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Electrochemical synthesis method of silicon carbide nanowire

A technology of silicon carbide nanowires and synthesis methods, which is applied in the preparation of nanomaterials and multidimensional nanomaterials, can solve the problems of low raw material requirements and low energy consumption, and achieve the effects of simple preparation process, high efficiency and simple operation

Active Publication Date: 2014-09-03
SHANGHAI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems of the prior art, the purpose of the present invention is to overcome the deficiencies of the prior art, to provide an electrochemical synthesis method of silicon carbide nanowires, and to propose a brand new method for the existing technical difficulties in preparing silicon carbide nanowires. A method for directly synthesizing silicon carbide nanowires from nano-silicon dioxide / nano-carbon powder mixture precursors through controllable deoxidation. The present invention realizes the combination of electrical deoxidation and carbonization reactions through electrochemical methods to achieve in-situ synthesis of silicon carbide nanowires, which greatly Improve the existing preparation method, with the characteristics of high efficiency, low raw material requirements, low energy consumption, etc.

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  • Electrochemical synthesis method of silicon carbide nanowire
  • Electrochemical synthesis method of silicon carbide nanowire
  • Electrochemical synthesis method of silicon carbide nanowire

Examples

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Effect test

Embodiment 1

[0027] In this example, figure 1 As shown, the electrochemical synthesis method of silicon carbide nanowires adopts a short-flow preparation process, which includes the following steps: realize weighing 0.5 grams of nanometer carbon dioxide that has been added with a mass fraction of 2% polyvinyl butyral binder and ball-milled uniformly. Silicon oxide / nano-carbon mixture raw material fine powder, wherein nano-silica powder and nano-carbon powder are mixed according to the molar ratio of stoichiometric ratio Si:C = 1:1, and the mixed fine powder is pressed under a pressure of 15 MPa For a single round flake 2. Then use foamed nickel 3 to wrap the pressed sheet in layers and wrap it with iron-chromium-aluminum wire to make a cathode, and use iron-chromium-aluminum wire 6 to draw it as an electrode lead, such as figure 2 As shown, the corundum crucible 1 is used as the electrolytic reaction vessel to avoid the introduction of carbon pollution into the vessel; the pressed sheet ...

Embodiment 2

[0030] This embodiment is basically the same as Embodiment 1, especially in that:

[0031] In this example, the nano-silica / nano-carbon powder mixture powder was added into 2 wt% polyvinyl butyral binder and ball-milled to make it uniform. Then take 0.5 gram of mixed fine powder and press it into circular flakes under the condition of 12 MPa. Wrap the compressed sheet with nickel foam 3 and wrap it with iron-chromium-aluminum wire 6 to make a nano-silica / nano-carbon powder cathode. The prepared cathode is placed in the molten salt electrolytic cell. The placement method can be divided into two cathodes connected in parallel or a single cathode containing multiple precursor sheets. An electrode assembled with an oxygen-permeable zirconia membrane tube with a molar ratio of 8% yttrium oxide is used as an anode system 5 to analyze pure anhydrous CaCl 2 It is a molten salt electrolyte 4, a stainless steel crucible 1 is a reaction vessel, high-purity argon is used as a protective...

Embodiment 3

[0033] This embodiment is basically the same as the previous embodiment, and the special features are:

[0034] In the present embodiment, take 1.0 gram and add the nano-silica / nano-carbon mixture raw material fine powder of 1.5% polyvinyl butyral binder and ball mill uniformly, the fine powder is mixed at 12 MPa Pressed into round flakes under the same conditions. Wrap the compressed sheet with nickel foam 3 and wrap it with iron-chromium-aluminum wire 6 to make a nano-silica / carbon cathode. Place the prepared cathode in the molten salt electrolytic cell. To analyze pure anhydrous CaCl 2 It is a molten salt electrolyte 4, the corundum crucible 1 is a reaction vessel, and high-purity argon is used as a protective gas to perform electrolysis in a sealed resistance furnace. The temperature is selected as 1000°C, the electrolysis voltage is 4.0 volts, and the electrode assembled with the oxygen-permeable membrane tube is used as the anode system. After 10 hours of electrolysis...

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Abstract

The invention discloses an electrochemical synthesis method of a silicon carbide nanowire. The electrochemical synthesis method comprises the following steps: by taking nano silicon dioxide as a raw material, adding nano carbon powder and 1-2wt% of polyvinyl butyral binder according to the chemical stoichiometric ratio of silicon carbide, and then ball-grinding to obtain fine powder; then preforming into sheets as a cathode for preparing the silicon carbide nanowire under 12-20MPa, wherein anhydrous calcium chloride is used as an electrolyte, and an inert gas is used as a protective gas; assembling an anode by 8% (mole ratio) of yttrium oxide-stabilized zirconia solid oxygen permeating membrane pipe to be used as a controllable anode system, and conducting direct deoxygenation under the voltage condition of 3.0-4.0V to directly synthesize the silicon carbide nanowire in situ through high-efficiency deoxygenation of the oxygen permeating membrane and accurate control of reaction processes. The one-step synthesis of silicon carbide from silicon dioxide / carbon precursor can be realized, the existing preparation method can be greatly improved, and the electrochemical synthesis method has the characteristics of being high in efficiency, low in requirement on the raw materials, low in energy consumption and the like.

Description

technical field [0001] The invention relates to a preparation method of a nanometer material, in particular to a preparation method of a multidimensional nanometer material, and belongs to the technical field of transition metal carbide synthesis technology. Background technique [0002] Due to its excellent physical and chemical properties such as ultra-high melting point, hardness, extremely high thermal stability and corrosion resistance, micro-nano-scale refractory metal carbide composites have great potential for application in cutting-edge fields such as aerospace, nuclear reactors, and high-performance ceramics. It has become one of the world's strategic materials in the new era. Especially silicon carbide (SiC), because of its band gap, high thermal conductivity, small dielectric constant, high hardness, good chemical stability and mechanical properties, excellent oxidation resistance, etc., is widely used in high temperature, high frequency, high power electronic d...

Claims

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Application Information

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IPC IPC(8): C25B1/00B82Y40/00
Inventor 邹星礼鲁雄刚路长远沈斌赖冠全谢学良周忠福钟庆东
Owner SHANGHAI UNIV
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