CN108620111A - 一种纳米氮化钛基复合材料及其制备方法和应用 - Google Patents
一种纳米氮化钛基复合材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种纳米氮化钛基复合材料及其制备方法和应用，属于无机非金属纳米材料制备与太阳能利用技术领域。具体为通过对纳米氮化钛材料的包裹，改变纳米氮化钛周围的介质环境以及对太阳光的响应特性，增强对太阳能的吸收以及能量的局域，以用于有机物的热分解以及光能的有效利用，可以直接用于可见光下有机物的分解和海水(高盐水)淡化技术。
Description
技术领域
本发明涉及无机非金属纳米材料制备与太阳能利用技术领域，具体为一种纳米氮化钛基复合材料及其制备方法和应用。
背景技术
近年来随着经济的发展，淡水使用量急剧增加，对淡水资源的开发势在必行，其中在缺水的沿海地区，海水淡化是一种解决淡水缺乏的有效途径。闪蒸海水淡化是将经过加热的海水，依次在多个压力逐渐降低的闪蒸室中进行蒸发，将蒸汽冷凝而得到淡水的过程。加热海水产生水蒸气，冷却凝结就可得到纯水，这是海水淡化技术的开始。因此，寻找可利用太阳能产生光热效应从而加热海水的新型材料成为热点。
Au、Ag等贵金属材料在太阳光照射下会产生表面等离子体共振效应，进而产生光热效应，因而可应用于海水的加热过程，但这些材料价格都较为昂贵并且在空气中会被缓慢氧化，因此寻找新的具有表面等离子体效应的非贵金属高效光催化材料是纳米技术领域、环境保护领域以及太阳能利用领域一个十分重要的研究方向。
氮化钛是一种熔点高、硬度大、具有优良的化学稳定性以及耐腐蚀性的材料，同时其具有优良的导电性，在涂层、光电材料以及超导材料等领域有着众多的研究。氮化钛、特别是纳米氮化钛材料具有与Au相类似的光电特性，因而利用氮化钛取代贵金属应用于太阳能闪蒸海水淡化技术是一个非常值得研究的方向。
发明内容
本发明的目的在于提供一种纳米氮化钛基复合材料及其制备方法和应用，利用水热法高温高压的反应特点，通过控制制备工艺，通过对纳米氮化钛材料的包裹，改变纳米氮化钛周围的介质环境以及对太阳光的响应特性，增强对太阳能的吸收以及能量的局域，以用于有机物的热分解以及光能的有效利用，可以直接用于可见光下有机物的分解和海水(高盐水)淡化技术。
本发明的技术方案是：
一种纳米氮化钛基复合材料，该复合材料是由纳米氮化钛和无定形碳构成的壳核结构，无定形碳包覆于纳米氮化钛表面。
所述纳米氮化钛是指尺寸在纳米级别的氮化钛材料，其为球状、多面体状、片状或线状形貌的低维纳米结构。
所述无定形碳的厚度为2-10nm。
该复合材料的制备方法，是采用水热法对纳米氮化钛基体进行表面修饰，在其表面包覆一层无定形碳，从而获得纳米氮化钛基复合材料。该方法包括如下步骤：
(1)葡萄糖溶液的制备：将葡萄糖溶于100mL溶剂中，搅拌使其溶解，获得浓度为0.1-0.5mol/L的葡萄糖溶液；
(2)将纳米氮化钛在超声条件下分散到步骤(1)所得葡萄糖溶液中，得到混合物料；其中：纳米氮化钛在葡萄糖溶液中的加入量为100-500mg/100mL；
(3)将步骤(2)所得混合物料在150-180℃条件下保温1-12h；
(4)将步骤(3)经保温处理后所得沉淀经离心和去离子水冲洗后，在50-100℃条件下干燥10-24h，即获得所述纳米氮化钛基复合材料。
上述步骤(1)中，所述溶剂为去离子水、无水乙醇或乙二醇。
制备氮化钛基复合材料过程中，通过控制步骤(1)制备的葡萄糖溶液的浓度和/或步骤(3)中的反应时间(保温时间)来调控所得氮化钛基复合材料中无定形碳的厚度。
制备氮化钛基复合材料过程中，所述葡萄糖溶液的浓度越高，所得复合材料中无定形碳厚度越大；步骤(3)中的反应时间(保温时间)越长，所得复合材料中无定形碳厚度越大。
该复合材料直接应用于可见光下有机物的降解以及海水(高盐水)淡化技术。
本发明的设计原理如下：
本发明利用水热法通过对纳米氮化钛材料的包裹，改变纳米氮化钛周围的介质环境以及对太阳光的响应特性，增强对太阳能的吸收以及能量的局域，以用于有机物的热分解以及光能的有效利用，可以直接用于可见光下有机物的分解和海水(高盐水)淡化技术。。
本发明的优点在于：
1.本发明通过简单的水热法制备纳米氮化钛基复合材料，该复合过程操作简单，易于控制，易于工业化生产。
2.本发明的复合方法能可控的修饰纳米氮化钛，从而调节复合材料中无定形碳的厚度
3.本发明的方法相比传统的复合方法，具有能耗低的优点。
附图说明：
图1为本发明实施例1中样品的XRD图。
图2为本发明实施例1中样品的TEM图片。
图3为本发明实施例4中对有机污染物罗丹明B降解效果图。
图4为本发明实施例5中蒸发海水的质量变化图。
图5为本发明实施例5中蒸发海水过程温度变化图。
具体实施方式：
以下结合附图及实施例详述本发明。
本发明制备纳米氮化钛基复合材料的方法，采用水热方法通过对纳米氮化钛材料的包裹，改变纳米氮化钛周围的介质环境以及对太阳光的响应特性，增强对太阳能的吸收以及能量的局域，以用于有机物的热分解以及光能的有效利用，可以直接用于可见光下有机物的分解和海水(高盐水)淡化技术。
实施例1
本实施例制备纳米氮化钛基复合材料的过程如下：
1)称量2.7024g的葡萄糖溶于100mL去离子水中，搅拌使其溶解；
2)称量120mg的纳米氮化钛粉体超声分散到步骤(1)所得葡萄糖溶液中；
3)在180℃条件下保温3h；
4)将所得沉淀经离心和去离子水冲洗后，在60℃条件下干燥12h，即获得所述纳米氮化钛基复合材料(样品1)。
图1所示为本实施例所得纳米氮化钛基复合材料样品的XRD结构表征图，由图1可以看出，所述纳米氮化钛基复合材料水热前后(PDF卡片号38-1420)均由氮化钛纯相组成，葡萄糖水热产物为无定形碳。
图2所示为本实施例所得氮化钛基复合材料的TEM图，由图2可以看出，氮化钛基复合材料为在氮化钛表面修饰了一层无定形碳，进而获得以纳米氮化钛为基的复合材料。
本实施例制备的纳米氮化钛基复合材料中无定形碳的厚度为2nm。
实施例2
本实施例制备纳米氮化钛基复合材料的过程如下：
1)称量5.4048g的葡萄糖溶于100mL乙醇中，搅拌使其溶解；
2)称量200mg纳米氮化钛粉体超声分散到步骤(1)所得葡萄糖溶液中；
3)在180℃条件下保温3h；
4)将所得沉淀经离心和去离子水冲洗后，在60℃条件下干燥12h，即获得所述纳米氮化钛基复合材料(样品2)。
本实施例制备的纳米氮化钛基复合材料中无定形碳的厚度为4nm。
实施例3
与实施例1不同之处在于，步骤3)中的保温时间为5h；最终制得的纳米氮化钛基复合材料中无定形碳的厚度为5nm。
实施例4
选择样品1进行有机染料罗丹明B的降解实验：
1)称取所得纳米氮化钛基复合材料样品0.01g，加入到50mL浓度为5mg/L的罗丹明B溶液中，超声分散10min，然后在黑暗条件搅拌，间隔不同时间取样5mL，在高速离心机上以12000r/min的转速离心处理，取上清液；
2)称取所得纳米氮化钛基复合光催化材料样品0.01g，加入到50mL浓度为5mg/L的罗丹明B溶液中，超声分散10min；打开加了滤光片(λ>400nm)的光源照射，间隔不同时间取样5mL，在高速离心机上以12000r/min的转速离心处理，取上清液；
3)利用紫外分光光度计测量其光吸收变化，其中1)为吸附所导致的光吸收降低，2)为吸附与光照共同作用所产生的光吸收降低，通过对比以此表征材料的可见光催化降解性能。图3所示为实施例1所得纳米氮化钛基复合材料在黑暗条件下吸附及与光照条件下降解罗丹明B效果对比图。
实施例5
选择样品1进行海水蒸发和加热的实验：
1)称取所得纳米氮化钛基复合材料样品0.01g，加入到50mL海水溶液的烧杯中，超声分散1min。
2)将烧杯放到电子天平上并放置于光源下，间隔5min原位记录溶液的质量变化。
3)利用热电偶原位记录溶液的温度变化。
图4为实施例1所得纳米氮化钛基复合材料在光照下海水质量变化图，以及与加入纳米氮化钛和未加材料纯海水光照的质量变化对比图。
图5为实施例1所得纳米氮化钛基复合材料在光照下海水温度变化图，以及与加入纳米氮化钛和未加材料纯海水光照的温度变化对比图。
实施例结果表明，本发明采用水热的手段通过对纳米氮化钛材料的包裹，改变纳米氮化钛周围的介质环境以及对太阳光的响应特性，增强对太阳能的吸收以及能量的局域，以用于有机物的热分解以及光能的有效利用，可以直接用于可见光下有机物的分解和海水(高盐水)淡化技术。
上述实例仅作参考，具有和本专利相似或者从本专利思路出发而延伸的纳米氮化钛材料及其制备方法和应用，均在本专利的保护范围。
Claims (9)
1.一种纳米氮化钛基复合材料，其特征在于：该复合材料是由纳米氮化钛和无定形碳构成的壳核结构，无定形碳包覆于纳米氮化钛表面。
2.根据权利要求1所述的纳米氮化钛基复合材料，其特征在于：所述纳米氮化钛是指尺寸在纳米级别的氮化钛材料，其为球状、多面体状、片状或线状形貌的低维纳米结构。
3.根据权利要求1所述的纳米氮化钛基复合材料，其特征在于：所述无定形碳的厚度为1-10nm。
4.根据权利要求1所述的纳米氮化钛基复合材料的制备方法，其特征在于：该方法是采用水热法对纳米氮化钛基体进行表面修饰，在其表面包覆一层无定形碳，从而获得纳米氮化钛基复合材料。
5.根据权利要求4所述的纳米氮化钛基复合材料的制备方法，其特征在于：该方法包括如下步骤：
(1)葡萄糖溶液的制备：将葡萄糖溶于100mL溶剂中，搅拌使其溶解，获得浓度为0.1-0.5mol/L的葡萄糖溶液；
(2)将纳米氮化钛在超声条件下分散到步骤(1)所得葡萄糖溶液中，得到混合物料；其中：纳米氮化钛在葡萄糖溶液中的加入量为100-500mg/100mL；
(3)将步骤(2)所得混合物料在150-180℃条件下保温1-12h；
(4)将步骤(3)经保温处理后所得沉淀经离心和去离子水冲洗后，在50-100℃条件下干燥10-24h，即获得所述纳米氮化钛基复合材料。
6.根据权利要求5所述的纳米氮化钛基复合材料的制备方法，其特征在于：步骤(1)中，所述溶剂为去离子水、无水乙醇或乙二醇。
7.根据权利要求5所述的纳米氮化钛基复合材料的制备方法，其特征在于：制备氮化钛基复合材料过程中，通过控制步骤(1)制备的葡萄糖溶液的浓度和/或步骤(3)中的反应时间来调控所得氮化钛基复合材料中无定形碳的厚度。
8.根据权利要求6所述的纳米氮化钛基复合材料的制备方法，其特征在于：制备氮化钛基复合材料过程中，所述葡萄糖溶液的浓度越高，所得复合材料中无定形碳厚度越大；步骤(3)中的反应时间越长，所得复合材料中无定形碳厚度越大。
9.根据权利要求1所述的纳米氮化钛基复合材料的应用，其特征在于：该复合材料直接应用于可见光下有机物的降解以及海水淡化技术。
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