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Preparation of layered metal organic framework material nano-array water oxidation electrocatalyst using LDH as template

A nano-array and layered structure technology, applied in the three-dimensional field with highly regular arrangement, can solve the problems of increased contact resistance of active sites, reduced catalytic activity, high energy consumption and structural loss of MOFs derived materials

Inactive Publication Date: 2019-04-19
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The main technical problem to be solved by the present invention is to overcome the shortcomings of low active site utilization and reduced catalytic activity of general MOFs-based water oxidation electrocatalysts due to poor orientation and conductivity, and avoid the disadvantages of conventional powder electrode preparation process. The introduction of conductive agents and binders leads to the coverage of active sites and increased contact resistance, as well as the high energy consumption and structural loss of MOFs derived materials. NiFe-LDH nanoarrays with easy-to-control composition and morphology are used as precursors and In situ growth of templates directly on conductive substrates to prepare highly regular 3D layered Fe 0.1 -Ni-MOF nanoarray water oxidation electrocatalyst, using doping to introduce impurity energy levels to regulate electronic configuration and induce intermetallic synergistic effects, and the formation of highly regularly arranged layered nanoarrays reduces series resistance and exposes more active sites point and promote the diffusion of electrolyte and evolved gas, as an electrocatalyst for water oxidation, exhibiting extremely high electrochemical energy conversion properties

Method used

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  • Preparation of layered metal organic framework material nano-array water oxidation electrocatalyst using LDH as template
  • Preparation of layered metal organic framework material nano-array water oxidation electrocatalyst using LDH as template
  • Preparation of layered metal organic framework material nano-array water oxidation electrocatalyst using LDH as template

Examples

Experimental program
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Effect test

example 1

[0023] 1) Preparation A: Ni(NO 3 ) 2 ·6H 2 O (2.025 mmol), Fe(NO 3 ) 3 9H 2 O (0.225 mmol), CO (NH 2 ) 2 (10mmol) and NH 4 F (4 mmol), dissolved in 40 mL deionized water, stirred evenly, one piece size is 2×3 cm 2 Nickel foam (NF) was pretreated with 5% dilute hydrochloric acid, deionized water and absolute ethanol for 10 min of ultrasonication;

[0024] 2) Hydrothermal reaction: transfer the solution and treated NF in step 1) to a 50 mL polytetrafluoroethylene autoclave, seal the autoclave, place it in a vacuum oven, and react at 120 °C for 6 h;

[0025] 3) Washing and drying: After the reaction in step 2) is completed, put the polytetrafluoroethylene autoclave in the air to cool to room temperature, take out the NF uniformly covered by the yellow-green substance, and ultrasonically wash it with deionized water and absolute ethanol successively. After that, it was vacuum dried at 60 ℃ for 6 h to prepare the NiFe-LDH / NF precursor;

[0026] 4) Prepare material B: C ...

example 2

[0031] 1) Preparation A: Ni(NO 3 ) 2 ·6H 2 O (4.05 mmol), Fe(NO 3 ) 3 9H 2 O (0.45 mmol), CO (NH 2 ) 2 (20mmol) and NH 4 F (8 mmol), dissolved in 80 mL deionized water, stirred evenly, one piece size is 4×6 cm 2 Nickel foam (NF) was pretreated with 5% dilute hydrochloric acid, deionized water and absolute ethanol for 10 min of ultrasonication;

[0032] 2) Hydrothermal reaction: transfer the solution and treated NF in step 1) to a 100 mL polytetrafluoroethylene autoclave, seal the autoclave, place it in a vacuum drying oven, and react at 120 °C for 6 h;

[0033] 3) Washing and drying: After the reaction in step 2) is completed, put the polytetrafluoroethylene autoclave in the air to cool to room temperature, take out the NF uniformly covered by the yellow-green substance, and ultrasonically wash it with deionized water and absolute ethanol successively. After that, it was vacuum dried at 60 ℃ for 6 h to prepare the NiFe-LDH / NF precursor;

[0034] 4) Prepare material ...

example 3

[0039] 1) Preparation A: Ni(NO 3 ) 2 ·6H 2 O (4.05 mmol), Fe(NO 3 ) 3 9H 2 O (0.45 mmol), CO (NH 2 ) 2 (20mmol) and NH 4 F (8 mmol), dissolved in 80 mL deionized water, stirred evenly, one piece size is 4×6 cm 2 Nickel foam (NF) was pretreated with 5% dilute hydrochloric acid, deionized water and absolute ethanol for 10 min of ultrasonication;

[0040] 2) Hydrothermal reaction: transfer the solution and treated NF in step 1) to a 100 mL polytetrafluoroethylene autoclave, seal the autoclave, place it in a vacuum drying oven, and react at 120 °C for 6 h;

[0041] 3) Washing and drying: After the reaction in step 2) is completed, put the polytetrafluoroethylene autoclave in the air to cool to room temperature, take out the NF uniformly covered by the yellow-green substance, and ultrasonically wash it with deionized water and absolute ethanol successively. After that, it was vacuum dried at 60 ℃ for 6 h to prepare the NiFe-LDH / NF precursor;

[0042] 4) Prepare material ...

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Abstract

The invention discloses a preparation method of a three-dimensional layered structure Fe-doped Ni-MOF nano-array (Fe0.1-Ni-MOF / NF) which is grown in situ on foamed nickel and has high regular array. Nickel foam is used as a conductive substrate. The NiFe-LDH nano-array (NiFe-LDH / NF) firstly grows by a hydrothermal method, and then terephthalic acid is used as an organic ligand to convert a NiFe-LDH / NF precursor template to Fe0.1-Ni-MOF / NF by a solvothermal method, and the product is used as an electrocatalyst for water oxidation reaction. The electrocatalyst shows excellent catalytic activity(eta 100mA cm-2=263mV) in 1M KOH electrolyte, which is much better than undoped Ni-MOF / NF material (eta 100mA cm-2=298mV). The invention fully utilizes the doping introduction impurity level to regulate the electronic configuration and induce the synergy effect between metals, and the highly regularly arranged layered structure nano-array reduces the series resistance, exposes more active sites and promotes the diffusion of electrolytes and evolved gases. A novel energy-transduction material with high electrocatalytic activity, good cycle stability, durability and low cost is constructed.

Description

technical field [0001] The invention relates to the preparation of metal-doped and highly regularly arranged three-dimensional layered structure metal-organic framework material nano-arrays and its application in the electrocatalysis of alkaline water oxidation reaction, especially to the in-situ growth on nickel foam (NF) Nickel-iron layered double hydroxide (NiFe-LDH / NF), and then by solvothermal treatment of NiFe-LDH / NF to prepare self-supporting iron-doped nickel-based organic framework material nanoarrays (Fe 0.1 -Ni-MOF / NF), and the application of this material in the field of electrocatalytic energy conversion. High-performance water oxidation electrocatalysts can be prepared only by a simple, controllable, environmentally friendly and economical synthesis method. Background technique [0002] Since modern times, due to the high dependence and over-exploitation of traditional fossil fuels, the global environment has continued to deteriorate, and the energy crisis has...

Claims

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Application Information

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IPC IPC(8): C25B11/06C25B1/04C25B11/03
CPCC25B1/04C25B11/031C25B11/091Y02E60/36
Inventor 姚亚东杨林朱贵磊文豪张节官鑫孙逊田文丽郑登超
Owner SICHUAN UNIV
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