CN110526289A - 一种蓝色锐钛矿相TiO2纳米晶体及其制备方法 - Google Patents
一种蓝色锐钛矿相TiO2纳米晶体及其制备方法 Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
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Abstract
本发明公开一种蓝色自掺杂锐钛矿相TiO2纳米晶的制备方法。以钛粉、氢氟酸和双氧水组成反应体系，180℃下水热釜中反应10小时，离心水洗并干燥后即可获得蓝色自掺杂TiO2纳米晶体。后续NaOH溶液中超声浸泡去除表面氟离子后，蓝色TiO2纳米晶体在紫外光照射下表现出优异的光催化降解水中有机污染物特性。本发明代替了氢化处理制备蓝色TiO2的传统工艺，过程简单且安全可控。
Description
技术领域
本发明方法涉及一种蓝色锐钛矿相TiO2纳米晶体制备技术，属于环境材料技术领域。
背景技术
随着环境污染和能源危机的不断加剧，光催化技术具有巨大的发展潜力，是一种有效的解决方案。二氧化钛具有化学稳定性好、成本低、无毒等优点，在光催化领域得到了广泛的应用。在常见的TiO2晶相(锐钛矿、金红石、板钛矿和TiO2(B))中，锐钛矿相拥有着最佳的光催化活性。
纳米级TiO2具有更大的比表面积，因而具有更高的光催化活性。除了减小催化剂的尺寸，改变催化剂的颜色，使其能够在可见光区和近红外区吸收光，也是一种有效的方法。此外，适当控制导致颜色变化的自掺杂Ti(III)离子和氧缺陷浓度，还可以引入电子陷阱，增大 TiO2光生载流子的空间分离，进而提升紫外光照下的光催化活性。常见的改变TiO2催化剂颜色的方法为氢化，即将TiO2在含氢气气氛中高温热处理。但是，氢气易燃易爆，具有一定的危险性，且高温过程耗费能源。因此，开发一种不需高温且不需氢气处理的制备蓝色TiO2光催化剂的技术路线有重要意义。
发明内容
本发明公开了一种蓝色锐钛矿相TiO2纳米晶体的制备方法，其技术方案如下：
一种蓝色锐钛矿相TiO2纳米晶体的制备方法，它包括以下步骤：
步骤1、配制质量百分比为3-5％的过氧化氢和0.2-0.3％的氢氟酸混合水溶液；
步骤2、称取50-150mg钛粉，添加到30毫升上述混合溶液中，置于容积为50mL的内衬PVC的不锈钢水热釜中，180-185℃下保温10-20小时，得到沉淀物；
步骤3、将步骤2的沉淀物离心、水洗并干燥，即制备得到蓝色锐钛矿相TiO2纳米晶。
上述的蓝色锐钛矿相TiO2纳米晶体的制法制得的蓝色锐钛矿相 TiO2纳米晶。
上述的蓝色锐钛矿相TiO2纳米晶为菱形或方形，其尺寸为50-80 nm。
上述的蓝色锐钛矿相TiO2纳米晶作为光催化剂在环境污染物光降解中的应用。
本发明公开的蓝色锐钛矿相TiO2纳米晶体制备方法不需加入模板，一步法水热合成。在氢氟酸和双氧水混合溶液中，通过改变钛粉的用量，即可调控锐钛矿相TiO2纳米晶的自掺杂浓度。反应一步完成，步骤简便，操作安全，是一种节能环保的合成蓝色锐钛矿相TiO2纳米晶的方法。合成的蓝色锐钛矿相TiO2纳米晶在紫外光区和可见光区均有增强的吸收，光催化活性优异。
附图说明
图1为实施例1制备所得TiO2纳米晶的场发射扫描电子显微镜照片；
图2为实施例1制备所得TiO2纳米晶的X射线衍射图谱；
图3为实施例2制备所得TiO2纳米晶的场发射扫描电子显微镜照片；
图4为实施例3制备所得TiO2纳米晶的场发射扫描电子显微镜照片；
图5为实施例4制备所得TiO2纳米晶的场发射扫描电子显微镜照片；
图6为实施例5制备所得TiO2纳米晶的场发射扫描电子显微镜照片；
图7为实施例1制备所得TiO2纳米晶紫外灯下降解苯酚的曲线。
具体实施方式
实施例1
称取100mg钛粉，量取3mL 30％的过氧化氢水溶液，0.1mL 氢氟酸均匀分散于27mL去离子水中，形成溶液，将100mg钛粉加入其中；
将所述溶液转入50mL不锈钢水热釜中，180℃下反应10小时，得到沉淀物；
所制得沉淀物6000r/min离心水洗三次，60℃干燥，即制备得到锐钛矿相蓝色TiO2纳米晶体。
按照实施例1制备得到TiO2纳米晶体的场发射扫描电子显微镜照片如图1所示。从图中可以看出，在180℃水热反应10小时后，按照实施例1所制备的TiO2纳米晶呈现出包括菱形、方形、球形和不规则晶体的形态，平均粒径为50-80纳米。
按照实施例1制备得到TiO2纳米晶的X射线衍射如图2所示，根据JCPDS卡片21-1272，所有样品均显示出良好的结晶度，且仅包含锐钛矿相，没有任何其他杂相。
实施例2
称取50mg钛粉，量取3mL 30％的过氧化氢水溶液，0.1mL氢氟酸均匀分散于27mL去离子水中，形成溶液，将50mg钛粉加入其中；
将所述溶液转入50mL不锈钢水热釜中，180℃下反应10小时，得到沉淀物；
所制得沉淀物6000r/min离心水洗三次，60℃干燥，即可制备得到锐钛矿相白色TiO2纳米晶体。
按照实施例2制备得到TiO2纳米晶体的场发射扫描电子显微镜照片如图3所示。
实施例3
称取150mg钛粉，量取3mL 30％的过氧化氢水溶液，0.1mL 氢氟酸均匀分散于27mL去离子水中，形成溶液，将150mg钛粉加入其中；
将所述溶液转入50mL不锈钢水热釜中，180℃下反应10小时，得到沉淀物；
所制得沉淀物6000r/min离心水洗三次，60℃干燥，即可制备得到锐钛矿相蓝色TiO2纳米晶体。
按照实施例3制备得到TiO2纳米晶体的场发射扫描电子显微镜照片如图4所示。
实施例4
称取100mg钛粉，量取3mL 30％的过氧化氢水溶液，0.1mL 氢氟酸均匀分散于27mL去离子水中，形成溶液，将100mg钛粉加入其中；
将所述溶液转入50mL不锈钢水热釜中，180℃下反应5小时，得到沉淀物；
所制得沉淀物6000r/min离心水洗三次，60℃干燥，即可制备得到锐钛矿相蓝色TiO2纳米晶体。
按照实施例4制备得到TiO2纳米晶的场发射扫描电子显微镜照片如图5所示。反应5h后，蓝色TiO2纳米晶体的形态不均匀，大小不一，说明晶体生长未完全完成。
实施例5
称取100mg钛粉，量取3mL 30％的过氧化氢水溶液，0.1mL 氢氟酸均匀分散于27mL去离子水中，形成溶液，将100mg钛粉加入其中；
将所述溶液转入50mL不锈钢水热釜中，180℃下反应20小时，得到沉淀物；
所制得沉淀物6000r/min离心水洗三次，60℃干燥，即可制备得到锐钛矿相蓝色TiO2纳米晶体。
按照实施例5制备得到TiO2纳米晶的场发射扫描电子显微镜照片如图6所示。反应20小时后的样品，TiO2纳米晶体生长均匀，与 10h制备所得样品相比形态保持不变，表明10小时后生长过程已经结束。
光催化降解苯酚性能测试
测试条件：采用紫外灯，光强为7.3mW/cm2，降解物为50mL初始浓度10ppm的苯酚水溶液，催化剂用量为25mg。为了消除纳米晶表面吸附氟离子的影响，光催化测试前，采用浓度为10摩尔/升到NaOH溶液超声浸泡蓝色TiO2纳米晶以去除氟离子，而后干燥备用。
测试结果：图7为按照实施例1制备得到TiO2蓝色纳米晶的光催化效果图。可以看出，紫外灯光照下，所制备纳米晶对苯酚具有优异的降解性能，4h可以降解超过90％的苯酚。
Claims (4)
1.一种蓝色锐钛矿相TiO2纳米晶体的制备方法，其特征是它包括以下步骤：
步骤1、配制质量百分比为3-5％的过氧化氢和0.2-0.3％的氢氟酸混合水溶液；
步骤2、称取50-150mg钛粉，添加到30毫升上述混合溶液中，置于容积为50mL的内衬PVC的不锈钢水热釜中，180-185℃下保温10-20小时，得到沉淀物；
步骤3、将步骤2的沉淀物离心、水洗并干燥，即制备得到蓝色锐钛矿相TiO2纳米晶。
2.根据权利要求1所述的蓝色锐钛矿相TiO2纳米晶体的制法制得的蓝色锐钛矿相TiO2纳米晶。
3.根据权利要求2所述的蓝色锐钛矿相TiO2纳米晶，其特征是：所述的蓝色锐钛矿相TiO2纳米晶为菱形或方形，其尺寸为50-80nm。
4.根据权利要求2所述的蓝色锐钛矿相TiO2纳米晶作为光催化剂在环境污染物光降解中的应用。
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