Formation of optimal surface of dental implants by CST SLA Process

Transcription

1 Formation of optimal surface of dental implants by CST SLA Process Research Report of Finish Line Materials & Processes Ltd with SEM-EDS analysis at Technion Research and Development Foundation Ltd January 2011 Revised October 2013

2 page 2 from 14 TABLE OF CONTENT 1. Goal, trying procedure and FDA Guidance 2. Process Sequence 3. Washing after machining implants view 4. Washing after machining surface structure 5. Washing after machining surface chemistry 6. Blasting implants view 7. Blasting surface structure 8. Blasting surface chemistry 9. Acid Treatment implants view 10.Acid Treatment surface structure 11.Acid Treatment surface chemistry 12.Conclusion: CST SLA Acid Treatment Process is an appropriate process for formation of optimal surface of implants

3 page 3 from Goal, trying procedure and FDA Guidance The subject of this Research is Dental Implants as they are manufactured by appropriate machining procedures. The goal is to prove that a Finish Line Comprehensive Surface Treatment (CST) Process for Dental Implants, implemented for these implants, will ensure surface structure and surface chemical composition and its purity grade as acceptable in the dental implants practice. The tested CST Process was Dry umina Blasting Process followed by CDS Finish Line Acid Treatment Process for Dental Implants, justified by technological and quality control results and especially by results of samples analyses by SEM-EDS technique. In case the results would be insufficient, other Finish Line processes might be tested. The FDA Guidance, Class II Special Controls Guidance Document for dental implants, part Blasted Surfaces Information, as cited below, was of our special consideration: identity of any surface treatments that blast the implant composition of the particles identity of any treatments to remove particles from implant surfaces identity of agents used in particle removal chemical analysis of the surface to verify that any chemicals used to remove particles have been washed from the surface photomicrographs of blasted surfaces to show whether or not there are particles remaining behind on the surface

4 page 4 from Process Sequence The CST Process Sequence is detailed in the Finish Line document Formation of Dental Implants Surface by Finish Line Comprehensive Surface Treatment Process SLA Version (FL CST SLA Process) and consists of the following main stages of the implants treatment: Washing from machining oils and emulsions Blasting for previous formation of surface morphology After blasting washing Chemical Treatment (*) for cleaning the surface from particles remaining after blasting and for completing of the surface structure formation and surface beneficiation Neutralization and washing using Ultrasonic bathes to ensure clear implants surface Drying Quality control at all stages of the treatment (*)Following the Finish Line document Formation of Dental Implants Surface, the Chemical Treatment comprises Double Acid Treatment Process (by other terminologies Double Etching ), including possibility of the process tuning for specific requirements of Customers

5 page 5 from Washing after machining implants view SEM photomicrographs of implants surfaces at Magnification X25 Sample after machining, before washing: the surface is heavily covered by foreign particles from occasional sources. Sample after machining and washing at Finish Line is reasonably clean and mostly free from foreign particles, enabling good conditions for further stages of the treatment.

6 page 6 from Washing after machining surface structure SEM photomicrographs of machining and washed after machining surfaces at Magnification X2000 show smooth metallic surface which is a good base for further blasting and acid treatment. Sample after machining : particles of amorphous geometry are seen on the surface. Sample after machining and washing at Finish Line is mostly free from foreign particles.

7 page 7 from Washing after machining surface chemistry Results of the surface chemical SEM-EDS analysis of machining and washed after machining implants Ti Ca S Cl P.1 P.2 Ti P.1 P P.2 Ca V Si S V Si Sample after machining Sample after machining and washing at Finish Line. Implant after machining (sample ,P.1): analysis of any not contaminated points on the surface show the original alloy composition (Ti, and V at appropriate ratio). Contaminants on such implants (sample ,P.2) are of occasional sources. Implant after machining and washing at Finish Line (sample ,P.1): practically any point on the surface shows the original alloy composition. Very rare contaminants (sample ,P.2) are still occasional inclusions.

8 page 8from Blasting Treatment implants view SEM photomicrographs of blasted surfaces at Magnification X25 show that after the blasting as needed for porous surface formation, many foreign particles remain dispersed on the surface and cover it heavily.. Sample underwent umina Blasting Sample underwent umina Blasting

9 page 9 from Blasting surface structure SEM photomicrographs of blasted surfaces at Magnification X Sample underwent umina Blasting Sample underwent umina Blasting Foreign particles dispersed on the surface (arrowed 2 and 3), seen as black spots on the SEM picture, have sharp geometric contours, revealing their crystalline nature. The surface morphology of the implants at this stage of treatment is disordered and not definite, when compared to the commonly acceptable regular morphology. To clean the surface and to complete and beneficiate its morphology, the acid treatment is needed.

10 page 10 from Blasting surface chemistry Ti Ti O O V V P. 1 P. 2 P. 1 P. 2 O O P. 3 Surface chemical composition by EDS analysis at various points of interest for sample underwent umina Blasting P. 3 Surface chemical composition by EDS analysis at various points of interest for sample underwent umina Blasting Clean areas (P.1 of and SG-16) represent an original alloy (Ti, and V at appropriate ratio). Crystalline foreign particles are revealed as fractures of alumina ( and O at appropriate ratio (p.2 and p.3 of and ). There are no other contaminants on the surface, except inclusions of umina used for the blasting. This achievement of the cleaning process and of the clean environment during the implants processing allows good cleaning quality of the final implants.

11 page 11 from Acid Treatment implants view SEM photomicrographs at Magnification X25 Sample Sample Sample Sample Samples of implants underwent umina Blasting and acid treatment After blasting and acid treatment, the implants surface is absolutely clean, with no foreign particles remain on the surface.

12 page 12 from Acid Treatment surface structure SEM photomicrographs at Magnification X2000 Sample Sample Sample Sample Samples of implants underwent umina Blasting and acid treatment Clean surface, no particles remaining behind the treatment. The Acid Treatment Process has completed and beneficiated a topography of the area as it was developed by alumina blasting. The porous structure is very definite, with porous of roughly microns diameter, within the surface area of 100X100 microns, while the pores walls and bottom are cratered by small pores of 1-3 microns diameter. The obtained structure of the dental implant surface is as acceptable in common practice of dental implantation.

13 Page 13 from Acid Treatment surface chemistry Surface chemical composition by EDS analysis at various points of interest for samples underwent umina Blasting and acid treatment P. 1 Ti Ti Ti Ti V V V V Sample Sample Sample Sample Samples of implants underwent umina Blasting and acid treatment Chemical analysis of occasional points of interest presented on the diagrams above show the original Titanium alloy composition of the implants surface (Ti, and V at appropriate ratio), with no contamination. Analysis of any other points on the micro-photographs have revealed the same chemical composition.

14 page 14 from Conclusion: CST SLA Acid Treatment Process is an appropriate process for formation of optimal surface of dental implants As follows from the results of this Research, Finish Line Comprehensive Surface Treatment CST Process for Dental Implants, SLA Version, including Dry umina Blasting and Acid Treatment Process, is an appropriate process for surface formation of dental implants. The Process is guided by ASTM B and is detailed in our Document Formation of Dental Implants Surface by Finish Line Comprehensive Surface Treatment Process, SLA Version. As learned from the SEM-EDS results, the Process ensures a definite porous structure, with porous of roughly microns diameter, within the surface area of 100X100 microns, while the pores walls and bottom are cratered by small pores of 1-3 microns diameter. The obtained morphology of the dental implant surface is as acceptable in common practice of dental implantation. The Process clears the implant surface from alumina residuals and remains of washing liquids used during the washing after machining and blasting, up to the cleaning degree equal and even exceeding performances of dental implants available on the market. Following FDA Guidance demands, there are no particles remaining behind on the surface, and all the chemicals used to remove particles are washed from the surface.