US3338725A - Novel plating process and composition - Google Patents

Novel plating process and composition Download PDF

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Publication number
US3338725A
US3338725A US367570A US36757064A US3338725A US 3338725 A US3338725 A US 3338725A US 367570 A US367570 A US 367570A US 36757064 A US36757064 A US 36757064A US 3338725 A US3338725 A US 3338725A
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United States
Prior art keywords
stannate
bath
potassium
alkali metal
tin
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Expired - Lifetime
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US367570A
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English (en)
Inventor
Clarence K Banks
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M&T Chemicals Inc
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M&T Chemicals Inc
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Publication date
Application filed by M&T Chemicals Inc filed Critical M&T Chemicals Inc
Priority to US367570A priority Critical patent/US3338725A/en
Priority to IL23441A priority patent/IL23441A/xx
Priority to CH628565A priority patent/CH471901A/de
Priority to NL6505834A priority patent/NL6505834A/xx
Priority to JP40027155A priority patent/JPS4927015B1/ja
Priority to GB20260/65A priority patent/GB1110770A/en
Priority to SE6272/65A priority patent/SE304150B/xx
Priority to FR17038A priority patent/FR1433207A/fr
Priority to DEP1270A priority patent/DE1270920B/de
Application granted granted Critical
Publication of US3338725A publication Critical patent/US3338725A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C18/00—Chemical 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
    • C23C18/16—Chemical 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
    • C23C18/31—Coating with metals

Definitions

  • the thickness of the tin layer deposited on aluminum by this process and the rate of deposition thereof increases at an undesirably high rate with increase of free alkali content. It is desirable to be able to control the thickness and rate of deposit and to operate the process so that the resulting plate meets a specified minimum thickness, but does not exceed a predetermined maximum thickness.
  • the stannic hydroxide sludge once formed, may be substantially impossible to redissolve during normal operation of the immersion tinning bath and represents lost tintA loss of tin (of as much as 25% of the tin present) in the form of sludge is not uncommon and this depletion considerably decreases the life of the bath. Furthermore, sludge particles in the bath may adhere to the surface of the work resulting in an unsatisfactory surface finish. Often the baths are prematurely discarded since sludge may build-up to such an extent that making up a new solution may be more economical than trying to rectify the old one.
  • condensed phosphates such as pyrophosphates and polyphosphates
  • pyrophosphates and polyphosphates may be employed to reduce problems of sludging and free hydroxide build-up.
  • these compounds must be present in the plating bath in relatively high concentrations. It may also be found that baths containing the condensed phosphates do not satisfactorily plate certain aluminum alloys, particularly those which contain a high percentage of copper.
  • the process of this invention for treating aluminum to form a surface layer of tin thereon may comprise immersing said aluminum in an aqueous bath containing a stannate salt selected from the group consisting of sodium stannate and potassium stannate, an alkali metal polyphosphate, and at least one soluble organic compound selected from the group consisting of alkylene polyamines, aminomonocarboxylic acids and aminoalcohols; maintaining said aluminum in said bath for time sufficient to deposit a surface layer of tin thereof; and withdrawing said aluminum from said bath.
  • a stannate salt selected from the group consisting of sodium stannate and potassium stannate
  • an alkali metal polyphosphate an alkali metal polyphosphate
  • at least one soluble organic compound selected from the group consisting of alkylene polyamines, aminomonocarboxylic acids and aminoalcohols
  • this invention provides novel alkaline aqueous immersion tinning baths comprising a stannate salt selected from the group consisting of sodium stannate and potassium stannate; an alkali metal polyphosphate; and at least one soluble organic compound selected from the group consisting of alkylene polyamines, aminocarboxylic acids and aminoalcohols.
  • the aluminum which may be treated by the practice of this invention may be commercially pure aluminum or an alloy of aluminum. Typical of such alloys may be those containing copper, magnesium, or both copper and magnesium.
  • One of the more common aluminum alloys which may be treated by the process of this invention may contain 2%-4%, say 3% copper, 1%1.5%, say 1.5% magnesium, 9%13%, say 10% silicon, and quantities of other metals such as zinc, iron, and nickel.
  • Such alloys are commonly used for the fabrication of aluminum pistons.
  • a specific illustration of one of these alloys may be that identified as Permanent Mold Casting Alloy D132 containing 3% copper, 1% magnesium, 10% silicon, 0.5% manganese, 0.5% zinc, and the remainder essentially aluminum.
  • the technique of this invention may be particularly advantageous for plating on higher copper alloys, e.g. permanent mold casting alloys containing greater than about 3.5% copper.
  • the immersion baths which may be used in practice of this invention may typically be made up by dissolving potassium stannate and/ or sodium stannate in water to form a bath containing from about 15 g./l. (grams per liter) to saturation, typically about 70 g./l. of the stannate salt, the resulting solution containing about 30 g./l. of tin.
  • Sufficient potassium hydroxide and/ or sodium hydroxide may be initially added to form a bath containing about 4 g./l. of the alkali metal hydroxide to prevent precipitation of tin due to low pH during makeup.
  • the free alkali metal hydroxide may be maintained between about 0.5 g./l.
  • the baths of this invention may contain an alkali metal polyphosphate.
  • Typical alkali metal polyphosphates which may be employed include sodium hexametaphosphate, tetrasodium pyrophosphate, sodium tripolyphosphate, potassium hexametaphosphate, tetrapotassium pyrophosphate,
  • potassium tripolyphosphate etc.
  • Sodium tripolyphosphate and potassium tripolyphosphate may be preferred.
  • the alkali metal polyphosphate may preferably be present in the plating bath in the concentration of about 1. -5 grams per liter (g./l.).
  • the novel baths may also contain at least one soluble organic compound selected from the group consisting of alkylene polyamines, aminomonocarboxylic acids, and amino-alcohols.
  • Alkylene polyamines may include alkylene diamines, alkylene triamines, alkylene tetra-amines, etc.
  • Suitable illustrative alkylene polyamines may include ethylenediamine, propylenediamine, butylenediamine, ethylenediamine, tetramethylenediamine, pentamethylenediamine, hexamethylenediamine, diethylenediarnine (piperazine), diethylenetriamine, etc.
  • Illustrative aminomonocarboxylic acids suitable for use in this invention may include glycine, alanine, valine, leucine, isoleucine, phenylalanine, proline, tryphophan, arginine, lysine, histidine, flaalanine, ot-aminobutyric acid, 'y-aminobutyric acid, a,y-diaminobutyric acid, Ornithine, etc. If desired, these materials may be employed in the form of their salts, typically as sodium or potassium salts.
  • Illustrative aminoalcohols which may be employed may include ethanolamine, diethanolamine, triethanolamine,
  • the soluble organic compound will be present in the bath in the amout of about 0.01-0.25 mole per liter, preferably about 0.1 mole/l. Smaller amounts may be used, but may not provide as great an improvement in these baths. Larger amounts may also be used, but little or no additional improvement may be realized thereby.
  • Immersion plating in accordance with this invention may be carried out between room temperature of e.g. 20 C. and 90 C., and preferably between 40 C. and 80 C., say 60 C. Immersion time may be as little as 30 seconds, but it is usually between 1-6 minutes, say 4 minutes. During this time, aluminum may be coated with a layer of tin of desired thickness, typically of the order of 1-4 microns.
  • novel baths of this invention may typically be prepared initially by dissolving about 1.5-5 grams of alkali metal polyphosphate, say sodium tripolyphosphate; 0.01- 0.25 mole, say 0.1 mole of the hereinbefore described soluble organic compound, say ethylenediamine or triethanolamine; 0.512 grams, say 4 grams of alkali metal hydroxide, say potassium hydroxide; and 15 grams to saturation, say 70 grams of stannate salt, say potassium stannate in suflicient water to give one liter of solution. Because of drag-out and depletion of tin through plating, it will be necessary periodically, to make additions to the bath during operation.
  • alkali metal polyphosphate say sodium tripolyphosphate
  • 0.01- 0.25 mole say 0.1 mole of the hereinbefore described soluble organic compound, say ethylenediamine or triethanolamine
  • alkali metal hydroxide say potassium hydroxide
  • 15 grams to saturation say 70 grams of stannate salt, say potassium stannate in suflicient
  • novel baths of this invention maintain a pH at the desired operating level, it may not be necessary to add either additional alkali metal hydroxide or neutralizing agent during operation.
  • Stannate salt may be added at a rate sufficient to make up for the loss of stannate in the bath through plating and because of drag-out.
  • the soluble organic compound and alkali metal polyphosphate may be added at a rate sufficient to compensate for drag-out.
  • Each of these components may be added separately, but preferably they may be added together. It may be found that the desired balance may be maintained in the bath by adding thereto a composition comprising about 7098 parts by weight stannate salt, 1-17 parts by weight of the noted soluble organic compound, and 1-14 parts by weight of the alkali metal polyphosphate.
  • the composition employed to maintain the novel baths may comprise 80-96 parts by weight stannate salt, 2-10 parts by weight soluble organic compound, and 2l0 parts by weight alkali metal polyphosphate.
  • compositions which may be employed to maintain the novel baths of this invention may include the following wherein the parts are parts by weght.
  • Potassium stannate Ethylene diamine 10 Potassium tripolyphosphate 5 Sodium stannate 87 Butylenediamine 8 Sodium tripolyphosphate 5 Potassium stannate 93
  • Diethylenediamine 4 Tetrapotassium pyrophosphate 3
  • Sodium stannate 74 Diethylenetriamine 15 Tetrasodium pyrophosphate 11
  • Glycine (K salt) 16 Potassium hexametaphosphate 5 Sodium stannate 88
  • [i-Alanine (Na salt) 6 Sodium tripolyphosphate 6 Potassium stannate 94
  • Leucine 3 Sodium hexametaphosphate 3
  • Proline 1 2 Potassium tripolyphosphate 1 Potassium stannate 8O Lys
  • Example 16 Four separate immersion tinning baths may be made up by dissolving 8 grams of potassium hydroxide and 140 grams of potassium stannate in about 1.5 liters of water, and diluting the resulting solutions to 2 liters with water. Prior to this dilution, the following materials are added to the solution and dissolved therein:
  • baths After dilution to 2 liters, all of the baths contain 70 g./l. potassium stannate, and 4 g./l. potassium hydroxide.
  • Bath A the control, contains no polyphosphate or soluble organic compound of this invention.
  • Baths B, C and D are prepared in accordance with this invention to contain:
  • Each of the baths may be heated to and maintained at 60 C.
  • three pieces of D-l32 aluminum 3 x 6 x A" may be degreased in trichloroethylene vapor, dipped for seconds in a solution of 30 g./l. of trisodium phosphate and 30 g./l. of sodium carbonate at 60 C., rinsed in cold water, dipped for 30 seconds in a mixture of one part of concentrated nitric acid and 3 parts of water, rinsed in cold water, and immersed in thetwo-liter bath for 4 minutes to deposit thereon a layer of tin.
  • the aluminum panels may then be withdrawn, rinsed, and the tin deposit stripped from them by immersing for one minute in the nitric acid solution, and rinsing under a stream of cold water.
  • the parts are then ready for the second dip in the baths.
  • a series of 10 successive dips and strippings is considered as one cycle, and the surface area plated in each cycle is 36.8 square decimeters per liter.
  • the baths may be analyzed for free hydroxide and tin, and the tin content brought up to 28 g./l. by addition of the following maintenance compositions.
  • suflicient maintenance composition is added to bring the tin content of the bath back to 28 g./l.
  • the thickness of tin plated may be determined by weighing a panel before and after stripping in nitric acid.
  • Bath A which is typical of prior art practice, shows a rapid increase in free hydroxide. After 2 cycles, the free hydroxide rises to 4.9 g./l.; after 5 cycles it is 8.5 g./l.; and after 6 cycles it is 9.8 g./l.
  • the thickness of tin deposited also undesirably increases to 157 x10 inches .after 2 cycles, 167 l0- inches after 4 cycles and 6 18 6 lO inches after 6 cycles.
  • the tin plate is streaky, gray and of generally poor appearance. A large quantity of sludge is formed during the test.
  • Baths B, C, and D which are operated in accordance with this invention, give smooth, adherent deposits with little streaking and good appearance throughout the test.
  • the thickness of tin deposited may fall within the range of 701l5 10 inches after each cycle. It may be found that the free hydroxide content of the bath reaches an equilibrium value in the range 1.6-3 g./ 1. Much less sludge is produced in these baths than in Bath A.
  • Bath A in accordance with prior art techniques, is characterized by streaky, gray plate, build-up of free hydroxide, excessive sludging, and lack of control over the thickness of tin plated.
  • Baths B, C and D illustrate the advantages obtained by use of the baths and processes of this invention, including good control of deposit thicknesses, little sludging, control of free hydroxide content, and smooth deposits of good appearance.
  • the process for treating aluminum to form -a surface layer of tin thereon which comprises immersing said aluminum in an aqueous bath containing a stannate salt selected from the group consisting of sodium stannate and potassium stannate, an alkali metal polyphosphate, and at least one soluble organic compound selected from the group consisting of alkylene polyamines, aminomonocarboxylic acids and aminoalcohols; maintaining said aluminum in said bath for time sufficient to deposit a surface layer of tin thereon; and withdrawing said aluminum from said bath.
  • a stannate salt selected from the group consisting of sodium stannate and potassium stannate
  • an alkali metal polyphosphate an alkali metal polyphosphate
  • at least one soluble organic compound selected from the group consisting of alkylene polyamines, aminomonocarboxylic acids and aminoalcohols
  • stannate salt selected from the group con-' sisting of sodium stannate and potassium stannate, 0.5-12 g./l. alkali metal hydroxide, 1.5-5 g./l. alkali metal polyphosphate, 0.01-0.25 mole/l. of at least one soluble organic compound selected from the group consisting of alkylene polyamines, aminomonocarboxylic acids and aminoalcohols, maintaining said bath at 40-80 C. during said immersion; maintaining said aluminum in said bath for time sufficient to deposit a surface layer of tin thereon; and withdrawing said aluminum from said bath.
  • a novel alkaline aqueous immersion tinning bath comprising a stannate salt selected from the group consisting of sodium stannate and potassium stannate; an alkali met-a1 polyphosphate; and at least one soluble organic compound selected from the group consisting of alkylene polyamines, aminomonocarboxylic acids and aminoalcohols.
  • novel alkaline aqueous immersion tinning bath of claim 3 which comprises 1.5-5 g./l. of said alkali metal polyphosphate.
  • novel alkaline aqueous immersion tinning bath of claim 3 which comprises 0.01-0.25 mole/l. of said soluble organic compound.
  • the novel alkaline aqueous immersion tinning bath which comprises 15 g./l. to saturation of a stannate salt selected from the group consisting of sodium stannate and potassium stannate; 0.5-12 g./l. alkali metal hydroxide; 1.5-5 g./1. alkali polyphosphate; and 0.01-0.25 mole/l. of at least one soluble organic compound selected from the group consisting of alkylene polyamines, aminomonocarboxylic acids and aminoalcohols.
  • a novel composition for use in maintaining alkaline aqueous immersion tinning bath which comprises a stannate salt selected from the group consisting of sodium stannate and potassium stannate; an alkali metal polyphosphate; and at least one soluble organic compound selected from the group consisting of alkylene polyamines, aminomonocarboxylic acids and arninoalcohols.
  • the novel composition for use in maintaining alkaline aqueous immersion tinning bath which comprises 70-98 parts of a stannate salt selected from the group consisting of sodium stannate and potassium stannate; 1-14 parts of an alkali metal polyphosphate; and l-17 parts of at least one soluble organic compound selected from the group consisting of alkylene polyamines, aminomonocarboxylic acids and arninoalcohols.
  • the novel composition for use in maintaining alkaline aqueous immersion tinning bath which comprises 80-96 parts of a stannate salt selected from the group consisting of sodium stannate and potassium stannate; 21O parts of an alkali metal polyphosphate; and 2-10 parts of at least one soluble organic compound selected from the group consisting of alkylene polyamines, aminomonocarboxylic acids and arninoalcohols.
  • a composition comprising a stannate salt selected from the group consisting of sodium stannate and potassium stannate; an alkali metal polyphosphate; and at least one soluble organic compound selected from the group consisting of alkylene polyamines, aminomonocarboxylic acids and aminoalcohol.

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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)
  • Chemically Coating (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
US367570A 1964-05-14 1964-05-14 Novel plating process and composition Expired - Lifetime US3338725A (en)

Priority Applications (9)

Application Number Priority Date Filing Date Title
US367570A US3338725A (en) 1964-05-14 1964-05-14 Novel plating process and composition
IL23441A IL23441A (en) 1964-05-14 1965-04-28 A process and composition for tinning aluminum and aluminum alloys
CH628565A CH471901A (de) 1964-05-14 1965-05-06 Verfahren zur Tauchverzinnung von Aluminium oder einer Aluminiumlegierung
NL6505834A NL6505834A (de) 1964-05-14 1965-05-07
JP40027155A JPS4927015B1 (de) 1964-05-14 1965-05-11
GB20260/65A GB1110770A (en) 1964-05-14 1965-05-13 Improvements in or relating to immersion plating
SE6272/65A SE304150B (de) 1964-05-14 1965-05-13
FR17038A FR1433207A (fr) 1964-05-14 1965-05-14 Procédé d'étamage par immersion et compositions pour sa mise en oeuvre
DEP1270A DE1270920B (de) 1964-05-14 1965-05-14 Bad fuer die Tauchverzinnung von Aluminium oder Aluminiumlegierungen

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Application Number Priority Date Filing Date Title
US367570A US3338725A (en) 1964-05-14 1964-05-14 Novel plating process and composition

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US3338725A true US3338725A (en) 1967-08-29

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US367570A Expired - Lifetime US3338725A (en) 1964-05-14 1964-05-14 Novel plating process and composition

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US (1) US3338725A (de)
JP (1) JPS4927015B1 (de)
CH (1) CH471901A (de)
DE (1) DE1270920B (de)
GB (1) GB1110770A (de)
IL (1) IL23441A (de)
NL (1) NL6505834A (de)
SE (1) SE304150B (de)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030155409A1 (en) * 2001-11-21 2003-08-21 Dockus Kostas F. Fluxless brazing
US20040035911A1 (en) * 2001-11-21 2004-02-26 Dockus Kostas F. Fluxless brazing
US20040035910A1 (en) * 2001-11-21 2004-02-26 Dockus Kostas F. Low temperature fluxless brazing
US20040038070A1 (en) * 2001-11-21 2004-02-26 Dockus Kostas F. Fluxless brazing
US20060027625A1 (en) * 2001-11-21 2006-02-09 Dana Canada Corporation Products for use in low temperature fluxless brazing
US20060102696A1 (en) * 2001-11-21 2006-05-18 Graham Michael E Layered products for fluxless brazing of substrates
US20070042122A1 (en) * 2005-08-22 2007-02-22 Rohm And Haas Electronic Materials Llc Aqueous solution for surface treatment of metal and method for preventing discoloration of metal surface

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2872346A (en) * 1956-05-21 1959-02-03 Miller Adolph Metal plating bath
US2947639A (en) * 1958-05-19 1960-08-02 Chrysler Corp Process and composition for immersion tin plating of aluminum and aluminum alloys
US3147154A (en) * 1961-05-25 1964-09-01 Texaco Inc Method of depositing metal-containing material onto an extended surface
US3231396A (en) * 1961-08-07 1966-01-25 Dow Chemical Co Stannate immersion coating for magnesium, magnesium-dissimilar metal couples, and other metals

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2822325A (en) * 1955-02-11 1958-02-04 Metal & Thermit Corp Process of, and composition for cleaning and tinning
US2947635A (en) * 1958-05-15 1960-08-02 Mayer & Co Inc O Method of preparing puffed skin products

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2872346A (en) * 1956-05-21 1959-02-03 Miller Adolph Metal plating bath
US2947639A (en) * 1958-05-19 1960-08-02 Chrysler Corp Process and composition for immersion tin plating of aluminum and aluminum alloys
US3147154A (en) * 1961-05-25 1964-09-01 Texaco Inc Method of depositing metal-containing material onto an extended surface
US3231396A (en) * 1961-08-07 1966-01-25 Dow Chemical Co Stannate immersion coating for magnesium, magnesium-dissimilar metal couples, and other metals

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060027625A1 (en) * 2001-11-21 2006-02-09 Dana Canada Corporation Products for use in low temperature fluxless brazing
US7000823B2 (en) 2001-11-21 2006-02-21 Dana Canada Corporation Fluxless brazing
US20040035911A1 (en) * 2001-11-21 2004-02-26 Dockus Kostas F. Fluxless brazing
US20040035910A1 (en) * 2001-11-21 2004-02-26 Dockus Kostas F. Low temperature fluxless brazing
US20040038070A1 (en) * 2001-11-21 2004-02-26 Dockus Kostas F. Fluxless brazing
US6815086B2 (en) 2001-11-21 2004-11-09 Dana Canada Corporation Methods for fluxless brazing
US20030197050A1 (en) * 2001-11-21 2003-10-23 Graham Michael E. Fluxless brazing method and compositions of layered material systems for brazing aluminum or dissimilar metals
US6913184B2 (en) 2001-11-21 2005-07-05 Dana Canada Corporation Alloy composition and method for low temperature fluxless brazing
US20030155409A1 (en) * 2001-11-21 2003-08-21 Dockus Kostas F. Fluxless brazing
US6959853B2 (en) 2001-11-21 2005-11-01 Dana Canada Corporation Fluxless brazing method and method for manufacturing layered material systems for fluxless brazing
US20060102696A1 (en) * 2001-11-21 2006-05-18 Graham Michael E Layered products for fluxless brazing of substrates
US7735718B2 (en) 2001-11-21 2010-06-15 Dana Canada Corporation Layered products for fluxless brazing of substrates
US7451906B2 (en) 2001-11-21 2008-11-18 Dana Canada Corporation Products for use in low temperature fluxless brazing
US20070042122A1 (en) * 2005-08-22 2007-02-22 Rohm And Haas Electronic Materials Llc Aqueous solution for surface treatment of metal and method for preventing discoloration of metal surface
US8043662B2 (en) * 2005-08-22 2011-10-25 Rohm And Haas Electronic Materials Llc Aqueous solution for surface treatment of metal and method for preventing discoloration of metal surface
KR101299114B1 (ko) 2005-08-22 2013-08-21 롬 앤드 하스 일렉트로닉 머트어리얼즈, 엘.엘.씨. 금속의 표면처리용 수용액 및 금속표면의 변색방지방법

Also Published As

Publication number Publication date
DE1270920B (de) 1968-06-20
IL23441A (en) 1968-07-25
NL6505834A (de) 1965-11-15
GB1110770A (en) 1968-04-24
CH471901A (de) 1969-04-30
JPS4927015B1 (de) 1974-07-13
SE304150B (de) 1968-09-16

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