, the preparation method of carbon compound film of the present invention is simple, at low cost, with obvious effects, applicable with preparation process
The technical advantages such as scope is wide；
3rd, upright opening carbon compound film of the invention can be applied to electrode of super capacitor, and macroporous structure is used to improve ion
Efficiency of transmission, increase electric conductivity；Meso-hole structure is used for increasing specific surface area, improves storage capacitance.
Description of the drawings
The micella formed in Fig. 1 embodiments 1 in performed polymer synthesis to block copolymer and of micella/performed polymer
Grain size test result；
The SEM figures of prepared carbon cloth/macromolecule laminated film in Fig. 2 embodiments 1；
The SEM figures of the prepared mesoporous carbon cloth/carbon compound film of upright opening in Fig. 3 embodiments 1；
The SEM figures of prepared nickel foam/macromolecule membrane in Fig. 4 embodiments 2；
The SEM figures of prepared upright opening mesoporous foam nickel carbon laminated film in Fig. 5 embodiments 2；
The SEM figures of prepared silicon chip/macromolecule membrane in Fig. 6 embodiments 4；
The SEM figures of the prepared mesoporous silicon chip/carbon compound film of upright opening in Fig. 7 embodiments 4；
The electrochemical property test of the prepared mesoporous carbon cloth/carbon compound film of upright opening in Fig. 8 embodiments 5；
The electrochemical property test of prepared upright opening mesoporous foam nickel carbon laminated film in Fig. 9 embodiments 6.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment is carried out lower based on the technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following examples.
Embodiment 1
The preparation of the mesoporous carbon cloth of upright opening/macromolecule laminated film
(1) synthesis of performed polymer：By the phenol of 0.6g, the formalin (37wt%) of 2.1mL, 15mL 0.1mol/L's
NaOH solution is added in the three-necked flask of 250mL, then stirs 2h at 50 DEG C.Triblock copolymer F127 (the MW=of 0.96g
12600, PEO106PPO70PEO106) be dissolved in 15mL ultra-pure waters, and be added in phenolic resin performed polymer, at a temperature of 50 DEG C
After stirring 4h, the ultra-pure water of 56mL is added in into above-mentioned solution, is continued 10~14h of stir about, is stopped when solution turned cloudy
Reaction takes out and stands dissolving to be precipitated, using the formation (as shown in Figure 1) of DLS tracking performed polymers.
(2) base treatment and absorption performed polymer：By carbon cloth acetone, ethyl alcohol and ultra-pure water ultrasound 30min, Ran Houyong
Ultra-pure water is cleaned and dried；The performed polymer that appropriate step (1) is prepared is taken fully to infiltrate the carbon cloth handled well, puts baking oven
80 DEG C of 3~10min of heating, this infiltration, heating process repeat 3~5 times to adsorb performed polymer.
(3) water-heat process：Above-mentioned absorption performed polymer carbon cloth is put into 25~100mL reaction kettles, addition 15~
Baking oven is put into after 75mL ultra-pure waters and static soak 4h, 100 DEG C of 6~48h of hydro-thermal reaction, after its cooling, taking out load has production
The carbon cloth of object after fully being cleaned with ultra-pure water, is put into 30~80 DEG C of dryings of baking oven, it is compound to obtain carbon cloth/macromolecule
Film (as shown in Figure 2).
(4) carbonisation：Argon of the carbon cloth/macromolecule membrane that step (3) drying is obtained at 400 DEG C~700 DEG C
1~3h is further carbonized in gas to obtain the mesoporous carbon cloth/carbon compound film (as shown in Figure 3) of upright opening.
Embodiment 2
The preparation of upright opening mesoporous foam nickel/macromolecule laminated film
(1) synthesis of performed polymer：By the phenol of 0.6g, the formalin (37wt%) of 2.1mL, 15mL 0.1mol/L's
NaOH solution is added in the three-necked flask of 250mL, then stirs 1h at 60 DEG C.Triblock copolymer F127 (the MW=of 0.96g
12600, PEO106PPO70PEO106) be dissolved in 15mL ultra-pure waters, and be added in phenolic resin performed polymer, at a temperature of 60 DEG C
After stirring 4h, the ultra-pure water of 56mL is added in into above-mentioned solution, is continued 10~14h of stir about, is stopped when solution turned cloudy
Reaction takes out and stands dissolving to be precipitated.
(2) base treatment and absorption performed polymer：It is dried after nickel foam is fully cleaned with dilute hydrochloric acid ultrasound 3min with ultra-pure water
It is dry；The performed polymer that appropriate step (1) is prepared is taken fully to infiltrate the nickel foam handled well, put 40 DEG C of baking oven heating 3~
10min, this infiltration, heating process repeat 1~3 time to adsorb performed polymer.
(3) water-heat process：Above-mentioned absorption performed polymer nickel foam is put into 25~100mL reaction kettles, adds in 15~75mL
Baking oven is put into after ultra-pure water and static soak 4h, 100 DEG C~150 DEG C 6~48h of hydro-thermal reaction, after its cooling, taking out load has
The nickel foam of product after fully being cleaned with ultra-pure water, is put into 40 DEG C of dryings of baking oven, obtains nickel foam/macromolecule laminated film
It prepares (as shown in Figure 4).
(4) carbonisation：Nickel foam/macromolecule membrane that step (3) drying is obtained is in 400~550 DEG C of argon gas
1~3h be further carbonized to obtain upright opening mesoporous foam nickel carbon laminated film (as shown in Figure 5).
Embodiment 3
The preparation of upright opening mesoporous foam nickel/macromolecule laminated film
(1) synthesis of performed polymer：By the phenol of 0.6g, the formalin (37wt%) of 2.1mL, 15mL 0.1mol/L's
NaOH solution is added in the three-necked flask of 250mL, then stirs 0.5h at 90 DEG C.Triblock copolymer F127 (the MW of 0.96g
=12600, PEO106PPO70PEO106) be dissolved in 15mL ultra-pure waters, and be added in phenolic resin performed polymer, in 90 DEG C of temperature
After lower stirring 2h, the ultra-pure water of 56mL is added in into above-mentioned solution, continues 10~14h of stir about, stops when solution turned cloudy
It only reacts, takes out and stand dissolving to be precipitated,
(2) base treatment and absorption performed polymer：It is dried after nickel foam is fully cleaned with dilute hydrochloric acid ultrasound 3min with ultra-pure water
It is dry；The performed polymer that appropriate step (1) is prepared is taken fully to infiltrate the nickel foam handled well, put 40 DEG C of baking oven heating 3~
10min, this infiltration, heating process repeat 3-5 times to adsorb performed polymer.
(3) water-heat process：Above-mentioned absorption performed polymer nickel foam is put into 25~100mL reaction kettles, adds in 15~75mL
Baking oven is put into after ultra-pure water and static soak 4h, 100 DEG C~150 DEG C hydro-thermal reaction 6h, after its cooling, taking out load has product
Nickel foam, after fully being cleaned with ultra-pure water, be put into 40 DEG C of dryings of baking oven, obtain the preparation of nickel foam/macromolecule laminated film.
(4) carbonisation：Nickel foam/macromolecule membrane that step (3) drying is obtained is in 500~700 DEG C of argon gas
3~5h be further carbonized to obtain upright opening mesoporous foam nickel carbon laminated film.
Embodiment 4
The preparation of the mesoporous silicon chip of upright opening/macromolecule laminated film
(1) synthesis of performed polymer：By the phenol of 0.6g, the formalin (37wt%) of 2.1mL, 15mL 0.1mol/L's
NaOH solution is added in the three-necked flask of 250mL, then stirs 0.5h at 50~80 DEG C.The triblock copolymer of 0.96g
F127 (MW=12600, PEO106PPO70PEO106) be dissolved in 15mL ultra-pure waters, and be added in phenolic resin performed polymer,
After stirring 2h at a temperature of 50~80 DEG C, the ultra-pure water of 56mL is added in into above-mentioned solution, continues stir about 10~14h, Zhi Daorong
Stop reaction when liquid becomes cloudy, take out and stand dissolving to be precipitated.
(2) base treatment and absorption performed polymer：It by silicon chip ethyl alcohol and ultra-pure water ultrasound 30min, then dries, afterwards will
The silicon chip that ultrasound is crossed is immersed in 6mL H2SO4, 2mLH2O2(H2SO4：H2O2=3:1) in mixed solution, impregnate at normal temperatures
10min is finally cleaned and dried with ultra-pure water；Then 6.60mL prepolymer solutions is taken to pour into 50mL reaction kettles, it will be treated
Silicon chip be put into solution, be standing and soak for 0.5~3 it is small when；It is eventually adding 30mL ultra-pure waters and is used for dilute solution, and static soak
0.5~4h makes it in the abundant self assembly of silicon chip surface.
(3) water-heat process：Above-mentioned absorption performed polymer silicon chip is put into 25~100mL reaction kettles, 15~75mL is added in and surpasses
Baking oven is put into after pure water and static soak 4h, 100 DEG C~150 DEG C hydro-thermal reaction 6h, after its cooling, taking out load has product
Silicon chip after fully being cleaned with ultra-pure water, is put into 40 DEG C of dryings of baking oven, obtains preparation (such as Fig. 6 of silicon chip/macromolecule laminated film
It is shown).
(4) carbonisation：Nickel foam/macromolecule membrane that step (3) drying is obtained is in 400~500 DEG C of argon gas
1~3h be further carbonized to obtain the mesoporous silicon chip/carbon compound film (as shown in Figure 7) of upright opening.
Embodiment 5
The electrochemical property test of the mesoporous carbon cloth/carbon compound film of upright opening
We using cyclic voltammetry by the mesoporous carbon cloth of upright opening made from three-electrode system testing example 1/
The chemical property of carbon compound film.Three electrodes are working electrode (vertical mesoporous carbon compound film) respectively, to electrode (metal platinum
Piece) and reference electrode (Ag/AgCl electrodes).The Na of 1mol/L2SO4 does electrolyte, obtained electrochemistry cyclic voltammetry curve
As shown in Figure 8.
Embodiment 6
The electrochemical property test of upright opening mesoporous foam nickel carbon laminated film
We using cyclic voltammetry by the mesoporous carbon cloth of upright opening made from three-electrode system testing example 2/
The chemical property of carbon compound film.Three electrodes are working electrode (vertical mesoporous carbon compound film) respectively, to electrode (metal platinum
Piece) and reference electrode (Ag/AgCl electrodes).The Na of 1mol/L2SO4Electrolyte is done, obtained electrochemistry cyclic voltammetry curve is such as
Shown in Fig. 9.
Claims (5)
1. a kind of vertical mesoporous carbon compound film for ultracapacitor, which is characterized in that the carbon compound film, which has, to hang down
Directly in the pore passage structure of substrate, which is multilevel hierarchy, while has macroporous structure and meso-hole structure feature, macropore
Aperture is 30-500 μm, and mesoporous aperture is 3-7nm；The carbon compound film main component is carbon.
A kind of 2. preparation method of vertical mesoporous carbon compound film as described in claim 1, which is characterized in that the method bag
Include following steps：
(1) the synthesis of performed polymer synthesizes the phenolic resin performed polymer of low molecular weight and the single-stranded micella of Spherical Carbon：
By phenol, the aqueous solution of formalin and NaOH are mixed, and 0.5-2h is stirred to react at 50-90 DEG C, obtain low point
The prepolymer reaction solution of son amount；Then, polyether block copolymer is dissolved in water, and the prepolymer reaction before addition is molten
It in liquid, after stirring 2~4h, adds water and dilutes solution, and futher stir at 50-90 DEG C to observing deposition；
(2) base treatment and absorption performed polymer：
Substrate is ultrasonically treated, after cleaning and drying, substrate is immersed in performed polymer made from step (1) simultaneously fully
Performed polymer is adsorbed in infiltration；
(3) water-heat process：
Substrate after step (2) adsorbs performed polymer is put into reaction kettle, baking oven is put into after adding in ultra-pure water and static soak,
Hydro-thermal reaction 6-48h is carried out at 100 DEG C -150 DEG C；After its cooling, taking out load has the substrate of product, fully after cleaning, puts
Enter 30-80 DEG C of drying of baking oven, obtain substrate/macromolecule laminated film；
(4) carbonisation：
Obtained substrate/macromolecule the laminated film of step (3) drying is further carbonized 1-5h in 400~700 DEG C of argon gas
To obtain vertical mesoporous carbon compound film；
Step (2) described substrate is carbon cloth, nickel foam or silicon chip；
, it is necessary to take at the performed polymer fully infiltration that appropriate step (1) is prepared when making substrate using carbon cloth or nickel foam
The carbon cloth or nickel foam managed put 40-80 DEG C of 3~10min of heating of baking oven, this infiltration, heating process repeat 1-5 times to inhale
Attached performed polymer；
It during using silicon chip as substrate, will be ultrasonically treated, after cleaning and drying, the silicon chip that ultrasound is crossed be immersed in volume
Than for 3:1 H2SO4And H2O2Mixed solution in, impregnate 10min at normal temperatures, finally cleaned and dried with ultra-pure water；Then
Silicon chip is immersed in performed polymer made from step (1) and is fully infiltrated, makes performed polymer in the abundant self assembly of silicon chip surface.
3. according to the method described in claim 2, it is characterized in that：The chemical property of the vertical mesoporous carbon compound film of test
When, pass through the chemical property of three-electrode system test compound film using cyclic voltammetry.
4. according to the method described in claim 3, it is characterized in that：Three electrodes are the vertical mesoporous carbon as working electrode respectively
Laminated film, as the metal platinized platinum to electrode and the Ag/AgCl electrodes as reference electrode, the Na of 1mol/L2SO4It is electrolysed
Matter, and as electrode of super capacitor, test its ultracapacitor correlated performance.
5. a kind of application in electrochemical field of vertical mesoporous carbon compound film as described in claim 1, which is characterized in that
The carbon compound film can be applied to electrode of super capacitor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610564328.5A CN106098396B (en) | 2016-07-18 | 2016-07-18 | It is a kind of for upright opening carbon compound film of ultracapacitor and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610564328.5A CN106098396B (en) | 2016-07-18 | 2016-07-18 | It is a kind of for upright opening carbon compound film of ultracapacitor and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106098396A CN106098396A (en) | 2016-11-09 |
| CN106098396B true CN106098396B (en) | 2018-05-29 |
Family
ID=57220536
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610564328.5A Active CN106098396B (en) | 2016-07-18 | 2016-07-18 | It is a kind of for upright opening carbon compound film of ultracapacitor and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106098396B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108179433B (en) * | 2016-12-08 | 2019-09-06 | 中国科学院大连化学物理研究所 | Ordered mesopore carbon loads nanometer iridium base electrocatalytic hydrogen evolution electrode and its preparation and application |
| CN109244354B (en) * | 2018-07-14 | 2021-03-02 | 哈尔滨工业大学 | Self-supporting composite electrode |
| CN109346339A (en) * | 2018-12-07 | 2019-02-15 | 南京理工大学 | A kind of Ni-based high load NiCo of foam2S4The preparation method of combination electrode |
| CN116799436A (en) * | 2023-06-19 | 2023-09-22 | 深圳材启新材料有限公司 | Capacitive film and preparation method and application thereof |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012562A (en) * | 2007-02-01 | 2007-08-08 | 上海交通大学 | Method for preparing carbon nano-tube coextruded film on single-crystal silicon slice surface |
| CN101134567A (en) * | 2007-07-26 | 2008-03-05 | 复旦大学 | High-stability large aperture ordered meso-porous carbon material and preparation method thereof |
| CN101244818A (en) * | 2008-03-20 | 2008-08-20 | 复旦大学 | Method for producing ordered mesoporous polymer, material with carbon element and composite material in macro amount |
| CN101538033A (en) * | 2009-04-13 | 2009-09-23 | 西安交通大学 | Method for preparing porous carbon material containing mesopores and macropores |
| CN102085475A (en) * | 2010-12-02 | 2011-06-08 | 上海师范大学 | Preparation method of integral mesoporous material attached to porous blocky matrix |
| CN102249213A (en) * | 2011-04-24 | 2011-11-23 | 大连理工大学 | Preparation method of foaming ordered mesoporous carbon integral material with graded tunnel structure |
| CN102759557A (en) * | 2012-07-12 | 2012-10-31 | 上海交通大学 | Method for improving performances of field effect gas sensor based on SWNTs (single walled carbon nanotubes) |
| CN103071396A (en) * | 2011-10-26 | 2013-05-01 | 沈阳工业大学 | Substrate induction method used for preparing ordered porous carbon film |
| CN103232266A (en) * | 2013-04-18 | 2013-08-07 | 上海交通大学 | Preparation method of silicon substrate surface oxidized carbon-nanotube self-assembly composite film |
| CN105531241A (en) * | 2013-09-20 | 2016-04-27 | 赫罗伊斯石英玻璃股份有限两合公司 | Method for producing a porous carbon product |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014060508A1 (en) * | 2012-10-18 | 2014-04-24 | Cic Energigune | Process for the preparation of hierarchically meso and macroporous structured materials |
| WO2016025532A1 (en) * | 2014-08-11 | 2016-02-18 | The Arizona Board Of Regents On Behalf Of The University Of Arizona | Aligned graphene-carbon nanotube porous carbon composite |
-
2016
- 2016-07-18 CN CN201610564328.5A patent/CN106098396B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012562A (en) * | 2007-02-01 | 2007-08-08 | 上海交通大学 | Method for preparing carbon nano-tube coextruded film on single-crystal silicon slice surface |
| CN101134567A (en) * | 2007-07-26 | 2008-03-05 | 复旦大学 | High-stability large aperture ordered meso-porous carbon material and preparation method thereof |
| CN101244818A (en) * | 2008-03-20 | 2008-08-20 | 复旦大学 | Method for producing ordered mesoporous polymer, material with carbon element and composite material in macro amount |
| CN101538033A (en) * | 2009-04-13 | 2009-09-23 | 西安交通大学 | Method for preparing porous carbon material containing mesopores and macropores |
| CN102085475A (en) * | 2010-12-02 | 2011-06-08 | 上海师范大学 | Preparation method of integral mesoporous material attached to porous blocky matrix |
| CN102249213A (en) * | 2011-04-24 | 2011-11-23 | 大连理工大学 | Preparation method of foaming ordered mesoporous carbon integral material with graded tunnel structure |
| CN103071396A (en) * | 2011-10-26 | 2013-05-01 | 沈阳工业大学 | Substrate induction method used for preparing ordered porous carbon film |
| CN102759557A (en) * | 2012-07-12 | 2012-10-31 | 上海交通大学 | Method for improving performances of field effect gas sensor based on SWNTs (single walled carbon nanotubes) |
| CN103232266A (en) * | 2013-04-18 | 2013-08-07 | 上海交通大学 | Preparation method of silicon substrate surface oxidized carbon-nanotube self-assembly composite film |
| CN105531241A (en) * | 2013-09-20 | 2016-04-27 | 赫罗伊斯石英玻璃股份有限两合公司 | Method for producing a porous carbon product |
Non-Patent Citations (3)
| Title |
|---|
| Preparation of a self-standing mesoporous carbon membrane with perpendicularly-ordered pore structures;K Kimijim 等;《Chemical Communications》;20081001;第44卷;第5809-5811页 * |
| Ultrahigh Strength and Stiffness in Cross-Linked Hierarchical Carbon Nanotube Bundles;T. Filleter等;《Advanced Materials》;20110429;第23卷;第2855-2860页 * |
| 大孔-介孔分级结构炭材料的制备及应用研究;王志超;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20100915(第09期);B014-11 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106098396A (en) | 2016-11-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| He et al. | Carbon layer-exfoliated, wettability-enhanced, SO3H-functionalized carbon paper: A superior positive electrode for vanadium redox flow battery | |
| Zhang et al. | Recent advances and challenges of electrode materials for flexible supercapacitors | |
| Xue et al. | Template-free, self-doped approach to porous carbon spheres with high N/O contents for high-performance supercapacitors | |
| Fan et al. | Ti3C2-MXene composite films functionalized with polypyrrole and ionic liquid-based microemulsion particles for supercapacitor applications | |
| Shi et al. | Flexible 3D carbon cloth as a high-performing electrode for energy storage and conversion | |
| Liang et al. | Highly compressible carbon sponge supercapacitor electrode with enhanced performance by growing nickel–cobalt sulfide nanosheets | |
| Wu et al. | NiS nanoparticles assembled on biological cell walls-derived porous hollow carbon spheres as a novel battery-type electrode for hybrid supercapacitor | |
| CN106784819B (en) | A kind of lithium sulfur battery anode material and preparation method thereof | |
| CN104466134B (en) | The preparation method of self-supporting graphene/carbon nano-tube hybrid foam support amino anthraquinones base polymer | |
| CN106098396B (en) | It is a kind of for upright opening carbon compound film of ultracapacitor and preparation method thereof | |
| CN105206430B (en) | Polyaniline nanotube array/graphene composite material electrode and its preparation method and application | |
| Wang et al. | Nitrogen-doped mesoporous carbon as low-cost counter electrode for high-efficiency dye-sensitized solar cells | |
| Mao et al. | High loading cotton cellulose-based aerogel self-standing electrode for Li-S batteries | |
| CN104176783B (en) | The preparations and applicatio method of the coated manganese dioxide nanowire of a kind of nitrogen carbon material | |
| Song et al. | High flexibility and electrocatalytic activity MoS2/TiC/carbon nanofibrous film for flexible dye-sensitized solar cell based photovoltaic textile | |
| CN106971860A (en) | A kind of MnO2The preparation method of@graphene fiber super capacitor electrode materials | |
| CN108922790A (en) | A kind of manganese dioxide/N doping porous carbon composite preparation method and application of sodium ion insertion | |
| Chen et al. | Three-dimensional ordered macroporous carbon as counter electrodes in dye-sensitized solar cells | |
| CN106024408A (en) | Ruthenium oxide-copper sulfide composite material, application thereof and electrode plate for supercapacitor | |
| Shao et al. | Hierarchical porous carbons as a metal-free electrocatalyst of triiodide reduction for dye-sensitized solar cells | |
| Wu et al. | Performance of V2O3@ C composites via a sol–gel precursor assisted by soluble starch as Pt-free counter electrodes for dye sensitized solar cells | |
| CN106816603A (en) | A kind of three-dimensional grapheme aeroge carries sulphur composite and its preparation method and application | |
| Chen et al. | Wood-derived scaffolds decorating with nickel cobalt phosphate nanosheets and carbon nanotubes used as monolithic electrodes for assembling high-performance asymmetric supercapacitor | |
| Liu et al. | Oxygen-directed porous activation of carbon nanospheres for enhanced capacitive energy storage | |
| Huang et al. | Hollow FeS2 nanospheres encapsulated in N/S co-doped carbon nanofibers as electrode material for electrochemical energy storage |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |