CN107195897A - A kind of nanometer Fe NbO4/ Graphene composites and its preparation and application - Google Patents
A kind of nanometer Fe NbO4/ Graphene composites and its preparation and application Download PDFInfo
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Abstract
The present invention relates to a kind of nanometer Fe NbO4/ Graphene composites and its preparation and application, belong to field of new energy technologies.A kind of nanometer Fe NbO4The preparation method of/Graphene composites, is by C10H5O20Nb、Fe(NO3)3·9H2O and Graphene carries out gained particle after hydro-thermal reaction in reactor and is calcined, wherein, hydrothermal reaction condition is：20~24h is incubated at 180~240 DEG C, particle is obtained；Roasting condition is：By particle obtained by hydro-thermal reaction under an argon atmosphere, 950~1000 DEG C are warming up to 3~5 DEG C/min speed and are incubated 6~10h；Room temperature is down to 2~3 DEG C/min speed, nanometer Fe NbO is obtained4/ Graphene composites.Gained nanometer Fe NbO4The chemical property of/Graphene composites is compared with the nanometer Fe NbO that hydro-thermal method is synthesized4And the micron FeNbO of solid sintering technology synthesis4Increase.
Description
Technical field
The present invention relates to a kind of nanometer Fe NbO4/ Graphene composites and its preparation and application, belong to new energy skill
Art field.
Background technology
As the increasingly depleteds of the non-renewable resources such as oil, natural gas, people are to the pay attention to day by day of environment and can be again
The produces day of the strong electric energy of natural disposition is tended towards superiority effect, just further should as the lithium ion battery of reserve power from portable electrical equipment
Use the strategic new industry such as new-energy automobile, intelligent grid.Either intelligent grid or new-energy automobile are to lithium-ion electric
The performances such as safety, power, the capacity in pond propose higher requirement.
Current commercialized lithium ion battery negative material has the Delanium and day of six sides or rhombus layer structure
Lithium titanate (LTO, the Li of the carbon negative pole materials such as right modified graphite and cubic spinel structure4Ti5O12).But when using graphite as
During negative material, the decomposition of electrolyte can be caused during first charge-discharge, serious reduces its reversible capacity, Er Qie
During charge and discharge cycles, it is embedded into the deintercalation and solvent molecule of lithium ion in graphite, easily causes carbon negative pole material
Volume Changes, so as to cause caving in for graphite linings.In addition diffusivity of the lithium ion in graphite linings is relatively low, causes its high rate performance
It is not good, while graphite surface easily forms Li dendrite when overcharging, cause internal short-circuit of battery.Although LTO materials have zero strain, steady
The advantages of fixed cycle performance and high thermal stability, but because its material sheet is as insulator, electronic conductivity and ionic conductance
Rate is very low, and (intrinsic conductivity is only 10-9S/cm), cause its high rate capability poor.In order to meet electrokinetic cell to electrode material
On the one hand the requirement of high-energy-density, long life and security, researcher updates and has been commercialized negative pole material
The performance of material, one side constantly research and probe novel anode material.Wherein silicon substrate, tin base cathode material rely on its high theory
Capacity is of great interest.Wherein silica-base material has a highest specific capacity, and lithiumation is into Li4.4During Si, its theoretical capacity reaches
It is existing more than ten times of graphite cathode material of commercialization to 4200mAh/g.But work as and lithium ion battery negative material is used as using silicon
When, in charge and discharge process, meeting alloying during due to being acted on lithium ion produces larger bulk effect, stereomutation reaches
400%, the structure of material is destroyed and electrode efflorescence, so that its cycle efficieny is substantially reduced.Current silicon-based anode material
The research of material is concentrated mainly on Si/M (M is metallic element) classes and Si/C class composites, use nanometer synthesis to alleviate it more
Volumetric expansion.Tin base cathode material mainly includes metallic tin, tin-based oxide and kamash alloy.Its theoretical capacity is more negative than graphite
It is high go out more than 500mAh/g, but there is also huge bulk effect during removal lithium embedded, stereomutation reaches that 260% is left
The right side, seriously deteriorates its cycle performance, and its first irreversible capacity it is larger, these all significantly limit it in actual life
Application in production.
Niobium base negative material mainly includes niobium oxide, titanium niobium oxide etc..Due to the fermi level of lithium ion wherein
It is larger, therefore niobium base negative material is higher to the current potential of lithium ion.And niobium element has many variation of valence, therefore niobium in itself
Base negative material typically has higher theoretical specific capacity.At present, the synthetic method of niobium base negative material be mainly solid phase method and
Hydro-thermal method.It is excessive, scattered uneven and reunite than more serious etc. that the material of conventional solid-state method synthesis often has grain diameter
Phenomenon, the specific surface area that this directly contributes material is too small, only abundant with electrolyte contacts, and easily adds in charge and discharge process
Come off process for the rupture-efflorescence-of acute material, while the particle of big particle diameter can increase the length of the diffusion path of lithium ion and reduction
The quantity of its diffusion path, so that the performance such as circulating ratio of severe exacerbation material.And individually using hydro-thermal method to a certain degree
It is upper to alleviate the adverse effect brought because particle is excessive, but the improvement degree to material electrochemical performance is relatively limited.
The content of the invention
In order to solve the above technical problems, the invention provides a kind of used as negative electrode of Li-ion battery nanometer Fe NbO4/
The preparation method of Graphene (FNO/Gra) composite, using the chemical property of the material obtained by this method compared with hydro-thermal method
The nanometer Fe NbO of synthesis4The micron FeNbO of (Nano FNO) and solid sintering technology synthesis4(Micro FNO) increases.
A kind of nanometer Fe NbO4The preparation method of/Graphene composites, is by C10H5O20Nb (niobium oxalate), Fe
(NO3)3·9H2O and Graphene (graphene) carries out gained particle after hydro-thermal reaction in reactor and is calcined, wherein,
Hydrothermal reaction condition is：20~24h is incubated at 180~240 DEG C, particle is obtained；
Roasting condition is：By particle obtained by hydro-thermal reaction under an argon atmosphere, 950 are warming up to 3~5 DEG C/min speed
~1000 DEG C and 6~10h of insulation；Room temperature is down to 2~3 DEG C/min speed, nanometer Fe NbO is obtained4/ Graphene composite woods
Material.
Hydro-thermal of the present invention, roasting technique can be carried out in equipment disclosed in prior art, such as polytetrafluoroethyl-ne alkene reaction
Kettle, Muffle furnace, tube furnace etc..
Further, the C10H5O20Nb and Fe (NO3)3·9H2O mol ratio is 1:1.
Further, the graphene and FeNbO obtained by target4Weight ratio be 15~18:100, wherein, obtained by target
FeNbO4Weight refer to C10H5O20Nb and Fe (NO3)3·9H2O is raw material by FeNbO obtained by the complete reaction theory of proportioning4Weight
Amount.
Further, graphene is scattered by being dissolved in deionized water and in ultrasound 30min in supersonic wave cleaning machine with complete
It is complete scattered, obtain the dispersion liquid of graphene；Further, the weight ratio of graphene and water is 0.213 in preferably described dispersion liquid
~0.255:100.
Further, by C10H5O20Nb and Fe (NO3)3·9H2O is dissolved in after water respectively to be remixed, and obtains mixed solution；More enter
One step, preferably described C10H5O20Nb concentration is 0.08~0.1mol/L, Fe (NO3)3·9H2O concentration be 0.08~
0.1mol/L。
Further, then by the dispersion liquid of above-mentioned mixed solution and graphene in supersonic wave cleaning machine ultrasound at least 2h
To be thoroughly mixed.
Further, the mixture that hydro-thermal method synthesizes washs three times with deionized water and absolute ethyl alcohol respectively, then
It is placed in 80 DEG C of drying boxes and is baked to, the product after drying is ground, the particle after grinding is calcined again.
A preferred technical scheme of the invention is：A kind of used as negative electrode of Li-ion battery electrode material receives FeNbO4/
The preparation method of Graphene composites, methods described includes following processing steps：
1. by graphene and FeNbO obtained by target4Weight ratio be 15~18:100 ratio weighs graphene, is surpassed
Sound 30min is allowed to be evenly dispersed in deionized water, obtains the dispersion liquid of graphene；
2. Nb is pressed：Fe=1:1 mol ratio weighs C10H5O20Nb and Fe (NO3)3·9H2O, will weigh thing be dissolved in respectively from
Sub- water, after both are completely dissolved, at 60 DEG C, both is mixed 30min to promote it sufficiently to mix, then carry out
30min is ultrasonically treated, obtains brown color settled solution, wherein, the C10H5O20Nb concentration is 0.08~0.1mol/L, Fe
(NO3)3·9H2O concentration is 0.08~0.1mol/L；
3. by the dispersion liquid and C of graphene10H5O20Nb and Fe (NO3)3·9H2O homogeneous solution mixing is simultaneously clear in ultrasonic wave
Ultrasound 2h obtains the mixed solution of black to be completely dispersed in washing machine；The mixed solution of black is anti-in reactor progress hydro-thermal
Should, hydrothermal reaction condition is：20~24h is incubated at 180~240 DEG C, product is obtained；
4. products therefrom is centrifuged, and with respectively washing 3 times of deionized water and absolute ethyl alcohol, is subsequently placed in 80 DEG C of dryings
It is baked in case, the product after drying is ground, black powder is obtained；
5. the black powder of gained is put into corundum crucible and existed in tube furnace by protective gas of high-purity argon gas, with 3
~5 DEG C/min speed is warming up to 950~1000 DEG C and is incubated 6~10h；Room temperature is down to 2~3 DEG C/min speed, finally
Obtain the FeNbO of black4/ Graphene materials (FNO/Gra).
It is a further object of the present invention to provide the nanometer Fe NbO as made from the above method4/ Graphene composites, institute
Material is stated for nanometer Fe NbO4Distribution of particles interweaves the composite wood that is formed in the irregular grid to be formed in individual layer Graphene
Material, wherein, nanometer Fe NbO4The average grain diameter of particle is 50~80nm.
Beneficial effects of the present invention are：Utilize FeNbO made from the method for the invention4/ Graphene composites, its
In, FeNbO4For monoclinic system nano particle, the distribution of particles interweaves in the irregular grid to be formed in individual layer Graphene,
And then constitute FeNbO4/ Graphene composites.The FeNbO4/ Graphene composites enter as ion cathode material lithium
Row charge-discharge test, and with the micron FeNbO of Solid phase synthesis4(synthesis technique：By Nb：Fe=1:1 mol ratio is weighed in right amount
Nb2O5And Fe2O3, weighed object is fitted into 100ml agate jar on planetary ball mill with 600r/min rotating speed
Ball milling 4h, corundum crucible is put into and in Muffle furnace to be calcined 24h in 1100 DEG C of air by powder obtained by ball milling) and hydro-thermal method conjunction
Into nanometer Fe NbO4(synthesis technique is with preparing FeNbO4/ Graphene composites are consistent, need not simply use graphene with
And high-purity argon gas and tube furnace, it is sintered in Muffle furnace) it is compared；Charge-discharge test voltage range be 0.01~
3V, test electric current has tetra- kinds of 40mA/g, 80mA/g, 200mA/g, 400mA/g, and test temperature is 25 DEG C.Test result shows not
Only it puts first, charging capacity 865.7mAh/g, 599.1mAh/g is compared with micron (483.9mAh/g, 378.7mAh/g) and nanometer
The charging capacity of putting first of (751.7mAh/g, 576.3mAh/g) increases, and cycle performance and high rate performance are also more preferable.
Brief description of the drawings
Fig. 1 is Micro FNO of the present invention, Nano FNO and FNO/Gra XRD spectrum, by XRD spectrum it can be seen that
Micro FNO, Nano FNO and FNO/Gra peak shape is sharp, almost occurs without miscellaneous peak, and main diffraction peak is and monoclinic crystal
It is FeNbO4(PDF-70-2275) diffraction maximum correspondence.It is possible thereby to judge synthesis obtained by material highly crystalline and without dephasign；
Fig. 2 be Micro FNO of the present invention, Nano FNO and FNO/Gra charge-discharge test voltage range be 0.01~
First charge-discharge collection of illustrative plates under 3V, 40mA/g electric current；
Fig. 3 is Micro FNO of the present invention, Nano FNO and FNO/Gra cycle performance collection of illustrative plates, by cycle performance figure from
Starting for the tenth time of tending towards stability is circulated to calculate to being recycled to the 50th time, Micro FNO, Nano FNO and FNO/Gra's
Capability retention is followed successively by 82.94%, 92.83%, 95.75%, per circulation primary capacity attenuation for 1.01mAh/g,
0.6875mAh/g、0.495mAh/g.Thus it can determine whether that FNO/Gra cycle performances are best；
Fig. 4 is Micro FNO of the present invention, Nano FNO and FNO/Gra high rate performance collection of illustrative plates；
Fig. 5 (a), (b), (c) they are respectively Micro FNO of the present invention, Nano FNO and FNO/Gra SEM spectrum, from
SEM figures are it can be seen that obtained Micro FNO, Nano FNO material crystal formations physically well develop, and uniform in size, degree of scatter is good,
Without obvious agglomeration.Being distributed in Micro FNO granular sizes between 0.5~1um, Nano FNO particles are then mainly distributed more
Between 50~80nm.Gra/FNO material surfaces are relatively obscured, and this is due to nano level FeNbO4Winding is wrapped in surface circle
In the lamella of sliding graphene so that particle originally loses clearly corner angle, seamed edge；
Fig. 6 (a), (b), (c) are respectively the TEM collection of illustrative plates of the FNO/Gra under different multiples of the present invention.
Embodiment
Following non-limiting examples can make one of ordinary skill in the art be more fully understood the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments, is conventional method unless otherwise specified；The reagent and material, such as
Without specified otherwise, commercially obtain.
Embodiment 1
A kind of used as negative electrode of Li-ion battery electrode material nanometer Fe NbO4The system of/Graphene (FNO/Gra) composite
Preparation Method, comprises the following steps：
Step 1, FeNbO is prepared4/ Graphene precursors：
(1) graphene 0.0638g is weighed, by its ultrasonic disperse in 30mL deionized waters, ultrasonic time 30min obtains stone
The dispersion liquid of black alkene；
(2) C is weighed10H5O20Nb1.076g、Fe(NO3)3·9H2O0.808g, is dissolved separately in 20mL deionized waters
In after two kinds of solution are mixed, at 60 DEG C, both are mixed 30min to promote it sufficiently to mix, then carry out 30min
It is ultrasonically treated, obtain brown color settled solution；
(3) by the dispersion liquid and C of graphene10H5O20Nb and Fe (NO3)3·9H2O homogeneous solution is mixed and in ultrasonic wave
Ultrasound 2h obtains the mixed solution of black to be completely dispersed in cleaning machine；
(4) the black mixed liquor of gained is placed in ptfe autoclave liner and fixed in a kettle., be put into baking
In being incubated 24h at 200 DEG C in case, room temperature is then naturally cooled to, the material being layered；
(5) remove the upper liquid of layer material, lower floor's material is washed three times with deionized water and absolute ethyl alcohol respectively, will
Gains are put into baking oven to be baked in 80 DEG C, and the product after drying is ground, black powder, as FeNbO is obtained4/
Graphene precursors.
The precursor powder of gained in step 1 is put into corundum crucible and in tube furnace using high-purity argon gas as protective gas
6h is calcined at 1000 DEG C, programming rate is 5 DEG C/min；Room temperature is down to 3 DEG C/min speed, the electrode of black is finally given
Material FeNbO4/Graphene composites (FNO/Gra).
The present invention is by hydro-thermal method synthetic composite material FNO/Gra, the micron synthesized with using conventional solid-state method
MicroFNO (synthesis techniques：By Nb：Fe=1:1 mol ratio weighs Nb2O5And Fe2O3, weighed object is loaded to 100ml agate
With 600r/min rotating speed ball milling 4h on planetary ball mill in ball grinder, by powder obtained by ball milling be put into corundum crucible and in
To be calcined 24h in 1100 DEG C of air in Muffle furnace) compare and Nano FNO (synthesis technique and preparation that hydro-thermal method is synthesized
FeNbO4/ Graphene composites are consistent, do not include graphene in raw material simply, and it is calcined and carried out in Muffle furnace, and
Without argon gas protection), its chemical property obtains different degrees of raising.Charge-discharge test voltage range is 0.01~3V,
Test electric current has tetra- kinds of 40mA/g, 80mA/g, 200mA/g, 400mA/g, and test temperature is 25 DEG C, is specifically shown in Fig. 4.
As shown in Fig. 2 charge-discharge test is carried out in the case where charge-discharge test voltage range is 0.01~3V, 40mA/g electric currents,
Test result shows that not only it puts first, charging capacity 865.7mAh/g, 599.1mAh/g compared with micron (483.9mAh/g,
378.7mAh/g) increased with the charging capacity of putting first of nanometer (751.7mAh/g, 576.3mAh/g), cycle performance and
High rate performance is also more preferable.
Claims (7)
1. a kind of nanometer Fe NbO4The preparation method of/Graphene composites, it is characterised in that：It is by C10H5O20Nb、Fe
(NO3)3·9H2O and Graphene carries out gained particle after hydro-thermal reaction in reactor and is calcined, wherein,
Hydrothermal reaction condition is：20~24h is incubated at 180~240 DEG C, particle is obtained；
Roasting condition is：By particle obtained by hydro-thermal reaction under an argon atmosphere, 950 are warming up to 3~5 DEG C/min speed~
1000 DEG C and 6~10h of insulation；Room temperature is down to 2~3 DEG C/min speed, nanometer Fe NbO is obtained4/ Graphene composites.
2. according to the method described in claim 1, it is characterised in that：The graphene and FeNbO obtained by target4Weight ratio be
15~18:100.
3. according to the method described in claim 1, it is characterised in that：The C10H5O20Nb and Fe (NO3)3·9H2O mol ratio
For 1:1.
4. according to the method described in claim 1, it is characterised in that：By C10H5O20Nb and Fe (NO3)3·9H2O is dissolved in water respectively
After remix, then above-mentioned mixed solution is mixed with being dispersed with the dispersion liquid of graphene, ultrasonic disperse at least 2h after mixing, its
In, C10H5O20Nb concentration is 0.08~0.1mol/L, Fe (NO3)3·9H2O concentration is 0.08~0.1mol/L, described point
The weight ratio of graphene and water is 0.213~0.255 in dispersion liquid:100.
5. according to the method described in claim 1, it is characterised in that：The mixture deionized water and nothing that hydro-thermal method is synthesized
Water-ethanol is washed three times respectively, is subsequently placed in 80 DEG C of drying boxes and is baked to, the product after drying is ground, after grinding
Particle be calcined again.
6. nanometer Fe NbO made from claim 1 methods described4/ Graphene composites, it is characterised in that：The material is
Nanometer Fe NbO4Distribution of particles interweaves the composite that is formed in the irregular grid to be formed in individual layer Graphene, wherein,
Nanometer Fe NbO4The average grain diameter of particle is 50~80nm.
7. nanometer Fe NbO described in claim 14/ Graphene composites as negative electrode of lithium ion battery application.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107895787A (en) * | 2017-11-17 | 2018-04-10 | 龙岩学院 | One kind uses 2D/2D self-assembled compound materials HNb3O8/ RGO lithium ion battery |
| CN109650460A (en) * | 2019-01-17 | 2019-04-19 | 内蒙古大学 | A kind of preparation method of niobic acid iron superfine powder |
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| CN102646817A (en) * | 2011-02-16 | 2012-08-22 | 中国科学院金属研究所 | Graphene/metal oxide composite cathode material for lithium ion battery and preparation |
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- 2017-06-13 CN CN201710442682.5A patent/CN107195897B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102646817A (en) * | 2011-02-16 | 2012-08-22 | 中国科学院金属研究所 | Graphene/metal oxide composite cathode material for lithium ion battery and preparation |
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| HYUU-WOO SHIM，等: "Hydrothermal synthesis and electrochemical properties of FeNbO4 nanospheres", 《JOURNAL OF THE CERAMIC SOCIETY OF JAPAN》 * |
| KUMARI, T. SRI DEVI;: "Electrochemical lithium insertion behavior of FeNbO4：structural relations and in situ conversion into FeNb2O6during carbon coating", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107895787A (en) * | 2017-11-17 | 2018-04-10 | 龙岩学院 | One kind uses 2D/2D self-assembled compound materials HNb3O8/ RGO lithium ion battery |
| CN107895787B (en) * | 2017-11-17 | 2020-06-12 | 龙岩学院 | 2D/2D self-assembly composite material HNb3O8Lithium ion battery of/RGO |
| CN109650460A (en) * | 2019-01-17 | 2019-04-19 | 内蒙古大学 | A kind of preparation method of niobic acid iron superfine powder |
| CN109650460B (en) * | 2019-01-17 | 2021-03-23 | 内蒙古大学 | Preparation method of iron niobate ultrafine powder |
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Granted publication date: 20200428 |