自组装制备PtIr合金气凝胶及其高效电催化氨氧化性能

doi:10.15541/jim20220684

无机材料学报 ›› 2023, Vol. 38 ›› Issue (5): 511-520.DOI: 10.15541/jim20220684

自组装制备PtIr合金气凝胶及其高效电催化氨氧化性能

张祥松(), 刘业通, 王永瑛, 武子瑞, 刘振中, 李毅(), 杨娟()

江苏大学材料科学与工程学院, 镇江 212013

收稿日期:2022-11-16 修回日期:2023-01-04 出版日期:2023-01-11 网络出版日期:2023-01-11
通讯作者: 李毅, 讲师. E-mail: liyi5482@ujs.edu.cn;
杨娟, 教授. E-mail: yangjuan6347@ujs.edu.cn
作者简介:张祥松(1996-), 男, 硕士研究生. E-mail: jsdaujszxs1996@163.com
基金资助:
国家自然科学基金(51972150);江苏省自然科学基金(SBK20210769);中国博士后科学基金(2022M711543);江苏大学2022年大创项目(202210299366X)

Self-assembled Platinum-iridium Alloy Aerogels and Their Efficient Electrocatalytic Ammonia Oxidation Performance

ZHANG Xiangsong(), LIU Yetong, WANG Yongying, WU Zirui, LIU Zhenzhong, LI Yi(), YANG Juan()

School of Materials and Engineering, Jiangsu University, Zhenjiang 212013, China

Received:2022-11-16 Revised:2023-01-04 Published:2023-01-11 Online:2023-01-11
Contact: LI Yi, lecturer. E-mail: liyi5482@ujs.edu.cn;
YANG Juan, professor. E-mail: yangjuan6347@ujs.edu.cn
About author:ZHANG Xiangsong (1996-), male, Master candidate. E-mail: jsdaujszxs1996@163.com
Supported by:
National Natural Science Foundation of China(51972150);Natural Science Foundation of Jiangsu Province(SBK20210769);China Postdoctoral Science Foundation(2022M711543);2022 Creative Project of Undergraduate Student at Jiangsu University(202210299366X)

摘要/Abstract

摘要：

氨具有低成本、易液化和高体积能量密度等特点, 是一种有吸引力的无碳燃料, 用其制成的直接氨燃料电池也备受科研人员青睐, 却受限于阳极氨氧化缓慢的动力学过程。本工作采用无表面活性剂的简单方法通过纳米颗粒(NPs)自组装制备了三维多孔网络结构的PtIr合金气凝胶高效氨氧化催化剂。该结构提供了丰富开放的互联质子传输通道和额外的催化活性位点, 有助于氨电催化氧化中NH₃分子的去质子化过程。当Pt和Ir物质的量比为80/20时, PtIr合金气凝胶展现出最优的氨氧化(AOR)催化活性。实验通过研究NH₃浓度和工作温度对催化剂氨氧化性能的影响发现, Pt₈₀Ir₂₀合金气凝胶催化剂的AOR性能随着氨水浓度或温度的上升而增强, 如当氨水浓度为0.5 mol/L时, 合金催化剂在0.5 V电位下的质量比活性为44.03 A·g^-1, 约是0.05 mol/L 氨水中的4倍。当温度上升至80 ℃ 时, 合金催化剂在0.5 V电位下的质量比活性为148.73 A·g^-1, 约为25 ℃下的12倍。在此温度变化区间, 其AOR起始电位下降了40 mV。利用Arrhenius方程计算发现, Pt₈₀Ir₂₀合金气凝胶催化剂的AOR反应活化能比商业Pt/C催化剂降低了~9.43 kJ·mol^-1。此外, 催化材料的稳定性测试结果表明, Pt₈₀Ir₂₀合金气凝胶催化剂经2000次循环伏安测试后的峰值质量比活性损失为~50.6%, 优于商业Pt/C催化剂(~74.9%)。

关键词: 自组装, PtIr合金, 气凝胶, 电催化氨氧化反应

Abstract:

Ammonia with low cost, easily liquefied and high volumetric energy density is an attractive carbon-free fuel. Utilizing ammonia as anodic fuel, direct ammonia fuel cells are showing great interests to researchers. However, such amazing fuel cell device is limited by the sluggish anodic ammonia oxidation reaction. In this work, PtIr alloy aerogels with a three-dimensional porous network structure were prepared by nanoparticles (NPs) self-assembled under a simple and surfactant-free conditions. This structure provided a rich open interconnected proton transport channel and additional catalytically active sites which contributed to the dehydrogenation process of NH₃ molecules in ammonia electrocatalytic oxidation. An optimal AOR activity was achieved at the 80/20 molar ratio of Pt/Ir. Effects of NH₃ concentration and operating temperature on catalyst's ammonia oxidation performance were studied, which revealed that the AOR performance of Pt₈₀Ir₂₀ alloy aerogel was improved with the increase of ammonia concentration or operating temperature. For example, the mass specific activity, at 0.50 V of the Pt₈₀Ir₂₀ alloy aerogel, was estimated to be 44.03 A·g^-1, which was about 4 times as that of the ammonia concentration at 0.05 mol/L. In the case of operating temperature effect, the mass activity was estimated to be 148.73 A·g^-1, which was almost 12 times as that of the temperature rising (from 25 ℃) to 80 ℃. Encouragingly, the onset potential of the optimal Pt₈₀Ir₂₀ alloy aerogel catalyst displayed about 40 mV reduction during such a temperature change. Further calculations using the Arrhenius equation showed that its activation energy was reduced by about 9.43 kJ·mol^-1 as compared with commercial Pt/C. Moreover, its AOR stability was improved as evidenced by a loss of ~50.6% mass activity after 2000 potential cycles when compared with commercial Pt/C (~74.9%).

Key words: self-assembly, PtIr alloy, aerogel, electrocatalytic ammonia oxidation reaction

中图分类号:

O646

张祥松, 刘业通, 王永瑛, 武子瑞, 刘振中, 李毅, 杨娟. 自组装制备PtIr合金气凝胶及其高效电催化氨氧化性能[J]. 无机材料学报, 2023, 38(5): 511-520.

ZHANG Xiangsong, LIU Yetong, WANG Yongying, WU Zirui, LIU Zhenzhong, LI Yi, YANG Juan. Self-assembled Platinum-iridium Alloy Aerogels and Their Efficient Electrocatalytic Ammonia Oxidation Performance[J]. Journal of Inorganic Materials, 2023, 38(5): 511-520.

图/表 20

图1 Pt100-xIrx合金气凝胶的合成流程图和机理图

Fig. 1 Diagram of preparation process and chemical mechanisms of Pt100-xIrx alloy aerogels

图S1 Pt80Ir20气凝胶的SEM照片

Fig. S1 SEM image of Pt80Ir20 aerogel

图2 Pt80Ir20合金气凝胶的结构和形貌表征

Fig. 2 Structure and composition of Pt80Ir20 alloy aerogel (a, b) TEM images; (c) HR-TEM image; (d) HAADF-STEM image and corresponding mapping images

图S2 Pt气凝胶的TEM照片

Fig. S2 TEM images of Pt aerogel

图S3 Pt80Ir20合金的TEM照片

Fig. S3 TEM images of Pt80Ir20 alloy

图S4 Pt80Ir20合金气凝胶的EDS能谱及其质量比和原子比

Fig. S4 EDS spectrum of Pt80Ir20 aerogel catalyst with inset showing its mass and atom ratios

图3 不同催化剂的XRD谱图(a)及其局部(2θ=35°~50°)XRD放大图谱(b)

Fig. 3 (a) XRD patterns of different catalysts, commercial Pt/C, and (b) corresponding enlarged XRD patterns in the range of 2θ=35°-50°

图4 (a)Pt80Ir20合金气凝胶的XPS全谱图, (b)不同样品的Pt4f XPS谱图, (c)Pt80Ir20合金气凝胶的Ir4f XPS谱图

Fig. 4 (a) XPS survey spectrum of Pt80Ir20 aerogel, (b) Pt4f XPS spectra of various Pt-based catalysts, and (c) Ir4f XPS spectrum of Pt80Ir20 aerogel

表S1 不同样品的XPS测试元素含量(%, 原子分数)

Table S1 Elemental quantification (%, in atom) determined by XPS for different Pt100-xIrx aerogel catalysts

Sample	Pt/%	Ir/%	Pt/Ir
Pt₅₅Ir₄₅	54.33	45.67	1.19
Pt₇₀Ir₃₀	67.24	32.76	2.05
Pt₈₀Ir₂₀	79.34	20.66	3.84
Pt₈₇Ir₁₃	88.36	11.64	7.59

表S2 不同样品与商业Pt/C样品Pt4f结合能的对比

Table S2 Comparison of binding energy between Pt4f with different Pt-based catalysts

Sample	Pt4f_5/2/eV	∆₁/eV	Pt4f_7/2/eV	∆₂/eV
Commercial Pt/C	75.10	-	71.70	-
Pt₈₇Ir₁₃ aerogel	74.85	-0.25	71.53	-0.17
Pt₈₀Ir₂₀ aerogel	74.88	-0.22	71.50	-0.20
Pt₇₀Ir₃₀ aerogel	74.92	-0.18	71.53	-0.17
Pt₅₅Ir₄₅aerogel	74.93	-0.17	71.57	-0.13

图5 (a)不同催化剂室温下的AOR催化CV曲线, (b)不同催化剂在0.5 V电极电势下的AOR活性对比, (c)Pt, Ir和Pt80Ir20纳米颗粒的最高占据分子轨道(HOMO)和最低未占据分子轨道(LUMO)的能量差, (d)Pt80Ir20合金纳米颗粒与Pt80Ir20合金气凝胶的电催化氨氧化示意图, (e)优选Pt80Ir20合金气凝胶催化剂在有/无NH3条件下的CV曲线, (f)不同催化剂的恒电位曲线

Fig. 5 (a) CV curves of Pt100-xIrx aerogels and commercial Pt/C catalysts under room temperature, (b) AOR activity comparison for Pt100-xIrx aerogels and commercial Pt/C catalysts at 0.5 V(vs. RHE), (c) energy difference between the highest occupied molecular orbital (HOMO) and the lowest unoccupied molecular orbital (LUMO) of Pt, Ir and Pt80Ir20 nanoparticles, (d) schematic diagram of electrocatalytic ammonia oxidation of Pt80Ir20 alloy nanoparticles and Pt80Ir20 alloy aerogel, (e) CV curves of the Pt80Ir20 catalyst in the presence and absence of NH3; (f) CA curves of Pt100-xIrx aerogels and commercial Pt/C catalysts Colorful figures are available on website

表S3 不同样品的AOR性能对比

Table S3 Comparison of AOR activity between different catalysts

Sample	Onset potential/V	Mass activity at 0.5 V (vs. RHE)/(mA·mg_PGM^-1)	Peak mass activity/ (mA·mg_PGM^-1)	Ref.
Pt₈₇Ir₁₃ aerogel	0.411	4.7	53.7	This work
Pt₈₀Ir₂₀ aerogel	0.368	19.4	86.3	This work
Pt₇₀Ir₃₀ aerogel	0.361	8.9	31.5	This work
Pt₅₅Ir₄₅aerogel	0.358	6.4	24.8	This work
Pt	0.511	1.1	31.5	This work
Ir	0.354	12.0	14.6	This work
Commercial Pt/C	0.495	8.4	62.9	This work
Commercial PtIr/C	0.428	10.4	25.1	[S1]
Ir-decorate Pt NCs/C	~ 0.43	-	100	[S2]
Polycrystalline PtIr	~ 0.41	-	-	[S3]
PtRh/C(Pt:Rh = 9:1)	0.44	9.0	93.8	[S4]
Pt-decorated Ni particles	~0.50	-	75.3	[S5]

图S5 Pt，Pt80Ir20气凝胶的电化学活性面积

Fig. S5 Electrochemical active surface area of Pt, Pt80Ir20 aerogels

图S6 Pt(紫罗兰色)，Pt80Ir20(蓝色)气凝胶以及商业Pt/C催化剂(灰色)的EIS阻抗曲线

Fig. S6 Nyquist plots of EIS spectra measured for Pt (violet), Pt80Ir20 aerogel (blue) and commercial Pt/C (gray) in 1.0 mol/L KOH electrolyte at the open circuit potential

图6 2000次CV循环后的电化学活性面积以及室温AOR性能对比

Fig. 6 Electrochemical active areas of catalysts and AOR performance before and after 2000 CV cycles (a, d) Pt80Ir20 aerogel; (b, e) Pt80Ir20 nanoparticles; (c, f) Commercial Pt/C

图S7 2000次循环稳定性测试前后的Pt80Ir20气凝胶XRD谱图

Fig. S7 XRD patterns of Pt80Ir20 aerogel before and after 2000 cycle stability tests

图S8 2000次循环稳定性测试(a)前(b)后的Pt80Ir20气凝胶TEM照片

Fig. S8 TEM images of Pt80Ir20 aerogel (a) before and (b) after 2000 cycle stability tests

图7 (a)不同NH3浓度下的Pt80Ir20合金气凝胶催化剂的AOR性能, (b)不同NH3浓度(mol/L)下, Pt80Ir20合金气凝胶与商业Pt/C在0.5 V(vs. RHE)电位下AOR活性对比, 不同NH3浓度下的Pt80Ir20合金气凝胶(c)与商业Pt/C(d)在0.65 V(vs. RHE)电位下的CA曲线

Fig. 7 (a) CV curves of the Pt80Ir20 aerogel tested in different NH3 concentrations, (b) AOR activity comparison for Pt80Ir20 aerogel and commercial Pt/C in different NH3 concentrations at 0.5 V(vs. RHE), and (c, d) CA curves of the Pt80Ir20 aerogel (c) and commercial Pt/C (d) at 0.65 V(vs. RHE)

图S9 不同NH3浓度下商业Pt/C的AOR性能

Fig. S9 CV curves of the commercial Pt/C in different NH3 concentrations

图8 (a~c)不同温度下的催化剂的AOR性能, (d)商业Pt/C、Pt气凝胶与Pt80Ir20合金气凝胶在0.5 V(vs. RHE)电极电势下的AOR活性对比, (e)不同工作温度下的Pt80Ir20合金气凝胶的恒电位曲线, (f)商业Pt/C催化剂、Pt气凝胶和Pt80Ir20合金气凝胶在0.5 V(vs. RHE)电极电势下的阿仑尼乌斯图

Fig. 8 (a-c) CV curves of catalysts at different temperatures, (d) AOR activity comparison for commercial Pt/C, Pt aerogel and Pt80Ir20 aerogel catalysts at different temperatures at 0.5 V(vs. RHE), (e) CA curves of the Pt80Ir20 aerogel at different temperatures at 0.65 V (vs. RHE), (f) Arrhenius plots for NH3 oxidation on commercial Pt/C, Pt aerogel and Pt80Ir20 aerogel catalysts at 0.5 V(vs. RHE)

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自组装制备PtIr合金气凝胶及其高效电催化氨氧化性能

Self-assembled Platinum-iridium Alloy Aerogels and Their Efficient Electrocatalytic Ammonia Oxidation Performance

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