CN104701033A - Preparation method of super-capacitor containing boron ion liquid - Google Patents
Preparation method of super-capacitor containing boron ion liquid Download PDFInfo
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- CN104701033A CN104701033A CN201510120213.2A CN201510120213A CN104701033A CN 104701033 A CN104701033 A CN 104701033A CN 201510120213 A CN201510120213 A CN 201510120213A CN 104701033 A CN104701033 A CN 104701033A
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- 229910052796 boron Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000003990 capacitor Substances 0.000 title description 3
- 239000007788 liquid Substances 0.000 title 1
- 239000002608 ionic liquid Substances 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 19
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 19
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 11
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 125000003368 amide group Chemical group 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 239000006258 conductive agent Substances 0.000 claims description 2
- 239000011888 foil Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 238000004146 energy storage Methods 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 239000011244 liquid electrolyte Substances 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract 1
- 239000003792 electrolyte Substances 0.000 description 18
- 238000006243 chemical reaction Methods 0.000 description 7
- 230000014759 maintenance of location Effects 0.000 description 6
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 4
- NQPJDJVGBDHCAD-UHFFFAOYSA-N 1,3-diazinan-2-one Chemical compound OC1=NCCCN1 NQPJDJVGBDHCAD-UHFFFAOYSA-N 0.000 description 3
- YAMHXTCMCPHKLN-UHFFFAOYSA-N imidazolidin-2-one Chemical compound O=C1NCCN1 YAMHXTCMCPHKLN-UHFFFAOYSA-N 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- QLNJFJADRCOGBJ-UHFFFAOYSA-N propionamide Chemical compound CCC(N)=O QLNJFJADRCOGBJ-UHFFFAOYSA-N 0.000 description 2
- 229940080818 propionamide Drugs 0.000 description 2
- 239000011829 room temperature ionic liquid solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000004693 imidazolium salts Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
- H01G11/58—Liquid electrolytes
- H01G11/62—Liquid electrolytes characterised by the solute, e.g. salts, anions or cations therein
-
- 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
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Manufacturing & Machinery (AREA)
- Secondary Cells (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
本发明公开了一种含硼离子液体超级电容器的制备方法，其制备方法为：在手套箱中氩气氛围条件下，按配比称取含硼锂盐及有机化合物；搅拌加热制成稳定均一透明的离子液体溶液；利用制备的活性炭电极组装成超级电容器。本发明的优点为：涉及的锂离子液体电解质具有良好的安全性及稳定性，而且无须添加任何添加剂，其较高电化学电压有利于提高超级电容器的能量储存，而且没有牺牲其良好的能量密度和循环性能。The invention discloses a method for preparing a boron-containing ionic liquid supercapacitor. The preparation method comprises: weighing boron-containing lithium salt and an organic compound according to the proportion in a glove box under an argon atmosphere; stirring and heating to make a stable, uniform and transparent The ionic liquid solution; use the prepared activated carbon electrode to assemble into a supercapacitor. The advantages of the present invention are: the lithium ion liquid electrolyte involved has good safety and stability, and does not need to add any additives, and its high electrochemical voltage is conducive to improving the energy storage of supercapacitors without sacrificing its good energy density and cycle performance.
Description
技术领域 technical field
本发明涉及电化学新能源领域，具体涉及一种含硼离子液体超级电容器的制备方法。 The invention relates to the field of electrochemical new energy, in particular to a method for preparing a boron-containing ionic liquid supercapacitor.
背景技术 Background technique
超级电容是一种介于物理电源和化学电源间的新型绿色储能能源，将能量存储于电极材料与电解质界面。其根本优势还在于它的双电层电荷储能，区别于化学电源电池，没有化学反应造成的体相变化，能够使充放电循环达到几十万（105 - 106）次，从根本上可以解决电池循环寿命短的问题，因此超级电容应用前景将会非常广阔。 Supercapacitor is a new type of green energy storage energy between physical power supply and chemical power supply, which stores energy at the interface between electrode materials and electrolytes. Its fundamental advantage lies in its electric double layer charge energy storage, which is different from chemical power batteries. There is no bulk phase change caused by chemical reactions, and it can achieve hundreds of thousands of charge and discharge cycles (10 5 - 10 6 ), fundamentally It can solve the problem of short cycle life of the battery, so the application prospect of the supercapacitor will be very broad.
目前水系超级电容器由于其电压低的缺点研制，应用有机溶剂电解液的超级电容的研制获得了较快的发展。由于其具有更高的工作电压（2.7V），表现出了高比能量、寿命长等特点，受到了广泛关注。但是，有机溶剂电解液的应用也带来了安全性问题也引起了消费者的注意，即在非常状态下，如冲撞、挤压、异常充放电等极端环境，发生燃烧等不安全行为。其内在原因就是现有超级电容采用了易燃易氧化的有机溶剂电解液。 At present, due to the disadvantage of low voltage of water-based supercapacitors, the research and development of supercapacitors using organic solvent electrolytes has achieved rapid development. Due to its higher operating voltage (2.7V), high specific energy, long life and other characteristics, it has received extensive attention. However, the application of organic solvent electrolyte also brings safety issues and attracts the attention of consumers, that is, in extreme conditions such as collision, extrusion, abnormal charging and discharging, etc., unsafe behaviors such as burning occur. The internal reason is that the existing supercapacitor uses a flammable and oxidizable organic solvent electrolyte.
本发明的目的是为了解决上述材料的不足，提供一种安全的新型含硼离子液体电解液并用于超级电容中。这种电解液中的锂盐具有较大阴离子及低晶格能，由于羰基氧与Li+的配位作用而导致锂盐的解离和有机单体间氢键的断裂，进而形成均一稳定的室温离子液体。与咪唑鎓盐或其它有机季胺离子类室温离子液体体系相比，N 上取代基结构简单，从而体系粘度降低、离子电导率增大。以这种离子液体为电解液组装碳对称超级电容器，电压可达3.5V以上，适合在273-363K温度区间使用。高温状态性能更优（如313-363K）。这种超级电容器克服了水系电容器电压低（1V）及有机系超级电容器高温使用电解液恶化造成容量衰减等缺点，具有一定的应用优势。 The object of the present invention is to provide a safe novel boron-containing ionic liquid electrolyte for use in supercapacitors in order to solve the deficiencies of the above materials. The lithium salt in this electrolyte has a large anion and low lattice energy. Due to the coordination between the carbonyl oxygen and Li + , the lithium salt dissociates and the hydrogen bond between the organic monomers is broken, thereby forming a uniform and stable lithium salt. room temperature ionic liquid. Compared with imidazolium salt or other organic quaternary ammonium ionic room temperature ionic liquid systems, the structure of the substituent on N is simple, so the viscosity of the system is reduced and the ion conductivity is increased. Using this ionic liquid as the electrolyte to assemble a carbon symmetric supercapacitor, the voltage can reach above 3.5V, and it is suitable for use in the temperature range of 273-363K. High temperature performance is better (such as 313-363K). This supercapacitor overcomes the shortcomings of the low voltage (1V) of the aqueous capacitor and the capacity fading caused by the deterioration of the electrolyte of the organic supercapacitor at high temperature, and has certain application advantages.
发明内容 Contents of the invention
本发明提供了一种含硼离子液体超级电容器的制备方法，该电容器电解质制作过程无须添加任何添加剂，在超级电容中应用具有良好的能量密度及循环性能。 The invention provides a method for preparing a boron-containing ionic liquid supercapacitor. The capacitor electrolyte does not need to add any additives in the production process, and has good energy density and cycle performance when applied in supercapacitors.
本发明采取的技术方案是：一种含硼离子液体超级电容器的制备方法，其特征在于制备方法如下： The technical scheme adopted by the present invention is: a preparation method of a boron-containing ionic liquid supercapacitor, which is characterized in that the preparation method is as follows:
（1）在手套箱中氩气氛围条件下，按配比称锂盐及有机化合物； (1) Under the condition of argon atmosphere in the glove box, weigh the lithium salt and the organic compound according to the ratio;
（2）搅拌加热制成稳定均一透明的离子液体电解液； (2) Stir and heat to make a stable, uniform and transparent ionic liquid electrolyte;
（3）利用制备的活性炭电极组装成超级电容器。 (3) The prepared activated carbon electrodes were used to assemble supercapacitors.
进一步，所述制成离子液体溶液所用的锂盐是下列锂盐的一种或几种； Further, the lithium salt used for making the ionic liquid solution is one or more of the following lithium salts;
。 .
进一步，所述制成离子液体溶液所用的有机化合物是指含有酰胺基团的有机物，如尿素、乙烯脲、丙烯脲、乙酰胺、丙酰胺等一种或几种。 Further, the organic compound used to prepare the ionic liquid solution refers to an organic compound containing an amide group, such as one or more of urea, ethylene urea, propylene urea, acetamide, and propionamide.
进一步，所述活性炭电极指活性炭、导电剂及粘结剂混溶于NMP涂膜而成。 Further, the activated carbon electrode is formed by dissolving activated carbon, conductive agent and binder in NMP coating film.
进一步，活性炭电极涂膜所涉及到的集流体是金属箔片或薄片。 Further, the current collector involved in the activated carbon electrode coating film is a metal foil or sheet.
优选：含硼锂盐与有机化合物的摩尔配比0.12-0.30，搅拌速度为20-100 r/min, 加热温度为50-90摄氏度，加热时间10-60分钟，采用该离子液体电解液组装的超级电容器，能量密度达到15-50Wh/kg以上, 循环10000次，容量保持60%以上。 Preferably: the molar ratio of boron-containing lithium salt to organic compound is 0.12-0.30, the stirring speed is 20-100 r/min, the heating temperature is 50-90 degrees Celsius, and the heating time is 10-60 minutes. The ionic liquid electrolyte is used to assemble the For supercapacitors, the energy density reaches above 15-50Wh/kg, the cycle is 10,000 times, and the capacity remains above 60%.
更优选：含硼锂盐与有机化合物的摩尔配比0.18-0.25，搅拌速度为40-60 r/min, 加热温度为60-80摄氏度，加热时间15-40分钟。采用该离子液体电解液组装的超级电容器，能量密度达到40Wh/kg以上, 循环10000次，容量保持70%以上。 More preferably: the molar ratio of the boron-containing lithium salt to the organic compound is 0.18-0.25, the stirring speed is 40-60 r/min, the heating temperature is 60-80 degrees Celsius, and the heating time is 15-40 minutes. The supercapacitor assembled with the ionic liquid electrolyte has an energy density of more than 40Wh/kg, cycles 10,000 times, and maintains more than 70% of the capacity.
本发明的优点为：本发明涉及的锂离子液体电解质具有良好的安全性及稳定性，而且无须添加任何添加剂，其较高电化学电压有利于提高超级电容器的能量储存，而且没有牺牲其良好的能量密度和循环性能。 The advantages of the present invention are: the lithium ion liquid electrolyte involved in the present invention has good safety and stability, and does not need to add any additives, and its higher electrochemical voltage is conducive to improving the energy storage of supercapacitors without sacrificing its good Energy density and cycle performance.
具体实施方式 Detailed ways
实施例1： Example 1:
将锂盐与丙烯脲充分干燥，并在手套箱中氩气氛按照摩尔配比0.12称量，混合样品在反应瓶中。搅拌速度为40 r/min, 加热温度为60摄氏度，加热时间15分钟。采用该离子液体电解液组装的超级电容器，能量密度达到31Wh/kg, 0.5A/g循环10000次，容量保持68%。 The lithium salt and propylene urea were fully dried, weighed in an argon atmosphere in a glove box according to a molar ratio of 0.12, and mixed samples were placed in a reaction flask. The stirring speed is 40 r/min, the heating temperature is 60 degrees Celsius, and the heating time is 15 minutes. The supercapacitor assembled with the ionic liquid electrolyte has an energy density of 31Wh/kg, a 0.5A/g cycle of 10,000 cycles, and a capacity retention of 68%.
实施例2： Example 2:
将锂盐与尿素充分干燥，并在手套箱中氩气氛按照摩尔配比0.12称量，混合样品在反应瓶中。搅拌速度为20r/min, 加热温度为50摄氏度，加热时间60分钟。采用该离子液体电解液组装的超级电容器，能量密度达到34Wh/kg, 0.5A/g循环10000次，容量保持68%。 Fully dry the lithium salt and urea, weigh them in an argon atmosphere in a glove box according to the molar ratio of 0.12, and mix the samples in a reaction bottle. The stirring speed is 20r/min, the heating temperature is 50 degrees Celsius, and the heating time is 60 minutes. The supercapacitor assembled with the ionic liquid electrolyte has an energy density of 34Wh/kg, a 0.5A/g cycle of 10,000 cycles, and a capacity retention of 68%.
实施例3： Example 3:
将锂盐与乙烯脲充分干燥，并在手套箱中氩气氛按照摩尔配比0.18称量，混合样品在反应瓶中。搅拌速度为60 r/min, 加热温度为90摄氏度，加热时间10分钟。采用该离子液体电解液组装的超级电容器，能量密度达到37Wh/kg, 0.5A/g循环10000次，容量保持72%。 The lithium salt and ethylene urea were fully dried, weighed in an argon atmosphere in a glove box according to a molar ratio of 0.18, and mixed samples in a reaction bottle. The stirring speed is 60 r/min, the heating temperature is 90 degrees Celsius, and the heating time is 10 minutes. The supercapacitor assembled with the ionic liquid electrolyte has an energy density of 37Wh/kg, a 0.5A/g cycle of 10,000 cycles, and a capacity retention of 72%.
实施例4： Example 4:
将锂盐与乙酰胺充分干燥，并在手套箱中氩气氛按照摩尔配比0.22称量，混合样品在反应瓶中。搅拌速度为100 r/min, 加热温度为70摄氏度，加热时间30分钟。采用该离子液体电解液组装的超级电容器，能量密度达到41Wh/kg, 0.5A/g循环10000次，容量保持78%。 The lithium salt and acetamide were fully dried, weighed in an argon atmosphere in a glove box according to a molar ratio of 0.22, and mixed samples were placed in a reaction bottle. The stirring speed is 100 r/min, the heating temperature is 70 degrees Celsius, and the heating time is 30 minutes. The supercapacitor assembled with the ionic liquid electrolyte has an energy density of 41Wh/kg, a 0.5A/g cycle of 10,000 cycles, and a capacity retention of 78%.
实施例5： Example 5:
将锂盐与丙酰胺充分干燥，并在手套箱中氩气氛按照摩尔配比0.26称量，混合样品在反应瓶中。搅拌速度为50r/min, 加热温度为80摄氏度，加热时间40分钟。采用该离子液体电解液组装的超级电容器，能量密度达到32 Wh/kg, 0.5A/g循环10000次，容量保持66%。 The lithium salt and propionamide were fully dried, weighed in an argon atmosphere in a glove box according to the molar ratio of 0.26, and mixed samples in a reaction bottle. The stirring speed is 50r/min, the heating temperature is 80 degrees Celsius, and the heating time is 40 minutes. The supercapacitor assembled with the ionic liquid electrolyte has an energy density of 32 Wh/kg, a 0.5A/g cycle of 10,000 cycles, and a capacity retention of 66%.
实施例6： Embodiment 6:
将锂盐与乙烯脲和丙烯脲充分干燥，并在手套箱中氩气氛按照摩尔配比0.3称量，混合样品在反应瓶中。搅拌速度为60r/min, 加热温度为70摄氏度，加热时间40分钟。采用该离子液体电解液组装的超级电容器，能量密度达到29 Wh/kg, 0.5A/g循环10000次，容量保持64%。 Fully dry the lithium salt, ethylene urea and propylene urea, weigh them in an argon atmosphere in a glove box according to the molar ratio of 0.3, and mix the samples in a reaction flask. The stirring speed is 60r/min, the heating temperature is 70 degrees Celsius, and the heating time is 40 minutes. The supercapacitor assembled with the ionic liquid electrolyte has an energy density of 29 Wh/kg, a 0.5A/g cycle of 10,000 cycles, and a capacity retention of 64%.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140113202A1 (en) * | 2012-10-22 | 2014-04-24 | Ut-Battelle, Llc | Electrolyte compositions for lithium ion batteries |
| CN104701032A (en) * | 2015-01-07 | 2015-06-10 | 南昌大学 | Preparation method of boron ionic liquid containing super capacitor |
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| PINGYING ZHAO等: "A Novle Solvent-free Room Temperature Molten Salt Electrolyte Based on LiODFB and 2-Oxazolidinone for EDLCs", 《ZEITSCHRIFT FUR PHYSIKALISCHE CHEMIE INTERNATIONAL JOURNAL OF RESEARCH IN PHYSICAL CHEMISTRY AND CHEMICAL PHYSICS》 * |
| ZHENYU YANG等: "a novel room temperature molten salt electrolyte based on libob and 2-oxazolidinone for electrochemical capacitors", 《ZEITSCHRIFT FUR PHYSIKALISCHE CHEMIE INTERNATIONAL JOURNAL OF RESEARCH IN PHYSICAL CHEMISTRY AND CHEMICAL PHYSICS》 * |
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