CN117599832A - 一种Tm/g-C3N4纳米复合光催化剂及其制备方法和应用 - Google Patents
一种Tm/g-C3N4纳米复合光催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及半导体光催化技术领域,具体涉及一种Tm/g‑C3N4纳米复合光催化剂及其制备方法和应用。Tm/g‑C3N4纳米复合光催化剂以g‑C3N4纳米片为前驱体,以硝酸铥为原料,以水和乙腈的极性混合溶液为溶剂,以二硫苏糖醇为还原剂,常温常压下通过微波活化制备。本发明方法能够简单快捷的制备Tm/g‑C3N4复合光催化剂材料,所得Tm/g‑C3N4复合光催化剂材料的微观结构为片状结构,具有可将光响应,能够在可见光下表现出优异的光催化产氢活性。
Description
技术领域
本发明涉及半导体光催化技术领域,具体涉及一种Tm/g-C3N4纳米复合光催化剂及其制备方法和应用。
背景技术
随着工业化的发展,大量的化石能源消耗用来支撑工业化的进程,人类社会面临的能源短缺和环境问题日益严峻。氢能被认为是最有效的绿色能源之一,氢能的大规模应用,能够有效的解决化石燃料的使用而造成的能源危机和环境污染问题。目前电解水制氢的技术成本较高,高温热解水制氢能化转换效率比较低,且耗能较大,有温室气体二次排放等问题。因此,需要发展清洁的制氢技术,例如光催化分解水产氢技术能够将无穷无尽的太阳能转化为氢能,是一种非常有潜力的氢能源利用技术。
在诸多的光催化分解水产氢的催化剂中,石墨相氮化碳(g-C3N4)作为一种高效稳定且化学性质稳定的光催化剂备受人们关注,但是其光生载流子的分离效率较低,且光催化性能难以令人满意。因此,需要对纯的g-C3N4光催化剂进行改性,例如将贵金属纳米颗粒沉积在g-C3N4表面能够极大的提升其光催化分解水产氢性能。
现阶段,一般采用水热合成的方法制备贵金属沉积石墨相氮化碳复合材料,然而水热法存在高温、高压且危险的缺点。因此开发一种简单的金属沉积石墨相氮化碳复合光催化剂合成方法,对于光催化剂的广泛应用及推广是一项非常有意义的研究工作。
发明内容
针对水热合成金属/石墨相氮化碳复合光催化剂存在的高温、高压且危险的技术问题,本发明提供一种Tm/g-C3N4纳米复合光催化剂及其制备方法和应用,以水和乙腈极性混合溶液为溶剂,以二硫苏糖醇为还原剂,在常温常压下采用微波活化方法,便能够简单快捷的制备Tm/g-C3N4复合光催化剂材料,所得Tm/g-C3N4复合光催化剂材料的微观结构为片状结构,具有可将光响应,能够在可见光下表现出优异的光催化产氢活性。
第一方面,本发明提供一种Tm/g-C3N4纳米复合光催化剂的制备方法,以g-C3N4纳米片为前驱体,以硝酸铥为原料,以水和乙腈的极性混合溶液为溶剂,以二硫苏糖醇为还原剂,常温常压下通过微波活化制备。
进一步的,具体步骤如下:
(1)将水和乙腈均匀混合,在超声条件下将g-C3N4纳米片和硝酸铥充分分散到水和乙腈的极性混合溶液中;
(2)然后在超声条件下,将二硫苏糖醇加入到步骤(1)的混合溶液中充分分散;
(3)将步骤(2)的混合溶液放置在微波反应仪中进行活化反应;
(4)反应结束后,洗涤产物,真空冷冻干燥产物。
进一步的,水和乙腈的摩尔比为1:1.5~2.5。
进一步的,水和乙腈的极性混合溶液的加入量为100~150mL。
进一步的,g-C3N4纳米片的加入量为170~200mg,硝酸铥的加入量为0.01~0.2mmol,二硫苏糖醇的加入量为0.02~0.035g。
进一步的,微波功率为100~150W,反应时间为2~5min。
进一步的,真空冷冻干燥的真空度<15Pa,温度≤-50℃。
第二方面,本发明提供一种采用上述制备方法制得的Tm/g-C3N4纳米复合光催化剂。
第三方面,本发明提供一种上述Tm/g-C3N4纳米复合光催化剂在光催化分解水产氢中的应用。
本发明的技术原理和有益效果如下:
本发明中,水和乙腈的极性混合溶液可以调节反应过程溶剂极性,使用二硫苏糖醇作为还原剂,配合常温常压下微波活化方法,使+3价铥元素还原成铥单质,并原位地沉积在石墨相氮化碳纳米片表面。同时,本发明使用微波活化法,可以均匀分散前驱体,防止过度生长,另一方面能够活化反应分子,降低反应能垒,有效降低制备温度。本发明方法克服了传统水热法制备光催化剂存在的高温、高压、高耗能和催化剂性能不高等问题。本发明方法制备的Tm/g-C3N4纳米复合光催化剂中,Tm颗粒均匀且形成较小纳米颗粒,提供更多的催化活性位点,非常有利于光催化活性的提升。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,对于本领域普通技术人员而言,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1是实施例1中所制备的5% Tm/g-C3N4纳米复合光催化剂的透射电镜图。
图2是实施例1中所制备的Tm/g-C3N4纳米复合光催化剂的XRD图。
图3是实施例1中所制备的Tm/g-C3N4纳米复合光催化剂与g-C3N4纳米片的红外光谱图。
图4是实施例1中所制备的Tm/g-C3N4纳米复合光催化剂与g-C3N4纳米片的紫外-可见吸收光谱图。
图5是实施例2中所制备的Tm/g-C3N4纳米复合光催化剂与g-C3N4纳米片的光催化分解水产氢性能图。
具体实施方式
为了使本技术领域的人员更好地理解本发明中的技术方案,下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都应当属于本发明保护的范围。
实施例1
(1)将水和乙腈按照摩尔比1:2的比例均匀混合,得到总体积为120mL的水和乙腈的极性混合溶液,在超声条件下将170mg g-C3N4纳米片和不同物质的量的Tm(NO3)3充分分散到上述极性混合溶液中;
(2)然后在超声条件下,将0.025g二硫苏糖醇作为还原剂加入到步骤(1)的混合溶液中充分分散;
(3)将步骤(2)的混合溶液放置在微波反应仪中进行活化反应,微波功率为150W,反应时间为3min;
(4)反应结束后,洗涤产物,采用真空冷冻干燥机彻底干燥产物,干燥的真空度<15Pa,温度为-50℃。
根据Tm(NO3)3加入量的不同,将Tm(NO3)3物质的量为0.01mmol时得到的产物命名为1% Tm/CN,将Tm(NO3)3物质的量为0.03mmol时得到的产物命名为3% Tm/CN,将Tm(NO3)3物质的量为0.05mmol时得到的产物命名为5% Tm/CN,将Tm(NO3)3物质的量为0.08mmol时得到的产物命名为8% Tm/CN,将Tm(NO3)3物质的量为0.1mmol时得到的产物命名为10% Tm/CN,将Tm(NO3)3物质的量为0.2mmol时得到的产物命名为20% Tm/CN。
使用透射电镜观察所制备的5% Tm/CN纳米复合光催化剂,结果如图1所示。图1左右两幅图为5% Tm/g-C3N4纳米复合光催化剂两个不同位置的透射电镜图片,可见整体Tm/g-C3N4复合材料呈现纳米片结构,直径约为1~5nm的铥金属单质均匀地沉积在g-C3N4的表面上。
对所制备的Tm/g-C3N4纳米复合光催化剂进行XRD表征,结果如图2所示,随着铥的含量增加,g-C3N4的XRD衍射峰强度逐渐的降低,这说明铥在g-C3N4表面且对x射线具有屏蔽作用,使其峰强度降低。
对所制备的Tm/g-C3N4纳米复合光催化剂进行红外测试,并与前驱体g-C3N4纳米片(图中标记为CN)对比,结果如图3所示,随着铥含量的增加,复合材料主要表现出g-C3N4的振动峰特性,而且没有改变其微观框架结构,这表明铥单质沉积在g-C3N4的表面。
对所制备的Tm/g-C3N4纳米复合光催化剂进行紫外-可见吸收光谱测定,并与前驱体g-C3N4纳米片(图中标记为CN)对比,结果如图4所示,随着铥含量的增加,Tm/g-C3N4纳米复合光催化剂的光吸收性能逐渐增强,这表明铥沉积在g-C3N4表面,能够显著增加其光吸收性质。
实施例2
(1)将水和乙腈按照摩尔比1:2的比例均匀混合,得到总体积为120mL的水和乙腈的极性混合溶液,在超声条件下将200mg g-C3N4纳米片和不同物质的量的Tm(NO3)3充分分散到上述极性混合溶液中;
(2)然后在超声条件下,将0.025g二硫苏糖醇作为还原剂加入到步骤(1)的混合溶液中充分分散;
(3)将步骤(2)的混合溶液放置在微波反应仪中进行活化反应,微波功率为150W,反应时间为3min;
(4)反应结束后,洗涤产物,采用真空冷冻干燥机彻底干燥产物,干燥的真空度<15Pa,温度为-50℃。
根据Tm(NO3)3加入量的不同,将Tm(NO3)3物质的量为0.01mmol时得到的产物命名为1% Tm/CN’,将Tm(NO3)3物质的量为0.03mmol时得到的产物命名为3% Tm/CN’,将Tm(NO3)3物质的量为0.05mmol时得到的产物命名为5% Tm/CN’,将Tm(NO3)3物质的量为0.08mmol时得到的产物命名为8% Tm/CN’,将Tm(NO3)3物质的量为0.1mmol时得到的产物命名为10% Tm/CN’,将Tm(NO3)3物质的量为0.2mmol时得到的产物命名为20% Tm/CN’。
分别使用实施例2制备的六种Tm/g-C3N4纳米复合光催化剂样品进行光催化分解水产氢实验,并以前驱体g-C3N4纳米片(图中标记为CN)作为对照,结果如图5所示,在可见光条件下,Tm/g-C3N4纳米复合光催化剂性能呈现先增加后减少的趋势。这主要是因为随着铥含量的增加,其对光生载流子的复合效应具有抑制作用,且能够促进光生载流子的传输以及析氢。但铥元素的过度沉积,对于光催化产氢性能的提升是不利的。
尽管通过参考附图并结合优选实施例的方式对本发明进行了详细描述,但本发明并不限于此。在不脱离本发明的精神和实质的前提下,本领域普通技术人员可以对本发明的实施例进行各种等效的修改或替换,而这些修改或替换都应在本发明的涵盖范围内/任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到变化或替换,都应涵盖在本发明的保护范围之内。
Claims (9)
1.一种Tm/g-C3N4纳米复合光催化剂的制备方法,其特征在于,以g-C3N4纳米片为前驱体,以硝酸铥为原料,以水和乙腈的极性混合溶液为溶剂,以二硫苏糖醇为还原剂,常温常压下通过微波活化制备。
2.如权利要求1所述的制备方法,其特征在于,具体步骤如下:
(1)将水和乙腈均匀混合,在超声条件下将g-C3N4纳米片和硝酸铥充分分散到水和乙腈的极性混合溶液中;
(2)然后在超声条件下,将二硫苏糖醇加入到步骤(1)的混合溶液中充分分散;
(3)将步骤(2)的混合溶液放置在微波反应仪中进行活化反应;
(4)反应结束后,洗涤产物,真空冷冻干燥产物。
3.如权利要求1或2所述的制备方法,其特征在于,水和乙腈的摩尔比为1:1.5~2.5。
4.如权利要求1或2所述的制备方法,其特征在于,水和乙腈的极性混合溶液的加入量为100~150mL。
5.如权利要求1或2所述的制备方法,其特征在于,g-C3N4纳米片的加入量为170~200mg,硝酸铥的加入量为0.01~0.2mmol,二硫苏糖醇的加入量为0.02~0.035g。
6.如权利要求1或2所述的制备方法,其特征在于,微波功率为100~150W,反应时间为2~5min。
7.如权利要求2所述的制备方法,其特征在于,真空冷冻干燥的真空度<15Pa,温度≤-50℃。
8.一种采用如权利要求1~7任一所述的制备方法制得的Tm/g-C3N4纳米复合光催化剂。
9.一种如权利要求8所述的Tm/g-C3N4纳米复合光催化剂在光催化分解水产氢中的应用。
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