CN104157853B - A kind of negative material, its preparation method and application - Google Patents
A kind of negative material, its preparation method and application Download PDFInfo
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- CN104157853B CN104157853B CN201410362731.0A CN201410362731A CN104157853B CN 104157853 B CN104157853 B CN 104157853B CN 201410362731 A CN201410362731 A CN 201410362731A CN 104157853 B CN104157853 B CN 104157853B
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- 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
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- 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
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- H—ELECTRICITY
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- 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
- H01M4/5835—Comprising fluorine or fluoride salts
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- 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 kind of negative material, comprise the Zinc oxide particles being coated with carbon-coating and the zinc ferrite particle being coated with carbon-coating, the granularity of Zinc oxide particles and zinc ferrite particle is all less than 5nm, the thickness of carbon-coating is 1 ~ 2nm, the Zinc oxide particles being coated with carbon-coating and the zinc ferrite particle packing being coated with carbon-coating form composite particles, in described composite particles, the weight ratio of Zinc oxide particles and zinc ferrite particle is 0.35 ~ 0.4:1, the granularity of composite particles is 100 ~ 300nm, forms hole between the Zinc oxide particles being coated with carbon-coating and the zinc ferrite particle being coated with carbon-coating.The hollow octahedra negative material specific capacity of the carbon that the present invention prepares coated zinc-base composite oxide is high, good rate capability, good cycling stability.
Description
Technical field
The present invention relates to field of lithium ion battery, be specifically related to a kind of negative material, its preparation method and application.
Background technology
Lithium ion battery has had the advantages such as high-energy-density, high working voltage, memory-less effect due to it and is used widely since commercialization.But along with the increase of the demand to the large-scale energy storage device stored for novel energy, the energy density of traditional commercial Li-ion batteries and power density can not satisfy the demands, exploitation has high power capacity, powerful battery material is extremely urgent.Current commercial lithium ion battery negative material adopts specific capacity to be the graphite material of 372mAh/g, although it has good cycle performance, but its specific capacity is lower, and easily produce potential safety hazard under high current charge-discharge condition, limit its application in extensive energy storage field.
Zinc-base ternary compound oxides has high power capacity, lower-price characteristic and being widely studied because of it.But it is subject to storing up the restriction that there is volumetric expansion in lithium process, researcher often adopts carbon-based material to carry out compound with it, and complex method is usually comparatively complicated, can not meet the requirement of industrialization large-scale production.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of preparation method of loose structure negative material, the electrode slice containing this negative material and containing the button cell of this electrode slice are provided, solve the problem that current negative material finite capacity, high rate performance are low, can not carry out suitability for industrialized production on a large scale.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of negative material, comprise the Zinc oxide particles being coated with carbon-coating and the zinc ferrite particle being coated with carbon-coating, the granularity of Zinc oxide particles and zinc ferrite particle is all less than 5nm, the thickness of carbon-coating is 1 ~ 2nm, the Zinc oxide particles being coated with carbon-coating and the zinc ferrite particle packing being coated with carbon-coating form composite particles, in described composite particles, the weight ratio of Zinc oxide particles and zinc ferrite particle is 0.35 ~ 0.4:1, the granularity of composite particles is 100 ~ 300nm, forms hole between the Zinc oxide particles being coated with carbon-coating and the zinc ferrite particle being coated with carbon-coating.
A preparation method for the hollow octahedra negative material of carbon coated zinc-base composite oxide of loose structure, comprises the following steps:
1) reaction precursor liquid is prepared: component A be dissolved in B component and make reaction precursor liquid; Wherein component A comprises following raw material by ratio of weight and the number of copies: zinc nitrate 14 ~ 15 parts, ferric acetyl acetonade 18 ~ 20 parts, terephthalic acid (TPA) 2 ~ 3 parts, molecular weight are the polyvinylpyrrolidone 63 ~ 64 parts of 30000 ~ 60000; B component is be the N of 4:3 ~ 2:1 preparation by volume, the mixed liquor of N – dimethyl formamide and ethanol; In the reaction precursor liquid of preparation, nitric acid zinc concentration is 3.43 ~ 3.53g/L;
2) by step 1) the reaction precursor liquid prepared refluxes 3 ~ 24 hours at 95 ~ 105 DEG C, product is used N respectively, in 60 ~ 120 DEG C of oven dry after N – dimethyl formamide and ethanol cyclic washing, obtain the metal-organic framework material with hollow octahedral structure;
3) metal-organic framework material after oven dry is risen to 500 ~ 600 DEG C with the heating rate of 0.5 ~ 3 DEG C/min in nitrogen atmosphere, naturally cool to room temperature immediately and can obtain negative material, it is Powdered for drying the product obtained.
A kind of electrode slice, comprises following raw material by ratio of weight and the number of copies:
Negative material 40 ~ 80 parts; Conductive black 10 ~ 40 parts; Lithium polyacrylate binding agent 10 ~ 20 parts.
A kind of button cell, comprises above-mentioned electrode slice.
The invention has the beneficial effects as follows:
1. the negative material specific capacity prepared is high, good rate capability;
2. the negative material good cycling stability prepared, coulombic efficiency is high first;
3. the negative material prepared has loose structure, and metal oxide surface carbon coating layer evenly and be interconnected to form 3D network, improves electrical conductivity performance and the ionic conduction performance of active material, inhibits bulk effect;
4. preparation method is simple, is applicable to large-scale production.
Accompanying drawing explanation
In Fig. 1, (a), (b) are field emission scanning electron microscope (FSEM) figure and transmission electron microscope (TEM) figure of the metal-organic framework material (MOF) of synthesis respectively.C (), (d) are FSEM figure and the TEM figure of the hollow octahedra negative material of carbon coated zinc-base composite oxide that metal-organic framework material (MOF) obtains after heat treatment in 500 DEG C of nitrogen respectively, (e), (f) are constituency high resolution transmission electron microscopy (HRTEM) figure;
Fig. 2 is X-ray diffraction (XRD) collection of illustrative plates of the hollow octahedra negative material of carbon coated zinc-base composite oxide;
Fig. 3 (a), (b) are nitrogen adsorption desorption curve and the graph of pore diameter distribution of the hollow octahedra negative material of carbon coated zinc-base composite oxide respectively;
Fig. 4 is the cyclic voltammetry curve of the hollow octahedra negative material of carbon coated zinc-base composite oxide, test specification 3-0.005V, sweep speed 0.2mV/s;
Fig. 5 is the charging and discharging curve figure of the hollow octahedra negative material of carbon coated zinc-base composite oxide under current density is 0.5A/g;
Fig. 6 is the cycle performance figure of the hollow octahedra negative material of carbon coated zinc-base composite oxide under current density 0.5A/g and 2A/g current density;
Fig. 7 is high rate performance and the cycle performance figure of electrode slice containing the hollow octahedra negative material of carbon coated zinc-base composite oxide.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.In addition, if below in described each execution mode of the present invention involved technical characteristic do not form conflict each other and just can mutually combine.
Embodiment one
The first step, preparation reaction precursor liquid: component A is dissolved in B component and makes reaction precursor liquid; Wherein component A comprises following raw material by ratio of weight and the number of copies: zinc nitrate 14 ~ 15 parts, ferric acetyl acetonade 18 ~ 20 parts, terephthalic acid (TPA) 2 ~ 3 parts, molecular weight are 30000 ~ 60000 polyvinylpyrrolidone 63 ~ 64 parts; B component is be the N of 4:3 ~ 2:1 preparation by volume, the mixed liquor of N – dimethyl formamide and ethanol; In the reaction precursor liquid be mixed with, nitric acid zinc concentration is 3.43 ~ 3.53g/L.
Preferred as above-mentioned number range, the ratio of weight and number of each raw material of component A is respectively: zinc nitrate can be 14.6 ~ 14.7 parts, ferric acetyl acetonade is 18.9 ~ 19.1 parts, terephthalic acid (TPA) is 2.9 ~ 3.1 parts, polyvinylpyrrolidone is 63 ~ 63.5 parts.
The present embodiment is preferred N further, the volume 300mL of N – dimethyl formamide (DMF), the volume 180mL of ethanol, after the two is mixed, add in mixed liquor again 1.67 grams of zinc nitrates, 2.16 grams of ferric acetyl acetonades, 0.34 gram of terephthalic acid (TPA) and 7.2 grams molecular weight be 55000 polyvinylpyrrolidone (PVP), stir and form orange-red reaction precursor liquid (polyvinylpyrrolidone added, ferric acetyl acetonade, zinc nitrate and terephthalic acid (TPA) are solid).In the reaction precursor liquid of preparation, the concentration of PVP is about 15g/L, and nitric acid zinc concentration is about 3.48g/L, and the concentration of ferric acetyl acetonade is about 4.5g/L, and the concentration of terephthalic acid (TPA) is about 0.71g/L.
Second step, refluxes reaction precursor liquid 3 ~ 24 hours, product is used N respectively at 95 ~ 105 DEG C, in 60 ~ 120 DEG C of oven dry after N – dimethyl formamide and ethanol cyclic washing, obtains the metal-organic framework material with hollow octahedral structure.
Preferred as above-mentioned number range, by reaction precursor liquid 99 ~ 101 DEG C of backflows 4 ~ 8 hours, can use N, in 60 ~ 120 DEG C of oven dry after N – dimethyl formamide and ethanol respectively wash 2 ~ 4 times respectively.
The present embodiment is preferred further to reflux reaction precursor liquid 6 hours at 100 DEG C, by the product centrifugation obtained, respectively washs with DMF and ethanol and is placed on 80 DEG C of oven dry for 3 times.
3rd step, is placed in tube furnace by the metal-organic framework material after drying, in nitrogen atmosphere, rises to 500 ~ 600 DEG C with the heating rate of 0.5 ~ 3 DEG C/min.
Preferred as above-mentioned number range, can be raised to 500 ~ 550 DEG C with the heating rate of 0.5 ~ 1.5 DEG C/min in nitrogen atmosphere.
The present embodiment preferably rises to 500 DEG C with the heating rate of 1 DEG C/min further in a nitrogen atmosphere, without the need to insulation, directly naturally cools to room temperature, can obtain the hollow octahedra negative material of carbon coated zinc-base composite oxide.
This negative material comprises the Zinc oxide particles being coated with carbon-coating and the zinc ferrite particle being coated with carbon-coating, the granularity of Zinc oxide particles and zinc ferrite particle is all less than 5nm, the thickness of carbon-coating is 1 ~ 2nm, the Zinc oxide particles being coated with carbon-coating and the zinc ferrite particle packing being coated with carbon-coating form composite particles, in described composite particles, the weight ratio of Zinc oxide particles and zinc ferrite particle is 0.35 ~ 0.4:1, the granularity of composite particles is 100 ~ 300nm, forms hole between the Zinc oxide particles being coated with carbon-coating and the zinc ferrite particle being coated with carbon-coating.
The shape of composite particles is hollow octahedral structure, the Zinc oxide particles being coated with carbon-coating and be coated with carbon-coating zinc ferrite particle packing after, form a lot of hole between particle, make octahedral structure be loose structure.
The hollow octahedra negative material of the coated zinc-base of the carbon with loose structure composite oxide prepared by said method has remarkable storage lithium performance, is a kind of desirable negative material.
Fig. 1 (a) is the FSEM figure of the metal-organic framework material (MOF) obtained, can observe that from figure it is the octahedral structure of particle diameter about 200nm clearly, can find out that it has obvious hollow-core construction from TEM figure (Fig. 1 (b)).And can confirm that metal-organic framework material (MOF) still can keep initial octahedral structure after Overheating Treatment in Fig. 1 (c) and Fig. 1 (d).Can be seen clearly by the high-resolution TEM figure of Fig. 1 (e) and be dispersed with in the grain edges of metal oxide the carbon-coating that one deck is about about 1nm equably.Fig. 1 (f) then shows metal oxide particle size and is less than 5nm.
Be the XRD figure of the hollow octahedra negative material of carbon coated zinc-base composite oxide in Fig. 2, determine that this sample is mainly made up of zinc oxide and zinc ferrite two kinds of components.
The specific area that can calculate the hollow octahedra negative material of carbon coated zinc-base composite oxide from the adsorption desorption curve of Fig. 3 is about 140m
2/ g, the pore size of formation differs, and the size of hole is mainly distributed in about 7.5nm.
Hollow for coated for carbon obtained above zinc-base composite oxide octahedra negative material is mixed by the weight ratio of 70:15:15 with conductive black, Lithium polyacrylate binding agent, through colding pressing, die-cutly makes electrode slice.Using metal lithium sheet as to electrode, with the LiPF of 1mol/L
6/ EC+DMC is electrolyte, and charging/discharging voltage scope is 3.0 ~ 0.001V.
Fig. 4 is the cyclic voltammetry curve figure of the electrode slice containing the hollow octahedra negative material of carbon coated zinc-base composite oxide.In cathodic scan process first, be the obvious reduction peak in 0.75V place appearance one place at voltage, it corresponds to the decomposition of the decomposition of electrolyte and the formation of SEI film and zinc oxide and zinc ferrite.The reduction peak occurred at 0.2V place subsequently corresponds to the alloy reaction of Li-Zn.In anodic scan process subsequently, the oxidation peak at 1.6V place corresponds to the oxidation reaction of Zn and Fe.From second week scanning, the reduction peak of first circle 0.75V is moved to 0.87V, and all the other peak positions and intensity are almost constant, embodies the electrochemical reaction of this material in storage lithium process and has high reversible.
Fig. 5 is the charging and discharging curve figure of the hollow octahedra negative material of carbon coated zinc-base composite oxide under current density is 0.5A/g.As can be seen from the curve of Fig. 5, in discharge process first, a discharge platform can be observed at 0.75V place, corresponded to ZnFe
2o
4be decomposed into Zn, Fe and Li
2o, its first charge-discharge capacity is respectively 1047 and 1385mAh/g, and coulombic efficiency is up to 75.6%.
Fig. 6 contains the cycle performance figure of electrode slice under the electric current of 500mA/g and 2A/g of the hollow octahedra negative material of carbon coated zinc-base composite oxide, experience put for 100 times-charging cycle after, capacity still can keep 1390mAh/g and 988mAh/g.Meanwhile, it still shows storage lithium ability free from worldly cares under high current density.
As shown in Figure 7, it still has the reversible capacity up to 762mAh/g under the condition of current density 10A/g (namely completing charging process in 5 minutes), embodies outstanding high rate performance.
Below in conjunction with a comparative example, the effect of the sample obtained in comparative example with the hollow octahedra negative material of carbon coated zinc-base composite oxide utilizing the method for the embodiment of the present invention one to prepare is contrasted.
Comparative example:
Comparative example is that the metal-organic framework material (MOF) first two steps of embodiment one obtained heat-treats with identical program in air atmosphere that (programming rate 1 DEG C/min rises to 500 DEG C, naturally cool to room temperature), the hollow octahedra negative material of the zinc-base composite oxide obtaining not having carbon coated.The negative material of comparative example gained is assembled into button cell by the mode identical with embodiment one, test electrical property.
Table 1 contrasts containing the button cell electrical property of embodiment one with comparative example negative material
In sum, the hollow octahedra negative material of carbon coated zinc-base composite oxide that the preparation method proposed according to the present invention prepares has excellent capacity and cycle performance, and preparation method is simple, is applicable to large-scale production.
It should be noted that, according to the above description the announcement of book and elaboration, those skilled in the art in the invention can also change above-mentioned execution mode and revise.Therefore, the present invention is not limited to embodiment disclosed and described above, also should in the protection range of claim of the present invention to equivalent modifications more of the present invention and change.In addition, although employ some specific terms in this specification, these terms just for convenience of description, do not form any restriction to the present invention.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. prepare the method for negative material for one kind, this negative material comprises the Zinc oxide particles being coated with carbon-coating and the zinc ferrite particle being coated with carbon-coating, the granularity of Zinc oxide particles and zinc ferrite particle is all less than 5nm, the thickness of carbon-coating is 1 ~ 2nm, the Zinc oxide particles being coated with carbon-coating and the zinc ferrite particle packing being coated with carbon-coating form composite particles, in described composite particles, the weight ratio of Zinc oxide particles and zinc ferrite particle is 0.35 ~ 0.4:1, the granularity of composite particles is 100 ~ 300nm, hole is formed between the Zinc oxide particles being coated with carbon-coating and the zinc ferrite particle being coated with carbon-coating, it is characterized in that:
Said method comprising the steps of:
1) reaction precursor liquid is prepared: component A be dissolved in B component and make reaction precursor liquid; Wherein component A comprises following raw material by ratio of weight and the number of copies: zinc nitrate 14 ~ 15 parts, ferric acetyl acetonade 18 ~ 20 parts, terephthalic acid (TPA) 2 ~ 3 parts, molecular weight are the polyvinylpyrrolidone 63 ~ 64 parts of 30000 ~ 60000; B component is be the N of 4:3 ~ 2:1 preparation by volume, the mixed liquor of N – dimethyl formamide and ethanol; In the reaction precursor liquid of preparation, nitric acid zinc concentration is 3.43 ~ 3.53g/L;
2) by step 1) the reaction precursor liquid prepared refluxes 3 ~ 24 hours at 95 ~ 105 DEG C, product is used N respectively, in 60 ~ 120 DEG C of oven dry after N – dimethyl formamide and ethanol cyclic washing, obtain the metal-organic framework material with hollow octahedral structure;
3) metal-organic framework material after oven dry is risen to 500 ~ 600 DEG C with the heating rate of 0.5 ~ 3 DEG C/min in nitrogen atmosphere, naturally cool to room temperature immediately.
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| CN106975489B (en) * | 2017-04-26 | 2019-12-31 | 浙江大学 | Preparation method of nickel oxide in-situ coated graphene nanocomposite |
| CN107611361B (en) * | 2017-07-26 | 2020-09-22 | 华南理工大学 | Nickel ferrite/carbon lithium ion battery nano composite negative electrode material with fusiform structure and preparation method and application thereof |
| CN107611425B (en) * | 2017-07-26 | 2020-09-22 | 华南理工大学 | Fusiform zinc ferrite/carbon lithium ion battery nano composite negative electrode material and preparation method and application thereof |
| CN107611362B (en) * | 2017-07-26 | 2020-09-22 | 华南理工大学 | Manganese ferrite/carbon lithium ion battery nano composite negative electrode material and preparation method and application thereof |
| CN107611363B (en) * | 2017-07-26 | 2020-09-22 | 华南理工大学 | Spindle-shaped cobalt ferrite/carbon lithium ion battery nano composite negative electrode material and preparation method and application thereof |
| CN107364897A (en) * | 2017-08-17 | 2017-11-21 | 大连理工大学 | A kind of preparation method of ferrous acid zinc nano material |
| CN111564610B (en) * | 2020-04-03 | 2021-06-08 | 华南师范大学 | Carbon-coated cuprous phosphide-copper composite particle modified by carbon nanotube and preparation method and application thereof |
| CN111584870A (en) * | 2020-05-15 | 2020-08-25 | 昆山宝创新能源科技有限公司 | Negative electrode material, preparation method thereof and battery |
| CN113707467A (en) * | 2021-09-10 | 2021-11-26 | 安徽工业大学 | MOF-derived ZnO @ C cubic electrode material, and preparation method and application thereof |
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| CN101759146A (en) * | 2010-01-20 | 2010-06-30 | 浙江师范大学 | Method for preparing ZnO/ZnFe2O4 compound nano hollow sphere |
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