化工学报 ›› 2020, Vol. 71 ›› Issue (8): 3403-3415.DOI: 10.11949/0438-1157.20200131
孙敬方1(),葛成艳2(),安冬琦1,仝庆1,高飞1,董林1()
收稿日期:
2020-02-15
修回日期:
2020-05-15
出版日期:
2020-08-05
发布日期:
2020-08-05
通讯作者:
董林
作者简介:
孙敬方(1987—),女,博士,中级工程师,基金资助:
Jingfang SUN1(),Chengyan GE2(),Dongqi AN1,Qing TONG1,Fei GAO1,Lin DONG1()
Received:
2020-02-15
Revised:
2020-05-15
Online:
2020-08-05
Published:
2020-08-05
Contact:
Lin DONG
摘要:
氧空位(oxygen vacancy, Ov)是金属氧化物缺陷的一种,在多相催化、储能材料、能源化工等众多领域都发挥着重要的作用,因而关于其在理论和实验方面的研究都得到了广泛关注。以稀土CeO2这一广泛应用于能源、环境等领域的催化材料为例,简单归纳了一些氧空位检测的常用表征方法,包括拉曼(Raman)、电子顺磁共振(EPR)、正电子湮没能谱(PALS)、固体核磁(ss-NMR)、X射线光电子能谱(XPS)和扫描隧道显微镜(STM)等,同时对各种表征方法的结果分析进行了举例说明。在此基础上,对氧空位表征技术未来的发展方向提出了一些看法。希望可以对稀土铈基催化材料缺陷相关的表征及研究提供支持。
中图分类号:
孙敬方, 葛成艳, 安冬琦, 仝庆, 高飞, 董林. 稀土铈基催化材料氧空位的表征方法综述[J]. 化工学报, 2020, 71(8): 3403-3415.
Jingfang SUN, Chengyan GE, Dongqi AN, Qing TONG, Fei GAO, Lin DONG. Review on characterization methods of oxygen vacancy in rare earth cerium-based catalysts[J]. CIESC Journal, 2020, 71(8): 3403-3415.
Surface | M1 | ΔEvac/eV | ΔQM1/e | ΔQM2/e | ΔQM3/e | ΔQM4/e | |
---|---|---|---|---|---|---|---|
(111) | Ce | +2.76 | +0.32 | +0.32 | 0.00 | +0.06 | +3.01 |
Zr | +1.63 | +0.02 | +0.32 | +0.28 | +0.06 | +2.02 | |
Pd | +0.71 | +0.43 | +0.05 | +0.05 | +0.03 | +2.78 | |
(110) | Ce | +2.10 | +0.32 | +0.32 | -0.01 | -0.01 | +3.91 |
Zr | +1.24 | +0.08 | +0.31 | +0.26 | +0.06 | +4.78 | |
Pd | -0.09 | +0.38 | +0.06 | +0.04 | +0.03 | +0.82 | |
(100) | Ce | +2.26 | +0.35 | +0.37 | +0.02 | +0.01 | — |
Zr | +1.84 | +0.07 | +0.30 | +0.26 | +0.03 | — | |
Pd | -0.05 | +0.51 | +0.08 | +0.01 | +0.02 | — |
表1 不同暴露晶面CeO2氧空位生成能[26]
Table 1 Oxygen vacancy formation energy of each surface of ceria[26]
Surface | M1 | ΔEvac/eV | ΔQM1/e | ΔQM2/e | ΔQM3/e | ΔQM4/e | |
---|---|---|---|---|---|---|---|
(111) | Ce | +2.76 | +0.32 | +0.32 | 0.00 | +0.06 | +3.01 |
Zr | +1.63 | +0.02 | +0.32 | +0.28 | +0.06 | +2.02 | |
Pd | +0.71 | +0.43 | +0.05 | +0.05 | +0.03 | +2.78 | |
(110) | Ce | +2.10 | +0.32 | +0.32 | -0.01 | -0.01 | +3.91 |
Zr | +1.24 | +0.08 | +0.31 | +0.26 | +0.06 | +4.78 | |
Pd | -0.09 | +0.38 | +0.06 | +0.04 | +0.03 | +0.82 | |
(100) | Ce | +2.26 | +0.35 | +0.37 | +0.02 | +0.01 | — |
Zr | +1.84 | +0.07 | +0.30 | +0.26 | +0.03 | — | |
Pd | -0.05 | +0.51 | +0.08 | +0.01 | +0.02 | — |
图4 (a)不同温度还原后CeO2纳米棒在室温的O2吸附拉曼结果[39]; (b) CeO2纳米颗粒与H2O2反应拉曼结果[43]
Fig.4 (a) Raman spectra of O2 adsorption at room temperature on different temperature reduced ceria nanorodsm[39]; (b) Raman spectra of CeO2 nanoparticles during the reaction with H2O2[43]
Signal | EPR parameters | Proposed assignment |
---|---|---|
OC1 type | gz = 2.031—2.030, gx = 2.017, gy = 2.011 | Ce4+-O2- species formed on isolated vacancies of three-dimensional particles |
g‖= 2.034—2.032, g⊥= 2.011—2.010 | ||
OC2 | gz = 2.042—2.039, gx = 2.009—2.008 | Ce4+-O2- species formed on isolated vacancies of three-dimensional particles |
gy = 2.010—2.009 | ||
OCZ | gz = 2.026—2.025, gx = 2.018—2.017 | Ce4+-O2- species formed on two-dimensional ceria-type patches |
gy = 2.011 | ||
OZ | gz = 2.037, 2.032, gy = 2.009 | Zr4+-O2- species |
gx = 2.002 |
表2 预先吸附O2后的样品在773 K下的EPR结果[46]
Table 2 Characteristic of the EPR signals obtained upon oxygen adsorption on the samples outgessed at 773 K[46]
Signal | EPR parameters | Proposed assignment |
---|---|---|
OC1 type | gz = 2.031—2.030, gx = 2.017, gy = 2.011 | Ce4+-O2- species formed on isolated vacancies of three-dimensional particles |
g‖= 2.034—2.032, g⊥= 2.011—2.010 | ||
OC2 | gz = 2.042—2.039, gx = 2.009—2.008 | Ce4+-O2- species formed on isolated vacancies of three-dimensional particles |
gy = 2.010—2.009 | ||
OCZ | gz = 2.026—2.025, gx = 2.018—2.017 | Ce4+-O2- species formed on two-dimensional ceria-type patches |
gy = 2.011 | ||
OZ | gz = 2.037, 2.032, gy = 2.009 | Zr4+-O2- species |
gx = 2.002 |
图5 773 K下先抽真空再O2吸附后的样品在77 K下的EPR结果[47]
Fig.5 EPR spectra at 77 K following oxygen adsorption at room temperature on the sample out gassed at 773 K[47]
Sample | τ1/ps | τ2/ps | τ3/ps | I1/% | I2/% | I3/% | I2/I1 |
---|---|---|---|---|---|---|---|
c-CeO2 | 187.0 | 350.2 | 1.50 | 35.99 | 63.16 | 0.85 | 1.75 |
1%-Ag/ c-CeO2 | 203.3 | 366.1 | 2.10 | 42.82 | 56.48 | 0.70 | 1.32 |
3%-Ag/ c-CeO2 | 198.9 | 360.7 | 1.74 | 40.6 | 58.5 | 0.9 | 1.44 |
r-CeO2 | 262.0 | 397.0 | 1.90 | 31.2 | 67.9 | 0.9 | 2.18 |
1%-Ag/ r-CeO2 | 230.2 | 384.7 | 1.71 | 21.72 | 77.06 | 1.22 | 3.55 |
3%-Ag/ r-CeO2 | 250.2 | 409.3 | 2.36 | 41.5 | 57.5 | 1.0 | 1.39 |
表3 不同样品的PALS峰拟合结果和Raman结果[52]
Table 3 Peak-fitting results of PALS spectra and Raman spectra of various samples[52]
Sample | τ1/ps | τ2/ps | τ3/ps | I1/% | I2/% | I3/% | I2/I1 |
---|---|---|---|---|---|---|---|
c-CeO2 | 187.0 | 350.2 | 1.50 | 35.99 | 63.16 | 0.85 | 1.75 |
1%-Ag/ c-CeO2 | 203.3 | 366.1 | 2.10 | 42.82 | 56.48 | 0.70 | 1.32 |
3%-Ag/ c-CeO2 | 198.9 | 360.7 | 1.74 | 40.6 | 58.5 | 0.9 | 1.44 |
r-CeO2 | 262.0 | 397.0 | 1.90 | 31.2 | 67.9 | 0.9 | 2.18 |
1%-Ag/ r-CeO2 | 230.2 | 384.7 | 1.71 | 21.72 | 77.06 | 1.22 | 3.55 |
3%-Ag/ r-CeO2 | 250.2 | 409.3 | 2.36 | 41.5 | 57.5 | 1.0 | 1.39 |
图8 CeO2和CeO2/Co3O4的Ce 3d高分辨XPS结果(a),CeO2和CeO2/Co3O4的O 1s(b)和 Co 2p (c) XPS结果,CeO2和CeO2/Co3O4的Co L-edge XANES结果(d) [63]
Fig.8 High-resolution Ce 3d XPS spectra of CeO2 and CeO2/Co3O4(a). High-resolution O 1s (b) and Co 2p (c) XPS spectra of CeO2 and CeO2/Co3O4. Co L-edge XANES of CeO2 and CeO2/Co3O4 (d) [63]
图10 900℃加热1 min(a)和5 min(b)后的CeO2(111)面的STM结果以及对应出现的各种氧空位信息。由图(a)和图(b)中统计出来的表面线性氧空位团簇(LSVC)分布图(c)[71]
Fig.10 STM images of the CeO2(111) surface obtained after 1 min (a) and 5 min (b) of annealing at 900℃, with corresponding representations of the observed defects. (c) Histogram of the LSVC distribution as evaluated from (a) (solid circles) and (b) (open squares)[71]
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摘要 1542
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