Development of high-barrier nickel oxide (BNiO) coatings for process chamber components

Abstract

Described herein is a chamber component that includes a metal layer that includes nickel and a barrier layer of nickel oxide on the metal layer. The nickel oxide barrier layer may be formed by treating the chamber component with an oxidizing agent that includes hydrofluoric acid and / or nitric acid.

Description

Technical Field

[0001] Embodiments of the present disclosure generally relate to corrosion-resistant metal oxide-coated chamber components, as well as methods of forming and using such coated chamber components.

Background Art

[0002] In the semiconductor industry, devices are fabricated by several manufacturing processes that produce structures with continuously shrinking sizes. As the device geometries shrink, it becomes much more difficult to control the process uniformity and reproducibility of the devices.

[0003] Various semiconductor manufacturing processes use high temperatures, high-energy plasmas (such as remote and direct fluorine plasmas like NF3, CF4, etc.), mixtures of corrosive gases, corrosive cleaning chemicals (such as hydrofluoric acid), and combinations thereof. Under these extreme conditions, reactions occur between the materials of the components within the process chamber and the plasma gas or corrosive gas, resulting in metal fluorides, particles, other trace metal contaminants, and high vapor pressure gases (such as AlF , ,

[0004] , x ) that can be formed. Such gases can easily sublime and deposit on other components within the chamber. During subsequent process steps, the deposited material can separate from other components such as particles and fall onto the wafer, potentially causing defects. Additional problems resulting from such reactions include deposition rate drift, etching rate drift, impaired film uniformity, and impaired etching uniformity. To limit sublimation and / or the formation of particles and metal contaminants on chamber components within the chamber, it is beneficial to reduce these defects with a stable non-reactive coating on the chamber components.

[0004] Therefore, to mitigate these defects, some semiconductor processing chamber components (e.g., liners, doors, lids, showerheads, etc.) include electroless nickel plated (ENP) surfaces. However, ENP surfaces are known to develop a fluorine-containing layer after use in a fluorine-based atmosphere and at higher temperatures above approximately 150°C. Without being limited to theory, the fluorine-containing layer develops due to contamination during use and can therefore be considered a contaminant layer. Furthermore, after processing hundreds of wafers, the fluorine-containing layer is known to shorten the lifespan of one or more components of the process chamber and the mean wafers between cleaning (MWBC) metric. [Overview of the project]

[0005] In some embodiments of this disclosure, a chamber component for a processing chamber may include a body, a metal plating on at least one surface of the body, wherein the metal plating contains nickel, and a barrier layer on the metal plating. In some embodiments, the barrier layer may contain nickel oxide. In some embodiments, the metal plating may contain nickel and phosphorus. In some embodiments, the metal plating may contain nickel but not phosphorus. In some embodiments, the body may include aluminum, an aluminum alloy, aluminum nitride, alumina, or a combination thereof. In some embodiments, the metal plating has a thickness of about 20 microns to about 75 microns, and the barrier layer has a thickness of about 2 nm to about 50 nm. In some embodiments, the barrier layer has an average surface roughness (Ra) of about 2 microinches to about 60 microinches. In some embodiments, the chamber component may be a showerhead for a process chamber.

[0006] In other embodiments of the present disclosure, a method for protecting a chamber component includes forming a metal plating on the body of the chamber component, wherein the metal plating may contain nickel, and contacting the metal plating with an oxidizing agent to form a barrier layer on the metal plating, wherein the barrier layer may contain nickel oxide. In some embodiments, the oxidizing agent may include at least one of hydrofluoric acid, oxalic acid, or nitric acid. In some embodiments, the barrier layer may have a thickness of about 2 μm to about 60 μm. In some embodiments, forming the metal plating may include performing electroless metal plating, wherein the metal plating further contains phosphorus. In some embodiments, the body may include an aluminum alloy, aluminum nitride, alumina, or a combination thereof. In some embodiments, the method may include removing native oxides from the metal plating before forming the barrier layer. In some embodiments, the method may include forming a nickel fluoride (NiF2) or nickel oxyfluoride layer on the metal plating by contacting the metal plating with ammonium fluoride after forming the metal plating. In some embodiments, the method may also include placing the chamber components in an acid bath containing 5-25% hydrofluoric acid and 75-95% water to bring the metal plating into contact with an oxidizing agent, then placing the chamber components in a deionizing water bath, then placing the chamber components in the acid bath, and then placing the chamber in a deionizing water bath.

[0007] In another embodiment of the present disclosure, a method for repairing a used chamber component may include removing a contamination layer from a metal plating on the used chamber component using a first acidic solution, wherein the metal plating contains nickel; and then contacting the metal plating with an oxidizing agent to form a barrier layer on the metal plating, wherein the barrier layer contains nickel oxide. In some embodiments, the contamination layer may contain nickel fluoride. In some embodiments, removing the contamination layer may include placing the used chamber component in a first acid bath, then rinsing the used chamber component with deionized water, then drying the used chamber component, then placing the used chamber component in a second acid bath, then rinsing the used chamber component with deionized water, and then drying the used chamber component. In some embodiments, the oxidizing agent may include at least one of hydrofluoric acid or nitric acid. In some embodiments, the barrier layer may have a thickness of about 2 μm to about 60 μm.

[0008] The present invention is illustrated, not limited to, examples in the figures of the accompanying drawings, where similar reference numerals indicate similar elements. Note that different references to “Embodiments” or “One Embodiment” in this disclosure do not necessarily refer to the same embodiment, but rather mean at least one. [Brief explanation of the drawing]

[0009] [Figure 1A] This figure shows a cross-sectional view of one embodiment of a processing chamber. [Figure 1B] This figure shows a cross-sectional view of one embodiment of a shower head for a processing chamber. [Figure 2] This figure shows one embodiment of a shower head, specifically a bottom view. [Figure 3A] This figure shows a method for forming a high-level barrier oxide layer according to one embodiment. [Figure 3B]This figure shows another method for repairing and forming a high-barrier oxide layer according to another embodiment. [Figure 4] This is a diagram illustrating an exemplary architecture of a manufacturing system. [Figure 5] This is a flowchart illustrating a method for forming a high-level barrier oxide layer according to one embodiment. [Figure 6] This is a flowchart illustrating a method for repairing and forming a high-level barrier layer according to another embodiment. [Figure 7] This flowchart illustrates a method, according to one embodiment, for forming a high-barrier layer having a nickel fluoride (NiF2) or nickel oxyfluoride (NiOF) layer on a metal-plated or metal-coated chamber component. [Modes for carrying out the invention]

[0010] Embodiments disclosed herein describe coated articles, coated chamber components, methods for coating articles and chamber components, methods for reducing or eliminating particles from a semiconductor processing chamber, and methods for using coated articles and chamber components, and processing chambers containing coated chamber components. A metal layer (which may be, for example, a metal coating or metal plating) having a barrier layer is included to reduce reactions between the constituent materials and reactive chemicals and / or plasma that form metal fluorides, particles, other trace metallic contaminants and / or high vapor pressure gases. The metal layer may be a nickel-containing layer (for example, a pure nickel layer, or a layer having nickel as the main component and further containing other materials such as phosphorus and / or vanadium). The barrier layer may be a nickel oxide layer formed under controlled conditions. The barrier layer may be added to new chamber components to improve the service life of the chamber components and / or to reduce or eliminate the accumulation of contaminant layers on the chamber components. Furthermore, to improve the lifespan of coated articles, or coated chamber parts (which may be new or used chamber parts), they may be treated to remove the contaminating layer and to add a barrier layer on top of the metal layer on the chamber part.

[0011] Adding oxides and / or fluorides to a metal layer, it is known that there is an interaction between fluorine and the metal layer on the chamber component (e.g., ENP containing nickel). Native oxides naturally occur on the metal layer due to exposure to air. However, native oxides have undesirable properties. In particular, native oxides interact with process gases (e.g., fluorine) to form a contamination layer. The interaction of native oxides with fluorine results in discoloration and the formation of a black film (contamination layer) on the metal coating, which produces particles that can contaminate the processed substrate. If a black film / contamination layer is present on a chamber component such as a showerhead, there may be a decrease in yield for substrates processed by a process chamber containing a showerhead with a contamination layer.

[0012] Furthermore, if a black film / contamination layer forms on the chamber components during use, the chamber components will be removed and replaced.

[0013] Therefore, embodiments improve the surface of chamber components, such as showerheads, to prevent the formation of a black film / contamination layer on the metal layer of the chamber component. It would be advantageous to have a protective barrier layer to prevent the chemical decomposition of the surface metal layer and the formation of a black film / contamination layer. Such chamber components having a protective barrier layer may also degrade and / or contaminate more slowly than chamber components without a barrier layer, thereby resulting in chamber components with a barrier layer on the metal layer having a higher average inter-cleanse wafer than chamber components with a metal layer but without a barrier layer. The average inter-cleanse wafer represents the average number of wafers processed between each cleans of the chamber component. Such an increased average inter-cleanse wafer may be particularly noticeable for chamber components used in chambers where the process is run at higher temperatures, such as about 200°C or above.

[0014] Embodiments disclosed herein include a processing chamber (e.g., a semiconductor processing chamber) comprising a chamber component for a processing chamber and / or such a chamber component, the chamber component comprising the chamber component and a metallic layer (e.g., metal plating or metallic coating) on ​​at least one surface of the chamber component. The metallic layer may, in embodiments, include a high barrier layer.

[0015] In some embodiments, the chamber component may include a metal layer on the surface of the substrate. The chamber component or part thereof may consist of, but are not limited to, one or more of the following metals, e.g., aluminum, stainless steel and / or titanium, and / or ceramics, e.g., alumina, silica and / or aluminum nitride, and / or combinations thereof. The metal layer may be an electroless metal plating containing nickel or an electrolytic metal plating containing nickel.

[0016] In some embodiments, chamber components may be plated using an electroless plating process to form an electroless metal plating on one or more surfaces of the chamber components. In embodiments, the electroless metal plating may be nickel-phosphorus plating. The electroless plating process can directly form a metal plating on the surface of the chamber components. In some embodiments, chamber components may be plated using an electrolytic metal plating process. For example, an electrolytic plating process may form a layer containing nickel, silver, and / or gold. In some embodiments, one or more surfaces of the chamber components may be coated using a sputtering process, such as a sputtering process that sputters a nickel-containing coating onto one or more surfaces of the chamber components. The nickel-containing coating may, for example, contain 98-99 atomic percent nickel and 1-2 atomic percent vanadium.

[0017] In some embodiments, when chamber components are coated by an electroless plating process, the chamber components are placed in a bath containing nickel and phosphorus. The bath may contain about 84% nickel and about 16% phosphorus, about 86% nickel and 14% phosphorus, about 88% nickel and about 12% phosphorus, about 90% nickel and about 10% phosphorus, about 92% nickel and about 8% phosphorus, about 94% nickel and about 6% phosphorus, and about 96% nickel and about 4% phosphorus. For example, the bath may contain about 84-96% nickel and about 4-16% phosphorus.

[0018] In some embodiments, when chamber components are plated by an electrolytic metal plating process, the coating does not contain phosphorus. For example, the plating may be 100% nickel. In some embodiments, chamber components are coated with sputtered nickel. Sputtered nickel may contain nickel and vanadium, as understood by those skilled in the art. Vanadium may be present in the sputtered nickel at a concentration of about 1% to about 2%.

[0019] In embodiments, when the chamber component includes a metal layer that is electroless nickel plating or electrolytic Ni plating, the layer can have a thickness of from about 20 microns to about 75 microns, from about 25 microns to about 70 microns, from about 30 microns to 60 microns, or from about 35 microns to about 50 microns.

[0020] In some embodiments, the metal layer can have a hardness of from about 450 HV to about 500 HV. The roughness of the metal layer can be less than 50 μinch in embodiments.

[0021] The thickness of the metal layer formed by electroless plating can be targeted based on the amount of time the chamber component is in the bath. The chamber component can be in the bath for from about 1 minute to about 3 minutes to form a metal layer having a target thickness.

[0022] In some embodiments, a contamination layer can be found on the metal layer. The contamination layer can include a combination of nickel, fluorine, and / or oxygen. In embodiments, the metal layer is a nickel layer that slowly fluorinates over time upon exposure to a fluorine-rich chemical. For example, a contamination layer of nickel fluoride and / or nickel oxyfluoride can be formed on the surface of the metal layer. The contamination layer can react with the process gas differently than the metal layer and can cause a slight change in the process chemistry. Further, or alternatively, the contamination layer can flake off the chamber component and / or cause particle contamination on the substrate being processed in the process chamber in which the chamber component is installed. As a result, periodic maintenance can be performed on the chamber component to remove those chamber components that include the contamination layer and replace the removed chamber components with new chamber components that do not have the contamination layer.

[0023] In embodiments, the chamber component includes a barrier layer containing nickel oxide on a metal layer (e.g., a nickel layer). In embodiments, the formation of the barrier layer (e.g., a nickel oxide barrier layer) on the metal layer protects the metal layer from attack by process gases, in particular from attack by fluorine-containing plasma and other fluorine-containing chemicals. The barrier layer is therefore sometimes referred to as a protective layer. The nickel oxide barrier layer may be formed using an oxidation process, which may involve immersing the chamber component (or the portion of the chamber component that should have the nickel oxide barrier layer) in a bath containing an oxidizing agent (e.g., a bath containing hydrofluoric acid and / or nitric acid along with water).

[0024] In some embodiments, the chamber component includes generating a nickel fluoride (NiF2) or nickel oxyfluoride (NiOF) layer after removing the contamination layer and before forming the barrier layer. The nickel fluoride or nickel oxyfluoride layer can be generated by placing the metal-plated chamber component in a bath containing an ammonium fluoride (NH4F) solution. The ammonium fluoride solution may have a concentration of about 0.5 M to about 3 M. The metal-plated chamber component remains in the bath at a temperature of about 35 to about 45°C for about 5 to about 60 minutes to form the nickel fluoride or nickel oxyfluoride layer. If a nickel fluoride layer is formed, Ni is present in an amount of about 60% by weight and F is present in an amount of about 40% by weight. If a nickel oxyfluoride layer is formed, Ni is present in an amount of about 62% by weight, F is present in an amount of about 20% by weight and O is present in an amount of about 17% by weight. After this nickel fluoride (NiF2) or nickel oxyfluoride (NiOF) layer is formed, a nickel oxide barrier layer may then be formed using the oxidation process described herein.

[0025] Experiments have shown that the use of a nickel oxide barrier layer over the nickel layer on chamber components increases the service life of the chamber components by a factor of 10. Therefore, preventive maintenance can be reduced by a factor of 2 to 10 in embodiments compared to the number and / or frequency of preventive maintenance performed to inspect and / or replace chamber components with exposed nickel layers.

[0026] Some embodiments described herein with respect to showerheads are particularly useful for coating chamber components having both high aspect ratio features and areas directly exposed to plasma impact. However, the barrier layers described herein can also be usefully used on many other chamber components having a metal layer exposed to plasma, such as chamber components for plasma etchers or other processing chambers (also known as plasma etch reactors), including walls, liners, bases, rings, viewports, lids, nozzles, substrate holding frames, electrostatic chucks (ESCs), faceplates, selectivity adjusters (SMDs), plasma sources, pedestals, etc.

[0027] Furthermore, embodiments relating to plated or coated chamber components and other articles that may result in reduced particulate contamination when used in process chambers for plasma-rich processes are described herein. However, it should be understood that the plated or coated articles described herein may also provide reduced particulate contamination when used in process chambers for other processes, such as non-plasma etchers, non-plasma purifiers, chemical vapor deposition (CVD) chambers, and physical vapor deposition (PVD) chambers.

[0028] Referring next to the drawings, Figure 1A is a cross-sectional view of a processing chamber 100 (e.g., a semiconductor processing chamber) having one or more chamber components including a metal layer and a nickel oxide-containing barrier layer on the metal layer, according to an embodiment of the present disclosure. The processing chamber 100 may be used for processes in which a corrosive plasma environment and / or corrosive chemicals are introduced therein. For example, the processing chamber 100 may be a chamber for a plasma etch reactor (also known as a plasma etcher), a plasma purifier, an ALD chamber for performing plasma-enhanced atomic layer deposition (ALD), or other deposition chambers. Examples of chamber components that may include a metal layer and a barrier layer on the metal layer include a substrate support assembly 148, an electrostatic chuck (ESC), a ring (e.g., a process kit ring or a single ring), a chamber wall, a base, a shower head 130, a gas distribution plate, a liner, a liner kit, a shield, a plasma screen, a flow equalizer, a cooling base, a chamber viewport, a chamber lid, a nozzle, a process kit ring, and the like.

[0029] In one embodiment, the metal layer is a nickel-containing layer (e.g., 100% nickel, or nickel combined with one or more additional materials such as phosphorus and / or vanadium). In one embodiment, the barrier layer is a nickel oxide-containing layer (e.g., 100% nickel oxide, or nickel oxide with one or more additional materials such as phosphorus and / or vanadium). The metal layer and the barrier layer may be conformal thin films.

[0030] In one embodiment, the processing chamber 100 includes a chamber body 102 and a shower head 130 surrounding an internal volume 106. The shower head 130 may or may not include a gas distribution plate. For example, the shower head may be a multi-piece shower head including a shower head base and a shower head gas distribution plate joined to the shower head base. Alternatively, the shower head 130 may be replaced in some embodiments by a lid and nozzles, or in other embodiments by a plurality of pie-shaped shower head compartments and a plasma generating unit. The chamber body 102 may be made of aluminum, stainless steel or other suitable material. The chamber body 102 generally includes side walls 108 and a bottom 110. The shower head 130 (or lid and / or nozzles), the side walls 108 and / or bottom 110 may all include a multilayer plasma-resistant coating.

[0031] To protect the chamber body 102, an outer liner 116 may be provided adjacent to the side wall 108. The outer liner 116 may be a halogen-containing gas-resistant material such as Al2O3 or Y2O3. In some embodiments, the outer liner 116 may be coated with a multilayer plasma-resistant ceramic coating.

[0032] An exhaust port 126 may be defined within the chamber body 102, and the internal volume 106 may be connected to a pump system 128. The pump system 128 may include one or more pumps and throttle valves used to vacuum the internal volume 106 of the processing chamber 100 and regulate its pressure.

[0033] The shower head 130 may be supported on the side wall 108 of the chamber body 102 and / or on the upper portion of the chamber body. The shower head 130 (or lid) may be open 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 supply process gases and / or cleaning gases to the internal volume 106 through the shower head 130 or through the lid and nozzle. The shower head 130 includes a plurality of gas supply holes 132 throughout the shower head 130. The shower head 130 may be or include aluminum, anodized aluminum, an aluminum alloy (e.g., Al6061), or anodized aluminum alloy. In some embodiments, the shower head includes a gas distribution plate (GDP) bonded to the shower head. The GDP may be, for example, Si or SiC. The GDP may further include a plurality of holes corresponding to the holes in the shower head.

[0034] Figure 1B shows an enlarged view of a portion of the shower head 130 in Figure 1A. Referring to Figure 1B, in embodiments, the shower head 130 is coated with a metal layer 150 and a barrier layer 152. In particular, in some embodiments, the surface of the shower head and the walls of the holes 132 in the shower head are coated with a thin conformal metal layer 150. Furthermore, the back surface of the shower head 130 and the outer walls of the shower head may also be coated with the conformal metal layer 150. Non-line-of-sight deposition techniques such as ALD or plating (e.g., electroplating or electroless plating) may be used to deposit or form the metal layer 150 on the surface of the shower head 130 and on the walls of the holes 132 in the shower head 130. Alternatively, a line-of-sight deposition technique such as sputtering may be used to form the metal layer. In embodiments, the metal layer 150 may be nickel, phosphorus-doped nickel, or vanadium-doped nickel.

[0035] The barrier layer 152 covers the metal layer 150 over some or all areas of the surface of the showerhead 130. The barrier layer 152 may be formed using an oxidation process, which may be a dry oxidation process or a wet oxidation process (for example, by immersing the showerhead 130 in a bath containing an oxidizing agent such as hydrofluoric acid or nitric acid). The barrier layer 152 may cover the metal layer on all surfaces of the chamber components, including on the inner walls of the holes in the showerhead 130. The barrier layer may be a grown layer and, in embodiments, may be conformal and uniform. A uniform barrier layer may, in embodiments, have a thickness difference of less than about 10% across the surface of the showerhead.

[0036] Examples of process gases that may be used to process the substrate in the processing chamber 100 include, among other things, halogen-containing gases such as C2F6, SF6, SiCl4, HBr, NF3, CF4, CHF3, CH2F3, F, Cl2, CCl4, BCl3, and SiF4, as well as other gases such as O2 or N2O. Examples of carrier gases include N2, He, Ar, and other gases (e.g., non-reactive gases) that are inert to the process gas. Fluorine-based gases may cause fluoride deposits to accumulate on the holes of a standard showerhead and / or form a contaminant layer on the holes of the showerhead. However, the holes 132 of the showerhead 130 may be resistant to such fluoride accumulation due to the barrier layer 152.

[0037] Referring again to Figure 1A, a substrate support assembly 148 is located below the showerhead 130 in the internal volume 106 of the processing chamber 100. The substrate support assembly 148 holds the substrate 144 (e.g., a wafer) during processing. The substrate support assembly 148 may include an electrostatic chuck for securing the substrate 144 during processing, a metal cooling plate bonded to the electrostatic chuck, and / or one or more additional components. An inner liner may cover the periphery of the substrate support assembly 148. The inner liner may be a halogen-containing gas resist material such as Al2O3 or Y2O3. The substrate support assembly, parts of the substrate support assembly, and / or the inner liner may be coated with a metal layer and a barrier layer in some embodiments.

[0038] Figure 2 shows one embodiment of a bottom view of the showerhead 200. The showerhead 200 may have a series of concentrically arranged gas conduits 204 (also called holes) that evenly distribute plasma gas directly onto the substrate or wafer to be etched or processed. The showerhead is shown here as having approximately 1100 gas conduits 204 arranged in an evenly distributed concentric ring for even distribution of gas. In another embodiment, the gas conduits 204 may be configured in an alternative geometric configuration on the bottom surface 205 of the showerhead (or on the bottom surface of the GDP coupled to the showerhead). For example, the showerhead may have a rectangular or square configuration with rows and columns of gas conduits 204. It should be understood that other shapes (e.g., triangles, pentagons, etc.) may be implemented and coated with ceramic coatings (e.g., HPM coatings) as described above. Depending on the type of reactor and / or process used, the showerhead 200 may have a large number of gas conduits 204 as shown, or a small number of gas conduits as appropriate.

[0039] In one embodiment, some or all of the gas conduits 204 do not have branches (for example, each gas conduit may have a single inlet point and a single outlet point). Furthermore, the gas conduits may have varying lengths and orientation angles. Gas may be supplied to the gas conduits 204 via one or more gas supply nozzles. Some gas conduits 204 may receive gas earlier than others (for example, by being closer to the gas supply nozzles). However, the gas conduits 204 may be configured to supply gas to the substrate below the showerhead almost simultaneously based on varying the orientation angle, diameter, and / or length of the gas conduits 204, or by using additional flow equalizers. For example, a gas conduit 204 that receives gas first may be longer and / or have a larger angle (for example, an angle greater than 90 degrees) than a conduit that receives gas later.

[0040] A schematic diagram 300 of oxidizing a metal-plated coated chamber component is shown, as can be seen in Figure 3A. In Figure 3A, the metal-plated chamber component comprises a nickel layer 301 and an exposed aluminum body 302 of the chamber component, with the nickel layer 301 on the surface of the exposed aluminum body 302. The metal-plated chamber component undergoes an oxidation process 305 according to the present disclosure. After oxidation, the metal-plated chamber component includes a high-density barrier layer 303 of nickel oxide on the surface of the nickel layer 301. The NiO barrier layer 303 can prevent discoloration of the metal layer. The barrier layer 303 can also prevent the chamber component from becoming a source of particles on the substrate being processed. The NiO barrier layer 303 can also suppress the reaction of fluorine with nickel in the nickel layer 301 to prevent the formation of a discolored / contaminated layer.

[0041] Furthermore, the barrier layer 303 can prevent the formation of native oxides on the nickel layer 1.

[0042] In some embodiments, the chamber component may be a used chamber component that has been used to perform one or more processes on a substrate, which exposed the substrate to a fluorine-rich environment. The chamber component may not have been coated with a barrier layer before use. Therefore, the chamber component may have a contamination layer on top of the metal layer 302. In some embodiments, the chamber component may be repaired by removing the contamination layer to expose the metal layer, and then forming a barrier layer on the metal layer. A schematic of such an embodiment is shown in schematic figure 350 of Figure 3B.

[0043] In Figure 3B, the chamber component includes an aluminum body 302 having a metal layer 301 disposed thereon, and a contamination layer 310 on the metal layer 301. The chamber component may undergo a cleaning process 315 to remove the contamination layer 310 from the metal layer 301. The chamber component having the cleaned metal layer 301 may then be treated using an oxidation process 305 to form a barrier layer 303, as described in more detail in this disclosure. After cleaning and oxidation, the contamination layer 310 is removed, and a high-density nickel oxide barrier layer 303 is present on the metal layer 301.

[0044] Figure 4 shows an exemplary architecture of the manufacturing system 400. The manufacturing system 400 may be a manufacturing system for applying plating and / or coating to articles, such as chamber parts. In one embodiment, the manufacturing system 400 includes a manufacturing machine 401 (e.g., processing equipment) connected to an automated equipment layer 415. The manufacturing machine may include a polisher 402, one or more wet cleaners 403, a plating system 404, a sputtering system 405, an oxidation system 406, and / or other machines. The manufacturing system 400 may further include one or more computing devices 420 connected to the automated equipment layer 415. In alternative embodiments, the manufacturing system 400 may include more or fewer components. For example, the manufacturing system 400 may include a manufacturing machine 401 that can be operated manually (e.g., offline) without an automated equipment layer 415 or computing devices 420.

[0045] A polisher 402 is a machine configured to polish or smooth the surface of an article, such as chamber components for a processing chamber. A polisher 402 may be, for example, a chemical mechanical planarization (CMP) device or an abrasive polisher. For example, an electric abrasive pad may be used to smooth the surface of an article. A sander may rotate or vibrate an abrasive pad while it is pressed against the surface of an article. The roughness achieved by the abrasive pad may depend on the pressure applied, the vibration or rotation rate and / or the roughness of the abrasive pad.

[0046] The wet scrubber 403 is a cleaning apparatus that cleans articles (e.g., articles) using a wet cleaning process. The wet scrubber 403 includes a wet bath filled with liquid, and a substrate is immersed in the wet bath to clean the substrate. The wet scrubber 403 may use ultrasound to agitate the wet bath during cleaning in order to improve the cleaning effect. This is referred to herein as sonicating the wet bath.

[0047] In some embodiments, the wet cleaner 403 includes a first wet cleaner containing deionized (DI) water and a second wet cleaner containing an acidic solution. The acidic solution may, in embodiments, be a hydrofluoric acid (HF) solution, a hydrochloric acid (HCl) solution, a nitric acid (HNO3) solution, or a combination thereof. The acidic solution may remove surface contaminants from an article and / or oxides from the surface of an article. Cleaning an article having a metal layer with an acidic solution before forming a barrier layer on the metal layer may improve the quality of the barrier layer formed on the metal layer. In one embodiment, an acidic solution containing about 5-15% by volume of HF is used to clean a chamber component having a nickel layer. In one embodiment, an acidic solution containing about 5-15% by volume of HNO3 is used to clean an article having a nickel layer.

[0048] The wet cleaner 403 can clean the article in multiple stages during processing. For example, the wet cleaner 403 can clean the article after the substrate has been polished, before plating (e.g., electroplating) is performed, or before a barrier layer is formed on the metal plating.

[0049] In other embodiments, alternative types of purifiers, such as dry purifiers, may be used to clean articles. Dry purifiers can clean articles by applying heat, gas, plasma, etc.

[0050] The plating system 404 is a system that performs electroplating (for example, of Ni) or electroless plating (for example, of Ni). The plating system 404 may be an electroplating system in which an electric current is applied to reduce the dissolved metal cations so that they form a thin, adhesive metal coating on an article (for example, on the surface of a chamber part, such as an aluminum chamber part). In particular, the article to be plated may be the cathode of the circuit, and the metal donor may be the anode of the circuit. The article and the metal donor may be immersed in an electrolyte containing one or more dissolved metal salts and / or other ions that increase the conductivity of the electrolyte. The metal from the metal donor then plates the surface of the article.

[0051] Another type of plating system that can be used is an electroless plating system. Also known as chemical plating or autocatalytic plating, electroless plating is a non-galvanic plating method involving several simultaneous reactions in an aqueous solution, where these reactions occur without the use of external power. The reaction is achieved when hydrogen is released and oxidized by a reducing agent, usually sodium hypophosphate or thiourea, thereby creating a negative charge on the surface of the part.

[0052] The equipment automation layer 415 may interconnect some or all of the manufacturing machines 401 with the computing device 420, other manufacturing machines, and measurement tools and / or other devices. The equipment automation layer 415 may include a network (e.g., a location area network (LAN)), routers, gateways, servers, data stores, etc. The manufacturing machines 401 may connect to the equipment automation layer 415 via the semiconductor manufacturing equipment communication standard / integrated manufacturing equipment interface, via an Ethernet interface, and / or other interfaces. In one embodiment, the equipment automation layer 415 allows process data (e.g., data collected by the manufacturing machine 401 during process execution) to be stored in a data store (not shown). In an alternative embodiment, the computing device 420 connects directly to one or more of the manufacturing machines 401.

[0053] In one embodiment, some or all of the manufacturing machines 401 include a programmable controller capable of loading, storing, and executing process recipes. The programmable controller may control temperature settings, gas and / or vacuum settings, time settings, etc., of the manufacturing machine 401. The programmable controller may include main memory (e.g., read-only memory (ROM), flash memory, dynamic random access memory (DRAM), static random access memory (SRAM), etc.) and / or secondary memory (e.g., a data storage device such as a disk drive). The main memory and / or secondary memory may store instructions for executing the heat treatment processes described herein.

[0054] A programmable controller may also include a processing device coupled to main memory and / or secondary memory (for example, via a bus) to execute instructions. The processing device may be a general-purpose processing device, such as a microprocessor or a central processing unit. The processing device may also be a dedicated processing device, such as an application-specific integrated circuit (ASIC), a field-programmable gate array (FPGA), a digital signal processor (DSP), or a network processor. In one embodiment, the programmable controller is a programmable logic control unit (PLC).

[0055] In one embodiment, the manufacturing machine 401 is programmed to execute recipes that cause the manufacturing machine to polish an article, clean an article, plate an article, form a barrier layer on an article, etc. In one embodiment, the manufacturing machine 401 is programmed to execute recipes that perform multi-step process operations for manufacturing an article having a metal layer and a barrier layer, as described with reference to Figures 5-6. The computing device 420 can store one or more plating recipes, oxidation recipes, cleaning recipes and / or polishing recipes 425 that can be downloaded to the manufacturing machine 401 to cause the manufacturing machine 401 to manufacture an article according to embodiments of the present disclosure.

[0056] Figure 5 is a flowchart representing a method 500 for repairing a high-barrier oxide layer and forming a high-barrier oxide layer on a chamber component, according to one embodiment. The method 500 may be performed on a chamber component having a metal layer (e.g., metal plating) that has been used to perform one or more cycles of one or more manufacturing processes that expose the chamber component to chemicals that cause a contamination layer to form on the metal layer. The contamination layer may include oxygen, fluorine and / or one or more process elements. The contamination layer may cause particulate contamination and / or adversely affect future processes performed in the process chamber, in embodiments. Therefore, in some embodiments of the present disclosure, when a contamination layer is present on the metal-plated chamber component, the chamber component is placed in a first bath 502. The first bath may include water and a first acid (e.g., hydrofluoric acid, nitric acid (HNO3), sulfuric acid (H2SO4), oxalic acid (HC2O4), or ammonium fluoride (NH4F)). Hydrofluoric acid may be present in the bath in an amount of about 5% to about 15% by weight, based on the total composition of the first bath. Water may be present in the bath in an amount of about 85% to about 95% by weight, based on the total composition of the bath. In some embodiments, the first bath contains about 5% by weight of hydrofluoric acid and about 95% by weight of water. The temperature of the first bath may be about 25°C to about 35°C. Used metal-plated chamber parts may be placed in the first bath for about 1 minute to about 30 minutes to remove the contaminant layer. After immersion in the first bath, the metal-plated chamber may contain the removed contaminant layer. The metal-plated chamber parts may then be rinsed (e.g., with deionized water) and dried in block 504 to remove the removed contaminant layer.

[0057] Subsequently, the metal-plated chamber components are placed in a first or second bath in block 506. The second bath contains water and an acid (e.g., hydrofluoric acid). The acid may be present in the bath in an amount of about 5% to about 15% by weight, based on the total composition of the first or second bath. The water may be present in the bath in an amount of about 85% to about 95% by weight, based on the total composition of the first or second bath. In some embodiments, the second bath contains about 5% by weight of hydrofluoric acid and about 95% of water. The temperature of the second bath may be about 25°C to about 35°C. Used metal-plated chamber components may be placed in the second bath for about 1 minute to about 30 minutes, during which time any remaining contaminant layer may be removed. After the second bath, the metal-plated chamber components may be rinsed (e.g., with deionized water) and dried 508.

[0058] The metal-plated chamber components may then be polished after the contamination layer has been removed.510 The metal-plated chamber components may be polished using an automatic polisher with different abrasive sheets, such as Scotch-Brite® sheets, or another advanced method, to uniformly polish the surface. In one embodiment, the metal-plated coated chamber components may be polished until the surface roughness is about 10 μin to about 20 μin. After polishing, the metal-plated coated chamber components may be subjected to an oxidation treatment.512 The oxidation treatment may be carried out by placing the metal-plated coated chamber components in a third bath. The third bath comprises water and an acid (for example, nitric acid (HNO3), sulfuric acid (H2SO4), oxalic acid (HC2O4), or ammonium fluoride (NH4F)). The acid may be present in the bath in an amount of about 5% to about 25% by weight, based on the total composition of the third bath. Water may be included in the bath in an amount of about 75% to about 95% by weight, based on the overall composition of the third bath. In some embodiments, the third bath may contain about 5% by weight of hydrofluoric acid and about 95% by weight of water. The temperature of the third bath may be about 25°C to about 35°C. The metal-plated chamber components may be placed in the third bath for about 1 minute to about 30 minutes. The oxidized metal-plated chamber components may be rinsed (for example with deionized water) to form a nickel oxide layer on the surface of the metal plating layer. In one embodiment, the nickel oxide layer may be between about 5 nanometers and about 35 nanometers.

[0059] In another embodiment, the metal-plated or coated chamber component may be a new component, which may be oxidized by the second method 600. Figure 6 is a flowchart illustrating a method for forming a high barrier layer on a metal-plated or metal-coated chamber component according to one embodiment. In the second method 600, the metal-plated chamber component is placed in a first bath 602. The first bath may contain water and an acid (e.g., hydrofluoric acid). The hydrofluoric acid may be present in the bath in an amount of about 5% to about 25% by weight, based on the total composition of the first bath. The water may be present in the bath in an amount of about 75% to about 95% by weight, based on the total composition of the bath. In some embodiments, the first bath contains about 5% by weight of hydrofluoric acid and about 95% by weight of water. The temperature of the first bath may be about 25°C to about 35°C. The metal-plated chamber component may be placed in the first bath for about 1 minute to about 30 minutes. After the first bath 604, the metal-plated chamber components may be rinsed (for example, with deionized water) and dried 606.

[0060] Once dried, the metal-plated chamber components may be treated with an acid (e.g., hydrofluoric acid or nitric acid (HNO3)) to oxidize the metal-plated layer and form a nickel oxide layer 608. The metal-plated coated chamber components may be treated for a time of about 1 minute to about 30 minutes until the target thickness of the nickel oxide layer is achieved. The nickel oxide layer may be between about 5 nanometers and about 30 nanometers, such as about 15 nanometers in the embodiment. The metal-plated coated chamber components are then rinsed with deionized water in block 610 and dried.

[0061] In another embodiment, the metal-plated or coated chamber component may have a nickel fluoride layer or a nickel oxyfluoride layer and may be a novel component that oxidizes the chamber component. Figure 7 is a flowchart illustrating a method for forming a high barrier layer on a metal-plated or metal-coated chamber component having a nickel fluoride (NiF2) layer or a nickel oxyfluoride (NiOF) layer according to one embodiment. The chamber component is placed in a first bath in steps 702-706, as described in steps 602-606 of Figure 6, and rinsed. After rinsing and drying the chamber component, it is then placed in a second bath containing an ammonium fluoride solution to form a nickel-fluorine layer or nickel-oxyfluorine layer. The ammonium fluoride solution has a concentration of about 0.5 M to about 3 M. The chamber component remains in the second bath for about 5 minutes to about 60 minutes, and the second bath is at a temperature of about 35-45°C to form the NiF2 or NiOF layer. The chamber components are then removed from the bath 710. The chamber components are then rinsed and dried in step 712, as described above for step 606 in Figure 6. After the formation of the NiF2 or NiOF layer, the chamber components may be treated with an acid (e.g., hydrofluoric acid or nitric acid (HNO3)) to oxidize the metal plating layer and form a nickel oxide layer, as described above for steps 512 and 608 in Figures 5 and 6, respectively.

[0062] In another embodiment, a metal-plated chamber component may be oxidized by an in-situ method. This method may be carried out in the same chamber in which the chamber component is coated with the nickel-plated coating, or in the chamber in which the component is used. In the first step of the in-situ method, the metal-plated chamber component may be treated with gas and moisture while the chamber component is in the chamber. The gas may be selected from the group consisting of NH3, NF3, HF, or H2, or a combination thereof. In some embodiments, the gas may be a combination of NH3 and NF3, or a combination of NH3, NF3, and HF. The gas may be concentrated at a concentration of about 5 sccm to about 2000 sccm of the total gas. The gas reacts with ambient moisture in the chamber. The chamber temperature may be about 150°C to about 220°C. The nickel oxide coating layer may have a thickness of about 4 nm to about 50 nm.

[0063] As described herein, by treating a portion with an oxidation treatment to form a barrier layer, the inventors have found that the lifespan of the portion can be more than 10 times longer than that of the original coating without the barrier layer. When chamber components with an ENP-coated layer are used, the standard lifespan is approximately 3,000 cycles. When a barrier nickel oxide layer is present on the ENP-coated layer, the lifespan of the portion is extended to more than 10 times the standard lifespan of the portion, exceeding 10,000 cycles.

[0064] Furthermore, the inventors discovered that oxidation methods can be used to coat new parts and to repair existing parts where a contaminated layer has formed. [Examples]

[0065] Exemplary example The following examples are provided to aid in understanding the present disclosure and should not be construed as expressly limiting the present disclosure described herein and claimed herein. Any variations of the present disclosure, including the substitution of all currently known or subsequently developed equivalents, including any modifications of the formulation or minor changes to the experimental design, which would be within the scope of a person skilled in the art, should be considered to fall within the scope of the present disclosure incorporated herein.

[0066] Example 1 - Pretreatment of shower heads to be coated with ENP This specification illustrates a shower head having nickel plating and a nickel oxide barrier layer on the nickel plating. First, the shower head was coated with a nickel layer using a metal plating process. A native oxide layer was formed on the nickel plating before the intentional formation of a nickel oxide layer. The native nickel oxide layer has inferior properties and also prevents the formation of a target nickel oxide layer that reduces particulate contamination and improves the lifespan of the chamber components. The native nickel oxide layer may have a thickness of about 2-3 nm. Next, the shower head was oxidized by placing it in a bath of 5% (5-25%) hydrofluoric acid and 95% water at a temperature between 25°C and 35°C. After 40 minutes, the shower head was removed from the bath and rinsed with deionized water. A barrier nickel oxide layer was formed on the nickel layer. The barrier nickel oxide (NiO) layer on the metal layer had a thickness of about 6 nm to about 22 nm.

[0067] Example 2 - Cleaning and oxidation of an ENP-coated shower head Shower heads with nickel plating (nickel ENP) used are illustrated herein, and a contaminated layer was formed on the shower heads as a result of use. The total thickness of the contaminated layer (i.e., the fluorine layer or oxyfluorine layer) exceeded 5 to 200 nm.

[0068] To remove the contaminated layer, the showerhead was cleaned by placing it in a first bath of 5% (5%-25%) hydrofluoric acid and 95% water at 25-40°C for 40 minutes. The showerhead was then removed from the first bath, rinsed with deionized water, and dried. After drying the showerhead, it was then placed in a second bath of 25% hydrofluoric acid and 75% water at 25-40°C for 40 minutes. The showerhead was then removed from the second bath, rinsed again with deionized water, and dried.

[0069] As a result of cleaning, the contaminating layer was removed from the showerhead. Next, to form a barrier layer on top of the ENP layer, the showerhead was treated and oxidized by placing it in a bath of 5% hydrofluoric acid. As a result of the treatment and oxidation, a barrier nickel oxide layer was formed on the ENP layer. The barrier nickel oxide (NiO) layer on the ENP coating layer had a composite thickness of approximately 22 nm. The EDS line profile of the barrier NiO layer on the ENP layer showed the presence of nickel in the barrier NiO layer and the absence of phosphorus in such a layer. TEM images and EDS line profiles of the inside of a small hole in the showerhead were also taken, showing that the barrier layer had a thickness between 6.3 nm and 31.2 nm.

[0070] Furthermore, it was measured that the barrier layer on the back surface of the showerhead had a thickness of approximately 19–30 nm. This was also shown in the EDS line profile. This confirms that the barrier nickel oxide layer was formed along the entire showerhead and was not limited to the front surface only.

[0071] Example 3 - Fluorination and oxidation of ENP-coated shower heads This specification illustrates a shower head having a nickel plating (nickel ENP) coating treated with an ammonium fluoride (NH4F) solution having a concentration of 0.5 M to 3 M in order to convert a fluoride (NiF2) or oxyfluoride (NiOF) layer having a thickness of approximately 6 nm to approximately 50 nm. The shower head was oxidized, in which the shower head was placed in a bath of 5% (5% to 25%) hydrofluoric acid and 95% water at a temperature between 25 and 35°C to achieve a NiO thickness of approximately 6 nm to approximately 50 nm.

[0072] Furthermore, SEM images of the barrier layer on the ENP-coated showerhead were taken. The weight percentages of C, O, P, and Ni were calculated from the SEM images and are presented in Table 1. Note that P originates from the ENP layer. TIFF0007862525000001.tif74170

[0073] The preceding description includes numerous specific details, such as examples of particular systems, components, and methods, to provide a good understanding of some embodiments of the present invention. However, it will be apparent to those skilled in the art that at least some embodiments of the present invention can be implemented without these specific details. In other cases, well-known components or methods are not described in detail or are presented in simple block diagram form to avoid unnecessarily obscuring the invention. Thus, the specific details described are merely examples. Certain implementations may differ from these exemplary details, but are intended to remain within the scope of the present invention.

[0074] Throughout this specification, any reference to “one embodiment” or “embodiment” means that a particular feature, structure, or characteristic described in relation to an embodiment is included in at least one embodiment. Therefore, occurrences of the phrase “in one embodiment” or “in one embodiment” in various places throughout this specification do not necessarily all refer to the same embodiment. Furthermore, the term “or” shall be inclusive, not exclusive. Where the terms “about” or “approximately” are used herein, this means that the presented nominal values ​​are accurate within ±10%.

[0075] Although the operation of the methods described herein has been illustrated and described in a specific order, the order of the operations of each method can be changed so that some operations can be performed in reverse order, or so that some operations can be performed at least partially concurrently with others. In another embodiment, instructions, or suboperations of separate operations, may be performed intermittently and / or alternately.

[0076] It should be understood that the above description is illustrative and not limiting. Many other embodiments will be apparent to those skilled in the art upon reading and understanding the above description. The scope of the present invention should therefore be determined with reference to the appended claims and together with the full scope of the equivalents to which such claims are granted.

Claims

1. Chamber component for processing chamber, The main unit and A nickel-containing metal plating on at least one surface of the main body, A barrier layer containing nickel oxide on the aforementioned metal plating, Directly above the metal plating and below the barrier layer, nickel fluoride (NiF ２ ) layer or nickel oxyfluoride layer A chamber component for a processing chamber, comprising:

2. The chamber component according to claim 1, wherein the metal plating includes nickel and phosphorus.

3. The chamber component according to claim 1, wherein the metal plating contains nickel but does not contain phosphorus.

4. The chamber component according to claim 1, wherein the main body comprises aluminum, an aluminum alloy, aluminum nitride, alumina, or a combination thereof.

5. The chamber component according to claim 1, wherein the metal plating has a thickness of 20 to 75 microns and the barrier layer has a thickness of 2 nm to 50 nm.

6. The chamber component according to claim 1, wherein the barrier layer has an average surface roughness (Ra) of 2 microinches to 60 microinches.

7. The chamber component according to claim 1, wherein the chamber component comprises a shower head for a process chamber.

8. A method for protecting chamber components, Forming a nickel-containing metal plating on the main body of the chamber component, Removing native oxides from the aforementioned metal plating, Subsequently, the metal plating is brought into contact with an oxidizing agent in order to form a barrier layer containing nickel oxide on the metal plating. A method for protecting chamber components, including those mentioned above.

9. The method according to claim 8, wherein the oxidizing agent comprises at least one of hydrofluoric acid, oxalic acid, or nitric acid.

10. The method according to claim 8, wherein the barrier layer has a thickness of 2 μm to 60 μm.

11. The method according to claim 8, wherein forming the metal plating comprises performing electroless metal plating, and the metal plating further comprises phosphorus.

12. The method according to claim 8, wherein the main body comprises an aluminum alloy, aluminum nitride, alumina, or a combination thereof.

13. After forming the metal plating, the metal plating is brought into contact with ammonium fluoride to form nickel fluoride (NiF) on the metal plating. ２ The method according to claim 8, further comprising forming a layer or a nickel oxyfluoride layer.

14. To bring the metal plating into contact with the oxidizing agent, the chamber component is placed in an acid bath containing 5 to 25% by weight of hydrofluoric acid and 75 to 95% by weight of water. Subsequently, the chamber component is placed in a deionized water bath, Subsequently, the chamber component is placed in the acid bath, Subsequently, the chamber component is placed in the deionized water bath. The method according to claim 8, further comprising:

15. A method for repairing used chamber parts, Using a first acidic solution, the contaminating layer is removed from the nickel-containing metal plating on the used chamber parts. Subsequently, the metal plating is brought into contact with an oxidizing agent in order to form a barrier layer containing nickel oxide on the metal plating. Methods that include...

16. The method according to claim 15, wherein the contamination layer contains nickel fluoride.

17. Removing the aforementioned contaminated layer The used chamber parts are placed in the first acid bath, Afterward, the used chamber parts are rinsed with deionized water. After that, the used chamber parts are dried, Subsequently, the used chamber parts are placed in the second acid bath, Afterward, the used chamber parts are rinsed with deionized water. After that, the used chamber parts are dried. The method according to claim 16, including the method described in claim 16.

18. The method according to claim 15, wherein the oxidizing agent comprises at least one of hydrofluoric acid or nitric acid.

19. The method according to claim 15, wherein the barrier layer has a thickness of 2 μm to 60 μm.

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