Solvothermal preparation method for in-situ electrode

An in-situ electrode and solvothermal technology, applied in circuits, capacitors, photovoltaic power generation, etc., can solve problems such as complex preparation processes

Active Publication Date: 2016-05-04
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the obtained metal sulfide powder still needs to be made into a slurry and then made into a film, and the preparation process is still relatively complicated.
There are also a lot of reports on the preparation of transparent sulfide in-situ electrodes, but most of them need to use highly toxic additives such as hydrazine hydrate to make the prepared electrodes transparent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] At room temperature, dissolve 5 mM nickel chloride in 68 mL of ethylene glycol solution, then add 25 mM thiourea, and add 2 mL of ethylene diamine after the thiourea is dissolved. After being uniformly dispersed, transfer the mixture to a 100mL hydrothermal kettle and add a piece of fluorine-doped tin oxide conductive glass with an area of ​​3cm*3.5cm. After the kettle is sealed, it is solvent-heated at 200°C for 6h, where the metal atoms and sulfur The atomic ratio of atoms is 1:5. The substrate is taken out, washed, and dried to obtain a translucent nickel sulfide in-situ electrode.

[0023] figure 1 The UV-visible light transmittance graph and digital photograph of the nickel sulfide electrode prepared in Example 1 are shown. Among them, the degree of transparency of the NiS electrode is equivalent to that of the pyrolytic Pt electrode, and the light transmittance in the ultraviolet-visible region is as high as 80% or more (not counting the light loss of the FTO glass)...

Embodiment 2

[0027] At room temperature, 5mM nickel chloride was dissolved in ethylene glycol solution, and then 5mM thiourea was added. After the thiourea is dissolved, the mixture is transferred to a hydrothermal kettle and a piece of fluorine-doped tin oxide conductive glass with an area of ​​3cm*3.5cm is added. After the kettle is sealed, it is solvent-heated at 200°C for 6h, where the metal atoms and sulfur The atomic ratio of atoms is 1:1. The substrate is taken out, washed and dried to obtain an opaque nickel sulfide in-situ electrode.

[0028] This example illustrates the effect of ethylenediamine additives to make electrodes transparent.

Embodiment 3

[0030] At room temperature, 3mM nickel nitrate was dissolved in the ethylene glycol solution, and then 10mM selenium powder was added and stirred for 30min. After the selenium powder was more uniformly dispersed, 1mL of ethylenediamine was added. After the ethylenediamine is uniformly dispersed, the mixture is transferred to a hydrothermal kettle and a piece of fluorine-doped tin oxide conductive glass with an area of ​​3cm*3.5cm is added. After the kettle is sealed, it is solvent-heated at 200℃ for 6h, where the metal atoms and The atomic ratio of selenium atoms is 1:3.33, and the completely transparent nickel selenide in-situ electrode can be obtained by taking out the substrate for cleaning and drying.

[0031] figure 1 The UV-visible light transmittance graph and digital photo of the nickel selenide electrode prepared in Example 3 are shown. Among them, NiSe 2 The transparency of the electrode is significantly higher than that of the pyrolytic Pt electrode, and is comparable ...

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Abstract

The invention discloses a solvothermal preparation method for an in-situ electrode. The solvothermal preparation method specifically comprises the following steps of dissolving metallic nickel salt, thiourea or selenium powder and ethylenediamine in ethylene glycol solution, adding a transparent substrate material, filling in a hydrothermal kettle, performing solvothermal at 140-230 DEG C for 3-24 h, taking out the transparent substrate, cleaning, and drying so as to obtain the transparent in-situ electrode. Areagent used in the invention is cheap; the preparation method is simple; and furthermore, the prepared in-situ nickel sulphide and nickel selenide electrode has relatively high electrocatalytic activity.

Description

Technical field [0001] The invention relates to an in-situ transparent electrode and a preparation method thereof, and belongs to the field of novel electrocatalytic materials. Background technique [0002] Metal chalcogenides are widely used in various fields because of their unique chemical properties and physical properties such as light, electricity, and magnetism. For example, optoelectronic materials, diagnostic materials, sulfide glass, industrial catalysts, luminescent materials, etc., can also be used Used as electrode material for lithium ion batteries, supercapacitors, fuel cells, dye-sensitized solar cells, quantum dot solar cells, etc. [0003] Although there have been a large number of reports on metal sulfide synthesis methods, these methods usually use high-temperature solid-phase or high-temperature gas-phase synthesis, electrochemical synthesis, ion exchange reaction synthesis, and organic thermal decomposition reaction, etc. These methods require more raw materia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01G9/20H01G9/042
CPCH01G9/2022Y02E10/542Y02P70/50
Inventor 黄妞孙小华孙盼盼项长华李文静
Owner CHINA THREE GORGES UNIV
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