CN105428629A - Efficient sulfur/carbon coated lithium nickelate positive electrode material and preparation method thereof - Google Patents

Efficient sulfur/carbon coated lithium nickelate positive electrode material and preparation method thereof Download PDF

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Publication number
CN105428629A
CN105428629A CN201511025359.5A CN201511025359A CN105428629A CN 105428629 A CN105428629 A CN 105428629A CN 201511025359 A CN201511025359 A CN 201511025359A CN 105428629 A CN105428629 A CN 105428629A
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lithium nickelate
sulphur
positive electrode
lithium
charcoal
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姜殿凯
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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
    • H01M4/362—Composites
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/5835—Comprising fluorine or fluoride salts
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Composite Materials (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention relates to an efficient sulfur/carbon coated lithium nickelate positive electrode material and a preparation method thereof. The efficient sulfur/carbon coated lithium nickelate positive electrode material is prepared from, by weight, 35 parts of sulfur/carbon composite, 55 parts of lithium nickelate, 25 parts of 45% ferric nitrate lithium solution, 7 parts of crystalline flake graphite and 7 parts of binding material. The defect that a lithium ion battery loses efficacy due to self discharge of a protection plate is overcome, self discharge of a whole battery pack is improved, the aim of prolonging the lithium battery storage time is achieved, and it is ensured that electric appliances can be stored for a long time after being used by users under the condition that charging is not conducted.

Description

Lithium nickelate positive electrode that a kind of efficient sulphur/charcoal is coated and preparation method thereof
Technical field
The present invention relates to coated lithium nickelate positive electrode of a kind of efficient sulphur/charcoal and preparation method thereof.
Background technology
Lithium ion battery is since commercialization, and lithium ion battery positive electrode used is mostly lithium nickelate, LiMn2O4 or ternary material etc., and its component mainly lithium nickelate adds conductive agent adding additives again, and described lithium nickelate is lithium nickelate, LiMn2O4 or ternary etc.; Negative material adopts graphite to be active material mostly, then adds some conductive agents and binding agent; Its advantage is that capacity is higher, has extended cycle life, but nickel resources is deficient, expensive and have toxicity, therefore seeks excellent honest and clean, the important research direction that dependable performance, eco-friendly positive electrode become lithium ion battery of price.Be that spinel-type positive electrode and the ternary material layered oxide of representative is in the past decade extensively studied with LiMn2O4, but constrain their development prospect due to its defect existed separately.In addition, the system of positive and negative pole material composition has a common feature to discharge the later stage exactly, especially at the end of electric discharge, voltage drop quickly, namely inside this voltage range, the capacity of lithium ion battery almost without.
Summary of the invention
The technical problem to be solved in the present invention is the above-mentioned defect how overcoming prior art, lithium nickelate positive electrode providing a kind of efficient sulphur/charcoal coated and preparation method thereof.
For solving the problems of the technologies described above, this lithium nickelate positive electrode that efficiently sulphur/charcoal is coated by weight, be prepared from according to shown ratio by following component, sulphur/carbon composite 35, the ferric nitrate lithium solution 25 of lithium nickelate 55,45%, crystalline flake graphite 7, binding material 7.
This lithium nickelate method for preparing anode material that efficiently sulphur/charcoal is coated comprises the following steps:
(1) according to above-mentioned weight ratio, material with carbon element and sublimed sulfur or Cosan are put into zirconium dioxide or agate jar, after ball grinder being injected high purity inert gas in glove box, be placed in ball milling 5h on planetary ball mill, rotational speed of ball-mill is 500r/min, and the mass ratio of elemental sulfur and carbon is 1:2 ~ 3: 2; Obtain sulphur/carbon composite, this sulphur/carbon composite is warming up to 150 DEG C with the rate of heat addition of 10 DEG C/min in an oven, and is incubated 24h at this temperature;
(2) be dispersed in by sulphur/carbon composite in the mixed solvent of the water that volume ratio is 3:1 and acetone, water or chloroform, ultrasonic or stirring, makes it disperse completely equably;
(3) by lithium nickelate, 45% ferric nitrate lithium solution, crystalline flake graphite, binding material add in mixed solution, again ultrasonic or stir, add or do not add dopant acid, whole mixed solution system is in acid, and its pH value is between 2 ~ 4;
(4) under ice-water bath and inert atmosphere protection, ammonium persulfate aqueous solution or FeCl is added 3chloroformic solution, stirring reaction 24h under constant temperature, then by product centrifugation, washing, the vacuum drying chamber putting into 60 DEG C is dried, and is ground to powder.
The coated lithium nickelate method for preparing anode material method of a kind of efficient sulphur/charcoal of the present invention is simple; with low cost; overcome lithium ion battery causes inefficacy defect because of baffle self discharge; thus improve the self discharge of whole battery pack; realize the object extending the lithium battery resting period, when ensureing that user uses electrical appliance and do not charge, the longer time can be stored.
Embodiment
This lithium nickelate positive electrode that efficiently sulphur/charcoal is coated by weight, is prepared from according to shown ratio by following component, sulphur/carbon composite 35, the ferric nitrate lithium solution 25 of lithium nickelate 55,45%, crystalline flake graphite 7, binding material 7.The ferric nitrate lithium solution of described 45% is the ferric nitrate lithium solution of 60%.Described positive electrode is lithium nickelate.Described conductive agent is crystalline flake graphite
This lithium nickelate method for preparing anode material that efficiently sulphur/charcoal is coated comprises the following steps:
(1) according to above-mentioned weight ratio, material with carbon element and sublimed sulfur or Cosan are put into zirconium dioxide or agate jar, after ball grinder being injected high purity inert gas in glove box, be placed in ball milling 5h on planetary ball mill, rotational speed of ball-mill is 500r/min, and the mass ratio of elemental sulfur and carbon is 1:2 ~ 3: 2; Obtain sulphur/carbon composite, this sulphur/carbon composite is warming up to 150 DEG C with the rate of heat addition of 10 DEG C/min in an oven, and is incubated 24h at this temperature;
(2) be dispersed in by sulphur/carbon composite in the mixed solvent of the water that volume ratio is 3:1 and acetone, water or chloroform, ultrasonic or stirring, makes it disperse completely equably;
(3) by lithium nickelate, 45% ferric nitrate lithium solution, crystalline flake graphite, binding material add in mixed solution, again ultrasonic or stir, add or do not add dopant acid, whole mixed solution system is in acid, and its pH value is between 2 ~ 4;
(4) under ice-water bath and inert atmosphere protection, ammonium persulfate aqueous solution or FeCl is added 3chloroformic solution, stirring reaction 24h under constant temperature, then by product centrifugation, washing, the vacuum drying chamber putting into 60 DEG C is dried, and is ground to powder.
The present invention includes but be not limited to above-mentioned execution mode, any product meeting these claims and describe, all falls within protection scope of the present invention.

Claims (2)

1. the lithium nickelate positive electrode that efficient sulphur/charcoal is coated, it is characterized in that: by weight, the coated lithium nickelate positive electrode of this efficient sulphur/charcoal is prepared from according to shown ratio by following component, sulphur/carbon composite 35, the ferric nitrate lithium solution 25 of lithium nickelate 55,45%, crystalline flake graphite 7, binding material 7.
2. the lithium nickelate method for preparing anode material that efficient sulphur/charcoal is coated, is characterized in that: the coated lithium nickelate positive electrode of described efficient sulphur/charcoal is the coated lithium nickelate positive electrode of efficient sulphur/charcoal according to claim 1, and its preparation method comprises the following steps:
(1) according to above-mentioned weight ratio, material with carbon element and sublimed sulfur or Cosan are put into zirconium dioxide or agate jar, after ball grinder being injected high purity inert gas in glove box, be placed in ball milling 25h on planetary ball mill, rotational speed of ball-mill is 2500r/min, and the mass ratio of elemental sulfur and carbon is 1:2 ~ 3: 2; Obtain sulphur/carbon composite, this sulphur/carbon composite is warming up to 155 DEG C with the rate of heat addition of 10 DEG C/min in an oven, and is incubated 24h at this temperature;
(2) be dispersed in by sulphur/carbon composite in the mixed solvent of the water that volume ratio is 3:1 and acetone, water or chloroform, ultrasonic or stirring, makes it disperse completely equably;
(3) by lithium nickelate, 45% ferric nitrate lithium solution, crystalline flake graphite, binding material add in mixed solution, again ultrasonic or stir, add or do not add dopant acid, whole mixed solution system is in acid, and its pH value is between 2 ~ 4;
(4) under ice-water bath and inert atmosphere protection, ammonium persulfate aqueous solution or FeCl is added 3chloroformic solution, stirring reaction 24h under constant temperature, then by product centrifugation, washing, the vacuum drying chamber putting into 60 DEG C is dried, and is ground to powder.
CN201511025359.5A 2015-12-30 2015-12-30 Efficient sulfur/carbon coated lithium nickelate positive electrode material and preparation method thereof Pending CN105428629A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201511025359.5A CN105428629A (en) 2015-12-30 2015-12-30 Efficient sulfur/carbon coated lithium nickelate positive electrode material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201511025359.5A CN105428629A (en) 2015-12-30 2015-12-30 Efficient sulfur/carbon coated lithium nickelate positive electrode material and preparation method thereof

Publications (1)

Publication Number Publication Date
CN105428629A true CN105428629A (en) 2016-03-23

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Application publication date: 20160323