CN106219515A - There is the synthetic method of the empty spherical nitrogen-doped carbon material of special crosslinking - Google Patents
There is the synthetic method of the empty spherical nitrogen-doped carbon material of special crosslinking Download PDFInfo
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- CN106219515A CN106219515A CN201610598581.2A CN201610598581A CN106219515A CN 106219515 A CN106219515 A CN 106219515A CN 201610598581 A CN201610598581 A CN 201610598581A CN 106219515 A CN106219515 A CN 106219515A
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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
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a kind of synthetic method with the empty spherical nitrogen-doped carbon material of special crosslinking, main introducing oxide/carbon nanometer tube in commercialization tripolycyanamide sponge hole, and it is coated with polyaniline at its surface aggregate, process preparation by high temperature pyrolysis and there is the nitrogen-doped carbon material of the empty spherical looks of special crosslinking, concrete drip irrigation device is: joined by oxide/carbon nanometer tube dispersion liquid in the acid solution of aniline monomer, adding oxidant Ammonium persulfate. causes aniline in the polyreaction of CNT, tripolycyanamide sponge is dipped in above-mentioned solution, the oxide/carbon nanometer tube of deposition polyaniline is formed in sponge hole, empty spherical nitrogen-doped carbon material is cross-linked through the preparation of high temperature pyrolysis carbonization treatment.Prepared nitrogen-doped carbon material is cross-linked by CNT, contribute to obtaining high electrical conductivity, the carbon nitrogen skeleton of nitrogen-doped carbon material is provided that good electrical capacitive and catalysis activity, is all provided that good capacitive property in convention acidic electrolyte and redox electrolytes plastidome.
Description
Technical field
The invention belongs to the synthesis technical field of electrode material for super capacitor, be specifically related to one and there is special crosslinking sky
The synthetic method of spherical nitrogen-doped carbon material.
Background technology
Porous carbon materials is owing to having high specific surface area, good chemical inertness and certain electric conductivity and mechanical property
Can, adsorbing, it is catalyzed, separates and electrochemical electrode Material Field has wide application prospects.Therefore, various different presomas with
And different preparation methoies is all widely used in preparing porous carbon materials.The doping energy Effective Regulation carbon material surface of heterogeneous element
Polarity and electronic configuration, can regulate the work content of material with carbon element simultaneously, therefore gives carbon material surface redox active, catalysis activity
And hydrophilic, in terms of catalysis, electrochemistry, there is huge potentiality to be exploited.Nitrogen element is a kind of important electron rich doped chemical,
In carbon base body, nitrogen element exists with forms such as pyridine type, Bi Kaxing, graphite moulds, and these nitrogen elements can significantly improve carbonaceous material
The redox active of material, catalysis activity and electric conductivity, therefore have more superior in terms of electrochemical catalysis and energy and material
Application performance.
The synthesis of nitrogen-doped carbon material mainly includes that the pyrolysis processing of nitrogenous precursor and the functionalization of carbonaceous material are repaiied
Decorations, wherein the former presoma selects face wider, and preparation method is simple, is suitable for large-scale production, and nitrogen element can mix carbon back
The surface of body is internal mutually with body, can more effectively regulate and control material with carbon element body structure surface characteristic and application performance.Use suitable precursors and
Rationally synthesis path prepares nitrogen-doped carbon material, inquires into its application in electrochemical energy storage field significant.
Summary of the invention
Present invention solves the technical problem that and there is provided a kind of synthesis with the empty spherical nitrogen-doped carbon material of special crosslinking
Method, this hollow nitrogen-doped carbon material being cross-linked with each other has large surface area and multidimensional conductive channel, at electrochemical energy storage
The device such as aspect such as electrode material for super capacitor and lithium ion battery negative material has preferable application prospect.
The present invention solves that above-mentioned technical problem adopts the following technical scheme that, there is the empty spherical nitrogen-doped carbon material of special crosslinking
The synthetic method of material, it is characterised in that concretely comprise the following steps:
Step (1), preparation molar concentration is the acid solution of 1mol/L, adds 0.2mL aniline after taking the cooling of 100mL acid solution ice bath
Monomer obtains solution A, adds 0.12g Ammonium persulfate. and obtain solution B after separately taking the cooling of 100mL acid solution ice bath；
Step (2), by 1-3mg oxide/carbon nanometer tube (by volume ratio concentrated sulphuric acid: business multilamellar is boiled in the nitration mixture boiling of concentrated nitric acid=1:3
CNT, as follows on) ultrasonic disperse forms suspension in 1mL deionized water, this suspension is joined in solution A in
Stir 10min under condition of ice bath and obtain solution C, then solution B is joined and solution C stirs 2min formation uniform dispersion；
Step (3), puts in above-mentioned uniform dispersion by the tripolycyanamide sponge of one piece of a size of 1cm × 2cm × 3cm, then
It is placed under condition of ice bath reaction 24-48h, in tripolycyanamide sponge hole, forms the oxide/carbon nanometer tube of deposition polyaniline, then use
Deionized water rinsing to flushing liquor is the colourless tripolycyanamide sponge obtaining green；
Step (4), puts into green tripolycyanamide sponge in baking oven and dries, be subsequently placed in tube furnace in nitrogen atmosphere in
600-800 DEG C of calcining 1-2h obtains having the empty spherical nitrogen-doped carbon material of special crosslinking.
Further preferably, the acid solution described in step (1) is sulfuric acid solution or hydrochloric acid solution.
The tripolycyanamide sponge that the present invention uses contains abundant nitrogen element, can make nitrogen-doped carbon material by calcining,
The armaticity polyaniline of oxide/carbon nanometer tube surface deposition can also make nitrogen-doped carbon material, carbon nanometer as good presoma
Pipe can simultaneously serve as good conductive channel, and therefore synthesized polyaniline hollow nitrogen-doped carbon ball can be had by CNT
Effect connects, and can improve the monolithic conductive of material；The frame structure of the most synthesized material contains abundant macropore, is conducive to electricity
Solving the quick scattering and permeating of matter, the most this kind of material can be used as the electrode material of ultracapacitor.Additionally, prepared carbonaceous material
In material, the nitrogen element of doping can reduce the work content of carbon skeleton, thus improves its catalysis activity.Therefore, this kind of material is also used as
High-performance catalytic electrode material, promotes the redox reaction of electrode surface electrolyte, can be by electrolysis in ultracapacitor
The fake capacitance contribution of matter significantly improves electrode ensemble specific volume.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the nitrogen-doped carbon material that the embodiment of the present invention 2 prepares；
Fig. 2 is the H at 1mol/L of the electrode obtained by the embodiment of the present invention 1,2,32SO4Cyclic voltammetry curve in electrolyte；
Fig. 3 is that the electrode obtained by the embodiment of the present invention 2 is containing 0.025mol/L, 0.05mol/L, 0.075mol/L neighbour's benzene two
The H of the 1mol/L of phenol2SO4Cyclic voltammetry curve in electrolyte；
Fig. 4 is the scanning electron microscope (SEM) photograph of the nitrogen-doped carbon material that the embodiment of the present invention 4 prepares.
Detailed description of the invention
By the following examples the foregoing of the present invention is described in further details, but this should be interpreted as this
The scope inventing above-mentioned theme is only limitted to below example, and all technology realized based on foregoing of the present invention belong to this
Bright scope.
Embodiment 1
Preparation molar concentration is the hydrochloric acid solution of 1mol/L, adds 0.2mL aniline monomer after taking the cooling of 100mL hydrochloric acid solution ice bath
Obtain solution A, add 0.12g Ammonium persulfate. after separately taking the cooling of 100mL hydrochloric acid solution ice bath and obtain solution B；1mg carbonoxide is received
Mitron ultrasonic disperse forms suspension in 1mL deionized water, is joined by this suspension in solution A and stirs under condition of ice bath
10min obtains solution C, then solution B is joined and stirs 2min formation uniform dispersion in solution C；By one piece of a size of 1cm
The tripolycyanamide sponge of × 2cm × 3cm is put in above-mentioned uniform dispersion, is subsequently placed under condition of ice bath reaction 24h, at trimerization
In cyanamide sponge hole formed deposition polyaniline oxide/carbon nanometer tube, then with deionized water rinsing to flushing liquor be colourless obtain green
The tripolycyanamide sponge of color；Green tripolycyanamide sponge is put in baking oven and dries, be subsequently placed in tube furnace at nitrogen gas
Atmosphere obtains nitrogen-doped carbon material in 600 DEG C of calcining 2h.
It is 80:15:5 by synthesized nitrogen-doped carbon material and acetylene black and polyvinylidene fluoride binding agent according to mass ratio
Ratio make slurry, be evenly coated in rustless steel collection liquid surface formed active area be 1cm2Electrode, Fig. 2 is that this electrode exists
Three-electrode system is tested the electrode H at 1mol/L2SO4Cyclic voltammetry curve in electrolyte, it can be seen that this electrode mainly in
Revealing electric double layer capacitance feature, this electrode specific volume under 1A/g electric current density is 136F/g.
Embodiment 2
Preparation molar concentration is the hydrochloric acid solution of 1mol/L, adds 0.2mL aniline monomer after taking the cooling of 100mL hydrochloric acid solution ice bath
Obtain solution A, add 0.12g Ammonium persulfate. after separately taking the cooling of 100mL hydrochloric acid solution ice bath and obtain solution B；1mg carbonoxide is received
Mitron ultrasonic disperse forms suspension in 1mL deionized water, is joined by this suspension in solution A and stirs under condition of ice bath
10min obtains solution C, then solution B is joined and stirs 2min formation uniform dispersion in solution C；By one piece of a size of 1cm
The tripolycyanamide sponge of × 2cm × 3cm is put in above-mentioned uniform dispersion, is subsequently placed under condition of ice bath reaction 48h, at trimerization
In cyanamide sponge hole formed deposition polyaniline oxide/carbon nanometer tube, then with deionized water rinsing to flushing liquor be colourless obtain green
The tripolycyanamide sponge of color；Green tripolycyanamide sponge is put in baking oven and dries, be subsequently placed in tube furnace at nitrogen gas
Atmosphere obtains nitrogen-doped carbon material in 800 DEG C of calcining 2h, as it is shown in figure 1, this nitrogen-doped carbon material to have special crosslinking empty spherical
Structure.
Synthesized nitrogen-doped carbon material is assembled three electrode test systems by embodiment 1, can from Fig. 2 cyclic voltammetry curve
To find out, this electrode mainly presents electric double layer capacitance feature, and this electrode is the H of 1mol/L under 1A/g electric current density2SO4Electrolysis
Specific volume under the conditions of matter is 304F/g.Meanwhile, at H2SO4Electrolyte introduces the catechol redox active of variable concentrations
Composition, electrode is obviously promoted effect (Fig. 3) to the redox reaction of catechol, when in electrolyte, catechol concentration is
During 0.05mol/L, catechol is provided that maximum fake capacitance, can improve nitrogen-doped carbon electrode specific volume to 403F/g.
Embodiment 3
Preparation molar concentration is the hydrochloric acid solution of 1mol/L, adds 0.2mL aniline monomer after taking the cooling of 100mL hydrochloric acid solution ice bath
Obtain solution A, add 0.12g Ammonium persulfate. after separately taking the cooling of 100mL hydrochloric acid solution ice bath and obtain solution B；2mg carbonoxide is received
Mitron ultrasonic disperse forms suspension in 1mL deionized water, is joined by this suspension in solution A and stirs under condition of ice bath
10min obtains solution C, then solution B is joined and stirs 2min formation uniform dispersion in solution C；By one piece of a size of 1cm
The tripolycyanamide sponge of × 2cm × 3cm is put in above-mentioned uniform dispersion, is subsequently placed under condition of ice bath reaction 48h, at trimerization
In cyanamide sponge hole formed deposition polyaniline oxide/carbon nanometer tube, then with deionized water rinsing to flushing liquor be colourless obtain green
The tripolycyanamide sponge of color；Green tripolycyanamide sponge is put in baking oven and dries, be subsequently placed in tube furnace at nitrogen gas
Atmosphere obtains nitrogen-doped carbon material in 700 DEG C of calcining 2h.
Synthesized nitrogen-doped carbon material is assembled three electrode test systems by embodiment 1, from the cyclic voltammetry curve of Fig. 2
It can be seen that this electrode mainly presents electric double layer capacitance feature, this electrode specific volume under 1A/g electric current density is 268F/g.
Embodiment 4
Preparation molar concentration is the sulfuric acid solution of 1mol/L, adds 0.2mL aniline monomer after taking the cooling of 100mL sulfuric acid solution ice bath
Obtain solution A, add 0.12g Ammonium persulfate. after separately taking the cooling of 100mL sulfuric acid solution ice bath and obtain solution B；3mg carbonoxide is received
Mitron ultrasonic disperse forms suspension in 1mL deionized water, is joined by this suspension in solution A and stirs under condition of ice bath
10min obtains solution C, then solution B is joined and stirs 2min formation uniform dispersion in solution C；By one piece of a size of 1cm
The tripolycyanamide sponge of × 2cm × 3cm is put in above-mentioned uniform dispersion, is subsequently placed under condition of ice bath reaction 48h, at trimerization
In cyanamide sponge hole formed deposition polyaniline oxide/carbon nanometer tube, then with deionized water rinsing to flushing liquor be colourless obtain green
The tripolycyanamide sponge of color；Green tripolycyanamide sponge is put in baking oven and dries, be subsequently placed in tube furnace at nitrogen gas
Obtaining nitrogen-doped carbon material in 700 DEG C of calcining 2h in atmosphere, as shown in Figure 4, this nitrogen-doped carbon material also presents and embodiment 2 sample
The empty chondritic of special crosslinking as condition, but empty ball content is relatively low.
By embodiment 1, synthesized nitrogen-doped carbon material is assembled three electrode test systems, and this electrode is close at 1A/g electric current
Specific volume under Du is 223F/g.
As can be seen from the above embodiments, the consumption of oxide/carbon nanometer tube and calcination processing temperature are to nitrogen-doped carbon material
Capacitive property has a major impact, and the consumption and the calcining carburizing temperature that control oxide/carbon nanometer tube can obtain optimal capacitance performance, with
Time this kind of nitrogen-doped carbon material can promote that the fake capacitance of redox active material in electrolyte is contributed, significantly improve electrode ratio
Hold.
Embodiment above describes the ultimate principle of the present invention, principal character and advantage, the technical staff of the industry should
Understanding, the present invention is not restricted to the described embodiments, and the simply explanation present invention's described in above-described embodiment and description is former
Reason, under the scope without departing from the principle of the invention, the present invention also has various changes and modifications, and these changes and improvements each fall within
In the scope of protection of the invention.
Claims (2)
1. there is the synthetic method of the empty spherical nitrogen-doped carbon material of special crosslinking, it is characterised in that concretely comprise the following steps:
Step (1), preparation molar concentration is the acid solution of 1mol/L, adds 0.2mL aniline after taking the cooling of 100mL acid solution ice bath
Monomer obtains solution A, adds 0.12g Ammonium persulfate. and obtain solution B after separately taking the cooling of 100mL acid solution ice bath；
Step (2), forms 1-3mg oxide/carbon nanometer tube ultrasonic disperse suspension in 1mL deionized water, is added by this suspension
Enter in solution A, under condition of ice bath, stir 10min and obtain solution C, then solution B is joined stirring 2min shape in solution C
Uniformly dispersion liquid；
Step (3), puts in above-mentioned uniform dispersion by the tripolycyanamide sponge of one piece of a size of 1cm × 2cm × 3cm, then
It is placed under condition of ice bath reaction 24-48h, in tripolycyanamide sponge hole, forms the oxide/carbon nanometer tube of deposition polyaniline, then use
Deionized water rinsing to flushing liquor is the colourless tripolycyanamide sponge obtaining green；
Step (4), puts into green tripolycyanamide sponge in baking oven and dries, be subsequently placed in tube furnace in nitrogen atmosphere in
600-800 DEG C of calcining 1-2h obtains having the empty spherical nitrogen-doped carbon material of special crosslinking.
The synthetic method with the empty spherical nitrogen-doped carbon material of special crosslinking the most according to claim 1, it is characterised in that:
Acid solution described in step (1) is sulfuric acid solution or hydrochloric acid solution.
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Cited By (12)
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| CN106892416A (en) * | 2017-03-07 | 2017-06-27 | 中国科学院上海高等研究院 | Nitrogen-doped carbon material with high nitrogen-containing and preparation method and application |
| CN107686105A (en) * | 2017-09-07 | 2018-02-13 | 太原理工大学 | A kind of efficiently preparation method of nitrogen-doped carbon nanometer pipe and its application of nitrogen-doped carbon nanometer pipe |
| CN107895786A (en) * | 2017-11-15 | 2018-04-10 | 晋中学院 | Flexible self-supporting SnS/ carbon foam composites and its preparation method and application |
| CN109167074A (en) * | 2018-08-08 | 2019-01-08 | 东华大学 | The nitrogen-doped carbon nanocomposite of hollow additive Mn cobalt oxide nickel coated and preparation |
| CN109360992A (en) * | 2018-10-23 | 2019-02-19 | 青岛科技大学 | A kind of metal-nitrogen-carbon nanosheet preparation method and application of three-dimensional continuous carbon skeleton adulteration |
| CN110148753A (en) * | 2019-05-22 | 2019-08-20 | 佛山科学技术学院 | A kind of Magnesium ion battery baseband processing method and Magnesium ion battery |
| CN110858651A (en) * | 2018-08-24 | 2020-03-03 | 清华大学 | Carbon nanotube composite structure and preparation method thereof |
| CN110980719A (en) * | 2019-12-12 | 2020-04-10 | 太原科技大学 | Preparation method of porous graphitized hollow carbon microspheres |
| CN112397320A (en) * | 2020-11-06 | 2021-02-23 | 大连理工大学 | Nitrogen-doped hierarchical pore integral carbon material applied to supercapacitor and preparation method thereof |
| CN112607735A (en) * | 2020-11-30 | 2021-04-06 | 河北大学 | Nitrogen/sulfur co-doped porous carbon material and preparation method and application thereof |
| CN114618555A (en) * | 2022-03-24 | 2022-06-14 | 大连理工大学 | Integral modified foam nano carbon-based catalyst and preparation method and application thereof |
| CN114852997A (en) * | 2022-05-26 | 2022-08-05 | 陕西科技大学 | Three-dimensional carbon nanotube-mesoporous carbon composite sponge, and preparation method and application thereof |
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| CN106892416A (en) * | 2017-03-07 | 2017-06-27 | 中国科学院上海高等研究院 | Nitrogen-doped carbon material with high nitrogen-containing and preparation method and application |
| CN107686105A (en) * | 2017-09-07 | 2018-02-13 | 太原理工大学 | A kind of efficiently preparation method of nitrogen-doped carbon nanometer pipe and its application of nitrogen-doped carbon nanometer pipe |
| CN107686105B (en) * | 2017-09-07 | 2020-03-27 | 太原理工大学 | Preparation method of high-efficiency nitrogen-doped carbon nano tube and application of nitrogen-doped carbon nano tube |
| CN107895786A (en) * | 2017-11-15 | 2018-04-10 | 晋中学院 | Flexible self-supporting SnS/ carbon foam composites and its preparation method and application |
| CN107895786B (en) * | 2017-11-15 | 2021-04-27 | 晋中学院 | Flexible self-supporting SnS/carbon foam composite material and preparation method and application thereof |
| CN109167074A (en) * | 2018-08-08 | 2019-01-08 | 东华大学 | The nitrogen-doped carbon nanocomposite of hollow additive Mn cobalt oxide nickel coated and preparation |
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| CN110148753A (en) * | 2019-05-22 | 2019-08-20 | 佛山科学技术学院 | A kind of Magnesium ion battery baseband processing method and Magnesium ion battery |
| CN110980719A (en) * | 2019-12-12 | 2020-04-10 | 太原科技大学 | Preparation method of porous graphitized hollow carbon microspheres |
| CN110980719B (en) * | 2019-12-12 | 2023-02-03 | 太原科技大学 | Preparation method of porous graphitized hollow carbon microspheres |
| CN112397320A (en) * | 2020-11-06 | 2021-02-23 | 大连理工大学 | Nitrogen-doped hierarchical pore integral carbon material applied to supercapacitor and preparation method thereof |
| CN112397320B (en) * | 2020-11-06 | 2022-02-15 | 大连理工大学 | Nitrogen-doped hierarchical pore integral carbon material applied to supercapacitor and preparation method thereof |
| CN112607735A (en) * | 2020-11-30 | 2021-04-06 | 河北大学 | Nitrogen/sulfur co-doped porous carbon material and preparation method and application thereof |
| CN114618555A (en) * | 2022-03-24 | 2022-06-14 | 大连理工大学 | Integral modified foam nano carbon-based catalyst and preparation method and application thereof |
| CN114852997A (en) * | 2022-05-26 | 2022-08-05 | 陕西科技大学 | Three-dimensional carbon nanotube-mesoporous carbon composite sponge, and preparation method and application thereof |
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