WO2007149813A2 - Système de détection électrochimique et d'analyse de données, appareil et procédé de galvanoplastie - Google Patents

Système de détection électrochimique et d'analyse de données, appareil et procédé de galvanoplastie Download PDF

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Publication number
WO2007149813A2
WO2007149813A2 PCT/US2007/071462 US2007071462W WO2007149813A2 WO 2007149813 A2 WO2007149813 A2 WO 2007149813A2 US 2007071462 W US2007071462 W US 2007071462W WO 2007149813 A2 WO2007149813 A2 WO 2007149813A2
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Prior art keywords
profile
combination
data
galvanostatic
defect
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PCT/US2007/071462
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English (en)
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WO2007149813A3 (fr
Inventor
Jianwen Han
Monica K. Hilgarth
Mackenzie King
Steven M. Lurcott
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Advanced Technology Materials, Inc.
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Priority to US12/305,650 priority Critical patent/US20090200171A1/en
Publication of WO2007149813A2 publication Critical patent/WO2007149813A2/fr
Publication of WO2007149813A3 publication Critical patent/WO2007149813A3/fr

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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00Processes for servicing or operating cells for electrolytic coating
    • C25D21/12Process control or regulation
    • GPHYSICS
    • G05CONTROLLING; REGULATING
    • G05BCONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
    • G05B19/00Programme-control systems
    • G05B19/02Programme-control systems electric
    • G05B19/418Total factory control, i.e. centrally controlling a plurality of machines, e.g. direct or distributed numerical control [DNC], flexible manufacturing systems [FMS], integrated manufacturing systems [IMS] or computer integrated manufacturing [CIM]
    • G05B19/41875Total factory control, i.e. centrally controlling a plurality of machines, e.g. direct or distributed numerical control [DNC], flexible manufacturing systems [FMS], integrated manufacturing systems [IMS] or computer integrated manufacturing [CIM] characterised by quality surveillance of production
    • GPHYSICS
    • G05CONTROLLING; REGULATING
    • G05BCONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
    • G05B2219/00Program-control systems
    • G05B2219/30Nc systems
    • G05B2219/32Operator till task planning
    • G05B2219/32182If state of tool, product deviates from standard, adjust system, feedback
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P90/00Enabling technologies with a potential contribution to greenhouse gas [GHG] emissions mitigation
    • Y02P90/02Total factory control, e.g. smart factories, flexible manufacturing systems [FMS] or integrated manufacturing systems [IMS]

Definitions

  • the present invention relates in various aspects to an electrochemical sensing and data analysis system, apparatus and method directed to control of electroplating of various metal(s) on a wafer (or other suitable substrate).
  • the present invention relates to an electrochemical data analysis system directed at predicting defects (probabilities of defect occurrence, for example) in and/or on a wafer (or other suitable substrate) upon which one or more of a variety of metals (e.g., copper, gold, cobalt, platinum or other suitable metal species, etc.) may be deposited.
  • a variety of metals e.g., copper, gold, cobalt, platinum or other suitable metal species, etc.
  • Results of the data analysis may be utilized to adjust, for example, plating bath compositions (e.g., concentrations of acid, chloride or other halide, accelerators, suppressors, and/or levelers, or replacement of plating bath due to presence of too many impurities or by-products or age of bath) in order to increase the percentage of acceptable plated wafers formed having defects below a set threshold level.
  • plating bath compositions e.g., concentrations of acid, chloride or other halide, accelerators, suppressors, and/or levelers, or replacement of plating bath due to presence of too many impurities or by-products or age of bath
  • the electroplated wafers are used in the manufacture of various microelectronic devices.
  • Miniaturization of microelectronic devices is a well accepted trend. Such devices are also being re-designed, re-tooled or otherwise improved to provide better performance. This miniaturization (and/or improved performance) is due in part to electronic circuit boards being developed that have smaller and more defined features.
  • Al aluminum
  • Cu copper
  • Cu deposition may be carried out in an electroplating bath.
  • Cu deposition in an electroplating bath is prone to several problems which, if left uncorrected, leads to the formation of undesirably defective microelectronic devices or components.
  • additives including, but not limited to, suppressors, accelerators, levelers and the like may be added to a copper electroplating bath.
  • Levelers are organic (or other) compound(s) added to Cu electroplating baths that improve the filling of various microelectronic device features so that the roughness of the so filled layer is reduced and/or its flatness is improved.
  • Suppressors are organic (or other) compound(s) added to Cu electroplating baths that improve the filling of various microelectronic device features so that unwanted "necking" or bridging over vias, troughs and the like is reduced so that the proper Cu filling of the various microelectronic device features is achieved.
  • Accelerators are organic (or other) compound(s) added to Cu electroplating baths that also improve the filling of various microelectronic device features so that proper Cu filling of the various microelectronic device features is achieved.
  • suppressors slow down the rate at which Cu is deposited via the use of Cu electroplating baths and accelerators have the opposite effect.
  • the proper combination of at least one accelerator together with at least one suppressor and/or at least one leveler is necessary to achieve the desired or proper Cu deposition on or within a microelectronic device or component.
  • the Cu deposition achieved by the combination of accelerator(s), suppressor(s) and/or leveler(s) is prone to wide variation because as the Cu deposition proceeds, a variety of by-products may be formed and/or the concentration of the accelerator(s), suppressor(s) and/or leveler(s) may be sufficiently changed to undesirably alter the deposition of Cu during the manufacture of microelectronic devices or components.
  • concentration of the accelerator(s), suppressor(s) and/or leveler(s) may be sufficiently changed to undesirably alter the deposition of Cu during the manufacture of microelectronic devices or components.
  • the time required to calibrate electroplating equipment and/or subsequent use of the same to measure and/or control the composition of Cu (and/or other metal) electroplating baths may be time consuming and sometimes cumbersome. According to an embodiment of the present invention, it is desirable to provide a more efficient system and/or method for controlling the chemistry of a Cu electroplating bath in order to reduce the number of defective devices or components made.
  • the invention relates in various aspects to a system for analysis of an electroplated substrate or for analysis for electroplating a substrate or for simply electroplating a substrate or adjusting the electroplating operating parameters (pursuant to the results of the analysis) during electroplating of a substrate.
  • the system for analysis of an electroplated substrate (or for electroplating a substrate) comprises:
  • a first multi-variate analysis component for correlating the galvanostatic data, the potentiodynamic data or the combination thereof with a defect profile of the electroplated substrate, a chemical profile of the plating bath, an electrical performance profile of the electroplated substrate or a combination thereof;
  • the present invention relates to a method for analysis of an electroplated substrate (or for analysis for electroplating a substrate) comprising using the aforementioned components of the above-noted system.
  • the present invention relates to a method for forming an electroplated substrate utilizing the benefit of the aforementioned analysis.
  • the present invention relates to an apparatus for analysis of an electroplated substrate or for analysis for forming an electroplated substrate or for adjusting the electroplating operating parameters of electroplating a substrate - either during ongoing electroplating or during future electroplating operations.
  • Such an apparatus pursuant to an embodiment comprises the aforementioned components of the above -described system - provided in a compact apparatus, for example.
  • a further aspect of the invention relates to a system adapted to defect analysis on an electroplated substrate or adapted to defect analysis for electroplating a substrate, said system comprising: a galvanostatic measurement component, a potentiodynamic measurement component or a combination thereof for measuring galvanostatic data, potentiodynamic data or a combination thereof from a plating bath; a storage component for storing said galvanostatic data, said potentiodynamic data or a combination thereof; and a component for comparing said data with a rule set for determining adjustment(s) to said plating bath.
  • the invention in another aspect relates to a method adapted to forming an electroplated substrate, said method comprising the steps of: performing or obtaining a galvanostatic measurement, a potentiodynamic measurement or a combination thereof relating to said electroplated substrate with a testing cell containing (aa) a reference electrode (RE), (bb) a working electrode (WE), (cc) a counter electrode (CE), (dd) electroplating driving electronics electrically and operatively coupled between the reference electrode (RE), the counter electrode (CE), and the working electrode (WE) to electroplate metal on said working electrode in a metal electroplating bath, and (ee) electrical potential measuring circuitry electrically and operatively coupled between the reference electrode (RE), the counter electrode (CE) and the working electrode (WE), wherein the electroplating driving electronics may further comprise stripping driving electronics to remove plated metal from the working electrode (WE); storing said galvanostatic measurement, said potentiodynamic measurement or said combination thereof; correlating said galvanostatic measurement, said potent
  • FIG. 1 is a side view of an example of a cell used for making galvanostatic measurements. A suitable cell or cells other than the one described in FIG. 1 may be used.
  • FIG. 2 is a top view of the cell of FIG. 1.
  • FIG. 3 is an example of galvanostatic data in the form of a plot of plating potential (mV) versus time for the electroplating of copper on a wafer.
  • FIG. 4 is an example of galvanostatic data in the form of a plot of plating potential (mV) versus time for the electroplating of copper on a wafer where the system shows "drift" in the galvanostatic measurement.
  • FIG. 5 is an example of galvanostatic data in the form of a plot of plating potential (mV) versus time for the electroplating of copper on a wafer where the system has been corrected to adjust for the "drift" in the galvanostatic measurement noted in FIG. 4.
  • FIG. 7 is a high pressure liquid chromatography (HPLC) chromatogram using a UV/VIS (ultra-violet/visible light) detector.
  • HPLC high pressure liquid chromatography
  • SPS refers to the original accelerator used.
  • Tri-species refer to the breakdown by-product of the SPS formed upon aging and/or use of the copper plating bath.
  • the label “Fresh sample” has the same meaning as noted above with regard to FIG. 6.
  • the label “4 Ah/L” has the same meaning as noted above with regard to FIG. 6.
  • the plot labeled "Fresh sample” is a HPLC chromatogram showing peaks for SPS and its breakdown by-product(s) Tri-species.
  • FIG. 8 is another HPLC plot (Gel Permeation Chromatography using an HPLC column and Refractive Index Detector) of a Cu plating bath containing suppressor.
  • the plot labeled "Target” is for fresh (and unused) Cu electroplating bath and the plots labeled 1, 2, 3, and 4 Ah/L refer to electroplating baths that are 1, 2, 3, and 4 hours old in units of amp- hours/liter (Ah/L), respectively.
  • FIG. 9 is another example of galvanostatic data in the form of a plot of plating potential (mV) versus time with the indicated amounts of accelerator breakdown by-product contained in the Cu electroplating bath.
  • the plating potential required for plating of Cu drops with increasing amounts of accelerator. Note that with increasing amounts of accelerator in the Cu electroplating bath, there is also a corresponding increase in the amount of accelerator breakdown by-product present in the same bath.
  • FIG. 10 is a plot of concentration of accelerator (all), accelerator (SPS), suppressor (all) and suppressor (original MW) versus sample identified by the date on which it was tested for a concentration measurement.
  • accelerator SPS
  • accelerator all
  • accelerator all
  • suppressor original MW
  • both the amounts of accelerator breakdown by-products and suppressor breakdown by-products gradually increase from 09/26 to 11/13 - a roughly 45 day time period.
  • FIG. 11 graphically shows the increase in the amount of suppressor and accelerator breakdown by-products over roughly the same time period (09/26 to 11/13). Note that the amount of accelerator breakdown by-products averages at about 5% of accelerator (all) and the amount of suppressor breakdown by-products averages at about 19% of suppressor (all).
  • FIG. 12 is a chart of accelerator breakdown rate versus six different electroplating baths used. Note that for baths A, B, C, and D (i.e., Tool A, Tool B, Tool C and Tool D, respectively), the electroplated wafers or substrates fell below the set acceptable defect threshold. However, for baths M and N (i.e., Tool M, and Tool N, respectively), the electroplated wafers or substrates exceeded the set acceptable defect threshold. The various bars show that when the accelerator breakdown by-products are below about 8.8%, the defect profile is acceptable (green bars) and that when the accelerator breakdown by-products are above about 8.8%, the defect profile is unacceptable (red bars).
  • the set acceptable defect threshold may be set and adjusted up or down - depending on the device into which the particular plated substrate is to be used and on the associated performance requirements for the particular device and/or plated substrate. Also note that FIG. 12 shows a good correlation between low accelerator by-product breakdown rates and acceptable defect profiles (green bars) and vice versa (i.e., unacceptable defect profiles (red bars), and high accelerator by-product breakdown rates).
  • FIG. 13 is similar to FIG. 12 except that instead of breakdown rates for accelerators, breakdown rates for suppressors are plotted. However, no clear correlation between acceptable defect profiles (green bars) and unacceptable defect profiles (red bars) and amount of suppressor breakdown by-products is readily discernable from the plotted data. Without being bound by theory, it appears that the amount of accelerator breakdown byproducts is better correlated to defect profiles than is the amount of suppressor breakdown byproducts as noted by comparison of FIGS. 12 and 13.
  • MVA multi-variate analysis
  • FIG. 14a describes/depicts in flow chart format the various steps involved in making defect profile predictions - using Defect Analysis Reduction Tool /MVA.
  • the text boxes in FIG. 14a are self-explanatory and are understood by those of ordinary skill when taken in conjunction with this application disclosure.
  • FIG. 14b describes/depicts in flow chart format another embodiment of various steps that may be involved in making defect profile predictions - using Defect Analysis Reduction Tool /MVA.
  • the text boxes in FIG. 14b are self-explanatory and are understood by those of ordinary skill when taken in conjunction with this application disclosure.
  • FIG. 15 depicts in plot form the correlation made between the actual defect profiles (blue) versus predicted defect profiles (red) obtained using Defect Analysis Reduction Tool /MVA - see FIGS. 14, 14a and 14b - for sample run nos. 09/26 to 11/01. Using the 09/26 to 11/01 correlation data set, for sample run nos. 11/03 to 11/11, predicted defect profiles (red) are plotted with actual defect profiles (green).
  • the predicted defect profile correlates fairly well with the actual defect profile (green). Knowing that a defect profile can be predicted using, for example, the collected galvanostatic data correlated with actual empirical defect profile data, one can begin to set the corresponding acceptable threshold defect profile values, corresponding threshold plating bath chemical profiles (i.e., how much suppressor, accelerator, and/or leveler to add or whether to adjust the concentration of other components such as chloride or other halide, acid, etc. or simply to replace the plating bath with fresh plating bath) and corresponding electrical profile values without actually having to measure the concentration of the chemical components in a electroplating bath each time.
  • 16 provides details of one cleaning regimen for cleaning the testing cell and all the relevant parts contained therein (e.g., WE, CE, RE, tubing, the testing cell itself etc.) between measurements made on different electroplating baths or the same baths at different time intervals after usage - as may be desirable.
  • Other suitable cleaning regimens may be used.
  • FIG. 17 provides a drawing of an embodiment of one system according to the present invention.
  • reference numeral 1 refers to a testing cell, sampling head or other measurement component.
  • Reference numeral 2 refers to a storage component that may be either long term memory, flash memory or some transient memory or no memory if the measurement(s) collected from 1 can be satisfactorily used without memory.
  • the storage component 2 is connected to 1 as depicted.
  • the storage component is also connected to the first multi-variate component 3. If present, the storage component 2 may also be connected to one or more of the second multi-variate component 4, the third multi-variate component 5, the fourth multi-variate component 6, and so on up to the n ⁇ multivariate component 7.
  • FIG. 18 provides a drawing of another embodiment of one system according to the present invention.
  • reference numeral 1 refers to a testing cell, sampling head or other measurement component.
  • Reference numeral 2 refers to a storage component that may be either long term memory, flash memory or some transient memory or no memory if the measurement(s) collected from 1 can be satisfactorily used without memory.
  • the storage component 2 is connected to 1 as depicted.
  • the storage component is also connected to the first multi-variate component 3.
  • the storage component 2 may also be connected to one or more of the second multi-variate component 4, the third multi-variate component 5, the fourth multi-variate component 6, and so on up to the n ⁇ multivariate component 7. Note that if the storage component 2 is not used or present, then 1 can be directly (or indirectly) connected to 3, 4, 5, 6, . . . . , 7 or some combination thereof.
  • FIG. 17 The difference between FIG. 17 and HG. 18 embodiments is that in HG. 18 components 3, 4, 5, 6, and 7 are connected to a comparator component 8 which in turn is connected to chemical profile manager 9 which also in turn is connected to plating bath 10. Note that the dashed lines in FIG. 18 denote optional connections. Other variations or arrangements than the one specifically depicted in FIG. 18 may be used.
  • Embodiments of the present invention relate to an electrochemical sensing and data analysis system adapted for control of electroplating of various metal(s) on a wafer or other suitable substrate, and to an apparatus and methods using the same. Fine or suitable control is desirable to reduce, minimize or attenuate the occurrence of defects on a wafer or other suitable substrate.
  • the present invention relates to a system (or method or apparatus) for analysis of an electroplated substrate (or for analysis for electroplating a substrate), in which the system comprises:
  • a first multi-variate analysis component for correlating said galvanostatic data, said potentiodynamic data or said combination thereof with a defect profile of said electroplated substrate, a chemical profile of said plating bath, an electrical performance profile of said electroplated substrate or a combination thereof;
  • a galvanostatic measurement includes, but is not limited to, application of a constant current over a given time period during which a measurement of a plating (or stripping) potential versus time is made.
  • FIGS. 3, 4, 5, 6, 9, and 14 contain plots of plating potential (mV) versus time. These plots are examples of suitable galvanostatic measurements.
  • any one of the following voltage ranges including (but not limited to) > 0.1V, > 0.2V, > 0.3V, > 0.4V, > 0.5V, > 0.6V, > 0.7V, > 0.8V, > 0.9V, > 1.0V, > 1.1V, > 1.2V, > 1.3V, . . . , > 1.9V, > 2.0V and so on.
  • SHE standard hydrogen electrode
  • a suitable cleaning regimen for cleaning the WE, CE, RE, the testing cell and all exposed surfaces therein is provided in FIG. 16.
  • Other suitable cleaning regimens may be used in conjunction with one or more embodiments of the present invention.
  • Suitable cleaning sequences for use in conjunction with one or more embodiments of the present invention may be carried out between various numbers of galvanostatic or potentiodynamic measurements made as is suited to the relevant substrate and plating bath being utilized.
  • cleaning/stripping e.g., exposing the testing cell to the cleaning solution followed by stripping the WE for at least about 30 seconds
  • a plating potential e.g., usually lower than the nucleating potential
  • the metal of choice e.g., Cu
  • a galvanostatic measurement component includes, but is not limited to, a working electrode (WE), a reference electrode (RE), and a counter electrode (CE) and all other necessary hardware/software, tubing, and electronics necessary for making the galvanostatic measurement.
  • the galvanostatic measurement component is one that includes the necessary electronics, hardware and may include software sufficient to make the necessary galvanostatic measurements of interest noted herein.
  • a testing cell as described with regard to FIG. 1 may be used (or an equivalent thereof) for making the galvanostatic measurement.
  • the term 'component' as used herein refers to a part of the system that can be in unitary, assembly or sub-assembly form, and can include hardware, firmware and/or software, as appropriate to its structural embodiment and implementation in the system.
  • a potentiodynamic measurement includes, but is not limited to, application of a non-static potential (i.e., non-static voltage) over a given time period during which a measurement of a plating (or stripping) current versus time is made.
  • a potentiodynamic measurement includes, but is not limited to, application of a non-static potential (i.e., non-static voltage) over a given time period during which a measurement of a plating (or stripping) current versus voltage is made.
  • a potentiodynamic measurement component includes, but is not limited to, a working electrode (WE), a reference electrode (RE), and a counter electrode (CE) and all other necessary hardware/software, tubing, and electronics necessary for making the potentiodynamic measurement.
  • the potentiodynamic measurement component is one that includes the necessary hardware and may include software sufficient to make the necessary potentiodynamic measurements of interest noted herein.
  • a testing cell as described with regard to FIG. 1 may be used (or an equivalent thereof) for making the potentiodynamic measurement.
  • the term 'component' as used herein refers to a part of the system that can be in unitary, assembly or sub-assembly form, and can include hardware, firmware and/or software, as appropriate to its structural embodiment and implementation in the system.
  • the WE may be the wafer itself being electroplated with or without a separate WE.
  • Galvanostatic data includes, but is not limited to, plating (or stripping) voltage as a function of time for a plurality of samples (e.g., substrates).
  • the galvanostatic data may include, but is not limited to, a plurality of galvanostatic measurements taken over time for the same sample (e.g., substrate).
  • Potentiodynamic data includes, but is not limited to, plating (or stripping) current as a function of time for a plurality of samples (e.g., substrates) or plating (or stripping) current as a function of voltage for a plurality of samples.
  • the potentiodynamic data may include, but is not limited to, a plurality of potentiodynamic measurements taken over time for the same sample (e.g., substrate).
  • any electrical data measurement or any electrical data of said electroplated substrate may be used that can be correlated with the defect profile of the electroplated substrate, the chemical profile of the plating bath or the electrical profile of the electroplated substrate.
  • a storage component includes, but is not limited to, any memory (e.g., physical memory, computer memory, data storage memory, magnetic storage memory, optical storage memory, flash memory or the like).
  • the storage component may be used for the storage of galvanostatic measurement(s), galvanostatic data, potentiodynamic measurement(s), potentiodynamic data, other relevant electrical measure ment(s), other relevant electrical data or a combination thereof.
  • such profile includes, but is not limited to, resistivity, electromigration, impedance, capacitance, electrical failure, and/or yield (% of devices formed that satisfy operating parameters, specifications or tolerances). Other electrical parameters may include those that affect the "electrical profile" of the electroplated substrate.
  • defect profile includes, but is not limited to, surface roughness, voids (whether on the surface or internally), bulk or surface hardness, surface contamination (e.g., reaction by-product, extraneous matter, other contaminants), crystallographic orientation (e.g., 90% 1,1,1 - Cu), grain size, bulk contamination (e.g., with organics in the Cu layer), and/or structural integrity (e.g., bulk or internal - delamination, stress cracking, stress corrosion etc.).
  • Other physical defect parameters may include those that affect the "electrical profile" of the electroplated substrate.
  • such profile includes, but is not limited to, concentrations of additives (e.g., accelerators, suppressors, levelers and/or combinations thereof), by-products, inorganics, organics, metal salts (e.g., copper sulfate), acids (e.g., sulfuric acid, HCl), halides, (e.g., chloride), other organic processing impurities (e.g., from prior processing steps), other inorganic processing impurities (e.g., from prior processing steps), dust, and/or air-borne contamination.
  • additives e.g., accelerators, suppressors, levelers and/or combinations thereof
  • by-products e.g., inorganics, organics, metal salts (e.g., copper sulfate), acids (e.g., sulfuric acid, HCl), halides, (e.g., chloride), other organic processing impurities (e.g., from prior processing steps), other inorganic processing impurities (e
  • the acceptable electrical threshold range should be set such that the electronic devices or components thereof made according to the present invention provide the necessary yield of acceptable devices or components.
  • acceptable electrical threshold range shall depend upon the device and components being made and their operating specifications and requirements.
  • the acceptable defect threshold range should be set such that the electronic devices or components thereof made according to the present invention provide the necessary yield of acceptable devices or components. Such acceptable defect threshold range shall depend upon the device and components being made and their operating specifications and requirements.
  • the acceptable chemical threshold range should be set such that the electronic devices or components thereof made according to the present invention provide the necessary yield of acceptable devices or components.
  • acceptable chemical threshold range shall depend upon the device and components being made and their operating specifications and requirements.
  • the defect threshold range is a range of values for one or more of the above- noted defect parameters that (if within that defect threshold range) produces acceptable yields (e.g., of acceptable electroplated substrates, devices or components) (e.g., yields of at least about 80%, at least about 85%, at least about 90%, at least about 91%, at least about 92%, at least about 93%, at least about 94%, at least about 95%, at least about 96%, at least about 97%, at least about 98%, at least about 99%, or 100%).
  • acceptable yields e.g., of acceptable electroplated substrates, devices or components
  • the electrical threshold range is a range of values for one or more of the above- noted electrical parameters that (if within that electrical threshold range) produces acceptable yields (e.g., of acceptable electroplated substrates, devices or components) (e.g., yields of at least about 80%, at least about 85%, at least about 90%, at least about 91%, at least about 92%, at least about 93%, at least about 94%, at least about 95%, at least about 96%, at least about 97%, at least about 98%, at least about 99%, or 100%).
  • acceptable yields e.g., of acceptable electroplated substrates, devices or components
  • the chemical threshold range is a range of values for one or more of the above- noted chemical parameters that (if within that chemical threshold range) produces acceptable yields (e.g., of acceptable electroplated substrates, devices or components) (e.g., yields of at least about 80%, at least about 85%, at least about 90%, at least about 91%, at least about 92%, at least about 93%, at least about 94%, at least about 95%, at least about 96%, at least about 97%, at least about 98%, at least about 99%, or 100%).
  • acceptable yields e.g., of acceptable electroplated substrates, devices or components
  • yields e.g., yields of at least about 80%, at least about 85%, at least about 90%, at least about 91%, at least about 92%, at least about 93%, at least about 94%, at least about 95%, at least about 96%, at least about 97%, at least about 98%, at least about 99%, or 100%.
  • Multi-variate analysis includes, but is not limited to, partial least squares (PLS) regression analysis (e.g., curve fitting using PLS Toolbox from Eigenvector), principle component analysis (e.g., another curve fitting method), etc.
  • PLS partial least squares regression analysis
  • principle component analysis e.g., another curve fitting method
  • a multi-variate analysis component includes, but is not limited to, software, hardware, a combination thereof for conducting the multi-variate analysis, for example, as noted above.
  • Correlating the defect profile using multi-variate analysis involves transformation of the galvanostatic data, the potentiodynamic data, or a combination thereof to an averaged data set (of the galvanostatic data, of the potentiodynamic data, or both) optionally including a linearized transformation of the same versus time against the defect profile corresponding to the galvanostatic data, the potentiodynamic data or a combination of the same. See FIGS. 14, 14a, and 14b.
  • One or more variations of the step(s) or procedure(s) of FIGS. 14, 14a, and/or 14b may be used in conjunctions with embodiments of the present invention.
  • Correlating the chemical profile using multi-variate analysis involves transformation of the galvanostatic data, the potentiodynamic data, or a combination thereof to an averaged data set (of the galvanostatic data, of the potentiodynamic data, or both) optionally including a linearized transformation of the same versus time against the chemical profile corresponding to the galvanostatic data, the potentiodynamic data or a combination of the same. See FIGS. 14, 14a, and 14b.
  • One or more variations of the step(s) or procedure(s) of FIGS. 14, 14a, and/or 14b may be used in conjunctions with embodiments of the present invention.
  • Correlating the electrical profile using multi-variate analysis involves transformation of the galvanostatic data, the potentiodynamic data, or a combination thereof to an averaged data set (of the galvanostatic data, of the potentiodynamic data, or both) optionally including a linearized transformation of the same versus time against the electrical profile corresponding to the galvanostatic data, the potentiodynamic data or a combination of the same. See FIGS. 14, 14a, and 14b.
  • One or more variations of the step(s) or procedure(s) of FIGS. 14, 14a, and/or 14b may be used in conjunctions with embodiments of the present invention.
  • any data collected may be used to iteratively improve the prediction ability of the MVA correlation by adding the collected data to the correlation rule set - as desired.
  • an on-line design can be used to continually monitor the process input parameters (copper bath components including additives etc.) and an updated correlation (iterative or non-iterative) with the defects can be incorporated into the MVA.
  • a Monte-Carlo type analysis e.g., Expected Value Analysis
  • a comparator component may be used (pursuant to an embodiment of the present invention) that determines if the defect profile, the chemical profile, or the electrical profile is outside a defect threshold range, a chemical threshold range, or an electrical threshold range, respectively.
  • the comparator component may be an automated piece of hardware or may be software or a combination of the two. Instead of a comparator component, a human operator may conduct the comparator function.
  • Another embodiment of the present invention may include a chemical profile manager (e.g., automated system of hardware, software or a combination thereof; a human operator etc.) for adjusting the chemical profile of the plating bath so that (1) if the defect profile is outside the defect threshold range, (2) if the chemical profile is outside the chemical threshold range, and/or (3) if the electrical profile is outside the electrical threshold range, - then the chemical profile manager may adjust the chemical profile to return (4) the defect profile to fall within the defect threshold range, (5) to return the chemical profile to fall within the chemical threshold range, and/or (6) to return the electrical profile to fall within the electrical threshold range, respectively.
  • a chemical profile manager e.g., automated system of hardware, software or a combination thereof; a human operator etc.
  • Output of the aforementioned analysis may be provided. Output may in the form of reports, electrical signals, or other ways for conveying and/or utilizing the analysis results in improving the electroplating of substrates described herein.
  • the electrochemical sensing part or end comprises a electroplating bath containing a reference electrode (RE), a working electrode (WE), a counter electrode (CE), sample tubing (for introducing a particular electroplating bath), solution tubing (for introducing cleaning solution), and a testing cell (inside which plating of copper occurs on the end of the WE residing in the electroplating bath contained in the testing cell).
  • a reference electrode RE
  • WE working electrode
  • CE counter electrode
  • sample tubing for introducing a particular electroplating bath
  • solution tubing for introducing cleaning solution
  • testing cell inside which plating of copper occurs on the end of the WE residing in the electroplating bath contained in the testing cell.
  • testing cell may also be equipped with or at least connected to the appropriate driving electronics and circuitry needed to make the relevant galvanostatic or potentiodynamic measurements suitable for use with embodiment(s) of the present invention. Details of suitable circuitry and driving electronics are provided in one or more of the U.S. patents or U.S. patent applications cited herein.
  • WE and CE are the working electrode and the counter electrode, respectively.
  • the working electrode contains a sample substrate (or a suitable substitute for the substrate) to be electroplated so that galvanostatic or potentiodynamic plating measurements (or other relevant electrical measurements) can be made during electroplating of the substrate.
  • the WE will contain a small piece of substrate on its end that mimics the behavior of the actual substrate(s) provided in the same electroplating bath being electroplated under essentially identical conditions - if in a different chamber - or - electroplated under identical conditions - if both the WE and the substrate are being electroplated in the same chamber or cell.
  • the testing cell may comprise (aa) a reference electrode (RE), (bb) a working electrode (WE), (cc) a counter electrode (CE), (dd) electroplating driving electronics electrically and operatively coupled between the reference electrode (RE), the counter electrode (CE), and the working electrode (WE) to electroplate metal on said working electrode in a metal electroplating bath, and (ee) electrical potential measuring circuitry electrically and operatively coupled between the reference electrode (RE), the counter electrode (CE) and the working electrode (WE), wherein the electroplating driving electronics may further comprise stripping driving electronics to remove plated metal from the working electrode (WE) - as necessary to make the required measurement(s).
  • a plating bath suitable for use in conjunction with the present invention comprises a metal salt, a halide, an acid and optionally a suppressor, an accelerator, a leveler or a combination thereof.
  • a suitable metal salt is copper sulfate.
  • a suitable halide includes, but is not limited to, a source of chloride.
  • a suitable acid includes, but is not limited to, sulfuric acid, hydrochloric acid, other acids, or a combination thereof.
  • the plating bath typically also contains water (e.g., de-ionized water or other water suitable for measuring the various kinds of measurements noted herein).

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)

Abstract

La présente invention concerne un système de détection électrochimique et d'analyse de données (un appareil et les procédés correspondants) conçu pour commander la galvanoplastie de divers métaux sur une tranche ou sur tout autre substrat approprié. Des constituants du système utilisent l'analyse à plusieurs variables et des mesures galvanoplastiques, potentiodynamiques ou d'autres mesures électriques (ou des combinaisons de ces dernières) pour prédire, ajuster ou commander les paramètres de galvanoplastie, par exemple, pour assurer un meilleur rendement de substrats recouverts présentant des niveaux acceptables de défauts (ou même aucun défaut).
PCT/US2007/071462 2006-06-20 2007-06-18 Système de détection électrochimique et d'analyse de données, appareil et procédé de galvanoplastie WO2007149813A2 (fr)

Priority Applications (1)

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US12/305,650 US20090200171A1 (en) 2006-06-20 2007-06-18 Electrochemical sensing and data analysis system, apparatus and method for metal plating

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US81520606P 2006-06-20 2006-06-20
US60/815,206 2006-06-20

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WO2007149813A3 WO2007149813A3 (fr) 2008-02-21

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TWI397615B (zh) * 2010-04-01 2013-06-01 Zhen Ding Technology Co Ltd 電鍍裝置
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US20030080000A1 (en) * 2001-08-09 2003-05-01 Robertson Peter M. Interference correction of additives concentration measurements in metal electroplating solutions
US20050224370A1 (en) * 2004-04-07 2005-10-13 Jun Liu Electrochemical deposition analysis system including high-stability electrode
US20050241948A1 (en) * 2004-04-30 2005-11-03 Jianwen Han Methods and apparatuses for monitoring organic additives in electrochemical deposition solutions

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WO2007149813A3 (fr) 2008-02-21
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