CN108630920A - A kind of nano-metal-oxide/MXene heterojunction structure composite material and preparation methods - Google Patents
A kind of nano-metal-oxide/MXene heterojunction structure composite material and preparation methods Download PDFInfo
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Abstract
The present invention provides a kind of nano-metal-oxide/MXene heterojunction structure composite material and preparation methods.The nano-metal-oxide/MXene heterojunction structure composite materials are that nano-metal-oxide is adsorbed on the surfaces sheet MXene by Van der Waals force and is uniformly dispersed in the integral structure composite material formed in above-mentioned sheet basis material.Wherein, size is that the metal oxide particle of 5 100nm accounts for the 10 90% of composite material gross mass；Nano-metal-oxide is TiO2、SnO2、Fe3O4、RuO2、MnO2One or more of；The pattern of nano-metal-oxide is one or more of nano bar-shape, nanometer threadiness, quantum dot.Nano-metal-oxide is uniformly dispersed on MXene lamellas in nano-metal-oxide/MXene heterojunction structure composite materials of the present invention, regular appearance, ratio is adjustable, significantly improve material electric conductivity, preparation method is simple, cost is relatively low, can prepare on a large scale, has excellent cycle performance and high rate performance for lithium ion battery or ultracapacitor composite material.
Description
Technical field
The present invention relates to a kind of nano-metal-oxide/MXene heterojunction structure composite material and preparation methods.
Background technology
Metal oxide materials have higher specific capacity, usually 2 ~ 3 times higher than porous carbon or graphite-based material, are a kind of
Very promising secondary cell and electrode material for super capacitor.However, logical using electrode material prepared by metal oxide
It is commonly present the deficiencies of conductivity is low, volume expansion is big in charge and discharge process, causes cyclical stability and high rate performance that cannot still expire
The demand of sufficient practical application.By the carbon nano-material of metal oxide and high conductivity（Graphene, carbon nanotube etc.）, porous charcoal
The progress such as material, conducting polymer is compound, is the effective way for improving metal oxide electrochemical performance.
Transition metal carbide or nitride, also referred to as MXene are the New Two Dimensional materials found for the first time for 2011, it
Have the characteristics that the high conductivity of graphene and graphene oxide are hydrophilic, minimum nanometer thickness flexibly adjustable but also with component
The advantages such as controllable, huge potentiality are presented in the application aspect of secondary cell and the electrode material of ultracapacitor.But due to
MXene lamellas are dense, and specific surface area is not high, and specific discharge capacity is relatively low.
In recent years, people have done some effort in terms of the composite material of MXene and metal oxide.MXene has height
Conductivity can make up the low deficiency of metal oxide conductivity, while its unique two-dimensional nanostructure can be used for
Volume expansion of the buffer metal oxide in charge and discharge process, to be expected to through metal oxide and the compound acquisitions of MXene
The combination electrode material of better performances.But in the method for preparing composite material reported at present, film is taken out using simple mixing
Or the preparation effect of the methods of mechanical mix grinding is poor, MXene reunites serious, it is difficult to form evenly dispersed composite construction；And it adopts
Complicated with the preparation process of the methods of CVD method, hydro-thermal method, cost is higher, is also easy to cause the oxidation deterioration of MXene.Therefore, such as
What is uniformly compound to prepare high performance combination electrode material or a challenging difficulty by MXene and metal oxide
Topic.
Invention content
In view of the problems of the existing technology, one of the objects of the present invention is to provide a kind of nano-metal-oxide/
MXene heterojunction structure composite materials, the composite material are acted on by Van der Waals self assembly so that nano-metal-oxide is uniform
MXene sheet surfaces are controllably adsorbed on, so that nano-metal-oxide can buffer it anti-using the lamellar structure of MXene
Volume expansion during answering can provide two-dimentional conductive mesh in addition, MXene has excellent electric conductivity for composite material
Network, and then improve the conductivity of composite material entirety.
The second object of the present invention is to provide that a kind of to prepare above-mentioned nano-metal-oxide/MXene heterojunction structures compound
The method of material.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of nano-metal-oxide/MXene heterojunction structure composite materials, which is characterized in that the nano metal
Oxide/MXene heterojunction structure composite materials are for nano-metal-oxide by Van der Waals force uniform adsorption in sheet MXene
Surface is formed；
The nano-metal-oxide size is in 5-100nm；
The nano-metal-oxide is TiO2、SnO2、Fe3O4、RuO2、MnO2One or more of；
Nano-metal-oxide quality accounting in the nano-metal-oxide/MXene heterojunction structure composite materials is
10-90%。
The pattern of the nano-metal-oxide is one or more of nano bar-shape, nanometer threadiness, quantum dot；
Wherein, the nano-metal-oxide/MXene heterojunction structure composite materials are prepared by the following method to obtain：
（1）With Ti3AlC2For raw material, MXene solution is prepared by etching；
（2）Nano-metal-oxide is dispersed in 500ml organic solvents, nano-metal oxide solution is obtained；
（3）The MXene solution is instilled into step dropwise（2）Described in nano-metal oxide solution；
（4）By step（3）The mixed liquor of gained is ultrasonically treated, and suction filtration obtains the nano-metal-oxide/MXene heterojunction structures
Composite material.
Optionally, the preparation of the MXene solution includes the following steps：
A, 0.99g LiF are added in the plastic bottle equipped with 10ml hydrochloric acid, stir 5min, adds 1 g Ti3AlC2, stirring
Uniformly;
B, the mixed liquor for obtaining step A is placed in 35 DEG C of thermostat water baths, is stirred to react for 24 hours;
C, the solution that step B is obtained is centrifuged plus water operates 4 times repeatedly, until pH value of solution ≈ 6, removes supernatant liquor, ultrasound
30min centrifuges 1h, collects upper solution, the MXene solution after being etched.
Optionally, step（1）Described in MXene solution a concentration of 1-2mg/ml.
Optionally, step（2）Described in organic solvent be NMP（N-Methyl pyrrolidone）、DMF（N, N- dimethyl formyl
Amine）、THF（Tetrahydrofuran）One or more of.
Optionally, step（3）Middle nano-metal-oxide is compound in the nano-metal-oxide/MXene heterojunction structures
Quality accounting is 10-90% in material.
Optionally, step（4）Middle ultrasonic time is 360 ~ 480min, ultrasonic power 40W.
Compared with prior art, this method has the following advantages：
1, the present invention provides a kind of nano-metal-oxide/MXene heterojunction structure composite materials, in the material, using with
The MXene of flexible sheet structure and high conductivity is compound with nano-metal-oxide, prepare with excellent electric conductivity and mostly from
The composite material of sub- transmission channel, to improve the cycle performance and high rate performance of material；
2, the present invention provides a kind of preparation methods of nano-metal-oxide/MXene heterojunction structure composite materials, with metal oxygen
Compound and MXene are raw material, are acted on by Van der Waals self assembly, by the nano metal particles uniform adsorption of nano-metal-oxide
It in two-dimentional MXene sheet surfaces, prevents MXene lamellas from stacking, curling, improves the specific surface area of composite material, increase reaction and live
Property region, while avoid nano-metal-oxide because interface can it is larger there is a phenomenon where reuniting, so that active material utilization is improved；
3, the present invention provides a kind of preparation method of nano-metal-oxide/MXene heterojunction structure composite materials, this method is anti-
Answer that mild condition, reaction time are short, packaging efficiency is high, low energy consumption, are suitable for mass producing；
4, the present invention provides a kind of preparation method of nano-metal-oxide/MXene heterojunction structure composite materials, this method is suitable
Nano-metal-oxide type is more, and pattern is various（Quantum dot, nanometer rods, nano wire）, and nano metal oxide
The mass ratio of object and MXene are controllable.
Description of the drawings
Fig. 1 is TiO prepared by the embodiment of the present invention 12The transmission electron microscopy of/MXene nano-heterogeneous structure composite materials
Mirror（TEM）Figure；
Fig. 2 is TiO prepared by the embodiment of the present invention 12/ MXene nano-heterogeneous structure composite materials are as negative electrode of lithium ion battery
The cycle performance curve graph of material；
Fig. 3 is SnO prepared by the embodiment of the present invention 22The TEM of/MXene nano-heterogeneous structure composite materials schemes；
Fig. 4 is SnO prepared by the embodiment of the present invention 22/ MXene nano-heterogeneous structure composite materials are as negative electrode of lithium ion battery
Material high rate performance figure；
Fig. 5 is Fe prepared by the embodiment of the present invention 33O4The TEM of/MXene nano-heterogeneous structure composite materials schemes；
Fig. 6 is Fe prepared by the embodiment of the present invention 33O4/ MXene nano-heterogeneous structure composite materials are compound as ultracapacitor
Material high rate performance figure.
Specific implementation mode
Further clear complete explanation is done to technical solution provided by the invention below by the mode of specific embodiment,
But they are not construed as limiting the invention.
Embodiment 1
（1）The synthesis of MXene
0.99g LiF are added in the plastic bottle equipped with 10ml hydrochloric acid, 5min is stirred, so that LiF is dissolved, add 1 g
Ti3AlC2, stir evenly.Obtained mixed liquor is placed in 35 DEG C of thermostat water baths, stirring etching is for 24 hours.It will be upper after etching reaction
Stating product adds water, centrifugation to operate 4 times repeatedly, until supernatant liquor pH ≈ 6, remove supernatant liquor, again plus water, ultrasonic 30min, from
Heart 1h collects upper solution, the MXene solution after being etched；
It measures 5ml MXene solution to filter, weigh after drying, a concentration of 2.6mg/ml of MXene is obtained, by prepared MXene water
Solution is diluted to 1 mg/ml；
（2）The synthesis of nano-metal-oxide/MXene heterojunction structure composite materials
Take 70mg nano bar-shapes TiO2In 500ml conical flasks, 500ml NMP, ultrasonic disperse 1h is added,
20ml MXene aqueous solutions are measured, instill TiO dropwise2In dispersion liquid.It is ultrasonically treated 360min, ultrasonic power 40W.It is super
It is filtered after sound and is dried in vacuo 10h and obtain target product；
（3）Material characterization
By TiO2/ MXene nano-heterogeneous structure composite materials carry out characterization test.TEM shows nano bar-shape TiO2It is uniformly distributed
In MXene sheet surfaces.XRD the result shows that, MXene interlamellar spacings increase 1.45nm after self assembly（Fig. 1）；
（3）Performance of lithium ion battery is tested
By above-mentioned material according to active material：Acetylene black：PVDF=80:10:10 ratio be mixed with electrode slice as negative
Pole, polypropylene porous film（Celgard 3501）Diaphragm, electrolyte are 1mol/L LiPF6/EC/DEC（V:V=1:1）Mixing
Solution.Battery is assembled in the glove box full of high-purity argon gas.Constant current charge-discharge test（Voltage range 0.01-3V）Table
Bright, after being recycled 200 times under the current density of 500mA/g, battery capacity is still up to 200mAh/g（Fig. 2）, when current density increases
After adding to 2000mA/g, battery capacity still keeps 138mAh/g, shows that the material has excellent cycle and high rate performance.
Embodiment 2
（1）The synthesis of MXene
0.99g LiF are added in the plastic bottle equipped with 10ml hydrochloric acid, 5min is stirred, so that LiF is dissolved, add 1 g
Ti3AlC2, stir evenly.Obtained mixed liquor is placed in 35 DEG C of thermostat water baths, stirring
Etching is for 24 hours.Water, centrifugation is added to operate 4 times repeatedly above-mentioned product after etching reaction, until supernatant liquor pH ≈ 6, go to upper layer
Clear liquid, again plus water, ultrasonic 30min centrifuge 1h, collect upper solution, the MXene solution after being etched；
It measures 5ml MXene solution to filter, weigh after drying, a concentration of 2.6mg/ml of MXene is obtained, by prepared MXene water
Solution is diluted to 2 mg/ml；
（2）The synthesis of nano-metal-oxide/MXene heterojunction structure composite materials
Take 70mg nanometers of threadiness SnO2In 500ml conical flasks, 500ml DMF, ultrasonic 1h is added,
15ml MXene aqueous solutions are measured, instill SnO dropwise2In dispersion liquid.It is ultrasonically treated 480min, ultrasonic power 40W.It is super
It is filtered after sound and is dried in vacuo 10h and obtain target product；
（3）Material characterization
By SnO2/ MXene nano-heterogeneous structure composite materials carry out characterization test.TEM shows nanometer threadiness SnO2It is uniformly distributed
In MXene sheet surfaces（Fig. 3）.XRD the result shows that, MXene interlamellar spacings increase 1.44nm after self assembly；
（3）Performance of lithium ion battery is tested
By above-mentioned material according to active material：Acetylene black：PVDF=80:10:10 ratio be mixed with electrode slice as negative
Pole, polypropylene porous film（Celgard 3501）Diaphragm, electrolyte are 1mol/L LiPF6/EC/DEC（V:V=1:1）Mixing
Solution.Battery is assembled in the glove box full of high-purity argon gas.Constant current charge-discharge test（Voltage range 0.01-3V）Table
Bright, after being recycled 500 times under the current density of 1000mA/g, battery capacity is still up to 530mAh/g, when current density increases to
After 5000mA/g, battery capacity still keeps 310mAh/g（Fig. 4）, show that the material has excellent cycle performance and forthright again
Energy.
Embodiment 3
（1）The synthesis of MXene
0.99g LiF are added in the plastic bottle equipped with 10ml hydrochloric acid, 5min is stirred, so that LiF is dissolved, add 1 g
Ti3AlC2, stir evenly.Obtained mixed liquor is placed in 35 DEG C of thermostat water baths, stirring etching is for 24 hours.It will be upper after etching reaction
Stating product adds water, centrifugation to operate 4 times repeatedly, until supernatant liquor pH ≈ 6, remove supernatant liquor, again plus water, ultrasonic 30min, from
Heart 1h collects upper solution, the MXene solution after being etched；
It measures 5ml MXene solution to filter, weigh after drying, a concentration of 2.6mg/ml of MXene is obtained, by prepared MXene water
Solution is diluted to 1 mg/ml；
（1）The synthesis of nano-metal-oxide/MXene heterojunction structure composite materials
Take 70mg Fe3O4500ml THF, ultrasonic disperse 1h is added in 500ml conical flasks in quantum dot,
30ml MXene aqueous solutions are measured, instill Fe dropwise3O4In dispersion liquid.It is ultrasonically treated 480min, ultrasonic power 40W,
It is filtered after ultrasound and is dried in vacuo 10h and obtain target product；
（3）Material characterization
By Fe3O4/ MXene nano-heterogeneous structure composite materials carry out characterization test, and TEM shows Fe3O4Quantum dot is evenly distributed on
MXene sheet surfaces（Fig. 5）, XRD the result shows that, MXene interlamellar spacings increase 1.46nm after self assembly；
（3）Capacitive property is tested
By above-mentioned material according to active material：Acetylene black：PTFE=85:10:5 ratio is mixed, and ethyl alcohol is added and stirs and modulates
At pureed, cut-parts are pressed in nickel foam, and electrode of super capacitor is made after dry.Using 6mol/L KOH as electrolyte, saturation is sweet
Mercury electrode is to carry out three electrode constant current charge-discharge tests to electrode.Test shows to recycle 3000 times under the current density of 2A/g
Afterwards, quality specific capacitance is up to 840F/g, current density is extended to 100A/g, capacity retention ratio is 60% or more（Fig. 6）,
Show that the material has excellent cycle performance and high rate performance.
Claims (8)
1. a kind of nano-metal-oxide/MXene heterojunction structure composite materials, which is characterized in that the nano-metal-oxide/
MXene heterojunction structure composite materials are for nano-metal-oxide by Van der Waals force uniform adsorption in the surfaces sheet MXene shape
At；
The nano-metal-oxide size is in 5-100nm；
The nano-metal-oxide is TiO2、SnO2、Fe3O4、RuO2、MnO2One or more of；
Nano-metal-oxide quality accounting in the nano-metal-oxide/MXene heterojunction structure composite materials is
10-90%；
The pattern of the nano-metal-oxide is one or more of nano bar-shape, nanometer threadiness, quantum dot.
2. a kind of preparation method of nano-metal-oxide/MXene heterojunction structure composite materials, which is characterized in that including as follows
Step：
（1）With Ti3AlC2For raw material, MXene solution is prepared by etching；
（2）Nano-metal-oxide is dispersed in 500ml organic solvents, nano-metal oxide solution is obtained；
（3）The MXene solution is instilled into step dropwise（2）Described in nano-metal oxide solution；
（4）By step（3）The mixed liquor of gained is ultrasonically treated, and suction filtration obtains the nano-metal-oxide/MXene heterojunction structures
Composite material.
3. a kind of preparation method of nano-metal-oxide according to claim 2/MXene heterojunction structure composite materials,
It is characterized in that, step（1）The preparation of the MXene solution includes the following steps：
A, 0.99g LiF are added in the plastic bottle equipped with 10ml hydrochloric acid, stir 5min, adds 1 g Ti3AlC2, stirring
Uniformly;
B, the mixed liquor for obtaining step A is placed in 35 DEG C of thermostat water baths, is stirred to react for 24 hours;
C, the solution that step B is obtained is centrifuged plus water operates 4 times repeatedly, until pH value of solution ≈ 6, removes supernatant liquor, ultrasound
30min centrifuges 1h, collects upper solution, the MXene solution after being etched.
4. a kind of preparation method of nano-metal-oxide according to claim 2/MXene heterojunction structure composite materials,
It is characterized in that, step（1）A concentration of 1-2mg/ml of the MXene solution.
5. a kind of preparation method of nano-metal-oxide according to claim 2/MXene heterojunction structure composite materials,
It is characterized in that, step（2）The organic solvent is NMP（N-Methyl pyrrolidone）、DMF（N,N-dimethylformamide）、THF
（Tetrahydrofuran）One or more of.
6. a kind of preparation method of nano-metal-oxide according to claim 2/MXene heterojunction structure composite materials,
It is characterized in that, step（3）Middle nano-metal-oxide is in the nano-metal-oxide/MXene
Quality accounting is 10-90% in heterojunction structure composite material.
7. a kind of preparation method of nano-metal-oxide according to claim 2/MXene heterojunction structure composite materials,
It is characterized in that, step（4）Middle ultrasonic time is 360 ~ 480min, ultrasonic power 40W.
8. lithium ion battery or ultracapacitor that a kind of method according to claims 2-7 any one is prepared
Electrode material.
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