CN107799758A - A kind of utilize sacrifices the method that template prepares the bar-shaped Zinc ion battery positive electrode of manganese sulfide/graphene oxide composite Nano - Google Patents
A kind of utilize sacrifices the method that template prepares the bar-shaped Zinc ion battery positive electrode of manganese sulfide/graphene oxide composite Nano Download PDFInfo
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- CN107799758A CN107799758A CN201711062295.5A CN201711062295A CN107799758A CN 107799758 A CN107799758 A CN 107799758A CN 201711062295 A CN201711062295 A CN 201711062295A CN 107799758 A CN107799758 A CN 107799758A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
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- 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
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Abstract
The invention discloses a kind of method for preparing the bar-shaped Zinc ion battery positive electrode of manganese sulfide/graphene oxide composite Nano using template is sacrificed, the molybdenum trioxide of nano bar-shape is prepared first, then molybdenum trioxide, surfactant, manganese salt, sulphur source, graphene oxide are stirred according to certain ratio at 20 ~ 40 DEG C and forms homogeneous solution, and then it is transferred in reactor, 150 ~ 180 DEG C of 12~24h of reaction are heated to, obtain molybdenum trioxide/manganese sulfide/graphene oxide composite material.Molybdenum trioxide is etched away using ammoniacal liquor, finally obtains manganese sulfide/graphene oxide composite material.This method preparation process is relatively easy, low production cost, environment friendly and pollution-free, and material has good storage zinc performance and cyclical stability, and prepared Zinc ion battery has a good application prospect.
Description
Technical field
The invention belongs to the preparation method of cell art, specially zinc ion secondary battery positive electrode material.
Background technology
The demand of the extensive energy-storage system of regenerative resource is increasingly increased at present, so as to accelerate people for new height
The invention of performance energy storage device.Human society is seeking new energy storage device always, and it has higher than advanced battery
Security, higher energy density and lower cost.At present, on the mobile apparatus, lithium ion battery is considered as before most having
Way, such as smart mobile phone, notebook computer and tablet personal computer.But in the market no matter hydrogen fuel cell or lithium ion battery,
Electrode material and manufacturing cost remain high, and these problems all limit its application, especially lithium ion battery
Potential safety hazard is present in the life of people all the time.Comparatively speaking, Zinc ion battery not only has high-energy-density, and
Have the characteristics that high power density, good high rate performance, cost are cheap and preparation technology is simple.Particularly Zinc ion battery
Inexpensive safe advantage, it will help its popularization and application in Battery Market.But grinding about Zinc ion battery positive electrode
Study carefully relatively fewer, the optional leeway of material is smaller, therefore positive electrode is the bottleneck for restricting Zinc ion battery development.Wenbao
Liu etc. have studied positive electrodes of the MnS as Zinc ion battery, under 500mAg1 current density, have 221 mAh
G-1 reversible capacity（CHEM COMMUN, 2017,53,6872-6874）.
However, the charging and discharging capacity that the cyclical stability of manganese sulfide is poor and low, it is therefore desirable to vulcanizing manganese material
It is modified research.
The content of the invention
The present invention seeks to be used as the template sacrificed by molybdenum trioxide, manganese sulfide is compound with graphene oxide, prepares
Bar-shaped manganese sulfide and the compound positive electrode of graphene oxide, so as to improve the electric conductivity of manganese sulfide and stable circulation
Property.
This method low raw-material cost, preparation process is relatively easy, and the positive electrode prepared has good circulation steady
Qualitative and higher reversible capacity.
To realize the purpose of the present invention, there is provided following technical scheme：
A kind of utilize sacrifices the side that template prepares the bar-shaped Zinc ion battery positive electrode of manganese sulfide/graphene oxide composite Nano
Method, it is characterised in that comprise the following steps：
（1）By molybdenum trioxide, nitric acid, hydrogen peroxide, deionized water according to volume ratio 1:8:8:20 ~ 25 stir 1 at 20~40 DEG C
~2 days, homogeneous solution is formed, is transferred to reactor, be placed in 150 ~ 200 DEG C of baking oven, 12~24h of successive reaction, passed through
Centrifugation obtains whiteness, then alternately washing several times, product is dried to obtain at 40~60 DEG C and received with ethanol, deionized water
The bar-shaped molybdenum trioxide of rice；
（2）By step（1）Products therefrom is with surfactant according to mol ratio 1:15~20 are dissolved in appropriate alcohol solution, stir
15~60min is mixed, forms solution A, by manganese salt and sulphur source according to mol ratio 1：1 is added separately to 10~20ml ethylene glycol solution
In, 15~60min is stirred, forms solution B；
（3）A certain amount of graphene oxide is added in deionized water, disperseed 2~6 hours under ul-trasonic irradiation, formation contains admittedly
Measure as 0.1~2 mg/ml graphene oxide suspension, by step（2）Described in solution A, B and graphene oxide mixed
Close, homogeneous suspension obtained in the presence of ultrasonic wave, solution is poured into reactor, under 150~180 DEG C of baking ovens, instead
12~24h is answered, the solid matter of black is obtained by centrifugation, alternately washing is carried out several times with ethanol, deionized water, by product
Vacuum drying obtains product at 40~60 DEG C；
（4）Above-mentioned product is scattered in appropriate ethanol solution, adds a certain amount of ammoniacal liquor, stir 1~4h, centrifugation is produced
Thing, washed respectively several times with ethanol and deionized water, obtain composite.
（5）Take step（4）In powdery product, acetylene black and Kynoar according to mass ratio 8:1:1, instill N- first
Base pyrrolidones, after 2~4h of ball mill ball milling, mixed slurry is coated on stainless steel foil, 80~110 DEG C of dryings under vacuum
10~14h, obtain positive electrode.
Further, step according to claim 1（2）Middle manganese salt is manganese acetate, manganese chloride, manganese sulfate therein one
Kind.
Further, step according to claim 1（2）Middle sulphur source is thioacetamide, thiocarbamide, sulphur simple substance, L- half
Cystine one kind therein.
Further, step according to claim 1（2）Middle alcohol solution is that ethanol, ethylene glycol, glycerine are therein
It is at least one.
It is further, a kind of according to claim 1 that using template method is sacrificed, to prepare manganese sulfide/graphene oxide compound
The content of graphene oxide is 2 ~ 4 wt% in nano bar-shape Zinc ion battery positive electrode.
It is characteristic of the invention that：Preparation process is relatively easy, low production cost, environment friendly and pollution-free, and material has good
Storage zinc performance and cyclical stability, discharge and recharge repeatedly can be carried out.It can predict that this Zinc ion battery can be in mobile electricity
Words, game machine and it is each in be widely used in mini miniaturized electronics.
Embodiment
Embodiment 1：
（1）0.6g molybdenum trioxides, 30ml nitric acid, 30ml hydrogen peroxide and 75ml deionized waters are stirred 2 days under the conditions of 25 DEG C, shape
Into homogeneous solution, it is transferred in reactor, in 160 DEG C of baking oven, reacts 24h, whiteness is obtained by centrifugation, then use
Alternately washing 3 times of ethanol, deionized water, product is dried to obtain to the molybdenum trioxide of nano bar-shape at 60 DEG C；
（2）Take step（1）In product 0.06g and 1.502g polyvinylpyrrolidones be dissolved in 30ml ethylene glycol, stir
1h, homogeneous solution A is formed, 0.9836g manganese acetate and 0.3002g thioacetamide are dissolved in 20ml ethylene glycol respectively
Among, 1h is stirred, both are mixed, forms homogeneous solution B;
（3）Take 0.044g graphene oxide to be dissolved in 30ml deionized water, 2h is disperseed under ul-trasonic irradiation, formation contains admittedly
Measure as 1.25 mg/ml graphene oxide suspension, by step（2）Described in solution A, B and graphene oxide mixed
Close, homogeneous suspension obtained in the presence of ultrasonic wave, solution is poured into reactor, under 180 DEG C of baking ovens, reaction
12h, the solid matter of black is obtained by centrifugation, alternately washing 3 times are carried out with ethanol, deionized water, by product at 60 DEG C
Vacuum drying obtains product；
（4）Taking the product 0.3g in step (3) to be added in 50ml ethanol, add 3ml ammoniacal liquor, stir 4h, centrifugation obtains product,
Washed respectively 3 times with ethanol and deionized water, obtain composite；
（5）Take above-mentioned steps（4）In composite 0.08g, acetylene black 0.01g and Kynoar 0.01g, instill N- methyl
Pyrrolidones, after ball mill grinding 4h, mixed slurry is coated on stainless steel foil, at 80 DEG C of vacuum, dries 10h, obtain
Positive electrode.
Embodiment 2：
（1）0.6024g molybdenum trioxides, 30ml nitric acid, 30ml hydrogen peroxide and 75ml deionized waters are stirred into 2d under the conditions of 25 DEG C
Homogeneous solution is formed, is placed in reactor, in 160 DEG C of baking oven, reacts 24h, centrifugation obtains white solid matter, then uses
Alternately washing 3 times of ethanol, deionized water, product is dried to obtain to the molybdenum trioxide of nano bar-shape at 60 DEG C；
（2）Take step（1）In product 0.082g and 0.513g neopelex be dissolved in 50ml deionized water,
Magnetic agitation 2h, solution A is formed, the thiocarbamide of 0.7916g manganese chlorides and 0.3044g is dissolved in 40ml deionized water, magnetic force
2h is stirred, forms homogeneous solution, referred to as solution B；
（3）Take 0.0512g graphene oxide to be dissolved in 50ml deionized water, 2h is disperseed under ul-trasonic irradiation, formed solid
Content is 1.002 mg/ml graphene oxide solution, by step（2）Described in solution A, B and graphene oxide mixed
Close, homogeneous solution obtained in the presence of ultrasound, solution is poured into reactor, under 200 DEG C of baking ovens, 15h is reacted, is led to
Cross centrifugation and obtain the solid matter of black, carry out alternately washing 3 times with ethanol and deionized water, be dried in vacuo and obtain at 80 DEG C
Product；
（4）Take the product 0.3g in step (3) to be added in 50ml ethanol, add 3ml ammoniacal liquor, 4h is stirred, by centrifuging
To product, washed respectively 3 times with ethanol and deionized water, obtain composite；
（5）Take above-mentioned steps（4）In dusty material 0.0512g, acetylene black 0.0064g and Kynoar 0.00651g, drop
Enter 1-METHYLPYRROLIDONE, after ball mill grinding 4h, mixed slurry is coated on stainless steel foil, at lower 80 DEG C of vacuum, do
Dry 12h, obtains positive electrode.
Embodiment 3：
（1）0.3562g molybdenum trioxides, 15ml nitric acid, 15ml hydrogen peroxide and 43ml deionized waters are stirred into 2d under the conditions of 25 DEG C,
Homogeneous solution is formed, is put into reactor, in 160 DEG C of baking oven, reacts 24h, white solid matter is obtained by centrifugation,
Again with alternately washing 3 times of ethanol and deionized water, product is dried to obtain bar-shaped molybdenum trioxide at 60 DEG C；
（2）Take step（1）In product 0.03g and 0.2g cetabs be dissolved in 30ml deionized water, stir
Mix 4h, form homogeneous solution, referred to as solution A, by 0.358g manganese nitrate and 0.484g Cys be dissolved in 30ml go from
In sub- water, 4h is stirred, forms homogeneous solution, referred to as solution B；
（3）Take 0.0321g graphene oxide to be dissolved in 30ml deionized water, 1h is disperseed under ul-trasonic irradiation, formed solid
Content is 1.07mg/ml graphene oxide suspension, by step（2）Described in solution A, B and graphene oxide mixed
Close, homogeneous suspension obtained in the presence of ultrasonic wave, solution is placed in reactor, under 180 DEG C of baking ovens, reaction
24h, centrifugation obtain the solid matter of black, carry out alternately washing 3 times with ethanol and deionized water, are dried in vacuo at 80 DEG C
To product；
（4）Take the product 0.2g in step (3) to be added in 40ml ethanol, add 2ml ammoniacal liquor, stir 1h, centrifugation is produced
Thing, washed respectively 3 times with ethanol and deionized water, obtain composite；
（5）Take above-mentioned steps（4）In dusty material 0.0521g, acetylene black 0.0064g and Kynoar 0.00651g, drop
Enter 1-METHYLPYRROLIDONE, after grinding 4h with ball mill ball, mixed slurry is coated on stainless steel foil, at lower 80 DEG C of vacuum,
14h is dried, obtains positive electrode.
Claims (5)
1. a kind of utilize sacrifices the side that template prepares the bar-shaped Zinc ion battery positive electrode of manganese sulfide/graphene oxide composite Nano
Method, it is characterised in that comprise the following steps：
（1）By molybdenum trioxide, nitric acid, hydrogen peroxide, deionized water according to volume ratio 1:8:8:20 ~ 40 are heated to after 20 ~ 25 mixing
DEG C and stir 1 ~ 2 day, form homogeneous solution, be transferred to reactor, be placed in 150 ~ 200 DEG C of baking oven, successive reaction 12 ~
24h, milky white solution is obtained, alternately washing several times, product is dried to obtain at 40 ~ 60 DEG C and received with ethanol and deionized water
The bar-shaped molybdenum trioxide of rice；
（2）By step（1）Products therefrom is with surfactant according to mol ratio 1:15 ~ 20 are dissolved in appropriate alcohol solution, stir
15 ~ 60min is mixed, forms uniform solution, referred to as solution A, by manganese salt and sulphur source according to mol ratio 1：1 is sequentially added 10 ~ 20ml's
In alcohol solution, 15~60min is stirred, forms uniform solution, referred to as solution B；
（3）A certain amount of graphene oxide is added in deionized water, 2~6h is disperseed under ul-trasonic irradiation, forms solid content
For 0.1~2 mg/ml graphene oxide suspension, by step（2）Described in solution A, B and graphene oxide mixed
Close, homogeneous suspension is obtained in the presence of ultrasonic wave, solution is poured into reactor, is positioned over 150 ~ 200 DEG C of baking oven
In, 12 ~ 24h of successive reaction, centrifugation obtains the solid matter of black, is alternately washed several times with ethanol and deionized water, 40 ~ 60
Vacuum drying obtains product at DEG C；
（4）Above-mentioned product is scattered in appropriate ethanol solution, adds a certain amount of ammoniacal liquor, stir 1~4h, centrifugation is produced
Thing, then washed respectively several times with ethanol and deionized water, obtain composite；
（5）Take step（4）In powdery product, acetylene black and Kynoar according to mass ratio 8:1:1, instill N- methyl pyrroles
Pyrrolidone, after 2~4h of ball mill grinding, mixed slurry is coated on stainless steel foil, it is dry in 80~110 DEG C under vacuum condition
Dry 10~14h, obtains positive electrode.
2. according to claim 1, it is a kind of using sacrifice template prepare manganese sulfide/bar-shaped zinc of graphene oxide composite Nano from
The method of sub- cell positive material, it is characterised in that the step（2）Middle manganese salt is that manganese acetate, manganese chloride, manganese sulfate are therein
It is a kind of.
3. according to claim 1, it is a kind of using sacrifice template prepare manganese sulfide/bar-shaped zinc of graphene oxide composite Nano from
The method of sub- cell positive material, it is characterised in that the step（2）Middle sulphur source is thioacetamide, thiocarbamide, sulphur simple substance, L-
Cysteine one kind therein.
4. according to claim 1, it is a kind of using sacrifice template prepare manganese sulfide/bar-shaped zinc of graphene oxide composite Nano from
The method of sub- cell positive material, it is characterised in that the step（2）Middle alcohol solution be ethanol, ethylene glycol, glycerine wherein
At least one.
5. according to claim 1, it is a kind of using sacrifice template prepare manganese sulfide/bar-shaped zinc of graphene oxide composite Nano from
The method of sub- cell positive material, it is characterised in that the step（3）The content of middle graphene oxide is 2~4 wt%.
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| CN201711062295.5A CN107799758A (en) | 2017-11-02 | 2017-11-02 | A kind of utilize sacrifices the method that template prepares the bar-shaped Zinc ion battery positive electrode of manganese sulfide/graphene oxide composite Nano |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110828802A (en) * | 2019-11-07 | 2020-02-21 | 吉首大学 | Preparation method of high-power aqueous zinc ion battery positive electrode material |
| CN113830820A (en) * | 2021-10-20 | 2021-12-24 | 安徽工程大学 | Tubular gallium oxide nano material and preparation method and application thereof |
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| CN101412541A (en) * | 2007-10-19 | 2009-04-22 | 中国科学院大连化学物理研究所 | Method for synthesizing rod-like and echinoid molybdena-based nano-material |
| CN104134783A (en) * | 2014-07-31 | 2014-11-05 | 北京科技大学 | Nano-NiS/graphene composite anode material and preparation method thereof |
| CN106159239A (en) * | 2016-08-30 | 2016-11-23 | 安徽师范大学 | The preparation method of a kind of Manganese monosulfide ./graphene nanocomposite material, lithium ion battery negative, lithium ion battery |
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2017
- 2017-11-02 CN CN201711062295.5A patent/CN107799758A/en active Pending
Patent Citations (3)
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| CN101412541A (en) * | 2007-10-19 | 2009-04-22 | 中国科学院大连化学物理研究所 | Method for synthesizing rod-like and echinoid molybdena-based nano-material |
| CN104134783A (en) * | 2014-07-31 | 2014-11-05 | 北京科技大学 | Nano-NiS/graphene composite anode material and preparation method thereof |
| CN106159239A (en) * | 2016-08-30 | 2016-11-23 | 安徽师范大学 | The preparation method of a kind of Manganese monosulfide ./graphene nanocomposite material, lithium ion battery negative, lithium ion battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110828802A (en) * | 2019-11-07 | 2020-02-21 | 吉首大学 | Preparation method of high-power aqueous zinc ion battery positive electrode material |
| CN113830820A (en) * | 2021-10-20 | 2021-12-24 | 安徽工程大学 | Tubular gallium oxide nano material and preparation method and application thereof |
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