CN108461299A - 柔性碳泡沫@镍铝双金属层状氧化物@石墨烯复合电极材料的制备方法 - Google Patents
柔性碳泡沫@镍铝双金属层状氧化物@石墨烯复合电极材料的制备方法 Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 34
- 239000007772 electrode material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229910052759 nickel Inorganic materials 0.000 title abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000012266 salt solution Substances 0.000 claims description 5
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000006260 foam Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 6
- 239000003792 electrolyte Substances 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 2
- 229910000943 NiAl Inorganic materials 0.000 abstract 1
- 239000002131 composite material Substances 0.000 abstract 1
- 229910000000 metal hydroxide Inorganic materials 0.000 abstract 1
- 150000004692 metal hydroxides Chemical class 0.000 abstract 1
- 241000446313 Lamella Species 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 5
- 150000001336 alkenes Chemical class 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
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- 229910016978 MnOx Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
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- 238000003763 carbonization Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
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- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000013305 flexible fiber Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种柔性碳泡沫@镍铝双金属层状氧化物@石墨烯复合电极材料的制备方法,其首先制备三维碳泡沫;利用水热法在该三维碳泡沫上沉积镍铝层状金属氢氧化物得到碳泡沫@镍铝层状氢氧化物;然后在碳泡沫@镍铝层状氢氧化物表面包裹石墨烯以增加其导电性;最后将碳泡沫@镍铝层状氢氧化物@石墨烯研磨成粉末置于管式炉中,通过设定管式炉中的温度等工艺条件,制备得到柔性复合电极材料。由于具有快速的电解液离子和电子传输通道,本发明制备得到的碳泡沫@NiAl‑LDO@石墨烯复合电极材料具有高的能量密度和功率密度。
Description
技术领域
本发明涉及复合电极材料的制备技术领域,具体涉及一种柔性石墨烯复合电极材料的制备方法。
背景技术
柔性电子器件由于具有可弯折性、便携性、可折叠型及可穿戴性等优势在信息、能源、医疗、国防等领域具有广泛应用前景。目前,柔性电极材料应用于传感器、光感器、环境检测器和其他可穿戴设备等引起了科学家们广泛的研究兴趣。尤其是超级电容器由于具有快速充放电、长循环寿命及安全易组装等特性被认为极其具有应用前景。
目前常见的制备高性能柔性超级电容器电极的方法为将高活性的金属氧化物或氢氧化物与柔性的碳薄膜或碳纳米纤维进行组装。由于石墨烯、碳纳米管等具有超强机械强度和柔韧性而常被用作柔性基底。现有技术中关于柔性电极材料的研究主要有:
He等人[ACS Nano,2012,7,174-182]利用化学气相沉积法制备了柔性三维石墨烯气凝胶,然后利用电化学沉积法负载MnO2制备柔性电容器材料。所制备的电极材料比电容最高可达130F·g-1,并且在不同弯曲状态时具有几乎相同的充放电行为,说明其作为柔性电极材料具有良好的性能。Xu等人[ACS Nano,2013,7,4042-4049]也利用水热法制备了石墨烯气凝胶作为柔性电极材料,其比电容能够达到186F·g-1,并且在弯折状态时比电容性能没有受到影响。此外还可通过真空抽滤法制备柔性电极材料,Hu等人[AdvancedFunctional Materials,2015,25,7291-7299]通过真空抽滤氧化石墨烯/MnOx悬浮液,制备了MnOx/GO薄膜作为柔性电极材料,所组装的柔性电容器具有高的体积能量密度和循环稳定性。
上述现有技术在柔性电极材料的研究方面取得了一定的进步和发展,然而石墨烯、碳纳米管等柔性基底内孔道常为间隙孔,孔径大小难以控制并且相互不连通,导致电解液离子传输受阻。此外,其制备成本高,制备工艺复杂,并且制备规模小。
发明内容
本发明的目的在于提供一种柔性碳泡沫@镍铝双金属层状氧化物@石墨烯复合电极材料的制备方法,通过该制备方法可以得到具有优异电化学性能的柔性电极材料。
其技术解决方案包括:
一种柔性电极材料的制备方法,所述制备方法依次包括以下步骤:
a制备三维碳泡沫的步骤;
b利用水热法在所述三维碳泡沫上沉积镍铝层状氢氧化物,得到碳泡沫@镍铝层状氢氧化物的步骤;
c在所述碳泡沫@镍铝层状氢氧化物表面包裹石墨烯,得到碳泡沫@镍铝层状氢氧化物@石墨烯;
d将碳泡沫@镍铝层状氢氧化物@石墨烯置于管式炉中,经加热、氧化,得到碳泡沫@镍铝层状氧化物@石墨烯柔性电极材料。
作为本发明的一个优选方案,步骤a中,所述三维碳泡沫的制备方法为:将密胺海绵置于管式炉中,在氩气气氛中,以2℃/min升温速率加热至850℃,在850℃碳化3h即得三维碳泡沫。
作为本发明的另一个优选方案,步骤b的具体步骤为:将Ni(NO3)2·6H2O、Al(NO3)3·9H2O和尿素溶于去离子水中得到金属盐溶液;取一定厚度的三维碳泡沫薄片浸入到所述的金属盐溶液中,然后在反应釜中晶化、烘干,即得碳泡沫@镍铝层状氢氧化物。
进一步的,在反应釜中于115℃晶化24h。
进一步的,步骤d中,在所述管式炉中,在室温下持续通入空气10min,升温至400℃保持2h,冷却,即得碳泡沫@镍铝层状氧化物@石墨烯柔性电极材料。
进一步的,空气的通入流速为200mL/min氧气。
进一步的,管式炉的升降温速率为2℃/min。
本发明所带来的有益技术效果为:
三维碳泡沫不仅可作为骨架进行NiAl-LDH的沉积,还能够增强复合物的电导性。NiAl-LDO垂直交叉分布在碳泡沫基底上,能有效防止片层堆叠,增加表面活性位含量,提高充放电过程中氧化还原反应的效率。此外,在LDO表面包裹石墨烯进一步提高电子在材料内部的传递速率。由于具有快速的电解液离子和电子传输通道,所制备的碳泡沫@NiAl-LDO@石墨烯复合电极材料具有高的能量密度和功率密度。
附图说明
下面结合附图对本发明做进一步说明:
图1、图2为本发明实施例1NiAl-LDH的扫描电子显微镜照片(SEM);
图3、4为本发明实施例1NiAl-LDH的透射电子显微镜照片(TEM);
图5为本发明实施例1SC@NiAl-LDO@G的扫描电子显微镜照片(SEM);
图6为本发明实施例1SC@NiAl-LDO@G的透射电子显微镜照片(TEM);
图7为本发明NiAl-LDH、SC@NiAl-LDH和SC@NiAl-LDO@G的X-射线衍射谱图。
具体实施方式
本发明提出了一种柔性碳泡沫@镍铝双金属层状氧化物@石墨烯复合电极材料的制备方法,为了使本发明的优点、技术方案更加清楚、明确,下面结合具体实施例对本发明做详细说明。
本发明所需原料均可通过商业渠道购买获得。
实施例1:
第一步、三维泡沫碳的制备
将密胺海绵置于管式炉中,在氩气气氛中,以2℃/min升温速率加热至850℃,在850℃碳化3h得到三维碳泡沫(SC);
第二步、碳泡沫@镍铝双金属层状氢氧化物的制备
利用水热法在碳泡沫上沉积镍铝层状双金属氢氧化物(NiAl-LDH);将Ni(NO3)2·6H2O、Al(NO3)3·9H2O和尿素适量溶于50mL去离子水中得到金属盐溶液;取适量5mm厚的SC薄片浸入到上述盐溶液中,然后在反应釜中于115℃晶化24h。将样品洗涤烘干,产品命名为SC@NiAl-LDH;
第三步、碳泡沫@镍铝双金属层状氢氧化物@石墨烯的制备
在所得SC@NiAl-LDH表面包裹石墨烯以增加其导电性,将SC@NiAl-LDH浸入到20mL氧化石墨烯悬浮液中保持两小时,并于室温干燥12h,将所得产品命名为SC@NiAl-LDH@G;
第四步、碳泡沫@镍铝双金属层状氧化物@石墨烯的制备
取0.16g SC@NiAl-LDH@G,研磨成粉末,置于管式炉中,首先在室温下持续通入空气10min,空气通入流速为200mL/min氧气;设置管式炉升降温速率为2℃/min,升温至400℃保持2h,待样品冷却,将样品从管式炉中取出,即得到碳泡沫@镍铝双金属层状氧化物@石墨烯,即SC@NiAl-LDO@G。
对本实施例制备得到的SC@NiAl-LDO@G进行分析,如图1、图2所示,NiAl-LDH均匀地覆盖整个碳泡沫骨架表面。NiAl-LDH片层交叉、垂直分布在碳骨架表面,形成开放的多孔结构,有利于电解液离子的快速传输。与碳泡沫复合后,NiMn-LDH片层没有明显的堆叠现象,说明碳泡沫能够提高NiMn-LDH片层的分散性。
如图3、4所示,图3、图4表明SC@NiAl-LDH中LDH片层厚度为7-12nm,包含大约12层LDH。与碳泡沫复合后LDH层数明显降低,使得LDH中表面活性位点增多,有利于提高氧化还原反应效率。通过在LDH表面包裹石墨烯进一步提高电极材料的电导性。如图5所示,经过石墨烯包裹并氧化后,电极材料的形貌没有受到明显的影响,碳泡沫表面LDO片层仍然呈花瓣状垂直分布。石墨烯不仅能够增加材料的电导性,使电子沿着LDO片层传输,还能够连接相邻的LDO片层,增强材料的机械稳定性。图6为SC@NiAl-LDO@G的透射电镜照片,从图中能清晰地观察到石墨烯的褶皱,并且石墨烯能够将相邻的LDO片层连通,增加电子的传导性及材料的机械稳定性。所制备样品的X-射线衍射谱图如图7所示,所有样品都具有典型的层状结构衍射峰。NiAl-LDH、SC@NiAl-LDH和SC@NiAl-LDO@G分别在11.6°、23.2°、35.1°、39.6°、46.9°、61.2°和62.4°出现明显的衍射峰,分别对应的是(003)、(006)、(012)、(015)、(018)、(011)和(113)晶面。XRD结果表明,所有样品都具有典型的层状结构,与SEM和TEM表征结果一致。在SC@NiAl-LDO@G样品中没有观察到有明显的石墨烯衍射峰出现,说明石墨烯在材料内分散均匀。
本发明中未述及的部分借鉴现有技术即可实现。
需要说明的是,在本说明书的教导下本领域技术人员所做出的任何等同方式,或明显变型方式均应在本发明的保护范围内。
Claims (7)
1.一种柔性电极材料的制备方法,其特征在于,所述制备方法依次包括以下步骤:
a制备三维碳泡沫的步骤;
b利用水热法在所述三维碳泡沫上沉积镍铝层状氢氧化物,得到碳泡沫@镍铝层状氢氧化物的步骤;
c在所述碳泡沫@镍铝层状氢氧化物表面包裹石墨烯,得到碳泡沫@镍铝层状氢氧化物@石墨烯的步骤;
d将碳泡沫@镍铝层状氢氧化物@石墨烯置于管式炉中,经加热、氧化,得到碳泡沫@镍铝层状氧化物@石墨烯柔性电极材料。
2.根据权利要求1所述的一种柔性电极材料的制备方法,其特征在于,步骤a中,所述三维碳泡沫的制备方法为:将密胺海绵置于管式炉中,在氩气气氛中,以2℃/min升温速率加热至850℃,在850℃碳化3h即得三维碳泡沫。
3.根据权利要求1所述的一种柔性电极材料的制备方法,其特征在于,步骤b的具体步骤为:将Ni(NO3)2·6H2O、Al(NO3)3·9H2O和尿素溶于去离子水中得到金属盐溶液;取一定厚度的三维碳泡沫薄片浸入到所述的金属盐溶液中,然后在反应釜中晶化、烘干,即得碳泡沫@镍铝层状氢氧化物。
4.根据权利要求3所述的一种柔性电极材料的制备方法,其特征在于:在反应釜中于115℃晶化24h。
5.根据权利要求1所述的一种柔性电极材料的制备方法,其特征在于,步骤d中,在所述管式炉中,在室温下持续通入空气10min,升温至400℃保持2h,冷却,即得碳泡沫@镍铝层状氧化物@石墨烯柔性电极材料。
6.根据权利要求5所述的一种柔性电极材料的制备方法,其特征在于:空气的通入流速为200mL/min氧气。
7.根据权利要求5所述的一种柔性电极材料的制备方法,其特征在于:管式炉的升降温速率为2℃/min。
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