CN106981650A - A kind of preparation method of nanoscale bismuth with elementary - Google Patents
A kind of preparation method of nanoscale bismuth with elementary Download PDFInfo
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- CN106981650A CN106981650A CN201710074141.1A CN201710074141A CN106981650A CN 106981650 A CN106981650 A CN 106981650A CN 201710074141 A CN201710074141 A CN 201710074141A CN 106981650 A CN106981650 A CN 106981650A
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- bismuth
- elementary
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- concentration
- trimethylammonium bromide
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 35
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 19
- 239000004744 fabric Substances 0.000 claims abstract description 15
- 150000001621 bismuth Chemical class 0.000 claims abstract description 12
- 238000009713 electroplating Methods 0.000 claims abstract description 12
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 11
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims abstract description 9
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims abstract description 9
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000003792 electrolyte Substances 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 238000004070 electrodeposition Methods 0.000 claims abstract description 4
- -1 wherein Chemical class 0.000 claims abstract description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical group Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 15
- 238000004146 energy storage Methods 0.000 abstract description 10
- 239000002086 nanomaterial Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229940075397 calomel Drugs 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 239000005486 organic electrolyte Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XZUAPPXGIFNDRA-UHFFFAOYSA-N ethane-1,2-diamine;hydrate Chemical compound O.NCCN XZUAPPXGIFNDRA-UHFFFAOYSA-N 0.000 description 1
- BEGBSFPALGFMJI-UHFFFAOYSA-N ethene;sodium Chemical group [Na].C=C BEGBSFPALGFMJI-UHFFFAOYSA-N 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
Classifications
-
- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a kind of preparation method of nanoscale bismuth with elementary, nanoscale bismuth with elementary is generated on conductive carbon cloth by electrochemical deposition method；Electrolyte is the mixed aqueous solution of bismuth salt, cetyl trimethylammonium bromide and disodium edta, wherein, bismuth salt concentration is（5~30）mmol/L；The cetyl trimethylammonium bromide concentration is（30~80）mmol/L；The disodium edta concentration is（0.1~0.3）mol/L；The electroplating voltage is 1 ~ 0V；The electroplating time is 10 ~ 90min.The preparation method energy consumption that the present invention is provided is low, raw material simplicity easily takes, it is simple to operate, it is easily achieved, the bismuth with elementary nano material prepared, specific surface area is high, electric conductivity is excellent, with good energy-storage property, good negative material is provided for current energy storage problem, possesses great application prospect.
Description
Technical field
The invention belongs to energy storage material preparing technical field, more particularly, to a kind of preparation side of nanoscale bismuth with elementary
Method.
Background technology
With the explosive growth and the fast development of society of population, one of society and the foundation stone promptly developed, people are used as
Class is also growing to the various demands of the energy.And the existing future society that can not have been met for a long time with traditional fossil energy is to energy
The various demands in source, in addition, along with the exploitation of fossil energy, greenhouse effects are increasingly serious, and ecological environment goes from bad to worse, and
The problems such as solving community energy skewness, reproducible green energy resource has become focus of concern.With society's warp
The development of Ji and science and technology, various new exploitation of energy resources and is realized newly using requiring to research and develop different types of energy accumulating device
The Efficient Conversion of the energy and utilization.Realize the deep development of new energy and efficiently utilization, new and effective, stable power storage dress
The development put is crucial.
The ion battery of traditional organic electrolyte has wide electrochemical window, but organic electrolyte is inflammable, poisonous, such as
Fruit can bring serious safety and environmental problem using incorrect.And water system electrolyte environment is friendly and safe, and its ion
High two orders of magnitude of Conductivity Ratio organic bath, are expected to realize the high power of battery, required for also avoiding organic bath
Strict manufacturing condition, greatly reduces production cost.Therefore water system ion battery is in the extensive energy storage field of power network rank
With important application prospect, with research deeply, researchers have had a profound understanding of the performance of water system battery to be improved, and key exists
In the high performance energy storage negative material of searching.
Cell negative electrode material common at present has carbon to bear material, such as is applied to the carbon materials of lithium ion battery,
Such material cost is relatively low easily to realize industrialization, but material capacity is relatively low, and alloy material and metal oxide materials are theoretical
Capacity is higher, but the life-span is poor.And bismuth with elementary is as a kind of emerging negative material, with high negative pole operating potential window and conjunction
Suitable current potential operation interval, theoretical specific capacitance value is higher, up to 78.9mAh/g.But bismuth with elementary cycle life is poor, big rule
Molding Preparation Method is immature, imperfection, and a variety of conditionality bismuth with elementary are applied in cell negative electrode material.
The bismuth with elementary material found at present, is used in terms of chemical industry, catalyst, semiconductor, electronic ceramics more.With it
He compares material, bismuth with elementary not only aboundresources, cheap, environment-friendly, and with good electric conductivity and suitable
Negative potential operation interval, thus be a kind of extremely potential high-performance negative material.But at present on bismuth with elementary nanometer material
The research of material is less, particularly energy storage field, and many report methods are not suitable for producing in enormous quantities.Therefore, develop a kind of easy
Easy, the efficient method for preparing bismuth with elementary nano material is significant.
The content of the invention
It is an object of the invention to overcome the deficiency such as existing, there is provided a kind of preparation method of nanoscale bismuth with elementary.
Above-mentioned purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of nanoscale bismuth with elementary, nanoscale bismuth with elementary is generated by electrochemical deposition method on conductive carbon cloth；
Electrolyte is the mixed aqueous solution of bismuth salt, cetyl trimethylammonium bromide and disodium edta, wherein, bismuth salt concentration
For（5~30）mmol/L；The cetyl trimethylammonium bromide concentration is（30~80）mmol/L；The sodium ethylene diamine tetracetate
Salinity is（0.1~0.3）mol/L；The electroplating voltage is -1 ~ 0V；The electroplating time is 10 ~ 90min.
Preferably, the concentration of bismuth salt is 20mmol/L, the cetyl trimethylammonium bromide concentration in the electrolyte
For 50mmol/L, the disodium edta concentration is 0.1mol/L.
Preferably, the electroplating voltage is -1V, the electroplating time 60min.
Preferably, the bismuth salt is five nitric hydrate bismuths.
Preferably, the working electrode is conductive carbon cloth, and described is graphite carbon rod to electrode, and the reference electrode is saturation
Calomel electrode.
Compared with prior art, the present invention has advantages below and beneficial effect：
The preparation method energy consumption that the present invention is provided is low, and raw material simplicity easily takes, simple to operate, it is easy to accomplish, the simple substance prepared
Bismuth nano material, specific surface area is high, and electric conductivity is excellent, and compared with the negative materials such as ripe commercial graphite, energy-storage property is significantly
Increase.The bismuth with elementary material of the direct high-specific surface area that is synthesized in the conductive carbon cloth of flexible substrates of this invention, while using electrification
Deposition process is learned, industrial production is can be widely applied to, provides good negative material for current energy storage problem, possess
Great application prospect.
Brief description of the drawings
(a) is high magnification ESEM (SEM) picture of bismuth with elementary in embodiment 1 in Fig. 1, and (b) is simple substance in embodiment 1
Bismuth low range ESEM (SEM) picture.
Fig. 2 is cyclic voltammetry curve of the bismuth with elementary of embodiment 1 under 100 mV/s.
Fig. 3 for embodiment 1 bismuth with elementary under different current densities discharge time.
Fig. 4 is the XRD of the bismuth with elementary 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.
Bismuth with elementary is synthesized by what electro-deposition was realized on carbon cloth.Before current load, carbon cloth (1cm × 3cm) according to
It is secondary to go to be cleaned by ultrasonic 10 minutes respectively from water, ethanol, acetone, deionized water, then 60 DEG C of dry for standby.By what is cleaned up
Carbon cloth immersion is equipped with 30ml bismuth nitrates（Five nitric hydrate bismuths）, cetyl trimethylammonium bromide and disodium edta
（Two ethylenediamine hydrate tetraacethyl sodium）In the three-electrode system of the aqueous solution mixed, wherein corresponding five nitric hydrate 300mg,
Correspondence cetyl trimethylammonium bromide 550mg, correspondence disodium edta 1.12g.Using carbon cloth as working electrode, with
Graphite carbon electrode is that, to electrode, saturation calomel is reference electrode, applies negative 1V on-load voltage to system, and keep reaction
60min.Reaction takes out carbon cloth after terminating, and gained sample is spent to be cleaned three times repeatedly from water, 60 DEG C of drying.
Embodiment 2 ~ 5
Based on the scheme of embodiment 1, the different reaction condition by regulating and controlling influences the growth of bismuth with elementary, its relation such as institute of table 1
Show.
Table 1
Comparative example 1：Other conditions be the same as Example 1, the difference is that electroplating time is 120min, can substantially observe bismuth with elementary shape
Reunite into powder, not the homoepitaxial on working electrode carbon cloth.
Comparative example 2：Other conditions be the same as Example 1, the difference is that the amount of bismuth nitrate is 800mg, can substantially be observed single
Matter bismuth forms reunion on working electrode carbon cloth, it is impossible to preferably growth.
Comparative example 3：Other conditions be the same as Example 1, unlike electroplating voltage be 2V, can substantially observe the voltage compared with
Height, obtains bulky grain powder, and bismuth with elementary can not be deposited preferably.
Comparative example 4：Other conditions be the same as Example 1, the difference is that the amount of cetyl trimethylammonium bromide is 700mg, can
Substantially to observe that bismuth with elementary more uniform can not be deposited on carbon cloth, its electric conductivity is influenceed.
From Fig. 1 and Fig. 4 from the point of view of result, bismuth with elementary nano material homoepitaxial is in carbon cloth substrate, and Fig. 3 is embodiment 1
Bismuth with elementary discharge time under different current densities.Cyclic voltammetry curve in Fig. 2 shows that this bismuth with elementary nano material has
Good invertibity and energy storage characteristic.It is 356.55mF/ by calculating the area specific capacitance value of this bismuth with elementary nano material
cm2, show its good energy-storage property.
Claims (5)
1. a kind of preparation method of nanoscale bismuth with elementary, it is characterised in that generated by electrochemical deposition method on conductive carbon cloth
Nanoscale bismuth with elementary；Electrolyte is the mixed aqueous solution of bismuth salt, cetyl trimethylammonium bromide and disodium edta,
Wherein, bismuth salt concentration is（5~30）mmol/L；The cetyl trimethylammonium bromide concentration is（30~80）mmol/L；It is described
Disodium edta concentration is（0.1~0.3）mol/L；The electroplating voltage is -1 ~ 0V；The electroplating time be 10 ~
90min。
2. preparation method according to claim 1, it is characterised in that the concentration of bismuth salt is 20mmol/ in the electrolyte
L, the cetyl trimethylammonium bromide concentration is 50mmol/L, and the disodium edta concentration is 0.1mol/L.
3. preparation method according to claim 1, it is characterised in that the electroplating voltage is -1V, the electroplating time
60min。
4. preparation method according to claim 1, it is characterised in that the bismuth salt is five nitric hydrate bismuths.
5. preparation method according to claim 1, it is characterised in that the working electrode is conductive carbon cloth, described to electricity
Extremely graphite carbon rod, the reference electrode is saturated calomel electrode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710074141.1A CN106981650B (en) | 2017-02-10 | 2017-02-10 | Preparation method of nanoscale elemental bismuth |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710074141.1A CN106981650B (en) | 2017-02-10 | 2017-02-10 | Preparation method of nanoscale elemental bismuth |
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| Publication Number | Publication Date |
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| CN106981650B CN106981650B (en) | 2020-03-13 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113193206A (en) * | 2021-03-26 | 2021-07-30 | 南通大学 | Preparation method of anode catalyst of ethanol fuel cell |
| 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 |
| CN115632132A (en) * | 2022-10-25 | 2023-01-20 | 辽宁金谷炭材料股份有限公司 | Preparation method of composite electrode of iron-chromium flow battery |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113193206A (en) * | 2021-03-26 | 2021-07-30 | 南通大学 | Preparation method of anode catalyst of ethanol fuel cell |
| 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 |
| CN115632132A (en) * | 2022-10-25 | 2023-01-20 | 辽宁金谷炭材料股份有限公司 | Preparation method of composite electrode of iron-chromium flow battery |
| CN115632132B (en) * | 2022-10-25 | 2023-10-24 | 辽宁金谷炭材料股份有限公司 | Preparation method of composite electrode of iron-chromium flow battery |
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| CN106981650B (en) | 2020-03-13 |
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