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Study of particle-current-electrocrystallization interactions in electroplating of Ni/SiC coatings
Jönköping University, School of Engineering, JTH, Materials and Manufacturing.ORCID iD: 0000-0001-7228-1188
2019 (English)Licentiate thesis, comprehensive summary (Other academic)
Abstract [en]

Composite coatings have great potential due to the possibility to combine properties of two different materials in one coating. This way, new surface properties can be tailored and applied to any material's surface. Among different manufacturing routes, electrodeposition has the biggest potential in creating composite metal matrix coatings, especially nanocomposites. Nevertheless, there is a knowledge gap between the deposition of composite coatings in laboratory conditions, described in the literature, and those that are now in place on an industrial level. While micro-composites have been industrialised for about ten years, the production of Ni/SiC nanocomposite coatings by electroplating is still far from an industrial manufacturing floor. This is due to the lack of understanding of the mechanisms of nanoparticles codeposition leading to scattering results.

The production of nanocomposite coatings is much more sensitive to the process parameters compared to microcomposite. The correlation between parameters and their influence on the codeposition are still not fully identified and understood. The codeposition models proposed in the literature are only valid in specific conditions, but composite depositions behave differently, or even opposite if some of the variables are modified.

The main objective of this work is to identify the particle-current-electrocrystallization interactions in the production of Ni/SiC nanocomposites. A series of experiments are designed to isolate single variables and identify the controlling parameters of these interactions and their impact on the final properties.

In this thesis, the effect of current density, type of current and particles size are identified as primary variables controlling the metal crystallisation and coatings properties.

Among many parameters, a specific current waveform in pulse reverse mode proved to increase the codeposition rate effectively, doubling the content of nanoparticles compared to other techniques. Ultrasound assistance is also considered as stirring method when particles are suspended in the deposition bath to increase their stability and dispersion. The effect of Ultrasound on the particles codeposition and metal crystallisation is studied and compared to silent condition.

Moreover, a surface treatment for the particle has been proven successful in making any particle to behave similarly in the Ni deposition bath. Furthermore, the codeposition rate doubled or tripled compared to untreated ones thanks to this treatment. Both ultrasonic agitation and surface treatment reduce the formation of aggregates, improving the particle dispersion and metal microstructure thus increasing the final hardness.

The work proved the synergistic effect between particle and metal microstructure which affected the final properties of the coating. Therefore, when tailoring the composite coating to improve hardness, it is not only the amount of the particles that should be considered but also their influence on the electrocrystallisation process.

Abstract [sv]

Kompositbeläggning har stort potential tack vare möjligheten att kombinera två material i samma ytskikt. På detta sätt kan nya ytegenskaper skräddarsys och appliceras på ett materials yta. Elektrodeposition är den tillverkningsmetod som har störst potential att uppnå kompositbeläggningar, i synnerhet nanokompositer. Ett kunskapsgap existerar mellan elektrodeposition under laboratorieförhållanden, som beskrivet i vetenskaplig litteratur, och hur processen går till i industriell miljö. Medan industriell tillämpning av mikrokompositer pågått ungefär tio år, så har produktion av Ni/SiC nanokompositbeläggningar fortfarande inte nått fabriksgolvet. Detta är en konsekvens av bristande förståelse kring mekanismer för samdeposition av nanopartiklar som leder till varierande resultat.

Produktion av nanokompositbeläggningar är mycket mer känslig för processparametrar jämfört med mikrokompositer. Korrelationer mellan parametrar och dess inverkan på samdeposition är fortfarande inte fullt identifierade och förstådda. Modeller för samdeposition som föreslås i vetenskaplig litteratur är endast giltiga under särskilda förhållanden. Kompositdeposition kan uppvisa avvikande eller till och med motsatt beteende om variabler förändras.

Huvudmålet med detta arbete är att identifiera interaktioner mellan partikel, ström och elektrokristallisering under tillverkning av Ni/SiC nanokompositer. En serie av experiment är utvecklade för att isolera variabler och identifiera de parametrarna som kontrollerar dessa interaktioner och dess inverkan på ytans egenskaper.

I denna avhandling identifieras strömtäthet, typ av ström, och partiklars storlek som primära variabler som kontrollerar metallkristallisering och beläggningens egenskaper.

Bland många parametrar, visades en specifik vågform på strömmen i omvänd pulsläge öka samdepositionen effektivt, ledande till en fördubbling av andelen nanopartiklar jämfört med andra tekniker. Ultraljud tillämpades som metod för omrörning av depositionsbadet för förbättrad stabilitet och fördelning. Effekten av ultraljud på samdepositionen av metallkristallisering studeras och jämfört med tyst tillstånd.

Dessutom har en ytbehandling för partiklarna visats framgångsrik för att få godtyckliga partiklar att bete sig likt Ni i depositionsbadet. Detta ledde till att samdepositionens takt ökade med en faktor av två till tre jämfört med obehandlade partiklar. Både ultraljud och ytbehandling av partiklarna ledde till minskad aggregation vilket förbättrade fördelningen av partiklar och metallstruktur och därigenom ökad hårdhet.

Arbetet bevisar synergieffekten mellan partiklar och metallstruktur vilket påverkar beläggningens slutliga egenskaper. Vid utveckling av nya ytbeläggningar ska därför inte bara mängden partiklar beaktas utan även dess interaktion med elektrokristalliseringsprocessen.

Place, publisher, year, edition, pages
Jönköping: Jönköping University, School of Engineering , 2019. , p. 45
Series
JTH Dissertation Series ; 039
Keywords [en]
Composite coatings; Nanoparticles; Electrocrystallisation; Microstructure; Surface treatment; Pulse plating; Ultrasound agitation
Keywords [sv]
Kompositbeläggningar; Nanopartiklar; Elektrokristallisering; Mikrostruktur; Ytbehandling; Pulsplätering; Ultraljudsomrörning
National Category
Mechanical Engineering
Identifiers
URN: urn:nbn:se:hj:diva-43548ISBN: 978-91-87289-41-5 (print)OAI: oai:DiVA.org:hj-43548DiVA, id: diva2:1307380
Supervisors
Available from: 2019-04-26 Created: 2019-04-26 Last updated: 2021-09-10Bibliographically approved
List of papers
1. Effects of SiC particles codeposition and ultrasound agitation on the electrocrystallisation of nickel-based composite coatings
Open this publication in new window or tab >>Effects of SiC particles codeposition and ultrasound agitation on the electrocrystallisation of nickel-based composite coatings
2021 (English)In: Journal of Materials Science, ISSN 0022-2461, E-ISSN 1573-4803, Vol. 56, p. 18463-18476Article in journal (Refereed) Published
Abstract [en]

This study analysed the influence of the codeposition of SiC particles with different sizes: 50 nm, 500 nm and 5 μm, and the type of bath agitation (stirring or ultrasonic) on the electrocrystallisation of nickel coatings. The composites matrix microstructure was analysed by means of SEM, EBSD and XRD, to evaluate the grain size, crystal orientation, and internal stresses and was benchmarked against pure nickel samples electrodeposited in equivalent conditions. The codeposition of nano- and microsize particles with an approximate content of 0.8 and 4 vol.%, respectively, caused only a minor grain refinement and did not vary the dominant < 100 > crystal orientation observed in pure Ni. The internal stress was, however, increased by particles codeposition, up to 104 MPa by nanoparticles and 57 MPa by microparticles, compared to the values observed in pure nickel (41 MPa). The higher codeposition rate (11 vol.%) obtained by the addition of submicron-size particles caused a change in the grain growth from columnar to equiaxial, resulting in deposits with a fully random crystal orientation and pronounced grain refinement. The internal stress was also increased by 800% compared to pure nickel. The ultrasound (US) agitation during the deposition caused grain refinement and a selective particle inclusion prompting a decrease in the content of the particles with the larger particles. The deposits produced under US agitation showed an increase in the internal stresses, with double values compared to stirring. The increase in the deposits microhardness, from 280 HV in pure Ni to 560 HV in Ni/SiC submicron-US, was linked to the microstructural changes and particles content.

Place, publisher, year, edition, pages
Springer, 2021
National Category
Metallurgy and Metallic Materials
Identifiers
urn:nbn:se:hj:diva-54594 (URN)10.1007/s10853-021-06483-z (DOI)000694607500002 ()2-s2.0-85114642705 (Scopus ID)HOA;;764677 (Local ID)HOA;;764677 (Archive number)HOA;;764677 (OAI)
Funder
Knowledge Foundation, 20310117
Note

Included in licentiate thesis in manuscript form with the title "Effects of particles codeposition and ultrasound agitation on the electrocrystallisation of Ni nanocomposites". Also included in doctoral thesis in manuscript form with the title "Effects of particles codeposition and ultrasound agitation on the electrocrystallization of metal matrix composites".

Available from: 2021-09-10 Created: 2021-09-10 Last updated: 2021-12-21Bibliographically approved
2. Electrocodeposition of Ni composites and surface treatment of SiC nano-particles
Open this publication in new window or tab >>Electrocodeposition of Ni composites and surface treatment of SiC nano-particles
2021 (English)In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 406, article id 126663Article in journal (Refereed) Published
Abstract [en]

This work has explored the surface modification of SiC submicron- and nanoparticles, and its influence on the particles' chemical behaviour and deposition rate in the electroplating of composite Ni/SiC coatings. SiC particles with different sizes (50, 60, 300 and 500 nm) were codeposited in their “as-produced” state. The ζ-potential measurements and alkaline titration for the “as-produced” particles showed differences in chemical behaviour for particles of different sizes, reporting pH buffering effect, even though the particles were inert and chemically the same (SiC). A surface treatment (ST) based on nitric acid was developed in an attempt to set a similar surface state, therefore a similar chemical behaviour in all particles. The ζ-potential measurements and alkaline titration of the “surface treated” particles showed similar results, independently of the size of particles. The pH buffering effect also decreased considerably by the ST. The codeposition rate was modified by the ST differently for each size compared to their as-produced state. The content of SiC50 and SiC500 was doubled (≈2% and ≈19%), tripled for SiC300 (≈7%) and more than halved for SiC60 (≈2%). The microhardness of these composite deposits was linked to the changes in the SiC codeposition.

Place, publisher, year, edition, pages
Elsevier, 2021
Keywords
Dispersion coating, Surface treatment, ζ-Potential, Grain refinement, Microhardness
National Category
Mechanical Engineering
Identifiers
urn:nbn:se:hj:diva-43545 (URN)10.1016/j.surfcoat.2020.126663 (DOI)000604750600023 ()2-s2.0-85098481602 (Scopus ID)HOA;intsam (Local ID)HOA;intsam (Archive number)HOA;intsam (OAI)
Funder
Knowledge Foundation, 20310117
Note

Included in thesis in manuscript form as: Pinate, S., Ispas, A., Leisner, P., Bund, A., Zanella, C. Electrocodeposition of Ni composites and surface modification of SiC nanoparticles.

Available from: 2019-04-26 Created: 2019-04-26 Last updated: 2021-04-28Bibliographically approved
3. Electrocodeposition of nano-SiC particles by pulse-reverse under an adapted waveform
Open this publication in new window or tab >>Electrocodeposition of nano-SiC particles by pulse-reverse under an adapted waveform
2019 (English)In: Journal of the Electrochemical Society, ISSN 0013-4651, E-ISSN 1945-7111, Vol. 166, no 15, p. D804-D809Article in journal (Refereed) Published
Abstract [en]

This work has explored the potential of using pulse reverse (PR) plating for increasing the deposited fraction of SiC nanoparticles. Two PR waveforms were selected, a short pulse (500 Hz) waveform and a newly modified and adapted pulsed sequence that equals the plating thickness to the particles’ diameter (50 nm) for the on-time and half-diameter during the anodic time. The pulse waveforms were designed with 4 and 10 A⋅dm−2 as the average current density and cathodic peak current density, respectively. Direct current (DC) deposits at the same values were also produced as reference. In all cases, the codeposition of nano-SiC particles influenced the microstructure. The electroplating under DC 10 A⋅dm−2 showed the strongest grain refinement and increased the content of the particles (up to 2% vol.) PR using high-frequency achieved a similar codeposition. The maximum particle incorporation was achieved by the proposed adapted pulse waveform, doubling the SiC content produced by other set-ups (up to 4% vol.); increasing the microhardness of the deposits to 400 HV, despite no grain refinement compared to the pure metal. From these results, it was observed a relationship between the influence of the plating method on the microstructure, the particle content, and the material's hardness.

Place, publisher, year, edition, pages
Electrochemical Society, 2019
Keywords
Electrodeposition, Composite coating, Electroplating, Pulse reverse current
National Category
Materials Engineering
Identifiers
urn:nbn:se:hj:diva-46770 (URN)10.1149/2.0441915jes (DOI)000494282300003 ()2-s2.0-85076115008 (Scopus ID)PP JTH 2019 (Local ID)PP JTH 2019 (Archive number)PP JTH 2019 (OAI)
Note

Included in licentiate thesis in manuscript form with the title: "Codeposition of nano-SiC particles by pulse-reverse electroplating".

Available from: 2019-11-04 Created: 2019-11-04 Last updated: 2021-04-28Bibliographically approved

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