EP0722515B1 - Verfahren zum galvanischen aufbringen einer oberflächenbeschichtung - Google Patents

Verfahren zum galvanischen aufbringen einer oberflächenbeschichtung Download PDF

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Publication number
EP0722515B1
EP0722515B1 EP94928407A EP94928407A EP0722515B1 EP 0722515 B1 EP0722515 B1 EP 0722515B1 EP 94928407 A EP94928407 A EP 94928407A EP 94928407 A EP94928407 A EP 94928407A EP 0722515 B1 EP0722515 B1 EP 0722515B1
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EP
European Patent Office
Prior art keywords
current
current density
process according
stages
seconds
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
EP94928407A
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German (de)
English (en)
French (fr)
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EP0722515A1 (de
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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Priority claimed from DE4334122A external-priority patent/DE4334122C2/de
Application filed by Winterthurer Metallveredelung AG, Heidelberger Druckmaschinen AG filed Critical Winterthurer Metallveredelung AG
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Classifications

    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B17/00—Methods preventing fouling
    • B08B17/02—Preventing deposition of fouling or of dust
    • B08B17/06—Preventing deposition of fouling or of dust by giving articles subject to fouling a special shape or arrangement
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B17/00—Methods preventing fouling
    • B08B17/02—Preventing deposition of fouling or of dust
    • B08B17/06—Preventing deposition of fouling or of dust by giving articles subject to fouling a special shape or arrangement
    • B08B17/065—Preventing deposition of fouling or of dust by giving articles subject to fouling a special shape or arrangement the surface having a microscopic surface pattern to achieve the same effect as a lotus flower
    • 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
    • C25D5/60—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
    • C25D5/627—Electroplating characterised by the visual appearance of the layers, e.g. colour, brightness or mat appearance

Definitions

  • the invention relates to a method for electrochemical (galvanic) application of a surface coating according to the German application with the file number DE 42 11 881.6-24.
  • Such surface structures are created by chemical Etching processes after the coating or through mechanical processing methods such as grinding or Sandblasting more or less well achieved. To that The created surface structure then becomes a Hard chrome layer applied.
  • mechanical processing methods such as grinding or Sandblasting more or less well achieved.
  • the created surface structure then becomes a Hard chrome layer applied.
  • Dispersion deposition processes used in which a specific surface structure through organic or inorganic foreign substances is achieved, for example be built into a chrome layer and / or growth block the chrome layer during the deposition process, so that rough surfaces arise.
  • the foreign substances are present as dispersants in the electrolyte.
  • DE 33 07 748 relates to a method for electrochemical Coating in which a pulsed current is used for nucleation is used. If an appropriate current density is used the resulting germs form a dendritic Structure. This allows rough, Generate dendritic structured surfaces. Under the Current density becomes the average current density at the Understand the cathode surface.
  • the invention has for its object an improved Process for the electrochemical application of Structural metal layers based on mechanical or chemical Post-treatments are dispensed with and with the varied Structural metal layers can be generated, as well as a To provide an apparatus for performing this method.
  • the structure layer is directly galvanically towards the coated object applied. This must be a have an electrically conductive surface, as a rule is sanded around a smooth base for the structural layer to offer.
  • the object Before the coating process, the object is after usual galvanotechnical rules cleaned and degreased. It is immersed as a cathode in a galvanic bath which also has an anode. The distance between the anode and cathode is usually in the range between 1 and 40 cm chosen.
  • Chromium electrolytes are preferred as electrolyte, especially sulfuric acid, chromium electrolytes, mixed acid Chromium electrolytes or alloy electrolytes are used.
  • a process voltage can be applied between the anode and the cathode and the flowing current causes an application of material to the object to be coated, which is used as the cathode.
  • the invention proposes applying positive current jumps to form germs.
  • the structure creation process consists of a nucleation phase and a germ growth phase.
  • the process voltage and process current are increased in several stages, each with a predeterminable change in the current density from 1 to 6 mA / cm 2 per stage, from an initial value to a structure current density.
  • the initial value is 0 mA / cm 2 , but this can also be higher if the nucleation phase immediately follows a previous galvanic process phase and the current in between is not reduced to zero.
  • the time between two current density increases is 0.1 to 30 seconds. step spacings of about 7 seconds are most commonly used. With each jump in current, new germs are formed. In contrast to pulse current coating, the process current does not go back to zero after every positive jump, but is increased further with every current jump. In this way, in particular round and more uniformly shaped germs or bodies can be deposited on the object than is possible with the known pulse current methods.
  • the current stages are applied to the bath in such a number until a structural layer consisting of a precipitate of individual or stacked, approximately spherical or dendritic bodies is reached on the surface of the object.
  • the nucleation phase Structural layer thickness of 4 ⁇ m to 10 ⁇ m is aimed for. To do this usually between 10 and 240 current steps necessary, particularly good results are achieved with 50 to 60 levels reached.
  • the reached after completion of the last current stage Current density is the structure current density.
  • current density is the nucleation phase that actual formation of the structure, largely completed.
  • the structure of the emerging structure is many Parameters, especially the selected structure current density, on the number, the amount and the time interval of the Current levels, the bath temperature and the used Depends on electrolytes.
  • Character of the current function can be different Surface structures are generated, the main thing are characterized by different roughness depths.
  • the ideal process parameters can simply be empirical be determined. As a rule, it can be said that at higher bath temperature and higher acidity of the Electrolytes also used a larger structure current density becomes.
  • This structure current density is usually two to three times the current density used in normal DC coating.
  • DC coating current densities in the range from 15 to 60 mA / cm 2 are used .
  • the value of the current density depends on the electrolyte and the bath temperature.
  • Current densities in the range from 30 to 180 mA / cm 2 are possible for structure coating.
  • the germ growth phase It is during a Predeterminable ramp working time with a process stream Current density in the range of 80% to 120% of the Structure current density created. During ramp work hours an approximately even current flows, which leads to growth the structure created on the object. Depending on the duration of the Ramp working time can do this structural layer more or be less pronounced. The growth takes place doing it faster at the highest points of the structure layer than at the lows between those in the nucleation phase bulky bodies. This initially results in one further increase in roughness during the germ growth phase.
  • the ramp working time is usually in a range from 1 to 600 seconds, preferably around 30 seconds.
  • the current levels are preferably in a range from -1 to -8 mA / cm 2 per level and the time between two current levels is preferably selected in the range from 0.1 to 1 second.
  • the object to be coated already becomes a few Time, preferably one minute before the start of the process in the bath immersed.
  • This waiting time mainly serves the Temperature adjustment, that is, the base material takes about the temperature of the electrolyte.
  • the device for carrying out the described method consists of a galvanic bath which contains an electrolytic bath solution containing a metal concentration.
  • Chromium electrolytes are preferred as the electrolyte, in particular sulfuric acid chromium electrolytes, mixed acid chromium electrolytes or alloy electrolytes.
  • a preferred electrolyte has a concentration of 180 to 300 grams of chromic acid CrO 3 per liter.
  • third-party additives such.
  • B. sulfuric acid H 2 SO 4 , hydrofluoric acid H 2 F 2 , silica hydrofluoric acid H 2 SiF 6 and mixtures thereof are added.
  • a preferred electrolyte contains 1 to 3.5 grams of sulfuric acid H 2 SO 4 per liter.
  • the galvanic bath is usually heated, the temperature of the electrolyte is preferably 30 to 55 degrees Celsius.
  • An anode and a cathode are immersed in the electrolytic bath solution, the object to be coated forming the cathode or being at least part of the cathode. If a chrome electrolyte is used, platinum-plated platinum or PbSn7 are preferably used as the anode material.
  • Anode and cathode are connected to a device for feeding a process current.
  • the process current can be increased from the initial value to the structure current density in several stages, each with a predeterminable change in the current density of 1 to 6 mA / cm 2 per stage.
  • the time intervals between two current increases can be set between 0.1 and 30 seconds.
  • a process current with a current density in the range of 80% to 120% of the structure current density can be applied for a predeterminable ramp working time.
  • the device can be equipped with a rotary drive for continuously rotating the object.
  • the distance between the anode and the object to be coated is selected in the range from 1 to 40 cm, preferably at 25 cm.
  • Fig. 1 shows the schematic representation of a device for the galvanic application of structural layers.
  • In the galvanic bath is a too coating object 2 and an anode 3 immersed. That too Coating object forms the cathode 2.
  • Anode and cathode are with a controlled electrical energy source 4th connected.
  • the energy source can be an electricity or be a voltage source.
  • the current respectively the Current density at the cathode is decisive for the coating is the process can be more accurate with a power source check.
  • the use of a voltage source has in contrast, the advantage of a lower electrical Circuit effort.
  • the bath temperature and the concentration of the electrolyte are not The process can also be significantly changed with a Check the voltage source well.
  • the electrical energy source 4 is from a programmable control unit 5 controlled.
  • the Control unit can be any time voltage, or specify current curves, which are then automatically via Energy source 4 are placed on the electrodes.
  • Fig. 2 shows the graphical representation of the temporal Process current density curve when generating a Structural layer.
  • 2 is the horizontal axis Time axis, on the vertical axis y is the current density shown. This is an exemplary embodiment for a possible procedure that follows is described in more detail.
  • Figures 3 and 4 show photographic representations of using this process generated structure layer.
  • a sulfuric acid chromium electrolyte with 200 grams of chromic acid CrO 3 and 2 grams of sulfuric acid H 2 SO 4 is used as the galvanic bath.
  • the workpiece to be coated is a rotationally symmetrical component, a dampening cylinder for the printing industry.
  • the cylinder consisting of St52 is first finely ground, with a roughness depth of Rz ⁇ 3 ⁇ m.
  • a 30 ⁇ m thick nickel layer and then a 10 ⁇ m thick, crack-free chrome layer are then applied according to the conditions customary in electroplating.
  • the workpiece prepared in this way is rotated for structural chrome plating in the galvanic bath in order to achieve a coating that is as uniform as possible.
  • the workpiece forms the cathode, platinum-plated titanium or PbSn7 is used as the anode.
  • the anode / cathode electrode spacing is set to 25 cm.
  • the process stream remains switched off during a first process phase 7.
  • This phase serves to acclimatize the workpiece to the galvanic bath.
  • the workpiece takes on the temperature of the electrolyte.
  • a direct current between the anode and cathode is switched on. This remains switched on during phase 8, which lasts about 600 seconds.
  • a chrome-G DC base layer is applied to the workpiece.
  • the current density used is also common for normal chrome plating, here 20 mA / cm 2 .
  • a second phase 9 follows without current.
  • the current density is increased in steps to the structure current density 14.
  • the characteristic data of the stages are varied during the ascent.
  • the current is increased in 16 steps to 40 mA / cm 2 . This corresponds to a change in the current density of 2.5 mA / cm 2 per stage.
  • the time 28 between two current stages is 5 seconds.
  • the current density during phase 11 is then increased in 62 further steps to the structure current density of 100 mA / cm 2 , the time between two current stages is 6 seconds (the current density curve shown in the graph in FIG. 2 is not to scale, the same applies to that in FIG 5 and 6 graphs).
  • this current density is maintained during the ramp working time 12.
  • the direct current flowing thereby leads to the growth of the structural layer produced in phases 10 and 11.
  • the ramp work time is 60 seconds.
  • the current density is again gradually reduced in 22 steps to the final value of 0 mA / cm 2 .
  • the time between two current steps is 4 seconds.
  • Chromium structure layer still a 4 to 8 ⁇ m thick micro-cracked Chrome layer applied. This happens among those in the Electroplating common DC conditions and will be here not explained in more detail.
  • FIG. 3 and 4 show microscopic images of the Chromium structural layer according to that described in FIG. 2 Process was generated.
  • the structure layer exists predominantly of spherical, individual and partial also bodies lying against each other.
  • the "load share” is also as "Material proportion" defined in accordance with DIN 4762.
  • FIG. 5 shows the current density profile over time of a further process sequence for the coating of structures.
  • the process phases 7, 8 and 9 have already been discussed in the explanations for FIG. 2.
  • the current density is increased in 110 identical steps to the structure current density of 100 mA / cm 2 .
  • the time between two current steps is 10 seconds.
  • the current density is reduced, this time in 22 identical steps, to the final value of O mA / cm 2 .
  • the time between two current steps is 4 seconds. Following this, after a brief current-free moment, the process cycle consisting of phases 15, 16 and 17 is repeated.
  • FIG. 6 shows the temporal current density profile of a further method profile.
  • a direct current pulse 18 which corresponds in its nature to the direct current pulse 8 in FIG. 2.
  • a nucleation phase 19 in which the current density is gradually increased to the structure current density 24.
  • the current density is then kept at the structure current density during the ramp working time 20 and is then ramped down to an end value 26 during the phase 21.
  • a nucleation phase 23 with a gradual increase in the current density up to the new structure current density 25.
  • the initial current density of the nucleation phase 23 is equal to the end value 26 to which the current density was reduced at the end of the previous structure generation cycle.
  • the current density is then kept at the structure current density 25 during the ramp working time 27 and subsequently abruptly reduced to the new final value of 0 mA / cm 2 .

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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)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
EP94928407A 1993-10-07 1994-10-01 Verfahren zum galvanischen aufbringen einer oberflächenbeschichtung Expired - Lifetime EP0722515B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4334122 1993-10-07
DE4334122A DE4334122C2 (de) 1992-04-09 1993-10-07 Verfahren zum elektrochemischen Aufbringen einer Oberflächenbeschichtung und Anwendung des Verfahrens
PCT/EP1994/003314 WO1995009938A1 (de) 1993-10-07 1994-10-01 Verfahren zum galvanischen aufbringen einer oberflächenbeschichtung

Publications (2)

Publication Number Publication Date
EP0722515A1 EP0722515A1 (de) 1996-07-24
EP0722515B1 true EP0722515B1 (de) 1998-01-28

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ID=6499571

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EP94928407A Expired - Lifetime EP0722515B1 (de) 1993-10-07 1994-10-01 Verfahren zum galvanischen aufbringen einer oberflächenbeschichtung

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EP (1) EP0722515B1 (zh)
JP (1) JP3293828B2 (zh)
KR (1) KR100332077B1 (zh)
CN (1) CN1044395C (zh)
AU (1) AU7784794A (zh)
BR (1) BR9405631A (zh)
CA (1) CA2172613C (zh)
CH (1) CH690273A5 (zh)
CZ (1) CZ286909B6 (zh)
DE (1) DE59405190D1 (zh)
ES (1) ES2114703T3 (zh)
FI (1) FI103674B (zh)
GR (1) GR3026689T3 (zh)
PL (1) PL177073B1 (zh)
SI (1) SI9420006B (zh)
SK (1) SK281999B6 (zh)
WO (1) WO1995009938A1 (zh)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1441157A1 (de) 2003-01-21 2004-07-28 Fuchs Technology AG Zylinderoberfläche
EP3000918A1 (de) 2014-09-24 2016-03-30 topocrom systems AG Verfahren und Vorrichtung zum galvanischen Aufbringen einer Oberflächenbeschichtung
US11136685B2 (en) 2015-11-05 2021-10-05 Topocrom Systems Ag Method and device for the galvanic application of a surface coating
EP4012074A1 (de) 2020-12-14 2022-06-15 topocrom systems AG Oberflächenbeschichtung und verfahren zu ihrer herstellung

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19828545C1 (de) * 1998-06-26 1999-08-12 Cromotec Oberflaechentechnik G Galvanisches Bad, Verfahren zur Erzeugung strukturierter Hartchromschichten und Verwendung
US6478943B1 (en) 2000-06-01 2002-11-12 Roll Surface Technologies, Inc. Method of manufacture of electrochemically textured surface having controlled peak characteristics
WO2003004732A1 (en) * 2001-07-05 2003-01-16 Roll Surface Technologies, Inc. Electrochemically textured surface having controlled peak characteristics and the method of manufacture
DE10255853A1 (de) 2002-11-29 2004-06-17 Federal-Mogul Burscheid Gmbh Herstellung strukturierter Hartchromschichten
DE102004019370B3 (de) 2004-04-21 2005-09-01 Federal-Mogul Burscheid Gmbh Herstellung einer strukturierten Hartchromschicht und Herstellung einer Beschichtung
DE102008017270B3 (de) 2008-04-04 2009-06-04 Federal-Mogul Burscheid Gmbh Strukturierte Chrom-Feststoffpartikel-Schicht und Verfahren zu deren Herstellung sowie beschichtetes Maschinenelement
AT506076B1 (de) * 2008-06-03 2009-06-15 Vassilios Dipl Ing Polydoros Verfahren zur herstellung von nanostrukturierten chromschichten auf einem substrat
EP2149447A1 (de) 2008-07-29 2010-02-03 Alcan Technology & Management Ltd. Verfahren zur Herstellung einer Materialbahn mit Oberflächenstruktur
CN102877098B (zh) * 2012-10-29 2015-06-17 东莞市若美电子科技有限公司 一种多波段输出的脉冲电镀方法
CN105734631B (zh) * 2014-12-10 2019-03-19 上海宝钢工业技术服务有限公司 冷轧轧辊毛化处理的电镀方法
CN110117802B (zh) * 2019-05-06 2020-05-22 浙江大学 一种多级三维微观结构的制备方法
CN111962120A (zh) * 2020-08-18 2020-11-20 重庆佰鸿机械设备有限公司 一种管件内壁表面处理工艺

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DD134785A1 (de) * 1978-01-25 1979-03-21 Hans Skilandat Verfahren zur elektrolytischen erzeugung eines kupfernen haftbelages auf kupferfolie
US4468293A (en) * 1982-03-05 1984-08-28 Olin Corporation Electrochemical treatment of copper for improving its bond strength
US5185073A (en) * 1988-06-21 1993-02-09 International Business Machines Corporation Method of fabricating nendritic materials
DE4211881C2 (de) * 1992-04-09 1994-07-28 Wmv Ag Verfahren zum elektrochemischen Aufbringen einer strukturierten Oberflächenbeschichtung

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1441157A1 (de) 2003-01-21 2004-07-28 Fuchs Technology AG Zylinderoberfläche
DE10302107A1 (de) * 2003-01-21 2004-07-29 Fuchs Technology Ag Zylinderoberfläche
EP3000918A1 (de) 2014-09-24 2016-03-30 topocrom systems AG Verfahren und Vorrichtung zum galvanischen Aufbringen einer Oberflächenbeschichtung
US11136685B2 (en) 2015-11-05 2021-10-05 Topocrom Systems Ag Method and device for the galvanic application of a surface coating
US11732373B2 (en) 2015-11-05 2023-08-22 Topocrom Systems Ag Method and device for the galvanic application of a surface coating
EP4012074A1 (de) 2020-12-14 2022-06-15 topocrom systems AG Oberflächenbeschichtung und verfahren zu ihrer herstellung

Also Published As

Publication number Publication date
CZ144795A3 (en) 1996-07-17
EP0722515A1 (de) 1996-07-24
CH690273A5 (de) 2000-06-30
DE59405190D1 (de) 1998-03-05
AU7784794A (en) 1995-05-01
PL177073B1 (pl) 1999-09-30
SI9420006A (en) 1995-12-31
SK86195A3 (en) 1996-03-06
CN1044395C (zh) 1999-07-28
SK281999B6 (sk) 2001-10-08
FI952774A0 (fi) 1995-06-06
SI9420006B (sl) 2002-02-28
ES2114703T3 (es) 1998-06-01
GR3026689T3 (en) 1998-07-31
WO1995009938A1 (de) 1995-04-13
CA2172613A1 (en) 1995-04-13
CA2172613C (en) 2003-06-17
CZ286909B6 (en) 2000-08-16
FI103674B1 (fi) 1999-08-13
JP3293828B2 (ja) 2002-06-17
FI952774A (fi) 1995-06-06
FI103674B (fi) 1999-08-13
JPH09503550A (ja) 1997-04-08
PL309286A1 (en) 1995-10-02
CN1115583A (zh) 1996-01-24
BR9405631A (pt) 1999-09-08
KR100332077B1 (ko) 2002-10-31

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