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SIONDICA project review on 20.6.07 V. Shklover About coatings for ADC General remarks (useful for our project) Remi

SIONDICA project review on 20.6.07 V. Shklover About coatings for ADC General remarks (useful for our project) Reminiscence of ICMCTF2007 Papers on Si-O-N system Patent search results Conclusions. Requirements to ADC materials B. Andresen, 2005

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SIONDICA project review on 20.6.07 V. Shklover About coatings for ADC General remarks (useful for our project) Remi

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  1. SIONDICA project review on 20.6.07 • V. Shklover • About coatings for ADC • General remarks (useful for our project) • Reminiscence of ICMCTF2007 • Papers on Si-O-N system • Patent search results • Conclusions

  2. Requirements to ADC materials • B. Andresen, 2005 • Fracture toughness (repeated contraction and expansion, • leading to heat checking) • Die lifetime can be enhanced by ~ 50% by decreasing gradient between Tmax and Tmin • (role of TC!) • Gross cracking resistance • Soldering resistance. Al alloys casting by Fe of die material at • high-temperature. Intermetallics FeAlx have lower TC, Al melt • cools at lower rate and separates from the rest of casting. • Soldering occurs at hot spots on the die surface

  3. Tribology study of coatings for ADC • O. Salas et al. 2003 • Functions of ADC coating system: • Adhesion to substrate • Accommodation of stress • Good tribological properties • Corrosion resistance • Non-wettability with molten Al as central issue • Best coatings (out of 15 studied) are • TiAlN, TiN/TiCN/ CrN

  4. Coatings for ADC • A. Lakare et al. 1999 • Main failure modes in ADC: • Soldering (corrosion, formation of Fe-Al-Si intermetallics due • to reaction H13 steel + Al as a result of H13 dissolving in Al) • Washout (erosion wear by high-velocity of cast metal of • 30-100 m/sec, injective pressure 50-80 MPa) • Thermal fatigue (heat checks, due to alternative • temperature change, 670-710 oC) • CrN was best coating

  5. PVD coatings for ADC E. Bernacchi et al., 1996 TiAlN is more suitable for Al die casting then CrN and CrC (resistance to wear and Al soldering were checked)

  6. Soldering prevention by oxide surface treatment • M. Z. Jahedi et al. 2001 • Production of compact oxide layer by oxidation in • CO2/H2 gas mixture: • Steel H13, 550 oC compact Fe3O4 layer • Incoloy MA956 (4.5wt% Al), 1100 oC compact -Al2O3 layer • Prevention of formation of intermetallic Al/steel phases during • Al pressure die casting (soldering)

  7. Design of coating systems for ADC • S. Carrera et al. 2001 • No one individual coating provides combination of properties: • Be non-wetting with liquid Al • Wear resistant • Oxidation resistant at casting conditions • Accommodate residual thermal stresses during shot cycling Working layer (non-wetting, wear- and oxidation resistance) Multilayer or graded layer (FGM) to minimize stresses Adhesion layer (~50 nm) with H13

  8. Design of coating systems for ADC • S. Carrera et al. 2001 • Composition of “working layer” depends on Al alloy • - Candidates for “working layer” (poor wettability with Al): • CrC, CrN, TiAlN, MoZrN, TiBCN, NoAl, TiCN • - Coatings exhibit different wettability with different Al alloys • - No best candidate was identified, though all were less wetting • than H13

  9. Corrosion of H13 steel in molten Al alloys • R. Aharonov et al. 2001 • CrN provides good protection against molten Al • Smoother surface finish and thicker coatings result in • better corrosion resistance • Optimum coating thickness is 4-5 µm • Substrate (H13) corrodes due to • presence of pinholes and • other defects • Thermal stresses around • asperities also lead to corrosion • Coatings with higher compressive • stress fail faster then low-stress • coatings

  10. General: possible relation lattice parameters - hardness Sirdeshmukh et al. 2006 - Chemical bonding is important for determination of the crystal hardness, assuming definition of hardness as resistance to dislocations movement - For NaCl structures, lattice constant can be used as parameter, characterizing hardness: the weaker is the bond, the larger is bond length and the lower is hardness ln(Hvx100) Gilman-Chin parameter (Hv/C44) Hv, kg/mm2 ln(C44x100) a, Å

  11. Nanoindentation at elevated temperature • - Micro Materials (UK), test measurements in LOT-Oriel GmbH • - Standard NanoTest hot stage (heated indenter) to 500 oC • - Hot stage operates to 750 oC • - Two samples, measurements at RT, 500, 600, 700 and 750 oC • Samples: • - CrSiON #1771 (best CrSiON sample) on WCo substrate • - CrN on WCo substrate (reference) • Results expected: • - End of June/beginning July

  12. General: texture formation in CrSiON films Typical for CrN films (200)-texture changes to (111) at increase of Si content in Cr1-xSixN (Martinez et al. 2004) Switch of texture and phase transformation (Lee et al. 2005) Solubility limit of Si in CrN (~11at.%, Kim et al. 2006)

  13. Understanding texture formation in CrSiON films • F. H. Baumann et al. • Monte Carlo modeling of thin-film growth is planned • Al film • Competition • of (001) and • (111) growth • three • different • temperatures

  14. General: Lab of Crystallography of ETH is buying instrument for TC measurements until 2000 oC

  15. Ultrathin SiON films • K. Muraoka et al. 2003 • Growth by by SiH4/N2/O2 plasma-enhanced CVD process • at Si(111) substrate temperature of 500 oC • Compositions on the line SiO2…Si3N4 considered • N and O content studied by angle-resolved XPS • (N1s and O1s bands) • Compositions of (Si3N4)x(SiO2)1-x • films deposited at 500 oC and • annealed at 850 oC

  16. Thermodynamics of Si-O-N system M. L. Green et al. 2001 Thermodynamic (bulk) phase diagram for Si-O-N system • Why N atoms incorporate into SiO2? • N can be trapped kinetically • N can be thermodynamically stable at • the interfaces • (There are also other explanations) M. Hillert et al. 1992 Calculated SiO2 - Si3N4 phase diagram

  17. Nitridation of SiO2 • D. Fischer et al, 2004 • Hydrogen passivation as a way to stabilization of • SiON in SiOxNy-z(NH)z structure • MD simulation of effect of nitridation on SiO2 • Up to nitrogen content of ~25%, basic structure of oxide is • preserved • Beyond critical N content, structural transitions are expected • Upper limit of N content may be different for bulk and films

  18. Properties of superhard Si-O-N system • L. Torrison et al. 2003 • Si2N2O has superior oxidation resistance and thermal shock • resistance compared to Si3N4. But no suitable synthesis • technique at relative low temperatures for Si2N2O is available • - Si2N2O has structure of high-pressure B2O3 • Characterization: RBS (with simulation), SIMS, HRTEM, FTIR • Structure of non-stoichiometric SiNxOy: predominantly Si3N4 • network with some lattice sites occupied by O • - Tuning of composition by growth parameters

  19. ICMCTF 2007: contributions related to our project

  20. ICMCTF 2007 (A1-2-11) DSC/TGA study of oxidation of CrN and CrAlN coatings on sacrificial supports J. Lin et al. 2007 Reactive sputtering onto stainless steel and glass covered with formvar (deposition temperature 150-250 oC) • - Different phase transitions correlated with XRD • - DSC, TGA and Kissinger plots for Cr0.78Al0.22N • Reactions are more pronounced with increasing heating rates • Reactions are shifted to higher temperatures with Cr content

  21. Patent search Software: Derwent Innovation Index (ISI Web of Knowledge) Patent Downloader (US, Japan, PCT) Search for: “ZrSiON” “ZrAlON” “TiAlON” “AlCrON” “Aluminium die casting coatings” “Oxynitride” “Coatings AND “die” “Chromium” AND “Silicon” AND “Oxynitride” “Chromium” AND “Silicon” AND “Nitride”

  22. ZrSiON 1)Guardian, 2)Sumimoto, 3)Mitsubishi, 4)Toshiba,5)Nippon Tungsten, 6)NGK Insulators, 7)Asahi Glass. No evidences for Al die casting, diffusion barriers, TC

  23. ZrAlON 1)Mitsubishi, 2)Shinko Kobelko, 3)Isuzu Motors, 4)Minnesota Mining, 5)Toshiba, 6)Nippon Tungsten. No evidences for to Al die casting, diffusion barriers, one TC

  24. TiAlON 1)Mitsubishi, 2)Sumimoto, 3)Juergen Bach, 4)Shanghai Tool, 5)Shinko Kobelko. One really TiAlON, no evidences for Al die casting, diffusion barriers, TC

  25. AlCrON 1)Shinko Kobelko, No evidences for to Al die casting, diffusion barriers, one TC

  26. Coatings for Al die casting (1) 1)Colorado school mines, 2)Unaxis, 3)Authors, 4)Ionbond, 5)Brush Wellman, 6)Daido Tokushuko, 7)Ube Ind, 8)Matsumoto, 9)Nippon steel.

  27. Coatings for Al die casting (2) 1)Nippon Steel, 2)Aisin Seiki, 3)Volvo AB, 4)Hitachi Metals, 5)Toyota, 6)Swiss Aluminium, 7)Mallory & Co.

  28. Oxynitrides-1 1)Kigam, 2)Mitsubishi (many similar patents), 3)Toshiba, 4)Kennametal (many), 5)Winkhlover, 6)ELEMENT SIX (high R coordination number), 7)DIAMORPH CERAMIC, 8)Hitachi, 9)Sumimoto, 10)Unaxis, 11)KYOCERA No evidences for Al die casting, diffusion barriers, TC

  29. Oxynitrides-2 1)Shanghai Tool, 2)Sumimoto, 3)Uni Donghua, 4)Mitsubishi, 5)Seramtec, 6)Shinko Kobelko, 7)Shinko Kobelko+Mitsubishi. No evidences for Al die casting, diffusion barriers, TC

  30. “Coatings” AND “die”-1 1)Kobe Seiko Sho. 2)TDY Ind. 3)Unaxis. 4)Sumimoto Electric. 5)Toshiba Tung. 6)Syndia. 7)Sumimoto Metal. 8)Zaporo Ind. 9)Nippon Steel.

  31. “Coatings” AND “die”-2 1)GTE Lab Inc. 2)Aluminium Co. America. 3)Idemitsu Petrochem. 4)British Petr. 5)Swiss Aluminium. 6)Mallory & Co. 7)Surface technology. 8)Fulmer Res. Inst. 9)Seiko Instr.

  32. Different 1)Shinko Kobelko, 2)Unaxis.

  33. Chromium AND silicon AND oxynitride (48, 8 relevant) 1)Toshiba Tungaloy, 2)Subimoto Denko, 3)Sumimoto Electric, 4)Mitsubishi, 5)NGK SPARK PLUG Co., 6)Kuratomi. No ADC, TC, DB.

  34. “Chromium” AND “Silicon” AND “Nitride” (a lot) 1)Ion Kogaku Kenkyusho,

  35. Conclusions • Three-layer system can be beneficial: • (1) Working layer (non-wetting, wear- and oxidation resistance) • (2) Multilayer or graded layer to minimize stresses • (3) Adhesion layer with H13 • - Working layer composition • - Smoother surface finish and thicker coatings result in • better corrosion resistance. Importance of wettability studies • ZrSiON: no patents for ADC • CrSiON: no patents for ADC • AlCrON: no patents for ADC • ZrAlON: no patents for ADC • TiAlON: one patent for ADC, no patents for DB, TC

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