CN101572191A - V2O5-ordered mesoporous carbon composite material and preparation method thereof - Google Patents
V2O5-ordered mesoporous carbon composite material and preparation method thereof Download PDFInfo
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- CN101572191A CN101572191A CNA2009100625242A CN200910062524A CN101572191A CN 101572191 A CN101572191 A CN 101572191A CN A2009100625242 A CNA2009100625242 A CN A2009100625242A CN 200910062524 A CN200910062524 A CN 200910062524A CN 101572191 A CN101572191 A CN 101572191A
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- mesoporous carbon
- ordered mesoporous
- composite material
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- carbon carrier
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Abstract
The invention discloses a V2O5-ordered mesoporous carbon composite material and a preparation method thereof. The V2O5-ordered mesoporous carbon composite material has a mesoporous structure, the V2O5 nano grain size is even, the nano grains are evenly scattered in an ordered mesoporous carbon carrier, the size of the V2O5 grains is 4 nanometers or less in nano scale, and the ratio of the ordered mesoporous carbon carrier to the V2O5 nano grains is 1:0.08-0.25. The method comprises the following steps: firstly, carrying out hydrophilic treatment for the ordered mesoporous carbon carrier, and then evenly scattering vanadium oxide precursor liquid into pore canals of the mesoporous carbon carrier under ultrasonic condition; and filtering and washing the mesoporous carbon carrier, and drying the mesoporous carbon carrier in vacuum at 120 DEG C to form the V2O5-ordered mesoporous carbon composite material. The prepared V2O5-ordered mesoporous carbon composite material shows that the discharge specific capacitance of the composite material is large and the stability is good in the charge/discharge research on cyclic volt-ampere and constant current of a three-electrode system. The method has the advantages of simple process and low requirement on equipment, can be realized under normal temperature, and has strong operability. Therefore, the composite material and the method can be widely applied to the aspects of electrode materials.
Description
Technical field
The invention belongs to nano material and field of nanometer technology, be specifically related to a kind of by the synthetic V of ultrasonic auxiliary liquid phase method
2O
5The new method of-ordered mesoporous carbon composite material.
Background technology
Ultracapacitor is the novel energy-storing device between ordinary capacitor and secondary cell, has both the high and high advantage of secondary cell energy density of ordinary capacitor power density, is the new green power of paying close attention to both at home and abroad in recent years.Usually, electrochemical capacitor can be divided into two kinds by energy storage mechanism: a kind of electrode/electrolyte interface charge that is based on is separated the electric double layer capacitance that is produced, and another is to utilize the surface of electrode and the middle mutually quick reversible redox reaction that takes place of body to form Faraday pseudo-capacitance.
At present, the double layer capacitor absorbent charcoal material, usually needing employing to activate engineering increases its specific area, and the specific area practical efficiency of this type of material with carbon element only is about 10%; In addition, it has higher resistance, has limited the application of double layer capacitor.Metal oxide is as RuO
x, IrO
x, TaO
xDeng performance with fake capacitance, though have bigger than electric capacity, energy density is high and characteristics that can fast charging and discharging, the specific area of metal oxide is less, unstable properties, and its high price has limited their commercialization.Therefore, need to be with double layer capacitor and the combination of fake capacitance device, in the hope of realizing the reasonable balance between material cost and the performance.
Vanadium is one of typical polyvalent metal element, can form many oxide, such as VO
2, V
2O
5, V
6O
13Deng.As far back as 1976, people were just to V
2O
5Study as anode material for lithium-ion batteries, but just come into one's own in recent years used as the research of electrode material for super capacitor.Jiang etc. pass through the chemical gaseous phase injection method with RuO
2XH
2O and mesoporous carbon are compound, and it is than the single porous carbon materials of capacity ratio be significantly increased (J.Power Sources 2003,123,79).But the problem that metal oxide particle is assembled appears in traditional infusion process easily.In addition, V
2O
5Fusing point lower and active higher, the high temperature such as chemical gaseous phase injection are processed and to be easy to cause structure to cave in and phase transition.Thereby select meso-porous carbon material as carrier, it is good, low-cost and preparation method that oxide can be evenly distributed in the carrier is significant to study a kind of controllability.
Summary of the invention
Purpose of the present invention aims to provide a kind of V
2O
5-ordered mesoporous carbon composite material, and provide a kind of implement effective, feasible, the preparation method of barium oxide-ordered mesoporous carbon composite material that mesoscopic structure remains intact.
Realize a kind of V of the object of the invention
2O
5-ordered mesoporous carbon composite material is characterized in that having mesoscopic structure, V
2O
5The nanoparticle size homogeneous, and be evenly dispersed in the phosphorus-ordered mesoporous carbon carrier V
2O
5Particle is of a size of 4nm or littler nano particle, phosphorus-ordered mesoporous carbon carrier and V
2O
5The mass fraction ratio of nano particle is 1: 0.08-0.25.
A kind of V of the present invention
2O
5The preparation method of-ordered mesoporous carbon composite material, be characterized in utilizing ultrasonic auxiliary liquid phase synthesizing method, the steps include: at room temperature, with phosphorus-ordered mesoporous carbon carrier material and barium oxide predecessor mix and blend, under ultrasound condition, process 1-3h then, filter, wash to filtrate colourlessly with deionized water, obtain the pitchy product; The pitchy product that obtains at 120 ℃ of vacuum drying 24h, is namely obtained V
2O
5-ordered mesoporous carbon composite material, V
2O
5Nano particle is evenly dispersed in the phosphorus-ordered mesoporous carbon carrier, and wherein, described barium oxide predecessor is V
2O
5Colloidal sol, concentration are 0.01-0.08mol/L; Phosphorus-ordered mesoporous carbon carrier and V
2O
5Colloidal sol is example 1 in mass ratio: 50-150 mixes.
In the method for the present invention, the self-control ordered mesoporous carbon material CMK-3 that described phosphorus-ordered mesoporous carbon carrier material is a hydrophilic treated (embodiment 5,6 is seen in its preparation); Described ultrasonic power is 100kHz.
This method has solved supported V in the mesoporous carbon carrier
2O
5The nano particle hard problem, the barium oxide predecessor enters in the duct of phosphorus-ordered mesoporous carbon carrier by ultrasonic assisting, and is uniformly dispersed, and the duct keeps relatively complete in order, has obtained V
2O
5The equally distributed V of nano particle
2O
5-ordered mesoporous carbon composite material.Its V
2O
5Particle is of a size of 4nm or littler nano particle.
The surface hydrophilic functionalization method of ordered mesopore carbon: with ordered mesopore carbon CMK-3 and 20wt%HNO
3Mix, mixed liquor is moved in the inner liner of reaction kettle of polytetrafluoroethylene hydro-thermal reaction 3h in 80 ℃ of baking ovens.Naturally cooling is filtered, and to neutral, 80 ℃ of oven dryings finally obtain the ordered mesopore carbon CMK-3 carrier of hydrophile function processing with the deionized water washing.
V of the present invention
2O
5-ordered mesoporous carbon composite material is particularly suitable as capacitor electrode material.
The present invention is by introducing object oxide V in the phosphorus-ordered mesoporous carbon carrier material
2O
5, form a kind of special construction, be intended to utilize effective proportioning of super large specific energy and the electric double layer capacitance of metal oxide, by electric double layer capacitance and Faraday pseudo-capacitance acting in conjunction, obtain high specific energy.Preparation technology of the present invention is simple, and is low for equipment requirements, and operability is good, and greatly reduces cost; Especially for the metal oxide of this class low melting point of barium oxide, multivalence attitude, just can realize that under lower temperature it is compound, structural deterioration and the variation of valence of having avoided high-temperature process to cause.
The V of the present invention's preparation
2O
5-ordered mesoporous carbon composite material studies show that at cyclic voltammetry and the constant current charge-discharge of three-electrode system, compares V with only using ordered mesopore carbon as electrode
2O
5The capacitive property of-ordered mesoporous carbon composite material electrode obviously improves, and stability better.
Description of drawings
Fig. 1 is the low angle XRD figure spectrum of embodiment 1 product
Fig. 2 is the wide-angle XRD figure spectrum of embodiment 1 product
Fig. 3 is the V 2p xps energy spectrum of embodiment 1 product
Fig. 4 is the TEM image of embodiment 1 product
Fig. 5 is the TEM image of CMK-3
Fig. 6 is the feature nitrogen adsorption-desorption isotherm of embodiment 1 product
Fig. 7 is the graph of pore diameter distribution of embodiment 1 product
Fig. 8 be embodiment 1 product as electrode at 1mol/L KNO
3Cyclic voltammetry curve in the solution
V shown in Figure 1
2O
5(100) face of the corresponding two-dimentional hexagonal structure in the position of the diffraction maximum of the low angle XRD collection of illustrative plates of-ordered mesoporous carbon composite material, with bibliographical information (Ryoo etc., J.Am.Chem.Soc.2000,122, the low angle XRD collection of illustrative plates of ordered mesoporous material 10712) matches, and shows that product has orderly meso-hole structure.
V shown in Figure 2
2O
5The corresponding orthohormbic structure V in the position of the diffraction maximum of the wide-angle XRD collection of illustrative plates of-ordered mesoporous carbon composite material
2O
5(101) and (002) peak, show that barium oxide in the composite is with V
2O
5Form exist; The intensity of diffraction maximum a little less than, show that the barium oxide particle size is littler, degree of crystallinity is not high.
V shown in Figure 3
2O
5The V 2p xps energy spectrum of-ordered mesoporous carbon composite material confirms that further barium oxide is V
2O
5
Fig. 4 illustrates V
2O
5Nano particle is evenly dispersed in the phosphorus-ordered mesoporous carbon carrier, V
2O
5The size of nano particle is about 4nm.
Fig. 5 illustrates that phosphorus-ordered mesoporous carbon carrier CMK-3 has that rule is arranged, the pore passage structure of size homogeneous.
Fig. 6 illustrates that product has the suction dissolubility indicatrix of typical mesoporous material.
Fig. 7 illustrates the narrow pore size distribution range of product.
Fig. 8 illustrates that the fake capacitance feature of product is comparatively obvious, shows that in the potential window scope, faraday's reaction has taken place for product and electrolyte, is wherein comprising a plurality of oxidation-reduction pairs continuous, reversible conversion.
Embodiment
V of the present invention
2O
5The preparation method of-ordered mesoporous carbon composite material, to utilize ultrasonic auxiliary liquid phase synthesizing method, the steps include: at room temperature, with phosphorus-ordered mesoporous carbon carrier material and barium oxide predecessor mix and blend, under ultrasound condition, process 1-3h then, filter, wash to filtrate colourlessly with deionized water, obtain the pitchy product; The pitchy product that obtains at 120 ℃ of vacuum drying 24h, is namely obtained V
2O
5-ordered mesoporous carbon composite material, wherein, described barium oxide predecessor is V
2O
5Colloidal sol, concentration are 0.01-0.08mol/L; Phosphorus-ordered mesoporous carbon carrier and V
2O
5Colloidal sol is example 1 in mass ratio: 50-150 mixes.
Embodiment 1
V
2O
5A preferred embodiment among the preparation method of-ordered mesoporous carbon composite material comprises the steps: V
2O
5Be 0.06mol/L V
2O
5Colloidal sol, phosphorus-ordered mesoporous carbon carrier are the CMK-3 of hydrophile function processing.At room temperature, 0.2g CMK-3 is joined 20g V
2O
5In the colloidal sol, stirring 3h, is ultrasonic processing 3h under the 100kHz at power then, filter, and washing, 120 ℃ of vacuum drying 24h obtain V
2O
5-ordered mesoporous carbon composite material.The low angle XRD figure spectrum of product is seen Fig. 1, and wide-angle XRD figure spectrum is seen Fig. 2, and V 2p xps energy spectrum is seen Fig. 3, TEM image such as Fig. 4, and feature nitrogen adsorption-desorption isotherm such as Fig. 6 of product, graph of pore diameter distribution is seen Fig. 7.
V
2O
5The preparation of-ordered mesoporous carbon composite material: V
2O
5Be 0.01mol/L V
2O
5Colloidal sol, phosphorus-ordered mesoporous carbon carrier are the CMK-3 of hydrophile function processing.At room temperature, 0.2g CMK-3 is joined 10g V
2O
5In the colloidal sol, stirring 3h, is ultrasonic processing 1h under the 100kHz at power then, filter, and washing, 120 ℃ of vacuum drying 24h obtain V
2O
5-ordered mesoporous carbon composite material.
Embodiment 3
V
2O
5The preparation of-ordered mesoporous carbon composite material: V
2O
5Be 0.08mol/L V
2O
5Colloidal sol, phosphorus-ordered mesoporous carbon carrier are the CMK-3 of hydrophile function processing.At room temperature, 0.2g CMK-3 is joined 30g V
2O
5In the colloidal sol, stirring 3h, is ultrasonic processing 3h under the 100kHz at power then, filter, and washing, 120 ℃ of vacuum drying 24h obtain V
2O
5-ordered mesoporous carbon composite material.
V
2O
5Synthesizing of colloidal sol: with 0.545g V
2O
5With 50mL H
2O
2Join in the 100mL round-bottomed flask, whole system remains on strong magnetic agitation in the ice bath, has become a kind of bright orange solution (system pH=1.5) behind about 20min, and behind the 24h, system changes generation rufous colloidal sol gradually, is V
2O
5Colloidal sol.The V of the configurable variable concentrations of this method
2O
5Colloidal sol.Used in the example 1 is the V of 0.06mol/L
2O
5Colloidal sol.
Embodiment 5
Ordered mesopore carbon CMK-3's is synthetic: 1g mesopore silicon oxide SBA-15 joins in the vitriolated aqueous sucrose solution (pressing 1.25g sucrose, 0.2g sulfuric acid and the preparation of 5g water), stirs.Mixture is placed in the drying box, 50 ℃ of insulation 12h, and subsequently, temperature rises to 160 ℃ of insulation 6h.Increase 0.75g sucrose, 0.1g sulfuric acid and 5g water take place to stir in the partially polymerized silica sample to sucrose, carry out same treatment under 50 ℃ and 160 ℃ in drying box.Speed with 250 ℃/h rises to 900 ℃ of insulation 6h under nitrogen protection atmosphere then, finishes whole carbonisation.Gained silicon/carbon dioxide combination product is removed template with the HF acid solution dipping of 8wt%.End product after filtration, deionized water is washed till neutrality, 100 ℃ of dryings obtain ordered mesopore carbon CMK-3, its TEM image is seen Fig. 5.The preparation of mesopore silicon oxide SBA-15 is referring to document (D.Y.Zhao etc., Science 1998,279,548).
The surface hydrophilic functionalization of ordered mesopore carbon: with the ordered mesopore carbon CMK-3 and the 20wt%HNO of embodiment 5 preparations
3Mix, mixed liquor is moved in the inner liner of reaction kettle of polytetrafluoroethylene hydro-thermal reaction 3h in 80 ℃ of baking ovens.Naturally cooling is filtered, and to neutral, 80 ℃ of oven dryings finally obtain the phosphorus-ordered mesoporous carbon carrier of hydrophile function processing with the deionized water washing.
Embodiment 7
The preparation of electrode: the mass ratio by 90: 10 takes by weighing V
2O
5The polytetrafluoroethylene (PTFE) of-ordered mesoporous carbon composite material and 12wt% (PTFE) emulsion with the mixed sample of an amount of isopropyl alcohol, after mixing, is dried under the infrared lamp.The oven dry sample is pressed on the nickel foam under the pressure of 10MPa, stand-by in 80 ℃ of vacuumize 24h.The surface area of the electrode slice of making is 1cm
2
Cyclic voltammetric test: be prepared into work electrode according to embodiment 7 with the foregoing description 1 product, saturated calomel electrode is as reference electrode, platinum electrode is formed the standard three-electrode system as to electrode, carries out the cyclic voltammetric test on Autolab PGATAT30 type electrochemical workstation.Fig. 8 is presented at the KNO of 1mol/L
3In the electrolyte, voltage scan range 0-0.8V, sweep speed is the following 20 times cyclic voltammetry curve of 5mV/s condition.
Embodiment 9
The constant current charge-discharge test: the constant current charge-discharge test is tested on Autolab PGATAT30 type electrochemical workstation, be prepared into work electrode with the foregoing description 1 product according to embodiment 7, saturated calomel electrode is as reference electrode, and platinum electrode is formed the standard three-electrode system as to electrode.When current density is got 0.2A/g, potential region 0-0.8V, discharge is 124F/g than electric capacity.
Claims (5)
1. V
2O
5-ordered mesoporous carbon composite material is characterized in that having mesoscopic structure, V
2O
5The nanoparticle size homogeneous, and be evenly dispersed in the phosphorus-ordered mesoporous carbon carrier V
2O
5Particle is of a size of 4nm or littler nano particle, phosphorus-ordered mesoporous carbon carrier and V
2O
5The mass fraction ratio of nano particle is 1: 0.08-0.25.
2. V
2O
5The preparation method of-ordered mesoporous carbon composite material, it is characterized in that utilizing ultrasonic auxiliary liquid phase synthesizing method, the steps include: at room temperature, with phosphorus-ordered mesoporous carbon carrier material and barium oxide predecessor mix and blend, under ultrasound condition, process 1-3h then, filter, wash to filtrate colourlessly with deionized water, obtain the pitchy product; The pitchy product that obtains at 120 ℃ of vacuum drying 24h, is namely obtained V
2O
5-ordered mesoporous carbon composite material, V
2O
5Nano particle is evenly dispersed in the phosphorus-ordered mesoporous carbon carrier, and wherein, described barium oxide predecessor is V
2O
5Colloidal sol, concentration are 0.01-0.08mol/L; Phosphorus-ordered mesoporous carbon carrier and V
2O
5Colloidal sol is example 1 in mass ratio: 50-150 mixes.
3. V according to claim 2
2O
5The preparation method of-ordered mesoporous carbon composite material is characterized in that: phosphorus-ordered mesoporous carbon carrier is the ordered mesoporous carbon material CMK-3 after the hydrophile function processing.
4. V according to claim 2
2O
5The preparation method of-ordered mesoporous carbon composite material is characterized in that: ultrasonic power is 100kHz.
5. the described V of claim 1
2O
5The application of-ordered mesoporous carbon composite material is characterized in that: as capacitor electrode material.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101834006A (en) * | 2010-04-27 | 2010-09-15 | 武汉理工大学 | MoO3 and ordered mesoporous carbon composite electrode material and preparation method thereof |
| CN102631914A (en) * | 2011-02-15 | 2012-08-15 | 中国石油化工股份有限公司 | Vanadium pentoxide catalyst taking mesoporous carbon as carrier, and preparation method thereof |
| CN103258653A (en) * | 2013-04-15 | 2013-08-21 | 武汉理工大学 | Vanadium oxide and carbon composite material with hierarchical pore structure and preparation method thereof |
| CN110391401A (en) * | 2019-06-25 | 2019-10-29 | 肇庆理士电源技术有限公司 | OMC based combined electrode and lead-acid battery |
| CN111584247A (en) * | 2020-05-20 | 2020-08-25 | 璧靛悍 | V-shaped groove2O5Nitrogen-sulfur-loaded double-doped porous carbon supercapacitor electrode material and preparation method thereof |
| CN112233910A (en) * | 2020-10-19 | 2021-01-15 | 成都先进金属材料产业技术研究院有限公司 | Preparation method of nano vanadium dioxide/natural porous carbon electrode material |
-
2009
- 2009-06-05 CN CN2009100625242A patent/CN101572191B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101834006A (en) * | 2010-04-27 | 2010-09-15 | 武汉理工大学 | MoO3 and ordered mesoporous carbon composite electrode material and preparation method thereof |
| CN102631914A (en) * | 2011-02-15 | 2012-08-15 | 中国石油化工股份有限公司 | Vanadium pentoxide catalyst taking mesoporous carbon as carrier, and preparation method thereof |
| CN103258653A (en) * | 2013-04-15 | 2013-08-21 | 武汉理工大学 | Vanadium oxide and carbon composite material with hierarchical pore structure and preparation method thereof |
| CN103258653B (en) * | 2013-04-15 | 2015-12-02 | 武汉理工大学 | There is the barium oxide and carbon composite and preparation method thereof of hierarchical porous structure |
| CN110391401A (en) * | 2019-06-25 | 2019-10-29 | 肇庆理士电源技术有限公司 | OMC based combined electrode and lead-acid battery |
| CN111584247A (en) * | 2020-05-20 | 2020-08-25 | 璧靛悍 | V-shaped groove2O5Nitrogen-sulfur-loaded double-doped porous carbon supercapacitor electrode material and preparation method thereof |
| CN112233910A (en) * | 2020-10-19 | 2021-01-15 | 成都先进金属材料产业技术研究院有限公司 | Preparation method of nano vanadium dioxide/natural porous carbon electrode material |
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