Corrosion at modular junctions of total hip replacements has been identified as a potential threat to implant longevity, resulting in efforts to determine appropriate countermeasures. Visual scoring and volumetric material loss measurements have been useful tools to elucidate various clinical and design factors associated with corrosion damage. However, corrosion involves electron exchange that results in chemical changes to biomedical alloys, and electrochemical assessment may therefore be a more appropriate approach to understand the phenomenon. The purpose of this pilot study was to electrochemically distinguish the severity of corrosion in retrieved femoral heads. A secondary goal was to identify the potential of electrochemical impedance spectroscopy (EIS) as a method to identify different forms of corrosion damage. Twenty femoral heads were identified from a larger study of total hip replacements, obtained as part of an ongoing multi- center IRB-approved retrieval program. Using a previously established 4-point scoring method, components were binned by taper damage: 10 components were identified as having severe damage, 7 with moderate damage and 2 with mild damage. One (1) unimplanted control was included to represent minimal corrosion damage. All components were then characterized using electrochemical impedance spectroscopy under the frequency domain: a 10 mV sinusoidal voltage, ranging from 20 kHz to 2 mHz, was applied to the taper of a femoral head (working electrode) filled with a 1M solution of PBS, a platinum counter electrode and a chlorided silver reference electrode. Absolute impedance at 2 mHz (|Z0.002|), and max phase angle (θ) were assessed relative to taper damage severity. After least-squares fitting of the EIS data to a Randles circuit with a constant phase element, circuit elements: polarization resistance (Rp), CPE-capacitance, and CPE-exponent were also evaluated. The seven (7) most severely corroded components were further examined with scanning electron microscopy to identify corrosion modes. For all statistical analyses, significance was determined at alpha=0.05.Introduction
Methods
Utilization of reverse total shoulder arthroplasty (RTSA) has steadily increased since its 2003 introduction in the American market. Although RTSA was originally indicated for elderly, low demand patients, it is now being increasingly used to treat rotator cuff arthropathy, humeral fractures, neoplasms and failed total and hemi shoulder arthroplasty. There is, therefore, a growing interest in bearing surface wear of RTSA polyethylene humeral liners. In the current study, we examined humeral liners retrieved as part of an IRB approved study to determine the amount of bearing surface wear. We hypothesized that wear of the bearing surface by intentional contact with the glenosphere (mode I) would be minor compared to that produced by scapular notching and impingement of the humeral liner (mode II). Twenty-three retrieved humeral liners were retrieved at revision surgery after an average of 1.5 years implantation time. The average age at implantation was 68 years (range 50–85). Shoulders were revised for loosening (7), instability (6), infection (6), pain (2), and other/unknown reasons (2). The liners were scanned using microCT at a resolution of 50 µm and then registered against unworn surfaces to estimate the bearing surface wear depth. The depth of surface penetration due to impingement of the liner with surrounding structures was measured and the location of the deepest penetration was noted. Mode I wear of the bearing surface was detectable for five of the retrieved liners. The penetration depth was 100 µm or less for four of the liners and approximately 250 microns for the fifth liner. It was noted that the liners with discernable mode I wear were those with longer implantation times (average 2.4 years). Material loss and abrasion of the rim due to mode II wear was noted with measurable penetration in 18 of the liners. Mode II wear penetrated to the bearing surface in 11 liners. It was generally noted that volumetric material loss was dominated by mode II wear (Figure 1). In this study of short to medium term retrieved RTSA humeral liners, mode I wear of the bearing surface was a minor source of material loss. Mode II wear due to scapular notching or impingement of the rim was the dominant source of volumetric wear. This is in agreement with a previous study that we have performed on a smaller cohort of seven liners. It is noteworthy that we were able to detect measurable mode I wear for liners with moderate implantation times. The quantity of bearing surface wear that will be seen in long term retrievals remains unknown at this time.
There is considerable interest in the orthopaedic community in understanding the multifactorial process of taper fretting corrosion in total hip arthroplasty (THA). Previous studies have identified some patient and device factors associated with taper damage, including length of implantation, stem flexural rigidity, and head offset. Due to the complexity of this phenomenon, we approached the topic by developing a series of matched cohort studies, each attempting to isolate a single implant design variable, while controlling for confounding factors to the extent possible. We also developed a validated method for measuring material loss in retrieved orthopaedic tapers, which contributed to the creation of a new international standard (ASTM F3129-16). Based on our implant retrieval collection of over 3,000 THAs, we developed independent matched cohort studies to examine (1) the effect of femoral head material (metal vs. ceramic, n=50 per cohort) and (2) stem taper surface finish (smooth vs. microgrooved, n=60 per cohort). Within each individual study, we adjusted for confounding factors by balancing implantation time, stem taper flexural rigidity, offset, and, when possible, head size. We evaluated fretting and corrosion using a four-point semiquantitative score. We also used an out-of-roundness machine (Talyrond 585) to quantify the material loss from the tapers. This method was validated in a series of experiments of controlled material removal on never-implanted components.Introduction
Methods
During revision surgery with a well-fixed stem, a titanium sleeve can be used in conjunction with a ceramic head to achieve better stress distribution across the taper surface. Previous studies have observed that the use of a ceramic head can mitigate the extent of corrosion damage at the taper. Moreover, Thirty sleeved ceramic heads (Biolox Option: CeramTec) were collected during revision surgery as part of a multi-center retrieval program. The sleeves were used in conjunction with a zirconia-toughened alumina femoral head. The femoral heads and sleeves were implanted between 0.0 and 3.25 years (0.8±0.9, Figure 1). The implants were revised predominantly for instability (n=14), infection (n=7), and loosening (n=5). Fifty percent of the retrievals were implanted during a primary surgery, while 50% had a history of a prior revision surgery. Fretting corrosion was scored using a previously described 4-point, semi-quantitative scoring system proposed by Higgs [2].Introduction
Materials and Methods
Previous studies of long-term CoCr alloy femoral components for TKA have identified 3rd body abrasive wear and inflammatory cell induced corrosion (ICIC). The extent of femoral condyle surface damage in contemporary CoCr femoral components is currently unclear. The purpose of this study was to investigate the prevalence and morphology of damage (3rd body scratches and ICIC) at the bearing surface in retrieved TKA femoral components from contemporary designs. 308 CoCr femoral TKA components were collected as part of an ongoing, multi-institutional orthopedic implant retrieval program. The collection included contemporary designs from Stryker (Triathlon n=48, NRG n=10, Scorpio n=31), Depuy Synthes (PFC n=27) and Zimmer (NexGen n=140, Persona n=1) and Biomet (Vanguard n=51). Hinged knee designs and unicondylar knee designs were excluded. Components were split into groups based on implantation time: short-term (1–3y, n=134), intermediate-term (3–5y, n=73) and long-term (6–15y, n=101). Each grouping was mainly revised for instability, infection and loosening. Third-body abrasive wear of CoCr was evaluated using a semi-quantitative scoring method similar to the Hood method (Figure 1). A score of 1 had minimal damage and a score of 4 corresponded to damage covering more than 50% of the evaluated area. ICIC damage was reported as location of affected area. A white light interferometer (Zygo New View 5000) was also used to analyze the topography of severe damage of the bearing surface. For this analysis, three representative components from each cohort were selected and analyzed in three locations on the apex of the bearing surface. We analyzed the following roughness parameters: Ra, Rsk, and Rku.Introduction
Methods
Highly crosslinked polyethylene (HXLPE) was clinically introduced approximately a decade and a half ago to reduce polyethylene wear rates and subsequent osteolysis. Clinical and radiographic studies have repeatedly shown increased wear resistance, however concerns of rim oxidation and fatigue fracture remain. Although short to intermediate term retrieval studies of these materials are available, the long-term behavior of these materials remains unclear. Between 2000 and 2015, 115 1st generation HXLPE acetabular liners implanted for 5 or more years were collected and analyzed as part of an ongoing, multi-institutional orthopaedic implant retrieval program. There were two material cohorts based on thermal processing (annealed (n=45) and remelted (n=70)). Each cohort was stratified into two more cohorts based on implantation time (5 – 10 years and >10 years). For annealed components, the intermediate-term liners (n=30) were implanted on average (±SD) for 7.3 ± 1.7 years while the long-term liners (n=15) were implanted for 11.3 ± 1.8 years. For remelted components, the intermediate-term liners (n=59) were implanted on average (±SD) for 7.2 ± 1.3 years while the long-term liners (n=11) were implanted for 11.3 ± 1.2 years. For each cohort, the predominant revision reasons were loosening, instability, and infection (Figure 1). Short-term liners (in-vivo <5ys) from previous studies were analyzed using the same protocol for use as a reference. For oxidation analysis, thin slices (∼200 μm) were taken from the superior/inferior axis and subsequently boiled in heptane for 6 hours to remove absorbed lipids that may interfere with the oxidation analysis. 3mm line profiles (in 100μm increments) were taken perpendicular to the surface at each region of interest. Oxidation indices were calculated according to ASTM 2102. Penetration was measured directly using a calibrated micrometer (accuracy=0.001mm).Introduction
Methods
Previous studies of retrieved CoCr alloy femoral heads have identified imprinting of the stem taper surface features onto the interior head bore, leading researchers to hypothesize that stem taper microgrooves may influence taper corrosion. However, little is known about the role of stem taper surface morphology on the magnitude of in vivo corrosion damage. We designed a matched cohort retrieval study to examine this issue. From a multi-institutional retrieval collection of over 3,000 THAs, 120 femoral head-stem pairs were analyzed for evidence of fretting and corrosion using a visual scoring technique based on the severity and extent of fretting and corrosion damage observed at the taper. A matched cohort design was used in which 60 CoCr head-stem pairs with a smooth stem taper were matched with 60 CoCr head-stem pairs having a micro-grooved surface, based on implantation time, flexural rigidity, apparent length of taper engagement, and head size. This study was adequately powered to detect a difference of 0.5 in corrosion scores between the two cohorts, with a power of 82% and 95% confidence. Both cohorts included CoCr and Ti-6-4 alloy femoral stems. A high precision roundness machine (Talyrond 585, Taylor Hobson, UK) was used to measure surface morphology and categorize the stem tapers into smooth vs. micro-grooved categories. Fretting and corrosion damage at the head/neck junction was characterized using a modified semi-quantitative adapted from the Goldberg method by three independent observers. This method separated corrosion damage into four visually determined categories: minimal, mild, moderate and severe damage.Introduction
Methods
Mechanically assisted crevice corrosion of taper interfaces was raised as a concern in total hip arthroplasty (THA) approximately 20 years ago (Gilbert 1993). In total shoulder replacement, however, comparatively little is known about the prevalence of fretting assisted crevice corrosion or the biomechanical and patient factors that influence this phenomenon. Given the comparatively lower loading experienced in the shoulder compared to the hip, we asked: (1) What is the prevalence of fretting assisted corrosion in modular total shoulder replacements, and (2) What patient and implant factors are associated with corrosion? Modular components were collected from 48 revision shoulder arthroplasties as part of a multi-center, IRB approved retrieval program. For anatomic shoulders, this included 40 humeral heads, 32 stems and four taper adapters from seven manufacturers. For reverse shoulders, there were eight complete sets of retrieved components from three manufacturers. The components were predominantly revised for instability, loosening and pain. Anatomical shoulders were implanted for an average of 3.1 years (st dev 3.8; range 0.1–14.5). Reverse shoulders were implanted for an average of 2.2 years (st dev 0.7; range 1.3–3.3). Modular components were disassembled and examined for taper damage. The modular junctions were scored for fretting corrosion using a semi-quantitative four-point scoring system adapted from Goldberg, et al. (Goldberg, 2002, Higgs 2013). The scoring system criteria was adapted from Goldberg and Higgs which is comprised of a one to four grading system (with one indicating little-to-no fretting/corrosion and four indicating extensive fretting/corrosion). The component alloy composition was determined using the manufacturer's laser markings and verified by x-ray fluorescence. Patient age, gender, hand dominance, alloy, flexural rigidity of the trunnion and taper geometry were assessed independently as predictors for fretting corrosion.INTRODUCTION
METHODS
In THA, fretting corrosion at the head-stem taper junction has emerged as a clinical concern that may result in adverse local tissue reactions, even in patients with a metal-on-polyethylene bearing [1]. Taper junctions that employ a ceramic head have demonstrated reduced corrosion at the interface [2]. However, during revision surgery with a well-fixed stem, a titanium sleeve is used in conjunction with a ceramic head to ensure proper fit of the head onto the stem and better stress distribution. In vitro testing has suggested that corrosion is not a concern in sleeved ceramic heads [3]; however, little is known about the in vivo fretting corrosion of the sleeves. The purpose of this study was to investigate fretting corrosion in sleeved ceramic heads. Between 2001 and 2014, 35 sleeved ceramic heads were collected during revision surgery as part of a multi-center retrieval program. The sleeves were all fabricated from titanium alloy and manufactured by 4 companies (CeramTec (n=14), Smith & Nephew (Richards, n=11), Stryker (n=5), and Zimmer (n=5)). The femoral heads were made from 3 ceramics (Alumina (n=7), Zirconia (n=11), and Zirconia-toughened Alumina (n=17)). Sleeve dimensions (length and thickness) were measured using calibrated calipers. Fretting corrosion of the sleeves and available associated stems was scored using a 4-point, semi-quantitative scoring system [4], with 1 being little-to-no damage, and 4 corresponded to severe fretting corrosion. Five sleeves could not be extracted; thus the external surface was not scored.Introduction
Materials and Methods
A variety of porous coatings and substrates have been used to obtain fixation at the bone-implant interface. Clinical studies of porous tantalum, have shown radiographically well-fixed implants with limited cases of loosening. However, there has been limited retrieval analysis of porous tantalum hip implants. The purpose of this study was to investigate factors affecting bone ingrowth into porous tantalum hip implants. 126 porous tantalum acetabular shells and 7 femoral stems, were collected under an IRB-approved multicenter retrieval program. Acetabular shells that were grossly loose, cemented or complex revisions were excluded. Shells with visible bone on the surface were chosen. 20 acetabular shells (10 primary) and all femoral stems were dehydrated, embedded, sectioned, polished and bSEM imaged (Figure-1). Main shell revision reasons were infection (n=10,50%), femoral loosening (n=3,15%) and instability (n=3,15%). Analyzed implants were implanted for 2.3±1.7 years (shells) and 0.3±0.3 years (stems). Eight slices per shell and 5–7 slices per stem were analyzed. The analysis included bone area/pore area (BA/PA), BA/PA zonal depth analysis, extent of ingrowth and maximum depth of bone ingrowth. BA/PA zone depths were: Zone-1 (0–500um), Zone-2 (500–1000um) and Zone-3 (1000um-full depth). Nonparametric statistical tests investigated differences in bone measurements by location within an implant and implant type (Friedman's Variance and Kruskal-Wallis). Post-hoc Dunn tests were completed for subsequent pairwise comparisons. Spearman's rank correlation identified correlations between bone measurements and patient related variables (implantation time, age, height, weight, UCLA Activity Score). Statistical analyses were performed using PASW Statistics package.Introduction
Methods
Retrieval analysis is an important aspect of medical device development. Examination of retrieved devices allows device developers to close the design loop, understand the performance of devices, and validate assumptions made and methods used during preclinical testing. We provide an overview of the implant retrieval analysis performed at the Implant Research Center at Drexel University on reverse total shoulder systems retrieved after short to medium term implantation. We have examined 18 reverse total shoulders, retrieved at revision surgery after short to mid-term implantation (average 1.4 years, maximum 3.3 years). The average age at revision was 71 years old (st dev 11 years). Our evaluations included analysis of glenosphere bearing surface damage, evaluation of tribocorrosion at the modular junctions, visual assessment of polyethylene humeral bearing surface damage, quantitative analysis of polyethylene wear.INTRODUCTION
METHODS
Recent implant design trends have renewed concerns regarding metal wear debris release from modular connections in THA. Previous studies regarding modular head-neck taper corrosion were largely based on cobalt chrome (CoCr) alloy femoral heads. Comparatively little is known about head-neck taper corrosion with ceramic femoral heads or about how taper angle clearance influences taper corrosion. This study addressed the following research questions: 1) Could ceramic heads mitigate electrochemical processes of taper corrosion compared to CoCr heads? 2) Which factors influence stem taper corrosion with ceramic heads? 3) What is the influence of taper angle clearance on taper corrosion in THA? 100 femoral head-stem pairs were analyzed for evidence of fretting and corrosion. A matched cohort design was employed in which 50 ceramic head-stem pairs were matched with 50 CoCr head-stem pairs based on implantation time, lateral offset, stem design and flexural rigidity. Fretting corrosion was assessed using a semi-quantitative scoring scale where a score of 1 was given for little to no damage and a score of 4 was given for severe fretting corrosion. The head and trunnion taper angles were measured using a roundness machine (Talyrond 585, Taylor Hobson, UK). Taper angle clearance is defined as the difference between the head and trunnion taper angles.Introduction
Methods
The release of metal debris and ions has raised concerns in joint arthroplasty. In THA metal debris and ions can be generated by wear of metal-on-metal bearing surfaces and corrosion at modular taper interfaces, currently understood to be mechanically assisted crevice corrosion (MACC) [1]. More recently, inflammatory-cell induced corrosion (ICIC) has been identified as a possible source of metal debris and/or ions [2]. Although MACC has been shown to occur at modular junctions in TKA, little is known about the prevalence of other sources. The purpose of this study was to determine the sources of metallic debris and ion release in long-term implanted (in vivo > 15y) TKA femoral components. Specific attention was paid to instances of ICIC as well as damage at the implant-bone interface. 1873 retrieved TKA components were collected from 2002–2013 as part of a multi-center, IRB-approved retrieval program. Of these, 52 CoCr femoral condyles were identified as long term TKA (Average: 17.9±2.8y). These components were predominantly revised for loosening, PE wear and instability. 40/52 of the components were primary surgeries. Components were examined using optical microscopy to confirm the presence of 5 damage mechanisms (polyethylene failure, MACC corrosion of modular tapers, corrosion damage between cement and backside, third-body wear, and ICIC). Third-body wear was evaluated using a semi-quantitative scoring method based on the percentage of damaged area. A score of 1 had minimal damage and a score of 4 corresponded to severe damage. Polyethylene components were scored using the Hood method and CoCr components were scored similarly to quantify metal wear. The total area damaged by ICIC was quantified using photogrammetry. Images were taken using a digital SLR with a calibrated ruler in the same focal plane. Using known pixel dimensions, the ICIC damaged area was calculated.Introduction
Methods
First generation highly crosslinked polyethylenes (HXPLEs) have proven successful in lowering both penetration and osteolysis rates. However, 1st generation annealing and remelting thermal stabilization have been associated with in vivo oxidation or reduced mechanical properties. Thus, 2nd generation HXLPEs were developed to improve oxidative stability while still maintaining material properties. Little is known about the in vivo clinical failure modes of these 2nd generation HLXPEs. The purpose of this study was to assess the revision reasons, wear, oxidative stability, and mechanical behavior of retrieved sequentially annealed Vitamin E diffused HXLPE in THA and TKA. 251 2nd Generation HXLPE hip and knee components were consecutively retrieved during revision surgeries and continuously analyzed in a prospective, IRB approved, multicenter study. 123 acetabular liners (Implanted 1.2y; Range 0–5.0y) and 117 tibial inserts (Implanted 1.6y; Range 0–5.8y) were highly crosslinked and annealed in 3 sequential steps (X3). Five acetabular liners (Implanted 0.6y; Range 0–2.0y) and six tibial inserts (Implanted 1.3y; Range 0.5–1.8y) were diffused with Vitamin E (E1). Patient information was collected from medical records (Table 1). Linear penetration of liners was measured using a calibrated digital micrometer (accuracy: 0.001 mm). Surface damage of tibial components was assessed using the Hood method. Thin sections were taken from the acetabular liners (along the superior/inferior axis) and the tibial components (along the medial condyle and central spine) for oxidation analysis and analyzed according to ASTM 2102. Mechanical behavior was assessed via the small punch test (ASTM 2183).Introduction:
Methods:
Degradation of modular head-neck tapers was raised as a concern in the 1990s (Gilbert 1993). The incidence of fretting and corrosion among modern, metal-on-polyethylene and ceramic-on-polyethylene THA systems with 36+ mm femoral heads remains poorly understood. Additionally, it is unknown whether metal debris from modular tapers could increase wear rates of highly crosslinked PE (HXLPE) liners. The purpose of this study was to characterize the severity of fretting and corrosion at head-neck modular interfaces in retrieved conventional and HXLPE THA systems and its effect on penetration rates. 386 CoCr alloy heads from 5 manufacturers were analyzed along with 166 stems (38 with ceramic femoral heads). Metal and ceramic components were cleaned and examined at the head taper and stem taper by two investigators. Scores ranging from 1 (mild) to 4 (severe) were assigned in accordance with the semi-quantitative method adapted from a previously published technique. Linear penetration of liners was measured using a calibrated digital micrometer (accuracy: 0.001 mm). Devices implanted less than 1 year were excluded from this analysis because in the short-term, creep dominates penetration of the head into the liner.Introduction:
Patients & Methods:
Previous studies regarding modular head-neck taper corrosion were largely based on cobalt chrome (CoCr) alloy femoral heads. Less is known about head-neck taper corrosion with ceramic femoral heads. We asked (1) whether ceramic heads resulted in less taper corrosion than CoCr heads; (2) what device and patient factors influence taper fretting corrosion; and (3) whether the mechanism of taper fretting corrosion in ceramic heads differs from that in CoCr heads.Background:
Questions/purposes:
Aseptic loosening continues to be a short and long-term complication for patients with cemented knee replacements. Changes in cemented total knee replacement (TKR) fixation have been limited to assessment of radiographic changes at the implant-bone interface and quantification of component migration. The goal of this study was to determine the interlock morphology between cement and trabecular bone using Twelve retrieved tibial components and two lab-prepared constructs with time in service from 0 to 20 years were sectioned in the transverse plane in 10 mm increments, imaged at high resolution, and the current contact fraction (INTRODUCTION:
METHODS:
Sequentially annealed highly crosslinked polyethylenes (HXLPEs) were introduced in total knee replacement (TKR) starting in 2005 to reduce wear and particle-induced osteolysis. Few studies have reported on the clinical performance of HXLPE knees. In this study, we hypothesized that due to the reduced free radicals, sequentially annealed HXLPE would have lower oxidation levels than gamma inert-sterilized controls. 145 tibial components were retrieved at consecutive revision surgeries at 7 different surgical centers. 74 components were identified as sequentially annealed HXLPE (X3, Stryker) while the remainder (n = 71) were conventional gamma inert sterilized polyethylene. The sterilization method was confirmed by tracing the lot numbers by the manufacturer. The conventional inserts were implanted for 1.7 years (Range: 0.0–9.3 years), while the X3 components were implanted 1.1 years (Range: 0.0–4.5 years). Surface damage was assessed using the Hood method. Oxidation analysis was performed in accordance with ASTM 2102 following submersion in boiling heptane for 6 hours to remove absorbed lipids. 30 of the conventional and 29 of the HXLPE inserts were available for oxidation analysis.Introduction
Methods
Wear debris generation in metal-on-metal (MOM) total hip arthroplasty (THA) has emerged as a compelling issue. In the UK, clinically significant fretting corrosion was reported at head-taper junctions of MOM hip prostheses from a single manufacturer (Langton 2011). This study characterizes the prevalence of fretting and corrosion at various modular interfaces in retrieved MOM THA systems used in the United States. 106 MOM bearing systems were collected between 2003 and 2012 in an NIH-supported, multi-institutional retrieval program. From this collection, 88 modular MOM THA devices were identified, yielding 76 heads and 31 stems (22 modular necks) of 7 different bearing designs (5 manufacturers) for analysis. 10 modular CoCr acetabular liners and 5 corresponding acetabular shells were also examined. Mean age at implantation was 58 years (range, 30–85 years) and implantation time averaged 2.2 ± 1.8 years (range, 0–11.0 years). The predominant revision reason was loosening (n=52). Explants were cleaned and scored at the head taper, stem taper, proximal and distal neck tapers (for modular necks), liner, and shell interfaces in accordance with the semi-quantitative method of Goldberg et al. (2002).Introduction
Methods and Materials
The purpose of this multicenter study was to assess the oxidative stability, mechanical behavior, wear and reasons for revision of 2nd generation sequentially annealed HXLPE, X3, and compare it to 1st generation XLPE, Crossfire. We hypothesized that X3 would exhibit similar wear rates but lower oxidation than Crossfire. 182 hip liners were consecutively retrieved during revision surgeries at 7 surgical centers and continuously analyzed over the past 12 years in a prospective, multicenter study. 90 were highly crosslinked and annealed (Crossfire; Implanted 4.2±3.4 years, max: 11 years), and 92 were highly crosslinked and annealed in 3 sequential steps (X3; Implanted 1.2±1.5 years; max: 5 years). Oxidation was characterized in accordance with ASTM 2102 using transmission FTIR performed on thin sections (∼200μm) from the superior/inferior axis. Mechanical behavior was assessed via the small punch test (ASTM 2183).Introduction
Methods
