JP3518947B2 - Cleaning method for inner surface of cylinder - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for cleaning the inner surface of a cylinder used for filling high purity gas or liquefied gas.

[0002]

2. Description of the Related Art In recent years, particularly in the field of semiconductor industry, five nines or higher gases of extremely high purity are required, but these are usually filled in cylinders and supplied commercially. However, when such a high-purity gas is used, the metal content on the inner surface of the cylinder mixes into the gas, which causes a problem that the purity of the high-purity gas at the time of manufacture deteriorates. In particular, hydrogen chloride, hydrogen bromide, hydrogen iodide, chlorine,
In the case of highly corrosive halogen gases such as boron chloride,
A slight amount of water or oxygen on the inner surface of the cylinder causes corrosion over time, and metal content is significantly mixed.

Generally, when the above-mentioned gas filled in a cylinder is used, a cylinder made of manganese steel or chromium molybdenum steel is often used. However, it is extremely difficult to completely remove a small amount of water and oxygen from the inside of these cylinders, and methods such as vacuum heating and substitution with an inert gas such as nitrogen or helium have been performed so far. , Not enough effect has been obtained.

[0004]

SUMMARY OF THE INVENTION An object of the present invention is to prevent impurities from being mixed in a high-purity gas when the high-purity gas is filled in a cylinder and stored or used after being discharged from the cylinder. A method for cleaning the inner surface of a cylinder is provided.

[0005]

In order to achieve the above object, the present inventors completed the present invention as a result of intensive studies on the relationship between the method of inner surface treatment of a cylinder and the impurities in the filling gas. Came to. That is, the method of cleaning the inner surface of the cylinder of the present invention is characterized by polishing the inner surface of the cylinder, washing with water, and then cleaning with a low-boiling point, hydrophilic solvent, which is used for manufacturing semiconductors and the like. This method can be applied to both corrosive gas and other gas containing cylinders.

[0006]

BEST MODE FOR CARRYING OUT THE INVENTION In carrying out the present invention, first, the inner surface of a cylinder is polished. The polishing method may be a known polishing method such as shot blast polishing or barrel polishing. Further, the inside of the cylinder is washed with water for the purpose of removing polishing residue and the like. After washing with water, the inside of the cylinder is washed with a low-boiling point, hydrophilic solvent.

The solvent used in the present invention includes
Any substance having a low boiling point, which has affinity for impurities such as surfactants and water used for polishing and which can be discharged out of the cylinder, can be used. For example, acetone, methanol, isopropyl alcohol (hereinafter referred to as IPA and (Abbreviated) and the like are preferably used. IP used in the present invention
As the solvent such as A, it is possible to use a solvent having a purity of quality standard for general industry, but in order to obtain a cylinder for high purity gas in which impurities of the present invention are extremely small for the purpose of the present invention, high purity with few particles is used. It is preferable to use the above-mentioned one.

The inner surface of the cylinder is treated with a solvent such as IPA. Specifically, a method of injecting a high-pressure solvent onto the inner surface of the cylinder by inserting a slide type nozzle into the cylinder with the mouth of the cylinder directly below, and the content of the solvent are described. Do this by rotating the container with the cylinder with half the volume of the container lying down and the mouth facing slightly downward.

The effect of this solvent treatment is superior to the treatment by washing with water only because it has excellent ability to dissolve surfactants used for polishing, water on the metal surface inside the cylinder, impurities such as oxygen, It is also considered that the affinity with the metal of the cylinder material is strong and the effect of removing impurities such as water and oxygen in the deep part of the material as well as on the surface of the cylinder is excellent. IPA
Cylinder after solvent treatment such as, heating vacuum, or nitrogen,
The solvent is removed by blowing and replacing with an inert gas such as helium.

[0010]

The present invention will be described in more detail with reference to the following examples.

Example 1 After barrel-polishing the inside of a cylinder made of manganese steel and having a capacity of 900 liters, the mouth of the cylinder was directed directly below, and 150 kgf / cm ² of high-pressure pure water was jetted from a slide type nozzle to make the inside 30 Wash for minutes. Then, it is similarly washed with high-pressure IPA of 150 kgf / cm ² for 2 minutes. Next, heating nitrogen at 5 kgf / cm ² is blown into the bomb to replace the atmosphere and heat-dry at 180 ° C.
Fill the cylinder thus treated with hydrogen chloride and keep it at 20-30 ° C.
After left at room temperature for 1 week, sample 250 ml of the liquid phase inside the bottle into a quartz bottle that has been cooled to about -80 ° C with dry ice-methanol. Then, after evaporating hydrogen chloride at room temperature, the metal salt was dissolved with ultrapure water, and the iron ion concentration was analyzed by ion plasma emission spectrometry. The results are shown in Table 1.

Example 2 The procedure of Example 1 was repeated except that acetone was used as the processing solvent. The results are shown in Table 1.

Example 3 Example 1 except that methanol was used as the treating solvent.
I went the same way. The results are shown in Table 1.

Example 4 Example 4 was repeated except that a cylinder made of chromium-molybdenum steel and having a capacity of 47 liters was used. The results are shown in Table 1.
Shown in.

Example 5 The same procedure as in Example 1 was carried out except that a 3.4 liter cylinder made of SUS 304 was used and charged with hydrogen iodide. The results are shown in Table 1.

Comparative Example 1 Example 1 was repeated except that the inner surface was treated with pure water instead of the solvent. The results are shown in Table 1.

[0017]

[Table 1]

[0018]

Industrial Applicability According to the method of the present invention, it is possible to prevent the deterioration of the purity of the high-purity gas for semiconductor during storage to a practically sufficient extent, which is of great industrial benefit.

─────────────────────────────────────────────────── ─── Continuation of the front page (58) Fields surveyed (Int.Cl. ⁷ , DB name) C23G 5/02 B08B 3/08 C11D 7/26 C11D 7/50

Claims (2)

(57) [Claims] 1. A method for cleaning the inner surface of a cylinder, which comprises polishing the inner surface of the cylinder, washing with water, and then washing with a solvent having a low boiling point and a hydrophilic property. 2. The method for cleaning the inner surface of a cylinder according to claim 1, wherein the low boiling point, hydrophilic solvent is at least one selected from isopropyl alcohol, methanol and acetone.