Skip to main content

Advertisement

SpringerLink
Log in

Characterization of Microplasma Sprayed Hydroxyapatite Coating

  • Peer Reviewed
  • Published:
Journal of Thermal Spray Technology Aims and scope Submit manuscript

Abstract

Microplasma sprayed (MIPS) HAP coatings on SS316L substrates were characterized by x-ray diffraction, Fourier transformed infrared spectroscopy, optical microscopy, scanning electron microscopy (SEM), field emission scanning electron microscopy (FE-SEM), atomic force microscopy and image analysis. The coating showed a high degree of crystallinity ~92%, a high porosity level of 20 vol.% and a moderate bonding strength of about 13 MPa. The displacement controlled three-point bend tests and associated results of optical microscopy indicated that crack deflection, crack branching, and also local crack bridging occurred during crack propagation in the coating. The nano-hardness (H) and Young’s modulus (E) of the MIPS-HAP coatings as measured by nanoindentation technique were about 6 and 92 GPa, respectively. The fracture toughness (K ic) of the coating was ~0.6 MPa·m0.5. From the nano-scratch experiments, the critical normal load at which localized microcracking led to delamination was measured to be ~400 mN.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9
Fig. 10
Fig. 11

Similar content being viewed by others

References

  1. K.A. Gross and C.C. Berndt, Biomedical Application of Apatites, Rev. Mineral. Geochem., 2002, 48(1), p 631-672

    Article  CAS  Google Scholar 

  2. W. Tong, J. Chen, X. Li, Y. Cao, Z. Yang, J. Feng, and X. Zhang, Effect of Particle Size on Molten States of Starting Powder and Degradation of the Relevant Plasma-Sprayed Hydroxyapatite Coating, Biomaterials, 1996, 17(15), p 1507-1513

    Article  CAS  PubMed  Google Scholar 

  3. L.L. Hench, Bioceramics, J. Am. Ceram. Soc., 1998, 81(7), p 1705-1733

    Article  CAS  Google Scholar 

  4. C.E. Mancini, C.C. Berndt, L. Sun, and A. Kucuk, Porosity Determinations in Thermally Sprayed Hydroxylapatite Coatings, J. Mater. Sci., 2001, 36(16), p 3891-3896

    Article  CAS  Google Scholar 

  5. R.S. Lima, K.A. Khor, H. Li, P. Cheang, and B.R. Marple, HVOF Spraying of Nanostructured Hydroxyapatite for Biomedical Applications, Mater. Sci. Eng. A, 2005, 396(1-2), p 181-187

    Article  CAS  Google Scholar 

  6. L. Zhao, K. Bobzin, F. Ernst, J. Zwick, and E. Lugscheider, Study on the Influence of Plasma Spray Processes and Spray Parameters on the Structure and Crystallinity of Hydroxylapatite Coatings, Materialwiss. Werkstoff., 2006, 37(6), p 516-520

    Article  CAS  Google Scholar 

  7. T.M. Sridhar, T.K. Arumugam, S. Rajeswari, and M. Subbaiyan, Electrochemical Behaviour of Hydroxyapatite-Coated Stainless Steel Implants, J. Mater. Sci. Lett., 1997, 16(23), p 1964-1966

    Article  CAS  Google Scholar 

  8. S. Kannan, A. Balamurugan, and S. Rajeswari, Development of Calcium Phosphate Coating on Type 316L SS In Vitro Response, Trend. Biomater. Artif. Org., 2002, 16(1), p 8-11

    Google Scholar 

  9. T.M. Sridhar, U.K. Mudali, and M. Subbaiyan, Sintering Atmosphere and Temperature Effects on Hydroxyapatite Coated Type 316L Stainless Steel, Corros. Sci., 2003, 45(10), p 2337-2359

    Article  CAS  Google Scholar 

  10. T.M. Sridhar, U.K. Mudali, and M. Subbaiyan, Preparation and Characterisation of Electrophoretically Deposited Hydroxyapatite Coatings on Type 316L Stainless Steel, Corros. Sci., 2003, 45(2), p 237-252

    Article  Google Scholar 

  11. A. Balamurugan, S. Kannan, and S. Rajeswari, Bioactive Sol-Gel Hydroxyapatite Surface for Biomedical Applications—In Vitro Study, Trend. Biomater. Artif. Org., 2002, 16(1), p 18-20

    Google Scholar 

  12. G. Ye and T. Troczynski, Hydroxyapatite Coatings by Pulsed Ultrasonic Spray Pyrolysis, Ceram. Int., 2008, 34(3), p 511-516

    Article  CAS  Google Scholar 

  13. A. Dey, A.K. Mukhopadhyay, S. Gangadharan, M.K. Sinha, and D. Basu, Development of Hydroxyapatite Coating by Microplasma Spraying, Mater. Manuf. Process., 2009 (in press)

  14. A. Dey, A.K. Mukhopadhyay, S. Gangadharan, M.K. Sinha and D. Basu, Anisotropy of Elastic Modulus on Bioactive HAP Coating, 20th Annual General Meeting, Feb 10-12, 2009 (Kolkata, India), Materials Research Society of India (MRSI), 2009, p 110

  15. A. Dey, A.K. Mukhopadhyay, S. Gangadharan, M.K. Sinha, D. Basu, and N.R. Bandyopadhyay, Nanoindentation Study of Microplasma Sprayed Hydroxyapatite Coating, Ceram. Int., 2009, 35(6), p 2295-2304

    Article  CAS  Google Scholar 

  16. A. Dey, A.K. Mukhopadhyay, S. Gangadharan, M.K. Sinha, and D. Basu, Mechanical Properties of Microplasma Sprayed HAP Coating, Interquadrennial Conference of International Congress on Fracture, B.K. Raghu Prasad and R. Narasimhan, Ed., Aug 3-7, 2008 (Bangalore, India), I. K. International Publishing House Pvt. Ltd., 2008, p 311-313

  17. E. Landi, A. Tampieri, G. Celotti, and S. Sprio, Densification Behaviour and Mechanisms of Synthetic Hydroxyapatites, J. Eur. Ceram. Soc., 2000, 20(14-15), p 2377-2387

    Article  CAS  Google Scholar 

  18. ASTM C 633-79. Standard Test Method for Adhesion or Cohesive Strength of Fame-Sprayed Coatings

  19. Y.C. Yang and E. Chang, Influence of Residual Stress on Bonding Strength and Fracture of Plasma-Sprayed Hydroxyapatite Coatings on Ti-6Al-4V Substrate, Biomaterials, 2001, 22(13), p 1827-1836

    Article  CAS  PubMed  Google Scholar 

  20. W.C. Oliver and G.M. Pharr, An Improved Technique for Determining Hardness and Elastic Modulus Using Load and Displacement Sensing Indentation Experiments, J. Mater. Res., 1992, 7(6), p 1564-1583

    Article  CAS  ADS  Google Scholar 

  21. A.G. Evans, B.R. Lawn, and D.B. Marshall, Elastic/Plastic Indentation Damage in Ceramics: The Median/Radial Crack System, J. Am. Ceram. Soc., 1980, 63(9-10), p 574-581

    Article  Google Scholar 

  22. D.R. Dukino and M.V. Swain, Comparative Measurement of Fracture Toughness with Berkovich and Vickers Indenters, J. Am. Ceram. Soc., 1992, 75(12), p 3299-3304

    Article  CAS  Google Scholar 

  23. J. Chen and S.J. Bull, Assessment of the Toughness of Thin Coatings Using Nanoindentation Under Displacement Control, Thin Solid Films, 2006, 494(1-2), p 1-7

    Article  CAS  ADS  Google Scholar 

  24. L.L. Hench and J. Wilson, An Introduction to Bioceramics: Advance Series in Ceramics, Vol 1, World Scientific Publishing Co. Pte. Ltd, Singapore, 1993, p 229-231

    Google Scholar 

  25. J.G. Morales, J.T. Burgues, T. Boix, J. Fraile, and R.R. Clemente, Precipitation of Stoichiometric Hydroxyapatite by a Continuous Method, Cryst. Res. Technol., 2001, 36(1), p 15-26

    Article  Google Scholar 

  26. L. Sun, C.C. Berndt, and C.P. Grey, Phase Structural Investigations of Plasma Sprayed Hydroxyapatite Coating, Mater. Sci. Eng. A, 2003, 360(1-2), p 70-84

    Article  CAS  Google Scholar 

  27. S.J. Ding, T.H. Hung, and C.T. Kao, Immersion Behavior of Plasma Sprayed Modified Hydroxyapatite Coatings After Heat Treatment, Surf. Coat. Technol., 2003, 165(3), p 248-257

    Article  CAS  Google Scholar 

  28. M.P. Mahabole, R.C. Aiyer, C.V. Ramakrishna, B. Sreedhar, and R.S. Khairnar, Synthesis, Characterization and Gas Sensing Property of Hydroxyapatite Ceramic, Bull. Mater. Sci., 2005, 28(6), p 535-545

    Article  CAS  Google Scholar 

  29. S. Nath, K. Biswas, and B. Basu, Phase Stability and Microstructure Development in Hydroxyapatite-Mullite System, Scr. Mater., 2008, 58(12), p 1054-1057

    Article  CAS  Google Scholar 

  30. P. Fauchais, J.F. Coudert, A. Verdelle, M. Verdelle, A. Grimaud, and P. Roumilhac, State of the Art for the Understanding of the Physical Phenomenon Involved in Plasma Spraying at Atmospheric Pressure, Thermal Spray: Advances in Coatings Technology, D.L. Houk, Ed., Sept 14-17, 1987 (Orlando, FL), ASM International, 1987, p 11-18

  31. C.Y. Yang, R.M. Lin, B.C. Wang, T.M. Lee, E. Chang, Y.S. Hang, and P.Q. Chen, In Vitro and In Vivo Mechanical Evaluations of Plasma-Sprayed Hydroxyapatite Coatings on Titanium Implants: The Effect of Coating Characteristics, J. Biomed. Mater. Res., 1997, 37(3), p 335-345

    Article  MATH  CAS  PubMed  Google Scholar 

  32. Y.C. Yang and E. Chang, The Bonding of Plasma-Sprayed Hydroxyapatite Coatings to Titanium: Effect of Processing, Porosity and Residual Stress, Thin Solid Films, 2003, 444(1-2), p 260-275

    Article  CAS  ADS  Google Scholar 

  33. Y.W. Gu, K.A. Khor, and P. Cheang, In Vitro Studies of Plasma-Sprayed Hydroxyapatite/Ti-6Al-4V Composite Coatings in Simulated Body Fluid SBF, Biomaterials, 2003, 24(9), p 1603-1611

    Article  CAS  PubMed  Google Scholar 

  34. Y.C. Yang, Influence of Residual Stress on Bonding Strength of the Plasma-Sprayed Hydroxyapatite Coating After the Vacuum Heat Treatment, Surf. Coat. Technol., 2007, 201(16-17), p 7187-7193

    Article  CAS  Google Scholar 

  35. R.G.T. Geesink, K. De Groot, and P.A.K.T. Christel, Chemical Implant Fixation Using Hydroxyapatite Coatings, Clin. Orthop. Relat. Res., 1987, 225, p 147-170

    CAS  PubMed  Google Scholar 

  36. B.C. Wang, E. Chang, C.Y. Yang, D. Tu, and C.H. Tasi, Characteristics and Osteoconductivity of Three Different Plasma-Sprayed Hydroxyapatite Coatings, Surf. Coat. Technol., 1993, 58(2), p 107-117

    Article  CAS  Google Scholar 

  37. E. Munting, M. Verhelpen, F. Li, and A. Vincent, CRC Handbook of Bioactive Ceramics, T. Yamamuro, L.L. Hench, and J. Wilson, Ed., CRC Press, FL, 1990, p 143-148

  38. K. de Groot, C.P.A.T. Klein, J.G.C. Wolke, and J.M.A. de Blieck-Hogervorst, CRC Handbook of Bioactive Ceramics, T. Yamamuro, L.L. Hench, and J. Wilson, Ed., CRC Press, FL, 1990, p 133-142

  39. H. Ji and P.M. Marquis, Effect of Heat Treatment on the Microstructure of Plasma-Sprayed Hydroxyapatite Coating, Biomaterials, 1993, 14(1), p 64-68

    Article  CAS  PubMed  Google Scholar 

  40. M.J. Filiaggi, N.A. Coombs, and R.M. Pilliar, Characterization of the Interface in the Plasma-Sprayed HA Coating/Ti-6Al-4V Implant System, J. Biomed. Mater. Res., 1991, 25(10), p 1211-1229

    Article  CAS  PubMed  Google Scholar 

  41. W.H. Duckworth, Discussion of Ryshkewitch Paper, J. Am. Ceram. Soc., 1953, 36(2), p 68

    Article  Google Scholar 

  42. G. Jiang and D. Shi, Coating of Hydroxyapatite on Highly Porous Al2O3 Substrate for Bone Substitutes, J. Biomed. Mater. Res. (Appl. Biomat.), 1998, 43(1), p 77-81

    Article  CAS  MathSciNet  Google Scholar 

  43. Y.C. Yang, E. Chang, B.H. Hwang, and S.Y. Lee, Biaxial Residual Stress States of Plasma-Sprayed Hydroxyapatite Coatings on Titanium Alloy Substrate, Biomaterials, 2000, 21(13), p 1327-1337

    Article  CAS  PubMed  Google Scholar 

  44. H.C. Gledhill, I.G. Turner, and C. Doyle, Direct Morphological Comparison of Vacuum Plasma Sprayed and Detonation Gun Sprayed Hydroxyapatite Coatings for Orthopaedic Applications, Biomaterials, 1999, 20(4), p 315-322

    Article  CAS  PubMed  Google Scholar 

  45. D. Gauthier, J.M. Bouler, E. Aguado, P. Pilet, and G. Daculsi, Macroporous Biphasic Calcium Phosphate Ceramics: Influence of Macropore Diameter and Macroporosity Percentage on Bone Ingrowth, Biomaterials, 1998, 19(1-3), p 133-139

    Article  CAS  PubMed  Google Scholar 

  46. L. Pawlowski, The Science and Engineering of Thermal Spray Coatings, Wiley, Chichester, 1995, p 414

    Google Scholar 

  47. R.B. Heimann, Thermal Spraying of Biomaterials, Surf. Coat. Technol., 2006, 201(5), p 2012-2019

    Article  CAS  Google Scholar 

  48. C. Kumar, S.K. Nandi, A. Dey, P. Mukherjee, B. Kundu, S. Roy, and D. Basu, Evaluation of Plasma Spray Coated Hydroxyapatite and Bi-Phasic Calcium Phosphate Coated Pin Intra-Medullarly for Repair of Bone Defects in Rabbit Model, First International Conference on “NANOBIO” Tissue Engineering and Stem Cell Research Using Nanomaterials, organized by the Amrita Centre for Nano Sciences and Amrita Institute of Medical Sciences, p 60 in Book of Abstracts, Kochi, India, 17-19 Feb, 2009

  49. S. Paolom, L. Matteo, and B. Luca, Residual Stresses in Plasma Sprayed Partially Stabilised Zirconia TBCs: Influence of the Deposition Temperature, Thin Solid Films, 1996, 278(1-2), p 96-103

    Article  Google Scholar 

  50. S. Takeuchi, M. Ito, and K. Takeda, Modelling of Residual Stress in Plasma-Sprayed Coatings: Effect of Substrate Temperature, Surf. Coat. Technol, 1990, 43-44(Part 1), p 426-435

    Article  Google Scholar 

  51. H. Li, L.Z. Sun, J.B. Li, and Z.G. Wang, X-Ray Stress Measurement and FEM Analysis of Residual Stress Distribution Near Interface in Bonded Ceramic/Metal Compounds, Scr. Mater., 1996, 34(9), p 1503-1508

    Article  CAS  Google Scholar 

  52. J.D. Lee, H.Y. Ra, K.T. Hong, and S.K. Hur, Analysis of Deposition Phenomena and Residual Stress in Plasma Spray Coatings, Surf. Coat. Technol., 1992, 56(1), p 27-37

    Article  CAS  Google Scholar 

  53. C. Ergun, R.H. Doremus, and W.A. Lanford, Interface Reaction/Diffusion in Hydroxylapatite-Coated SS316L and CoCrMo Alloys, Acta Mater., 2004, 52(16), p 4767-4772

    Article  CAS  Google Scholar 

  54. U. Senturk, R.S. Lima, C.R.C. Lima, and C.C. Berndt, Deformation of Plasma Sprayed Thermal Barrier Coatings, J. Eng. Gas Turb. Power, 2000, 122(3), p 387-392

    Article  CAS  Google Scholar 

  55. B.D. Ratner, A.S. Hoffman, F.J. Schoen, and J.E. Lemons, Biomaterials Science: An Introduction to Materials in Medicine, 2nd ed., Elsevier Academic Press, USA, 2004, p 143

    Google Scholar 

  56. A.R.J. Franco, G. Pintaúde, A. Sinatora, C.E. Pinedo, and A.P. Tschiptschin, The Use of a Vickers Indenter in Depth Sensing Indentation for Measuring Elastic Modulus and Vickers Hardness, Mater. Res., 2004, 7(3), p 483-491

    Google Scholar 

  57. J. Wen, Y. Leng, J. Chen, and C. Zhang, Chemical gradient in plasma-sprayed HA coatings, Biomaterials, 2000, 21(13), p 1339-1343

    Article  CAS  PubMed  Google Scholar 

  58. C. Zhang, Y. Leng, and J. Chen, Elastic and Plastic Behavior of Plasma-Sprayed Hydroxyapatite Coatings on a Ti–6Al–4V Substrate, Biomaterials, 2001, 22(11), p 1357-1363

    Article  CAS  PubMed  Google Scholar 

  59. K.A. Khor, H. Li, and P. Cheang, Characterization of the Bone-Like Apatite Precipitated on High Velocity Oxy-Fuel HVOF Sprayed Calcium Phosphate Deposits, Biomaterials, 2003, 24(5), p 769-775

    Article  CAS  PubMed  Google Scholar 

  60. G.J. Cheng, D. Pirzada, M. Cai, P. Mohanty, and A. Bandyopadhyay, Bioceramic Coating of Hydroxyapatite on Titanium Substrate with Nd-YAG Laser, Mater. Sci. Eng. C, 2005, 25(4), p 541-547

    Article  CAS  Google Scholar 

  61. T.G. Nieh, A.F. Jankowski, and J. Koike, Processing and Characterization of Hydroxyapatite Coatings on Titanium Produced by Magnetron Sputtering, J. Mater. Res., 2001, 16(11), p 3238-3245

    Article  CAS  ADS  Google Scholar 

  62. T.G. Nieh, B.W. Choi, and A.F. Jankowski, Synthesis and Characterization of Porous Hydroxyapatite and Hydroxyapatite Coatings, A report submitted to Minerals, Metals, and Materials Society Annual Meeting and Exhibition, New Orleans, LA, Feb 11-15, 2001

  63. R.W. Rice, Porosity Effects on Machining Direction-Strength Anisotropy and Failure Mechanisms, J. Am. Ceram. Soc., 1994, 77(8), p 2232-2236

    Article  CAS  Google Scholar 

  64. H. Li, K.A. Khor, and P. Cheang, Young’s Modulus and Fracture Toughness Determination of High Velocity Oxy-Fuel-Sprayed Bioceramic Coatings, Surf. Coat. Technol., 2002, 155(1), p 21-32

    Article  CAS  Google Scholar 

  65. H. Li, K.A. Khor, and P. Cheang, Titanium Dioxide Reinforced Hydroxyapatite Coatings Deposited by High Velocity Oxy-Fuel HVOF Spray, Biomaterials, 2002, 23(1), p 85-91

    Article  CAS  PubMed  Google Scholar 

  66. L. Fu, K.A. Khor, and J.P. Lim, Yttria Stabilized Zirconia Reinforced Hydroxyapatite Coatings, Surf. Coat. Technol., 2000, 127(1), p 66-75

    Article  CAS  Google Scholar 

  67. L. Fu, K.A. Khor, and J.P. Lim, Processing, Microstructure and Mechanical Properties of Yttria Stabilized Zirconia Reinforced Hydroxyapatite Coatings, Mater. Sci. Eng. A, 2001, 316(1-2), p 46-51

    Article  Google Scholar 

  68. M. Wang, X.Y. Yang, K.A. Khor, and Y. Wang, Preparation and Characterization of Bioactive Monolayer and Functionally Graded Coatings, J. Mater. Sci.: Mater. Med., 1999, 10(5), p 269-273

    Article  Google Scholar 

  69. K. Balani, R. Anderson, T. Laha, M. Andara, J. Tercero, E. Crumpler, and A. Agarwal, Plasma-Sprayed Carbon Nanotube Reinforced Hydroxyapatite Coatings and Their Interaction with Human Osteoblasts In Vitro, Biomaterials, 2007, 28(4), p 618-624

    Article  CAS  PubMed  Google Scholar 

  70. K. Cheng, S. Zhang, W. Weng, K.A. Khor, S. Miao, and Y. Wang, The Adhesion Strength and Residual Stress of Colloidal-Sol Gel Derived β-Tricalcium-Phosphate/Fluoridated-Hydroxyapatite Biphasic Coatings, Thin Solid Films, 2008, 516(10), p 3251-3255

    Article  CAS  ADS  Google Scholar 

Download references

Acknowledgments

The authors are grateful to Director, Central Glass and Ceramic Research Institute (CGCRI), Kolkata, for his kind permission to publish this paper and to Dr. D. K. Bhattacharya, Head, Analytical Facility Division of CGCRI, for his kind encouragement during the course of this work. One of the authors (A.D.) also sincerely acknowledges the support and encouragements received from Prof. N. R. Bandyopadhyay of the School of Materials Science and Engineering, Bengal Engineering and Science University (BESU), Shibpur. In addition, the authors appreciate the infrastructural support received from all colleagues and particularly those received from the colleagues of the Mechanical Test Section and Bio Ceramics and Coating Division at CGCRI. Finally, the authors gratefully acknowledge financial support received from DST-SERC (Project No: GAP 0216) and CSIR (Network Project TAREMAC No: NWP 0027).

Author information

Authors and Affiliations

  1. Bio-Ceramics and Coating Division, Central Glass and Ceramic Research Institute, Kolkata, 700 032, India

    Arjun Dey, S. Gangadharan, Mithilesh K. Sinha & Debabrata Basu

  2. Mechanical Test Section, Analytical Facility Division, Central Glass and Ceramic Research Institute, Kolkata, 700 032, India

    Arjun Dey & Anoop K. Mukhopadhyay

Authors
  1. Arjun Dey
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Anoop K. Mukhopadhyay
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. S. Gangadharan
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Mithilesh K. Sinha
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Debabrata Basu
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Anoop K. Mukhopadhyay.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Dey, A., Mukhopadhyay, A.K., Gangadharan, S. et al. Characterization of Microplasma Sprayed Hydroxyapatite Coating. J Therm Spray Tech 18, 578–592 (2009). https://doi.org/10.1007/s11666-009-9386-2

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s11666-009-9386-2

Keywords

Search

Navigation