CN105803399B - 一种Ti@C@g-C3N4纳米复合物及其制备方法 - Google Patents
一种Ti@C@g-C3N4纳米复合物及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种Ti@C@g‑C3N4纳米复合物及其制备方法，属于纳米材料制备技术领域。该纳米复合物材料微观结构为Ti@C核壳结构纳米胶囊嵌入g‑C3N4纳米片中，纳米胶囊的粒径为5～100nm。本发明采用等离子电弧放电法，将钛粉和三聚氰胺粉按一定原子百分比压制成块体作为阳极靶材材料，采用石墨作为阴极材料，引用氩气和甲烷作为工作气体，阴极石墨电极与阳极靶材钛‑三聚氰胺粉末块体之间保持一定距离，阳极与阴极之间起电弧放电，即得Ti@C@g‑C3N4纳米复合物。该纳米复合物可见光催化活性高且制备过程简单、无后处理工序、成本低、易于实现工业化生产。
Description
技术领域
本发明属于材料制备技术领域，具体涉及一种Ti@C@g-C3N4纳米复合物及其制备方法。
背景技术
当前经济社会快速发展，环境污染问题严重影响人类的生存和发展。光催化技术能吸收太阳能降解和矿化环境中的污染物，将太阳能转化为可储存的氢能，因此在解决能源和环境问题方面有着重要的应用前景。光催化技术的核心是高效光催化材料的设计与合成。g-C3N4是一类似石墨结构的新型半导体，具有合适的半导体宽度(约2.7eV)、结构稳定、耐酸碱、无毒且生物兼容性好、成本低及易于化学改性等优点，已经被用于光催化合成反应、光催化降价污染物、光解水产氢和产氧以及氧化还原反应中。g-C3N4光生电子-空穴对分离效率低，从而导致光催化性能较低。异质结构有利于电子和空穴对的分离，从而提高量子效率。纳米金属粒子稳定性差、易团聚等缺陷限制其广泛应用，然而与g-C3N4复合后，其较好的导电性能促进了电子转移，增强了g-C3N4光催化活性。如：专利20120387276.0公开了一种Au/g-C3N4复合型微纳米材料的制备方法。其采用的是将g-C3N4粉末加入氯金酸溶液中制成悬浊液，然后加热，添加柠檬酸钠，搅拌干燥，即得到Au/g-C3N4复合型微纳米材料。专利201310606627.7公开了金属/类石墨氮化碳复合物催化剂及其制备方法。其方法是将类石墨氮化碳制成溶液，在搅拌条件下加入硝酸银，开启光源，进行光还原，得到最终产物。专利201310220362.7公开了载Co介孔石墨相氮化碳可见光催化剂的制备方法和应用。该材料是先将单氰胺通过高温焙烧，得到介孔石墨相氮化碳，然后将钴的前驱体溶液浸入，并于马弗炉内进行二次高温焙烧，制得负载型催化剂 Co/g-C3N4。经检索，Ti@C@g-C3N4纳米复合物未见报导。
发明内容
为克服现有技术的不足，本发明的目的是提供一种Ti@C@g-C3N4纳米复合物及其制备方法。
本发明提供了一种Ti@C@g-C3N4纳米复合物，该纳米复合物微观结构为 Ti@C核壳结构纳米胶囊嵌入g-C3N4纳米片中；该纳米胶囊的粒径为5～100nm。
本发明还提供了上述Ti@C@g-C3N4纳米复合物的制备方法，该材料是利用等离子体电弧放电技术，在工作气体下原位制备得到；其中：
采用石墨电极为阴极，钛-三聚氰胺粉末块体为阳极靶材，阴极与阳极靶材之间保持2～30mm的距离；电弧放电的电压为10～40V；工作气体为氩气和甲烷气体。
所述阳极靶材为钛-三聚氰胺粉末块体，将钛粉和三聚氰胺粉在压强1MPa～ 1Gpa下压制成块体作为等离子电弧炉的阳极靶材材料，所述阳极靶材材料中钛所占的质量百分比为70～90％。
所述工作气体氩气的分压为0.01～0.5MPa,甲烷气体的分压为0.01～0.3 MPa。
相对现有技术，本发明的突出优点在于
1)本发明首次制备出了Ti@C@g-C3N4纳米复合物；
2)本发明制备过程条件简单，易于控制，一次性生成产物，为 Ti@C@g-C3N4纳米复合物的实际应用提供了条件；
3)本发明所制备的Ti@C@g-C3N4纳米复合物，由于Ti@C的存在能较好地增加导电性能，促进了电子转移，使Ti@C@g-C3N4纳米复合物具有良好的光催化活性，对于有机污染物降解提供了有效的解决方法。
附图说明
图1为本发明制备的Ti@C@g-C3N4纳米复合物的装置示意图；
图中标号：1、上盖；2、阴极；3、阀；4、阳极靶材；5、观察窗；6、挡板；7、铜阳极；8、夹头；9、石墨坩埚；10、直流脉动电源；a、冷却水；b、氩气；c、甲烷气。
图2为本发明实施例1所制备的Ti@C@g-C3N4纳米复合物的X-射线衍射 (XRD)图谱；
根据JCPDS PDF卡片,可以检索出纳米复合物主相为Ti晶相构成；2θ＝27.5o和13o处的两个峰为g-C3N4(JCPDS卡，No.87-1562)的特征峰,由于C处于外壳，所以XRD无法检测出C相。
图3为本发明实施例1所制备的Ti@C@g-C3N4纳米复合物的透射电子显微镜(TEM)图像；
从图中可以看出Ti@C纳米胶囊分布在g-C3N4纳米片中，其纳米胶囊的粒径为5～100nm。
图4为本发明实施例1所制备的Ti@C@g-C3N4纳米复合物的高分辨透射电子显微镜图像；
从图中可以看出所得Ti@C@g-C3N4纳米复合物为Ti@C核壳结构纳米胶囊嵌入g-C3N4纳米片中。
图5为本发明实施例1所制备的Ti@C@g-C3N4纳米复合物和g-C3N4对甲基橙的降解性能比较图(用量0.03g/25ml甲基橙溶液)；
从图中可以看到所得Ti@C@g-C3N4纳米复合物的光催化性能相对g-C3N4有明显的提高。
具体实施方式
下面结合实施例对本发明作进一步的描述，但本发明不局限于下述实施例。
实施例1
将图1所示的装置上盖1打开，用石墨作阴极2固定在夹头8上，所消耗阳极靶材4的成分为纯钛粉与三聚氰胺粉(质量比90:10)压成的块体，放在通冷却水的铜阳极7上，在铜阳极7和阳极靶材4之间是石墨坩埚9。阴极2与阳极靶材4之间保持30mm的距离。盖上装置上盖1，通冷却水a，通过阀3把整个工作室抽真空后，通入氩气b和甲烷气c，氩气的分压为0.5MPa，甲烷气的分压为0.3MPa,接通直流脉动电源10，电压为40V，弧光放电过程中调节工作电流与电压保持相对稳定，制得Ti@C@g-C3N4纳米复合物。该纳米复合物微观结构为Ti@C核壳结构纳米胶囊嵌入g-C3N4纳米片，其中：Ti@C纳米胶囊的粒径为5～100nm，如图3、图4所示。测试该纳米复合物对甲基橙的光催化性能，如图5所示，发现其光催化性能相对g-C3N4有明显的提高。
实施例2
将图1所示的装置上盖1打开，用石墨作阴极2固定在夹头8上，所消耗阳极靶材4的成分为纯钛粉与三聚氰胺粉(质量比70:30)压成的块体，放在通冷却水的铜阳极7上，在铜阳极7和阳极靶材4之间是石墨坩埚9。阴极2与阳极靶材4之间保持30mm的距离。盖上装置上盖1，通冷却水a，通过阀3把整个工作室抽真空后，通入氩气b和甲烷气c，氩气的分压为0.5MPa，甲烷气的分压为0.3MPa,接通直流脉动电源10，电压为10V，弧光放电过程中调节工作电流与电压保持相对稳定，制得Ti@C@g-C3N4纳米复合物。该纳米复合物微观结构为Ti@C核壳结构纳米胶囊嵌入g-C3N4纳米片，其中：Ti@C纳米胶囊的粒径为5～100nm。
实施例3
将图1所示的装置上盖1打开，用石墨作阴极2固定在夹头8上，所消耗阳极靶材4的成分为纯钛粉与三聚氰胺粉(质量比90:10)压成的块体，放在通冷却水的铜阳极7上，在铜阳极7和阳极靶材4之间是石墨坩埚9。阴极2与阳极靶材4之间保持30mm的距离。盖上装置上盖1，通冷却水a，通过阀3把整个工作室抽真空后，通入氩气b和甲烷气c，氩气的分压为0.5MPa，甲烷气的分压为0.3MPa,接通直流脉动电源10，电压为20V，弧光放电过程中调节工作电流与电压保持相对稳定，制得Ti@C@g-C3N4纳米复合物。该纳米复合物微观结构为Ti@C核壳结构纳米胶囊嵌入g-C3N4纳米片，其中：Ti@C纳米胶囊的粒径为5～100nm。
实施例4
将图1所示的装置上盖1打开，用石墨作阴极2固定在夹头8上，所消耗阳极靶材4的成分为纯钛粉与三聚氰胺粉(质量比80:20)压成的块体，放在通冷却水的铜阳极7上，在铜阳极7和阳极靶材4之间是石墨坩埚9。阴极2与阳极靶材4之间保持30mm的距离。盖上装置上盖1，通冷却水a，通过阀3把整个工作室抽真空后，通入氩气b和甲烷气c，氩气的分压为0.2MPa，甲烷气的分压为0.2MPa,接通直流脉动电源10，电压为30V，弧光放电过程中调节工作电流与电压保持相对稳定，制得Ti@C@g-C3N4纳米复合物。该纳米复合物微观结构为Ti@C核壳结构纳米胶囊嵌入g-C3N4纳米片，其中：Ti@C纳米胶囊的粒径为5～100nm。
实施例5
将图1所示的装置上盖1打开，用石墨作阴极2固定在夹头8上，所消耗阳极靶材4的成分为纯钛粉与三聚氰胺粉(质量比80:20)压成的块体，放在通冷却水的铜阳极7上，在铜阳极7和阳极靶材4之间是石墨坩埚9。阴极2与阳极靶材4之间保持30mm的距离。盖上装置上盖1，通冷却水a，通过阀3把整个工作室抽真空后，通入氩气b和甲烷气c，氩气的分压为0.01MPa，甲烷气的分压为0.01MPa,接通直流脉动电源10，电压为40V，弧光放电过程中调节工作电流与电压保持相对稳定，制得Ti@C@g-C3N4纳米复合物。该纳米复合物微观结构为Ti@C核壳结构纳米胶囊嵌入g-C3N4纳米片，其中：Ti@C纳米胶囊的粒径为5～100nm。
Claims (1)
1.一种Ti@C@g-C3N4纳米复合物，其特征在于，该纳米复合物微观结构为Ti@C核壳结构纳米胶囊嵌入g-C3N4纳米片中；该纳米胶囊的粒径为5～100nm；
该纳米复合物是利用等离子体电弧放电技术，在工作气体下原位制备得到；其中：
采用石墨电极为阴极，钛-三聚氰胺粉末块体为阳极靶材，阴极与阳极靶材之间保持2～30mm的距离；电弧放电的电压为10～40V；所述工作气体为氩气和甲烷气体；所述阳极靶材中钛所占的质量百分比为70～90％；所述氩气的分压为0.01～0.5MPa,甲烷气体的分压为0.01～0.3MPa。
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