Metal compound, material for forming thin film and method for preparing thin film

一种金属化合物、制造方法的技术，应用在薄膜的制造领域，能够解决不具有挥发性等问题

Inactive Publication Date: 2007-01-17
ADEKA CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As the lead compound, bis(dipivaroylmethanato) lead using di-t-valerylmethane as a ligand is used, but it does not have sufficient volatility

Method used

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  • Metal compound, material for forming thin film and method for preparing thin film
  • Metal compound, material for forming thin film and method for preparing thin film
  • Metal compound, material for forming thin film and method for preparing thin film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] [Example 1] Production of Compound No.1

[0051] Under a dry argon atmosphere, add 0.478 mol of lead dichloride, 2000 ml of dehydrated diethyl ether, 0.935 mol of bis(trimethylsilyl)amide lithium in a light-shielding reaction flask, and stir at 25°C for 24 Hour. Diethyl ether was distilled off as a solvent, 3000 ml of dehydrated hexane was added to the obtained residue, and the solid phase was filtered to obtain a solution. 1.03 mol of 1-dimethylamino-2-methyl-2-propanol was added dropwise to this solution, and after stirring at 25°C for 24 hours, hexane and by-product hexamethyldisilazide were distilled off. alkyl. White crystals were obtained at a yield of 38% from fractions at 13 to 15 Pa and a tower top temperature of 90 to 95°C. The white crystals were further purified by distillation under reduced pressure to obtain crystals. The recovery rate of this purification was 90%. The obtained crystal was identified as the target compound No.1. The analytical values...

Embodiment 2

[0058] [Example 2] Preparation of Compound No.13

[0059] Under a dry argon atmosphere, drop 0.100 mol of tetrakis(2-propoxy)titanium, 60 ml of dehydrated xylene, 0.440 mol of 1-dimethylamino-2-methyl-2 into the reaction flask -propanol, by-product 2-propanol was distilled off while reacting at 135°C for 18 hours. Xylene was distilled off, and the obtained residue was distilled off under reduced pressure. A light yellow liquid was obtained at a yield of 48% from the fraction at 5-7 Pa and a tower top temperature of 122-124°C. The light yellow liquid was further purified by distillation under reduced pressure to obtain a liquid. The recovery rate of this purification was 94%. The resulting liquid was identified as the target compound No.13. The analytical values ​​of the obtained liquid are shown below.

[0060] (analytical value)

[0061] (1) Elemental analysis (metal analysis: ICP-AES)

[0062] Titanium: 9.43% by mass (theoretical value: 9.34%)

[0063] (2) 1 H-NMR (...

Embodiment 3

[0066] [Example 3] Preparation of Compound No.25

[0067] Under a dry argon atmosphere, 0.100 moles of tetrakis(2-propoxy) zirconium 2-propanol adduct, 60 ml of dehydrated xylene, 0.440 moles of 1-dimethyl Amino-2-methyl-2-propanol, while distilling off the by-product 2-propanol, reacted at 135°C for 10 hours. Xylene was distilled off, and the obtained residue was distilled off under reduced pressure. A colorless liquid was obtained at a yield of 53% from the fraction at 8 to 10 Pa and a tower top temperature of 139 to 140°C. This colorless liquid was further purified by distillation under reduced pressure to obtain a liquid. The recovery rate of this purification was 92%. The resulting liquid was identified as the target compound No. 25. The analytical values ​​of the obtained liquid are shown below.

[0068] (analytical value)

[0069] (1) Elemental analysis (metal analysis: ICP-AES)

[0070] Zirconium: 16.8% by mass (theoretical value is 16.4%)

[0071] (2) 1 H-NMR...

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Abstract

The metal compound has a low melting point and thus can be transported in a liquid state, has a high vapor pressure and thus is easy to vaporize, and is free from the change in its quality due to the exchange of ligands or a chemical reaction also when mixed with another metal compound, and thus it is suitable as a material for use in a method for preparing a thin film, such as the CVD method forming a thin film through the vaporization of a metal compound. The metal compound represented by the following general formula (I), wherein R<1>, R<2>, R<3>, and R<4> each represent an alkyl group having one to four carbon atoms, A represents an alkanediyl group having one to eight carbon atoms, M represents a lead atom, a titanium atom or a zirconium atom, and n represents 2 when M is a lead atom and represents 4 when M is a titanium or zirconium atom.

Description

technical field [0001] The present invention relates to a novel metal compound (lead compound, titanium compound, and zirconium compound) using a specific aminoalcohol as a ligand, a raw material for forming a thin film containing the metal compound, and production of a metal-containing thin film using the raw material method. Background technique [0002] Thin films containing lead, titanium, or zirconium are mainly used as components of electronic components such as high dielectric capacitors, ferroelectric capacitors, gate insulating films, and barrier films. [0003] Examples of methods for producing the above-mentioned thin film include MOD methods such as flame deposition methods, sputtering methods, ion plating methods, coating pyrolysis methods, and sol-gel methods, and chemical vapor phase growth (hereinafter sometimes simply referred to as CVD) methods. However, the chemical vapor phase growth method including the ALD (Atomic Layer Deposition) method is the best m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/08C07F7/00C07F7/24C07F7/28C23C16/40C23C16/18
CPCC23C16/18C07F7/006C23C16/409C07F7/003C07F7/24C07F7/28C23C16/40C07C215/08
Inventor 樱井淳山田直树
Owner ADEKA CORP
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