Solid-state deposition of dense ceramic coatings

Abstract

A ceramic coating is deposited onto at least one surface of a chamber component for a process chamber using a cold spray deposition process. The cold spray deposition process propels agglomerates of nanoparticles of a ceramic and deposits the agglomerated nanoparticles of the ceramic onto the at least one surface to form the ceramic coating without causing the particles to undergo a phase change.

Description

SOLID-STATE DEPOSITION OF DENSE CERAMIC COATINGSTECHINCAL FIELD

[0001] Embodiments of the present disclosure relate, in general, to cold spray deposition coatings on articles and to a method for applying a cold spray deposition coating to a process chamber component.BACKGROUND

[0002] Ceramic coatings may be used to provide a protective coating for an article or component for use in an electronics processing system. In an electronics processing system, components of the processing system are exposed to high temperatures, high energy plasma, and corrosive fluids. These conditions mat erode chamber components, corrode chamber components, and increase the components’ susceptibility to defects. To reduce the defects and increase the lifespan of the component of an electronics processing system, protective coatings may be applied to improve a components resistance to damaging conditions.

[0003] Deposition of protective coatings for process chamber components include reactive chemical species (e.g. YOF, YF) that can alter in composition and / or stoichiometry during the coating process. Current deposition techniques generally occur under elevated temperatures. The increased temperature of current deposition methods has a thermal effect on the constituent chemical 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 example, the materials may change from a solid source to a gas or liquid phase during deposition, and back to a solid phase after deposition is complete.

[0004] Current methods of depositing dense ceramic coatings have a limit to the thickness of coating that can be achieved. Dense ceramic coatings established with conventional aerosol deposition methods that are performed at elevated temperatures typically have limited thicknesses of 70 - 100 pm and may suffer from residual stress or cracking from thermal stress induced by the deposition process. Current strategies may also suffer from expensive materials and deposition methods. These methods also use expensive chambers that a deposition occurs in, resulting in size restrictions for the components that can be coated and an increase in cost.SUMMARY

[0005] The following is a simplified summary of the disclosure in order to provide a basic understanding of some aspects of the disclosure. This summary is not an extensiveoverview of the disclosure. It is intended to neither identify key or critical elements of the disclosure, nor delineate any scope of the particular implementations 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 is presented later.

[0006] In one aspect of the disclosure, a method includes depositing a ceramic coating onto at least one surface of a chamber component for a process chamber using a cold spray deposition process. The cold spray deposition process propels agglomerates of ceramic nanoparticles of a ceramic onto the at least one surface to form the ceramic coating without causing the nanoparticles to undergo a phase change.

[0007] In one aspect of the disclosure, an article includes a component for use in a manufacturing chamber. The article further includes a conformal protective layer on at least one surface of the component. The conformal protective layer has a thickness of 100-200 pm and a porosity of less than 1%.BRIEF DESCRIPTION OF THE DRAWINGS

[0008] The present disclosure is illustrated by way of example, and not by way of limitation, in the figures of the accompanying drawings in which like references indicate similar elements. It should be noted that different references to “an” or “one” embodiment in this disclosure are not necessarily to the same embodiment, and such references mean at least one.

[0009] FIG. 1 is a top schematic view of an example electronic processing system, according to embodiments of the present disclosure.

[0010] FIG. 2 is a top schematic view of an example cold spray deposition chamber, according to embodiments of the present disclosure.

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

[0012] FIG. 4 depicts a coating composition on the surface of a process chamber component, according to embodiments of the present disclosure.

[0013] FIG. 5 is flow chart for a method of depositing a ceramic coating onto at least one surface of a process chamber component, according to embodiments of the present disclosure.

[0014] FIG. 6 is flow chart for a method of forming agglomerated nanostructured particles for ceramic coating deposition, according to embodiments of the present disclosure.

[0015] FIG. 7 is flow chart for a method of forming agglomerated nanostructured particles for ceramic coating deposition, according to embodiments of the present disclosure.DETAILED DESCRIPTION OF EMBODIMENTS

[0016] Deposition of protective coatings for process chamber components often include reactive chemical species (e.g. YOF, YF). These chemical species are thermally reactive and their stoichiometries can change in the presence of other compounds when deposited at high temperature. The increased temperature of current deposition methods has 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 example, the materials may change from a solid source to a gas or liquid phase during deposition, and back to a solid phase after deposition is complete.

[0017] Methods of ceramic coating deposition that occur at higher temperatures are more likely to alter the chemical integrity of the deposited coating. Moreover, methods of ceramic coating deposition that occur at elevated temperatures cause a material to be deposited to undergo one or more phase changes during the deposition process. For example, a solid ceramic material may be vaporized or melted during the deposition process, and may reform into a solid film on a coated component. Such phase changes can cause the coatings to have inferior coating properties as opposed to coatings that are formed without a deposited ceramic material undergoing a phase change. In embodiments, cold spray deposition methods are used to avoid complications introduced by depositing at elevated temperatures by operating at reduced coating process temperatures. Lower deposition temperature also mitigates residual stress that results from a liquid to solid transition. Reduced deposition temperatures also mitigate thermal expansion differences of the process chamber component being coated and the ceramic coating being applied. Additionally, dense ceramic coatings (e.g., ceramic coatings having a density of greater than 99%, i.e., a porosity of less than 1% of volume) conventionally have limited thickness (e.g. 70 - 100 pm). Cold spray deposition methods described herein allow for thicker ceramic coatings up to 200 pm thick, with reduced stress and cracking.

[0018] Embodiments of the present disclosure relate to a method of depositing a ceramic coating onto at least one surface of a process chamber component of an electronics processing system. In embodiments, a cold spray deposition process is performed that includes forming an agglomerate of nanoparticles of a ceramic and depositing the nanostructured particles of the ceramic onto at least one surface of a process chambercomponent to form a ceramic coating without causing the ceramic particles to undergo a phase change. 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, removing limitations of the size of the process chamber components that can receive a coating via this deposition method. For example, components that are larger than can fit inside of an ALD, PVD or CVD chamber may be coated using a cold spray coating process according to embodiments.

[0019] In some embodiments, a deposited ceramic coating formed using a cold spray deposition process has a thickness of at least 100 pm and a porosity of less than 1%, exceeding the thickness of dense coatings that is generally possible with conventional methods. The dense ceramic coatings may include a porosity 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%, and so on.

[0020] In embodiments, the cold spray deposition process is performed using ceramic particles that may include nanostructured agglomerates of a predetermined stoichiometry. The predetermined stoichiometry may correspond to the stoichiometry (e.g., to the exact stoichiometry) of the final coating due to the particles not undergoing a phase change during the deposition process. This allows for the stoichiometry of the target coating for the process chamber component to be determined by the chemical make up of the input agglomerate material. Accordingly, the final stoichiometry is not reliant on chemical changes or phase changes induced by the deposition process (e.g., operation temperature, operation pressure) in embodiments. In some embodiments, the agglomerate may include sintered agglomerates of nanoparticles.

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

[0022] In some embodiments, an article includes a component for use in a manufacturing chamber. In some embodiments, an article may include a component for using in a process chamber. In some embodiments, an article may include a component for use in an electronics processing system. In embodiments, the article may include a conformal protective layer on at least one surface of the article. The porosity of the conformal protective layer is less than1% in embodiments. In embodiments, the thickness of the conformal protective layer is at least 100 pm.

[0023] In embodiments, the conformal protective layer may include materials that are metal fluorides. These metal fluorides may be deposited as agglomerated nanostructured powders in a cold spray deposition method. The cold spray deposition method avoids exposing fluoride-containing coating materials to extreme conditions such as elevated temperatures or plasmas. This enables a deposition method that avoids oxidation of fluoride- containing coating materials.

[0024] FIG. 1 is a sectional view of a semiconductor processing chamber 100 having one or more chamber components that may be coated with a ceramic coating in accordance with embodiments of the present disclosure. The base materials of the processing chamber 100 may include one or more of aluminum (Al), titanium (Ti), stainless steel (SST), aluminum oxide, aluminum nitride, and / or other metals and / or ceramics. The processing chamber 100 may be used for processes in which a corrosive plasma environment having plasma processing conditions is provided. For example, the processing chamber 100 may be a chamber for a plasma etcher or plasma etch reactor, a plasma cleaner, plasma enhanced chemical vapor deposition (CVD) or ALD reactors and so forth. Examples of chamber components that may include a coating layer (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 single ring 146), a chamber wall, a base, a gas distribution plate, a showerhead, a liner, a liner kit, a shield, a plasma screen, a flow equalizer, a cooling base, a chamber viewport, a chamber lid, and so on. For example, the substrate support assembly 148 may have a ceramic coating , in accordance with one embodiment. 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 spray, as described in aspects of the present disclosure.

[0025] Referring to FIG. 1, in one embodiment, the processing chamber 100 includes a chamber body 102 and a showerhead 130 that enclose an interior volume 106. The showerhead 130 may include a showerhead base and a showerhead gas distribution plate. Alternatively, the showerhead 130 may be replaced by a lid and a nozzle in some embodiments, or by multiple pie shaped showerhead compartments and plasma generation units in other embodiments. The chamber body 102 may be fabricated from aluminum, stainless steel or other suitable material, such as titanium. The chamber body 102 generally includes sidewalls 108 and a bottom 110. One or more of the showerhead 130 (or lid and / ornozzle), sidewalls 108 and / or bottom 110 may include a coating deposited according to embodiments described herein.

[0026] An outer liner 116 may be disposed adjacent the sidewalls 108 to protect the chamber body 102. The outer liner 116 may be fabricated and / or coated with a coating layer. In one embodiment, the outer liner 116 is fabricated from aluminum oxide.

[0027] An exhaust port 126 may be defined in the chamber body 102, and may couple the interior volume 106 to a pump system 128. The pump system 128 may include one or more pumps and throttle valves utilized to evacuate and regulate the pressure of the interior volume 106 of the processing chamber 100.

[0028] The showerhead 130 may be supported on the sidewall 108 of the chamber body 102. The showerhead 130 (or lid) may be opened to allow access to the interior volume 106 of the processing chamber 100, and may provide a seal for the processing chamber 100 while closed. A gas panel 158 may be coupled to the processing chamber 100 to provide process and / or cleaning gases to the interior volume 106 through the showerhead 130 or lid and nozzle. Showerhead 130 may be used for processing chambers used for dielectric etch (etching of dielectric materials). The showerhead 130 includes a gas distribution plate (GDP) 133 having multiple gas delivery holes 132 throughout the GDP 133. The showerhead 130 may include the GDP 133 bonded to an aluminum or an anodized aluminum showerhead base 104. The GDP 133 may be made from Si or SiC, or may be a ceramic such as Y2O3, AI2O3, YAG, and so forth.

[0029] For processing chambers used for conductor etch (etching of conductive materials), a lid may be used rather than a showerhead 130. The lid may include a center nozzle that fits into a center hole of the lid. The lid may be a ceramic such as AI2O3, Y2O3, YAG, or a ceramic compound composed of Y4AI2O9 and a solid-solution of Y2O3-ZrO2. The nozzle may also be a ceramic, such as Y2O3, YAG, or the ceramic compound composed of Y4AI2O9 and a solid-solution of Y2O3-ZrO2. The lid, showerhead base 104, GDP 133 and / or nozzle may optionally be coated with a ceramic coating.

[0030] Examples of processing gases that may be used to process substrates in the processing chamber 100 include halogen-containing gases, such as C2F6, SFe, SiCh, HBr, NF3, CF4, CHF3, CH2F3, F, NF3, Ch, CCI4, BCI3 and SiF4, among others, and other gases such as O2, or N2O. The coating layer may be resistant to erosion from some or all of these gases and / or plasma generated from these gases. Examples of carrier gases include N2, He, Ar, and other gases inert to process gases (e.g., non-reactive gases).

[0031] The substrate support assembly 148 is disposed in the interior volume 106 of the processing chamber 100 below the showerhead 130 or lid. 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 may protect the covered portion from exposure to plasma during processing. The ring 146 may be silicon or quartz in one embodiment.

[0032] An inner liner 118 may be coated on the periphery of the substrate support assembly 148. The inner liner 118 may be a halogen-containing gas resistant material such as those discussed with reference to the outer liner 116. In one embodiment, the inner liner 118 may be fabricated from the same materials of the outer liner 116. Additionally, 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 pedestal 152, and an ESC assembly 150. The ESC assembly 150 further includes a thermally conductive base 164 and an electrostatic puck 166 bonded to the thermally conductive base by a bond 138, which may be a silicone bond in one embodiment. An upper surface of the electrostatic puck 166 may be covered by a ceramic coating. In one embodiment, the ceramic coating is disposed on the upper surface of the electrostatic puck 166. In another embodiment, the ceramic coating is disposed on the entire exposed surface of the ESC assembly 150 including the outer and side periphery of the thermally conductive base 164 and the electrostatic puck 166. The mounting plate 162 is coupled to the bottom 110 of the chamber body 102 and includes passages for routing utilities (e.g., fluids, power lines, sensor leads, etc.) to the thermally conductive base 164 and the electrostatic puck 166.

[0034] The thermally conductive base 164 and / or electrostatic puck 166 may include one or more optional embedded heating elements 176, embedded thermal isolators 174 and / or conduits 168, 170 to control a lateral temperature profile of the substrate support assembly 148. The conduits 168, 170 may be fluidly coupled to a fluid source 172 that circulates a temperature regulating fluid through the conduits 168, 170. The embedded isolator 174 may be disposed between the conduits 168, 170 in one embodiment. The heating elements 176 are regulated by a heater power source 178. The conduits 168, 170 and heating elements 176 may be utilized to control the temperature of the thermally conductive base 164, thus heating and / or cooling the electrostatic puck 166 and a substrate e.g., a wafer) 144 being processed. The temperature of the electrostatic puck 166 and the thermally conductive base 164 may be monitored using a plurality of temperature sensors 190, 192, which may be monitored using a controller 195.

[0035] The electrostatic puck 166 may further include multiple gas passages such as grooves, mesas and other surface features, which may be formed in an upper surface of the puck 166 and / or the ceramic coating layer 136. The gas passages may be fluidly coupled to a source of a heat transfer (or backside) gas such as helium via holes drilled in the puck 166. In operation, the backside gas may be provided at controlled pressure into the gas passages to enhance the heat transfer between the electrostatic puck 166 and the substrate 144. The electrostatic puck 166 includes at least one clamping electrode 180 controlled by a chucking power source 182. The electrode 180 (or other electrode disposed in the puck 166 or base 164) may further be coupled to one or more RF power sources 184, 186 through a matching circuit 188 for maintaining a plasma formed from process and / or other gases within the processing chamber 100. The sources 184, 186 are generally capable of producing an RF signal having a frequency from about 50 kHz to about 3 GHz, with a power output of up to about 10,000 Watts.

[0036] The cold spray solid state deposition technique of embodiments of the present disclosure enables a conformal coating of relatively uniform thickness and low levels of porosity on the surfaces of chamber components. The coating may be plasma resistant to reduce plasma interactions and improve a component’s durability without impacting its performance. A thick coating (e.g., greater than 100 microns, greater than 150 microns, greater than 200 microns, 100-200 microns, etc. in thickness) deposited with cold spray solid state deposition techniques may maintain the electrical properties and relative shape and geometric configuration of the component so as to not disturb its functionality. The coating may also reduce the volatility of the component’s materials and may form reactants having a lower vapor pressure than the component’ s underlying materials.

[0037] The resistance of the coating to plasma may be measured through “etch rate” (ER), which may have units of micrometer / hour (pm / hr) or Angstrom / hour (A / hr), throughout the duration of the coated components’ operation and exposure to plasma. Measurements may be taken after different processing times. For example, measurements may be taken before processing, or at about 50 processing hours, or at about 150 processing hours, or at about 200 processing hours, and so on. Variations in the composition of the coating grown or deposited on the heater support and / or other components may result in multiple different plasma resistances or erosion rate values. Additionally, a coating with a single composition exposed to various plasmas could have multiple different plasma resistances or erosion rate values. For example, a plasma resistant material may have a firstplasma 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] FIG. 2 illustrates an exemplary architecture of a cold spray deposition system 200. The cold spray deposition system 200 can be for applying a ceramic coating to a process chamber component for semiconductor manufacturing or other electronics manufacturing via cold spray deposition. Cold spraying is a process in which powder particles are used to form a coating by means of ballistic impingement upon an article. Unlike traditional thermal spray processes, such as plasma spraying or flame spraying, which use heat to melt the coating material before it is deposited, cold spray deposition does not rely on the material reaching its melting point. Instead, cold spray coating relies on kinetic energy to achieve bonding and coating. In cold spray coating, solid particles of the coating material are accelerated to high velocities (typically above the material's critical particle velocity) using a carrier gas, such as nitrogen or helium. These high-velocity particles are directed towards a substrate, which can be made of various materials like metals, ceramics, plastics, or composites. Upon impact with the substrate, the high-energy particles deform and adhere to the surface, creating a dense and uniform coating layer.

[0039] In embodiments, powders used for the cold spray coating range in particle sizes from 5 to 100 microns (e.g., for metal particles) and are accelerated by injection into a high- velocity stream of gas. The particles are then accelerated by a main nozzle gas flow and impacted on the article. Upon impact, the solid particles deform and create a bond with the substrate. When solid particles are sprayed toward a substrate, there are various phenomena that are generally observed on the substrate surface in relation to the process parameters such as substrate hardness, ductility, velocity size, incident angle, etc. However, if the velocity of particles is sufficiently fast, they can be embedded in the surface through a deposition process. Cold spraying relies upon plastic deformation of the feedstock particles for adhesion to the substrate. In particular, mechanical interlocking of submicron powders with a local presence of agglomerates of powders may be achieved via cold spray coating.

[0040] In some embodiments, the cold spray deposition system 200 may include a deposition chamber 202, which can include a stage 204 for mounting a processing chamber component 206. In some embodiments, air pressure in the deposition chamber 202 may be reduced via a vacuum system 208. In some embodiments, a container 210 containing an 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 214for directing the agglomerated nanostructured powder 216 onto the processing chamber component 206 to form a coating.

[0041] The processing chamber component 206 can be a component used for semiconductor manufacturing. The component may be a component of an etch reactor, or a thermal reactor, of a semiconductor processing chamber, and so forth. Examples of components include a heater, an electrostatic chuck, a nozzle, a gas distribution plate, a showerhead, an electrostatic chuck component, a chamber wall, a liner, a liner kit, a gas line, a lid, a chamber lid, a nozzle, a single ring, a processing kit ring, a base, a shield, a plasma screen, a flow equalizer, a cooling base, a chamber viewport, a bellow, a faceplate, and a selectivity modulating device. The processing chamber component 206 can be formed of a material such as aluminum, silicon, quartz, bulk Yttria, bulk alumina, a bulk ceramic compound of Y4AI2O9 and a solid-solution of Y2Os-ZrO2, silicon carbide, or any other material used in a semiconductor manufacturing chamber component.

[0042] In some embodiments, the processing chamber component 206 may be mounted on the stage 204 in the deposition chamber 202 during deposition of a coating. In some embodiments, the processing chamber component 206 may be mounted on a stage 204 that is not within a deposition chamber 202, allowing for larger chamber components to be coated. The stage 204 can be moveable stage (e.g., motorized stage) that can be moved in one, two, or three dimensions, and / or rotated / tilted about in 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 agglomerated nanostructured powder 216 being propelled from the nozzle 214. For example, since application of the coating via a spray is a line of sight process, the stage 204 can be moved to coat different portions or sides of the processing chamber component 206. If the processing chamber component 206 has different sides that are to be coated or a complicated geometry, the stage 204 can adjust the position of the processing chamber component 206 with respect to the nozzle 214 so that the whole assembly can be coated. In other words, the nozzle 214 can be selectively aimed at certain portions of the processing chamber component 206 from various angles and orientations.

[0043] The gas container 212 holds pressurized carrier gas 218, such as Nitrogen, Argon, compressed air, or Helium. The pressurized carrier gas 218 travels under pressure from the gas container 212 to the chamber 210. As the pressurized carrier gas 218 travels from the chamber 210 to the nozzle 214, the carrier gas 218 propels some of the agglomerated nanostructured powder 216 towards the nozzle 214.

[0044] In one embodiment, the particles of the coating powder are nanosized, and the agglomerated nanostructured powder 216 has a certain fluidity. Further, rather than coating a single oxide such as Yttria (which may not be compatible for certain chemistries), the agglomerated nanostructured powder 216 can include mixtures of multiple oxides for forming a composite coating, according to one embodiment. For example, coating powder can be a composite ceramic material or a mixture of multiple metal oxides, metal fluorides and / or metal oxy-fluorides. Examples of materials for the agglomerated nanostructured powder 216 include Y2O3, YxOy, MgxOy, Mg2Os, ZrCE, AI2O3, YxZryOz, YvZrxOyFz, Y3AI5O12, Y4AI2O9, YF3, YxOyFz, E^Ch, ErjAhOn, ErFs, ErxOyFz, La2C>3, LU2O3, SC2O3, SCF3, ScxOyFz, Gd2C>3, GdFs, GdxOyFz, Sm2O3, or Dy2O3, or combinations thereof.

[0045] The agglomerated nanostructured powder may be formed of a target final stoichiometry in embodiments. Different materials in an agglomerated nanostructured powder may not change their stoichiometry on deposition onto an article 206 in embodiments. The coatings formed from these agglomerated nanostructured powders can have a low erosion rate and provide an improved on-wafer particle performance during use in a semiconductor manufacturing chamber. In embodiments, agglomerates of nanostructured powders may have a particle size range of 2-50 microns, 5-20 microns, or other size ranges.

[0046] With reference to the ceramic compound that may be the composition of the agglomerates (and of the ultimate coating that is formed), in one embodiment, the ceramic compound can include YOF in the range of 50-80 mol% and YF in the range of 20-50 mol%. IN some embodiments, TiCE powders are composed of nanometer primary particles. In some embodiments, the agglomerates may include pores. In some embodiments, the agglomerated nanostructured powders include agglomerate particles that are of a predetermined stoichiometry that is intended to correspond to the stoichiometry of the ceramic coating. In some embodiments, the agglomerates include at least one of TiCE or alumina. In some embodiments, the ceramic compound can include Y2O3 in a range of 50-75 mol%, ZrCE in a range of 10-30 mol% and AI2O3 in a range of 10-30 mol%. In another embodiment, the ceramic compound can include Y2O3 in a range of 40-100 mol%, ZrCE in a range of 0-60 mol% and AI2O3 in a range of 0-10 mol%. In another embodiment, the ceramic compound can include Y2O3 in a range of 40-60 mol%, ZrCE in a range of 30-50 mol% and AI2O3 in a range of 10-20 mol%. In another embodiment, the ceramic compound can include Y2O3 in a range of 40-50 mol%, ZrCE in a range of 20-40 mol% and AI2O3 in a range of 20-40 mol%. In another embodiment, the ceramic compound can include Y2O3 in a range of 70-90 mol%, ZrCE in a range of 0-20 mol% and AI2O3 in a range of 10-20 mol%. In another embodiment,the ceramic compound can include Y2O3 in a range of 60-80 mol%, ZrCh in a range of 0-10 mol% and AI2O3 in a range of 20-40 mol%. In another embodiment, the ceramic compound can include Y2O3 in a range of 40-60 mol%, ZrCh in a range of 0-20 mol% and AI2O3 in a range of 30-40 mol%. In other embodiments, other distributions may also be used for the ceramic compound.

[0047] As the carrier gas 218 propelling a suspension of the agglomerated nanostructured powder 216 enters the deposition chamber 202 from an opening in the nozzle 214, the agglomerated nanostructured powder 216 is propelled towards the processing chamber component 206. In one embodiment, the carrier gas 218 is pressurized such that the agglomerated nanostructured powder 216 is propelled towards the processing chamber component 206 at a rate in a range of about 10 mm / s to about 100 mm / s. In another embodiment, the rate may be in a range of about 20 mm / s to about 90 mm / s. In another embodiment, the rate may be in a range of about 30 mm / s to about 80 mm / s. In another embodiment, the rate may be in a range of about 40 mm / s to about 70 mm / s. In another embodiment, the rate may be in a 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 range of the distance may be about 5 mm to about 15 mm. In another embodiment, the range of the distance may be 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 20-700 °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 embodiments, the chamber component 206 is moved 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 embodiments, a low pressure cold spray is used, where the carrier gas may be nitrogen or air, for example. In some embodiments, a high pressure cold spray is performed using, for example, nitrogen or helium.

[0048] In one embodiment, the nozzle 214 is formed to be wear resistant. Due to the movement of the agglomerated nanostructured powder 216 through the nozzle 214 at a high velocity, the nozzle 214 can rapidly wear and degrade. However, the nozzle 214 can be formed in a shape and from a material such that wear is minimized or reduced. Upon impacting the processing chamber component 206, the particles of the agglomerated nanostructured powder 216 may fracture and deform (e.g., via plastic deformation) from the kinetic energy to produce an anchor layer that adheres to the processing chamber component206. As the application of the agglomerated nano structured powder 216 continues, the particles become a coating or film by bonding to themselves. The coating on the processing chamber component 206 continues to grow by continuous collision of the particles of the agglomerated nanostructured powder 216 on the processing chamber component 206. In other words, the particles are mechanically colliding with each other and the substrate at a high speed under a vacuum or atmospheric pressure to break into smaller pieces to form a dense layer, rather than undergoing a phase change. In some embodiments, the initial layer of the coating is achieved by plastic deformation of the substrate (e.g., particularly if the substrate is a ductile metallic substrate) when the particles are embedded into the substrate, optionally without any additional binding agent or calcination procedure. In some embodiments, the coating / substrate interface is relatively rough when the particle hits the substrate at a high speed. As a result, the powder particles may be embedded in the substrate. Roughness may cause mechanical entanglement for improved adhesion. In one embodiment, the particle crystal structure of the particles of the agglomerated nanostructured powder 216 remains after application to the processing chamber component 206.

[0049] In one embodiment, the formation of a barrier layer between a coating and a processing chamber component 206 prohibits the reaction of process chemistry that penetrates the coating with an underlying substrate. This may minimize the occurrence of delamination. The barrier layer may increase adhesion strength of the ceramic coating and may minimize peeling. In some embodiments, the porosity of the ceramic coating has a porosity of less than about 1%. In other the 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 of greater than 100 microns, 100-200 microns, or thicker.

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

[0051] In one embodiment, the aerosol deposition takes place in a chamber 202 of the cold spray deposition system 200 may be evacuated using the vacuum system 208, such that a vacuum is present in the deposition chamber 202. In some embodiments, the operating pressure of the deposition process may be in the range of about 2 MPa to about 6 MPa. In other embodiments, the operating pressure of the deposition process may be in the range of about 4 MPa to about 5 MPa. In other embodiments, the operating pressure of the deposition process may be in the range of about 3 MPa to about 5 MPa. Providing a vacuum in thedeposition chamber 202 can facilitate application of the coating for alternative deposition processes (e.g. aerosol deposition).

[0052] For example, in an aerosol deposition process, the agglomerated nanostructured powder 216 includes an aerosolized deposition feedstock instead. The aerosolized deposition feedstock may include particles of the same stoichiometry as the cold spray deposition process. The aerosolized deposition feedstock propelled from the nozzle encounters less resistance as the aerosolized particles travel to the processing chamber component 206 when the deposition chamber 202 is under a vacuum. Therefore, the aerosolized feedstock can impact the processing chamber component 206 at a higher rate of speed, which facilitates adherence to the processing chamber component 206 and formation of the coating.

[0053] FIG. 3 depicts a schematic of a cold spray ceramic deposition apparatus. As shown, a gas inlet 310 provides a carrier gas that is accelerated through a gas heater 320 towards an article 350. Further, a powder feeder 340 provides agglomerated nanostructured powders to a nozzle 330 such that the agglomerated powders are mixed with the flow of carrier gas provided by the gas inlet 310 from the gas heater 320.

[0054] As the flow of carrier gas is mixed with the agglomerated nanostructured powder, a suspension of the agglomerated nanostructured powder 345 in the gas forms. The suspension 345 of agglomerated nanostructured powder and carrier gas is propelled towards the processing chamber component 350.

[0055] An additional parameter that may be adjusted for the cold spray solid state deposition process is the process operating temperature during deposition. In one embodiment, the gas heater 320 heats the flow of carrier gas to an operating temperature. In some embodiments, the operating temperature is in the range of about 100 degrees C to about 800 degrees C. In other embodiments, the operating temperature is between 200 degrees C and 700 degrees C. In other embodiments, the operating temperature is between 300 degrees C and 600 degrees C. In other embodiments, the operating temperature is between 400 degrees C and 500 degrees C. The lower operating temperature can result in the deposited protective layer having fewer stress and thermal cracking.

[0056] In some embodiments, at least one surface of the processing 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] FIG. 4 illustrates an article 400 including a coating 420 on a processing chamber component 410 according to one embodiment. The coating 420 can be formed using a cold spray solid state deposition process as described in aspects of the present disclosure.

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

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

[0060] In embodiments, the agglomerated nanostructured powder may have the same stoichiometry as the ceramic coating. In some embodiments, the different materials in an agglomerated nanostructured powder may not change their stoichiometry during the deposition process. In some embodiments, the deposition method produces interlocking of submicron powders with a local presence of the 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, the cold spray deposition of agglomerated nanostructured powders increases the adhesion strength of the TiO2 coatings. In some embodiments, the lower temperatures of the cold spray deposition method reduce the residual stress of the ceramic coating.

[0061] FIG. 5 is a flow chart 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 process chamber component is provided. At block 520, at least one surface of the chamber component is cleaned with acetone prior to the deposition of the coating. At block 530, a ceramic coating is deposited onto at least one surface of a chamber component for a process chamber using a cold spray deposition process. The cold spray deposition process deposits particles of a ceramic onto the at least one surface to form the ceramic coating without causing the ceramic particles to undergo a phase change. The cold spray deposition process may be performed using any of the parameters described above. In embodiments, the ceramic coating is a fluoride coating (e.g., YF3) that does not include oxygen (or that includes a barely measurable amount of oxygen). For materials such a fluorides that are highly reactive, deposition techniques thatcause a phase change during deposition (e.g., such as plasma spraying) are generally not capable of forming coatings that lack oxygen due to the reactive nature of the material (e.g., of fluorine). Such processes cause at least some oxidation, which results in an oxy -fluoride coating, for example, when a fluoride material may be the goal.

[0062] In embodiments, the ceramic coating is a protective layer that is a hermetic coating that has the same microstructure as the processing chamber component provided. In embodiments, the conformal protective layer includes stacked agglomerated nanostructured ceramic powders.

[0063] Various techniques may be used to form agglomerated nanostructured powders used for cold spray deposition in embodiments.

[0064] FIG. 6 is a flow chart for a method 600 of forming agglomerated nanostructured particles for cold spray solid-state deposition, according to embodiments of the present disclosure. At block 610, a solution of nitrate or citrate salt of a metal ion is provided to an anodized aluminum oxide membrane. At block 620 of method 600, the solution is heat treated to nucleate metal oxide particles within the pores of the membrane. At block 630, agglomerated nanostructured particles are allowed to nucleate from the solution. In some embodiments, the agglomerated nanostructured powders have an average size of about 5 pm to about 40 pm. In other embodiments, the agglomerated nanostructured powders have an average size of about 10 pm to about 20 pm. In some embodiments, the agglomeration process may include the addition of an inorganic salt.

[0065] FIG. 7 is a flow chart for a method 700 of forming agglomerated nanostructured particles for cold spray solid-state deposition, according to embodiments of the present disclosure. At block 710, a solution of nitrate or citrate salt of a metal ion is provided to a stirrer. These salts may facilitate agglomeration. At block 720 of method 700, the temperature of the stirred solution is reduced.

[0066] At block 730, an oxidizing agent is added to the stirred solution. At block 740, agglomerated nanostructured particles are allowed to nucleate from the solution. In some embodiments, the agglomerated nanostructured powders have an average size of about 5 pm to about 40 pm. In other embodiments, the agglomerated nanostructured powders have an average size of about 10 pm to about 20 pm.

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

[0068] Hydrothermal approaches may be used to agglomerate nanoparticles for microagglomerate powder in embodiments. A hydrothermal treatment may be performed bysoaking the powder (e.g., of Y2O3 nanoparticles) in distilled water with addition of ammonium sulfate ((NEU^SOf). The solution may be stirred in an oil bath to keep a target temperature (e.g., at 150 °C) for a target amount of time (e.g., for 4 hours). The particle size, for example, may have an average size of 30 nm, which may be agglomerated to 2 pm particle agglomerates driven by surface energy. After adding inorganic sulfate (NHf SC , the particles may agglomerate into a near spherical structure like a snowball. Increasing the addition of (NEU^SCU, the agglomeration of the particles may become compact, and the morphology of the particle may become rougher, with small particles adsorbed at the surface of the big, agglomerated particles.

[0069] Reference throughout this specification to “one embodiment” or “an embodiment” means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, the appearances of the phrase “in one embodiment” or “in an embodiment” in various places throughout this specification are not necessarily all referring to the same embodiment. In addition, the term “or” is intended to mean an inclusive “or” rather than an exclusive “or.” When the term “about” or “approximately” is used herein, this is intended to mean that the nominal value presented is precise within ± 10%.

[0070] Although the operations of the methods herein are shown and described in a particular order, the order of operations of each method may be altered so that certain operations may be performed in an inverse order so that certain operations may be performed, at least in part, concurrently with other operations. In another embodiment, instructions or sub-operations of distinct operations may be in an intermittent and / or alternating manner.

[0071] The preceding description sets forth numerous specific details such as examples of specific systems, components, methods, and so forth in order to provide a good understanding of several embodiments of the present disclosure. It will be apparent to one skilled in the art, however, that at least some embodiments of the present disclosure may be practiced without these specific details. In other instances, well-known components or methods are not described in detail or are presented in simple block diagram format in order to avoid unnecessarily obscuring the present disclosure. Thus, the specific details set forth are merely exemplary. Particular implementations may vary from these exemplary details and still be contemplated to be within the scope of the present disclosure.

[0072] It is understood that the above description is intended to be illustrative, and not restrictive. Many other embodiments will be apparent to those of skill in the art upon reading and understanding the above description. The scope of the disclosure should, therefore, bedetermined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled.

Claims

CLAIMSWhat is claimed is:

1. A method comprising: depositing a ceramic coating onto at least one surface of a chamber component for a process chamber using a cold spray deposition process, wherein the cold spray deposition process propels nanoparticles of a ceramic and deposits the agglomerated particles of the ceramic onto the at least one surface to form the ceramic coating without causing the particles to undergo a phase change.

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

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

4. The method of claim 1, wherein the ceramic coating has a thickness of at least 100 microns 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 comprising agglomerates of a predetermined stoichiometry corresponding to a stoichiometry of the ceramic coating.

6. The method of claim 5, wherein the agglomerates are sintered agglomerates of nanoparticles.

7. The method of claim 5, wherein the agglomerates comprise at least one of TiCh or alumina.

8. The method of claim 5, wherein the agglomerates further comprise at least one of Y2O3, YxOy, MgxOy, ZrO2, AI2O3, YxZryOz, YvZrxOyFz, Y3A150I2, Y4AI2O9, YF3, YxOyFz, Er2O3, ErjAFOn, ErFs, ErxOyFz, La2O3, LU2O3, SC2O3, ScFs, ScxOyFz, Gd2O3, GdFs, GdxOyFz, Sm2O3, or Dy2O3.

9. The method of claim 1, wherein the deposition further comprises agglomerates of the ceramic particles with a process gas.

10. The method of claim 9, wherein the process 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 300-600 °C.

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

13. The method of claim 1, wherein agglomerate powders are prepared using a hydrothermal process.

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

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

16. An article comprising; a component for use in a manufacturing chamber; and a conformal protective layer on at least one surface of the component, wherein a porosity of the conformal protective layer is less than 1%, and wherein the conformal protective layer has a thickness of 100-200 pm.

17. The article of claim 16, wherein the conformal protective layer comprises at least one of Y2O3, YxOy, MgxOy, ZrO2, AI2O3, YxZryOz, YvZrxOyFz, Y3A150I2, Y4AI2O9, YF3, YxOyFz, Er2O3, ErjAFOn, ErFs, ErxOyFz, La2O3, LU2O3, SC2O3, ScFs, ScxOyFz, Gd2O3, GdFs, GdxOyFz, Sm2O3, or Dy2O3.

18. The article of claim 16, wherein the article is selected from a group consisting of: a heater, an electrostatic chuck, a nozzle, a gas distribution plate, a showerhead, an electrostaticchuck component, a chamber wall, a liner, a liner kit, a gas line, a lid, a chamber lid, a nozzle, a single ring, a processing kit ring, a base, a shield, a plasma screen, a flow equalizer, a cooling base, a chamber viewport, a bellow, a faceplate, and a selectivity modulating device.

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

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

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