CN103594725A - Preparation method of lithium ion battery solid electrolyte material Li7La3Zr2O12 - Google Patents
Preparation method of lithium ion battery solid electrolyte material Li7La3Zr2O12 Download PDFInfo
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- 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
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- 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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Abstract
The invention relates to a lithium ion battery solid electrolyte material, and especially relates to a preparation method of the lithium ion battery solid electrolyte material Li7La3Zr2O12. The preparation method is used for solving problems of existing technical preparation methods that operating conditions are harsh, processing procedures are complicated, and production cost is high. The preparation method comprises following steps: raw materials are dispersed in a dispersion medium, and the mixture is subjected to ball milling for uniform mixing; the mixture is dried so as to obtain a predecessor, the predecessor is uniformly mixed with glucose or sucrose, and the mixed material is subjected to precalcination; after precalcination, the predecessor is dispersed in the dispersion medium, and is subjected to ball milling; an obtained product is uniformly mixed with glucose or sucrose, and is subjected to calcining and grinding so as to obtain finished products of Li7La3Zr2O12. The preparation method is performed under normal pressure, and in air atmosphere; operating conditions are mild; processing procedures are simple; production cost is low; and stability and conductivity of obtained Li7La3Zr2O12 are high, and charge transferring resistance is low.
Description
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, continuous lifting along with continuous prosperity and the modern science and technology level of national economy, lithium ion battery has been expanded again its application greatly at society, with stylish service condition, again lithium ion battery has been proposed to more harsh and high-end requirement.At present, what on market, the lithium ion battery of extensive use adopted is the electrolyte of liquid state or gel state, both common ground are to have used inflammable and explosive organic substance and had certain mobility, this has brought potential safety hazard to the use of lithium ion battery, battery under certain conditions can be due to bad leakage of encapsulation, or when raising, temperature blasts, poor stability, simultaneously for some specific occasion, as for superintegrated small-sized electronic product provides energy, lithium-ion electric pool technology has been proposed to new requirement.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 conditions, so the research and development of lithium ion battery solid electrolyte material have a great deal of practical meanings.
In open day on August 8th, 2007 of Chinese patent, publication number CN101013761A, discloses a kind ofly for solid lithium battery solid electrolyte material material system and preparation method, and 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 compounds are combined with each other according to certain mol ratio; form diluted system; for lithium ion transmission provides space; thereby obtain higher ionic conductivity; and material has wider thermally-stabilised scope (room temperature ~ 200 ℃); described solid electrolyte material solid phase reaction under vacuum condition then quench after ball milling make, ball milling carries out under argon shield.Weak point is: need under vacuum and argon shield, carry out, operating condition is harsh, processed complex, and production cost is high, and the electrolyte self structure poor stability making reacts and can produce the hydrogen sulfide of gaseous state with water in air.
Summary of the invention
the operating condition harshness, processed complex, the production cost that the object of the invention is to solve prior art preparation method are high, the deficiency of electrolyte self structure poor stability, provide that a kind of operating condition is gentle, processing is simple, production cost is low, the lithium ion battery solid electrolyte material Li of electrolyte self structure good stability
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) according to the mol ratio of Li, La and Zr, to be 7 ~ 8:3:2 mix Li source compound, lanthanum source compound and zirconium source compound to be placed on thoroughly in decentralized medium, carries out ball milling mixing;
2) mixture that step 1) obtains is dry 8 ~ 12h under 95 ~ 105 ℃ of conditions, and then grind into powder obtains predecessor, and predecessor is mixed to rear precalcining with glucose or sucrose, and precalcining temperature is 500 ~ 800 ℃, and the time is 12 ~ 24 hours;
3) predecessor after precalcining is scattered in decentralized medium and 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 ℃, the time is 24 ~ 36 hours.
The present invention is by mixing raw material ball milling in decentralized medium of preparing solid electrolyte material, and then dry and grind into powder, makes raw material height dispersed, solid phase reaction speed homogeneous during follow-up calcining, the Li making
7la
3zr
2o
12solid electrolyte material homogeneity is good, precalcining and calcining before the raw material of high degree of dispersion is mixed with glucose or sucrose, take glucose or sucrose as carbon source, calcining heat is low, calcine effective, the Li making
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, the Li making
7la
3zr
2o
12solid electrolyte material cost is low.
As preferably, in step 1), Li source compound is selected from a kind of 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 a kind of 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 decentralized medium dispersive property is good, and raw material is follow-up after disperseing, and decentralized medium can be not residual when dry, do not affect the purity of raw material.
As preferably, the drum's speed of rotation that in step 1), ball milling mixes 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 is 10 ~ 60% of predecessor quality.Glucose or dosage of sucrose are reasonable, calcine effective, the Li making
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 are reasonable, calcine effective, the Li making
7la
3zr
2o
12solid electrolyte material Charge-transfer resistance reduces.
The invention has the beneficial effects as follows: (1) solid phase reaction speed of the present invention homogeneous, the Li making
7la
3zr
2o
12solid electrolyte material homogeneity is good; (2) to adopt sucrose or glucose be carbon source in the present invention, and calcining heat is low, calcine effective, the Li making
7la
3zr
2o
12solid electrolyte material Charge-transfer resistance reduces; (3) the electrolyte good stability that the present invention makes, 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) according to the mol ratio of Li, La, Za, 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, 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) mictoplasm obtaining is placed in to the baking oven of 105 ℃ and is dried, the time is 8 hours; Then grind and obtain Powdered predecessor, precalcining 24 hours under air atmosphere in tube furnace after predecessor adds 1.03g glucose (predecessor quality 10%) to mix, precalcining temperature is 500 ℃;
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 after mixing with 5.2g glucose (predecessor quality 50%) in tube furnace sintering 36 hours under air atmosphere, sintering temperature is 600 ℃, and resulting powder is ground and obtains Li
7la
3zr
2o
12sample.
embodiment 2:
1) according to the mol ratio of Li, La, Za, 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, 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) mictoplasm obtaining is placed in to the baking oven of 95 ℃ and is dried, the time is 12 hours; Then grind and obtain Powdered predecessor, precalcining 12 hours under air atmosphere in tube furnace after predecessor adds 8.49g glucose (predecessor quality 60%) to mix, precalcining temperature is 800 ℃;
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 after mixing with 2.83g sucrose (predecessor quality 20%) in tube furnace sintering 24 hours under air atmosphere, sintering temperature is 900 ℃, and resulting powder is ground and obtains Li
7la
3zr
2o
12sample.
embodiment 3:
1) according to the mol ratio of Li, La, Za, 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, 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) mictoplasm obtaining is placed in to the baking oven of 100 ℃ and is dried, the time is 10 hours; Then grind and obtain Powdered predecessor, precalcining 18 hours under air atmosphere in tube furnace after predecessor adds 3.637g sucrose (predecessor quality 35%) to mix, precalcining temperature is 650 ℃;
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, after the powder obtaining and 3.637g sucrose (predecessor quality 35%) are mixed in tube furnace sintering 30 hours under air atmosphere, sintering temperature is 750 ℃, and resulting powder is ground and obtains Li
7la
3zr
2o
12sample.
embodiment 4:
1) according to the mol ratio of Li, La, Za, 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, 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) mictoplasm obtaining is placed in to the baking oven of 100 ℃ and is dried, the time is 10 hours; Then grind and obtain Powdered predecessor, precalcining 18 hours under air atmosphere in tube furnace after predecessor adds 4.099g sucrose (predecessor quality 35%) to mix, precalcining temperature is 650 ℃;
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, after the powder obtaining and 4.099g sucrose (predecessor quality 35%) are mixed in tube furnace sintering 30 hours under air atmosphere, sintering temperature is 750 ℃, and resulting powder is ground and obtains 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 makes
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 makes
7la
3zr
2o
12sEM figure.
2) the solid electrolyte material Li that the present invention makes
7la
3zr
2o
12total ionic conductivity at room temperature by electrochemical impedance spectral method, measure, main test parameter is: alternating voltage amplitude 5 ~ 20mV, frequency range 40Hz ~ 110MHz(electric impedance analyzer), the electrochemical impedance data that obtain entered to calculate the total conductivity of sample, the blocking electrode that utilizes electric impedance analyzer to measure sample resistance is Au electrode, the solid electrolyte material Li that embodiment 1 ~ 4 makes
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) the solid electrolyte material Li under room temperature, the present invention being made in air
7la
3zr
2o
12chemical stability study, in air, 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 a kind of preferably scheme of the present invention, not the present invention is done to any pro forma restriction, also has other variant and remodeling under the prerequisite that does not exceed the technical scheme that claim records.
Claims (7)
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) according to the mol ratio of Li, La and Zr, to be 7 ~ 8:3:2 mix Li source compound, lanthanum source compound and zirconium source compound to be placed on thoroughly in decentralized medium, carries out ball milling mixing;
2) mixture that step 1) obtains is dry 8 ~ 12h under 95 ~ 105 ℃ of conditions, and then grind into powder obtains predecessor, and predecessor is mixed to rear precalcining with glucose or sucrose, and precalcining temperature is 500 ~ 800 ℃, and the time is 12 ~ 24 hours;
3) predecessor after precalcining is scattered in decentralized medium to ball-milling treatment again, then mixes rear calcining with glucose or sucrose, then grind to obtain Li
7la
3zr
2o
12sample, calcining heat is 600 ~ 900 ℃, the time is 24 ~ 36 hours.
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 a kind of 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 a kind of 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. according to a kind of lithium ion battery solid electrolyte material Li described in claim 1 or 2 or 3
7la
3zr
2o
12preparation method, it is characterized in that: the drum's speed of rotation that in step 1), ball milling mixes is 200 ~ 500rpm, the time that ball milling mixes is 12 ~ 24 hours.
5. according to a kind of lithium ion battery solid electrolyte material Li described in 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.
6. according to a kind of lithium ion battery solid electrolyte material Li described in claim 1 or 2 or 3
7la
3zr
2o
12preparation method, it is characterized in that: step 2) in the consumption of glucose or sucrose be 10 ~ 60% of predecessor quality.
7. according to a kind of lithium ion battery solid electrolyte material Li described in claim 1 or 2 or 3
7la
3zr
2o
12preparation method, it is characterized in that: in step 3), the consumption of glucose or sucrose is 20 ~ 50% of predecessor quality after precalcining.
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Cited By (14)
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CN104124467A (en) * | 2014-07-22 | 2014-10-29 | 武汉理工大学 | Method for preparing solid electrolyte by using lithium lanthanum zirconium oxide precursor coated powder |
CN104332651A (en) * | 2014-11-06 | 2015-02-04 | 山东大学 | Method for preparing garnet type Li7La3Zr2O12 electrolyte powder with molten-salt method |
CN105428706A (en) * | 2015-11-24 | 2016-03-23 | 青岛能迅新能源科技有限公司 | Praparation method for garnet type lithium lanthanum zirconate based solid electrolyte material |
CN105428707A (en) * | 2015-11-24 | 2016-03-23 | 青岛能迅新能源科技有限公司 | Sintering method for reducing lithium ion loss of solid-state lithium ion electrolyte material Li7La3Zr2O12 |
CN105470565A (en) * | 2014-09-30 | 2016-04-06 | 精工爱普生株式会社 | Composition for forming lithium reduction resistant layer, method for forming membrane, and lithium secondary battery |
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CN110137567A (en) * | 2019-06-03 | 2019-08-16 | 哈尔滨工业大学 | The preparation method and applications of high-compactness carbuncle type all solid state electrolyte under a kind of low temperature |
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CN104124467A (en) * | 2014-07-22 | 2014-10-29 | 武汉理工大学 | Method for preparing solid electrolyte by using lithium lanthanum zirconium oxide precursor coated powder |
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CN105470565A (en) * | 2014-09-30 | 2016-04-06 | 精工爱普生株式会社 | Composition for forming lithium reduction resistant layer, method for forming membrane, and lithium secondary battery |
CN104332651A (en) * | 2014-11-06 | 2015-02-04 | 山东大学 | Method for preparing garnet type Li7La3Zr2O12 electrolyte powder with molten-salt method |
CN105428707A (en) * | 2015-11-24 | 2016-03-23 | 青岛能迅新能源科技有限公司 | Sintering method for reducing lithium ion loss of solid-state lithium ion electrolyte material Li7La3Zr2O12 |
CN105428706A (en) * | 2015-11-24 | 2016-03-23 | 青岛能迅新能源科技有限公司 | Praparation method for garnet type lithium lanthanum zirconate based solid electrolyte material |
CN109361014A (en) * | 2018-09-12 | 2019-02-19 | 北京理工大学 | A kind of lithium secondary battery solid state electrolysis composite material, preparation method and lithium secondary battery |
CN109638348A (en) * | 2018-12-20 | 2019-04-16 | 天津市捷威动力工业有限公司 | A method of lithium lanthanum zirconium oxygen solid electrolyte is prepared using rheological phase reaction |
CN109687019A (en) * | 2019-01-22 | 2019-04-26 | 广东天劲新能源科技股份有限公司 | A method of improving oxide solid electrolyte electric conductivity |
CN109786845A (en) * | 2019-01-23 | 2019-05-21 | 蜂巢能源科技有限公司 | Sulfide electrolyte slurry and its preparation method and application |
CN109879316A (en) * | 2019-02-27 | 2019-06-14 | 上海空间电源研究所 | LLZO preparation method, thermal cell quasi-solid electrolyte and preparation method thereof |
CN110137567A (en) * | 2019-06-03 | 2019-08-16 | 哈尔滨工业大学 | The preparation method and applications of high-compactness carbuncle type all solid state electrolyte under a kind of low temperature |
CN110229003A (en) * | 2019-06-04 | 2019-09-13 | 上海应用技术大学 | A kind of LiNiLaZrO method for preparing solid electrolyte and application |
CN110229003B (en) * | 2019-06-04 | 2021-12-07 | 上海应用技术大学 | Preparation method and application of LiNiLaZrO solid electrolyte |
KR20210107926A (en) * | 2020-02-22 | 2021-09-02 | 인하대학교 산학협력단 | Glass ceramics for low temperature co-sintering of electrode and electrolyte and solid state battery using the same |
CN115588741A (en) * | 2022-09-14 | 2023-01-10 | 国联汽车动力电池研究院有限责任公司 | Composite solid electrolyte material for solid anode and preparation method and application thereof |
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