现代化工

现代化工 ›› 2025, Vol. 45 ›› Issue (8) : 111-116. DOI: 10.16606/j.cnki.issn0253-4320.2025.08.021

科研与开发

AgI/BiOI复合材料的制备及其光催化性能研究

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Preparation of AgI/BiOI composite material and study on its photocatalytic properties

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文章历史 +

Received		Published
2024-11-04		2025-08-20
Issue Date	Revised Date
2025-08-15	2024-11-04

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摘要

采用简单的离子交换法制备了Z型AgI/BiOI异质结光催化剂,通过XRD、SEM、TEM、UV-Vis DRS和PL等手段对其结构和形貌等进行了表征分析,并考察了可见光下这些光催化剂对土霉素(OTC)的光降解性能。结果表明,在可见光照射 150 min后,S2光催化剂(AgI占AgI/BiOI摩尔百分比为50%)对OTC的降解效果最佳,OTC去除率为76.1%,高于单一AgI或BiOI的降解效果。此外,S2光催化剂在5次光降解循环使用后对OTC的去除率并未明显下降,显示良好的循环稳定性。AgI/BiOI复合材料光催化活性的增强源于AgI和BiOI之间形成了Z型异质结,使体系中载流子实现了有效的分离。

Abstract

Z-type AgI/BiOI heterojunction photocatalysts are prepared via a simple ion exchange method,and their structure and morphology are characterized by means of XRD,SEM,TEM,UV-Vis DRS,and PL techniques.The photodegradation performance of the AgI/BiOI photocatalysts to oxytetracycline is examined under visible light.It is shown that after 150 min of visible light irradiation,the S2 photocatalyst (the molar percentage of AgI in AgI/BiOI is 50%) has the best degradation effect on oxytetracycline,delivering a removal efficiency of 76.1%,higher than that AgI or BiOI alone does.In addition,the removal efficiency of oxytetracycline by the S2 photocatalyst does not decrease significantly after five cycles of photocatalytic degradation,indicating a good cycling stability.The enhanced photocatalytic activity of AgI/BiOI composite is due to the formation of a Z-type heterojunction between AgI and BiOI,which enables charge carriers in the system to separate effectively.

Graphical abstract

关键词

AgI / 土霉素 / 降解 / 可见光 / BiOI

Key words

AgI / oxytetracycline / degradation / visible light / BiOI

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tenantId=1226480274814496768, journalId=1226484258170171394, articleId=1240720110505128461, xref=null, ext=[AuthorCompanyExt(id=1241416396225082249, tenantId=1226480274814496768, journalId=1226484258170171394, articleId=1240720110505128461, companyId=1241416396220887944, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Department of Chemistry and Chemical Engineering, Taiyuan Institute of Technology, Taiyuan 030008, China), AuthorCompanyExt(id=1241416396229276554, tenantId=1226480274814496768, journalId=1226484258170171394, articleId=1240720110505128461, companyId=1241416396220887944, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=太原工业学院化学与化工系,山西太原 030008)])])] 唐建可,马春蕾,康燕,薛彦峰. AgI/BiOI复合材料的制备及其光催化性能研究[J]. 现代化工, 2025, 45(8): 111-116 DOI:10.16606/j.cnki.issn0253-4320.2025.08.021

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四环素类抗生素(TCs)是目前世界上应用最广泛的抗生素之一^[1-2],在临床医学以及牲畜业中发挥着重要作用。但医疗行业过量使用或畜牧业未被动物有效代谢的四环素未得到有效处理而通过生活、生产废水排入生态系统,成为影响人类健康安全和生态可持续发展而迫在眉睫需要解决的问题。土霉素是一种常用的四环素类抗生素,对含土霉素废水的降解具有现实意义。

光催化降解技术凭借操作简单、反应温和、成本低、对目标降解物无选择性等优势,成为降解水体有机污染物的一种有效手段。碘氧化铋(BiOI)是一种p型半导体材料,其特殊的层状结构、合适的禁带宽度、较高的化学稳定性和催化活性,使其成为光催化领域研究的热点。但是由于其内部电子-空穴对的快速复合,使其表现出较低的量子效率和较高的载流子复合率,进而限制了单一BiOI的实际应用,而通过构建异质结是一种非常有效的提升其半导体光催化性能的方法^[3-4]。异质结形式通常包括Ⅱ型、p-n型、Z型等,其中,构建Z型异质结光催化体系对于实现污染物高效降解具有一定的优势,它能将电子和空穴在不同半导体材料上实现空间分离,最大程度地保留较低还原电势电子和较高氧化电势空穴,增强体系氧化还原能力,从而提高单一半导体光催化活性^[5-7]。AgI的价带位置和BiOI的导带位置相近,两者具备构成Z型异质结的条件^[8]。

本研究针对单一BiOI可见光降解活性有限的问题,采用简易离子交换法制备Z型AgI/BiOI异质结光催化剂,有效提升BiOI可见光降解活性。利用不同的表征手段对AgI/BiOI进行表征分析,并将其用于可见光下土霉素的光降解以研究其光催化活性,最后提出AgI/BiOI复合材料光催化活性提升的机理。

1 实验部分

1.1 BiOI的制备

在15 mL乙二醇中加入0.97 g Bi(NO₃)₃·5H₂O,超声处理10 min,在室温搅拌下向上述体系中匀速滴加15 mL的KI水溶液(含0.332 g KI),滴加完成后在室温下继续搅拌反应1 h,随后再离心、水洗、醇洗,在60℃烘箱中下干燥10 h^[9]。

1.2 AgI/BiOI的制备

通过简易离子交换法制备AgI/BiOI复合材料。室温搅拌下将一定量的AgNO₃加入100 mL乙二醇中形成溶液A,随后向A溶液中加入0.35 g BiOI固体,超声处理5 min,继续搅拌反应5 h,离心收集样品,水洗、醇洗,60℃下干燥10 h。通过改变AgNO₃的加入量,制得AgI占AgI/BiOI复合物摩尔百分比分别为25%、50%和75%的复合材料,分别标记为S1、S2和S3。

1.3 表征

采用X射线衍射仪(XRD,Rigaku SmartLab型)、扫描电子显微镜(SEM,JEOL JSM-7200F型)、X射线能谱仪(EDS,NORAN System 7型)、透射电子显微镜(TEM,JEOL JEM-2100F型)、X射线光电子能谱仪(XPS,ESCALAB 250Ⅺ型)、紫外-可见近红外分光光度计(UV-VIS-NIR,岛津UV-3600型)对样品的晶体结构、微观形貌、表面元素组成、光吸收性能进行表征;采用荧光光谱仪(PL,Hitachi F-7000型)在325 nm的激发波长下获得样品光致发光光谱;采用电子顺磁共振波谱仪(ESR,Bruker A300型)测试光催化过程中产生的自由基。

1.4 光催化降解土霉素测试

在可见光(300 W氙灯,420 nm截止滤光片过滤紫外光)条件下,对AgI、BiOI和AgI/BiOI复合材料降解土霉素的光催化活性进行测试。将40 mg的5种光催化剂分别以超声分散于100 mL土霉素(20 mg/L)溶液中,随后在黑暗中连续搅拌30 min,保证光催化剂和待降解物达到吸附-解吸平衡。打开光源,每隔30 min取出3 mL反应液,离心后取上清液,用分光光度计测其吸光度来分析土霉素浓度以得到去除率数据。

2 结果与讨论

2.1 催化剂表征分析

2.1.1 XRD分析

样品AgI、BiOI、S1、S2和S3的XRD谱图如图1所示。AgI的XRD谱图显示为立方相γ-AgI(JCPDS No.09-0399)和六方相β-AgI(JCPDS No.09-0374)的混相,位于22.3°的衍射峰对应为β-AgI的(100)晶面。BiOI的衍射峰均与四方相BiOI(JCPDS No.73-2062)相对应。在S1、S2和S3的XRD谱图中,BiOI和AgI的特征峰共存,随着AgI/BiOI复合材料中BiOI含量的下降,29.7°和31.7°处对应的BiOI衍射峰强度也逐渐减弱。3种AgI/BiOI复合材料均未出现杂质峰,表明在制备过程中没有产生与Bi或I相关的杂质。

2.1.2 SEM、EDS及TEM分析

用扫描电子显微镜对BiOI、AgI、S1、S2和S3样品形貌进行观察,如图2所示。BiOI为纳米片组装成的类球形结构,AgI为类球状颗粒。在AgI/BiOI复合材料中,AgI分布在BiOI上,复合材料保留了BiOI微球结构,并且分布在BiOI表面的AgI相较于单一AgI的尺寸明显减小。随着复合材料中AgI含量增加,BiOI表面颗粒状物质也逐渐增多。如图3所示,S2的EDS谱图中出现了O、Bi、Ag和I元素,进一步表明经离子交换法得到了AgI/BiOI复合材料。S2的TEM和HRTEM图如图4所示。图4(a)中红色椭圆圈住的为AgI颗粒,表明AgI分布在BiOI上;图4(b)中0.282 nm的晶格间距对应于BiOI的(110)晶面,0.375 nm晶格间距对应于β-AgI的(002)晶面和γ-AgI的(111)晶面,以上结果表明成功制备了AgI/BiOI异质结光催化剂。

2.1.3 XPS分析

图5为S2的XPS谱图。从全谱图中观察到Bi、Ag、O和I元素在S2复合材料中共存。Bi 4f谱图中位于159.1 eV和164.4 eV的峰分别对应Bi 4f_7/2和Bi 4f_5/2。Ag 3d谱图中368.3 eV和374.3 eV处出现的2个峰,各自对应Ag 3d_5/2和Ag 3d_3/2轨道。I 3d谱图中2个峰值619.2 eV和630.7 eV分别对应I 3d_5/2和I 3d_3/2。O 1s经过拟合的谱图,在530.0 eV和532.1 eV出现了2个峰,分别对应BiOI中Bi—O键和S2表面吸附的羟基中氧。

2.1.4 UV-Vis DRS分析

图6为AgI、BiOI、S1、S2和S3的UV-Vis DRS谱图。AgI在450 nm以下的可见光区域有良好的吸收能力,BiOI在可见光区域的吸收能力有明显提升。S1、S2和S3复合材料在可见光区域的吸收能力介于AgI和BiOI之间,表明它们均可用作可见光催化剂。禁带宽度(E_g)可由下式计算得出^[10-11]:

α h ν = A (h ν - E g) n / 2

式中,α为吸收系数,h为普朗克常数,ν为光频率,A为常数,n取决于光学跃迁类型,AgI跃迁方式为直接跃迁,对应的n值为1^[12]。通过对紫外-可见漫反射光谱数据处理后得到AgI的E_g,以能量(hν)为横坐标,(αhν)²为纵坐标作图,图中切线与X轴交点即为AgI的E_g,具体见图7,数值为2.77 eV。BiOI的禁带宽度在本课题组之前报道中做过计算,为1.76 eV^[13]。

2.1.5 PL分析

光催化剂光生载流子能否有效分离是决定其光催化性能的重要因素之一。荧光光谱(PL)是研究光催化剂的光生电子和空穴的复合几率高低的一个重要途径。图8给出了AgI、BiOI、S1、S2和S3的荧光光谱,激发波长为325 nm。未观测到BiOI的荧光发射峰,因为BiOI属于间接跃迁半导体,被激发的电子有可能通过热辐射或其他方式返回了基态^[14-15]。AgI的荧光发射峰强度最高,远高于3种AgI/BiOI复合材料,表明与AgI相比,AgI/BiOI复合材料电子和空穴的复合明显受到抑制。

2.2 光催化性能分析

AgI、BiOI、S1、S2和S3对OTC进行光催化降解的时间-去除率曲线如图9(a)所示。在可见光照射150 min后,AgI与BiOI对OTC的去除率分别为64.1%和39.9%。与AgI和BiOI相比,AgI/BiOI复合材料表现出更高的OTC去除率,其中S2对OTC去除率最高,达76.1%。AgI/BiOI复合材料相比于单一AgI和BiOI具有更高的载流子分离效率,因此具有更高的光催化活性。将不同光催化剂降解OTC过程进行拟合,得到图9(b)所示的一级反应动力学曲线。AgI、BiOI、S1、S2和S3光催化剂的反应动力学常数(k)分别为0.007 4、0.001 6、0.007 8、0.008 8 min^-1和0.007 9 min^-1,其中S2的k值最大,同样表明S2具有最高的光催化活性。

2.3 光催化剂的循环使用性能分析

通过对OTC进行5次光降解来评估S2光催化剂的循环使用性能,结果如图10(a)所示。在5次循环使用后,S2对OTC的去除率并未出现明显的下降,表明S2光催化剂具有良好的稳定性。进一步对比了S2在光催化循环实验前后的XRD谱图,具体见图10(b),发现循环实验结束后其XRD谱图并无明显变化,同样表明S2具有良好的循环稳定性。

2.4 光催化机理分析

通过自由基捕获实验研究S2对OTC的光降解过程起主要作用的活性物质,具体结果见图11。当添加EDTA-2Na或苯醌(BQ)时,可以观察到OTC的去除率显著降低,表明空穴(h⁺)和超氧自由基($\cdot \text O_{2}^{-}$)共同参与了OTC的光降解反应,h⁺在OTC光降解中起更关键的作用。加入异丙醇(IPA)对OTC的降解几乎无影响,说明在OTC降解过程中无羟基自由基(·OH)参与反应。通过电子顺磁共振(ESR)法来验证S2光催化体系是否产生了$\cdot \text O_{2}^{-}$,具体见图12。发现在黑暗条件下没有DMPO-$\cdot \text O_{2}^{-}$信号,在可见光照射20 min后出现了明显的DMPO-$\cdot \text O_{2}^{-}$信号,表明光照条件下S2体系确实产生了$\cdot \text O_{2}^{-}$。

AgI的价带值(E_VB)和导带值(E_CB)可通过E_VB=X-E^c+0.5E_g和E_CB=E_VB-E_g进行计算^[16]。X为半导体的绝对电负性,AgI的X值为5.35 eV^[17-18],E^c是氢谱的自由电子能(约4.5 eV)。算得AgI的E_VB和E_CB分别为2.24 eV和-0.53 eV。BiOI能带位置在本课题组先前报道中做过计算,其E_VB和E_CB分别为2.32 eV和0.56 eV^[13]。如图13(a)所示,若AgI/BiOI复合材料符合传统Ⅱ型载流子转移机制,AgI导带电子转移至BiOI导带,BiOI导带值大于O₂/$\cdot \text O_{2}^{-}$的氧化还原电势,因此BiOI导带电子不会和O₂发生反应,体系不能产生$\cdot \text O_{2}^{-}$,这与自由基捕获实验结论相矛盾。

图13(b)为Z型载流子转移机制。AgI价带位置和BiOI导带位置较为接近,可见光激发后AgI价带空穴和BiOI导带电子发生快速复合,实现了AgI/BiOI体系电子和空穴的有效分离。AgI导带电子可以与溶解氧反应生成$\cdot \text O_{2}^{-}$,BiOI价带空穴直接OTC的降解。以上过程证明, $\cdot \text O_{2}^{-}$和h⁺共同参与了OTC的光降解反应。

3 结论

在制得BiOI基础上,通过离子交换法得到AgI/BiOI复合材料(光催化剂)。AgI/BiOI复合光催化剂对OTC具有较好的降解活性,降解过程符合伪一级动力学模型。其中样品S2具有最高的光催化活性,在可见光照射150 min后,对OTC的去除率为76.1%,高于单一AgI和BiOI。在经过5次光降解循环后,S2对OTC的去除率下降并不明显,表明S2光催化剂稳定性良好。自由基捕获实验表明h⁺和 $\cdot \text O_{2}^{-}$共同参与了OTC的光降解反应。AgI/BiOI光催化剂活性的提升源于负载AgI和BiOI之间形成了Z型异质结,实现了体系电子和空穴的有效分离。

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