CN106847552B - A kind of Fe3O4/C3N4 composite material and preparation method - Google Patents
A kind of Fe3O4/C3N4 composite material and preparation method Download PDFInfo
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- CN106847552B CN106847552B CN201611022775.4A CN201611022775A CN106847552B CN 106847552 B CN106847552 B CN 106847552B CN 201611022775 A CN201611022775 A CN 201611022775A CN 106847552 B CN106847552 B CN 106847552B
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of Fe3O4Nanometer rods/graphite mould C3N4Functional composite material and preparation method thereof just prepares g-C by dinectly bruning first3N4, then composite material synthesized by one step hydro thermal method, there is very high commercial viability.Wherein Fe3O4Nanorod diameter is 50nm, is evenly distributed in sheet g-C3N4Surface shows good chemical property, and the application for 1D/3D material in energy storage field has some reference value.The advantage of the invention is that cost is relatively low, preparation process is simple, environmental-friendly pollution-free, can quantify to produce.Prepared Fe3O4Nanometer rods/g-C3N4Functional composite material shows good chemical property, has very big application prospect in the energy storage devices such as supercapacitor and electrode material field.
Description
Technical field
The present invention relates to a kind of Fe3O4Nanometer rods/graphite mould C3N4(g-C3N4) functional composite material preparation method and its
Application in energy storage field.Fe has been prepared by simple one step of hydro-thermal method3O4Nanometer rods/g-C3N4Function and service material
Material.This method preparation step is simple, possesses good chemical property, as supercapacitor, the electrode material of lithium ion battery
Material has good application prospect in new energy storage device field.
Background technique
With scientific development and technological progress, people require higher and higher, supercapacitor conduct to energy storage device
A kind of novel energy storage device possesses high energy density and power density, receives more and more attention, but its property
Can be still greatly improved space.And electrode material is the main factor for determining performance of the supercapacitor, therefore big at present
Quantifier elimination person is dedicated to improving the performance of electrode material.
Electrode material for super capacitor mainly has carbon material, metal oxide and conducting polymer.Carbon material is using illegally
It draws the electrostatic process to provide electric double layer capacitance, possesses the advantages that specific surface area is high, conductivity is high, cycle life is high, cause wide
General concern and research.But its contact situation with electrolyte is to be improved, and electrode material is contacted with the effective of electrolyte
The effective ratio area of material will be increased, and then improve the chemical property of electrode material.g-C3N4As a kind of novel class stone
Electrode ink material possesses unique structure and good chemical stability, while nitrogen-atoms can be effectively improved electrode material and exist
Wetability in electrolyte starts to receive more and more attention.
Metal oxide provides fake capacitance by the redox reaction of surface Rapid reversible, can significantly improve material
Capacitance.But its intrinsic resistance is high, and biggish volume change is possessed in prolonged charge and discharge process, affects its machine
Tool performance and cyclical stability.
g-C3N4Since its conductivity is lower, specific surface area is smaller, electrochemistry when separately as electrode material for super capacitor
Performance is poor.By with Fe3O4Nanometer rods are compound, form 1D/3D composite material, can efficiently against the inherent shortcoming of the two,
The capacitance of reinforcing material improves the chemical property of material.
Summary of the invention
The object of the present invention is to provide a kind of good 1D/3D composite material patterns of complex form.By this pattern, change
Kind g-C3N4Lower specific capacity and Fe3O4The stability poor caused by biggish volume change in charge and discharge process,
Improve the chemical property of material.
Fe in the present invention3O4Nanometer rods/g-C3N4Composite material has stable structure.Fe3O4Nanorod diameter is
50nm is dispersed in g-C3N4Sheet surfaces.As shown in Figure 1.
Fe in the present invention3O4Nanometer rods/g-C3N4Composite material is compared to g-C3N4Monomer, chemical property significantly mention
It rises.Constant current charge-discharge test when by voltage range be -0.8-0.2V, current density is 1.0A/g, it can be found that 1D/3D
The chemical property of composite material is significantly higher than g-C3N4Monomer.As shown in Figure 2.Realize the technical scheme adopted by the invention is as follows:
A kind of Fe3O4Nanometer rods/g-C3N4Functional composite material is made by one step hydro thermal method, has simple process, low in cost, green
The advantages that color is pollution-free, gained Fe3O4Nanometer rods are evenly distributed on g-C3N4Sheet surfaces, and show excellent electrochemistry
Performance, preparation step are as follows:
(1) urea is placed in calcining vessel, is calcined in air, heating rate is 5 DEG C/min, and calcination temperature is
550 DEG C, calcination time 4h, cooled to room temperature.
(2) calcined product is ground, carries out ultrasound in deionized water, ultrasonic time 2h is allowed to disperse in water
It is even, form g-C3N4Suspension.
(3) in g-C3N4FeCl is added in suspension3·6H2O and L-AA, magnetic agitation at room temperature, then slowly
NaHCO is added3, gained mixture is transferred in reaction kettle after stirring, reacts 6h at 150 DEG C.
Further, g-C3N4、FeCl3·6H2O, L-AA and NaHCO3Mass ratio be 2000:3548:440:
3308, g-C3N4The concentration of suspension is 2.22g/L, FeCl3·6H2The concentration of O is
3.94g/L, the concentration of L-AA are 0.49g/L, NaHCO3Concentration be 3.68g/L.
Further, the time of magnetic agitation is 1h.
Further, mixing time 5min.
(4) it takes out and is cooled to room temperature after reaction, with deionized water and ethyl alcohol centrifuge washing, and in a vacuum drying oven
It is dry.The test of gained sample magnet is magnetic, and illustrates Fe3O4With g-C3N4It is compound.
Compared with prior art, the present invention by reducing FeCl3·6H2O, L-AA and NaHCO3Concentration so that
Fe in composite material3O4Pattern nanometer rods are become by nano particle, this is primarily due in nucleation process, material concentration
Reduction can make seed crystal concentration reduction, each seed crystal has more fully space next life long crystal, so that Fe3O4Microcosmic shape
Looks have become nanometer rods from nano particle.Nanorod structure can effectively improve the transmittability of electronics in the composite, change
The kind nano particle insufficient defect of electric conductivity in the composite, to improve the chemical property of composite material.
Detailed description of the invention
Fig. 1 is Fe3O4Nanometer rods/g-C3N4The scanning electron microscope (SEM) photograph of composite material.
Fig. 2 is Fe3O4Nanometer rods/g-C3N4Composite material and g-C3N4Constant current of the monomer when current density is 1.0A/g
Charge and discharge comparison diagram.
Specific embodiment
Embodiment of the present invention is a kind of simple process, low in cost, environmentally protective one step hydro thermal method, is prepared
Fe3O4Nanometer rods/g-C3N4Composite material, the compound shape characteristic with 1D/3D, improves the chemical property of material.
Fe in the present invention3O4Nanometer rods/g-C3N4Composite material has good chemical property.Pass through voltage range
Constant current charge-discharge test when for -0.8-0.2V, current density being 1.0A/g, it can be found that the electrification of 1D/2D composite material
It learns performance and is significantly higher than g-C3N4Monomer.
Excellent in design chemical property Fe of the present invention3O4Nanometer rods/g-C3N4The preparation side of composite material functional composite material
Method, comprising the following steps:
(1) 10g urea is placed in calcining vessel, is calcined in air, heating rate is 5 DEG C/min, calcining temperature
Degree is 550 DEG C, calcination time 4h, cooled to room temperature.
(2) calcined product is ground, weighs 0.2g, ultrasound is carried out in 30mL deionized water, ultrasonic time 2h is allowed to
It is uniformly dispersed in water.
(3) in g-C3N40.3548g FeCl is added in suspension3·6H2O and 0.044g L-AA, at room temperature
Magnetic agitation 1h is slow added into 0.3308g NaHCO3, stir 5min.Gained mixture is transferred in 125mL reaction kettle,
6h is reacted at 150 DEG C.
(4) it takes out and is cooled to room temperature after reaction, with deionized water and ethyl alcohol centrifuge washing, and in a vacuum drying oven
It is dry.
Claims (5)
1. a kind of Fe3O4/C3N4The preparation method of composite material, it is characterised in that: in g-C3N4FeCl is added in suspension3·
6H2O and L-AA, magnetic agitation, is slow added into NaHCO at room temperature3, gained mixture is transferred to instead after stirring
It answers in kettle, 6h is reacted at 150 DEG C, take out be cooled to room temperature after reaction, with deionized water and ethyl alcohol centrifuge washing, and
It is dry in vacuum oven；By reducing FeCl3·6H2O, L-AA and NaHCO3Concentration so that in composite material
Fe3O4Pattern nanometer rods are become by nano particle, the reduction of material concentration can make the reduction of seed crystal concentration, each seed crystal
There is more fully space next life long crystal, so that Fe3O4Microscopic appearance nanometer rods have been become from nano particle；Nanorod structure
It can effectively improve the transmittability of electronics in the composite, improving nano particle, electric conductivity is insufficient scarce in the composite
It falls into, to improve the chemical property of composite material；The g-C3N4、FeCl3·6H2O, L-AA and NaHCO3Matter
Amount is than being 2000:3548:440:3308, g-C3N4The concentration of suspension is 2.22g/L, FeCl3·6H2The concentration of O is 3.94g/
L, the concentration of L-AA are 0.49g/L, NaHCO3Concentration be 3.68g/L.
2. a kind of Fe as described in claim 13O4/C3N4The preparation method of composite material, it is characterised in that: magnetic agitation when
Between be 1h.
3. a kind of Fe as described in claim 13O4/C3N4The preparation method of composite material, it is characterised in that: mixing time is
5min。
4. a kind of Fe as described in claim 13O4/C3N4The preparation method of composite material, it is characterised in that: the Fe3O4/
C3N4Composite material, Fe3O4Nanorod diameter is 50nm, is dispersed in g-C3N4Sheet surfaces.
5. the Fe of preparation method preparation as described in claim 13O4/C3N4Composite material is used for the use of electrode material for super capacitor
On the way.
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| CN110429246B (en) * | 2019-06-26 | 2022-06-07 | 合肥国轩高科动力能源有限公司 | alpha-Fe uniformly coated by graphite-like phase carbon nitride2O3Material, and preparation method and application thereof |
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