EP0049192B1 - Dispositif perfectionné pour l'oxydation anodique par électrolyse au tampon et électrolytes mis en oeuvre dans ce dispositif - Google Patents

Dispositif perfectionné pour l'oxydation anodique par électrolyse au tampon et électrolytes mis en oeuvre dans ce dispositif Download PDF

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Publication number
EP0049192B1
EP0049192B1 EP81401459A EP81401459A EP0049192B1 EP 0049192 B1 EP0049192 B1 EP 0049192B1 EP 81401459 A EP81401459 A EP 81401459A EP 81401459 A EP81401459 A EP 81401459A EP 0049192 B1 EP0049192 B1 EP 0049192B1
Authority
EP
European Patent Office
Prior art keywords
electrolyte
cathode
tube
mass
gripping means
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP81401459A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0049192A1 (fr
Inventor
François Baburek
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
NOUVELLE DALIC Ste
Original Assignee
Dalic Laboratoire SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dalic Laboratoire SA filed Critical Dalic Laboratoire SA
Priority to AT81401459T priority Critical patent/ATE27191T1/de
Publication of EP0049192A1 publication Critical patent/EP0049192A1/fr
Application granted granted Critical
Publication of EP0049192B1 publication Critical patent/EP0049192B1/fr
Expired legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/10—Electrodes, e.g. composition, counter electrode
    • C25D17/14—Electrodes, e.g. composition, counter electrode for pad-plating
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/005—Apparatus specially adapted for electrolytic conversion coating
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids

Definitions

  • the present invention relates to an improved device for anodic oxidation by buffer electrolysis, of the type in which the electrolyte is retained in an absorbent mass in contact with a cathode comprising an internal cooling circuit, connected to the negative pole of a source of electricity and carried by an electrically insulated gripping member.
  • the cathode in particular used for the anodic oxidation of aluminum and its alloys, is constituted by a graphite block comprising an interior chamber in which cooling water circulates. It is also provided with a tapping opening into said chamber and intended to receive the threaded rod of a gripping member consisting of a conductive mass covered with an insulating cap and connected to the positive pole of a source of electricity. . Finally, in the interior chamber of the cathode open a water supply conduit and a water discharge conduit, both integral with the gripping member, and which ensure a circulation of water in said chamber.
  • the object of the present invention is therefore to remedy the drawbacks mentioned above and to do this, it provides a device which is characterized in that the cathode is constituted by a stainless steel tube comprising at least two branches, the at least one of these branches being held locally by the gripping member, and the free end of one or more of these branches being connected to a supply of cooling fluid, the free end of the remaining branch (s) being connected to a coolant outlet.
  • the cathode is constituted by a stainless steel tube comprising at least two branches, the at least one of these branches being held locally by the gripping member, and the free end of one or more of these branches being connected to a supply of cooling fluid, the free end of the remaining branch (s) being connected to a coolant outlet.
  • stainless steel resist particularly well to the operating conditions required for anodic oxidation, but it is also possible to conform it to a tube whose cooling by internal circulation of a cooling fluid is extremely effective. Indeed, in anodic oxidation by buffer electrolysis, it is essential to obtain a protective coating of good quality and of sufficient thickness, to operate at temperatures as low as possible, hence the absolute need to evacuate the calories released at the cathode due to the very high current intensities applied to the latter.
  • connection between the cathode-forming tube and the negative pole is ensured by means of a conductive mass of the electric current contained in the gripping member, at least one of the branches of the tube being in contact with this conductive mass.
  • the cathode will preferably be substantially U-shaped, the two branches of which are held in the gripping member in the vicinity of their free end.
  • the resulting device is therefore compact, easy to handle and makes it possible, by choosing the length of the branches of the U-shaped tube, to treat areas of difficult or even impossible access with the devices of the prior art.
  • the cooling fluid can consist of the electrolyte, the cathode being pierced, in the vicinity of the part in contact with the absorbent mass, fine orifices for the flow of the electrolyte.
  • the cooling fluid can consist of the electrolyte, the cathode being pierced, in the vicinity of the part in contact with the absorbent mass, fine orifices for the flow of the electrolyte.
  • the device according to the invention will preferably include an electrolyte supply disposed in the vicinity of the cathode and of the absorbent mass, so that the latter can absorb the electrolyte flowing from this supply, the latter being maintained locally by the gripping member.
  • the cathode remains refrigerated by the cooling fluid which passes through it and the electrolyte comes from a source other than the cathode, a source which, when it is constituted by a stainless steel tube closed at one of its ends, pierced with fine orifices delivering passage to the electrolyte, and maintained in the gripping member in the vicinity of its free end, is intimately incorporated within the anodizing device and forms a compact whole with the latter.
  • This arrangement has the advantage over that described above, of making it possible to regulate at will the quantity of electrolyte to be poured onto the absorbent mass, without however harming re cooling of the cathode and without increasing the size of the anodizing device and complicating its structure and handling.
  • the electrolyte supply tube is disposed substantially in the longitudinal plane of symmetry of the U-shaped tube.
  • the size of the cathode-tube assembly d The supply of electrolyte is minimal and by choosing the location of the orifices suitably, it is possible to keep the absorbent mass perfectly imbibed in electrolyte at the working area of the cathode.
  • the electrolyte supply tube is located slightly above the plane formed by the two branches of the U-shaped cathode, it is possible, always by choosing the position of the orifices made in this tube, to ensure that the electrolyte flowing from these orifices spreads over one and / or the other of the branches of the cathode, thus contributing to the cooling of the latter.
  • the electrolyte supply tube may be in contact with the conductive mass of the electric current and in this case, it will also play the role of cathode and may contribute to anodic oxidation.
  • the branch or branches of the cathode in contact with the conductive mass and possibly the electrolyte supply tube are immobilized respectively in bores provided in this conductive mass. This type of assembly not only allows good electrical contact, but also gives good rigidity to the device.
  • the absorbent mass is in the form of a sleeve closed at one of its ends, fitting over all or part of the cathode portion and optionally of the electrolyte supply tube, not maintained in the gripping member.
  • the cathode-tube assembly for supplying electrolyte is thus surrounded by the absorbent mass, which prevents the electrolyte from inadvertently dripping and thus allows the anodization device to be used in any position.
  • the present invention also relates to a new type of absorbent mass, usable in particular in the anodizing device described above and below. More specifically, this absorbent mass consists of polyester wadding enclosed in a sheath made of woven polypropylene or polyester fibers.
  • this polyester in the form of wadding or woven fibers, is that resulting from the copolymerization of glycols and various aromatic diacids, and preferably that resulting from the copolymerization of glycol and terephthalic acid.
  • the polypropylene used to make the sheath will preferably be a polymer of isotactic structure of the MERAKLON type ".
  • the present invention also relates to new electrolytes for anodic oxidation by buffer electrolysis, usable in particular in the anodization device which is the subject of the present application.
  • these electrolytes consist of an aqueous solution of concentrated sulfuric acid, chromic anhydride, sulfamic acid and optionally magnesium sulfate. These are particularly suitable for the anodic oxidation of aluminum.
  • They can also contain magnesium sulphate and are therefore particularly suitable for the anodic oxidation of light aluminum alloys.
  • the device which is the subject of these figures comprises a block 1 of plastic material, of substantially frustoconical shape, provided with a handle 2, the fixing of the latter to the block 1 being ensured, for example, by simply screwing in a threaded rod (not shown) carried by the handle, in a thread (not shown) formed in said block.
  • the small base 3 of the frustoconical block 1 has an opening 4 which extends into an interior chamber in which is housed by force a cylindrical conductive mass 5, preferably made of stainless steel, and the axis of which coincides with the axis of the block frustoconical 1.
  • This mass 5 is provided with three bores (6, 7, 8) situated respectively in the extension of bores of the same section (6a, 7a, 8a) produced in block 1.
  • two of the three pairs of complementary bores (6, 6a) and (7, 7a) are substantially in the horizontal plane of symmetry of the block 1, on either side and at equal distance from the vertical plane of symmetry of this same block 1, while the third pair of complementary bores (8, 8a) is situated substantially in this vertical plane of symmetry, under the two pairs of bores (6, 6a) and (7, 7a).
  • the position in block 1 described above of these different bores is the most rational, but could be any other without this in any way modifying the spirit of the invention.
  • the pairs of bores (6, 6a) and (7, 7a) could be in a plane different from the horizontal plane of symmetry and / or in two separate planes.
  • the pair of bores (8, 8a) could be outside the vertical plane of symmetry and / or above the pairs of bores (6, 6a) and (7, 7a).
  • the mass 5 is extended, by a projection 9, towards the large base 10 of the frustoconical block 1 without however reaching this base.
  • This projection 9 is provided with a thread 11 perpendicular to the base 10 and located in the extension of a bore 12 of the same section made in the block 1 and starting from said base 10, thread which receives the threaded rod 13 of a electrical connection plug 14 capable of being connected to the negative pole of an electrical source (not shown).
  • the position of the projection 9 and the method of fixing the plug 14 on this projection could be any other without this in any way modifying the operation of the anodizing device.
  • pairs of bores (6, 6a) and (7, 7a) are forced in and so as to pass right through the block 1, respectively the two branches (15,16) of a U-shaped tube 17 made of stainless steel, which are each bent slightly in front of the base 3, the bent parts (18, 19) being slightly inclined towards each other, and extending respectively by two horizontal sections (20, 21) connecting to the bottom of the U and located in the same plane itself located below block 1.
  • the free end of the tube 15 emerging from the base 10 is intended to be connected to an inlet (not shown) in cooling fluid, for example water, the free end of the tube 16 also emerging from the base 10 being, in turn, intended to be connected to an outlet (not shown) in cooling fluid.
  • cooling fluid for example water
  • a tube 22 of stainless steel In the bore torque (8, 8a) is also forced in and so as to pass right through the block 1, a tube 22 of stainless steel also bent, the bent part 23 extending by a horizontal section 24 closed at its end and located just above the plane formed by the sections (20, 21), this section 24 being provided with two rows of fine orifices (25, 26) each facing each other respectively with said sections ( 20, 21).
  • the free end of the tube 22, that is to say that emerging from the base 10 is for its part intended to be connected to an electrolyte supply.
  • a sleeve 27 substantially cylindrical and closed at one of its ends is threaded on the sections (20, 21, 24) which are therefore totally surrounded by this sleeve.
  • the latter consists of polyester wadding 28 enclosed in a sheath 29 made of woven fibers of polypropylene MERAKLON.
  • the shape of this sleeve is not limited to the cylindrical shape, but will in fact depend on the shape of the cathode. In the embodiment described, this cathode is U-shaped, but it could be different and adapted to the geometry of the surface to be anodized.
  • the operation of the device described above is as follows.
  • the ends of the branches (15, 16) are connected respectively to an inlet and to an outlet for cooling fluid, fluid whose circulation is for example ensured by a pump.
  • the end of the tube 22 is connected to an electrolyte supply, itself connected to an electrolyte supply pump, the flow rate of which is adjustable.
  • plug 14 is connected to the negative pole of an appropriate current generator, the part to be anodized being connected to the positive pole of this same generator.
  • the generator can be of any type, for example direct current or pulsed current.
  • the actual anodization is carried out by moving this sleeve over the surface to be treated while monitoring the supply of electrolyte to compensate for evaporation and ensure that the sleeve always remains perfectly supplied with electrolyte.
  • the electrode will be refrigerated to the maximum and the electrolyte used will be at the lowest possible temperature, and preferably at a temperature equal to or lower than 20 ° C.
  • the operating voltages of the device according to the invention will generally be of the order of 25 to 50 volts, values at which the efficiency of the anodization will be substantially constant, the current densities possibly varying between 15 and 250 A / d m2 .
  • the part to be anodized may consist of any metal capable of undergoing anodic oxidation, such as for example aluminum and its light alloys, as well as titanium and its alloys.
  • the electrolytes to be used in the device according to the invention will of course depend on the nature of the metal constituting this part.
  • the electrolyte will preferably consist of an aqueous solution containing 30 to 100 g / l, and more particularly approximately 35 g / l, of sulfamic acid; 10 to 60 g / l, and more particularly approximately 17 g / l, of chromic anhydride; and 9 to 55 g / l, and more particularly approximately 13 g / l, of concentrated sulfuric acid.
  • the electrolyte will preferably consist of an aqueous solution containing 30 to 100 g / l, and more particularly about 100 g / l, sulfamic acid; 10 to 60 g / l, and more particularly approximately 48 g / l, of chromic anhydride; 9 to 55 g / l, and more particularly approximately 37 g / l, of concentrated sulfuric acid; and about 100 g / l of magnesium sulfate heptahydrate.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electrochemical Coating By Surface Reaction (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Electrolytic Production Of Metals (AREA)
EP81401459A 1980-09-22 1981-09-18 Dispositif perfectionné pour l'oxydation anodique par électrolyse au tampon et électrolytes mis en oeuvre dans ce dispositif Expired EP0049192B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT81401459T ATE27191T1 (de) 1980-09-22 1981-09-18 Vorrichtung fuer die anodische oxydation nach dem tamponverfahren und hierfuer verwendeter elektrolyt.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8020341 1980-09-22
FR8020341A FR2490685A1 (fr) 1980-09-22 1980-09-22 Dispositif perfectionne pour l'oxydation anodique par electrolyse au tampon et electrolytes mis en oeuvre de ce dispositif

Publications (2)

Publication Number Publication Date
EP0049192A1 EP0049192A1 (fr) 1982-04-07
EP0049192B1 true EP0049192B1 (fr) 1987-05-13

Family

ID=9246171

Family Applications (1)

Application Number Title Priority Date Filing Date
EP81401459A Expired EP0049192B1 (fr) 1980-09-22 1981-09-18 Dispositif perfectionné pour l'oxydation anodique par électrolyse au tampon et électrolytes mis en oeuvre dans ce dispositif

Country Status (14)

Country Link
EP (1) EP0049192B1 (US07922777-20110412-C00004.png)
JP (1) JPS57114699A (US07922777-20110412-C00004.png)
AR (1) AR224587A1 (US07922777-20110412-C00004.png)
AT (1) ATE27191T1 (US07922777-20110412-C00004.png)
AU (1) AU7552181A (US07922777-20110412-C00004.png)
BR (1) BR8106139A (US07922777-20110412-C00004.png)
CA (1) CA1188652A (US07922777-20110412-C00004.png)
DE (1) DE3176188D1 (US07922777-20110412-C00004.png)
DK (1) DK418081A (US07922777-20110412-C00004.png)
ES (1) ES8300355A1 (US07922777-20110412-C00004.png)
FR (1) FR2490685A1 (US07922777-20110412-C00004.png)
NO (1) NO156173C (US07922777-20110412-C00004.png)
NZ (1) NZ198430A (US07922777-20110412-C00004.png)
PT (1) PT73714B (US07922777-20110412-C00004.png)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3507927A1 (de) * 1985-03-06 1986-09-11 Dr.Ing.H.C. F. Porsche Ag, 7000 Stuttgart Verfahren und handgeraet zum halbmechanischen verzinken von blechoberflaechen
US6939447B2 (en) 1998-04-06 2005-09-06 Tdao Limited Method of providing conductive tracks on a printed circuit and apparatus for use in carrying out the method
GB2336161B (en) 1998-04-06 2003-03-26 John Michael Lowe Method of providing conductive tracks on a printed circuit and apparatus for use in carrying out the method
CN102492975A (zh) * 2011-12-30 2012-06-13 中国科学院力学研究所 一种电解液喷射放电生长陶瓷涂层的装置及方法
CN103184498B (zh) * 2013-03-08 2015-08-26 华南理工大学 滚刷式微弧氧化处理方法及装置
GB2535805A (en) * 2015-02-27 2016-08-31 Biomet Uk Healthcare Ltd Apparatus and method for selectively treating a surface of a component
US11686012B2 (en) * 2017-10-26 2023-06-27 Unison Industries, Llc Mandrel for electroforming
EP4194590A1 (de) * 2021-12-09 2023-06-14 Aalberts Surface Technologies GmbH Verfahren und zusammensetzung zur selektiven anodisation

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL68330C (US07922777-20110412-C00004.png) * 1950-11-03
US3349014A (en) * 1964-08-28 1967-10-24 Mc Donnell Douglas Corp Method and composition for the treatment of an aluminum surface

Also Published As

Publication number Publication date
NO813204L (no) 1982-03-23
PT73714A (fr) 1981-10-01
NO156173B (no) 1987-04-27
EP0049192A1 (fr) 1982-04-07
ATE27191T1 (de) 1987-05-15
PT73714B (fr) 1982-12-30
NO156173C (no) 1987-08-12
FR2490685A1 (fr) 1982-03-26
AR224587A1 (es) 1981-12-15
JPH026839B2 (US07922777-20110412-C00004.png) 1990-02-14
FR2490685B1 (US07922777-20110412-C00004.png) 1984-06-22
DK418081A (da) 1982-03-23
JPS57114699A (en) 1982-07-16
CA1188652A (en) 1985-06-11
AU7552181A (en) 1982-04-01
ES505636A0 (es) 1982-11-01
NZ198430A (en) 1985-03-20
DE3176188D1 (en) 1987-06-19
BR8106139A (pt) 1982-06-15
ES8300355A1 (es) 1982-11-01

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