Method for producing high purity organic amine tantalum compound

A technology of tantalum compounds and production methods, which is applied in the field of high-purity organic amine tantalum compounds, can solve the problems of low concentration, poor operating conditions, and high requirements for equipment materials, and achieve the effects of simple equipment, friendly production environment, and short production process

Inactive Publication Date: 2008-08-27
CENT SOUTH UNIV
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process for preparing organic amine tantalum compounds has the following disadvantages: the organic amine lithium and tantalum halide are used as raw materials, which are expensive, and this method is not compatible with the existing wet extraction process for tantalum, requiring separate chlorination and rectification equipment , the equipment material requirements are high, chlorine gas is a toxic gas, and the operating conditions are poor; in the process of synthesizing organic amine tantalum compounds, due to the formation of a large number of fine particles of lithium halide precipitation, a large amount of organic amine tant...

Method used

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  • Method for producing high purity organic amine tantalum compound

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Embodiment 1

[0023]Get 12L of diethylamine, add 0.04mol / L conductive agent (CH 3 ) 4 NCl is the electrolyte, the tantalum plate is the anode, the area is 44cm×34cm, the stainless steel is the cathode, the area is 44cm×34cm, the distance between the cathode and the anode is 2cm; the constant current density is 140A / m 2 , the starting temperature is normal temperature, slowly and automatically heat up to boiling, the tank voltage is 20-35V, the volatilized diethylamine is returned to the electrolysis by cooling and reflux, and the diethylamine is continuously added to maintain the solution volume, and the electrolysis is continued for 4 days (96h) . The mixed solution of diethylamine tantalum-diethylamine obtained by electrolysis, first slowly raise the temperature under normal pressure, distill to above the boiling point of diethylamine, make diethylamine volatilize from the solution, and then raise the temperature to At about 90-100°C, a small amount of impurity organic amines are distil...

Embodiment 2

[0025] Get 1.2L of dipropylamine, 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 12cm×12cm, the distance between the cathode and the anode is 8cm; at a current density of 400A / m 2 , The tank voltage is 100-120V, and the temperature is electrolyzed under the condition of boiling. The volatilized dipropylamine is returned to the electrolysis by cooling and reflux, and the dipropylamine is continuously added to maintain the solution volume, and the electrolysis is continued for 2 days (48h). The mixed solution of dipropylamine tantalum and dipropylamine obtained by electrolysis, first slowly raise the temperature under normal pressure, distill to above the boiling point of dipropylamine (109°C), make the dipropylamine volatilize from the solution, and then raise the temperature At about 140°C, a small amount of impurity organic amines are distilled off, a...

Embodiment 3

[0027] Take 1.2L of dibutylamine, 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 at room temperature. The volatilized organic amine is returned to the electrolysis by cooling and reflux, and the electrolysis is continued for 5 days (120h). The mixed solution of organic amine tantalum compound obtained by electrolysis-organic amine, first slowly raise the temperature under normal pressure, distill to above the boiling point of dibutylamine (159°C), make dibutylamine volatilize from the solution, and then raise the temperature When the temperature reaches about 180°C, a small amount of impurity organic amines are distilled off, and dibutylamine is cooled and recovered. Turn on the vacuum pump while it ...

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Abstract

The invention relates to a method for producing organic amine tantalum compound with high purity, which comprises following steps: taking metallic tantalum and organic amine as raw materials, adding conductive agent in the organic amine as electrolyte, taking the metallic tantalum as an anode, adopting an electrochemical method of a 'sacrificial' anode to synthesize mixed solution of the organic amine tantalum compound and the organic amine, distilling the mixed solution, and lastly decompressing and distilling to obtain the organic amine tantalum compound with high purity. In the products of the organic amine tantalum compound which is obtained through adopting the method of the invention, impurity elements such as Al, As, B, Ba, Ca and the like are less than or equal to 0.0001%, Nb is less than or equal to 0.0010%, the purity of the products is more than 99.99%, the production process flow is short, the equipment is simple, and the production environment is friendly.

Description

technical field [0001] The invention relates to a production method of a high-purity organic amine tantalum compound. Background technique [0002] In recent years, with the development of microelectronic silicon chips to ultra-large-scale integrated circuits (ULSI), the size of devices has been further reduced to the nanoscale range, and a series of technological changes have taken place in the field of microelectronics manufacturing. For example, copper has replaced aluminum as the interconnect material in sub-0.5 μm VLSI due to its higher electrical conductivity and less electromigration properties than silver. Using copper as the interconnection material can reduce the resistance of the interconnection lines on the chip, or reduce the thickness of the interconnection metal while keeping the resistance constant to reduce the coupling capacitance between the interconnection lines in the same layer, thereby reducing the coupling Noise and signal delay on interconnect lines...

Claims

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Application Information

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IPC IPC(8): C25B3/12B01D3/00C25B3/13
Inventor 杨建广杨声海何静唐朝波唐谟堂鲁君乐
Owner CENT SOUTH UNIV
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