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Control of particles codeposition and strengthening mechanisms in nickel based nanocomposite coatings
Jönköping University, School of Engineering, JTH, Materials and Manufacturing.ORCID iD: 0000-0001-7228-1188
2021 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Surface durability is a key factor in the service life of components. Depending on the aggressiveness of the environment, surface deterioration by wear or corrosion leads to failure of the bulk material and eventually to the loss of functionality of the component. Therefore, designing surfaces to withstand service requirements is a critical aspect for industrial product realisation.

Electroplating is an attractive technique to mass-produce affordable protective coatings due to its low cost and high performance, easy maintenance of the process, and adjustable production times. Producing nanocomposite coatings by electroplating has received significant attention for decades due to their potential to provide excellent wear and corrosion protection.

Nanocomposites provide the possibility of combining different materials to achieve multifunctionality and, due to the nanometer size of the reinforcer phase, promote additional strengthening effects in the matrix not present in microcomposites. Additionally, the reduction in the size of the reinforcer provides advantages in wear protection as the risk of third-body abrasion is reduced. However, the industrial applicability remains limited due to the lack of control in their production process.

The present work focuses on the relationship between the input parameters and the codeposition of SiC, MoS2 and graphite particles, identifying critical factors and providing methods to control the process better. Furthermore, a correlation between the nickel matrix microstructure and codeposition is established, linking them to the strengthening effects and final performance of the nanocomposite coating.

New methods were developed to provide a reproducible electroplating process. A surface treatment for the reinforcing powder minimised the differences between the particles surface state deriving from different batches, supplier or production routes. Composites produced with surface-treated nanoparticles showed reproducible results displaying similar codeposition rate andhardness values. Additionally, a pulse-reverse plating waveform, adapted to the SiC particles average size, was designed and optimised to deposit a reproducible and improved particles content even in the presence of anionic surfactants, typically used to reduce coatings porosity and defects.

The study of the impact of the reinforcer phase on the electrocrystallisation of the nickel matrix showed that the microstructure was significantly affected by the size, chemistry and dispersion of the particles, promoting changes in the preferred crystal orientation, grains morphology and size. The strengthening mechanisms were linked to the microstructural changes resulting from the process parameters, particles codeposition and the agitation mode. Different models were used to predict the hardness of the composites based on the contribution and combination of each strengthening factor: Hall-Petch, Orowan, enhanced dislocation density and particles incorporation, showing a good agreement with the experimental data.

Furthermore, the wear behaviour of the composites was analysed and connected to the hardening effects. The analysis highlighted how particles content, dispersion, type and size of the reinforcer contribute to the protection against wear.

A novel multifunctional composite coating based on a dual dispersion mix of hard SiC particles and self-lubricant MoS2 particles was designed, resulting in a surface with high hardness, low friction and low wear.

Abstract [sv]

Ytors robusthet är en nyckelfaktor för komponenters livslängd. I krävande applikationsmiljöer kan ytan skadas av korrosion eller nötning som fortplantar sig till basmaterialet vilket kan leda till att komponenten förlorar sin funktionalitet. Det är därför viktigt att under produktutveckling konstruera komponentytor som motstår tilltänkta driftsmiljöer.

Elektroplätering är en attraktiv metod for kostnadseffektiv volymtillverkning av skyddande funktionella beläggningar då processen är flexibel och enkel att underhålla. Därför har också möjligheten att elektroplätera nano-kompositbeläggningar med utmärkta nötnings- och korrosionsegenskaper uppmärksammats de senaste decennierna.

Nano-kompositer öppnar för möjligheten att kombinera olika material för att uppnå multifunktionalitet. Nano-partiklarna bidrar med en härdningseffekt utöver vad som kan uppnås med mikro-partiklar. Ytterligare är risken för nötningsskadar på grund av lösrivna partiklar mindre för nano-kompositer. Dock är den industriella användningen begränsat av att tillverkningsprocessen är svår att kontrollera.

Denna avhandling fokuserar på förhållandet mellan ingångsparametrar och inkorporering av SiC-, MoS2- och grafitpartiklar genom att identifiera kritiska faktorer och tillhandahåller metoder för bättre processkontroll. Dessutom har ett samband mellan nickelmatrisens mikrostruktur och inkorporerade partiklar identifierats som förklarar härdningseffekten och kompositbeläggningens egenskaper.

Nya metoder för att skapa en reproducerbar pläteringsprocess har utvecklats. En förberedande ytbehandling av partiklarna minskar skillnader i ytkemiska egenskaper härstammande från olika leveranser, producenter och tillverkningsmetoder. Kompositbeläggningar tillverkade med ytbehandlade partiklar var reproducerbara med avsikt på partikelhalt och hårdhet. Ytterligare designades en bipolär strömpuls anpassad efter SiC-partiklarnasgenomsnittliga storlek så att en reproducerbar ökad partikelmängd kan inkorporeras. Detta gäller även i närvaro av anjoniska ytaktiva medel, som vanligtvis används för att minska beläggningens porositet och defekter.

Studien av partiklarnas påverkan på elektrokristallisationen av nickelmatrisen visade att partiklarnas storlek, sammansättning och spridning hade en avsevärd effekt på mikrostrukturen. Partiklarna påverkade den föredragna kristallorienteringen samt kornens form och storlek. Härdningsegenskaperna kopplades till förändringar i mikrostrukturen beroende på processparametrar, partikelinkorporering och omrörningsläget. Olika modeller användes för att förutsäga kompositernas hårdhet baserat på bidrag från följande härdningsfaktor: Hall-Petch, Orowan, ökad dislokationstäthet och partikelinkorporering, vilka visade god överensstämmelse med experimentella data.

Slutligen undersöktes kompositbeläggningarnas nötningsegenskaper och kopplades till partikelhärdning. Särskild vikt lades på hur partikelhalten, -spridningen, -typen och -storleken bidrar till skyddet mot slitage.

En ny multifunktionell komposit baserad på en dubbel dispersionsblandning av hårda SiC-partiklar och självsmörjande MoS2-partiklar utvecklades och resulterade i en yta med hög hårdhet, låg friktion och lågt slitage.

Place, publisher, year, edition, pages
Jönköping: Jönköping University, School of Engineering , 2021. , p. 110
Series
JTH Dissertation Series ; 063
Keywords [en]
Dispersion coatings; nanocomposite; Controlled particles codeposition; Surface treatment; ζ-potentials; Pulse-reverse deposition; Ultrasound agitation; Electrocrystallisation; Microstructure; Strengthening mechanisms; Hardness; Wear
Keywords [sv]
Dispersionsbeläggning; nanokomposit; kontrollerad inkorporering av partiklar; ytbehandling; zeta-potential; bipolär pulsplätering; ultraljudsomrörning; elektrokristallisation; mikrostruktur; härdningsmekanism; hårdhet; nötning
National Category
Metallurgy and Metallic Materials
Identifiers
URN: urn:nbn:se:hj:diva-52335ISBN: 978-91-87289-67-5 (print)OAI: oai:DiVA.org:hj-52335DiVA, id: diva2:1548036
Public defence
2021-05-31, Gjuterisalen (E1405), School of Engineering, Jönköping, 13:30 (Swedish)
Opponent
Supervisors
Funder
Knowledge Foundation, 20310117Available from: 2021-04-28 Created: 2021-04-28 Last updated: 2021-09-10Bibliographically approved
List of papers
1. 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
2. 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
3. Role of anodic time in pulse-reverse electrocodeposition of nano-SiC particles
Open this publication in new window or tab >>Role of anodic time in pulse-reverse electrocodeposition of nano-SiC particles
2021 (English)In: Journal of the Electrochemical Society, ISSN 0013-4651, E-ISSN 1945-7111, Vol. 168, no 6, article id 062509Article in journal (Refereed) Published
Abstract [en]

This work focuses on the significance of the particle's residence time in composite electrodeposition. Ni-SiC were produced using different pulse-reverse (PR) waveforms based on the average particle diameter (60 nm). The waveform was designed to deposit a metal thickness equivalent to the average diameter during the cathodic pulse and strip half during the anodic pulse. The shape of the waveform was modified to study its effect on particle codeposition by changing the cathodic and anodic pulse current density peaks and cycle time while maintaining the same charge. For benchmark, samples were also produced under direct current (DC), matching the cathodic pulse current density peaks and average. The electrodeposition was done in an additive-free and SDS-Watts bath. ζ-potential measurements were employed to determine the interaction between particles and electrolyte. A relation was established between particle incorporation rate and residence time at the electrode interface, examining. The microhardness of the deposits was also studied. The SiC content was more than doubled by PR compared to DC, from 2 vol.% to 5.5 vol.% even after SDS addition. The increase in codeposition rate was related to the anodic pulse time, supported by the existing models on the mechanisms of particle codeposition.

Place, publisher, year, edition, pages
Institute of Physics (IOP), 2021
Keywords
Pulse reverse current, Nanocomposite coatings, Surfactant, ζ-potential, Residence time
National Category
Metallurgy and Metallic Materials
Identifiers
urn:nbn:se:hj:diva-52331 (URN)10.1149/1945-7111/ac0a27 (DOI)000663498300001 ()2-s2.0-85109073165 (Scopus ID)PPembargo0;intsam;1548023 (Local ID)PPembargo0;intsam;1548023 (Archive number)PPembargo0;intsam;1548023 (OAI)
Funder
Knowledge Foundation, 20310117
Note

Included in thesis in manuscript form.

Available from: 2021-04-28 Created: 2021-04-28 Last updated: 2021-07-15Bibliographically approved
4. 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
5. Wear behavior of Ni-based composite coatings with dual nano-SiC: Graphite powder mix
Open this publication in new window or tab >>Wear behavior of Ni-based composite coatings with dual nano-SiC: Graphite powder mix
2020 (English)In: Coatings, ISSN 2079-6412, Vol. 10, no 11, article id 1060Article in journal (Refereed) Published
Abstract [en]

This work explores the surface protection against wear provided by electroplated metal matrix composite coatings containing hard and lubricant particles. The second phase mix was selected to provide wear resistance by hardening the material and decreasing the friction coefficient. In this study, the capacity of providing wear protection by nano-SiC and self-lubrication by submicron graphite was addressed. Nickel-based composites with a dual powder mix of SiC 60 nm and graphite 400 nm, combined on a 10:10 g L&minus;1 ratio, were produced by electrocodeposition. In addition, to better understand their synergy, mono-composites with SiC 60 nm or Graphite 400 nm with a powder load of 10 g L&minus;1 were also produced. Pure nickel was also electrodeposited under the same conditions as a benchmark. Electron backscatter diffraction (EBSD) maps and chemical composition analysis were used to correlate the results from microhardness, wear resistance, and friction to the microstructure and particle incorporation rate. The wear rate tested by pin-on-disc decreased when the codeposition fraction and microhardness increased. Three main factors were determined to contribute to the coating hardness: Intrinsic hardness of the particle type, strengthening by grain refinement, and dispersion strengthening. The composites containing SiC provided the best wear protection due to the highest microhardness and grain refinement.

Place, publisher, year, edition, pages
MDPI, 2020
Keywords
electroplating, dual dispersion mix, wear, lubrication
National Category
Metallurgy and Metallic Materials
Identifiers
urn:nbn:se:hj:diva-51041 (URN)10.3390/coatings10111060 (DOI)000593597900001 ()2-s2.0-85095994601 (Scopus ID)GOA JTH 2020 (Local ID)GOA JTH 2020 (Archive number)GOA JTH 2020 (OAI)
Funder
Knowledge Foundation, 20100280
Available from: 2020-11-25 Created: 2020-11-25 Last updated: 2021-04-28Bibliographically approved
6. Wear resistance and self-lubrication of electrodeposited Ni-SiC:MoS2 mixed particles composite coatings
Open this publication in new window or tab >>Wear resistance and self-lubrication of electrodeposited Ni-SiC:MoS2 mixed particles composite coatings
2021 (English)In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 421, article id 127400Article in journal (Refereed) Published
Abstract [en]

Ni-based mixed particles composite coatings were designed to achieve superior wear resistance by combining hard carbides and solid lubricants as a reinforcing particles mix. Pure nickel and single-particles composites were electrodeposited in the same conditions for benchmarking. A pre-study was carried out to optimise the current density to avoid loss of process efficiency due to hydrogen evolution. The production process was also improved by employing ultrasounds to avoid porosity and dendritic growth in the metal caused by conductive MoS2 particles. The presence of MoS2 particles led to nanocrystallinity in the nickel matrix, confirmed by electron backscatter diffraction (EBSD) maps and transmission electron microscopy (TEM). The microstructural changes and codeposition in the different composites were correlated to microhardness and pin-on-disc tests. An extremely high hardness was observed in the mixed particles composite (≈1110 HV) due to the combined effect of the nanocrystalline matrix and high codeposition rate (≈15 vol% SiC and ≈8 vol% MoS2). The codeposition of MoS2 particles provided a self-lubrication capability to the coating, reducing the friction coefficient compared to pure Ni from 0.15 to 0.07. The wear rate was reduced more than 12 times by the mixed reinforcement compared to pure Ni and more than 6 times compared to Ni-SiC.

Place, publisher, year, edition, pages
Elsevier, 2021
Keywords
Electroplating; Mixed dispersion coating; Nanocrystalline nickel; Microhardness; Wear; Self-lubrication
National Category
Metallurgy and Metallic Materials
Identifiers
urn:nbn:se:hj:diva-52333 (URN)10.1016/j.surfcoat.2021.127400 (DOI)000666583900036 ()2-s2.0-85109159405 (Scopus ID)HOA;;1548025 (Local ID)HOA;;1548025 (Archive number)HOA;;1548025 (OAI)
Funder
Knowledge Foundation, 20310117
Note

Included in doctoral thesis in manuscript form with the title: Wear resistance and self-lubrication of electrodeposited Ni-SiC:MoS2 dual composite coatings.

Available from: 2021-04-28 Created: 2021-04-28 Last updated: 2021-07-16Bibliographically approved
7. Strengthening mechanisms and wear behavior of electrodeposited Ni–SiC nanocomposite coatings
Open this publication in new window or tab >>Strengthening mechanisms and wear behavior of electrodeposited Ni–SiC nanocomposite coatings
2022 (English)In: Journal of Materials Science, ISSN 0022-2461, E-ISSN 1573-4803, Vol. 57, no 35, p. 16632-16648Article in journal (Refereed) Published
Abstract [en]

The present paper describes the study of the synergism between the matrix microstructure and reinforcement phase in electrodeposited nanocomposite coatings. Adding hard nanoparticles into the metallic matrix leads to hardening of the coating. The effects of particle load, size and dispersion on hardening as well as their influence on metal microstructure refinement were studied. The relative contributions of strengthening factors in Ni/nano-SiC composites, namely, Hall–Petch strengthening, Orowan strengthening, enhanced dislocation density and particles incorporation, were evaluated. The production of various coatings under different stirring conditions and powders resulted in dissimilarities in the incorporation of particles. The Hall–Petch relationship for pure nickel was determined using samples produced under different current densities. Additionally, the grain refinement resulting from the particle codeposition and agitation mode were identified as influential factors in grain-size strengthening. Dislocation density strengthening was significant in electrodeposits produced using ultrasonic agitation, while it was negligible in layers produced under other conditions. Particles codeposition affected the magnitude of Orowan strengthening, resulting in cases where strengthening was negligible despite the presence of particles. The sum of contributions and the modified Clyne methods were used to calculate the hardness of the composites based on the contribution of each strengthening factor, and the calculation results were in good agreement with experimental data. The wear behavior of the composites was analyzed by pin-on-disk measurements, and the results correlated with the strengthening mechanisms. Particle size, dispersion and content increased the strengthening effects as well as the hardness and wear resistance of the coatings.

Place, publisher, year, edition, pages
Elsevier, 2022
National Category
Metallurgy and Metallic Materials
Identifiers
urn:nbn:se:hj:diva-52334 (URN)10.1007/s10853-022-07655-1 (DOI)000852259400003 ()2-s2.0-85137600367 (Scopus ID)HOA;;1548027 (Local ID)HOA;;1548027 (Archive number)HOA;;1548027 (OAI)
Funder
Knowledge Foundation, 20310117
Note

Included in doctoral thesis in manuscript form with the title "Strengthening mechanisms by particles codeposition and wear behaviour of electroplated Ni-SiC coatings".

Available from: 2021-04-28 Created: 2021-04-28 Last updated: 2022-09-22Bibliographically approved

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