KR102605327B1 - Processing method of rare earth oxide coating layer - Google Patents

Abstract

The present invention relates to a processing method of a rare earth oxide coating layer for removing and reprocessing the rare earth oxide coating layer coated on a shield member. The processing method of the rare earth oxide coating layer of the present invention involves cleaning the rare earth oxide coating layer by soaking it in a cleaning solution, thereby removing the rare earth oxide coating layer from the shield member. The rare earth oxide coating layer can be effectively peeled off without damaging the (aluminum alloy), and the degree of peeling off the coating layer and work stability can be improved by using a water jet method that sprays water at high pressure without using solid beads. there is.

Description

Processing method of rare earth oxide coating layer}

The present invention relates to a processing method of a rare earth oxide coating layer for removing and reprocessing the rare earth oxide coating layer coated on a shield member.

Generally, among a series of processes for semiconductor manufacturing, there are processes for treating base materials for semiconductor manufacturing with a reaction atmosphere (e.g., process gas) inside a chamber, and these processes are carried out in a chamber device with a chamber space of a certain size.

The inner surface of the chamber of these chamber devices is exposed to the reaction atmosphere, which can easily cause the surface to become contaminated or damaged due to erosion or corrosion. To compensate for this, shield members (Shield Parts) are made removable inside the chamber. The inside of the chamber is protected from various reaction atmospheres by these shield members.

The shield members are upper electrode, GDP (Gas Distribution Plate), Pinnacle, Outer liner, Inner liner, Baffle, Wall liner, Upper. It is used as plasma process chamber parts such as upper liner, door liner, and shower head.

The shield member is made of a metal (e.g. aluminum, anodized aluminum) or non-metal (e.g. ceramic) material with a coating layer (e.g. yttria coating layer) having corrosion resistance to various reaction atmospheres on the surface. When exposed to the reactive atmosphere inside the chamber, the corrosion-resistant coating layer gradually becomes contaminated or damaged and loses its original function, so it is reused after periodic maintenance treatment (e.g., cleaning and restoration of the coating layer).

The method of maintaining the shield member is to peel and remove the damaged or contaminated coating layer and then re-coat the corrosion-resistant coating layer. In particular, to improve maintenance quality, only the existing coating layer is removed without damaging the surface of the shield member. It is important to proceed with re-coating while the delamination has been reliably removed. If the surface of the shield member is damaged, it may cause installation errors and various work errors after it is installed inside the chamber device.

However, in the existing shield cleaning method of a metal deposition chamber, in order to remove process by-products and coating films from the surface of the shield, bead blasting, first cleaning, and first drying operations are followed by plasma treatment, second cleaning, and second drying operations. Since it is carried out through drying operations, the work process is complex, making it difficult to expect satisfactory work efficiency, the lifespan is reduced due to component damage, and devices (equipment) that match each process are required, resulting in excessive cost and time. There is a downside to this.

In particular, the method of removing metal foreign substances from the shield surface through bead blasting can easily cause damage to the shield surface during the removal process, requiring additional work to polish the shield surface each time, further reducing work efficiency. .

Accordingly, the industry is demanding the development of technology that can remove peeling while minimizing surface damage to the shield member.

In order to meet the needs of this industry and improve the conventional method of removing the corrosion-resistant coating layer, the present applicant has developed a method that can minimize surface damage to the shield member when peeling and removing the corrosion-resistant coating layer on the surface of the chamber shield member. We have developed and applied for a technology that can carry out peeling removal work in its original state, and it has been suggested that the quality of peeling removal and work stability of the corrosion-resistant coating layer can be further improved through the technologies proposed by the applicant.

Accordingly, the present applicant would like to propose below a technology that can provide a more improved corrosion resistance coating layer peeling effect compared to previously applied corrosion resistance coating layer peeling technologies.

Republic of Korea Patent Publication No. 10-2019-0048040

The present invention was developed in consideration of and to solve the above-described conventional problems, and is a rare earth oxide that can prevent damage to the shield member while effectively removing the rare earth oxide coating layer formed on the shield member using a cleaning liquid composition containing a nitric acid solution. The purpose is to provide a processing method for the coating layer.

The present invention includes the steps of cleaning a shield member having a rare earth oxide coating layer on its surface by soaking it in a cleaning liquid composition; And a step of re-coating the shield member that has undergone the cleaning step with a rare earth coating composition,

The rare earth oxide coating layer and the composition for rare earth oxide coating are independently Y ₂ O ₃ , YOF, YF3, YAG, YAM, YAS, YSZ, Y ₂ SiO ₅ , Y ₂ Si ₂ O ₇ , Dy ₂ O ₃ , Er ₂ O ₃ and Sm ₂ O ₃ , the cleaning liquid composition is made of nitric acid, and the cleaning step peels the rare earth oxide coating layer from the shield member.

According to the present invention, the rare earth oxide coating layer can be effectively peeled off without damaging the shield member (aluminum alloy) by cleaning the rare earth oxide coating layer by soaking it in a cleaning liquid.

In addition, according to the present invention, the processing method of the rare earth oxide coating layer can improve the degree of peeling of the coating layer of the shield member and work stability by using a water jet method that sprays water at high pressure without using solid beads.

Figure 1 is a schematic process diagram shown to explain the processing method of the coating layer according to an embodiment of the present invention.
2 to 15 are data showing the physical properties and evaluation of peeled samples according to the composition of the cleaning solution used in the step of removing the coating layer in the coating layer processing method according to an embodiment of the present invention.
16 to 22 are data showing the physical properties and evaluation of peeled samples according to the type of coating layer and cleaning time in the coating layer processing method according to an embodiment of the present invention.
Figures 23 to 26 show data showing the physical properties and evaluation of peeled samples according to additional cleaning conditions in the coating layer processing method according to an embodiment of the present invention.
Figures 27 to 29 are data showing the physical properties and evaluation of the peeled anodized aluminum substrate according to the cleaning time of the anodized aluminum substrate in the coating layer processing method according to an embodiment of the present invention.

Preferred embodiments of the present invention will be described with reference to the accompanying drawings as follows. Through this detailed description, the purpose and configuration of the present invention and its characteristics will be better understood.

Hereinafter, in the present invention, we would like to propose a method of efficiently removing the coating layer while reducing damage to the base material compared to the existing method of peeling the coating layer of a shield member by spraying high-pressure water in addition to using a cleaning liquid composition consisting of nitric acid and additives. .

To this end, the processing method of the rare earth oxide coating layer according to an embodiment of the present invention includes the steps of cleaning the shield member (S100), as shown in FIG. 1; and a step (S200) of recoating the shield member that has undergone the cleaning step with a rare earth coating composition. Specifically, the processing method of the rare earth oxide coating layer of the present invention includes the steps of first cleaning the shield member; A step of secondarily cleaning the firstly cleaned shield member; And it may include the step of re-coating the shield member that has gone through the cleaning step with a rare earth coating composition.

The step of cleaning the shield member (S100) is a step of cleaning the shield member with a rare earth oxide coating layer on its surface by immersing it in a cleaning liquid composition.

In the cleaning step (S100), the shield member is a member installed to enable shielding inside the chamber device used in the semiconductor manufacturing process, for example, having a circular peripheral portion to match the chamber shape inside the cylindrical chamber device. It may be in the form of a LINER.

The shield member includes an anodizing layer formed using an anodic oxidation method (including one or more of the sulfuric acid method, hydroxy acid method, chromic acid method, and mixed acid method), and a coating layer formed by a rare earth oxide coating composition on the anodizing layer. You can have

The shield member may not include an anodizing layer.

The shield member may be aluminum or anodized aluminum.

The rare earth oxide coating layer is at least one of Y ₂ O ₃ , YOF, YF3, YAG, YAM, YAS, YSZ, Y ₂ SiO ₅ , Y ₂ Si ₂ O ₇ , Dy ₂ O ₃ , Er ₂ O ₃ and Sm ₂ O ₃ It may contain more than one.

The cleaning step (S100) may be performed to peel off the rare earth oxide coating layer without damaging the surface of the shield member or the anodizing layer formed on the shield member.

In the cleaning step (S100), the shield member may be masked so that only the rare earth oxide coating layer portion of the shield member can be removed.

The cleaning step (S100) includes first cleaning the shield member provided with the rare earth oxide coating layer by placing it in a cleaning liquid composition; And it may include a second cleaning step by spraying high-pressure water on the shield member that has undergone the first cleaning step.

In the first cleaning step, the cleaning liquid composition may consist of nitric acid. Specifically, the cleaning liquid composition may be a nitric acid solution.

The concentration of the nitric acid solution may be 63 to 75%.

By using the cleaning liquid composition as described above, only the rare earth oxide coating layer formed on the shield member can be efficiently removed without damaging the anodizing layer formed on the surface of the shield member.

In the first cleaning step, the shield member can be soaked in a cleaning liquid composition at a temperature of 20°C to 25°C for 30 minutes to 11 hours, 1 hour to 5 hours, 2 hours to 8 hours, or 5 hours to 10 hours. there is.

In the secondary cleaning step, high-pressure water can be sprayed on the shield member that has undergone the primary cleaning step to further peel off the coating layer remaining on the shield member.

The secondary cleaning step can be performed by spraying high-pressure water using a high-pressure spray gun at a pressure of 50 to 200 bar.

As described above, not only can the rare earth oxide coating layer formed on the shield member of the present invention be effectively peeled off by secondary cleaning by spraying high-pressure water, but the peeling method is simple compared to the case of peeling using beads, and the shield member By removing impurities present on the surface, the adhesion between the shield member and the coating layer can be improved when the coating layer is formed again later.

Accordingly, in the cleaning step (S100), the average weight reduction rate of the cleaned shield member may be 0.01% to 0.35% or 0.01% to 0.02%.

Additionally, the average color difference of the shield member cleaned in the cleaning step may be 15 L* to 25 L* or 18 L* to 22 L*.

The re-coating step (S200) is a step of re-coating the shield member from which the rare earth oxide coating layer has been peeled off through the cleaning step using a rare earth coating composition.

In the recoating step (S200), the rare earth coating composition is independently Y ₂ O ₃ , YOF, YF3, YAG, YAM, YAS, YSZ, Y ₂ SiO ₅ , Y ₂ Si ₂ O ₇ , Dy ₂ O It may include at least one of ₃ , Er ₂ O ₃ and Sm ₂ O ₃ .

In the recoating step (S200), the average adhesion of the recoated coating layer may be 1 Mpa to 20 Mpa.

Meanwhile, in the following, in the yttria coating removal method according to the present invention consisting of the above-described steps, tests were conducted to evaluate the coating removal efficiency and physical properties of the substrate according to the cleaning solution used in this method, and the results are It is shown in Tables 1 to 7 and Figure 2.

An experiment was conducted to determine the optimal composition of the cleaning liquid composition for removing the yttria coating in the test examples of the present invention.

In order to confirm the degree of coating layer removal and anodizing damage depending on the cleaning solution composition in the present invention, a total of 10 cleaning solution compositions having the composition ratios shown in Table 1 below were used.

Input amount (volume) Temperature of deionized water (℃) Nitric acid solution deionized water Example 1 One 0 25 Comparative Example 1 One One 25 Comparative Example 2 One One 100 Comparative Example 3 2 One 25 Comparative Example 4 5 One 25 Comparative Example 5 10 One 25

When the anodized aluminum substrate on which the yttria coating layer (SPS Y203 coating) was formed was cleaned using the cleaning liquid composition, the weight of the anodized aluminum substrate was measured to observe the coating layer removal rate and damage to the aluminum substrate, and the results were It is shown in Figures 2 to 4 and Table 2.

cleaning time Anodizing R _a (μinch) Anodizing thickness (㎛) Comparative Example 1 0hr Max 114 Max 44 Min 99 Min 42 Avg 106 Avg 43 30min Max 110 Max 42 Min 87 Min 40 Avg 98 Avg 41 Comparative Example 2 0hr Max 46 Max 46 Min 38 Min 44 Avg 41 Avg 45 30min Max 50 Max 44 Min 46 Min 41 Avg 47 Avg 43

Figure 2 is a photographic image of the anodized aluminum substrate on which the SPS Y2O3 coating layer was formed using the cleaning liquid compositions of Example 1, Comparative Example 1, and Comparative Example 2 after cleaning the anodized aluminum substrate for 3 hours or 30 minutes. and an image taken with Hirox RH-200. Figure 3 is an image of an anodized aluminum substrate with an SPS Y2O3 coating layer after cleaning it for 30 minutes using the cleaning liquid compositions of Comparative Example 1 and Comparative Example 2. This is a graph showing thickness and roughness.

Figure 4 shows the anodized aluminum substrate on which the SPS Y2O3 coating layer was formed using the cleaning solution compositions of Comparative Example 1 and Comparative Example 2, and the coating layer and the anodized aluminum substrate were photographed with a Hirox RH-200 after cleaning them for 3 hours or 30 minutes. It is one image.

Table 2 shows the thickness and roughness of the anodized aluminum substrate on which the SPS Y2O3 coating layer was formed using the cleaning liquid compositions of Comparative Examples 1 and 2 after cleaning the anodized aluminum substrate for 3 hours or 30 minutes.

Looking at Figures 2 to 4 and Table 2, when cleaning with the cleaning solution composition of Example 1, only the yttria coating layer was removed, but when cleaning with the cleaning solution compositions of Comparative Examples 1 and 2, the anodized aluminum base was removed. You can see that the anodizing layer is damaged.

Through this, it can be seen that cleaning using a nitric acid solution is the most efficient in peeling off the rare earth oxide coating layer.

Additionally, when cleaning the inner liner on which the yttria coating layer (SPS Y203 or APS Y2O3 coating) was formed using the cleaning liquid composition, the thickness and roughness of the aluminum substrate and the weight of the inner liner were measured to determine the coating layer removal rate and aluminum Damage to the substrate was observed, and the results are shown in Figures 5 and 6.

Figure 5 is a photographic image of an anodized aluminum substrate after cleaning the inner liner on which the SPS Y2O3 coating layer or the APS Y2O3 coating layer was formed using the cleaning liquid composition of Example 1 for 3 hours, and an image taken with Hirox RH-200. .

Figure 6 is a photographic image of an anodized aluminum substrate after cleaning the inner liner on which the SPS Y2O3 coating layer or the APS Y2O3 coating layer was formed using the cleaning solution composition of Comparative Example 1 for 30 minutes, and an image taken with Hirox RH-200. .

Looking at Figures 5 and 6, when the inner liner was cleaned for 3 hours using the cleaning liquid composition of Example 1, it was confirmed that the SPS Y2O3 coating layer was peeled off and the APS Y2O3 coating layer was partially peeled off. When the inner liner was cleaned for 30 minutes using the cleaning liquid composition, the coating layer was peeled off, but some of the coating layer remained, and the thickness of the anodizing layer decreased from 50㎛ to 46㎛, confirming that the anodizing layer was partially damaged.

Through this, it can be seen that the composition of Example 1 efficiently removes the coating layer without damaging the anodizing layer of the shield member in the processing method of the rare earth oxide coating layer of the present invention.

In addition, the anodized aluminum substrate on which the yttria coating layer (SPS Y203 coating, APS Y2O3 coating) was formed using the cleaning liquid composition for 10 minutes, 30 minutes, 1 hour, 2 hours, 3 hours, 5 hours, or 17 hours, respectively. When cleaning, the roughness, thickness, weight, and weight reduction rate of the anodized aluminum substrate were measured to observe the coating layer removal rate and damage to the anodized aluminum substrate. The results are shown in Figures 7 to 15 and Table 3. .

division sejung
hour Anodizing R _a (μinch) Anodizing thickness (㎛) Weight (g) Weight reduction rate (%) Example 1 0hr 53.2 50.0 - - 10min 54.1 49.7 - - 30min 45.3 49.0 - - 1hr 46.0 49.0 - - 2hr 47.2 48.8 - 3hr 51.1 48.6 - - 5hrs 52.7 49.8 - - Comparative Example 3 0hr 97.89 46.9 36.629 - 10min 94.01 46.5 32.624 -0.015 30min 95.59 46.9 32.623 -0.018 1hr 93.71 47.3 32.622 -0.021 2hr 89.64 45.9 32.622 -0.021 3hr 96.72 47.9 32.617 -0.037 5hrs 97.17 45.5 32.612 -0.052 Comparative Example 4 0hr 89.57 43.7 33.079 - 10min 91.33 44.9 33.077 -0.006 30min 81.16 46.0 33.075 -0.012 1hr 74.43 47.4 33.073 -0.018 2hr 83.35 46.3 33.072 -0.021 3hr 87.35 44.8 33.066 -0.039 5hrs 81.67 46.0 33.064 -0.045 Comparative Example 5 0hr 82.64 45.5 33.051 - 10min 81.21 44.2 33.050 -0.003 30min 76.15 44.5 33.047 -0.012 1hr 77.12 45.8 33.047 -0.012 2hr 83.07 44.4 33.046 -0.015 3hr 78.28 44.4 33.043 -0.024 5hrs 79.05 45.5 33.041 -0.030

Figure 7 shows the anodized aluminum substrate on which the Y2O3 coating layer was formed using the cleaning liquid compositions of Example 1, Comparative Example 1, and Comparative Examples 3 to 5 for 10 minutes, 30 minutes, 1 hour, 2 hours, 3 hours, and 5 hours. This is a photographic image of an anodized aluminum substrate after cleaning for 1 hour or 17 hours. Figure 8 shows an anodized image in which an APS Y2O3 coating layer was formed using the cleaning solution compositions of Example 1, Comparative Example 1, and Comparative Examples 3 to 5. This is a photographic image of an anodized aluminum substrate after cleaning the treated aluminum substrate for 10 minutes, 30 minutes, 1 hour, 2 hours, 3 hours, 5 hours, or 17 hours.

Table 3 shows the anodized aluminum substrate on which the SPS Y2O3 coating layer or the APS Y2O3 coating layer was formed using the cleaning liquid compositions of Example 1, Comparative Example 1, and Comparative Example 2 for 10 minutes, 30 minutes, 1 hour, 2 hours, 3 hours, This shows the thickness, roughness, weight, and weight reduction rate of anodized aluminum substrate after cleaning for 5 or 17 hours.

Looking at Figures 7, 8, and Table 3, when the cleaning liquid composition of Example 1 was used, the coating layer began to peel when the cleaning time (supporting time) was 2 hours or more, and the coating layer completely peeled off when it was 3 hours or more. Comparative Example 1 It was confirmed that the coating layer of the cleaning solution composition of Comparative Example 3 peeled off after 30 minutes, that of the cleaning solution composition of Comparative Example 3, the coating layer peeled off after 1 hour, and that of the cleaning solution compositions of Comparative Examples 4 and 5, the coating layer peeled off after 2 hours.

9 and 11 show the anodized aluminum substrate without forming a coating layer using the cleaning liquid compositions of Example 1 and Comparative Examples 3 to 5 for 10 minutes, 30 minutes, 1 hour, 2 hours, 3 hours, This is a photographic image of an anodized aluminum substrate after cleaning for 5 or 8 hours.

10 and 12 show an anodized aluminum substrate without a coating layer formed using the cleaning liquid compositions of Example 1 and Comparative Examples 3 to 5 for 10 minutes, 30 minutes, 1 hour, 2 hours, 3 hours, This is an image taken with Hirox RH-200 of an anodized aluminum substrate after cleaning for 5 or 8 hours.

Figure 13 shows an anodized aluminum substrate without a coating layer formed using the cleaning liquid compositions of Example 1 and Comparative Examples 3 to 5 for 10 minutes, 30 minutes, 1 hour, 2 hours, 3 hours, or 5 hours. This is a graph showing the thickness and roughness of an anodized aluminum substrate after cleaning.

Figure 14 shows an anodized aluminum substrate without a coating layer formed using the cleaning solution composition of Example 1 for 10 minutes, 20 minutes, 30 minutes, 1 hour, 2 hours, 3 hours, 5 hours, 8 hours, and 12 hours. Alternatively, this is a graph showing the colorimeter (3nh Technology, NS800) and weight difference of an anodized aluminum substrate after cleaning for 17 hours, and an image taken of the anodized aluminum substrate.

Figure 15 shows an anodized aluminum substrate without a coating layer formed using the cleaning solution composition of Comparative Example 4 for 10 minutes, 20 minutes, 30 minutes, 1 hour, 2 hours, 3 hours, 5 hours, 8 hours, and 12 hours. Alternatively, this is a graph showing the colorimeter (3nh Technology, NS800) and weight difference of an anodized aluminum substrate after cleaning for 17 hours, and an image taken of the aluminum substrate.

9 to 15, when the aluminum substrate including the anodizing layer was immersed in the cleaning liquid composition of Example 1, the anodizing layer was not damaged, but when immersed in the cleaning liquid composition of Comparative Examples 3 to 5, the aluminum substrate was damaged. It was confirmed that the anodizing layer was damaged.

In addition, when cleaning an anodized aluminum substrate with a yttria coating layer (SPS Y203 coating, APS Y2O3 coating, APS YOF coating) or an anodized aluminum substrate (sulfuric acid method or oxalic acid method) using the cleaning liquid composition of Example 1, , the thickness and roughness of the coating layer and the roughness and thickness of the aluminum substrate were measured to observe the coating layer removal rate and damage to the aluminum substrate, and the results are shown in Figures 16 to 22 and Table 4 and Table 5.

SPSY2O3 APSY2O3 APS YOF sejung
hour Coating layer R _a
(μinch) Coating layer thickness (㎛) Coating layer R _a
(μinch) Coating layer thickness (㎛) Coating layer R _a
(μinch) Coating layer thickness (㎛) 0hr 83.7 144 176.8 177 151.7 201 10min 86.0 145 199.6 183 149.8 202 30min 82.9 147 197.8 78 150.9 202 1hr 68.9 140 195.4 182 146.2 200 2hr - 45 172.3 182 145.1 182 3hr Coating layer peeling 182.7 177 Coating layer peeling 5hrs 138.8 162 8hr - - 17hrs - 34.0 Sulfuric acid method anodizing Oxalic acid anodizing sejung
hour R _a of Al
(μinch) Thickness of Al (㎛) R _a of Al
(μinch) Thickness of Al (㎛) 0hr 53.2 50.0 26.0 22.4 10min 54.1 49.7 23.0 21.8 30min 45.3 49.0 24.7 21.5 1hr 46.0 49.0 23.8 20.6 2hr 47.2 48.8 23.3 20.4 3hr 51.1 48.6 24.0 20.7 5hrs 52.6 49.8 21.9 21.8 8hr 52.2 46.6 24.9 19.7 17hrs - - - -

Figure 16 shows cleaning of an anodized aluminum substrate with a yttria coating layer (SPS Y203 coating, APS Y2O3 coating, APS YOF coating) or anodized aluminum substrate (sulfuric acid method or oxalic acid method) using the cleaning liquid composition of Example 1. This is an image taken of a sample after cleaning. Figure 17 is an image taken of the surface of an aluminum substrate after cleaning the anodized aluminum substrate (sulfuric acid method or oxalic acid method) using the cleaning liquid composition of Example 1.

Figure 18 shows the anodized aluminum substrate on which the yttria coating layer (SPS Y203 coating, APS Y2O3 coating, APS YOF coating) was formed using the cleaning liquid composition of Example 1 for 10 minutes, 30 minutes, 1 hour, 2 hours, and 3 hours. Alternatively, this is an image taken of an aluminum substrate after cleaning for 17 hours.

Figure 19 is an image taken of an aluminum substrate that was anodized (sulfuric acid method or oxalic acid method) using the cleaning liquid composition of Example 1 after cleaning it for 10 minutes, 30 minutes, 1 hour, or 3 hours.

Figure 20 shows an anodized aluminum substrate on which a yttria coating layer (SPS Y203 coating, APS Y2O3 coating, APS YOF coating) was formed or an anodized aluminum substrate (sulfuric acid method or oxalic acid method) using the cleaning liquid composition of Example 1 for 10 minutes. , This is a graph measuring the thickness and roughness of the aluminum substrate after cleaning for 30 minutes, 1 hour, 2 hours, 3 hours, 5 hours, 8 hours, or 17 hours.

Looking at Figures 16 to 20 and Table 4, a test was conducted to peel off the coating layer on an anodized aluminum substrate. The SPS Y2O3 coating layer began to peel off 2 hours after being immersed in the cleaning solution composition of Example 1, and the coating layer completely peeled off after 3 hours, and the APS Y2O3 coating layer began peeling off 17 hours after being immersed in the cleaning solution composition of Example 1. It was confirmed that the APS YOF coating layer peeled off 3 hours after being immersed in the cleaning liquid composition of Example 1, and accordingly, the roughness of the aluminum substrate was confirmed to be reduced. In addition, it was confirmed that the surface of the anodizing layer formed by the sulfuric acid method or the oxalic acid method was not damaged even when immersed in the cleaning liquid composition of Example 1 for 8 hours, and the surface roughness was also constant.

Meanwhile, even after performing Example 1, a partial coating layer remains as shown in FIG. 16, and high-pressure DI Spray is required to effectively remove it. The APS Y203 coating layer peels off 17 hours after being immersed in the cleaning liquid composition of Example 1, and this can be reduced by using high-pressure DI Spray.

division sejung
hour Coating layer R _a
(μinch) Coating layer thickness (㎛) R _a of Al
(μinch) Thickness of Al (㎛) Weight (g) Weight reduction rate (%) coupon 0hr 59 156 36 61 35.729 - 10min 59 156 38 61 35.710 -0.05 30min 72 154 39 61 35.625 -0.24 1hr 56 154 39 61 35.586 -0.11 3hr 73 54 36 60 35.133 -1.27

Figure 21 is an image taken of an anodized aluminum substrate on which a yttria coating layer (SPS Y203 coating) was formed using the cleaning liquid composition of Example 1 after cleaning for 10 minutes, 30 minutes, 1 hour, or 3 hours. 22 shows the thickness of the anodized aluminum substrate on which the yttria coating layer (SPS Y203 coating) was formed using the cleaning liquid composition of Example 1 after cleaning for 10 minutes, 30 minutes, 1 hour, or 3 hours. and a graph showing roughness.

Table 5 shows the thickness and roughness of the coating layer after cleaning the anodized aluminum substrate on which the yttria coating layer (SPS Y203 coating) was formed using the cleaning solution composition of Example 1 for 10 minutes, 30 minutes, 1 hour, or 3 hours, It shows the thickness, roughness, weight, and weight reduction rate of the aluminum substrate.

Looking at Figures 21, 22, and Table 5, it was confirmed that the thickness of the coating layer was reduced and peeled off after 3 hours of immersion in the cleaning liquid composition of Example 1 for the aluminum substrate including the SPS Y2O3 coating layer, but the anodizing layer was not damaged. It was confirmed that the surface roughness was almost constant. At this time, high-pressure DIW Spray is used to remove the remaining coating film.

Additionally, after cleaning the SEMES inner liner baffle on which the yttria coating layer (SPS Y203 coating, APS Y2O3 coating, APS YOF coating) was formed using the cleaning liquid composition of Example 1, whether or not additional treatment was performed. Depending on the type, the thickness and roughness of the baffle and the roughness and thickness of the aluminum substrate were measured before and after cleaning to observe the coating layer removal rate and damage to the aluminum substrate. The results are shown in Figures 23 to 26 and Table 6 and Table 7. .

Before dipping Thickness (㎛) Roughness R _a (μinch) point1 point2 point3 point1 point2 point3 wall
(SPS)
coating award 186 181 185 93 54 63 middle 175 177 168 77 59 63 under 190 208 213 89 58 69 wing surface
(APS)
coating award 187 171 182 133 116 141 middle 178 197 179 137 123 147 under 181 199 196 143 130 147 interior
Anod award 75.3 72.4 74.5 59 53 55 middle 77.3 72.6 80.8 51 78 56 under 77.6 72.8 74.7 56 70 43 Out
Anod award Not measurable middle under After soaking for 4 hours and 30 minutes Thickness (㎛) Roughness R _a (μinch) point1 point2 point3 point1 point2 point3 wall
(SPS)
coating award Coating layer peeling middle under wing surface
(APS)
coating award 162 90.3 167 116 121 120 middle 166 179 176 97 101 111 under 165 173 85.6 102 126 125 interior
Anod award 69.6(-5.7) 70(-2.4) 72.1(-2.4) 69 75 46 middle 76(-1.3) 72.1(-0.5) 79.4(-1.4) 59 87 66 under 70.8(-6.8) 70.9(-1.9) 72.6(-2.1) 51 61 64 Out
Anod award 45 45 47.8 105 144 116 middle 47.3 46.5 53.3 120 141 102 under 44.8 49 50.3 106 114 114

division Thickness of Al (anodizing) (㎛) point1 point2 point3 point4 Before loading 53 50 53 51 Soak for 1 hour Process 50 48 49 53 Bead #320 21.1 28.1 22.8 23.2 Bead #120 18.9 19.5 19.4 18.4 Hold for 2 hours and 30 minutes Power wash 49.5 44.7 48.6 53.4

division Thickness of coating layer (㎛) point1 point2 point3 point4 Before loading 61 62.3 60.4 61.1 Soak for 3 hours top 62.0 61.6 63.2 61.4 Power wash 49.8 50.1 48.7 49.5

Figure 23 shows that when cleaning the SPS Y2O3 coated inner liner baffle using the cleaning solution composition of Example 1, CO ₂ (6) is added after cleaning by soaking in the cleaning solution composition for 30 minutes or 1 hour. bar), BEAD 400 5kgf, and high pressure water. Figure 24 and Table 6 show that when cleaning the SPS Y2O3 coated inner liner, the cleaning solution composition is applied for 1 hour or 2 hours 30 minutes. This is a table showing the images taken after carrying and cleaning and additionally performing one or more of BEAD #120, BEAD #320, and high pressure water (power wash), and the thickness of the inner liner after cleaning.

Figure 25 is an image taken after cleaning the SPS Y2O3 coated inner liner by soaking it in the cleaning liquid composition for 2 hours and then additionally performing BEAD #120 and BEAD #320.

Figure 26 is an image taken after cleaning the SPS Y2O3 coated inner liner by soaking it in the cleaning liquid composition for 1 hour or 2 hours and then performing additional high-pressure water (power wash).

Table 7 shows the thickness of the liner measured after cleaning the SPS Y2O3 coated wall liner by soaking it in the cleaning liquid composition for 3 hours and then performing additional high-pressure water (power wash).

Looking at Figures 23 to 26, Table 6, and Table 7, Bead and CO2 Blast were performed as a technology to partially remove the coating film remaining when Example 1 was applied to the product. Beads damage anodizing, and CO2 blast does not partially remove the coating, so high-pressure DIW Spray is used to remove the remaining coating.

In addition, when the anodized aluminum substrate was cleaned using the cleaning liquid composition of Example 1, the thickness, roughness, weight, and color difference of the aluminum substrate before and after cleaning were measured, and damage to the aluminum substrate was observed. As a result, is shown in Figures 27 to 29.

Figure 27 is an image and table showing the thickness, roughness, weight, and color difference of the aluminum substrate before and after cleaning when the anodized aluminum substrate was cleaned using the cleaning liquid composition of Example 1.

Figure 28 is a graph showing the change in thickness, roughness, weight, and color difference of the aluminum substrate before and after cleaning when the anodized aluminum substrate was cleaned using the cleaning liquid composition of Example 1.

Figure 29 is a graph showing the change in withstand voltage (BDV) of the aluminum substrate before and after cleaning when the anodized aluminum substrate was cleaned using the cleaning liquid composition of Example 1, and an image taken of the aluminum substrate.

Looking at Figures 27 to 29, the change over time in Example 1 is measured, and the anodizing thickness reduction and BDV value change significantly from 11 hours or more. Since horizontal cracks occur after 12 hours and the withstand voltage value decreases significantly, it can be seen that soaking and cleaning for up to 11 hours effectively removes the coating layer without damaging the surface of the shield member.

Claims (10)

A step of cleaning a shield member having a rare earth oxide coating layer on its surface by soaking it in a cleaning liquid composition; and
Recoating the shield member that has undergone the cleaning step with a rare earth oxide coating composition; Including,
The rare earth oxide coating layer and the composition for rare earth oxide coating are independently Y ₂ O ₃ , YOF, YF3, YAG, YAM, YAS, YSZ, Y ₂ SiO ₅ , Y ₂ Si ₂ O ₇ , Dy ₂ O ₃ , Er ₂ O Contains at least one or more of ₃ and Sm ₂ O ₃ ,
The cleaning liquid composition consists of a nitric acid solution with a concentration of 63-75%,
The average weight reduction rate of the shield member cleaned in the cleaning step is 0.01% to 0.35%,
The cleaning step is a method of processing a rare earth oxide coating layer wherein the rare earth oxide coating layer is peeled from the shield member. According to paragraph 1,
The cleaning step is,
A step of first cleaning a shield member provided with a rare earth oxide coating layer by submerging it in a cleaning liquid composition; and
A method of processing a rare earth oxide coating layer comprising the step of secondary cleaning by spraying high-pressure water on the shield member that has undergone the primary cleaning step.
According to paragraph 1,
In the cleaning step, the shield member is immersed in a cleaning liquid composition at a temperature of 20 ℃ to 25 ℃ for 30 minutes to 11 hours.
According to paragraph 1,
The shield member is a processing method of a rare earth oxide coating layer including an anodizing layer formed using an anodic oxidation method.

According to clause 4,
A method of processing a rare earth oxide coating layer, characterized in that the anodic oxidation method includes at least one of the sulfuric acid method, hydroxy acid method, chromic acid method, and mixed acid method.
delete According to paragraph 1,
A method of processing a rare earth oxide coating layer, characterized in that the average adhesion of the re-coated coating layer in the re-coating step is 1 Mpa to 20 Mpa.
delete According to paragraph 2,
A method of processing a rare earth oxide coating layer, characterized in that using a high-pressure spray gun with a pressure of 50 bar to 200 bar when spraying high-pressure water in the cleaning step. According to paragraph 1,
A method of processing a rare earth oxide coating layer, characterized in that the shield member is aluminum or anodized aluminum.