CN112897510A - 一种管壁坍缩的碳纳米管及其应用 - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 39
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 39
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 5
- 150000003624 transition metals Chemical class 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 4
- 238000011065 in-situ storage Methods 0.000 claims abstract description 3
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
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- 238000010532 solid phase synthesis reaction Methods 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- 229910001414 potassium ion Inorganic materials 0.000 description 8
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 238000012983 electrochemical energy storage Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
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- 239000007767 bonding agent Substances 0.000 description 1
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- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
-
- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/36—Diameter
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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
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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
本发明公开了一种管壁坍缩的碳纳米管及其应用,碳纳米管管壁具有坍缩结构,实现碳纳米管缺陷的增加,使用该管壁坍缩的碳纳米管制备的电极和电池,使电池结构更加稳定,提高电池的倍率与循环性能;采用固相法实现过渡金属Ni催化碳纳米管,再通过酸洗掉过多的Ni金属单质,最后得到管壁坍缩的碳纳米管,增加大量缺陷;过渡金属Ni原位催化生长的碳纳米管,可显著提升材料在充放电过程中的导电性和结构稳定性。
Description
技术领域
本发明属于复合材料合成领域,具体涉及一种管壁坍缩的碳纳米管及其应用。
背景技术
电化学储能技术的应用有效的解决了清洁能源的存储、利用和转换方面的问题,在未来具有广阔的发展前景。目前锂离子电池由于其本身优异的性能比如能量密度高、能量转换率高和安全性好等优点被广泛应用于电化学储能领域。但是随着锂离子电池相关研究的不断进行,锂离子电池的容量已经出现了难以提升的情况。为了满足不断发展的大型储能设备的需求,我们开始将目光转移到其他的电池体系。近年来,钠离子电池(SIBs)和钾离子电池(PIBs)因Na源和K源在地壳中丰度高(Na和K分别为2.36wt.%和2.09wt.%),因而受到广泛的关注。尤其对于PIBs,K/K+的氧化还原电位(-2.93V)低于Na/Na+(-2.71V),从而保证了储钾电池更高的工作电压和能量密度,有望成为新一代高能量密度和低成本电化学能储能系统。然而,由于PIBs具有较大的K+半径、较慢的反应动力学等特性,其应用仍然面临着极大的挑战。
碳质材料由于其具有可调节的微观结构,低成本和环境友好等特性,已成为钾离子电池(PIB)最有希望的阳极之一。其中碳纳米管是一种常见的碳材料,碳纳米管具有良好的石墨化结构,导电性能十分优异。更重要的是,钾离子可以嵌入到石墨层中形成KC8,就像锂离子一样可具有较大的比容量(279mAh g-1),低工作电压平台(<0.5V)和较高的初始库伦效率(ICE),所有这些都有助于PIB的实际应用。
发明内容
本发明的目的在于提供一种管壁坍缩的碳纳米管及其应用,碳纳米出现管壁坍缩,使电池结构更加稳定,提高电池的倍率与循环性能。
为实现上述目的,本发明采用如下技术方案予以实现:
一种管壁坍缩的碳纳米管,碳纳米管管壁具有坍缩结构。
进一步,碳纳米管通过过渡金属Ni原位催化生长得到,然后经酸洗掉过多的Ni金属单质形成管壁坍缩的碳纳米管。
进一步,碳纳米管管径为200nm。
同时,提供一种管壁坍缩的碳纳米管电池正极,含有权利要求1至3任一项所述的管壁坍缩的碳纳米管。
还提供一种电池,含有管壁坍缩的碳纳米管电池正极。
本发明具有以下有益效果:
1)本发明通过控制反应过程中的工艺条件,再配合不同金属催化剂催化碳纳米管生长,实现碳纳米管缺陷的增加,碳管的出现管壁坍缩,得到管壁坍缩的碳纳米管,在钾离子嵌入的过程中坍缩的管壁提供了更多的反应位点,并且由于碳管高度石墨化的结构可以有效地抑制充放电反应过程中的体积膨胀问题,使电池结构更加稳定,提高电池的倍率与循环性能。使用该管壁坍缩的碳纳米管制备的电极和电池,使电池结构更加稳定,提高电池的倍率与循环性能。
2)本发明首先采用固相法实现过渡金属Ni催化碳纳米管,再通过酸洗掉过多的Ni金属单质,最后得到管壁坍缩的碳纳米管,增加大量缺陷。
3)本发明所制备的过渡金属Ni原位催化生长的碳纳米管,有高度的石墨化的管壁,有良好的电子传输路径和机械强度,可显著提升材料在充放电过程中的导电性和结构稳定性。
4)本发明所使用的原料廉价易得,制备方法简单,研究该材料结构对电化学储钾性能的影响,建立该材料在储钾过程中的构效机制,为拓展钾离子电池电极材料体系和性能的提升提供参考依据。
附图说明
图1为实施例1样品的扫描电镜图
图2为实施例1样品的钠离子电池循环性能图
具体实施方式
本发明的管壁坍缩的碳纳米管制备方法为:
实施例1:
1)将1g硝酸镍、2g三聚氰胺在研钵中充分研磨,并将研磨后产物置于石英或氧化铝坩埚,并将坩埚置于管式炉中,在氩气气氛下,以5℃/min的升温速率匀速升温至700℃。达到温度后停止加热,将产物置于温度为0-80℃的低温冷阱中0.5~2h,快速降温至冷阱温度;
2)待产物自然冷却收集得到产物1Ni/C。
3)将获得的产物在浓度为3M的硝酸中静置,腐蚀掉大多数的镍金属单质,为产物2。
将该样品在扫描电镜下进行观察,从图1中可以看出,产物为管径为200nm且出现管壁坍缩的碳管。将所得的产物制备成纽扣式钾离子电池,具体的封装步骤如下:将活性粉,导电剂(Super P),粘接剂(PVDF)按照质量比为8:1:1的配比研磨均匀后,制成浆料,用涂膜器均匀地将浆料涂于铜箔上,然后在真空干燥箱80℃干燥12h。之后将电极片组装成钾离子电池,采用新威电化学工作站对电池进行恒流充放电测试,测试电压为0.01V-3.0V,将所得材料装配成为纽扣电池测试其钾离子电池负极材料性能,倍率性能如图2所示。
实施例2:
1)将2g硫酸镍、3g尿素研钵中充分研磨,并将研磨后产物置于石英或氧化铝坩埚,并将坩埚置于管式炉中,在氩气气氛下,以10℃/min的升温速率匀速升温至700℃,达到温度后停止加热,将产物置于温度为0-80℃的低温冷阱中0.5~2h,快速降温至冷阱温度;
2)待产物自然冷却收集得到产物1Ni/C。
3)将获得的产物在浓度为1M的硝酸中静置,腐蚀掉大多数的Ni金属单质,为产物2。
Claims (5)
1.一种管壁坍缩的碳纳米管,其特征在于:碳纳米管管壁具有坍缩结构。
2.如权利要求1所述的管壁坍缩的碳纳米管,其特征在于:碳纳米管通过过渡金属Ni原位催化生长得到,然后经酸洗掉过多的Ni金属单质形成管壁坍缩的碳纳米管。
3.如权利要求1所述的管壁坍缩的碳纳米管,其特征在于:碳纳米管管径为200nm。
4.一种管壁坍缩的碳纳米管电池正极,其特征在于,含有权利要求1至3任一项所述的管壁坍缩的碳纳米管。
5.一种电池,其特征在于,含有权利要求4所述的管壁坍缩的碳纳米管电池正极。
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