EP0565070B1 - Procédé d'électrodéposition - Google Patents

Procédé d'électrodéposition Download PDF

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Publication number
EP0565070B1
EP0565070B1 EP93105726A EP93105726A EP0565070B1 EP 0565070 B1 EP0565070 B1 EP 0565070B1 EP 93105726 A EP93105726 A EP 93105726A EP 93105726 A EP93105726 A EP 93105726A EP 0565070 B1 EP0565070 B1 EP 0565070B1
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EP
European Patent Office
Prior art keywords
pulse
layer
surface coating
structured surface
voltage
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 - Lifetime
Application number
EP93105726A
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German (de)
English (en)
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EP0565070A1 (fr
Inventor
Karl Müll
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.)
Winterthurer Metallveredelung AG
Heidelberger Druckmaschinen AG
Original Assignee
Winterthurer Metallveredelung AG
Heidelberger Druckmaschinen AG
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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
    • C25D5/18—Electroplating using modulated, pulsed or reversing current
    • 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
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C25D5/14—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium two or more layers being of nickel or chromium, e.g. duplex or triplex layers
    • 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
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/605—Surface topography of the layers, e.g. rough, dendritic or nodular layers
    • 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
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/625—Discontinuous layers, e.g. microcracked layers

Definitions

  • the invention relates to a method for the electrochemical (galvanic) application of a surface coating to an object, preferably a machine component, in particular a machine roller, using an electrical variable of the galvanic process which causes the layer application.
  • a hard chrome layer is then applied to the surface structure created in this way.
  • These various work steps required for the creation are quite complex and require complicated process engineering. The costs are essentially determined by the complex processing steps such as mechanical grinding to size and chemical structure etching; these machining processes are relatively expensive.
  • US 3,318,786 discloses a method for the deposition of Ni strike, bright nickel and chrome as a multilayer system.
  • the anode and cathode are included a cyclically varying unidirectional voltage.
  • the voltage curve is controlled in such a way that during a first period t 1 CrH x is deposited, during a subsequent further period t 2 the deposition of CrH x ceases and finally ends and the duration of the period t 2 is dimensioned such that it is greater than Is 0.5 ms and leads to a decay of deposited CrH x and leads to the deposition of pure chromium.
  • the current flow to the cathode and anode is blocked.
  • the invention is therefore based on the object of specifying a method for the electrochemical application of a surface coating to an object, which enables the desired, structured surface topographies to be created in a simple and inexpensive manner.
  • an electrical voltage and / or an electrical current is used as the electrical variable such that the initial pulse and / or the subsequent pulse have a defined shape by means of a corresponding voltage and / or current function as a function of time Has.
  • the structured surface coatings preferably by means of galvanic chromium or chromium alloy electrolytes, by means of galvanic nickel or nickel alloy electrolytes, by means of galvanic cobalt or cobalt alloy electrolytes, by means of galvanic copper or copper alloy electrolytes or by means of galvanic noble metal or noble metal alloy electrolytes.
  • the structure forms defined lubricant deposits or has a storage capacity for substances that come into contact with the surface.
  • the structuring leads to low-glare devices, for example in medical or optical technology.
  • a multilayer structure is provided, at least one of the layers being provided with the structured surface topography.
  • a nickel strike layer is preferably first applied to the object.
  • This nickel strike layer is applied with a thickness of 0.2 to 2 ⁇ m, preferably ⁇ 1 ⁇ m.
  • the application is preferably carried out by means of a galvanic process.
  • the object is, for example, a roller or a cylinder of a printing press.
  • the cylinder is preferably made of steel (St.52 / Nirosta).
  • a sulfamate-nickel layer is applied to the nickel strike layer.
  • This layer is preferably produced with a thickness of 25 to 40 ⁇ m, in particular 30 ⁇ m.
  • a chromium layer in particular a low-crack chromium layer
  • This chrome layer preferably has a thickness of 5 up to 15 ⁇ m, in particular from 10 ⁇ m.
  • the structured surface coating generated by means of the initial and subsequent pulse is applied to the chrome layer.
  • This surface coating is preferably designed as a structured chromium layer, a chromium or a chromium alloy electrolyte being used in the galvanic process.
  • the application is carried out by first applying germs of the deposition material to the surface to be coated (for example the mentioned chrome layer) by means of at least one initial pulse of the electrical quantity of the galvanic process.
  • the structured surface coating is preferably produced with a maximum thickness of 5 to 20 ⁇ m, preferably 7 to 10 ⁇ m.
  • the "maximum thickness” is understood to mean the measure up to the highest elevations, since due to the structuring, that is to say higher and lower areas, a measure of the thickness is not otherwise clearly defined.
  • the so-called "load share”, which is also defined as the “material share” according to DIN 4762, can also be used as the design. This load-bearing component is the percentage ratio of the length of the profile cut in a certain cutting line to a reference distance.
  • the profile results from the surface structure, the cutting line being below the highest elevations of the structure, so that it cuts the corresponding elevations leads in some areas between the surveys.
  • the method according to the invention preferably achieves a load share of 25%, the cutting line being 2 ⁇ m below the highest point of the structure.
  • a finishing layer of micro-cracked chromium is applied to the structured surface coating.
  • This final layer is preferably produced with a thickness of 5 to 20 ⁇ m, in particular 8 to 10 ⁇ m.
  • the structured surface coating produced by means of the method according to the invention has the correspondingly desired roughness or the correspondingly desired proportion of load bearing
  • the other layers mentioned here nickel strike layer, sulfamate nickel layer, low-crack chrome layer (base layer) and finishing layer made of micro-cracked chromium ) on the other hand, to be regarded as having the same thickness and unstructured.
  • a chromium electrolyte is used for the electrochemical process for applying the structured surface coating.
  • This chrome electrolyte preferably has a temperature of about 45 ° C.
  • the object is set in rotation while the structured surface coating is being applied.
  • this takes place in the cylinders of the printing presses mentioned in that they are rotated about their longitudinal central axis.
  • Anodes made of PbSn7 or platinized titanium are particularly preferably used when applying the structured surface coating.
  • the object to be coated forms the cathode when the structured surface coating is applied.
  • a trapezoidal initial voltage pulse and also an approximately trapezoidal subsequent voltage pulse are preferably used to generate the structure of the surface coating.
  • the machine component is immersed in the electrolytes, in particular chrome electrolytes, and the initial pulse is only started after a voltage-free or current-free waiting time has elapsed.
  • This waiting time serves, among other things, to adjust the temperature, i.e. the base material (machine component) assumes approximately the temperature of the electrolyte.
  • This waiting time is preferably 60 s.
  • This intermediate period is thus between the section of the nucleation mentioned above and the growth phase of the deposition process.
  • a basic pulse (voltage or current pulse) is connected upstream of the initial pulse.
  • a starting edge of a follows the initial pulse
  • the current in the galvanic process is increased to a maximum current of approx. 950 A based on a standard area. This maximum current is now maintained over a period of approximately 60s.
  • the dampening cylinder 1 shows a longitudinal section through a dampening cylinder 1 of a printing press.
  • the dampening cylinder 1 has a cylindrical base body 2, the outer surface 3 of which is provided with a layer structure 4.
  • the layer structure 4 is identified by the dash-dot line in FIG. 1. It is guided around the edge regions 5 of the dampening cylinder 1 with the length of a portion of the radius.
  • the layer structure 4 is composed of individual layers, each of which is applied electrochemically, that is to say by means of galvanic processes.
  • FIG. 2 shows a section through the layer structure 4.
  • a nickel strike layer 6 is electrodeposited on the base body 2 of the dampening cylinder 1.
  • the basic body is made of steel St.52 / Nirosta.
  • the nickel strike layer 6 is a pre-nickel plating.
  • the electrolyte used for this is very acidic with a high chloride concentration.
  • the nickel strike layer 6 has a uniform thickness of preferably 1 to 2 ⁇ m.
  • a sulfamate-nickel layer 7 is applied electrolytically to the nickel strike layer 6.
  • This sulfamate-nickel layer 7 is sulfur-free; it has a thickness of 30 to 40 ⁇ m and a Vickers hardness of 200 to 250 HV.
  • a low-crack chrome layer 8 is electroplated onto the sulfamate-nickel layer 7; it has a uniform thickness of 10 to 15 ⁇ m and forms a so-called base layer.
  • a structured surface coating 9 is applied to the chrome layer 8 by means of a galvanic process.
  • This surface coating 9 represents a structured chrome layer 10. Due to the structuring there are corresponding elevations and depressions, the maximum thickness, measured from the sole to the apex of the maximum elevation, being 7 to 10 ⁇ m.
  • FIG. 3 shows a voltage-time diagram which illustrates the control of an electrical variable (voltage U) of the galvanic process for applying the base layer and for subsequently applying the structured surface coating 9.
  • the dampening cylinder 1 is switched as a cathode and anodes made of PbSn7 or platinized titanium are used.
  • the electrode distance between the anode and cathode is set to approx. 25 cm.
  • the dampening cylinder 1 is continuously rotated about its longitudinal axis 12 (FIG. 1) while the structured surface coating 9 is being applied.
  • the electrochemical process for applying the base layer (chrome layer 8) and the structured surface coating 9 is carried out as follows:
  • the base body 2 of the dampening cylinder 1 is introduced into a chrome electrolyte at a temperature of approximately 45 ° C., after which Initially, a waiting time t w passes, which is approximately 60 s long. During this time (without applying current or voltage) the temperature of the base material (base body 2) is adjusted to the electrolyte temperature.
  • an electrical base pulse 13 is first applied between the anode and cathode after the waiting time t w . Then, by means of an initial and a subsequent pulse 14, nucleation of the separating material (initial pulse 14 ') and then growth of the separating material nuclei by addition with further separating material is then brought about (subsequent pulse 14''), as a result of which the structured surface coating 9 is formed.
  • the basic pulse 13 and the initial and subsequent pulse 14 are designed as follows:
  • the basic pulse 13 is a voltage pulse with a trapezoidal shape.
  • the start and follow pulse 14 is also a voltage pulse, which is composed of the start pulse 14 'and the immediately following pulse 14''and also has a trapezoidal shape; the pure trapezoidal shape is disturbed insofar as the starting edge (leading edge) of the starting pulse 14 'has a different slope than the starting edge of the following pulse 14''. This will be discussed in more detail below.
  • An intermediate time period t z then follows, which is current-free or voltage-free and has a length of 60 s.
  • the starting pulse 20 'is immediately followed by the starting edge 20 of the following pulse 14 ", which has a slope ⁇ U / ⁇ t 0.1 V / 6 s.
  • the starting edge 20 is used to increase the current on which the galvanic process is based increased to a maximum current I max of 950 A. This maximum current I max is maintained over a period of 60 s.
  • This is followed by a trailing edge 21 of the following pulse 14 ", which drops ⁇ U / ⁇ t 0.5 V / 4 s having. At the end of the trailing edge 21 there is no current or voltage.
  • the total edge formed by the initial pulse 14 'and the subsequent pulse 14 " is designated by 19. It is composed of the two starting edges 18 and 20.
  • finishing layer 11 is applied to the structured surface coating 9 produced according to the invention using a conventional electrochemical process.
  • FIG. 4 shows — in a 200-fold magnification — the structural chrome of the structured surface coating 9.
  • FIG. 5 shows a 500-fold magnification. It can be clearly seen that there is a very uniform structured distribution.
  • FIGS. 6 and 7 show a comparison of a known surface coating with the surface coating according to the invention: namely, FIG. 6 shows a conventional surface coating subjected to a grinding and etching process in 200 times magnification and FIG. 7 shows the structured surface coating 9 according to the invention, also in FIG 200x magnification. It can clearly be seen that the structure according to the invention is constructed in a substantially more uniform and orderly manner than in the case of the prior art.
  • the nickel strike layer 6 Only then is the nickel strike layer 6, then the sulfamate nickel layer 7 and then the chrome layer 8 applied.
  • the structured surface coating 9 is then deposited and then the finishing layer 10, which consists of micro-cracked chromium and with which the dimensional accuracy can be controlled, is applied.
  • the invention is not restricted to chromium or chromium alloy layers, but can also be carried out with other deposition materials.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)

Claims (31)

  1. Procédé de dépôt électrochimique (galvanique) d'un revêtement de surface sur un objet, de préférence sur un composant de machine, en particulier un rouleau de machine, à l'aide d'une grandeur électrique du processus galvanique qui provoque le dépôt de couche,
       caractérisé
       en ce que, pour l'obtention d'une topographie structurée souhaitée de surface, des formations de germes de la matière précipitation sur la surface à revêtir ont lieu au moyen d'au moins une impulsion initiale (14') de la grandeur électrique et en ce qu'ensuite une croissance des germes de la matière de précipitation est provoquée par incrustation d'un complément de matière de précipitation au moyen d'au moins une impulsion séquentielle (14"), l'impulsion séquentielle (14") faisant suite immédiatement à l'impulsion initiale (14') et la fin du flanc de départ (18) de l'impulsion initiale (14') forme une transition continue avec le début du flanc de départ (20) de l'impulsion séquentielle (14") et le flanc de départ (18) de l'impulsions initiale (14') a une autre pente que celle de l'impulsion de départ (20) de l'impulsion séquentielle (14").
  2. Procédé selon la revendication 1,
       caractérisé
       en ce que la grandeur électrique est une tension électrique (U) et/ou un courant électrique qui est utilisé de manière que l'impulsion initiale (14') et/ou que l'impulsion séquentielle (14") aie une forme définie qui est produite par une fonction correspondante de tension et/ou de courant par rapport au temps (t).
  3. Procédé selon la revendication 1,
       caractérisé
       en ce qu'une couche de fond de nickel (6) est déposée sur l'objet.
  4. Procédé selon la revendication 3,
       caractérisé
       en ce que la couche de fond en nickel (6) a une épaisseur de 0,2 µm à 2 µm, de préférence < 1 µm.
  5. Procédé selon la revendication 3,
       caractérisé
       en ce qu'une couche de sulfamate et de nickel (7) est déposée sur la couche de fond en nickel (6).
  6. Procédé selon la revendication 5,
       caractérisé
       en ce que la couche de sulfamate et de nickel (7) est réalisée à une épaisseur de 25 µm à 40 µm, en particulier de 30 µm.
  7. Procédé selon la revendication 5,
       caractérisé
       en ce qu'une couche de chrome (8), en particulier une couche de chrome ayant peu de criques, est déposée sur la couche de sulfamate et de nickel (7).
  8. Procédé selon la revendication 7,
       caractérisé
       en ce que la couche de chrome (8) est réalisée à une épaisseur de 5 µm à 15 µm, en particulier de 10 µm.
  9. Procédé selon la revendication 7,
       caractérisé
       en ce que la couche de chrome (8) est une couche de base qui est déposée par voie galvanique au moyen d'une impulsion électrique de base (13).
  10. Procédé selon la revendication 9,
       caractérisé
       en ce qu'un revêtement structuré de surface (9) produit par l'impulsion initiale et l'impulsion séquentielle (14 ou 14' et 14") est déposé sur la couche de chrome (8).
  11. Procédé selon la revendication 10,
       caractérisé
       en ce que le revêtement structuré de surface (9) est constitué d'une couche structurée de chrome (10),
  12. Procédé selon la revendication 10,
       caractérisé
       en ce que le revêtement structuré de surface (9) est réalisé à une épaisseur maximale de 5 µm à 20 µm, de préférence de 7 µm à 10 m.
  13. Procédé selon la revendication 10,
       caractérisé
       en ce qu'une couche finale (11) de chrome ayant des criques microscopiques est déposée sur le revêtement structuré de surface (9).
  14. Procédé selon la revendication 10,
       caractérisé
       en ce qu'un électrolyte de chrome est utilisé pour le processus électrochimique de dépôt du revêtement structuré de surface (9).
  15. Procédé selon la revendication 14,
       caractérisé
       en ce que l'électrolyte de chrome a une température d'environ 45°C.
  16. Procédé selon la revendication 1,
       caractérisé
       en ce que l'objet est entraîné en rotation pendant le dépôt du revêtement structuré de surface (9).
  17. Procédé selon la revendication 10,
       caractérisé
       en ce que des anodes de PbSn7 ou de titane platiné sont utilisées pour le dépôt du revêtement structuré de surface (9).
  18. Procédé selon la revendication 1,
       caractérisé
       en ce que l'objet, en particulier le composant de machines à revêtir, forme la cathode pendant le dépôt revêtement structuré de surface (9).
  19. Procédé selon la revendication 1,
       caractérisé
       en ce qu'une distance entre électrodes, qui est comprise entre l'anode et la cathode, de 10 cm à 40 cm, en particulier de 25 cm est maintenue lors du dépôt revêtement structuré de surface (9).
  20. Procédé selon la revendication 1,
       caractérisé
       en ce qu'une impulsion de tension à peu près trapézoïdale est utilisée pour la création de la structure du revêtement de surface (9).
  21. Procédé selon la revendication 1,
       caractérisé
       en ce que l'objet, en particulier le composant de machines, est immergé dans l'électrolyte, en particulier dans l'électrolyte de chrome, pour la formation de la couche de chrome (8) formant la couche de base et ce n'est qu'après écoulement d'un temps d'attente (tw) sans tension ni courant que l'impulsion initiale (14') est déclenchée.
  22. Procédé selon les revendications 1 et 9,
       caractérisé
       en ce qu'un intervalle de temps intermédiaire (tz) sans tension ni courant s'écoule entre la fin de l'impulsion de base (13) et le début de l'impulsion initiale (14').
  23. Procédé selon la revendication 9,
       caractérisé
       en ce que l'impulsion de base (13) a un flanc initial (15) ayant une pente de croissance de U/t = env. 0,25 V/5 s.
  24. Procédé selon la revendication 23,
       caractérisé
       en ce qu'une amplitude constante d'environ 4 V fait suite au flanc initial (15) pendant un intervalle de temps d'environ 600 s.
  25. Procédé selon la revendication 9,
       caractérisé
       en ce que l'impulsion de base (13) comprend un flanc de fin (17) qui fait suite à l'amplitude constante et qui a une pente de croissancee de U/t = env. 0,4 V/5 s.
  26. Procédé selon la revendication 9,
       caractérisé
       en ce que l'intervalle de temps intermédiaire (tz) fait suite au flanc de fin (17).
  27. Procédé selon la revendication 1,
       caractérisé
       en ce que l'impulsion initiale (14') comporte un flanc de départ (18) ayant une pente ascendante de U/t = env. 0,3 V/5 s, cette pente ascendante étant conservée jusqu'à une amplitude (A) d'environ 5 V.
  28. Procédé selon la revendication 1,
       caractérisé
       en ce que flanc de départ (20) de l'impulsion séquentielle (14") a une pente de croissance de U/t = env. 0,1 V/6 s, le courant croissant jusqu'à une intensité maximale (Imax) d'environ 950 A par rapport à une surface normalisée.
  29. Procédé selon la revendication 28,
       caractérisé
       en ce que l'intensité maximale (Imax) est conservée pendant un intervalle de temps d'environ 60 s.
  30. Procédé selon la revendication 1.
       caractérisé
       en ce que l'impulsion séquentielle (14") comporte un flanc arrière (21) qui fait suite à l'intensité maximale (Imax) et qui présente une pente de décroissance de U/t = env. 0,5 V/4 s, et qui décroît jusqu'à l'absence de courant et de tension.
  31. Procédé selon l'une des revendications précédentes,
       caractérisé
       en ce que lesdites valeurs mentionnées de tension et/ou de courant et/ou les valeurs de différence de tension et/ou les valeurs de temps et/ou de différence de temps sont utilisées avec des écarts de ±10%, de préférence de ± 5%.
EP93105726A 1992-04-09 1993-04-07 Procédé d'électrodéposition Expired - Lifetime EP0565070B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4211881A DE4211881C2 (de) 1992-04-09 1992-04-09 Verfahren zum elektrochemischen Aufbringen einer strukturierten Oberflächenbeschichtung
DE4211881 1992-04-09

Publications (2)

Publication Number Publication Date
EP0565070A1 EP0565070A1 (fr) 1993-10-13
EP0565070B1 true EP0565070B1 (fr) 1997-07-30

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US (1) US5415761A (fr)
EP (1) EP0565070B1 (fr)
AT (1) ATE156201T1 (fr)
DE (1) DE4211881C2 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
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EP3000918A1 (fr) 2014-09-24 2016-03-30 topocrom systems AG Procédé et dispositif d'application galvanique d'un revêtement de surface
EP4012074A1 (fr) 2020-12-14 2022-06-15 topocrom systems AG Revêtement de surface et son procédé de fabrication

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EP4012074A1 (fr) 2020-12-14 2022-06-15 topocrom systems AG Revêtement de surface et son procédé de fabrication

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US5415761A (en) 1995-05-16
DE4211881C2 (de) 1994-07-28
ATE156201T1 (de) 1997-08-15
EP0565070A1 (fr) 1993-10-13

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