CN112536056B - 一种二硫化钨量子点/c掺杂类石墨相氮化碳纳米片异质结构光催化剂及其制备方法 - Google Patents
一种二硫化钨量子点/c掺杂类石墨相氮化碳纳米片异质结构光催化剂及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种WS2量子点/C掺杂g‑C3N4纳米片异质结构光催化剂的制备方法，包括：(1)C掺杂g‑C3N4纳米片的制备：碳源与碳氮源混合并进行煅烧，制得C掺杂g‑C3N4，煅烧后进行研磨，研磨后再次煅烧，制得C掺杂g‑C3N4纳米片；(2)WS2量子点的制备：将钨源与硫源混合超声，转入高压反应釜反应，制得WS2量子点；(3)将WS2量子点与C掺杂g‑C3N4纳米片混合超声，得到WS2量子点/C掺杂g‑C3N4纳米片异质结构光催化剂。还公开了上述方法制得的WS2量子点/C掺杂g‑C3N4纳米片异质结构光催化剂在光催化析氢方面的应用。
Description
技术领域
本发明涉及一种光催化材料，具体涉及一种WS2量子点/C掺杂g-C3N4纳米片异质结构光催化剂的制备方法，属于材料合成技术领域。
背景技术
随着人类社会的发展，汽车、轮船、飞机等交通工具的出现和普及，以及工业制造的规模化，地球上的化石能源不断被消耗，石油、天然气等化石能源并不是取之不尽用之不竭的，能源危机以已经成为人类面临的严峻问题。因此，开发新能源刻不容缓。半导体材料吸收太阳能可以裂解水产生氢气，光催化技术在利用太阳能制造清洁能源(氢能)等领域显示了广阔的应用前景。
类石墨相氮化碳(g-C3N4)被认为是具有巨大潜力的光催化剂材料，因为它可以吸收太阳光谱中小于460nm的蓝紫光，其导带和价带跨过了水的氧化还原窗口，理论上可以在可见光下实现水的全分解，带隙(2.7eV)窄，热、化学稳定性好，成本低，易于制备。然而，g-C3N4存在比表面积小、光生电子和空穴复合率高以及不能充分利用太阳光中可见光部分的能量等问题，导致其在实际应用中仍存在很多困难。为了提高g-C3N4的光催化活性，常采用元素掺杂、纳米化改性、与其他材料复合形成异质结结构等方法抑制光生电子空穴对的复合、拓宽光谱响应范围。元素掺杂一般导致g-C3N4中的C、N等元素被金属元素或者非金属元素所取代，从而达到光生电子-空穴对高效分离的效果，最终导致光催化性能的提高。
WS2是一种带隙为1.35eV半导体材料，它的光吸收区域扩展到了910nm，并且和g-C3N4类似，也是一种层状结构材料，WS2纳米片具有很高的紫外和可见光光催化活性，它是一种独特的全太阳光谱光催化剂。此外，WS2可以作为助催化剂来替代Pt等贵金属用于光催化析氢反应。与WS2纳米片相比，WS2量子点提供更大的表面积，更丰富的活性位点，更短的电荷扩散距离和更强的光生电子和空穴的的氧化还原能力。由于强大的量子约束效应和减少的共轭长度，与WS2纳米片相比，WS2量子点的带隙大大增加，这对光催化析氢反应是有利的，本发明人首次合成了WS2量子点/C掺杂g-C3N4纳米片异质结构光催化剂，制备方法操作简单，能耗低，反应条件温和，绿色环保，具有良好的光催化析氢能力，产氢速率是原始g-C3N4材料的300多倍。
发明内容
采用热解法合成C掺杂g-C3N4纳米片，再将其与合成的WS2量子点混合超声制备WS2量子点/C掺杂g-C3N4纳米片光催化剂，以三乙二醇、甲醇、乙醇等为牺牲剂探索了WS2量子点/C掺杂g-C3N4纳米片光催化剂的析氢性能，所制备的WS2量子点/C掺杂g-C3N4纳米片光催化剂的光催化析氢性能较纯g-C3N4显著提升。
本发明提供一种WS2量子点/C掺杂g-C3N4纳米片复合光催化剂的制备方法，其特征在于，该方法包括以下步骤：
(1)C掺杂g-C3N4纳米片的制备：将碳源与碳氮源混合并进行煅烧，制得C掺杂g-C3N4，煅烧后进行研磨，研磨后再次煅烧，得到C掺杂g-C3N4纳米片，再次研磨；
(2)WS2量子点的制备：将钨源与硫源混合超声，转入高压反应釜反应，反应结束后冷却至室温；
(3)将WS2量子点与步骤1制得的C掺杂g-C3N4纳米片混合超声，得到WS2量子点/C掺杂g-C3N4纳米片复合光催化剂并干燥。
在上述制备方法中，所述步骤(1)中，碳源可选为乙醇、多孔碳泡沫葡萄糖、氰尿酸等。
在上述制备方法中，所述步骤(1)中，碳氮源可选为单胺、二氰二胺、三聚氰胺、尿素或硫脲。
在上述制备方法中，所述步骤(1)中，第一次煅烧温度为300～1000℃，再次煅烧温度为100～500℃。
在上述制备方法中，所述步骤(2)中，钨源可选为三氧化钨、钨酸、钨酸钠、四硫代钨酸铵等。
在上述制备方法中，所述步骤(2)中，硫源可选为硫代乙酰胺、半胱氨酸、升华硫等。
在上述制备方法中，所述步骤(2)中，超声时间为1～10min。
在上述制备方法中，所述步骤(2)中，水热箱中温度为100～240℃。
在上述制备方法中，所述步骤(2)中，水热箱加热时间为10～30h。
在上述制备方法中，所述步骤(3)中，超声时间为0.5～2h。
在上述制备方法中，所述步骤(3)中，干燥温度为10～50℃。
采用本技术制备的WS2量子点/C掺杂g-C3N4纳米片复合光催化剂制备过程简单，反应温和，经济环保，所制备光催化剂产氢速率达到了520.8μmolg-1h-1，是纯g-C3N4的300多倍。
附图说明
图1是本发明实施例1所制得的WS2量子点/C掺杂g-C3N4纳米片光催化剂的XRD图
图2是本发明实施例1所制得的WS2量子点/C掺杂g-C3N4纳米片光催化剂的光催化析氢性能图。
具体实施方式
下面结合实施例对本发明的技术方案做进一步说明。
本发明提出一种高性能WS2量子点/C掺杂g-C3N4纳米片复合光催化剂制备方法，其特征在于，所述方法采用热解法合成C掺杂g-C3N4纳米片，再将其与合成的WS2量子点混合超声制备WS2量子点/C掺杂g-C3N4纳米片光催化剂，包括以下步骤和内容：
(1)碳源可选为乙醇、多孔碳泡沫、葡萄糖、氰尿酸等。
(2)碳氮源可选为单胺、二氰二胺、三聚氰胺、尿素或硫脲等。
(3)将碳源和碳氮源混合，放置在坩埚中，于马弗炉中煅烧两次，第一次煅烧温度为300～1000℃，再次煅烧温度为100～500℃，制得C掺杂g-C3N4纳米片
(4)钨源可选为三氧化钨、钨酸、钨酸钠、四硫代钨酸铵等。
(5)硫源可选为硫代乙酰胺、半胱氨酸、升华硫等。
(6)将钨源与硫源混合超声，超声时间为1～10min；再转入高压反应釜反应，反应温度为100～240℃，时间为10～30h；反应结束后冷却至室温，制得WS2量子点。
(7)将WS2量子点与C掺杂g-C3N4纳米片混合超声，超声时间为0.5～2h；最后在10～50℃条件下干燥得到WS2量子点/C掺杂g-C3N4纳米片复合光催化剂。
总之，用本技术能得到高性能的WS2量子点/C掺杂g-C3N4纳米片复合光催化剂。
实施例1：称取尿素20g，葡萄糖0.005g，充分研磨，置于干净的瓷坩埚中并盖好盖子，将其置于550℃中的马弗炉煅烧4h，制得C掺杂g-C3N4，研磨，置于干净的瓷舟中，将其置于450℃的马弗炉中煅烧6h，制得C掺杂g-C3N4纳米片，称取0.125g钨酸钠，1g半胱氨酸，超声10min，转移至反应釜中在220℃反应24h，制得WS2量子点，称取0.1g C掺杂g-C3N4纳米片与一定量WS2量子点混合超声1h，制得WS2量子点/C掺杂g-C3N4纳米片复合光催化剂。
所合成的WS2量子点/C掺杂g-C3N4纳米片复合光催化剂制备过程简单，经济环保，成本低廉，产氢速率达到了520.8μmolg-1h-1。
Claims (1)
1.一种WS2量子点/C掺杂g-C3N4纳米片复合产氢光催化剂的制备方法，其特征在于，该方法包括以下步骤：
(1)C掺杂g-C3N4纳米片的制备：将碳源与碳氮源混合并，在300～1000℃进行煅烧，制得C掺杂g-C3N4，煅烧后进行研磨，研磨后再次在100～500℃条件下煅烧，得到C掺杂g-C3N4纳米片，再次研磨；
(2)上述步骤(1)中所述碳源可选为多孔碳泡沫、葡萄糖、氰尿酸中的一种或多种；
(3)上述步骤(1)中碳氮源可选为单胺、二氰二胺、三聚氰胺、尿素或硫脲中的一种或多种；
(4)WS2量子点的制备：将钨源与硫源混合超声，转入高压反应釜，在水热箱中100～240℃，加热时间为10～30h，反应结束后冷却至室温；
(5)上述步骤(4)中所述钨源可选为钨酸、钨酸钠、四硫代钨酸铵中的一种；
(6)上述步骤(4)中所述硫源可选为硫代乙酰胺、半胱酸铵、升华硫中的一种；
(7)将WS2量子点与步骤1制得的纳米片混合超声0.5～2h，得到WS2量子点/C掺杂g-C3N4纳米片复合光催化剂并干燥。
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| CN109967095A (zh) * | 2019-04-17 | 2019-07-05 | 南昌航空大学 | 一种全晶体异质结光催化材料及其制备方法和应用 |
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| CN109967095A (zh) * | 2019-04-17 | 2019-07-05 | 南昌航空大学 | 一种全晶体异质结光催化材料及其制备方法和应用 |
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