铁基非晶条带催化降解性能的退火晶化调控机理

余秀冬; 刘海顺; 薛琳; 张响; 杨卫明

doi:10.7498/aps.73.20240249

摘要

非晶合金是原子结构长程无序的亚稳态材料, 具有优异的催化降解性能, 同时也很容易发生晶化, 但晶化对催化降解性能的影响机理目前尚不明确. 本文研究了退火晶化对Fe-Si-B-Cu-Nb工业非晶条带微观结构及其对酸性橙7催化降解性能的影响. 研究发现: 经460—580 ℃退火后, 条带的催化降解性能大幅下降, 其反应速率常数低于0.01 min^–1, α-Fe析出相导致其非晶结构的破坏, 降低了羟基自由基的形成速率; 而经过650—700 ℃退火后, 条带的催化降解性能显著提高, 反应速率可提升至退火前的3.77倍, 降解15 min时的脱色率达99.22%, 为退火前的1.12倍, 催化降解性能的提高得益于晶化相与金属化合物间的原电池效应及富集Cu团簇和零价铁之间的置换反应. 本研究揭示了退火晶化对偶氮染料的铁基非晶条带催化降解性能的作用机理, 为利用老化的铁基非晶工业条带处理印染废水、实现“以废治废”, 提供了有益的理论与实验支撑.

关键词:

Abstract

Amorphous alloys are meta-stable materials with long-range disordered atomic structure, which have excellent catalytic degradation performance and are also susceptible to crystallization, but the mechanism of the effect of crystallization on their catalytic properties has not been clarified. Therefore, the effect of the annealing crystallization process on the microstructure of Fe-Si-B-Cu-Nb industrial amorphous ribbons and their catalytic degradation properties for acid orange 7 are investigated in this work. It is found that the catalytic degradation performance of the ribbons decreases dramatically after having been annealed at 460–580 ℃ , and its reaction rate constant is less than 0.01 min^–1. The main reason is the formation of α-Fe precipitation phase in the ribbons after having been annealed at high temperatures and the destruction of the substable amorphous structure. These reduce the rate of hydroxyl radical formation. In contrast, the catalytic degradation performance of the 650–700 ℃ annealed ribbons increases significantly, which increases to 3.77 times the degradation rate of the as-cast ribbons. The decolorization rate of acid orange 7 by the annealed ribbons reaches 99.22% within 15 min, which is 1.12 times that of the as-cast ribbons. The improvement of the catalytic degradation performance is attributed to the primary cell effect between the crystalline phase and the metal compounds and the substitution reaction between the Cu-enriched clusters and zero-valent iron. In this study, the influence mechanism of annealing crystallization on the performance of Fe-Si-B-Cu-Nb industrial amorphous ribbons for degrading azo dyes is revealed, which provides theoretical and experimental support for using aged iron-based amorphous ribbons to purify printing and dyeing waste-water and achieve “purification of waste-water by using alloy waste”.

Keywords:

作者及机构信息

1.
中国矿业大学材料与物理学院, 徐州　221116

2.
河海大学力学与材料学院, 南京　210098

3.
中国矿业大学力学与土木工程学院, 徐州　221116

通信作者: 刘海顺, Liuhaishun@cumt.edu.cn

基金项目: 国家自然科学基金(批准号: 52371167)、江苏省科研创新计划(批准号: KYCX23_2653)和中国矿业大学硕士生“杰出人才”助力计划(批准号: 2023WLJCRCZL272)资助的课题.

Authors and contacts

1.
School of Materials and Physics, China University of Mining and Technology, Xuzhou 221116, China

2.
School of Mechanics and Materials, Hohai University, Nanjing 210098, China

3.
School of Mechanics and Civil Engineering, China University of Mining and Technology, Xuzhou 221116, China

Corresponding author: Liu Hai-Shun, Liuhaishun@cumt.edu.cn

Funds: Project supported by the National Natural Science Foundation of China (Grant No. 52371167), the Scientific Research and Innovation Program of Jiangsu Province, China (Grant No. KYCX23_2653), and the China University of Mining and Technology Master’s Degree “Distinguished Talent”Booster Program (Grant No. 2023WLJCRCZL272).

文章全文 : translate this paragraph

参考文献

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[10]	邵梓桥, 毕恒昌, 谢骁, 万能, 孙立涛 2018 67 167802 Google Scholar Shao Z Q, Bi H C, Xie R, Wan N, Sun L T 2018 Acta Phys. Sin. 67 167802 Google Scholar
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[13]	Zuo M Q, Yi S H, Choi J 2021 J. Environ. Sci. 105 116 Google Scholar
[14]	Miao F, Wang Q Q, Di S Y, Yun L, Zhou J, Shen B L 2020 J. Mater. Sci. Technol. 53 163 Google Scholar
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[22]	Hou L, Wang Q Q, Fan X D, Miao F, Yang W M, Shen B L 2019 New J. Chem. 43 6126 Google Scholar
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[26]	Lassoued A, Li J F 2023 J. Phys. Chem. Solids 180 111475 Google Scholar
[27]	Yang W M, Wang Q Q, Li W Y, Xue L, Liu H S, Zhou J, Mo J Y, Shen B L 2019 Mat. Design 161 136 Google Scholar
[28]	Zheng K L, Qin X D, Zhu Z W, Zheng S J, Li H L, Fu H M, Zhang H F 2020 J. Mat. Chem. A 8 10855 Google Scholar
[29]	Luo X K, Li R, Zong J Y, Zhang Y, Li H F, Zhang T 2014 Appl. Surf. Sci. 305 314 Google Scholar
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施引文献

图 1 Fe-Si-B-Cu-Nb工业条带的(a) XRD和(b) DSC图谱

Fig. 1. (a) XRD spectrum and (b) DSC spectrum of Fe-Si-B-Cu-Nb industrial ribbon.

下载: 全尺寸图片幻灯片

图 2 Fe-Si-B-Cu-Nb工业条带不同温度退火后的XRD图谱

Fig. 2. XRD patterns of Fe-Si-B-Cu-Nb industrial ribbons after annealing at different temperatures.

下载: 全尺寸图片幻灯片

图 3 工业非晶条带及其经不同温度退火20 min后降解酸性橙7的紫外光谱图　(a) 工业非晶条带; (b) 460℃; (c) 520 ℃; (d) 580 ℃; (e) 650 ℃; (f) 700 ℃

Fig. 3. UV spectra of industrial amorphous ribbons and their degraded acid orange 7 after annealing at different temperatures for 20 min: (a) Industrial amorphous ribbon; (b) 460℃; (c) 520 ℃; (d) 580 ℃; (e) 650 ℃; (f) 700 ℃.

下载: 全尺寸图片幻灯片

图 4 Fe-Si-B-Cu-Nb工业非晶条带及其经不同温度退火后对酸性橙7的降解　(a) C_t/C₀归一曲线; (b)染料脱色率; (c) －ln函数; (d)反应速率常数柱状图

Fig. 4. Degradation of acid orange II processed by Fe-Si-B-Cu-Nb industrial amorphous ribbons in the as-cast state and after different annealing temperatures: (a) C_t/C₀ normalized graph; (b) dye decolorization rate graph; (c) variation of the －ln function graph; (d) histogram of reaction rate constants.

下载: 全尺寸图片幻灯片

图 5 不同温度退火条带降解酸性橙7后的表面SEM图　(a)—(d)未退火; (e)—(h) 580 ℃退火; (i)—(l) 700 ℃退火

Fig. 5. SEM images of the alloy surface after degrading the acid orange II: (a)–(d) As-cast alloys without annealing; (e)–(h) after annealing at 580 ℃; (i)–(l) after annealing at 700 ℃.

下载: 全尺寸图片幻灯片

图 6 700 ℃退火20 min后条带表面(a) SEM图像及对应的(b) Cu, (c) O, (d) C, (e) Fe和(f) Si元素分布图像

Fig. 6. SEM images of Fe-Si-B-Cu-Nb alloy after annealing at 700 ℃ for 20 min (a); the corresponding elemental distribution maps of (b) Cu, (c) O, (d) C, (e) Fe, and (f) Si.

下载: 全尺寸图片幻灯片

表 1 用于偶氮染料催化降解的典型非晶合金比较

Table 1. Comparison of typical amorphous alloys for catalytic degradation of azo dyes.

合金成分	样品状态	染料种类	反应速率常数(k_obs)	循环次数	参考文献
Fe₈₃Si₅B₈P₄	条带	亚甲基蓝	0.514	—	[13]
(Fe₇₈Si₉B₁₃)₉₉Zr₁	条带	亚甲基蓝	0.24	—	[14]
Fe₈₄B₁₆	条带	直接蓝6	0.110	—	[16]
Fe₇₈Si₉B₁₃	条带	甲基蓝	0.085	—	[17]
Fe₇₈Si₁₁B₉P₂	条带	酸性橙7	0.082	17	[20]
Fe₈₀P₁₃C₇	条带	亚甲基蓝	0.56	23	[21]
Cu₄₆Zr_44.5Al_7.5Gd₂	条带	酸性橙7	0.48	80	[28]
Mg₆₅Cu₂₅Y₁₀	粉末	直接蓝6	0.585	—	[29]
Co₆₅Mo₁₅B₂₀	非晶丝	直接蓝6	2.31	20	[30]
Cu_47.5Zr₄₆Al_6.5	条带	酸性橙7	0.165	10	[31]
Co₇₈Si₈B₁₄	粉末	酸性橙7	—	8	[32]
FeSiBCuNb	条带	酸性橙7	0.094	50	本工作
FeSiBCuNb (700℃退火后)	条带	酸性橙7	0.36	—	本工作

下载: 导出CSV

表 2 α-Fe晶粒尺寸计算结果

Table 2. Calculation results of α-Fe grain size.

	温度/℃
	460	520	580	650	700
β_hkl/(°)	0.80	0.71	0.66	0.27	0.21
D_hkl/nm	11.54	12.68	13.72	33.74	42.52
(hkl)	(220)	(220)	(220)	(220)	(220)

下载: 导出CSV

map

[1]	杨卫明, 刘海顺, 敦超超, 赵玉成, 窦林名 2012 61 106802 Google Scholar Yang W M, Liu H S, Dun C C, Zhao Y C, Dou L M 2012 Acta Phys. Sin. 61 106802 Google Scholar
[2]	柳延辉 2017 66 176106 Google Scholar Liu Y H 2017 Acta Phys. Sin. 66 176106 Google Scholar
[3]	柯海波, 蒲朕, 张培, 张鹏国, 徐宏扬, 黄火根, 刘天伟, 王英敏 2017 66 176104 Google Scholar Ke H B, Pu Z, Zhang P, Zhang P G, Xu H Y, Huang H G, Liu T W, Wang Y M, 2017 Acta Phys. Sin. 66 176104 Google Scholar
[4]	Lai L M, Liu T H, Cai X H, Wang M, Zhang S B, Chen W, Guo S F 2021 Scripta Mater 203 114095 Google Scholar
[5]	孙奕韬, 王超, 吕玉苗, 胡远超, 罗鹏, 刘明, 咸海杰, 赵德乾, 丁大伟, 孙保安, 潘明祥, 闻平, 白海洋, 柳延辉, 汪卫华 2018 67 126101 Google Scholar Sun Y T, Wang C, Lu Y M, Hu Y C, Luo P, Liu M, Xian H J, Zhao D Q, Ding D W, Sun B A, Pan M X, Wen P, Bai H Y, Liu Y H, Wang W H 2018 Acta Phys. Sin. 67 126101 Google Scholar
[6]	姚可夫, 施凌翔, 陈双琴, 邵洋, 陈娜, 贾蓟丽 2018 67 016101 Google Scholar Yao K F, Shi L X, Chen S Q, Shao Y, Chen N, Jia J L 2018 Acta Phys. Sin. 67 016101 Google Scholar
[7]	Ge Y, Cheng J, Mo J, Xue L, Zhang B, Hong S, Wu Y, Liang X, Zhang X 2024 J. Alloy Compd. 976 173173 Google Scholar
[8]	Liu H, Jiang Y, Yang D, Jiang Q, Yang W 2023 J. Mat. Res. Technol. 26 3070 Google Scholar
[9]	Li X, Wang J G, Ke H B, Yang C, Wang W H 2022 Mater. Today Phys. 27 100782 Google Scholar
[10]	邵梓桥, 毕恒昌, 谢骁, 万能, 孙立涛 2018 67 167802 Google Scholar Shao Z Q, Bi H C, Xie R, Wan N, Sun L T 2018 Acta Phys. Sin. 67 167802 Google Scholar
[11]	Qiao J C, Wang Q, Pelletier J M, Kato H, Casalini R, Crespo D, Pineda E, Yao Y, Yang Y 2019 Prog. Mater. Sci. 104 250 Google Scholar
[12]	Liang S X, Jia Z, Zhang W C, Li X F, Wang W M, Lin H C, Zhang L C 2018 Appl. Catal. B-Environ. 221 108 Google Scholar
[13]	Zuo M Q, Yi S H, Choi J 2021 J. Environ. Sci. 105 116 Google Scholar
[14]	Miao F, Wang Q Q, Di S Y, Yun L, Zhou J, Shen B L 2020 J. Mater. Sci. Technol. 53 163 Google Scholar
[15]	Chen Q, Yan Z C, Zhang H, Zhang L C, Ma H J, Wang W L, Wang W M 2020 Materials 13 3694 Google Scholar
[16]	Tang Y, Shao Y, Chen N, Yao K F 2015 Rsc Adv. 5 6215 Google Scholar
[17]	Jia Z, Duan X G, Qin P, Zhang W C, Wang W M, Yang C, Sun H Q, Wang S B, Zhang L C 2017 Adv. Funct. Mat. 27 1702258 Google Scholar
[18]	Liang S X, Wang X Q, Zhang W C, Liu Y J, Wang W M, Zhang L C 2020 Appl. Mat. Today 19 100543 Google Scholar
[19]	Wang X Q, Zhang Q Y, Liang S X, Jia Z, Zhang W C, Wang W M, Zhang L C 2020 Catalysts 10 48 Google Scholar
[20]	Ji L, Chen J W, Zheng Z G, Qiu Z G, Peng S Y, Zhou S H, Zeng D C 2020 J. Phys. Chem. Solids 145 109546 Google Scholar
[21]	Wang Q Q, Chen M X, Lin P H, Cui Z Q, Chu C L, Shen B L 2018 J. Mat. Chem. A 6 10686 Google Scholar
[22]	Hou L, Wang Q Q, Fan X D, Miao F, Yang W M, Shen B L 2019 New J. Chem. 43 6126 Google Scholar
[23]	Chen S Q, Li M, Ji Q M, Chen X, Lan S, Feng T, Yao K F 2021 J. Non-Cryst. Solids 571 121070 Google Scholar
[24]	Tan L, Wang X Y, Wang S K, Qin X R, Xiao L F, Li C L, Sun S Q, Hu S Q 2023 New J. Chem. 47 11723 Google Scholar
[25]	Wei J, Zheng Z G, Zhao L, Qiu Z G, Zeng D C 2023 Colloid Surface A 666 131227 Google Scholar
[26]	Lassoued A, Li J F 2023 J. Phys. Chem. Solids 180 111475 Google Scholar
[27]	Yang W M, Wang Q Q, Li W Y, Xue L, Liu H S, Zhou J, Mo J Y, Shen B L 2019 Mat. Design 161 136 Google Scholar
[28]	Zheng K L, Qin X D, Zhu Z W, Zheng S J, Li H L, Fu H M, Zhang H F 2020 J. Mat. Chem. A 8 10855 Google Scholar
[29]	Luo X K, Li R, Zong J Y, Zhang Y, Li H F, Zhang T 2014 Appl. Surf. Sci. 305 314 Google Scholar
[30]	Tang M F, Lai L M, Ding D Y, Liu T H, Kang W Z, Guo N, Song B, Guo S F 2022 J. Non-Cryst. Solids 576 121282 Google Scholar
[31]	Zhao B W, Zhu Z W, Qin X D, Li Z K, Zhang H F 2020 J. Mat. Sci. Technol. 46 88 Google Scholar
[32]	Qin X D, Zhu Z W, Liu G, Fu H M, Zhang H W, Wang A M, Li H, Zhang H F, 2015 Sci. Rep. 5 18226 Google Scholar
[33]	Xie S H, Huang P, Kruzic J J, Zeng X, Qian H 2016 Sci. Rep. 6 21947 Google Scholar
[34]	陈双琴 2018 博士学位论文 (北京: 清华大学) Chen S Q 2018 Ph. D Dissertation (Beijing: Tsinghua University
[35]	Xie S H, Xie Y L, Jamie J, Gu K M, Yang H P, Deng Y M, Zeng X R 2020 Chemcatchem 12 750 Google Scholar

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