Method for producing high-density yttrium oxide film by atmospheric plasma spray method and yttrium oxide thermal spray coating film produced using same

Abstract

The present invention relates to a method for manufacturing a yttrium oxide thermal spray coating film, and more particularly, to a method for manufacturing a yttrium oxide thermal spray coating film, which forms a yttrium oxide thermal spray coating film on a substrate by disposing a spray unit at a distance of 50-130 mm from the substrate and performing atmospheric plasma spray of a Y2O3 thermal spray powder, and supplying water together with the powder for Y2O3 thermal spraying at a speed of 50 ml / m to 400 ml / m from a position 25 mm to 50 mm from a plasma forming nozzle, thereby manufacturing the powder for Y2O3 thermal spraying, which has low porosity, is very dense, and has excellent plasma resistance.

Description

Technical Field

[0001] The present invention relates to a method for manufacturing a high-density yttrium oxide thermal spray coating by using an atmospheric plasma spraying method of Y2O3 thermal spray powder. Background Art

[0002] In the semiconductor manufacturing process, the importance of plasma dry etching is becoming increasingly prominent in order to achieve microfabrication for highly integrated circuits on substrates such as silicon wafers.

[0003] In order to use in such an environment, it has been proposed to use materials with excellent plasma resistance as chamber components or to form a film with a material with excellent plasma resistance on the surface of the component to increase the service life of the component.

[0004] Among them, the technology of imparting new functionality by coating the surface of a substrate with various materials has been used in various fields. As one of such surface coating technologies, for example, a thermal spraying method is known, in which thermal spraying particles composed of materials such as ceramics are sprayed on the surface of a substrate in a softened or molten state by combustion or electrical energy to form a thermal spraying film.

[0005] Generally speaking, thermal spray coating is performed by heating fine powder to melt it and then spraying the molten powder onto the surface of the base material to be coated. When the sprayed molten powder is rapidly cooled, the molten powder solidifies and is deposited on the surface of the coating object mainly by mechanical bonding force.

[0006] In the above-mentioned thermal spray coating, plasma thermal spray coating using a high-temperature plasma flame to melt the powder is necessary for coating high-melting-point metals (such as tungsten or molybdenum) and ceramics. The thermal spray coating takes advantage of the material properties of the base material, which is not only conducive to the production of highly functional materials, but also exhibits the characteristics of wear resistance, corrosion resistance, heat resistance, thermal barrier, superhardness, oxidation resistance, insulation, friction characteristics, heat dissipation, and biological function radiation resistance, and, compared with other coating methods such as chemical vapor deposition or physical vapor deposition, it can also coat a wide area of ​​objects in a short time.

[0007] Moreover, in the manufacturing field of semiconductor equipment, etc., micro-machining is usually performed on the surface of the semiconductor substrate by dry etching (Etcher) using plasma of halogen gases such as fluorine, chlorine, and bromine. In addition, after dry etching, oxygen plasma is used to clean the inside of the chamber (vacuum container) from which the semiconductor substrate is removed. At this time, inside the chamber, components exposed to highly reactive oxygen plasma or halogen gas plasma may be corroded. Moreover, if the corroded (eroded) part falls off from the corresponding component in the form of ions, such particles adhere to the semiconductor substrate and become foreign matter that causes circuit defects (hereinafter, the corresponding foreign matter will be referred to as particles).

[0008] Therefore, conventionally, in semiconductor device manufacturing equipment, a thermal spray coating of a ceramic having plasma erosion resistance has been provided on a member exposed to plasma of oxygen gas, halogen gas, or the like in order to reduce particle generation.

[0009] The factors causing the generation of the particles include the peeling of the reaction products attached to the vacuum chamber and the deterioration of the chamber due to the use of halogen gas plasma or oxygen plasma. In addition, the inventors have found through research that the number and size of particles generated from the thermal spray film in a dry etching environment are caused by the strength of the bonding force between the particles constituting the thermal spray film, the presence of unmelted particles, or high porosity.

[0010] In particular, the higher the density of the coating inside the ceramic thermal spray film, the lower the degree of adsorption of CFx series process gases caused by defects such as pores in the dry etching process, thereby reducing etching caused by plasma ion collisions.

[0011] Generally, as a coating method for forming a high-density thermal spray coating, there is a suspension plasma spray method (SPS). Compared with the air plasma spray method (APS), the suspension plasma spray method (SPS) has the disadvantages of a complicated manufacturing method and an increased manufacturing unit price.

[0012] As for the suspension plasma spraying (SPS) technology, when coating is performed in a semiconductor chamber with the help of a relatively high heat source, the process temperature is high, so problems such as product deformation occur. As the particle size decreases, the particle flight distance becomes shorter, and the working distance between the plasma equipment and the substrate to be coated becomes closer, which limits local operations. In addition, because the SPS technology is a suspension state of water and particle dispersion, when the same volume is injected, the film formation speed of the coating is low, and additional process time occurs, resulting in high manufacturing costs.

[0013] In addition, as semiconductor process conditions become more severe, RF plasma high-power equipment is required to form a stable thick film of more than 150μm. However, when SPS technology forms a thick film of more than 150μm, internal cracks or peeling caused by residual stress occur, resulting in technical limitations in achieving a coating thickness of several hundred μm.

[0014] Therefore, it is necessary to develop a technology for realizing a high-density thermal spray coating using the existing atmospheric plasma spraying (APS).

[0015] The powder of the thermal spray material used in the conventional APS thermal spray method is a granular powder of 20 to 40 μm formed by primary particles of several μm level gathered together, so a method of increasing the density of the thermal spray film by forming the primary powder constituting such a thermal spray material to be less than 1 μm has been proposed. However, in the case of this method, as the specific surface area of ​​the granular powder increases, heat cannot be uniformly transferred to the primary powder inside the particles, so that a film including a non-melted or re-melted state is formed on the surface or inside of the thermal spray film, which becomes a cause of particle generation in the dry etching process.

[0016] In addition, if the secondary particles formed by the granular powder become too small, the electrostatic attraction between the granular powders will cause multiple particles to agglomerate, making it difficult to transfer them in the air. Or after the particles are transferred, they may not be transferred to the frame in the center due to their low mass and are likely to be dispersed to other places.

[0017] As another method of forming a high-density coating layer, there is a method of coating by shortening the spacing distance (the distance between the base material and the plasma). Since the kinetic energy of the molten particles (Particles), that is, the powder for thermal spraying, is large and the cooling time is short, it is possible to form a relatively high-density coating.

[0018] However, due to the short spacing, the moving distance of the molten thermal spray powder becomes short, and deoxidation occurs, causing the surface of the thermal spray film to partially or completely turn black, and the film color is different from the conventional one, which leads to the following problems.

[0019] When the thermal spray coating is black, it is difficult to distinguish from wastewater after use in semiconductor processes, making it difficult to predict the arrival of cleaning and recoating cycles. In addition, the color change of the thermal spray coating will change the emissivity, resulting in the need to change the semiconductor process conditions.

[0020] In order to solve this problem, the surface of the thermal sprayed film can be restored to white by heat treating the thermal sprayed film that has turned black in an atmospheric (oxygen-containing) atmosphere. However, the additional heat treatment process leads to a decrease in production speed and an increase in manufacturing cost. In addition, since most semiconductor chambers are made of metal materials, the base material will be thermally damaged during the heat treatment process.

[0021] As a prior art, according to the thermal spraying material disclosed in Korean Patent Publication No. 10-2016-0131918 (November 16, 2016), as constituent elements include rare earth element oxyhalide (RE-OX) including rare earth elements (RE), oxygen (O) and halogen elements (X), and the molar ratio of the halogen element to the rare earth element (X / RE) is greater than 1.1, thereby improving plasma resistance and improving properties such as porosity and hardness.

[0022] As described above, although many technologies for manufacturing yttrium oxyfluoride thermal spray materials with improved physical properties such as porosity and hardness have been proposed so far in order to overcome the limitations of the physical properties of yttrium oxide thermal spray materials, in reality, the industry continues to need to develop technologies for manufacturing dense thermal spray films to improve plasma resistance. Summary of the invention

[0023] Problem that the invention aims to solve

[0024] The main purpose of the present invention is to solve the above-mentioned problems and provide a method for manufacturing an yttrium oxide thermal spray coating, by supplying water (distilled water) together with Y2O3 thermal spray powder to prevent deoxidation of yttrium oxide, thereby preventing the thermal spray coating from changing color, and by configuring the spacing distance of the spraying units (the distance between the base material and the plasma) to be relatively close, using the large kinetic energy of the thermal spray powder to manufacture a dense yttrium oxide thermal spray coating.

[0025] Means used to solve problems

[0026] In order to achieve the above-mentioned purpose, one embodiment of the present invention provides a method for manufacturing a yttrium oxide thermal spray coating, characterized in that a spray unit is arranged at a distance of 50 mm to 130 mm from a substrate, Y2O3 thermal spray powder is subjected to atmospheric plasma spraying to form a yttrium oxide thermal spray coating on the substrate, and water is supplied together with the Y2O3 thermal spray powder at a speed of 50 to 400 ml / m.

[0027] In a preferred embodiment of the present invention, the atmospheric plasma thermal spraying can configure the spraying unit at a distance of 80 mm to 120 mm from the substrate.

[0028] In a preferred embodiment of the present invention, water may be supplied together with the Y2O3 thermal spray powder at a rate of 200 ml / m to 350 ml / m.

[0029] In a preferred embodiment of the present invention, the water is supplied at a position where the distance between the plasma forming nozzle and the substrate is 2:8 to 8:2.

[0030] In a preferred embodiment of the present invention, the water is supplied at a position between the plasma forming nozzle and the substrate at a distance of 3:7 to 5:5.

[0031] In a preferred embodiment of the present invention, the position where the water is supplied may be 25 mm to 50 mm away from the plasma forming nozzle.

[0032] In a preferred embodiment of the present invention, four water supply nozzles for supplying the water may be arranged at intervals of 90° from each other so as to supply water from four directions.

[0033] In a preferred embodiment of the present invention, eight water supply nozzles for supplying the water may be arranged at intervals of 45° from each other so as to supply water from eight directions.

[0034] In a preferred embodiment of the present invention, the orifice of the nozzle for supplying the water is circular, and the size of the orifice may be 0.007 inches (in) to 0.011 inches.

[0035] In a preferred embodiment of the present invention, the average particle size of the Y2O3 thermal spraying powder may be 5 μm to 60 μm.

[0036] In a preferred embodiment of the present invention, the thickness of the yttrium oxide thermal spray film may be 100 μm to 300 μm.

[0037] In another preferred embodiment of the present invention, the present invention provides an yttrium oxide thermal spraying film formed by the method for manufacturing the yttrium oxide thermal spraying film.

[0038] In a preferred embodiment of the present invention, the colorimeter measurement value L of the yttrium oxide thermal spraying film may be greater than 85.

[0039] In a preferred embodiment of the present invention, the porosity of the yttrium oxide thermal spray coating may be less than 2.6%.

[0040] In a preferred embodiment of the present invention, the porosity of the yttrium oxide thermal spray film may be less than 1.0%.

[0041] Effects of the Invention

[0042] The yttrium oxide thermal spray film manufactured according to the present invention forms a high-density and whitened thermal spray coating with a density of less than 1.5%, thereby reducing the etching rate of the process gas in the dry etching process, thereby having excellent durability when used as a coating material for components in a semiconductor chamber, and suppressing the detachment of the coating caused by the etching phenomenon, thereby contributing to improving the yield of semiconductor wafers.

[0043] Furthermore, the method for producing the yttria thermal spray coating according to the present invention provides a reasonable process time by whitening the surface of the coating layer during the production process, and can provide a high-quality thermal spray coating without adding additional costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 This is a schematic diagram of supplying water (distilled water) in the method for producing an yttria thermal spray coating according to the present invention.

[0045] Figure 2 These are scanning electron microscope (SEM) photographs of the thermal spray coating surfaces of (a) Comparative Example 1, (b) Comparative Example 2, (c) Example 1, and (d) Example 2 according to the present invention.

[0046] Figure 3 These are low-magnification SEM photographs of the side surfaces of the thermal sprayed films of (a) Comparative Example 1, (b) Comparative Example 2, (c) Example 1, and (d) Example 2 according to the present invention.

[0047] Figure 4 These are high-magnification SEM photographs of the side surfaces of the thermal sprayed films of (a) Comparative Example 1, (b) Comparative Example 2, (c) Example 1, and (d) Example 2 according to the present invention.

[0048] Figure 5 Displays the meaning of the axis values ​​of the colorimeter.

[0049] Figure 6 These are the results of X-ray diffraction (XRD) analysis of yttrium oxide, SPS coating film, comparative example 1, and thermal spray coating of Example 2.

[0050] Figure 7 These are SEM photographs of the thermal spray coating surfaces according to Comparative Example 1 and Example 2. DETAILED DESCRIPTION

[0051] Unless otherwise defined, all technical and scientific terms used in this specification have the same meaning as those commonly understood by those of ordinary skill in the art to which the present invention belongs. Generally speaking, the nomenclature used in this specification is well known and commonly used in the art.

[0052] Throughout the specification of the present application, when it is mentioned that a certain part “includes” a certain constituent element, unless there is a particular description to the contrary, it means that other constituent elements are not excluded and other constituent elements may be included.

[0053] In the semiconductor manufacturing process, gate etching devices, insulating film etching devices, resistive film etching devices, sputtering devices, CVD devices, etc. are used. At the same time, in the liquid crystal manufacturing process, etching devices for forming thin film transistors are used. In addition, in these manufacturing devices, a configuration including a plasma generating mechanism is adopted for the purpose of high integration through micro-processing.

[0054] In these manufacturing processes, as processing gases, halogen-based corrosive gases such as fluorine-based and chlorine-based gases are used in the above-mentioned devices due to their high reactivity. As fluorine-based gases, SF6, CF4, CHF3, ClF3, HF, NF3, etc. can be included, and as chlorine-based gases, Cl2, BCl3, HCl, CCl4, SiCl4, etc. can be included. When microwaves or high frequencies are connected to the atmosphere into which these gases are introduced, these gases will be plasmatized. The device components exposed to these halogen-based gases or their plasma are required to have little metal other than the material components on their surfaces and have high corrosion resistance.

[0055] Therefore, the present invention aims to provide a method for producing a thermal spray coating having excellent plasma resistance for covering a member for a plasma etching apparatus.

[0056] The method for manufacturing a yttrium oxide thermal spray coating according to the present invention is characterized in that a spray unit is arranged at a distance of 50 mm to 200 mm relative to a substrate, an yttrium oxide thermal spray coating is formed on the substrate by atmospheric plasma spraying of Y2O3 thermal spray powder, and water is supplied together with the Y2O3 thermal spray powder at a speed of 50 ml / m to 400 ml / m.

[0057] In the atmospheric plasma spraying method for producing the thermal spray coating of the present invention, there is a method of coating by shortening the spacing distance between the base material (the object to be coated) and the plasma unit so as to form a high-density coating.

[0058] However, due to the short spacing, the movement distance of the molten thermal spray powder becomes short, resulting in deoxidation, causing the surface of the thermal spray film to turn black. The film color, which is different from the past, makes it difficult to distinguish from contaminants after use in the semiconductor process, making it difficult to predict the arrival of the cleaning and recoating cycle. In addition, the color change of the thermal spray film will change the emissivity, resulting in the need to change the semiconductor process conditions.

[0059] Therefore, according to the manufacturing method of the yttrium oxide thermal spray coating of the present invention, the spray unit is arranged at a close distance (50mm to 130mm) relative to the substrate, and at the same time, in order to prevent the deoxidation of the yttrium oxide component, water (distilled water) is supplied together with the Y2O3 thermal spray powder at a rate of 50ml / m to 400ml / m, thereby forming a low porosity and dense yttrium oxide thermal spray coating.

[0060] In the atmospheric plasma thermal spray coating, a spray gun melts a coating material using a plasma flame and thermally sprays the melted coating material onto a substrate. For example, the plasma flame may be formed by dissociating a portion of a plasma gas including argon (Ar), nitrogen (N2), hydrogen (H2), helium (He), etc.

[0061] In the atmospheric plasma thermal spray coating, as thermal spray process variables, preferably, the flow rate of the inert gas is 320 SCFH to 420 SCFH, the flow rate of the nitrogen gas is 120 SCFH to 160 SCFH, and the flow rate of the hydrogen gas is 120 SCFH to 160 SCFH.

[0062] Furthermore, in the atmospheric plasma thermal spray coating, preferably, the plasma generation current is 360A to 460A, and more preferably, may be 380A to 440A.

[0063] In the atmospheric plasma thermal spray coating, preferably, the spray unit is arranged at a distance of 50 mm to 130 mm relative to the substrate, and more preferably, it can be arranged at a distance of 80 mm to 120 mm relative to the substrate.

[0064] If the distance between the spray unit and the surface of the substrate is less than about 50 mm, the base material is deformed due to the close distance between the substrate and the plasma, and there is a risk of peeling of the coating layer due to the high thermal energy. If it is farther than 130 mm, as the flight distance of the yttrium oxide powder increases, the granular powder that melts when it reaches the substrate solidifies and the kinetic energy decreases, forming pores in the film, thereby forming a low-density film.

[0065] Among them, in order to prevent the deoxidation phenomenon of the yttrium oxide component, water can be supplied together with the Y2O3 thermal spray powder to form a white yttrium oxide thermal spray film.

[0066] At this time, water (distilled water) may be supplied together with the Y2O3 thermal spray powder at a rate of 50 to 400 ml / m, preferably, water (distilled water) may be supplied together with the Y2O3 thermal spray powder at a rate of 200 to 350 ml / m.

[0067] In addition, as an example, the water supply position may be between a distance of 2:8 to 8:2 between the plasma forming nozzle and the substrate. Preferably, the water supply position may be between a distance of 3:7 to 5:5 between the plasma forming nozzle and the substrate.

[0068] As an embodiment, when the distance between the plasma forming nozzle and the substrate surface is 100 mm, the water supply position may be 20 mm to 80 mm away from the plasma forming nozzle. Preferably, the water supply position may be 30 mm to 50 mm away from the plasma forming nozzle.

[0069] As an embodiment, when the distance between the plasma forming nozzle and the substrate surface is 50 mm, the water supply position may be 10 mm to 40 mm away from the plasma forming nozzle. Preferably, the water supply position may be 15 mm to 25 mm away from the plasma forming nozzle.

[0070] In addition, as an embodiment, the water supply position may be 25 mm to 50 mm away from the plasma forming nozzle. Preferably, the water supply position may be 35 mm to 45 mm away from the plasma forming nozzle.

[0071] In addition, the plurality of water supply nozzles for supplying water may be arranged irregularly or regularly. For example, four water supply nozzles may be arranged at 90° intervals from each other so as to supply water from four directions. Preferably, as follows Figure 1 As shown, the eight water supply nozzles for supplying water are arranged at 45° intervals from each other so as to supply water from eight directions, thereby uniformly supplying water (distilled water) to the Y2O3 thermal spray powder, thereby effectively preventing the deoxidation of yttrium oxide.

[0072] In addition, as an example, the orifice used for the water supply nozzle may be of any shape, but preferably a circular orifice is used, and the size of the orifice is not limited, but preferably 0.007 inches to 0.011 inches (in).

[0073] In the atmospheric plasma thermal spray coating method, the yttrium oxide thermal spray coating is preferably formed to have a thickness of 50 μm to 500 μm, and more preferably, formed to have a thickness of 100 μm to 300 μm.

[0074] At this time, the average particle size of the Y2O3 thermal spraying powder is preferably 5 μm to 60 μm, preferably 10 μm to 40 μm, and more preferably 15 μm to 30 μm.

[0075] If the size of the Y2O3 thermal spray powder is less than 5 μm, the fluidity of the powder is low during thermal spray coating and a uniform film cannot be achieved. The powder is oxidized before being transferred to the frame or cannot be transferred to the center of the frame, making it difficult to meet the droplet flight speed and heat required to form a dense film, and a film with high pores or low hardness is formed. If the average diameter of the Y2O3 thermal spray powder exceeds 60 μm, the melting specific surface area of ​​the particle powder is reduced and it cannot be completely melted, resulting in the formation of an unmelted portion in the coating film, making it difficult to meet the quality of the thermal spray film required by the present invention.

[0076] In addition, in the present invention, there is no particular limitation on the substrate coated with the thermal spray film. For example, as long as the material contained in the substrate is a material provided to the thermal spraying material for these thermal spraying materials so that it can have the required resistance, its material or shape is not particularly limited. As the material constituting the substrate for these thermal sprayings, it is preferably selected from a combination of one or more of aluminum, nickel, chromium, zinc and alloys thereof, aluminum oxide, aluminum nitride, silicon nitride, silicon carbide and quartz glass, which constitute components for semiconductor manufacturing equipment, etc.

[0077] Such a substrate may be, for example, a member constituting a semiconductor device manufacturing apparatus, or may be a member exposed to highly reactive oxygen gas plasma or halogen-based gas plasma.

[0078] Before plasma thermal spraying, the substrate surface is preferably treated according to the ceramic thermal spraying operation standard specified in JIS H9302. For example, after removing rust or grease from the substrate surface, grinding particles such as Al2O3 and SiC are sprayed to roughen it, and pre-treated to make it easy for thermal spraying particles to adhere.

[0079] Conventional yttrium oxide thermal spraying films form high porosity in the coating layer. In contrast, in the present invention, the spraying unit is arranged at a distance of 50 mm to 130 mm relative to the substrate, and a high-density yttrium oxide thermal spraying film is formed on the substrate by atmospheric plasma spraying of Y2O3 thermal spraying powder. In addition, water is supplied together with the Y2O3 thermal spraying powder at a rate of 50 ml / m to 400 ml / m from 25 mm to 50 mm away from the plasma forming nozzle, thereby suppressing the deoxidation of yttrium oxide in a short distance to produce a whitened and high-density yttrium oxide thermal spraying film.

[0080] Therefore, the yttria thermal spray film produced by the method has an excellent porosity level compared to conventional thermal spray films, and can be applied to semiconductor chambers used in existing etching processes, exhibiting excellent durability and suppressing the phenomenon of coating detachment due to etching gas.

[0081] As an example, the colorimeter measurement value L of the yttrium oxide thermal sprayed coating formed by the method for manufacturing the yttrium oxide thermal sprayed coating may be greater than 85.

[0082] Furthermore, as an example, the porosity of the yttria thermal sprayed coating formed by the method for manufacturing the yttria thermal sprayed coating may be less than 2.6%, preferably less than 1.5%, and more preferably less than 1%.

[0083] Hereinafter, the present invention will be described in more detail by way of examples. However, the following examples are merely examples of the present invention, and the present invention is not limited to the following examples.

[0084] Comparative Examples 1-2 and Examples 1-2

[0085] Using the Y2O3 thermal spray material and plasma gun, argon, nitrogen and hydrogen are flowed as heat source gases, and plasma is generated at a power of 80kW to 120kW while the thermal spray gun is moved. The generated plasma is used to melt the raw material powder to form a coating film on the base material. The coating film is formed to have a thickness of 150μm to 250μm, and the experimental conditions are shown in Table 1 below. In addition, Figure 2 The CCD photograph of the thermal sprayed film surface is shown. Figure 3 and Figure 4 A scanning electron microscope photograph of the side surface of the produced thermal sprayed film is shown.

[0086] Table 1

[0087] Serial number Is water supplied? Separation distance Porosity (%) Hardness(Hv) L a b Comparative Example 1 × 160 4.32 450 91.17 -0.22 0.18 Comparative Example 2 × 100 2.33 525 41.89 -0.43 -0.62 Example 1 O 160 2.54 512 91.57 -0.33 0.17 Example 2 O 100 0.85 535 91.18 -0.32 0.19

[0088] Experimental Example 1: Observation of thermal spray coating

[0089] Down Figure 3 and Figure 4 The scanning electron microscope (SEM) photographs of the surface and side of the thermal spray coatings of Comparative Examples 1 to 2 and Examples 1 to 2 of the present invention are shown in FIG. Figure 3 and Figure 4 The scanning electron microscope (SEM) photograph of the side of the thermal sprayed film confirmed that a dense thin film with low porosity was formed in the thermal sprayed film according to Example 2.

[0090] In addition, the porosity was measured as follows. That is, the thermal spray coating was cut into a plane perpendicular to the substrate surface, the obtained cross section was resin embedded and polished, and an electron microscope (JEOL, JS-6010) was used to take a cross-sectional image ( Figure 3 and Figure 4The image was analyzed using image analysis software (MEDIA CYBERNETICS, Image Pro), and the area of ​​the pores in the specific cross-sectional image was calculated to determine the ratio of the area of ​​the pores to the overall cross-sectional area. The porosity obtained by the area of ​​the pores appearing in the cross-sectional area of ​​the thermal spray coating is shown in Table 1.

[0091] Examples 1 and 2 showed a porosity value of less than 2.6%, indicating that the density of the yttrium oxide thermal sprayed film according to the present invention was increased compared to the conventional thermal sprayed film. In addition, the colorimeter L value was 85 or more, confirming that a whitened yttrium oxide thermal sprayed film was formed.

[0092] Experimental Example 2: Crystal structure analysis

[0093] as follows Figure 6 As shown, the results of x-ray diffraction (XRD) analysis of the thermal sprayed film according to Example 2 using a scanning electron microscope (SEM) confirmed that the existence ratio of the cubic structure was higher than that of the monoclinic structure compared to the well-known suspension plasma spraying method (SPS) with high-density coating.

[0094] Experimental Example 3: Hardness Measurement

[0095] The "Hardness" column in Table 1 shows the Vickers hardness measurement results of each thermal spray coating. The Vickers hardness is measured using a micro hardness tester and is the Vickers hardness (Hv0.2) obtained when a 294.2 mN test force is applied by a diamond indenter with an angle of 136° between the opposing surfaces.

[0096] As shown in Table 1 above, it was confirmed that the thermal sprayed films of Examples 1 and 2 showed hardness in a similar range to that of the thermal sprayed films of Comparative Examples 1 and 2.

[0097] Experimental Example 4: Roughness Measurement

[0098] The surface roughness (μm) of the coating films prepared in Example 2 of the present invention and Comparative Example 1 was measured using a roughness meter (SJ-201). The results are as follows: Figure 7 shown.

[0099] as follows Figure 7 As shown, it was confirmed that when a thermal spray coating was formed using a powder of 10 μm to 60 μm, the thermal spray coating according to Comparative Example 1 showed a surface roughness of 3 μm to 6 μm, whereas the thermal spray coating according to Example 2 showed a surface roughness of 1 μm to 4 μm. This confirmed that the roughness can be reduced by using water.

[0100] Experimental Example 5: Measuring the thermal sprayed surface using a colorimeter

[0101] Down Figure 2 These are CCD photographs of the thermal spray coating surfaces of Comparative Examples 1 and 2 and Examples 1 and 2 according to the present invention. It was confirmed that among Comparative Example 2 and Example 2 having the same separation distance, Example 2 using water showed white color.

[0102] In the above Table 1, the columns L, a, and b show the colorimeter measurement results of the thermal spray coating surface. Among them, the L value represents brightness, and the larger the value, the brighter it is. This confirms that in Comparative Example 2 and Example 2 at the same spacing distance, Example 2 using water shows a larger value, and therefore shows white.

[0103] The above describes in detail certain parts of the present invention. It is clear to those skilled in the art that these specific techniques are only preferred embodiments and are not intended to limit the scope of the present invention. Therefore, the essential scope of the present invention should be defined by the appended claims and their equivalents.

Claims

1. A method for manufacturing a yttrium oxide thermal spray coating, characterized in that: Place the spray unit 50mm to 130mm away from the substrate. Y2O3 thermal spray powder is sprayed by atmospheric plasma to form a yttrium oxide thermal spray film on the substrate. Water is supplied together with the Y2O3 thermal spray powder at a rate of 50 ml / m to 400 ml / m.

2. The method for manufacturing a yttrium oxide thermal spray coating according to claim 1, characterized in that: In the atmospheric plasma spraying, the spraying unit is arranged at a distance of 80 mm to 120 mm from the substrate.

3. The method for manufacturing a yttrium oxide thermal spray coating according to claim 1, characterized in that: Water was supplied together with the Y2O3 thermal spray powder at a rate of 200 to 350 ml / m.

4. The method for manufacturing a yttrium oxide thermal spray coating according to claim 1, characterized in that: The water is supplied at a position where the distance between the plasma forming nozzle and the substrate is 2:8 to 8:

2.

5. The method for manufacturing a yttrium oxide thermal spray coating according to claim 4, characterized in that: The water is supplied at a position between the plasma forming nozzle and the substrate at a distance of 3:7 to 5:

5.

6. The method for manufacturing a yttrium oxide thermal spray coating according to claim 1, characterized in that: The water is supplied at a position 25 mm to 50 mm away from the plasma forming nozzle.

7. The method for manufacturing a yttrium oxide thermal spray coating according to claim 1, characterized in that: Four water supply nozzles for supplying the water are arranged at intervals of 90° from each other so as to supply water from four directions.

8. The method for manufacturing a yttria thermal spray coating according to claim 1, characterized in that: Eight water supply nozzles for supplying the water are arranged at intervals of 45° from each other so as to supply water from eight directions.

9. The method for manufacturing a yttria thermal spray coating according to claim 1, characterized in that: The orifice of the nozzle for supplying said water is circular, The orifice size is 0.007 inches to 0.011 inches.

10. The method for manufacturing a yttria thermal spray coating according to claim 1, characterized in that: The average particle size of the Y2O3 thermal spraying powder is 5 μm to 60 μm.

11. The method for manufacturing a yttrium oxide thermal spray coating according to claim 1, characterized in that: The thickness of the yttrium oxide thermal spraying film is 100 μm to 300 μm.

12. A yttrium oxide thermal spray coating, characterized in that: The yttrium oxide thermal spray coating is formed by the method for producing the yttrium oxide thermal spray coating according to any one of claims 1 to 11.

13. The yttrium oxide thermal spray coating according to claim 12, characterized in that: The colorimeter measurement value L of the yttrium oxide thermal spraying film is 85 or more.

14. The yttrium oxide thermal spray coating according to claim 12, characterized in that: The porosity of the yttrium oxide thermal spraying film is less than 2.6%.

15. The yttrium oxide thermal spray coating according to claim 12, characterized in that: The porosity of the yttria thermal spraying film is less than 1.0%.

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