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Method for preparing powder material with electrochemical cathode

A powder material and electrochemical technology, which is applied in the field of electrochemical cathode preparation of powder materials, can solve the problems of high cost, complicated process, and low output.

Active Publication Date: 2013-08-07
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The particle distribution of powder materials prepared by these chemical methods is relatively uniform, but the synthesis process requires precursor salts and organic protective agents. The process is relatively complicated, the cost is high, and the output is low, which is not suitable for industrial scale production.

Method used

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  • Method for preparing powder material with electrochemical cathode

Examples

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Embodiment 1

[0038] Embodiment 1: Cathodic corrosion of metal tin in ionic liquid prepares nano-tin powder

[0039] Such as device figure 1 As shown, the Pt sheet is used as the anode, the Sn rod is used as the cathode, and the ionic liquid 1-n-butyl-1-methylpyrrolidine bis(trifluoromethylsulfonyl)imide is used as the electrolyte, and the constant voltage is –20V The cathode was polarized for 6 hours, and then the product obtained from the cathode was washed 6 times with absolute ethanol, ultrasonically dispersed (80W, 30kHz, 1min), centrifuged at a high speed of 13300 rpm, and finally the product was vacuum-dried at 40°C to obtain tin powder. figure 2 Scanning electron microscope (SEM) and transmission electron microscope (TEM) images of the prepared Sn powder material. Obviously, the prepared tin powder is nano tin powder.

Embodiment 2

[0040] Example 2: Prepare nano-tin powder by corroding a tin rod at cathode-25V in tetraethylammonium hexafluorophosphate solution

[0041]With the Pt sheet as the anode and the Sn rod as the cathode, in a DMF solution of 0.5mol / L tetrabutylammonium hexafluorophosphate, the constant voltage -25V strong cathodic polarization for 12h, and then the product obtained from the cathode was washed with absolute ethanol for 6 Second, ultrasonic dispersion (80W, 30kHz, 1min), high-speed centrifugation at 12,000 rpm, and finally the product was vacuum-dried at 50°C to obtain tin powder. TEM ( image 3 ) shows that the prepared tin powder is nano-tin powder with a uniform particle size of about 5nm.

Embodiment 3

[0042] Example 3: Preparation of Nano Antimony Powder by Cathode-25V Corrosion Antimony Rod in Tetraethylammonium Hexafluorophosphate Solution

[0043] With the Pt sheet as the anode and the Sb rod as the cathode, in a DMF solution of 0.5mol / L tetrabutylammonium hexafluorophosphate, a constant voltage of -25V was used for strong cathodic polarization for 12 hours, and then the product obtained from the cathode was washed with absolute ethanol for 6 Second, ultrasonic dispersion (80W, 30kHz, 1min), high-speed centrifugation at 12,000 rpm, and finally the product was vacuum-dried at 50°C to obtain antimony powder. TEM ( Figure 4 ) shows that the prepared antimony powder is nano-antimony powder with uniform particle size of about 15nm.

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Abstract

The invention relates to the field of new materials, and discloses a method for preparing a powder material with an electrochemical cathode. By using an inert electrode as an anode, a massive metal, semiconductor and alloy as a cathode, and a lithium salt / sodium salt / quaternary ammonium salt organic solution, pyrrole, quaternary ammonium salt or piperidine ionic liquid or strongly alkaline water solution as an electrolyte, strong cathode polarization is carried out under constant voltage; under the action of the strong cathode voltage, the massive metal, semiconductor and alloy surface forms an unstable intermediate Mx+Ny- (M+ is an electrolyte cation, and N represents metal, semiconductor or alloy) and becomes corroded; the intermediate is very unstable in the electrolyte, and is quickly decomposed to generate an atomic cluster; the atomic cluster continues aggregate to obtain a nanoparticle sol; and finally, the sol is centrifuged / washed, and dried to obtain the powder material. The prepared powder material can be widely used in the fields of lithium ion batteries, supercapacitors, (electric) catalysis, biosensing, photovoltaic devices, micro-electronics and the like.

Description

technical field [0001] The invention relates to the field of new materials, in particular to a method for preparing powder materials by electrochemical cathodes. Background technique [0002] Materials are the material basis for human survival and development. The development and breakthrough of material science can promote the changes of the times, promote human material civilization and social progress, and have a major impact on the world's economic structure and social development. Micro / nano-scale powder materials can be widely used in lithium-ion batteries, supercapacitors, (electric) catalysis, biosensing, photovoltaic devices, microelectronics and other fields. Traditional methods for preparing micro / nano-scale powder materials can be divided into two categories: physical methods and chemical methods. The physical methods include mechanical ball milling, mechanical crushing, and electric spark discharge. These physical methods are simple to operate and low in cost,...

Claims

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Application Information

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IPC IPC(8): C25C5/02
Inventor 纪效波杨应昌朱裔荣鲁放陈启元李叙
Owner CENT SOUTH UNIV
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