CN107670681A - 一种氮掺杂TiO2粉的制备方法 - Google Patents
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Abstract
一种氮掺杂TiO2粉的制备方法，属于材料技术领域，包括如下步骤：(1)将四甲基氢氧化铵滴加到无水乙醇中，搅拌获得混合液；(2)将钛酸异丙酯滴加到混合液中，得到溶胶；(3)将铜板浸没于溶胶底部，陈化后在60～80℃干燥，取出；(4)向铜板通入直流电，利用铜板发热将表面的胶体烧结；(5)烧结完成后将铜板表面的烧结物料刮掉，被刮掉的物料为氮掺杂TiO2粉。本发明的合成工艺简单，反应条件温和，样品烧结时间大大缩短，烧结后样品形态更好，结构更稳定，制备的氮掺杂TiO2对亚甲基蓝的降解率显著提高。
Description
技术领域
本发明属于材料技术领域，特别涉及一种氮掺杂TiO2粉的制备方法。
背景技术
TiO2光催化剂因化学性能稳定、制备成本可控、无毒，以及可利用太阳光，无二次污染等在污染废水的处理方面应用前景广阔，但纯TiO2被用作光催化剂时，因带隙较宽，只能吸收长小于387nm的光子，而且光生电子－空穴复合率高导致量子产率低、光催化效率低，极大限制了其实际应用范围，故须常采用金属离子掺杂、阴离子掺杂、不同半导体复合、贵金属修饰等方法提高TiO2的光催化活性。通过掺杂，可以有效抑制光生电子－空穴复合，在TiO2晶格中引入缺陷位，改变并扩展其光谱响应范围，提高光催化效率。氮掺杂TiO2后在分子内有N-Ti配位健生成，可以使可见光吸收带发生红移，显著提高在可见光区的吸收性能，增强TiO2的光催化活性，在甲醛、甲基橙、罗丹明B等降解方面有较好的应用前景。
目前制备氮掺杂TiO2采用电阻炉烧结法，该方法需要梯度升温，烧结时间长，样品形态较差。
发明内容
针对现有烧结法制备氮掺杂TiO2存在的技术问题，本发明提供一种氮掺杂TiO2粉的制备方法，通过在铜表面沉积胶体，然后进行电热烧结，简化工艺的同时，制备性能优良的氮掺杂TiO2粉。
本发明的方法包括如下步骤：
1、将10～20mL四甲基氢氧化铵(TMAH)在搅拌条件下滴加到30～40mL无水乙醇中，然后继续搅拌至少10min，获得无色透明的混合液；
2、将70～80mL钛酸异丙酯(IOPT)在搅拌条件下滴加到混合液中，得到无色半透明的溶胶；
3、将铜板浸没于溶胶底部，陈化10～12h，再在60～80℃干燥20～22h，然后取出表面覆盖有胶体的铜板；
4、向表面覆盖有胶体的铜板通入直流电，控制通电电流为500～600A，通电时间15～25min，利用铜板发热将表面的胶体烧结；
5、烧结完成后将铜板表面的烧结物料刮掉，被刮掉的物料为氮掺杂TiO2粉。
上述的铜板材质为纯度≥99.9％的铜。
上述的步骤3中，表面覆盖有胶体的铜板上胶体的厚度为2～3mm。
上述的步骤1和2中，搅拌速度为5～15rpm。
上述的步骤1和2中，进行滴加时，控制全部滴加时间为10～15min。
本发明的有益效果是：合成工艺简单，反应条件温和，样品烧结时间大大缩短，烧结后样品形态更好，结构更稳定，同时极大减低生产成本，可重复性好，制备的氮掺杂TiO2光催化剂对亚甲基蓝的降解率显著提高；钛酸异丙酯与四甲基氢氧化铵的反应，使分子内生成N-Ti配位键，改变了TiO2晶格并引起晶格位置缺陷，可以使可见光吸收带发生红移，显著提高在可见光区的吸收性能，增强TiO2的光催化活性。
附图说明
图1为本发明实施例1制得的氮掺杂TiO2粉的SEM照片图。
具体实施方式
本发明实施例中SEM观测采用的设备为JSM-7500F冷场发射扫描电子显微镜。
本发明实施例中采用的四甲基氢氧化铵、无水乙醇和钛酸异丙酯为市购分析纯试剂。
本发明实施例中铜板材质为纯度≥99.9％的铜。
本发明实施例中的铜板在使用前经过打磨去除表面氧化层。
本发明实施例中干燥后的铜板表面胶体的厚度为2～3mm。
本发明实施例中搅拌速度为5～15rpm。
本发明实施例中进行滴加时，控制全部滴加时间为10～15min。
本发明实施例中将被刮掉的物料用研钵研磨10～20min，使全部物料形成粉末。
本发明的氮掺杂TiO2粉粒度50～200nm；平均粒度100～130nm。
本发明实施例中通入直流电时电压为5～10V。
本发明实施例中进行光催化降解测试方法采用GB/T23762-2009《光催化材料水溶液体系净化性能测试方法》。
以下结合实例进一步说明本发明的内容，由技术常识可知，本发明也可通过其它的不脱离本发明技术特征的方案来描述，因此所有在本发明范围内或等同本发明范围内的改变均被本发明包含。
实施例1
将10mL四甲基氢氧化铵在搅拌条件下滴加到30mL无水乙醇中，然后继续搅拌25min，获得无色透明的混合液；
将70mL钛酸异丙酯在搅拌条件下滴加到混合液中，得到无色半透明的溶胶；控制全部滴加时间为10min；
将铜板浸没于溶胶底部，陈化10h，再在60℃干燥22h，然后取出表面覆盖有胶体的铜板；铜板表面胶体的厚度为2mm；
向表面覆盖有胶体的铜板通入直流电，控制通电电流为500A，通电时间25min，利用铜板发热将表面的胶体烧结；
烧结完成后将铜板表面的烧结物料刮掉，被刮掉的物料为氮掺杂TiO2粉，研磨至粉末状；电子显微镜显微镜观测结果如图1所示；平均粒度120nm；
通过光催化降解测试验，掺杂氮后的产品光催化效果明显比纯二氧化钛效果好，未掺杂时，光催化降解率为25％左右，掺杂氮元素后，光催化降解率达95％，提高了在可见光区的吸收性能，增强了TiO2的光催化活性。
实施例2
方法同实施例，不同点在于：
(1)将15mL四甲基氢氧化铵在搅拌条件下滴加到40mL无水乙醇中，然后继续搅拌10min；
(2)将75mL钛酸异丙酯滴加到混合液中，全部滴加时间为12min；
(3)陈化11h，再在70℃干燥21h，铜板表面胶体的厚度为2.4mm；
(4)通电电流为550A，通电时间20min；
(5)氮掺杂TiO2粉平均粒度130nm；
(6)通过光催化降解测试验，光催化降解率达80％。
实施例3
方法同实施例，不同点在于：
(1)将20mL四甲基氢氧化铵在搅拌条件下滴加到35mL无水乙醇中，然后继续搅拌15min；
(2)将78mL钛酸异丙酯滴加到混合液中，全部滴加时间为14min；
(3)陈化12h，再在75℃干燥20h，铜板表面胶体的厚度为2.8mm；
(4)通电电流为560A，通电时间18min；
(5)氮掺杂TiO2粉平均粒度100nm；
(6)通过光催化降解测试验，光催化降解率达85％。
实施例4
方法同实施例，不同点在于：
(1)将20mL四甲基氢氧化铵在搅拌条件下滴加到30mL无水乙醇中，然后继续搅拌20min；
(2)将80mL钛酸异丙酯滴加到混合液中，全部滴加时间为15min；
(3)陈化12h，再在80℃干燥20h，铜板表面胶体的厚度为3mm；
(4)通电电流为600A，通电时间15min；
(5)氮掺杂TiO2粉平均粒度105nm；
(6)通过光催化降解测试验，光催化降解率达90％。
Claims (3)
1.一种氮掺杂TiO2粉的制备方法，其特征在于包括如下步骤：
(1)将10～20mL四甲基氢氧化铵在搅拌条件下滴加到30～40mL无水乙醇中，然后继续搅拌至少10min，获得无色透明的混合液；
(2)将70～80mL钛酸异丙酯在搅拌条件下滴加到混合液中，得到无色半透明的溶胶；
(3)将铜板浸没于溶胶底部，陈化10～12h，再在60～80℃干燥20～22h，然后取出表面覆盖有胶体的铜板；
(4)向表面覆盖有胶体的铜板通入直流电，控制通电电流为500～600A，通电时间15～25min，利用铜板发热将表面的胶体烧结；
(5)烧结完成后将铜板表面的烧结物料刮掉，被刮掉的物料为氮掺杂TiO2粉。
2.根据权利要求1所述的一种氮掺杂TiO2粉的制备方法，其特征在于所述的铜板材质为纯度≥99.9％的铜。
3.根据权利要求1所述的一种氮掺杂TiO2粉的制备方法，其特征在于所述的表面覆盖有胶体的铜板上胶体的厚度为2～3mm。
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