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Preparation method for graphite-phase carbon nitride thin film modified electrode

A graphite-phase carbon nitride and modified electrode technology, which is applied in the manufacture of circuits, electrical components, and final products, can solve problems such as uneven graphite-phase carbon nitride powder, unsatisfactory thermoelectric performance, and unstable electrode materials. Achieve good application potential, improve thermoelectric performance, and simple preparation method

Inactive Publication Date: 2016-12-07
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the graphite phase carbon nitride powder is usually prepared on the surface of the electrode material by methods such as drop coating and spin coating; the graphite phase carbon nitride powder obtained on the electrode surface is uneven and easy to fall off, resulting in uneven electrode material. Stablize
In addition, the carbon nitride powder is sol-treated (Angew.Chem.-Int.Edit., 2015, 54, 6297), or the melamine cyanuric acid mixture is sandwiched between the substrates for heat treatment (Angew.Chem., 2014, 126, 3728), or a combination of vapor deposition and microcontact printing technology (Adv.Mater., 2015,27,712) to prepare thin films, but the resulting thin films are still not uniform
In addition, the carbon nitride films obtained in the prior art are mostly used in photoelectrochemical water splitting, photoluminescence, etc. However, due to the unsatisfactory thermoelectric performance, they cannot be used for thermoelectric power generation

Method used

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preparation example Construction

[0023] A kind of preparation method of graphite phase carbon nitride film modified electrode of the present invention, comprises the following steps:

[0024] (1) Under a protective atmosphere, heat nitrogen at 450°C to 550°C (preferably 500°C to 550°C to ensure gasification and deamination of the carbon nitride raw material while preventing excessive decomposition of the formed carbon nitride precursor) Carbonize the raw material for 1 minute to 6 hours, so that the carbon nitride raw material is gasified and attached to the surface of the heat-resistant carrier to form a carbon nitride precursor;

[0025] Wherein, protective atmosphere can be nitrogen, helium, argon or its mixed gas; Carbon nitride raw material is melamine, dicyandiamide, one or more in cyanamide, urea or thiourea, and is preferably melamine, cyanogen amine or dicyandiamide to ensure that the obtained carbon nitride film has good thermoelectric properties.

[0026] The heat-resistant carrier can be graphite...

Embodiment 1

[0030] S1. Add 3g of melamine to the crucible, then wrap the crucible and place it in a tube furnace, pretreat it with nitrogen for 20 minutes, and raise the temperature to 550°C at a heating rate of 2°C / min under nitrogen atmosphere, and keep it warm 4 hours, then lowered to room temperature to complete the first heat treatment to obtain a carbon nitride precursor with a thickness of about 1.3mm, and deposited on the crucible;

[0031] S2. Use fluorine-doped tin oxide (FTO) as the substrate, put it under the crucible deposited with carbon nitride after the first heat treatment, then wrap it in a tube furnace, and pre-treat it with nitrogen gas; under nitrogen atmosphere, With a heating rate of 2°C / min, the temperature was raised to 550°C, kept for 4 hours, and then lowered to room temperature to complete the second heat treatment; a yellow film with a thickness of about 150 nm on the FTO was formed as a carbon nitride film.

Embodiment 2

[0033] S1. Add 3g of dicyandiamide to the crucible, then wrap the crucible and place it in a tube furnace, pretreat with nitrogen for 20 minutes, and raise the temperature to 500°C at a heating rate of 5°C / min under nitrogen atmosphere , keep warm for 2 hours, then lower to room temperature to complete the first heat treatment, obtain a carbon nitride precursor with a thickness of about 1.4mm, and deposit it on the crucible;

[0034] S2. Use FTO as the substrate, put it under the crucible with carbon nitride deposited after the first heat treatment, then wrap it in a tube furnace, and pre-treat it with nitrogen gas; under nitrogen atmosphere, at a heating rate of 5°C / min , raise the temperature to 500°C, keep it warm for 2 hours, and then lower it to room temperature to complete the second heat treatment; a yellow film is formed on the FTO, which is a graphitic carbon nitride film with a thickness of about 150nm.

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Abstract

The invention discloses a preparation method for a graphite-phase carbon nitride thin film modified electrode. The preparation method comprises the steps of heating a carbon nitride raw material in protective atmosphere at a temperature of 450-550 DEG C for 1min-6h firstly to gasify the carbon nitride raw material, and enabling the gasified carbon nitride raw material to be attached to the surface of a heat-resistant carrier to form a carbon nitride precursor; and then heating the heat-resistant carrier which is adhered by the carbon nitride precursor at a temperature of 500-550 DEG C for 1min-6h to gasify the carbon nitride precursor and to form a graphite-phase carbon nitride thin film with thickness of 10-150nm on the surface of a conductive substrate, and obtaining the modified electrode. According to the preparation method, a vapor deposition method is adopted to modify the graphite-phase carbon nitride thin film on the surface of the conductive substrate, thereby improving the thermoelectric property of the electrode, the uniformity and the stability of the carbon nitride thin film.

Description

technical field [0001] The invention belongs to the field of thin film preparation technology and photoelectric catalysis, and more specifically relates to a preparation method of a graphite phase carbon nitride thin film modified electrode. Background technique [0002] Since 2009, Professor Wang Xinchen of Fuzhou University first reported graphitic carbon nitride (g-C 3 N 4 ) can be used as a photocatalyst for splitting water to produce hydrogen since this milestone work, g-C 3 N 4 The related researches have received extensive attention from the scientific research community, and its core and highlights are that it is an organic photocatalyst that does not contain any metal elements. This work has added a new member to the photocatalyst family, so g-C 3 N 4 It has also become a star material in photocatalytic research. Graphite carbon nitride can also be used as a catalyst for oxygen evolution, hydrogen evolution, water decomposition, pollutant degradation, CO 2 Red...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01L31/0224H01L31/18
CPCH01L31/022425H01L31/18Y02P70/50
Inventor 申燕吕晓伟
Owner HUAZHONG UNIV OF SCI & TECH
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