Synthesis, Structure and Electrochemical Properties of Sulfonylcalix[4]arene Supported Co16 Cluster †

doi:10.7503/cjcu20190236

Abstract

Abstract:

A new sulfonylcalix[4]arene-supported tetrahedral Co₁₆ cage cluster [Co₁₆(TC4A-SO₂)₄(OH)₄·(L)₈][(C₈H₂₀N)(C₄H₁₂N)₂(C₂H₈N)]·solvent(Abbr. Co₁₆-TC4A-SO₂) was synthesized from CoCl₂·6H₂O, p-tert-butylsulfonylcalix[4]arene(H₄TC4A-SO₂) and asymmetric 3-(1H-tetrazol-5-yl)benzoic acid(H₂L) under solvothermal condition. The complex was characterized by single crystal X-ray diffraction(XRD), powder X-ray diffraction(PXRD), thermogravimetric analysis(TGA), and infrared spectroscopy(FTIR). Directly loading Co₁₆-TC4A-SO₂ onto carbon paper(Co₁₆-TC4A-SO₂/CP) as a working electrode exhibited efficient oxygen evolution reaction(OER) catalytic performance. In 1 mol/L KOH, Co₁₆-TC4A-SO₂/CP gained a current density of 10.0 mA/cm ² at a catalytic reaction overpotential of 343.8 mV, a Tafel slope of 79.31 mV/dec, and catalytic stability for 48 h at 20.0 mA/cm ².

Key words: Sulfonylcalix[4]arene, Tetrahedral coordination cage, Electrocatalytic oxygen evolution reaction

CLC Number:

O614

TrendMD:

ZHANG Min, CHEN Mengwei, GAO Hong, BI Yanfeng. Synthesis, Structure and Electrochemical Properties of Sulfonylcalix[4]arene Supported Co₁₆ Cluster ^†[J]. Chem. J. Chinese Universities, 2019, 40(10): 2052.

Figures/Tables 5

Scheme 1 Synthetic route of Co16-TC4A-SO2

Formula	C₂₄₂H₂₆₄Co₁₆N₃₆O₆₈S₁₆	Volume/nm³	16.2702(19)
Molecular weight	6220.66	Z	2
Crystal system	Triclinic	Temperature/K	150
Space group	P $1 ˉ$	D_c/(g·cm^-3)	1.270
a/nm	2.26250(16)	μ/mm^-1	0.965
b/nm	2.38320(15)	Reflections collected	251116
c/nm	3.0258(2)	Unique data(R_int)	57738(0.059)
α/(°)	89.566(2)	GOF on F²	1.014
β/(°)	87.354(2)	$R 1 a$ [I>2σ(I)]	0.0480
γ/(°)	86.684(2)	w $R 2 b$	0.1366

Formula	C₂₄₂H₂₆₄Co₁₆N₃₆O₆₈S₁₆	Volume/nm³	16.2702(19)
Molecular weight	6220.66	Z	2
Crystal system	Triclinic	Temperature/K	150
Space group	P $1 ˉ$	D_c/(g·cm^-3)	1.270
a/nm	2.26250(16)	μ/mm^-1	0.965
b/nm	2.38320(15)	Reflections collected	251116
c/nm	3.0258(2)	Unique data(R_int)	57738(0.059)
α/(°)	89.566(2)	GOF on F²	1.014
β/(°)	87.354(2)	$R 1 a$ [I>2σ(I)]	0.0480
γ/(°)	86.684(2)	w $R 2 b$	0.1366

Fig.1 Crystal structure of Co16-TC4A-SO2 (A) Molecular structure of Co16-TC4A-SO2; (B) a tetranuclear Co4(TC4A-SO2)(OH) unit with four L ligands; (C) coordination mode of L ligand; (D) tetrahedral packing of tetranuclear units.

Fig.2 OER electrocatalytic activities of the Co16-TC4A-SO2 (A) LSV curves of the Co16-TC4A-SO2/CP with different mass loading; (B) comparison of Co16-TC4A-SO2/CP, Mixture/CP, and pure CP polarization curves; (C) Tafel plots of the electrodes; (D) prolonged chronoamperometric profiles of Co16-TC4A-SO2/CP at 343.8 mV(η10) for 12 h(a) and 373.8 mV(η20) for 48 h(b). Inset: polarization curves before(a) and after(b) 48 h-long electrocatalytic OER.

Fig.3 Nyquist plots of Co16-TC4A-SO2/CP before and after 12 h-long electrocatalytic OER(A) and plots of the charging current density against scan rates of Co16-TC4A-SO2/CP(B) Insets: (A) the equivalent circuit model for electrochemical impedance tests; (B) cyclic voltammetry curves.

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Synthesis, Structure and Electrochemical Properties of Sulfonylcalix[4]arene Supported Co₁₆ Cluster ^†

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