CN109742342A - A method of preparing high-performance zinc oxide/zinc ferrite combination electrode material - Google Patents
A method of preparing high-performance zinc oxide/zinc ferrite combination electrode material Download PDFInfo
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- CN109742342A CN109742342A CN201811559946.6A CN201811559946A CN109742342A CN 109742342 A CN109742342 A CN 109742342A CN 201811559946 A CN201811559946 A CN 201811559946A CN 109742342 A CN109742342 A CN 109742342A
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Abstract
High-performance zinc oxide/zinc ferrite combination electrode material method is prepared the invention discloses a kind of.Respectively using Zinc vitriol and green vitriol as zinc source and source of iron, it is greater than 1:2 by adjusting zinc-iron ratio, prepares zinc oxide/zinc ferrite (ZnO/ZnFe using chemical coprecipitation combination Freeze Drying Technique2O4) combination electrode material.The method of the present invention very simple, at low cost, yield is high, preparation condition is easily controllable, the ZnO/ZnFe of preparation2O4Composite material has preferable storage lithium performance as lithium ion battery negative material.
Description
Technical field
The present invention relates to the technical fields of lithium ion battery negative material, and in particular to a kind of high-performance zinc oxide/ferrous acid
Zinc (ZnO/ZnFe2O4) combination electrode material preparation method.
Background technique
The fast development of mobile electronic device, electric vehicle industry and large-scale energy-storage system, proposes the performance of lithium ion battery
Go out increasingly higher demands, designs and develops the electrode material with height ratio capacity, good circulation stability and high rate performance
Key as the development of next-generation lithium ion battery.Currently, lithium ion battery negative material is mainly using graphite negative electrodes,
Its theoretical specific capacity is only 372mAh/g, and this greatly limits the promotions of battery overall performance.Transition metal oxide due to
Theoretical specific capacity (500~1000mAh/g), good safety and cheap price with higher and be considered as most
One of novel anode material of development prospect.In these transition metal oxide negative electrode materials, ZnFe2O4With ZnO material in addition to
It can be stored up outside lithium with conversion reaction mechanism, lithium can also be stored up by alloy mechanism, there is up to~1000mAh/g theoretical specific capacity
And by the concern of researcher.But ZnFe2O4Have with the poorly conductive of ZnO material and in charge and discharge process significant
Bulk effect causes its cycle performance to be deteriorated.The synergistic effect of different materials can be given full play to by preparing combination electrode material, into
And improve the chemical property of electrode material.Based on considerations above, the present invention proposes a kind of foolproof preparation high-performance
ZnO/ZnFe2O4The method of combination electrode material.
Summary of the invention
High-performance zinc oxide/zinc ferrite (ZnO/ZnFe is prepared the purpose of the present invention is to provide a kind of2O4) combination electrode material
The method of material.
Specific steps are as follows:
(1) ZnSO for being 1.25~1.75:2 by zinc-iron molar ratio4·7H2O and FeSO4·7H2O is dissolved with distilled water, is matched
Zinc-iron solution is set, and makes the molar concentration 0.10mol/L of Fe ion in solution.
(2) configuration molar concentration is 0.32mol/L ammonia spirit.
It (3) is 25 DEG C in temperature, under conditions of speed of agitator is 400 revs/min, into zinc-iron solution obtained by step (1)
Step (2) gained ammonia spirit, the volume of the ammonia spirit of dropwise addition and the volume of zinc-iron solution is added dropwise with constant pressure buret
The ratio between be 5:2, the reaction time 6 hours, stand 10~24 hours, filtration washing to neutrality obtains filter cake.
(4) filter cake obtained by step (3) is freeze-dried, then will be freeze-dried complete filter cake and be placed in Muffle furnace
In air atmosphere, 600 DEG C are warming up to 5 DEG C/min of heating rate since room temperature, and after keeping the temperature 2 hours at 600 DEG C
Cooled to room temperature to get arrive zinc oxide/zinc ferrite (ZnO/ZnFe2O4) combination electrode material.
The present invention prepares high-performance ZnO/ZnFe using chemical coprecipitation combination Freeze Drying Technique2O4Combination electrode material
Material, method very simple, at low cost, yield is high, preparation condition is easily controllable.
Detailed description of the invention
Fig. 1 is zinc oxide/zinc ferrite (ZnO/ZnFe obtained by Examples 1 to 32O4) combination electrode material XRD spectrum.
Fig. 2 is zinc oxide/zinc ferrite (ZnO/ZnFe obtained by Examples 1 to 32O4) combination electrode material cycle performance figure.
Fig. 3 is zinc oxide/zinc ferrite (ZnO/ZnFe obtained by Examples 1 to 32O4) combination electrode material high rate performance figure.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below, it is pointed out that following embodiment be in order to
Those skilled in the art more fully understands the present invention, rather than limiting the scope of the invention, the technology people in the field
Member can make some nonessential modifications and adaptations according to above content.
Embodiment 1:
(1) by 1.79g ZnSO4·7H2O and 2.78g FeSO4·7H2O mixing is dissolved and fixed with distilled water with distilled water
Hold into 100mL volumetric flask, configure zinc-iron solution, the molar concentration of Fe ion is 0.10mol/L in solution at this time.
(2) ammonia spirit that configuration molar concentration is 0.32mol/L.
It (3) is 25 DEG C in temperature, it is molten to zinc-iron obtained by 100mL step (1) under conditions of speed of agitator is 400 revs/min
250mL step (2) gained ammonia spirit is added dropwise with constant pressure buret in liquid, is stirred to react 6 hours, stands 10 hours, mistake
Filter washing obtains filter cake to neutrality.
(4) filter cake obtained by step (3) is freeze-dried, then will be freeze-dried complete sample and be placed in Muffle furnace
In air atmosphere, 600 DEG C are warming up to from room temperature with 5 DEG C/min of heating rate, and natural after keeping the temperature 2 hours at 600 DEG C
It is cooled to room temperature to get zinc oxide/zinc ferrite (ZnO/ZnFe2O4) combination electrode material.
Embodiment 2:
(1) by 2.15g ZnSO4·7H2O and 2.78g FeSO4·7H2O mixing is dissolved and fixed with distilled water with distilled water
Hold into 100mL volumetric flask, configure zinc-iron solution, the molar concentration of Fe ion is 0.10mol/L in solution at this time.
(2) configuration molar concentration is 0.32mol/L ammonia spirit.
It (3) is 25 DEG C in temperature, under conditions of speed of agitator is 400 revs/min, to the zinc-iron solution of 100mL step (1)
The middle ammonia spirit 250mL that step (2) configuration is added dropwise with constant pressure buret, is stirred to react 6 hours, stands 10 hours, mistake
Filter washing is to neutrality.
(4) step (3) resulting filter cake is freeze-dried, then will be freeze-dried complete sample and be placed in Muffle furnace
In in air atmosphere, be warming up to 600 DEG C from room temperature with 5 DEG C/min of heating rate, and after keeping the temperature 2 hours at 600 DEG C from
So it is cooled to room temperature to get zinc oxide/zinc ferrite (ZnO/ZnFe2O4) combination electrode material.
Embodiment 3:
(1) by 2.50g ZnSO4·7H2O and 2.78g FeSO4·7H2O mixing, is dissolved with a certain amount of distilled water and is used in combination
Distilled water is settled in 100mL volumetric flask, configures zinc-iron solution, and the molar concentration of Fe ion is 0.10mol/L in solution at this time.
(2) configuration molar concentration is about 0.32mol/L ammonia spirit.
It (3) is 25 DEG C in temperature, under conditions of speed of agitator is 400 revs/min, to the zinc-iron solution of 100mL step (1)
The middle ammonia spirit 250mL that step (2) configuration is added dropwise with constant pressure buret, is stirred to react 6 hours, stands 10 hours, mistake
Filter washing is to neutrality.
(4) step (3) resulting filter cake is freeze-dried, then will be freeze-dried complete sample and be placed in Muffle furnace
In in air atmosphere, be warming up to 600 DEG C from room temperature with 5 DEG C/min of heating rate, and after keeping the temperature 2 hours at 600 DEG C from
So it is cooled to room temperature to get zinc oxide/zinc ferrite (ZnO/ZnFe2O4) combination electrode material.
Electrochemical property test: the zinc oxide/zinc ferrite (ZnO/ZnFe for respectively preparing Examples 1 to 32O4) compound electric
For pole material as active material, conductive black (Super P) is used as conductive agent, and Kynoar (PVDF) presses matter as binder
The ratio mixed grinding measured than 6:3:1 is uniform, and about after sixty minutes, suitable N- methyl -2- pyrrolidines is then added in milling time
Ketone (NMP) continues to be ground to form sticky uniform slurry, and finally slurry is uniformly coated on copper foil, and it is dry to be placed in vacuum
It is dried at 80 DEG C in dry case to constant weight, obtains electrode slice after being punched with SZ-50-15 type tablet press machine.With the electricity obtained after punching
Pole piece is working electrode, and metal lithium sheet is to electrode, and polypropylene porous film (Celgard 2400) is diaphragm, 1mol/L LiPF6
Ethylene carbonate (EC), dimethyl carbonate (DMC) and diethyl carbonate (DEC) mixed liquor (v (EC): v (DMC): v (DEC)
=1:1:1) it is electrolyte, CR2016 type button cell is assembled into the glove box full of argon gas.Using new prestige battery testing
System (model BTS-5V1A) carries out constant current charge-discharge test to the battery after assembling and high rate performance is tested, charge and discharge electricity
Pressure range is 0.01~3.0V, and wherein the current density of cycle performance test is 0.5A/g, and charge and discharge cycles 500 are enclosed, forthright again
The current density that can be tested is respectively 0.5,1,2,3,4,5,0.5A/g, and specific test result is listed in Tables 1 and 2.
Table 1: the cycle performance test result of Examples 1 to 3 sample
As shown in table 1 and attached drawing 2, the resulting electrode material of Examples 1 to 3 has stronger storage lithium activity, preferably follows
Ring stability.
Table 2: the high rate performance test result of Examples 1 to 3 sample
As shown in Table 2 and Fig. 3, the resulting electrode material of Examples 1 to 3 has preferable high rate performance, especially implements
The resulting electrode material of example 1 has relatively better high rate performance.
As shown in Figure 1, for Examples 1 to 3 preparation electrode material XRD spectrum, as can be seen from the figure embodiment 1~
The sample of 3 preparations is ZnO/ZnFe2O4Combination electrode material.
Claims (1)
1. a kind of prepare high-performance zinc oxide/zinc ferrite combination electrode material method, it is characterised in that specific steps are as follows:
(1) ZnSO for being 1.25 ~ 1.75:2 by zinc-iron molar ratio4·7H2O and FeSO4·7H2O is dissolved with distilled water, configures zinc
Ferrous solution, and make 0.10 mol/L of molar concentration of Fe ion in solution；
(2) configuration molar concentration is 0.32 mol/L ammonia spirit；
(3) it is 25 DEG C in temperature, under conditions of speed of agitator is 400 revs/min, is used into zinc-iron solution obtained by step (1)
Constant pressure buret is added dropwise ammonia spirit obtained by step (2), the volume of the volume of the ammonia spirit of dropwise addition and zinc-iron solution it
Than the reaction time 6 hours, standing 10 ~ 24 hours, filtration washing to neutrality obtains filter cake for 5:2；
(4) filter cake obtained by step (3) is freeze-dried, then will be freeze-dried complete filter cake and be placed in Muffle furnace
Under air atmosphere, 600 DEG C are warming up to 5 DEG C/min of heating rate since room temperature, and keeps the temperature 2 hours at 600 DEG C
Afterwards cooled to room temperature to get arrive zinc oxide/zinc ferrite combination electrode material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112678874A (en) * | 2020-12-20 | 2021-04-20 | 桂林理工大学 | N-doped FeMnO3Preparation method and application of electrode material |
| CN114824217A (en) * | 2022-04-28 | 2022-07-29 | 江苏理工学院 | Modified ferrite electrochemical material and preparation method and application thereof |
Citations (5)
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| WO2012163426A1 (en) * | 2011-06-01 | 2012-12-06 | Westfälische Wilhelms Universität | Electrode material for lithium and lithium ion batteries |
| CN103094558A (en) * | 2012-12-18 | 2013-05-08 | 深圳市贝特瑞新能源材料股份有限公司 | Zinc-ferrite-based nanometer composite as well as preparation method and application thereof |
| CN104617268A (en) * | 2015-01-23 | 2015-05-13 | 重庆大学 | Zinc cathode material of nickel-zinc battery as well as preparation method and application of zinc cathode material |
| CN106025271A (en) * | 2016-05-31 | 2016-10-12 | 山东玉皇新能源科技有限公司 | Preparation method of negative electrode material zinc ferrite |
| CN107311234A (en) * | 2017-06-28 | 2017-11-03 | 大连理工大学 | A kind of preparation method of zinc oxide/zinc ferrite nano composite material and application |
-
2018
- 2018-12-20 CN CN201811559946.6A patent/CN109742342A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012163426A1 (en) * | 2011-06-01 | 2012-12-06 | Westfälische Wilhelms Universität | Electrode material for lithium and lithium ion batteries |
| CN103094558A (en) * | 2012-12-18 | 2013-05-08 | 深圳市贝特瑞新能源材料股份有限公司 | Zinc-ferrite-based nanometer composite as well as preparation method and application thereof |
| CN104617268A (en) * | 2015-01-23 | 2015-05-13 | 重庆大学 | Zinc cathode material of nickel-zinc battery as well as preparation method and application of zinc cathode material |
| CN106025271A (en) * | 2016-05-31 | 2016-10-12 | 山东玉皇新能源科技有限公司 | Preparation method of negative electrode material zinc ferrite |
| CN107311234A (en) * | 2017-06-28 | 2017-11-03 | 大连理工大学 | A kind of preparation method of zinc oxide/zinc ferrite nano composite material and application |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112678874A (en) * | 2020-12-20 | 2021-04-20 | 桂林理工大学 | N-doped FeMnO3Preparation method and application of electrode material |
| CN114824217A (en) * | 2022-04-28 | 2022-07-29 | 江苏理工学院 | Modified ferrite electrochemical material and preparation method and application thereof |
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