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Industrialized production method for tetra(methylethylamino)hafnium

A production method, the technology of ethyl amino, applied in the field of microelectronic material production, can solve the problems of high cost and troublesome operation process, achieve the effects of peaceful reaction process, increase production efficiency and reduce production cost

Inactive Publication Date: 2017-07-04
苏州复纳电子科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for the industrial production of tetra(methylethylamino) hafnium, to solve the problems of troublesome and high cost in the industrial production of tetra(methylethylamino) hafnium

Method used

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  • Industrialized production method for tetra(methylethylamino)hafnium

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Experimental program
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Effect test

Embodiment 1

[0027] Under an inert atmosphere, add 50 liters of n-butyllithium n-heptane solution (concentration is 2.5mol / L) in the reactor, and under stirring condition, add 8.1Kg of N-methylethylamine dropwise in the reactor, Control the dropping rate and keep the solution temperature at -20°C, react for 10 hours, then add hafnium tetrachloride 9.1Kg in batches, keep the system temperature at -20°C during the addition, react for 10 hours, and then reflux for 4 hours. After cooling, the solution is transferred to a distiller through a solid-liquid separator, and the pressure is reduced to 50mmHg to distill off the solvent n-heptane, and the temperature is 60°C. The product was then decompressed to 5 mmHg and rectified to distill the product at a temperature of 120° C. to obtain 10.6 Kg of tetrakis(methylethylamino)hafnium (TEMAH) with a yield of 92.8%.

Embodiment 2

[0029] Under an inert atmosphere, add 50 liters of n-butyllithium n-heptane solution (2.5mol / L) into the reaction kettle, and add 7.5Kg of N-methylethylamine dropwise to the reaction kettle under stirring conditions, and control the dropwise Adding temperature is between -10°C, keep system temperature at -10°C after dropwise addition, react for 8 hours, then add hafnium tetrachloride 10.0Kg in batches, maintain system temperature at -15°C during addition, finish adding at -15°C °C for 8 hours, then reflux for 4 hours. After cooling, pass through the solid-liquid separator, transfer to the distiller, first reduce the pressure to 40mmHg to distill out the solvent n-heptane, and the temperature is 50°C. The product was then rectified under reduced pressure of 4 mmHg at a temperature of 130° C. to obtain 10.2 Kg of tetrakis(methylethylamino)hafnium (TEMAH) with a yield of 79.4%.

Embodiment 3

[0031] Under an inert atmosphere, add 50 liters of n-butyllithium n-hexane solution (2.5mol / L) into the reaction kettle, and add 8.1Kg of N-methylethylamine dropwise to the reaction kettle under stirring conditions, and control the dropwise addition Keep the temperature at -15°C during the dropwise addition, keep the system temperature at -15°C, react for 12 hours, then add 9.1Kg of hafnium tetrachloride in batches, maintain the system temperature at -15°C during the addition, and react at -15°C after adding 12 hours, then reflux reaction for 8 hours. After cooling, pass through a solid-liquid separator and transfer to a distiller. First, reduce the pressure to 30mmHg to distill out the solvent n-hexane at a temperature of 50°C. Finally, the product was rectified under a reduced pressure of 30 mmHg at a temperature of 110° C. to obtain 10.2 Kg of tetrakis(methylethylamino) hafnium (TEMAH) with a yield of 87.3%.

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Abstract

The invention discloses a synthesis and industrialized purification method for tetra(methylethylamino)hafnium. The method comprises the following steps: adding an n-butyl lithium.alkane CnH(2n+2) (n is not smaller than 6) solution into an inert atmosphere shielded reactor, dropwise adding N-methylethylamine into the reactor under the condition of stirring, carrying out a reaction, keeping the temperature of a reaction system to 0 DEG C to -30 DEG C, and carrying out a reaction for 8 to 12 hours while keeping the temperature to 0 DEG C to -30 DEG C after dropwise adding is completed; then, adding hafnium tetrachloride in a staged manner, carrying out a reaction for 8 to 12 hours while keeping the temperature to 0 DEG C to -30 DEG C, and maintaining a reflux reaction for 4 to 8 hours; and carrying out cooling, then, removing a byproduct, i.e., lithium chloride through a solid-liquid separator, transferring a solution to a distiller, carrying out depressurizing firstly until the pressure intensity is 10mmHg to 50mmHg to distill off an alkane CnH(2n+2) (n is not smaller than 6) solvent, and then, carrying out depressurizing until the pressure intensity is 1mmHg to 2mmHg, so as to distill off the product, i.e., tetra(methylethylamino)hafnium (TEMAH). According to the method disclosed by the invention, selected reagents are moderately-priced and readily available, and the reaction process is moderate and is free of potential safety hazards; due to high-boiling-point alkane, the reaction yield is increased; by arranging a buffer tank, the production efficiency is increased; and the reaction is free of wastes, so that the method is pollution-free to environments.

Description

technical field [0001] The invention relates to the field of microelectronic material production, in particular to an industrialized production method of tetrakis(methylethylamino)hafnium, a raw material for production of metal electrode materials. Background technique [0002] Hafnium nitride (HfN) film has high density, high melting point, high hardness and bright metallic luster, and has important applications in the anti-wear and anti-corrosion treatment of cutting tools and spare parts. At the same time, due to its high electrical conductivity, appropriate metal work function, good thermal and chemical stability, it also has important applications in the field of integrated circuits. For example, it can be used as the gate of metal-oxide-semiconductor field effect transistor (MOSFET) and anti-diffusion barrier layer material in integrated circuit copper interconnection technology. [0003] Hafnium dioxide (HfO 2 ) is a ceramic material with a wide bandgap and a high d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/00
CPCC07F7/003
Inventor 不公告发明人
Owner 苏州复纳电子科技有限公司
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