CN105720305A - Preparation method of lithium ion polymer battery - Google Patents

Preparation method of lithium ion polymer battery Download PDF

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Publication number
CN105720305A
CN105720305A CN201410727285.9A CN201410727285A CN105720305A CN 105720305 A CN105720305 A CN 105720305A CN 201410727285 A CN201410727285 A CN 201410727285A CN 105720305 A CN105720305 A CN 105720305A
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Prior art keywords
lithium
dehydrated alcohol
rare earth
products therefrom
concentration
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CN201410727285.9A
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段维宽
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ZTE Corp
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ZTE Corp
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Priority to CN201410727285.9A priority Critical patent/CN105720305A/en
Priority to PCT/CN2015/075147 priority patent/WO2016086553A1/en
Publication of CN105720305A publication Critical patent/CN105720305A/en
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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
    • H01M4/58—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
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a preparation method of a lithium ion polymer battery. Potassium ethoxide, neodymium nitrate, lithium nitrate, high concentration hydrofluoric acid (with content of 49wt%) and anhydrous ethanol as raw materials are processed to form multicomponent rare earth fluoride K5NdLi2F10 particles according to a preset ratio in a preset order. The preparation method reduces preparation requirements, can be realized easily, has simple reaction conditions and has short time consumption. The product has small particle sizes, uniform dispersity and good heat stability.

Description

A kind of preparation method of lithium ion polymer battery
Technical field
The present invention relates to lithium battery material, the preparation method particularly relating to a kind of lithium ion polymer battery, mainly the multielement rare earth fluoride fluorine lithium acid neodymium potassium (K in described battery5NdLi2F10) preparation method.
Background technology
Multielement rare earth fluoride K5NdLi2F10It it is the high concentration crystal of fluoride obtaining stimulated emission the earliest.Therefore suffer from the concern of numerous laser material researcher.As a kind of excellent laser crystal.Having activated ion concentration height, luminous power is strong, and fluorescence lifetime is long, and phonon energy is low waits many merits.K traditionally5NdLi2F10What material was main is applied in laser field, and materials synthesis mainly adopts fused salt slow cooling method, unstable under molten condition during due to fluoride high temperature, very easily etching apparatus, and volatilizes toxic gas.Traditional preparation methods requires with argon shield, and in platinum crucible, by relevant fluoride proportionally mix homogeneously, 800-1000 DEG C of heating, to molten condition, with 9 DEG C/h, is gradually cooling to room temperature.The defects such as it has equipment requirements height, severe reaction conditions, prepares length consuming time, and product reunion caking phenomenon is serious, and dispersion liquid is muddy.
The present invention mentions a kind of multielement rare earth fluoride K5NdLi2F10A kind of simple method for preparing of nano-particle.By short hydrothermal process, the K that pattern is good can be obtained5NdLi2F10Nano-particle.Reduce reaction condition and preparation difficulty, simplify process step, energy efficient, improve product quality.When material is at big electric current, when repeatedly circulating, still to exceed more than 10% than the Capacity Ratio of existing anode material for lithium-ion batteries.K in hot environment5NdLi2F10Showing good heat stability, therefore it has bigger potential using value on the positive electrode field of lithium ion battery.
Summary of the invention
The problem to be solved in the present invention is that prior art prepares multielement rare earth fluoride K5NdLi2F10Nano-particle, higher for equipment requirements, severe reaction conditions, prepare length consuming time, the defects such as product reunion caking phenomenon is serious, and dispersion liquid is muddy, it is provided that a kind of equipment is simple, condition is easy to preparation method.
The present invention solves above-mentioned technical problem by the following technical programs: the preparation method of a kind of lithium ion polymer battery, described lithium ion polymer battery, using potassium ethoxide, neodymium nitrate, lithium nitrate high concentration of hydrofluoric acid (49wt%) and dehydrated alcohol as raw material, makes multielement rare earth fluoride K according to preset ratio and preset order5NdLi2F10Granule.
Preferably, described preset order is: gel process, water-heat process and ultrasonication.
Preferably, described gel process, water-heat process and ultrasonication specifically include:
A. potassium ethoxide is dissolved in dehydrated alcohol, is configured to the alcoholic solution of the potassium ethoxide that concentration is 0.01-0.1mol/L,
B. alcohol-soluble rare earth salts is dissolved in dehydrated alcohol, is configured to the alcoholic solution containing rare earth ion that concentration is 0.01-0.1mol/L,
C. alcohol-soluble lithium salts is dissolved in dehydrated alcohol, be configured to concentration be 0.01-0.1mol/L containing lithium alcoholic solution,
D. by step a, b, c tri-step gained solution according to preset ratio mix, in mixed process add surfactant 1.5mL-3.5mL TritonX-100,
E. high concentration of hydrofluoric acid (49wt%) dropwise being instilled in step d gained mixed solution, making mixture is gel,
F. being transferred to by gelatinous mixture in the hydro-thermal reaction device that politef is liner, react in air dry oven, temperature is 150 DEG C-200 DEG C, and the time is 10 hours to 24 hours,
G. use 40-60mL dehydrated alcohol by fully dispersed for upper step gained nano-particle, ultrasonoscope carry out supersound process,
H. being transferred in centrifuge tube by step f products therefrom, be centrifuged for medium with dehydrated alcohol, centrifugal speed is 4000-12000r/ minute,
I. being transferred to by step g products therefrom and be dried in vacuum drying oven, temperature is 60 DEG C,
J., after described step g products therefrom naturally cools to room temperature, described step h products therefrom is ground.
Preferably, described grinding is to carry out in Achates body.
Preferably, the potassium contained respectively in described potassium ethoxide, neodymium nitrate, lithium nitrate and high concentration of hydrofluoric acid (49wt%): neodymium: lithium: fluorine element ratio is 5:1:2:10.
Accompanying drawing explanation
Fig. 1 is the multielement rare earth fluoride K that the embodiment of the present invention 1 prepares5NdLi2F10Nano-particle circulation electric discharge figure.
Fig. 2 is the multielement rare earth fluoride K that the embodiment of the present invention 1 prepares5NdLi2F10The TEM figure of nano-particle.
Fig. 3 is the multielement rare earth fluoride K that the embodiment of the present invention 1 prepares5NdLi2F10The XRD figure of nano-particle.
Fig. 4 is the K that the embodiment of the present invention 1 prepares5ReLi2F10The fluorescence spectrum figure of nano-particle.
Fig. 5 is the multielement rare earth fluoride K that the embodiment of the present invention 2 prepares5NdLi2F10The TEM figure of nano-particle.
Fig. 6 is the multielement rare earth fluoride K that the embodiment of the present invention 2 prepares5NdLi2F10The XRD figure of nano-particle.
Fig. 7 is the multielement rare earth fluoride K that the embodiment of the present invention 2 prepares5NdLi2F10The TG figure of nano-particle.
Detailed description of the invention
Present pre-ferred embodiments is provided, to describe technical scheme in detail below in conjunction with accompanying drawing
Embodiment 1:
A, potassium ethoxide is dissolved in dehydrated alcohol, is configured to the alcoholic solution of the potassium ethoxide that concentration is 0.01-0.1mol/L, is placed in beaker, stir 15 minutes；
B, alcohol-soluble rare earth salts is dissolved in dehydrated alcohol, is configured to the alcoholic solution containing rare earth ion that concentration is 0.01-0.1mol/L, is placed in beaker, stir 15 minutes；
C, alcohol-soluble lithium salts is dissolved in dehydrated alcohol, be configured to concentration be 0.01-0.1mol/L containing lithium alcoholic solution, be placed in beaker, stir 15 minutes；
D, a, b, c gained solution mixes according to proper proportion, adds surfactant 1.5mL TritonX-100, stir 30 minutes in mixed process.
E, by high concentration of hydrofluoric acid (49wt%) under agitation, dropwise instills in step d gained mixed solution, and making mixture is gel.
F, being transferred to by gelatinous mixture in the hydro-thermal reaction device that politef is liner, reaction carries out in air dry oven, and reaction temperature is 200 DEG C, and the response time is 10 hours.
G, use 40-60mL dehydrated alcohol are by fully dispersed for upper step gained nano-particle.With certain power ultrasonic in high-power ultrasonics instrument, continuous ultrasound 20 minutes.
H, being transferred in centrifuge tube by step f products therefrom, centrifugal speed is 4000-12000r/ minute, and centrifugal 10-30 minute every time, employing dehydrated alcohol was medium, repeated centrifugation process 5-6 time.
I, by step g product, dry in vacuum drying oven, baking temperature is 60 DEG C, and drying time is 24-48 hour.
J, naturally cool to room temperature after, product is ground in agate mortar, multielement rare earth fluoride K can be obtained5NdLi2F10Nano-particle.
The TEM figure of product is shown in Fig. 1, and size is homogeneous, is uniformly dispersed；XRD figure is shown on Fig. 2, figure it can be seen that being further characterized by obtaining product is multielement rare earth fluoride K5NdLi2F10Nano-particle.Fluorescence spectrum figure is shown in Fig. 3, and this product is mainly at near-infrared section emitting fluorescence.
Multielement rare earth fluoride K prepared by this method5NdLi2F10The source of middle potassium element is potassium ethoxide, and the reaction needed in step f occurs in hydro-thermal reaction, also needs products therefrom is waken up with a start long-time supersound process in subsequent step, and products therefrom has higher heat stability.
Embodiment 2:
A, potassium ethoxide is dissolved in dehydrated alcohol, is configured to the alcoholic solution of the potassium ethoxide that concentration is 0.01-0.1mol/L, is placed in beaker, stir 15 minutes；
B, alcohol-soluble rare earth salts is dissolved in dehydrated alcohol, is configured to the alcoholic solution containing rare earth ion that concentration is 0.01-0.1mol/L, is placed in beaker, stir 15 minutes；
C, alcohol-soluble lithium salts is dissolved in dehydrated alcohol, be configured to concentration be 0.01-0.1mol/L containing lithium alcoholic solution, be placed in beaker, stir 15 minutes；
D, a, b, c gained solution mixes according to proper proportion, adds surfactant 1.5mL TritonX-100, stir 30 minutes in mixed process.
E, by high concentration of hydrofluoric acid (49wt%) under agitation, dropwise instills in step d gained mixed solution, and making mixture is gel.
F, being transferred to by gelatinous mixture in the hydro-thermal reaction device that politef is liner, reaction carries out in air dry oven, and reaction temperature is 150 DEG C, and the response time is 24 hours.
G, use 40-60mL dehydrated alcohol are by fully dispersed for upper step gained nano-particle.With certain power ultrasonic in high-power ultrasonics instrument, continuous ultrasound 20 minutes.
H, being transferred in centrifuge tube by step f products therefrom, centrifugal speed is 4000-12000r/ minute, and centrifugal 10-30 minute every time, employing dehydrated alcohol was medium, repeated centrifugation process 5-6 time.
I, by step g product, dry in vacuum drying oven, baking temperature is 60 DEG C, 24-48 hour drying time.
J, naturally cool to room temperature after, product is ground in agate mortar, multielement rare earth fluoride K can be obtained5NdLi2F10Nano-particle.
The TEM figure of product is shown in Fig. 4, and size is homogeneous, is uniformly dispersed；XRD figure is shown on Fig. 5, figure it can be seen that being further characterized by obtaining product is multielement rare earth fluoride K5NdLi2F10Nano-particle, TG figure is shown in that the melt temperature of Fig. 6 product is more than 500 DEG C, has good heat stability.
When same as the previously described embodiments, the response time in step f is set to 18 hours, it is also possible to obtain the nano-particle described in g step, and finally obtain multielement rare earth fluoride fluorine lithium acid neodymium potassium (K5NdLi2F10)。
By above several embodiments and accompanying drawing it can be seen that the preparation method of this invention proposition, reducing reaction condition and preparation difficulty, process step simple, energy consumption is low, product quality height, and reactant is cheap and easy to get, has significantly expanded the range of application of the method；K in the product obtained5NdLi2F10Nano-particle size is all comparatively homogeneous, pattern rule, and luminosity is good, and transmitance is high.Simultaneously in big electric current, high loop test, the level that material capacity is higher than remaining in that, is the anode material for lithium-ion batteries of a kind of bigger potential using value.
Although the foregoing describing the specific embodiment of the present invention, it will be appreciated by those of skill in the art that these are merely illustrative of, protection scope of the present invention is defined by the appended claims.Those skilled in the art is under the premise without departing substantially from principles of the invention and essence, it is possible to these embodiments are made various changes or modifications, but these change and amendment each falls within protection scope of the present invention.

Claims (5)

1. the preparation method of a lithium ion polymer battery, it is characterized in that, described lithium ion polymer battery, using potassium ethoxide, neodymium nitrate, lithium nitrate high concentration of hydrofluoric acid (49wt%) and dehydrated alcohol as raw material, makes multielement rare earth fluoride K according to preset ratio and preset order5NdLi2F10Granule.
2. method according to claim 1, it is characterised in that described preset order is: gel process, water-heat process and ultrasonication.
3. method according to claim 2, it is characterised in that described gel process, water-heat process and ultrasonication specifically include:
Gel process includes:
A. potassium ethoxide is dissolved in dehydrated alcohol, is configured to the alcoholic solution of the potassium ethoxide that concentration is 0.01-0.1mol/L,
B. alcohol-soluble rare earth salts is dissolved in dehydrated alcohol, is configured to the alcoholic solution containing rare earth ion that concentration is 0.01-0.1mol/L,
C. alcohol-soluble lithium salts is dissolved in dehydrated alcohol, be configured to concentration be 0.01-0.1mol/L containing lithium alcoholic solution,
D. by step a, b, c tri-step gained solution according to preset ratio mix, in mixed process add surfactant 1.5mL-3.5mL TritonX-100,
E. high concentration of hydrofluoric acid (49wt%) dropwise being instilled in step d gained mixed solution, making mixture is gel,
Water-heat process includes:
F. being transferred to by described gelatinous mixture in the hydro-thermal reaction device that politef is liner, react in air dry oven, temperature is 150 DEG C-200 DEG C, and the time is 10 hours to 24 hours,
Ultrasonication includes:
G. use 40-60mL dehydrated alcohol by fully dispersed for step f gained nano-particle, ultrasonoscope carry out supersound process,
H. being transferred in centrifuge tube by step g products therefrom, be centrifuged for medium with dehydrated alcohol, centrifugal speed is 4000-12000r/ minute,
I. being transferred to by step hour products therefrom and be dried in vacuum drying oven, temperature is 60 DEG C,
J., after described step i products therefrom naturally cools to room temperature, described step i products therefrom is ground.
4. the method according to claim 3, described in after described step i products therefrom naturally cools to room temperature, described step i products therefrom is ground, it is characterised in that described grinding is to carry out in Achates body.
5. method as claimed in any of claims 1 to 4, it is characterised in that the potassium contained respectively in described potassium ethoxide, neodymium nitrate, lithium nitrate and high concentration of hydrofluoric acid (49wt%): neodymium: lithium: fluorine element ratio is 5:1:2:10.
CN201410727285.9A 2014-12-03 2014-12-03 Preparation method of lithium ion polymer battery Withdrawn CN105720305A (en)

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PCT/CN2015/075147 WO2016086553A1 (en) 2014-12-03 2015-03-26 Method for preparing lithium ion polymer battery

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003007296A (en) * 2001-06-20 2003-01-10 Sanyo Electric Co Ltd Nonaqueous electrolyte secondary battery
CN1785800A (en) * 2005-12-23 2006-06-14 清华大学 Preparation method of rare earth doped iron lithium phosphate powder
CN103723758A (en) * 2013-12-12 2014-04-16 南京邮电大学 Preparation method of polyphyletic terrae rare fluoride nano particles and transparent lighting dispersive solution thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102942932B (en) * 2012-11-15 2014-01-29 中国科学院西安光学精密机械研究所 Preparation method of rare earth doped fluoride nano dispersion liquid

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003007296A (en) * 2001-06-20 2003-01-10 Sanyo Electric Co Ltd Nonaqueous electrolyte secondary battery
CN1785800A (en) * 2005-12-23 2006-06-14 清华大学 Preparation method of rare earth doped iron lithium phosphate powder
CN103723758A (en) * 2013-12-12 2014-04-16 南京邮电大学 Preparation method of polyphyletic terrae rare fluoride nano particles and transparent lighting dispersive solution thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
WEIKUAN DUAN等: "Synthesis and near-infrared fluorescence of K5NdLi2F10 nanocrystals and their dispersion with high doping concentration and long lifetime", 《NANOSCALE》 *

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Application publication date: 20160629