CN105529455A - Prismatic assembly ball shaped SnO2 sodium-ion battery anode material and preparation method thereof - Google Patents

Prismatic assembly ball shaped SnO2 sodium-ion battery anode material and preparation method thereof Download PDF

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CN105529455A
CN105529455A CN201610049015.6A CN201610049015A CN105529455A CN 105529455 A CN105529455 A CN 105529455A CN 201610049015 A CN201610049015 A CN 201610049015A CN 105529455 A CN105529455 A CN 105529455A
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solution
ion battery
anode material
preparation
lithium
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CN105529455B (en
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殷立雄
柴思敏
刘长青
马建中
黄剑锋
王菲菲
孔新刚
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Shaanxi University of Science and Technology
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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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • H—ELECTRICITY
    • 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
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • H01M4/131—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
    • H01M4/13—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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Secondary Cells (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Primary Cells (AREA)

Abstract

The invention discloses a prismatic assembly ball shaped SnO2 sodium-ion battery anode material and a preparation method thereof. The preparation method of the prismatic assembly ball shaped SnO2 sodium-ion battery anode material comprises the following steps: 1) independently dissolving SnCl4.5H2O and C6H12N4 into deionized water, and preparing to obtain solution A and solution B; 2) under a function of continuous magnetic stirring, slowly adding the solution B into the solution A to form even solution C, and adding NaOH solution E into the solution C dropwise to form solution D; 3) carrying out homogeneous phase hydrothermal reaction; and 4) after the reaction ends, taking out a precursor, washing to obtain the white precursor, and freezing and drying to obtain the prismatic assembly ball shaped SnO2 sodium-ion battery anode material. The preparation method has the advantages of being low in cost, simple in operation and short in preparation period. The prepared prismatic assembly ball shaped SnO2 sodium-ion battery anode material is characterized in that the length of a prismatic block is 500nm, the diameter of the prismatic block is 30nm, the size of the assembly ball is about tens of micrometers, and the assembly ball has the advantages of high purity, high crystallinity and even morphology and has a high volume retention rate when the assembly ball is applied to the sodium-ion battery anode.

Description

Spherical SnO assembled by a kind of prism 2anode material of lithium-ion battery and preparation method thereof
Technical field
The present invention relates to sodium-ion battery technical field, particularly a kind of anode material of lithium-ion battery and preparation method thereof.
Background technology
Sodium-ion battery is a kind of model electrochemical power supply; have that raw material resources is abundant, cost is lower, specific capacity and efficiency comparatively advantages of higher; comparatively meet the requirement of scale stored energy application; in the extensive regenerative resource grid integration ability of lifting, raising electric energy service efficiency and the quality of power supply, there is application potential; simultaneously due to significant advantages such as its specific capacity are high, quality is light, the life-span is long and without memory, also have a wide range of applications in fields such as Aero-Space, hybrid-electric car and portable electric appts.In this context, sodium-ion battery causes the extensive concern in worldwide in recent years, and critical material and relation technological researching progress are rapidly.But lithium ion relatively, sodium ion has larger ionic radius (0.102nmvs.0.076nmofLi), and this makes to find suitable embedding sodium material tool and acquires a certain degree of difficulty.
Summary of the invention
A kind of prism is the object of the present invention is to provide to assemble spherical SnO 2anode material of lithium-ion battery and preparation method thereof, cost is low, simple to operate, manufacturing cycle is short, and the prism block of acquisition assembles spherical SnO 2anode material of lithium-ion battery excellent performance.
To achieve these goals, the present invention adopts following technical scheme:
Spherical SnO assembled by a kind of prism 2the preparation method of anode material of lithium-ion battery, comprises the following steps:
1) by SnCl 45H 2o and C 6h 12n 4be dissolved in respectively in aliquots of deionized water, be mixed with solution A and solution B; Wherein, m in mass ratio snCl45H2O: m c6H12N4=1:0.3 ~ 1:1.5;
2) B solution is slowly added solution A under continuing magnetic force stirring action and form homogeneous solution C, in solution C, dropwise add NaOH solution E, form solution D; The volume of solution C and the volume ratio of solution E are 5:1 ~ 2:4;
3) after question response terminates, solution D is put into hydrothermal reaction kettle and seals, carry out homogeneous phase hydro-thermal reaction;
4) after question response terminates, take out presoma, washing obtains white presoma, and freeze drying obtains prism and assembles spherical SnO 2anode material of lithium-ion battery.
Further, in solution A, the concentration of Sn is 0.4 ~ 1.3mol/L.
Further, the solubility of NaOH solution E is 0.5 ~ 1.5mol/L.
Further, the condition of homogeneous phase hydro-thermal reaction is: reaction temperature controls at 120 ~ 240 DEG C, and the reaction time controls at 8 ~ 48h.
Further, described washing is specially and distinguishes centrifuge washing 2 ~ 3 times through deionized water and absolute ethyl alcohol.
Further, described freeze drying is specially prepared presoma at the subzero 50-60 of the refrigerating chamber of freeze drier DEG C freezing 4-5h, then dry 10-12h under vacuum drying cabinet room temperature.
Spherical SnO assembled by a kind of prism 2spherical SnO assembled by prism prepared by the preparation method of anode material of lithium-ion battery 2anode material of lithium-ion battery.
Relative to prior art, the present invention has following beneficial effect:
Preparation method's cost of the present invention is low, simple to operate, manufacturing cycle is short; Prepared prism block assembles spherical SnO 2anode material of lithium-ion battery, prism block length is about 500nm, diameter is about 30nm, assembling ball size is about tens microns, and purity is high, crystallinity is strong, pattern is even, is applied to sodium-ion battery negative pole, charge-discharge performance is excellent, under the current density of 100mA/g, its first discharge capacity can reach 408.768mAh/g, circulate after 40 times and there is higher capability retention.
Accompanying drawing explanation
Fig. 1 is that spherical SnO assembled by the prism prepared by example 1 of the present invention 2the SEM figure of anode material of lithium-ion battery.
Fig. 2 is that spherical SnO assembled by the prism prepared by example 1 of the present invention 2anode material of lithium-ion battery chemical property figure.
Embodiment
Embodiment 1
Spherical SnO assembled by a kind of prism 2the preparation method of anode material of lithium-ion battery, comprises the following steps:
1) by SnCl 45H 2o is dissolved in deionized water, is mixed with the solution A that concentration is 0.4mol/L; M in mass ratio snCl45H2O: m c6H12N4=1:0.3 is by hexamethylenetetramine (C 6h 12n 4) add in aliquots of deionized water, be mixed with solution B;
2) B solution is slowly added solution A under continuing magnetic force stirring action and form homogeneous solution C, in solution C, dropwise add 0.5mol/LNaOH solution E, form solution D, rear Keep agitation 0.5; The volume of solution C and the volume ratio of solution E are 5:1;
3) after question response terminates, solution D is put into hydrothermal reaction kettle and seals, put into homogeneous phase hydro-thermal reaction instrument, reaction temperature controls at 120 DEG C, and the reaction time controls at 8h;
4) after question response terminates, take out presoma, centrifuge washing 2 times are distinguished through deionized water and absolute ethyl alcohol, obtain white presoma, by prepared presoma at the subzero 50 DEG C of freezing 5h of the refrigerating chamber of freeze drier, then under vacuum drying cabinet room temperature, namely dry 10h obtains prism and assembles spherical SnO 2anode material of lithium-ion battery.
Fig. 1 is that spherical SnO assembled by the prism prepared by the embodiment of the present invention 1 2the SEM figure of anode material of lithium-ion battery.As can be seen from the figure the surface of sample is that the length of prism block is approximately 500nm by prism block self assembly chondritic.Fig. 2 is that spherical SnO assembled by the prism prepared by the embodiment of the present invention 1 2anode material of lithium-ion battery chemical property figure.As can be seen from the figure, spherical SnO assembled by prepared prism 2anode material of lithium-ion battery under the current density of 100mA/g, its first discharge capacity can reach 408.768mAh/g, circulate after 40 times and there is higher capability retention.
Embodiment 2
Spherical SnO assembled by a kind of prism 2the preparation method of anode material of lithium-ion battery, comprises the following steps:
1) by SnCl 45H 2o is dissolved in deionized water, is mixed with the solution A that concentration is 1.3mol/L; M in mass ratio snCl45H2O: m c6H12N4=1:1.0 is by hexamethylenetetramine (C 6h 12n 4) add in aliquots of deionized water, be mixed with solution B;
2) B solution is slowly added solution A under continuing magnetic force stirring action and form homogeneous solution C, in solution C, dropwise add 1.5mol/LNaOH solution E, form solution D, rear Keep agitation 0.5; The volume of solution C and the volume ratio of solution E are 3:2;
3) after question response terminates, solution D is put into hydrothermal reaction kettle and seals, put into homogeneous phase hydro-thermal reaction instrument, reaction temperature controls at 180 DEG C, and the reaction time controls at 36h;
4) after question response terminates, take out presoma, centrifuge washing 3 times are distinguished through deionized water and absolute ethyl alcohol, obtain white presoma, by prepared presoma at the subzero 60 DEG C of freezing 4h of the refrigerating chamber of freeze drier, then under vacuum drying cabinet room temperature, namely dry 11h obtains prism and assembles spherical SnO 2anode material of lithium-ion battery.
Embodiment 3
Spherical SnO assembled by a kind of prism 2the preparation method of anode material of lithium-ion battery, comprises the following steps:
1) by SnCl 45H 2o is dissolved in deionized water, is mixed with the solution A that concentration is 0.9mol/L; M in mass ratio snCl45H2O: m c6H12N4=1:1.5 is by hexamethylenetetramine (C 6h 12n 4) add in aliquots of deionized water, be mixed with solution B;
2) B solution is slowly added solution A under continuing magnetic force stirring action and form homogeneous solution C, in solution C, dropwise add 1.0mol/LNaOH solution E, form solution D, rear Keep agitation 2; The volume of solution C and the volume ratio of solution E are 2:4;
3) after question response terminates, solution D is put into hydrothermal reaction kettle and seals, put into homogeneous phase hydro-thermal reaction instrument, reaction temperature controls at 240 DEG C, and the reaction time controls at 48h;
4) after question response terminates, take out presoma, centrifuge washing 2 ~ 3 times are distinguished through deionized water and absolute ethyl alcohol, obtain white presoma, by prepared presoma at the subzero 60 DEG C of freezing 5h of the refrigerating chamber of freeze drier, then under vacuum drying cabinet room temperature, namely dry 12h obtains prism and assembles spherical SnO 2anode material of lithium-ion battery.
SnO 2crystal has tetragonal crystal system and rhombic system two kinds, and wherein orthorhombic phase is unstable, only occurs under high-temperature and high-pressure conditions, therefore synthesizes the SnO obtained under normal circumstances 2crystal belongs to the rutile-type of tetragonal crystal system, cell parameter a=0.4738nm, c=0.3187nm.Research in recent years shows SnO 2nano material all has stronger application prospect in photocatalysis, gas sensor, transistor, Li-Ion rechargeable battery and solar cell etc., is considered to one of semiconductor nano material having application prospect most.SnO 2the electrode material of base has large (the theoretical reversible capacity 781mAhg of embedding lithium capacity -1), good cycle, the doubly forthright advantage such as good, its theoretical reversible capacity is high, and its actual reversible capacity is also much larger than the theoretical reversible capacity of various lithium battery carbon negative pole materials commercial in the market.
Because granule-morphology also may affect to the chemical property of sample, particle is less, specific area is larger, then the contact of material and electrolyte is better, Na +migration distance also can shorten, be so more conducive to the lifting of anode material of lithium-ion battery high rate performance.
The inventive method, have the advantages that preparation cost is low, simple to operate, manufacturing cycle is short, prepared prism block assembles spherical SnO 2anode material of lithium-ion battery, prism block length is about 500nm, and diameter is about 30nm, and assembling ball size is about tens microns, and purity is high, crystallinity is strong, pattern is even, is applied to sodium-ion battery negative pole and has excellent charge-discharge performance.

Claims (7)

1. spherical SnO assembled by a prism 2the preparation method of anode material of lithium-ion battery, is characterized in that, comprises the following steps:
1) by SnCl 45H 2o and C 6h 12n 4be dissolved in respectively in aliquots of deionized water, be mixed with solution A and solution B; Wherein, m in mass ratio snCl45H2O: m c6H12N4=1:0.3 ~ 1:1.5;
2) B solution is slowly added solution A under continuing magnetic force stirring action and form homogeneous solution C, in solution C, dropwise add NaOH solution E, form solution D; The volume of solution C and the volume ratio of solution E are 5:1 ~ 2:4;
3) after question response terminates, solution D is put into hydrothermal reaction kettle and seals, carry out homogeneous phase hydro-thermal reaction;
4) after question response terminates, take out presoma, washing obtains white presoma, and freeze drying obtains prism and assembles spherical SnO 2anode material of lithium-ion battery.
2. spherical SnO assembled by a kind of prism according to claim 1 2the preparation method of anode material of lithium-ion battery, is characterized in that, in solution A, the concentration of Sn is 0.4 ~ 1.3mol/L.
3. spherical SnO assembled by a kind of prism according to claim 1 2the preparation method of anode material of lithium-ion battery, is characterized in that, the solubility of NaOH solution E is 0.5 ~ 1.5mol/L.
4. spherical SnO assembled by a kind of prism according to claim 1 2the preparation method of anode material of lithium-ion battery, is characterized in that, the condition of homogeneous phase hydro-thermal reaction is: reaction temperature controls at 120 ~ 240 DEG C, and the reaction time controls at 8 ~ 48h.
5. spherical SnO assembled by a kind of prism according to claim 1 2the preparation method of anode material of lithium-ion battery, is characterized in that, described washing is specially distinguishes centrifuge washing 2 ~ 3 times through deionized water and absolute ethyl alcohol.
6. spherical SnO assembled by a kind of prism according to claim 1 2the preparation method of anode material of lithium-ion battery, is characterized in that, described freeze drying is specially prepared presoma at the subzero 50-60 of the refrigerating chamber of freeze drier DEG C freezing 4-5h, then dry 10-12h under vacuum drying cabinet room temperature.
7. spherical SnO assembled by a kind of prism according to any one of claim 1 to 6 2spherical SnO assembled by prism prepared by the preparation method of anode material of lithium-ion battery 2anode material of lithium-ion battery.
CN201610049015.6A 2016-01-25 2016-01-25 A kind of spherical SnO of prism assembling2Anode material of lithium-ion battery and preparation method thereof Active CN105529455B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109167019A (en) * 2018-09-03 2019-01-08 大同新成新材料股份有限公司 A kind of cell negative electrode material and preparation method thereof and preparation facilities

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CN104528808A (en) * 2014-12-27 2015-04-22 陕西科技大学 Preparation method of hollow tin dioxide microsphere
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CN104528808A (en) * 2014-12-27 2015-04-22 陕西科技大学 Preparation method of hollow tin dioxide microsphere
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109167019A (en) * 2018-09-03 2019-01-08 大同新成新材料股份有限公司 A kind of cell negative electrode material and preparation method thereof and preparation facilities

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