EP2276875B1 - Verfahren zum entschichten von werkstücken und entschichtungslösung - Google Patents

Verfahren zum entschichten von werkstücken und entschichtungslösung Download PDF

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Publication number
EP2276875B1
EP2276875B1 EP09737802.0A EP09737802A EP2276875B1 EP 2276875 B1 EP2276875 B1 EP 2276875B1 EP 09737802 A EP09737802 A EP 09737802A EP 2276875 B1 EP2276875 B1 EP 2276875B1
Authority
EP
European Patent Office
Prior art keywords
solution
stripping
treatment
workpiece
coatings
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.)
Active
Application number
EP09737802.0A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP2276875A1 (de
Inventor
Tamara Andreoli
Udo Rauch
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.)
Oerlikon Surface Solutions AG Pfaeffikon
Original Assignee
Oerlikon Surface Solutions AG Pfaeffikon
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 Oerlikon Surface Solutions AG Pfaeffikon filed Critical Oerlikon Surface Solutions AG Pfaeffikon
Priority to PL09737802T priority Critical patent/PL2276875T3/pl
Publication of EP2276875A1 publication Critical patent/EP2276875A1/de
Application granted granted Critical
Publication of EP2276875B1 publication Critical patent/EP2276875B1/de
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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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/32—Alkaline compositions
    • C23F1/36—Alkaline compositions for etching aluminium or alloys thereof
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/44—Compositions for etching metallic material from a metallic material substrate of different composition
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/32—Alkaline compositions
    • C23F1/38—Alkaline compositions for etching refractory metals
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/20—Other heavy metals
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/20—Other heavy metals
    • C23G1/205—Other heavy metals refractory metals
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/22—Light metals

Definitions

  • the present invention relates to the field of wet chemical stripping of workpieces, in particular of tools and components, which are coated with a hard material layer.
  • a particular focus is on the stripping of hard coatings containing oxides, in particular chromium aluminum oxides (AlCrO layers).
  • Coatings optimized for wear resistance and hardness are also used on others Used components that are exposed to comparable conditions in use and therefore require similar properties; Example are bearing parts and components for the automotive industry such as coated pistons, injectors, etc.
  • the diverse application requirements result in a whole range of specialized layers and layer systems, which in turn entail different stripping requirements.
  • the stripping should be economical (fast, no complicated equipment, cheap consumables, for as many layers applicable), safe (minimize the risk of hazardous substances), environmentally friendly and last but not least the layer-bearing tool or the component should not be damaged by the stripping.
  • the prior art in particular for titanium-containing coatings such as TiN, TiCN, TiAlN, a variety of approaches for wet chemical stripping methods and solutions known. These are usually based on hydrogen peroxide with a stabilizer.
  • the EP 1 029 117 proposes a stripping process using hydrogen peroxide, a base and at least one acid or the salt of an acid.
  • the patent application DE 4339502 describes the non-destructive stripping of carbide substrates, coated with TiAlN layers.
  • the advantages over previous methods are indicated that in addition to the conventional complexing agents and stabilizers, inhibitors for the purpose of corrosion protection, other adjuvants are used, and the solution is adjusted to a pH, in conjunction with the other reagents, a release of Co from the Workpiece prevented. Disadvantages of this solution are the comparatively long stripping time for TiAlN and other coatings, the relatively high use of chemicals and the associated costs, the relatively complicated (because to be observed exactly) formulations and reaction conditions and the use of fluorine-containing reagents.
  • a higher pH range between 9 and 14 is recommended, with a lower permanganate concentration, for example between 10 and 30 g / l, sufficient even at room temperature (approx 15 to 30 ° C) to achieve a complete stripping of 2 to 10 microns thick AlCrN layers within 15 to 60 minutes.
  • a permanganate concentration above 30 g / l is indicated that the rate of disintegration is increased again.
  • US 2005/241679 A1 discloses the complete stripping of 2 to 10 ⁇ m thick AlCrN layers at surface temperature, within 15 to 60 minutes with an alkaline permanganate solution containing 1-3 wt% KMnO4.
  • DE 23 39 608 A1 discloses an alkaline permanganate solution containing 4-6 wt% KMnO4, 8-11 wt% NaOH, 8-11 wt% Na2CO3, and the remainder water.
  • the object of the invention is to provide a method for stripping or a stripping solution, which allow to economically remove hard material layers of at least AlCr, AlCrN and / or AlCrO from a workpiece without substantially damaging the workpiece itself.
  • this object is achieved by a method according to claim 1, wherein the material system for detaching a layer system from a workpiece as an aqueous alkaline solution with 4 Gweichtsprozent KMnO4 da suit, wherein at the same time the alkaline content between 8 and 11 weight percent, preferably 10 weight percent.
  • the alkaline portion is formed in one embodiment by KOH or NaOH, the pH of the solution being above 13, preferably above 13.5.
  • a workpiece which is to be subjected to a method according to the invention has a layer system on the workpiece which comprises at least one layer which in turn comprises at least one of the following materials: metallic TiAlCr and other AlCr alloys; or one of their nitrides, carbides, borides, oxides or their combination and aluminum oxides.
  • the inventive method for detaching this layer system provides to bring the workpiece in a stripping solution according to the above description and to treat it there for a predetermined time.
  • the solution may be agitated during treatment, e.g. B. by stirring or moving the workpiece.
  • the treatment is preferably carried out at room temperature, e. G. between 15 and 30 ° C, but is also at higher temperatures e. G.
  • the z. B. include chemical or mechanical surface treatments. This includes at least one of the following treatment options: rinsing, cleaning, ultrasonic bath treatment, drying, blasting, brushing, heat treatment.
  • the materials 1.2379, ASP2023 (1.3343), 1.2344, SDK (1.3344) and QRS (1.2842) denote various types of steel, including high-alloy steels and high-speed steels.
  • TTX, THM and TTR are indexable tungsten carbide inserts of different composition.
  • Helica refers to an AlCr-based layer material known on the market under the trade name Balinit® Helica.
  • Alcrona refers to an AlCrN coating that is marketed as Balinit® Alcrona.
  • Table 1 Solution Workpiece / material test piece: stripped: 2K / 2Na SDK 11 4K / 10Na SDK 27 4K / 10K SDK 28 2K / 2Na THM 6 4K / 10Na THM 11 4K / 10K THM 12
  • the decoating times were determined under standardized, comparable conditions for different specimens and different layers.
  • the table indicates in which time (minutes) a 4 ⁇ m thick layer is completely removed from the workpiece.
  • Test specimens with a 0.8 ⁇ m high carbon tungsten carbide coating were stripped at 4K / 10Na and 4K / 10K. After 12 hours reaction time with 4K / 10K the test piece was stripped, with 4K / 10Na not yet.
  • Table 7 shows that, although in the first application of the solutions 4K / 10Na and 4K / 10K a stronger removal from the substrate takes place than in the solution according to the prior art. Over time, however, it emerges that in particular the solution 4K / 10K only insignificantly higher removal caused than 4K / 10Na. This is surprising, since actually the high proportion of potassium hydroxide should attack the base material stronger than the otherwise comparable solution with sodium hydroxide.
  • Table 1 shows that the solutions according to the invention are on average twice as effective and permit significantly shorter reaction times (Table 1).

Landscapes

  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • ing And Chemical Polishing (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Chemically Coating (AREA)
  • Weting (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Physical Vapour Deposition (AREA)
EP09737802.0A 2008-05-02 2009-04-09 Verfahren zum entschichten von werkstücken und entschichtungslösung Active EP2276875B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL09737802T PL2276875T3 (pl) 2008-05-02 2009-04-09 Sposób usuwania powłok z obrabianych przedmiotów i roztwór do usuwania powłok

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US4989008P 2008-05-02 2008-05-02
PCT/EP2009/002631 WO2009132758A1 (de) 2008-05-02 2009-04-09 Verfahren zum entschichten von werkstücken und entschichtungslösung

Publications (2)

Publication Number Publication Date
EP2276875A1 EP2276875A1 (de) 2011-01-26
EP2276875B1 true EP2276875B1 (de) 2019-10-09

Family

ID=40810251

Family Applications (1)

Application Number Title Priority Date Filing Date
EP09737802.0A Active EP2276875B1 (de) 2008-05-02 2009-04-09 Verfahren zum entschichten von werkstücken und entschichtungslösung

Country Status (14)

Country Link
US (1) US9057134B2 (enrdf_load_stackoverflow)
EP (1) EP2276875B1 (enrdf_load_stackoverflow)
JP (1) JP5730189B2 (enrdf_load_stackoverflow)
KR (1) KR101599085B1 (enrdf_load_stackoverflow)
CN (1) CN102016122A (enrdf_load_stackoverflow)
BR (1) BRPI0911617B1 (enrdf_load_stackoverflow)
CA (1) CA2723136C (enrdf_load_stackoverflow)
ES (1) ES2764249T3 (enrdf_load_stackoverflow)
MX (1) MX347701B (enrdf_load_stackoverflow)
PL (1) PL2276875T3 (enrdf_load_stackoverflow)
PT (1) PT2276875T (enrdf_load_stackoverflow)
RU (1) RU2507311C2 (enrdf_load_stackoverflow)
SG (1) SG188875A1 (enrdf_load_stackoverflow)
WO (1) WO2009132758A1 (enrdf_load_stackoverflow)

Families Citing this family (15)

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US20110086914A1 (en) * 2009-10-13 2011-04-14 Bailes Julian E Methods for Treating Traumatic Brain Injury
DE102011105645A1 (de) 2011-06-07 2012-12-13 Oerlikon Trading Ag, Trübbach Entschichtungsverfahren für harte Kohlenstoffschichten
MX346032B (es) 2011-06-07 2017-03-02 Oerlikon Surface Solutions Ag Pfäffikon Proceso para retirar capas duras de carbono.
CN102277587B (zh) * 2011-07-29 2013-06-05 沈阳大学 一种多组元氮化物硬质反应膜的退除方法
WO2015139731A1 (de) * 2014-03-18 2015-09-24 Platit Ag Verfahren zum entschichten von keramischen hartstoffschichten von stahl- und hartmetall-substraten
US9406534B2 (en) * 2014-09-17 2016-08-02 Lam Research Corporation Wet clean process for cleaning plasma processing chamber components
JP6334500B2 (ja) * 2015-11-19 2018-05-30 株式会社ジーテクト アルミニウムめっき鋼板の溶接方法
CN106884168A (zh) * 2017-04-07 2017-06-23 苏州星蓝纳米技术有限公司 一种硬质合金退涂液及其配制和使用方法
CN107829090A (zh) * 2017-11-15 2018-03-23 温州职业技术学院 Dlc涂层的脱除方法
CN110541169B (zh) * 2018-06-29 2021-12-28 蓝思科技股份有限公司 一种用于脱除工件表面镀层的褪镀液及褪镀方法
US11377745B2 (en) 2018-08-21 2022-07-05 Oerlikon Surface Solutions Ag, Pfäffikon Stripping of coatings Al-containing coatings
CN111676448A (zh) * 2020-06-12 2020-09-18 艾瑞森表面技术（苏州）股份有限公司 一种可褪涂的TiAlCrN纳米复合涂层的制备方法
CN112323136A (zh) * 2020-10-26 2021-02-05 深圳市裕展精密科技有限公司 退镀液以及退镀方法
CN115637433A (zh) * 2022-09-28 2023-01-24 国营川西机器厂 Al/BN封严涂层去除方法
CN120322570A (zh) 2022-12-20 2025-07-15 沃尔弗拉姆矿业与冶炼股份公司 制备用于回收的硬质合金废料的方法

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Also Published As

Publication number Publication date
US9057134B2 (en) 2015-06-16
MX2010011871A (es) 2010-11-30
MX347701B (es) 2017-05-09
PT2276875T (pt) 2020-01-17
RU2507311C2 (ru) 2014-02-20
CA2723136A1 (en) 2009-11-05
RU2010149274A (ru) 2012-06-10
CN102016122A (zh) 2011-04-13
BRPI0911617B1 (pt) 2023-11-07
BRPI0911617A2 (enrdf_load_stackoverflow) 2017-07-25
WO2009132758A1 (de) 2009-11-05
ES2764249T3 (es) 2020-06-02
KR20110003507A (ko) 2011-01-12
JP5730189B2 (ja) 2015-06-03
SG188875A1 (en) 2013-04-30
EP2276875A1 (de) 2011-01-26
PL2276875T3 (pl) 2020-06-01
US20110056914A1 (en) 2011-03-10
JP2011520033A (ja) 2011-07-14
CA2723136C (en) 2017-11-07
KR101599085B1 (ko) 2016-03-14

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