CN111905715A - 一种等离子体诱导Bi2MoO6光催化剂的制备方法 - Google Patents
一种等离子体诱导Bi2MoO6光催化剂的制备方法 Download PDFInfo
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- 229910002900 Bi2MoO6 Inorganic materials 0.000 claims abstract description 31
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- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 7
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- 229910015667 MoO4 Inorganic materials 0.000 abstract 1
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 abstract 1
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Abstract
本发明公开了一种等离子体诱导Bi2MoO6光催化剂的制备方法。该光催化剂微观形貌为纳米片组装而成的团簇结构,团簇结构直径800 nm–1000 nm;其制备步骤如下:1.将五水合硝酸铋(Bi(NO3)3·5H2O)、十六烷基三甲基溴化铵(CTAB)与二水合钼酸钠(Na2MoO4·2H2O)搅拌混合成混合液;2.将混合液转入水热釜反应,水洗醇洗烘干后,得到团簇结构的Bi2MoO6材料;3.将团簇结构的Bi2MoO6放入乙醇中,机械搅拌至均匀分散,并在石英片上烘干固定后放入Ar/H2混合气氛围中进行等离子体处理,得到含BiO2‑x 纳米粒子的Bi2MoO6团簇结构材料。所制备的材料扩大了光催化剂光吸收的范围、促进了光生载流子的分离、提高了催化剂的稳定性,因此得到更广泛的利用。
Description
技术领域
本发明涉及光催化剂,特指一种可控的等离子体诱导Bi2MoO6光催化剂及其制备方法,属于光催化材料的制备方法技术领域。
背景技术
Bi2MoO6作为一种Aurivillius相氧化物半导体材料,不仅具有合适的禁带宽度来有效利用可见光,而且具有优异的物理化学性质,如:较好的化学和热稳定性、优异的光电性能等。因此,Bi2MoO6被广泛应用于固氮、光催化CO2还原及可见光下降解有机污染物领域。然而,对于普通的Bi2MoO6存在与CO2之间的亲和力较弱、电子–空穴分离效率低等缺点,这严重限制了其在光催化领域的应用。因此需要设计合理的能带结构、电子结构适宜,且具有较大的比表面积和光吸收范围来提升其吸附CO2能力、选择性和催化效率。现有的光催化剂改性方法主要有形貌调控、缺陷调控、贵金属沉积和半导体复合等。近年来出现的利用等离子体对光催化剂进行表面缺陷调控可以大大提高催化剂催化性能。
等离子体指部分或完全电离的气体,且自由电子和离子所带正、负电荷的总和完全抵消,宏观上呈现电中性。根据等离子体的温度可以划分成高温等离子体(热核聚变等离子)和低温等离子体。低温等离子体又包括热等离子体(等离子体弧、等离子体炬等)和冷等离子体(低气压交直流、射频、微波等离子体以及高气压介质阻挡放电、电晕放电、RF放电等)。低温冷等离子体中存在着大量的活性粒子,能够和所接触的材料表面发生反应,因此它们被用来对材料表面进行改性处理.。
介质阻挡放电(DBD)是有绝缘介质插入放电空间的一种非平衡态气体放电又称介质阻挡电晕放电或无声放电。介质阻挡放电能够在高气压和很宽的频率范围内工作,通常能够在常压下产生等离子体,电源频率可从50 Hz至1M Hz。介质阻挡放电等离子体处理光催化剂具有处理条件温和、反应时间短、能耗低等特点。
发明内容
本发明的目的在于提供一种可控的等离子体诱导Bi2MoO6光催化剂的制备方法,并用于CO2光催化还原研究。该方法首先通过水热的方法得到形貌规整的纳米片团簇,再通过等离子体诱导得到这种形貌很好的Bi2MoO6纳米团簇。利用Bi2MoO6纳米团簇结构本身的特性,解决现有光催化剂对可见光利用率不高、载流子分离效率低等问题。
为实现上述目的,本发明采用如下技术方案:
一种等离子体诱导Bi2MoO6光催化剂的制备方法,先通过水热的方法得到形貌规整的Bi2MoO6纳米片团簇,再通过等离子体诱导得到Bi2MoO6纳米团簇。
在上述的制备方法中,具体包括如下步骤:
(1)称取Bi(NO3)3·5H2O和CTAB超声溶于去离子水和乙二醇混合溶液中,然后再加入Na2MoO4·2H2O搅拌;
(2)将混合溶液转移进高压反应釜中,接着将高压釜放进烘箱中,并加热反应;将所得到的产物收集并用去离子水和无水乙醇洗涤数次,在真空干燥后得到Bi2MoO6纳米片组成的簇状物;
(3)称取Bi2MoO6纳米片簇状物,放入乙醇机械搅拌均匀分散,并在石英片上烘干固定,然后将石英片放入放电反应器中,采用介质阻挡放电(DBD)的形式产生等离子体处理Bi2MoO6。
作为优选的,在上述制备方法中:所述步骤(1)的Bi(NO3)3·5H2O、CTAB和Na2MoO4·2H2O的摩尔比为1~2 : 0. 137~0. 274 : 0. 5~1;去离子水和乙二醇的体积比1~2 : 0.32~0.64;所述的搅拌的时间为40~80 min。
作为优选的,在上述制备方法中:所述步骤(2)的加热温度为100~140℃,反应时间为20~26 h;真空干燥温度为70℃,真空干燥的时间为12 h。
作为优选的,在上述制备方法中:所述步骤(3)的等离子处理的功率为50~200 W;处理时间为5–15 min,气流速为200 mL min-1,气体为Ar/H2(v/v,95%/5%)混合气。
本发明所得到的等离子体诱导Bi2MoO6光催化剂的团簇结构不仅由纳米片构成,团簇的表面还均匀分布了BiO2-x 纳米粒子。团簇结构的直径为800 nm–1000 nm,BiO2-x 纳米粒子的大小为5 nm–10 nm。通过等离子体不同处理时间调节该材料生成BiO2-x 纳米粒子的含量,随着等离子体处理时间的延长,其CO2还原性能也随之发生改变。
与现有技术相比,本发明具有如下有益效果:本发明制备的等离子体诱导后的Bi2MoO6与普通的Bi2MoO6相比,具有很高的量子效率及低的电子复合率,并具有更高的光催化降解效率。其次本发明的可控的等离子体诱导Bi2MoO6的制备方法简单易行、产量高、操作简单、重复性好、可控性强、合成条件温和以及材料性状稳定。
附图说明
图1为本发明制备的可控的等离子体诱导Bi2MoO6的XRD图谱;
图2为本发明制备的可控的等离子体诱导Bi2MoO6的SEM、HRTEM图;
图3为本发明制备的可控的等离子体诱导Bi2MoO6的UV–vis图谱;
图4为本发明制备的可控的等离子体诱导Bi2MoO6的PL图谱;
图5为本发明制备的可控的等离子体诱导Bi2MoO6光催化剂不同等离子体处理时间下光催化还原CO2活性对比图。
具体实施方式
下面结合附图对本发明作进一步详细地阐述,而不是限制本发明。
下述实施例中使用的实验方法如无特殊说明,均为常规方法。
下述实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。
实施例1:
制备Bi2MoO6纳米片团簇:将2 mmol的Bi(NO3)3·5H2O和0.1 g的CTAB加入40 mL去离子水和40 mL乙二醇混合溶液中,然后再加入1 mmol的Na2MoO4·2H2O,常温磁力搅拌分散,得到混合分散液。在搅拌60 min后,将混合溶液转移进100 mL的聚四氟乙烯内衬的高压反应釜中,待反应釜自然冷却至室温,并静置后12000 r/min下离心3 min,然后将所得到的产物收集并用去离子水和乙醇各洗涤三次,在60℃下真空干燥后得到Bi2MoO6纳米片团簇。
将50 mg Bi2MoO6超薄纳米片簇状物放入乙醇机械搅拌均匀分散,并在石英片上烘干固定,然后将石英片放入放电反应器中,采用介质阻挡放电(DBD)的形式产生等离子体处理Bi2MoO6。开始放电前,需要先将石英反应器抽真空,然后充入Ar/H2(v/v,95%/5%)混合气作为反应气体,气流速保持在200 mL min-1。整个等离子体处理过程在室温下进行,放电装置维持50 W的输入功率,处理时间为5 min,即得到1–Bi2MoO6。
实施例2:
制备Bi2MoO6纳米片团簇:将2 mmol的Bi(NO3)3·5H2O和0.1 g的CTAB加入40 mL去离子水和40 mL乙二醇混合溶液中,然后再加入1 mmol的Na2MoO4·2H2O,常温磁力搅拌分散,得到混合分散液。在搅拌60 min后,将混合溶液转移进100 mL的聚四氟乙烯内衬的高压反应釜中,待反应釜自然冷却至室温,并静置后12000 r/min下离心3 min,然后将所得到的产物收集并用去离子水和乙醇各洗涤三次,在60℃下真空干燥后得到Bi2MoO6纳米片团簇。
将50 mg Bi2MoO6超薄纳米片簇状物放入乙醇机械搅拌均匀分散,并在石英片上烘干固定,然后将石英片放入放电反应器中,采用介质阻挡放电(DBD)的形式产生等离子体处理Bi2MoO6。开始放电前,需要先将石英反应器抽真空,然后充入Ar/H2(v/v,95%/5%)混合气作为反应气体,气流速保持在200 mL min-1。整个等离子体处理过程在室温下进行,放电装置维持50 W的输入功率,处理时间为10 min,即得到2–Bi2MoO6。
实施例3:
制备Bi2MoO6纳米片团簇:将2 mmol的Bi(NO3)3·5H2O和0.1 g的CTAB加入40 mL去离子水和40 mL乙二醇混合溶液中,然后再加入1 mmol的Na2MoO4·2H2O,常温磁力搅拌分散,得到混合分散液。在搅拌60 min后,将混合溶液转移进100 mL的聚四氟乙烯内衬的高压反应釜中,待反应釜自然冷却至室温,并静置后12000 r/min下离心3 min,然后将所得到的产物收集并用去离子水和乙醇各洗涤三次,在60℃下真空干燥后得到Bi2MoO6纳米片团簇。
将50 mg Bi2MoO6超薄纳米片簇状物放入乙醇机械搅拌均匀分散,并在石英片上烘干固定,然后将石英片放入放电反应器中,采用介质阻挡放电(DBD)的形式产生等离子体处理Bi2MoO6。开始放电前,需要先将石英反应器抽真空,然后充入Ar/H2(v/v,95%/5%)混合气作为反应气体,气流速保持在200 mL min-1。整个等离子体处理过程在室温下进行,放电装置维持50 W的输入功率,处理时间为15 min,即得到3–Bi2MoO6。
通过上述实施例分析,我们对相同质量的Bi2MoO6超薄纳米片簇状物,以相同的电功率在氩氢混合气氛下进行不同时间的等离子体处理,发现对催化剂进行10 min等离子体处理(实施例2),其催化效果最佳。
制备的Bi2MoO6的结构测试是在Bruker D8 AdvanceX射线衍射仪上进行的(Cu–Kα射线,λ=1.5418 Å,范围是10°–80°,扫描速度为7°min-1),通过X射线晶体衍射(XRD)表征所制备的光催化剂的相结构。由图1可知,原始Bi2MoO6的XRD衍射图谱中的衍射峰,分别对应于Bi2MoO6的标准卡片(JDPS:77–1246)中的晶面,说明了经过水热法合成的光催化剂为Bi2MoO6。同时,经Ar/H2等离子体处理后的2–Bi2MoO6的衍射峰没有出现Bi2MoO6的标准衍射峰外的其他峰,说明Ar/H2等离子体处理未能对Bi2MoO6光催化剂结构产生影响,但同时也未能显现出BiO2-x 的衍射峰,这可能是由于BiO2-x 的含量低于XRD的检出限,同时Bi2MoO6的衍射峰和BiO2-x 比较接近,掩盖了衍射峰。
使用JEOL JEM–2010型透射电镜(电压为10 kV,Japan)与FEI Tecnai–F20型透射电镜(电压为200 kV,USA)进行光催化剂形貌和尺寸的测定。图2为本实施例所制备出的可控的等离子体诱导Bi2MoO6光催化剂的扫描电镜和高倍透射电镜图片。从图2可以清晰的看出,所制备出的样品的确是一种簇团结构以及BiO2-x 纳米粒子在团簇结构上的均匀分布。另外,簇团结构的直径大约为800 nm–1000 nm。
使用紫外可见分光光度计(Shimadzu UV–2450,Japan)获得光催化剂的紫外–可见光吸收光谱(UV–vis)图。由图3可以看出,Ar/H2等离子体处理对于增加Bi2MoO6在可见光段的吸收有着显著的作用。
使用QuantaMaster和TimeMaster光谱荧光计获得了光致发光(PL)光谱图。由图4可知,等离子体处理后的Bi2MoO6光生电子–空穴的分离效率明显提高。
光催化活性测试:在光反应系统(Labsolar–6A,PerfectLight,Beijing)上进行合成样品的光催化CO2还原的实验。
实施例4:称取10 mg催化剂置于配好的溶液中(6 mL乙腈,4 mL去离子水,2 mL三乙醇胺),超声3 min使其溶解充分,进而在温度为10°C,压强为0.75 MPa的CO2气氛环境中,以300 W氙灯(PLS–SXE 300C(BF),Perfectlight)下照射进行光催化CO2反应
图5为本实施例所制备出的可控的等离子体诱导Bi2MoO6光催化剂在不同等离子体处理时间下光催化还原CO2活性图。由图5可知,Ar/H2等离子体处理有效提升了Bi2MoO6光催化还原CO2产CO的性能,其中,最高活性的光催化剂是经过Ar/H2等离子体处理10 min后所得到的。
以上所揭露的仅为本发明的较佳实施例而已,当然不能以此来限定本发明之权利范围,因此依本发明权利要求所作的等同变化,仍属于本发明所涵盖的范围。
Claims (5)
1.一种等离子体诱导Bi2MoO6光催化剂的制备方法,其特征在于:先通过水热的方法得到形貌规整的Bi2MoO6纳米片团簇,再通过等离子体诱导得到Bi2MoO6纳米团簇。
2.如权利要求1所述的制备方法,其特征在于:包括如下步骤:
(1)称取Bi(NO3)3·5H2O和CTAB超声溶于去离子水和乙二醇混合溶液中,然后再加入Na2MoO4·2H2O搅拌;
(2)将混合溶液转移进高压反应釜中,接着将高压釜放进烘箱中,并加热反应;将所得到的产物收集并用去离子水和无水乙醇洗涤数次,在真空干燥后得到Bi2MoO6纳米片组成的簇状物;
(3)称取Bi2MoO6纳米片簇状物,放入乙醇机械搅拌均匀分散,并在石英片上烘干固定,然后将石英片放入放电反应器中,采用介质阻挡放电的形式产生等离子体处理Bi2MoO6。
3.如权利要求2所述的制备方法,其特征在于:所述步骤(1)的Bi(NO3)3·5H2O、CTAB和Na2MoO4·2H2O的摩尔比为1~2 : 0. 137~0. 274 : 0. 5~1;去离子水和乙二醇的体积比1~2 : 0.32~0.64;所述搅拌的时间为40~80 min。
4.如权利要求2所述的制备方法,其特征在于:所述步骤(2)的加热温度为100~140℃,反应时间为20~26 h;真空干燥温度为70℃,真空干燥的时间为12 h。
5.如权利要求2所述的制备方法,其特征在于:所述步骤(3)的等离子处理的功率为50~200 W;处理时间为5–15 min,气流速为200 mL min-1,气体为Ar/H2混合气。
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