无机材料学报 ›› 2021, Vol. 36 ›› Issue (3): 225-244.DOI: 10.15541/jim20200224 CSTR: 32189.14.10.15541/jim20200224
• 特邀综述 • 下一篇
周煜筑1(
), 张友魁2, 宋礼1()
收稿日期:2020-04-26
修回日期:2020-07-01
出版日期:2021-03-20
网络出版日期:2020-10-10
通讯作者:
宋 礼, 教授. E-mail: song2012@ustc.edu.cn
作者简介:周煜筑(1998 -), 男, 硕士研究生. E-mail: zyz12345@mail.ustc.edu.cn
基金资助:
ZHOU Yuzhu1(), ZHANG Youkui2, SONG Li1()
Received:2020-04-26
Revised:2020-07-01
Published:2021-03-20
Online:2020-10-10
Contact:
SONG Li, professor. E-mail: song2012@ustc.edu.cn
About author:ZHOU Yuzhu(1998 -), male, Master candidate. E-mail: zyz12345@mail.ustc.edu.cn
Supported by:摘要：
电催化技术是可再生能源储存和转换领域中最有吸引力的技术之一, 其中贵金属纳米材料具有优异的电催化活性。贵金属在地球中的储量少且开发成本高, 如何在减少贵金属用量的同时提高催化剂活性和稳定性一直是电催化应用领域的研究焦点。贵金属磷化物作为新型电催化剂因其多功能活性位点、可调的结构和组分以及新颖的物理化学性质等优点, 受到了研究人员的广泛关注。与过渡金属磷化物相比, 贵金属磷化物具有更高的本征活性, 且在酸性条件下具有更好的稳定性。本综述介绍了近年来贵金属磷化物电催化剂的设计合成、结构调控、X射线吸收谱表征及其在电催化应用中的研究进展, 据此讨论当前所面临的机遇和挑战, 并展望原位同步辐射X射线表征技术在未来贵金属磷化物电催化剂研究中的应用前景。
中图分类号:
周煜筑, 张友魁, 宋礼. 贵金属磷化物催化剂及其同步辐射X射线吸收谱[J]. 无机材料学报, 2021, 36(3): 225-244.
ZHOU Yuzhu, ZHANG Youkui, SONG Li. Noble Metal Phosphide Electrocatalysts and Their Synchrotron-based X-ray Absorption Spectroscopy[J]. Journal of Inorganic Materials, 2021, 36(3): 225-244.
图1 铂族金属磷化物的结构示意图, 其中灰色为金属原子, 红色为磷原子[11]
Fig. 1 The structures of selected platinum group metal (PGM) phosphides. The metal atoms displayed in grey and the phosphorus atoms displayed in red[11] (a) Rh2P crystallizes in the anti-CaF2 structure; (b) Rh2P3; (c) Rh4P3; (d) RhP2 crystallizes in the CoSb2 structure forming P2 dimers; (e) RhP3 crystallizes in the CoAs3 structure forming Rh4-4 rings; (f) Co2P structure with chains of slightly distorted prisms
图2 Ru-Ru2P/PC(a)[40]与RhP/rGO(b)[15]的制备示意图
Fig. 2 Schematic illustration of the synthetic process for Ru-u2P/PC (a)[40] and RhP/rGO (b)[15]
图3 MPx@NPGC的合成示意图及X射线衍射(XRD)图谱(a)[45]和Ru2P@PNC/CC-900的合成示意图(b)[53]
Fig. 3 General synthesis procedure of MPx@NPGC and corresponding XRD patterns (a)[45], schematic illustration of preparation for Ru2P@PNC/CC-900 (b)[53]
图4 Rh-P/CP中Rh-P颗粒的TEM(a)和HRTEM(b)照片, 单个Rh-P粒子Rh(c)和P(d)的STEM照片与元素分布图[56], Ru-Ru2PΦNPC和NPC@RuO2的合成示意图(e)[59];
Fig. 4 TEM (a) and HRTEM (b) images of single Rh-P particle of Rh-P/CP, STEM and elemental mapping images for single Rh-P particle Rh (c) and P (d)[56], synthesis diagram of Ru-Ru2PΦNPC and NPC@RuO2 (e)[59]
图5 RhPx@NPC的XRD图谱和Rh3d和P2p的XPS图谱(a), Rh(111)、Rh2P(200)和RhP2(ˉ111)表面Rh原子d轨道上的态密度(PDOS)(b)[65], 在0.1 mol/L KOH中Pt/C、Rh NS/c和w-Rh2P NS/C的电催化性能(c), 在碱性条件下P端(PT-Rh2P(200))、Rh端(RhT-Rh2P(200))和Rh(100)表面反应过程自由能变化(?G)(d)[71]
Fig. 5 XRD patterns for RhPx@NPC and XPS spectra for the Rh3d and P2p regions of RhPx@NPC catalysts (a)[65], Partial density of states (PDOS) projected on the d orbitals of Rh atoms at the surfaces of Rh(111), Rh2P(200) and RhP2(ˉ111) (b) (The red dash and yellow solid lines indicate the Fermi level (EF) and the location of d-bands center, respectively), electrocatalytic activities of Pt/C, Rh NS/C, and w-Rh2P NS/C in 0.1 mol/L KOH (c), free energy pathways (?G) for HER of P-terminated (PT-Rh2P (200)), Rh-terminated (RhT-Rh2P (200)), and Rh (100) surfaces, respectively, under alkaline condition (d)[71]
图6 OER/HER测试前后IrP2/NPC的Ir4f XPS光谱图(a, b)[32], RuxPNFs在碱性环境下的HER原理图(c)[75], 在1 mol/L KOH电解液中进行耐久性测试前(d)试验后(e)PdP2@CB的TEM、HR-TEM照片, 以及PdP2@CB在0.5 mol/L H2SO4的HER活性(f)[69]
Fig. 6 XPS results (a, b): Ir4f for IrP2/NPC before and after the OER/HER tests[32], schematic of the HER processes by RuxPNFs under alkaline conditions (c)[75], TEM, HR-TEM images of PdP2@CB before durability test in 1 mol/L KOH electrolyte (d) after durability test in 1 mol/L KOH electrolyte (e), and HER performance (f) of PdP2@CB in 0.5 mol/L H2SO4[69]
图7 RuPx/NPG催化剂的合成和结构示意图(a)[77], NC、NPC、Rh@NC、RhPx@NPC纳米壳的TEM照片(b)[78], Rh2P@NPC和RhP2@NPC的合成和结构示意图(c)[65], RhP2@NPC的TEM照片和元素分布图(d)[65], PtNiP-MNs的SEM照片(e)[73]
Fig. 7 Schematic illustration of the synthesis and structure of the RuPx/NPG electrocatalyst (a)[77], TEM images of NC, NPC, Rh@NC, and RhPx@NPC nanoshells (b)[78], schematic illustration of the synthesis and structure of Rh2P@NPC and RhP2@NPC (c)[65], TEM image and EDS elemental mapping of Rh, P, C and N for RhP2@NPC (d), and SEM image of the PtNiP MNs (e)[73]
图8 不同温度合成RuPx的XRD图谱(a)[44], DFT计算中使用的理论模型以及在这些模型的表面H*的吸附位置, Ru2P、RuP和RuP2在平衡势下的HER自由能(b)[46], RuP(121)和RuP2(101)晶面水离解途径和势垒(c)[54]
Fig. 8 XRD patterns of RuPx synthesized in different temperatures (a)[44], theoretical models used in DFT calculations and adopted adsorption sites of H* on the surface of these models, calculated free-energy diagram of HER at equilibrium potential for Ru2P, RuP, and RuP2 (b)[46], the calculated water dissociation barrier and water dissociation pathway for RuP (121) and RuP2 (101) surfaces (c)[54]
图9 Ru-Ru2PΦNPC的HRTEM照片(a)和FFT图像(b), Ru-Ru2PΦNPC、Ru/C、Ru2P/C、NPC和20wt%Pt/C在0.5 mol/L H2SO4中的性能(c)[59], Ru-Ru2P/PC的HAADF-STEM(d)和HR-TEM(e)照片, Ru-Ru2P/P C和Pt/C催化剂Tafel斜率与pH关系及循环稳定性(f)[40], 空心Ru-RuPx-CoxP多面体的合成过程示意图(g), Co2P和Ru-RuPx-CoxP模型表面不同电位下OER过程Gibbs自由能(h)[85]。
Fig. 9 HRTEM (a) and FFT (b) images of Ru-Ru2PΦNPC, HER performance of Ru-Ru2PΦNPC, Ru/C, Ru2P/C, NPC, and 20wt% Pt/C, ?GH* calculated at the equilibrium potential of different models (c)[59], high-resolution HAADF-STEM(d) and HR-TEM (f) images of a Ru-Ru2P nanoparticle, pH dependences of the Tafel slopes of the Ru-Ru2P/PC and Pt/C catalysts, cyclic stability of the Ru-Ru2P/PC (f)[40], schematic illustration of a formation process for the hollow Ru-RuxP-CoxP polyhedra (g), Gibbs free energy diagram for the OER at different potentials on the surface of Co2P and Ru-RuPx-CoxP models (h)[85]
图10 不同BP含量的BPed-Pt/GR XPSβPt4f光谱(a), PtNP的化学态随BP含量变化(b), 不同Pt-P含量体系中的ΔGH*(c)[88], 0.1%-RP/g-CN的光催化析氢机理(d)[89], Pt/g-C3N4和RhPx/g-C3N4-5%产氢曲线(e1~e2)[90]
Fig. 10 Pt4f core level of BPed Pt/GR with different amounts of BP (a), chemical state contents of the PtNPs as a function of BP adding amount (b), free energy diagram for HER with different Pt-P contents with ΔGH* in each system (c)[88], proposed photocatalytic mechanism of 0.1%-RP/g-CN for H2 evolution (d)[89], kinetics curves of H2 production over Pt/g-C3N4 and RhPx/g-C3N4-5%, cyclic running kinetics curves of H2 production over RhPx/g-C3N4-5% (e1-e2)[90]
图11 Rh2P@NC的TEM(a, b)和HRTEM(c)照片, Rh2P@NC的HER稳定性测试(d)[51], Ru2P/RGO-20、Ru2P和Pt/C在1.0 mol/L KOH中的HER性能(e), RGO、Ru2P、Pt和Ru2P/RGO-20的HER自由能图(f)[81], RuP2和RuP2@NPC的能带结构(g)[93], 纯金属磷化物和不同金属磷化物与石墨烯的物理混合物在0.5 mol/L H2SO4和1 mol/L KOH中的极化曲线(h)[45]
Fig. 11 TEM (a,b), and HRTEM (c) images of Rh2P@NC, polarization curves for Rh2P@NC (initial and after 1000 CV scanning) and time-dependent current density curve for Rh2P@NC under static overpotential of 20 mV for 10 h (d)[51], electrocatalytic properties for the HER in 1.0 mol/L KOH of Ru2P/RGO-20, Ru2P and Pt/C (e), free-energy diagram of the HER for RGO, Ru2P, Pt and Ru2P/RGO-20 (f)[81], band structure of pure RuP2 (left) and RuP2@NPC hybrid (right) (g)[93], HER polarization curves of the pure metal phosphides and the physical mixture of different metal phosphides and graphene in 0.5 mol/L H2SO4 and 1 mol/L KOH (h)[45]
图12 Ru-MnFeP/NF催化剂制备示意图(a), Fe2P-Ru h和Mn2P-Ru结构的电荷分布(b)[98], Ru-NiFe-P和NiFe-P的XPS谱图(c), Ru-NiFe-P的吸收模型表面(d), 平衡电势下计算的?GH*(e), Ru-NiFe-P和NiFe-P的总态密度(f)[99]
Fig. 12 Schematic illustration of the fabrication of Ru-MnFeP/NF catalysts (a), calculated charge density differences of Fe2P-Ru and Mn2P-Ru structures (b)[98], high-resolution XPS spectra of Ni2p, Fe2p and P2p in the Ru-NiFe-P and the NiFe-P (c), the absorption modeled surfaces of Ru-NiFe-P (d), calculated ΔGH* for Ru-NiFe-P, NiFe-P, Ru-Ni-P, Ni-P, Ru-Fe-P and Fe-P (e), total density of states of Ru-NiFe-P and NiFe-P (f)[99]
图13 PdNP-CN的HRTEM照片(a), PdPNP-CN(b)和PdPSA-CN(c)的HAADF-STEM照片, PdNP-CN(d)、PdPNP-CN(e)和PdPSA-CN(f)的几何结构, Pd K边XANES光谱图(g), EXAFS在R(h)和k(i)空间对应的k3加权傅里叶变换谱图[103], RuCl3@HPN和Ru SAs@PN的EXAFS光谱图(j), Ru SAs@PN、Ru箔和RuCl3@HPN的小波变换谱(k), N的K边(l)、P的L边(m)NEXAFS光谱图, PN和Ru SAs@PN的质子去耦31P固态MAS NMR谱图(n)[104]
Fig. 13 HRTEM image of PdNP-CN (a), HAADF-STEM images of PdPNP-CN (b) and PdPSA-CN (c), the geometry structures of PdNP-CN (d), PdPNP-CN (e) and PdPSA-CN (f), Pd K-edge XANES spectra (g) and the corresponding k3-weighted FT spectra at R(h) and k(i) space[ 103], EXAFS spectra (j) of RuCl3@HPN and Ru SAs@PN, Wavelet transform (k) of Ru SAs@PN, Ru foil and RuCl3@HPN samples, N K edge (l) and P L edge (m) NEXAFS spectra, 31P solid state MAS NMR spectra at room temperature using a direct acquisition with proton decoupling of PN and RuβSAs@PN (n)[104] (1 ?=10 nm)
图14 AgP2 NCs、AgO、Ag2O和Ag箔的原位K边XANES(a)和EXAFS光谱(b), AgP2和Ag中CO、CO:H2、法拉第效率与Agδ+的关系(c), AgP2 NCs的Ag K边与拟合结果(d), 在RHE=-0.8 V恒电位下CRR, AgP2-NCs的Ag K边XANES谱(e), RHE=-0.8 V, AgO和Ag2O在测试前与CRR 50 s后的Ag-K边光谱(f)[38]
Fig. 14 In situ silver K-edge XANES (a) and EXAFS spectra (b) of AgP2 NCs, AgO, Ag2O, and Ag foil, Faradaic efficiency of the CO and CO:H2 ratio as a function of Agδ+ in AgP2 and Ag (c), linear combination of AgO, Ag2O, and Ag spectra (solid line) compared to the raw Ag K-edge (d), Ag K-edge XANES spectra of AgP2 NCs with respect to CRR time under a constant applied potential of -0.8 V (vs. RHE) (e), Ag K-edge spectra of AgO and Ag2O references before and after CRR at -0.8 V (vs. RHE) for 50 s (f)[38]
图15 Ni@Ni2P-Ru HNRs合成示意图(a), Ni@Ni2P-Ru、Ni@Ni2P和Ni箔的Ni K边XANES光谱图(b)和EXAFS光谱图(c), Ni@Ni2P-Ru和Ru箔的Ru K边XANES光谱图(d), Ni@Ni2P-Ru HNRs的Ru(0)和Ru(IV)分布(e)[108], Ni5P4-Ru和Ni5P4的Ni2p XPS谱图(f)和Ni L边XANES(g), Ni5P4-Ru、Ni5P4、Ni箔和NiO在Ni K边的XANES(h)和EXAFS光谱图(i), Ru箔、Ni5P4-Ru和RuO2的Ru K边XAFS光谱图(j)和EXAFS谱图(k)[97]
Fig. 15 Schematic illustration of the formation of Ni@Ni2P-Ru HNRs (a), Ni K-edge XANES spectra (b) and Fourier transformed k3-weighted EXAFS spectra of Ni@Ni2P-Ru, Ni@Ni2P, and reference Ni foil (c), Ru K-edge XANES spectra of Ni@Ni2P-Ru and reference Ru foil (d), dependence of the Ru(0) and Ru(IV) atomic fractions of the Ni@Ni2P-Ru HNRs as a function of photon energy (e)[108], Ni2p XPS comparison (f) and Ni L edge XANES comparison between Ni5P4-Ru and Ni5P4 (g), XANES (h) and EXAFS (i) results of Ni5P4-Ru, Ni5P4, Ni foil, and NiO at Ni K edge, respectively, Ru K-edge XAFS spectra (j) and the Ru K-edge k2-weighted EXAFS profiles of Ru foil, Ni5P4-Ru, and RuO2 (k)[97]
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