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Synthesis method of tri(dimethylamino) antimony

A dimethylamino, synthetic method technology, applied in the field of triantimony synthesis, to achieve the effects of high yield, reduced synthesis cost and reaction toxicity, and good operability

Inactive Publication Date: 2017-09-01
JIANGSU NATA OPTO ELECTRONICS MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, there is no report on the synthesis method of tris(dimethylamino)antimony in China

Method used

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  • Synthesis method of tri(dimethylamino) antimony

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Effect test

Embodiment 1

[0031] Under an inert atmosphere, add 90g of dimethylamine and 300mL of n-hexane into a 2L reaction flask, keep the temperature of the system at about -10-10°C, and add 500mL of 2.5mol / L n-butyllithium n-hexane solution dropwise while stirring, After the dropwise addition was completed, the mixture was warmed to room temperature and kept stirring for 4 hours.

[0032] Dissolve 95g of antimony trichloride in 50mL of ether and 100mL of n-hexane, and add it dropwise to the above reaction system, keeping the temperature of the reaction system at about -30-10°C. Keep the system temperature not lower than 60°C and heat to reflux for 4 hours.

[0033] After the reaction was finished, the system was filtered, then the solvent was removed by distillation under normal pressure, and then the distillation under reduced pressure was collected to collect the distilled fraction, which was the target compound tris(dimethylamino)antimony, and 85g of the product was obtained, with a yield of 80...

Embodiment 2

[0035] Under an inert atmosphere, add 300g of dimethylamine and 1000mL of n-hexane into a 5L reaction flask, keep the temperature of the system at about -10-10°C, and add 1500mL of 2.5mol / L n-butyllithium n-hexane solution dropwise while stirring, After the dropwise addition was completed, the mixture was warmed to room temperature and kept stirring for 4 hours.

[0036] Dissolve 285g of antimony trichloride in 150mL of ether and 300mL of n-hexane, and add it dropwise to the above reaction system, keeping the temperature of the reaction system at about -30-10°C. Keep the system temperature not lower than 60°C and heat to reflux for 4 hours.

[0037] After the reaction was finished, the system was filtered, then the solvent was removed by distillation under normal pressure, and then the distillation under reduced pressure was collected to collect the distilled fraction, which was the target compound tris(dimethylamino)antimony, and 238g of the product was obtained with a yield ...

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Abstract

The invention discloses a synthesis method of tri(dimethylamino) antimony. The method comprises the steps of firstly adding dimethylamine and varsol into a reactor under inert atmosphere protection; adding a hydrocarbon and ether mixed solution of antimony trichloride to a system; and carrying out filtration and distillation after reaction is completed to obtain the tri(dimethylamino) antimony. According to the synthesis method, only a small amount of ether solvent is needed, so that the synthesis cost and the reaction toxicity are reduced, and the synthesis method has better operability and relatively high yield, and is conducive to large-scale production.

Description

technical field [0001] The invention relates to a method for synthesizing tris(dimethylamino)antimony. Background technique [0002] With the continuous development of VLSI technology, the size of MOS transistors as its basic devices continues to shrink. When SiO 2 When the thickness of the gate dielectric is reduced to the nanometer level, through SiO 2 The leakage current of SiO increases exponentially with the thickness reduction, such a huge leakage current not only seriously affects the performance of the device, but also eventually leads to SiO 2 Can not play an insulating role. Replace SiO with high dielectric constant materials 2 It is currently the most promising way to solve this problem. [0003] The continuous development of the semiconductor manufacturing industry makes it necessary to find high-K and metal gate material precursors suitable for ALD and CVD. For the 32nm technology node, issues such as material volatility, transport mode, and purity become c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/90
CPCC07F9/90C07F9/902
Inventor 张得来范广鹏许从应林俊元潘兴华万欣常华
Owner JIANGSU NATA OPTO ELECTRONICS MATERIAL
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