CN107394188A - A kind of preparation method of the spherical niobium oxide electrode material of lithium ion battery hollow out - Google Patents

A kind of preparation method of the spherical niobium oxide electrode material of lithium ion battery hollow out Download PDF

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CN107394188A
CN107394188A CN201710524784.1A CN201710524784A CN107394188A CN 107394188 A CN107394188 A CN 107394188A CN 201710524784 A CN201710524784 A CN 201710524784A CN 107394188 A CN107394188 A CN 107394188A
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washed
hollow out
electrode material
lithium ion
reaction
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CN107394188B (en
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黄剑锋
仵婉晨
李嘉胤
曹丽云
吴建鹏
周磊
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Shaanxi University of Science and Technology
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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
    • 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
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion 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
    • 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

Abstract

A kind of preparation method of the spherical niobium oxide electrode material of lithium ion battery hollow out, is added to hydrochloric acid solution by analytically pure oxalic acid hydrate niobium first and obtains A；Rape pollen is suspended in hydrochloric acid solution and obtains B；B is washed, is placed in culture dish after alcohol is washed and is added cetyl trimethylammonium bromide thereto again and obtain C；A and C are added in reactor, carry out hydro-thermal reaction after sealing in homogeneous reaction instrument, reaction precipitates after naturally cooling to room temperature after terminating；Sediment is washed respectively, is placed in culture dish after alcohol is washed, is transferred in vacuum drier and is dried in vacuo to obtain D；Predecessor D is taken in dry pot, is heat-treated under oxygen protection, furnace cooling afterwards, produces target product Nb2O5.The present invention using hydro-thermal calcining combined techniques efficiently and rapidly prepare be evenly distributed, the spherical Nb of the hollow out of good crystallinity2O5Crystal.Using rape pollen as Nb2O5Template, simple production process, cost are low, green, are advantageous to regulate and control the structure and pattern of prepared material.

Description

A kind of preparation method of the spherical niobium oxide electrode material of lithium ion battery hollow out
Technical field
The invention belongs to battery material technical field, is related to and prepares a kind of method of anode material for lithium-ion batteries, specifically It is related to a kind of preparation method of the spherical niobium oxide electrode material of lithium ion battery hollow out.
Background technology
Lithium ion battery has high energy density, longer as a kind of efficient energy storage device during use Service life, good security performance etc., can not only be used for multiple times, and it is a kind of more satisfactory not have pollution to environment " green " chemical energy source [Sun Xueliang, Qin Xiujuan, Bu Limin, wait carbon negative electrode material of lithium ion cell progress [J] coloured Metal engineering, 2011,63 (2):147-151].The structure of lithium ion battery is mainly made up of four parts：Positive electrode, electrolysis Liquid, barrier film, negative material, the electrode material proportion highest in the manufacturing cost of battery, and electrode material and battery The performances such as specific capacity and service life cycle are closely related, so in the research of lithium ion battery, the research one of electrode material It is directly the focus of research.
The positive electrode of lithium ion battery is typically lithium and cobalt oxides, lithium nickel oxide, lithium manganese oxide, manganese nickel cobalt at present Composite oxides, lithium-barium oxide, oxide/lithium ferrite etc., the positive electrode of the lithium ion battery of commercialization typically use LiCoO2、LiNiO2、LiMn2O4、LiCoO2、LiMn2O4[Zhang Hui, Zheng point is firm, Li Decheng, waits novel lithium battery positive electrodes Preparation and Electrochemical Properties [J] power technologies, 2013,37 (3):366-369], but its theoretical capacity is all smaller, it is real Border capacity is smaller, and has a series of influence in use.Positive electrode institute in the manufacturing process of lithium ion battery The cost occupied is highest, and the capacity of positive electrode is well below the capacity of negative material, while lithium ion battery Chemical property is heavily dependent on the structure and pattern of positive electrode, so positive electrode turns into lithium-ion electric in recent years The focus of pond research.Nb base oxides have the high capacity of comparison, have very big potentiality, Nb as anode material for lithium-ion batteries Base oxide mainly has：Nb2O5、NbO2、Nb2O3And NbO, wherein Nb2O5It is relatively most stable of.
Dunn[Kim J W,Augustyn V,Dunn B.The effect of crystallinity on the rapid pseudocapacitive response of Nb2O5[J].Advanced Energy Materials,2011,2 (1):141-148] et al. research show that T-Nb2O5 has higher theoretical capacity and operating potential window, Nb2O5 conducts Cell positive material hardly deforms upon in battery charging and discharging cyclic process, so being had little to no effect to the structure of battery [Lou Shuaifeng, Cheng Xinqun, horse Yulin, wait lithium ion batteries niobium base oxide negative material [J] chemical progress, 2015,27 (2): 000297-309], it is a kind of more satisfactory cell positive material compared to conventional electrode materials.But due to Nb2O5Itself Electric conductivity is poor, so the discharge performance of its big multiplying power has limited, therefore, improves Nb2O5Electric conductivity, change as a result, Its reaction site is improved, increases its specific surface area, so as to improve Nb2O5High rate performance and cycle performance.
By controlling Nb2O5Structure and morphology, Nb can be greatly enhanced2O5The cyclical stability of electrode material, however, The Nb that current report uses2O5Pattern be mostly nano bar-shape, nano particle, nanometer bulk etc., or need complicated preparation Technique, which greatly improves the production cost of electrode material, is unfavorable for producing in enormous quantities.Therefore, it is special to develop a kind of structure, Be advantageous to improve Nb2O5Electric conductivity, cost is cheap, the preparation Nb of simple process2O5The method of electrode material has extremely important Meaning.
The content of the invention
A kind of the shortcomings that it is an object of the invention to overcome above-mentioned existing structure, there is provided the heat treatment system that hydro-thermal calcining combines The method of the spherical niobium oxide electrode material of standby lithium ion battery hollow out.Morphology controllable can be prepared using the inventive method, The spherical Nb of the homogeneous hollow out of granular size2O5Electrode material.And preparation technology is simple, reaction time is short, and cost is low, has wide Wealthy development prospect.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：
1) it is 0.1-0.5mol/l's the analytically pure oxalic acid hydrate niobiums of 0.80-1.0g to be added into 30-70ml concentration first Hydrochloric acid solution, stir, then ultrasonic disperse obtains clear solution A；
2) take 4.3-4.7g rape pollen to be suspended in the hydrochloric acid solution that 10-50ml concentration is 0.2-0.7mol/l, stir Mix uniform mixed liquid B；
3) mixed liquid B is washed respectively, the cetyl three for adding 0.5-1g thereto again is placed in culture dish after alcohol is washed Methyl bromide ammonium, heating stirring is uniform, obtains mixed liquor C；
4) gained clear solution A and mixed liquor C are added in reactor, carry out hydro-thermal after sealing in homogeneous reaction instrument Reaction, reaction precipitate after naturally cooling to room temperature after terminating；
5) sediment obtained by step 4) is washed respectively, is placed in culture dish after alcohol is washed, is transferred in vacuum drier, It is dried in vacuo under the conditions of 100 DEG C, obtains predecessor D；
6) predecessor D is taken in dry pot, and 500-600 is risen to 5 DEG C/min heating rate from room temperature under oxygen protection DEG C processing 5h, furnace cooling afterwards, produce target product Nb2O5。
Described step 1) ultrasonic disperse 60-120min.
Packing ratio is 30-60% in described step 4) reactor, and homogeneous reaction instrument reaction temperature is 80-120 DEG C, reaction Time is 11-15h.
Beneficial effects of the present invention are embodied in：
1) using hydro-thermal calcining combined techniques efficiently and rapidly prepare be evenly distributed, the spherical Nb of the hollow out of good crystallinity2O5It is brilliant Body.
2) using rape pollen as Nb2O5Template, simple production process, cost are low, green, are advantageous to regulate and control The structure and pattern of prepared material.
Brief description of the drawings
Fig. 1 is the spherical Nb of hollow out prepared by embodiment 12O5The XRD spectrum of electrode material.
Fig. 2 is the spherical Nb of hollow out prepared by embodiment 12O5The SEM photograph of electrode material.
Fig. 3 is the spherical Nb of hollow out prepared by embodiment 12The high rate performance picture of O electrode materials.
Embodiment
Embodiment 1：
1) the analytically pure oxalic acid hydrate niobiums of 0.80g are added to the hydrochloric acid solution that 30ml concentration is 0.1mol/l first, stirred Mix uniformly, then ultrasonic disperse 60min obtains clear solution A；
2) 4.3g rape pollen is taken to be suspended in the hydrochloric acid solution that 10ml concentration is 0.2mol/l, stirring to mix Liquid B；
3) mixed liquid B is washed respectively, the cetyl front three for adding 0.5g thereto again is placed in culture dish after alcohol is washed Base ammonium bromide (CTAB), heating stirring is uniform, obtains mixed liquor C；
4) gained clear solution A and mixed liquor C are added in reactor, it is 30% to control packing ratio, equal after sealing Hydro-thermal reaction is carried out in phase reaction instrument, controlling reaction temperature is 80 DEG C, reaction time 11h, and reaction naturally cools to after terminating Precipitated after room temperature；
5) sediment obtained by step 4) is washed respectively, is placed in culture dish after alcohol is washed, is transferred in vacuum drier, It is dried in vacuo under the conditions of 100 DEG C, obtains predecessor D；
6) predecessor D is taken in dry pot, is risen under oxygen protection from room temperature with 5 DEG C/min heating rate at 500 DEG C 5h is managed, furnace cooling afterwards, produces target product Nb2O5。
Nb can successfully be prepared by being combined as can be seen from Figure 1 using hot calcination method2O5Electrode material.Nb2O5Diffraction maximum With 27-1003Nb2O5Standard card is corresponding.
As can be seen from Figure 2, prepared Nb2O5Combination electrode material is that have multiple hollow out apertures also uniform It is spherical.
Fig. 3 is the spherical Nb of prepared hollow out2The high rate performance picture of O electrode materials, current density be respectively 50mA, Under 100mA, 200mA, 500mA and 1000mA, the specific capacity of product is respectively 220,200,190,175,157mAhg-1；And When current density turns again to 50mA, product specific capacity may return to 217mAhg-1(98%), it can be seen that Nb2O5 Positive electrode high rate performance is more prominent.
Embodiment 2：
1) the analytically pure oxalic acid hydrate niobiums of 0.85g are added to the hydrochloric acid solution that 40ml concentration is 0.2mol/l first, stirred Mix uniformly, then ultrasonic disperse 80min obtains clear solution A；
2) 4.4g rape pollen is taken to be suspended in the hydrochloric acid solution that 20ml concentration is 0.3mol/l, stirring to mix Liquid B；
3) mixed liquid B is washed respectively, the cetyl front three for adding 0.6g thereto again is placed in culture dish after alcohol is washed Base ammonium bromide (CTAB), heating stirring is uniform, obtains mixed liquor C；
4) gained clear solution A and mixed liquor C are added in reactor, it is 35% to control packing ratio, equal after sealing Hydro-thermal reaction is carried out in phase reaction instrument, controlling reaction temperature is 90 DEG C, reaction time 12h, and reaction naturally cools to after terminating Precipitated after room temperature；
5) sediment obtained by step 4) is washed respectively, is placed in culture dish after alcohol is washed, is transferred in vacuum drier, It is dried in vacuo under the conditions of 100 DEG C, obtains predecessor D；
6) predecessor D is taken in dry pot, is risen under oxygen protection from room temperature with 5 DEG C/min heating rate at 525 DEG C 5h is managed, furnace cooling afterwards, produces target product Nb2O5。
Embodiment 3：
1) the analytically pure oxalic acid hydrate niobiums of 0.90g are added to the hydrochloric acid solution that 50ml concentration is 0.3mol/l first, stirred Mix uniformly, then ultrasonic disperse 100min obtains clear solution A；
2) 4.5g rape pollen is taken to be suspended in the hydrochloric acid solution that 30ml concentration is 0.4mol/l, stirring to mix Liquid B；
3) mixed liquid B is washed respectively, the cetyl front three for adding 0.7g thereto again is placed in culture dish after alcohol is washed Base ammonium bromide (CTAB), heating stirring is uniform, obtains mixed liquor C；
4) gained clear solution A and mixed liquor C are added in reactor, it is 40% to control packing ratio, equal after sealing Hydro-thermal reaction is carried out in phase reaction instrument, controlling reaction temperature is 100 DEG C, reaction time 13h, and reaction naturally cools to after terminating Precipitated after room temperature；
5) sediment obtained by step 4) is washed respectively, is placed in culture dish after alcohol is washed, is transferred in vacuum drier, It is dried in vacuo under the conditions of 100 DEG C, obtains predecessor D；
6) predecessor D is taken in dry pot, is risen under oxygen protection from room temperature with 5 DEG C/min heating rate at 550 DEG C 5h is managed, furnace cooling afterwards, produces target product Nb2O5。
Embodiment 4：
1) the analytically pure oxalic acid hydrate niobiums of 0.95g are added to the hydrochloric acid solution that 60ml concentration is 0.4mol/l first, stirred Mix uniformly, then ultrasonic disperse 110min obtains clear solution A；
2) 4.6g rape pollen is taken to be suspended in the hydrochloric acid solution that 40ml concentration is 0.6mol/l, stirring to mix Liquid B；
3) mixed liquid B is washed respectively, the cetyl front three for adding 0.8g thereto again is placed in culture dish after alcohol is washed Base ammonium bromide (CTAB), heating stirring is uniform, obtains mixed liquor C；
4) gained clear solution A and mixed liquor C are added in reactor, it is 50% to control packing ratio, equal after sealing Hydro-thermal reaction is carried out in phase reaction instrument, controlling reaction temperature is 110 DEG C, reaction time 14h, and reaction naturally cools to after terminating Precipitated after room temperature；
5) sediment obtained by step 4) is washed respectively, is placed in culture dish after alcohol is washed, is transferred in vacuum drier, It is dried in vacuo under the conditions of 100 DEG C, obtains predecessor D；
6) predecessor D is taken in dry pot, is risen under oxygen protection from room temperature with 5 DEG C/min heating rate at 575 DEG C 5h is managed, furnace cooling afterwards, produces target product Nb2O5。
Embodiment 5：
1) the analytically pure oxalic acid hydrate niobiums of 1.0g are added to the hydrochloric acid solution that 70ml concentration is 0.5mol/l, stirring first Uniformly, then ultrasonic disperse 120min obtains clear solution A；
2) 4.7g rape pollen is taken to be suspended in the hydrochloric acid solution that 50ml concentration is 0.7mol/l, stirring to mix Liquid B；
3) mixed liquid B is washed respectively, the cetyl trimethyl for adding 1g thereto again is placed in culture dish after alcohol is washed Ammonium bromide (CTAB), heating stirring is uniform, obtains mixed liquor C；
4) gained clear solution A and mixed liquor C are added in reactor, it is 60% to control packing ratio, equal after sealing Hydro-thermal reaction is carried out in phase reaction instrument, controlling reaction temperature is 120 DEG C, reaction time 15h, and reaction naturally cools to after terminating Precipitated after room temperature；
5) sediment obtained by step 4) is washed respectively, is placed in culture dish after alcohol is washed, is transferred in vacuum drier, It is dried in vacuo under the conditions of 100 DEG C, obtains predecessor D；
6) predecessor D is taken in dry pot, is risen under oxygen protection from room temperature with 5 DEG C/min heating rate at 600 DEG C 5h is managed, furnace cooling afterwards, produces target product Nb2O5。

Claims (3)

1. a kind of preparation method of the spherical niobium oxide electrode material of lithium ion battery hollow out, it is characterised in that including following step Suddenly：
1) the analytically pure oxalic acid hydrate niobiums of 0.80-1.0g are added to the hydrochloric acid that 30-70ml concentration is 0.1-0.5mol/l first Solution, stir, then ultrasonic disperse obtains clear solution A；
2) 4.3-4.7g rape pollen is taken to be suspended in the hydrochloric acid solution that 10-50ml concentration is 0.2-0.7mol/l, stirring is equal It is even to obtain mixed liquid B；
3) mixed liquid B is washed respectively, the cetyl trimethyl for adding 0.5-1g thereto again is placed in culture dish after alcohol is washed Ammonium bromide, heating stirring is uniform, obtains mixed liquor C；
4) gained clear solution A and mixed liquor C are added in reactor, progress hydro-thermal is anti-in homogeneous reaction instrument after sealing Should, reaction precipitates after naturally cooling to room temperature after terminating；
5) sediment obtained by step 4) is washed respectively, be placed in culture dish after alcohol is washed, is transferred in vacuum drier, in It is dried in vacuo under the conditions of 100 DEG C, obtains predecessor D；
6) predecessor D is taken in dry pot, is risen under oxygen protection from room temperature with 5 DEG C/min heating rate at 500-600 DEG C 5h is managed, furnace cooling afterwards, produces target product Nb2O5。
2. the preparation method of the spherical niobium oxide electrode material of lithium ion battery hollow out according to claim 1, its feature It is：Described step 1) ultrasonic disperse 60-120min.
3. the preparation method of the spherical niobium oxide electrode material of lithium ion battery hollow out according to claim 1, its feature It is：Packing ratio is 30-60% in described step 4) reactor, and homogeneous reaction instrument reaction temperature is 80-120 DEG C, during reaction Between be 11-15h.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110010960A (en) * 2019-04-10 2019-07-12 陕西科技大学 A kind of indefinite form bulk Nb2O5The preparation method of anode material for lithium-ion batteries
CN111977689A (en) * 2020-07-09 2020-11-24 南阳师范学院 Niobium pentoxide microsphere with hollow structure and preparation method and application thereof

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CN105552334A (en) * 2016-01-11 2016-05-04 杭州电子科技大学 Preparation method for carbon-film-coated zinc oxide hollow sphere
CN105712403A (en) * 2016-04-15 2016-06-29 合肥国轩高科动力能源有限公司 Preparation method for nanometer niobium pentoxide powder for lithium ion battery cathode material

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110010960A (en) * 2019-04-10 2019-07-12 陕西科技大学 A kind of indefinite form bulk Nb2O5The preparation method of anode material for lithium-ion batteries
CN111977689A (en) * 2020-07-09 2020-11-24 南阳师范学院 Niobium pentoxide microsphere with hollow structure and preparation method and application thereof

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