CN103594725B - A kind of lithium ion battery solid electrolyte material Li 7la 3zr 2o 12preparation method - Google Patents

A kind of lithium ion battery solid electrolyte material Li 7la 3zr 2o 12preparation method Download PDF

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CN103594725B
CN103594725B CN201210292370.8A CN201210292370A CN103594725B CN 103594725 B CN103594725 B CN 103594725B CN 201210292370 A CN201210292370 A CN 201210292370A CN 103594725 B CN103594725 B CN 103594725B
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CN103594725A (en
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付正伟
吕豪杰
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Wanxiang 123 Co Ltd
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Wanxiang Electric Vehicle Co Ltd
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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
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562—Solid materials
    • 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

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Abstract

The present invention relates to a kind of electrolyte, especially relate to a kind of lithium ion battery solid electrolyte material Li 7la 3zr 2o 12preparation method, be intended to solve the operating condition harshness of prior art preparation method, processed complex, deficiency that production cost is high, this preparation method comprises the following steps: raw material ball milling in decentralized medium to mix; Drying and grinding obtains predecessor, and predecessor mixes precalcining with glucose or sucrose; Predecessor after precalcining is ball-milling treatment in decentralized medium again; Then mix after calcining with glucose or sucrose and grind to obtain Li 7la 3zr 2o 12finished product.The method is carried out under normal pressure, air atmosphere, and operating condition is gentle, processing is simple, production cost is low, obtained Li 7la 3zr 2o 12good stability, conductivity is high, and Charge-transfer resistance reduces.

Description

A kind of lithium ion battery solid electrolyte material Li 7la 3zr 2o 12preparation method
Technical field
The present invention relates to a kind of electrolyte, especially relate to a kind of lithium ion battery solid electrolyte material Li 7la 3zr 2o 12preparation method.
Background technology
Lithium ion battery has higher energy density and power density, be widely used in mobile phone, notebook computer and digital camera field, along with the continuous prosperity of national economy and the continuous lifting of modern science and technology level, lithium ion battery extends its application again greatly at society, proposes more harsh Yu high-end requirement again with stylish service condition to lithium ion battery.At present, what the lithium ion battery of extensive use on market adopted is electrolyte that is liquid or gel state, both common ground are the use of inflammable and explosive organic substance and have certain mobility, this brings potential safety hazard to the use of lithium ion battery, battery can leak owing to encapsulating bad under certain conditions, or blast when temperature raises, poor stability, simultaneously for some specific occasion, as provided energy for superintegrated small-sized electronic product, new requirement is proposed to lithium ion battery technology.Solid electrolyte material is due to physics, the chemical property of self uniqueness, fail safe is good, solid electrolyte material generally has good thermal stability and machining property simultaneously, can meet a lot of harsh environmental requirement and service condition, therefore the research and development of lithium ion battery solid electrolyte material have a great deal of practical meanings.
Chinese patent publication date on August 8th, 2007, publication number CN101013761A, disclose a kind of for solid lithium battery solid electrolyte material material system and preparation method, this solid electrolyte material material is Li2S and other sulfide B/S(B/S=SiS 2, PS 5/2, GeS 2, BS 3/2) and iodide A/I(A/I=AII 3, ZnI 2, LaI 3) several different compound is combined with each other according to certain mol ratio; form diluted system; for lithium ion transport provides space; thus obtain higher ionic conductivity; and material has wider thermally-stabilised scope (room temperature ~ 200 DEG C); described solid electrolyte material under vacuum solid phase reaction then quench after ball milling obtain, ball milling carries out under argon shield.Weak point is: need to carry out under vacuum and argon shield, and operating condition is harsh, processed complex, and production cost is high, and obtained electrolyte self structure poor stability, reacts with water in atmosphere and can produce the hydrogen sulfide of gaseous state.
Summary of the invention
The object of the invention is to solve that operating condition harshness of prior art preparation method, processed complex, production cost are high, the deficiency of electrolyte self structure poor stability, provide that a kind of operating condition is gentle, processing simply, the lithium ion battery solid electrolyte material Li of low, the electrolyte self structure good stability of production cost 7la 3zr 2o 12preparation method.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of lithium ion battery solid electrolyte material Li 7la 3zr 2o 12preparation method, described preparation method comprises the following steps:
1) be that Li source compound, lanthanum source compound and zirconium source compound are mixed thoroughly to be placed in decentralized medium and carried out ball milling mixing by 7 ~ 8:3:2 according to the mol ratio of Li, La and Zr;
2) mixture that obtains of step 1) dry 8 ~ 12h under 95 ~ 105 DEG C of conditions, then grind into powder obtains predecessor, and predecessor is mixed rear precalcining with glucose or sucrose, and precalcining temperature is 500 ~ 800 DEG C, and the time is 12 ~ 24 hours;
3) predecessor after precalcining is scattered in decentralized medium carries out ball-milling treatment again, then mix rear calcining with glucose or sucrose, then grind to obtain Li 7la 3zr 2o 12sample, calcining heat is 600 ~ 900 DEG C, and the time is 24 ~ 36 hours.
The present invention will be by preparing raw material ball milling mixing in decentralized medium of solid electrolyte material, and then dry also grind into powder, raw material high uniformity is disperseed, and solid phase reaction speed during subsequent calcination is homogeneous, obtained Li 7la 3zr 2o 12solid electrolyte material homogeneity is good, and mixed with glucose or sucrose by the raw material of high degree of dispersion before precalcining and calcining, with glucose or sucrose for carbon source, calcining heat is low, calcines effective, the Li obtained 7la 3zr 2o 12solid electrolyte material Charge-transfer resistance reduces, and the present invention carries out in condition of normal pressure, air atmosphere, and calcining heat is lower, and operating condition is gentle, and processing is simple, obtained Li 7la 3zr 2o 12solid electrolyte material cost is low.
As preferably, in step 1), Li source compound is selected from the one in lithium acetate, lithium carbonate, lithium oxalate, lithium hydroxide, and lanthanum source compound is selected from least one in lanthana and lanthanum hydroxide, and zirconium source compound is selected from the one in zirconia, zirconium hydroxide.Preferred Li source compound, lanthanum source compound and zirconium source compound wide material sources, be easy to obtain, and is easy to store.
As preferably, the decentralized medium in step 1) and step 3) is deionized water, ethanol or acetone.Preferred dispersion medium performance is good, and after stock dispersion, during follow-up drying, decentralized medium can not remain, and does not affect the purity of raw material.
As preferably, in step 1), the drum's speed of rotation of ball milling mixing is 200 ~ 500rpm, and the time is 12 ~ 24 hours.Ball milling good mixing effect, simple to operate.
As preferably, in step 3), the drum's speed of rotation of ball-milling treatment is 300 ~ 500rpm again, and the time of ball-milling treatment is 24 ~ 36 hours again.Ball-milling treatment is effective, simple to operate.
As preferably, step 2) in the consumption of glucose or sucrose be 10 ~ 60% of predecessor quality.Glucose or dosage of sucrose rationally, are calcined effective, obtained Li 7la 3zr 2o 12solid electrolyte material Charge-transfer resistance reduces.
As preferably, in step 3), the consumption of glucose or sucrose is 20 ~ 50% of predecessor quality.Glucose or dosage of sucrose rationally, are calcined effective, obtained Li 7la 3zr 2o 12solid electrolyte material Charge-transfer resistance reduces.
The invention has the beneficial effects as follows: (1) solid phase reaction of the present invention speed is homogeneous, obtained Li 7la 3zr 2o 12solid electrolyte material homogeneity is good; (2) the present invention adopts sucrose or glucose to be carbon source, and calcining heat is low, calcines effective, obtained Li 7la 3zr 2o 12solid electrolyte material Charge-transfer resistance reduces; (3) the electrolyte good stability that obtains of the present invention, conductance is high, simple to operate, and production cost is low, is easy to industrial-scale production.
Accompanying drawing explanation
Fig. 1 is solid electrolyte material Li prepared by the present invention 7la 3zr 2o 12xRD figure;
Fig. 2 is pure phase solid electrolyte material Li prepared by the present invention 7la 3zr 2o 12sEM figure.
Embodiment
Below by specific embodiment, and by reference to the accompanying drawings, technical scheme of the present invention is described in further detail.
embodiment 1:
1) be that 7:3:2 takes respectively after lithium hydroxide 2.9385g, lanthana 4.8876g and zirconia 2.4644g mix thoroughly and adds in 250ml ball grinder according to the mol ratio of Li, La, Za, add deionized water, ratio of grinding media to material is 10:1, and at normal temperatures, the drum's speed of rotation ball milling of 200rpm mixes 24 hours;
2) baking oven mictoplasm obtained being placed in 105 DEG C carries out drying, and the time is 8 hours; Then grinding obtains Powdered predecessor, predecessor add 1.03g glucose (10% of predecessor quality) mix after precalcining 24 hours in air atmosphere in tube furnace, precalcining temperature is 500 DEG C;
3)predecessor after precalcining is put into the ball grinder of 250ml, add deionized water, ratio of grinding media to material is 10:1, the drum's speed of rotation ball milling of 300rpm mixes 36 hours at normal temperatures, then in tube furnace, 36 hours are sintered under air atmosphere after mixing with 5.2g glucose (50% of predecessor quality), sintering temperature is 600 DEG C, and obtained powder mull is obtained Li 7la 3zr 2o 12sample.
embodiment 2:
1) be that 8:3:2 takes respectively after lithium acetate 5.2792g, lanthanum hydroxide 5.697g and zirconium hydroxide 3.189g mix thoroughly and adds in 250ml ball grinder according to the mol ratio of Li, La, Za, add deionized water, ratio of grinding media to material is 10:1, and at normal temperatures, the drum's speed of rotation ball milling of 500rpm mixes 12 hours;
2) baking oven mictoplasm obtained being placed in 95 DEG C carries out drying, and the time is 12 hours; Then grinding obtains Powdered predecessor, predecessor add 8.49g glucose (60% of predecessor quality) mix after precalcining 12 hours in air atmosphere in tube furnace, precalcining temperature is 800 DEG C;
3) predecessor after precalcining is put into the ball grinder of 250ml, add deionized water, ratio of grinding media to material is 10:1, the drum's speed of rotation ball milling of 500rpm mixes 24 hours at normal temperatures, then in tube furnace, 24 hours are sintered under air atmosphere after mixing with 2.83g sucrose (20% of predecessor quality), sintering temperature is 900 DEG C, and obtained powder mull is obtained Li 7la 3zr 2o 12sample.
embodiment 3:
1) be that 7.5:3:2 takes respectively after lithium carbonate 2.771g, lanthana 3.258g, lanthanum hydroxide 1.899g and zirconia 2.4644g mix thoroughly and adds in 250ml ball grinder according to the mol ratio of Li, La, Za, add deionized water, ratio of grinding media to material is 10:1, at normal temperatures, the drum's speed of rotation ball milling of 350rpm mixes 18 hours;
2) baking oven mictoplasm obtained being placed in 100 DEG C carries out drying, and the time is 10 hours; Then grinding obtains Powdered predecessor, predecessor add 3.637g sucrose (35% of predecessor quality) mix after precalcining 18 hours in air atmosphere in tube furnace, precalcining temperature is 650 DEG C;
3) predecessor after precalcining is put into the ball grinder of 250ml, add deionized water, ratio of grinding media to material is 10:1, the drum's speed of rotation ball milling of 400rpm mixes 30 hours at normal temperatures, in tube furnace, 30 hours are sintered under air atmosphere after being mixed with 3.637g sucrose (35% of predecessor quality) by the powder obtained, sintering temperature is 750 DEG C, and obtained powder mull is obtained Li 7la 3zr 2o 12sample.
embodiment 4:
1) be that 7.5:3:2 takes respectively after lithium oxalate 3.821g, lanthana 1.629g, lanthanum hydroxide 3.798g and zirconia 2.4644g mix thoroughly and adds in 250ml ball grinder according to the mol ratio of Li, La, Za, add deionized water, ratio of grinding media to material is 10:1, at normal temperatures, the drum's speed of rotation ball milling of 350rpm mixes 18 hours;
2) baking oven mictoplasm obtained being placed in 100 DEG C carries out drying, and the time is 10 hours; Then grinding obtains Powdered predecessor, predecessor add 4.099g sucrose (35% of predecessor quality) mix after precalcining 18 hours in air atmosphere in tube furnace, precalcining temperature is 650 DEG C;
3) predecessor after precalcining is put into the ball grinder of 250ml, add deionized water, ratio of grinding media to material is 10:1, the drum's speed of rotation ball milling of 400rpm mixes 30 hours at normal temperatures, in tube furnace, 30 hours are sintered under air atmosphere after being mixed with 4.099g sucrose (35% of predecessor quality) by the powder obtained, sintering temperature is 750 DEG C, and obtained powder mull is obtained Li 7la 3zr 2o 12sample.
Li 7la 3zr 2o 12properties of sample measurement result:
1) Fig. 1 is the solid electrolyte material Li that the present invention prepares gained 7la 3zr 2o 12xRD collection of illustrative plates, as shown in Figure 1, the solid electrolyte material Li that the present invention obtains 7la 3zr 2o 12with Li 7la 3zr 2o 12standard sample is compared has similar vertical direction structure, and Fig. 2 is the pure phase solid electrolyte material Li that the present invention obtains 7la 3zr 2o 12sEM figure.
2) the solid electrolyte material Li that obtains of the present invention 7la 3zr 2o 12total ionic conductivity at room temperature measured by electrochemical impedance spectral method, primary test parameter is: alternating voltage amplitude 5 ~ 20mV, frequency range 40Hz ~ 110MHz(electric impedance analyzer), the electrochemical impedance data obtained entered to calculate the total conductivity of sample, the blocking electrode utilizing electric impedance analyzer to measure sample resistance is Au electrode, the solid electrolyte material Li that embodiment 1 ~ 4 is obtained 7la 3zr 2o 12total conductivity in table 1
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4
Total ionic conductivity 2.0×10 -4Scm -1 2.1×10 -4Scm -1 2.05×10 -4Scm -1 2.14×10 -4Scm -1
3) in atmosphere under room temperature to the solid electrolyte material Li that the present invention obtains 7la 3zr 2o 12chemical stability study, in atmosphere place 15 days, then measure conductivity over time, test result show ontology resistance components is constant, shows solid electrolyte material Li 7la 3zr 2o 12good at air at room temperature stability inferior.
Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.

Claims (5)

1. a lithium ion battery solid electrolyte material Li 7la 3zr 2o 12preparation method, it is characterized in that, described preparation method comprises the following steps:
1) be that Li source compound, lanthanum source compound and zirconium source compound are mixed thoroughly to be placed in decentralized medium and carried out ball milling mixing by 7 ~ 8:3:2 according to the mol ratio of Li, La and Zr;
2) mixture that obtains of step 1) dry 8 ~ 12h under 95 ~ 105 DEG C of conditions, then grind into powder obtains predecessor, and predecessor is mixed rear precalcining with glucose or sucrose, and precalcining temperature is 500 ~ 800 DEG C, and the time is 12 ~ 24 hours; The consumption of glucose or sucrose is 10 ~ 60% of predecessor quality;
3) predecessor after precalcining to be scattered in decentralized medium ball-milling treatment again, then to mix rear calcining with glucose or sucrose, then grind to obtain Li 7la 3zr 2o 12sample, calcining heat is 600 ~ 900 DEG C, and the time is 24 ~ 36 hours; The consumption of glucose or sucrose is 20 ~ 50% of the predecessor quality after precalcining.
2. a kind of lithium ion battery solid electrolyte material Li according to claim 1 7la 3zr 2o 12preparation method, it is characterized in that, in step 1), Li source compound is selected from the one in lithium acetate, lithium carbonate, lithium oxalate, lithium hydroxide, and lanthanum source compound is selected from least one in lanthana and lanthanum hydroxide, and zirconium source compound is selected from the one in zirconia, zirconium hydroxide.
3. a kind of lithium ion battery solid electrolyte material Li according to claim 1 7la 3zr 2o 12preparation method, it is characterized in that: the decentralized medium in step 1) and step 3) is deionized water, ethanol or acetone.
4. a kind of lithium ion battery solid electrolyte material Li according to claim 1 or 2 or 3 7la 3zr 2o 12preparation method, it is characterized in that: in step 1) ball milling mixing drum's speed of rotation be 200 ~ 500rpm, ball milling mixing time be 12 ~ 24 hours.
5. a kind of lithium ion battery solid electrolyte material Li according to claim 1 or 2 or 3 7la 3zr 2o 12preparation method, it is characterized in that: in step 3), the drum's speed of rotation of ball-milling treatment is 300 ~ 500rpm again, the time of ball-milling treatment is 24 ~ 36 hours again.
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