CN109449390A - A kind of iron oxide/graphene aerogel composite negative pole material and preparation method thereof - Google Patents
A kind of iron oxide/graphene aerogel composite negative pole material and preparation method thereof Download PDFInfo
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- CN109449390A CN109449390A CN201811166448.5A CN201811166448A CN109449390A CN 109449390 A CN109449390 A CN 109449390A CN 201811166448 A CN201811166448 A CN 201811166448A CN 109449390 A CN109449390 A CN 109449390A
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Abstract
The present invention relates to a kind of iron oxide/graphene aerogel composite negative pole materials and preparation method thereof, and this method first disperses graphene oxide in deionized water, obtains graphene oxide dispersion；Then a certain amount of soluble ferric iron salt and urea are dissolved completely in the graphene oxide dispersion, obtain mixed solution；Microwave hydrothermal reacts 30~60min at a temperature of mixed solution is placed in 100~170 DEG C again, obtains iron oxide/graphene hydrogel, washs to the iron oxide/graphene hydrogel, freeze-drying process, obtains iron oxide/graphene aerogel first product；Finally under inert gas protection, iron oxide/graphene aerogel first product is made annealing treatment, iron oxide/graphene aerogel composite negative pole material can be obtained.Preparation process of the invention is not necessarily to high temperature, high energy consumption, environmentally friendly；Prepared iron oxide/graphene aerogel composite negative pole material coulombic efficiency is maintained at 98% or more, shows the excellent cyclical stability and high rate performance.
Description
Technical field
The present invention relates to technical field of lithium ion more particularly to a kind of iron oxide/graphene aerogel composite negative poles
Material and preparation method thereof.
Background technique
Lithium ion battery is the theme of current new energy circle development, its energy density is high, is had extended cycle life, charge and discharge
Pollution is not generated in journey, is a kind of outstanding energy storage device.With extensive use of the current lithium ion battery on electric car,
Higher and higher energy density is pursued, is the importance that lithium ion battery is studied at present.Existing lithium ion battery, cathode material
Material generally uses graphite, and the theoretical capacity of graphite is only 350mAhg-1, the low capacity impact energy of lithium ion battery entirety
Metric density.
Transition metal oxide is a kind of negative electrode material with high theoretical capacity, such as iron oxide (Fe2O3) theoretical capacity
It can achieve 1008mAhg-1, be three times of graphite or so, and ferro element rich reserves, easily exploitation purification, be it is a kind of have compared with
The lithium ion battery negative material of good prospect.But the electric conductivity of iron oxide is poor, and can generate in charge and discharge process compared with
Big volume expansion, and then electrode material structure is caused to be destroyed, on a current collector the problems such as dusting peeling, so that the service life of battery
Shorten, stability and high rate performance reduce.
Summary of the invention
In view of the above-mentioned problems, the object of the present invention is to provide a kind of iron oxide/graphene aerogel composite negative pole materials
And preparation method thereof, which has good high rate performance and stability, and its preparation process is not necessarily to high temperature, height
Energy consumption, it is at low cost, it is pollution-free, it is environmentally friendly.
In order to solve the above-mentioned technical problem, it is compound to provide a kind of iron oxide/graphene aerogel for the first aspect of the present invention
The preparation method of negative electrode material, this method comprises:
S1: dispersing graphene oxide in deionized water, obtains graphene oxide dispersion；
S2: a certain amount of soluble ferric iron salt and urea are dissolved completely in the graphene oxide dispersion, mixed
Close solution；
S3: microwave hydrothermal reacts 30~60min at a temperature of the mixed solution is placed in 100~170 DEG C, is aoxidized
Iron/graphene hydrogel；
S4: washing the iron oxide/graphene hydrogel, freeze-drying process, obtains iron oxide/graphene gas
Gel first product；
S5: under inert gas protection, the iron oxide/graphene aerogel first product is made annealing treatment, institute is obtained
State iron oxide/graphene aerogel composite negative pole material.
Further, before step S1, the method also includes the preparation of the graphene oxide, the graphite oxide
The preparation method of alkene is Hummers method, Brodie method, any one in Staudenmaier method.
Further, in step S2, the soluble ferric iron salt is FeNH4(SO4)2·12H2O、FeCl3·6H2O、Fe
(NO3)3、Fe2(SO4)3In any one.
Further, in step S2, the molar ratio of soluble ferric iron salt and urea in the mixed solution be (1:2)~
(1:20)。
Further, in step S2, the molar ratio of soluble ferric iron salt and graphene oxide in the mixed solution be (1:
1)~(1:4).
Further, in step S5, the temperature of the annealing is 350~500 DEG C, the time of annealing is 30~
120min。
Further, in step S1, using graphene oxide described in ultrasonic disperse in deionized water, ultrasonic time 30
~60min.
Further, in step S4, the temperature of the freeze-drying process is -70~-50 DEG C, and pressure is 5~15Pa.
The second aspect of the present invention also provides a kind of iron oxide/graphene aerogel composite negative pole material, the iron oxide/stone
Black alkene aeroge composite negative pole material is multiple for any one the iron oxide/graphene aerogel provided using first aspect present invention
The preparation method for closing negative electrode material is prepared.
A kind of iron oxide/graphene aerogel composite negative pole material of the invention and preparation method thereof has following beneficial
Effect:
Preparation method of the invention can greatly shorten the reaction time using microwave-assisted hydrothermal synthesis technology, reduce reaction
Temperature is conducive to improve production efficiency；And reaction raw materials are non-toxic, environmentally friendly.
In addition, the ferric oxide nanometer particle in negative electrode material prepared by the present invention has more uniform particle size, graphite
Alkene aeroge can effectively improve the electric conductivity and flexibility of negative electrode material entirety as the substrate of composite material, and then improve cathode
The conductivity of material, and the volume expansion that ferric oxide particles occur in charge and discharge process can be absorbed in graphene aerogel, keeps away
Exempt from that electrode material is destructurized, has extended service life and the stability of battery.In addition, the 3D that graphene aerogel is highly cross-linked
Self supporting structure has great porosity, can reduce tortuosity, promote the high rate performance of material.
Detailed description of the invention
It, below will be to required in embodiment or description of the prior art in order to illustrate more clearly of technical solution of the present invention
The attached drawing used is briefly described.It should be evident that drawings in the following description are only some embodiments of the invention, it is right
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings
Its attached drawing.
Fig. 1 is the stream of iron oxide provided in an embodiment of the present invention/graphene aerogel composite negative pole material preparation method
Cheng Tu；
Fig. 2 is that the iron oxide/graphene aerogel composite negative pole material XRD diffraction prepared in the embodiment of the present invention 1 shines
Piece；
Fig. 3 is iron oxide/graphene aerogel composite negative pole material charge-discharge cycle prepared by the embodiment of the present invention 1
It can curve.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art without making creative work it is obtained it is all its
His embodiment, shall fall within the protection scope of the present invention.
Embodiment 1
The present embodiment provides a kind of iron oxide/graphene aerogel composite negative pole material preparation methods, as shown in Figure 1,
Method includes the following steps:
S1: preparing graphene oxide by Hummers method, then weighs the graphene oxide and ultrasound point of 0.12g preparation
It dissipates in 60ml deionized water, ultrasonic time is 30~60min, obtains graphene oxide dispersion.
The step can form the graphene oxide dispersion of uniform dispersion, be conducive to the uniformity of following liquid-phase reaction.
S2: 1.62g FeCl is weighed3·6H2O and 1.2g urea is dissolved in above-mentioned graphene oxide dispersion, magnetic agitation
5min obtains mixed solution to being completely dissolved.
S3: mixed solution obtained above being transferred in microwave hydrothermal reaction kettle and is mixed, and the microwave hydrothermal is reacted
Kettle is placed in the microwave synthesizer with magnetic stirring apparatus and is heated to 120 DEG C, is cooled to room after keeping the temperature 40min at such a temperature
Fe can be obtained in temperature2O3/ graphene oxide hydrogel.
In the step ,-NH in urea is utilized2Hydrogen bond action between surface of graphene oxide oxygen-containing functional group makes oxygen
The lamella of graphite alkene is distorted alternation, forms three-dimensional net structure.Meanwhile Fe3+The OH solved with urea water-It is formed
FeOOH is further formed α-Fe at the reaction temperatures2O3, the characteristic auxiliary water that is heated up using microwave to polar substances Quick uniform
Heat shortens the reaction time, and allows iron oxide to be attached to graphene and show nucleating growth, and then form Fe2O3/ graphene oxide water
Gel complex material.
S4: by Fe obtained above2O3/ graphene oxide hydrogel is washed with deionized is put into freeze-drying afterwards for several times
Low temperature drying in machine forms Fe after removing moisture removal2O3/ graphite oxide aerogel first product.
Wherein, the temperature of low temperature drying is -58 DEG C in freeze drier, pressure 5Pa.Material is being kept under vacuum and low temperature
Moisture in materials is removed while original structure pattern, forms aerogel material.
S5: by Fe obtained above2O3/ graphite oxide aerogel first product is put into tube furnace, under nitrogen protection in
60min is made annealing treatment at a temperature of 400 DEG C, Fe can be obtained2O3/ graphite oxide aerogel composite negative pole material.
Annealing in the step can remove graphene surface partial oxidation functional group, reduce the later period as lithium ion
First circle irreversible capacity when cell negative electrode material.Obtained Fe2O3α-in/graphite oxide aerogel composite negative pole material
Fe2O3Nano particle is attached in graphene aerogel 3D network structure.
It is illustrated in figure 2 Fe2O3The XRD diffraction images of/graphite oxide aerogel composite negative pole material, can be with from figure
Find out that there are iron oxide in material manufactured in the present embodiment, and nearby has a relatively wide in range diffraction maximum corresponding in 2 θ=22 °
In the disordered structure of graphene aerogel.
Embodiment 2
The present embodiment provides a kind of iron oxide/graphene aerogel composite negative pole material preparation methods, as shown in Figure 1,
Method includes the following steps:
S1: graphene oxide is prepared by Hummers method, then according to FeNH4(SO4)2·12H2O and graphene oxide
Molar ratio be 1:3, weigh FeNH respectively4(SO4)2·12H2O and graphene oxide.
By above-mentioned weighed graphene oxide ultrasonic disperse in 60ml deionized water, ultrasonic time is 30~60min, is obtained
To graphene oxide dispersion.
S2: according to FeNH4(SO4)2·12H2The molar ratio of O and urea is 1:2, weighs urea；By above-mentioned weighed FeNH4
(SO4)2·12H2O and urea are dissolved in above-mentioned graphene oxide dispersion, and magnetic agitation 5min is mixed to being completely dissolved
Solution.
S3: mixed solution obtained above being transferred in microwave hydrothermal reaction kettle and is mixed, and the microwave hydrothermal is reacted
Kettle is placed in the microwave synthesizer with magnetic stirring apparatus and is heated to 100 DEG C, is cooled to room after keeping the temperature 60min at such a temperature
Fe can be obtained in temperature2O3/ graphene oxide hydrogel.
S4: by Fe obtained above2O3/ graphene oxide hydrogel is washed with deionized is put into freeze-drying afterwards for several times
Low temperature drying in machine forms Fe after removing moisture removal2O3/ graphite oxide aerogel first product.
Wherein, the temperature of low temperature drying is -50 DEG C in freeze drier, pressure 15Pa.
S5: by Fe obtained above2O3/ graphite oxide aerogel first product is put into tube furnace, under nitrogen protection in
120min is made annealing treatment at a temperature of 350 DEG C, Fe can be obtained2O3/ graphite oxide aerogel composite negative pole material.
Embodiment 3
The present embodiment provides a kind of iron oxide/graphene aerogel composite negative pole material preparation methods, as shown in Figure 1,
Method includes the following steps:
S1: graphene oxide is prepared by Hummers method, then according to Fe (NO3)3Molar ratio with graphene oxide is
1:2 weighs Fe (NO respectively3)3And graphene oxide.
By above-mentioned weighed graphene oxide ultrasonic disperse in 60ml deionized water, ultrasonic time is 30~60min, is obtained
To graphene oxide dispersion.
S2: according to Fe (NO3)3Molar ratio with urea is 1:10, weighs urea；By above-mentioned weighed Fe (NO3)3And urine
Element is dissolved in above-mentioned graphene oxide dispersion, and magnetic agitation 5min obtains mixed solution to being completely dissolved.
S3: mixed solution obtained above being transferred in microwave hydrothermal reaction kettle and is mixed, and the microwave hydrothermal is reacted
Kettle is placed in the microwave synthesizer with magnetic stirring apparatus and is heated to 150 DEG C, is cooled to room after keeping the temperature 50min at such a temperature
Fe can be obtained in temperature2O3/ graphene oxide hydrogel.
S4: by Fe obtained above2O3/ graphene oxide hydrogel is washed with deionized is put into freeze-drying afterwards for several times
Low temperature drying in machine forms Fe after removing moisture removal2O3/ graphite oxide aerogel first product.
Wherein, the temperature of low temperature drying is -58 DEG C in freeze drier, pressure 10Pa.
S5: by Fe obtained above2O3/ graphite oxide aerogel first product is put into tube furnace, under nitrogen protection in
90min is made annealing treatment at a temperature of 450 DEG C, Fe can be obtained2O3/ graphite oxide aerogel composite negative pole material.
Embodiment 4
The present embodiment provides a kind of iron oxide/graphene aerogel composite negative pole material preparation methods, as shown in Figure 1,
Method includes the following steps:
S1: graphene oxide is prepared by Hummers method, then according to Fe2(SO4)3Molar ratio with graphene oxide is
1:1 weighs Fe respectively2(SO4)3And graphene oxide.
By above-mentioned weighed graphene oxide ultrasonic disperse in 60ml deionized water, ultrasonic time is 30~60min, is obtained
To graphene oxide dispersion.
S2: according to Fe2(SO4)3Molar ratio with urea is 1:20, weighs urea；By above-mentioned weighed Fe2(SO4)3And urine
Element is dissolved in above-mentioned graphene oxide dispersion, and magnetic agitation 5min obtains mixed solution to being completely dissolved.
S3: mixed solution obtained above being transferred in microwave hydrothermal reaction kettle and is mixed, and the microwave hydrothermal is reacted
Kettle is placed in the microwave synthesizer with magnetic stirring apparatus and is heated to 170 DEG C, is cooled to room after keeping the temperature 30min at such a temperature
Fe can be obtained in temperature2O3/ graphene oxide hydrogel.
S4: by Fe obtained above2O3/ graphene oxide hydrogel is washed with deionized is put into freeze-drying afterwards for several times
Low temperature drying in machine forms Fe after removing moisture removal2O3/ graphite oxide aerogel first product.
Wherein, the temperature of low temperature drying is -55 DEG C in freeze drier, pressure 5Pa.
S5: by Fe obtained above2O3/ graphite oxide aerogel first product is put into tube furnace, under nitrogen protection in
30min is made annealing treatment at a temperature of 500 DEG C, Fe can be obtained2O3/ graphite oxide aerogel composite negative pole material.
Performance test:
With the Fe of the above-mentioned preparation of the present embodiment 12O3/ graphite oxide aerogel composite negative pole material as working electrode, with
Lithium piece is used as to electrode, and the electrolyte used is dissolved in ethylene carbonate (EC): carbon for the lithium hexafluoro phosphate of 0.5~0.8mol/L
Sour methyl ethyl ester (EMC): diethyl carbonate (DEC) is by volume in 1:1:1 mixed solution；Diaphragm is the production of Celgard company
2400 type polypropylene screens are assembled into CR2025 type button cell.At room temperature, within the scope of 0.001~3V charging/discharging voltage, with
The current density of 100mA/g carries out charge-discharge performance test, and test result is shown in Fig. 3.
From the figure 3, it may be seen that the Fe2O3/ graphite oxide aerogel composite negative pole material is surveyed under the current density of 100mA/g
Discharge capacity is up to 1620mAhg for the first time for examination-1, the discharge capacity of the second circle is 1001mAhg-1, capacity is protected after circulation 150 is enclosed
It holds in 750mAhg-1And decaying is not sent, it is higher by the theoretical capacity (350mAhg of graphite significantly-1), coulombic efficiency is maintained at 98%
More than, show the excellent cyclical stability and high rate performance.
To sum up, preparation method of the invention can greatly shorten the reaction time using microwave-assisted hydrothermal synthesis technology, drop
Low reaction temperatures are conducive to improve production efficiency；And reaction raw materials are non-toxic, environmentally friendly.
In addition, the ferric oxide nanometer particle in negative electrode material prepared by the present invention has more uniform particle size, graphite
Alkene aeroge can effectively improve the electric conductivity and flexibility of negative electrode material entirety as the substrate of composite material, and then improve cathode
The conductivity of material, and the volume expansion that ferric oxide particles occur in charge and discharge process can be absorbed in graphene aerogel, keeps away
Exempt from that electrode material is destructurized, has extended service life and the stability of battery.In addition, the 3D that graphene aerogel is highly cross-linked
Self supporting structure has great porosity, can reduce tortuosity, promote the high rate performance of material.
Above description sufficiently discloses a specific embodiment of the invention.It should be pointed out that being familiar with the field
Range of any change that technical staff does a specific embodiment of the invention all without departing from claims of the present invention.
Correspondingly, the scope of the claims of the invention is also not limited only to previous embodiment.
Claims (9)
1. a kind of iron oxide/graphene aerogel composite negative pole material preparation method, which is characterized in that the described method includes:
S1: dispersing graphene oxide in deionized water, obtains graphene oxide dispersion；
S2: a certain amount of soluble ferric iron salt and urea are dissolved completely in the graphene oxide dispersion, obtain mixing molten
Liquid；
S3: microwave hydrothermal reacts 30~60min at a temperature of the mixed solution is placed in 100~170 DEG C, obtains iron oxide/stone
Black alkene hydrogel；
S4: washing the iron oxide/graphene hydrogel, and freeze-drying process obtains iron oxide/graphene aerogel
First product；
S5: under inert gas protection, the iron oxide/graphene aerogel first product is made annealing treatment, the oxygen is obtained
Change iron/graphene aerogel composite negative pole material.
2. a kind of preparation method of iron oxide/graphene aerogel composite negative pole material according to claim 1, feature
It is, before step S1, the method also includes the preparation of the graphene oxide, the preparation method of the graphene oxide
For any one in Hummers method, Brodie method, Staudenmaier method.
3. a kind of preparation method of iron oxide/graphene aerogel composite negative pole material according to claim 1, feature
It is, in step S2, the soluble ferric iron salt is FeNH4(SO4)2·12H2O、FeCl3·6H2O、Fe(NO3)3、Fe2(SO4)3In
Any one.
4. a kind of preparation method of iron oxide/graphene aerogel composite negative pole material according to claim 1, feature
It is, in step S2, the molar ratio of soluble ferric iron salt and urea in the mixed solution is (1:2)~(1:20).
5. a kind of preparation method of iron oxide/graphene aerogel composite negative pole material according to claim 1, feature
It is, in step S2, the molar ratio of soluble ferric iron salt and graphene oxide in the mixed solution is (1:1)~(1:4).
6. a kind of preparation method of iron oxide/graphene aerogel composite negative pole material according to claim 1, feature
It is, in step S5, the temperature of the annealing is 350~500 DEG C, and the time of annealing is 30~120min.
7. a kind of preparation method of iron oxide/graphene aerogel composite negative pole material according to claim 1, feature
It is, in step S1, using graphene oxide described in ultrasonic disperse in deionized water, ultrasonic time is 30~60min.
8. a kind of preparation method of iron oxide/graphene aerogel composite negative pole material according to claim 1, feature
It is, in step S4, the temperature of the freeze-drying process is -70~-50 DEG C, and pressure is 5~15Pa.
9. a kind of iron oxide/graphene aerogel composite negative pole material, which is characterized in that the iron oxide/graphene aerogel
Composite negative pole material is using a kind of iron oxide/graphene aerogel composite negative pole material described in any one of claim 1~8
The preparation method of material is prepared.
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| CN110563960A (en) * | 2019-09-16 | 2019-12-13 | 中国科学院生态环境研究中心 | Nitrogen-doped iron-based graphene gel, and preparation method and application thereof |
| CN112018379A (en) * | 2020-08-25 | 2020-12-01 | 湖北工程学院 | Iron oxide composite graphene oxide nano material containing temperature-sensitive material and preparation method and application thereof |
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| CN110563960A (en) * | 2019-09-16 | 2019-12-13 | 中国科学院生态环境研究中心 | Nitrogen-doped iron-based graphene gel, and preparation method and application thereof |
| CN110563960B (en) * | 2019-09-16 | 2021-04-02 | 中国科学院生态环境研究中心 | Nitrogen-doped iron-based graphene gel, and preparation method and application thereof |
| CN112018379A (en) * | 2020-08-25 | 2020-12-01 | 湖北工程学院 | Iron oxide composite graphene oxide nano material containing temperature-sensitive material and preparation method and application thereof |
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| CN113329606A (en) * | 2021-05-28 | 2021-08-31 | 南京信息工程大学 | Magnetic metal/reduced graphene oxide aerogel composite wave absorbing agent and preparation method thereof |
| CN113329606B (en) * | 2021-05-28 | 2022-11-29 | 南京信息工程大学 | Magnetic metal/reduced graphene oxide aerogel composite wave absorbing agent and preparation method thereof |
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| CN113871209A (en) * | 2021-08-30 | 2021-12-31 | 兰州大学 | Carbon-coated graphene-iron oxide composite electrode material and preparation method and application thereof |
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