Institute of Metallurgy and Materials Science, Polish Academy of Sciences

Metal-ceramic composites and nanocomposites for aerospace and automotive industry (POIG.01.03.01-14-013/08)

Posted by Jerzy from Institute of Metallurgy and Materials Science, Polish Academy of SciencesResponsive · Knowhow and Research output · Poland

Summary of the technology

Nanocrystalline alloy (Ni-Mo, Ni-W) and composite (Ni-Mo/Al2O3, Ni-Mo/Al2O3) coatings

Metallic alloys of Ni-Mo and Ni-W were deposited from solutions containing sodium molybdate (Na2MoO4) or sodium tungstate (Na2WO4), and nickel sulphate (NiSO4), as the source of Mo(VI), W(VI) and Ni(II) ions, respectively. As the complexing agent citrate ions (C6H5O73-) were used, introduced into solutions in the form of sodium citrate (Na3C6H5O7). In the bath for Ni-W coatings electrodeposition, sodium chloride (NaCl) and ammonium chloride (NH4Cl) were additionally added as factors increasing the conductivity of the solution. The pH of the electrolyte solution was adjusted with the appropriate amount of H2SO4 or NH4OH.

Description of the technology

Nanocrystalline alloy (Ni-Mo, Ni-W) and composite (Ni-Mo/Al2O3, Ni-Mo/Al2O3) coatings

Metallic alloys of Ni-Mo and Ni-W were deposited from solutions containing sodium molybdate (Na2MoO4) or sodium tungstate (Na2WO4), and nickel sulphate (NiSO4), as the source of Mo(VI), W(VI) and Ni(II) ions, respectively. As the complexing agent citrate ions (C6H5O73-) were used, introduced into solutions in the form of sodium citrate (Na3C6H5O7). In the bath for Ni-W coatings electrodeposition, sodium chloride (NaCl) and ammonium chloride (NH4Cl) were additionally added as factors increasing the conductivity of the solution. The pH of the electrolyte solution was adjusted with the appropriate amount of H2SO4 or NH4OH.

The coating electrodeposition was conducted in a model system with a rotating disc electrode (RDE), using a PAR 273A potentiostat/galvanostat under galvanostatic or potentiostatic conditions, in a 0.5 L or 0.75 L glass cell. Low carbon steel (S235JR) discs (about 0.03 dm2) were used as cathodes, which, prior to experiments were degreased in the acetone and then chemically polished in a solution of hydrogen peroxide and oxalic acid. The edges of the discs were masked with a non-conductive varnish in order to isolate the side surface of the cathode from the electrolyte solution.The cathode potentials were referred to the saturated calomel electrode (SCE) and were corrected for ohmic drop by the current interupt method (CI). A platinum wire (about 0.5 dm2) was used as an anode.

To prevent particle agglomeration during deposition of composite coating, prior to experiments, the alumina powder was mechanically dispersed in the bath using a mechanical stirrer (IKA Yellow line, 500 rpm) for 24 h. During the last 1 h the suspension was additionally treated by ultrasound of 35 kHz frequency (ELMA TI-H-160). In electrodeposition process, additionally to the disc cathode rotating, the intensive mechanical stirring was employed, in order to maintain the Al2O3 powder in suspension. In part of experiments, during the composite coatings electrodeposition process the outer field of ultrasound at a frequency of 35 kHz or 130 kHz was used. After electrolysis the samples were ultrasonically cleaned in ethanol for 1 min to remove loosely adsorbed particles from the coating surface and then dried.

Based on systematic, experimental investigations, the electrolyte solutions with following composition were selected:

- for electrodeposition Ni-Mo alloys: 0.2M NiSO4, 0.3M Na3C6H5O7, 0.006M Na2MoO4, pH 9,

- for electrodeposition Ni-W alloys: 0.1M NiSO4, 0.2M Na2WO4, 0.5M Na3C6H5O7, 0.5M NH4Cl and 0.1M NaCl, pH 8.

Consequently, the baths of the above, optimised compositions, containing the nanocrystalline Al2O3 ceramic phase (analysed concentration range from 5 g/L to 100 g/L), were used for electrodeposition Ni-Mo/Al2O3 and Ni-W/Al2O3 nanocomposite coatings.

The result of the project (task KCM3) was presented in:

- monography: Indukowane elektroosadzanie nanokrystalicznych powłok metalicznych i kompozytowych typu Ni-W(Mo)/ Al2O3 – autor prof. dr hab. Ewa Bełtowska-Lehman

- PhD thesis:

dr inż. Paulina Indyka - Optymalizacja mikrostruktury i właściwości powłok Ni-W osadzanych elektrochemicznie

dr Agnieszka Bigos - Wpływ wybranych parametrów elektroosadzania na właściwości nanokrystalicznych powłok metalicznych Ni-Mo oraz kompozytowych Ni-Mo/Al2O3

- publications:

1. E. Beltowska-Lehman, A. Bigos, P. Indyka, Characterization of electrodeposited nanocrystalline Ni-Mo protective coatings, Physicochemical Mechanics of Materials, 8 (2010) 324-329

2. E. Beltowska-Lehman, A. Bigos, P. Indyka, L. Tarkowski, M. Kot, J. Morgiel, Electrodeposition of nanocrystalline Ni-Mo coatings from citrate electrolyte solution, Inżynieria Materiałowa, 3 (2010) 369-372

3. M. Kot, E. Beltowska-Lehman, A. Bigos, P. Indyka, J. Morgiel, W. Rakowski, Mechanical and tribological properties of electrodeposited Ni-Mo coatings, Inżynieria Materiałowa, 3 (2010) 373-376

4. P. Indyka, E. Beltowska-Lehman, A. Bigos, J. Morgiel, M. Kot, L. Tarkowski, Optimization of galvanic bath composition and operating parameters for electrodeposition of Ni-W coatings, Inżynieria Materiałowa, 3 (2010) 377-381

5. P. Indyka, E. Beltowska-Lehman, M. Faryna, K. Berent, Microstructural and microchemical characterization of the nickel-based thin films prepared by electrodeposition, Archives of Metallurgy and Materials, 55 (2010) 421-427

6. A. Bigos, E. Beltowska-Lehman, P. Indyka, J. Morgiel, Electrodeposition of nanocrystalline matrix Ni-Mo/Al2O3 composites, Composites, 11(2) (2011) 157-162

7. M. Kot, E. Bełtowska-Lehman, A. Bigos, P. Indyka, J. Morgiel, S. Zimowski, Właściwości powłok Ni-Mo nakładanych metodą elektrochemiczną, Tribologia, 235 (2011) 65-72

8. E. Beltowska-Lehman, P. Indyka, A. Bigos, M. Kot, L. Tarkowski, Electrodeposition of nanocrystalline Ni-W coatings strengthened by ultrafine alumina particles, Surface & Coatings Technology, 211 (2012) 62-66

9. E. Beltowska-Lehman, A. Bigos, P. Indyka, M. Kot, Electrodeposition and characterization of nanocrystalline Ni-Mo functional coatings, Surface & Coatings Technology, 211 (2012) 67-71

10. E. Beltowska-Lehman, P. Indyka, Kinetics of Ni-Mo electrodeposition from Ni-rich citrate baths, Thin Solid Films, 520 (2012) 2046-2051

11. P. Indyka, E. Beltowska-Lehman, J. Morgiel, M. Bieda, L. Tarkowski, Microstructure and deposition relations in alumina particle strengened Ni-W matrix composites, Solid State Phenomena, 186 (2012) 234-238

12. A. Bigos, E. Beltowska-Lehman, P. Indyka, Microstructure and mechanical properties of nanocrystalline Ni-Mo protective coatings, IOP Conference Series: Materials Science and Engineering, 32 (2012) doi:10.1088/1757-899X/32/1/012002

13. P. Indyka, E. Beltowska-Lehman, A. Bigos, Microstructural characterization of electrodeposited coatings of metal matrix composite with alumina nanoparticles, IOP Conference Series: Materials Science and Engineering, 32 (2012) doi:10.1088/1757-899X/32/1/012010

14. A. Bigos, E. Bełtowska-Lehman, P. Indyka, M.J. Szczerba, M. Kot, Electrodeposition and properties of nanocrystalline Ni-based alloys containing refractory metal obtained from citrate baths, Archives of Metallurgy and Materials 58(1) (2013) 247-253

15. K.P. Mroz, A. Bigos, S. Kucharski, K. Dolinski, E. Bełtowska-Lehman, Ni-W Electrodeposited Coatings on Low Carbon Steel Substrate: Fatigue Observations, Journal of Materials Engineering and Performance, 23(10) (2014) 3459-3466

16. K.P. Mróz, S. Kucharski, K. Doliński, A. Bigos, G. Mikułowski, E. Beltowska-Lehman, P. Nolbrzak, Failure modes of coatings on steel substrate, Bulletin of the Polish Academy of Sciences, Technical Sciences, 64(1) (2016) 249-256

- KomCerMet yearbooks: Metal-ceramic composites and nanocomposites for aerospace and automotive industry, 2009, 2010, 2011, http://www.komcermet.ippt.gov.pl/

-presentations:

E-MRS SPRING MEETING - Advanced Functional Materials, Symposium P: Protective Coatings and Thin Films, 2009, Strasbourg, France, Book of Abstracts, P-9, PP7 11

- poster: Electrochemical deposition of Nickel-Molybdenum coatings in Ni-rich citrate baths

EMAS 2009 11th European Workshop on Modern Developments and Applications, 2009, Gdynia/Rumia, Poland, Book of Tutorials and Abstracts, p. 257

- poster: Microstructural and microchemical, evaluation of nickel-based coatings produced by electrodeposition

Physical Metallurgy and Materials Science Conference, Advanced Materials and Technologies AMT 2010, Zakopane, Poland

- poster: Optimization of galvanic bath composition and operating parameters for electrodeposition of Ni-W coatings, XIXth

X International Conference and Exhibition Corrosion Problems and Antiсorrosive Protection of Construction Materials, 2010, Lviv, Ukraine

- poster: Characterization of electrodeposited nanocrystalline Ni-Mo protective coatings

EMAS 2010 9th Regional Workshop on Electron Probe Microanalysis of Materials Today-Practical Aspects, 2010, Amsterdam, The Netherlands

- poster: Microstructural and Electrochemical studies of codeposited Ni-W/Al2O3 nanocomposite coatings

Presentation in WSK PZL-Rzeszów S.A.,Poland

- presentation: Powłoki Ni-W(Mo)/Al2O3 wytwarzane techniką elektrochemiczną

KOMPOZYTEXPO 2011,Krakow, Poland

- presentation: Powłoki nanokompozytowe Ni-W/Al2O3 wytwarzane techniką elektrochemiczną

XII International Conference: EMAS: European Workshop on Modern Developements and Applications in Microbeam Analysis, 2011, Angers, France

- poster: Microstructure and mechanical properties of nanocrystalline Ni-Mo protective coatings

- poster: Microstructural characterization of electrodeposited coatings of metal matrix composite with alumina nano-particles

E-MRS 2011 Spring Meeting & Bilateral Energy Conference, Symposium K: Protective coatings and thin films, 2011, Nice, France

- poster: Electrodeposition and characterisation of nanocrystalline Ni-Mo functional coatings

- poster: Microstructural characterization of electrodeposited coatings of metal matrix composite with alumina nano-particles

E-MRS 2011 Spring Meeting & Bilateral Energy Conference, Symposium M: X-ray techniques for materials research - from laboratory sources to free electron lasers, 2011, Nice, France,

- presentation: XRD characterization of Ni-based coatings prepared by electrodeposition

XV Sympozjum: Kompozyty – teoria i praktyka, 2011, Spała, Poland
- prezentacja: Electrodeposition of nanocrystalline matrix Ni-Mo/Al2O3 composites

The XIVth International Conference on Electron Microscopy, 2011, Wisla, Poland,

Electron Microscopy XIV- selected, peer reviewed papers, p. 234

- poster: Microstructure and deposition relations in alumina particle strengthened Ni-W matrix composites

Joint PhD Seminar, 2012, Radeburg, Germany,

- presentation: Electrodeposition and characterization of nanocrystalline Ni-Mo and Ni-Mo/Al2O3 coatings.

European Advanced Training Course: Nano-scale Materials and Advanced Characterization Techniques, 2012, Drezden, Germany

- presentation: Microstructure control and property optimization of electrodeposited coatings

11th International Symposium on Electrochemical/Chemical Reactivity
of Metastable Materials
, 2012, Kraków, Polska

-presentation: Electrodeposition and properties of nanocrystaline Ni-Mo alloys obtained from citrate-ammonia baths

Wiosenne Zjazdy Sekcji Studenckiej PTChem, 2012, Łazy, Polska,

- presentation: Electrodeposition of the Ni-Mo matrix nanocomposites reinforced by Al2O3 particles from ammonia-citrate bath

Scientific projects which are a continuation of works started in the KomCerMet:

- NCN 2011/01/B/ST8/03974, Nanocomposite Ni-W/ZrO2 coatings obtained by electrochemical deposition as an alternative to toxic chromium coatings - preparation, characterisation and properties – project manager – prof. dr hab. Ewa Bełtowska-Lehman

- Functional properties optimization of amorphous and nanocrystalline Ni-W coatings produced by electrochemical technique through heat treatment – project manager – dr inż. Paulina Indyka

Technology Owner

Institute of Metallurgy and Materials Science, Polish Academy of Sciences

Non-Profit Research Organization

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About Institute of Metallurgy and Materials Science, Polish Academy of Sciences

Non-Profit Research Organization from Poland

The Institute of Metallurgy and Materials Science, Polish Academy of Sciences is one of the leading research centers in the field of fundamental and applied materials science. The research activities correspond to the priorities of Ministry of Science and Education, Polish Academy of Sciences and programs of the European Community. The research is performed based a long-term co-operation with large number of scientific institutions in Poland and such countries as: Austria, Canada, France, Germany, South Africa, Hungary, Israel, Japan, Korea, Russia, Spain, Slovakia, USA, Japan, Holland, Slovenia, Ukraine, Taiwan and Korea. Eighty-nine people are employed in the institute, including 45 scientific staff: 9 full professors, 15 associate professors (with D.Sc.), 19 assistant professors (with Ph.D.) and 2 assistants (with MSc).
For many years, Institute has been authorized to award the Ph.D. and D.Sc. degrees, conducts doctoral studies and is recognized by the Polish Academy of Sciences and Government Evaluation Committees as one of the best in the field of materials science.

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