CN105047989B - A kind of electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide - Google Patents
A kind of electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide Download PDFInfo
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Abstract
The present invention relates to field of lithium ion battery, a kind of electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide is particularly disclosed.The electrochemical preparation method prepares the mixture of lanthana and titanium dioxide according to lanthanum titanium ratio, then titanium dioxide is embedded in lithium ion by electrochemical method, and then annealing obtains the LLTO of high-purity.The present invention can be with precise control Li-La-Ti ratio, solving the volatilization of the long lithium salts of usual solid phase method at high temperature causes the problem of product purity is relatively low, raw material is cheap simultaneously, and technique is simple, and the lithium lanthanum titanium oxide of high-purity is can be obtained by by two steps of electrochemistry and high-temperature process.
Description
（One）Technical field
The present invention relates to field of lithium ion battery, more particularly to a kind of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide
Electrochemical preparation method.
（Two）Background technology
The popularization of new-energy automobile can reduce environmental pollution, and wherein electrokinetic cell is key factor, and electrokinetic cell is usual
From liquid electrolyte, on fire or blast may be caused in abuse conditions, there is potential safety hazard.Use the complete of solid electrolyte
Solid state battery is greatly improved without using incendive liquid electrolyte, security, while the charge capacity of all-solid-state battery is more, defeated
Go out power also bigger, but the low ionic conductivity of solid electrolyte hinders the practicality of all-solid-state battery.
In solid electrolyte, perovskite structure compound lithium lanthanum titanium oxide Li3xLa2/3-xTiO3（LLTO）Room-temperature ion
Electrical conductivity is up to 10-3S/cm, particularly attracts people's attention close to business level of electrolyte.Synthesis Li-La-Ti oxidation common at present is closed
The method of thing mainly includes solid phase method and sol-gal process, and solid phase method technique is simple, but long-time high-temperature calcination cause energy consumption compared with
Height, and cause product purity relatively low because lithium salts volatilizees at high temperature, sol-gal process is using expensive alkoxide, and cost is very high,
It is only suitable for laboratory research.
（Three）The content of the invention
There is provided a kind of control of ratio is accurate, product purity is high, can advise greatly in order to make up the deficiencies in the prior art by the present invention
The electrochemical preparation method of the Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide of modelling production.
The present invention is achieved through the following technical solutions：
A kind of electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide, with titanium dioxide and oxidation
Lanthanum is raw material, is comprised the following steps：
（1）Raw material titanium dioxide, lanthana, binding agent and conductive agent is well mixed rear tabletted；
（2）With step（1）The piece of middle compacting is positive pole, and lithium piece is assembled into battery for negative pole, according to the quality of titanium dioxide
The electricity that embedding lithium needs is calculated with the ratio of lithium titanium, is discharged on electric discharge instrument；
（3）After discharge off, the positive pole of embedding lithium is taken out, degeneration at high temperature processing obtains lithium lanthanum titanium oxide.
The present invention more excellent scheme be：
The titanium dioxide is nano particle, and granular size is 25nm；Bulky grain adds the difficulty of Lithium-ion embeding, can
Embedding lithium can be caused uneven, purity is reduced, short grained cost is higher, operating difficulties, and 25nm titanium dioxide granule is current
Ripe commercial materials, are the optimal sizes of combination property.
Step（1）In, binding agent is Kynoar or polytetrafluoroethylene (PTFE), and conductive agent is in acetylene black and Super P
It is one or two kinds of.
Step（1）In, the mol ratio of lanthana and titanium dioxide is 2/3-x：2, wherein, 0.06≤x≤1/6；Li-La-Ti
Oxygen compound Li3xLa2/3-xTiO3There is a compound of a variety of different proportions, the mol ratio of lanthanum and titanium is the ratio according to final product
It is determined that；Binding agent ensure that the intensity of compressing tablet, but can influence the electric conductivity of compressing tablet too much and increase cost, and bonding is not had very little
Effect, mass fraction is optimal proportion for 5-20%.Conductive agent ensure that electric conductivity of the compressing tablet in discharge process, but too many meeting
Influence the difficulty of film-making and increase cost, act on very little not substantially, mass fraction is optimal proportion for 5-20%.
Step（1）In, the mixed method of the raw material is ball-milling method or polishing.
Step（2）In, the battery is button cell.
Step（2）In, discharge capacity is the electricity that the embedding lithium calculated according to the quality of titanium dioxide and the ratio of lithium titanium needs
Amount, lithium lanthanum titanium oxide Li3xLa2/3-xTiO3Middle lithium titanium mol ratio is 3x:1, then certain mass titanium dioxide insertion corresponding amount
Electricity computing formula required for lithium is：MAh, wherein m are gram of titanium dioxide
Number, M is the molecular weight of titanium dioxide, discharges into the lithium-inserting amount of now titanium dioxide exactly 3x.
Step（2）In, electric discharge instrument is cell tester or electrochemical workstation, is selected as far as possible under conditions of range is met
The cell tester of lower range is selected, discharge current is controlled in below 0.1C, it is ensured that lithium ion can be uniformly embedded into titanium dioxide
In titanium.
Step（3）In, high annealing is divided into pre-burning and two stages of sintering, and pre-burning can ensure to remove the bonding in material
Agent, conductive agent and other impurities and the gas for decomposing generation.The sintering of higher temperature can ensure abundant reaction, and generation crystal grain can
The lithium lanthanum titanium oxide of control.
The present invention can be with precise control Li-La-Ti ratio, and solving the volatilization of the long lithium salts of usual solid phase method at high temperature causes
The problem of product purity is relatively low, while raw material is cheap, technique is simple, can just be obtained by two steps of electrochemistry and high-temperature process
To the lithium lanthanum titanium oxide of high-purity.
（Four）Brief description of the drawings
The present invention is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is Li prepared by the embodiment of the present invention 10.33La0.557TiO3XRD；
Fig. 2 is Li prepared by the embodiment of the present invention 20.485La0.505TiO3XRD.
（Five）Embodiment
The present invention is described in further detail below by specific embodiment, but these embodiments are only that citing
Illustrate, the scope of the present invention is not defined.
Embodiment 1：
Weigh in 0.7987g titanium dioxide, 0.9068g lanthanas, 0.2132g PVDF and 0.2132g acetylene blacks, mortar
Grinding half an hour is sufficiently mixed uniformly, takes 0.2g mixtures to be put under mould, 20MPa pressure and suppresses 1 minute in flakes.Compressing tablet is done
Positive pole, from CR2032 button cell shells, according to negative electrode casing, spring leaf, pad, lithium piece, barrier film, positive pole, anode cover order
Assembled battery, is added dropwise 5 and drips lithium-ion battery electrolytes, button cell is prepared with sealing machine sealing.The button cell of preparation is put
Onto cell tester, the capacity of 0.05C constant-current discharges to 8.30mAh.Take out in the compressing tablet after embedding lithium, Muffle furnace 800 DEG C it is pre-
Burn 5 hours, after grinding 1000 DEG C again sintering obtain Li within 10 hours0.33La0.557TiO3。
Embodiment 2：
Weigh 0.7987g titanium dioxide, 0.8226g lanthanas, 0.2027g PVDF and 0.2027g Super P, mortar
Middle grinding half an hour is sufficiently mixed uniformly, takes 0.2g mixtures to be put under mould, 20MPa pressure and suppresses 1 minute in flakes.By compressing tablet
Do positive pole, from CR2032 button cell shells, according to negative electrode casing, spring leaf, pad, lithium piece, barrier film, positive pole, anode cover it is suitable
Sequence assembled battery, is added dropwise 5 and drips lithium-ion battery electrolytes, button cell is prepared with sealing machine sealing.By the button cell of preparation
It is put on cell tester, the capacity of 0.05C constant-current discharges to 12.83mAh.800 DEG C are taken out in the compressing tablet after embedding lithium, Muffle furnace
Pre-burning 5 hours, after grinding 1000 DEG C again sintering obtain Li within 10 hours0.485La0.505TiO3。
Embodiment 3：
7.987g titanium dioxide, 9.068g lanthanas, 0.9475g PVDF and 0.9475g Super P are weighed, is put into
100ml ball grinders, ratio of grinding media to material is 3:1, grinding is sufficiently mixed uniformly for 2 hours, takes 0.2g mixtures to be put into mould, 20MPa pressure
It is lower to suppress 1 minute in flakes.Compressing tablet is done into positive pole, from CR2032 button cell shells, according to a negative electrode casings, spring leaf, pad, lithium
Piece, barrier film, positive pole, the order assembled battery of anode cover, are added dropwise 5 and drip lithium-ion battery electrolytes, knob is prepared with sealing machine sealing
Detain battery.The button cell of preparation is put on cell tester, the capacity of 0.05C constant-current discharges to 9.33mAh.Take out embedding lithium
550 DEG C of pre-burnings 5 hours in compressing tablet afterwards, Muffle furnace, after grinding 1200 DEG C again sintering obtain Li within 10 hours0.33La0.557TiO3。
Claims (9)
1. a kind of electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide, with titanium dioxide and lanthana
For raw material, it is characterized in that, comprise the following steps：（1）Raw material titanium dioxide, lanthana, binding agent and conductive agent are well mixed
It is tabletted afterwards；（2）With step（1）The piece of middle compacting is positive pole, and lithium piece is assembled into battery for negative pole, according to the matter of titanium dioxide
Amount and the ratio of lithium titanium calculate the electricity that embedding lithium needs, and are discharged on electric discharge instrument；（3）After discharge off, embedding lithium is being taken out just
Pole, the high temperature anneal obtains lithium lanthanum titanium oxide.
2. the electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide according to claim 1, its
It is characterised by：The titanium dioxide is nano particle, and granular size is 25nm.
3. the electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide according to claim 1, its
It is characterised by：Step（1）In, binding agent is Kynoar or polytetrafluoroethylene (PTFE), and conductive agent is in acetylene black and Super P
It is one or two kinds of.
4. the electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide according to claim 1, its
It is characterised by：Step（1）In, the mol ratio of lanthana and titanium dioxide is 2/3-x：2, wherein, 0.06≤x≤1/6；Binding agent
For the 5-20% of raw material gross mass, conductive agent is the 5-20% of raw material gross mass.
5. the electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide according to claim 1, its
It is characterised by：Step（1）In, the mixed method of the raw material is polishing.
6. the electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide according to claim 1, its
It is characterised by：Step（2）In, the battery is button cell.
7. the electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide according to claim 1, its
It is characterised by：Step（2）In, discharge capacity is the electricity that the embedding lithium calculated according to the quality of titanium dioxide and the ratio of lithium titanium needs
Amount, lithium lanthanum titanium oxide Li3xLa2/3-xTiO3Middle lithium titanium mol ratio is 3x:1, then certain mass titanium dioxide insertion corresponding amount
Electricity computing formula required for lithium is：MAh, wherein m are gram of titanium dioxide
Number, M is the molecular weight of titanium dioxide, discharges into the lithium-inserting amount of now titanium dioxide exactly 3x.
8. the electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide according to claim 1, its
It is characterised by：Step（2）In, electric discharge instrument is cell tester or electrochemical workstation, and discharge current is controlled in below 0.1C.
9. the electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide according to claim 1, its
It is characterised by：Step（3）In, high annealing is divided into pre-burning and two stages of sintering.
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| CN201510401508.7A CN105047989B (en) | 2015-07-09 | 2015-07-09 | A kind of electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide |
| PCT/CN2016/085322 WO2017005077A1 (en) | 2015-07-09 | 2016-06-08 | Electrochemical preparation method for perovskite-type solid electrolyte lithium-lanthanum-titanium oxide compound |
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| CN105047989B (en) * | 2015-07-09 | 2017-07-11 | 山东玉皇新能源科技有限公司 | A kind of electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide |
| CN109390626B (en) * | 2017-08-08 | 2021-09-21 | 深圳格林德能源集团有限公司 | Inorganic solid electrolyte synthesis process and solid battery thereof |
| CN109285983B (en) * | 2018-09-28 | 2020-07-14 | 东北大学 | Button lithium battery with lithium ion solid electrolyte sheet as diaphragm and preparation method thereof |
| 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 |
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| CN102859779A (en) * | 2010-04-13 | 2013-01-02 | 丰田自动车株式会社 | Solid electrolyte material, lithium battery, and manufacturing method for solid electrolyte material |
| CN104051782A (en) * | 2013-03-12 | 2014-09-17 | 华为技术有限公司 | Lithium lanthanum titanate (LLTO) composite solid-state lithium ion electrolyte material, preparation method and application thereof |
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| JP5230713B2 (en) * | 2010-10-29 | 2013-07-10 | 株式会社東芝 | Battery active material, non-aqueous electrolyte battery and battery pack |
| CN103210529B (en) * | 2011-02-18 | 2016-03-02 | 株式会社东芝 | Rechargeable nonaqueous electrolytic battery and manufacture method thereof |
| JP5793442B2 (en) * | 2012-02-09 | 2015-10-14 | 株式会社東芝 | Battery active material, non-aqueous electrolyte battery and battery pack |
| JP5998411B2 (en) * | 2012-07-27 | 2016-09-28 | 東邦チタニウム株式会社 | Method for producing sintered lithium lanthanum titanium oxide |
| CN103290426B (en) * | 2013-07-12 | 2015-07-01 | 广州有色金属研究院 | Preparation method of lithium titanate |
| KR101683949B1 (en) * | 2013-11-14 | 2016-12-07 | 주식회사 엘지화학 | The synthesis of solid electrolyte nano particle for lithium secondary battery using flame spray pyrolysis |
| CN105036182B (en) * | 2015-06-15 | 2017-03-08 | 山东玉皇新能源科技有限公司 | A kind of preparation method and applications of high-purity lithium titanate anode material |
| CN105047989B (en) * | 2015-07-09 | 2017-07-11 | 山东玉皇新能源科技有限公司 | A kind of electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide |
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| CN102859779A (en) * | 2010-04-13 | 2013-01-02 | 丰田自动车株式会社 | Solid electrolyte material, lithium battery, and manufacturing method for solid electrolyte material |
| CN104051782A (en) * | 2013-03-12 | 2014-09-17 | 华为技术有限公司 | Lithium lanthanum titanate (LLTO) composite solid-state lithium ion electrolyte material, preparation method and application thereof |
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