CN107146915A - A kind of preparation method of porous bismuth carbon composite - Google Patents
A kind of preparation method of porous bismuth carbon composite Download PDFInfo
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- CN107146915A CN107146915A CN201710227930.4A CN201710227930A CN107146915A CN 107146915 A CN107146915 A CN 107146915A CN 201710227930 A CN201710227930 A CN 201710227930A CN 107146915 A CN107146915 A CN 107146915A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0416—Methods of deposition of the material involving impregnation with a solution, dispersion, paste or dry powder
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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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
- H01M4/362—Composites
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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
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- 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
The invention discloses a kind of preparation method of porous bismuth carbon composite, comprise the following steps：S1. polyacrylonitrile is dispersed in dimethyl sulfoxide (DMSO), then adds bismuth salt, form sol precursor；S2. carbon cloth is immersed in S1 in sol precursor, heating, drying；S3. the carbon cloth in S2 by heating, drying is impregnated in potassium hydroxide-ethanol solution, dries, porous bismuth carbon composite is obtained after calcining；Sol precursor of the present invention be bismuth salt, polyacrylonitrile, the uniform and stable dispersion of dimethyl sulfoxide (DMSO), by carbon cloth film forming calcining obtain porous bismuth carbon composite.The present invention is simple to operate, consumes energy low, and raw material sources are wide, with low cost, easily mass produce.Obtained flexible negative pole has high carrying capacity, high-capacitance, excellent high rate performance and preferable cyclical stability advantage without outer adding additives, conductive agent and metal collector.
Description
Technical field
The invention belongs to energy storage material technical field, more particularly, to a kind of preparation side of porous bismuth-carbon composite
Method.
Background technology
The energy is the important foundation resource of human social development.But due to the world energy sources resource place of production and energy-consuming center
It is apart from each other, the sharp increase and the continuous improvement of living standards of the people of development, world population in particular with World Economics, the world
Demand for energy persistently increases, and thus causes the contention to energy resources to be growing more intense, environmental pollution exacerbation and environmental protection pressure add
Greatly.Accordingly, it would be desirable to energy-storage system is researched and developed efficiently to utilize the energy, and can repeated charge, efficiency high and environment adaptation
The strong secondary cell of property is then the important research direction of energy storage technology.
Water system battery is the secondary cell using the aqueous solution as electrolyte, and it overcomes traditional organic system battery electrolyte and held high
The shortcomings of expensive, poisonous, inflammable, ionic conductivity is low, cost of manufacture is high, as after most potential after wind energy, solar energy
One of green energy resource.Therefore, water system battery has important application prospect in the extensive energy storage field of power network rank.With material
The development of material technology, people increasingly improve to the demand of novel high-performance electrode material, in the urgent need to high performance by finding
Energy storage material is to improve the performance of water system battery, the need for meeting industry and life.
Although having had the progress of many to the positive electrode of water system battery, negative material is seldom studied, and
It is extremely potential high-performance negative pole because bismuthino material has good electric conductivity and suitable negative potential operation interval
Material.Bismuthino compound because its low cost, hypotoxicity, it is high lead oxygen, good photocatalysis and dielectric properties, used extensively
Make catalyst, optical material, gas sensor etc..But application study of the bismuthino material in energy storage field at present is seldom, at present
Almost application study not on bismuth-carbon composite in water system battery.Therefore, a kind of simple efficient, power consumption is developed low
Bismuth-carbon composite preparation method and improve bismuthino material energy-storage property it is significant.
The content of the invention
The present invention relates to a kind of high carrying capacity, high-capacitance, excellent high rate performance and preferable cyclical stability it is porous
The preparation method of bismuth-carbon composite, while being related to composite and its preparing water system that above-mentioned preparation method prepares
Application in battery.
The purpose of the present invention is achieved through the following technical solutions：
The invention provides a kind of preparation method of porous bismuth-carbon composite, comprise the following steps：
S1. polyacrylonitrile is dispersed in dimethyl sulfoxide (DMSO), then adds bismuth salt, form sol precursor；
S2. carbon cloth is immersed in S1 in sol precursor, heating, drying；
S3. the carbon cloth in S2 by heating, drying is impregnated in potassium hydroxide-ethanol solution, dries, obtain porous after calcining
Bismuth-carbon composite；
Every gram of polyacrylonitrile is added in S1（50~400） mmol L-1Bismuth salt；0.5 ~ 1.5g is added per 10ml dimethyl sulfoxide (DMSO)s
Polyacrylonitrile；The temperature of calcining is 600 ~ 800 DEG C, in potassium hydroxide-ethanol solution, and the concentration of potassium hydroxide is 0 ~ 6 mmol L-1。
Preferably, the bismuth salt is five nitric hydrate bismuths.
Preferably, the concentration of potassium hydroxide is 6 mol L in potassium hydroxide-ethanol solution-1。
Preferably, every gram of polyacrylonitrile adds 200mmol L in S1-1Bismuth salt；1g is added per 10ml dimethyl sulfoxide (DMSO)s to gather
Acrylonitrile.
Preferably, calcining is to be fired to 700 DEG C under nitrogen atmosphere and be incubated 1 hour in S3.
Preferably, carbon cloth is through over cleaning before using, and cleaning method is to go successively from water, ethanol, acetone, deionized water
It is middle to be cleaned by ultrasonic 10 minutes, then 60 DEG C of drying.
The present invention protects obtained porous bismuth-carbon composite prepared by above-mentioned preparation method simultaneously.
The present invention also protects application of the described porous bismuth-carbon composite in water system battery is prepared.
Further, the porous bismuth-carbon composite as water system battery negative material.
Compared with prior art, the invention has the advantages that and beneficial effect：
The preparation method that the present invention is provided is simple to operate, and raw material simplicity easily takes, and with low cost, energy consumption is low, it is easy to accomplish, it is prepared into
The porous bismuth arrived-carbon composite and flexible negative material is without outer adding additives, conductive agent and metal collector, and specific surface area is high, leads
Excellent electrical property, with high power capacity and excellent high rate performance, compared with the negative materials such as ripe commercial graphite electrode, storage
Energy performance is significantly increased.This material is prepared by simple directly soak with the method for calcining, large area synthesis and can be answered extensively
For industrial production, high performance negative material is provided for current water system battery, possesses great application prospect.
Brief description of the drawings
(a) is high magnification ESEM (SEM) picture of porous bismuth-carbon composite in embodiment 1 in Fig. 1, and (b) is real
Apply porous bismuth in example 1-carbon composite low range ESEM (SEM) picture.
Fig. 2 is the X-ray diffraction of porous bismuth-carbon composite of embodiment 1（XRD）Figure.
Fig. 3 is that cyclic voltammetric of the porous bismuth-carbon composite of embodiment 1 in 6 M KOH solution under 100 mV/s is bent
Line（CV）.
Fig. 4 is specific discharge capacity of the porous bismuth-carbon composite of embodiment 1 under different current densities.
Fig. 5 is the cycle life curve of porous bismuth-carbon composite of embodiment 1.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiments and the drawings, but embodiment does not do any to the present invention
The restriction of form.Unless stated otherwise, the reagent of the invention used, method and apparatus is the art conventional reagent, methods
And equipment.
Unless stated otherwise, agents useful for same and material of the present invention are purchased in market.
Embodiment 1：
Porous bismuth-carbon composite is realized by high temperature sintering.The step of synthetic method, is as follows:
(a) carbon cloth (2 cm × 3 cm) is going to be cleaned by ultrasonic 10 minutes respectively from water, ethanol, acetone, deionized water successively, so
60 DEG C of dry for standby afterwards.
(b) by 1 g polyacrylonitrile, dispersed with stirring forms colourless in 10 mL dimethyl sulfoxide (DMSO)s under the conditions of 90 DEG C of oil baths
Vitreosol, is cooled to after room temperature and adds the nitric hydrate bismuths of 970.1 mg five（Concentration is 200 mmol L-1）, continue stir until
Form transparent homogeneous colloidal sol.
(c) by carbon cloth complete wetting in the colloidal sol prepared by step (b), after carbon cloth is placed on surface plate at 60 DEG C
Baking oven in drying and natural cooling, the ganoine thin film of conductive carbon cloth surfaces one layer of shallow white uniformity of formation.
(d) carbon cloth for obtaining step (c) is impregnated in 25 mL 6 mol L-130 min in potassium hydroxide-ethanol solution,
Then dried in 60 DEG C of baking ovens, the shallow white uniformity ganoine thin film carbon cloth of carbon cloth surfaces changes into orange-yellow ganoine thin film；
(e) carbon cloth for obtaining step (d) is placed in tube furnace, and 700 DEG C are fired under nitrogen atmosphere and is heated 1 hour, natural
Porous bismuth-the carbon composite of target product is obtained after cooling.
The conditional of embodiment 1 ~ 7 and it the results are shown in Table shown in 1：
Table 1：Preparation condition and result in embodiment 1 ~ 7
| Embodiment | Polyacrylonitrile | Dimethyl sulfoxide (DMSO) | The concentration of five nitric hydrate bismuths | Potassium hydroxide-ethanol solution Concentration | Calcining heat | Conclusion |
| 1 | 1 g | 10 mL | 200 mmol L-1 | 6 mol L-1 | 700℃ | Carbon cloth surfaces have one layer of black deposit, and carrying capacity is 16.93mg cm-1, electric discharge quality specific capacitance is 91.64 mA h g-1, area specific capacitance is 1.55 mA h cm -2。 |
| 2 | 1 g | 10 mL | 50 mmol L-1 | 6 mol L-1 | 700℃ | Carbon cloth surfaces have layer black deposit, and area specific capacitance is 0.9294 mA h cm -2。 |
| 3 | 1 g | 10 mL | 100 mmol L-1 | 6 mol L-1 | 700℃ | Carbon cloth surfaces have one layer of black deposit, and area specific capacitance is 0.9447 mA h cm -2。 |
| 4 | 1 g | 10 mL | 400 mmol L-1 | 6 mol L-1 | 700℃ | Carbon cloth surfaces have one layer thicker black deposit and black powder, and area specific capacitance is 0.8719 mA h cm -2。 |
| 5 | 1 g | 10 mL | 200 mmol L-1 | 0 | 700℃ | Carbon cloth surfaces have one layer of black deposit, and there is metallic luster on surface, and area specific capacitance is 0.6965 mA h cm -2。 |
| 6 | 1 g | 10 mL | 200 mmol L-1 | 6 mol L-1 | 600℃ | Carbon cloth surfaces have one layer of thicker black deposit, and area specific capacitance is 0.7106 mA h cm -2。 |
| 7 | 1 g | 10 mL | 200 mmol L-1 | 6 mol L-1 | 800℃ | Carbon cloth surfaces black deposit is not obvious, and area specific capacitance is 0.1487 mA h cm -2。 |
Bismuth-carbon composite energy homoepitaxial is in carbon cloth substrate and with loose structure as can be seen from Figure 1, and Fig. 2 XRD is bent
Line shows that the material obtained by preparation only has two kinds of materials of bismuth with elementary and carbon.Fig. 3 CV curves show this porous bismuth-carbon compound electric
The redox reaction of high reversible can occur in aqueous KOH solution for pole, can be used as a kind of high performance water system GND
Material.Fig. 4 shows that this porous bismuth-carbon composite has very high discharge capacity and excellent high rate performance, passes through meter
Calculate, the carrying capacity of this porous bismuth-carbon composite is 16.93mg cm-1, electric discharge quality specific capacitance is 91.64 mA h g-1, face
Product specific capacitance is 1.55 mA h cm -2, it is shown that its extremely excellent energy storage characteristic.Fig. 5 cycle life curve shows this many
Hole bismuth-carbon composite electrode has excellent cyclical stability, and initial capacity can be still kept after 10000 cycle charge-discharges
83%。
Claims (9)
1. a kind of preparation method of porous bismuth-carbon composite, it is characterised in that comprise the following steps：
S1. polyacrylonitrile is dispersed in dimethyl sulfoxide (DMSO), then adds bismuth salt, form sol precursor；
S2. carbon cloth is immersed in S1 in sol precursor, heating, drying；
S3. the carbon cloth in S2 by heating, drying is impregnated in potassium hydroxide-ethanol solution, dries, obtain porous after calcining
Bismuth-carbon composite；
Every gram of polyacrylonitrile is added in S1（50~400） mmol L-1Bismuth salt；0.5 ~ 1.5g is added per 10ml dimethyl sulfoxide (DMSO)s to gather
Acrylonitrile；The temperature of calcining is 600 ~ 800 DEG C, in potassium hydroxide-ethanol solution, and the concentration of potassium hydroxide is 0 ~ 6 mmol L-1。
2. preparation method according to claim 1, it is characterised in that the bismuth salt is five nitric hydrate bismuths.
3. preparation method according to claim 1, it is characterised in that the concentration of potassium hydroxide in potassium hydroxide-ethanol solution
For 6 mol L-1。
4. according to any described preparation method of claims 1 to 3, it is characterised in that every gram of polyacrylonitrile is added in S1
200mmol L-1Bismuth salt；1g polyacrylonitrile is added per 10ml dimethyl sulfoxide (DMSO)s.
5. preparation method according to claim 4, it is characterised in that calcining is to be fired to 700 under nitrogen atmosphere in S3
DEG C and be incubated 1 hour.
6. preparation method according to claim 1, it is characterised in that carbon cloth is through over cleaning before using, and cleaning method is
It is cleaned by ultrasonic successively in going from water, ethanol, acetone, deionized water 10 minutes, then 60 DEG C of drying.
7. obtained porous bismuth-carbon composite prepared by any described preparation method of claim 1 to 6.
8. application of the porous bismuth-carbon composite in water system battery is prepared described in claim 7.
9. application according to claim 8, it is characterised in that the porous bismuth-carbon composite is used as water system battery
Negative material.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109742327A (en) * | 2018-12-29 | 2019-05-10 | 西安鸿钧睿泽新材料科技有限公司 | Preparation method of self-supporting flexible lithium ion battery carbon cloth loaded LiFePO4 positive electrode material |
| CN109909511A (en) * | 2019-03-22 | 2019-06-21 | 中国工程物理研究院化工材料研究所 | A kind of preparation method and application of bismuthino hollow nano-material |
| CN111477864A (en) * | 2020-04-13 | 2020-07-31 | 山东鲁北国际新材料研究院有限公司 | Preparation method and application of superfine metal bismuth nano material |
| CN112349881A (en) * | 2020-11-17 | 2021-02-09 | 河南电池研究院有限公司 | Manufacturing method of flexible current collector-free electrode |
| CN112442892A (en) * | 2020-11-02 | 2021-03-05 | 中国船舶重工集团公司第七一八研究所 | Method for catalytically hydrolyzing polyacrylonitrile material under acidic condition |
| CN113130873A (en) * | 2021-05-20 | 2021-07-16 | 武汉科技大学 | Porous bismuth-carbon material, preparation method and application thereof |
| CN113258025A (en) * | 2021-05-07 | 2021-08-13 | 西北工业大学 | Bismuth-based negative electrode for high-performance water-based battery and preparation method |
| CN114823153A (en) * | 2022-04-24 | 2022-07-29 | 华星先进科学技术应用研究(天津)有限公司 | Flexible sodium ion capacitor electrode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109742327A (en) * | 2018-12-29 | 2019-05-10 | 西安鸿钧睿泽新材料科技有限公司 | Preparation method of self-supporting flexible lithium ion battery carbon cloth loaded LiFePO4 positive electrode material |
| CN109909511A (en) * | 2019-03-22 | 2019-06-21 | 中国工程物理研究院化工材料研究所 | A kind of preparation method and application of bismuthino hollow nano-material |
| CN109909511B (en) * | 2019-03-22 | 2022-05-03 | 中国工程物理研究院化工材料研究所 | Preparation method and application of bismuth-based hollow nano material |
| CN111477864A (en) * | 2020-04-13 | 2020-07-31 | 山东鲁北国际新材料研究院有限公司 | Preparation method and application of superfine metal bismuth nano material |
| CN112442892A (en) * | 2020-11-02 | 2021-03-05 | 中国船舶重工集团公司第七一八研究所 | Method for catalytically hydrolyzing polyacrylonitrile material under acidic condition |
| CN112349881A (en) * | 2020-11-17 | 2021-02-09 | 河南电池研究院有限公司 | Manufacturing method of flexible current collector-free electrode |
| CN113258025A (en) * | 2021-05-07 | 2021-08-13 | 西北工业大学 | Bismuth-based negative electrode for high-performance water-based battery and preparation method |
| CN113258025B (en) * | 2021-05-07 | 2023-02-28 | 西北工业大学 | Bismuth-based negative electrode for high-performance water-based battery and preparation method |
| CN113130873A (en) * | 2021-05-20 | 2021-07-16 | 武汉科技大学 | Porous bismuth-carbon material, preparation method and application thereof |
| CN114823153A (en) * | 2022-04-24 | 2022-07-29 | 华星先进科学技术应用研究(天津)有限公司 | Flexible sodium ion capacitor electrode material |
| CN114823153B (en) * | 2022-04-24 | 2023-11-03 | 华星先进科学技术应用研究(天津)有限公司 | Flexible sodium ion capacitor electrode material |
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