Abstract: Disclosed are apparatus, systems, and methods for electroplating cobalt, nickel, and alloys thereof in interconnect features of partially or fully fabricated electronic devices. During electroplating, cobalt, nickel, or alloys thereof fill features by a bottom up electrofill mechanism. Examples of features that may be electrofilled with cobalt, nickel, or alloys thereof include micro TSVs, contacts for devices, and certain gates for transistors. Electroplating apparatus may include electroplating cells along with one or more instances of each of a post-electrofill module, an anneal chamber, a plasma pretreatment module, and a substrate pre-wetting module.

Abstract: An apparatus and method of adjusting a plating solution are described. Suppressor is added to the plating solution until a comparison to reference data of an RDE potential taken at a first time during a constant current experiment indicates a threshold suppressor concentration is present. The amount of suppressor added to reach the threshold suppressor concentration is used to determine suppressor concentration of the solution. Another amount of suppressor is added to a new plating solution so that the new plating solution has a specific suppressor concentration. The RDE potential or slope of RDE potential change of the new plating concentration with the specific suppressor concentration taken at a second time during another constant current experiment is compared with the reference data to determine the leveler concentration. The suppressor and leveler concentrations of the original plating solution are adjusted before a semiconductor substrate is plated.

Abstract: Tungsten-containing metal films may be deposited in recessed features of semiconductor substrates by electrodeposition. The tungsten-containing metal film is electrodeposited under conditions so that the tunsten-containing metal film is free or substantially free of oxide. Conditions are optimized during electrodeposition for pH, tungsten concentration, and current density, among other parameters. The tungsten-containing metal film may include cobalt tungsten alloy, cobalt nickel tungsten alloy, or nickel tungsten alloy, where a tungsten content in the tungsten-containing metal film is between about 1-20 atomic %.

Abstract: An example electroplating method comprises feeding fresh electrolyte solution into a bath reservoir via a first inlet of the bath reservoir, and bleeding used electrolyte solution out of the bath reservoir via first outlet of the bath reservoir. Recycled electrolyte solution is received into the bath reservoir via a second inlet of the bath reservoir, and electrolyte solution is discharged from the bath reservoir via a second outlet of the bath reservoir. By-products generated by a plating cell are extracted using an extraction column. A first particle filter is disposed in a fluid pathway between the second outlet of the bath reservoir and the inlet of the plating cell, and a second particle filter is disposed in a fluid pathway between the outlet of the extraction column and the second inlet of the bath reservoir.

Abstract: Methods and apparatus for determining whether a substrate includes an unacceptably high amount of oxide on its surface are described. The substrate is typically a substrate that is to be electroplated. The determination may be made directly in an electroplating apparatus, during an initial portion of an electroplating process. The determination may involve immersing the substrate in electrolyte with a particular applied voltage or applied current provided during or soon after immersion, and recording a current response or voltage response over this same timeframe. The applied current or applied voltage may be zero or non-zero. By comparing the current response or voltage response to a threshold current, threshold voltage, or threshold time, it can be determined whether the substrate included an unacceptably high amount of oxide on its surface. The threshold current, threshold voltage, and/or threshold time may be selected based on a calibration procedure.

Abstract: An example electroplating method comprises feeding fresh electrolyte solution into a bath reservoir via a first inlet of the bath reservoir, and bleeding used electrolyte solution out of the bath reservoir via first outlet of the bath reservoir. Recycled electrolyte solution is received into the bath reservoir via a second inlet of the bath reservoir, and electrolyte solution is discharged from the bath reservoir via a second outlet of the bath reservoir. By-products generated by a plating cell are extracted using an extraction column. A first particle filter is disposed in a fluid pathway between the second outlet of the bath reservoir and the inlet of the plating cell, and a second particle filter is disposed in a fluid pathway between the outlet of the extraction column and the second inlet of the bath reservoir.

Abstract: In one aspect, an apparatus includes a plating cell, a degassing device configured to remove oxygen from the plating solution prior to the plating solution flowing into the plating cell; an oxidation station configured to increase an oxidizing strength of the plating solution after the plating solution flows out of the plating cell; and a controller. The controller includes program instructions for causing a process that includes operations of: reducing an oxygen concentration of the plating solution where the plating solution contains a plating accelerator; then, contacting a wafer substrate with the plating solution having reduced oxygen concentration and electroplating a metal such that the electroplating causes a net conversion of the accelerator to a less-oxidized accelerator species within the plating cell; then increasing the oxidizing strength of the plating solution causing a net re-conversion of the less-oxidized accelerator species back to the accelerator outside the plating cell.

Abstract: In one example, an electroplating system comprising a bath reservoir having a first inlet for feeding fresh electrolyte solution into the bath reservoir and a first outlet for bleeding used electrolyte solution out of the bath reservoir, a second inlet for receiving recycled electrolyte solution into the bath reservoir, and a second outlet for discharge of electrolyte solution from the bath reservoir. A plating cell is providing for electroplating an object, the plating cell has an inlet in direct or indirect fluid communication with the bath reservoir, and an outlet for discharge of electrolyte solution from the plating cell. An extraction column extracts by-products generated by the plating cell and has an inlet in direct or indirect fluid communication with the outlet of the plating cell, and an outlet for discharge of electrolyte solution from the extraction column.

Abstract: Methods and apparatus for determining whether a substrate includes an unacceptably high amount of oxide on its surface are described. The substrate is typically a substrate that is to be electroplated. The determination may be made directly in an electroplating apparatus, during an initial portion of an electroplating process. The determination may involve immersing the substrate in electrolyte with a particular applied voltage or applied current provided during or soon after immersion, and recording a current response or voltage response over this same timeframe. The applied current or applied voltage may be zero or non-zero. By comparing the current response or voltage response to a threshold current, threshold voltage, or threshold time, it can be determined whether the substrate included an unacceptably high amount of oxide on its surface. The threshold current, threshold voltage, and/or threshold time may be selected based on a calibration procedure.

Abstract: Methods and apparatus for determining whether a substrate includes an unacceptably high amount of oxide on its surface are described. The substrate is typically a substrate that is to be electroplated. The determination may be made directly in an electroplating apparatus, during an initial portion of an electroplating process. The determination may involve immersing the substrate in electrolyte with a particular applied voltage or applied current provided during or soon after immersion, and recording a current response or voltage response over this same timeframe. The applied current or applied voltage may be zero or non-zero. By comparing the current response or voltage response to a threshold current, threshold voltage, or threshold time, it can be determined whether the substrate included an unacceptably high amount of oxide on its surface. The threshold current, threshold voltage, and/or threshold time may be selected based on a calibration procedure.

Abstract: In one example, an electroplating system comprising a bath reservoir having a first inlet for feeding fresh electrolyte solution into the bath reservoir and a first outlet for bleeding used electrolyte solution out of the bath reservoir, a second inlet for receiving recycled electrolyte solution into the bath reservoir, and a second outlet for discharge0 of electrolyte solution from the bath reservoir. A plating cell is providing for electroplating an object, the plating cell has an inlet in direct or indirect fluid communication with the bath reservoir, and an outlet for discharge of electrolyte solution from the plating cell. An extraction column extracts by-products generated by the plating cell and has an inlet in direct or indirect fluid communication with the outlet of the plating cell, and an outlet for discharge of electrolyte solution from the extraction column.

Abstract: Method and apparatus for reducing metal oxide surfaces to modified metal surfaces and cooling the metal surfaces are disclosed. By exposing a metal oxide surface to remote plasma, the metal oxide surface on a substrate can be reduced to pure metal. A remote plasma apparatus can treat the metal oxide surface as well as actively cool, load/unload, and move the substrate within a single standalone apparatus. The remote plasma apparatus can be configured to actively cool the substrate during and/or after reducing the metal oxide to pure metal using an active cooling system. The active cooling system can include one or more of an actively cooled pedestal, an actively cooled showerhead, and one or more cooling gas inlets for delivering cooling gas to cool the substrate.

Abstract: Methods and apparatus for determining whether a substrate includes an unacceptably high amount of oxide on its surface are described. The substrate is typically a substrate that is to be electroplated. The determination may be made directly in an electroplating apparatus, during an initial portion of an electroplating process. The determination may involve immersing the substrate in electrolyte with a particular applied voltage or applied current provided during or soon after immersion, and recording a current response or voltage response over this same timeframe. The applied current or applied voltage may be zero or non-zero. By comparing the current response or voltage response to a threshold current, threshold voltage, or threshold time, it can be determined whether the substrate included an unacceptably high amount of oxide on its surface. The threshold current, threshold voltage, and/or threshold time may be selected based on a calibration procedure.

Abstract: In one aspect, an apparatus includes a plating cell, a degassing device configured to remove oxygen from the plating solution prior to the plating solution flowing into the plating cell; an oxidation station configured to increase an oxidizing strength of the plating solution after the plating solution flows out of the plating cell; and a controller. The controller includes program instructions for causing a process that includes operations of: reducing an oxygen concentration of the plating solution where the plating solution contains a plating accelerator; then, contacting a wafer substrate with the plating solution having reduced oxygen concentration and electroplating a metal such that the electroplating causes a net conversion of the accelerator to a less-oxidized accelerator species within the plating cell; then increasing the oxidizing strength of the plating solution causing a net re-conversion of the less-oxidized accelerator species back to the accelerator outside the plating cell.

Abstract: Apparatus and methods for electroplating metal onto substrates are disclosed. The electroplating apparatus comprise an electroplating cell and at least one oxidization device. The electroplating cell comprises a cathode chamber and an anode chamber separated by a porous barrier that allows metal cations to pass through but prevents organic particles from crossing. The oxidation device (ODD) is configured to oxidize cations of the metal to be electroplated onto the substrate, which cations are present in the anolyte during electroplating. In some embodiments, the ODD is implemented as a carbon anode that removes Cu(I) from the anolyte electrochemically. In other embodiments, the ODD is implemented as an oxygenation device (OGD) or an impressed current cathodic protection anode (ICCP anode), both of which increase oxygen concentration in anolyte solutions. Methods for efficient electroplating are also disclosed.

Abstract: Method and apparatus for reducing metal oxide surfaces to modified metal surfaces are disclosed. By exposing a metal oxide surface to a remote plasma, the metal oxide surface on a substrate can be reduced to pure metal and the metal reflowed. A remote plasma apparatus can treat the metal oxide surface as well as cool, load/unload, and move the substrate within a single standalone apparatus. The remote plasma apparatus includes a processing chamber and a controller configured to provide a substrate having a metal seed layer in a processing chamber, form a remote plasma of a reducing gas species where the remote plasma includes radicals, ions, and/or ultraviolet (UV) radiation from the reducing gas species, and expose a metal seed layer of the substrate to the remote plasma to reduce oxide of the metal seed layer to metal and to reflow the metal.

Abstract: Methods, systems, and apparatus for plating a metal onto a work piece with a plating solution having a low oxygen concentration are described. In one aspect, a method includes reducing an oxygen concentration of a plating solution. The plating solution includes about 100 parts per million or less of an accelerator. After reducing the oxygen concentration of the plating solution, a wafer substrate is contacted with the plating solution in a plating cell. The oxygen concentration of the plating solution in the plating cell is about 1 part per million or less. A metal is electroplated with the plating solution onto the wafer substrate in the plating cell. After electroplating the metal onto the wafer substrate, an oxidizing strength of the plating solution is increased.

Abstract: Apparatus and methods for electroplating metal onto substrates are disclosed. The electroplating apparatus comprise an electroplating cell and at least one oxidization device. The electroplating cell comprises a cathode chamber and an anode chamber separated by a porous barrier that allows metal cations to pass through but prevents organic particles from crossing. The oxidation device (ODD) is configured to oxidize cations of the metal to be electroplated onto the substrate, which cations are present in the anolyte during electroplating. In some embodiments, the ODD is implemented as a carbon anode that removes Cu(I) from the anolyte electrochemically. In other embodiments, the ODD is implemented as an oxygenation device (OGD) or an impressed current cathodic protection anode (ICCP anode), both of which increase oxygen concentration in anolyte solutions. Methods for efficient electroplating are also disclosed.

Abstract: Method and apparatus for characterizing metal oxide reduction using metal oxide films formed in an anneal chamber are disclosed. Oxygen is provided into an anneal chamber. A substrate including a metal seed layer is exposed to the oxygen and exposed to a heated substrate support in the anneal chamber to form a metal oxide of the metal seed layer. The oxidized substrate can be stored for later use or transferred to a processing chamber for reducing the metal oxide to metal. The oxidized substrates formed in this manner provide metal oxides that are repeatable, uniform, and stable. The oxidized substrate is exposed to a reducing treatment under conditions that reduce the metal oxide to metal in the form of a film integrated with the metal seed layer.

Abstract: In some method and apparatus disclosed herein, the profile of current delivered to the substrate provides a relatively uniform current density on the substrate surface during immersion. These methods include controlling the current density applied across a substrate's surface during immersion by dynamically controlling the current to account for the changing substrate surface area in contact with electrolyte during immersion. In some cases, current density pulses and/or steps are used during immersion, as well.