Solid state deposition of dense ceramic coatings

Abstract

A cold spray deposition process is used to deposit a ceramic coating onto at least one surface of a chamber component for processing a chamber. This cold spray deposition process advances an agglomeration of ceramic nanoparticles and deposits these agglomerated nanoparticles onto the at least one surface to form the ceramic coating without subjecting the particles to a phase transition.

Description

Technical Field

[0001] Embodiments of this disclosure generally relate to cold spray deposited coatings on articles of manufacture, and to a method for applying a cold spray deposited coating to a processed chamber component. Background Technology

[0002] Ceramic coatings can be used to provide protective coatings for articles or components used in electronic processing systems. In electronic processing systems, components are exposed to high temperatures, high-energy plasmas, and corrosive fluids. These conditions can corrode and damage chamber components, and increase the susceptibility to defects. To reduce defects and increase the lifespan of components in electronic processing systems, protective coatings can be applied to improve the components' resistance to damaging conditions.

[0003] The deposition of protective coatings for treating chamber components involves reactive chemical species (e.g., YOF, YF) that can alter composition and / or stoichiometry during the coating process. Current deposition techniques typically occur at high temperatures. The elevated temperatures of current deposition methods have a thermal effect on the constituent compounds of the coating. This causes the materials used to form the coating to undergo, for example, a phase change during the coating process. For instance, the material may change from a solid source to a gaseous or liquid phase during deposition and return to the solid phase after deposition is complete.

[0004] Current methods for depositing dense ceramic coatings limit the achievable coating thickness. Dense ceramic coatings built using conventional aerosol deposition methods performed at high temperatures typically have a limited thickness of 70 μm–100 μm and may suffer from residual stress or cracking due to thermal stress caused by the deposition process. Current strategies are also limited by expensive materials and deposition methods. These methods also utilize expensive chambers in which deposition takes place, resulting in limitations on the size of the parts that can be coated and increased costs. Summary of the Invention

[0005] The following is a simplified overview of this disclosure to provide a basic understanding of some aspects thereof. This disclosure is not a broad summary of the present invention. It is not intended to identify key or essential elements of the disclosure, nor is it intended to depict any scope of any particular implementation of the disclosure or any scope of the claims. Its sole purpose is to present some concepts of the disclosure in a simplified form as a prelude to the more detailed description that follows.

[0006] In one aspect of this disclosure, a method includes using a cold spray deposition process to deposit a ceramic coating onto at least one surface of a chamber component for processing a chamber. The cold spray deposition process propels aggregates of ceramic nanoparticles onto the at least one surface to form the ceramic coating without subjecting the nanoparticles to a phase transition.

[0007] In one aspect of this disclosure, an article of article includes components for manufacturing a cavity. The article of article further includes a conformal protective layer on at least one surface of the component. The conformal protective layer has a thickness of 100 μm-200 μm and a porosity of less than 1%. Attached Figure Description

[0008] In the figures of the accompanying drawings, the present disclosure is shown by way of example rather than limitation, wherein the same element symbols indicate similar elements. It should be noted that different references to “a” or “one” embodiments in this disclosure do not necessarily refer to the same embodiment, and such references mean at least one.

[0009] Figure 1 This is a top view schematic diagram of an example electronic processing system according to an embodiment of the present disclosure.

[0010] Figure 2 This is a top view schematic diagram of an example cold spray deposition chamber according to an embodiment of the present disclosure.

[0011] Figure 3 This is an example cold spray deposition apparatus according to embodiments of the present disclosure.

[0012] Figure 4 The coating composition on the surface of a processing chamber component according to embodiments of the present disclosure is depicted.

[0013] Figure 5 This is a flowchart of a method for depositing a ceramic coating onto at least one surface of a processing chamber component according to an embodiment of the present disclosure.

[0014] Figure 6 This is a flowchart of a method for forming agglomerated nanostructured particles for ceramic coating deposition according to embodiments of the present disclosure.

[0015] Figure 7 This is a flowchart of a method for forming agglomerated nanostructured particles for ceramic coating deposition according to embodiments of the present disclosure. Detailed Implementation

[0016] The deposition of protective coatings for treating chamber components typically involves reactive chemical species (e.g., YOF, YF). These chemical species are thermally reactive, and their stoichiometry can be altered in the presence of other compounds when deposited at high temperatures. The elevated temperatures of current deposition methods have a thermal effect on the constituent compounds of the coating. This causes the materials used to form the coating to undergo, for example, a phase transition during the coating process. For instance, the material may change from a solid source to a gaseous or liquid phase during deposition and return to the solid phase after deposition is complete.

[0017] Methods involving ceramic coating deposition at higher temperatures are more likely to alter the chemical integrity of the deposited coating. Furthermore, high-temperature ceramic coating deposition methods cause the material to be deposited to undergo one or more phase transitions during the deposition process. For example, solid ceramic materials can evaporate or melt during the deposition process and can be reduced to a solid film on the coated part. This phase transition can result in coatings with poorer properties compared to coatings formed where the deposited ceramic material has not undergone a phase transition. In the embodiments, cold spray deposition methods are used to avoid concurrency issues introduced by operating at high-temperature deposition temperatures at lower coating process temperatures. Lower deposition temperatures also mitigate residual stresses resulting from the liquid-to-solid transition. Lower deposition temperatures also mitigate the difference in thermal expansion between the coated processing chamber component and the applied ceramic coating. Additionally, dense ceramic coatings (e.g., ceramic coatings with a density greater than 99%, i.e., a porosity less than 1% by volume) typically have limited thicknesses (e.g., 70 μm–100 μm). The cold spray deposition methods described herein allow for thicker ceramic coatings up to 200 μm thick while reducing stress and cracking.

[0018] Embodiments of this disclosure relate to a method of depositing a ceramic coating onto at least one surface of a processing chamber component of an electronic processing system. In embodiments, a cold spray deposition process is performed, comprising forming aggregates of ceramic nanoparticles and depositing ceramic nanostructure particles onto at least one surface of the processing chamber component to form a ceramic coating without subjecting the ceramic particles to a phase transition. In some embodiments described herein, the cold spray deposition process is performed at atmospheric pressure. In some embodiments, the cold spray deposition process may not be performed in a deposition chamber, thereby eliminating limitations on the size of the processing chamber component that can receive the coating via this deposition method. For example, the cold spray coating process according to embodiments can be used to coat components larger than those capable of being fitted into an ALD, PVD, or CVD chamber.

[0019] In some embodiments, the deposited ceramic coating formed using a cold spray deposition process has a thickness of at least 100 μm and a porosity of less than 1%, exceeding the thickness of dense coatings that are typically possible using conventional methods. Dense ceramic coatings may include porosities of less than about 1%, less than about 0.8%, less than about 0.5%, less than about 0.3%, less than about 0.1%, etc.

[0020] In embodiments, the cold spray deposition process uses ceramic particles, which may comprise nanostructured agglomerates with a predetermined stoichiometry. The predetermined stoichiometry may correspond to the stoichiometry of the final coating (e.g., precise stoichiometry) because the particles do not undergo a phase transition during the deposition process. This allows the stoichiometry of the target coating for treating the chamber component to be determined by inputting the chemical composition of the agglomerate material. Therefore, in embodiments, the final stoichiometry does not rely on chemical changes or phase transitions induced by the deposition process (e.g., operating temperature, operating pressure). In some embodiments, the agglomerates may comprise sintered agglomerates of nanoparticles.

[0021] In some embodiments, the method includes depositing nanostructured ceramic particles using a process gas. Process gases compatible with the cold spray deposition process of this disclosure may include, for example, compressed air or nitrogen. These process gases are inexpensive compared to gases used in some conventional deposition methods, such as helium and argon. In some embodiments, helium and / or argon are used in the deposition process.

[0022] In some embodiments, the article of manufacture includes components for use in a manufacturing chamber. In some embodiments, the article of manufacture includes components for use in a processing chamber. In some embodiments, the article of manufacture includes components for use in an electronic processing system. In an embodiment, the article of manufacture includes a conformal protective layer on at least one surface of the article of manufacture. In an embodiment, the porosity of the conformal protective layer is less than 1%. In an embodiment, the thickness of the conformal protective layer is at least 100 μm.

[0023] In one embodiment, the conformal protective layer may comprise a material that is a metal fluoride. These metal fluorides can be deposited as aggregated nanostructured powder in a cold spray deposition method. The cold spray deposition method avoids exposing the fluoride-containing coating material to extreme conditions, such as high temperatures or plasma. This enables deposition methods that prevent oxidation of the fluoride-containing coating material.

[0024] Figure 1This is a cross-sectional view of a semiconductor processing chamber 100 having one or more chamber components that can be coated with a ceramic coating, according to an embodiment of the present disclosure. The substrate of the processing chamber 100 may include one or more of aluminum (Al), titanium (Ti), stainless steel (SST), alumina, aluminum nitride, and / or other metals and / or ceramics. The processing chamber 100 can be used in processes in which a corrosive plasma environment with plasma processing conditions is provided. For example, the processing chamber 100 may be a chamber for a plasma etcher or plasma etching reactor, a plasma cleaner, a plasma-enhanced chemical vapor deposition (CVD) or ALD reactor, etc. Examples of chamber components that may include a coating (e.g., a ceramic coating) include a substrate support assembly 148, an electrostatic chuck (ESC) assembly 150, a ring (e.g., a process kit ring or a single ring 146), a chamber wall, a base, a gas distribution plate, a spray head, a liner, a liner kit, a shield, a plasma screen, a flow equalizer, a cooling base, a chamber viewport, a chamber cover, etc. For example, according to one embodiment, the substrate support assembly 148 may have a ceramic coating. However, it should be understood that any of the other chamber components (such as those listed above) may also include a coating deposited by cold spraying, as described in various aspects of this disclosure.

[0025] refer to Figure 1 In one embodiment, the processing chamber 100 includes a volumetric chamber body 102 and a spray head 130, the chamber body and the spray head surrounding an internal volume 106. The spray head 130 may include a spray head base and a spray head gas distribution plate. Alternatively, in some embodiments, the spray head 130 may be replaced by a cap and nozzle, or in other embodiments by a plurality of disc-shaped spray head compartments and a plasma generation unit. The chamber body 102 may be made of aluminum, stainless steel, or other suitable materials such as titanium. The chamber body 102 typically includes sidewalls 108 and a bottom 110. One or more of the spray head 130 (or cap and / or nozzle), sidewalls 108, and / or bottom 110 may include a coating deposited according to the embodiments described herein.

[0026] The outer liner 116 may be disposed adjacent to the sidewall 108 to protect the chamber body 102. The outer liner 116 may be manufactured and / or coated. In one embodiment, the outer liner 116 is made of aluminum oxide.

[0027] The exhaust port 126 may be defined within the chamber body 102 and may be coupled to the internal volume 106 to the pump system 128. The pump system 128 may include one or more pumps and throttle valves for evacuating and regulating the pressure of the internal volume 106 of the processing chamber 100.

[0028] The spray head 130 may be supported on the sidewall 108 of the chamber body 102. The spray head 130 (or cover) may be opened to allow access to the internal volume 106 of the processing chamber 100 and may provide a seal for the processing chamber 100 when closed. A gas panel 158 may be coupled to the processing chamber 100 to provide process and / or cleaning gases to the internal volume 106 via the spray head 130 or cover and nozzles. The spray head 130 may be used in a processing chamber for dielectric etching (etching of dielectric materials). The spray head 130 includes a gas distribution plate (GDP) 133 having a plurality of gas delivery holes 132 throughout the GDP 133. The spray head 130 may include the GDP 133 bonded to an aluminum or anodized aluminum spray head base 104. The GDP 133 may be made of Si or SiC, or may be a ceramic such as Y2O3, Al2O3, YAG, etc.

[0029] For processing chambers used for conductor etching (etching of conductive materials), a cover may be used instead of the spray head 130. The cover may include a central nozzle fitted into a central hole in the cover. The cover may be ceramic, such as Al2O3, Y2O3, YAG, or a ceramic compound consisting of a solid solution of Y4Al2O9 and Y2O3-ZrO2. The nozzle may also be ceramic, such as Y2O3, YAG, or a ceramic compound consisting of a solid solution of Y4Al2O9 and Y2O3-ZrO2. The cover, spray head base 104, GDP 133, and / or nozzle may be coated with a ceramic coating, depending on the application.

[0030] Examples of processing gases that can be used to process the substrate in processing chamber 100 include halogen-containing gases such as C2F6, SF6, SiCl4, HBr, NF3, CF4, CHF3, CH2F3, F, NF3, Cl2, CCl4, BCl3, and SiF4, as well as other gases such as O2 or N2O. The coating is resistant to some or all of these gases and / or plasma generated by these gases. Examples of carrier gases include N2, He, Ar, and other gases inert to the processing gases (e.g., non-reactive gases).

[0031] A substrate support assembly 148 is disposed within the internal volume 106 of the processing chamber 100, below the spray head 130 or cover. The substrate support assembly 148 holds the substrate 144 during processing. A ring 146 (e.g., a single ring) may cover a portion of the ESC assembly 150 and protect the covered portion from exposure to plasma during processing. In one embodiment, the ring 146 may be silicon or quartz.

[0032] The inner liner 118 may be coated on the periphery of the substrate support assembly 148. The inner liner 118 may be a halogen-resistant gas-resistant material, such as those discussed with reference to the outer liner 116. In one embodiment, the inner liner 118 may be made of the same material as the outer liner 116. Alternatively, the inner liner 118 may be coated with a ceramic coating.

[0033] In one embodiment, the substrate support assembly 148 includes a mounting plate 162 supporting a base 152 and an ESC assembly 150. The ESC assembly 150 further includes a thermally conductive base 164 and an electrostatic disk 166 engaged to the thermally conductive base by a joint 138, which in one embodiment may be a silicone joint. The upper surface of the electrostatic disk 166 may be covered with a ceramic coating. In one embodiment, the ceramic coating is disposed on the upper surface of the electrostatic disk 166. In another embodiment, the ceramic coating is disposed on the entire exposed surface of the ESC assembly 150, including the outer and side peripheries of the thermally conductive base 164 and the electrostatic disk 166. The mounting plate 162 is coupled to the bottom 110 of the chamber body 102 and includes channels for routing utilities (e.g., fluid, power lines, sensor leads, etc.) to the thermally conductive base 164 and the electrostatic disk 166.

[0034] The thermally conductive base 164 and / or the electrostatic disk 166 may include one or more optional embedded heating elements 176, embedded thermal isolators 174, and / or conduits 168, 170 to control the lateral temperature distribution of the substrate support assembly 148. The conduits 168, 170 may be fluidly coupled to a fluid source 172 that circulates temperature-regulating fluid through the conduits 168, 170. In one embodiment, the embedded isolator 174 may be disposed between the conduits 168, 170. The heating element 176 is regulated by a heater power supply 178. The conduits 168, 170 and the heating element 176 can be used to control the temperature of the thermally conductive base 164, thereby heating and / or cooling the electrostatic disk 166 and the processed substrate (e.g., wafer) 144. Multiple temperature sensors 190, 192 may be used to monitor the temperature of the electrostatic disk 166 and the thermally conductive base 164, and these temperature sensors may be monitored using a controller 195.

[0035] The electrostatic disk 166 may further include multiple gas channels, such as grooves, mezzanines, and other surface features, which may be formed in the upper surface of the disk 166 and / or in the ceramic coating 136. The gas channels may be fluidly coupled to a heat transfer (or back-side) gas source, such as helium, via holes drilled in the disk 166. In operation, a back-side gas may be supplied to the gas channels under controlled pressure to enhance heat transfer between the electrostatic disk 166 and the substrate 144. The electrostatic disk 166 includes at least one clamping electrode 180 controlled by a clamping power supply 182. The electrode 180 (or other electrodes disposed in the disk 166 or the base 164) may be further coupled via a matching circuit 188 to one or more RF power supplies 184, 186 for sustaining plasma formed by process and / or other gases within the processing chamber 100. The sources 184, 186 are typically capable of generating RF signals with frequencies from about 50 kHz to about 3 GHz and power outputs up to about 10,000 watts.

[0036] The cold spray solid-state deposition technique of embodiments of this disclosure enables the formation of conformal coatings with relatively uniform thickness and low porosity levels on the surface of chamber components. The coating can be plasma-resistant to reduce plasma interactions and improve component durability without affecting its performance. Thick coatings deposited using cold spray solid-state deposition (e.g., thicknesses greater than 100 micrometers, greater than 150 micrometers, greater than 200 micrometers, equal to 100-200 micrometers, etc.) can maintain the electrical properties of the component as well as its relative shape and geometry so as not to interfere with its functionality. The coating can also reduce the volatility of component materials and can form reactants with lower vapor pressures than the underlying component materials.

[0037] The resistance of a coating to plasma can be measured by the "etch rate" (ER), which can be in units of micrometers per hour (µm / hr) or angstroms per hour (Å / hr), throughout the entire duration of operation of the coated component and exposure to plasma. Measurements can be taken after different processing times. For example, measurements can be taken before processing, or at approximately 50 processing hours, or at approximately 150 processing hours, or at approximately 200 processing hours, etc. Variations in the composition of the coating grown or deposited on the heater support and / or other components can result in multiple different plasma resistance or erosion rate values. Furthermore, coatings with a single composition exposed to various plasmas can have multiple different plasma resistance or erosion rate values. For example, a plasma-resistant material may have a first plasma resistance or erosion rate associated with a first type of plasma and a second plasma resistance or erosion rate associated with a second type of plasma.

[0038] Figure 2An exemplary architecture of a cold spray deposition system 200 is shown. The cold spray deposition system 200 can be used to apply ceramic coatings to process chamber components used in semiconductor manufacturing or other electronic manufacturing via cold spray deposition. Cold spraying is a process that uses powder particles to form a coating on an article of work by means of ballistic impact. Unlike conventional thermal spraying processes (such as plasma spraying or flame spraying) that use heat to melt the coating material before deposition, cold spray deposition does not rely on the material reaching its melting point. Instead, cold spraying relies on kinetic energy to achieve bonding and coating. In cold spraying, a carrier gas (such as nitrogen or helium) is used to accelerate solid particles of the coating material to high speeds (generally above the material's critical particle velocity). These high-speed particles are guided to a substrate, which can be made of various materials such as metals, ceramics, plastics, or composites. Upon impact with the substrate, the high-energy particles deform and adhere to the surface, forming a dense and uniform coating.

[0039] In this embodiment, the powder used for cold spray coating has a particle size range of 5 to 100 micrometers (e.g., for metal particles) and is accelerated by being injected into a high-speed gas flow. The particles are then accelerated by the main nozzle gas flow and impact the workpiece. Upon impact, the solid particles deform and form an adhesion with the substrate. When solid particles are sprayed onto the substrate, various phenomena related to process parameters (such as substrate hardness, ductility, velocity, angle of incidence, etc.) are typically observed on the substrate surface. However, if the particle velocity is high enough, they can be embedded into the surface via a deposition process. Cold spraying relies on the plastic deformation of the raw material particles to adhere to the substrate. In particular, the mechanical interlocking of submicron powder with locally present powder agglomerates can be achieved via cold spraying.

[0040] In some embodiments, the cold spray deposition system 200 may include a deposition chamber 202, which may include a stage 204 for mounting a processing chamber component 206. In some embodiments, the gas pressure in the deposition chamber 202 may be reduced via a vacuum system 208. In some embodiments, a container 210 containing agglomerated nanostructured powder 216 is coupled to a gas container 212 containing a carrier gas 218 for propelling the agglomerated nanostructured powder 216 and a nozzle 214 for guiding the agglomerated nanostructured powder 216 onto the processing chamber component 206 to form a coating.

[0041] Processing chamber component 206 can be a component used in semiconductor manufacturing. This component can be a part of an etching reactor or thermal reactor, etc., within a semiconductor processing chamber. Examples of components include heaters, electrostatic chucks, nozzles, gas distribution plates, spray heads, electrostatic chuck components, chamber walls, gaskets, gasket kits, gas lines, covers, chamber covers, nozzles, single rings, processing kit rings, bases, shielding components, plasma windows, flow equalizers, cooling bases, chamber viewports, bellows, panels, and selective modulation devices. Processing chamber component 206 can be formed from bulk ceramic compounds such as aluminum, silicon, quartz, bulk yttrium oxide, bulk alumina, Y4Al2O9 and Y2O3-ZrO2 solid solutions, silicon carbide, or any other material used for semiconductor manufacturing chamber components.

[0042] In some embodiments, the processing chamber component 206 may be mounted on a stage 204 within the deposition chamber 202 during coating deposition. In some embodiments, the processing chamber component 206 may be mounted on a stage 204 not within the deposition chamber 202, thereby allowing a larger chamber component to be coated. The stage 204 may be a movable stage (e.g., a motorized stage) that can move in one, two, or three dimensions and / or rotate / tilt about one or more directions, such that the stage 204 can be moved to different positions to facilitate coating of the processing chamber component 206 with aggregated nanostructured powder 216 advanced from the nozzle 214. For example, since applying a coating via spraying is a line-of-sight process, the movable stage 204 can be used to coat different portions or sides of the processing chamber component 206. If the processing chamber component 206 has different sides to be coated or a complex geometry, the stage 204 can adjust the position of the processing chamber component 206 relative to the nozzle 214 so that the entire assembly can be coated. In other words, the nozzle 214 can selectively target certain portions of the processing chamber component 206 from various angles and orientations.

[0043] Gas container 212 contains pressurized carrier gas 218, such as nitrogen, argon, compressed air, or helium. Pressurized carrier gas 218 travels under pressure from gas container 212 into chamber 210. As pressurized carrier gas 218 travels from chamber 210 to nozzle 214, it pushes some agglomerated nanostructured powder 216 toward nozzle 214.

[0044] In one embodiment, the coating powder particles are nano-sized, and the agglomerated nanostructured powder 216 has a certain degree of flowability. Further, according to one embodiment, the agglomerated nanostructured powder 216 may comprise a mixture of multiple oxides for forming the composite coating, rather than coating with a single oxide such as yttrium oxide (which may be incompatible with certain chemicals). For example, the coating powder may be a composite ceramic material or a mixture of multiple metal oxides, metal fluorides, and / or metal fluoride oxides. Examples of materials used for the agglomerated nanostructured powder 216 include Y₂O₃, ... xO y Mg x O y Mg2O3, ZrO2, Al2O3, Y x Zr y O z Y v Zr x O y F z Y3Al5O 12 Y4Al2O9, YF3, Y x O y F z Er2O3, Er3Al5O 12 ErF3, Er x O y F z , La2O3, Lu2O3, Sc2O3, ScF3, Sc x O y F z Gd2O3, GdF3, Gd x O y F z Sm2O3 or Dy2O3, or combinations thereof.

[0045] In this embodiment, the agglomerated nanostructured powder may be formed by a target final stoichiometry. In this embodiment, the different materials in the agglomerated nanostructured powder may not change their stoichiometry when deposited onto article 206. Coatings formed from these agglomerated nanostructured powders may have low erosion rates and provide improved on-wafer particle properties during use in semiconductor manufacturing chambers. In this embodiment, the agglomerates of the nanostructured powder may have a particle size range of 2-50 micrometers, 5-20 micrometers, or other size ranges.

[0046] Regarding the ceramic compound that may be a component of the agglomerates (and the final coating formed), in one embodiment, the ceramic compound may include 50-80 mol% YOF and 20-50 mol% YF. In some embodiments, the TiO2 powder consists of nano-primary particles. In some embodiments, the agglomerates may include pores. In some embodiments, the agglomerated nanostructured powder comprises agglomerated particles having a predetermined stoichiometry intended to correspond to the stoichiometry of the ceramic coating. In some embodiments, the agglomerates comprise at least one of TiO2 or alumina. In some embodiments, the ceramic compound may include 50-75 mol% Y2O3, 10-30 mol% ZrO2, and 10-30 mol% Al2O3. In another embodiment, the ceramic compound may include 40-100 mol% Y2O3, 0-60 mol% ZrO2, and 0-10 mol% Al2O3. In another embodiment, the ceramic compound may include 40-60 mol% Y₂O₃, 30-50 mol% ZrO₂, and 10-20 mol% Al₂O₃. In another embodiment, the ceramic compound may include 40-50 mol% Y₂O₃, 20-40 mol% ZrO₂, and 20-40 mol% Al₂O₃. In another embodiment, the ceramic compound may include 70-90 mol% Y₂O₃, 0-20 mol% ZrO₂, and 10-20 mol% Al₂O₃. In yet another embodiment, the ceramic compound may include 60-80 mol% Y₂O₃, 0-10 mol% ZrO₂, and 20-40 mol% Al₂O₃. In another embodiment, the ceramic compound may include 40-60 mol% Y₂O₃, 0-20 mol% ZrO₂, and 30-40 mol% Al₂O₃. In other embodiments, other proportions may also be used for the ceramic compound.

[0047] As a carrier gas 218 propelling a suspension of agglomerated nanostructured powder 216 enters the deposition chamber 202 through an opening in the nozzle 214, the agglomerated nanostructured powder 216 is propelled toward the processing chamber component 206. In one embodiment, the carrier gas 218 is pressurized such that the agglomerated nanostructured powder 216 is propelled toward the processing chamber component 206 at a rate ranging from about 10 mm / s to about 100 mm / s. In another embodiment, the rate may be in the range of about 20 mm / s to about 90 mm / s. In another embodiment, the rate may be in the range of about 30 mm / s to about 80 mm / s. In another embodiment, the rate may be in the range of about 40 mm / s to about 70 mm / s. In another embodiment, the rate may be in the range of about 50 mm / s to about 60 mm / s. In some embodiments, the distance between the nozzle 214 and the processing chamber component 206 is in the range of about 1 mm to about 20 mm. In another embodiment, the distance may range from about 5 mm to about 15 mm. In another embodiment, the distance may range from about 15 mm to about 25 mm. In some embodiments, the carrier gas is unheated. In some embodiments, the carrier gas is heated to a temperature of about 20°C to 700°C (e.g., 100°C, 200°C, 300°C, 400°C, 500°C, 600°C, etc.). In some embodiments, the carrier gas is provided at a pressure of about 1-5 MPa (e.g., 2 MPa, 3 MPa, 4 MPa, etc.). In an embodiment, the chamber component 206 moves relative to the nozzle 214 at a traversal speed of about 1000 mm / s to about 5000 mm / s (e.g., about 2000 mm / s). In an embodiment, low-pressure cold spraying is used, wherein the carrier gas may be, for example, nitrogen or air. In some embodiments, high-pressure cold spraying is performed using, for example, nitrogen or helium.

[0048] In one embodiment, nozzle 214 is formed to be abrasion resistant. As the agglomerated nanostructured powder 216 moves through nozzle 214 at high speed, nozzle 214 can wear and degrade rapidly. However, nozzle 214 can minimize or reduce wear and material formation. Upon impact processing chamber component 206, the particles of agglomerated nanostructured powder 216 can fracture and deform due to kinetic energy (e.g., via plastic deformation) to create an anchoring layer adhered to processing chamber component 206. As the application of agglomerated nanostructured powder 216 continues, the particles become a coating or film by bonding to themselves. The coating on processing chamber component 206 continues to grow through continuous collisions of particles of agglomerated nanostructured powder 216 on processing chamber component 206. In other words, the particles collide with each other and the substrate at high speed under vacuum or atmospheric pressure to break into smaller fragments to form a dense layer, rather than undergoing a phase transition. In some embodiments, the initial layer of the coating is achieved through plastic deformation of the substrate (e.g., particularly if the substrate is a ductile metal substrate) when the particles are embedded in the substrate, without any additional binder or calcination process. In some embodiments, the coating / substrate interface is relatively rough when the particles impact the substrate at high speed. As a result, the powder particles can be embedded in the substrate. Roughness may lead to mechanical entanglement to improve adhesion. In one embodiment, the particle crystal structure of the aggregated nanostructured powder 216 is retained after application to the processing chamber component 206.

[0049] In one embodiment, a barrier layer is formed between the coating and the processing chamber component 206 to prevent process chemicals penetrating the coating from reacting with the underlying substrate. This minimizes delamination. The barrier layer increases the adhesion strength of the ceramic coating and minimizes peeling. In some embodiments, the ceramic coating has a porosity of less than about 1%. In other embodiments, the ceramic coating has a porosity of less than 5%. In other embodiments, the ceramic coating has a porosity of less than 0.1%. In embodiments, the coating has a thickness greater than 100 micrometers, 100-200 micrometers, or more.

[0050] In some embodiments, the deposition process may be an aerosol deposition process.

[0051] In one embodiment, aerosol deposition occurs in a chamber 202 of a cold spray deposition system 200, which can be evacuated using a vacuum system 208, such that a vacuum exists within the deposition chamber 202. In some embodiments, the operating pressure of the deposition process can be in the range of about 2 MPa to about 6 MPa. In other embodiments, the operating pressure of the deposition process can be in the range of about 4 MPa to about 5 MPa. In other embodiments, the operating pressure of the deposition process can be in the range of about 3 MPa to about 5 MPa. Providing a vacuum in the deposition chamber 202 can facilitate the application of coatings for alternative deposition processes, such as aerosol deposition.

[0052] For example, in an aerosol deposition process, agglomerated nanostructured powder 216 alternatively comprises an aerosolized deposition feedstock. The aerosolized deposition feedstock may comprise particles of the same stoichiometry as those in a cold spray deposition process. When the deposition chamber 202 is under vacuum, the aerosolized deposition feedstock propelled from the nozzle encounters less resistance as the aerosolized particles travel to the processing chamber component 206. Therefore, the aerosolized feedstock can impact the processing chamber component 206 at a higher rate, which is beneficial for adhesion to the processing chamber component 206 and the formation of a coating.

[0053] Figure 3 A schematic diagram of a cold spray ceramic deposition apparatus is shown. As shown, gas inlet 310 provides a carrier gas accelerated toward article 350 via gas heater 320. Additionally, powder feeder 340 provides agglomerated nanostructured powder to nozzle 330, such that the agglomerated powder is mixed with the carrier gas flow provided from gas heater 320 via gas inlet 310.

[0054] When the carrier gas flow mixes with the agglomerated nanostructured powder, a suspension of agglomerated nanostructured powder 345 is formed in the gas. The suspension 345 of agglomerated nanostructured powder and carrier gas is then pushed toward the processing chamber component 350.

[0055] An additional parameter that can be adjusted for the cold spray solid deposition process is the process operating temperature during deposition. In one embodiment, a gas heater 320 heats the carrier gas stream to the operating temperature. In some embodiments, the operating temperature is in the range of about 100°C to about 800°C. In other embodiments, the operating temperature is between 200°C and 700°C. In other embodiments, the operating temperature is between 300°C and 600°C. In other embodiments, the operating temperature is between 400°C and 500°C. Lower operating temperatures can result in less stress and thermal cracking in the deposited protective layer.

[0056] In some embodiments, at least one surface of the chamber component may be cleaned with acetone prior to the deposition process. In some embodiments, the cold spray deposition process is performed at atmospheric pressure.

[0057] Figure 4 An article 400 comprising a coating 420 on a processing chamber component 410 according to one embodiment is shown. The coating 420 may be formed using a cold spray solid deposition process as described in aspects of this disclosure.

[0058] In one embodiment, the coating may be about 10 µm to about 200 µm thick. In other embodiments, the coating may be about 50 µm to about 150 µm thick. In other embodiments, the coating may be about 100 µm to about 200 µm thick. In other embodiments, the coating may be about 150 µm to about 250 µm thick.

[0059] In one embodiment of the heat-treated article 400, a barrier layer 430 may be formed between the processing chamber component 410 and the coating 420. The barrier layer 430 may improve the adhesion of the coating 420 to the processing chamber component 410 and / or improve the on-wafer particle performance of the article 400 during use in a semiconductor manufacturing chamber.

[0060] In some embodiments, the agglomerated nanostructured powder may have the same stoichiometry as the ceramic coating. In some embodiments, the different materials in the agglomerated nanostructured powder may not change their stoichiometry during the deposition process. In some embodiments, the deposition method produces an interlock between submicron powder and locally present agglomerates. In some embodiments, the microhardness of the ceramic coating is in the range of about 300 Hv to about 350 Hv. In other embodiments, the microhardness of the ceramic coating is in the range of about 310 Hv to about 340 Hv. In other embodiments, the microhardness of the ceramic coating is in the range of about 320 Hv to about 330 Hv. In some embodiments, the ceramic coating may have a porosity of less than 1%. In some embodiments, cold spray deposition of the agglomerated nanostructured powder increases the adhesion strength of the TiO2 coating. In some embodiments, the lower temperature of the cold spray deposition method reduces the residual stress of the ceramic coating.

[0061] Figure 5 This is a flowchart of a method 500 for depositing a ceramic coating onto at least one surface of a chamber component using a cold spray deposition process, according to embodiments of the present disclosure. At block 510, a chamber component is provided for processing. At block 520, at least one surface of the chamber component is cleaned with acetone prior to coating deposition. At block 530, a ceramic coating is deposited onto at least one surface of the chamber component for processing the chamber using a cold spray deposition process. The cold spray deposition process deposits ceramic particles onto at least one surface to form a ceramic coating without subjecting the ceramic particles to a phase transition. The cold spray deposition process can be performed using any of the parameters described above. In an embodiment, the ceramic coating is a fluoride coating (e.g., YF3) that does not contain oxygen (or contains an almost immeasurable amount of oxygen). For highly reactive materials such as fluorides, deposition techniques that induce a phase transition during deposition (e.g., plasma spraying) typically cannot form an oxygen-deficient coating due to the reactive nature of the material (e.g., fluorine). For example, when a fluoride material may be the target, such processes induce at least some oxidation, resulting in a fluoride oxide coating.

[0062] In one embodiment, the ceramic coating is a protective layer, which is a sealing coating having the same microstructure as the provided processing chamber component. In another embodiment, the conformal protective layer comprises stacked, aggregated nanostructured ceramic powder.

[0063] In the embodiments, various techniques can be used to form agglomerated nanostructured powders for cold spray deposition.

[0064] Figure 6 This is a flowchart of a method 600 for forming agglomerated nanostructured particles for cold spray solid deposition according to embodiments of the present disclosure. At block 610, a solution of a nitrate or citrate of metal ions is provided to an anodic aluminum oxide film. At block 620 of method 600, the solution is heat-treated to nucleate metal oxide particles within the pores of the film. At block 630, agglomerated nanostructured particles are allowed to nucleate from the solution. In some embodiments, the agglomerated nanostructured powder has an average size of about 5 μm to about 40 μm. In other embodiments, the agglomerated nanostructured powder has an average size of about 10 μm to about 20 μm. In some embodiments, the agglomeration process may include the addition of an inorganic salt.

[0065] Figure 7 This is a flowchart of a method 700 for forming aggregated nanostructured particles for cold spray solid deposition according to embodiments of the present disclosure. At block 710, a solution of a nitrate or citrate salt of metal ions is provided to a stirrer. These salts promote aggregation. At block 720 of method 700, the temperature of the stirred solution is reduced.

[0066] At box 730, an oxidant is added to the stirred solution. At box 740, agglomerated nanostructured particles are allowed to nucleate from the solution. In some embodiments, the agglomerated nanostructured powder has an average size of about 5 μm to about 40 μm. In other embodiments, the agglomerated nanostructured powder has an average size of about 10 μm to about 20 μm.

[0067] In some embodiments, the agglomeration process may include the addition of inorganic salts.

[0068] In this embodiment, a hydrothermal method can be used to agglomerate nanoparticles to obtain microagglomerated powder. The hydrothermal treatment can be performed by immersing the powder (e.g., Y₂O₃ nanoparticles) in distilled water with added ammonium sulfate ((NH₄)₂SO₄). The solution can be stirred in an oil bath to maintain a target temperature (e.g., at 150°C) for a target time (e.g., up to 4 hours). For example, the particle size can have an average size of 30 nm, which can agglomerate into 2 μm particle agglomerates under surface energy-driven conditions. Upon addition of the inorganic sulfate (NH₄)₂SO₄, the particles can agglomerate into a near-spherical structure resembling snowballs. Increasing the amount of (NH₄)₂SO₄ added can make the particle agglomeration more compact, and the particle morphology can become coarser, with smaller particles adsorbed on the surface of larger agglomerated particles.

[0069] Throughout this specification, references to "one embodiment" or "an embodiment" mean that a particular feature, structure, or characteristic described in connection with that embodiment is included in at least one embodiment. Therefore, the phrases "in one embodiment" or "in an embodiment" appearing in various places throughout this specification do not necessarily all refer to the same embodiment. Additionally, the term "or" is intended to mean inclusive "or," not exclusive "or." When the terms "about" or "approximately" are used herein, this is intended to mean that the presented nominal values ​​are exactly within ±10%.

[0070] Although the operations of the methods described herein are shown and described in a specific order, the order of operations for each method may be changed, such that some operations may be performed in reverse order, or that some operations may be performed at least partially concurrently with other operations. In another embodiment, instructions or sub-operations of different operations may be performed intermittently and / or alternately.

[0071] The foregoing description sets forth numerous specific details, such as examples of particular systems, components, methods, etc., to provide a good understanding of several embodiments of this disclosure. However, it will be apparent to those skilled in the art that at least some embodiments of this disclosure can be practiced without these specific details. In other instances, well-known components or methods have not been described in detail, or have been presented in a simple block diagram format so as not to unnecessarily obscure the disclosure. Therefore, the specific details set forth are merely exemplary. Specific implementations may differ from these exemplary details and are still contemplated as being within the scope of this disclosure.

[0072] It will be understood that the above description is intended to be illustrative and not restrictive. Many other embodiments will become apparent to those skilled in the art upon reading and understanding the above description. Therefore, the full scope of this disclosure, together with the equivalents of such claims, should be determined with reference to the appended claims.

Claims

1. A method comprising: A cold spray deposition process is used to deposit a ceramic coating onto at least one surface of a chamber component for processing a chamber, wherein the cold spray deposition process advances ceramic nanoparticles and deposits agglomerated ceramic particles onto the at least one surface to form the ceramic coating without subjecting the particles to a phase transition.

2. The method of claim 1, further comprising: Before depositing the ceramic coating onto the at least one surface, the at least one surface of the chamber component is cleaned with acetone.

3. The method of claim 1, wherein the cold spray deposition process is performed under atmospheric pressure.

4. The method of claim 1, wherein the ceramic coating has a thickness of at least 100 micrometers and a porosity of less than about 1%.

5. The method of claim 1, wherein the cold spray deposition process is performed using ceramic particles, the ceramic particles comprising agglomerates having a predetermined stoichiometry corresponding to the stoichiometry of the ceramic coating.

6. The method of claim 5, wherein the agglomerate is a sintered agglomerate of nanoparticles.

7. The method of claim 5, wherein the agglomerate comprises at least one of TiO2 or alumina.

8. The method of claim 5, wherein the agglomerate further comprises at least one of: Y₂O₃, Y x O y Mg x O y ZrO2, Al2O3, Y x Zr y O z Y v Zr x O y F z Y3Al5O 12 Y4Al2O9, YF3, Y x O y F z Er2O3, Er3Al5O 12 ErF3, Er x O y F z , La2O3, Lu2O3, Sc2O3, ScF3, Sc x O y F z Gd2O3, GdF3, Gd x O y F z Sm2O3 or Dy2O3.

9. The method of claim 1, wherein the deposition further comprises the agglomeration of the ceramic particles and the processing gas.

10. The method of claim 9, wherein the processing gas comprises at least one of compressed air or nitrogen.

11. The method of claim 1, wherein the deposition occurs at an operating temperature of 300°C-600°C.

12. The method of claim 1, wherein the deposition occurs at an operating pressure of 2 MPa-5 MPa.

13. The method of claim 1, wherein the agglomerate powder is prepared using a hydrothermal process.

14. The method of claim 13, wherein the agglomerate powder particles have an average size of 8 μm to 30 μm.

15. The method of claim 13, wherein the agglomerate powder is prepared using a spray drying process.

16. An article comprising: Components used in manufacturing chambers; as well as A conformal protective layer is provided on at least one surface of the component, wherein the porosity of the conformal protective layer is less than 1%, and wherein the conformal protective layer has a thickness of 100 μm-200 μm.

17. The article of claim 16, wherein the conformal protective layer comprises at least one of the following: Y₂O₃, ... x O y Mg x O y ZrO2, Al2O3, Y x Zr y O z Y v Zr x O y F z Y3Al5O 12 Y4Al2O9, YF3, Y x O y F z Er2O3, Er3Al5O 12 ErF3, Er x O y F z , La2O3, Lu2O3, Sc2O3, ScF3, Sc x O y F z Gd2O3, GdF3, Gd x O y F z Sm2O3 or Dy2O3.

18. The article of claim 16, wherein the article is selected from the group consisting of: heater, electrostatic chuck, nozzle, gas distribution plate, spray head, electrostatic chuck component, chamber wall, liner, liner kit, gas line, cover, chamber cover, nozzle, single ring, treatment kit ring, base, shield, plasma window, flow equalizer, cooling base, chamber viewport, bellows, panel, and selective modulation device.

19. The article of claim 16, wherein the conformal protective layer is a sealing coating having the same microstructure as the component.

20. The article of claim 16, wherein the conformal protective layer comprises stacked agglomerated ceramic powder.

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