CN105568322A - Method for preparing nickel-based battery material - Google Patents

Method for preparing nickel-based battery material Download PDF

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Publication number
CN105568322A
CN105568322A CN201510850757.4A CN201510850757A CN105568322A CN 105568322 A CN105568322 A CN 105568322A CN 201510850757 A CN201510850757 A CN 201510850757A CN 105568322 A CN105568322 A CN 105568322A
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CN
China
Prior art keywords
battery material
electrolysis
cathode
molten salt
graphite carbon
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Pending
Application number
CN201510850757.4A
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Chinese (zh)
Inventor
郝青
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Shaanxi Huanke Biotechnology Co Ltd
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Shaanxi Huanke Biotechnology Co Ltd
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Application filed by Shaanxi Huanke Biotechnology Co Ltd filed Critical Shaanxi Huanke Biotechnology Co Ltd
Priority to CN201510850757.4A priority Critical patent/CN105568322A/en
Publication of CN105568322A publication Critical patent/CN105568322A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C3/00Electrolytic production, recovery or refining of metals by electrolysis of melts
    • C25C3/36Alloys obtained by cathodic reduction of all their ions
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C3/00Electrolytic production, recovery or refining of metals by electrolysis of melts
    • C25C3/34Electrolytic production, recovery or refining of metals by electrolysis of melts of metals not provided for in groups C25C3/02 - C25C3/32
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/38Selection of substances as active materials, active masses, active liquids of elements or alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/38Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/383Hydrogen absorbing alloys
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention relates to a method for preparing nickel-based battery material and belongs to the field of battery material preparation. The method is characterized by including: mixing CeO2, NiO and SnO2 powder into binder, preparing into a circular piece after wet grinding, and sintering; hanging the sintered piece on an iron-chromium-aluminum wire to serve as a cathode, and wrapping the periphery of the sintered piece with the iron-chromium-aluminum wire; slowly heating CaCl2 in a muffle furnace; placing into an alumina crucible after cooling, and placing at the bottom of a reactor; suspending the cathode and a graphite carbon bar above molten salt for preheating during the heating process of an electrolytic furnace, and feeding argon at the same time; inserting the cathode and the graphite carbon bar into the molten salt, and applying direct currents to start electrolysis; taking out a cathode product after the electrolysis is completed, washing with distilled water, and drying under normal temperature. The method for preparing the nickel-based battery material has the advantages that the process is improved, a method which directly electrolyzes metal oxide in the molten salt to prepare metal or alloy is used, process simpleness is achieved, and the method is easy in synthesizing control, low in production cost and free of pollution.

Description

A kind of method preparing nickel radical battery material
Technical field
The invention belongs to battery material preparation field, particularly relate to a kind of method preparing nickel radical battery material.
Background technology
In recent years, along with the fast development of economy, the industries such as communication, power truck also along with and fast-developing, wherein battery is widely applied, and wherein, nickel metal hydride battery and lithium battery applications are the widest, and nickel-base alloy, as LaNi 5, CeNi 5, Ni 3sn 2deng, be the battery material comparatively commonly used.LaNi 5the industrial production process of shaped material is alloy melting method, Ni 3sn 2industrial production process have electrodip process, powder sintering etc.But the needing of these methods uses traditional method for extracting pure metal, long flow path, pollute heavy and cost is high.
Summary of the invention
The present invention is intended to solve the problem, and provides a kind of method preparing nickel radical battery material.
A kind of method preparing nickel radical battery material of the present invention, is characterized in that comprising the steps:
(1) by CeO 2, NiO, SnO 2powder is mixed into binding agent, wet-milling 2h in ball mill, is pressed into disk, sinters 5h after central bore at 850-1250 DEG C after taking out drying under 45MPa;
(2) sintered sheets is suspended on as negative electrode on Fe-Cr-Al wire, peripheral with Fe-Cr-Al wire parcel, to increase current density, accelerate speed of reaction; By CaCl 2450 DEG C are slowly warming up to, insulation 5h in retort furnace; Be placed on after cooling in alumina crucible, be placed in reactor bottom;
(3) in electrolytic furnace temperature-rise period, negative electrode and graphite carbon rod are suspended in preheating above fused salt, pass into argon gas simultaneously; Temperature of molten salt reaches 800 DEG C, negative electrode and graphite carbon rod is inserted in fused salt, passes to direct current and start electrolysis;
(4) cathode product takes out after completing by electrolysis, with distilled water flushing, dry under normal temperature.
The method preparing nickel radical battery material of the present invention, is characterized in that: described in step (1), the diameter of disk is 10mm, and quality is 2.5g.
The method preparing nickel radical battery material of the present invention, is characterized in that: described in step (3), electrolysis voltage is 3.1V, electrolysis time 12h.
The method preparing nickel radical battery material of the present invention, by improving the lifting of technique, the method of metal or alloy is prepared through Direct Electrolysis metal oxide in fused salt, technique is simple, and the method preparing nickel radical battery material of the present invention also has, and synthesis is easy to control, production cost is low and free of contamination advantage.
Embodiment
A kind of method preparing nickel radical battery material of the present invention, comprises the steps:
(1) by CeO 2, NiO, SnO 2powder is mixed into binding agent, wet-milling 2h in ball mill, is pressed into disk, sinters 5h after central bore at 850-1250 DEG C after taking out drying under 45MPa;
(2) sintered sheets is suspended on as negative electrode on Fe-Cr-Al wire, peripheral with Fe-Cr-Al wire parcel, to increase current density, accelerate speed of reaction; By CaCl 2450 DEG C are slowly warming up to, insulation 5h in retort furnace; Be placed on after cooling in alumina crucible, be placed in reactor bottom;
(3) in electrolytic furnace temperature-rise period, negative electrode and graphite carbon rod are suspended in preheating above fused salt, pass into argon gas simultaneously; Temperature of molten salt reaches 800 DEG C, negative electrode and graphite carbon rod is inserted in fused salt, passes to direct current and start electrolysis;
(4) cathode product takes out after completing by electrolysis, with distilled water flushing, dry under normal temperature.
The method preparing nickel radical battery material of the present invention, described in step (1), the diameter of disk is 10mm, and quality is 2.5g.
The method preparing nickel radical battery material of the present invention, described in step (3), electrolysis voltage is 3.1V, electrolysis time 12h.When electrolysis starts, electric current is maximum; Along with the carrying out of reaction, electric current declines rapidly, starts again to rise after about 20min; After electrolysis is about 2h, electric current slowly declines, and about 5h drops to minimum, occurs an electric current platform subsequently.Between electrode during on load voltage, the first electrolysis deoxidation of the peripheral oxide compound near wire of sample, this part sample directly contacts with fused salt, and the rate of diffusion of oxonium ion is fast, and therefore electric current is larger.Along with reaction is carried out gradually to sample inside, the compact metal that the transmission of oxonium ion will go out through the outer electrolysis of sample, be subject to diffusional resistance impact, therefore electric current declines rapidly.Electrolytic reaction continues to carry out to sample inside, forms fused salt-oxide-metal three phase boundary.Three phase boundary region expands gradually, and electric current is increased, and the metal level that the peripheral electrolysis of sample simultaneously goes out thickens, and diffusional resistance increases.When the impact of diffusional resistance exceedes affecting of three phase boundary increase, electric current starts to reduce.

Claims (3)

1. prepare a method for nickel radical battery material, it is characterized in that comprising the steps:
(1) by CeO 2, NiO, SnO 2powder is mixed into binding agent, wet-milling 2h in ball mill, is pressed into disk, sinters 5h after central bore at 850-1250 DEG C after taking out drying under 45MPa;
(2) be suspended on as negative electrode on Fe-Cr-Al wire using sintered sheets, periphery Fe-Cr-Al wire wraps up; By CaCl 2450 DEG C are slowly warming up to, insulation 5h in retort furnace; Be placed on after cooling in alumina crucible, be placed in reactor bottom;
(3) in electrolytic furnace temperature-rise period, negative electrode and graphite carbon rod are suspended in preheating above fused salt, pass into argon gas simultaneously; Temperature of molten salt reaches 800 DEG C, negative electrode and graphite carbon rod is inserted in fused salt, passes to direct current and start electrolysis;
After electrolysis completes, cathode product is taken out, with distilled water flushing, dry under normal temperature.
2. the method preparing nickel radical battery material according to claim 1, is characterized in that: described in step (1), the diameter of disk is 10mm, and quality is 2.5g.
3. the method preparing nickel radical battery material according to claim 2, is characterized in that: described in step (3), electrolysis voltage is 3.1V, electrolysis time 12h.
CN201510850757.4A 2015-11-30 2015-11-30 Method for preparing nickel-based battery material Pending CN105568322A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510850757.4A CN105568322A (en) 2015-11-30 2015-11-30 Method for preparing nickel-based battery material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510850757.4A CN105568322A (en) 2015-11-30 2015-11-30 Method for preparing nickel-based battery material

Publications (1)

Publication Number Publication Date
CN105568322A true CN105568322A (en) 2016-05-11

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510850757.4A Pending CN105568322A (en) 2015-11-30 2015-11-30 Method for preparing nickel-based battery material

Country Status (1)

Country Link
CN (1) CN105568322A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111705336A (en) * 2020-06-11 2020-09-25 华北理工大学 Method for recovering nickel simple substance from waste lithium battery

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111705336A (en) * 2020-06-11 2020-09-25 华北理工大学 Method for recovering nickel simple substance from waste lithium battery

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Application publication date: 20160511