铂基金属间化合物纳米晶的最新进展：可控合成与电催化应用

doi:10.3866/PKU.WHXB202003047

物理化学学报 >> 2020, Vol. 36 >> Issue (9): 2003047.doi: 10.3866/PKU.WHXB202003047

所属专题：精准纳米合成

铂基金属间化合物纳米晶的最新进展：可控合成与电催化应用

杨天怡¹, 崔铖¹, 戎宏盼¹^,*(), 张加涛¹, 王定胜²^,*()

¹ 北京理工大学材料学院，结构可控先进功能材料与绿色应用北京市重点实验室，北京 100081
² 清华大学化学系，北京 100084

收稿日期:2020-03-19 录用日期:2020-04-17 发布日期:2020-04-24
通讯作者: 戎宏盼,王定胜 E-mail:rhp@bit.edu.cn;wangdingsheng@mail.tsinghua.edu.cn
作者简介:戎宏盼，2015年获清华大学博士学位；现任北京理工大学材料学院特别副研究员。主要从事金属纳米材料的制备与应用、单原子材料制备及电催化性能研究|王定胜，2009年获清华大学化学系博士学位；国家优秀青年基金获得者，现任清华大学化学系副教授，博导。主要从事纳米材料制备与性能、金属纳米催化研究
基金资助:
北京理工大学青年教师学术启动计划;中国国家重点研发计划(2018YFA0702003);中国国家重点研发计划(2016YFA0202801);国家自然科学基金(51631001);国家自然科学基金(51872030);国家自然科学基金(51702016);国家自然科学基金(51902023);国家自然科学基金(21801015);国家自然科学基金(21890383);国家自然科学基金(21671117);国家自然科学基金(21871159);北京市科学技术委员会(Z191100007219003)

Recent Advances in Platinum-based Intermetallic Nanocrystals: Controlled Synthesis and Electrocatalytic Applications

Tianyi Yang¹, Cheng Cui¹, Hongpan Rong¹^,*(), Jiatao Zhang¹, Dingsheng Wang²^,*()

¹ Beijing Key Laboratory of Construction-Tailorable Advanced Functional Materials and Green Applications, School of Materials Science & Engineering, Beijing Institute of Technology, Beijing 100081, P. R. China
² Department of Chemistry, Tsinghua University, Beijing 100084, P. R. China

Received:2020-03-19 Accepted:2020-04-17 Published:2020-04-24
Contact: Hongpan Rong,Dingsheng Wang E-mail:rhp@bit.edu.cn;wangdingsheng@mail.tsinghua.edu.cn
Supported by:
The project was supported by the Beijing Institute of Technology Research Fund Program for Young Scholars, China;the National Key R&D Program of China(2018YFA0702003);the National Key R&D Program of China(2016YFA0202801);the National Natural Science Foundation of China(51631001);the National Natural Science Foundation of China(51872030);the National Natural Science Foundation of China(51702016);the National Natural Science Foundation of China(51902023);the National Natural Science Foundation of China(21801015);the National Natural Science Foundation of China(21890383);the National Natural Science Foundation of China(21671117);the National Natural Science Foundation of China(21871159);the Beijing Municipal Science & Technology Commission, China(Z191100007219003)

摘要/Abstract

摘要：

铂基金属间化合物纳米晶因其高度有序的结构特点，优异的抗氧化及耐腐蚀性能，作为电极材料被广泛应用于各类电催化反应，目前已有的PtCo金属间化合物纳米晶在燃料电池阴极反应(氧还原反应)中的活性和稳定性均达到了美国能源部(DOE) 2020年的目标。为了进一步提高金属间化合物纳米晶的电催化性能，需要对影响纳米晶电催化性能的因素进行深入研究。本文综述了铂基金属间化合物纳米晶的研究现状，着重介绍了铂基金属间化合物的可控合成策略及其在电催化领域的最新研究进展，分析总结了该领域存在的问题，并展望了其未来发展方向。

关键词: 铂基金属间化合物, 纳米晶, 可控合成, 结构有序, 电催化反应

Abstract:

Fuel cells, whose energy source can be hydrogen, formic acid, methanol, or ethanol, have received considerable attention in recent years because of their environmentally friendly characteristics. A high Pt loading is often required to achieve a practical power density in fuel cells, thus leading to high costs and limited applications. Meanwhile, the high Pt loading promotes aggregation during cycling under harsh electrocatalytic conditions, which reduces the surface area of the catalyst and leads to a decrease in catalytic activity. The formation of alloy or intermetallic nanocrystals via the addition of non-precious metals along with precious metals is one strategy to effectively reduce the cost. Due to the electronic and geometric effects introduced by the non-precious metals, the catalytic performance of these bimetallic nanocrystals can be retained or even improved. Compared to the metallic alloy nanocrystals, the intermetallic ones are more stable in critical catalytic conditions. Due to their highly ordered structures, Pt-based intermetallic nanocrystals are widely used as electrode materials for various electrocatalytic reactions in fuel cells, and they show high stability against oxidation and etching. PtCo intermetallic nanocrystals have attained performances that exceed the 2020 target of the U.S. Department of Energy (DOE) for Pt activity and stability for the cathode reaction of fuel cells (oxygen reduction reaction). Decreasing the size of intermetallic compounds to the nanometer scale can significantly increase their active site densities due to the large specific surface area. However, the preparation of intermetallic nanocrystals is more complicated than that of alloys. Therefore, to further improve the electrocatalytic properties of intermetallic nanocrystals, an in-depth study of the factors affecting the electrocatalytic properties of nanocrystals is necessary. This review summarizes recent advances in Pt-based intermetallic nanocrystals. First, we highlight the controlled synthesis strategies, including direct liquid-phase synthesis, the thermal annealing approach, and chemical vapor deposition. Of these strategies, direct liquid-phase synthesis is the most common approach to prepare the intermetallic nanocrystals. Second, the diverse potential applications of different electrocatalytic reactions are summarized. The reactions include the hydrogen evolution reaction (HER), oxygen reduction reaction (ORR), and hydrogen oxidation reaction (HOR), as well as the oxidation reactions of formic acid (FAOR), methanol (MOR), and ethanol (EtOR). Of these reactions, ORR is the most important, and it has been widely studied. Some advanced characterization techniques and machine learning research based on density functional theory (DFT) are also mentioned. Finally, the challenges and the future perspectives of intermetallic nanocrystals are outlined.

Key words: Platinum-based intermetallic compounds, Nanocrystals, Controlled synthesis, Structure-ordered, Electrocatalytic reactions

杨天怡, 崔铖, 戎宏盼, 张加涛, 王定胜. 铂基金属间化合物纳米晶的最新进展：可控合成与电催化应用[J]. 物理化学学报, 2020, 36(9), 2003047. doi: 10.3866/PKU.WHXB202003047

Tianyi Yang, Cheng Cui, Hongpan Rong, Jiatao Zhang, Dingsheng Wang. Recent Advances in Platinum-based Intermetallic Nanocrystals: Controlled Synthesis and Electrocatalytic Applications[J]. Acta Physico-Chimica Sinica 2020, 36(9), 2003047. doi: 10.3866/PKU.WHXB202003047

链接本文: https://www.whxb.pku.edu.cn/CN/10.3866/PKU.WHXB202003047

https://www.whxb.pku.edu.cn/CN/Y2020/V36/I9/2003047

图/表 13

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表2

图1

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表3

近年在各类电催化反应中性能优异的铂基金属间化合物催化剂的电化学性能"

	Ref.	Pt (w, %)	Main catalytic performances					Electrolyte/(mol?L^?1)
	Ref.	Pt (w, %)	η/(mV@10 mA?cm^?2) vs RHE	Tafel slope/(mV?decade^?1)	SA/(mA?cm^?2)	MA/(A?mg^?1)	Cycling tests	Electrolyte/(mol?L^?1)
HER	Lim, 2019	86.72	27	43.3	145.2 @ 50 mV	0.55 @ 50 mV	Retain ~95% in current	0.5 H₂SO₄
	Pt₃Ga ⁶⁸	(ICP-MS)					density (10000 cycle)
	^#Li, 2019	1	32.7	32.3	17.17 @ 50 mV	1.305 @ 50 mV	The η reduced by 2.3 mV (2000 cycle)	0.1 HClO₄
	Pt/Ti₃C₂T_x ⁶¹	(ICP-MS)
	^#Lim, 2019	76.4	53	37	56.2 @ ?0.1 V	0.3678 @ ?0.1 V	No obvious loss of performance (10000 cycle)	0.5 H₂SO₄
	Pt₃Ge ⁶⁹	(ICP-MS)
	Maccio, 2005,	–	150	121	–	/	–	1 NaOH
	PtHo ⁷⁰
	^*Pt black,	–	30	47.6	137.6 @ 50 mV	0.45 @ 50 mV	–	0.5 H₂SO₄
	7440-06-4 ⁶⁸
	^*Pt/C, 599002 ⁶⁸	20	31	51.4	104.1 @ 50 mV	1.7 @ 50 mV	The η reduced by 7 mV (10000 cycle) ⁵⁷	0.5 H₂SO₄
	^*commercial Pt/Vulcan ⁶¹	20	55.8	–	1.79 @ 50 mV	0.397 @ 50 mV	–	0.1 HClO₄
	Ref.	Pt : M	HOR onset potential/V	Tafel slope/(mV?decade^?1)	CO-tolerance		Cycling tests	Electrolyte
HOR	^#Liu, 2011	Pt : Fe =	0 V vs SCE (1000 ppm CO, balance H₂)	–	Exhibit sharp CO oxidation peaks		No obvious loss of catalytic performance (500 cycles)	0.5 H₂SO₄
	Pt₃Fe@Pt ⁹⁰	63 : 37
	Innocente 2007,	Pt : Sb =	–	57	CO-covered PtSb surfaces achieved current densities higher than equivalent Pt surfaces		–	0.15 HClO₄
	PtSb ⁸⁹	1 : 1
	Ref.	Pt (w, %)	Half-wave potential/V vs RHE	Electrochemical active surface area/(m²?g^?1)	SA/(mA?cm^?2)	MA/(A?mg^?1) @ 0.9 V	Cycling tests	Electrolyte/(mol?L^?1)
ORR	^#Li, 2019, L1₀-CoPt@Pt ²²	8 (ICP-MS)	–	26.4	8.26 @ 0.9 V	2.26	18% MA loss (30000 cycles)	0.1 HClO₄
	^#Wang, 2018	–	0.92	45	5.1 @ 0.85 V	1.15	Half wave potential loss	0.1 HClO₄
	Pt₃Co ⁷⁴						12 mV (30000 cycles)
	^#Xiao, 2018	–	–	–	–	4.93	Half wave potential loss	0.1 HClO₄
	PdFe@Pt ⁸⁰						6 mV (10000 cycles)
	^#Kuttiyiel, 2018,	–	0.9	–	0.53 @ 0.9 V	0.68	Half wave potential loss	0.1 HClO₄
	L1₀-AuPtCo@Pt ⁷⁸						7 mV (10000 cycles)
	^#Xiong, 2018,	35.49	0.943	51	1.1 @ 0.9 V	0.5	Half wave potential loss	0.1 HClO₄
	Pt₃Co/C ⁷⁶	(TGA)					25 mV (4000 cycles)
	^#Wang, 2017,	–	–	58.8	4.33 @ 0.9 V	2.55	15.4% loss of	0.1 HClO₄
	PdCuB₂@Pt-Cu ³⁰						activity(10000 cycles)
	^#Bu, 2016,	–	–	55	7.8 @ 0.9 V	4.3	7.7% loss of mass activity	0.1 HClO₄
	PtPb@Pt ⁴³						(50000 cycles)
	^#Chung, 2015, fct-	–	–	–	2.3 @ 0.9 V	1.6	A little ESCA is lost	0.1 HClO₄
	PtFe@N-C ⁶⁷						(10000 cycles)
	^#Li, 2015, fct?FePt ⁵⁷	–	0.927	–	3.16 @ 0.9 V	0.69	Fe : Pt ratio reduced from	0.5 H₂SO₄
							50 : 50 to 47 : 53
							(20000 cycles)
	^#Wang, 2014, AuCu@Pt ⁷⁹	2.8 (XRF)	–	–	0.37 @ 0.9 V	0.56	29% MA loss	0.1 HClO₄
							(10000 cycles)
	^#Na, 2008,	9.3 (TGA)	0.791	129.4	–	0.296	11% MA loss	0.1 HClO₄
	Pt/ITO/CB ⁶⁶						(3000 cycles)
	Ref.	Pt (w, %)	Main catalytic performances					Electrolyte/(mol?L^?1)
	Ref.	Pt (w, %)	η/(mV@10 mA?cm^?2) vs RHE	Tafel slope/(mV?decade^?1)	SA/(mA?cm^?2)	MA/(A?mg^?1)	Cycling tests	Electrolyte/(mol?L^?1)
FAOR	^*Commercial Pt/C ²¹	–	–	–	0.22 @ 0.9 V	0.12	85% MA loss	0.1 HClO₄
							(30000 cycles)
	^*Pt/C Tanaka Kikinzoku ⁷⁸	46.6	0.86	–	0.25 @ 0.9 V	0.22	Half wave potential loss	0.1 HClO₄
							12 mV (10000 cycles)
	^*Pt/C(Johnson Matthey Co.) ⁶⁷	20	–	–	0.22 @ 0.9 V	0.14	The ESCA decreased significantly (10000 cycles)	0.1 HClO₄
	^*Pt catalyst	18.6	0.872	81.8	–	> 0.9	Half wave potential loss	0.1 HClO₄
	(HiSPEC 2000) ⁶⁶						65 mV (3000 cycles)
	^#Rong, 2016, Pt₃Sn ²⁶	–	–	5.1	27.6	1.7	lost about 5% of initial peak current density,	0.1 HClO₄
	^#Zhang, 2012, fct-FePtAu ⁵⁸	–	?0.2 vs Ag/AgCl	–	–	2.8099	Retain 92.5% of this MA(13 h)	0.5 H₂SO₄
	^#Abe, 2008, Pt₃Ti ³⁵	–	0.05 vs Ag/AgCl	–	–	–	–	0.1 H₂SO₄
	^*Commercial Pt/C ²⁶	20	–	70.9	–	–	Lost about 80% of initial peak current density	0.1 HClO₄
	Ref.	Pt (w, %)	Oxidation onset potential/V	Electrochemical active surface area/(m²?g^?1)	SA/(mA?cm^?2)	MA/(A?mg^?1)	Cycling tests	Electrolyte/(mol?L^?1)
MOR	^#Wang, 2019,	–	0.39 vs RHE	53	1.3	0.69	–	0.1 HClO₄
	PtFe@PtRuFe ³³
	^#Feng, 2019,	–	–	–	7.195	1.09	The loss of peak current density is negligible	0.5 H₂SO₄
	₃Ga@Pt ⁴⁴						(1000 cycles)
	^#Feng, 2017,	/	/	60.5	–	–	–	0.1 HClO₄
	Au@Ag₂S@Pt 102
	^#Qi, 2017,	/	0.154 vs Ag/AgCl	–	1.08	0.612	3% SA loss	0.5 H₂SO₄
	PtZn/MWNT ³¹						(1000 cycles)
	^*Commercial Pt/C(JM) ³³	20	0.83 vs RHE	71	0.15	0.11	–	0.1 HClO₄
	^*Commercial PtRu/C ³³	/	0.43 vs RHE	49	0.83	0.41	–	0.1 HClO₄
	^*Commercial	/	0.247 vs Ag/AgCl	–	–	–	50% SA loss	0.5 H₂SO₄
	Pt/Vulcan ³¹						(1000 cycles)
	Ref.	Pt (w, %)	Oxidation onset potential/V	Completely oxidizes ethanol to CO₂	SA/(mA?cm^?2)	MA/(A?mg^?1)	Cycling tests	Electrolyte/(mol?L^?1)
EtOR	^#Yuan, 2018, PtBi@Pt³²	–	–	–	136.5 vs RHE	5.95	No significant change in the size and shape (10000 s)	1 NaOH
	^#Zhang, 2016, Pt₃Co@Pt ¹⁰⁴	–	–	No	–	0.79	–	0.1 HClO₄
	^#Kodiyath, 2015, Pt₃Ta ¹¹¹	–	0.27 V vs Ag/AgCl	Yes	–	–	Retain 85% in ESCA (10000 cycles)	0.5 H₂SO₄
	^*Commercial	20	–	–	22.2 vs RHE	0.689	Serious aggregation	1 NaOH
	Pt/C ³²						(10000 s)

表3

图5

图6

图7

图8

图9

图10

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Characteristic	Units	2020 Targets
Cost	＄·kW^-1	3
Mass activity	A·mg^-1 @ 900 mV	0.44
Loss in initial catalytic activity	% mass activity loss	< 40
Electrocatalyst support stability	% mass activity loss	0.44
Platinum group metal total loading (both electrodes)	mg·cm^-2 electrode area	0.125
Rated power (150 kPa)	mW·cm^-2	1000

Method	Catalysts	Surfactants & solvents	Metal precursor		Reaction time/h	Reaction temperature/℃	Ref.	Year
Method	Catalysts	Surfactants & solvents	A	B	Reaction time/h	Reaction temperature/℃	Ref.	Year
Solvothermal reactions	Pt₃Sn	PVP, DMF	Pt(acac)₂	SnCl₂	6	180	26	2016
	PtZn	PVP, DMF	Pt(acac)₂	Zn(acac)₂	9	180	38	2014
Oil phase synthesis	Pt₄₅Sn₂₅Bi₃₀	ODE, OAm, AA, CTAB	Pt(acac)₂	SnCl₂, Bi(act)₃	1	220	45	2019
	Pt₃Ga@Pt	ODE, OAm	Pt(acac)₂	GaCl₃	12	300	44	2018
	PtPb	ODE, OAm, AA	Pt(acac)₂	Pb(acac)₂	5	160	43	2016
Polyol process	PtSn/ATO	EG	H₂PtCl₆	SnCl₄	3	200	41	2019
	PtBi/Pt	PVP, DEG	Pt(acac)₂	C₃₀H₅₇BiO₆	0.5	150	32	2018
	PtSn	TEG	K₂PtCl₆	SnCl₂	0.5	550	42	2008
	PtPb	TEG	K₂PtCl₆	Pb(C2H3O2)₂	0.5	550	42	2008
	PtBi	TEG	K₂PtCl₆	Bi(NO₃)₃	0.5	550	42	2008
	FePt₃	TEG	K₂PtCl₆	FeCl₃	0.5	550	42	2008
Method	Catalysts	Metal precursor			Reaction time/h	Reaction temperature/℃	Ref.	Year
Method	Catalysts	A		B	Reaction time/h	Reaction temperature/℃	Ref.	Year
Annealing	PtZn/HNCNT	H₂PtCl₆		ZnO	1	800	56	2019
	Pt₃Ti	Pt(NH₃)₄(NO₃)₂		TiH₂	0.5	700	61	2019
	L1₀-CoPt	Pt(acac)₂		Co(acac)₂	6	650	22	2019
	L1₀-FePt	Pt(acac)₂		Fe(CO)₅	6	700	57	2015
	FeCuPt	Pt(acac)₂		Cu(acac)₂, Fe(CO)₅	1	220	59	2014
	Pt₃Co/C	H₂PtCl₆		CoCl₂	2	700	49	2012
	fct-FePtAu	Pt(acac)₂		Fe(CO)₅, HAuCl₄	1	600	58	2012
	FePt/MgO	Pt(acac)₂		Fe(CO)₅	6	750	46	2010
CVD	Pt₃Co	H₂PtCl₆		Co(acac)₂	6	550	70	2015
	PtGe	Pt(NH₃)₄Cl₂		Ge(acac)₂Cl₂	1	550	69	2000

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铂基金属间化合物纳米晶的最新进展：可控合成与电催化应用

Recent Advances in Platinum-based Intermetallic Nanocrystals: Controlled Synthesis and Electrocatalytic Applications

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