CN114602482B - 一种铋层结构压电异质结催化剂及其制备方法 - Google Patents
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Abstract
一种铋层结构压电异质结催化剂及其制备方法,属于光催化技术领域。通过熔盐法制备高质量片状NBT粉体,进而通过液相还原法将纳米级的Cu颗粒附着在具有铁电性质的NBT光催化剂表面,得到一种具有高催化性能的新型催化剂。该催化剂制备方法简单,成本低廉,重现性好,催化活性高,在污染物催化降解等领域具有广阔的应用前景。
Description
技术领域
本发明属于光催化技术领域,具体涉及一种用于降解有机物的铋层结构压电异质结催化剂及其制备方法。
背景技术
在工业技术迅速发展的大背景下,水污染问题日益严重,如何治理水污染成为各国政府、学术界乃至广大公众所共同关注的问题。在现有的众多物理化学方法中,利用太阳光的光催化技术,具有无毒、绿色、环保的优点,拥有广阔的发展前景。然而,目前报道的许多光催化剂由于光吸收范围窄、黑暗中无响应、电子-空穴复合严重等问题,光催化效率很低。为了提高光催化效率,大量的研究投入在调整材料的能带结构、掺杂和异质结构的形成。然而由于光诱导载体复合的时间短,导致电子和空穴在开始催化过程之前就已复合,光催化活性受到阻碍,因此仍然存在稳定性差、量子效率低的问题。近年来,人们发现将铁电/压电材料与光催化相结合有望开发出催化性能更高的催化剂,是一种很有前景的技术。
Na0.5Bi4.5Ti4O15(NBT)是一种重要的铋层状无铅铁电材料。其具有独特的(Bi2O2)2+层和(A3B4O13)2-交错的带电层结构,使材料沿c轴方向形成了层间内建电场。此外,阴离子层基团中金属-氧键会产生非零偶极矩使得材料具有极性,晶体沿偶极矩方向定向生长时非零偶极矩累积形成自发极化,使得能带弯曲,抑制电子-空穴对的复合。同时,(Bi2O2)2+层容易产生氧空位,具有良好的光吸收性质,能够提高剩余极化和导电率,促进电子-空穴对的分离。因此,同时具有铁电性以及光电性质的NBT能够用于催化有机物的降解,但单独的NBT催化效率只能达到40%。
在本发明中,我们首次将具有铁电性的NBT与Cu纳米粒子复合,制备出一种新型铋层结构的NBT@Cu压电异质结催化剂,该催化剂具有优异的光催化性能。
发明内容
本发明提供了一种具有高催化活性的铋层结构NBT@Cu压电异质结催化剂及其制备方法。为实现上述目的,本发明采取以下技术方案:
该催化剂的化学组成为:NBT@x wt.%Cu,x的数值为5~30(对应Cu的含量),进一步优选金属Cu的含量为20wt.%。
本发明上述具有高催化性能的铋层结构复合材料催化剂的制备方法为熔盐法与液相还原法。具体包括以下步骤:
(1)NBT片状粉体通过熔盐法制备;首先,按照NBT的摩尔元素比例称量原料Na2CO3、Bi2O3、TiO2,同时称量熔盐NaCl和KCl,均烘干,其中NBT原料:熔盐的质量比为1:20%,NaCl:KCl的摩尔比1:1;随后,以无水乙醇为介质通过行星式球磨机球磨10~12h,然后100℃条件下烘干;干燥的混合物在850℃保温4h煅烧,煅烧后的粉体用去离子水洗涤8~10次,然后100℃条件下烘干以获得NBT片状粉体;
(2)通过液相还原法在NBT表面附着纳米Cu颗粒;将NBT粉体与Cu(Ac)2·H2O混合后,加入去离子水搅拌,随后加入柠檬酸溶液,继续搅拌;在再加入氨水及NaOH溶液,将溶液水浴加热至40℃保持10min,再加入水合肼溶液,待溶液由深蓝色变成黄棕色后,继续搅拌30min,静置2h倒掉上清液,用去离子水和乙醇溶液洗涤3~5次,随后烘干得到目标压电异质结粉体。
进一步优选每1gNBT粉体对应加入20ml去离子、5ml浓度0.1M的柠檬酸溶液、0.5ml质量浓度25%NH3·H2O、5ml浓度2M NaOH溶液、5ml质量浓度1.6%水合肼溶液。
将得到目标压电异质结粉体在光照加搅拌的条件下降解甲基橙溶液,进行催化性能测试。所述的光为紫外可见光,如对应的功率为300W的氙灯,甲基橙的浓度为10mg/L,每100ml甲基橙溶液中加入0.1g压电异质结粉体。
其中,最佳样品组成为:NBT@20wt%Cu,其降解甲基橙溶液的降解率可达到96%。
在本发明中,NBT@Cu压电异质结催化剂的制备方法简单,耗时短,成本低廉,重现性好,具有典型的片层状结构,催化活性高,是潜在的应用于污染物催化降解的高效催化剂。
附图说明
图1为NBT@Cu压电异质结催化剂的XRD图。
图2为NBT@Cu压电异质结催化剂的SEM图。
图3为NBT@Cu压电异质结催化剂的降解效率图。
具体实施方式
下面通过实施例进一步阐明本发明的实质性特点和显著优点。应该指出,本发明决非仅局限于所陈述的实施例。
实施例1:
按化学式NBT@5wt.%Cu称量出1g的NBT和Cu(Ac)2·H2O,放于100ml的烧杯中,加入20ml去离子水搅拌10min,随后加入5ml,0.1M的柠檬酸,继续搅拌10min。再加入0.5mlNH3·H2O(25%)及5ml NaOH(2M)溶液,将溶液水浴加热至40℃保持10min。再加入5ml水合肼溶液(1.6%),待溶液由深蓝色变成黄棕色后,继续搅拌30min,静置2h倒掉上清液,用去离子水和乙醇溶液洗涤3~5次,随后置于40℃烘箱烘干得到目标复合材料。
实施例2:
按化学式NBT@10wt.%Cu称量称量出NBT和Cu(Ac)2·H2O,其它同实施例1。
实施例3:
按化学式NBT@15wt.%Cu称量称量出NBT和Cu(Ac)2·H2O,其它同实施例1。
实施例4:
按化学式NBT@20wt.%Cu称量称量出NBT和Cu(Ac)2·H2O,其它同实施例1。
实施例5:
按化学式NBT@25wt.%Cu称量称量出NBT和Cu(Ac)2·H2O,其它同实施例1。
实施例6:
按化学式NBT@30wt.%Cu称量出NBT和Cu(Ac)2·H2O,其它同实施例1。
表1上述实施例性能对比表
。
Claims (7)
1.一种铋层结构压电异质结催化剂,其特征在于,该催化剂的化学组成为:NBT@xwt.%Cu,x的数值为5~30;
其制备方法,包括以下步骤:
包括以下步骤:(1)NBT片状粉体通过熔盐法制备;首先,按照NBT的摩尔元素比例称量原料Na2CO3、Bi2O3、TiO2,同时称量熔盐NaCl和KCl,均烘干,其中NBT原料:熔盐的质量比为1:20%,NaCl:KCl的摩尔比1:1;随后,以无水乙醇为介质通过行星式球磨机球磨10~12h,然后100℃条件下烘干;干燥的混合物在850℃保温4h煅烧,煅烧后的粉体用去离子水洗涤8~10次,然后100℃条件下烘干以获得NBT片状粉体;
(2)通过液相还原法在NBT表面附着纳米Cu颗粒;将NBT粉体与Cu(Ac)2·H2O混合后,加入去离子水搅拌,随后加入柠檬酸溶液,继续搅拌;在再加入氨水及NaOH溶液,将溶液水浴加热至40℃保持10min,再加入水合肼溶液,待溶液由深蓝色变成黄棕色后,继续搅拌30min,静置2h倒掉上清液,用去离子水和乙醇溶液洗涤3~5次,随后烘干得到目标压电异质结粉体。
2.按照权利要求1所述的一种铋层结构压电异质结催化剂,其特征在于,金属Cu的含量为20wt.%。
3.权利要求1或2所述的一种铋层结构压电异质结催化剂的制备方法,其特征在于,包括以下步骤:(1)NBT片状粉体通过熔盐法制备;首先,按照NBT的摩尔元素比例称量原料Na2CO3、Bi2O3、TiO2,同时称量熔盐NaCl和KCl,均烘干,其中NBT原料:熔盐的质量比为1:20%,NaCl:KCl的摩尔比1:1;随后,以无水乙醇为介质通过行星式球磨机球磨10~12h,然后100℃条件下烘干;干燥的混合物在850℃保温4h煅烧,煅烧后的粉体用去离子水洗涤8~10次,然后100℃条件下烘干以获得NBT片状粉体;
(2)通过液相还原法在NBT表面附着纳米Cu颗粒;将NBT粉体与Cu(Ac)2·H2O混合后,加入去离子水搅拌,随后加入柠檬酸溶液,继续搅拌;在再加入氨水及NaOH溶液,将溶液水浴加热至40℃保持10min,再加入水合肼溶液,待溶液由深蓝色变成黄棕色后,继续搅拌30min,静置2h倒掉上清液,用去离子水和乙醇溶液洗涤3~5次,随后烘干得到目标压电异质结粉体。
4.按照权利要求3所述的制备方法,其特征在于,每1gNBT粉体对应加入20ml去离子、5ml浓度0.1M的柠檬酸溶液、0.5ml质量浓度25%NH3·H2O、5ml浓度2M NaOH溶液、5ml质量浓度1.6%水合肼溶液。
5.利要求1或2所述的一种铋层结构压电异质结催化剂的应用,在光照加搅拌的条件下降解甲基橙溶液。
6.按照权利要求5所述的应用,所述的光为紫外可见光,甲基橙的浓度为10mg/L,每100ml甲基橙溶液中加入0.1g压电异质结粉体。
7.按照权利要求5所述的应用,NBT@20wt%Cu,其降解甲基橙溶液的降解率可达到96%。
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