US2686756A - Chromium plating - Google Patents

Chromium plating Download PDF

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Publication number
US2686756A
US2686756A US356188A US35618853A US2686756A US 2686756 A US2686756 A US 2686756A US 356188 A US356188 A US 356188A US 35618853 A US35618853 A US 35618853A US 2686756 A US2686756 A US 2686756A
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alkali metal
bath
silicofluoride
sulfate
chromium
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US356188A
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Jesse E Stareck
Dow Ronald
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United Chromium Inc
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United Chromium Inc
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Priority to US356188A priority Critical patent/US2686756A/en
Priority to DEU2742A priority patent/DE1040338B/de
Priority to GB12351/54A priority patent/GB771925A/en
Priority to FR1110280D priority patent/FR1110280A/fr
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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
    • C25D3/04—Electroplating: Baths therefor from solutions of chromium

Definitions

  • This invention relates to chromium plating using a chromic acid plating bath having a selfregulated catalyst acid radical content.
  • the invention particularly relates to a method for producing crack-free deposits of chromium.
  • crack-free chromium plate can be deposited by maintaining, over a range of chromic acid concentration, a particular and well defined range of concentration of the catalyst acid radicals, as hereinafter described, and
  • the present method is applicable to general chromium plating, such as described in said copending application. It is particularly applicable to the plating of metals that are subject to -]corrosion, such as steel, and has special applil cation to the deposition of decorative plate which heretofore required corrosion resistant undercoats of nickel, or copper, or nickel and copper, etc.
  • attempts to deposit decorative chromium plate having the usual thickness of this type of plate in the absence of a protective undercoat results in a porous, noncorrosion resistant plate which does not cover the pores in the surface of the basis metal; on the other hand, the deposition directly on the basis metal of chromium plate of greater thickness results in a cracked plate which is not corrosion resistant.
  • the bumper may 1 be plated with 2mils of nickel and 0.01 mil of chromium; or with l mil of copper, 1 mil of nickel, and 0.01 mil of chromium; or with 1 mil ofcopper, 2.0 mils of nickel and 0.01 mil of the decorative plate range, viz. 0.01 to 0.02 mil. 6
  • the present chromium plate as the coating, a harder finish is provided which is desirable for many kinds of articles, and the plate can be buffed to a bright appearance where brightness is required. It will also be apparent that the present plate can be deposited in place of conventional chromium plate, that is, over conventional undercoats, and in such cases a corrosionresistant product is obtained which is superior to the conventional product and whose total deposit (undercoats plus chromium) as thinner.
  • Crack-free plate, particu arly heavy plate, but including other kinds as well, can be produced on parts and articles useful in engineering applications such as on chemical and manufacturing equipment, engine and machine parts, and the like, in order to meet unusual problems of corrosion and erosion, wear and abrasion, temperature efiects, etc.
  • The'bath solution used in the method comprises chromic acid, two catalyst-supplying compounds, namely, a sulfate radical bearing salt and a. silicofiuoride radical bearing salt, each having a limited solubility in the chromic acid bath, and two soluble non-catalytic compounds one of which is a, compound of the cation. associated with the sulfate salt and the other of which is a compound of the cation associated with the silicofluoride salt.
  • the non-catalytic compounds have the effect of controlling the concentrations of the dissolved sulfate and silicofluoride radicals in the bath by influencing the solubility of the salts used to introduce the radicals into the bath.
  • the specific catalyst-supplying compounds are strontium sulfate and an alkali metal silicoiluoride, the alkali metal being selected from the class consisting of potassium and sodium.
  • Specific non-catalytic compoiuids are strontium carbonate, strontium oxide, strontium chromate, strontium hydroxide, potassium hydroxide, potassium bichromate, potassium carbonate, potassium chromate, sodium. bichromate, sodium carbonate, sodium hydroxide, sodium chromate.
  • the concentration of the chromic acid, expressed as CrOe, in the bath is about 200 to 900 g./l.
  • the amount of the strontium sulfate and of the alkali metal silicofluoride is, in each case, sufficient to saturate the bath with dissolved sulfate and silicofluoride and to provide an insoluble residue of each salt in the bath.
  • the soluble non-catalytic strontium and alkali metal compounds are each present in an amount sufiicient to adjust or suppress the concentration of the strontium sulfate and alkali metal silicofiuoride, respectively, in solution in the bath from the unsuppressed saturation concentration of the latter two compounds to a lower concentration equivalent to 1.5 to 11.7 g./l.
  • the concentration of dissolved sulfate may vary from 0.3 to 5.5 g./l. and that of dissolved silicofluoride from 1.0 to 11.4 g./l., with the sum of the two catalysts lying in the range of 1.5 to 11.7 g./l.
  • the sum of the dissolved sulfate and silicofiuoride required varies with the dissolved CIOs in the manner defined by the area ABCD of the graph shown in the accompanying drawing.
  • the graph shows the variation of the chromic acid concentration in grams per liter with the concentration, in grams per liter, of the sum of dissolved sulfate and silicofiuoride.
  • the chromic acid varies from 200 to 900 g./l.
  • the required catalyst content varies from a low of 1.5 g./l. to a high of 11.7 g./l.
  • the plate that is deposited is crack-free and has the other advantages described hereinafter.
  • the plate is nodular and unsuitable.
  • Table 1 which also shows how the sulfate and
  • the amounts of the non-catalytic strontium and alkali metal compounds are such as to suppress the concentration of the strontium sulfate and alkali metal silicofiuoride, respectively, in solution in the bath from the unsuppressed D
  • the plate is cracked, and at catasaturation concentration of the latter two compounds to a lower concentration equivalent to 1.9 to 7.6 g./l.
  • the preferred concentration of dissolved sulfate may vary 0.3 to 4.5 g./l. and that of dissolved silicofiuoride from 1.5 to 6.3 g./l. with the preferred sum of the two catalysts lying in the range of 1.9 to 7.6 g./l.
  • the preferred variation of the sum of the dissolved catalyst radicals with the CrOe concentration therefore, is as defined by the area JKLM of the graph, and is also set forth in the following Table 2:
  • the concentration of sulfate should exceed that of silicofiuoride in the area EBF of the graph and that the concentra- Sum of S04 and SiFa CrOa, g./l. Range in Range in which $04 which Sil a shoulgl exceed should exceed F5 so.
  • the chromic acid content may be supplied by adding chromic acid as such to the bath, although chromate, sodium bichromate, strontium chromate, etc. It will be understood that in referring to the bath chromic acid content, it is intended to include, unless specified otherwise, the ClOa added per se and any CIO3 added in the form of one of the foregoing non-catalytic compounds.
  • the plating bath may be made up by adding a mixture of the solid ingredients, in subdivided form, to water and stirring until equilibrium is obtained.
  • the bath may also be maintained in thisway.
  • the plating method comprises passing current in the range of 0.5 to 8, preferably 1 to 3, amperes per square inch (A. S. I.) from an anode to an article cathode immersed in the bath.
  • the bath is operated at a minimum temperature of F., it having been found that below this temperature the plate that is produced is cracked.
  • the upper temperature may extend to the boiling point of the bath but prefhigher, and higher current densities are used.
  • the crack-free quality of the chromium plate produced by the present method is not only determinable visually but also by means of other tests, one of which is the Dubpernell test for detecting cracks in chromium plate as described in Baker et al., S. A. E. Journal, 22pages 321-334, note page 334 (March 1928) Baker et al., Trans. Am. Electro-Chem. Soc., 54 pages 337-346, note page 338 (September 22, 1928).
  • acid copper is plated on the chromium plated article, and if there are any cracks in the chromium plate, the copper will deposit preferentially in them. This test showed the present plate to be crack-free.
  • Another test is microscopic examination, using from to 200 power magnification. No cracks were found in the present plate by microscopic examination.
  • Another test is the anodic etch test in which, with the chromium plated article as the anode, chromium is dissolved away from the article; if cracks are present or incipient, they are developed during this test and become readily visible. Even on anodic etching, the present plate showed no cracks.
  • the crack-free plate of the invention is also characterized by having a hardness of about 425 to about 825, usually 550 to 700, Knoop.
  • the plate is relatively soft and ductile as compared with conventional chromium plate. It has a smooth texture, a satiny finish, and a dull, matte, white color. It is easy to polish or bufi.
  • EXAMPLE 1 A solid, finely divided mixture was made up consisting of 50% CrOs, 26.25% potassium dichromate, 5.25% strontium chromate, 12.5% potassium silicofiuoride, and 6.0% strontium sulfate, these percentages being on a weight basis.
  • the ClOs content was equivalent to the'total hexavalent chromium in solution.
  • a mild or low carbon steel rod was plated in this solution at 140 F. for 2 hours using 3 A. S. I.
  • anodic etching was carried out by making the rod anode in the same solution and passing 2.5 A. S. I. for 10 minutes; inspection of the chromium plate with a 10-power microscope showed that it was crack-free.
  • EXAMPLE 2 A mixture was prepared consisting of, on a weight basis, 34.4% CrOs, 61.9% sodium dichromate, 2.0% strontium chromate, 1.1% sodium silicofiuoride, and 0.6% strontium sulfate.
  • EXAMPLE 4 A sheet steel panel, 3" x 4", identified as No. l, was plated in a commercial chromium plating hath made from chromic acid, potassium silicofiuoride, strontium sulfate, potassium dichromate, and strontium chromate, and having 204.0 g./l., of dissolved CIOs, 12.8 g./l. of dissolved potassium silicofiuoride, and 6.2 g./l. of dissolved strontium chromate; the bath temperature was 120 F. and the current density 2 A. S. I. A thickness of approximately 0.3 mil of chromium was plated on the panel. At the same time three sheet steel panels (Nos.
  • EXAMPLE 5 Fifteen sheet steel panels, identified by the letters A to 0, were plated in various ways, described below, and subjected to outdoor exposure tests. Following the exposure, the ap pearance and condition of the exposed side of each panel was noted and is briefly described in the following table.
  • Panels A to F were chromium plated directly, panels A and D in the same commercial chro- 7" mium plating'batht and using, the same bath c n ditions as. described in Example 4-, and: panels B; C; E: and E according to the method of Ex ample, 2;. Panels 6- and. F were buffed following the plating. The six panels were subjected to outdoor exposure for; 142 days in Detroit, the time of the exposure being from January to May, a time of the year when corrosion is most severe.
  • a second group. of panels identified as G, H and I were, conventionally plated with undercoatsbefore being chromium plated by the method of Example 2.
  • Panel G was plated first with copper, then with nickel, and then with chromium;
  • panel H was plated with nickel, then chromium;
  • panel I With copper followed by chromium. This group of panels was exposed out-of-doors in Detroit during January to June for. 177 d ys. v
  • Panels J K and L were conventionally plated with copper and then with conventional chromium plate, using the conventional bath and conditions described at the end of Example 4, While panels. M, N and 0 were conventionally plated with copper. then with nickel, and then with the conventional chromium plate. Panels J. to 0- were all. exposed out-of-doors in Detroit during January to, June for 1 77 days.
  • EXAMPLE 7 A mixture comprising 54.7% chromic acid, 33.2% potassium dichromate, 8.6% strontium chromate, 2.5% potassium silicofiuoride, and 0.9% strontium sulfate, all percentages being by weight, was prepared and added to water to pro! vide a solution having 200 g./l. of dissolved CrOa. 2.8 g./l. of dissolved silicofluoride, and 0.5 g./l-. of dissolved sulfate. A steel mandrel, 4- long x diameter, was plated in this solution at 6 A. S. I. for one hour at 160 F., a crack-free chromium deposit being produced that was dull and smooth. The thickness of the deposit was 2.5 mils.
  • the plated mandrel was then anodical. 1y treated in the same solution at 1 A. S. I. for 5 minutes to develop any crack structure that might be present, but no cracks were found.
  • Another mandrel of the same size as the preceding one was then plated in the same bath solution at 8 A. S. I. for 0.5 hour at 180 F., there being produced on the mandrel a crack-free deposit of 35 chromium that was dull and smooth and had a Chromium plate Undercmt' thickness, mils Outdoor Panel. 7 r V expo- Thick- P C M f Remarks Metal: mess rior rae ree ays mils Plate ate A 0.2 142 Entire area heavily rusted Fr, 0.5 buffed. 142
  • Example 5 Whether plated directly on the basis metal or over undercoats, it will be seen from Example 5 that the crack-free plate, of the invention is superior to the prior plate.
  • weight percentages of the ingredientsof the solid mixture for making up the bath solution can also be expressed as parts by weight.
  • Deposits of varying thicknesses may be plated by the present method, ranging for example from a thickness just sufiicient to cover the pores of the basis metal to any practical desired thicker deposit for which a demand may exist.
  • the invention is useful for articles made of any of a variety of basis metals, such as plain carbon steels, alloy steels including stainless steel, iron, cast iron, copper and copper alloys, nickel and nickel alloys, zinc and zinc alloys, alumium and alumium alloys, tin and tin alloys, lead and lead alloys, etc.
  • basis metal may be any metal, or an undercoat on a metal, that can be chromium plated.
  • a method of electrodepositing crack-free, chromium plate on an article of metal which comprises essentially: passing current in the range of 0.5 to 8 amperes per square inch from an anode to said article as a cathode immersed in an aqueous chromium plating bath at a temperature of 140 F. to the boiling point of the bath, said bath comprising essentially 200 to 900 g./l.
  • strontium sulfate and an alkali metal silicofluoride each in an amount sufiicient to saturate said bath and to provide therein an undissolved residue of strontium sulfate and alkali metal silicofiuoride, respectively, said alkali metal being selected from the class consisting of potassium and sodium, a soluble non-catalytic strontium compound in an amount sufficient to adjust the concentration of the strontium sulfate in solution in said bath to 0.3 to 5.5 g./l.
  • a method according to claim 1 in which the metal article that is chromium plated is an article of plain carbon steel.
  • chromium plate on a metal article which comprises essentially: passing current in the range of 1 to 3 amperes per square inch from'an anode to said article as a cathode immersed in an aqueous chromium plating bath at a temperature of 145 to 155 F., said bath comprising essentially 200 to 900 g./l.
  • strontium sulfate and an alkali metal silicofluoride each in an amount sufiicient to saturate said bath and to provide therein an undissolved residue of strontium sulfate and alkali metal silicofluoride, respectively, said alkali metal being selected from the class consisting of potassium and sodium, a soluble non-catalytic strontium compound in an amount sufficient to suppress the concentration of the strontium sulfate in solution in said bath from the unsuppressed saturation concentration of the latter to a lower concentration equivalent to 0.3 to 4.5 g./l.
  • sulfate (S05) sulfate
  • a soluble non-catalytic alkali metal compound in an amount sufficient to suppress the concentration of the alkali metal silicofluoride in solution in said bath from the unsuppressed saturation concentration of thelatter to a lower concentration equivalent to 1.5 to 6.3 g./l.
  • silicofiuoride SiFeF
  • the sum of said dissolved sulfate and silicofluoride being in, the range of 1.9 to 7.6 g./l., said sum of dissolved sulfate and silicofluoride varying with the CrOs concentration in the manner defined by the area JKLM of the graph shown in the accompanying drawing, the alkali metal of said non-catalytic compound being the same as the alkali metal of said alkali metal silicofiuoride.
  • alkali metal silicofiuoride is potassium silicofluoride and the alkali metal compound is a potassium compound.
  • alkali metal silicofluoride is sodium silicofluoride and the alkali metal compound is a sodium compound.
  • a method of electrodepositing crack-free, chromium plate on a metal article which comprises essentially: passing current in the range of 0.5 to 8 amperes per square inch from an anode to said article as a cathode immersed in an aqueous chromium plating bath at a temperature of to F., said bath comprising essentially 200 to 900 g./l.
  • strontium sulfate and an alkali metal silicoi'luoride each in an amount sufficient to saturate said bath and to provide therein an undissolved residue of strontium sulfate and alkali metal silicofluoride, respectively, said alkali metal being selected from the class consisting of potassium and sodium, a soluble non-catalytic strontium compound and a soluble non-catalytic alkali metal compound each in an amount sufficient to suppress the ooncentration of the strontium sulfate and alkali metal silicofluoride, respectively, in solution in said bath from the unsuppressed saturation concentration of the latter two compounds to a lower concentration equivalent to 1.5 to 11.7 g./l.
  • An improved method of producing a corrosion resistant chromium plated metal article cornprising plating the unplated article, in a single plating operation, in an aqueous bath comprising essentially 200 to 900 g./l. CrO3, strontium sulfate and an alkali metal silicofiuoride each in an amount sufficient to saturate said bath and to provide therein an undissolved residue of strontium sulfate and alkali metal silicofluoride, respectively, a soluble non-catalytic strontium compound and a soluble non-catalytic alkali metal compound each in an amount sufiicient to suppress the concentrations of the strontium sulfate and alkali metal silicofluoride, respectively, in solution in said bath from the unsuppressed saturation concentrations of the latter two compounds to lower concentrations equivalent to 0.3

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  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Electroplating Methods And Accessories (AREA)
US356188A 1953-05-20 1953-05-20 Chromium plating Expired - Lifetime US2686756A (en)

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US356188A US2686756A (en) 1953-05-20 1953-05-20 Chromium plating
DEU2742A DE1040338B (de) 1953-05-20 1954-04-22 Verfahren zur elektrolytischen Herstellung rissfreier Chromueberzuege auf Metallgegenstaenden
GB12351/54A GB771925A (en) 1953-05-20 1954-04-28 Electro-deposition of chromium plate
FR1110280D FR1110280A (fr) 1953-05-20 1954-05-20 Procédé de chromage électrolytique

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2787589A (en) * 1954-08-12 1957-04-02 Metal & Thermit Corp Chromium plating
US2787588A (en) * 1954-08-12 1957-04-02 Metal & Thermit Corp Chromium plating
US2800436A (en) * 1955-07-26 1957-07-23 Metal & Thermit Corp Method of chromium plating
US2800443A (en) * 1955-07-26 1957-07-23 Metal & Thermit Corp Method of chromium plating
US2800437A (en) * 1955-07-26 1957-07-23 Metal & Thermit Corp Chromium plating
US2800438A (en) * 1955-07-26 1957-07-23 Metal & Thermit Corp Chromium plating
US2907273A (en) * 1953-11-12 1959-10-06 Chrome Steel Plate Corp Lithographic plates
US2916424A (en) * 1957-11-07 1959-12-08 Metal & Thermit Corp Process for chromium plating
DE1078840B (de) * 1956-12-24 1960-03-31 Deinert & Co Spezialbetr E Fue Verwendung von galvanisch abgeschiedenen Chromueberzuegen
US2950234A (en) * 1958-02-26 1960-08-23 Metal & Thermit Corp Chromium plating process and bath
US3151048A (en) * 1960-02-18 1964-09-29 Clevite Corp Method of making copper foil, and the apparatus therefor
US3418220A (en) * 1963-08-26 1968-12-24 Roggendorf Wilhelm Electrodeposition of chromium and duplex micro-crack chromium coatings
US6197183B1 (en) * 2000-02-18 2001-03-06 Richard C. Iosso Electrodeposition bath for wear-resistant zinc articles
EP1133220A2 (de) * 2000-03-10 2001-09-12 Olin Corporation Kupferfolie mit Niedrigprofil-Adhäsionsverbesserung
CN102712254A (zh) * 2010-01-23 2012-10-03 约翰逊控制技术公司 装饰元件、仪表板和用于制造装饰元件的方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2640022A (en) * 1950-11-07 1953-05-26 United Chromium Inc Composition, bath, and process for chromium plating

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2640022A (en) * 1950-11-07 1953-05-26 United Chromium Inc Composition, bath, and process for chromium plating

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2907273A (en) * 1953-11-12 1959-10-06 Chrome Steel Plate Corp Lithographic plates
US2787588A (en) * 1954-08-12 1957-04-02 Metal & Thermit Corp Chromium plating
US2787589A (en) * 1954-08-12 1957-04-02 Metal & Thermit Corp Chromium plating
US2800436A (en) * 1955-07-26 1957-07-23 Metal & Thermit Corp Method of chromium plating
US2800443A (en) * 1955-07-26 1957-07-23 Metal & Thermit Corp Method of chromium plating
US2800437A (en) * 1955-07-26 1957-07-23 Metal & Thermit Corp Chromium plating
US2800438A (en) * 1955-07-26 1957-07-23 Metal & Thermit Corp Chromium plating
DE1078840B (de) * 1956-12-24 1960-03-31 Deinert & Co Spezialbetr E Fue Verwendung von galvanisch abgeschiedenen Chromueberzuegen
DE1122344B (de) * 1957-11-07 1962-01-18 Metal & Thermit Corp Verfahren zum elektrolytischen Abscheiden von glaenzenden rissfreien Chromueberzuegen
US2916424A (en) * 1957-11-07 1959-12-08 Metal & Thermit Corp Process for chromium plating
US2950234A (en) * 1958-02-26 1960-08-23 Metal & Thermit Corp Chromium plating process and bath
US3151048A (en) * 1960-02-18 1964-09-29 Clevite Corp Method of making copper foil, and the apparatus therefor
US3418220A (en) * 1963-08-26 1968-12-24 Roggendorf Wilhelm Electrodeposition of chromium and duplex micro-crack chromium coatings
US6197183B1 (en) * 2000-02-18 2001-03-06 Richard C. Iosso Electrodeposition bath for wear-resistant zinc articles
EP1133220A2 (de) * 2000-03-10 2001-09-12 Olin Corporation Kupferfolie mit Niedrigprofil-Adhäsionsverbesserung
EP1133220B1 (de) * 2000-03-10 2011-05-11 GBC Metals, LLC Kupferfolie mit Niedrigprofil-Adhäsionsverbesserung
CN102712254A (zh) * 2010-01-23 2012-10-03 约翰逊控制技术公司 装饰元件、仪表板和用于制造装饰元件的方法
US20130059108A1 (en) * 2010-01-23 2013-03-07 Johnson Controls Technology Company Decorative element, dashboard, and method for manufacturing a decorative element
US8822007B2 (en) * 2010-01-23 2014-09-02 Johnson Controls Technology Company Decorative element, dashboard, and method for manufacturing a decorative element
CN102712254B (zh) * 2010-01-23 2016-10-05 约翰逊控制技术公司 装饰元件、仪表板和用于制造装饰元件的方法

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GB771925A (en) 1957-04-10
FR1110280A (fr) 1956-02-10

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