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Orthopaedic Proceedings
Vol. 99-B, Issue SUPP_3 | Pages 25 - 25
1 Feb 2017
McEntire B Zhu W Pezzotti G Marin E Sugano N Bal B
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Introduction

Femoral heads made from zirconia-toughened alumina (ZTA) are the most advanced bioceramic available for total hip arthroplasty. ZTA's superior mechanical properties result from the polymorphic transformation of its zirconia (ZrO2) phase in the presence of a propagating crack. In vitro derived activation energies predict that several human lifetimes are needed to reach a state of significant transformation;1 but in vivo confirmation of material stability is still lacking. This investigation determined if transition metal ions might be responsible for triggering the tetragonal to monoclinic (t®m-ZrO2) phase transformation in this bioceramic.

Materials and Methods

BIOLOX®delta femoral heads (CeramTec GmbH, Plochingen, Germany) were acquired and characterized for their surface monoclinic content, Vm, using Raman spectroscopy. Then they were physiologically scratched with different metals (i.e., Ti, CoCr, and Fe, n=3 each) to simulate in vivo staining as a result of acetabular shell impingement due to subluxation or dislocation. They were subsequently hydrothermally aged for up to 100 h in an autoclave at 98∼132°C and 1 bar pressure. Raman maps, each consisting of 120 spectra, were compiled and monoclinic contents, Vm, calculated for zones adjacent to and away from the metal stains.2 Activation energies for the t®m transformation in stained and non-stained zones were derived and compared to retrieved heads having service lives of between ∼45 days and ∼8 years.


Orthopaedic Proceedings
Vol. 99-B, Issue SUPP_3 | Pages 26 - 26
1 Feb 2017
Bal B Puppulin L McEntire B Pezzotti G
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Introduction

The longevity of highly cross-linked polyethylene (XLPE) bearings is primarily determined by its resistance to long-term oxidative degradation. Addition of vitamin E to XLPE is designed to extend in vivo life, although it has unintended consequences of inducing higher frictional torque and increased wear when articulating against metallic femoral heads.1–3 Conversely, lower friction was observed when oxide ceramic heads were utilized.3 Previous studies suggest that oxide ceramics may contribute to XLPE oxidation, whereas a non-oxide ceramic, silicon nitride (Si3N4), might limit XLPE's degradation.4 To corroborate this observation, an accelerated hydrothermal ageing experiment was conducted using static hydrothermal contact between XLPE and commercially-available ceramic femoral heads.

Materials and Methods

Two sets of four types of ceramic femoral heads, consisting of three oxides (Al2O3 BIOLOX®forte, and ZTA BIOLOX®delta, CeramTec, GmbH, Plochingen, Germany; and m-ZrO2 OXINIUMTM, Smith & Nephew, Memphis, TN, USA) and one non-oxide (MCSi3N4, Amedica Corp., Salt Lake City, UT, USA) were cut into hemispherical sections. Six highly crosslinked polyethylene liners (X3TM Stryker Orthopedics, Inc., Mahwah, New Jersey, USA) were also sectioned, gamma irradiated (32 kGy), and mechanically clamped (25 kN) to the convex surfaces of the ceramic heads (Figure 1(a)). All surfaces were dipped in water and placed into an autoclave at 121°C under adiabatic conditions for 24 hr. The test was repeated three times using two couples for each material along with XLPE-on-XLPE controls. Each XLPE sample was characterized before and after ageing using Raman spectroscopy for variations in their crystalline phase and oxidation indices using the intensities of unpolarized vibrational bands at 1296, 1305, and 1418 cm−1. Significance (p<0.05) was determined using Student's t-test with a sample size of n=18.


Orthopaedic Proceedings
Vol. 99-B, Issue SUPP_3 | Pages 47 - 47
1 Feb 2017
McEntire B Pezzotti G Bock R Zhu W Marin E Adachi T Bal B
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Introduction

Due to its remarkable stoichiometric flexibility and surface chemistry, hydroxyapatite (HAp) is the fundamental structural material in all vertebrates. Natural HAp's properties inspired an investigation into silicon nitride (Si3N4) to see if similar functionality could be engineered into this bioceramic. Biological and in situ spectroscopic analyses were used to monitor the response of osteosarcoma cells (SaOS-2) to surface-modulated Si3N4 and a titanium alloy after long-term in vitro exposure.

Materials and Methods

Four groups of Si3N4 discs, Ø12.7×1.0mm, (Amedica Corporation, Salt Lake City, UT USA) were subjected to surface treatments: (i) “As-fired;” (ii) HF-etched (5% HF solution for 45 s); (iii) Oxidized (1070°C for 7 h); and (iv) Nitrogen-annealed (1400°C for 30 min, 1.1 bar N2 gas).1 Titanium alloy discs (Ti6Al4V, ASTM F136) were used as a control group. SaOS-2 cells cultured for 24 h at 37°C were deposited (5×105 cells/ml) and incubated on the UV sterilized discs in an osteogenic medium for 7 days at 37°C. Cell proliferation was monitored using scanning electron and laser microscopy. The Receptor Activator of NF-kB Ligand (sRANKL) and the insulin growth factor 1 (IGF-1) were used to evaluate osteoclast formation and cell proliferation efficiency, respectively. In situ Raman spectroscopy was employed to monitor metabolic cell activity. Statistics (n≥3) were analyzed using the Student's t-test or one-way Analysis of Variance with p<0.05 considered significant.


Orthopaedic Proceedings
Vol. 99-B, Issue SUPP_4 | Pages 146 - 146
1 Feb 2017
McEntire B Jones E Bock R Ray D Bal B Pezzotti G
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Introduction

Periprosthetic infections are leading causes of revision surgery resulting in significant increased patient comorbidities and costs. Considerable research has targeted development of biomaterials that may eliminate implant-related infections.1 This in vitro study was developed to compare biofilm formation on three materials used in spinal fusion surgery – silicon nitride, PEEK, and titanium – using one gram-positive and one gram-negative bacterial species.

Materials and Methods

Several surface treated silicon nitride (Si3N4, MC2®, Amedica Corporation, Salt Lake City, UT), poly-ether-ether-ketone (PEEK, ASTM D6262), and medical grade titanium (Ti6Al4V, ASTM F136) discs Ø12.7 × 1mm were prepared or acquired for use in this well-plate study. Each group of discs (n=3) were ultrasonically cleaned, UV-sterilized, inoculated with 105Staphylococcus epidermidis (ATCC® 25922™) or Escherichia coli (ATCC® 14990™) and placed in a culture medium of phosphate buffered saline (PBS) containing 7% glucose and 10% human plasma on a shaking incubator at 37°C and 120 rpm for 24 or 48 hrs. Coupons were retrieved, rinsed in PBS to remove planktonic bacteria, placed in a centrifuge with fresh PBS, and vortexed. The bacterial solutions were serially diluted, plated, and incubated at 37°C for 24 to 48 hrs. Colony forming units (CFU/mm2) were counted using applicable dilution factors and surface areas. A two-tailed, heteroscedastic Student's t-test (95% confidence) was used to determine statistical significance.


Orthopaedic Proceedings
Vol. 98-B, Issue SUPP_7 | Pages 28 - 28
1 May 2016
Bal B McEntire B Rahaman M Pezzotti G
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Introduction

Oxide-based alumina (Al2O3) is used to manufacture femoral heads for total hip arthroplasty (THA). Silicon nitride (Si3N4) is a non-oxide ceramic used to make spinal implants. Ceramic materials are believed to be bioinert, (i.e., stable under hydrothermal conditions). Indeed, clinical data have shown 15–20 year longevity of Al2O3 bearings in THA. In this work, we examined the surfaces of Al2O3 and Si3N4 after exposure to physiologic conditions to see if these ceramics are truly inert.

Materials and Methods

Four self-mated Ø28 mm diameter Al2O3 femoral heads (n=2 each of BIOLOX®forte, CeramTec, Plochingen, Germany; and BIOCERAM®, Kyocera Co., Kyoto, Japan), were retrieved during revision THA, between 7.7–10.7 years post-implantation. To simulate in vivo material aging, comparable, new Al2O3 and Si3N4 femoral heads (AMEDICA Corporation, Salt Lake City, UT, USA) were exposed to autoclave conditions (100°C-121°C; 300 hrs; n=3 heads, per material). Advanced Raman and cathodoluminescence spectroscopy, and electron microscopy were used to examine surface characteristics of each specimen, and quantify oxygen ion vacancy formation and composition.


Orthopaedic Proceedings
Vol. 98-B, Issue SUPP_9 | Pages 130 - 130
1 May 2016
Pezzotti G Puppulin L Boffelli M McEntire B Rahaman M Yamamoto K Bal B
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Introduction

In total hip arthroplasty (THA), polyethylene (PE) liner oxidation leads to material degradation and increased wear, with many strategies targeting its delay or prevention. However, the effect of femoral head material composition on PE degradation for ceramic-PE articulation is yet unknown. Therefore, using two different ceramic materials, we compared PE surface alterations occurring during a series of standard ceramic-PE articulation tests.

Materials and Method

Ceramic-PE THA bearings were tested in a simulator, using ASTM F2003-02, ASTM F1714-96 (2013) and ISO 14242:1–3 standards. Acetabular liners (Apex-Link PolyTM, OMNI Life Science, East Taunton, MA, USA) were articulated against Ø28 mm Si3N4 femoral heads (Amedica Corp., Salt Lake City, UT, USA). For comparison, ArCom® PE liners (Biomet Inc. Warsaw, IN, USA) were also tested against Ø28 mm zirconia-toughened alumina (ZTA) femoral heads (BIOLOX®delta, CeramTec GmbH, Plochingen, Germany), under the same conditions. After 5 million cycles of wear, all specimens were examined using nano-spectroscopy tools. Evaluations were performed on six couples per group, plus 3 untested control couples; n= 6 (+3). Spectrographic examinations generated 8 maps of 400 points each randomly selected on the wear zones of each liner, with each map area being 20 µm2 at an in-plane spatial resolution of 1 µm.


Orthopaedic Proceedings
Vol. 98-B, Issue SUPP_9 | Pages 29 - 29
1 May 2016
McEntire B Bal B Rahaman M Pezzotti G
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Introduction

The in vivo evolution of surface material properties is important in determining the longevity of bioceramics. Fracture toughness is particularly relevant because of its role in wear resistance. Some bioceramics, such as zirconia (ZrO2) undergo in vivo phase transformation, resulting in a marked reduction in toughness and commensurate increased wear. Here, we investigated the effect of accelerated aging on the surface toughness of alumina (Al2O3), zirconia-toughened alumina (ZTA), and silicon nitride (Si3N4) femoral heads, in order to identify the optimal ceramic material for in vivo implantation and long-term durability.

Materials

A newly developed Raman microprobe-assisted indentation method was applied to evaluate and compare surface fracture toughness mechanisms operative in Si3N4 (Amedica Corporation, Salt Lake City, UT, USA), Al2O3 and ZTA (BIOLOX® forte, and delta, respectively, CeramTec, GmbH, Plochingen, Germany) bioceramics. The Al2O3 and ZTA materials have long established histories in total hip arthroplasty; whereas Si3N4 has been newly developed for this purpose. The improved method proposed here consisted in coupling the “traditional” indentation technique with quantitative assessments of microscopic stress fields by confocal Raman microprobe piezo-spectroscopy. Concurrently, crack opening displacement (COD) profiles were also monitored by Raman spectroscopy. Toughness measurements were determined using both as-received and hydrothermally exposed (100–121°C for up to 300 hours) femoral heads.


Orthopaedic Proceedings
Vol. 98-B, Issue SUPP_7 | Pages 45 - 45
1 May 2016
Bock R McEntire B Bal B Rahaman M Boffelli M Pezzotti G
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Introduction

Silicon nitride (Si3N4) is a ceramic material presently implanted during spine surgery. It has a fortunate combination of material properties such as high strength and fracture toughness, inherent phase stability, scratch resistance, low wear, biocompatibility, hydrophilic behavior, easier radiographic imaging and resistance to bacterial biofilm formation, all of which make it an attractive choice for orthopaedic applications beyond spine surgery. Unlike oxide ceramics, (e.g., alumina or Al2O3) the surface chemistry and topography of Si3N4 can be precisely engineered to address in vivo demands. Si3N4 can be manufactured to have an ultra-smooth, or highly fibrous, or porous morphology. Its chemistry can be varied from that of a silica-like surface composed of silanol moieties to one which is predominately comprised of silicon-amine functional groups.

Methods

In the present study, a Si3N4 bioceramic formulation was exposed to thermal, chemical, and mechanical treatments in order to induce changes in surface composition and features. The treatments included grinding and polishing, etching in hydrofluoric acid solution, and heating in nitrogen or air. Resulting surfaces were characterized using a variety of microscopy techniques to assess morphology. Surface chemical and phase composition were determined using x-ray photoelectron and Raman spectroscopy, respectively. Streaming potential measurements evaluated surface charging, and sessile water drop techniques assessed wetting behavior.


Orthopaedic Proceedings
Vol. 86-B, Issue SUPP_I | Pages 10 - 11
1 Jan 2004
Oonishi H Kim S Clarke I Asano T Bal B Kyomoto M Masuda S
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According to the knee simulator test results in 1970s, the total decrease in thickness of UHMWPE tibial tray in combination with ceramic femoral component [F-Comp] was less than one tenth as that of the combination with metal [1]. These advantages led to development of total knee prosthesis [TKP] with alumina ceramics. In this study, we report the wear surface observation, the clinical wear and the oxidation of the retrieved TKP used clinically for 23 years, comparing with a metal TKP.

The retrieved TKP was implanted in 1979, and retrieved on January 9th in 2002. This TKP consisted of an alumina ceramic F-Comp and a UHMWPE tray combined with a alumina ceramic tibial component. Observations of the surface of alumina F-Comp and UHMWPE tray were carried out using SEM. Shape of UHMWPE tray was determined three-dimensionally. Comparing the result with original shape based on the product’s plan, liner wear and volumetric wear were calculated. Oxidation index was determined by Fourier transform infrared spectrophotometry.

Alumina F-Comp did not have any scratch on the surface by seeing with naked eye. UHMWPE tray had deformation and scratches obviously. The liner wear rate was 37 micrometer/year and volumetric wear rate was 18.8 mm3/year. The oxidation indexes were 0.6 in the unworn area, 1.2 in the worn area and 0.2 in the inner area.

SEM observations of the F-Comp demonstrated no scratch or pit. In contrast, many scratches were clearly observed on the UHMWPE tray. However, higher magnification observations did not demonstrate severe wear, which was shown on the wear analysis of a metallic F-Comp. Oxidation degradation is a problem to solve. However, the low wear rate and mild wear pattern demonstrate that ceramic F-Comp reduced UHMWPE wear.