CN105590760A - 一种锂离子电容器负极新型预嵌锂方法 - Google Patents
一种锂离子电容器负极新型预嵌锂方法 Download PDFInfo
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- 239000003990 capacitor Substances 0.000 title claims abstract description 35
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 27
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
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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
- H01G11/66—Current collectors
- H01G11/68—Current collectors 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
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Abstract
本发明为一种锂离子电容器负极新型嵌锂方法以及利用其制造锂离子超级电容器的方法。在负极集流体先表面形成一层稳定的锂源——锂金属薄膜或锂化合物,然后将负极可嵌锂活性材料涂覆到负极集流体上,涂覆采用新的双面垂直式共挤出涂布法,将涂布制备好的极片与隔膜、正极片交替层叠或卷绕,最后组装成超级电容器单体,经真空干燥条件下注入相关电解液,由于负极活性材料与锂金属或锂化合物是直接接触,且每一层都有相对应的接触,因此可以更高效、可靠地进行负极活性材料的预嵌锂,大大降低了预嵌锂的时间,同时可以确保每层极片嵌锂量的一致性,从而可以大改善锂离子超级电容器的一致性和单体的循环寿命。
Description
[技术领域]
本发明涉及电极、电极制备方法以及电容器,具体涉及锂离子电容器、负极及其嵌锂方法。
[背景技术]
超级电容器,也称电化学电容器(ElectrochemicalCapacitor),最初的电化学电容器是由1957年的美国通用电气公司Becker提出,并于1968年美国标准石油公司率先研制成功商业化的碳基双电层超级电容器。1975~1980年之间,加拿大的康维(B.E.Conway)及合作者通过对氧化钌电容特性的研究工作,系统阐述了氧化钌表面氧化还原反应的赝电容机理,大大地扩展了超级电容器的研究范围。目前,超级电容器储能的机理可分为两类:第一类是通过界面电荷分离形成的双电层来储存能量,称之为双电层电容器(electricdouble-layercapacitors,EDLC);第二类是以电极表面或体相的二维或准二维空间上的氧化还原反应而产生的与电极电位相关的法拉第准电容机理来储存能量,相关的电容器被称之为法拉第准电容器或赝电容器。
通过采用高比容量的活性炭材料、耐高电压电解质以及采用有机体系电解液等措施,传统的EDLC的比能量已经达到5~10Wh·kg-1的发展瓶颈,为进一步提高超级电容器的能量密度,研究者开始将目光投向锂离子电池(LIB)与EDLC相结合的新型超级电容器——含锂混合电容器。经过最近几十年的发展,研究者开发多种类型的含锂混合电容器,包括含锂化合物/AC、含锂化合物+AC/AC、含锂化合物+AC/钛氧化物、AC/钛氧化物、AC/预嵌锂碳材料等体系。其中,日本富士重工SUBARU技术研究中心的Hatozaki将正极为活性炭,负极为预嵌入锂的石墨、软炭、硬炭等锂子电池碳材料的混合电容器体系命名为锂离子电容器(Lithium-ionCapacitor,LIC)。
虽然LIC的名称最初由日本的富士重工公司提出,但较早之前,类似的体系已经出现,Amatucci等首报道了以活性炭为正极,锂钛氧化物Li4Ti5O12为负极的混合超级电容,通过选用纳米Li4Ti5O12作为负极,提高负极的表观反应速率,在1.5mol/L的LiPF6/乙腈溶液,制作的模拟电容器比能量可达到20Wh/kg,在10C充放电倍率下的容量保持率达到90%,5000次循环后,容量损失为10~15%。然而,该体系也存在材料因有的差的扩散系数和差的电子电导率等问题。
在工业化生产中,生产锂离子超级电容器需要对负极进行预嵌锂,因此LIC的制造技术工艺要比EDLC和锂离子电池复杂,寻找合适的可靠的预嵌锂技术是公认的技术难点。最初的预嵌锂方式多采用Li金属与负极短路的方式。富士重工公布的技术是在最外层相对于负极引入第三极金属锂箔,同时正、负极集流体使用具有多孔结构的金属铜、铝箔,预嵌锂过程是将锂箔与负极短路来实现,此方法对环境要求苛刻,而且不容易控制锂的嵌入量及均一性。三星电机株式会社公布了的技术是在隔膜表面通过真空气相沉积形成一层锂薄膜,组装成将锂薄膜与负极直接接触,这种方法可以缩短掺杂的时间,提高产品的生产能力。吴锋等采用在正极引入非金属锂第三极来对负极进行深度为5~60%的预嵌锂处理,该第三极主要成份为具有一定不可逆脱锂性质的富锂化合物,在对电容器活化过程中实现对负极的预嵌锂。Zheng等使用粒径为10~200nm,表面具有钝化膜的的稳定金属锂粉(SLMP)作为锂源,与负极硬炭材料混合后用干法制成极片,活性炭为正极组装成LIC单体,此种方法可以在干燥房中实现,对环境要求要好于富士重工工艺,且SLMP也有商品化产品。
[发明内容]
本发明的目的在于降低预嵌锂的时间,改善锂离子超级电容器的一致性和单体的循环寿命。
为了实现上述目的提供一种锂离子电容器负极嵌锂方法,包括以下步骤:
a.所用的负极集流体预先表面形成一层稳定的锂源,
b.将负极可嵌锂活性材料涂覆到已经有锂源的负极集流体正反两面上。
所述的涂敷为双面垂直式共挤出涂敷。
所述的锂源是锂金属薄膜或锂化合物。
所述的锂化合物是:
LiMO2,M=Co、Ni、Mn、Cu或Fe,
LiNixZ1-xO2,Z=Co、Ni、Mn、Cu、Fe、La、V、Al、Mg或Zn,0<x<1,
锂硫复合物,
或锂聚合物中的一种。
所述的锂金属颗粒形成的薄膜层采用稳定化金属锂(stabilizedlithiummetalpowder,SLMP)。
所述的锂金属颗粒形成的薄膜层的形成采用真空气相沉积法、磁控溅射法、采用SLMP分散液涂布法,或锂化合物涂布法形成。
负极可嵌锂活性材料为硬炭、聚偏氟乙烯PVDF、导电炭黑的混合物。
本发明还包括一种锂离子电容器负极采用上述锂离子电容器负极嵌锂方法制备得到。
本发明还包括一种超级电容器,通过上述的锂离子电容器负极与隔膜、正极片交替层叠或卷绕,组装成超级电容器单体后,经真空干燥条件下注入相关电解液制备得到。
本发明同现有技术相比:
(1)采用新型负极预嵌锂方法,可以确保每一层负极活性物层都有锂直接接触,更好的进行负极预嵌锂,通过控制负极集流体上涂覆或沉积的锂金属或锂化化合物的量,来控制负极预嵌锂的量,从而确保每一层活性物的精确嵌锂量;
(2)采用本方法进行负极的预嵌锂,可以尽量不采用现在预嵌锂方法中所用的有孔集流体,因此可以大大节约成本,同时可以保证单体的更低的内阻,提高超级电容器的输出功率;
[附图说明]
图1为本发明采用有锂金属薄膜的铜集流体进行负极活性物涂覆的示意图;
图2为本发明锂离子超级电容器示意图;
图中10.收卷辊20.干燥炉30.浆料40.挤出头50.放卷辊60有锂薄膜的铜集流体70.挤出头80.浆料
91.铝集流体92.硬碳93.铜集流体94.锂金属薄膜95.隔膜96.活性炭。
[具体实施方式]
以下,结合实施例和附图对于本发明做进一步说明,应当理解,实施例和附图仅用于解释说明而不用于限定本发明的保护范围。
(1)正极片制作步骤:按一定的质量比例称取活性炭、石墨粉、导电炭黑(SP)、羧甲基纤维素(CMC)、丁苯橡胶乳液(SBR),按一定次序混合均匀,搅拌成浆料,然后涂布在集流体(铝箔)上,经120~130℃真空烘干后,碾压后,裁剪成需要的尺寸。
(2)负极片制作前处理(负极集流体锂金属薄膜化):将稳定化锂金属粉末(SLMP)、碳纳米管按1:1~9:1比例分散至甲苯溶液中,然后涂覆至铜箔上,干燥后得到表面有锂金属薄膜的铜负极集流体。(或在真空中沉积一层锂金属薄膜)。通过调节稳定化锂金属粉末中单质锂与负极所涂覆活性物质的比例可以达到负极不同预嵌锂量。
(3)负极片制作步骤:按一定的质量比例称取硬炭、聚偏氟乙烯PVDF、导电炭黑,按一定次序混合均匀,搅拌成浆料,然后采用双面垂直式共挤出涂布法进行涂敷,这种方法对于本领域的技术人员是清楚的。本实施例给出一个头涂敷的例子,如图2所示,通过一放卷辊与松卷辊传递有锂薄膜的铜集流体,在靠近放卷辊的位置的集流体正反两面位置附近分别设置挤出头,挤出头内灌有混合后的负极浆料,浆料通过挤出头挤出后涂敷在铜集流体的两个面上,在涂敷后通过设置在放卷与收卷辊之间的干燥炉进行90~130℃真空烘干后,再经过碾压后,裁剪成一定的尺寸,即得到本发明中所需的负极片。
(4)将上述取得的正极极片、隔膜、负极极片按层叠或卷绕方式组装成电芯,如图2所示,顺序依次为正极极片/隔膜/负极极片,然后将叠好的电芯的正、负极极群焊接在相应极耳上,最后将电芯封装好在成型的铝塑膜或铝质或钢质壳中。经注液、化成、老化等工序后,即可得到本发明所述的锂离子超级电容器。
通过调节稳定化锂金属粉末的涂覆量,来控制负极不同预嵌锂量,具体实施例如下(同时与采用锂片预嵌锂方法和负极未预锂样品进行对比,数据见对比样):
Claims (9)
1.一种锂离子电容器新型负极预嵌锂方法,其特征在于包括以下步骤:
a.所用的负极集流体预先表面形成一层稳定的锂源,
b.将负极可嵌锂活性材料涂覆到已经有锂源的负极集流体正反两面上。
2.如权利要求1所述的一种锂离子电容器新型负极预嵌锂方法,其特征在于所述的涂敷为双面垂直式共挤出涂敷。
3.如权利要求1所述的一种锂离子电容器新型负极预嵌锂方法,其特征在于所述的锂源是锂金属颗粒形成的薄膜层或锂化合物涂覆层。
4.如权利要求2所述的一种锂离子电容器新型负极预嵌锂方法,其特征在于所述的锂化合物是:
LiMO2,M=Co、Ni、Mn、Cu或Fe,
LiNixZ1-xO2,Z=Co、Ni、Mn、Cu、Fe、La、V、Al、Mg或Zn,0<x<1,
锂硫复合物,
或锂聚合物中的一种。
5.如权利要求2所述的一种锂离子电容器新型负极预嵌锂方法,其特征在于所述的锂金属颗粒形成的薄膜层采用稳定化金属锂。
6.如权利要求2所述的一种锂离子电容器新型负极预嵌锂方法,其特征在于所述的锂金属颗粒形成的薄膜层的形成采用真空气相沉积法、磁控溅射法、SLMP分散液涂布法,或锂化合物涂布法形成。
7.如权利要求1所述的一种锂离子电容器新型负极预嵌锂方法,其特征在于负极可嵌锂活性材料为硬炭、聚偏氟乙烯PVDF、导电炭黑的混合物。
8.一种锂离子电容器负极,其特征在于采用权利要求1~7任一所述的锂离子电容器负极嵌锂方法制备得到。
9.一种超级电容器,其特征在于通过将权利要求7所述的锂离子电容器负极与隔膜、正极片交替层叠或卷绕,组装成超级电容器单体后,经真空干燥条件下注入相关电解液制备得到。
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