US3415723A - Method of stop-off of cathode pieces in chromium plating baths - Google Patents

Method of stop-off of cathode pieces in chromium plating baths Download PDF

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Publication number
US3415723A
US3415723A US291988A US29198863A US3415723A US 3415723 A US3415723 A US 3415723A US 291988 A US291988 A US 291988A US 29198863 A US29198863 A US 29198863A US 3415723 A US3415723 A US 3415723A
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United States
Prior art keywords
areas
plate
chromium
selected areas
cathode
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US291988A
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English (en)
Inventor
Bedi Ram Dev
Dubpernell George
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
M&T Chemicals Inc
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M&T Chemicals Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority to NL297569D priority Critical patent/NL297569A/xx
Priority to US291986A priority patent/US3350287A/en
Application filed by M&T Chemicals Inc filed Critical M&T Chemicals Inc
Priority to US291988A priority patent/US3415723A/en
Priority to CH1233168A priority patent/CH477562A/de
Priority to CH1233068A priority patent/CH477561A/de
Priority to CH1098763A priority patent/CH479716A/de
Priority to CH1232968A priority patent/CH493644A/de
Priority to DE19631496894 priority patent/DE1496894A1/de
Priority to FR946796A priority patent/FR1373907A/fr
Priority to GB35313/63A priority patent/GB1064295A/en
Priority to SE09807/63A priority patent/SE339153B/xx
Priority to FR951345A priority patent/FR84638E/fr
Priority to JP38057330A priority patent/JPS4820971B1/ja
Priority to DE19631496895 priority patent/DE1496895A1/de
Priority to CH1480563A priority patent/CH467868A/de
Priority to SE2022/64A priority patent/SE310970B/xx
Priority to GB10693/64A priority patent/GB1064296A/en
Priority to GB10694/64A priority patent/GB1064297A/en
Priority to GB10698/64A priority patent/GB1063782A/en
Priority to GB10696/64A priority patent/GB1063503A/en
Priority to GB10697/64A priority patent/GB1064443A/en
Priority to GB10695/64A priority patent/GB1063781A/en
Priority to US725956A priority patent/US3573175A/en
Priority to US754105A priority patent/US3511758A/en
Application granted granted Critical
Publication of US3415723A publication Critical patent/US3415723A/en
Priority to US786040A priority patent/US3477920A/en
Priority to US821135A priority patent/US3702809A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/02—Electroplating of selected surface areas
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S204/00—Chemistry: electrical and wave energy
    • Y10S204/07—Current distribution within the bath

Definitions

  • ABSTRACT OF THE DISCLOSURE A process for electroplating a chromium plate from a chromium plating bath onto a workpiece having predetermined areas to be chromium plated and selected areas to be stopped-off which comprises placing a piece of etched high'carbon iron alloy immediately adjacent to and in electrical contact with said selected areas, subjecting said selected areas to plating current density whereby said plate is deposited onto the predetermined areas while the selected areas remain stopped-off, and to chromium plated products produced by said process.
  • This invention relates to a method of treating cathodes. More particularly, this invention relates to a method of treating selected areas of cathodes to effect stopping-off, he to permit control of selected areas of a cathode used e.g. in a chromium plating bath so that they may be free from plate which is to be deposited on other areas of the cathode.
  • metals may be immersed in various baths in the course of different treating processes wherein desired portions of the metal may, for example, be subjected to electroplating.
  • electroplating of various metals typically nickel, copper, tin, zinc, or chromium may be effected in baths of varying acidity and composition; many of these baths may contain chloride or fluoride which may be an integral part of the bath or present as an additive.
  • chromium plating baths may undesirably be plated sufficiently to alter the dimensions substantially and/or to spoil the appearance of the finished article.
  • the problem of stopoff may be present in various baths, typified by chromium plating baths, nickel plating baths, acid copper baths, acid tin baths, zinc baths, etc.; for purpose of convenience, reefrence will hereinafter be made to chromium plating baths.
  • the areas of the cathode on which plate is not desired may be covered or painted with a masking or stop-off material which prevents deposition and build-up of the plate on these high current density areas which would normally be plated.
  • the masking or stop-off coatings are commonly subjected to severe corrosive conditions for an extended period of time. For example, in chromium plating these materials may remain in position for extended periods of time, often for days, under the most severe oxidizing conditions in contact with baths which may contain sulfuric acid and chromic acid together wth numerous other chemicals.
  • the stop-olf material must be resistant to the highly erosive effect of the hydrogen which is liberated.
  • chromium plating for example may be effected by use of a bath containing chromic acid and sulfate together with other compounds which may be employed to effect various de- 3,415,723 Patented Dec. 10, 1968 sirable results. Typical of these additive compounds may be fluoride or fluoride complexes.
  • Other illustrative chromium plating systems may include soluble catalyst systems containing e.g. chromic acid and sulfate such as sulfuric acid in amount sufiicient to give the desired concentration of sulfate ion, or self-regulating baths, typically those containing silicofluorides together with sulfate.
  • chromium plating from baths typified by the foregoing, it is common to operate at a temperature which may vary depending upon the type and purpose of the plating operation. Commonly however the temperature of operation may be 34 C.-72 C. and typically 48 C.- 63 C.
  • the cathodic current density may preferably be controlled to fall in the range of 8-100, and typically 12-45 a.s.d. (i.e. amperes per square decimeter) on the selected areas of high current density whereon plating may occur. However, because there may be certain selected high current density areas which are not to be chromium plated, it is desired to stop-off these areas.
  • paints or tapes may include plastic materials such as polymers of vinyl chloride or vinyl acetate which may contain plasticizers, pigments, solvents, etc. These may be applied by painting onto the desired portions of the workpiece which are not to be subjected to the action of the solution.
  • Masking tapes which may be employed for the same purpose may be wrapped around the piece and cover the areas which are to be protected or stopped-off.
  • the process of this invention for electroplating a plate metal from a bath onto a cathode having predetermined areas to be plated and selected areas to be stopped-off comprises protecting said selected areas with a piece of etched high-carbon iron alloy, and subjecting said cathode including said selected areas to plating current density whereby said plate metal is deposited on to said predetermined areas and said selected areas remain stopped-off.
  • Typical of the plate metal with which the process of this invention may find use may be the aforementioned chromium plate including hard chromium plate.
  • This invention will be especially suitable for use with the noted chromium plating baths, including the soluble or sparingly soluble catalyst-containing chromium plating baths.
  • the cathodes which may be used in the practice of this invention may be those basis metal articles upon which a plate, typically a chromium plate is desired. Typically these basis metals may be characterized by their high hydrogen overvoltage. Hydrogen overvoltage is a measure of the amount of work required to liberate hydrogen at the cathode. Thus, it is conventionally expressed as the difference between the potential of the electrode when hydrogen is liberated during electrolysis and the potential of the reversible hydrogen electrode, both potentials being referred to the same electrolyte. A cathode having a lower hydrogen overvoltage will, therefore, generate hydrogen at a lower voltage than a cathode having a higher hydrogen overvoltage.
  • High hydrogen overvoltage basis metals may include ferrous metals such as iron or steel, including stainless steels, low carbon steels, nickel steels, chromium steels, chromium-nickel steels, etc., particularly when these metals are in bright, solid, highly polished condition.
  • ferrous metals such as iron or steel, including stainless steels, low carbon steels, nickel steels, chromium steels, chromium-nickel steels, etc., particularly when these metals are in bright, solid, highly polished condition.
  • the selected areas of the cathode on which it is not desired that plating occur may be protected with a piece of etched high-carbon iron alloy.
  • the high-carbon iron alloys which may be employed may be preferably selected from the group consisting of cast iron and high-carbon steels.
  • Cast iron may be iron containing l.76% carbon which is not malleable over a wide range of temperatures. It may normally exist in the form of white cast iron and gray cast iron, the formerly apparently containing a chemical compound or alloy of iron and carbon, the latter containing a substantial portion of a mixture of the two materials.
  • cast iron may contain other materials such as phosphorus, sulfur, silicon, copper, manganese, nickel, tungsten, etc., it will not normally have any substantial amount of added alloying metals.
  • a typical cast iron may be one containing 4.2% combined carbon and 0.2% graphite and melting at 1088 C.
  • the high carbon steels which may be used in practice of this invention may include steel containing 0.60%- 0.90% carbon together with other optional preferred alloying metals. Typically these alloying metals may include manganese, chromium, nickel, and molybdenum.
  • a typical high carbon steel which may be employed may be SAE Steel No. 1090 containing Percent Carbon 0.850.98
  • the high-carbon iron alloy piece may be etched by immersion for 1-10 seconds or longer, say seconds in mineral acid, e.g., hydrochloric acid, sulfuric acid, etc. at C.30 0, say 25 C. During this immersion the surface of the piece may become etched as hydrogen is liberated.
  • the etched surface of the high-carbon iron alloy may be in low hydrogen overvoltage form commonly characterized by finely divided surface condition.
  • the high-carbon iron alloy may be used to protect those selected areas of the surface to be stopped-off. It may be employed to protect the cleaner or prepared surface of the basis metal in a number of ways.
  • One highly convenient method for placing the high-carbon iron alloy in position to protect the selected areas of the cathode may be by use of a thin foraminous sheet, including mesh, expanded metal, perforated metal, etc. This may be in intimate electrical contact with, and preferably positioned immediately adjacent to and electrically connected to, the cathode areas to be stopped-off.
  • the portion of the cathode to be stopped-off may preferably be overlaid with and contiguous to the thin foraminous sheet.
  • a foraminous sheet immediately adjacent to and electrically connected to the cathode permits plating predetermined areas of the cathode while satisfactorily stopping-off selected areas.
  • the etched high-carbon iron alloy will substantially envelope, surround, or isolate the selected areas.
  • the piece of etched highcarbon iron alloy which may be employed in practice of this invention may be a jig or fixture in which or by means of which the piece to be plated is mounted in the rack.
  • the portion of the piece to be stopped-off may be, e.g., the threads on a bolt
  • the threads may be protected by use of a nut threaded thereover which covers the threads.
  • the nut may be formed of a high-carbon iron alloy the surface of which has been etched as hereinbefore noted supra.
  • the high-carbon iron alloy may be etched in the plating bath prior to electroplating.
  • the bath e.g. a chromium plating bath is sufficiently corrosive to the particular high-carbon iron alloy
  • the assembly including this alloy may be permitted to remain in the bath for 30-120, say 60 seconds prior to electroplating. It may be found that this will etch the surface sufficiently to permit stop-off.
  • etching may be effected by making the assembly including the highcarbon alloy anode for 560 seconds, say 10 seconds prior to plating e. g. with chromium.
  • the alloy may retain its activity indefinitely and it may not be readily poisoned or deactivated during normal operation of baths including chromium plating baths. In fact, the slightest corrosion or pickling action of the bath on the high carbon iron alloy serves to further activate the stop-off ability of the alloy. It is economical to use, in that it may be employed over and over again an almost unlimited number of times, and is conveniently removed after plating.
  • Example 1 In this example, pieces 10, 11, and 12 of high-carbon iron alloy (having dimensions as hereinafter described) fabricated of plain cast iron were etched by immersion in hydrochloric acid for 10 seconds. They were then washed, dried and assembled in manner shown in FIG. 1. As is apparent, the pieces 10 and 11 may be fitting pieces of cast iron wherein the portion 14 of bolt 13 fits; the piece 12 in this embodiment may be a nut which fits over most of the threads 15 on bolt 13. The pieces 10 and 11 may be secured together by means not shown.
  • the entire assembly may be placed as cathode within a chromium plating bath containing 250 g./l. chromic acid, 1.25 g./l. sulfate ion as sulfuric acid, and 2.5 g./l. of silicofluoride ion SiF Power was supplied to maintain an effective cathode current density of 50 a.s.d. at C. for 5 hours. During this time, a plate 17 of 250 microns thickness was deposited on the predetermined area 16. The ends 18 .and 19 of the plate stopped at the begininng of the selected area 14 and the thread 15 of the bolt 13. These selected areas were free of plate. It was apparent that the novel technique of this invention permitted electroplating on the predetermined areas while simultaneously stoppingotl selected areas.
  • Example 2 In this example the procedure of Example 1 was duplicated except that the pieces 10, 11, and 12 of cast iron were not etched prior to immersion in the chromium plating bath. Etching of these pieces was effected by allowing the assembly containing these pieces to rest in the bath, without current for 60 seconds prior to plating.
  • Example 3 In this example, the procedure of Example 1 was duplicated except that the pieces 10, 11, and 12 of cast iron were not etched prior to immersion in the chromium plating bath. Etching of the pieces was eifected by making the assembly including pieces 10, 11, and 12 anode for 510 seconds.
  • a plated product prepared according to the process of this invention is unexpectedly novel in that it is characterized by a layer of plate of predetermined thickness which plate in its deposited form possesses smoothly delineated edges which gradually decrease in thickness over the transition area between the plate and the unplated metal base whereby the plate gradually blends into the metal base.
  • This plated piece need not be ground to remove growths etc. at the end of the plated area as is common with pieces plated by standard e.g. chromium plating techniques.
  • the novel technique of this invention for stopping-off cathodes by protecting selected areas thereon with high carbon iron alloys permits .attainment of superior results.
  • These high carbon iron alloys which, when protecting i.e. when in intimate electrical contact with the cathode, permit attainment of this unexpected and superior result, may be readily fabricated in various forms.
  • the high carbon iron alloys may be in the form of or a portion of the cathode-holding mechanism, it may be possible to use therein foraminous sheets including mesh, expanded metal, and perforated metal, which preferably may contain a plurality of holes of very small size, typically less than about 1 mm. in diameter.
  • a novel product comprising a metal base and a layer of chromium metal plate on portions thereof, said layer of metal plate in its deposited form being characterized by smoothly delineated edges which gradually decrease in thickness over the transition areas between the plate portions and the unplated metal base.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Prevention Of Electric Corrosion (AREA)
US291988A 1962-09-06 1963-07-01 Method of stop-off of cathode pieces in chromium plating baths Expired - Lifetime US3415723A (en)

Priority Applications (26)

Application Number Priority Date Filing Date Title
NL297569D NL297569A (instruction) 1962-09-06
US291988A US3415723A (en) 1962-09-06 1963-07-01 Method of stop-off of cathode pieces in chromium plating baths
US291986A US3350287A (en) 1962-09-06 1963-07-01 Method of preventing etch on cast iron in plating baths
CH1233068A CH477561A (de) 1962-09-06 1963-09-05 Verfahren zur Verhinderung des Anätzens bei der Elektroplattierung von Stahl und Eisen und Vorrichtung zur Ausführung des Verfahrens
CH1233168A CH477562A (de) 1962-09-06 1963-09-05 Verfahren zur Verhinderung des Anätzens bei der Elektroplattierung von Gusseisen und Vorrichtung zur Ausführung des Verfahrens
CH1098763A CH479716A (de) 1962-09-06 1963-09-05 Verfahren zur Verhinderung des Anätzens bei der Elektroplattierung von Metallen
CH1232968A CH493644A (de) 1962-09-06 1963-09-05 Verfahren zur Verhinderung des Anätzens bei der Elektroplattierung eines Metalls und Vorrichtung zur Ausführung des Verfahrens
DE19631496894 DE1496894A1 (de) 1962-09-06 1963-09-05 Verfahren zur Elektroplattierung von Grundmetallen ohne AEtzen
FR946796A FR1373907A (fr) 1962-09-06 1963-09-06 Procédé de dépôt électrolytique sélectif
GB35313/63A GB1064295A (en) 1962-09-06 1963-09-06 Improvements in or relating to electroplating
SE09807/63A SE339153B (instruction) 1962-09-06 1963-09-06
FR951345A FR84638E (fr) 1962-09-06 1963-10-22 Procédé de dépôt électrolytique sélectif
JP38057330A JPS4820971B1 (instruction) 1962-09-06 1963-10-28
DE19631496895 DE1496895A1 (de) 1962-09-06 1963-11-21 Verfahren zum Abdecken des Grundmetalls beim Elektroplattieren
CH1480563A CH467868A (de) 1962-09-06 1963-12-04 Verfahren zum Abdecken von Metallen beim Elektroplattieren
SE2022/64A SE310970B (instruction) 1962-09-06 1964-02-19
GB10695/64A GB1063781A (en) 1962-09-06 1964-03-13 Improvements in or relating to electroplating
GB10698/64A GB1063782A (en) 1962-09-06 1964-03-13 Improvements in or relating to electroplating
GB10696/64A GB1063503A (en) 1962-09-06 1964-03-13 Improvements in or relating to electroplating on cast iron
GB10697/64A GB1064443A (en) 1962-09-06 1964-03-13 Improvements in or relating to electroplating
GB10693/64A GB1064296A (en) 1962-09-06 1964-03-13 Improvements in or relating to electroplating
GB10694/64A GB1064297A (en) 1962-09-06 1964-03-13 Improvements in or relating to electroplating onto steel or iron
US725956A US3573175A (en) 1962-09-06 1968-05-01 Method of stopping-off plating in electroplating baths
US754105A US3511758A (en) 1962-09-06 1968-08-13 Method of preventing etch on steel and iron in plating baths
US786040A US3477920A (en) 1962-09-06 1968-12-23 Method of treating electrodes for use in electroplating baths
US821135A US3702809A (en) 1962-09-06 1969-05-01 Method of preventing etch in plating baths

Applications Claiming Priority (11)

Application Number Priority Date Filing Date Title
US22187962A 1962-09-06 1962-09-06
US29198763A 1963-07-01 1963-07-01
US29192563A 1963-07-01 1963-07-01
US29196063A 1963-07-01 1963-07-01
US29191763A 1963-07-01 1963-07-01
US291988A US3415723A (en) 1962-09-06 1963-07-01 Method of stop-off of cathode pieces in chromium plating baths
US291986A US3350287A (en) 1962-09-06 1963-07-01 Method of preventing etch on cast iron in plating baths
US72595668A 1968-05-01 1968-05-01
US75410568A 1968-08-13 1968-08-13
US78604068A 1968-12-23 1968-12-23
US82113569A 1969-05-01 1969-05-01

Publications (1)

Publication Number Publication Date
US3415723A true US3415723A (en) 1968-12-10

Family

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Family Applications (6)

Application Number Title Priority Date Filing Date
US291986A Expired - Lifetime US3350287A (en) 1962-09-06 1963-07-01 Method of preventing etch on cast iron in plating baths
US291988A Expired - Lifetime US3415723A (en) 1962-09-06 1963-07-01 Method of stop-off of cathode pieces in chromium plating baths
US725956A Expired - Lifetime US3573175A (en) 1962-09-06 1968-05-01 Method of stopping-off plating in electroplating baths
US754105A Expired - Lifetime US3511758A (en) 1962-09-06 1968-08-13 Method of preventing etch on steel and iron in plating baths
US786040A Expired - Lifetime US3477920A (en) 1962-09-06 1968-12-23 Method of treating electrodes for use in electroplating baths
US821135A Expired - Lifetime US3702809A (en) 1962-09-06 1969-05-01 Method of preventing etch in plating baths

Family Applications Before (1)

Application Number Title Priority Date Filing Date
US291986A Expired - Lifetime US3350287A (en) 1962-09-06 1963-07-01 Method of preventing etch on cast iron in plating baths

Family Applications After (4)

Application Number Title Priority Date Filing Date
US725956A Expired - Lifetime US3573175A (en) 1962-09-06 1968-05-01 Method of stopping-off plating in electroplating baths
US754105A Expired - Lifetime US3511758A (en) 1962-09-06 1968-08-13 Method of preventing etch on steel and iron in plating baths
US786040A Expired - Lifetime US3477920A (en) 1962-09-06 1968-12-23 Method of treating electrodes for use in electroplating baths
US821135A Expired - Lifetime US3702809A (en) 1962-09-06 1969-05-01 Method of preventing etch in plating baths

Country Status (7)

Country Link
US (6) US3350287A (instruction)
JP (1) JPS4820971B1 (instruction)
CH (5) CH479716A (instruction)
DE (2) DE1496894A1 (instruction)
GB (7) GB1064295A (instruction)
NL (1) NL297569A (instruction)
SE (2) SE339153B (instruction)

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US6197664B1 (en) 1999-01-12 2001-03-06 Fujitsu Limited Method for electroplating vias or through holes in substrates having conductors on both sides
US6193860B1 (en) * 1999-04-23 2001-02-27 Vlsi Technolgy, Inc. Method and apparatus for improved copper plating uniformity on a semiconductor wafer using optimized electrical currents
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US6923252B2 (en) * 2003-04-17 2005-08-02 The Regents Of The University Of California Borehole sounding device with sealed depth and water level sensors
US20080169199A1 (en) * 2007-01-17 2008-07-17 Chang Gung University Trivalent chromium electroplating solution and an electroplating process with the solution
US20090211914A1 (en) * 2008-02-21 2009-08-27 Ching-An Huang Trivalent Chromium Electroplating Solution and an Operational Method Thereof
CN103088373A (zh) * 2011-10-31 2013-05-08 肖云捷 一种电铸过程中防止烧焦的有效方法
CN103122470B (zh) * 2011-11-17 2015-12-09 符士正 汽车铸铁模具镀液
US9752232B2 (en) * 2015-05-13 2017-09-05 Dan Porodo Method of electrolessly plating nickel on tubulars

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GB1064443A (en) 1967-04-05
CH493644A (de) 1970-07-15
US3573175A (en) 1971-03-30
CH477561A (de) 1969-08-31
CH477562A (de) 1969-08-31
CH467868A (de) 1969-01-31
US3350287A (en) 1967-10-31
GB1063782A (en) 1967-03-30
GB1063503A (en) 1967-03-30
CH479716A (de) 1969-10-15
SE339153B (instruction) 1971-09-27
NL297569A (instruction)
GB1064296A (en) 1967-04-05
DE1496895A1 (de) 1969-09-18
US3477920A (en) 1969-11-11
US3511758A (en) 1970-05-12
JPS4820971B1 (instruction) 1973-06-25
US3702809A (en) 1972-11-14
GB1064295A (en) 1967-04-05
GB1063781A (en) 1967-03-30
DE1496894A1 (de) 1969-08-14
GB1064297A (en) 1967-04-05
SE310970B (instruction) 1969-05-19

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