The fabrication steps for the formulations employed and the rationale for their use can be found elsewhere [8 (link)]. The PCM (n-Nonadecane, Sigma-Aldrich, St. Louis, MO, United States) was melted using a water bath and then mixed with Part A (resin) of EpoFix (Struers Inc., Cleveland, OH, United States) using a dual asymmetric speed mixer (Flacktek, Landrum, SC, United States). The thickening agent (Carbopol, Sigma-Aldrich, St. Louis, MO, United States) was then added, followed by the thermally conducting fillers, carbon nanofibers (CNF, 2 wt.%) and boron nitride (BN, 10 wt.%) particles, both of which were procured from Sigma Aldrich. Part B (hardener) of the EpoFix was finally added to the mixture, and the formulation was left to cure at room temperature in flexiform molds for 24 h (Struers, Inc. Cleveland, OH, United States). The samples containing CNF and BN powders were designated as EC-PCM40-CNF2 and EC-PCM40-BN10, respectively. The sample preparation steps for the specimen without thermally conductive fillers, designated as EC-PCM40, were identical than for the other formulations except the filler addition. Detailed sample formulations are presented in Table 1 .
Epofix
Manufactured by Struers
Sourced in Denmark, United States, Germany
EpoFix is a cold-mounting resin designed for embedding samples for metallographic analysis. It is a two-component epoxy resin that cures at room temperature to form a hard, durable mount. The core function of EpoFix is to provide a stable and uniform platform for subsequent grinding and polishing of samples.
Automatically generated - may contain errors
Lab products found in correlation
Discoplan ts, by Struers (4 mentions)
Isomet, by Buehler (3 mentions)
Ips e max cad, by Ivoclar Vivadent (3 mentions)
S 3500n sem, by Hitachi (2 mentions)
K450 carbon coater, by Quorum Technologies (2 mentions)
Isocut fluid, by Buehler (2 mentions)
Metadi 3, by Buehler (2 mentions)
Ecomet 250 grinder polisher, by Buehler (2 mentions)
Sic abrasive paper, by Struers (2 mentions)
Zhu0 2 z2, by Zwick Roell (2 mentions)
Ultracut r, by Electron Microscopy Sciences (2 mentions)
Ultra afm, by Electron Microscopy Sciences (2 mentions)
Histo, by Electron Microscopy Sciences (2 mentions)
Citovac chamber, by Struers (2 mentions)
Planopol 5, by Struers (2 mentions)
Phoenix beta, by Buehler (2 mentions)
Md dac, by Struers (2 mentions)
Ecomet 3, by Buehler (1 mentions)
Tm3030plus, by Hitachi (1 mentions)
Sc7620, by Quorum Technologies (1 mentions)
51 protocols using epofix
1
Thermally Conductive Epoxy-PCM Composites
2
Mechanical Characterization of Dental Fibers
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Specimens prepared from WildCat 175 and WildCat 215 were cut into 15-mm segments using a low speed oil-cooled diamond saw (IsoMet, Buehler, Lake Bluff, Il). Then the segments were embedded longitudinally in an epoxy resin (EpoFix, Struers, Ballerup, Denmark) and were ground and polished up to 1-μm alumina slurry in a grinding/polishing machine (EcoMet III, Buehler). Fifteen EverStic fibers were randomly divided in three groups (n=5). Each fiber was cut in almost equal parts of 2 mm with a surgical lancet. The fiber of first group were immersed in StickResin (ESRE) of second one in FlowTain (ESFT) while no resin was used in third group (ES). The fibers were aligned together along their long axis and placed between two slabs. The slabs were pressed slightly one against the other and each point was cured for 40 sec as described above.
Force-indentation depth curves were monitored applying 4.9 N with a 2-s dwell time by a Vickers indenter employing an Instrumented Indentation Testing machine ZHU0.2/Z2.5 (Zwick Roell). Five readings were taken from each specimen, and the mean value was used as representative of the specimen. Martens Hardness (HM), Indentation Modulus (EIT) and elastic index (ηΙΤ) which represents the ratio of elastic to total indentation work were derived from forceindentation depth curves.
Force-indentation depth curves were monitored applying 4.9 N with a 2-s dwell time by a Vickers indenter employing an Instrumented Indentation Testing machine ZHU0.2/Z2.5 (Zwick Roell). Five readings were taken from each specimen, and the mean value was used as representative of the specimen. Martens Hardness (HM), Indentation Modulus (EIT) and elastic index (ηΙΤ) which represents the ratio of elastic to total indentation work were derived from forceindentation depth curves.
3
Interferometry and SEM Analysis of HA Pellets
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HA was synthesized by a sol-gel precipitation method [42 (link)]. Discs (12 mm diameter, 1 mm thickness) were formed in a pellet press and were then sintered at 700 °C for 4 h. Pellets were then embedded in EpoFix (Struers) resin and were polished with silicon carbide discs (Struers) of decreasing grain size, down to 5 μm.
Interferometry was carried out on a MicroXAM2 (Omniscan), using green light. Scans on day 0 were carried out over a depth of 20 μm, while scans on day 7 were carried out over a depth of 30 μm. All scans had a noise reduction of 0.05. Scanning electron microscopy (SEM) images were taken using secondary electron detection, with a TM3030 Plus (Hitachi) at 15 kV. Embedded pellets were attached to a steel mount with carbon tape, sputter coated with 15 nm of gold, and connected to the mounting with copper tape to improve conductivity. Pellets were analyzed via both modalities, and then, 40 μL of 2 w/v% alginate with or without 0.2 M HMP was applied. The pellets were stored in a closed container with water to create a humid environment and reduce evaporation. The formulation was removed with deionized water, the pellets were dried with absorbent paper, taking care not to scratch the surface, and formulation was reapplied in the same location. This was repeated daily, for 5 days, before reanalysis of the pellet surfaces.
Interferometry was carried out on a MicroXAM2 (Omniscan), using green light. Scans on day 0 were carried out over a depth of 20 μm, while scans on day 7 were carried out over a depth of 30 μm. All scans had a noise reduction of 0.05. Scanning electron microscopy (SEM) images were taken using secondary electron detection, with a TM3030 Plus (Hitachi) at 15 kV. Embedded pellets were attached to a steel mount with carbon tape, sputter coated with 15 nm of gold, and connected to the mounting with copper tape to improve conductivity. Pellets were analyzed via both modalities, and then, 40 μL of 2 w/v% alginate with or without 0.2 M HMP was applied. The pellets were stored in a closed container with water to create a humid environment and reduce evaporation. The formulation was removed with deionized water, the pellets were dried with absorbent paper, taking care not to scratch the surface, and formulation was reapplied in the same location. This was repeated daily, for 5 days, before reanalysis of the pellet surfaces.
4
Specimen Preparation and SEM Analysis
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Specimens were embedded using Struers EpoFix® resin and left to cure for at least 24 h. Sections were cut using a Buehler IsoMet® low speed saw. Cut surfaces were impregnated using Buehler EPO THIN® resin. Small specimens were then mounted in 25 mm diameter aluminium rings using Buehler EpoFix®. All specimens were ground manually using P800 to P4000 grit paper. Buehler IsoCut Fluid was used for lubrication during grinding. Large sections were polished manually using Buehler MetaDi® 3 and 1 µm Diamond Paste. Following 24h curing, specimens were ground manually using P1200 to P4000 grit paper. Specimens mounted in aluminium rings were polished using a Buehler Ecomet® 250 Grinder–Polisher using Buehler MetaDi® 3 and 1µm suspensions. Selected polished sections were etched using 5% orthophosphoric acid (H3PO4) for between 1 -2 minutes. Polished specimens were carbon coated using the Emitech K450 carbon coater. Images were taken using a Hitachi S-3500N SEM. SEM analysis was conducted at the University of Bristol School of Earth Science’s Electron Microbeam Facility.
5
Specimen Preparation and SEM Analysis
6
Stomatopod Raptorial Club Structure Analysis
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Stomatopods of the species Odontodactylus scyllarus were acquired from aquarist vendors in Singapore and Stockholm. The animals obtained from Singapore were kept in aquaria with artificial seawater in the same manner as in our previous work (Chua et al., 2023 ▸ ; Amini et al., 2019 ▸ ). From the live animals, three mature clubs were collected when shed during moulting (clubs 1, 2 and 6), and another club was collected one week after moulting (club 7). The animals obtained from the aquarist vendor in Stockholm were sacrificed on arrival in Aarhus, stored in 50% ethanol for one day, followed by 70% ethanol, and their right clubs (clubs 3–5) were subsequently isolated from the ethanol-preserved specimens.
For synchrotron radiation experiments, the clubs were first embedded in epoxy resin (EpoFix, Struers, Ballerup, Denmark), after which, axial sections were cut with a low-speed saw using a diamond cut-off wheel (accutom-5, with M1D15, Struers, Ballerup, Denmark). Then the slices were polished with SiC abrasive paper (Struers, Ballerup, Denmark) to a thickness below 100 µm.
For synchrotron radiation experiments, the clubs were first embedded in epoxy resin (EpoFix, Struers, Ballerup, Denmark), after which, axial sections were cut with a low-speed saw using a diamond cut-off wheel (accutom-5, with M1D15, Struers, Ballerup, Denmark). Then the slices were polished with SiC abrasive paper (Struers, Ballerup, Denmark) to a thickness below 100 µm.
7
Fracture Resistance of Dental Crowns
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The crowns were cemented to epoxy models (EpoFix; Struers, Ballerup, Denmark) of the preparations with zinc phosphate oxide cement (De Trey Zink; Dentsply DeTrey, Konstanz, Germany). The cement was chosen to minimize the bonding effect of the cement. Excess cement was removed, and after a 5‐min setting time the crowns were placed in distilled water at 37°C for 24 (range ± 2) h. The crowns were subsequently loaded centrally at the occlusal fossa with a horizontal cylindrical steel indenter of 13 mm in diameter, cushioned with a 2‐mm‐thick ethylene propylene diene rubber disc of hardness 90 Shore A (EPDM 90) to avoid contact damage. The cylinder was placed centrally to ensure even distribution of load between the cusps. The load was applied in a servo hydraulic testing system at 0.5 mm min−1 until fracture occurred (MTS 852 MiniBionix II; MTS Systems, Eden Prairie, MN, USA). The procedures were performed while the crowns were immersed in water at room temperature. Load at fracture was recorded. At 3,300 N, the procedure was halted because of equipment limitation. The fractured crowns were analyzed, using fractographic methods, to identify the fracture origin and direction of crack propagation 16 , 37 . The fracture initiation area was compared with the crown margins before fracture, to assess whether pre‐existing defects were the fracture initiators or not.
8
Electrode Sample Preparation for SEM
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The electrode sample was A small disc with a diameter of 2 mm was laser micro-machined from the as-dried electrode sample and clamped vertically using a small metal clip. The clip was fully immersed in a 15:2 ratio of epoxy resin to epoxy hardener (EpoFix, Struers) inside a plastic mould of 20 mm diameter. The mould, containing the resin, clip and sample, was placed in a desiccator and degassed under dynamic vacuum for 1 h before being left in the desiccator overnight under static vacuum to ensure minimal gas remained in the sample. The as-cured puck was subsequently hand-ground using a set of incrementally finer SiC papers (CarbiMet, Buehler), starting at P320 coarseness and finishing at P4000 coarseness, with interim IPA cleaning in a sonicator and visual inspection with an optical microscope (VHX-7000, Keyence)
to ensure the previous grinding grooves had disappeared. To minimise charging in the scanning electron microscope (EVO 10, Carl Zeiss), the smoothed epoxy-puck was Au-coated (SC7620, Quorum) for 60 s at 18 mA, giving a Au-coating thickness of the order of tens of nanometres.
to ensure the previous grinding grooves had disappeared. To minimise charging in the scanning electron microscope (EVO 10, Carl Zeiss), the smoothed epoxy-puck was Au-coated (SC7620, Quorum) for 60 s at 18 mA, giving a Au-coating thickness of the order of tens of nanometres.
9
Histological Sectioning of Bone Samples
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Histological sections were prepared from 1.5 cm-thick samples of the midshaft region following standard procedures [21] –[24] . Bone samples were embedded in epoxy resin EpoFix (Struers), the cutting surface was ground and polished with a Buehler low-speed Isomet with SiC grinding papers (SiC-800, SiC-1200; Struers) and fixed to a glass-slide with epoxy resin. Subsequently, 200 µm-thick sections were cut using a Struers Discoplan TS diamond saw, and finally ground and polished to a final thickness of 100 µm with the use of different SiC grinding papers (SiC-800, SiC-1200; Struers). All necessary permits were obtained for the described study, which complied with all relevant regulations (Vertebrate Paleontology Collection Department, Museo Nacional de Ciencias Naturales – CSIC, Madrid, Spain). All histological sections employed in the present paper are deposited in the Vertebrate Paleontology Collection of the MNCN and are available to researchers. High resolution images of the analyzed sections can be obtained from the corresponding author of this article.
10
Preparation of Dental Specimens for Mechanical Testing
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Bovine mandibular incisors (n = 150) were extracted (from bovine cadaver, 4–6 years old, Nortura), cut 2 cm length and embedded in epoxy resin (EpoFix, Struers) with buccal surface exposed. Embedded teeth were ground at DP-U2 with rotating 500-grit silicon carbide paper (Struers, Denmark) under water until 5 × 5 mm dentin surface was obtained and further stored in distilled water.
Circular zirconia (n = 100, Starceram Z, H.C. Starck Ceramics GmbH, Germany) and lithium disilicate (n = 50, IPS e.max CAD, Ivoclar Vivadent, Lichtensein) rods with diameter of 5 mm and length of 11.5 mm were produced by CAD/CAM technique. Rods were produced with a notch in the circumference (Figure 1 ) facilitating the grip during tensile testing.
One end of the rods was ground with 500 grit silicon carbide sandpaper under water to reflect use of a fine bur in a clinical situation [11 ,12 ], and to obtain uniform surface roughness. There after cleaned with a dental steam cleaner (Steamer X3, Amann Girrbach, Austria) and thoroughly air-dried.
Circular zirconia (n = 100, Starceram Z, H.C. Starck Ceramics GmbH, Germany) and lithium disilicate (n = 50, IPS e.max CAD, Ivoclar Vivadent, Lichtensein) rods with diameter of 5 mm and length of 11.5 mm were produced by CAD/CAM technique. Rods were produced with a notch in the circumference (
One end of the rods was ground with 500 grit silicon carbide sandpaper under water to reflect use of a fine bur in a clinical situation [11 ,12 ], and to obtain uniform surface roughness. There after cleaned with a dental steam cleaner (Steamer X3, Amann Girrbach, Austria) and thoroughly air-dried.
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