CN105118962A - Carbon sphere/ferroferric oxide composite material, preparation and application method thereof - Google Patents
Carbon sphere/ferroferric oxide composite material, preparation and application method thereof Download PDFInfo
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- CN105118962A CN105118962A CN201510428069.9A CN201510428069A CN105118962A CN 105118962 A CN105118962 A CN 105118962A CN 201510428069 A CN201510428069 A CN 201510428069A CN 105118962 A CN105118962 A CN 105118962A
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- composite material
- oxide composite
- carbon ball
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- ferriferrous oxide
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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
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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
- 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
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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
- H01M4/48—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
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- 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 relates to a carbon sphere/ferroferric oxide composite material, and a preparation and application method thereof. The preparation method includes: fully mixing carbon spheres with a trivalent iron salt, then carrying out water bath reaction to obtain a carbon sphere/iron oxide composite material; then conducting thermal reduction on the carbon sphere/iron oxide composite material under a protective atmosphere to obtain the carbon sphere/ferroferric oxide composite material. According to the invention, ferroferric oxide particles grow on surfaces of the carbon spheres so as to prepare the carbon sphere/ferroferric oxide composite material. On the one hand, the electrical conductivity and lithium storage performance of the material is enhanced, and on the other hand, carbon spheres are taken as the attachment substrate of ferroferric oxide, and the agglomeration problem of ferroferric oxide particles is well improved.
Description
Technical field
What the present invention relates to is a kind of technology of field of nanocomposite materials, specifically a kind of carbon ball/ferriferrous oxide composite material and methods for making and using same thereof.
Background technology
On the market of lithium rechargeable battery, material with carbon element is used as negative pole main active substances because of the chemical property of its excellence always.In recent years, along with the further investigation to carbonaceous material, more and more pattern material with carbon element that is different, different properties is found and prepares.Wherein, spherical carbon material particularly nano level carbon ball because having larger specific area, higher tap density and gaining great popularity.However, also there is the low shortcoming of specific capacity in carbon ball itself.
Compared with material with carbon element, the metal that some chemical properties are active and metal oxide have higher theoretical capacity.Tri-iron tetroxide is because having specific capacity high (926mAh/g), the good (σ=2*104S/m of electron conduction, be better than other transition metal oxides), cheap, aboundresources, the feature such as nontoxic and environmentally friendly, development potentiality is had much in lithium ion battery negative material, but exist in battery charge and discharge process simultaneously and easily volumetric expansion occurs, the problems such as easy reunion.Patent publication No. is a kind of method that the Chinese patent of CN101699641A discloses ironic citrate pyrolysis and prepares tri-iron tetroxide, but the ferriferrous oxide particles of preparation is comparatively large, and it is serious to reunite.
For the defect that material with carbon element and tri-iron tetroxide are applied in lithium ion battery, researchers attempt constructing compound new material to make up the deficiency of homogenous material: Chinese patent literature CN104117329A discloses a kind of method of carbon-coated magnetic tri-iron tetroxide, this technology first prepares the coated di-iron trioxide of carbon by hydro thermal method, then obtains the composite material of carbon coated ferriferrous oxide by microwave heating high-temperature calcining.The preparation method of this technology and composite material is complicated, complex steps and high to equipment requirement, causes a definite limitation to the application involved by material.
Chinese patent literature CN104269536A, open (bulletin) day 2015.01.07, discloses a kind of composite material and preparation method of graphene-supported Spherical Carbon coated iron oxide.The structure of this material is the particle of load carbon coated iron oxide in two-layer graphene film, and the core in particle is concentric spherical iron oxide, and particle skin is carbon-coating.The method process comprises: by Fe (NO
3)
3the aqueous solution joins in graphene oxide water solution, add hydrazine hydrate, washing, freeze-drying after stirring in water bath, obtain presoma, presoma is put in quartz tube furnace, be warming up to 500 ~ 600 DEG C with given pace under argon gas, insulation a period of time, heat up 800 ~ 900 DEG C with given pace, in tube furnace, pass into methane, in argon gas, be finally cooled to the composite material that room temperature obtains the Spherical Carbon coated iron oxide of black alkene load.But the hydrazine hydrate used in this technology is poisonous, and easily blasts, the popularization of this technology is made to be subject to a definite limitation.
Chinese patent literature CN102623692A, open (bulletin) day 2012.08.01, discloses the preparation method of a kind of tri-iron tetroxide-carbon composite lithium ion battery negative material.The technical process of the method is: first, takes raw material in the ratio of carbon in ferro element in source of iron and graphite.Then, the raw material taken and abrading-ball are joined in ball grinder, then in ball grinder, add a certain amount of distillation or deionized water wet ball grinding, or directly dry grind.Be put into by ball grinder on ball mill, with certain rotating speed, ball milling certain hour, discharging obtains product.Be hydroxide for source of iron, chloride, during various molysite, to the product after ball milling discharging, under the protection of inert gas, heat treatment several hours.Product is carried out Magneto separate, isolates the graphite granule of not fully compound.Finally sieve successively by different pore size, the product for wet-milling needs drying and processing before sieving, and sieves to choose to obtain carbon back ferric oxide composite material.But this technical matters relative complex is higher to the requirement of equipment.
Summary of the invention
The present invention is directed to prior art above shortcomings, a kind of carbon ball/ferriferrous oxide composite material and methods for making and using same thereof are proposed, by at carbon ball superficial growth ferriferrous oxide particles, prepare the composite material of carbon ball/tri-iron tetroxide, improve conductivity and the storage lithium performance of material on the one hand; On the other hand, using carbon ball as the attaching substratum of tri-iron tetroxide, the good agglomeration traits improving ferriferrous oxide particles.
The present invention is achieved by the following technical solutions:
The present invention relates to a kind of carbon ball/ferriferrous oxide composite material, for black powder and tri-iron tetroxide uniform be grown on carbon ball surface, bar-shaped in wolf's fang.
The present invention relates to the preparation method of above-mentioned composite material, carbon ball is fully mixed rear water-bath with trivalent iron salt, obtain carbon ball/silicon/iron oxide composite material; Again the thermal reduction under protective atmosphere of carbon ball/silicon/iron oxide composite material is obtained carbon ball/ferriferrous oxide composite material.
Described trivalent iron salt refers to ferric trichloride, ferric nitrate or ferric sulfate.
Described carbon ball is by biomass carbon source Hydrothermal Synthesiss such as glucose, sucrose, starch.
Described abundant mixing refers to: ferriferous oxide the growth response temperature on carbon ball surface be 20 ?70 DEG C, the reaction time be 5 ?48h, mixing speed be 10 ?100r/min.
Described water-bath, carries out washing dry after being preferably reaction, wherein dry is vacuumize, and temperature is 50 ?110 DEG C.
Described protective atmosphere is nitrogen, argon gas, hydrogen or wherein any both or the gaseous mixture of three or the mixed atmosphere of inert gas and reducing gas.
Described reducing gas is the mixed atmosphere of hydrogen and argon gas.
Described thermal reduction refers to: 300 ?under 2000 DEG C of environment heat treatment 1 ?10h.
The present invention relates to a kind of lithium ion battery based on above-mentioned carbon ball/ferriferrous oxide composite material, comprise: positive pole, negative pole, barrier film and electrolyte, wherein: negative pole by N ?methyl pyrrolidone (NMP), carbon ball/ferriferrous oxide composite material, conductive black and polyvinyladine floride (PVDF) form.
Described negative pole, with N ?methyl pyrrolidone (NMP) for solvent, to there is the mixing of the powder of carbon ball/ferriferrous oxide composite material, conductive black and polyvinyladine floride (PVDF), be stirred into muddy be coated on copper foil surface and make after drying, wherein: the mass ratio of the powder of carbon ball/ferriferrous oxide composite material, conductive black and polyvinyladine floride (PVDF) is preferably 80:10:10.
Described drying refers to vacuumize 12 hours.
Described positive pole adopts lithium metal.
Described barrier film adopts capillary polypropylene (Celgard2300) film.
Described electrolyte is by lithium hexafluoro phosphate (LiPF
6)/ethylene carbonate (EC), diethyl carbonate (DEC), methyl ethyl ester (EMC) are mixed, and its component and content are preferably: 1mol/LLiPF
6/ EC, DEC, EMC are that 1:1:1 mixes with volume ratio.
Described lithium ion battery is preferably assembled and is obtained in the glove box being full of high-purity argon gas.
Technique effect
Compared with prior art, the present invention prepares in the process of composite material, without the need to reducing agent, raw material and product be not containing any harmful substance, and available equipment scope is wide, and preparation method is simple and direct, and the product of different iron-carbon ratio example can be prepared as required, for the diversity of material provides precondition.
Accompanying drawing explanation
Fig. 1 is carbon ball field emission scanning electron microscope (SEM) schematic diagram in the embodiment of the present invention 1;
Fig. 2 is carbon ball in the embodiment of the present invention 1/silicon/iron oxide composite material field emission scanning electron microscope (SEM) schematic diagram;
Fig. 3 is carbon ball in the embodiment of the present invention 1/ferriferrous oxide composite material field emission scanning electron microscope (SEM) schematic diagram;
Fig. 4 be in the embodiment of the present invention 1 carbon ball/ferriferrous oxide composite material as lithium ion battery negative material charge and discharge cycles 30 performance schematic diagrames under 100mAh/g discharge and recharge condition;
Fig. 5 be in the embodiment of the present invention 1 carbon ball/ferriferrous oxide composite material as lithium ion battery negative material charge-discharge performance schematic diagram under different current density condition.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The present embodiment relates to the preparation of carbon ball/ferriferrous oxide composite material, and its concrete steps comprise:
1) 0.05 gram of carbon ball (as shown in Figure 1) and 1.35 grams of Iron(III) chloride hexahydrates are uniformly dispersed in 100mL deionized water, water bath with thermostatic control 24h in 30 DEG C of bath temperatures, low whipping speed 20r/min clock stirs.
2) carbon ball/solid iron oxides product is obtained through filtering and washing, as shown in Figure 2.
3) dry 12 hours are placed in vacuum drying chamber under 80 DEG C of conditions.
4) dried product is placed in quartz tube furnace, under high pure nitrogen protection, is warming up to 400 DEG C and constant temperature 3h with the speed of 20 DEG C/min, stops heating subsequently and naturally cool, obtaining carbon ball/ferriferrous oxide composite material.As shown in Figure 3.
The present embodiment adopts above-mentioned composite material to prepare the negative pole of lithium ion battery, be specially: with N ?methyl pyrrolidone (NMP) for solvent, 80:10:10 in mass ratio, carbon ball/ferriferrous oxide composite material powder, conductive black and polyvinyladine floride (PVDF) are mixed, is stirred into muddy and is coated on copper foil surface; Vacuumize 12 hours, the negative plate that diameter is 10mm made by compressing tablet.
The present embodiment adopts above-mentioned negative pole to prepare lithium ion battery, is specially: using lithium metal as with reference to positive pole, with capillary polypropylene (Celgard2300) film for barrier film, with 1mol/LLiPF
6/ EC+DEC+EMC (volume ratio is 1:1:1) is electrolyte.In the glove box being full of high-purity argon gas, be assembled into CR2032 button cell.Leave standstill and carry out electrochemical property test after 12 hours.
The simulated battery that prepared by the present embodiment adopts blue electric battery test system (LANDCT ?2001A) to carry out charge-discharge performance test, as shown in Figure 4 and Figure 5.With different charge-discharge magnification (0.1,0.2,0.5,1 and 2A/g), in 0 ~ 3V voltage range, charge-discharge performance test is carried out to carbon ball/ferriferrous oxide composite material powder sample.
Embodiment 2
Compared with embodiment 1,0.05 gram of carbon ball and 1 gram of ferric sulfate are uniformly dispersed by the present embodiment in 100mL deionized water, water bath with thermostatic control 24h in 40 DEG C of bath temperatures, keep magnetic agitation speed 40r/min.Rear suction filtration, washing obtains carbon ball/solid iron oxides product.To be placed in vacuum drying chamber under 80 DEG C of conditions dry 12 hours.Dried product is placed in quartz tube furnace, under high pure nitrogen protection, is warming up to 500 DEG C and constant temperature 2h with the speed of 20 DEG C/min, stop subsequently heating and naturally cooling to room temperature, obtain carbon ball/ferriferrous oxide composite material.
Charge-discharge performance test is carried out to carbon ball/tri-iron tetroxide sample that the present embodiment obtains.Charge and discharge cycles test result shows: specific capacity during 0.1A/g discharge and recharge is about 503mAh/g.
Embodiment 3
Compared with embodiment 1,0.05 gram of carbon ball and 1.2 grams of ferric nitrates are uniformly dispersed by the present embodiment in 100mL deionized water, water bath with thermostatic control 12h in 40 DEG C of bath temperatures, keep magnetic agitation speed 60r/min.Rear suction filtration, washing obtains carbon ball/solid iron oxides product.To be placed in vacuum drying chamber under 80 DEG C of conditions dry 12 hours.Dried product is placed in quartz tube furnace, with high-purity argon gas by the air emptying in quartz ampoule, is warming up to 600 DEG C and constant temperature 1h with the speed of 20 DEG C/min,
Stop subsequently heating and naturally cooling to room temperature, obtain carbon ball/ferriferrous oxide composite material.
Charge-discharge performance test is carried out to carbon ball/tri-iron tetroxide sample that the present embodiment obtains.Charge and discharge cycles test result shows: specific capacity during 0.1A/g discharge and recharge is about 429mAh/g.
Claims (11)
1. a preparation method for carbon ball/ferriferrous oxide composite material, is characterized in that, carbon ball is fully mixed rear water-bath with trivalent iron salt, obtains carbon ball/silicon/iron oxide composite material; Again the thermal reduction under protective atmosphere of carbon ball/silicon/iron oxide composite material is obtained carbon ball/ferriferrous oxide composite material.
2. method according to claim 1, is characterized in that, described trivalent iron salt refers to ferric trichloride, ferric nitrate or ferric sulfate.
3. method according to claim 1, is characterized in that, described carbon ball is by glucose, sucrose, starch Hydrothermal Synthesis.
4. method according to claim 1, is characterized in that, described abundant mixing refers to: ferriferous oxide the growth response temperature on carbon ball surface be 20 ?70 DEG C, the reaction time be 5 ?48h, mixing speed be 10 ?100r/min.
5. method according to claim 1, is characterized in that, carry out washing after described water-bath and vacuumize, baking temperature is 50 ?110 DEG C.
6. method according to claim 1, is characterized in that, described thermal reduction refers to: 300 ?under 2000 DEG C of environment heat treatment 1 ?10h.
7. carbon ball/ferriferrous oxide composite material that method prepares according to above-mentioned arbitrary claim, is characterized in that, for black powder and tri-iron tetroxide uniform be grown on carbon ball surface, bar-shaped in wolf's fang.
8. the lithium ion battery based on the carbon ball/ferriferrous oxide composite material described in above-mentioned arbitrary claim, it is characterized in that, comprise: positive pole, negative pole, barrier film and electrolyte, wherein: negative pole by N ?methyl pyrrolidone, carbon ball/ferriferrous oxide composite material, conductive black and polyvinyladine floride form.
9. lithium ion battery according to claim 8, it is characterized in that, described negative pole, with N ?methyl pyrrolidone for solvent, by having the mixing of the powder of carbon ball/ferriferrous oxide composite material, conductive black and polyvinyladine floride, being stirred into muddy and being coated on copper foil surface and making after drying.
10. lithium ion battery according to claim 9, is characterized in that, the mass ratio of the powder of described carbon ball/ferriferrous oxide composite material, conductive black and polyvinyladine floride is 80:10:10.
11. lithium ion batteries according to claim 8, is characterized in that, described electrolyte is mixed by lithium hexafluoro phosphate/ethylene carbonate, diethyl carbonate, methyl ethyl ester, and its component and content are: 1mol/LLiPF
6/ EC, DEC, EMC are that 1:1:1 mixes with volume ratio.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244381A (en) * | 2018-07-24 | 2019-01-18 | 昆明理工大学 | A kind of preparation method of carbon coated ferriferrous oxide nanosphere |
| CN111389400A (en) * | 2020-03-23 | 2020-07-10 | 广东石油化工学院 | Preparation method of catalyst for fused salt electrochemical synthesis of ammonia |
| CN114989844A (en) * | 2022-06-09 | 2022-09-02 | 武汉轻工大学 | Method for co-producing high-quality bio-oil and porous graphite carbon by catalytic pyrolysis of biomass and polyolefin plastic |
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| CN103219510A (en) * | 2013-03-21 | 2013-07-24 | 华中科技大学 | Lithium battery negative electrode material preparation method and its product |
| CN104393284A (en) * | 2014-11-17 | 2015-03-04 | 天津大学 | Nickel oxide nano-particle loaded porous hard carbon sphere negative electrode material and preparation method thereof |
| CN104409225A (en) * | 2014-11-28 | 2015-03-11 | 西北师范大学 | Preparation method of manganese dioxide/ carbon microspheres composite material and application of composite material serving as supercapacitor electrode material |
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2015
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| CN103219510A (en) * | 2013-03-21 | 2013-07-24 | 华中科技大学 | Lithium battery negative electrode material preparation method and its product |
| CN103157438A (en) * | 2013-04-10 | 2013-06-19 | 哈尔滨工业大学 | Preparation method of carbon microsphere/nanometer iron oxide magnetic composite material |
| CN104393284A (en) * | 2014-11-17 | 2015-03-04 | 天津大学 | Nickel oxide nano-particle loaded porous hard carbon sphere negative electrode material and preparation method thereof |
| CN104409225A (en) * | 2014-11-28 | 2015-03-11 | 西北师范大学 | Preparation method of manganese dioxide/ carbon microspheres composite material and application of composite material serving as supercapacitor electrode material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244381A (en) * | 2018-07-24 | 2019-01-18 | 昆明理工大学 | A kind of preparation method of carbon coated ferriferrous oxide nanosphere |
| CN111389400A (en) * | 2020-03-23 | 2020-07-10 | 广东石油化工学院 | Preparation method of catalyst for fused salt electrochemical synthesis of ammonia |
| CN111389400B (en) * | 2020-03-23 | 2022-09-27 | 广东石油化工学院 | Preparation method of catalyst for fused salt electrochemical synthesis of ammonia |
| CN114989844A (en) * | 2022-06-09 | 2022-09-02 | 武汉轻工大学 | Method for co-producing high-quality bio-oil and porous graphite carbon by catalytic pyrolysis of biomass and polyolefin plastic |
| CN114989844B (en) * | 2022-06-09 | 2023-06-09 | 武汉轻工大学 | Method for co-production of high-quality bio-oil and porous graphite carbon by catalytic pyrolysis of biomass and polyolefin plastics |
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