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Production process of high purity tantalum alkoxide

An alkoxide, high-purity technology, applied in the direction of electrolytic organic production, electrolytic process, electrolytic components, etc., can solve the problems of unguaranteed removal of metal cations, low recovery rate, and difficult industrialization

Inactive Publication Date: 2008-09-10
ZHUZHOU HARD ALLOY GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In terms of the purification of tantalum alkoxides, the prior art mainly proposes some schemes for the removal of halogen ions, but there are few reports on the removal of metal cations in tantalum alkoxides, and when tantalum alkoxides are used for the above purposes, their purity The requirements are very high. For example, when tantalum alkoxide is used in electronic materials, Ta 2 o 5 and TaN thin films are used for dynamic random access memory, integrated circuits, on Ta 2 o 5 The content of transition metals (Fe, Ni, Cr, etc.) and alkali metals (Na, K), Th, U, and Cu in the TaN film should be as low as possible, otherwise it will adversely affect the electrical signal. Therefore, the current halide Synthetic production of tantalum alkoxide not only has long process, poor and toxic production environment, low recovery rate, not easy to industrialize, but also has no guarantee in the removal of metal cations

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Get 12L of absolute ethanol, add 0.04mol / L conductive agent (CH 3 ) 4 NCl is the electrolyte, the tantalum plate is the anode, the area is 40cm×34cm, the stainless steel is the cathode, the area is 44cm×32cm, the distance between the cathode and the anode is 2.2cm; the constant current density is 150A / m 2 , the starting temperature is normal temperature, slowly and automatically heat up to boiling, the cell voltage is 20-30V, the volatilized alcohol is returned to the electrolysis by cooling and reflux, and the alcohol is continuously added to maintain the solution volume, and the electrolysis continues for 4 days (96h). For the mixed solution of tantalum alkoxide-alcohol obtained by electrolysis, slowly increase the temperature under normal pressure, distill until the alcohol boiling point (78°C) is above, let the alcohol evaporate from the solution, and then raise the temperature to about 150°C, A small amount of higher boiling esters are distilled off, and the alcoh...

Embodiment 2

[0021] After taking 1.2L of anhydrous isopropanol, add 0.02mol / L conductive agent (CH 3 ) 4 NHSO 4 As the electrolyte, the tantalum plate is the anode, the area is 12cm×12cm, the stainless steel is the cathode, the area is 10cm×12cm, the distance between the cathode and the anode is 10cm; at a current density of 400A / m 2 , The tank voltage is 100-120V, and the temperature is boiling under the condition of electrolysis. The volatilized alcohol is returned to the electrolysis by cooling and reflux, and the alcohol is continuously added to maintain the solution volume, and the electrolysis is continued for 2 days (48h). For the mixed solution of tantalum alkoxide-alcohol obtained by electrolysis, slowly increase the temperature under normal pressure, distill it to above the boiling point of the alcohol, make the alcohol volatilize from the solution, then raise the temperature to about 160°C, and distill a small amount of Esters with a higher boiling point are recovered by cooli...

Embodiment 3

[0023] After taking 1.2L of anhydrous n-butanol, add 0.1mol / L conductive agent NH 4 Br is the electrolyte, the tantalum plate is the anode, the area is 12cm×12cm, the stainless steel is the cathode, the area is 10cm×12cm, the distance between the cathode and the anode is 2.0cm; at a current density of 50A / m 2 , The cell voltage is 15-20V, and the temperature is electrolyzed under the condition of normal temperature. The volatilized alcohol is returned to the electrolysis by cooling and reflux, and the electrolysis is continued for 5 days (120h). For the mixed solution of tantalum alkoxide-alcohol obtained by electrolysis, first slowly raise the temperature under normal pressure, distill until the alcohol is above the boiling point, make the alcohol volatilize from the solution, add 0.5g metal sodium solid while stirring, and then raise When the temperature reaches about 180°C, a small amount of esters with higher boiling points will be distilled out, and the alcohol will be re...

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PUM

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Abstract

The production process of high purity tantalum alkoxide with metal tantalum as anode and anhydrous alcohol added with conducting agent as electrolyte, and through electrochemical sacrificial anode process to synthesize mixed tantalum alkoxide-alcohol solution, distilling the mixed solution to volatilize alcohol and ester, and decompression rectification for separation to obtain high purity tantalum alkoxide. The said process can obtain high purity tantalum alkoxide for use in microelectronic industry, acoustic surface wave filter, etc. The present invention has short technological process and good production environment, and is easy use in industrial production.

Description

technical field [0001] The invention relates to a method for producing high-purity tantalum alkoxide technical background [0002] High-purity tantalum alkoxide is mainly used for the preparation of optoelectronic plating oxide film and metal-organic compound vapor deposition (MOCVD) large-area Ta 2 o 5 or TaN film, while Ta 2 o 5 And TaN thin films are more and more widely used in dynamic random access memory, integrated circuits, etc. Tantalum alkoxides are also used in the production of piezoelectric, pyroelectric, ferroelectric ceramic materials and insoluble anodes for electrolysis. In addition, tantalum alkoxide compounds (such as tantalum pentaethoxide and tantalum penta-n-butoxide) can be properly treated to obtain ultra-fine tantalum pentoxide with good activity, high dispersion, spherical particles, and high purity. It is mainly used as Raw materials for lithium tantalate single crystals and special optical glass additives for surface acoustic filters. [000...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/12C25B3/13
Inventor 杨声海李朝晖潘泽强谢康德何坤池
Owner ZHUZHOU HARD ALLOY GRP CO LTD