CN105921112A - 一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法 - Google Patents
一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法,包括如下步骤:1)取氧化石墨烯于反应釜中,设压力为5×10‑4‑10‑3Pa,温度为200‑700℃,等离子体产生的微波功率为300‑500W,预先通入一段时间的O2,在氧化石墨烯微粒表面形成均匀密集的成核点;2)在惰性气氛中利用激光光源脉冲冲击金属靶材,金属靶材气化形成金属脉冲气源通入至反应釜中,在等离子体作用下,金属脉冲气源与氧化石墨烯微粒表面的O2发生化学反应,形成纳米金属氧化物因子均匀充分的负载在氧化石墨烯微粒表面,得到石墨烯基纳米金属氧化物光催化吸附材料;其中,所述纳米金属氧化物为半导体纳米金属氧化物。得到的石墨烯基纳米金属氧化物光催化吸附材料具有高活性和高吸附性。
Description
技术领域
本发明涉及到净化吸附材料制备的技术领域,特别涉及到一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法。
背景技术
随着城市化和工业化的进程越来越快,特别是改革开放以来,城市化和工业化都进入了一个高潮,而随之而来的是一系列导致城市不可持续发展的环境污染问题,特别是空气污染和水污染已经成为人类生存的重大威胁,成为人类健康、经济和社会可持续发展的重大障碍。特别是近些年来,人们对家居环境的追求,对室内装潢的要求越来越高,但是装修材料中的甲苯甲醛及其他挥发性有机物质,使室内空气污染严重,引发呼吸道疾病与生理机能障碍,以及眼鼻等粘膜组织受到刺激而患病等危害。
现有技术中因为活性炭呈毛细结构,具有很强的吸附能力,所以多采用竹炭等活性炭包吸附污染气体,净化空气,保持空气清新。但由于活性炭在使用过程中,常会过量的吸附污染气体,转换成吸附物质,覆在活性炭表面,使活性炭失活。
石墨烯是单原子厚度的二维碳原子晶体具有独特的电子,物理和化学性质。其独特的二维结构,使得石墨烯成为一个非常理想的纳米粒子的载体来制备石墨烯基的复合材料,现有技术中,制备石墨烯基的纳米复合材料多采用凝胶-溶胶法或者液相复合法,如专利201410355247.5公开了一种石墨烯/二氧化钛光催化复合材料及其制备方法,以钛源经过溶胶-凝胶法和水热处理制备得到二氧化钛纳米颗粒,再通过液相复合氧化石墨烯溶液,经过超声、干燥、加热、冷却得到石墨烯/二氧化钛光催化复合材料,该方法制备的光催化吸附剂以三维石墨烯骨架和纳米二氧化钛颗粒组成,所述石墨烯具有大孔结构,所述二氧化钛为介孔二氧化钛,大孔和介孔相互连通,所述纳米二氧化钛颗粒分散于石墨烯纳米片上,所述纳米二氧化钛颗粒填充于所述石墨烯的大孔内,方法制备的光催化剂较纯的二氧化钛,具有高活性、高吸附性。但是采用上述方法,二氧化钛纳米片很难均匀充分的分布在石墨烯片的表面,石墨烯片表面部分区域团聚有大量的纳米颗粒,部分区域又没有纳米颗粒分布,从而导致复合材料的光催化吸附活性降低。
发明内容
本发明的目的在于一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法,纳米金属氧化物因子均匀充分的负载在氧化石墨烯表面,避免了纳米金属氧化物因子在氧化石墨烯表面发生团聚的问题,使纳米金属氧化物因子与氧化石墨烯相互作用,具有高活性和高吸附性。
为此,本发明采用以上技术方案:
一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法,包括如下步骤:
1)取氧化石墨烯于反应釜中,设压力为5×10-4-10-3Pa,温度为200-700℃,等离子体产生的微波功率为300-500W,预先通入一段时间的O2,在氧化石墨烯微粒表面形成均匀密集的成核点;
2)在惰性气氛中利用激光光源脉冲冲击金属靶材,金属靶材气化形成金属脉冲气源通入至反应釜中,在等离子体作用下,金属脉冲气源与氧化石墨烯微粒表面的O2发生化学反应,形成纳米金属氧化物因子均匀充分的负载在氧化石墨烯微粒表面,得到石墨烯基纳米金属氧化物光催化吸附材料;
优选的,所述纳米金属氧化物为半导体纳米金属氧化物。
优选的,所述O2的通入时间为20min-80min。
优选的,所述惰性气氛为Ar气氛。
优选的,所述激光光源能量为50-200mJ/pulse,频率为2-10HZ,每个脉冲时间为5-20ns,间隔时间为5-20ns。
优选的,所述金属脉冲气源通入的时间为5-20min。
优选的,所述纳米金属氧化物因子的直径为5-500nm。
优选的,所述金属靶材为Ti、Zn、Fe或者W,所述半导体纳米金属氧化物为纳米TiO2、ZnO、Fe2O3或者WO3。
优选的,所述氧化石墨烯为Hummers法制备得到的。
本发明采用以上技术方案,利用激光光源脉冲冲击金属靶材,金属靶材气化形成金属脉冲气源通入至反应釜中,与氧化石墨烯微粒表面的O2发生化学反应,形成纳米金属氧化物因子均匀充分的负载在氧化石墨烯微粒表面,避免了避免了纳米金属氧化物因子在氧化石墨烯表面发生团聚的问题,利用了氧化石墨烯比表面积大的特点,最大量的负载纳米金属氧化物因子,使纳米金属氧化物因子与氧化石墨烯相互作用,具有高活性和高吸附性,以及吸附稳定性和长久性。
附图说明
图1为本发明得到石墨烯基纳米金属氧化物光催化吸附材料颗粒的结构示意图。
图2为本发明激光光源脉冲冲击方式示意图。
具体实施方式
为了使本发明的目的、特征和优点更加的清晰,以下结合附图及实施例,对本发明的具体实施方式做出更为详细的说明,在下面的描述中,阐述了很多具体的细节以便于充分的理解本发明,但是本发明能够以很多不同于描述的其他方式来实施。因此,本发明不受以下公开的具体实施的限制。
一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法,包括如下步骤:
1)取氧化石墨烯于反应釜中,设压力为5×10-4-10-3Pa,温度为200-700℃,等离子体产生的微波功率为300-500W,预先通入一段时间的O2,在氧化石墨烯微粒表面形成均匀密集的成核点;
2)在惰性气氛中利用激光光源脉冲冲击金属靶材,金属靶材气化形成金属脉冲气源通入至反应釜中,在等离子体作用下,金属脉冲气源与氧化石墨烯微粒表面的O2发生化学反应,形成纳米金属氧化物因子1均匀充分的负载在氧化石墨烯微粒0表面,如图1所示,得到石墨烯基纳米金属氧化物光催化吸附材料;
其中,所述纳米金属氧化物为半导体纳米金属氧化物。
其中,所述O2的通入时间为20min-80min。
其中,所述惰性气氛为Ar气氛。
其中,所述激光光源能量为50-200mJ/pulse,频率为2-10HZ,每个脉冲时间为5-20ns,间隔时间为5-20ns,其方式如图2所示。
其中,所述金属脉冲气源通入的时间为5-20min。
其中,所述纳米金属氧化物因子的直径为5-500nm。
其中,所述金属靶材为Ti、Zn、Fe或者W,所述半导体纳米金属氧化物为纳米TiO2、ZnO、Fe2O3或者WO3。
其中,所述氧化石墨烯为Hummers法制备得到的。
实施例一
一种石墨烯基纳米TiO2光催化吸附材料的制备方法,包括如下步骤:
1)取氧化石墨烯于反应釜中,设压力为5×10-4-10-3Pa,温度为200-700℃,等离子体产生的微波功率为300-500W,预先通入一段时间的O2,在氧化石墨烯微粒表面形成均匀密集的成核点;
2)在惰性气氛中利用激光光源脉冲冲击Ti靶材,Ti靶材气化形成Ti脉冲气源通入至反应釜中,在等离子体作用下,Ti脉冲气源与氧化石墨烯微粒表面的O2发生化学反应,形成纳米TiO2因子均匀充分的负载在氧化石墨烯微粒表面,得到墨烯基纳米TiO2光催化吸附材料。
其中,所述O2的通入时间为20min-80min。
其中,所述惰性气氛为Ar气氛。
其中,所述激光光源能量为50-200mJ/pulse,频率为2-10HZ,每个脉冲时间为5-20ns,间隔时间为5-20ns。
其中,所述Ti脉冲气源通入的时间为5-20min。
其中,所述纳米TiO2因子的直径为5-500nm。
其中,所述氧化石墨烯为Hummers法制备得到的。
采用上述方法得到的石墨烯基纳米TiO2光催化吸附材料,以去除甲醛气体为例,其吸附平均率可达到99.2%。
实施例二
一种石墨烯基纳米ZnO光催化吸附材料的制备方法,包括如下步骤:
1)取氧化石墨烯于反应釜中,设压力为5×10-4-10-3Pa,温度为200-700℃,等离子体产生的微波功率为300-500W,预先通入一段时间的O2,在氧化石墨烯微粒表面形成均匀密集的成核点;
2)在惰性气氛中利用激光光源脉冲冲击Zn靶材,Zn靶材气化形成Zn脉冲气源通入至反应釜中,在等离子体作用下,Zn脉冲气源与氧化石墨烯微粒表面的O2发生化学反应,形成纳米ZnO因子均匀充分的负载在氧化石墨烯微粒表面,得到墨烯基纳米ZnO光催化吸附材料。
其中,所述O2的通入时间为20min-80min。
其中,所述惰性气氛为Ar气氛。
其中,所述激光光源能量为50-200mJ/pulse,频率为2-10HZ,每个脉冲时间为5-20ns,间隔时间为5-20ns。
其中,所述Zn脉冲气源通入的时间为5-20min。
其中,所述纳米ZnO因子的直径为5-500nm。
其中,所述氧化石墨烯为Hummers法制备得到的。
采用上述方法得到的石墨烯基纳米ZnO光催化吸附材料以去除甲醛气体为例,其吸附平均率可达到98.7%。
实施例三
一种石墨烯基纳米Fe2O3光催化吸附材料的制备方法,包括如下步骤:
1)取氧化石墨烯于反应釜中,设压力为5×10-4-10-3Pa,温度为200-700℃,等离子体产生的微波功率为300-500W,预先通入一段时间的O2,在氧化石墨烯微粒表面形成均匀密集的成核点;
2)在惰性气氛中利用激光光源脉冲冲击Fe靶材,Fe靶材气化形成Zn脉冲气源通入至反应釜中,在等离子体作用下,Fe脉冲气源与氧化石墨烯微粒表面的O2发生化学反应,形成纳米Fe2O3因子均匀充分的负载在氧化石墨烯微粒表面,得到墨烯基纳米Fe2O3光催化吸附材料。
其中,所述O2的通入时间为20min-80min。
其中,所述惰性气氛为Ar气氛。
其中,所述激光光源能量为50-200mJ/pulse,频率为2-10HZ,每个脉冲时间为5-20ns,间隔时间为5-20ns。
其中,所述Fe脉冲气源通入的时间为5-20min。
其中,所述纳米Fe2O3因子的直径为5-500nm。
其中,所述氧化石墨烯为Hummers法制备得到的。
采用上述方法得到的石墨烯基纳米Fe2O3光催化吸附材料以去除环境污水中Cr为例,其吸附平均率可达到98.3%。
实施例四
一种石墨烯基纳米WO3光催化吸附材料的制备方法,包括如下步骤:
1)取氧化石墨烯于反应釜中,设压力为5×10-4-10-3Pa,温度为200-700℃,等离子体产生的微波功率为300-500W,预先通入一段时间的O2,在氧化石墨烯微粒表面形成均匀密集的成核点;
2)在惰性气氛中利用激光光源脉冲冲击W靶材,W靶材气化形成Zn脉冲气源通入至反应釜中,在等离子体作用下,W脉冲气源与氧化石墨烯微粒表面的O2发生化学反应,形成纳米WO3因子均匀充分的负载在氧化石墨烯微粒表面,得到墨烯基纳米WO3光催化吸附材料。
其中,所述O2的通入时间为20min-80min。
其中,所述惰性气氛为Ar气氛。
其中,所述激光光源能量为50-200mJ/pulse,频率为2-10HZ,每个脉冲时间为5-20ns,间隔时间为5-20ns。
其中,所述W脉冲气源通入的时间为5-20min。
其中,所述纳米WO3因子的直径为5-500nm。
其中,所述氧化石墨烯为Hummers法制备得到的。
采用上述方法得到的石墨烯基纳米WO3光催化吸附材料以去除环境污水中亚甲基蓝为例,其吸附平均率可达到97.8%。
综上,本发明利用激光光源脉冲冲击金属靶材,金属靶材气化形成金属脉冲气源通入至反应釜中,与氧化石墨烯微粒表面的O2发生化学反应,形成纳米金属氧化物因子均匀充分的负载在氧化石墨烯微粒表面,避免了避免了纳米金属氧化物因子在氧化石墨烯表面发生团聚的问题,利用了氧化石墨烯比表面积大的特点,尽可能负载纳米金属氧化物因子,使纳米金属氧化物因子与氧化石墨烯相互作用,具有高活性和高吸附性,以及吸附稳定性和长久性。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (8)
1.一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法,其特征在于:包括如下步骤:
1)取氧化石墨烯于反应釜中,设压力为5×10-4-10-3Pa,温度为200-700℃,等离子体产生的微波功率为300-500W,预先通入一段时间的O2,在氧化石墨烯微粒表面形成均匀密集的成核点;
2)在惰性气氛中利用激光光源脉冲冲击金属靶材,金属靶材气化形成金属脉冲气源通入至反应釜中,在等离子体作用下,金属脉冲气源与氧化石墨烯微粒表面的O2发生化学反应,形成纳米金属氧化物因子均匀充分的负载在氧化石墨烯微粒表面,得到石墨烯基纳米金属氧化物光催化吸附材料;
其中,所述纳米金属氧化物为半导体纳米金属氧化物。
2.根据权利要求1所述的一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法,其特征在于:所述O2的通入时间为20min-80min。
3.根据权利要求1所述的一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法,其特征在于:所述惰性气氛为Ar气氛。
4.根据权利要求1所述的一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法,其特征在于:所述激光光源能量为50-200mJ/pulse,频率为2-10HZ,每个脉冲时间为5-20ns,间隔时间为5-20ns。
5.根据权利要求1所述的一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法,其特征在于:所述金属脉冲气源通入的时间为5-20min。
6.根据权利要求1所述的一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法,其特征在于:所述纳米金属氧化物因子的直径为5-500nm。
7.根据权利要求1所述的一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法,其特征在于:所述金属靶材为Ti、Zn、Fe或者W,所述半导体纳米金属氧化物为纳米TiO2、ZnO、Fe2O3或WO3。
8.根据权利要求1所述的一种石墨烯基纳米金属氧化物光催化吸附材料的制备方法,其特征在于:所述氧化石墨烯为Hummers法制备得到的。
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