MEDICAL DEVICES VI: Proceedings from the Materials and Processes for Medical Devices Conference August 8-10, 2011 Minneapolis, MN, USA

196 Pages·2013·16.254 MB·English

Medical Device Materials VI

Proceedings from the
Materials and Processes for Medical Devices
Conference

August 8–10, 2011
Hilton Minneapolis
Minneapolis, Minnesota, USA

Sponsored by

ASM International®
Materials Park, OH 44073-0002
www.asminternational.org
Copyright  2013
by
ASM International®
All rights reserved

No part of this book may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means,
electronic, mechanical, photocopying, recording, or otherwise, without the written permission of the copyright
owner.

First printing, February 2013

Great care is taken in the compilation and production of this book, but it should be made clear that NO
WARRANTIES, EXPRESS OR IMPLIED, INCLUDING, WITHOUT LIMITATION, WARRANTIES OF
MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE, ARE GIVEN IN CONNECTION WITH
THIS PUBLICATION. Although this information is believed to be accurate by ASM, ASM cannot guarantee that
favorable results will be obtained from the use of this publication alone. This publication is intended for use by
persons having technical skill, at their sole discretion and risk. Since the conditions of product or material use are
outside of ASM's control, ASM assumes no liability or obligation in connection with any use of this information. No
claim of any kind, whether as to products or information in this publication, and whether or not based on negligence,
shall be greater in amount than the purchase price of this product or publication in respect of which damages are
claimed. THE REMEDY HEREBY PROVIDED SHALL BE THE EXCLUSIVE AND SOLE REMEDY OF
BUYER, AND IN NO EVENT SHALL EITHER PARTY BE LIABLE FOR SPECIAL, INDIRECT OR
CONSEQUENTIAL DAMAGES WHETHER OR NOT CAUSED BY OR RESULTING FROM THE
NEGLIGENCE OF SUCH PARTY. As with any material, evaluation of the material under end-use conditions prior
to specification is essential. Therefore, specific testing under actual conditions is recommended.

Nothing contained in this book shall be construed as a grant of any right of manufacture, sale, use, or reproduction,
in connection with any method, process, apparatus, product, composition, or system, whether or not covered by
letters patent, copyright, or trademark, and nothing contained in this book shall be construed as a defense against any
alleged infringement of letters patent, copyright, or trademark, or as a defense against liability for such infringement.

Comments, criticisms, and suggestions are invited, and should be forwarded to ASM International.

ISBN-13: 978-1-62708-009-5
ISBN-10: 1-62708-009-0
SAN: 204-7586

ASM International®
Materials Park, OH 44073-0002
www.asminternational.org

Printed in the United States of America
MPMD 2011 Organizing Committee

Your 2011 organizers are dedicated to building the most comprehensive and current
programming available. If you can only attend one medical device conference, make it MPMD –
it’ll be worth it.

MPMD 2011 Co-chairs

Dr. Brad James, P.E.
Exponent Failure Analysis Associates

Brad James is a Principal Engineer with Exponent Failure Analysis Associates, specializing in
failure analysis, metallurgy, fracture, fatigue, corrosion and material degradation issues. Dr.
James has conducted hundreds of medical device failure analysis investigations for both
industrial and legal clients. He also helps medical device companies with general materials
and/or metallurgical issues, as well as premarket validation for fatigue, fracture and corrosion
performance.

Dr. James is also an adjunct professor at the Santa Clara University School of Engineering where
he teaches graduate-level fracture mechanics and failure analysis courses.

Dr. Dana J. Medlin, P.E., FASM
South Dakota School of Mines and Technology

Dana Medlin is the NUCOR Professor of Metallurgy in the Materials and Metallurgical
Engineering Department at the South Dakota School of Mines and Technology. Dr. Medlin’s
areas of expertise include physical and mechanical metallurgy, materials selection and design,
failure analysis, corrosion engineering, and metallic biomaterials. He is also the proprietor of
MES Incorporated, a forensic engineering consulting company. His previous professional
experience includes research and development positions at the Colorado School of Mines, LTV
Steel, The Timken Company, and Zimmer, Inc., where he was Global Metallurgy Leader. Dr.
Medlin is a consultant for a variety of clients and firms, primarily in the area of failure analysis,
engineering design, and maintenance metallurgy.
iii
Contents

Poster Session

Plasma Sterilization of Ultrasound Contrast Agents ............................................................ 1
L. Albala, Drexel University, Philadelphia, PA, USA

Inducing the Bone Growth on Different Titanium Alloys ...................................................... 4
J. Mirza Rosca1, D. Herrera Santana1, D. Gonzalez Martin2
(1) Las Palmas de Gran Canaria University, Canary Islands, Spain
(2) Technological Institute of Canarias, Canary Islands, Spain

A Novel Polymeric Composite for Orthopaedic Applications .............................................. 7
A.O. Tiamiyu1, S.A. Ibitoye2, I. A. Inyang2
(1) University of Cape Town, South Africa
(2) Obafemi Awolowo University, Nigeria

Passive Layer on Some Titanium Alloys ............................................................................. 11
J. Mirza Rosca, D. Herrera Santana, A. Santana Lopez
Las Palmas de Gran Canaria University, Canary Islands, Spain

Fracture Mechanics and Micro Crack Detection in Bone —
A Short Communication ........................................................................................................ 15
A.M. Al-Mukhtar1, C. Konke2
(1) Technische Universitat Bergakademie Freiberg, Germany
(2) Bauhaus-Universitat Weimar, Germany

ADSC Cells with Different Medium in Polycaprolactone/Hydroxyapatite
Whiskers Scaffolds an Initial Study ..................................................................................... 20
G.B.C. Cardoso, S.L.F. Ramos, C.A.C. Zavaglia,
P. B. Rego, S.T.O. Saad, A.C.F. Arruda,
State University of Campinas, Brazil

A Microstructural Overview of Oxide Ceramics for Medical Implants .............................. 24
A. Nield, J. Haftel, S. Hughes
C5 Medical Werks, LLC, Grand Junction, CO, USA

Mechanical Performances of Biomedical Beta-type Titanium
Alloy Through Heat Treatment and Severe Plastic Deformation ....................................... 27
T. Akahori1, M. Niinomi2, M. Nakai2, H. Yilmazer2, H. Fukui3, Y. Todaka4
(1) Meijo University, Japan
(2) Tohoku University, Japan
(3) Aichi-Gakuin University, Japan
(4) Toyohashi University of Technology, Japan

iv
Fabrication Processes for Medical Devices — I

Electropolishing and Throughmask ElectroEtching of Nitinol
Stents and Other Materials in an Aqueous Electrolyte ....................................................... 31
M. Inman1, E.J. Taylor1, A. Lozano-Morales2, L. Zardiackas3
(1) Faraday Technology, Clayton, OH, USA
(2) Eltron Research, Boulder, CO, USA
(3) University of Mississippi Medical Center, Jackson, MS, USA

Effect of Thermo-Set Process on MP35N Cable .................................................................. 37
B. Li, H. Zhang, L. Wang, Medtronic Corporation, Minneapolis, MN, USA

Evaluation of Metal Injection Molded 17-4 PH Stainless Steel for Instruments ................ 41
A. Craft, D. Campbell, B. Aboud,
DePuy Orthopaedics, Inc., Warsaw, IN, USA

Materials Modeling

Designing with Materials — Applying Materials Data and Rational
Materials Selection Methodologies in Medical Device Design ........................................... 47
S. Egan, S. Warde, Granta Design, Cambridge, UK

Effect of Strain Rate on Nitinol Constitutive
Modeling in the Clinically Relevant Strain Range ............................................................... 52
P. Briant, R. Siskey, A. Rau, S. Easley, B. James
Exponent Inc., Menlo Park, CA, USA

Fatigue Life and Durability of Medical Devices — I

Why are Implantable Cardioverter-Defibrillators and
Pacemakers being Revised Today? ..................................................................................... 57
J.A. Hanzlik1,2, J.D. Patel1,2, S.M. Kurtz1,2, Q.C. Horn2,
Y.P. Shkolnikov2, J.A. Ochoa2, B.B. Pavri3, A.J. Greenspon3,
(1) Drexel University, Philadelphia, PA, USA
(2) Exponent Inc., Seattle, WA, USA
(3) Thomas Jefferson University Hospital, Philadelphia, PA, USA

Comparative Failure Analysis of Retrieved UHMWPE Tibial Components ....................... 63
N. Camacho, S.W. Stafford, L. Trueba Jr.
University of Texas, El Paso, TX, USA

Advanced Materials and Emerging Technologies — I

Qualification of Hot Isostatic Pressing Processes ............................................................. 69
K. Rivard, A. Craft, T. Smith, B. Aboud
DePuy Orthopaedics, Inc., Warsaw, IN, USA

v
Bioactive Improving the Bioresponse to Polymers Using
Zirconium and Tantalum Hybridization ................................................................................ 74
J. Jarrell1, J. Walters2, N. Thomas2, M. Young2, P. Tran3, N. Tran3, R. Hayda3, C. Born3

(1) BioIntraface, Inc., East Providence, RI, USA
(2) Brown University, Providence, RI, USA
(3) Orthopaedic Trauma Research, Providence, RI, USA

Fatigue Life and Durability of Medical Devices — II

Ultrasonic Detection of Defects in Multilayered Ceramic
Capacitors for Active Implantable Medical Devices ........................................................... 80
S.A. Kim1, W.L. Johnson1, G.S. White1, R. Roberts2
(1) National Institute of Standards and Technology, Boulder, CO, USA
(2) Vishay Corp., Columbus, NE, USA

Medical Device Feedthrough Fatigue Characterization ...................................................... 86
J. Popp, J. Taylor, J. Hendrickson, Meditronic Inc., Minneapolis, MN, USA

Prediction of Hip Prosthesis Fatigue Properties — Influence of the Process .................. 92
M. Puget1, C. Doudard1, S. Calloch1 F. Boucher2
(1) Laboratoire Brestois de Mecanique et des Systemes, France
(2) Stryker Benoist Girard, France

Fabrication Processes for Medical Devices — III

The Functionality of Ti-15Mo in Creating 3-D Porous Surfaces via
Laser Powder Deposition for the Use in Dental Prosthetics .............................................. 98
J. Fuerst1, K. Kennedy1, M. Carter1, J. Sears1, D.J. Medlin2
(1) South Dakota School of Mines and Technology, Rapid City, SD, USA
(2) Engineering Systems Incorporated, Omaha, NE, USA

Corrosion

In-vitro Degradation and Cytocompatibility Assessment of
Mg-Zn and Mg-Zn-Ca Alloys ................................................................................................ 104
P. Gill, N. Munroe, R. Dua, S. Ramaswamy,
Florida International University, Miami, FL, USA

Potentiodynamic and Potentiostatic Characterization of CVD Alumina
Coating for Orthopaedic Implant Wear Reduction ............................................................ 108
R. Overholser, E. Gulley, B. Smith
DePuy Orthopaedics Inc., Warsaw, IN, USA

Fabrication Processes for Medical Devices — IV

Improved Resolution and Mechanical Properties of
Porous Coatings and Cellular Structures in Ti6Al4V
Manufactured with Electron Beam Melting ........................................................................ 113
S. Fager Franzén, M. Svensson, U. Ackelid, I. Elfström
Arcam AB, Sweden

vi
Influence of Interstitials on Material Properties of TI6AL4V
Fabricated with Electron Beam Melting (ebm®) ................................................................ 119
M. Svensson, Arcam AB, Sweden

Next Generation of Bio Materials

Surface Integrity of Biodegradable Orthopedic Magnesium-Calcium
Alloy Processed by High Speed Machining ....................................................................... 125
M. Salahshoor, Y.B. Guo,
The University of Alabama, Tuscaloosa, AL, USA

Materials Research & Development — I

Phase Transformation Study on MP35N Wire for Lead Conductor ................................. 131
B.Q. Li, D. Sorensen, T. Steigauf,
Medtronic, Minneapolis, MN, USA

Factors Causing Compressive Damage-Induced Cracking in Nitinol ............................ 139
A. Chinubhai, A. Kueck, P. Saffari, K. Senthilnathan, L. Vien, A.R. Pelton,
Nitinol Devices & Components, Fremont, CA, USA

Surface Engineering of Medical Devices

Bioactive Hybrid Material Surface Treatments for Infection
Resistant Implants without Drugs ...................................................................................... 143
J. Jarrell1, N. Thomas2, M. Young2, C. Baker2,
J. Morgan2, P. Tran3, N. Tran3, R. Hayda3, C. Born3
(1) BioIntraface, Inc., East Providence, RI, USA
(2) Brown University, Providence, RI, USA
(3) Orthopaedic Trauma Research, Providence, RI, USA

Evaluation of Diffusion Hardened Oxidized Zr-2.5wt%Nb for
Hard-on-Hard Articulation in Total Hip Arthroplasty ........................................................ 149
V. Pawar, C. Weaver, A. Parikh, S. Jani,
Smith and Nephew Inc., Memphis, TN, USA

Adsortion of Fibronectin into Titanium Implant Surface .................................................. 153
P.A. Gravina1, C.N. Elias1, F.C. Silva2,
(1) Instituto Militar de Engenharia, Brazil
(2) Instituto de Biofísica, Brazil

LASER Powder Deposition of Titanium – Tantalum
Alloy Structured Interfaces for Use in Orthopedic Devices ............................................. 159
J. Fuerst1, M. Carter1, M. Huber1, J. Sears1 D.J. Medlin2, G.F. Vander Voort3
(1) South Dakota School of Mines and Technology, Rapid City, SD, USA
(2) Engineering Systems Incorporated, Omaha, NE, USA
(3) Vander Voort Consulting, Wadsworth, IL, USA

vii
Materials Research & Development — II

Young’s Modulus Change due to Deformation-Induced Phase
Transformation in Beta-type Titanium Alloys for Biomedical Applications ................... 165
M. Nakai, M. Niinomi, X.L. Zhao, X.F. Zhao
Tohoku University, Sendia, Japan

Improved Properties of Light Alloys (Ti-, Ti-Alloys) Using
Near-Nano and Nano-Based Materials for Biomedical Applications ............................... 169
C. Melnyk1, B. Weinstein1, D. Grant1, R. Gansert2
(1) California Nanotechnologies Inc., Cerritos, CA, USA
(2) Advanced Materials & Technology Services, Inc., Simi Valley, CA, USA

Characterization of Microstructure and Dynamic
Mechanical Properties of Biomedical Nitinol Alloy ........................................................... 175
J.E. McKinney, J.Z. Snyder, Y.B. Guo
The University of Alabama, Tuscaloosa, AL, USA

Materials Research & Development — III

Design and Optimization of a Permeation Testing
System for Polymer Coatings ............................................................................................. 181
A. Verwolf, National Institute of Standards and Technology, Boulder, CO, USA

Author Index ......................................................................................................................... 187

viii
Medical Device Materials VI
Proceedings from the Materials and Processes for Copyright © 2013 ASM International®
Medical Devices Conference All rights reserved
August 8–10, 2011, Minneapolis, Minnesota, USA www.asminternational.org
Plasma Sterilization of Ultrasound Contrast Agents

L. Albala
Drexel University, Philadelphia, PA, USA

Abstract Ultrasound-targeted microbubble destruction is a non-invasive
method of administering drugs. UCA are less than 6 µm in
The presence of contrast agents in ultrasound imaging has diameter and show enhanced permeation and retention effects
made a substantial impact on account of the physical in vascular circulation. Non-ionic surfactant-based
similarities between tissues and fluids in the human body. microbubbles can be ‘loaded’ in a variety of different ways
Perfluorocarbon gas-filled microbubbles have been shown to with drugs (electrostatic binding, encapsulation within the
possess great viability as both ultrasound contrast agents hydrophobic core, etc.), allowing for simultaneous imaging
(UCA) and as therapeutic targeted drug-delivery vehicles. and drug delivery aimed at targeted drug release. Ultrasound
PFC gas has extremely low solubility (in blood), the bubbles sonication causes a contraction and expansion of the bubbles
are safe in concordance with the human body and are small (corresponding to the sound waves’ harmonic oscillation),
enough (less than 6µm) to pass through the smallest vessels, which, at clinical ultrasound frequencies, can cause the bubble
and most importantly, their acoustical impedance greatly to implode, thereby releasing its contents.
enhances contrast.
Ultrasound can be applied to a specific area of the body (e.g. a
An important consideration of anything injected and tumor/mass) where the bubbles in circulation need to release
circulating in the human body is its sterility, especially to their contents. The force of the microbubbles’ destruction is
avoid risk of infection (and satisfy FDA requirements). Short also known to cause transient pore opening, which allows for
of production in a “clean” facility, microbubbles are far from enhanced drug uptake. Microbubbles of different types are
sterile. This focus of this experiment is to employ gas plasma being applied clinically already for enhanced ultrasound
to sterilize bubbles freeze-dried for storage. The goal is to imaging, and the importance of future applications is clear, in
identify the ideal plasma setting to sterilize the sample. terms of delivering medication in high concentration to the
target, sparing toxicity to the rest of the body.
Sterility was difficult to achieve with this UCA, but poly lactic
acid bubbles can be sterilized with similar setup [2], perhaps The sterility of contrast agents is of utmost importance. The
due to non-sterile pre-plasma injection of PFC gas. More possible complications and confusion that can arise with
studies need to be done to understand sterilization possibilities bacteriological infections or reactions are unacceptable. The
with surfactant bubbles. goal is to sterilize two important types of surfactant-based
microbubbles—both are made with a combination of Span 60
Introduction and a either Polysorbate/Tween 80 or Vitamin E. The
microbubble solution is flash-frozen in liquid nitrogen and
The microbubbles are generated in a solution by sonication,
vacuum-dried to achieve the final product, a powder. This is
and stabilized by a layer of nonionic surfactant molecules. The
the medium that is sterilized because packaging, storing, and
combination of surfactants has a certain hydrophile-lipophile
sterilization applications of microbubbles show that
balance to reduce head-group repulsion. These bubbles are
conservation in a solid powder state after freeze-drying is
highly echogenic and small enough to pass through the
likely favorable.
pulmonary capillary bed.
Plasma gas is the chosen method of sterilization because of the
low probability that it will react with the bubbles and of its
low-thermal nature. Plasma is a partially ionized gas mainly
composed of ions, electrons, and radicals. In turn, radicals
disrupt the metabolism of microorganisms, thus making this
permeating gas medium ideal in annihilating bacteria. This
experiment explored the different power setting and durations
of plasma setting of a bench-top plasma cleaner for the

optimal sterilization setting.
Figure 1: Proposed molecular arrangement of the surfactants
by Wheatley et. Al. [5].
1
Microbubble stability and echogenicity in an ultrasound bath could mean that there are either fewer microbubbles or that
and sterility tests are done to ensure that incubation in RPMI they survive the ultrasound less:
growth media does not cause contamination.
Results have shown possibility for sterilization in addition to
maintenance of echogenicity, though future work with plasma-
treated liquids seems to be a feasible solution in the
manufacturing process of the microbubbles
Primary Goals
 Maximize retention of enhancement with appropriate SE61
and ST68 bubble size after sterilization of freezedried bubble
solutions.
 Maintain sterile conditions in RPMI growth media up to 48

hours after incubation with plasma-sterilized bubbles.
 Avoid compromising echogenicity and stability of the bubbles Figure 2: Acoustic response; the response of different
amounts of reconstituted microbubbles per liter.
while maintaining sterility by optimizing sterilization settings.
Methodology
Microbubble Manufacture: Span60, NaCl, and PBS are mixed
with either Tween80 or TPGS to form ST68 or SE61
suspensions. Suspensions are autoclaved and bubbles are
generated by sonication (3 min, 110 W) and purging with
PFC. Wash and gravity separation of microbubbles at 4º C
with 3 cold PBS washes. Pipetted 2ml of bubbles in
lyophilization vials with 2 ml glucose/PBS solution (maintain
1:1) and freeze-dry. Injected PFC gas into vials. 0.05g of
powder are transferred to vials. Plasma sterilized at
appropriate settings. Bubbles reconstituted with RPMI media

to test size, echogenicity, or sterility.
Figure 3: Acoustic stability; the response of a fixed amount of
Plasma Sterilization Process: Extracted cap on lyophilization
reconstituted microbubbles per liter over a period of time.
vials to open position. With a rubber band, wrapped Kimwipe
around vial so opening is covered. Connected plasma cleaner As for contamination of microbubbles, all the controls showed
to gas tank, inserted vials into chamber. Initiated vacuum no contamination under microscopy examination. Controls
inside chamber, turned on machine and allowed gas in for were simply petri dishes with RPMI medium. This confirmed
chosen time. Turned off vacuum, allowed gas to enter and that the experimenter’s aseptic method was adequate. An
pressure to equalize. Opened chamber, quickly closed caps increasing trend of plasma treatment led to an increasing
and placed samples in container sprayed with alcohol. number of sterile dishes:
Acoustic Setup: 5 MHz Transducer focused through an Table 1: The percentage of uncontaminated petri dishes with
acoustic window in vessel with 50 ml PBS. Signal amplified respect to plasma sterilization setting:
to 40 dB and analyzed using Labview [1].
Sterility Testing: Another portion of plasma sterilized samples
are reconstituted with RPMI media and incubated in small
petri dishes for 48 hours at 37 C. Microscopy was used to
explore for bacteria contamination.
Data & Results

Microbubbles maintained a diameter from 1 to 3 microns
(tested using dynamic light scattering). As for echogenicity, it
seems that various settings of plasma gas do not cause
significant loss in response. However, the duration of
echogenic response is slightly decreased over time, which
2