CN105118975B - The preparation method of the Zinc oxide nanoparticle lithium ion battery negative material of height ratio capacity - Google Patents

The preparation method of the Zinc oxide nanoparticle lithium ion battery negative material of height ratio capacity Download PDF

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CN105118975B
CN105118975B CN201510422204.9A CN201510422204A CN105118975B CN 105118975 B CN105118975 B CN 105118975B CN 201510422204 A CN201510422204 A CN 201510422204A CN 105118975 B CN105118975 B CN 105118975B
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zinc oxide
oxide nanoparticle
colloidal sol
ion battery
zinc
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CN105118975A (en
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张永光
李海鹏
韦亚琼
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Hebei University of Technology
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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
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • 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
    • 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 present invention is a kind of preparation method of the Zinc oxide nanoparticle lithium ion battery negative material of height ratio capacity, and this method comprises the following steps：（1）It is dissolved at 40 DEG C~75 DEG C of zinc acetate in absolute ethyl alcohol；（2）It is cooled to 0~20 DEG C；（3）Lithium hydroxide crystalline solid is dissolved in absolute ethyl alcohol at room temperature；The mol/L of concentration 0.07~0.2 of gained lithium hydroxide solution；（4）Resulting solution in step 3 is added dropwise in step 2 solution, ultrasonic disperse 1 ~ 7 day obtains colloidal sol；Wherein, mol ratio is zinc acetate：Lithium hydroxide=1.3：1；（5）By colloidal sol eccentric cleaning obtained by step 4, and colloidal sol is dried under the conditions of 50 ~ 100 DEG C obtain Zinc oxide nanoparticle.Not only technical process is simple, cost is low by the present invention, and avoids in each link of preparation technology introducing external contaminant.Zinc oxide nanoparticle obtained by this method has good chemical property.

Description

The preparation method of the Zinc oxide nanoparticle lithium ion battery negative material of height ratio capacity
Technical field
The present invention relates to a kind of preparation of the Zinc oxide nanoparticle lithium ion battery negative material of height ratio capacity, belong to and receive Rice material is prepared and new energy devices field.
Background technology
Lithium ion battery is current to have a wide range of applications in the work, life of people, such as mobile mobile phone, digital phase Occupy critical role in terms of the portable type electronic product such as machine and notebook computer and electric automobile, extensive energy storage device. A key factor for influenceing performance of lithium ion battery is exactly its electrode material, the negative material of current commercial Li-ion battery Typically use graphite.Graphite-structure is stable, the reversible capacity in charge and discharge cycles with stabilization, but graphite cathode material Theoretical specific capacity only has 372mAh g-1, it is difficult to fast-developing electronic equipment is met to the higher and higher energy density of lithium battery It is required that, therefore novel anode material of the development with more height ratio capacity is the study hotspot of current lithium battery.Metal oxide is (such as ZnO, CuO, FeO, NiO etc.) due to being got most of the attention with higher theoretical specific capacity, while researcher has found nano material chi Very little smaller, the relative volume change of material is also smaller during discharge and recharge, can effectively improve battery performance.
Zinc oxide material is 978mAh g as theoretical capacity during lithium ion battery negative material-1, it is the 3 of graphite electrode Times or so, it is considered to be the important replacement of lithium cell cathode material of future generation.And the zinc oxide of nanostructured can give lithium Ion and electronics provide bigger contact area and shorter transmission path, have the nanostructured zinc oxide of excellent properties for this It is one of most promising material of negative electrode of lithium ion battery.
Zinc oxide has high breakdown strength and saturated electrons migration rate, can be used as high temperature, high energy, high-velocity electrons device Part.Zinc oxide also has piezo-electric effect, pyroelectric effect and chemical sensitisation characteristic, there is important application in sensor field.In addition, Zinc oxide has good chemical stability, and Antiradiation injury ability is strong, is potential space application material.
The reaction mechanism of zinc oxide is to be reacted with lithium, is converted into the nano particle and lithia of zinc, subsequent zinc and lithium ion Alloy is formed, the reaction of its reversible electrochemical can be expressed as follows：
The process that nano material is prepared in existing technology is a lot, such as carbothermic method, vapour deposition process, thermal evaporation Method, direct oxidation method, solvent-thermal method, anodic oxidation aluminium formwork electrochemical deposition, hydro-thermal method, sol-gal process etc..But gas The requirement of phase sedimentation is under depositing temperature, and reactant must have sufficiently high vapour pressure；The product of reaction, except required Deposit is that remaining all must be gaseous state outside solid film.Thermal evaporation is not readily available the film of crystalline texture.Colloidal sol-solidifying The key reaction step of glue method is that predecessor is dissolved in solvent into the uniform solution of (water or organic solvent) formation, solute and solvent Produce hydrolysis or alcoholysis reaction, reaction product is gathered into 1nm or so ion and composition solvent, be dried by evaporation be changed into it is solidifying Glue, gel is by drying, sintering curing forms required material.
The Zinc oxide nanoparticle lithium cell cathode material prepared at present needs by (400 DEG C -600 of high temperature process mostly DEG C) [see Chinese invention patent 201410696127；Chinese invention patent 201110419502], low cost, height in a new generation In the research and development of the Zinc oxide nanoparticle lithium cell cathode material of specific capacity, we have proposed a kind of new utilization collosol and gel The method that method prepares Zinc oxide nanoparticle.
The content of the invention
The present invention seeks to the deficiency for current techniques, the one-step hydrolysis method synthesizing zinc oxide nanometer of collosol and gel one is utilized Grain.This method better than be in place of other Traditional Methods can a step make Zinc oxide nanoparticle and be used in negative electrode of lithium ion battery first On material, this method is ultrasonic mixing liquid at room temperature, and accurate measurement, feasibility is high, overcomes sample in heat treatment or calcined Agglomeration in journey, it is most important that the small nano particle of purity height, good dispersion, particle diameter can be made with a step, it is obtained Zinc oxide nanoparticle is uniform in size, about 7nm.Because Zinc oxide nanoparticle size is small made from this method, lithium battery is used as Negative pole, during the deintercalation of lithium, reduces the expansion of volume, so as to maintain the morphosis of material, improves it in lithium Chemical property in ion battery, has very big application prospect on field of lithium ion battery is prepared.Patent of the present invention can be with The uniform nano zine oxide of synthesis particle is prepared under cryogenic conditions (being less than 100 degrees Celsius).
The technical scheme is that：
A kind of preparation method of the Zinc oxide nanoparticle lithium ion battery negative material of height ratio capacity, including following step Suddenly：
(1) zinc acetate is dissolved in absolute ethyl alcohol as presoma at 40 DEG C~75 DEG C, gained acetic acid zinc solution concentration 0.1~0.2mol/L；
(2) solution prepared by step one is by being cooled to 0~20 DEG C；
(3) lithium hydroxide crystalline solid is dissolved in absolute ethyl alcohol at room temperature；The concentration of gained lithium hydroxide solution 0.07~0.2mol/L；
(4) resulting solution in step 3 is added dropwise in step 2 solution, time for adding is 15~30 minutes, then in room The lower ultrasonic disperse of temperature 1~7 day, obtains colloidal sol；Wherein, mol ratio is zinc acetate：Lithium hydroxide=1.3：1；
(5) by colloidal sol eccentric cleaning obtained by step 4, and colloidal sol is dried under the conditions of 50~100 DEG C obtain zinc oxide nano The Zinc oxide nanoparticle lithium ion battery negative material of rice grain, i.e. height ratio capacity.
Beneficial effects of the present invention are：
The Zinc oxide nanoparticle that the present invention is obtained has high specific surface area and relatively short lithium ion solid-state diffusion Path, effectively improves its solid-state diffusion dynamics, increases active material and is contacted with interelectrode, is reduced in battery Resistance, so as to significantly improve the chemical property of battery.Compared with block zinc oxide material, Zinc oxide nanoparticle is used as lithium GND possesses good chemical property.In embodiment 1, as shown in figs. 4 and 5, under 0.1C multiplying power, it puts first Capacitance is up to 1652mAh g-1, and discharge capacity can still keep 318mAh g after 100 circulations-1。
Nano material has the architectural feature and surface characteristic different from block materials, is showed as electrode material of lithium battery Go out obvious advantage, be embodied in：
(l) nano material is relative to block materials, and surface and interface atom proportion is big, and reactivity is high, makes a lot Possibility is able to from the irrealizable reaction of traditional view；
(2) material particle size is small, and the insert depth of lithium ion wherein is shallow, and diffusion path is short, is conducive to lithium ion at it In deintercalation, electrode process has good kinetic property；
(3) high voidage of nano material provides free space for the migration of organic solvent molecule, at the same also to lithium from The intercalation/deintercalation of son provides substantial amounts of space, further improves embedding lithium capacity and energy density；
(4) nano material also has stronger Structural flexibility, can be subjected to deformation and stress caused by electrochemical process, Effectively alleviate the volumetric expansion of non-carbon negative material, reaction invertibity is improved, improve the cycle performance of electrode.
Brief description of the drawings
Fig. 1 is route artwork of the invention；
Fig. 2 is X-ray diffraction (XRD) figure for the Zinc oxide nanoparticle that embodiment 1 is obtained；
Fig. 3 is transmission electron microscope (TEM) figure for the Zinc oxide nanoparticle that embodiment 1 is obtained；
Fig. 4 is that discharge and recharge of the obtained Zinc oxide nanoparticle of embodiment 1 as cathode of lithium battery under 0.1C multiplying powers is bent Line chart；
Fig. 5 is cyclic curve of the obtained Zinc oxide nanoparticle of embodiment 1 as cathode of lithium battery under 0.1C multiplying powers Figure；
Fig. 6 is high rate performance figure of the obtained Zinc oxide nanoparticle of embodiment 1 as cathode of lithium battery.
Embodiment
Embodiment 1
1) 13mmol zinc acetate is placed in 130mL absolute ethyl alcohols, under magnetic stirring 50 DEG C of heating for dissolving；
2) after zinc acetate is completely dissolved, add absolute ethyl alcohol and keep liquor capacity to be 130mL, and be cooled to 10 DEG C；
3) 10mmol crystalline lithium hydroxide is dissolved in 130mL absolute ethyl alcohols by magnetic agitation at room temperature；
4) by step 3) obtained by lithium hydroxide solution be added drop-wise to step 2 under agitation) solution in, drip within 20 minutes Into；
5) disperse above-mentioned mixed liquor 4 days with ultrasonic echography at room temperature, obtain the colloidal sol of white；
6) by colloidal sol centrifugation, the cleaning of gained；
7) it is put at drying box, 60 DEG C and dries 24 hours, obtains the zinc oxide nano of Zinc oxide nanoparticle, i.e. height ratio capacity Rice grain lithium ion battery negative material.
XRD (XRD, smart Lab, the production of Rigaku company) analysis is carried out to prepared product.As shown in Figure 2, Sample belongs to zincite (a=0.3249nm, c=0.5206nm, JCPDS 36-1451).Impurity peaks are not detected, show to close Into obtaining pure oxidized zinc products.Scherrer (Scherre) formula calculates the average crystalline substance of the nano granular of zinc oxide of high degree of dispersion Particle size is 6.8nm.
TEM (TEM, JEM-2100F, the production of Optical Co., Ltd of JEOL) analysis is carried out to prepared sample.Such as the institute of accompanying drawing 3 Show, the ZnO nano particle of synthesis is high degree of dispersion, uniform in size, and its size is about 7nm or so.
Chemical property analysis (BTS-5V5mA, new prestige) is carried out to prepared sample.As shown in figs. 4 and 5, exist Under 0.1C multiplying power, its first discharge capacity up to 1652mAh g-1, and discharge capacity can still keep 318mAh after 100 circulations g-1。
Chemical property analysis (BTS-5V5mA, new prestige) is carried out to prepared sample.As shown in Figure 6,0.5C's Under multiplying power, reversible discharge capacity can also reach 550mAh g after circulating twice-1.Under 1C and 1.5C, reversible discharge amount is respectively 313mAh g-1With 229mAh g-1.When current density drops to 0.5C, reversible discharge amount can still reach 329mAh g-1, this Phenomenon shows that the presence of nano zine oxide improves the high rate performance of electrode composite material really.
Embodiment 2
1) 15mmol zinc acetate is placed in 100mL absolute ethyl alcohols, under magnetic stirring 40 DEG C of heating for dissolving；
2) after zinc acetate is completely dissolved, it is diluted to 100mL again with absolute ethyl alcohol, and be cooled to 10 DEG C；
3) 11.5mmol crystalline lithium hydroxide is dissolved in 150mL absolute ethyl alcohols by magnetic agitation at room temperature；
4) by step 3) obtained by lithium hydroxide solution be added drop-wise to step 2 under agitation) solution in, drip within 25 minutes Into；
5) the above-mentioned mixed liquor of ultrasonic echography is used at room temperature 7 days, obtain the colloidal sol of white；
6) by colloidal sol centrifugation, the cleaning of gained；
7) it is put at drying box, 60 DEG C and dries 24 hours, obtains the zinc oxide nano of Zinc oxide nanoparticle, i.e. height ratio capacity Rice grain lithium ion battery negative material.
Embodiment 3
1) 18mmol zinc acetate is placed in 90mL absolute ethyl alcohols, under magnetic stirring 75 DEG C of heating for dissolving；
2) after zinc acetate is completely dissolved, it is diluted to 90mL again with absolute ethyl alcohol, and be cooled to 0 DEG C；
3) 13.8mmol crystalline lithium hydroxide is dissolved in 150mL absolute ethyl alcohols by magnetic agitation at room temperature；
4) by step 3) obtained by lithium hydroxide solution be added drop-wise to step 2 under agitation) solution in, drip within 25 minutes Into；
5) the above-mentioned mixed liquor of ultrasonic echography is used at room temperature 4 days, obtain the colloidal sol of white；
6) by colloidal sol centrifugation, the cleaning of gained；
7) it is put at drying box, 60 DEG C and dries 24 hours, obtains the zinc oxide nano of Zinc oxide nanoparticle, i.e. height ratio capacity Rice grain lithium ion battery negative material.
Embodiment 4
1) 20mmol zinc acetate is placed in 200mL absolute ethyl alcohols, under magnetic stirring 60 DEG C of heating for dissolving；
2) after zinc acetate is completely dissolved, it is diluted to 200mL again with absolute ethyl alcohol, and be cooled to 20 DEG C；
3) 15.4mmol crystalline lithium hydroxide is dissolved in 100mL absolute ethyl alcohols by magnetic agitation at room temperature；
4) by step 3) obtained by lithium hydroxide solution be added drop-wise to step 2 under agitation) solution in, drip within 16 minutes Into；
5) the above-mentioned mixed liquor of ultrasonic echography is used at room temperature 4 days, obtain the colloidal sol of white；
6) by colloidal sol centrifugation, the cleaning of gained；
7) it is put at drying box, 60 DEG C and dries 24 hours, obtains the zinc oxide nano of Zinc oxide nanoparticle, i.e. height ratio capacity Rice grain lithium ion battery negative material.
Embodiment 5
1) 24mmol zinc acetate is placed in 160mL absolute ethyl alcohols, under magnetic stirring 50 DEG C of heating for dissolving；
2) after zinc acetate is completely dissolved, it is diluted to 160mL again with absolute ethyl alcohol, and be cooled to 20 DEG C；
3) 18.5mmol crystalline lithium hydroxide is dissolved in 100mL absolute ethyl alcohols by magnetic agitation at room temperature；
4) by step 3) obtained by lithium hydroxide solution be added drop-wise to step 2 under agitation) solution in, drip within 16 minutes Into；
5) the above-mentioned mixed liquor of ultrasonic echography is used at room temperature 7 days, obtain the colloidal sol of white；
6) by colloidal sol centrifugation, the cleaning of gained；
7) it is put at drying box, 60 DEG C and dries 24 hours, obtains the zinc oxide nano of Zinc oxide nanoparticle, i.e. height ratio capacity Rice grain lithium ion battery negative material.
In summary, substantive distinguishing features of the invention are the system there is provided the nano structure of zinc oxide under a kind of cryogenic conditions Preparation Method, is a kind of preparation method by sol-gal process synthesizing zinc oxide nanostructured.Collosol and gel rule is fairly simple, The uniformity of molecular level can be obtained in a short period of time, when forming gel, be likely between reactant in molecule It is uniformly mixed in level；Chemical reaction will be carried out easily, and only need relatively low synthesis temperature.This method not only technique Process is simple, cost is low, and avoids in each link of preparation technology introducing external contaminant.Oxidation obtained by this method Zinc nanoparticles have good chemical property.
Unaccomplished matter of the present invention is known technology.

Claims (1)

1. the preparation method of the Zinc oxide nanoparticle lithium ion battery negative material of a kind of height ratio capacity, it is characterized in that including such as Lower step：
（1）Zinc acetate is dissolved in absolute ethyl alcohol as presoma at 40 DEG C~75 DEG C, and gained acetic acid zinc solution concentration 0.1~ 0.2 mol/L；
（2）Solution prepared by step one is by being cooled to 0~20 DEG C；
（3）Lithium hydroxide crystalline solid is dissolved in absolute ethyl alcohol at room temperature；The concentration 0.07 of gained lithium hydroxide solution~ 0.2 mol/L；
（4）Resulting solution in step 3 is added dropwise in step 2 solution, time for adding is 15~30 minutes, then at room temperature Ultrasonic disperse 1 ~ 7 day, obtains colloidal sol；Wherein, mol ratio is zinc acetate：Lithium hydroxide=1.3：1；
（5）By colloidal sol eccentric cleaning obtained by step 4, and colloidal sol is dried under the conditions of 50 ~ 100 DEG C obtain zinc-oxide nano Grain, i.e. the Zinc oxide nanoparticle lithium ion battery negative material of height ratio capacity.
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CN105591090B (en) * 2016-03-04 2018-06-05 河源广工大协同创新研究院 A kind of preparation method of zinc oxide/nitrogen-doped carbon composite material available for negative electrode of lithium ion battery
CN109647584A (en) * 2018-12-10 2019-04-19 桂林理工大学 A kind of sand milling method of modifying of lithium ion battery mineral negative electrode material
CN113809272A (en) * 2020-06-16 2021-12-17 Tcl科技集团股份有限公司 Zinc oxide nano material, preparation method, electron transmission film and light emitting diode

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1686819A (en) * 2005-04-06 2005-10-26 浙江大学 Method for preparing nano granular of zinc oxide in monodisperse
CN1887720A (en) * 2006-07-26 2007-01-03 中国科学院上海硅酸盐研究所 Prepn process of nanometer Zinc oxide powder
CN101628731A (en) * 2009-07-28 2010-01-20 西北工业大学 Zinc oxide nanoparticle preparation method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1686819A (en) * 2005-04-06 2005-10-26 浙江大学 Method for preparing nano granular of zinc oxide in monodisperse
CN1887720A (en) * 2006-07-26 2007-01-03 中国科学院上海硅酸盐研究所 Prepn process of nanometer Zinc oxide powder
CN101628731A (en) * 2009-07-28 2010-01-20 西北工业大学 Zinc oxide nanoparticle preparation method

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