自定义暴露晶面: 最佳晶面各向异性和欧姆异质结的协同效应促进光催化析氢

doi:10.1016/S1872-2067(25)64690-0

摘要/Abstract

摘要：

过渡金属硫化物如Cd_0.5Zn_0.5S (CZS)固溶体, 由于能带可调和光生载流子的高效分离而备受关注. 近年来, 利用掺杂、空位工程和异质结构设计等策略来提高光催化性能的研究得到了广泛的关注. 通过调控暴露晶面来获得最佳的晶面各向异性, 是提高异质结的光催化活性的有效的手段之一. 虽然传统的异质结构可以在一定程度上提高光生载流子的分离效率, 但在异质结形成过程中, 两种材料的暴露晶体面不能很好协同, 导致异质结界面表现出不理想的晶面各向异性. 如果在异质结构建时预先调节光催化剂的暴露晶面(即构建自定义晶面异质结)可以使不同材料之间最佳的晶面相互作用, 从而提升光催化效率.

本文采用溶剂热法和煅烧法分别合成了暴露(111)晶面的六边形Co₃O₄、暴露(110)晶面的棒状Co₃O₄和暴露(100)晶面的立方体形Co₃O₄ (分别命名为HCO, NCO和CCO), 并成功与Cd_0.5Zn_0.5S (CZS)偶联. 在这些复合材料中, HCOCZS20表现出最佳的析氢活性. 在5 h内, HCOCZS20的析氢总量分别是CZS和HCO的209.12倍和6.20倍, 明显高于NCOCZS20和CCOCZS20. 结合密度泛函理论计算和飞秒瞬态吸收光谱分析发现, HCO与CZS之间的晶面相互作用使该复合催化剂在晶面载流子输运、晶面反应活性位点和晶面电子结构等方面表现出较好的各向异性. 这种相互作用诱导电子在CZS和HCO接触界面处重新排布, 从而建立了由HCO指向CZS的内建电场(IEF), 促进了HCO和CZS之间欧姆异质结的形成. 当CZS和HCO接触时, 由于费米能级的差异, 界面处的电子将从HCO向CZS转移, 直至达到费米能级平衡. 在光照条件下, IEF的存在有利于光生电子从CZS的CB向HCO迁移, 而保留在VB上的空穴则被牺牲试剂有效消除. HCO上的光生电子向催化剂表面迁移参与水的还原反应. 欧姆异质结和异质结晶面各向异性的协同作用不仅显著的降低了氢吸附的吉布斯自由能, 而且促进了电子-空穴对的高效空间分离和快速转移.

综上, 调控光催化剂暴露的晶面并构建特定的晶面异质结能有效提升光催化剂的光催化活性. 本研究为定制晶面异质结提供了一种思路, 即异质结晶面之间的各向异性相互作用可以有效增强光催化析氢.

关键词: 晶面异质结, 晶面相互作用, 欧姆异质结, 各向异性, 光催化制氢

Abstract:

The design of customized crystal plane heterojunction can effectively leverage the optimal anisotropic interaction of crystal plane, thereby enhancing photocatalytic activity. In this study, Co₃O₄ exposed (111), (110), and (100) crystal planes (designated as HCO, NCO, and CCO, respectively) were synthesized and successfully coupled with Cd_0.5Zn_0.5S (CZS). Among these composites, the HCO/CZS exhibited best hydrogen evolution activity. In conjunction with DFT calculations and femtosecond transient absorption spectroscopy, it has been found that: the crystal plane interaction between HCO and CZS enabled the composite catalyst to exhibit optimal anisotropy in crystal plane carrier transport, crystal plane active sites, and crystal plane electronic structure. This interaction induces a redistribution of electrons at their contact interface, thereby establishing a built-in electric field that facilitates the formation of ohmic heterojunction between HCO and CZS. The synergistic effect of the ohmic heterojunction and crystal plane anisotropy not only decreases the Gibbs free energy of hydrogen adsorption but also facilitates the efficient spatial separation and rapid transfer of electron-hole pairs. This study offers valuable insights into the customization of crystal plane heterojunctions, aiming to maximize anisotropic interactions between crystal planes in order to enhance photocatalytic hydrogen evolution.

Key words: Crystal plane heterojunction, Crystal plane interaction, Ohmic heterojunction, Crystal plane anisotropy, Photocatalytic hydrogen evolution

周正宇, 靳治良. 自定义暴露晶面: 最佳晶面各向异性和欧姆异质结的协同效应促进光催化析氢[J]. 催化学报, 2025, 74: 294-307.

Zhengyu Zhou, Zhiliang Jin. Custom exposed crystal facets: Synergistic effect of optimum crystal facet anisotropy and Ohmic heterojunction boosting photocatalytic hydrogen evolution[J]. Chinese Journal of Catalysis, 2025, 74: 294-307.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64690-0

https://www.cjcatal.com/CN/Y2025/V74/I7/294

图/表 14

Scheme 1. Flow chart for preparing materials.

Fig. 1. (a) XRD pattern of CZS. (b) XRD patterns of HCO, NCO and CCO. XRD patterns of HCOCZSX (c), NCOCZSX (d), and CCOCZSX (e).

Fig. 2. (a,b) SEM images of CZS. (c-h) SEM images of HCO, NCO, CCO, HCOCZS20, NCOCZS20, CCOCZS20. (i-k) Element maps of HCOCZS20, NCOCZS20, CCOCZS20. (l,m) TEM and HRTEM images of HCOCZS20. (n-p) Measurement of lattice spacing. (q) SAED of HCOCZS20.

Fig. 3. (a) XPS total spectrum of HCOCZS20. (b-f) XPS fine spectra of S 2p, Zn 2p, Cd 3d, Co 2p, and O 1s.

Fig. 4. (a) UV-vis absorption spectrum. (b) Kubelka-Munk pattern. (c,d) PL and TRPL spectra.

Table 1 Attenuation parameters of CZS, HCOCZS20, NCOCZS20 and CCOCZS20.

Materials	Lifetime, τ (ns)	Rel (%)	<τ> (ns)	χ²
CZS	τ₁ = 0.35 τ₂ = 1.89 τ₃ = 10.92	A₁ = 55.86 A₂ = 36.28 A₃ = 7.86	0.56	1.45
HCOCZS20	τ₁ = 1.72 τ₂ = 9.68 τ₃ = 0.29	A₁ = 36.63 A₂ = 9.40 A₃ = 53.97	0.49	1.27
NCOCZS20	τ₁ =0.29 τ₂ = 1.71 τ₃ = 9.51	A₁ = 53.33 A₂ = 37.77 A₃ = 8.90	0.48	1.32
CCOCZS20	τ₁ =1.85 τ₂ = 0.33 τ₃ = 11.26	A₁ = 36.11 A₂ = 55.65 A₃ = 8.24	0.53	1.32

Fig. 5. (a) Hydrogen production of HCO, CZS and HCOCZSX in 5 h. (b) Hydrogen production of NCO, CZS and NCOCZSX in 5 h. (c) Hydrogen production of CCO, CZS and CCOCZSX in 5 h. (d) Hydrogen production of HCOCZS20, NCOCZS20 and CCOCZS20. (e) Cycle stability test of HCOCZS20. (f) AQE of HCOCZS20.

Table 2 Comparison of hydrogen production of other CZS-based photocatalysts.

Photocatalyst	Optical source	Sacrificial reagent	Hydrogen production	Ref.
HCOCZS20	LED 10 W	lactic acid	18.03 mmol/(g·h)	This work
Zn_0.4Cd_0.6S-0/MC	Xenon lamp 300 W	—	12.2 mmol/(g·h)	[58]
5CHCZS	Xenon lamp 300 W	Na₂S/Na₂SO₃	5.34 mmol/(g·h)	[59]
Zn_0.5Cd_0.5S-STA-Ni	Mercury lamp 500W	lactic acid	1.06 mmol/(g·h)	[60]
CZS-Solvothermal method)	Xenon lamp 300 W	lactic acid	12.15 mmol/(g·h)	[61]
CZS/CMS-10	Xenon lamp 300 W	Na₂S/Na₂SO₃	13.1 mmol/(g·h)	[62]
FMZCS	Xenon lamp 300 W	Na₂S/Na₂SO₃	19.08 mmol/(g·h)	[63]
ZnCdS@ZnInS/MoS	Xenon lamp 300 W	TEOA	8.50 mmol/(g·h)	[64]
Zn_0.5Cd_0.5S/CoP-3	Xenon lamp 300 W	—	9.26 mmol/(g·h)	[65]

Fig. 6. (a) Photocurrent response curve. (b) EIS impedance spectra. (c-f) Mott-Schottky diagram of HCO, NCO, CCO, and CZS.

Fig. 7. (a-d) Φ of HCO, NCO, CCO, and CZS. (e-g) The (111), (110), and (001) crystal facet of CO. (h) Charge density distribution curve and charge density difference map (Blue signifies electron accumulation, while yellow indicates electron depletion). (i) Total state density of HCOCZS20, NCOCZS20 and CCOCZS20. (j-k) D-band centers of Zn and Cd. (l) ΔGH* of different materials.

Table 3 Es, Eb, As, n, and Ei of (001), (110), and (111) lattice plane.

E_s (eV)	E_b (eV)	A_s (Å²)	n	E_i (eV/Å²)	Lattice plane
-3.90E+04	-9.75E+03	61.82	4	1.02E-01	(0 0 1)
-3.90E+04	-9.75E+03	92.71	4	1.11E-01	(1 1 0)
-7.79E+04	-9.75E+03	240.77	8	1.45E-01	(1 1 1)

Fig. 8. In-situ XPS analysis of S 2p (a), Zn 2p (b), Cd 3d (c), and Co 2p (d).

Fig. 9. Transient absorption spectra of HCOCZS20 (a,d), NCOCZS20 (b,e), and CCOCZS20 (c,f). Corresponding fitted GSB recovery kinetics of HCOCZS20 (g), NCOCZS20 (h), and CCOCZS20 (i) at 470 nm.

Scheme 2. Diagram of photocatalytic mechanism.

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