CN108172409A - 一种三维花状结构石墨烯量子点/氢氧化锰复合材料的制备方法 - Google Patents
一种三维花状结构石墨烯量子点/氢氧化锰复合材料的制备方法 Download PDFInfo
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Abstract
本发明提供了一种三维花状结构石墨烯量子点/氢氧化锰(GQDs/Mn(OH)2)复合材料的制备方法,以石墨烯材料为碳源,通过浓酸和氧化剂氧化处理得到石墨烯量子点;然后将所得的石墨烯量子点溶液还原处理,得到具有绿色荧光的石墨烯量子点;再向溶液中加入NaOH调节溶液pH值至中性,析出三维花状结构的石墨烯量子点GQDs/Mn(OH)2复合材料。扫描电镜显示,本发明制备的三维花状结构石墨烯量子点GQDs/Mn(OH)2复合材料花状形貌规整、尺寸均一、重现性好,并且具有极大的比表面积,可广泛应用于石墨烯量子点或氢氧化锰相关的复合材料研究中。
Description
技术领域
本发明涉及一种石墨烯量子点/氢氧化锰复合材料的制备方法,尤其涉及一种三维花状结构石墨烯量子点/氢氧化锰(GQDs/ Mn(OH)2)复合材料的制备方法,属于纳米材料技术领域。
背景技术
石墨烯量子点作为一种最新的碳材料,由于其良好的水溶性、生物相容性、低毒性、稳定的荧光等特点受到了研究者广泛的关注和研究,同时石墨烯量子点相关的复合材料研究中,石墨烯量子点也体现出了前所未有的优势,主要应用在能源、环境和生物医学领域。
氢氧化锰是一种重要的过渡金属氢氧化物,由于其具有与二氧化锰相同的电化学电容特性,近年来吸引了越来越多科学家眼球。有研究报道,将氢氧化锰沉积在阴极上和二氧化锰的阳极制备不对称电容器,表现出优秀的超级电容器电化学性能。氢氧化锰和石墨烯量子点结合形成的复合材料,在氢氧化锰优势的基础上表现出石墨烯量子点的优异性能,可作为一种荧光响应的超级电容器电极,极大地拓宽了氢氧化锰和石墨烯量子点的应用范围,将在超级电容器和石墨烯量子点的复合材料中具有广泛的应用价值。
发明内容
本发明的目的是提供一种三维花状结构石墨烯量子点/氢氧化锰复合材料的制备方法。
一、石墨烯量子点/氢氧化锰复合材料的制备
(1)石墨烯量子点的制备:将石墨烯材料分散于质量浓度为95~98%的浓硫酸中,在0~5℃下磁力搅拌10~15min;缓慢加入KMnO4,加热至50~55℃,恒温搅拌反应12~15h,石墨烯材料被完全切割成石墨烯量子点;再将反应液缓慢倒入快速搅拌的0~5℃冰水中,冷却至室温;然后向其中滴加H2O2,得亮黄色石墨烯量子点溶液。
所述石墨烯材料为氧化石墨,石墨烯,氧化石墨烯,石墨烯纳米颗粒,碳纳米管中的一种。
KMnO4的加入量为石墨烯材料质量的8~10%;H2O2的加入量为KMnO4质量的10~30%。
(2)三维花状结构石墨烯量子点/氢氧化锰复合材料的制备:将步骤(1)所得石墨烯量子点溶液过滤,收集滤液;在搅拌下加入NaOH溶液(浓度为2~5mol/L)调节溶液pH值至6~8,溶液中析出白色沉淀物;过滤,洗涤,在-50 ~ -60℃下真空冷冻干燥10 ~ 12h,得到三维花状结构量子点GQDs/Mn(OH)2复合材料。
二、石墨烯量子点/氢氧化锰复合材料的形貌
下面通过扫描电镜、元素分析、荧光光谱、氮气吸附脱附等温线对本发明制备三维花状结构的石墨烯量子点GQDs/Mn(OH)2复合材料构成和形貌进行分析说明。
1、扫描电镜分析
图1为不同石墨烯材料制备的三维花状结构石墨烯量子点GQDs/Mn(OH)2复合材料的扫描电镜图。图a为以网络状还原氧化石墨烯为原料制备的GQDs/Mn(OH)2复合材料。从图a可以看出,花瓣状结构明显,而且很有规律,石墨烯量子点附着在氢氧化锰特有的花状结构上。图b是图a中三维花状结构GQDs/Mn(OH)2复合材料的高倍率下的扫描电镜图,从图中可以明显看出,花状结构构成完整,且基低上无散落的氢氧化锰片层。图c为多壁碳纳米管为碳源反应制备的三维花状结构GQDs/Mn(OH)2复合材料的扫描电镜图。从图c中可以看出,复合材料的花状形貌完整,粒径约为6µm,相对于图b中的形貌,其花瓣结构显得更加丰富和无序,说明不同的石墨烯材料,对复合材料的花状形貌具有一定的影响。图d为以氧化石墨为原料三维花状结构GQDs/Mn(OH)2复合材料。而从图d中可以看出,氧化石墨制备的三维花状结构具有明显的花状结构,且与图a相比花瓣略大,但整体与图a相似,都具有完整的花状结构,但其尺寸大小相比图a不均一。可见花状结构GQDs/Mn(OH)2复合材料的大小和形态可以通过原料和反应时间进行微调。
通过上述扫描电镜分析可见,制备三维花状结构过程中的反应原料和热处理时间对产物形貌有一定的影响;反应原料越规整有序,反应时间越长,形成的三维花状结构越规整,尺寸越小,且其形貌可以通过改变实验条件而实现调控。
2、EDS分析图
图2为图1a样品对应的元素分析图。其中,a为图1a样品对应的扫描电镜图;b为a中选中的元素分布区域中Mn的分层图像;c为b中对应分布区域Mn元素的点分布图;d为b中对应分布区域C元素的点分布图。从图a可观察到图1a样品对应的三维花状形貌;从图b可得出锰元素的分层图像中锰元素均匀分布在花状结构表面;从图c可得出Mn元素的点分布图中的Mn的分布经多次扫描之后均匀分布在花状结构表面;从图d可得出C元素的点分布图中的C的分布经多次扫描之后均匀分布在花状结构表面。这种元素面分布扫描图能很好地说明氢氧化锰和石墨烯量子点的良好复合,并且由于石墨烯量子点的纳米尺度,使其能够很好的通过非共价键的作用附着在氢氧化锰的表面,说明石墨烯量子点和氢氧化锰的复合成功。
3、荧光发射谱图
图3为本发明实施例1制备的三维花状结构GQDs/Mn(OH)2复合材料的荧光光谱图。从图3可以看出,所制得的氮掺杂量子点在280nm波长激发下具有很好的荧光发射,发射峰出现在425nm处。GQDs/Mn(OH)2复合材料荧光发射峰的出现不仅说明了石墨烯量子点的荧光发射,也证明这种复合材料成功地结合了石墨烯量子点优异的发光特性。
4、氮气吸附脱附曲线
图4为三维花状结构GQDs/Mn(OH)2复合材料的氮气吸附脱附等温线,属于IUPAC分类中的V类型,H3滞后环。H3滞后回环形状与材料结构有关,归因于花状结构上的片层聚集形成的中孔,这种类型出现在具有狭长型裂口型结构的片层材料当中。滞后回环的吸附分支曲线在较高相对压力区域不表现出极限吸附量,吸附量随压力的增加单调递增。由BET计算出GQDs/Mn(OH)2复合材料的比表面积为18.04m2˙g-1。
综上所述,本发明将石墨烯材料先通过强酸和强氧化剂氧化处理获得石墨烯量子点,再在碱性沉淀作用下原位制备了三维花状结构GQDs/Mn(OH)2复合材料。该复合材料大的比表面积能够有效提高电极材料的氧化还原反应速率,从而增大比电容;石墨烯量子点不仅会进一步增大氢氧化锰的比表面积,而且使其充放电速率更快,更加可逆。石墨烯量子点作为一种优秀的发光材料,经过巧妙的设计可开发为一种荧光响应的超级电容器电极材料,在超级电容器领域有广阔的应用前景。另外,本发明通过一步法制备GQDs/Mn(OH)2复合材料,其制备工艺简单,环境友好,而且避免了传统方法制备量子点时提纯困难的问题,同时可将溶液中的锰离子作为反应物再次利用。
附图说明
图1为不同石墨烯材料制备的三维花状结构GQDs/Mn(OH)2复合材料的扫描电镜图。
图2为实施例1中制备的三维花状结构GQDs/Mn(OH)2复合材料的元素分析图。
图3为本发明制备的三维花状结构GQDs/Mn(OH)2复合材料的荧光发射光谱图。
图4为本发明制备的三维花状结构GQDs/Mn(OH)2复合材料的氮气吸附脱附等温线。
具体实施方式
实施例1
(1)石墨烯量子点的制备:称取0.1g还原氧化石墨烯分散于120 mL浓硫酸中,在5 ℃下磁力搅拌10 min;缓慢加入0.8g KMnO4,加热至50 ℃,恒温搅拌反应15 h,还原氧化石墨烯被完全切割成石墨烯量子点,随后将浓酸反应液缓慢倒入快速搅拌的5 ℃冰水中;冷却至室温,向其中滴加3mL H2O2(30%),得到亮黄色的石墨烯量子点溶液。
(2)三维花状结构GQDs/Mn(OH)2复合材料的制备:上述所得石墨烯量子点的溶液过滤,收集滤液;在搅拌下加入2mol/L NaOH溶液,调节溶液PH值至7,溶液中析出白色的沉淀物,过滤,洗涤,干燥,得到白色的三维花状结构的石墨烯量子点GQDs/Mn(OH)2复合材料,粒径约为5µm。其扫描电镜见图1a、1b。
实施例2
(1)石墨烯量子点的制备:称取0.1g多壁碳纳米管分散于125mL浓硫酸中,在5℃下磁力搅拌10min;缓慢加入0.8g KMnO4,加热至55℃,恒温搅拌反应15h,多壁碳纳米管被完全切割成石墨烯量子点,随后将浓酸反应液缓慢倒入快速搅拌的5℃冰水中;冷却至室温,向其中滴加3mL H2O2(30%),得到亮黄色的石墨烯量子点溶液。
(2)三维花状结构GQDs/Mn(OH)2复合材料的制备:同实施例1。得到白色的三维花状结构的石墨烯量子点GQDs/Mn(OH)2复合材料,粒径约为6µm。其扫描电镜见图1c。
实施例3
(1)石墨烯量子点的制备:称取0.1g氧化石墨分散于120mL浓硫酸中,在5℃下磁力搅拌15min;缓慢加入0.8g KMnO4,加热至50℃,恒温搅拌反应12h,氧化石墨被完全切割成石墨烯量子点,随后将浓酸反应液缓慢倒入快速搅拌的5℃冰水中;冷却至室温,向其中滴加3mLH2O2(30%),得到亮黄色的石墨烯量子点溶液。
(2)三维花状结构GQDs/Mn(OH)2复合材料的制备:同实施例1。得到白色的三维花状结构的石墨烯量子点GQDs/Mn(OH)2复合材料,粒径约为8µm。其扫描电镜见图1d。
Claims (7)
1.一种三维花状结构石墨烯量子点/氢氧化锰复合材料的制备方法,包括以下工艺步骤:
(1)石墨烯量子点的制备:将石墨烯材料分散于浓硫酸中,在0~5℃下磁力搅拌10~15min;缓慢加入KMnO4,加热至50~55℃,恒温搅拌反应12~15h,氧化石墨被完全切割成石墨烯量子点;随后将反应液缓慢倒入快速搅拌的0~5℃冰水中,冷却至室温,向其中滴加H2O2,得亮黄色石墨烯量子点溶液;
(2)三维花状结构复合材料的制备:将上述所得石墨烯量子点溶液过滤,收集滤液;在搅拌下加入NaOH溶液调节溶液pH值至6~8,溶液中析出白色沉淀物,过滤,洗涤,干燥,得到三维花状结构复合材料GQDs/Mn(OH)2。
2.如权利要求1所述的三维花状结构石墨烯量子点/氢氧化锰复合材料的制备方法,其特征在于:步骤(1),石墨烯材料为氧化石墨、石墨烯、氧化石墨烯、石墨烯纳米颗粒、碳纳米管中的至少一种。
3.如权利要求1所述的三维花状结构石墨烯量子点/氢氧化锰复合材料的制备方法,其特征在于:步骤(1)中,浓硫酸质量百分比浓度为95~98%。
4.如权利要求1所述的三维花状结构石墨烯量子点/氢氧化锰复合材料的制备方法,其特征在于:步骤(1)中,KMnO4加入量为碳材料质量的8~10%。
5.如权利要求1所述的三维花状结构石墨烯量子点/氢氧化锰复合材料的制备方法,其特征在于:步骤(1)中,所述的H2O2的加入量为KMnO4质量的10~30%。
6.如权利要求1所述三维花状结构石墨烯量子点/氢氧化锰复合材料的制备方法,其特征在于:步骤(2)中,所述的NaOH溶液浓度为2~5mol/L。
7.如权利要求1所述一种三维花状结构GQDs/Mn(OH)2复合材料的制备方法,其特征在于:步骤(2)中,所述的干燥是在-50~-60℃下真空冷冻干燥10~12h。
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