CN104733717A - Microwave preparation method of alpha-Fe2O3/rGO composite material - Google Patents

Microwave preparation method of alpha-Fe2O3/rGO composite material Download PDF

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Publication number
CN104733717A
CN104733717A CN201510147601.XA CN201510147601A CN104733717A CN 104733717 A CN104733717 A CN 104733717A CN 201510147601 A CN201510147601 A CN 201510147601A CN 104733717 A CN104733717 A CN 104733717A
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rgo
microwave
graphene oxide
preparation
fe2o3
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刁国旺
朱守圃
任文吉
杨吉人
孙静
瞿姗姗
李忠翠
狄健
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Yangzhou University
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Yangzhou University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention provides a microwave preparation method of an alpha-Fe2O3/rGO composite material, belonging to the field of material production technology and application. According to the method, Fe(OH)3 sol is used as a precursor of alpha-Fe2O3, the Fe(OH)3 sol is uniformly dispersed on the surface of graphene oxide (GO) by means of the acting force between oxygen-containing groups on the surface of GO and electropositive iron ions; The Fe(OH)3 sol is in situ converted into alpha-Fe2O3 by means of microwave radiation under the action of hydrazine hydrate, and GO is converted into rGO to prepare the alpha-Fe2O3/rGO composite material with alpha-Fe2O3 loaded on the surface of rGO. By adopting the method, the solution is uniformly mixed by means of magnetic stirring, hydrazine hydrate is added into the mixed solution and is subjected to magnetic stirring and mixing instead of ultrasonic mixing, so that occurrence of side reaction can be avoided.

Description

A kind of α-Fe 2o 3the microwave preparation of/rGO composite material
Technical field
The invention belongs to manufacture of materials technology and application, be specifically related to as lithium ion battery negative material---α-Fe 2o 3the technology of preparing of/rGO composite material.
Background technology
Ferriferous oxide has the features such as raw material are extensive, cheap, environmental friendliness.α-Fe 2o 3have good thermodynamic stability and electro-chemical activity, by investigation and application widely, its negative material as lithium ion battery has had higher theoretical capacity, up to 1005mAhg -1.But, α-Fe 2o 3as the negative material of lithium ion battery in charge and discharge process because volume difference significant between ferriferous oxide and iron atom can produce large deformational stress, cause the fragmentation of electrode material, cause the continuous decay of battery capacity and the shortening of cycle life.To be engaged with material with carbon element by ferriferous oxide and prepare compound, on the one hand can quasi-complement α-Fe 2o 3the deficiency of conductivity, can maintain the complete of its crystalline structure on the other hand.This will greatly improve its charge-discharge performance as lithium ion battery negative material.
The advantages such as microwave reaction has power adjustable, and the reaction time is short, energy-conservation, and the simple and repeatability of device is strong.Microwave has good penetrability, when microwave penetrates medium, certain interaction will be there is with medium, the microwave of such as frequency 2450MHZ will make the vibrations of the molecule of medium generation per second 2,400,000,000 five thousand ten thousand times, by the friction between medium molecule, the temperature of medium is raised, the heat temperature raising while of making dielectric material inside, outside almost, completes reaction instantaneously.
Summary of the invention
The object of the invention is to propose one simple to operate, be beneficial to production in enormous quantities, repeatable strong one prepares graphene-supported α-Fe with microwave method 2o 3composite material, for lithium ion battery negative.
The present invention includes following steps:
1) by FeCl 3or FeCl 36H 2the aqueous solution of O is dropwise added drop-wise to obtained Fe (OH) in boiling water 3colloidal sol;
2) graphene oxide is added in deionized water, make the graphene oxide water solution of 1 ~ 20 mg/mL through ultrasonic vibration;
3) by Fe (OH) 3colloidal sol and graphene oxide water solution mixing, after magnetic agitation is even, more dropwise drip hydrazine hydrate, obtain reactant liquor;
4) above-mentioned reactant liquor is moved into microwave reaction in microwave reactor, to backflow, to react and terminate;
5) collect reaction precipitation thing, and after water and alcohol washing, drying, obtains α-Fe 2o 3/ rGO composite material.
The present invention mainly sets about from the conductivity of reinforcing material while preventing the fragmentation of ferriferous oxide structure, prepares graphene-supported Fe by microwave method 2o 3composite material and for the negative pole of lithium ion battery, to improve its cycle life and high rate during charging-discharging etc.
The present invention is with Fe (OH) 3colloidal sol is α-Fe 2o 3presoma, graphene oxide (GO) surface oxy radical and positively charged iron ion between active force make Fe (OH) 3colloidal sol is dispersed in GO surface uniformly.Fe (OH) is made by microwave under the effect of hydrazine hydrate 3colloidal sol is converted into α-Fe in position 2o 3, GO is converted into rGO simultaneously, obtained α-Fe 2o 3be carried on the α-Fe on rGO surface 2o 3/ rGO composite material.The magnetic agitation of carrying out in the present invention is to be mixed by solution, is added in above-mentioned mixed liquor by hydrazine hydrate and carries out magnetic agitation mixing, instead of ultrasonic mixing, is the generation avoiding side reaction.
By α-Fe 2o 3/ rGO composite material, as lithium ion battery negative material, has carried out assembling and the performance test of button cell.Result shows α-Fe 2o 3/ rGO composite material is at 1.0 A g -1lower 50 charge and discharge cycles of current density after still retain 892.6 mAh g -1discharge capacity, present high charge-discharge performance.
FeCl of the present invention 3or FeCl 36H 2the aqueous solution of O and the volume ratio of boiling water are 1:100 ~ 5:100.FeCl 3or FeCl 36H 2the concentration of O is the solution of 2 M ~ saturated, the relative FeCl of volume of water 3or FeCl 36H 2the aqueous solution of O is conducive to more greatly Fe (OH) 3the generation of colloid, according to the volume ratio that the concentration of the colloidal sol of preparation can select both suitable.
Described Fe (OH) 3fe (OH) in colloidal sol 3be 0.5 ~ 2:1 with the mixing quality ratio of graphene oxide in graphene oxide water solution.Wherein Fe (OH) 3for α-Fe 2o 3presoma, graphene oxide is the presoma of reduction graphite, and along with mass loss when graphene oxide is converted into reduced graphene, this mixing ratio can prepare reduced graphene and α-Fe 2o 3α-the Fe of certain proportion scope 2o 3/ rGO composite material.
Microwave power during described microwave reaction is 600 ~ 1000 W.Generally commercially available microwave oven can meet the microwave power of this reaction, is beneficial to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the Fe (OH) of preparation 3the transmission electron microscope picture of/rGO compound.
Fig. 2 is partial enlarged drawing in Fig. 1.
Fig. 3 is the α-Fe of preparation 2o 3the transmission electron microscope picture of/rGO compound.
Fig. 4 is Fig. 3 partial enlarged drawing.
Fig. 5 is the α-Fe of preparation 2o 3transmission electron microscope picture.
Fig. 6 is the α-Fe of preparation 2o 3/ rGO compound, α-Fe 2o 3, rGO and GO x-ray diffraction pattern.
Fig. 7 is the α-Fe of preparation 2o 3the TG-DTA curve chart of/rGO compound.
Fig. 8 is the α-Fe of preparation 2o 3/ rGO compound, α-Fe 2o 3and rGO tri-kinds of material assembled batteries are at 1A g -1performance test figure under current density.
Fig. 9 is the α-Fe of preparation 2o 3the performance test figure of/rGO compound under different current density.
Figure 10 is the α-Fe of preparation 2o 3/ rGO compound, α-Fe 2o 3, rGO and GO tetra-kinds of materials Raman spectrogram.
Figure 11 is in Figure 10, α-Fe 2o 3/ rGO compound, α-Fe 2o 3with the partial enlarged drawing of the Raman spectrogram of rGO tri-kinds of materials.
Embodiment
One, preparation method:
1, Fe (OH) 3preparation: in 100 mL beaker, add 30 ~ 60 mL deionized waters and add 2 zeolites, be then positioned over asbestos gauge is housed electric furnace on be heated to boiling, pipette the FeCl of 0.5 ~ 1.0 mL, 1 ~ 2 M with liquid-transfering gun 3or FeCl 36H 2the O aqueous solution, is dropwise added drop-wise in above-mentioned boiling water, continues to boil 1 ~ 4 min after dropwising, obtained Fe (OH) 3colloidal sol.
2, the preparation of graphene oxide water solution: by Hummer legal system for graphene oxide, also can market buying graphene oxide.Taking 50 ~ 80 mg graphene oxides (GO) adds in 50 mL centrifuge tubes or round-bottomed flask, then adds 15 ~ 30 mL deionized waters wherein, by ultrasonic vibration 20 ~ 60 min, obtains the deionized water solution of the graphene oxide of 1 ~ 20 mg/mL.
3, the preparation of reactant liquor: by the Fe (OH) of above-mentioned preparation 3the deionized water solution of colloidal sol and graphene oxide proceeds in 100 mL round-bottomed flasks, then magnetic agitation 5 ~ 15 min makes two liquid mix, pipetting 1.25mL hydrazine hydrate with liquid-transfering gun adds in above-mentioned mixed liquor, obtained reactant liquor after continuing stirring 5 ~ 15 min.
Meanwhile, contrast test is carried out doing different reactant liquors: in reactant liquor, do not add hydrazine hydrate respectively, do not add graphene oxide and do not add Fe (OH) 3.
4, microwave reaction: the above-mentioned 100 mL round-bottomed flasks that each reactant liquor is housed are inserted microwave reaction device, then load upper air set pipe and spherical condensation tube, open and stir, under 600 ~ 1000 W microwave powers, microwave is to obvious reactant liquor backflow, stop microwave, cessation reaction.
5, reactant separation, washing with drying: reactant liquor is proceeded in 50 mL centrifuge tubes, with the rotating speed of 5000 ~ 10000 r/min, centrifugation is carried out to reactant, 3 washings and 3 alcohol washes are carried out to the product be separated, obtain sediment, sediment is put in the vacuum drying chamber of 60 DEG C and dries 24 h and obtain product.
In said method, Fe (OH) 3the preparation of/GO composite material refers to that not adding hydrazine hydrate carries out microwave reaction, owing to not adding hydrazine hydrate, under microwave heating condition, and Fe (OH) 3colloidal sol does not change α-Fe into 2o 3, GO does not change rGO into yet.By Fe (OH) obtained after microwave heating 3/ GO composite material.α-Fe described in the present invention 2o 3the preparation of material refers to and replaces the GO aqueous solution to carry out microwave reaction, Fe (OH) under the effect of hydrazine hydrate with the deionized water of blank 3α-Fe will be converted into 2o 3, obtained α-Fe 2o 3nano particle.The preparation of the rGO material described in the present invention refers to the deionized water of blank replacement Fe (OH) 3colloidal sol carries out microwave reaction, and under the effect of hydrazine hydrate, GO will be converted into rGO.
Adopt above method, respectively obtained α-Fe 2o 3, Fe (OH) 3/ rGO and α-Fe 2o 3/ rGO.
Two, the material of preparation is carried out the Integration Assembly And Checkout of lithium ion battery as lithium ion battery negative material.
The wherein assembling instruction of battery: the mass ratio of active material, binding agent and carbon black is that the ratio of 8:1:1 is coated on Copper Foil, and wherein active material is the α-Fe of preparation 2o 3/ rGO composite material, binding agent be Kynoar (PVDF) or by mixing quality than being that the sodium carboxymethylcellulose (CMC) of 0.5 ~ 1:1 and chlorobenzene rubber (SBR) form, under 50 ~ 90 DEG C of conditions, dry 3 ~ 10 h, under the vacuum condition of 100 ~ 130 DEG C dry 8 ~ 24 h, in 4 ~ 7MPa lower sheeting, drying, weigh, active material proceeded to rapidly in glove box after the operation such as dry again, be that the assembling of 2032 half-cells is carried out to investigate its performance to electrode with lithium sheet.
The charge-discharge test of battery is respectively with α-Fe 2o 3/ rGO composite material, α-Fe 2o 3be basis with the quality of RGO, with 0.5,1.0,2.0,5.0,10.0 and 1.0 A g -1electric current be α-Fe to active material 2o 3the half-cell of/rGO composite material carries out charge-discharge test, voltage range 0.01 ~ 3.0 V, to investigate the charge-discharge performance under its different current density.Simultaneously to Fe 2o 3, rGO and α-Fe 2o 3/ rGO composite material three kinds of materials are with 1.0 A g -1current density carry out charge-discharge test to contrast its performance.
Three, performance characterization:
Fig. 1 is with the Fe of 1 mM (OH) 3the Fe (OH) prepared under the condition of hydrazine hydrate is not being added with the proportioning of 80 mg graphene oxides (GO) 3the transmission electron microscope picture of/GO compound, Fig. 2 is partial enlarged drawing in Fig. 1, by finding out Fe (OH) in Fig. 1,2 3diameter distribution is all covered in surface of graphene oxide, Fe (OH) in the lump uniformly 3diameter is less than 10 nm.
Fig. 3 is with the Fe of 1 mM (OH) 3product α-the Fe prepared with the proportioning of 80 mg graphene oxides 2o 3the transmission electron microscope picture of/rGO, Fig. 4 is partial enlarged drawing in Fig. 3, can find out Fe by Fig. 3,4 2o 3be scattered in GO surface equably, and α-Fe 2o 3pattern more homogeneous, its diameter is at about 40 nm.
Fig. 5 is with the Fe of 1mM (OH) 3the product Fe (OH) prepared under the condition of graphene oxide (GO) is not being added with the proportioning of 1.25mL hydrazine hydrate 3/ α-Fe 2o 3transmission electron microscope picture, α-Fe obtained as can be seen from Figure 2o 3pattern homogeneous, α-Fe in itself and Fig. 3 2o 3α-Fe in/rGO compound 2o 3pattern basically identical.
Fig. 6 is α-Fe prepared by the present invention 2o 3/ rGO compound, α-Fe 2o 3, rGO and GO x-ray diffraction pattern, its abscissa is the angle of diffraction of 2 times, and ordinate is relative intensity.The diffraction maximum marked in figure and α-Fe 2o 3standard spectrogram one_to_one corresponding, characterize α-Fe 2o 3/ rGO compound and α-Fe 2o 3crystal structure.The diffraction maximum of rGO and GO is significantly different, indicates the reduction of hydrazine hydrate to GO.Due to α-Fe 2o 3in/rGO compound, the surface major part of rGO is by α-Fe 2o 3cover, simultaneously the strong diffraction maximum of rGO and α-Fe 2o 3(012) face have certain repeatability, therefore α-Fe 2o 3/ rGO compound fails significantly to demonstrate the diffraction maximum of rGO.
Fig. 7 is that the present invention is with the Fe of 1mM (OH) 3the product Fe prepared with the proportioning of 80 mg GO 2o 3the TG-DTA curve chart of/rGO, drawn by thermogravimetric weight loss and a small amount of moisture, rGO is at α-Fe 2o 3content in/rGO compound is 21.3%.Meanwhile, Fig. 7 also shows, rGO is converted into CO or CO 2reaction mainly between 300 DEG C and 520 DEG C occur, and reaction be the endothermic reaction.
Fig. 8 is α-Fe prepared by the present invention 2o 3/ rGO compound, α-Fe 2o 3and the battery of rGO tri-kinds of material assemblings is at 1 A g -1performance test figure under current density.Fig. 8 shows α-Fe 2o 3/ rGO compound has higher capacity and good cyclical stability.
Fig. 9 is α-Fe prepared by the present invention 2o 3/ rGO compound is discharge performance under different current density, as can be seen from Figure 9 at 1 A g -1time discharge capacity be 900 mA h g -1left and right, even if 10 A g -1time, discharge capacity is still up to 550 mA h g -1, indicate α-Fe 2o 3/ rGO compound has good charge-discharge performance as lithium ion battery.
Figure 10 is α-Fe in the present invention 2o 3/ rGO compound, α-Fe 2o 3, rGO and GO tetra-kinds of materials Raman spectrogram, as can be seen from the figure, rGO has stronger D peak (1350 cm -1), GO has stronger G peak (1600 cm -1), this shows GO by reduction to a certain degree.Meanwhile, α-Fe 2o 3d peak in/rGO compound and α-Fe 2o 3in the strongest Raman spectral peaks have coincidence to a certain degree.
Figure 11 is in Figure 10, α-Fe 2o 3/ rGO compound, α-Fe 2o 3with rGO tri-kinds of materials at 150 ~ 750 cm -1the partial enlarged drawing of Raman figure, as can be seen from the figure α-Fe 2o 3/ rGO compound and α-Fe 2o 3there is consistent Raman spectrogram, and rGO does not have obvious Raman shift peak in this Raman shift interval, this demonstrate that α-Fe 2o 3at α-Fe 2o 3existence in/rGO compound.

Claims (4)

1. α-the Fe as lithium ion battery negative material 2o 3/ rGO Composite Microwave preparation method, is characterized in that comprising the steps:
1) by FeCl 3or FeCl 36H 2the aqueous solution of O is dropwise added drop-wise to obtained Fe (OH) in boiling water 3colloidal sol;
2) graphene oxide is added in deionized water, make the graphene oxide water solution of 1 ~ 20 mg/mL through ultrasonic vibration;
3) by Fe (OH) 3colloidal sol and graphene oxide water solution mixing, after magnetic agitation is even, more dropwise drip hydrazine hydrate, obtain reactant liquor;
4) above-mentioned reactant liquor is moved into microwave reaction in microwave reactor, to backflow, to react and terminate;
5) collect reaction precipitation thing, and after water and alcohol washing, drying, obtains α-Fe 2o 3/ rGO composite material.
2. preparation method according to claim 1, is characterized in that described FeCl 3or FeCl 36H 2the aqueous solution of O and the volume ratio of boiling water are 1:100 ~ 5:100.
3. preparation method according to claim 1, is characterized in that described Fe (OH) 3fe (OH) in colloidal sol 3be 0.5 ~ 2:1 with the mixing quality ratio of graphene oxide in graphene oxide water solution.
4. preparation method according to claim 1 or 2 or 3, microwave power when it is characterized in that described microwave reaction is 600 ~ 1000 W.
CN201510147601.XA 2015-03-31 2015-03-31 Microwave preparation method of alpha-Fe2O3/rGO composite material Pending CN104733717A (en)

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CN105950109A (en) * 2016-04-29 2016-09-21 安徽理工大学 Reduced graphene oxide, tin dioxide and ferric oxide composite material
CN106129373A (en) * 2016-08-25 2016-11-16 陕西科技大学 A kind of hollow ball Fe2o3the preparation method of/rGO lithium ion battery negative material
CN106328937A (en) * 2016-09-13 2017-01-11 武汉理工大学 Method molecular self-assembly and preparation of Fe2O3-graphene negative electrode material
CN107528046A (en) * 2016-06-21 2017-12-29 张家港市思杰五金工具有限公司 Preparation method, negative pole and the lithium ion battery of graphene/ferric oxide nano composite
CN108390046A (en) * 2018-03-16 2018-08-10 福州大学 A kind of preparation method of rodlike α-di-iron trioxide/GN lithium cell negative pole materials
CN109906499A (en) * 2016-08-30 2019-06-18 斯威本科技大学 Capacitor, electrode, redox graphene and the method and apparatus of manufacture
CN111039283A (en) * 2020-01-16 2020-04-21 中原工学院 Microwave-assisted preparation of metal oxide/graphene nano-structure material and preparation method thereof

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105950109A (en) * 2016-04-29 2016-09-21 安徽理工大学 Reduced graphene oxide, tin dioxide and ferric oxide composite material
CN105950109B (en) * 2016-04-29 2018-09-28 安徽理工大学 Redox graphene, stannic oxide and ferric oxide composite material
CN107528046A (en) * 2016-06-21 2017-12-29 张家港市思杰五金工具有限公司 Preparation method, negative pole and the lithium ion battery of graphene/ferric oxide nano composite
CN106129373A (en) * 2016-08-25 2016-11-16 陕西科技大学 A kind of hollow ball Fe2o3the preparation method of/rGO lithium ion battery negative material
CN106129373B (en) * 2016-08-25 2018-12-25 陕西科技大学 A kind of hollow sphere Fe2O3The preparation method of/rGO lithium ion battery negative material
CN109906499A (en) * 2016-08-30 2019-06-18 斯威本科技大学 Capacitor, electrode, redox graphene and the method and apparatus of manufacture
CN106328937A (en) * 2016-09-13 2017-01-11 武汉理工大学 Method molecular self-assembly and preparation of Fe2O3-graphene negative electrode material
CN106328937B (en) * 2016-09-13 2018-08-07 武汉理工大学 A kind of molecular self-assembling preparation Fe2O3The method of@graphene negative materials
CN108390046A (en) * 2018-03-16 2018-08-10 福州大学 A kind of preparation method of rodlike α-di-iron trioxide/GN lithium cell negative pole materials
CN108390046B (en) * 2018-03-16 2020-06-12 福州大学 Preparation method of rod-shaped α -ferric oxide/GN lithium battery negative electrode material
CN111039283A (en) * 2020-01-16 2020-04-21 中原工学院 Microwave-assisted preparation of metal oxide/graphene nano-structure material and preparation method thereof

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Application publication date: 20150624