WO2006078549A1 - Procede de placage par impulsions pour depot d'un alliage or/etain - Google Patents

Procede de placage par impulsions pour depot d'un alliage or/etain Download PDF

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Publication number
WO2006078549A1
WO2006078549A1 PCT/US2006/001218 US2006001218W WO2006078549A1 WO 2006078549 A1 WO2006078549 A1 WO 2006078549A1 US 2006001218 W US2006001218 W US 2006001218W WO 2006078549 A1 WO2006078549 A1 WO 2006078549A1
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Prior art keywords
gold
solution
tin
alloy
asf
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PCT/US2006/001218
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English (en)
Inventor
Fred Hayward
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Technic Inc
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Technic Inc
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/60—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of tin
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/62—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of gold
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/18—Electroplating using modulated, pulsed or reversing current
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/615—Microstructure of the layers, e.g. mixed structure
    • C25D5/617—Crystalline layers
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/627—Electroplating characterised by the visual appearance of the layers, e.g. colour, brightness or mat appearance

Definitions

  • Gold-tin alloys are useful in many microelectronic applications including chip bonding and wafer bump plating.
  • the 80-20 wt% (70-30 at%) gold-tin eutectic alloy is particularly desirable as a solder.
  • the alloy may be applied by vacuum deposition or as a solid preform, however, electrodeposition, due to its low cost, is a preferred method of application.
  • Prior art electroplating baths for the deposition of gold-tin alloy have been found by the current inventor to be incapable of depositing the eutectic alloy over a usable current density range.
  • U.S. Patent No. 4,013,523 by Stevens et al. describes a bath using trivalent gold complex and tin as stannic halide complex.
  • the pH is less than 3 and the bath allegedly is capable of depositing an 80-20 wt% gold alloy.
  • U.S. Patent Application No. 2002063063-A1 by Uchida et al. describes a non- cyanide formulation where the gold complexes used include gold chloride, gold sulfite, gold thiosulfite among others.
  • the electrolyte includes stannic and stannous salts of sulfonic acids, sulfosuccinates, chlorides, sulfates, oxides and oxalates.
  • the tin is complexed with EDTA, DTPA, NTA, IDA, IDP, HEDTA 5 citric acid, tartaric acid, gluconic acid, and glucoheptonic acid among others.
  • the deposit is brightened by a cationic macromolecular surfactant. Oxalate is listed among the possible buffer compounds.
  • Japanese patent application 56136994 describes a solution which uses sulfite gold complex in combination with stannous tin pyrophosphate complex at a pH of 7 to 13.
  • German patent DE 4406434 describes a solution using the trivalent cyanide gold complex in conjunction with stannic tin complexes.
  • the pH is 3-14 and an 80-20 eutectic alloy deposit allegedly may be provided.
  • U.S. Patent No. 6,245,208 by Ivey et al. discloses a non-cyanide formulation which uses gold chloride in combination with sodium sulfite, stannous tin, a complexing agent (ammonium citrate), and uses ascorbic acid as a stabilizer.
  • Eutectic alloy deposits are claimed and bath stability on the order of weeks is reported. As noted above these baths are not always stable and have been found to be insufficient in providing eutectic gold tin alloys on electroplatable substrates, particularly when small parts for electronic components or composite substrates are to be plated.
  • U.S. Patent Nos. 6,071,398 and 6,402,924 disclose methods of electrodepositing a metal such as copper onto a substrate.
  • the methods comprise applying a pulsed periodic reverse current across the electrodes of a plating cell utilizing a peak reverse current density and peak forward current density; and varying the ratio of peak reverse current density to peak forward current density in periodic cycles to provide metal deposits of uniform thickness and appearance upon the substrate.
  • the deposition of metal alloys is not mentioned in these patents.
  • Polyalkylene imines are generally known in the art as useful additives to gold electroplating baths.
  • 3,864,222 discloses that polyalkylene imines can be incorporated into gold and gold alloy plating baths as agents for the general improvement of the brightness and other properties of the resulting electrodeposit. While certain alloys of gold-silver and gold-nickel are disclosed, gold tin is not mentioned, possibly due to the difficulties in obtaining a stable bath of such alloys.
  • the invention relates to a solution for use in connection with the deposition of a gold-tin alloy on an electroplatable substrate.
  • solution generally comprises water, stannous tin ions, a complexing agent to render the stannous tin ions soluble, complexed gold ions, and an alloy stabilization agent that includes an imine functional group.
  • the alloy stabilization agent is present in an amount sufficient to stabilize the deposited alloy and enable a eutectic gold-tin deposit to be provided over a usable current density range.
  • the solution has a pH of between about 2 and about 10 and the deposit having a gold content of less than 90% by weight and a tin content greater 10% by weight.
  • Polyalkylene imines are advantageously used as alloy stabilization agents, with polyethylene imines having a molecular weight of between about 600 and about 2000 being most preferred.
  • the deposit preferably has a gold content of between about 70% and about 80 % by weight and a tin content of between about 20% and about 30% by weight.
  • the complexing agent for the stannous tin ions generally is an organic acid or a salt thereof, with oxalic acid, citric acid, gluconic acid, malonic acid, ascorbic acid, iminodiacetic acid or a solution soluble salt thereof being preferred.
  • the complexed gold ions are advantageously gold cyanide or gold sulfite complexes.
  • the invention also relates to a method for electroplating of a gold-tin alloy deposit on a substrate.
  • the method comprises contacting the substrate with a solution comprising water, stannous tin ions, a complexing agent to render the stannous tin ions soluble, complexed gold ions, and an alloy stabilization agent, with the solution having a pH of between about 2 and about 10 so that the deposit will have a gold content less than 90% by weight and a tin content greater than 10% by weight.
  • a pulsed current is applied though the solution to provide the gold-tin alloy electrodeposit upon the substrate.
  • the pulsed current preferably comprises an uninterrupted, sequential, off-on, continuously repeating pulsing sequence across plating cell electrodes that applies high and low current densities in the solution for predetermined millisecond time periods.
  • the pulsed current is generally off from about 1 to 25 milliseconds and then is turned on for about 1 to 25 milliseconds to provide the pulsed current.
  • a base current can be provided with the pulsed current being applied upon the base current.
  • a typical base current is between about 1 ASF and about 20 ASF with the pulsed current ranging from 0.1 to 8 ASF.
  • a preferred base current is between about 2 ASF and about 10 ASF with the pulsed current ranging from 0.2 to 5 ASF.
  • the pulsed current is preferably on for a shorter time than when it is off.
  • the pulsed current can be off for between about 5 milliseconds and about 10 milliseconds followed by being on for about 1 millisecond to about 4 milliseconds.
  • This method is preferably used for electroplating a gold-tin alloy deposit on composite articles that include electroplatable and non-electroplatable portions in order to provide a gold-tin alloy metal electrodeposit on the electroplatable portions of the articles without deleteriously affecting the non-electroplatable portions of the articles.
  • the term "about,” when modifying a numerical value, is used to refer to a variance ranging from 0% to 20% of the value of the number being modified.
  • the term “about 20” refers to a numerical value of 20 (0% variance) or a numerical range of 18-22 (10% variance) or a maximal numerical range of 16 to 24 (20% variance).
  • other numerical ranges are contemplated by the invention.
  • the electrolyte solution comprises water, stannous tin ions, a complexing agent to render the stannous tin ions soluble, complexes gold ions, and an alloy stabilization agent.
  • the tin ions can be added in any solution soluble form that provides stannous ions. Any two-valent tin salt, including sulfate, chloride, methane sulfonate, oxalate, or any other suitable stannous tin salt, can be used to provide these stannous ions, and the specific tin salt is not critical.
  • Stannic tin may also be added to the solution; however, some stannous tin must be present in the electrolyte for the invention to function properly.
  • the stannous tin ion concentration in the inventive solution is between about 1 g/1 and about 20 g/1 and more preferably between about 2 g/1 and about 10 g/1. Also, the concentration of stannous ions may be adjusted in relation to the gold ion concentration to provide the desired alloy.
  • Figure 2 illustrates the relationship between metal ion concentration ratio in the solution and the composition of the deposited alloy.
  • An antioxidant or reducing agent is preferably included to help maintain the tin ions as stannous tin.
  • Catechol, hydroquinone, or phenolsulfonic acid, or other agents known it the art to prevent tin oxidation can be used with catechol being preferred.
  • the amount of this agent is between about 0.1 g/1 and about 5 g/1, and preferably between about 0.5 g/1 and 2 g/1.
  • a complexing agent is present in the solution to assist hi rendering and maintaining the stannous tin ions soluble in the solution at the operational pH.
  • Any suitable organic acid can be used for this purpose.
  • complexing agents useful in the present invention include but are not limited to oxalic acid, citric acid, ascorbic acid, gluconic acid, malonic acid, and iminodiacetic acid.
  • carboxylic acids are preferred, but iminodiacetic acid and ascorbic acid, which are not carboxylic acids, are also preferred complexors.
  • any other complexing agent that can complex the stannous tin in the solution can be used.
  • the most preferred complexing agents are oxalic, citric, gluconic and malonic acids. Salts of these acids can also be used.
  • the complexing agent is present in the solution in at least a sufficient concentration to maintain the stannous tin soluble at the solution pH. Additionally, it is desirable to maintain an excess of complexing agent beyond the minimum concentration to improve solution conductivity and to provide pH buffering.
  • the complexer concentration is typically between about 10 g/1 and about 300 g/1 and is most preferably between about 40 g/1 and about 150 g/1.
  • the gold ions are preferably provided in the solution as a gold cyanide complex, most preferably monovalent gold cyanide, although, trivalent gold cyanide may also be used.
  • Non-cyanide sulfite gold complex can also be used in the present invention when short solution lives are acceptable; otherwise this complex would not be preferred as the stability of this complex is inferior to the others.
  • the most preferred gold ion complex is potassium gold cyanide.
  • the preferred concentration of gold ion complex in the present invention is between about 2 g/1 and about 20 g/1 and most preferably between about 3 g/1 and about 10 g/1.
  • an alloy stabilization agent having an imine functional group will produce an electrolyte, which will deposit the desired eutectic or similar alloys over an acceptable range of current densities.
  • the deposit may be either tin or gold rich or may have tin or gold rich regions in different areas caused by different current densities.
  • the alloy stabilization agent is important to the proper operation of the present invention.
  • the most effective alloy stabilization agents are those which have imine functional groups.
  • the preferred alloy stabilization agents are polyalkylene imine compounds, with polyethylene imine polymers being most preferred. These polymers are formed by the polymerization of ethylene imines or substituted ethylene imines or are derived from the addition of ethylene imines to organic or inorganic molecules. Typical polymers include polyethylene imines, polypropylene imines, polyhydroxyethylene imines, polyethylene imine adducts, and ethylene imine adducts. Of these, the polymers having molecular weights of 600 to 2000 have found to be most effective.
  • the concentration of the alloy stabilization agent is in the range of 0.1 to 10 ml/1 and is most preferably in the range of 0.5 to 2 ml/1.
  • additives can be added to the solution to modify the grain structure of the deposit. These include metallic additives such as nickel, cobalt, arsenic, lead, thallium, or selenium. Organic additives such as those described in U.S. Patent Application No. 2002063063 may also be used, if desired. Additionally, other salts or buffers may be optionally added to the electrolyte to improve conductivity or pH stability. Examples, of such additives include simple salts such as potassium MSA, potassium sulfate, as well as others well known in the art.
  • the pH of the electrolyte is between about 2 and about 10, is generally less than 8 and is most preferably between about 3 and about 5.5.
  • the preferred pH of the solution is generally dependent upon the gold complex that is used. For instance, potassium gold cyanide is not stable below a pH of 3.5, but a trivalent cyanide gold complex is stable at lower pH values. Sulfite gold complexes are generally not stable below pH 6 and are most stable at pH 8 and higher. Since the solution of the present invention is useful in microelectronics applications, it is desirable to have a pH of less than 8 and preferably less than 7 to prevent solution attack on photoresist masks that are often applied to the electrodeposition substrates.
  • tin containing alloys begins to degrade at pH values greater than about 4.7.
  • the pH can be adjusted to the desired ranges using an acid or base, as necessary.
  • the solution temperature is typically between about 2O 0 C and about 7O 0 C and is most preferably between about 38 0 C and about 5O 0 C. Temperature has a direct effect on the composition of the deposited alloy, with higher temperature resulting in higher gold concentrations.
  • Figure 1 shows the relationship between electrolyte temperature and deposit alloy composition. As is clearly shown the alloy composition can be varied very effectively by controlling temperature.
  • the electrolyte of the present invention may be operated using insoluble anodes including platinized titanium, platinized niobium, or iridium oxide electrode. It is also possible to use soluble anodes, however, this is not typically practiced in precious metals plating.
  • Gold/Tin deposits can be controlled to a large extent by bath chemistry, but plating at varying current densities can change the proportions of the metals in the deposit. For example, at a given gold to tin ratio in the bath, the alloy of the plated deposit will very greatly by increasing or decreasing the current density. At higher current densities, the deposit tends to be higher in gold content, while at lower current densities, the deposit tends to be higher in tin. Thus, variations from the desired eutectic 80 gold-20 tin deposit can be encountered depending upon applied current density.
  • the content of the alloy deposit can be more accurately controlled by varying the applied current density. Pulse plating also decreases plating time when thick deposits (5-25 microns) are to be provided. In addition, the possibility of burning in the high current density portions on parts with sharp geometries is reduced or eliminated.
  • the process is primarily suited for plating typical substrates such as metallized silicon wafers with photo resist masking or a metallic substrate that has a photo resist masking. The metallic or metallized portions are readily platable while the masking is not easily platable, thus enabling the deposited metal to be applied in a circuit or other metal pattern.
  • the pulsed current preferably comprises an uninterrupted, sequential, off- on, continuously repeating pulsing sequence across plating cell electrodes that applies high and low current densities in the solution.
  • One way to do this is to apply a pulsed current that is at a low value from about 1 to 25 milliseconds and then is increased to a higher current density for a second period of about 1 to 25 milliseconds to provide the pulsed current.
  • a preferred way to do this is to provide a constant base current and then apply a smaller, pulsed current upon the base current.
  • a typical base current is between about 1 ASF and about 20 ASF with the pulsed current ranging from 0.1 to 8 ASF.
  • a preferred base current is between about 2 ASF and about 10 ASF with the pulsed current ranging from about 0.2 ASF to about 5 ASF.
  • the pulsed current is preferably on for a shorter time than when it is off.
  • the most preferred embodiment includes pulse plating using a combination of a constant current with a superimposed pulsed current.
  • a constant D. C. current density at low current densities of about 4 ASF to about 5 ASF produces a gold rich alloy at good deposition rate.
  • a pulsed current such as about 1 ASF to about 1.5 ASF at about 2 seconds on and about 8 seconds off using a separate rectifier wired in parallel, the electrolyte is refreshed at the plated interface and then is spiked at the higher current density, thus reducing the possibility of burning the deposit.
  • An additional benefit is the ability to control the tin accurately in the deposit by simply increasing the current on the pulse rectifier.
  • the pulsed current can be off for between about 5 milliseconds and about 10 milliseconds followed by being on for 1 to 4 milliseconds to achieve optimum results for the bath chemistries disclosed herein.
  • the interval of the direct current pulses is on the order of milliseconds to seconds.
  • the alloy composition may be adjusted by varying the relative lengths of the intervals.
  • the desired pulsing direct current may be obtain by connecting a constant current DC rectifier in parallel with a pulsing (on/off) constant current power supply. This configuration produces a current source which fluctuates between high and low current densities.
  • values which have been successfully used are a low current density of 5 ASF for 8 milliseconds and a high current density of 6.25 ASF for 2 milliseconds. Other values can be used and the previous conditions are given as one preferred example only.
  • a skilled artisan can determine by routine testing the most preferred pulse plating conditions for any particular electroplating solution to achieve the desired alloy content of the deposit.
  • Other electroplating processes of the invention may include two constant voltage power supplies connected in series to produce two alternating voltages, or a programmable power supply such as a galvanostat or potentiostat used to supply the current for the plating process.
  • a programmable power supply such as a galvanostat or potentiostat used to supply the current for the plating process.
  • other wave forms such as a sinusoidal wave form, can be superimposed on a direct current and act in the same fashion as the pulsed current processing technique described herein.
  • a eutectic gold-tin alloy electrodeposit is obtained from the following solution and under the following electroplating conditions.
  • the above electrolyte will deposit a matte to semibright 80-20 wt% gold-tin alloy at current densities up to 10 ASF at temperatures between 105 0 F (40.5 0 C) and 12O 0 F (48.8 0 C).
  • a eutectic gold-tin alloy electrodeposit is obtained from the following solution and under the following electroplating conditions.
  • Catechol 1 g/1 pH adjusted with KOH 4 The above electrolyte will deposit a matte to semibright 80-20 wt% gold-tin alloy at current densities up to about 10 ASF at temperatures between 100°F(37.7°C) to 120 0 F (48.8 0 C).
  • a eutectic gold-tin alloy electrodeposit is obtained from the following solution and under the following electroplating conditions.
  • the above electrolyte will deposit a matte to semibright 80-20 wt% gold-tin alloy at current densities up to 10 ASF at temperatures between 105°F (40.5 0 C) and 13O 0 F (54.4 0 C).
  • the pulsed plating technique of the present invention can help provide a more uniform alloy deposit, one that is closer to the eutectic composition so that a lower melting (or refiow) temperature can be used.
  • This experiment was designed to test the effect of pulse rectification modification on increasing tin in the deposit.
  • the following one liter solution was prepared with a Gold:Tin ratio of 1 : 1.25.
  • Sample IA was electroplated at 5 ASF (No Pulse).
  • the resultant gold:tin alloy had a thickness of 5 microns, a composition of 82.1 % gold, an SEM-measured gold value of 86.2% and a melting temperature of 590-608 0 F (310-320 0 C).
  • Sample IB was electroplated at 5 ASF with pulsing at 2.5 ASF on for 2 milliseconds and an 8 millisecond off interval.
  • the resultant gold:tin alloy had a thickness of 5 microns, a composition of 72.7% gold, an SEM-measured gold value of 80.06% and a melting temperature of 572 0 F (300 0 C).
  • Sample 1C was electroplated at 5 ASF with pulsing at 5 ASF for 2 milliseconds and an 8 millisecond off interval.
  • the resultant gold:tin alloy had a thickness of 5 microns, a composition of 70.6% gold, an SEM-measured gold value of 83.48% and did not remelt to liquid.
  • Sample ID was electroplated at 5 ASF with pulsing at 1.25 ASF for 2 milliseconds and an 8 millisecond off interval.
  • the resultant gold:tin alloy had a thickness of 5 microns, a composition of 75.9% gold, an SEM-measured gold value of 83.24% and a melting temperature of 617 0 F (325 0 F).
  • Sample IE was electroplated at 5 ASF with pulsing at 1.25 ASF for 2 milliseconds and an 8 millisecond off interval.
  • the resultant gold:tin alloy had a thickness of 10 microns, a composition of 75.5% gold, an SEM-measured gold value of 75.94% and a melting temperature of 527 0 C (275 0 F).
  • Sample IF was electroplated at 5 ASF with pulsing at 1.25 ASF for 2 milliseconds and an 8 millisecond off interval.
  • the resultant gold:tin alloy had a thickness of 15 microns, a composition of 76.7% gold, an SEM-measured gold value of 74.96% and a melting temperature of 572 0 F (300 0 F).
  • Sample IG was electroplated at 5 ASF with pulsing at 1.25 ASF for 2 milliseconds and an 8 millisecond off interval.
  • the resultant gold:tin alloy had a thickness of 20 microns, a composition of 77.2% gold, an SEM-measured gold value of 76.1 and a melting temperature of 536 0 F (28O 0 C).
  • Sample IH was electroplated at 5 ASF with pulsing at 1.25 ASF for 2 milliseconds and an 8 millisecond off interval.
  • the resultant gold:tin alloy had a thickness of 25 microns, a composition of 77.4% gold, an SEM-measured gold value of 73.8% and a melting temperature of 527 0 F (275 0 F). Alloy thickness and measurement of percent Au was determined by X-ray diffraction and represent an average from 5 measurements. (Numerical values with sample C were obtained with 3 measurements) Scanning Electron Microscopy was also used to separately measure the gold percentage of the alloy.

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

L'invention porte sur une solution s'utilisant en relation avec le dépôt d'un alliage or/argent sur un substrat adéquat. Ladite solution comporte sensiblement: de l'eau, des ions d'étain stanneux, un agent de complexage solubilisant les ions d'étain stanneux, des ions d'or complexés, et un agent stabilisateur comportant un groupe fonctionnel imino. Ledit agent de stabilisation est présent en quantité suffisante pour stabiliser la composition du dépôt or/étain sur une plage utilisable de densités de courant. La solution présente un pH compris entre environ 2 et environ 10, tandis que le dépôt présente une teneur en or de moins d'environ 90 % en poids et une teneur en étain de plus d'environ 10 % en poids. Une manière avantageuse d'obtenir le dépôt désiré est de recourir à la technique du placage par impulsions.
PCT/US2006/001218 2005-01-21 2006-01-13 Procede de placage par impulsions pour depot d'un alliage or/etain Ceased WO2006078549A1 (fr)

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CN104087983A (zh) * 2014-06-30 2014-10-08 江西理工大学 一种硫酸盐光亮电镀锡的溶液
CN110230079A (zh) * 2015-01-16 2019-09-13 哈钦森技术股份有限公司 金电镀溶液和方法

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CN102732918B (zh) * 2012-04-17 2018-09-07 广州天极电子科技有限公司 一种金锡共晶焊料(AuSn20)电镀液及制备方法
US10260159B2 (en) * 2013-07-05 2019-04-16 The Boeing Company Methods and apparatuses for mitigating tin whisker growth on tin and tin-plated surfaces by doping tin with gold

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US3764489A (en) * 1968-11-28 1973-10-09 Oxy Metal Finishing Corp Electrodeposition of gold alloys
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CN104087983A (zh) * 2014-06-30 2014-10-08 江西理工大学 一种硫酸盐光亮电镀锡的溶液
CN110230079A (zh) * 2015-01-16 2019-09-13 哈钦森技术股份有限公司 金电镀溶液和方法
CN110230079B (zh) * 2015-01-16 2022-03-11 哈钦森技术股份有限公司 金电镀溶液和方法
US12173423B2 (en) 2015-01-16 2024-12-24 Hutchinson Technology Incorporated Gold electroplating solution and method

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