US3647646A - Method and apparatus for electroplating cylindrical objects - Google Patents

Method and apparatus for electroplating cylindrical objects Download PDF

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US3647646A
US3647646A US710035A US3647646DA US3647646A US 3647646 A US3647646 A US 3647646A US 710035 A US710035 A US 710035A US 3647646D A US3647646D A US 3647646DA US 3647646 A US3647646 A US 3647646A
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plating
electrolyte solution
anode
cylinder
nickel
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William M Tucker
Barrie M Gardner
John W Hayford
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Eastman Kodak Co
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Eastman Kodak Co
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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
    • C25D5/08—Electroplating with moving electrolyte e.g. jet electroplating

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  • the cylindrical object has been mounted in a fixed position within the bath, while in other instances it has been subjected to rotary and/or oscillatory movement to effect agitation of the electrolyte solution in the region immediately adjacent the cathode surface.
  • metal coatings meeting ordinary quality requirements such techniques are generally quite satisfactory.
  • very stringent quality standards such as is the case in nickel plating of steel rolls used as film transport rolls in the manufacture of photographic film.
  • serious difiiculties are encountered.
  • numerous small pit-like defects are formed in the nickel plating, either as a result of gas bubbles which are trapped on the surface of the roll while plating and subsequently plated in, i.e.
  • the present invention comprises a novel method and apparatus for electroplating a cylindrical object with a metal coating which is adapted to use in diverse applications in the electroplating arts where a high quality plating is required. While the invention is specifically described herein with reference to nickel plating of rolls used as film transport rolls in the manufacture of photographic film, it may be utilized in many other electroplating applications, as long as the workpiece is either a cylinder or of a generally cylindrical shape and the plating system is one in which a high degree of agitation of the bath is not detrimental.
  • the cylindrical object which is to be plated is mounted in the electroplating bath in such manner that it is only partially submerged in the electrolyte solution, i.e., so that part of it is below the level of electrolyte solution and the remaining part is exposed. More specifically, the cylinder is mounted in a generally horizontal position so that its longitudinal axis is substantially parallel to the free surface of the electrolyte solution, i.e., the surface of the electrolyte solution when the bath is in a quiescent state, and at such a level that the uppermost point on the cylindrical surface is above the free surface of the electrolyte solution.
  • the cylinder may be positioned so that its longitudinal axis is coincident with the surface of the electrolyte solution or so that it is above or below such surface, so long as a substantial portion of the cylindrical surface is immersed within the solution.
  • the cylindrical object serves as the cathode in the plating process and an anode, which may be an insoluble anode or a soluble anode composed of the plating metal, is mounted within the bath in close proximity thereto.
  • the electrolyte solution is agitated and preferably, the cylindrical object is rotated about its longitudinal axis.
  • the method of effecting agitation is not critical but the solution must be agitated with sufiicient force that the portion of the cylindrical object which is exposed, i.e., above the free surface of the solution, is at all times maintained completely awash with the solution, i.e. continuously and completely covered with a layer of the solution.
  • the cylindrical object is at all times completely surrounded with electrolyte solution which acts to convey the electric current to its surface so as to effect plating at an effective rate over the entire area and yet the static head of liquid above any point on the upwardfacing surface is very low.
  • Rotation of the cylindrical object which is being plated may be etfected in a continuous or intermittent manner, as desired, and agitation of the electrolyte solution may be accomplished by any suitable means known to the art such as (gas sparging, solution sparging, or the use of mechanical stirring apparatus.
  • the method of this invention provides a high plating rate and, at the same time, facilitates formation of a high quality plate which is substantially free of defects.
  • the high plating rate achieved is primarily attributable to the fact that the high degree of agitation of the electrolyte solution efi'ectively replenishes metal ions as they are depleted from immediately adjacent the plating surface.
  • Improvement in the quality of the deposit i.e., freedom from in plate defects, is believed to be a result of the fact that rising bubbles in the solution attributable to the sparging, or other agitation, break as they come in contact with the surface of the cylindrical object and release the gas in such manner that it is not entrapped within the plate, as well as the fact that there is little or no opportunity for particles in the plating bath to settle out onto the rotating cylinder since above any point on the upward-facing cylindrical surface there is only a relatively small depth of solution. Moreover, as the rising bubbles reach the surface of the solution and break they violently scrub the face of the cylinder and wash away any solid particles or minute gas bubbles which have temporarily attached themselves to the cylinder and this action also contributes greatly to the elimination of in plate defects.
  • FIG. 1 is a partial top plan view of electroplating apparatus in accordance with this invention, illustrating particularly the relative positions of the anode and cathode within the plating tank.
  • FIG. 2 is an end view of the apparatus taken along line 2-2 of FIG. 1, illustrating particularly the position of the cathode relative to the surface of the electrolyte solution.
  • FIG. 3 is a longitudinal elevation view of the apparatus taken along the line 33 of FIG. 1, illustrating particularly the construction of the anode and showing means provided for recirculation, heating, and filtering of the electrolyte solution.
  • FIG. 4 is a longitudinal elevation view of the apparatus taken along line 4-4 of FIG. 1, illustrating particularly the relative positions within the plating tank of the cathode and the means provided for agitating the electrolyte solution.
  • plating tank 10 which is rectangular in shape and made of steel plate coated on the interior side with an electrically non-conductive, chemically-resistant coating, such as rubber or polyvinyl chlo.,- ride, 'is partially filled with electrolyte solution 12.
  • an electrically non-conductive, chemically-resistant coating such as rubber or polyvinyl chlo.,- ride
  • electrolyte solution 12 Arranged within tank in two longitudinally extending rows are a series of identical vertically disposed anodes 14, each of which is in the form of a hollow cylinder filled with chunks of electrolytic nickel and is completely immersed within electrolyte solution 12. A total of ten anodes 14are shown and these are arranged so that there are five in each row positioned so they are equally spaced from one another.
  • Anodes 14 are made of titanium and have perforated walls adapted to retain the nickel chunks while admitting electrolyte solution 12 into the interior of the cylinder and thereby into contact with the nickel. Positioned between the rows of anodes 14 is a longie tudinally extending, horizontally disposed, cylindrical roll -16 which serves as the cathode in the electroplating process. Roll 16 is made of steel and, after being plated with nickel, is to be used as a film transport roll in the manufacture of photographic film. At each end of roll' 16, shaft sections 18 extend a short distance beyond the end of the roll.
  • anodes 14 and roll 16 can be of any reasonable magnitude, for example,.anode s 14 can be two feet high and a few inches in diameter and roll 16 can be five feet in length and a few inches in diameter. In the drawings there are five anodes 14 in each row positioned at substantially equal increments along the length of roll 16 but a lesser or greater number of anodes may be used depending on the relative sizes of the anodes and the roll being plated. Moreover, in practice a single plating tank would usually be used to electroplate at the same time a number of rolls arranged within the tank in several parallel rows, with each row being made up of two or more rolls linked together.
  • Anode support rods 22 are fixedly secured to the end walls of plating tank 10 by braces 28 and cathode support rod 26 is similarly secured to the end walls of plating tank 10,
  • Anode hangers 20. and cathode. hangers 24 are insulated with an inert coating, such as a vinyl plastisol insulation, over their entire surface except at the points of contact with the support rods and with the anode or cathode.
  • roll 16 be mounted so that it is only partially submerged in electrolyte solution 12, Le. so that part of roll 16 is below the free surface of electrolyte solution 12 (the term free surface being used herein and in the appended claims to mean the upper surface of the solution when it is in a quiescent state) and the remaining part is above the free surface of electrolyte solution 12-and thus exposed to the surrounding atmosphere.
  • free surface being used herein and in the appended claims to mean the upper surface of the solution when it is in a quiescent state
  • the remaining part is above the free surface of electrolyte solution 12-and thus exposed to the surrounding atmosphere.
  • roll 16 should be mounted with its axis substantially parallel to the free surface of electrolyte solution 12 and preferably at such a level that about 40 to about 90 percent of the total surface area of roll 16 is immersed within electrolyte solution 12 when it is in a quiescent state. It is particularly preferred that roll 16 be mounted so that from about 50' to about 75 percent of the total surface area thereof is immersed within electrolyte solution 12.
  • the electric current required for the process is provided by a conventional direct current source, indicated by the numeral 32, such as a low voltage high amperage generator or rectifier, connected by power supply lines 34 and 36 to anode hangers 20 and cathode hangers 24 which serve to convey the current.
  • a conventional direct current source indicated by the numeral 32, such as a low voltage high amperage generator or rectifier, connected by power supply lines 34 and 36 to anode hangers 20 and cathode hangers 24 which serve to convey the current.
  • electrolyte solution 12 is withdrawn from tank 10 via outlet pipe 38 and pumped by means of pump 40 through filter 42 and heat exchanger.v
  • v series of-orifices 50 which may take the form of slots or Blower 54 can, of course, be replaced by any other suit able source of air which will maintain an adequate volumetric flow rate to effectively agitate electrolyte solution 12 and which provides air which is free of oil or other contaminants.
  • sparging pipe 48 is positioned in the bath so that it is immediately below and substantially parallel to roll 16 so that the streams of bubbles S1 emerging from .orifices 50 and rising through electrolyte solution 12 will uniformly contact the surface of roll 16.
  • variable speed motor 56 is connected by way of drive shaft 58, which extends through a seal in the wallet tank 10, and coupling 60 to shaft section 18 at oneend of roll 16.
  • roll 16 which is to be plated with nickel, is mounted in pisition within tank and connected to the drive shaft of motor 56 which is then started so as to rotate roll 16 about its axis.
  • Blower 54 is then put into operation with the result that a continuous stream of bubbles 51 rises from each of slots 50 in sparging .pipe 48 and breaks over roll 16 causing electrolyte solution 12Ito' be violently agitated and carried up and over, the'exposed surface of rotating roll 16'so asto keep such surface completely and continuously coveredwith alayer if electrolyte solution 12.
  • the object to be plated may have a cross-sectional configuration which takes the form ofan o val,' an ellipse,,or a polygon. All such objects are intended toibeincluded within .the scope of the term out silver plating, zinc plating, or copper plating of cylindrical objects, as Well as nickel plating.
  • the cylindrical object which is to be plated is mounted so that its axis is substantially parallel to the free surface of the electrolyte solution and either coincident with or spaced therefrom so that a portion of the object is immersed in the solution and the remaining portion extends above the free surface ran objectof generally cylindrical shape as employed herein and-inthe appended claims; Moreover, if a cylinderis -provided with shaft sections at its ends, as is frequently the case, then these sections will also be plated as will the entire ends of the cylinder.
  • Pat. 1,918,627 in which this is not "accomplished. -Al-' though it has been specifically illustrated herein with reference' to nickel plating the 'rnethod of this invention is applicable' tofplatihg"with other' 'metals so long as the plating system: is not' one in which vigorous agitationof the electrolyte isdetrimental, as is the case, for example, in'jch'romium plat' g'.
  • the optimum position for the cylindrical object will depend on a number of factors, particularly the diameter of the object and the degree of agitation imparted to the electrolyte solution.
  • the recirculation rate should be sufficient to circulate each hour a volume of electrolyte solution which is equal to at least the total volume of solution in the tank, i.e. a tank turnover rate of at least one time per hour, and preferably equal to at least 1.5 times the total volume of solution in the tank.
  • make-up solution should be added during the plating process.
  • a weir (not shown in the drawing) is preferably provided at one end of the tank.
  • the circulating system can then be arranged to remove some solution from near the bottom of the plating tank and some from the weir box. Any other suitable arrangement for maintaining a constant level of solution in the plating tank can, of course, be employed in place of a Weir.
  • the temperature of the electroplating bath is not ordinarily critical but it will frequently be desirable to provide means for heating the electrolyte solution so that operation at temperatures above room temperature is rendered possible.
  • the plating tank may be jacketed and a suitable heat transfer fluid passed through thejacket, or, in recircuIating the electrolyte solution may be passed through a heat exchanger where the temperature is raised to the necessary level before it is returned to the plating tan-k.
  • the vcirculation system include a filter to, effect removal of any solid particles which are present in the electrolyte; solution.
  • Any conventional type of filter may be employed, but in nickel electroplating with the method of this invention it is preferred to employ a filter capable of retaining one hundred percent of the particles greater than fi ve microns in size.
  • the essential requirements of the method of this invention are (1) that the cylindrical object be properly positioned with reference to the level of electrolyte solution, as hereinbefore described, and (2) that the electrolyte solution be agitated with sufficient force that it washes over the portion of the cylindrical object extending above the free surface of the electrolyte solution, so as to scrub this portion, yet maintains this portion continuously and completely covered to an extent adequate to ensure that plating occurs thereon. It will ordinarily also be highly advantageous to rotate the cylindrical object about its axis so as to ensure uniformity of plating and the preferred embodiments of this invention include such rotation.
  • the method of this invention is operable without such rotation, particularly where completely uniform plate thickness is not essential, since by maintaining the exposed surface of the object completely awash with electrolyte solution plating is taking place over the entire surface throughout the entire plating period and it is thus not necessary to rotate in order to effect plating of the entire surface.
  • plating action is taking place at all times over the entire surface of the cylinder and the purpose of rotating is to compensate for the fact that all points on the plating surface are not equidistant from the anode so as to provide a plate of uniform thickness in spite of the lack of equidistant spacing.
  • rotation of the cylindrical object may be continuous, or it may be intermittent with a short interval during which the cylinder is stationary between each period of rotation, or it may be incremental in nature with the cylinder being turned successively by a quarter turn or a half turn each time.
  • the exact speed of rotation is not critical, but it is preferred in electroplating with nickel to employ a speed of 5 to revolutions per minute.
  • the required agitation of the electrolyte solution can be accomplished by any suitable means as long as the solution is agitated with sufficient force to continuously and completely cover the portion of the cylindrical object above the quiescent level of the bath with a layer of electrolyte solution of adequate thickness, for example, one quarter inch or more, to ensure that electrolytic deposition can occur at all points on the surface defined by the rotating cylinder.
  • the agitation must be such that the solution rolls over the rotating cylinder and keeps its upper surface awash at all times. This provides the desired scrubbing action at the surface of the cylinder while at the same time ensuring that plating current is carried to all portions of the cylinder at all times.
  • Such agitation may be accomplished by sparging with air or other inert gas such as argon or nitrogen, by solution sparging, i.e. by injecting streams of electrolye solution through a multiplicity of jets located within the bath directly below the rotating cylinder, or by mechanical stirring such as by the use of paddle wheels located near the rotating cylinder.
  • inert gas such as argon or nitrogen
  • solution sparging i.e. by injecting streams of electrolye solution through a multiplicity of jets located within the bath directly below the rotating cylinder, or by mechanical stirring such as by the use of paddle wheels located near the rotating cylinder.
  • the sparging pipe is preferably located so that it is parallel to and in line with' the longitudinal axis of the cylinder and at a distance of about 2 to about 8 inches below the bottom surface of the cylinder.
  • the 'slots or holes should be of such size that the air bubbles will be at least /2-inch in diameter, and preferably larger, when they break at the surface, as this provides the most effec tive scrubbing action.
  • the air supplied to the sparging pipe should be pressurized, with the optimum pressure depending on the position of the pipe within the bath. Good results are obtained by providing a pressure of about one'p.s.i.g. for each 18 inches of solution above the top surface-of the sparging pipe.
  • the volume of air required for sparging will, of course, depend upon the specific geometry'of the plating system involved, but, in general, should be at least 2 cubic feet per minute for each square foot of surface being plated, and preferably 3 to 4 cubic feet per minute for each square foot of surface. i I
  • the plating tank may be of any convenient geometry but will ordinarily be of a rectangular shape.
  • the anodes may also be of any suitable shape but must be positioned in the tank in such manner that they do not interfere with the sparging pipe, or other agitating means, and should be arranged so as to provide a live anode surface extending longitudinally over at least the central three-quarters of the cylinder.
  • a convenient and effective procedure is to utilize anodes in which the plating metal is in the form of chunks carried in perforated baskets which are suspended in the electrolyte solution, as illustrated herein.
  • the anode may be a horizontally positioned perforated basket of comparable length to the cathode which is immersed in the electrolyte solution and supported in proximity to the cathode.
  • Any conventional anode construction would be permissible in carrying out the method of this invention so long as the anode is disposed so as to be effective over the full length of the object being plated and does not interfere with the gas sparging or other means employed for agitating the electrolyte solution.
  • the anode need not be a soluble anode as illustrated herein but 'may be an. inert or insoluble anode, in which instance the plating metal would be supplied from the electrolyte.
  • nickel plating can be effected using a suitable-solution of soluble nickel salts as the electrolyte and an insolu-j ble anode composed of lead, platinum, platinized titanium, or graphite.
  • the optimum current desnity for operation of the process will depend upon the specific situation involved, including such factors as the composition and temperature of the bath, the relative positions of anode and. cathode, and so forth. It has been found that current densities of 50 to amperes per square foot ofplar ing surface, or more, are ordinarily feasible in nickel plating in the manner described herein. i
  • the method of this invention is particularly amenable to the production of a hard nickel plate such as is required for film transport rolls used in the manufacture of photographic film.
  • a typical plating bath will'contain nickel sulfate hexahydrate and/or nickel sulfate heptahydrate in an amount of about 24 to about 48 ounces per gallon, nickel chloride in an amount of about 4 to about 6 ounces per gallon, oric acid in an amount of about 4 to about 5 ounces per gallon, saccharin in an amount of about 0.2 to about 0.4 ounce per gallon, ammonium bifluoride in an amount of about 0.2 to about 0.4 ounce per gallon, and a low foaming surfactant in an amount sufiicient to provide a surface tension of less than about 45 dynes per square centimeter.
  • this may be readily accomplished by using a similar plating bath in which the saccharin is omitted
  • the method of this invention provides a very high plating rate while at the same time providing a very high quality plate.
  • nickel electroplating using a free dissolving form of electrolytic nickel plating rates of from about 0.004 inch per hour to as high as about 0.006 inch per hour can be attained. These rates are achieved primarily as a result of the fact that the vigorous agitation provided results in adequate replenishment of the electrolyte surface film at the cathode to sustain a high plating rate.
  • the nickel plate is substantially improved over that obtained by methods heretofore known with respect to the presence of in plate defects. Such defects are substantially eliminated, or at least greatly reduced in number, as a result of the washing action of the electrolyte solution over the surface of the cylinder.
  • Apparatus constructed in accordance wlth the disclosure herein was operated to nickel plate film transport rolls with excellent results. Both 4-inch diameter by 48- inch long steel rolls and 2-inch diameter by 48-inch long aluminum rolls were plated at a current density of 75 amperes per square foot. The plating bath was maintained at a pH of approximately 4 and a temperature of approximately 145 F.
  • the bath was recirculated at a rate suificient to turn the solution over about 1.5 times per hour and passed through a filter which retained all particles above 5 microns in size.
  • the roll was suspended in the bath so that it was a little more than half immersed in the el ectrolyte solution and was adjacent to an anode cons1st1ng of 1" x 1" x /2" nickel chips contained in 2 /z-1nch diameter by 24-inch long perforated titanium baskets.
  • Botation of the roll was at a rate of 7 /2 revolutions per minute with large bu-bble air sparging at a rate suflicient that the electrolyte solution was violently agitated and washed over the rotating roll at all times.
  • a plating rate of about 0.006 inch per hour was achieved and the resulting plate was uniform in thickness, bright, hard, and abrasion resistant and almost completely free of in plate defects.
  • the object to be plated is either a cylinder or of a generally cylindrical shape, said object serves as cathode in the plating process and is positioned adjacent to an anode which is immersed within an electrolyte solution, and an electric potential is impressed across said anode and said object to effect plating; the improvement comprising partially immersing the object in the electrolyte solution with its longitudinal axis substantially parallel to the free surface of the electrolyte solution so that a portion of the object is below said free surface and within the electrolyte solution and the remaining portion of the object extends above said free surface, and agitating the electrolyte solutron during plating of the object by sparging with a fluid introduced into the electrolyte solution directly beneath the object with suflicient force that the electrolyte solutron washes over the portion of the object extending above said free surface to maintain said portion continuously and completely covered with electrolyte solution to an extent adequate to ensure that plating occurs thereon.
  • :--1(5) means fox-impressing an electric potential across said anode-andsaid object.
  • Apparatus as described in claim 15 including means for recirculating a portion of said electrolyte solution.
  • Apparatus as described in claim 15 including means for heating said electrolyte solution.
  • Apparatus as described in claim 15 including means for filtering said electrolyte solution to remove solid particles therefrom.
  • Apparatus for electroplating a cylinder with a nickel coating comprising:
  • a sparging pipe positioned-within said electrolyte solution directly below said cylinder for agitating said electrolyte solution during plating of-saidcylinde'r' so that it washes ov'er the portion of said cylinder extending above said free surface to maintainsaid portion continuously.

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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3933601A (en) * 1974-03-13 1976-01-20 Mitsubishi Denki Kabushiki Kaisha Electroplating method and apparatus
US4138638A (en) * 1974-09-06 1979-02-06 Kabushiki Kaisha Meidensha Apparatus for examining liquid quality
US4265940A (en) * 1977-04-04 1981-05-05 Fuji Photo Optical Co., Ltd. Pressure applying rollers for instant photographic cameras and method of producing the same
FR2477580A1 (ro) * 1980-03-07 1981-09-11 Nippon Steel Corp
FR2501244A1 (fr) * 1981-03-06 1982-09-10 Western Electric Co Procede de galvanoplastie utilisant un electrolyte sous forme de mousse
US4530748A (en) * 1984-05-17 1985-07-23 New Horizons Manufacturing Ltd. Cell configuration for apparatus for electrolytic recovery of silver from spent photographic processing solutions
US4615966A (en) * 1985-07-03 1986-10-07 Polaroid Corporation Color transfer photographic processes and products with indole phthalein filter dyes
US5484513A (en) * 1993-02-05 1996-01-16 Sundwiger Eisenhutte Maschinenfabrik Gmbh & Co. Process and apparatus for producing a rough generated surface on a cylindrical body of rotation
US5925231A (en) * 1996-11-22 1999-07-20 Metzger; Hubert F. Method for electroplating rotogravure cylinder using ultrasonic energy
US6197169B1 (en) 1996-11-22 2001-03-06 Hubert F. Metzger Apparatus and method for electroplating rotogravure cylinder using ultrasonic energy
US6231728B1 (en) 1996-11-22 2001-05-15 Hubert F. Metzger Electroplating apparatus
US6547936B1 (en) 1996-11-22 2003-04-15 Chema Technology, Inc. Electroplating apparatus having a non-dissolvable anode
US20040089554A1 (en) * 2002-11-08 2004-05-13 Schepel Chad M. Apparatus and method for electroplating a metallic film on a rocket engine combustion chamber component
US20050000814A1 (en) * 1996-11-22 2005-01-06 Metzger Hubert F. Electroplating apparatus
US6929723B2 (en) 1996-11-22 2005-08-16 Hubert F. Metzger Electroplating apparatus using a non-dissolvable anode and ultrasonic energy
US20100170801A1 (en) * 1999-06-30 2010-07-08 Chema Technology, Inc. Electroplating apparatus
US20190267607A1 (en) * 2014-07-04 2019-08-29 Semiconductor Energy Laboratory Co., Ltd. Fabricating method and fabricating apparatus for secondary battery

Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3933601A (en) * 1974-03-13 1976-01-20 Mitsubishi Denki Kabushiki Kaisha Electroplating method and apparatus
US4138638A (en) * 1974-09-06 1979-02-06 Kabushiki Kaisha Meidensha Apparatus for examining liquid quality
US4265940A (en) * 1977-04-04 1981-05-05 Fuji Photo Optical Co., Ltd. Pressure applying rollers for instant photographic cameras and method of producing the same
FR2477580A1 (ro) * 1980-03-07 1981-09-11 Nippon Steel Corp
NL8101059A (nl) * 1980-03-07 1981-10-01 Nippon Steel Corp Inrichting voor het elektrolytisch behandelen van een metalen strook.
FR2501244A1 (fr) * 1981-03-06 1982-09-10 Western Electric Co Procede de galvanoplastie utilisant un electrolyte sous forme de mousse
US4530748A (en) * 1984-05-17 1985-07-23 New Horizons Manufacturing Ltd. Cell configuration for apparatus for electrolytic recovery of silver from spent photographic processing solutions
US4615966A (en) * 1985-07-03 1986-10-07 Polaroid Corporation Color transfer photographic processes and products with indole phthalein filter dyes
US5484513A (en) * 1993-02-05 1996-01-16 Sundwiger Eisenhutte Maschinenfabrik Gmbh & Co. Process and apparatus for producing a rough generated surface on a cylindrical body of rotation
US6547936B1 (en) 1996-11-22 2003-04-15 Chema Technology, Inc. Electroplating apparatus having a non-dissolvable anode
US20090255819A1 (en) * 1996-11-22 2009-10-15 Metzger Hubert F Electroplating apparatus
US6231728B1 (en) 1996-11-22 2001-05-15 Hubert F. Metzger Electroplating apparatus
US5925231A (en) * 1996-11-22 1999-07-20 Metzger; Hubert F. Method for electroplating rotogravure cylinder using ultrasonic energy
US7914658B2 (en) 1996-11-22 2011-03-29 Chema Technology, Inc. Electroplating apparatus
US20050000814A1 (en) * 1996-11-22 2005-01-06 Metzger Hubert F. Electroplating apparatus
US6929723B2 (en) 1996-11-22 2005-08-16 Hubert F. Metzger Electroplating apparatus using a non-dissolvable anode and ultrasonic energy
US6197169B1 (en) 1996-11-22 2001-03-06 Hubert F. Metzger Apparatus and method for electroplating rotogravure cylinder using ultrasonic energy
US7556722B2 (en) 1996-11-22 2009-07-07 Metzger Hubert F Electroplating apparatus
US20100170801A1 (en) * 1999-06-30 2010-07-08 Chema Technology, Inc. Electroplating apparatus
US8298395B2 (en) 1999-06-30 2012-10-30 Chema Technology, Inc. Electroplating apparatus
US8758577B2 (en) 1999-06-30 2014-06-24 Chema Technology, Inc. Electroplating apparatus
US7306710B2 (en) * 2002-11-08 2007-12-11 Pratt & Whitney Rocketdyne, Inc. Apparatus and method for electroplating a metallic film on a rocket engine combustion chamber component
US20040089554A1 (en) * 2002-11-08 2004-05-13 Schepel Chad M. Apparatus and method for electroplating a metallic film on a rocket engine combustion chamber component
US20190267607A1 (en) * 2014-07-04 2019-08-29 Semiconductor Energy Laboratory Co., Ltd. Fabricating method and fabricating apparatus for secondary battery
US10593929B2 (en) 2014-07-04 2020-03-17 Semiconductor Energy Laboratory Co., Ltd. Fabricating method and fabricating apparatus for secondary battery
US10615404B2 (en) * 2014-07-04 2020-04-07 Semiconductor Energy Laboratory Co., Ltd. Fabricating method and fabricating apparatus for secondary battery

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