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Ge (II) precursor as well as preparation method and application thereof

A technology of precursor and reaction, which is applied in the field of microelectronic materials, can solve problems such as the difficulty of obtaining germanium precursors, and achieve the effects of mild conditions, low energy consumption, and excellent thermal stability

Inactive Publication Date: 2020-06-26
紫石能源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the CVD / ALD process technology, the properties of the germanium precursor are very important. It requires the precursor to have excellent thermal stability, film formation, volatility, low thermal weight loss temperature, low deposition temperature, and a simple preparation process to facilitate production and use, but the germanium precursors involved in the above prior art are difficult to achieve

Method used

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  • Ge (II) precursor as well as preparation method and application thereof
  • Ge (II) precursor as well as preparation method and application thereof
  • Ge (II) precursor as well as preparation method and application thereof

Examples

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Embodiment 1

[0069] This embodiment provides a Ge(II) precursor for vapor deposition—bis(N-cyano-N-n-propylamine)germanium, the structure of which is shown in formula (a).

[0070]

[0071] Its preparation method is: under the protection of nitrogen, dissolve N-cyano-N-n-propylamine (0.80mmol, 0.110g) in anhydrous n-hexane to form a light yellow transparent solution. Add methyllithium ether solution (1.60M, 0.50mL) at -78°C, and the solution immediately becomes cloudy. After returning to 25°C, continue to stir and stir for 3 hours. There is no obvious change in the system. After the reaction is completed, filter and collect the filter residue, which is the product lithium salt, and store it in a glove box.

[0072] Weigh lithium salt (0.80mmol, 0.170g) in the glove box and dissolve it in anhydrous ether under the protection of nitrogen, transfer it to a constant pressure dropping funnel, and drop it into the germanium dichloride-dioxane complex at -78°C (0.40mmol, 0.090g) in ether solu...

Embodiment 2

[0081] This embodiment provides a Ge(II) precursor for vapor deposition—bis(N-cyano-N-tert-butylamine)germanium, the structure of which is shown in formula (b).

[0082]

[0083] Its preparation method is: under the protection of nitrogen, dissolve N-cyano-N-tert-butylamine (0.80mmol, 0.130g) in anhydrous n-hexane to form a light yellow transparent solution. Add methyllithium ether solution (1.60M, 0.50mL) at -78°C, and the solution immediately becomes cloudy. After returning to 25°C, continue to stir and stir for 3 hours. There is no obvious change in the system. After the reaction is completed, filter and collect the filter residue, which is the product lithium salt, and store it in a glove box.

[0084] Weigh lithium salt (0.80mmol, 0.190g) in the glove box and dissolve it in anhydrous ether under the protection of nitrogen, transfer it to a constant pressure dropping funnel, and drop it into the germanium dichloride-dioxane complex at -78°C (0.40mmol, 0.090g) in ether ...

Embodiment 3

[0093] This embodiment provides a Ge(II) precursor for vapor deposition—bis(N-cyano-N-p-tolylamine)germanium, the structure of which is shown in formula (c).

[0094]

[0095] Its preparation method is: under the protection of nitrogen, dissolve N-cyano-N-p-tolylamine (0.80mmol, 0.260g) in anhydrous n-hexane to form a light yellow transparent solution. Add methyllithium ether solution (1.60M, 0.50mL) at -78°C, and the solution immediately becomes cloudy. After returning to 25°C, continue to stir and stir for 3 hours. There is no obvious change in the system. After the reaction is completed, filter and collect the filter residue, which is the product lithium salt, and store it in a glove box.

[0096] Lithium salt (0.80mmol, 0.30g) was weighed in the glove box and dissolved in anhydrous ether under nitrogen protection, transferred to a constant pressure dropping funnel, and dropped into the germanium dichloride-dioxane complex at -78°C (0.40mmol, 0.090g) in ether solution, ...

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Abstract

The invention relates to a Ge (II) precursor as well as a preparation method and application thereof. The Ge (II) precursor is a coordination compound formed by coordination of a ligand shown in a formula (A), a formula (B) or a formula (C) and dichloride of germanium, wherein the dichloride of germanium comprises germanium dichloride, a germanium dichloride hydrate or a germanium dichloride complex. The preparation method comprises the following steps: under the protection of a protective gas, reacting the ligand with lithium alkyl to obtain a lithium salt; and reacting the lithium salt withthe dichloride of germanium to obtain the Ge (II) precursor. The preparation method is simple in preparation process, mild in condition, low in raw material cost, low in energy consumption, economicaland environmentally friendly, and the prepared Ge (II) precursor has excellent thermal stability, volatility and film-forming property.

Description

technical field [0001] The invention belongs to the field of microelectronic materials, and in particular relates to a Ge(II) precursor and its preparation method and application, in particular to a Ge(II) precursor for vapor deposition and its preparation method and application. Background technique [0002] With the rapid development of information technology, the performance of microelectronic devices such as memory is also developing towards low voltage, low power consumption, high speed, and high density. Along with this, the manufacturing technology of devices has also undergone changes. [0003] The world's major semiconductor companies have invested a lot of energy in the research and development of related technologies. With the advancement of process nodes, the device structure has changed from a flat plate type to a nano-limited hole type with lower power consumption. The device size is continuously shrinking and the device structure is deep. The continuous increa...

Claims

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Application Information

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IPC IPC(8): C07C261/04C07C243/14C07C245/06C23C16/18C07C241/02
CPCC07C261/04C07C243/14C07C245/06C23C16/18
Inventor 王权刘琦
Owner 紫石能源有限公司
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