Abstract: Exemplary methods of producing a semiconductor substrate may include plating a metal within a plurality of vias on the semiconductor substrate. A target average fill thickness of the metal within the plurality of vias may be between about a thickness equal to an average via radius of the plurality of vias and a thickness twice the average via radius of the plurality of vias. At least one via of the plurality of vias may be filled to a height below the target average fill thickness of the metal. The methods may include heating the metal to cause reflow of the metal within each via of the plurality of vias. The reflow may adjust the metal within the at least one via to increase in height towards the target average fill thickness.

Abstract: Exemplary methods of electroplating a metal with a nanotwin crystal structure are described. The methods may include plating a metal material into at least one opening on a patterned substrate, where at least a portion of the metal material is characterized by a nanotwin crystal structure. The methods may further include polishing an exposed surface of the metal material in the opening to reduce an average surface roughness of the exposed surface to less than or about 1 nm. The polished exposed surface may include at least a portion of the metal material characterized by the nanotwin crystal structure. In additional examples, the nanotwin-phased metal may be nanotwin-phased copper.

Abstract: Electroplating methods may include providing an electrolyte feedstock comprising copper to a first compartment of an electrochemical cell. The methods may include providing an acidic solution to a second compartment of the electrochemical cell. The first compartment and second compartment may be separated by a membrane. The methods may include applying a current to an anode of the electrochemical cell. The anode of the electrochemical cell may be disposed proximate the first compartment and across from the membrane. The methods may include forming an anolyte and catholyte precursor.

Abstract: Embodiments of the present technology include electroplating methods that include providing a first portion of an electrolyte feedstock to a first compartment of an electrochemical cell. The first portion of an electrolyte feedstock may be characterized by an initial metal ion concentration and an initial acid concentration. The methods may include providing a second portion of an electrolyte feedstock to a second compartment of the electrochemical cell. The second compartment and first compartment may be separated by a first membrane. The methods may include providing an acidic solution to a third compartment of the electrochemical cell. The third compartment and second compartment may be separated by a second membrane. The acidic solution may be characterized by an initial acid concentration. The methods may include applying a current to an anode of the electrochemical cell. The anode of the electrochemical cell may be disposed proximate the first compartment and across from the first membrane.

Abstract: Exemplary methods of electroplating include contacting a patterned substrate with a plating bath in an electroplating chamber, where the pattern substrate includes at least one opening having a bottom surface and one or more sidewall surfaces. The methods may further include forming a nanotwin-containing metal material in the at least one opening. The metal material may be formed by two or more cycles that include delivering a forward current from a power supply through the plating bath of the electroplating chamber for a first period of time, plating a first amount of the metal on the bottom surface of the opening on the patterned substrate and a second amount of the metal on the sidewall surfaces of the opening, and delivering a reverse current from the power supply through the plating bath of the electroplating chamber to remove some of the metal plated in the opening on the patterned substrate.

Abstract: Electroplating methods and systems are described that include adding a metal-ion-containing starting solution to a catholyte to increase a metal ion concentration in the catholyte to a first metal ion concentration. The methods and systems further include measuring the metal ion concentration in the catholyte while the metal ions electroplate onto a substrate and the catholyte reaches a second metal ion concentration that is less than the first metal ion concentration. The methods and systems additionally include adding a portion of an anolyte directly to the catholyte when the catholyte reaches the second metal ion concentration. The addition of the portion of the anolyte increases the metal ion concentration in the catholyte to a third metal ion concentration that is greater than or about the first metal ion concentration.

Abstract: Electroplating methods and systems are described that include adding a metal-ion-containing starting solution to a catholyte to increase a metal ion concentration in the catholyte to a first metal ion concentration. The methods and systems further include measuring the metal ion concentration in the catholyte while the metal ions electroplate onto a substrate and the catholyte reaches a second metal ion concentration that is less than the first metal ion concentration. The methods and systems additionally include adding a portion of an anolyte directly to the catholyte when the catholyte reaches the second metal ion concentration. The addition of the portion of the anolyte increases the metal ion concentration in the catholyte to a third metal ion concentration that is greater than or about the first metal ion concentration.

Abstract: Electrochemical deposition systems and methods are described that have enhanced crystallization prevention features. The systems may include a bath vessel operable to hold an electrochemical deposition fluid having a metal salt dissolved in water. The systems may also include sensors including a thermometer and concentration sensor operable to measure characteristics of the electrochemical deposition fluid. The systems further include a computer configured to perform operations that include receiving system data from the electrochemical system and generating a control signal to change a characteristic of the electrochemical deposition fluid to prevent crystallization of a metal salt in the fluid. The computer generates the control signal based on processing that may include comparing an actual metal salt concentration in the electrochemical deposition fluid to a theoretical solubility limit for the metal salt in the fluid.

Abstract: Exemplary methods of electroplating include contacting a patterned substrate with a plating bath in an electroplating chamber, where the pattern substrate includes at least one opening having a bottom surface and one or more sidewall surfaces. The methods may further include forming a nanotwin-containing metal material in the at least one opening. The metal material may be formed by two or more cycles that include delivering a forward current from a power supply through the plating bath of the electroplating chamber for a first period of time, plating a first amount of the metal on the bottom surface of the opening on the patterned substrate and a second amount of the metal on the sidewall surfaces of the opening, and delivering a reverse current from the power supply through the plating bath of the electroplating chamber to remove some of the metal plated in the opening on the patterned substrate.

Abstract: Exemplary methods of electroplating a metal with a nanotwin crystal structure are described. The methods may include plating a metal material into at least one opening on a patterned substrate, where at least a portion of the metal material is characterized by a nanotwin crystal structure. The methods may further include polishing an exposed surface of the metal material in the opening to reduce an average surface roughness of the exposed surface to less than or about 1 nm. The polished exposed surface may include at least a portion of the metal material characterized by the nanotwin crystal structure. In additional examples, the nanotwin-phased metal may be nanotwin-phased copper.

Abstract: Exemplary methods of electroplating include contacting a patterned substrate with a plating bath in an electroplating chamber, where the pattern substrate includes at least one opening having a bottom surface and one or more sidewall surfaces. The methods may further include forming a nanotwin-containing metal material in the at least one opening. The metal material may be formed by two or more cycles that include delivering a forward current from a power supply through the plating bath of the electroplating chamber for a first period of time, plating a first amount of the metal on the bottom surface of the opening on the patterned substrate and a second amount of the metal on the sidewall surfaces of the opening, and delivering a reverse current from the power supply through the plating bath of the electroplating chamber to remove some of the metal plated in the opening on the patterned substrate.

Abstract: Exemplary methods of producing a semiconductor substrate may include plating a metal within a plurality of vias on the semiconductor substrate. A target average fill thickness of the metal within the plurality of vias may be between about a thickness equal to an average via radius of the plurality of vias and a thickness twice the average via radius of the plurality of vias. At least one via of the plurality of vias may be filled to a height below the target average fill thickness of the metal. The methods may include heating the metal to cause reflow of the metal within each via of the plurality of vias. The reflow may adjust the metal within the at least one via to increase in height towards the target average fill thickness.

Abstract: Exemplary methods of producing a semiconductor substrate may include characterizing a substrate pattern to identify a zonal distribution of a plurality of vias and a height and a radius of each via of the plurality of vias. The methods may include determining a fill rate for each via within the zonal distribution of the plurality of vias. The methods may include modifying a die pattern to adjust via fill rates between two zones of vias. The methods may also include producing a substrate according to the die pattern.

Abstract: Exemplary methods of producing a semiconductor substrate may include characterizing a substrate pattern to identify a zonal distribution of a plurality of vias and a height and a radius of each via of the plurality of vias. The methods may include determining a fill rate for each via within the zonal distribution of the plurality of vias. The methods may include modifying a die pattern to adjust via fill rates between two zones of vias. The methods may also include producing a substrate according to the die pattern.

Abstract: Electroplating systems according to the present technology may include a two-bath electroplating chamber including a separator configured to provide fluid separation between a first bath configured to maintain a catholyte during operation and a second bath configured to maintain an anolyte during operation. The system may include a catholyte tank fluidly coupled with the first bath of the two-bath electroplating chamber. The system may also include a contaminant retrieval system configured to remove contaminant ions from the catholyte.