CN108538642A - 一种稳定化金属锂粉的制备方法 - Google Patents
一种稳定化金属锂粉的制备方法 Download PDFInfo
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- CN108538642A CN108538642A CN201810076532.1A CN201810076532A CN108538642A CN 108538642 A CN108538642 A CN 108538642A CN 201810076532 A CN201810076532 A CN 201810076532A CN 108538642 A CN108538642 A CN 108538642A
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 44
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000000843 powder Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 230000000087 stabilizing effect Effects 0.000 title claims abstract description 7
- 239000010453 quartz Substances 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 7
- 229920005989 resin Polymers 0.000 claims abstract description 7
- 229910052786 argon Inorganic materials 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 6
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000002923 metal particle Substances 0.000 claims abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 9
- 239000003990 capacitor Substances 0.000 abstract description 9
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 9
- 238000003682 fluorination reaction Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 3
- 239000007772 electrode material Substances 0.000 abstract description 3
- 239000005486 organic electrolyte Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012946 outsourcing Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
Classifications
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- 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
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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
- H01G11/04—Hybrid capacitors
- H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
-
- 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
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- 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
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- 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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- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
一种稳定化金属锂粉的制备方法，其特征是按如下步骤：取适量的全氟树脂和金属锂粉，分别放置在两个石英杯中，再将两个石英杯一起放入管式炉中，在持续通入氩气的氛围下，加热到350℃保温2小时，再降温到175℃保温12小时，使锂金属颗粒表面生成氟化锂，从而制得稳定化金属锂粉。表面氟化的稳定金属锂粉可以在空气中长时间稳定保存，当应用于电极材料时，可以有效的阻止有机电解液对锂粉的腐蚀作用和防止锂金属枝状晶体的形成。不仅为锂粉的储存带来便利，而且为锂离子电容器的预锂化过程带来方便，大大提高锂离子电容器的性能。本发明方法简单可行。
Description
技术领域
本发明涉及一种稳定化金属锂粉的制备工艺。
背景技术
锂离子电容器中的锂源主要来源于电解液中的锂离子，但在充放电过程中负极表面形成固体电解质界面（SEI）膜消耗的锂以及嵌入负极材料中难以脱嵌的不可逆锂会造成锂离子大量的流失，势必影响电容器的容量和循环性能，因此对负极的预先补锂尤为重要。实践证明，稳定金属锂粉补锂是锂离子电容器负极预锂化的一个简单有效的方式。过去常用的稳定金属锂粉是通过锂粉外包一层聚合物保护层来达到隔绝水分和氧气的目的，然而这种方式形成的稳定金属锂粉在空气中稳定存在的时间较短，当应用于电极材料时，在循环的过程中过多的锂粉会形成枝状晶体，会破坏隔膜和电极表面，造成电池的损坏。
发明内容
本发明的目的在于提出一种稳定化金属锂粉的制备方法，通过锂粉表面氟化的方式提高金属锂粉的稳定性，解决电容器循环过程中锂枝晶的形成，提高锂离子电容器的倍率、容量和循环性能。
本发明是通过以下技术方案实现的。
本发明所述的一种稳定化金属锂粉的制备方法，按如下步骤：取适量的全氟树脂（CYTOP）置于石英杯中，再加入一定量的金属锂粉，为避免二者混合，金属锂粉和全氟树脂分别放置在两个石英杯中，再将石英杯一起放入管式炉中，在持续通入氩气的氛围下，加热到350℃保温2小时，再降温到175℃保温12小时，使锂金属颗粒表面生成氟化锂，从而制得稳定化金属锂粉。
表面氟化的稳定金属锂粉可以在空气中长时间稳定保存，当应用于电极材料时，可以有效的阻止有机电解液对锂粉的腐蚀作用和防止锂金属枝状晶体的形成。不仅为锂粉的储存带来便利，而且为锂离子电容器的预锂化过程带来方便，大大提高锂离子电容器的性能。本发明方法简单可行。
附图说明
图1 为本发明制备工艺示意图。
具体实施方式
本发明将通过以下实施例作进一步说明。但本发明并不限于以下实施例。
实施例1。
在充满氩气的手套箱中，量取10ml全氟树脂（CYTOP）置于石英杯底部，将多微孔箔片固定在石英杯顶部，再称取0.5g金属锂粉置于箔片上，将石英杯在密封的情况下转移至持续通入氮气的管式炉中，加热到350℃保温2小时，再降温到175℃保温12小时，即得到表面氟化的稳定金属锂粉。
实施例2。
在充满氩气的手套箱中，量取10ml全氟树脂（CYTOP）置于石英杯底部左侧，再称取0.5g金属锂粉置于石英杯底部右侧，石英杯加盖，将石英杯在密封的情况下转移至持续通入氮气的管式炉中，加热到350℃保温2小时，再降温到175℃保温12小时，即得到表面氟化的稳定金属锂粉。
实施例3。
在充满氩气的手套箱中，称取0.5g金属锂粉和10ml全氟树脂（CYTOP）置于石英杯中，用多孔隔层将CYTOP和金属锂粉上下隔开放置，将石英杯在密封的情况下转移至持续通入氮气的管式炉中，加热到350℃保温2小时，再降温到175℃保温12小时，即得到表面氟化的稳定金属锂粉。
Claims (1)
1.一种稳定化金属锂粉的制备方法，其特征是按如下步骤：取适量的全氟树脂和金属锂粉，分别放置在两个石英杯中，再将两个石英杯一起放入管式炉中，在持续通入氩气的氛围下，加热到350℃保温2小时，再降温到175℃保温12小时，使锂金属颗粒表面生成氟化锂，制得稳定化金属锂粉。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101213039A (zh) * | 2005-07-05 | 2008-07-02 | Fmc公司 | 应用于锂离子的经稳定的金属锂粉的制备方法 |
| US20130122318A1 (en) * | 2009-12-18 | 2013-05-16 | Chemetall Gmbh | Surface-passivated lithium metal and method for the production thereof |
| CN104185522A (zh) * | 2012-01-13 | 2014-12-03 | 罗克伍德锂有限责任公司 | 稳定化的用形成合金的元素涂覆的锂金属成型体及其制备方法 |
| CN104393267A (zh) * | 2014-10-24 | 2015-03-04 | 上海四驱新能源科技有限公司 | 一种高稳定性金属锂微球粉末的制备方法 |
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2018
- 2018-01-26 CN CN201810076532.1A patent/CN108538642A/zh active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101213039A (zh) * | 2005-07-05 | 2008-07-02 | Fmc公司 | 应用于锂离子的经稳定的金属锂粉的制备方法 |
| US20130122318A1 (en) * | 2009-12-18 | 2013-05-16 | Chemetall Gmbh | Surface-passivated lithium metal and method for the production thereof |
| CN104185522A (zh) * | 2012-01-13 | 2014-12-03 | 罗克伍德锂有限责任公司 | 稳定化的用形成合金的元素涂覆的锂金属成型体及其制备方法 |
| CN104393267A (zh) * | 2014-10-24 | 2015-03-04 | 上海四驱新能源科技有限公司 | 一种高稳定性金属锂微球粉末的制备方法 |
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