GB2050435A - Method for chemical nickelling of metal parts - Google Patents

Method for chemical nickelling of metal parts Download PDF

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Publication number
GB2050435A
GB2050435A GB8016257A GB8016257A GB2050435A GB 2050435 A GB2050435 A GB 2050435A GB 8016257 A GB8016257 A GB 8016257A GB 8016257 A GB8016257 A GB 8016257A GB 2050435 A GB2050435 A GB 2050435A
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Prior art keywords
solution
nickelling
work solution
work
chemical
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GB8016257A
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GB2050435B (en
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Vmei Lenin
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Vmei Lenin
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Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601Process or apparatus
    • C23C18/1633Process of electroless plating
    • C23C18/1675Process conditions
    • C23C18/168Control of temperature, e.g. temperature of bath, substrate
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601Process or apparatus
    • C23C18/1633Process of electroless plating
    • C23C18/1655Process features
    • C23C18/1658Process features with two steps starting with metal deposition followed by addition of reducing agent
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601Process or apparatus
    • C23C18/1633Process of electroless plating
    • C23C18/1675Process conditions
    • C23C18/1676Heating of the solution
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601Process or apparatus
    • C23C18/1633Process of electroless plating
    • C23C18/1675Process conditions
    • C23C18/1683Control of electrolyte composition, e.g. measurement, adjustment
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31Coating with metals
    • C23C18/32Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C23C18/34Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • C23C18/36Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Chemically Coating (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

In the electroless deposition of nickel, three concentrated solutions are used, the first containing a nickel salt and an accelerator, the second a reducing agent, a complexing agent, stabiliser and a wetting agent, and the third the same reducing agent as the second solution, a complexing agent and a stabiliser. The work solution is prepared by mixing the said first and second concentrated solutions together with water in a predetermined ratio to give a bath of predetermined chemical composition suitable for effecting chemical nickelling; and the composition of the work solution is regulated in the course of the chemical nickelling by direct addition of equal volumes of the said first and the third solutions, the volumes used being chosen as a function of the area loading of the work solution. The temperature of the work solution is preferably increased linearly in the course of the nickelling, starting from the optimal work temperature and reaching a temperature of 2 DEG C lower than the boiling temperature of the work solution.

Description

SPECIFICATION Method for chemical nickelling of metal parts This invention relates to a method for chemical nickelling of metal parts e.g. parts for use in mechan ical engineering, instrument making, electrical engineering and in the production of computers and control systems.
Methods for chemical nickelling of metal parts exist, in which the regulation of the composition of the work solution is effected by direct additions to the work bath when adjustment is needed depend ing on the pH of the system. Another method is known for making up and regulating solutions for chemical nickelling wherein two concentrated solu tions and demineralized water are used in the prep aration of the work solution for chemical nickelling and regulation is effected through direct addition of two concentrated solutions depending on the con centration of both nickel and hypophosphite ions in the bath, the regulation involving complicated analytical procedures.Still another, more compli cated method for chemical nickelling is known wherein the regulation of the work solution is effected as a function of five of the constituents of the work solution for chemical nickelling.
A common disadvantage of the above methods consists of the need for complex analytical proce dures when, irrespective of the continuity of the pro cess of regulation, the rate of metal deposition for a prolonged period of time (for example 100 hours) is decreasing.
An object of this invention is to provide a method for chemical nickelling of metal parts wherein simp lification of the regulation of the work solution, a constant rate of deposition, a constant work bath composition and good properties of the coating can be achieved.
According to the present invention, there is provided a method for chemical nickelling of metal parts, which involves immersing the parts to be tre ated in a bath of a work solution, wherein the method makes use of three concentrated solutions the first of which contains a nickel salt and an accelerator, the second of which contains a reducing agent, a complexing agent, stabiliser and a wetting agent, and the third of which contains the same reducing agent as the second solution, a complexing agent and a stabiliser; and wherein (a) the work solution is prepared by mixing the said first and second concentrated solutions together with water in a pre determined ratio to give a bath of predetermined chemical composition suitable for effecting chemical nickelling; and (b) the composition of the work solu tion is regulated in the course of the chemical nickel ling by direct addition of equal volumes of the said ,first and the third solutions, the volumes used being chosen as a function of the area loading of the work solution.
Preferably, the regulation of the composition of the work solution during nickelling is effected by the addition to the work solution of equal volumes of the first and third solutions everyx minutes, wherex equals numerically the starting concentration of nickel (in grams per litre) in the work solution.
The work solution is preferably formed by combining 10-20 parts by volume of the first solution, 10-20 parts by volume of the second solution, and 60-80 parts by volume of demineralised water.
The additions of the first and third solutions are advantageously effected at the working temperature of the work solution.
The temperature of the work solution is preferably brought to the optimum value forthe start-up of chemical nickelling before the metal parts to be treated are immersed in the bath of work solution.
More preferably, the temperature of the work solution is increased linearly throughout the nickelling starting from the said optimal temperature and reaching a temperature which is 2"C lower than the boiling temperature of the work solution at the end ofthe nickelling.
The concentrations of the first, second and third solutions and the start-up composition of the work solution, will be selected to permit the nickelling in the desired manner and to enable the regulation of the composition of the work solution during the course of the nickelling to proceed in the manner specified above, so that operating conditions are controlled as desired.
The advantages of the invention over the known methods for chemical nickelling of metal parts consist of the following: the admission to the work bath of equal quantities of the regulating solutions results in a significant simplification of the process of regulation; the analysis of the components' concentration can be omitted; the requirement of measuring the pH is avoided; and the reliability of the process is increased while obtaining the deposition at a constant rate of a nickel coating of high quality.
The following Example illustrates the method of the inventions with reference to the accompanying drawing.
Example The drawing is a schematic representation of apparatus for accomplishing the method, the apparatus comprising a work bath 1 filled-up with a work solution 2 wherein the metal parts to be treated are immersed. 4 is a filter-pump, 5 is a temperature controller, 6 is a thermometer, 7 is a device for feeding with an energy supplier, while 8, 9, and 10 are tanks containing the first, second and third concentrated solutions, respectively. 11 is a demineralized water container. 12, 13 and 14 are proportioning devices for the first, second and third concentrated solutions, respectively. 15 is a proportioning device for demineralized water. 16 is a time measuring unit and 17 is a control unit for the proportioning devices 12 to 16.The tank 8 is filled with the first concentrated solution which has been prepared by dissolving in demineralized water the following substances (as the nickel salt and accelerator): nickelous chloride (heptahydrate) -200 g/l' ammonium fluoride (anhydrous) -10 gll The tank 9 is filled with the second concentrated solution which has been prepared by dissolving in demineralized water the following substances (as the reducing agent, complexing agent, stabiliser and wetting agents):: sodium hypophosphite (monohydrate) -245 gll sodium acetate (trihydrate) -120 g/l lactic acid (90%) -195 ml/l lead hydroxycarbonate (anhydrous) -10 mg/l sodium laurylsulphate --80 mg/l The tank 10 is filled with the third concentrated solution which has been prepared by dissolving in demineralized water the following substances (as reducing agent, complexing agent and stabiliser):: sodium hypophosphite (monohydrate) -200 g/l lactic acid (90 /O) -50 ml/l sodium acetate (trihydrate) 40 g/l ammonium hydroxide (25%) -150 ml/l sodium thiosulphate (pentahydrate) -100 mg/I The working bath 1 is filled with the work solution 2 in the following manner: the proportioning device 15 admits demineralized water in a quantity which constitutes 80% (by volume) of the working volume of the bath. Both proportioning devices 12 and 13 admit 10% (by volume) of the working volume of the bath of first and second concentrated solutions respectively. The work solution thus prepared is of 5 gll nickel content.
Then, the filter-pump 4 is actuated which filters and simultaneously agitates the work solution.
Under the commands given by the unit 16, the temperature controller 5 and the device 7 supply energy to the work bath 1 for heating the work solu tion 3. The temperature is measured by the ther mometer 6 placed in the work solution. When the temperature of the work solution reaches the opti mal temperature (in this case 92"C), the unit 16 gives an orderto a transport device (not shown in the drawing) to put the metal parts 3 being treated into the work solution 2 thereby starting the process of chemical nickelling. The area loading of the work solution is 0.75 dim2/1.
The time measuring unit 16 actuates the unit 17 which, in turn, at period of 5 min length (this period being numerically equal to the nickel content, expre ssed in grams/litre, of the work solution) actuates the proportioning devices 12 and 14 which admit directly into the bath 1 the adjusting additives which consist of the first and third concentrated solutions, respectively, in quantities of 2 ml/l of work solution.
During the active time of the work solution 2, the time measuring unit 16, through the temperature controller 5, and the energy supply device 7, increases the temperature of the work solution start ing from the optimal temperature (of 92"C) and reaching a temperature 2"C lower than the boiling temperature of the work solution. Thereby, a coeffi cient of deposition of metal from the solution over the parts being treated which is more than 10 is achieved art a rate of deposition of 22 microns/hour and a coating of a constant composition and of good physical and chemical properties such as hardness, wear resistance, corrosion resistance, etc. is obtained.

Claims (11)

1. A method for chemical nickelling of metal parts, which involves immersing the parts to be treated in a bath of a work solution, wherein the method makes use of three concentrated solutions the first of which contains a nickel salt and an accelerator, the second of which contains a reducing agent, a complexing agent, a stabiliser and a wetting agent and the third of which contains the same reducing agent as the second solution, a complexing agent and a stabiliser; and wherein (a) the work solution is prepared by mixing the said first and second concentrated solutions together with water in a predetermined ratio to give a bath of predetermined chemical composition suitable for effecting chemical nickelling; and (b) the composition of the work solution is regulated in the course of the chemical nickelling by direct addition of equal volumes of the said first and the third solutions, the volumes used being chosen as a function of the area loading of the work solution.
2. A method according to claim 1, wherein the regulation of the composition of the work solution during nickelling is effected by the addition to the work solution of equal volumes of the first and third solutions everyx minutes, wherex equals numerically the starting concentration of nickel (in grams per litre) in the work solution.
3. A method according to claim 1 or2,wherein the work solution is formed by combining 10-20 parts by volume of the first solution, 10-20 parts by volume of the second solution, and 60-80 parts by volume of demineralised water.
4. A method according to claim 1,2 or 3, wherein the additions of quantities of the first and third solutions during the nickelling process are effected at the working temperature ofthe work solution.
5. A method according to claim 1,2,3,or4, wherein the temperature of the work solution is broughtto the optimum value for the start-up of chemical nickelling before the metal parts to be treated are immersed in the bath of work solution.
6. A method according to claim 5, wherein the temperature of the work solution is increased linearly throughout the nickelling starting from the said optimal temperature and reaching a temperature which is 2"C lowerthan the boiling temperature of the work solution at the end of the nickelling.
7. A method according to any preceding claim, wherein the reducing agent used is a hypophos phite.
8. A method according to claim 7, wherein the first solution consists of nickelous chloride and ammonium fluoride; the second solution consists of sodium hypophosphite, sodium acetate, lactic acid, lead hydroxycarbonate and sodium laurylsulphate; and the third solution consists of sodium hypophos phite, sodium acetate, ammonium hydroxide and sodium thiosulphate.
9. A method for chemical nickelling as claimed in claim 1, and substantially as hereinbefore described.
10. A method for chemical nickelling substan tially as described in the foregoing Example.
11. Metal parts whenever nickel-coatedby a method as claimed in any preceding claim.
GB8016257A 1979-05-18 1980-05-16 Method for chemical nickelling of metal parts Expired GB2050435B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
BG7943647A BG32650A1 (en) 1979-05-18 1979-05-18 Method for chemical nickelplating of metal parts

Publications (2)

Publication Number Publication Date
GB2050435A true GB2050435A (en) 1981-01-07
GB2050435B GB2050435B (en) 1983-02-16

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GB8016257A Expired GB2050435B (en) 1979-05-18 1980-05-16 Method for chemical nickelling of metal parts

Country Status (9)

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BG (1) BG32650A1 (en)
CS (1) CS241955B1 (en)
DD (1) DD160945A3 (en)
DE (1) DE3018511C2 (en)
FR (1) FR2456786A1 (en)
GB (1) GB2050435B (en)
HU (1) HU182797B (en)
IT (1) IT8048703A0 (en)
RO (1) RO79638A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150307995A1 (en) * 2014-04-29 2015-10-29 Lam Research Corporation ELECTROLESS DEPOSITION OF CONTINUOUS PALLADIUM LAYER USING COMPLEXED Co2+ METAL IONS OR Ti3+ METAL IONS AS REDUCING AGENTS
US20150307994A1 (en) * 2014-04-29 2015-10-29 Lam Research Corporation ELECTROLESS DEPOSITION OF CONTINUOUS NICKEL LAYER USING COMPLEXED Ti3+ METAL IONS AS REDUCING AGENTS

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1179734A (en) * 1957-07-23 1959-05-27 Improved chemical nickel plating process and apparatus
US3709715A (en) * 1966-05-31 1973-01-09 Dow Chemical Co Electroless nickel plating of hollow containers
DE1621344A1 (en) * 1967-08-04 1971-05-13 Siemens Ag Bath and process for chemical nickel plating of a solid body made of metal, plastic or ceramic
US3934054A (en) * 1969-08-25 1976-01-20 Electro Chemical Engineering Gmbh Electroless metal plating

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150307995A1 (en) * 2014-04-29 2015-10-29 Lam Research Corporation ELECTROLESS DEPOSITION OF CONTINUOUS PALLADIUM LAYER USING COMPLEXED Co2+ METAL IONS OR Ti3+ METAL IONS AS REDUCING AGENTS
US20150307994A1 (en) * 2014-04-29 2015-10-29 Lam Research Corporation ELECTROLESS DEPOSITION OF CONTINUOUS NICKEL LAYER USING COMPLEXED Ti3+ METAL IONS AS REDUCING AGENTS

Also Published As

Publication number Publication date
RO79638A (en) 1982-08-17
IT8048703A0 (en) 1980-05-16
FR2456786A1 (en) 1980-12-12
BG32650A1 (en) 1982-09-15
GB2050435B (en) 1983-02-16
CS241955B1 (en) 1986-04-17
FR2456786B1 (en) 1984-12-07
HU182797B (en) 1984-03-28
DE3018511C2 (en) 1983-12-15
DD160945A3 (en) 1984-07-04
DE3018511A1 (en) 1980-11-27

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