Preparation method of yttrium oxide coating with low roughness

Abstract

The invention discloses a preparation method of a low-roughness yttrium oxide coating, which comprises the following steps: performing meltallizing on a Y2O3 material on a base material by adopting a plasma spraying technology to form a yttrium oxide meltallizing coating; the surface of the yttrium oxide meltallizing coating is coated with a liquid inorganic nanometer yttrium oxide crystal material for the first time, standing is conducted, and then drying is conducted for 6-10 h in the environment at the temperature of 80-100 DEG C; and carrying out polishing treatment on the yttrium oxide meltallizing coating coated with the inorganic nano yttrium oxide crystal material. According to the method, the surface roughness of the yttrium oxide coating can be effectively improved.

Description

Technical Field

[0001] The present application belongs to the field of plasma spraying technology, and in particular relates to a method for preparing a low-roughness yttrium oxide coating. Background Art

[0002] Plasma spraying technology is a coating preparation method that heats powder particles through a high-temperature flame and sprays the powder particles onto the surface of the substrate. This method can not only effectively solidify and melt high-temperature materials, but also avoid the burning of conventional materials. Therefore, it also has the characteristics of high spraying efficiency and adhesion of different materials.

[0003] In the wafer manufacturing etching process, the reacted derivatives will adhere to the surface of the yttrium oxide (Y2O3) coating. Due to the rough surface of the yttrium oxide coating, the attachments will accumulate and agglomerate. When the agglomeration reaches a certain level, the attachments will peel off, causing wafer defects. Therefore, in order to reduce the aggregation of attachments on the yttrium oxide coating in the wafer manufacturing etching process, it is necessary to reduce the roughness of the yttrium oxide coating.

[0004] At present, the thickness and uniformity of the coating are usually adjusted by changing the process parameters (such as powder feeding rate, powder particle size, voltage, etc.) to change the roughness and density of the coating. However, due to the high melting point of yttrium oxide powder, the yttrium oxide coating prepared by the existing plasma spraying process contains a large number of unmelted yttrium oxide particles, resulting in the generation of voids and poor coating density, which in turn causes the surface roughness of the yttrium oxide coating after polishing (generally Ra 1.0μm) to fail to reach the surface roughness in a smooth state (i.e., less than Ra 0.03μm).

[0005] Therefore, how to reduce the surface roughness of yttrium oxide coating is a problem that needs to be solved urgently. Summary of the invention

[0006] In order to solve the above technical problems, the present application provides a method for preparing a low-roughness yttrium oxide coating to reduce the surface roughness of the yttrium oxide coating.

[0007] The above application objectives of this application are achieved through the following technical solutions:

[0008] A method for preparing a low-roughness yttrium oxide coating comprises the following steps:

[0009] S1, plasma spraying technology is used to spray Y2O3 material on the substrate to form a yttrium oxide spray coating;

[0010] S2, brushing the surface of the yttrium oxide spray coating with a liquid inorganic nano yttrium oxide crystal material, leaving it to stand, and then drying it in an environment of 80° C. to 100° C. for 6 h to 10 h;

[0011] S3, polishing the yttrium oxide spray coating coated with the inorganic nano-yttrium oxide crystal material.

[0012] Preferably, the following steps are also included between step S2 and step S3:

[0013] S2', using liquid inorganic nano yttrium oxide crystal material to brush the surface of the yttrium oxide spray coating for a second time, and then letting it stand, and then drying it in an environment of 80° C. to 100° C. for 6 h to 10 h.

[0014] Preferably, the standing time in step S2 and step S3 is 1 hour.

[0015] Preferably, in step S2 and step S3, the ambient temperature is 90° C. and the drying time is 8 hours.

[0016] Preferably, in step S2 and step S3, the ambient temperature is 100° C. and the drying time is 6 hours.

[0017] Preferably, in step S1, the thickness of the yttrium oxide spray coating is 180 μm to 220 μm, and the surface roughness Ra of the yttrium oxide spray coating is 5 μm to 7 μm.

[0018] Preferably, before step S1, the method further comprises:

[0019] S0, performing sandblasting on the substrate to make the surface of the substrate reach a uniform roughness, and the surface roughness Ra of the substrate is 3 μm to 4 μm.

[0020] Preferably, step S3 comprises:

[0021] The yttrium oxide spray coating coated with inorganic nano-yttrium oxide crystal material was polished three times using diamond suspension grinding and polishing liquids with different particle sizes. The particle sizes of the diamond suspension grinding and polishing liquids for the three polishing treatments were 2.5 μm, 1.0 μm, and 0.5 μm, respectively.

[0022] Preferably, the polishing conditions for the three polishing treatments are:

[0023] The single-point pressure was 20N, the grinding time was 300s, the grinding disc speed was 300r / min, and the head speed was 50r / min.

[0024] Preferably, the substrate is stainless steel, aluminum or titanium.

[0025] The above technical solution of the present application has the following advantages compared with the prior art:

[0026] The present application uses an inorganic nano-yttrium oxide crystal material to infiltrate the yttrium oxide spray coating, and then densifies the coating through heat treatment, thereby effectively filling the gaps caused by the unmelted yttrium oxide particles contained in the yttrium oxide coating prepared by the plasma spraying process, improving the density of the coating, and forming a low-roughness coating on the surface of the polished substrate. In this way, the coating surface is smoother, thereby reducing the adhesion ability of derivatives generated during the etching process, so that they can be better extracted out of the cavity through a vacuum pump, thereby effectively avoiding wafer defects caused by the peeling of attachments after the accumulation and agglomeration of attachments during the wafer manufacturing etching process. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0028] Figure 1 Schematic diagram of a process for preparing a low-roughness yttrium oxide coating in an embodiment of the present application. DETAILED DESCRIPTION

[0029] In order to enable those skilled in the art to better understand the technical solutions in this application, the technical solutions in the embodiments of this application will be clearly and completely described below. Obviously, the described embodiments are only part of the embodiments of this application, not all of them. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0030] In the embodiments provided in the present application, it should be understood that the disclosed methods and systems can be implemented in other ways. The system embodiments described below are merely schematic. For example, the division of units and modules is only a logical function division. There may be other division methods in actual implementation, such as: multiple units or modules can be combined, or can be integrated into another system, or some features can be ignored, or not executed. In addition, the coupling, direct coupling, or communication connection between the components shown or discussed can be through some interfaces, indirect coupling or communication connection of devices or modules, which can be electrical, mechanical or other forms.

[0031] In addition, all functional units in the embodiments of the present application may be integrated into one processor, or each unit may be a separate device, or two or more units may be integrated into one device; each functional unit in the embodiments of the present application may be implemented in the form of hardware or in the form of hardware plus software functional units.

[0032] A person skilled in the art can understand that all or part of the steps of the following method embodiments can be completed by program instructions and related hardware. The aforementioned program instructions can be stored in a computer-readable storage medium. When the program instructions are executed, the steps of the following method embodiments are executed; and the aforementioned storage medium includes: a mobile storage device, a read-only memory (ROM), a magnetic disk or an optical disk, and other media that can store program codes.

[0033] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of this application, "multiple" and "several" mean two or more, unless otherwise clearly and specifically defined.

[0034] like Figure 1 As shown, the present application embodiment provides a method for preparing a low-roughness yttrium oxide coating, which may include the following steps:

[0035] S1, plasma spraying technology is used to spray Y2O3 material on the substrate to form a yttrium oxide spray coating;

[0036] S2, using liquid inorganic nano yttrium oxide crystal material to brush the surface of the yttrium oxide spray coating once, and then let it stand, and then dry it in an environment of 80° C. to 100° C. for 6 h to 10 h;

[0037] S3, polishing the yttrium oxide spray coating coated with the inorganic nano-yttrium oxide crystal material.

[0038] The preparation method of the low-roughness yttrium oxide coating of this embodiment is as follows: first, a plasma spraying technology is used to spray Y2O3 material on a substrate to form an yttrium oxide spray coating, and then a liquid inorganic nano yttrium oxide crystal material is used to brush the surface of the yttrium oxide spray coating, and the surface is allowed to stand, and then the surface is dried in an environment of 80°C to 100°C for 6h to 10h, and finally the yttrium oxide spray coating coated with the inorganic nano yttrium oxide crystal material is polished. In the method, the yttrium oxide spray coating is infiltrated with an inorganic nano-yttrium oxide crystal material, and then the coating is densified by heat treatment, thereby effectively filling the gaps caused by the unmelted yttrium oxide particles contained in the yttrium oxide coating prepared by the plasma spraying process, improving the density of the coating, and forming a low-roughness coating on the surface of the polished substrate. In this way, the coating surface is smoother, thereby reducing the adhesion ability of derivatives generated during the etching process, so that they can be better extracted out of the cavity by a vacuum pump, thereby effectively avoiding wafer defects caused by the peeling of the attachments after the accumulation and agglomeration of the attachments during the wafer manufacturing etching process.

[0039] In one embodiment, the following steps are further included between step S2 and step S3:

[0040] S2', the surface of the yttrium oxide spray coating is brushed twice with a liquid inorganic nano yttrium oxide crystal material, and the coating is left to stand, and then dried in an environment of 80°C to 100°C for 6h to 10h. The surface of the yttrium oxide spray coating is brushed once, and the surface of the yttrium oxide spray coating is brushed twice and dried, so that the surface of the yttrium oxide spray coating can be more evenly and comprehensively coated with the inorganic nano yttrium oxide crystal material, further improving the penetration effect of the inorganic nano yttrium oxide crystal material on the yttrium oxide spray coating, improving the compactness of the coating, and then improving the smoothness of the polished coating, that is, further reducing the surface roughness of the coating.

[0041] In one embodiment, the standing time in step S2 and step S3 is 1 hour.

[0042] In one embodiment, in step S2 and step S3, the ambient temperature is 90° C. and the drying time is 8 hours.

[0043] In one embodiment, in step S2 and step S3, the ambient temperature is 100° C. and the drying time is 6 hours.

[0044] In one embodiment, in step S1, the thickness of the yttrium oxide spray coating is 180 μm to 220 μm, and the surface roughness Ra of the yttrium oxide spray coating is 5 μm to 7 μm.

[0045] In one embodiment, before step S1, the method further comprises:

[0046] S0, sandblast the substrate to make the surface of the substrate reach a uniform roughness, and the surface roughness Ra of the substrate is 3μm to 4μm. Before using plasma spraying technology to spray Y2O3 material on the substrate, the substrate is sandblasted first to increase the adhesion of the coating on the substrate and extend the durability of the coating.

[0047] In one embodiment, step S3 includes:

[0048] The yttrium oxide spray coating coated with inorganic nano-yttrium oxide crystal material was polished three times using diamond suspension grinding and polishing liquids with different particle sizes. The particle sizes of the diamond suspension grinding and polishing liquids for the three polishing treatments were 2.5μm, 1.0μm, and 0.5μm, respectively. By polishing the yttrium oxide spray coating coated with inorganic nano-yttrium oxide crystal material multiple times, and the particle sizes of the diamond suspension grinding and polishing liquids for multiple polishings are reduced successively, the polishing effect is effectively improved and the surface roughness of the coating after polishing is reduced.

[0049] In one embodiment, the polishing conditions of the three polishing processes are:

[0050] The single-point pressure was 20N, the grinding time was 300s, the grinding disc speed was 300r / min, and the head speed was 50r / min.

[0051] In one embodiment, the substrate is stainless steel, aluminum, or titanium.

[0052] In order to better understand the advantages of the method for preparing the low-roughness yttrium oxide coating of the embodiment of the present application, the technical effects thereof are demonstrated and described with a group of comparative examples below (in the comparative examples, the substrate is aluminum):

[0053] Embodiment 1:

[0054] The specific process is as follows:

[0055] 1. Sandblast the substrate to achieve uniform surface roughness. The surface roughness Ra of the substrate after sandblasting is between 3μm and 4μm;

[0056] 2. Spray powdered Y2O3 material on the surface of the substrate after sandblasting to form an yttrium oxide spray coating, the thickness of the spray layer is t=180μm-220μm, and the surface roughness Ra of the yttrium oxide spray coating after spraying is between 5μm and 7μm;

[0057] 3. The surface of the substrate with the yttrium oxide sprayed coating was polished three times at room temperature. The polishing conditions for each time were: single-point pressure 20N, grinding time 300s, grinding disc speed 300r / min, head speed 50r / min, and the polishing liquid was diamond suspension grinding and polishing liquid. The particle sizes of the diamond suspension grinding and polishing liquid for the three polishing treatments were 2.5μm, 1.0μm, and 0.5μm, respectively.

[0058] After treatment, the surface roughness of the yttrium oxide coating was measured.

[0059] Embodiment 2:

[0060] The specific process is as follows:

[0061] 1. Sandblast the substrate to achieve uniform surface roughness. The surface roughness Ra of the substrate after sandblasting is between 3μm and 4μm;

[0062] 2. Spray powdered Y2O3 material on the surface of the substrate after sandblasting to form an yttrium oxide spray coating, the thickness of the spray layer is t=180μm-220μm, and the surface roughness Ra of the yttrium oxide spray coating after spraying is between 5μm and 7μm;

[0063] 3. Use liquid inorganic nano yttrium oxide crystal material to brush the surface of yttrium oxide spray coating once, let it stand for 1 hour, and then dry it in an environment of 90°C for 8 hours;

[0064] 4. Use liquid inorganic nano yttrium oxide crystal material to brush the surface of yttrium oxide spray coating for the second time, let it stand for 1 hour, and then dry it in an environment of 90°C for 8 hours;

[0065] 5. The surface of the substrate with the yttrium oxide sprayed coating was polished three times at room temperature. The polishing conditions for each time were: single-point pressure 20N, grinding time 300s, grinding disc speed 300r / min, head speed 50r / min, and the polishing liquid was diamond suspension grinding and polishing liquid. The particle sizes of the diamond suspension grinding and polishing liquid for the three polishing treatments were 2.5μm, 1.0μm, and 0.5μm, respectively.

[0066] After treatment, the surface roughness of the yttrium oxide coating was measured.

[0067] Embodiment 3:

[0068] The specific process is as follows:

[0069] 1. Sandblast the substrate to achieve uniform surface roughness. The surface roughness Ra of the substrate after sandblasting is between 3μm and 4μm;

[0070] 2. Spray powdered Y2O3 material on the surface of the substrate after sandblasting to form an yttrium oxide spray coating, the thickness of the spray layer is t=180μm-220μm, and the surface roughness Ra of the yttrium oxide spray coating after spraying is between 5μm and 7μm;

[0071] 3. Use liquid inorganic nano yttrium oxide crystal material to brush the surface of yttrium oxide spray coating once, let it stand for 1 hour, and then dry it in an environment of 80°C for 10 hours;

[0072] 4. Use liquid inorganic nano yttrium oxide crystal material to brush the surface of yttrium oxide spray coating for the second time, let it stand for 1 hour, and then dry it in an environment of 80°C for 10 hours;

[0073] 5. The surface of the substrate with the yttrium oxide sprayed coating was polished three times at room temperature. The polishing conditions for each time were: single-point pressure 20N, grinding time 300s, grinding disc speed 300r / min, head speed 50r / min, and the polishing liquid was diamond suspension grinding and polishing liquid. The particle sizes of the diamond suspension grinding and polishing liquid for the three polishing treatments were 2.5μm, 1.0μm, and 0.5μm, respectively.

[0074] After treatment, the surface roughness of the yttrium oxide coating was measured.

[0075] Embodiment 4:

[0076] The specific process is as follows:

[0077] 1. Sandblast the substrate to achieve uniform surface roughness. The surface roughness Ra of the substrate after sandblasting is between 3μm and 4μm;

[0078] 2. Spray powdered Y2O3 material on the surface of the substrate after sandblasting to form an yttrium oxide spray coating, the thickness of the spray layer is t=180μm-220μm, and the surface roughness Ra of the yttrium oxide spray coating after spraying is between 5μm and 7μm;

[0079] 3. Use liquid inorganic nano yttrium oxide crystal material to brush the surface of yttrium oxide spray coating once, let it stand for 1 hour, and then dry it in an environment of 100°C for 6 hours;

[0080] 4. Use liquid inorganic nano yttrium oxide crystal material to brush the surface of yttrium oxide spray coating for the second time, let it stand for 1 hour, and then dry it in an environment of 100°C for 6 hours;

[0081] 5. The surface of the substrate with the yttrium oxide sprayed coating was polished three times at room temperature. The polishing conditions for each time were: single-point pressure 20N, grinding time 300s, grinding disc speed 300r / min, head speed 50r / min, and the polishing liquid was diamond suspension grinding and polishing liquid. The particle sizes of the diamond suspension grinding and polishing liquid for the three polishing treatments were 2.5μm, 1.0μm, and 0.5μm, respectively.

[0082] After treatment, the surface roughness of the yttrium oxide coating was measured.

[0083] It should be noted that, in order to ensure the accuracy of the experimental results, the above embodiments were tested 5 times according to the corresponding process flow, and the surface roughness Ra of the yttrium oxide spray coating was measured as shown in the following table;

[0084] The experimental results comparison table of the above four embodiments is as follows

[0085]

[0086]

[0087] In the above four embodiments, embodiment 1 is a comparative example, that is, the surface of the yttrium oxide spray coating is not coated with liquid inorganic nano yttrium oxide crystal material;

[0088] In Examples 2 to 4, liquid inorganic nano-yttrium oxide crystal material is used to coat the surface of the yttrium oxide spray coating, but the drying temperature and drying time after coating are different.

[0089] By comparing the measurement results of the above four embodiments, it can be seen that, relative to Example 1, after Examples 2 to 4 use liquid inorganic nano yttrium oxide crystal material to coat the surface of the yttrium oxide sprayed coating, the surface roughness Ra of the polished yttrium oxide sprayed coating is significantly reduced, and under the experimental conditions in Example 3, the surface roughness Ra of the polished yttrium oxide sprayed coating can be reduced to below 0.03 μm, achieving the target smooth state, indicating that the present application can effectively reduce the surface roughness of the yttrium oxide coating.

[0090] In this specification, each embodiment is described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the embodiments can be referred to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant parts can be referred to the method part.

[0091] Professionals may further appreciate that the units and algorithm steps of each example described in conjunction with the embodiments disclosed in this embodiment can be implemented with electronic hardware, computer software, or a combination of the two. In order to clearly illustrate the interchangeability of hardware and software, the composition and steps of each example have been generally described in terms of function in the above description. Whether these functions are performed in hardware or software depends on the specific application and design constraints of the technical solution. Professionals and technicians may use different methods to implement the described functions for each specific application, but such implementation should not be considered to be beyond the scope of this application.

[0092] The steps of the method or algorithm described in the embodiments disclosed in this embodiment can be directly implemented by hardware, software modules executed by a processor, or a combination of the two. The software module can be placed in a random access memory (RAM), a memory, a read-only memory (ROM), an electrically programmable ROM, an electrically erasable programmable ROM, a register, a hard disk, a removable disk, a CD-ROM, or any other form of storage medium known in the technical field.

[0093] The above description of the disclosed embodiments enables those skilled in the art to implement or use the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined in the present embodiment may be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to the embodiments shown in the present embodiment, but will conform to the widest scope consistent with the principles and novel features disclosed in the present embodiment.

Claims

1. A method for preparing a low-roughness yttrium oxide coating, characterized in that: The steps include: S1, plasma spraying technology is used to spray Y2O3 material on the substrate to form a yttrium oxide spray coating; S2, brushing the surface of the yttrium oxide spray coating with a liquid inorganic nano yttrium oxide crystal material, leaving it to stand, and then drying it in an environment of 80° C. to 100° C. for 6 h to 10 h; S3, polishing the yttrium oxide spray coating coated with the inorganic nano-yttrium oxide crystal material.

2. The method for preparing a low-roughness yttrium oxide coating according to claim 1, characterized in that: The following steps are also included between step S2 and step S3: S2', using liquid inorganic nano yttrium oxide crystal material to brush the surface of the yttrium oxide spray coating for a second time, and then letting it stand, and then drying it in an environment of 80° C. to 100° C. for 6 h to 10 h.

3. The method for preparing a low-roughness yttrium oxide coating according to claim 2, characterized in that: The standing time in step S2 and step S3 is 1 hour.

4. The method for preparing a low-roughness yttrium oxide coating according to claim 2, characterized in that: In step S2 and step S3, the ambient temperature is 90° C. and the drying time is 8 hours.

5. The method for preparing a low-roughness yttrium oxide coating according to claim 2, characterized in that: In step S2 and step S3, the ambient temperature is 100° C. and the drying time is 6 hours.

6. The method for preparing a low-roughness yttrium oxide coating according to claim 1, characterized in that: In step S1, the thickness of the yttrium oxide spray coating is 180 μm to 220 μm, and the surface roughness Ra of the yttrium oxide spray coating is 5 μm to 7 μm.

7. The method for preparing a low-roughness yttrium oxide coating according to any one of claims 1 to 6, characterized in that: Before step S1, the method further includes: S0, performing sandblasting on the substrate to make the surface of the substrate reach a uniform roughness, and the surface roughness Ra of the substrate is 3 μm to 4 μm.

8. The method for preparing a low-roughness yttrium oxide coating according to any one of claims 1 to 6, characterized in that: Step S3 includes: The yttrium oxide spray coating coated with inorganic nano-yttrium oxide crystal material was polished three times using diamond suspension grinding and polishing liquids with different particle sizes. The particle sizes of the diamond suspension grinding and polishing liquids for the three polishing treatments were 2.5 μm, 1.0 μm, and 0.5 μm, respectively.

9. The method for preparing a low-roughness yttrium oxide coating according to claim 8, characterized in that: The polishing conditions for the three polishing treatments are: The single-point pressure was 20N, the grinding time was 300s, the grinding disc speed was 300r / min, and the head speed was 50r / min.

10. The method for preparing a low-roughness yttrium oxide coating according to claim 1 or 2 or 3 or 4 or 5 or 6 or 9, characterized in that: The substrate is stainless steel, aluminum or titanium.

Images