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Method for cleaning ALD source steel cylinder

A steel cylinder and post-cleaning technology, which is applied in the direction of liquid cleaning methods, cleaning methods and utensils, chemical instruments and methods, etc., can solve problems affecting downstream applications of thin film deposition, difficult to clean, and contamination of high-purity ALD precursors

Pending Publication Date: 2021-12-21
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

[0004] At present, the cylinder cleaning process is emptying the residual liquid, opening oxidation, alkali washing, pickling, and ultrapure water washing. Such precursors, the oxidation process will form a dense oxide film inside the steel cylinder and the valve core, which is difficult to clean. It will pollute the high-purity ALD precursor during filling and affect downstream applications such as film deposition.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In the clean room, put the ALD source steel cylinder in an anhydrous and oxygen-free glove box, and use anhydrous n-hexane to carry out preliminary cleaning on the steel cylinder; fill the above-mentioned cleaned steel cylinder with n-hexane, and set the temperature to 1000W at 25 Ultrasonic cleaning at ℃ for 15 minutes; after ultrasonic cleaning, move the steel cylinder out of an anhydrous and oxygen-free environment, and add 10% NaOH-isopropanol mixed solution, 10% HNO 3 The solution and ultrapure water were ultrasonically cleaned. After cleaning, it was filled with ultrapure water and left to stand for 24 hours. The amount of metal impurities remaining in the cylinder was analyzed by ICP-OES, and the results showed that the total metal impurities were less than 1ppb.

Embodiment 2

[0031] In the clean room, put the ALD source steel cylinder in an anhydrous and oxygen-free glove box, and use anhydrous n-hexane to carry out preliminary cleaning on the steel cylinder; fill the above-mentioned cleaned steel cylinder with n-hexane, and set the temperature to 1000W at 25 Ultrasonic cleaning at ℃ for 15 minutes; after ultrasonic cleaning, the steel cylinder was removed from the anhydrous and oxygen-free environment, and 10% NaOH-ethanol mixed solution, 10% HNO 3 The solution and ultrapure water were ultrasonically cleaned. After cleaning, it was filled with ultrapure water and left to stand for 24 hours. The amount of metal impurities remaining in the cylinder was analyzed by ICP-OES, and the results showed that the total metal impurities were less than 1ppb.

Embodiment 3

[0033] In the clean room, the ALD source steel cylinder is placed in an anhydrous and oxygen-free glove box, and the steel cylinder is initially cleaned with anhydrous n-heptane; Ultrasonic cleaning at 25°C for 15 minutes; after ultrasonic cleaning, remove the steel cylinder from an anhydrous and oxygen-free environment, and add 10% NaOH-ethanol mixed solution, 10% HNO 3 The solution and ultrapure water were ultrasonically cleaned. After cleaning, it was filled with ultrapure water and left to stand for 24 hours. The amount of metal impurities remaining in the cylinder was analyzed by ICP-OES, and the results showed that the total metal impurities were less than 1ppb.

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Abstract

The invention discloses a method for cleaning an ALD source steel cylinder. The method for cleaning the ALD source steel cylinder comprises the following steps: (1) in a water-free and oxygen-free glove box, adding anhydrous alkane into the ALD precursor source steel cylinder for cleaning; (2) fully filling the steel cylinder cleaned in the step (1) with the anhydrous alkane, and carrying out ultrasonic cleaning; (3) moving the steel cylinder out of the glove box, and cleaning with an organic solvent-alkali system, an acid solution system and an ultrapure water system in sequence; and (4) fully filling the cleaned steel cylinder with ultrapure water, standing, carrying out ICP-OES detection, and drying for later use after the detection is qualified. By means of the cleaning method, precursors, oil substances, oxide impurities and metal impurity particles in the ALD precursor source steel cylinder can be cleaned, the ALD source filling requirement is met, the method is simple to operate, the cleaning process is safe and easy to operate, the cleaning raw materials are low in cost and short in period, and the requirements for purifying, filling and producing the steel cylinder can be rapidly provided.

Description

technical field [0001] The invention relates to a chemical process method, in particular to a cleaning method for an ALD source steel cylinder. Background technique [0002] As the key precursor material of atomic layer deposition technology, ALD source can deposit TiN and TiO 2 、TaN x , HfO 2 , ZrO 2 , HfZr x o y , La 2 o 3 and other types of film. These new materials have a wide range of applications in high-K gate oxide layers, storage capacitive electrolytes, special fiber doping, optical thin films, solar cells and other fields. [0003] The ALD source steel cylinder, as the precursor transportation system of atomic layer deposition technology, provides a 6N ALD source; in order to prevent the remaining source residue from polluting the steel cylinder and the cylinder valve during the treatment process, it is particularly important to study how to deal with and clean the steel cylinder. [0004] At present, the cylinder cleaning process is emptying the residual...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23G5/024C23G1/19C23G1/08B08B3/12
CPCC23G5/024C23G1/19C23G1/085C23G1/08B08B3/12
Inventor 任大平
Owner 苏州源展材料科技有限公司
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