EP3617350A1 - Procédé de revêtement d'une pièce métallique destinée à être soumise à de hautes pressions de contact et pièce métallique obtenue à partir de celui-ci - Google Patents

Procédé de revêtement d'une pièce métallique destinée à être soumise à de hautes pressions de contact et pièce métallique obtenue à partir de celui-ci Download PDF

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Publication number
EP3617350A1
EP3617350A1 EP18382639.5A EP18382639A EP3617350A1 EP 3617350 A1 EP3617350 A1 EP 3617350A1 EP 18382639 A EP18382639 A EP 18382639A EP 3617350 A1 EP3617350 A1 EP 3617350A1
Authority
EP
European Patent Office
Prior art keywords
layer
range
metal part
comprised
copper
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.)
Pending
Application number
EP18382639.5A
Other languages
German (de)
English (en)
Inventor
Huirong LE
Maozhou MENG
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.)
Tubacex Upstream Technologies SA
Original Assignee
Tubacex Upstream Technologies 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 Tubacex Upstream Technologies SA filed Critical Tubacex Upstream Technologies SA
Priority to EP18382639.5A priority Critical patent/EP3617350A1/fr
Priority to PCT/EP2019/073222 priority patent/WO2020043882A1/fr
Publication of EP3617350A1 publication Critical patent/EP3617350A1/fr
Pending legal-status Critical Current

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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
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • 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
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1646—Characteristics of the product obtained
    • C23C18/165—Multilayered product
    • C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
    • 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
    • C23C18/52—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 using reducing agents for coating with metallic material not provided for in a single one of groups C23C18/32 - C23C18/50
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/38—Electroplating: Baths therefor from solutions of copper
    • 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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/003—Threaded pieces, e.g. bolts or nuts

Definitions

  • the present invention relates to coatings.
  • coatings that improve anti-galling and frictional properties of metal parts.
  • Threaded joints of oil and gas ducts are subjected to high contact pressures that cause the opposite contact surfaces to bond, i.e. to weld in the atomic level. Since the joined parts have to move relative to each other during make and breaks, this bond may lead to galling of the contact surfaces.
  • the production of galling can be minimized by reducing the stiction and coefficient of friction between the parts.
  • a solution to prevent galling is to coat the parts.
  • electrolytic plating and electroless plating are known.
  • the electrolytic deposition techniques are based on the application of electric current.
  • One of the advantages of these known techniques is the speed of deposition, which makes them particularly suitable when it comes to depositing relatively thick layers, such as, for example, of the order of 10 ⁇ m.
  • the coating is obtained without the application of current.
  • This technique allows for obtaining very uniform coatings, especially when the coating to be deposited is relatively thin, say 1 ⁇ m.
  • a major advantage of the uniformity is that it results in an improved performance of the joint.
  • US2015159277 discloses an aqueous electroless nickel plating bath for forming electroless nickel coatings that includes nickel, a hypo phosphorous reducing agent, zinc, a bismuth stabilizer, and a complexing agent.
  • WO8201015A1 (Shipley company Inc.) discloses combinations of copper/ nickel electroless coating where copper amounts to up to 70%, nickel being excluded from being an important part of the coating due to its bad electrical conducting properties.
  • a secondary objective is to reduce the use of lubricating greases containing polluting metals.
  • the invention provides an efficient method for coating a metal part destined to be subjected to high contact pressures, an external surface of the metal part forming a substrate to be coated, which comprises the following steps:
  • the proposed method allows for reducing the stiction and coefficient of friction, and thus improving the anti-galling properties and corrosion resistance. Moreover, thanks to the stiction and coefficient of friction reduction, it is possible to use non-contaminant greases while keeping the performance of lead containing greases. In particular, the friction or anti-galling properties of the coating produced satisfies the standard requirements when an environmentally friendly lubricant is used.
  • the proposed method achieves its beneficial effects thanks to the combination of three clearly differentiated layers, as well as the created bronze interface.
  • the electrolytic plating has proved in the present case to be an efficient process to generate the thickness required for the second layer.
  • the method is especially efficient when is applied to carbon steel, stainless steel or nickel-based alloys, which are generally used for OCTG (Oil Country Tubular Goods) pipes in API5CT, API5CRA and API6A standards.
  • the step a) of the method is carried out with an immersion in a solution containing hydrochloric acid (HCI) and nickel chloride hexahydrate (NiCl 2 ⁇ 6H 2 O).
  • HCI hydrochloric acid
  • NiCl 2 ⁇ 6H 2 O nickel chloride hexahydrate
  • the hydrochloric acid concentration is in the range of 5% - 10% in weight and the nickel chloride hexahydrate is in the range of 150 - 300 g/L, the anode being nickel having at least a 99.5% purity.
  • This concentration allows to improve significantly the adhesion of the subsequent layer.
  • the thickness of the first layer is comprised in the range of 0.1-1 ⁇ m. This thickness provides a good bonding between coating film and substrate material.
  • the nickel strike is processed at room temperature.
  • the electrolytic plating is carried out in a solution containing copper sulphate pentahydrate (CuSO 4 ⁇ 5H 2 O) and sulfuric acid (H 2 SO 4 ).
  • An advantage is that the coating does not delaminate while allowing a high yield coating method.
  • Another advantage is that it allows to control the thickness of the deposited copper layer, ensuring an appropriate adhesion strength.
  • the thickness of the second layer is comprised in the range of 6 - 12 ⁇ m, and is preferably 10 ⁇ m.
  • the step c) comprises an electroless coating.
  • the advantage of electroless method is to deposit a uniform layer of coating, regardless of the surface profile of substrate and avoid the 'shielding' effect in electrolytic plating process.
  • a further advantage of the electroless method is that it allows to control the thickness of the coating of a rough surface.
  • the electroless coating is applied with a solution containing stannous sulphate (SnSO 4 ), thiourea (CH 4 N 2 S) and sulfuric acid (H 2 SO 4 ).
  • SnSO 4 stannous sulphate
  • thiourea CH 4 N 2 S
  • sulfuric acid H 2 SO 4
  • the thickness of the third layer is comprised in the range of 0,4 -- 0,6 ⁇ m and is preferably 0,5 ⁇ m.
  • the method comprises a further step d) consisting in baking the obtained coating at 150-200 °C.
  • the baking at 150-200 °C improves the coating quality by two reasons: a) releasing residual stress; b) strengthening the third layer itself and the bonding with the copper layer underneath.
  • the metal part is a pin and/or a box of a threaded joint for oil and gas applications.
  • the present invention provides a metal part destined to be subjected to high contact pressures, the metal part having an external layer which forms a substrate, the substrate having a coating, wherein the coating comprises:
  • the metal part is a pin and/or a box of a threaded joint for oil and gas applications
  • the present invention relates to a method for coating a metal part P destined to be subjected to high contact pressures, in particular to pin and/or a box of a threaded joint for oil and gas applications.
  • the metal part P forms the substrate S to be coated.
  • the method comprises the following steps:
  • Step a is carried out with a bath in a solution containing hydrochloric acid HCl and nickel chloride hexahydrate NiCl 2 ⁇ 6H 2 O, wherein the hydrochloric acid concentration is in range 5% - 10% in weight and the nickel chloride hexahydrate is in the in range 150 - 300 g/L, the anode being nickel having at least a 99.5% purity.
  • the first layer 1 is comprised in the range of 0.1-1 ⁇ m.
  • the electrolytic plating is carried out in a solution containing copper sulphate pentahydrate CuSO 4 ⁇ 5H 2 O and sulfuric acid H 2 SO 4 , wherein:
  • the electronic current density on anode should be less than 5 A/cm 2 without agitation, or 17 A/cm 2 with agitation.
  • the second layer 2 is comprised in the range of 6 - 12 ⁇ m, and is preferably 10 ⁇ m.
  • Step c is an electroless coating applied with a solution containing stannous sulphate SnSO 4 , thiourea CH 4 N 2 S and sulfuric acid H 2 SO 4 , and wherein:
  • Step c) has to be applied such that the thickness of the third layer 3 is comprised in the range of 0,4 and 0,6 ⁇ m and is preferably 0,5 ⁇ m.
  • the electroless process applies a very thin layer of tin on top of the copper layer.
  • the electroless bronze solution contains stannous sulphate (S n SO 4 ), thiourea (CH 4 N 2 S) and sulfuric acid (H 2 SO 4 ).
  • the thiourea reduces the electrode potential of copper, so that it reduces stannous ion, and then an ultrathin tin layer is formed on top of copper.
  • Name Formula g/L mol/L Stannous sulphate S n SO 4 4.5 0.021 Thiourea CH 4 N 2 S 50 0.658 Sulfuric acid H 2 SO 4 20 0.204
  • the S n SO 4 and CH 4 N 2 S must be dissolved in H 2 SO 4 and deionized water respectively first, and then mixed together.
  • the electroless bronze can be processed at room temperature.
  • the deposition initiates automatically when the part to be coated is immersed into the electroless bronze solution. After a few minutes (about 2 minutes), the process is stopped automatically when all the surface of copper is covered by tin.
  • coated parts P obtained can be used in dry-type joints, their preferred use will be with in wet joints, that is with the use of a lubricating grease interposed between the two parts (threaded pin and box for oil and gas applications) subjected to high mutual pressures.
  • API is harmful due to its heavy metal content
  • the green dope is respectful of the environment.
  • Figure 2 represents the evolution of the coefficient of friction after applying several pressure cycles with the tests disclosed in " Characterisation of friction and lubrication regimes in premium tubular connections" from F. Stewart, H.R.Le, J.A.Williams, A.Leech, B.Bezensek, A.Roberts .
  • the objective of this test is to determine the behavior of the coating in the long term and what is obtained is the surprising result illustrated.
  • FIG. 3 is the graph obtained with the use of green dope. The result is maintained in a reduction with the aforementioned percentage, i.e. 15%.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Chemically Coating (AREA)
EP18382639.5A 2018-08-31 2018-08-31 Procédé de revêtement d'une pièce métallique destinée à être soumise à de hautes pressions de contact et pièce métallique obtenue à partir de celui-ci Pending EP3617350A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP18382639.5A EP3617350A1 (fr) 2018-08-31 2018-08-31 Procédé de revêtement d'une pièce métallique destinée à être soumise à de hautes pressions de contact et pièce métallique obtenue à partir de celui-ci
PCT/EP2019/073222 WO2020043882A1 (fr) 2018-08-31 2019-08-30 Procédé d'application de revêtement sur une pièce métallique destinée à être soumise à de fortes pressions de contact et pièce métallique ainsi obtenue

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP18382639.5A EP3617350A1 (fr) 2018-08-31 2018-08-31 Procédé de revêtement d'une pièce métallique destinée à être soumise à de hautes pressions de contact et pièce métallique obtenue à partir de celui-ci

Publications (1)

Publication Number Publication Date
EP3617350A1 true EP3617350A1 (fr) 2020-03-04

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP18382639.5A Pending EP3617350A1 (fr) 2018-08-31 2018-08-31 Procédé de revêtement d'une pièce métallique destinée à être soumise à de hautes pressions de contact et pièce métallique obtenue à partir de celui-ci

Country Status (2)

Country Link
EP (1) EP3617350A1 (fr)
WO (1) WO2020043882A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113186522A (zh) * 2021-05-26 2021-07-30 西南科技大学 一种用于钛合金表面化学镀的锡盐敏化活化方法

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1982001015A1 (fr) 1980-09-15 1982-04-01 Shipley Co Placage d'alliages sans courant electrique
US4527815A (en) 1982-10-21 1985-07-09 Mobil Oil Corporation Use of electroless nickel coating to prevent galling of threaded tubular joints
US4758025A (en) 1985-06-18 1988-07-19 Mobil Oil Corporation Use of electroless metal coating to prevent galling of threaded tubular joints
US4816070A (en) * 1985-08-29 1989-03-28 Techo Instruments Investments Ltd. Use of immersion tin and alloys as a bonding medium for multilayer circuits
WO2003060198A1 (fr) * 2001-12-24 2003-07-24 Hunting Oilfield Services (Uk) Ltd Element tubulaire presentant un revetement anti-eraillure$i( )
US20040086656A1 (en) 2001-11-06 2004-05-06 Kohl Paul A. Electroless copper plating solutions and methods of use thereof
EP2128506A1 (fr) * 2007-03-02 2009-12-02 SUMITOMO METAL INDUSTRIES, Ltd. Joint à vis pour tuyau en acier
WO2013073712A1 (fr) * 2011-11-18 2013-05-23 Nippon Steel & Sumitomo Metal Corporation Raccord fileté tubulaire aux performances de couple élevé améliorées
US20150159277A1 (en) 2012-07-17 2015-06-11 Coventya, Inc. Electroless nickel coatings and compositions and methods for forming the coatings

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1982001015A1 (fr) 1980-09-15 1982-04-01 Shipley Co Placage d'alliages sans courant electrique
US4527815A (en) 1982-10-21 1985-07-09 Mobil Oil Corporation Use of electroless nickel coating to prevent galling of threaded tubular joints
US4758025A (en) 1985-06-18 1988-07-19 Mobil Oil Corporation Use of electroless metal coating to prevent galling of threaded tubular joints
US4816070A (en) * 1985-08-29 1989-03-28 Techo Instruments Investments Ltd. Use of immersion tin and alloys as a bonding medium for multilayer circuits
US20040086656A1 (en) 2001-11-06 2004-05-06 Kohl Paul A. Electroless copper plating solutions and methods of use thereof
WO2003060198A1 (fr) * 2001-12-24 2003-07-24 Hunting Oilfield Services (Uk) Ltd Element tubulaire presentant un revetement anti-eraillure$i( )
EP2128506A1 (fr) * 2007-03-02 2009-12-02 SUMITOMO METAL INDUSTRIES, Ltd. Joint à vis pour tuyau en acier
WO2013073712A1 (fr) * 2011-11-18 2013-05-23 Nippon Steel & Sumitomo Metal Corporation Raccord fileté tubulaire aux performances de couple élevé améliorées
US20150159277A1 (en) 2012-07-17 2015-06-11 Coventya, Inc. Electroless nickel coatings and compositions and methods for forming the coatings

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113186522A (zh) * 2021-05-26 2021-07-30 西南科技大学 一种用于钛合金表面化学镀的锡盐敏化活化方法
CN113186522B (zh) * 2021-05-26 2022-01-28 西南科技大学 一种用于钛合金表面化学镀的锡盐敏化活化方法

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