CN111634956B - 一种含氧金属化合物氧空位的合成方法 - Google Patents
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000001301 oxygen Substances 0.000 title claims abstract description 46
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 26
- 150000002736 metal compounds Chemical class 0.000 title claims abstract description 13
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 10
- 239000010453 quartz Substances 0.000 claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052786 argon Inorganic materials 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 10
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- 239000000126 substance Substances 0.000 abstract description 6
- 238000002474 experimental method Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 229910052719 titanium Inorganic materials 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 6
- 229910000428 cobalt oxide Inorganic materials 0.000 description 6
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000005215 recombination Methods 0.000 description 5
- 230000006798 recombination Effects 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 206010021143 Hypoxia Diseases 0.000 description 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
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- 238000005984 hydrogenation reaction Methods 0.000 description 1
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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Abstract
本发明公开了一种含氧金属化合物氧空位的合成方法，包括以下步骤：a.石英管抽真空，用氩气洗，反复充洗；b.钛粉和研磨后的CoO分别放在两个不同的石英舟里，将两个石英舟平行放入炉中；c.调节加热温度，加热一段时间；d.自然冷却后研磨收样。本发明利用金属单质钛在真空条件下吸收含氧金属化合物晶格中的氧，使其产生表面缺陷，光催化性能显著提高。本发明方法实验方法简单，可作性强，仪器要求简单，不需要特定的气氛条件，安全性高。
Description
技术领域
本发明涉及多元半导体复合材料技术领域，特别涉及一种含氧金属化合物氧空位的合成方法。
背景技术
当前能源危机环境恶化，光催化引起了人们极大的兴趣。在各种含氧半导体中，例如SrTiO3,TiO2,ZnO等由于其优异的电子和光学性质，光化学稳定性，低成本和高催化效率而成为有前途的光催化剂。太阳能驱动光催化过程的高效性很大程度上取决于半导体的吸收可见光和红外光的能力，已经抑制光生电子-空穴的复合能力。但是许多含氧半导体材料带隙较宽，它仅在紫外光照射下才有活性。并且许多半导体材料的电子-空穴复合较高导致低的光催化活性。
众所周知，氧空位在光催化过程中起重要作用。氧空位的存在会在导带下面插入一个施主能级，减小带隙，进而扩大其光响应区间。表面氧空位可作为光致电荷缺陷和吸附位点，其中电荷可转移到被吸附的化合物上，从而阻止了光生电荷载流子的重组，从而改善了光催化性能。
目前，氧空位的合成方法有很多种。气氛脱氧法，就是由特定的气氛种，利用高温使氧从物质中脱离，这种方法需要较高的能量且需要稳定的无氧气流环境；离子掺杂法，利用不同元素离子价态的不同，通过缺氧来使其中价态为零，但是掺杂的方法困难比例难以确定；加温氢化法，高温条件下氢气吸收化合物中的氧，但是氢气气流较危险易爆；化学反应法是通过强还原剂降低金属元素价态，电荷守恒就会缺失氧形成空位，而强还原剂实验亦存在风险；机械化学力法，使用机械力使晶格中的氧脱离，这种方法很容易破坏原有物质结构；高能粒子轰击法，通过高能离子使氧解离，但是设备要求较高，且由辐射危险。
发明内容
针对现有技术存在的不足，本发明的目的是提供一种含氧金属化合物氧空位的合成方法，用于探索光解水制氢和有机染料降解等光催化性能，以降低催化成本，提高催化效率。
本发明的上述技术目的是通过以下技术方案得以实现的：
一种含氧金属化合物氧空位的合成方法，包括以下步骤：
a.石英管抽真空，用氩气洗，反复充洗；
b.钛粉和研磨后的CoO分别放在两个不同的石英舟里，将两个石英舟平行放入炉中；
c.调节加热温度，加热一段时间；
d.自然冷却后研磨收样。
进一步，步骤b中钛粉的加入量为10mml，CoO的加入量为10mmol。
优选的，步骤b中钛粉的加入量为10mml，CoO的加入量为10mmol。
进一步，步骤c中加热温度为630℃，加热8-12小时。
优选的，步骤c中加热温度为630℃，加热10小时。
本发明具有以下有益效果：
本发明利用金属单质钛在真空条件下吸收含氧金属化合物晶格中的氧，使其产生表面缺陷，以提高光催化活性。本发明方法实验方法简单，可作性强，仪器要求简单，不需要特定的气氛条件，安全性高，具有广阔的应用前景。
附图说明
图1是本发明方法实施例1-3制备的具有氧空位的氧化钴催化剂的XRD图；
图2是本发明方法实施例1-3制备的具有氧空位的氧化钴催化剂固体紫外以及物质颜色变化图；
图3是本发明方法实施例1-3制备的具有氧空位的氧化钴催化剂的荧光图。
具体实施方式
以下结合附图对本发明作进一步详细说明。
实施例1
一种含氧金属化合物氧空位的合成方法，包括以下步骤：
a.石英管抽真空，用氩气洗，反复充洗，目的是为了清楚关内残留氧气；
b.10mml钛粉和10mmol研磨后的CoO分别放在两个不同的石英舟里，将两个石英舟平行放入炉中；
c.调加热温度为630℃，时间为8小时；
d.自然冷却后研磨收样。
实施例2
一种含氧金属化合物氧空位的合成方法，包括以下步骤：
a.石英管抽真空，用氩气洗，反复充洗，目的是为了清楚关内残留氧气；
b.10mml钛粉和10mmol研磨后的CoO分别放在两个不同的石英舟里，将两个石英舟平行放入炉中；
c.调加热温度为630℃，时间为10小时；
d.自然冷却后研磨收样。
实施例3
一种含氧金属化合物氧空位的合成方法，包括以下步骤：
a.石英管抽真空，用氩气洗，反复充洗，目的是为了清楚关内残留氧气；
b.10mml钛粉和10mmol研磨后的CoO分别放在两个不同的石英舟里，将两个石英舟平行放入炉中；
c.调加热温度为630℃，时间为12小时；
d.自然冷却后研磨收样。
性能测试：
图1为依据本发明实施例1-3制备的具有氧空位的氧化钴催化剂的XRD图；图中CoO与Ti在630℃ 8h煅烧后，样品xrd衍射峰在31.4°，36.8°，59.3°，65.2°出现Co3O4的峰。说明该物质中有CoO和Co3O4两种组分。CoO与Ti在630℃ 10h煅烧后，样品xrd衍射峰在36.5°，42.4°，61.5°，77.5°出现的峰值与CoO准备卡片一一对应，说明该物质为纯净的CoO。CoO与Ti在630℃ 12h煅烧后，样品xrd衍射峰在43.8°，52.4°出现了钴单质的衍射峰，说明CoO中的晶格氧被完全烧出产生钴。从以上结果分析表明630℃ 8h,10h,12h中，630℃10小时为实验的最优条件，物象CoO更纯。
图2为依据本发明实施例1-3制备的具有氧空位的氧化钴催化剂固体紫外以及物质颜色变化图；CoO与Ti在630℃ 8h,10h,12h煅烧后,颜色出现明显变化，由黑色变为棕色。与CoO原样相比实验后的三组样品在可见光区紫外吸收明显提高。630℃ 12h煅烧的样品在300nm-450nm的吸收值更高，630℃ 12h煅烧的样品在450nm-800nm吸收值更高，说明其可见光活性更强。
图3为依据本发明实施例1-3制备的具有氧空位的氧化钴催化剂荧光图。CoO原样，CoO与Ti在630℃ 8h,12h,10h煅烧后的样品，其荧光强度逐渐降低，说明630℃ 10h电子复合率最低，光催化活性最好。
以上三个方面说明CoO与Ti在630℃8h,10h,12h煅烧的最优实验条件为630℃10h，其物象更纯，可见光吸收能力更强，电子复合率更低，表征效果表明其光催化活性明显强于CoO原样。
本具体实施方式的实施例均为本发明的较佳实施例，并非依此限制本发明的保护范围，故：凡依本发明的结构、形状、原理所做的等效变化，均应涵盖于本发明的保护范围之内。
Claims (1)
1.一种含氧金属化合物氧空位的合成方法，其特征在于：包括以下步骤：
a .石英管抽真空，用氩气洗，反复充洗；
b.钛粉和研磨后的CoO分别放在两个不同的石英舟里，将两个石英舟平行放入炉中；钛粉的加入量为10mml，CoO的加入量为10mmol；
c.调节加热温度，加热一段时间；加热温度为630℃，加热10小时；
d .自然冷却后研磨收样。
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