Cu1.94S-SnS纳米异质结的合成及其光催化降解研究

doi:10.6023/A23030090

化学学报 ›› 2023, Vol. 81 ›› Issue (7): 725-734.DOI: 10.6023/A23030090 上一篇下一篇

研究论文

Cu_1.94S-SnS纳米异质结的合成及其光催化降解研究

刘嘉文^a^,^b^,^c, 林玮璜^a^,^b^,^c, 王惟嘉^c^,^d, 郭学益^a^,^b^,^c^,^*(), 杨英^a^,^b^,^c^,^*()

a 中南大学冶金与环境学院长沙 410083
b 中南大学有色金属资源循环利用湖南省重点实验室长沙 410083
c 中南大学有色金属资源循环利用国家地方联合工程中心长沙 410083
d 海南医学院第二附属医院临床医学研究所海口 570311

投稿日期:2023-03-27 发布日期:2023-05-23
基金资助:
湖南省自然科学基金(2022JJ30757); 清远市创新创业科研团队项目(2018001); 广东省科技计划(2018B030323010); 国家自然科学基金(52262040); 海南省自然科学基金(821QN411)

Synthesis and Photocatalytic Degradation of Cu_1.94S-SnS Nano-heterojunction

Jiawen Liu^a^,^b^,^c, Weihuang Lin^a^,^b^,^c, Weijia Wang^c^,^d, Xueyi Guo^a^,^b^,^c(), Ying Yang^a^,^b^,^c()

a School of Metallurgy and Environment, Central South University, Changsha 410083
b Hunan Key Laboratory of Nonferrous Metal Resources Recycling, Central South University, Changsha 410083
c National & Regional Joint Engineering Research Center of Nonferrous Metal Resources Recycling, Changsha 410083
d Institute of Clinical Medicine (ICM), the Second Affiliated Hospital of Hainan Medical University, Haikou 570311

Received:2023-03-27 Published:2023-05-23
Contact: *E-mail: xyguo@csu.edu.cn; muyicaoyang@csu.edu.cn
Supported by:
Natural Science Foundation of Hunan Province(2022JJ30757); Qingyuan Innovation and Entrepreneurship Research Team Project(2018001); Science and Technology Program of Guangdong Province(2018B030323010); National Natural Science Foundation of China(52262040); Natural Science Foundation of Hainan Province, China(821QN411)

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1. Supporting Information-A23030090.pdf(228KB)

摘要/Abstract

为提高光催化降解有害染料的活性, 采用热注入-阳离子交换法合成了Cu_1.94S-SnS单颗粒纳米异质结构材料. 探究在不同温度下(80, 120和160 ℃), Sn^2＋作为客体离子进行阳离子部分交换所得产物的差异. 通过高分辨率透射电子显微镜(HRTRM)图像、高角度环形暗场扫描透射电子显微镜(HAADF-STEM)图像、扫描透射电子显微镜能量色散光谱(STEM-EDS)、X射线衍射和X射线光电子能谱仪等分析手段对样品进行表征. 紫外-可见-近红外吸收光谱表明, 合成的Cu_1.94S-SnS纳米异质结构在可见光范围内具有更高的光吸收度. 通过光催化降解亚甲基蓝和四环素, 对产物的光催化性能进行表征, 发现异质结结构有效提高了单一硫化物的光催化活性, 亚甲基蓝(MB)的光降解率从56%(母体材料Cu_1.94S)提高到98% (Cu_1.94S-SnS纳米异质结), 四环素(TC)的光降解速率也提高了约5倍, 合成的异质结结构具有更高的光催化活性.

关键词: 硫化铜, 硫化锡, 纳米异质结构, 亚甲基蓝, 光催化

In this study, Cu_1.94S-SnS nano-heterostructures were synthesized using the methods of thermal injection-cation exchange to enhance the activity of photocatalytic degradation of hazardous dyes. First, we stirred and mixed octadecene, oleylamine and copper chloride under argon atmosphere and raised the temperature to 180 ℃ for 15 min. The precursor of Cu_1.94S was cooled to 140 ℃, and then tert-dodecanethiol (t-DDT) was added. This solution was rapidly raised to 180 ℃ for 30 min, and then cooled in ice water to obtain the product of Cu_1.94S. Similarly, tin chloride and oleylamine were mixed under argon atmosphere and raised to 160 ℃ for 30 min, then cooled to 80, 120 and 160 ℃, respectively. The Cu_1.94S and tri-n-octylphosphine suspensions were injected into the precursor solution to react for 30 min. The samples were characterized using various analytical techniques, including high-resolution transmission electron microscopy (HRTEM), high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) images, STEM energy-dispersive spectroscopy (STEM-EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS). At lower temperatures (80 and 120 ℃), sheet-like Cu_1.94S-SnS single-particle nano-heterojunctions were obtained with size of about 57 nm. In contrast, regular shaped heterojunctions could not be obtained at a high temperature (160 ℃). The Uv-visible near infrared spectrophotometer (UV-Vis-NIR) absorption spectra revealed that the synthesized Cu_1.94S-SnS nano-heterostructures exhibited higher light absorption in the visible range. Photocatalytic degradation of methylene blue and tetracycline was used to evaluate the photocatalytic performance of the products. The results showed that the heterostructure effectively improved the photocatalytic activity of the parent material. Specifically, the photodegradation rate of methylene blue (MB) increased from 56% (parent material Cu_1.94S) to 98% (Cu_1.94S-SnS nano-heterojunction), indicating a significant enhancement in photocatalytic activity. And the photodegradation rate of tetracycline (TC) was also increased by about 5 times. Overall, the synthesized Cu_1.94S-SnS heterostructures possessed superior photocatalytic activity, which could be attributed to the effective charge sep-aration and improved light absorption properties. This study provided a new approach to the design and fabrication of efficient photocatalytic materials for environmental remediation.

Key words: Cu_1.94S, SnS, nano-heterojunction, methylene blue, photocatalysis

引用此文

刘嘉文, 林玮璜, 王惟嘉, 郭学益, 杨英. Cu_1.94S-SnS纳米异质结的合成及其光催化降解研究[J]. 化学学报, 2023, 81(7): 725-734.

Jiawen Liu, Weihuang Lin, Weijia Wang, Xueyi Guo, Ying Yang. Synthesis and Photocatalytic Degradation of Cu_1.94S-SnS Nano-heterojunction[J]. Acta Chimica Sinica, 2023, 81(7): 725-734.

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图/表 13

图1. Cu1.94S纳米颗粒和不同温度下(80, 120和160 ℃)进行Sn2＋部分交换的产物XRD图谱

Figure 1. X-ray diffraction patterns of Cu1.94S and nanoparticles of Sn2＋cation half-exchange at 80, 120 and 160 ℃

图2. (a1) Cu1.94S和(b1) 80, (c1) 120, (d1) 160 ℃温度点下进行部分交换的纳米颗粒的TEM图像; (a2) Cu1.94S和(b2) 80, (c2) 120, (d2) 160 ℃温度下部分交换产物对应的HRTEM图; (a3) Cu1.94S和(b3) 80, (c3) 120, (d3) 160 ℃温度下部分交换产物对应的FFT模式; (a4) Cu1.94S和(b4) 80, (c4) 120, (d4) 160 ℃温度下部分交换产物对应的粒径尺寸分布直方图

Figure 2. TEM images of (a1) Cu1.94S and products with semi-exchange at (b1) 80, (c1) 120, (d1) 160 ℃; HRTEM images of (a2) Cu1.94S and products with semi-exchange at (b2) 80, (c2) 120, (d2) 160 ℃; FFT mode of (a3) Cu1.94S and products with semi-exchange at (b3) 80, (c3) 120, (d3) 160 ℃ and grain size distribution of (a4) Cu1.94S and products with semi-exchange at (b4) 80, (c4) 120, (d4) 160 ℃

图3. (a)六方密堆积Cu1.94S的晶体结构; (b) Cu1.94S的(080)面的阴离子排列; (c)正交SnS的晶体结构; (d) SnS的(021)面的阴离子排列

Figure 3. (a) Crystal structure of hexagonal dense stacked Cu1.94S; (b) anion alignment for (080) crystal plane of Cu1.94S; (c) crystal structure of orthogonal SnS and (d) anion alignment for (021) crystal plane of SnS

图4. 分别在(a) 80, (b) 120和(c) 160 ℃下进行Sn阳离子部分交换的产物的HAADF-STEM图像和STEM-EDS元素图及对应的EDS线扫图谱

Figure 4. HAADF-STEM images, STEM-EDS images and EDS of products by partial cation exchange at (a) 80, (b) 120 and (c) 160 ℃

图5. 80和120 ℃温度下通过阳离子部分交换过程形成的Cu1.94S-SnS的示意图

Figure 5. Diagram of Cu1.94S-SnS formed by partial exchange of cations at 80 and 120 ℃

图6. (a) Cu1.94S以及在不同交换温度下阳离子交换后的产物的XPS光谱; (b~d) Cu 2p, Sn 3d和S 2p的高分辨率XPS光谱(HR-XPS)

Figure 6. (a) XPS survey spectra of Cu1.94S and products by partial exchange at different temperatures; (b~d) HR-XPS of Cu 2p, Sn 3d and S 2p

图7. Cu1.94S以及在80, 120, 160 ℃下部分交换后的产物的(a) UV-Vis-NIR吸收光谱图和(b) TAUC图

Figure 7. (a) UV-Vis-NIR absorption spectra and (b) TAUC of Cu1.94S and products with semi-exchange at 80, 120, 160 ℃

图8. 在(25±1) ℃下用氙灯(模拟太阳光)照射下不同材料光催化降解MB水溶液的UV-Vis吸收光谱图. (a) 20 mg (120 ℃下) Cu1.94S-SnS催化剂及2 mL的H2O2; (b) 20 mg的Cu1.94S催化剂及2 mL的H2O2; (c)仅2 mL的H2O2; (d) 20 mg (80 ℃下) Cu1.94S-SnS催化剂及2 mL的H2O2; (e) 20 mg (160 ℃下) SnS催化剂及2 mL的H2O2; (f) 20 mg Cu1.94S催化剂无H2O2

Figure 8. UV-Vis absorption spectra of aqueous solutions of different materials for the photocatalytic degradation of MB under irradiation with a xenon lamp (simulated sunlight) at (25±1) ℃. (a) 20 mg Cu1.94S-SnS catalyst and 2 mL of H2O2 at 120 ℃; (b) 20 mg Cu1.94S catalyst and 2 mL of H2O2; (c) 2 mL of H2O2 only; (d) 20 mg Cu1.94S-SnS catalyst and 2 mL of H2O2 at 80 ℃; (e) 20 mg SnS catalyst and 2 mL of H2O2 at 160 ℃; (f) 20 mg Cu1.94S catalyst without H2O2

图9. (a)在(25±1) ℃模拟太阳光照射下, 不同催化剂的溶液中的MB归一化浓度(来自664 nm处的吸光度测量数据)与时间的关系图; (b)模拟太阳光照射下Cu1.94S-SnS催化剂的光生电荷转移机制和光催化机理示意图

Figure 9. (a) Plot of MB normalized concentration (from absorbance measurements at 664 nm) versus time in solution for the different catalysts under simulated sunlight at (25±1) ℃; (b) schematic diagram of the photogenerated charge transfer mechanism and photocatalytic mechanism of the Cu1.94S-SnS catalyst under xenon lamp (simulated sunlight) radiation

材料	χ	E_g/eV	E_CB/eV	E_VB/eV
Cu_1.94S	5.01	2.52	－0.76	1.76
SnS	5.17	1.44	－0.05	1.39

表1. Cu1.94S和SnS的CB和VB电位的计算

Table 1. Calculation of the CB and VB potentials of Cu1.94S and SnS

图10. 在(25±1) ℃模拟太阳光照射下(a) 120 ℃下部分交换的Cu1.94S-SnS催化剂降解MB的循环实验; (b)各催化剂对TC溶液的光催化降解; (c) 不同催化剂的溶液中TC归一化浓度与时间的关系图; (d) 120 ℃下部分交换的Cu1.94S-SnS催化剂降解TC的循环实验

Figure 10. Under irradiation with a xenon lamp (simulated sunlight) at (25±1) ℃. (a) stability test of 120 ℃ Cu1.94S-SnS catalyst for photocatalytic degradation of MB; (b) degradation of TC over the prepared photocatalyst; (c) plot of TC-normalized concentration versus time in solutions with different catalysts; (d) recycle of 120 ℃ Cu1.94S-SnS catalyst for photocatalytic degradation of TC

图11. Cu1.94S, Cu1.94S-SnS和SnS催化剂的EIS光谱

Figure 11. EIS spectra of Cu1.94S, Cu1.94S-SnS and SnS catalysts

材料	光源	辐照时间/min		参考文献
Cu_1.94S-SnS	300 W氙灯(AM 1.5G)	60	98	当前工作
Cu掺杂ZnO/SnS	150 W氙灯(AM 1.5G)	120	97.2	[46]
ZTPG	紫外光(60 W, 365 nm)	90	98.1	[42]
Cu_2-_xS-DE复合物	500 W氙灯	40	99.1	[39]
Cu@CuS	300 W氙灯	200	90.6	[7]
UiO-66/g-C₃N₄	350 W氙灯	240	100	[47]

表2. 纳米复合材料降解MB的光催化效率比较

Table 2. Comparison of the photocatalytic efficiency of different materials for the degradation of MB

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Cu_1.94S-SnS纳米异质结的合成及其光催化降解研究

Synthesis and Photocatalytic Degradation of Cu_1.94S-SnS Nano-heterojunction

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Cu1.94S-SnS纳米异质结的合成及其光催化降解研究

Synthesis and Photocatalytic Degradation of Cu1.94S-SnS Nano-heterojunction

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Cu_1.94S-SnS纳米异质结的合成及其光催化降解研究

Synthesis and Photocatalytic Degradation of Cu_1.94S-SnS Nano-heterojunction