Z-型异质结光催化剂的设计、制备和应用研究进展

张梦凡; 张振民; 贾静雯; 余长林; 杨凯

doi:10.13264/j.cnki.ysjskx.2020.03.003

Z-型异质结光催化剂的设计、制备和应用研究进展

张梦凡¹,
张振民¹,
贾静雯¹,
余长林^{1, 2,},
杨凯¹

1.
江西理工大学化学化工学院，江西赣州 341000
2.
广东石油化工学院化学工程学院，广东茂名 525000

基金项目:

国家自然科学基金资助项目 21567008

国家自然科学基金资助项目 21707055

广东省珠江学者特聘教授资助计划 2019

江西省主要学科学术带头人 20172BCB22018

广东省自然科学基金资助项目 2019A1515011249

广东省普通高等学校重点研究项目（自然） 2019KZDXM010

详细信息

作者简介:
余长林（1974-），男, 教授, 主要从事纳米催化材料研究与光催化技术及其应用。E-mail：yuchanglinjx@163.com

中图分类号: O643.36
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- 文章访问数: 333
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出版历程
- 收稿日期: 2019-12-17
- 发布日期: 2020-06-29
- 刊出日期: 2020-05-31

Research progress in the design, fabrication and application of Z-scheme heterojunction photocatalysts

1.
School of Chemistry and Chemical Engineering, Jiangxi University of Science and Technology, Ganzhou 341000, China
2.
School of Chemical Engineering, Guangdong University of Petrochemical Technology, Maoming 525000, China

摘要

摘要: 传统异质结具有扩大光响应范围、促进载流子分离的优点，但存在氧化-还原能力不够的问题。Z-型异质结是根据自然界植物光合作用模拟的人工光合作用而提出的，相对于单一光催化剂与传统异质结光催化剂具有能有效分离电子空穴对、减少复合几率、保留强氧化-还原活性位点、扩大光响应范围、提高光催化活性等优点。文中综述了近年来，液相Z-型异质结光催化剂、全固态Z-型异质结光催化剂、直接Z-型异质结光催化剂的反应机理、构建方法与在光解水产氢、CO₂还原、有机物的降解、水中重金属离子的还原等应用方面的研究进展。并对比几类Z-型异质结光催化剂的特点，提出了Z-型光催化体系发展的未来挑战和前景。
- 液相Z-型异质结 /
- 全固态Z-型异质结 /
- 直接Z-型异质结 /
- 制氢 /
- 降解
Abstract: Traditional heterojunction boasts such advantages as enlargement in optical response range and facilitation in carrier separation. However, its redox ability is insufficient. Z-scheme heterojunction is put forward based on artificial photosynthesis, a simulation of plant photosynthesis in nature. With respect to the single photocatalyst and traditional heterojunction, Z-scheme heterojunction has distinct advantages, e.g. the effective separation of electron-hole pairs, reduced recombination of photo-induced carrier, strong redox active site, expanded light response range, high photocatalytic activity, etc. In this paper, the reaction mechanism, construction method and application of liquid phase Z-scheme heterojunction, all-solid-state Z-scheme heterojunction and direct Z-scheme heterojunction are reviewed. Finally, the characteristics of several types of Z-scheme heterojunction were briefly summarized and compared, and the challenges and prospects for the development of Z-scheme photocatalytic systems are proposed.
- liquid phase Z-scheme heterojunction /
- all-solid-state Z-scheme heterojunction /
- direct Z-scheme heterojunction /
- hydrogen production /
- degradation

HTML全文

稀土Yb不仅对铝、镁等合金材料的力学、耐腐蚀性能的改善作用非常显著,还能与其他金属形成功能合金。开发Yb的功能合金材料,拓宽其应用领域的前景非常广阔^[1-3]。目前,Yb的单质金属生产主要是通过真空镧热还原Yb₂O₃获得,产能低、作业不连续、成本高。同时混熔法制备Yb合金,烧损率高且易偏析,而熔盐电解法直接制备稀土金属合金能够克服热还原和混熔法的不足,提高稀土合金制备的效率^[4-5]。前期研究表明采用LiF-CaF₂-Yb₂O₃体系,Ni作为自耗阴极能制备出Ni-Yb合金,具有良好的应用前景^[6]。为进一步改善电解工艺参数、降低能耗、提高电解效率,需要全面系统地研究LiF-CaF₂-Yb₂O₃体系的物理化学性质。其中,表面张力是熔盐的一种界面性质,也是熔盐重要的物理参数之一,对界面反应以及熔盐电解过程均有较大的影响,直接关系电解过程中阳极效应以及金属产物的氧化过程^[7-8]。对熔盐表面张力进行深入探讨,可为熔盐中质点间的相互作用力、熔盐电解机理、熔盐离子结构的研究提供关键数据,从而为电解工艺参数的选择提供理论依据。为此,本文采用拉筒法^[9]对Yb₂O₃溶解度范围内的LiF-CaF₂-Yb₂O₃体系的黏度进行测量,并通过数学模型对Ni-Yb合金表面张力进行分析和计算,从而为优化电解工艺参数提供依据,同时,为深入研究和分析LiF-CaF₂-Yb₂O₃体系的结构及其电解机理提供必要的基础数据。

1 实验部分

分析纯CaF₂、LiF、Yb₂O₃在423 K下烘干48 h；光谱纯石墨坩埚经乙醇清洗后,在353 K下烘干24 h。表面张力测量系统如图1所示,主要由精密电子天平与钨测头通过钢丝连接组成,当垂直的圆筒状测头与液体接触时,液体的表面张力对测头产生向下的拉力,通过测量液体表面上的圆筒测头拉离液体表面时的最大拉力（F_max）以及圆筒周长,然后通过式（1）计算熔体的表面张力。测量流程包括：①钨测头（Φ15 mm）通过钢丝悬挂在精准电子天平上,调整电子天平和测头的位置使测头在炉膛中心处且侧头平稳没有倾斜；②通过测量高纯水在293 K下的表面张力值和在不同温度下的熔融NaCl的表面张力来校准实验装置；③校正结束后,将干燥脱水且混匀后的待测样品放入坩埚,然后利用仪器自带的高温电阻炉对样品坩埚进行加热至实验温度,并恒温20 min后,确保测头位置与校正实验时的位置相同,运行表面张力测量程序对待测样品进行表面张力测量。

σ = F_{m a x} / 2 π r

(1)

图 1 表面张力测量装置示意

1. 高温炉；2. 黏度仪；3. 控制箱；4. 刚玉套管；5. 碳化硅坩埚；6. 石墨坩埚；7. 钨制测头；8. 熔盐；9. 导电仪；10. 天平仪。

Figure 1. Schematic diagram of the surface tension measuring device

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式（1）中：σ为表面张力数值,单位mN/m；r为长度数值,单位m。

2 结果与讨论

2.1 LiF-CaF₂-Yb₂O₃熔盐体系的表面张力研究

2.1.1 LiF-CaF₂体系表面张力模型及数据评估

LU 等^[10]及LIAO等^[11]研究表明Santos方程^[12]能用于二元熔盐体系表面张力的预测,且能够描述二元体系的表面张力及其表面相与体相组成的关系。通过拉筒实验测量值对Santos方程预测LiF-CaF₂表面张力的适用性进行评估。Santos预测二元混合熔盐体系表面张力的模型如式（2）所示,AQRA 等^[13]、HARA等^[14]及MARCUS^[15]研究报道的纯组元LiF和CaF₂的标准表面张力值如表1所列。

表 1 纯组元LiF与CaF₂的标准表面张力值

Table 1. Standard surface tension values of pure components LiF and CaF₂

物质	表面张力/（mN/m）	K_T_,i/GPa^-1
LiF	γ（LiF）=373.2-0.109T	0.093
CaF₂	γ（CaF₂）=459.0-0.095 6T	0.064

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| 显示表格

\{\begin{matrix} X_{A}^{B} {[1 + \frac{(σ_{i d} - σ_{A})}{V_{A}} {(\frac{\partial S_{A}}{\partial p})}_{T}]}^{\frac{V_{A} S_{A}}{R T {(\frac{\partial S_{A}}{\partial p})}_{T}}} + X_{B}^{B} {[1 + \frac{(σ_{i d} - σ_{B})}{V_{B}} {(\frac{\partial S_{B}}{\partial p})}_{T}]}^{\frac{V_{B} S_{B}}{R T {(\frac{\partial S_{B}}{\partial p})}_{T}}} = 1 \\ X_{i}^{S} = X_{i}^{B} {[1 + \frac{(σ_{i d} - σ_{i})}{V_{i}} {(\frac{\partial S_{i}}{\partial p})}_{T}]}^{\frac{V_{i} S_{i}}{R T {(\frac{\partial S_{i}}{\partial p})}_{T}}} \\ {(\frac{\partial S_{i}}{\partial p})}_{T} = - \frac{2}{3} S_{i} K_{T, i} \\ S_{i (c c)} = N_{0}^{\frac{1}{3}} {(\frac{M_{i}}{ρ_{i}})}^{\frac{2}{3}} \end{matrix}

(2)

式（2）中： $X_{A}^{B}$ 、 $X_{B}^{B}$ 分别为体相A、B的摩尔分数；σ_id为理想纯组元的表面张力数值,单位N/m；σ_A、σ_B分别为纯组元A、B的表面张力数值,单位N/m；V_A、V_B分别为纯组元A、B的摩尔体积数值,单位m³/mol； ${(\partial S_{A} / \partial p)}_{T}$ 、 ${(\partial S_{B} / \partial p)}_{T}$ 分别为恒温条件下纯组元A、B摩尔表面积与压力的偏导数；R为气体常数（8.314 J/K/mol）；T为绝对温度数值,单位K；K_T_,i为组元i的等温压缩系数数值,单位Pa^-1；N₀为阿伏伽德罗常数（6.02×10²³ mol^-1）；M_i为组元i的摩尔质量数值,单位kg/mol；ρ_i为组元i的密度数值,单位kg/m³。

图2（a）中实验测量获得的表面张力数据表明,随着温度的升高,表面张力均可近似为呈线性降低,其中,LiF-CaF₂共晶体系表面张力与温度呈线性关系如式（3）所示。因为熔盐体内部及表面离子或分子间的动能增加,间距增大,离子或分子间相互吸引力减小,分子或离子的相互作用也弱化,导致表面张力值降低。根据图2（a）中数据对比可知：Santos方程计算值与不同组分LiF-CaF₂体系表面张力测量值的最大估算误差为6.55%,表明Santos模型能够较好地预测LiF-CaF₂表面张力。进一步利用Santos模型分析LiF-CaF₂体系表面相与体相组成关系,可以看出,表面张力值随着CaF₂在表面相组成的增加而增大,温度升高导致CaF₂在表面相的组成减少,CaF₂相对于LiF不易与在熔体表面层表面相聚集,推测与CaF₂在熔体中的结构形式有关。

图 2 LiF-CaF₂熔盐体系表面张力（a）实验值与Santos模型计算值比较和（b） CaF₂在表面相与体相含量关系

Figure 2. （a） Comparison between the experimental values and the related values calculated by the Santos model and （b） relationship between the CaF₂content in the surface phase and bulk phase of the surface tension of the LiF-CaF₂ molten salt system

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σ = 371.13 - 0.10 T

(3)

2.1.2 LiF-CaF₂-Yb₂O₃体系表面张力变化规律

廖春发等^[16]研究表明在1 173～1 523 K温度范围内,（LiF-CaF₂）_etu体系中Yb₂O₃溶解度低于2%（质量分数）,因此,图3（a）中为一定Yb₂O₃含量下（LiF-CaF₂）_etu -Yb₂O₃体系表面张力随温度的变化规律,可以看出,在1 173～1 523 K范围内, 一定Yb₂O₃含量的（LiF-CaF₂）_etu -Yb₂O₃体系表面张力随着温度的升高而降低,原因是温度的升高致使熔体表面层离子或团簇具备较高的动能和较低的解离能,阴阳离子之间的相互吸引作用减弱。图3（b）为特定温度下（LiF-CaF₂）_etu-Yb₂O₃体系表面张力随Yb₂O₃含量的变化规律,可以看出,表面张力与Yb₂O₃的溶解度之间密切相关。当Yb₂O₃的质量分数为0～2%时,Yb₂O₃在LiF-CaF₂体系内被充分溶解,体系的表面张力在Yb₂O₃的质量分数为1%时达到最高值。随着Yb₂O₃的质量分数进一步增加,达到过饱和状态,体系的表面张力出现减小,分析原因认为Yb₂O₃的加入会导致（LiF-CaF₂）_etu体系的离子构成形式发生变化,从而使表面层和体相离子团簇构成形式发生变化。由于（LiF-CaF₂）_etu体系中Yb₂O₃的溶解度较小,（LiF-CaF₂）_etu体系中主体结构不会发生根本性变化,但可以确定在Yb₂O₃的溶解量为0～2%（质量分数）时,体系内部会产生吸引作用力强的离子团簇,使其表面张力增加。随着Yb₂O₃含量的增加,体系表面层中离子结构发生变化,削弱了表面层离子或团簇的吸引作用,导致表面张力下降。拟合图3（b）中数据可以得到LiF-CaF₂-Yb₂O₃熔盐体系表面张力的回归方程式（4）。

σ = 363.190 - 0.940 x - 0.092 T

(4)

图 3 温度（a）和Yb₂O₃含量（b）对LiF-CaF₂熔盐体系表面张力的影响

Figure 3. Effect of temperature （a） and Yb₂O₃ content （b） on the surface tension of the LiF-CaF₂ molten salt system

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2.2 Ni-Yb合金的表面张力

综合LiF-CaF₂-Yb₂O₃体系和Ni-Yb合金表面张力变化规律,表明随电解温度的升高,LiF-CaF₂-Yb₂O₃熔盐体系的表面张力减小,但仅在220～260 mN/m较小范围内变化。Yb₂O₃在LiF-CaF₂-Yb₂O₃体系中的含量引起的张力变化范围同样不显著,在1 173～1 523 K温度区间表面张力波动范围小于20 mN/m。因此,Ni-Yb合金的表面张力值随组分和温度的变化决定合金与LiF-CaF₂-Yb₂O₃体系的分离。

Butler方程^[17]如式（5）所示,该方程经过完善后被广泛应用于二元及三元合金内的表面张力的预测^[18-19],经对多种合金体系的验证,预测值与实验值较吻合。利用Butler模型,结合Yb、Ni纯金属的标准物理参数^[20],见表2所列,得到图4所示高于Ni-Yb合金熔点100～600 K和Yb摩尔百分含量0～100%范围内的表面张力曲面预测值。同时,图4中给出了LiF-CaF₂-Yb₂O₃体系在1 173～1 523 K温度区间以及Yb₂O₃质量分数在0～4%范围内的表面张力曲面预测值,当合金中Yb的摩尔分数低于10%时, 合金的表面张力变化梯度大, 在600～ 1 700 mN/m迅速增大。当Yb的摩尔分数高于10%时,合金的表面张力变化梯度小,在200～600 mN/m范围内缓慢减小。对比LiF-CaF₂-Yb₂O₃体系的张力曲面,当合金中Yb的摩尔分数低于10%时,合金与熔盐的表面张力差值范围在340～1 480 mN/m间波动,远高于熔盐体系。合金与熔盐体系润湿性差,液态合金易于团聚。合金中Yb的摩尔分数高于10%时,合金与熔盐的表面张力差值仅在20～340 mN/m小范围内波动,合金与熔盐体系润湿性好,液态合金不易团聚。总体上, 在温度1 173～1 523 K范围内的LiF-CaF₂-Yb₂O₃体系下,熔盐体系的黏度相对稳定,Yb摩尔分数高于10%的Ni-Yb合金产物与LiF-CaF₂-Yb₂O₃熔盐表面张力差值较小,润湿性更好,有利于收集。

表 2 纯金属Ni、Yb的标准物理参数

Table 2. Standard physical parameters for the pure metals Ni and Yb

组元	表面张力（σ）/（mN/m）
Ni	1 834-0.376×（T-1 455）
Yb	320-0.102×（T-824）

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| 显示表格

图 4 Ni-Yb合金与LiF-CaF₂-Yb₂O₃体系表面张力曲面对比

Figure 4. Comparison diagram of the surface tension curved surface of the LiF-CaF₂-Yb₂O₃ system and Ni-Yb alloy

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\{\begin{matrix} σ = σ_{i} + \frac{R T}{S_{i}} l n \frac{X_{i}^{s}}{X_{i}^{b}} + \frac{1}{S_{i}} ({}^{E} G_{i}^{S} - {}^{E}G G_{i}^{B}) \\ \sum_{i = 1}^{n} X_{i}^{S} = 1 0 \leq X_{i}^{s} \leq 1 \\ {}^{E} G_{i}^{S} = \frac{Z^{s}}{Z^{b}} {}^{E}G G_{i}^{B} = β {}^{E}G G_{i}^{B} \\ S_{i (h c p)} = 1.091 N_{0}^{\frac{1}{3}} {(\frac{M_{i}}{ρ_{i}})}^{\frac{2}{3}} \\ {}^{E} G_{i}^{B} = G^{E} + (1 - x_{i}) \frac{\partial G^{E}}{\partial x_{i}} \end{matrix}

(5)

式（5）中： $β$ =0.75,σ和σ_i为溶体和纯组分i的表面张力数值,单位mN/m；R为气体常数（8.314 J/mol/K）；T为绝对温度数值,单位K；X_i^S和X_i^B分别为组分i在表面相和体相中的摩尔分数；S_i为组分i纯物质的单层表面积数值,单位m²； ${}^{E} G_{i}^{S}$ 和 ${}^{E} G_{i}^{B}$ 分别为表面相和体相中组分i的偏摩尔吉布斯自由能数值,单位J/mol；Z^S和Z^B分别是表面相和体相的配位数； N_o为阿伏伽德罗常数（6.02×10²³mol^-1）；M_i为组分i的摩尔质量数值,单位kg；ρ_i为密度数值,单位kg/m³。

3 结论

1）在1 173～1 523 K范围内,随着温度的升高,LiF-CaF₂体系的表面张力呈线性降低。Santos方程能较好预测LiF-CaF₂体系二元熔盐体系表面张力和描述表面相与体相组成的关系；在1 173～1 523 K范围内,LiF-CaF₂-Yb₂O₃体系表面张力随温度的升高而降低；在Yb₂O₃的质量分数为1%～4%范围内,体系的表面张力先增后减,在质量分数为1%时达到最高。

2）当高于熔点200～600 K范围内,液态Ni-Yb合金中Yb的摩尔分数低于10%时,其表面张力在600～1 700 mN/m迅速增大。当Yb的摩尔分数高于10%时,合金的表面张力在200～600 mN/m范围内缓慢减小。温度为1 173～1 523 K范围内的LiF-CaF₂-Yb₂O₃体系的表面张力在220～260 mN/m较小范围内波动,相对稳定,与Yb摩尔分数高于10%的Ni-Yb合金表面张力差值较小,润湿性更好。

图 1 异质结机理

Fig 1. Heterojunction mechanism

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图 2 Z-型异质结机理

Fig 2. Z-scheme heterojunction mechanism diagrams

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图 3 交错能带构型的半导体示意^[56]

Fig 3. Semiconductor schematic diagram of staggered energy band configurations^[56]

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图 4 双Z-型异质结机理

Fig 4. Mechanism diagram of double Z-scheme heterojunction

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图 5 Zn₃（VO₄）₂·2H₂O相变构建三元异质相结模型

Fig 5. Ternary heterojunction model constructed by Zn₃(VO₄)₂·2H₂O phase transition

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图 6 Z-型异质结光催化产氢机理

Fig 6. Mechanism diagram of photocatalytic hydrogen production of Z-scheme heterojunction

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图 7 CO₂还原机理^[86-88]

Fig 7. CO₂ reduction mechanism diagram^[86-88]

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图 8 Ag₃PO₄ / Ag₂MoO₄ /Ag电荷分离转移示意^[99]

Fig 8. Charge separation and transfer diagram of Ag₃PO₄ / Ag₂MoO₄ /Ag^[99]

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表 1 Z-型异质结构建方法

Table 1 Construction method of Z-scheme heterojunction

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表 2 用于光解水产氢产氧的Z-型异质结光催化剂

Table 2 Hydrogen and oxygen production over Z-scheme heterojunction photocatalysts

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表 3 CO₂还原产物及电势

Table 3 CO₂ reduction products and potential

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表 4 用于CO₂还原的Z-型异质结光催化剂

Table 4 Reduction of CO₂ over Z-scheme heterojunction photocatalysts

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表 5 用于降解有机污染物的Z-型异质结光催化剂

Table 5 Degradation of organic pollutants over Z-scheme heterojunction photocatalysts

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1 实验部分
2 结果与讨论
2.1 LiF-CaF2-Yb2O3熔盐体系的表面张力研究
2.1.1 LiF-CaF2体系表面张力模型及数据评估
2.1.2 LiF-CaF2-Yb2O3体系表面张力变化规律
2.2 Ni-Yb合金的表面张力
3 结论

Z-型异质结光催化剂的设计、制备和应用研究进展

作者简介: 余长林（1974-），男, 教授, 主要从事纳米催化材料研究与光催化技术及其应用。E-mail：yuchanglinjx@163.com

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