IP Library Granted Patent US 12,226,550
Granted Patent B2
US 12,226,550 · App. 18/086,506 · Granted Feb 18, 2025

Method of manufacturing a bioimplant

Inventors: Masaaki Mawatari (Saga, JP); Masatsugu Tsukamoto (Saga, JP); Iwao Noda (Osaka, JP)
Assignees: SAGA UNIVERSITY; KYOCERA CORPORATION
A61L27/54A61L27/32A61L2300/104A61L2300/404A61L2420/02
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Quick Facts
Patent No.
US 12,226,550
App. No.
18/086,506
Granted
Feb 18, 2025
Kind
B2
Abstract

Provided is a bioimplant which is capable to inhibit the biofilm formation over a long period of time after an operation. The bioimplant of the present invention comprises a base material of metal, ceramic, or plastic and a thermal spraying film of a calcium phosphate-based material formed at least partially thereon and the silver concentration in the thermal-spray film is 0.05 wt % to 3.00 wt %.

Claims (14)

1. A method of manufacturing a bioimplant, comprising: providing a base material of the bioimplant;

forming a coating comprising a calcium phosphate-based material and a silver material on at least a part of a surface of the base material;

after forming the coating, heating the coating at a predetermined temperature under a predetermined pressure to form oxyapatite in the coating; and

immersing the coating in purified water to convert oxyapatite present in the coating to hydroxyapatite, wherein the immersing results in fine crystals of the hydroxyapatite being formed on a surface of the coating, wherein a size of the fine crystals of hydroxyapatite is in a range of 0.01 μm to 2.00 μm in length, thickness or width, and

wherein a temperature of the purified water is in a range of 60 to 100 degrees Celsius.

2. The method according to claim 1 , wherein said calcium phosphate-based material is a compound or a mixture of two or more compounds selected from the group consisting of hydroxyapatite, alpha-tricalcium phosphate, beta-tricalcium phosphate, and tetracalcium phosphate.

3. The method according to claim 1 , wherein the base material comprises a metal.

4. The method according to claim 1 , wherein the base material comprises ceramic.

5. The method according to claim 1 , wherein the base material comprises a plastic.

6. The method according to claim 1 , wherein:

the heating is performed at a temperature range of 550 to 850 degrees Celsius for a period of time in the range of 1 to 5 hours; and

the immersing is performed for a period of time in the range of 10 to 60 μminutes.

7. The method according to claim 1 , wherein the resulting coating comprises a silver concentration in the range of 0.05 wt % to 3.00 wt %.

8. The method according to claim 1 , wherein the forming the coating is performed by applying a thermal sprayed film comprising a calcium phosphate-based material and a silver material.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 15, 2026
From: KYOCERA CORPORATION
To: KYOCERA MEDICAL CORPORATION
Reel/Frame 074671/0210 →
Priority Claims (1)
JP 2012-022205 · Feb 3, 2012 · national
Continuity (4)
Continuation 17080460 · Oct 26, 2020
Continuation 15405156 · Jan 12, 2017
Continuation In Part 14376183
Related Publication 20230121881A1 · Apr 20, 2023
References Cited (113)
US 5482731A · Vargas-Gutierrez · 1996 [cited by applicant]
US 5732469A · Hamamoto et al. · 1998 [cited by applicant]
US 6113993A · Gao et al. · 2000 [cited by applicant]
US 6207218B1 · Layrolle et al. · 2001 [cited by applicant]
US 6365028B1 · Shatrov · 2002 [cited by applicant]
US 6426114B1 · Troczynski · 2002 [cited by applicant]
US 6582715B1 · Barry et al. · 2003 [cited by applicant]
US 6994883B2 · Layrolle et al. · 2006 [cited by applicant]
US 8821911B2 · Gan et al. · 2014 [cited by applicant]
US 10004604B2 · Hotokebuchi · 2018 [cited by applicant]
US 10610614B2 · Hotokebuchi · 2020 [cited by applicant]
US 10814039B2 · Mawatari · 2020 [cited by examiner]
US 11278642B2 · Hotokebuchi · 2022 [cited by applicant]
US 20010024662A1 · Yang · 2001 [cited by applicant]
US 20010036530A1 · Noda et al. · 2001 [cited by applicant]
US 20050221259A1 · Anderson · 2005 [cited by applicant]
US 20060210494A1 · Rabiei et al. · 2006 [cited by applicant]
US 20090198344A1 · Prentice et al. · 2009 [cited by applicant]
US 20090215009A1 · Noishiki et al. · 2009 [cited by applicant]
US 20090280156A1 · Hotokebuchi et al. · 2009 [cited by applicant]
US 20100286790A1 · Gruner et al. · 2010 [cited by applicant]
US 20110008407A1 · Gan et al. · 2011 [cited by applicant]
US 20130138223A1 · Mawatari et al. · 2013 [cited by applicant]
US 20150018965A1 · Mawatari · 2015 [cited by applicant]
US 20170119932A1 · Mawatari et al. · 2017 [cited by applicant]
CA 2416201A1 · 2003 [cited by applicant]
CN 1454101A · 2003 [cited by applicant]
EP 0410711A1 · 1991 [cited by applicant]
EP 1231299B1 · 2012 [cited by applicant]
JP H04144555A · 1992 [cited by applicant]
JP 2001518827A · 2001 [cited by applicant]
JP 2004503333A · 2004 [cited by applicant]
JP 2005506879A · 2005 [cited by applicant]
JP 2005097052A · 2005 [cited by applicant]
JP 2005523380A · 2005 [cited by applicant]
JP 2005297435A · 2005 [cited by applicant]
JP 2006151729A · 2006 [cited by applicant]
JP 2008073098A · 2008 [cited by applicant]
JP 2011512959A · 2011 [cited by applicant]
JP 2014050610A · 2014 [cited by examiner]
KR 20060056093A · 2006 [cited by applicant]
WO 1998042390A1 · 1998 [cited by applicant]
WO 1999031303A1 · 1999 [cited by applicant]
WO 2001012883A1 · 2001 [cited by applicant]
WO 2002005862A1 · 2002 [cited by applicant]
WO 03035123A1 · 2003 [cited by applicant]
WO 2003055449A1 · 2003 [cited by applicant]
WO 2005027801A1 · 2005 [cited by applicant]
WO 2006033956A2 · 2006 [cited by applicant]
WO 2006104628A2 · 2006 [cited by applicant]
WO 2007022211A2 · 2007 [cited by applicant]
WO 2007089894A2 · 2007 [cited by applicant]
WO 2008029612A1 · 2008 [cited by applicant]
WO 2009053670A2 · 2009 [cited by applicant]
WO 2009111307A2 · 2009 [cited by applicant]
WO 2012023510A1 · 2012 [cited by applicant]
Ding et al. (Surface and Coatings Technology 2003;165:248-257) (Year: 2003). [cited by examiner]
English translation of JP2014050610A; 2014: 9 pages. (Year: 2014). [cited by examiner]
Sigma Phosphate Buffered Saline ([online] retrieved on Mar. 25, 2024 from https://www.sigmaaldrich.com/US/en/product/sigma/806552; 1 page). (Year: 2024). [cited by examiner]
Estridge and Reynolds. Basic Clinical Laboratory Techniques 2011; p. 111 (2 pages). (Year: 2011). [cited by applicant]
Lee, M.S., Reference Book for Composites Technology vol. 2 1989, CRC Press; p. 82 (Year: 1989). [cited by applicant]
Ong et al. Critical REviews in Biomedical Engineering 1999;28(5&6): 1-41 (Year: 1999). [cited by applicant]
Chai (Dr. Cameron Chai, Hydroxyapatite—Thermal Stability of Synthetic Hydroxyapatites, (Jun. 2002), [Retrieved from internet <URL: . https://www.azom.com/article.aspx?Article1D=1462 >], 3 pages) (Year: 2002). [cited by applicant]
Chai et al. Hydroxyapatite_13 Thermal Stability of Synthetic Hydroxyapatites (2002) (Source: International Ceramic Monographs, vol. 1, No. 1, pp. 79-85 (1994)) (Year: 2002). [cited by applicant]
Gross et al., Oxyapatite in hydroxyapatite coatings, Journal of Materials Science, (1998), 33: 3985-3991 (Year: 1998). [cited by applicant]
Extended European Search Report issued Aug. 6, 2015 in counterpart European Patent Application No. 13743971.7, 7 pages. [cited by applicant]
International Search Report issued Feb. 4, 2013, in counterpart Japanese Patent Application No. PCT/JP2013/050661, 2 pages (English translation). [cited by applicant]
International Preliminary Report on Patentability issued Aug. 5, 2014, in counterpart Japanese Patent Application No. PCT/JP2013/050661, 6 pages (English translation). [cited by applicant]
Noda, et al., “Development of Novel Thermal Sprayed Antibacterial Coating and Evaluation of Release Properties of Silver Ions”, Journal of Biomedical Materials Research, Part B: Applied Biomaterials, May 2009, 89(2):456… [cited by applicant]
Shimizaki et al., “In vivo antibacterial and silver-releasing properties of novel thermal sprayed silver-containing hydroxyapatite coating”, Journal of Biomedical Materials Research Part B: Applied Biomaterials, 2009, p… [cited by applicant]
Ando et al., “Development of antibacterial biomaterials”, Orthopaedic Surgery and Traumatology, Apr. 2010, 53(5):467-475 (Partial English Translation). [cited by applicant]
Miyamoto et al, “Development of novel antibacterial biomaterials”, Antibiotics & Chemotherapy, 2010, 26(9):125-129 (Partial English Translation). [cited by applicant]
Noda et al., “Silver-containing hydroxyapatite coating”, Journal of Japanese Society for Biomaterials, 2010, 29-4:266-270 (Partial English Translation). [cited by applicant]
Noda et al., “Development of Thermal Spraying Technique for Silver-Containing Hydroxyapatite (The 4th Report)”, The 40th Annual Meeting of the Japanese Society for Replacement Arthroplasty Program/Abstract, 2010, p. 350… [cited by applicant]
Noda et al., “Development of Thermal Spraying Technique for Silver-Containing Hydroxyapatite (The 5th Report)”, The 41st Annual Meeting of the Japanese Society for Replacement Arthroplasty Program/Abstract, 2011, p. 371… [cited by applicant]
Ando et al., “Development of Silver Antibacterial Biomaterials”, The 34th Annual Meeting of the Japanese Society for Study of Bone and Joint Infection Program/Abstract, 2011, p. 64 (Partial English Translation). [cited by applicant]
Non-Final Office Action issued in corresponding application U.S. Appl. No. 17/080,460 dated Apr. 19, 2022, in 23 pages. [cited by applicant]
Final Office Action issued in corresponding application U.S. Appl. No. 17/080,460 dated Jul. 27, 2022, in 8 pages. [cited by applicant]
Gross et al. (J Mater Sci. 1998;33:3985-3991 ). (Year: 1998). [cited by applicant]
Bai et Bai et al. (J Biomed Mater Res Part B. 2012; 100B:553-561) (Year: 2012). [cited by applicant]
Iwao Noda et al., “Ginkei Kokin Seitai Zaiiyo no Kaihatsu (1)—Gin Ha Yosha Gijutsu no Kaihatsu to Gin Ion Yoshutsu Tokusei”, Japanese Society for Study of Bone and Joint Infections Program Shorokushu, vol. 30, p. 43, 20… [cited by applicant]
Chinese Office Action for Application No. 200780033447.7 dated Jan. 11, 2012, English translation provided. [cited by applicant]
Faust et al., “Biofunctionalised Biocompatible Titania Coatings for Implants”, Key Emerging Materials, vols. 206-213, 2002, p. 1547-1550. [cited by applicant]
Giavaresi et al., “Histomorphometric, ultrastructural and microhardness eveluation of the osseointegration of nanostructured titanium oxide coating by metal-organic chemical vapour deposition: an in vivo study”, Biomate… [cited by applicant]
Japanese Office Action dated Apr. 17, 2012, for Application No. 2006-244479 with the English translation. [cited by applicant]
Japanese Office Action dated May 15, 2012, for Application No. 2006-252933 with the English translation. [cited by applicant]
Lee et al., “Hydroxyapatite-Ti02 Hybrid Coating on Ti Implants”, Journal of Biomaterials Applications, vol. 20, Jan. 2006, p. 195-208. [cited by applicant]
Lin et al., “Characterization of Electrolytic Ti02 Coating on Ti for Biomedical Applications”, Journal of the Electrochemical Society, vol. 151, No. 12, 2004, p. D127-D133. [cited by applicant]
Macionczyk et al., “Repassivationg tantalum/tantalum oxide surface modification on stainless steel implants”, Surface and Coatings Technology, vols. 142-144, 2001, p. 1084-1087. [cited by applicant]
Müller et al., “Surface engineering of Stainless steel materials by covalent collagen immobilization to improve implant biocompatibility”, Biomaterials, vol. 26, 2005, p. 6962-6972. [cited by applicant]
Yao et al., “Anodization: A Promising Nano-Modification Technique of Titanium Implants for Orthopedic Applications”, Journal of Nanoscience and Nanotechnology, vol. 6, 2006, 2682-2692. [cited by applicant]
Yen et al., “Characterization of electrolytic Zr02 coating on Co-Cr-Mo implant alloys of hip prosthesis”, Biomaterials, vol. 22, 2001, p. 125-133. [cited by applicant]
Ando et al. (In Vitro Antibacterial Properties of Thermal Sprayed Silver-Containing Hydroxyapatite Coating against Methicillin- Resistant [cited by applicant]
Documentation of meeting date for Ando reference, [Retrieved from internet <URL: http://www.ors.org/past-meetings/>], [Downloaded Sep. 30, 2016], 1 page. [cited by applicant]
Kofstad et al., Oxidation of titanium in the temperature range of 800-1200 ° C., Journal of the Less Common Metals, Apr. 1961, vol. 3, Issue 2, pp. 89-97, [Retrieved from internet <URL: http://www.sciencedirect.com/scie… [cited by applicant]
Kofstad et al., High-temperature oxidation of titanium, Journal of the Less Common Metals, Jun. 1967, vol. 12, Issue 6, pp. 449-464, [Retrieved from internet <URL: http://www.sciencedirect.com/science/article/pii/002250… [cited by applicant]
Murakami et al. (Evaluation of the structure of Ag in thermal sprayed Ag-containing hydroxyapatite coatings, Journal of the Chemical Society of Japan (2015), 123 (8): 667-671). [cited by applicant]
Chen et al. (In vitro anti-bacterial and biological properties of magnetron co-sputtered silver-containing hydroxyapatite coating, Biomaterials (on-line Jul. 26, 2006) 27:5512-5517) (6 pages). [cited by applicant]
Yang et al. (A review on calcium phosphate coatings produced using sputtering process—an alternative to plasma spraying, Biomaterials (2005) 26: 327-337 (cited by Chen, as ref. 39)) (11 pages). [cited by applicant]
Xue et al. (Effect of hydroxyapatite coating crystallinity on dissolution and osteointegration in vivo, Journal of Biomedical Materials Research Part A (Wiley Interscience, published online Jul. 15, 2005), vol. 74 A, Is… [cited by applicant]
Xue bibliographic information for verification of Journal information, [Retrieved from internet <URL: http://onlinelibrary.wiley.com/doi/10.1002/jbm.a.30323/abstract >], (printed Mar. 5, 2016), 3 pages. [cited by applicant]
Lee et al. (In vitro characterization of postheat-treated plasma-sprayed hydroxyapatite coatings, Surface Coatings & Technology (2005; available on-line Nov. 11, 2004) 197: 367-374), 8 pages. [cited by applicant]
JP 1994-069582 (machine translation obtained from file wrapper for U.S. Appl. No. 11/816,811, which was published as Noishiki et at., US 2009/0215009 A1) (cited on IOS filed Nov. 23, 2011), 4 pages. [cited by applicant]
Mukherjee et al. (Antimicrobial activity of aluminium oxide nanoparticles for potential clinical applications (Science against microbial pathogens: communicating current research and technological advances, A. Mendez-Vi… [cited by applicant]
Clyne et al. (2.1 Fundamental Studies of the PEO Process (pub. Univ. Cambridge, UK; Composites and Coatings Group, Dept. of Materials Science and Metallurgy) [From internet <URL: http://www.ccg.msm.cam.ac.uk/directory/ … [cited by applicant]
Clyne et al. [Downloaded Feb. 19, 2014], 3 pages. [cited by applicant]
Keronite PEO (Keronite, What is plasma electrolytic oxidation? [Retrieved from internet <URL: http://www.keronite.com/page- view.php?pagename=What-is-Plasma-Electrolytic-Oxidation? >] [Downloaded Feb. 19, 2014], 1 page). [cited by applicant]
Keronite Properties (Keronite, General Properties of Keronite Layers, [Retrieved from internet <URL: http://www.keronite.com/page-view.php?pagename=Plasma-Electrolytic-Oxidation-Material-Characteristics >] [Downloaded F… [cited by applicant]
Overgaard et al. (The influence of crystallinity of the hydroxyapatite coating on the fixation of implants: Mechanical and Histomorphometric Result, The Journal of Bone and Joint Surgery, (British Editorial Society of B… [cited by applicant]
Dumbleton et al. (Hydroxyapatite-Coated Prostheses in Total Hip and Knee Arthoplasty, Journal of Joint and Bone Surgery (British) (Nov. 2004) 86 (11): 2526-2540; available from ProQuest), 16 pages. [cited by applicant]
De Groot et al (Proc Instn Mech Engrs, vol. 212, 1998, pp. 137-147) (Year: 1998). [cited by applicant]
Johnson et al (The Journal of Infectious Diseases, 1990, vol. 162, pp. 1145-1150, abstract) (Year: 1990). [cited by applicant]
Uskokovic et al (Biointerphases, May 2019, vol. 14, pp. 1-20) (Year: 2019). [cited by applicant]