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Preparation method of atomic layer deposition precursor material based on alkaline earth metal

An atomic layer deposition, alkaline earth metal technology, applied in metallocene, chemical instruments and methods, organic chemistry and other directions, can solve the problems of high risk of reducing agent potassium hydride, high raw material price, restricting mass production and application of products, etc. The effect of eliminating risk factors, reducing costs, and increasing feasibility

Pending Publication Date: 2022-03-15
合肥安德科铭半导体科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw materials used in this route are expensive (SrI 2 / BaI 2 , KH), the reducing agent potassium hydride is highly dangerous, and the by-product is hydrogen, which greatly limits the mass production and application of the product

Method used

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  • Preparation method of atomic layer deposition precursor material based on alkaline earth metal
  • Preparation method of atomic layer deposition precursor material based on alkaline earth metal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A method for preparing a strontium-based atomic layer deposition precursor material, comprising the following steps:

[0028] 1. Preparation of iPr 3 Cp (or write Cp 3i ): Add 4.2L of KOH solution, 180g of cyclopentadiene monomer, and 40g of methyl trioctylammonium chloride into a 5L three-neck round bottom flask, and stir. 1.33Kg of isopropane bromide was added dropwise to the system, and stirred overnight at 0°C. During the stirring period, 200 g of KOH solid was added, and the mixture was fully stirred. After the reaction was completed, it was left to settle, filtered and extracted to separate the upper organic phase, and the organic phase was dried and distilled under reduced pressure. Cp 3i Product 457g, yield 88%.

[0029] 2. Preparation of NaCp 3i : Weigh 48.812g NaNH 2 , transferred to a 2L three-neck round bottom flask, and added 1.2L THF. Add Cp dropwise to the system 3i Liquid 210g, heated to reflux and stirred overnight. Filtrate, concentrate and rem...

Embodiment 2

[0034] A preparation method of a barium-based atomic layer deposition precursor material, comprising the following steps:

[0035] 1. Preparation of iPr 3 Cp (or write Cp 3i ): same as embodiment one.

[0036] 2. Preparation of KCp 3i : Weigh 239.38g bis(trimethylsilyl)potassium amide (KHMDS), transfer to a 2L three-neck round bottom flask, add 1.5L THF. Add Cp dropwise to the system 3i Liquid 210g, heated to reflux and stirred overnight. Filter, concentrate and remove solvent, obtain KCp 3i Solid 227.5g, yield 90%.

[0037] 3. Preparation of Ba(Cp 3i ) 2 : In the glove box, add BaCl to a 2L three-neck round bottom flask 2 Solid 42.69g (0.205mol) and KI solid 2.0g (catalyst), add THF about 1.0L, heat and stir. Add KCp to the system 3i Solid 100g, heated to reflux for 36h. Stop heating, after returning to room temperature, filter and concentrate, then add 600mL of toluene to extract and wash the product. The solvent toluene was distilled off, and the distilled tolu...

Embodiment 3

[0041] A method for preparing a strontium-based atomic layer deposition precursor material, comprising the following steps:

[0042] 1. Preparation of tBu 3 Cp (or write Cp 3t ): Add 2.0 L of KOH solution, 90 g of cyclopentadiene monomer, and 25 g of methyl trioctyl ammonium chloride into a 5 L three-neck round bottom flask, and stir. Add 740 g of bromo-tert-butane dropwise to the system, and stir overnight at -10°C. During stirring, 100 g of KOH solid was added, and stirred thoroughly. After the reaction was completed, it was left to settle, filtered and extracted to separate the upper organic phase, and the organic phase was dried and distilled under reduced pressure. Cp 3t Product 271.5g, yield 92%.

[0043] 2. Preparation of KCp 3t : Weigh 34.48g KNH 2 , transferred to a 1L three-neck round bottom flask, and added 500mL THF. Add Cp dropwise to the system 3t Liquid 128g, heated to reflux and stirred overnight. Filter, concentrate and remove solvent, obtain KCp 3t...

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Abstract

The invention discloses a preparation method of an atomic layer deposition precursor material based on alkaline earth metal. The preparation method comprises the following steps: (1) preparing trialkyl-substituted cyclopentadiene R3Cp; (2) reacting the R3Cp prepared in the step (1) with alkali B to obtain corresponding (R3Cp) M salt; and (3) after the (R3Cp) M is obtained, adding NCl2 and NI2 into the (R3Cp) M, and reacting by taking tetrahydrofuran or diethyl ether as a solvent to obtain (R3Cp) 2N. According to the invention, amino metal MNH2 or amino metal MN (SiMe3) 2 is used for replacing KH to react with R3Cp in the traditional process, and a byproduct is ammonia gas or hexamethyldisilazane HMDS, so that the cost of raw materials is reduced, dangerous factors in production are eliminated, and the feasibility of batch production of cyclopentadiene coordination compounds of alkaline earth metal is improved.

Description

technical field [0001] The invention relates to the field of semiconductor materials, in particular to a preparation method of an alkaline earth metal-based atomic layer deposition precursor material. Background technique [0002] In current DRAM memory chips, ZrO with high dielectric constant is commonly used 2 , HfO 2 The thin film acts as the dielectric layer of the capacitor. However, with the further improvement of storage requirements, it is necessary to introduce materials with higher dielectric constants. Strontium titanate (SrTiO 3 ), barium titanate (BaTiO 3 ), barium strontium titanate ((Ba,Sr)TiO 3 ) has been extensively studied due to its higher dielectric constant and has great potential for application in DRAM memory. Since the trench aspect ratio of DRAM capacitors is very high, usually in the range of 40:1 to 200:1, ALD deposition of the above thin films has become the only option. In addition, perovskite-structured SrTiO 3 , BaTiO 3 Due to its exce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/00
CPCC07F17/00
Inventor 张学奇袁磊朱思坤李建恒
Owner 合肥安德科铭半导体科技有限公司