CN105762361A - Novel graphene composite material and preparation method thereof - Google Patents

Novel graphene composite material and preparation method thereof Download PDF

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CN105762361A
CN105762361A CN201610291864.2A CN201610291864A CN105762361A CN 105762361 A CN105762361 A CN 105762361A CN 201610291864 A CN201610291864 A CN 201610291864A CN 105762361 A CN105762361 A CN 105762361A
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composite material
preparation
graphene
mno
graphene composite
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刘高志
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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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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 a novel graphene composite material and a preparation method thereof. The preparation method of the novel composite material comprises the following two steps: synthesis of graphene oxide and preparation of a novel MnO-Cr2O3 graphene composite material. The novel graphene composite material provided by the invention has excellent rate performance and excellent cycling performance; a recycled material can also maintain good structure stability even under large current. The advantages of the novel graphene composite material may be related to the ratio of parts by weight of sodium silicate to that of sodium lauryl sulfate in the preparation method; when the ratio of parts by weight of the sodium silicate to that of the sodium lauryl sulfate is (4-6):1, the prepared novel graphene composite material is optimal in performance.

Description

A kind of Graphene composite material and preparation method thereof
Technical field
The invention belongs to field of new, relate to graphene battery material, be specifically related to MnO-Cr2O3-Graphene composite material Preparation 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 material 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, to reduce volume Expand, 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 the 60ml concentrated sulfuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g sodium metasilicate and sodium lauryl sulfate, it is stirred overnight；Remove the unreacted that solution upper strata is floating Expanded graphite, mixed solution is poured in 240ml tri-distilled water stir, until beaker cool down after, add 10ml mass fraction be The hydrogen peroxide of 30%, obtains jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain brown color Graphene oxide colloidal sol；Wherein, the weight ratio of described sodium metasilicate and sodium lauryl sulfate is 4～6:1；
Step S2, MnO-Cr2O3The preparation of-Graphene composite material: take 0.5g PEO-PPOX-polycyclic oxygen Ethane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 system Standby graphene oxide colloidal sol, proceeds to the oxide yellow graphene solution obtained in 80 DEG C of water-baths after stirring 30min；Subsequently, Manganese nitrate solution and 3g sodium metasilicate that 6ml mass fraction is 50% is added in graphene oxide solution, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through suction 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 sodium metasilicate and The weight ratio of sodium lauryl sulfate 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-Cr2O3The 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 the 60ml concentrated sulfuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g sodium metasilicate and sodium lauryl sulfate, it is stirred overnight；Remove the unreacted that solution upper strata is floating Expanded graphite, mixed solution is poured in 240ml tri-distilled water stir, until beaker cool down after, add 10ml mass fraction be The hydrogen peroxide of 30%, obtains jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain brown color Graphene oxide colloidal sol；Wherein, the weight ratio of described sodium metasilicate and sodium lauryl sulfate is 5:1；
Step S2, MnO-Cr2O3The preparation of-Graphene composite material: take 0.5g PEO-PPOX-polycyclic oxygen Ethane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 system Standby graphene oxide colloidal sol, proceeds to the oxide yellow graphene solution obtained in 80 DEG C of water-baths after stirring 30min；Subsequently, Manganese nitrate solution and 3g sodium metasilicate that 6ml mass fraction is 50% is added in graphene oxide solution, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through suction 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-Cr2O3The 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 the 60ml concentrated sulfuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g sodium metasilicate and sodium lauryl sulfate, it is stirred overnight；Remove the unreacted that solution upper strata is floating Expanded graphite, mixed solution is poured in 240ml tri-distilled water stir, until beaker cool down after, add 10ml mass fraction be The hydrogen peroxide of 30%, obtains jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain brown color Graphene oxide colloidal sol；Wherein, the weight ratio of described sodium metasilicate and sodium lauryl sulfate is 4:1；
Step S2, MnO-Cr2O3The preparation of-Graphene composite material: take 0.5g PEO-PPOX-polycyclic oxygen Ethane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 system Standby graphene oxide colloidal sol, proceeds to the oxide yellow graphene solution obtained in 80 DEG C of water-baths after stirring 30min；Subsequently, Manganese nitrate solution and 3g sodium metasilicate that 6ml mass fraction is 50% is added in graphene oxide solution, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through suction 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-Cr2O3The 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 the 60ml concentrated sulfuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g sodium metasilicate and sodium lauryl sulfate, it is stirred overnight；Remove the unreacted that solution upper strata is floating Expanded graphite, mixed solution is poured in 240ml tri-distilled water stir, until beaker cool down after, add 10ml mass fraction be The hydrogen peroxide of 30%, obtains jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain brown color Graphene oxide colloidal sol；Wherein, the weight ratio of described sodium metasilicate and sodium lauryl sulfate is 6:1；
Step S2, MnO-Cr2O3The preparation of-Graphene composite material: take 0.5g PEO-PPOX-polycyclic oxygen Ethane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 system Standby graphene oxide colloidal sol, proceeds to the oxide yellow graphene solution obtained in 80 DEG C of water-baths after stirring 30min；Subsequently, Manganese nitrate solution and 3g sodium metasilicate that 6ml mass fraction is 50% is added in graphene oxide solution, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through suction 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, sodium metasilicate and sodium lauryl sulfate 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 the 60ml concentrated sulfuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g sodium metasilicate and sodium lauryl sulfate, it is stirred overnight；Remove the unreacted that solution upper strata is floating Expanded graphite, mixed solution is poured in 240ml tri-distilled water stir, until beaker cool down after, add 10ml mass fraction be The hydrogen peroxide of 30%, obtains jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain brown color Graphene oxide colloidal sol；Wherein, the weight ratio of described sodium metasilicate and sodium lauryl sulfate is 3:1；
Step S2, MnO-Cr2O3The preparation of-Graphene composite material: take 0.5g PEO-PPOX-polycyclic oxygen Ethane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 system Standby graphene oxide colloidal sol, proceeds to the oxide yellow graphene solution obtained in 80 DEG C of water-baths after stirring 30min；Subsequently, Manganese nitrate solution and 3g sodium metasilicate that 6ml mass fraction is 50% is added in graphene oxide solution, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through suction 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, sodium metasilicate and sodium lauryl sulfate 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 the 60ml concentrated sulfuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g sodium metasilicate and sodium lauryl sulfate, it is stirred overnight；Remove the unreacted that solution upper strata is floating Expanded graphite, mixed solution is poured in 240ml tri-distilled water stir, until beaker cool down after, add 10ml mass fraction be The hydrogen peroxide of 30%, obtains jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain brown color Graphene oxide colloidal sol；Wherein, the weight ratio of described sodium metasilicate and sodium lauryl sulfate is 7:1；
Step S2, MnO-Cr2O3The preparation of-Graphene composite material: take 0.5g PEO-PPOX-polycyclic oxygen Ethane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 system Standby graphene oxide colloidal sol, proceeds to the oxide yellow graphene solution obtained in 80 DEG C of water-baths after stirring 30min；Subsequently, Manganese nitrate solution and 3g sodium metasilicate that 6ml mass fraction is 50% is added in graphene oxide solution, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through suction 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 current densities, (0.2A/g, 5A/g and 10A/g) measures the composite material of embodiment 1～5 preparation respectively Capacity (mAh/g) after first circle reversible capacity, circulation 5 circle and circulation 100 circle, result see table:
Upper table illustrates, the composite material of embodiment 1～3 preparation has reduced along with the increase of current density, capacity, but still tool There is higher conservation rate, and coulombic efficiency is close to 100%, be significantly better than the composite material of embodiment 4～5 preparation.And, real Execute example 1～3 preparation composite material through 10A/g circulation 100 circle after, when current density is recalled to again to 0.2A/g, fill Discharge capacity remains to recover to 880～890, illustrates that composite material still keeps good structure after high current charge-discharge Stability.The composite material of embodiment 4～5 preparation is after 10A/g circulation 100 circle, and current density is recalled to again to 0.2A/g Time, charge/discharge capacity is lower than the charge/discharge capacity after 0.2A/g circulation 5 circle, cannot recover at all, its structural stability is described The most poor.
By above experimental result, it is known that the composite material that the present invention provides has the high rate performance of excellence and excellent following Ring performance, even if recycled material also can keep good structural stability under big electric current.These of composite material of the present invention are excellent Point may be relevant with the weight ratio of sodium metasilicate in preparation method and sodium lauryl sulfate, and the weight ratio of the two is 4～6:1 Time, prepared composite material best performance.
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 the 60ml concentrated sulfuric acid, add 0.5g nitric acid Sodium, and it is slowly added to the mixture of 3g sodium metasilicate and sodium lauryl sulfate, it is stirred overnight；Remove the unreacted that solution upper strata is floating Expanded graphite, mixed solution is poured in 240ml tri-distilled water stir, until beaker cool down after, add 10ml mass fraction be The hydrogen peroxide of 30%, obtains jonquilleous graphene oxide solution；It is centrifuged and washs 4～5 times with tri-distilled water, obtain brown color Graphene oxide colloidal sol；Wherein, the weight ratio of described sodium metasilicate and sodium lauryl sulfate is 4～6:1；
Step S2, MnO-Cr2O3The preparation of-Graphene composite material: take 0.5g PEO-PPOX-polycyclic oxygen Ethane triblock copolymer P123 is dissolved in 100ml water, is stirred vigorously to a large amount of foams of generation, adds 1g step S1 system Standby graphene oxide colloidal sol, proceeds to the oxide yellow graphene solution obtained in 80 DEG C of water-baths after stirring 30min；Subsequently, Manganese nitrate solution and 3g sodium metasilicate that 6ml mass fraction is 50% is added in graphene oxide solution, after reaction 10min, Add 0.5g pyrroles；80 DEG C of water-baths of thing mixed above reacted after 12h through suction 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 rapid S1, the weight ratio of described sodium metasilicate and sodium lauryl sulfate is 5:1.
3. the MnO-Cr described in claim 1 or 22O3-Graphene composite material answering in preparing lithium ion battery negative With.
CN201610291864.2A 2016-05-04 2016-05-04 Novel graphene composite material and preparation method thereof Pending CN105762361A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109473635A (en) * 2017-09-08 2019-03-15 镇江瑞德新材料科技研发有限公司 A kind of graphene composite material and preparation method thereof
CN110743500A (en) * 2019-10-11 2020-02-04 南京师范大学 Modified graphene oxide adsorbent and preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109473635A (en) * 2017-09-08 2019-03-15 镇江瑞德新材料科技研发有限公司 A kind of graphene composite material and preparation method thereof
CN110743500A (en) * 2019-10-11 2020-02-04 南京师范大学 Modified graphene oxide adsorbent and preparation method and application thereof

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