CN110743583A - 一种0d/2d磷化铁/硫化镉复合光催化剂及制备方法和应用 - Google Patents
一种0d/2d磷化铁/硫化镉复合光催化剂及制备方法和应用 Download PDFInfo
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Abstract
本发明属无机纳米材料制备技术领域,公开了一种零维(0D)/二维(2D)磷化铁纳米颗粒/硫化镉纳米片复合可见光光催化剂及制备方法和应用。主要是对2D硫化镉进行了复合,采用原位一步磷化法将0D的磷化铁颗粒负载2D的硫化镉纳米片上,增强了其光生载流子的分离效率,使得催化活性大大提高。本发明制备出的0D/2D磷化铁/硫化镉复合可见光光催化剂结构明晰,易于生产,具良好的光催化分解水产氢性能,产氢效率显著提高。且该制备方法简单,可靠,重复性好,具有较好的应用前景。
Description
技术领域
本发明属于无机纳米材料制备技术领域,特别涉及一种光催化剂磷化铁/硫化镉复合材料的制备方法。
技术背景
通过光催化水分解反应将太阳能转化为可直接利用的氢能被认为是应对能源危机的一种重要解决方法。其中,光催化剂的选取对光催化反应尤其重要。最近,大量的半导体基光催化剂被用于光催化产氢,比如:石墨相氮化碳 (g-C3N4),二氧化钛 (TiO2),硫化镉(CdS)等。但是,光吸收能力差,载流子利用低等问题严重制约了光催化剂的使用。
硫化镉(CdS)由于其具有合适的能带位置(禁带宽度2.4 eV,可见光响应)以及出色的还原能力,被认为是一种出色的光催化剂。其中,片状的2D CdS纳米片具有面内各向异性、出色的电子迁移能力以及高暴露的活性位点等特性,这些特性导致其具有更为出色的光催化产氢活性。但是,片状CdS光催化剂的广泛使用一直受制于其较快的光生载流子复合。
近些年,采用助催化剂提高光催化剂的载流子分离效率被认为是一种切实可行的措施。贵金属(Pt,Au等)由于其具有较低的费米能级可以促进光生载流子的分离,而被广泛用于产氢助催化剂。但是,高成本以及地球储量低等原因使其无法广泛应用于实际。磷化铁(FeP),一种过渡金属磷化物,由于其具有出色的电导性和稳定性而被作为一种可以代替贵金属的产氢助催化剂。本专利中,将零维的(0D)的FeP纳米颗粒负载在二维(2D)CdS纳米片上构筑一种0D/2D异质结光催化剂,这种0D/2D异质结不仅仅可以增强0DFeP的分散性,还可以增强2DCdS的光生载流子的分离效率,提高其光催化产氢性能。
发明内容
本发明针对单一的硫化镉光催化产氢性能欠佳的问题,提供了一种0D/2D磷化铁/硫化镉复合材料。
所述的0D/2D磷化铁/硫化镉复合光催化剂指的是一种零维/二维磷化铁/硫化镉复合光催化剂。
本发明采取的技术方案如下:
本发明提供的一种0D/2D磷化铁/硫化镉复合光催化剂,首次采用原位磷化法将0D的磷化铁颗粒负载在2D的硫化镉纳米片上。
硫化镉的质量与磷化铁的质量比为1:0.01~0.1,其中,硫化镉与磷化铁的质量比为1:0.05光催化产氢效果最佳;原位磷化法制备的0D磷化铁纳米颗粒可以与2D硫化镉纳米片基底结合更紧密,构筑了一种0D/2D异质结,加速了光生电子的传输,使得硫化镉中光生载流子可以更加高效的分离,减轻了硫化镉本身的光腐蚀,提高的其光催化产氢活性;同时,磷化铁可以作为光催化产氢活性位点,提高光催化活性。
所述的制备方法具体步骤如下:
(1)将200 mg的2D片状硫化镉超声溶解在去离子水中,形成片状硫化镉水溶液,超声震荡;
(2)在避光条件下,向步骤(1)所得的硫化镉水溶液中分别加入2.3 mL~23.2 mL的2 g/L的Fe(NO3)3·9H2O溶液,搅拌,得混合溶液A;
(3)反应完成后,离心洗涤,收集沉淀物,用去离子水和酒精分别清洗三遍,干燥,将50mg干燥所得沉淀物与500 mg 的NaH2PO2放入瓷舟下半部和上半部,并放入管式炉中煅烧,得到磷化铁/硫化镉复合光催化剂,煅烧时间为2 h,升温速率2 oC/min,保护气为氩气。
步骤(1)中,所述2D片状硫化镉采用水热法合成,具体方法为:将 0.365 gCdCl3·2.5H2O和0.16 g S粉溶解在30 mL二乙烯三胺的溶液中,搅拌2 h后然后倒入50ml聚四氟乙烯内衬的不锈钢反应釜中,在干燥箱80℃条件下保温48小时。之后洗涤、离心,即得片状CdS。
步骤(1)中,超声时间为2~3 h。
步骤(2)中,避光时间为3~4 h。
本发明的有益效果为:
(1)本发明以片状硫化镉为基底,先通过分子间作用力吸附溶液中游离的三价铁离子,在干燥过程中,三价铁离子会结合空气中的氧气形成氢氧化氧铁,然后通过NaH2PO2在300 oC下热分解产生的PH3气体将硫化镉镉表面形成的氢氧化氧铁转化为磷化铁。这种原位生成的磷化铁可以与片状硫化镉结合的更紧密,更有利于光生载流子在界面之间的传输,抑制了光生载流子的复合,也降低了硫化镉的光腐蚀,大大提高了光催化剂的催化活性和催化稳定性。同时,片状的硫化镉可以均匀的吸附三价铁离子,使得磷化铁可以均匀的分布在片状硫化镉表面,抑制了磷化铁颗粒的团聚。
本发明制备0D/2D磷化铁/硫化镉复合光催化剂是一种非均相光催化剂,具有各向异性,电子传输能力强以及高比率暴露活性位点等优点。同时,本发明制备的催化剂具有较高的可见光光响应,可以在大于460 nm波长的光源下被激发。
本发明制备的2D硫化镉与0D磷化铁复合可见光光催化剂可用于光催化产氢领域,能够提供一种有效的清洁能源,且不会造成环境污染,还可以实现太阳能与清洁能源的转化。
本发明的制作工艺简单,生产成本低,材料性能优越,具有较好的应用前景。
附图说明
图1是2D硫化镉纳米片和0D磷化铁纳米颗粒与2D硫化镉纳米片复合可见光光催化剂FeP/CdS-5的XRD图。
图2为0D磷化铁纳米颗粒与2D硫化镉纳米片复合光催化剂中FeP/CdS-5的SEM图。
图3为2D硫化镉纳米片以及0D磷化铁纳米颗粒与2D硫化镉纳米片复合可见光光催化剂的产氢速率图。
具体实施步骤
下面将结合附图和实施例对本发明做进一步的详细说明。
实施例1
将200 mg水热法制备的2D硫化镉纳米片溶于200 mL去离子水中,制成浓度为1 g/L的溶液,在超声机中超声2 h,保持水温在15℃左右。接着加入4.6 mL浓度为2 g/L的Fe(NO3)3·9H2O溶液。在避光条件下反应3 h。反应结束后,溶液静置30min后,倒出上清液,在离心管中分别用去离子水和酒精交替清洗。离心机的转速设置为8000r/min。最后将离心管中清洗好的沉淀放在60℃的烘干箱中干燥15h。将NaH2PO2与所得干燥物按质量比为10:1,分别放入瓷舟上风口和下风口,并置于管式炉中煅烧,煅烧时间为2 h,升温速率2 oC/min,保护气为氩气。所得产物标记为FeP/CdS-2。
实施例2
将200 mg水热法制备的2D硫化镉纳米片溶于200 mL去离子水中,制成浓度为1 g/L的溶液,在超声机中超声2 h,保持水温在15℃左右。接着加入11.6 mL浓度为2 g/L的Fe(NO3)3·9H2O溶液。在避光条件下反应3 h。反应结束后,溶液静置30min后,倒出上清液,在离心管中分别用去离子水和酒精交替清洗。离心机的转速设置为8000r/min。最后将离心管中清洗好的沉淀放在60℃的烘干箱中干燥15h。将NaH2PO2与所得干燥物按质量比为10:1,分别放入瓷舟上风口和下风口,并置于管式炉中煅烧,煅烧时间为2 h,升温速率2 oC/min,保护气为氩气。所得产物标记为FeP/CdS-5。XRD结果如图1所示,电子扫描结果如图2所示。
由图1的2D CdS纳米片与FeP/CdS-5的XRD图可以看出,对于纯硫化镉纳米片来说,在25.52°, 26.76°, 28.42°, 36.81°, 43.89°, 48..28°和51.82°的特征峰分别对应六方晶相CdS的 (100), (002), (101), (102), (110), (103)和(112)晶面。然而在FeP/CdS-5复合材料中并没有发现FeP峰的存在,这是由于FeP的含量较少和结晶度较低导致的。
由图2可以看出,磷化铁纳米颗粒负载在硫化镉纳米片上,证明了磷化铁纳米颗粒与硫化镉纳米片结合紧密,以及0D/2D 磷化铁/硫化镉复合材料的成功合成。
实施例3
将200 mg水热法制备的2D硫化镉纳米片溶于200 mL去离子水中,制成浓度为1 g/L的溶液,在超声机中超声2 h,保持水温在15℃左右。接着加入18.6 mL浓度为2 g/L的Fe(NO3)3·9H2O溶液。在避光条件下反应3 h。反应结束后,溶液静置30 min后,倒出上清液,在离心管中分别用去离子水和酒精交替清洗。离心机的转速设置为8000 r/min。最后将离心管中清洗好的沉淀放在60℃的烘干箱中干燥15h。将NaH2PO2与所得干燥物按质量比为10:1,分别放入瓷舟上风口和下风口,并置于管式炉中煅烧,煅烧时间为2 h,升温速率2 oC/min,保护气为氩气。所得产物标记为FeP/CdS-8。
实施例4
将200 mg水热法制备的2D硫化镉纳米片溶于200 mL去离子水中,制成浓度为1 g/L的溶液,在超声机中超声2 h,保持水温在15℃左右。接着加入23.2 mL浓度为2 g/L的Fe(NO3)3·9H2O溶液。在避光条件下反应3 h。反应结束后,溶液静置30min后,倒出上清液,在离心管中分别用去离子水和酒精交替清洗。离心机的转速设置为8000r/min。最后将离心管中清洗好的沉淀放在60℃的烘干箱中干燥15h。将NaH2PO2与所得干燥物按质量比为10:1,分别放入瓷舟上风口和下风口,并置于管式炉中煅烧,煅烧时间为2 h,升温速率2 oC/min,保护气为氩气。所得产物标记为FeP/CdS-10。
对上述实例所得到的0D/2D磷化铁/硫化镉复合可见光光催化剂进行产氢性能测试:
光催化产氢测试在一个密封的100 mL三口烧瓶中进行,使用300 W的氙灯作为光源,并且配备420 nm的滤光片。称取所制得的上述0D/2D磷化铁/硫化镉复合光催化剂25 mg加入到80 mL 10 vol%的乳酸溶液中,超声溶解10 min。随后,采用氮气置换出三口烧瓶中的空气,置换时间为15 min。然后将反应器置于磁力搅拌器搅拌,转速为200 r/min,并且打开光源。光照1 h后,从反应器中抽取0.4 mL气体注入气相色谱中进行分析,得出产氢量。光催化产氢反应总共进行5 h,并计算出其产氢速率。以纯CdS纳米片作为对照。通过对比发现,0D/2D FeP/CdS复合可见光光催化剂的产氢速率比纯CdS纳米片有了明显的提高。由图3可以看出,其中0D/2D FeP/CdS复合可见光光催化剂中FeP/CdS-5产氢速率达到10.98 mmol/g/h,在各产物中产氢速率最高。可以发现磷化铁与硫化镉复合光催化剂可以改善光催化活性,使产氢速率大幅度提升。是一种较为理想的复合光催化剂。
Claims (6)
1.一种0D/2D磷化铁/硫化镉复合光催化剂,其特征在于,所述的0D/2D磷化铁/硫化镉复合光催化剂是0D磷化铁颗粒附着在2D硫化镉纳米片上,其中磷化铁与硫化镉的质量比为0.01-0.1:1。
2.如权利要求1所述的一种0D/2D磷化铁/硫化镉复合光催化剂的制备方法,其特征在于,具体包括如下步骤:
(1)将200 mg的2D片状硫化镉超声溶解在去离子水中,形成片状硫化镉水溶液,超声震荡;
(2)在避光条件下,向步骤(1)所得的硫化镉水溶液中分别加入2.3 mL~23.2 mL的2 g/L的Fe(NO3)3·9H2O溶液,搅拌,得混合溶液A;
(3)反应完成后,离心洗涤,收集沉淀物,用去离子水和酒精分别清洗三遍,干燥,将50mg干燥所得沉淀物与500 mg 的NaH2PO2放入瓷舟下半部和上半部,并放入管式炉中煅烧,得到磷化铁/硫化镉复合光催化剂,煅烧时间为2 h,升温速率2 oC/min,保护气为氩气。
3.如权利要求2所述的一种0D/2D磷化铁/硫化镉复合光催化剂的制备方法,其特征在于:步骤(1)中,所述2D片状硫化镉采用水热法合成,具体方法为:将0.365 g CdCl3·2.5H2O和0.16 g S粉溶解在30 mL二乙烯三胺的溶液中,搅拌2~3 h后倒入50ml聚四氟乙烯内衬的不锈钢反应釜中,在干燥箱80℃条件下保温48小时之后洗涤、离心,即得片状CdS。
4.如权利要求2所述的一种0D/2D磷化铁/硫化镉复合光催化剂的制备方法,其特征在于:步骤(1)中,超声时间为2~3 h。
5.如权利要求2所述的一种0D/2D磷化铁/硫化镉复合光催化剂的制备方法,其特征在于:步骤(2)中,避光时间为3~4 h。
6.如权利要求2所述的一种0D/2D磷化铁/硫化镉复合光催化剂的制备方法,其特征在于:步骤(3)中,所述干燥温度为60~70℃,干燥时间为8~15h。
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CN114471639A (zh) * | 2022-02-21 | 2022-05-13 | 内蒙古科技大学 | 过渡金属元素掺杂及具有硫空位的硫化镉负载过渡金属磷化物光催化材料及其制备方法 |
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CN114471639A (zh) * | 2022-02-21 | 2022-05-13 | 内蒙古科技大学 | 过渡金属元素掺杂及具有硫空位的硫化镉负载过渡金属磷化物光催化材料及其制备方法 |
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