相转移有机前驱体BiOAc0.6Br0.2I0.2固溶体合成表面富有氧空位的棒状S型Bi4O5I2/Bi4O5Br2异质结

doi:10.1016/S1872-2067(20)63768-8

摘要/Abstract

摘要：

近年来, 卤氧铋(BiOX, X = Cl, Br, I)作为多功能半导体光催化材料, 因其具有独特的层状结构和电子结构, 吸引了广泛关注. 然而, 相对低的导带(CB)和高的价带(VB)位置导致其氧化还原能力弱, 从而限制了其实际应用. 研究表明, 通过富铋策略调控BiOX中元素化学计量比, 可以实现对其能带结构的可控调控. 尽管富铋半导体材料被视为有效的可见光光催化剂的候选材料之一, 但是单一组分的富铋光催化剂不利于光生载流子的分离和迁移. 具有匹配能带结构的富铋基复合光催化剂的构建已被证实可以加速光生电子-空穴对的分离和迁移. 与传统的Ⅱ型异质结构相比, S型异质结既可以有效地分离光生载流子, 又可以增强其氧化还原能力. 如果双富铋基半导体之间能形成S型异质结, 不仅可以拓展可见光响应, 而且还可以增强光生电荷的氧化还原能力. 基于Bi₄O₅I₂和Bi₄O₅Br₂的匹配能带, 制备具有强氧化还原能力的S型Bi₄O₅I₂/Bi₄O₅Br₂异质结是可行的.
除了电子结构外, 表面缺陷的引入也对改善光催化性能起到了重要作用. 氧空位(OVs)作为一种典型的缺陷, 可以捕获电子来抑制光诱导载流子的复合, 并加速这些捕获载流子向吸附剂的转移. 此外, 它们还可以充当有机污染物和分子氧的吸附位点, 促进吸附和降解效率. 目前, 光催化材料中OVs的形成通常需要复杂、苛刻的条件, 如高温、高压、惰性或还原气氛处理等, 因此寻找简便有效的方法生成OVs仍然具有挑战性. 此外, 在无惰性或还原气氛下对有机前驱体进行热处理被认为是形成OVs的有效方法. 鉴于此, 本文通过低温煅烧二维纳米片有机前驱体BiOAc_0.6Br_0.2I_0.2 (Ac ^- = CH₃COO ^-)固溶体, 成功合成了表面富有氧空位的一维纳米棒状的S型Bi₄O₅I₂/Bi₄O₅Br₂异质结(Bi₄O₅I₂/Bi₄O₅Br₂-OV).
X射线衍射、高分辨率透射电子显微镜电子顺磁共振以及X射线光电子能谱分析(XPS)等结果均证实了表面氧空位的存在. 同时, 根据吸收光谱图和肖特基曲线计算出Bi₄O₅I₂和Bi₄O₅Br₂的能带结构, 而且通过XPS价带谱进一步证实了所计算的价带的可靠性. 根据捕获剂实验、氯化硝基四氮唑蓝(NBT)转移以及对苯二甲酸荧光均证实了h ⁺、•OH和•O₂ ^-是参与光催化降解的主要活性物种. 再结合上述能带结构以及活性物种的类型推断出光生载流子的迁移方式将遵循S型机制, 而不是传统的II型异质结. 而且, 通过光电流、阻抗和稳态荧光均证实了表面OVs和S型异质结的协同效应, 有利于提高Bi₄O₅I₂/Bi₄O₅Br₂-OV的光生电子空穴对的分离效率, 并延长其寿命, 从而有效地提高其光催化性能.
在可见光照射下, OVs和S型异质结的协同效应赋予Bi₄O₅I₂/Bi₄O₅Br₂-OV显著的可见光光催化性能, 对抗生素四环素和染料罗丹明B的去除率分别高达90.2%和97.0%, 均高于Bi₄O₅I₂(56.8%和71.8%)、Bi₄O₅Br₂(47.4%和68.4%)、固溶体BiOAc_0.6Br_0.2I_0.2(67.0%和84.0%)以及表面具有低氧空位浓度的Bi₄O₅I₂/Bi₄O₅Br₂-P(30.6%和40.4%). 此外, 在实际废水或电解质存在下, S型Bi₄O₅I₂/Bi₄O₅Br₂-OV异质结仍呈现出优异的光催化性能. 本文不仅为OVs修饰的富铋基异质结的设计提供了有效策略, 也为界面载流子的分离和迁移提供了切实可行的途径.

关键词: 焙烧, 有机基团固溶体, 相变, 氧空位, S型异质结, 光催化

Abstract:

To improve separation efficiency of the photogenerated electron-hole pairs, constructing a heterojunction is considered to be a promising strategy. However, the fabrication of heterojunction via a facile route to achieve a substantial improvement in photocatalytic performance is still challenging. In this work, a well-designed nanosheet-based rodlike step-scheme (S-scheme) heterojunction Bi₄O₅I₂/Bi₄O₅Br₂ with rich oxygen vacancies (OVs) (Bi₄O₅I₂/Bi₄O₅Br₂-OV) was easily synthesized by calcining BiOAc_0.6Br_0.2I_0.2 (Ac ^- = CH₃COO ^-) precursor. The as-prepared Bi₄O₅I₂/Bi₄O₅Br₂-OV exhibited excellent visible light photocatalytic performance towards antibiotic tetracycline (TC) and dye rhodamine B (RhB) degradation and removal rate reached 90.2% and 97.0% within 120 min, respectively, which was higher than those of Bi₄O₅I₂-OV (56.8% and 71.8%), Bi₄O₅Br₂-OV (47.4% and 68.4%), solid solution BiOAc_0.6Br_0.2I_0.2 (67.0% and 84.0%) and Bi₄O₅I₂/Bi₄O₅Br₂ with poor oxygen vacancies (Bi₄O₅I₂/Bi₄O₅Br₂-P) (30.6% and 40.4%). Owing to the release of heat and generation of reducing carbon during calcining the precursor with Ac ^-, it could not only reduce the generation temperature of Bi-rich bismuth oxyhalides, which thus decreased particle size and increased surface areas, but also introduce surface OVs, which could trap photoelectrons and inhibit the recombination of carriers. In addition, the calcination of single solid solution precursor benefited to the formation of well-alloyed interfaces with larger contact areas between 2D/2D nanosheet-like materials, which facilitates charge carriers transfer at the interfaces. The Bi₄O₅I₂/Bi₄O₅Br₂-OV also shows the desirable removal rate for TC and RhB in actual wastewater or in the presence of some electrolytes. This study provides an effective and simple strategy for designing OVs modified Bi-rich oxyhalides heterojunctions.

Key words: Calcination, Organic group-based solid solution, Phase transformation, Oxygen vacancy, S-scheme heterojunction, Photocatalysis

贾雪梅, 沈紫晨, 韩巧凤, 毕慧平. 相转移有机前驱体BiOAc_0.6Br_0.2I_0.2固溶体合成表面富有氧空位的棒状S型Bi₄O₅I₂/Bi₄O₅Br₂异质结[J]. 催化学报, 2022, 43(2): 288-302.

Xuemei Jia, Zichen Shen, Qiaofeng Han, Huiping Bi. Rod-like Bi₄O₅I₂/Bi₄O₅Br₂ step-scheme heterostructure with oxygen vacancies synthesized by calcining the solid solution containing organic group[J]. Chinese Journal of Catalysis, 2022, 43(2): 288-302.

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图/表 11

Fig. 1. Schematic illustration of the synthetic procedures of Bi4O5I2, Bi4O5Br2, Bi4O5I2/Bi4O5Br2-OV and Bi4O5I2/Bi4O5Br2-P.

Fig. 2. XRD patterns of calcinated products of different precursors (a) and BiOAc0.6I0.2Br0.2at different temperatures (b).

Fig. 3. SEM and TEM images of Bi4O5I2/Bi4O5Br2-P (a,c,e) and Bi4O5I2/Bi4O5Br2-OV (b,d,f); STEM image of Bi4O5I2/Bi4O5Br2-OV and the corresponding EDX elemental mapping of Bi, O, I and Br (g).

Fig. 4. The high-resolution XPS spectra Bi 4f (a) and O 1s (b) of Bi4O5I2/Bi4O5Br2-OV and Bi4O5I2/Bi4O5Br2-P; (c) EPR spectra for the as-obtained samples; (d) The production of •O2- by the as-obtained samples detected by the NBT method under visible light.

Fig. 5. (a) UV-vis diffuse reflectance spectra of the as-prepared samples, and the plots of the (ahv)1/2 vs. photon energy (hv) of Bi4O5Br2-OV and Bi4O5I2-OV (inset); Mott-Schottky plots (b) and valence band XPS spectra (c) of Bi4O5Br2-OV and Bi4O5I2-OV; (d) The energy band structures of the samples before and after calcination.

Fig. 6. Photocatalytic activities (a,c), and the corresponding reaction rate constants kapp (b,d) for the as-obtained photocatalysts for TC (a,b) and RhB (c,d) degradation under visible light (λ > 420 nm), and the insets in (b) and (d) showing the corresponding simulated kinetic curves.

Table 1 Comparison of degradation efficiency (DE) of TC and RhB over different photocatalysts.

Sample	Pollutant (mg/L)	Dosage (g/L)	t (min)	Light source	DE (%)	Ref.
Bi_mO_nBr_z Bi₄O₅Br₂ Bi₄O₅I₂-Bi₅O₇I Bi₇O₉I₃-OVR Bi_xO_yI_z/g-C₃N₄ Bi₄O₅I₂/Bi₄O₅Br₂-OV BiOCl/Bi₂₄O₃₁Cl₁₀ Bi₄O₅I₂-Bi₅O₇I BiOI/BiOAc	20 ^a 30 ^a 10 ^a 20 ^a 10 ^a 20 ^a 10 ^b 10 ^b 5 ^b 10 ^b 10 ^b	1.0 0.6 1.0 0.6 1.0 0.4 1.0 1.0 0.4	120 120 240 40 240 120 40 240 80	400W halogen 1000 W Xe 500 W Xe 300 W Xe 500 W Xe 500 W Xe 500 W Xe 500 W Xe 500 W Xe	98.9 75.0 78.0 70.0 40.0 90.2 98.1 79.0 96.0	[41] [12] [37] [34] [42] This work [43] [37] [44]
Bi₇O₉I₃-OVR Bi₄O₅I₂/Bi₄O₅Br₂-OV		0.4 0.4	60 120	300 W Xe 500W Xe	85.0 97.0	[34] This work

Fig. 7. (a) Effect of initial pH on photocatalytic degradation of TC and RhB on Bi4O5I2/Bi4O5Br2-OV; (b) Point of zero charge of Bi4O5I2/Bi4O5Br2-OV; Effect of (c) water sources and (d) electrolytes on the degradation of TC and RhB on Bi4O5I2/Bi4O5Br2-OV.

Fig. 8. (a) Cycling runs of Bi4O5I2/Bi4O5Br2-OV for the degradation of TC and RhB under visible light (λ > 420 nm) and (b) XRD patterns of fresh and used Bi4O5I2/Bi4O5Br2-OV.

Fig. 9. (a) Influence of different scavengers on the degradation of TC and RhB on Bi4O5I2/Bi4O5Br2-OV heterostructures; (b) Nitro blue tetrazolium (NBT) transformation efficiency and (c) fluorescence spectra of TAOH in Bi4O5I2/Bi4O5Br2-OV photocatalytic system under visible light irradiation; (d-f) Schematic illustration of heterostructure: (d) before contact, (e) after contact in darkness and (f) photogenerated charge carrier transfer process in S-scheme heterojunction under illumination.

Fig. 10. Transient photocurrent response of (a) the as-prepared samples and (b) heterojunction Bi4O5I2/Bi4O5Br2-OV and Bi4O5I2/Bi4O5Br2-P with or without K2S2O8; (c) EIS Nyquist plots of the as-prepared samples and the proposed equivalent circuit (insets); (d) PL spectra of as-prepared Bi4O5I2, Bi4O5Br2 and Bi4O5I2/Bi4O5Br2-OV samples.

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相转移有机前驱体BiOAc_0.6Br_0.2I_0.2固溶体合成表面富有氧空位的棒状S型Bi₄O₅I₂/Bi₄O₅Br₂异质结

Rod-like Bi₄O₅I₂/Bi₄O₅Br₂ step-scheme heterostructure with oxygen vacancies synthesized by calcining the solid solution containing organic group

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