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A kind of preparation method of ald precursor titanium complex

A technology of titanium complexes and precursors, applied in the fields of organic chemistry and microelectronic materials, can solve the problems of low chemical purity, long-term heating, and difficult storage of products, and achieve high product yields, easy storage, and cheap prices.

Active Publication Date: 2021-11-30
苏州源展材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problems of this method are: the raw materials are expensive and difficult to store, and the cost is high; the reaction needs to be heated for a long time, and the energy consumption is large; some silica impurities are not removed during the preparation process, resulting in low chemical purity of the product

Method used

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  • A kind of preparation method of ald precursor titanium complex
  • A kind of preparation method of ald precursor titanium complex
  • A kind of preparation method of ald precursor titanium complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Under nitrogen protection, add 2,2,6,6-tetramethyl-3,5-heptanedione (36.86g, 0.2mol), titanium tetrachloride (18.97g, 0.1mol) into a 2L reaction flask , add n-hexane (800 mL), drop diethylamine (32.18 g, 0.44 mol) into the reaction solution through a constant pressure dropping funnel, and stir at room temperature for 3 hours. Then add isopropanol (13.21g, 0.22mol) dropwise through a constant pressure dropping funnel, filter, evaporate the filtrate to dryness to obtain a white solid, add a small amount of tetrahydrofuran to dissolve, add n-hexane, cool to -20°C, filter, use cold n-hexane The filter cake was washed to obtain a white solid (46.87 g, 0.088 mol) with a yield of 88%.

[0033] NMR: 1 H NMR (500 MHz, C 6 D. 6 ) d (ppm): 5.85 (CH), 4.95 (CH), 1.40[(CH 3 ) 2 ], 1.06[C(CH 3 ) 3 ].

[0034] The metal purity of the sample was determined by means of elemental analysis, and the result showed that the metal purity of the sample was 5N.

Embodiment 2

[0036]Under nitrogen protection, add 2,2,6,6-tetramethyl-3,5-heptanedione (36.86g, 0.2mol), titanium tetrachloride (18.97g, 0.1mol) into a 2L reaction flask , add n-hexane (800 mL), drop triethylamine (44.52 g, 0.44 mol) into the reaction solution through a constant pressure dropping funnel, and stir at room temperature for 3 hours. Then add isopropanol (13.21g, 0.22mol) dropwise through a constant pressure dropping funnel, filter, evaporate the filtrate to dryness to obtain a white solid, add a small amount of tetrahydrofuran to dissolve, add n-hexane, cool to -20°C, filter, use cold n-hexane The filter cake was washed to obtain a white solid (43.14 g, 0.081 mol) with a yield of 81%.

[0037] After testing, the metal purity of the sample was 5N.

Embodiment 3

[0039] Under nitrogen protection, add 2,2,6,6-tetramethyl-3,5-heptanedione (36.86g, 0.2mol), titanium tetrachloride (18.97g, 0.1mol) into a 2L reaction flask , add n-hexane (800 mL), drop diethylamine (32.18 g, 0.44 mol) into the reaction solution through a constant pressure dropping funnel, and stir at room temperature for 6 hours. Then add isopropanol (13.21g, 0.22mol) dropwise through a constant pressure dropping funnel, filter, evaporate the filtrate to dryness to obtain a white solid, add a small amount of tetrahydrofuran to dissolve, add n-hexane, cool to -20°C, filter, use cold n-hexane The filter cake was washed to obtain a white solid (46.33 g, 0.087 mol) with a yield of 87%.

[0040] After testing, the metal purity of the sample was 5N.

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Abstract

The invention discloses a preparation method of an ALD precursor titanium complex, which comprises the following steps: (1) combining 2,2,6,6-tetramethyl-3,5-heptanedione, titanium tetrachloride and organic Mix the solvent evenly, drop the organic amine, and react under stirring; (2) After the reaction, add isopropanol dropwise to the reaction solution, stir and filter to remove the precipitate; (3) Evaporate the filtrate to dryness under reduced pressure , that is, the ALD precursor titanium complex is obtained. The process operating conditions of the present invention are convenient, and the target product can be obtained by one-pot method; the reaction process is gentle, without heating, low energy consumption, and high safety; the source of raw materials is extensive and cheap, the product yield is high, and the process stability is good; Other metal elements (except titanium), the obtained products have high metal purity and meet the requirements of ALD technology.

Description

technical field [0001] The invention relates to the technical fields of organic chemistry and microelectronic materials, in particular to a preparation method of an ALD precursor titanium complex. Background technique [0002] Titanium dioxide (TiO 2 ) film has many excellent physical properties, such as: high dielectric constant, high thermal conductivity, strong resistance to radiation damage, strong resistance to alkali ion penetration, and transparent characteristics in a wide wavelength range. Therefore, TiO 2 Thin films are widely used in many fields such as microelectronic devices, electroluminescent devices, and anti-corrosion coatings. Especially in microelectronic devices, TiO 2 Thin film is one of the important materials commonly used as gate dielectric due to its large dielectric constant and large energy band shift in contact with Si. Usually TiO 2 Thin film preparation methods include: magnetron reactive sputtering, pulsed plasma deposition, molecular beam...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/28
CPCC07F7/003
Inventor 陈鹏宇
Owner 苏州源展材料科技有限公司