CN105826529A - Preparation of MnO-Cr2O3-graphene composite and application of MnO-Cr2O3-graphene composite in lithium ion battery negative electrodes - Google Patents

Preparation of MnO-Cr2O3-graphene composite and application of MnO-Cr2O3-graphene composite in lithium ion battery negative electrodes Download PDF

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CN105826529A
CN105826529A CN201610168198.3A CN201610168198A CN105826529A CN 105826529 A CN105826529 A CN 105826529A CN 201610168198 A CN201610168198 A CN 201610168198A CN 105826529 A CN105826529 A CN 105826529A
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mno
graphene
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graphene composite
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陈波
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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
    • H01M4/364—Composites as mixtures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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 discloses preparation of a MnO-Cr2O3-graphene composite and application of the MnO-Cr2O3-graphene composite in lithium ion battery negative electrodes. The preparation of the composite includes the two steps of synthesis of graphene oxide and preparation of the MnO-Cr2O3-graphene composite. The composite has excellent rate capability and cycling performance and still can keep good structural stability even in cycling under large current. The advantages of the composite are possibly related to the weight ratio of potassium permanganate to potassium dichromate in the preparation method, and when the weight ratio of potassium permanganate to potassium dichromate is (4-6):1, the prepared composite has the optimum performance.

Description

MnO-Cr2O3The preparation of-graphene composite material and the application in lithium ion battery negative
Technical field
The invention belongs to energy field, relate to graphene battery material, be specifically related to MnO-Cr2O3The system of-graphene composite material Standby and application in lithium ion battery negative.
Background technology
Mn oxide due to its abundant raw material, cheap and advantages of environment protection, be widely used in ultracapacitor, lithium from Sub-battery electrode material, fuel cell homenergic store and in conversion equipment.Wherein, MnO, due to Stability Analysis of Structures, has up to The theoretical specific capacity of 755mAh/g, is widely studied as lithium ion battery negative.But, with other transition metal oxide phases Seemingly, MnO electronic conductivity is relatively low, thus high rate performance is poor.Meanwhile, during conversion reaction, MnO shows bigger Volumetric expansion, cause active substance to come off from collector in charge and discharge process, capacity is decayed rapidly.
Generally, the nano-particle of transition metal oxide is loaded to has the material with carbon element of highly electron conductive (such as Graphene, carbon Nanotube etc.) on skeleton, it is possible to it is effectively improved the electronic conductivity of material, thus improves the high rate performance of material.But, Even if transition metal oxide nano particulate load is on the carbon material, its volumetric expansion can not well be improved, big electric current Under the relatively long circulating cycle, still show obvious capacity attenuation.
Summary of the invention
It is an object of the invention to overcome above-mentioned deficiency, it is provided that a kind of MnO-Cr2O3-graphene composite material, swollen to reduce volume Swollen, reduce big electric current and the capacity attenuation under the relatively long circulating cycle.
The above-mentioned purpose of the present invention is achieved by techniques below scheme:
A kind of MnO-Cr2O3The preparation method of-graphene composite material, comprises the steps:
Step S1, the synthesis of graphene oxide: take 0.5g expanded graphite and mix with the stirring of 60ml concentrated sulphuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g potassium permanganate and potassium dichromate, it is stirred overnight；Remove floating unreacted in solution upper strata Expanded graphite, pours into mixed solution in 240ml tri-distilled water and stirs, and after beaker cools down, adding 10ml mass fraction is 30% Hydrogen peroxide, obtain jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain the oxidation of brown color Graphene sol；Wherein, the weight ratio of described potassium permanganate and potassium dichromate is 4～6:1；
Step S2, MnO-Cr2O3The preparation of-graphene composite material: take 0.5g poly(ethylene oxide)-poly(propylene oxide)-polycyclic oxygen second Alkane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 and prepares Graphene oxide colloidal sol, stirring 30min after the oxide yellow graphene solution obtained is proceeded in 80 DEG C of water-baths；Subsequently, to Graphene oxide solution adds manganese nitrate solution and 3g potassium permanganate that 6ml mass fraction is 50%, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through sucking filtration, wash, dry and obtain presoma；By forerunner Body proceeds to N2In atmosphere tube type stove, 1000 DEG C of calcining 2h, i.e. obtain end product.
Further, described MnO-Cr2O3In preparation method step S1 of-graphene composite material, described potassium permanganate and The weight ratio of potassium dichromate is 5:1.
Described MnO-Cr2O3The application in the preparing lithium ion battery negative of-graphene composite material.
Advantages of the present invention:
The MnO-Cr that the present invention provides2O3-graphene composite material as lithium ion battery negative, shows good the most forthright Can, it is possible to reduce volumetric expansion, reduce big electric current and the capacity attenuation under the relatively long circulating cycle, at the big electric current of 5 and 10A/g Under density, remain to show the cycle performance of excellence.
Detailed description of the invention
Further illustrate the essentiality content of the present invention below in conjunction with embodiment, but do not limit scope with this.To the greatest extent The present invention is explained in detail by pipe with reference to preferred embodiment, it will be understood by those within the art that, can be to the present invention Technical scheme modify or equivalent, without deviating from the spirit and scope of technical solution of the present invention.
Embodiment 1:MnO-Cr 2 O 3 The preparation of-graphene composite material
A kind of MnO-Cr2O3The preparation method of-graphene composite material, comprises the steps:
Step S1, the synthesis of graphene oxide: take 0.5g expanded graphite and mix with the stirring of 60ml concentrated sulphuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g potassium permanganate and potassium dichromate, it is stirred overnight；Remove floating unreacted in solution upper strata Expanded graphite, pours into mixed solution in 240ml tri-distilled water and stirs, and after beaker cools down, adding 10ml mass fraction is 30% Hydrogen peroxide, obtain jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain the oxidation of brown color Graphene sol；Wherein, the weight ratio of described potassium permanganate and potassium dichromate is 5:1；
Step S2, MnO-Cr2O3The preparation of-graphene composite material: take 0.5g poly(ethylene oxide)-poly(propylene oxide)-polycyclic oxygen second Alkane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 and prepares Graphene oxide colloidal sol, stirring 30min after the oxide yellow graphene solution obtained is proceeded in 80 DEG C of water-baths；Subsequently, to Graphene oxide solution adds manganese nitrate solution and 3g potassium permanganate that 6ml mass fraction is 50%, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through sucking filtration, wash, dry and obtain presoma；By forerunner Body proceeds to N2In atmosphere tube type stove, 1000 DEG C of calcining 2h, i.e. obtain end product.
Embodiment 2:MnO-Cr 2 O 3 The preparation of-graphene composite material
A kind of MnO-Cr2O3The preparation method of-graphene composite material, comprises the steps:
Step S1, the synthesis of graphene oxide: take 0.5g expanded graphite and mix with the stirring of 60ml concentrated sulphuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g potassium permanganate and potassium dichromate, it is stirred overnight；Remove floating unreacted in solution upper strata Expanded graphite, pours into mixed solution in 240ml tri-distilled water and stirs, and after beaker cools down, adding 10ml mass fraction is 30% Hydrogen peroxide, obtain jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain the oxidation of brown color Graphene sol；Wherein, the weight ratio of described potassium permanganate and potassium dichromate is 4:1；
Step S2, MnO-Cr2O3The preparation of-graphene composite material: take 0.5g poly(ethylene oxide)-poly(propylene oxide)-polycyclic oxygen second Alkane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 and prepares Graphene oxide colloidal sol, stirring 30min after the oxide yellow graphene solution obtained is proceeded in 80 DEG C of water-baths；Subsequently, to Graphene oxide solution adds manganese nitrate solution and 3g potassium permanganate that 6ml mass fraction is 50%, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through sucking filtration, wash, dry and obtain presoma；By forerunner Body proceeds to N2In atmosphere tube type stove, 1000 DEG C of calcining 2h, i.e. obtain end product.
Embodiment 3:MnO-Cr 2 O 3 The preparation of-graphene composite material
A kind of MnO-Cr2O3The preparation method of-graphene composite material, comprises the steps:
Step S1, the synthesis of graphene oxide: take 0.5g expanded graphite and mix with the stirring of 60ml concentrated sulphuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g potassium permanganate and potassium dichromate, it is stirred overnight；Remove floating unreacted in solution upper strata Expanded graphite, pours into mixed solution in 240ml tri-distilled water and stirs, and after beaker cools down, adding 10ml mass fraction is 30% Hydrogen peroxide, obtain jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain the oxidation of brown color Graphene sol；Wherein, the weight ratio of described potassium permanganate and potassium dichromate is 6:1；
Step S2, MnO-Cr2O3The preparation of-graphene composite material: take 0.5g poly(ethylene oxide)-poly(propylene oxide)-polycyclic oxygen second Alkane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 and prepares Graphene oxide colloidal sol, stirring 30min after the oxide yellow graphene solution obtained is proceeded in 80 DEG C of water-baths；Subsequently, to Graphene oxide solution adds manganese nitrate solution and 3g potassium permanganate that 6ml mass fraction is 50%, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through sucking filtration, wash, dry and obtain presoma；By forerunner Body proceeds to N2In atmosphere tube type stove, 1000 DEG C of calcining 2h, i.e. obtain end product.
Embodiment 4: the weight ratio of the contrast of embodiment 1, potassium permanganate and potassium dichromate is 3:1
A kind of MnO-Cr2O3The preparation method of-graphene composite material, comprises the steps:
Step S1, the synthesis of graphene oxide: take 0.5g expanded graphite and mix with the stirring of 60ml concentrated sulphuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g potassium permanganate and potassium dichromate, it is stirred overnight；Remove floating unreacted in solution upper strata Expanded graphite, pours into mixed solution in 240ml tri-distilled water and stirs, and after beaker cools down, adding 10ml mass fraction is 30% Hydrogen peroxide, obtain jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain the oxidation of brown color Graphene sol；Wherein, the weight ratio of described potassium permanganate and potassium dichromate is 3:1；
Step S2, MnO-Cr2O3The preparation of-graphene composite material: take 0.5g poly(ethylene oxide)-poly(propylene oxide)-polycyclic oxygen second Alkane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 and prepares Graphene oxide colloidal sol, stirring 30min after the oxide yellow graphene solution obtained is proceeded in 80 DEG C of water-baths；Subsequently, to Graphene oxide solution adds manganese nitrate solution and 3g potassium permanganate that 6ml mass fraction is 50%, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through sucking filtration, wash, dry and obtain presoma；By forerunner Body proceeds to N2In atmosphere tube type stove, 1000 DEG C of calcining 2h, i.e. obtain end product.
Embodiment 5: the weight ratio of the contrast of embodiment 1, potassium permanganate and potassium dichromate is 7:1
A kind of MnO-Cr2O3The preparation method of-graphene composite material, comprises the steps:
Step S1, the synthesis of graphene oxide: take 0.5g expanded graphite and mix with the stirring of 60ml concentrated sulphuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g potassium permanganate and potassium dichromate, it is stirred overnight；Remove floating unreacted in solution upper strata Expanded graphite, pours into mixed solution in 240ml tri-distilled water and stirs, and after beaker cools down, adding 10ml mass fraction is 30% Hydrogen peroxide, obtain jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain the oxidation of brown color Graphene sol；Wherein, the weight ratio of described potassium permanganate and potassium dichromate is 7:1；
Step S2, MnO-Cr2O3The preparation of-graphene composite material: take 0.5g poly(ethylene oxide)-poly(propylene oxide)-polycyclic oxygen second Alkane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 and prepares Graphene oxide colloidal sol, stirring 30min after the oxide yellow graphene solution obtained is proceeded in 80 DEG C of water-baths；Subsequently, to Graphene oxide solution adds manganese nitrate solution and 3g potassium permanganate that 6ml mass fraction is 50%, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through sucking filtration, wash, dry and obtain presoma；By forerunner Body proceeds to N2In atmosphere tube type stove, 1000 DEG C of calcining 2h, i.e. obtain end product.
Embodiment 6: effect example
Under different electric current densities, (0.2A/g, 5A/g and 10A/g) measures the head of the composite of embodiment 1～5 preparation respectively Capacity (mAh/g) after circle reversible capacity, circulation 5 circle and circulation 100 circle, result see table:
Upper table illustrates, the composite of embodiment 1～3 preparation has reduced along with the increase of electric current density, capacity, but still has Higher conservation rate, and coulombic efficiency is close to 100%, is significantly better than the composite of embodiment 4～5 preparation.And, embodiment The composite of 1～3 preparations is after enclosing through 10A/g circulation 100, when electric current density is recalled to again to 0.2A/g, and charge and discharge electric capacity Amount remains to recover to 870～880, illustrates that composite still keeps good structural stability after high current charge-discharge. The composite of embodiment 4～5 preparation is after 10A/g circulation 100 circle, when electric current density is recalled to again to 0.2A/g, and charge and discharge Capacitance is lower than the charge/discharge capacity after 0.2A/g circulation 5 circle, cannot recover at all, illustrate that its structural stability is the most poor.
By above experimental result, it is known that the composite that the present invention provides has the high rate performance of excellence and excellent circulation Performance, even if recycled material also can keep good structural stability under big electric current.These advantages of composite of the present invention can Can be relevant with the weight ratio of potassium permanganate in preparation method and potassium dichromate, when the weight ratio of the two is 4～6:1, institute The composite property of preparation is optimum.
The effect of above-described embodiment indicates that the essentiality content of the present invention, but does not limit protection scope of the present invention with this. It will be understood by those within the art that, technical scheme can be modified or equivalent, and not take off Essence and protection domain from technical solution of the present invention.

Claims (3)

1. a MnO-Cr2O3The preparation method of-graphene composite material, it is characterised in that comprise the steps:
Step S1, the synthesis of graphene oxide: take 0.5g expanded graphite and mix with the stirring of 60ml concentrated sulphuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g potassium permanganate and potassium dichromate, it is stirred overnight；Remove floating unreacted in solution upper strata Expanded graphite, pours into mixed solution in 240ml tri-distilled water and stirs, and after beaker cools down, adding 10ml mass fraction is 30% Hydrogen peroxide, obtain jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain the oxidation of brown color Graphene sol；Wherein, the weight ratio of described potassium permanganate and potassium dichromate is 4～6:1；
Step S2, MnO-Cr2O3The preparation of-graphene composite material: take 0.5g poly(ethylene oxide)-poly(propylene oxide)-polycyclic oxygen second Alkane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 and prepares Graphene oxide colloidal sol, stirring 30min after the oxide yellow graphene solution obtained is proceeded in 80 DEG C of water-baths；Subsequently, to Graphene oxide solution adds manganese nitrate solution and 3g potassium permanganate that 6ml mass fraction is 50%, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through sucking filtration, wash, dry and obtain presoma；By forerunner Body proceeds to N2In atmosphere tube type stove, 1000 DEG C of calcining 2h, i.e. obtain end product.
MnO-Cr the most according to claim 12O3The preparation method of-graphene composite material, it is characterised in that: step In S1, the weight ratio of described potassium permanganate and potassium dichromate is 5:1.
3. the MnO-Cr described in claim 1 or 22O3The application in the preparing lithium ion battery negative of-graphene composite material.
CN201610168198.3A 2016-03-22 2016-03-22 Preparation of MnO-Cr2O3-graphene composite and application of MnO-Cr2O3-graphene composite in lithium ion battery negative electrodes Pending CN105826529A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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CN102185143A (en) * 2011-04-02 2011-09-14 浙江大学 Transition metal oxide/ graphene composite material and preparation method thereof
CN102941042A (en) * 2012-10-25 2013-02-27 北京理工大学 Graphene/metal oxide hybrid aerogel, preparation method and applications thereof
CN103066289A (en) * 2012-12-07 2013-04-24 上海锦众信息科技有限公司 Preparation method of chromium-nitrogen composite cathode material of lithium ion battery
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US20110033746A1 (en) * 2009-08-10 2011-02-10 Jun Liu Self assembled multi-layer nanocomposite of graphene and metal oxide materials
CN102173414A (en) * 2011-03-18 2011-09-07 中国地质大学（武汉） Method for preparing graphene oxide by chemical peeling
CN102185143A (en) * 2011-04-02 2011-09-14 浙江大学 Transition metal oxide/ graphene composite material and preparation method thereof
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