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43 protocols using supra 50vp

1

Dentin Tubules Obturation Analysis

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Specimens were fixed in 2.5% phosphate-buffered glutaraldehyde solution for 1 d. After rinsing for 3 times in phosphate buffer solution, samples were exsiccated in an ascending ethanol row (50–96%). Samples were then saturated for 72 h and fixed in photo-curing one-component methacrylate-based resin (Technovit 7200 VLC, Haereus Kulzer, Hanau, Germany). Samples were then placed on SEM holders and got sputter-coated with a standardized gold layer of 8.0 nm (Sputter CCU-010, Safematic GmbH, Bad Ragaz, Switzerland).
A surface assessment was performed at 10 kV (Zeiss Supra 50 VP, Zeiss, Oberkochen, Germany). Photos were taken at 1000x and 10,000x magnification. Images were taken from a standardized area (300 μm to “right” and “above” from the discs’ central point) Assessment of dentin tubules obturation was performed using the Olley score with values from one to five indicating the degree of occlusion (1 – occluded, 2 – partially unoccluded, 3 – equally occluded/unoccluded, 4 – partially occluded, 5 – unoccluded) [34 (link)].
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2

Scaffold surface characterization by SEM

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Before and after respective storage, sterilization or release experiments, small pieces of the scaffolds were mounted on metal stubs with conductive double-sided tape. The samples were sputter coated (SCD 500, Bal-tec) with 10 nm platinum coating and then examined by SEM (Zeiss SUPRA 50 VP, Zeiss, Cambridge, UK), at an accelerating voltage of 5 kV.
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3

SEM Imaging of Dry Microcapsules

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Dry microcapsules or dry C–A scaffolds with incorporated microcapsules were directly mounted onto aluminium stubs with double-sided adhesive tabs. The samples were sputter-coated with a 3 nm-thick platinum–palladium layer and imaged using a Zeiss Supra 50VP SEM (Carl Zeiss SMT Inc.) with an accelerating voltage of 6 kV and a working distance of 5 mm.
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4

Characterizing Dentin Tubule Obturation via EDX Analysis

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In order to characterize the material that obturated the dentin tubules of DentinoCer specimens, energy-dispersive X-ray spectroscopy (EDX, Zeiss Supra V50, Carl Zeiss, Oberkochen, Germany) was used. Proportions of different chemical elements of interest were detected and reported as percentage of the whole composition. The respective analysis was performed from two directions, top view and vertical intersections. For the latter, specimens were cut centrally (Buehler, ISOMET® low speed saw, Prüfmaschinen AG, Dietikon, Diamant Cut-off Wheel, Struers GmbH, Birmensdorf, Switzerland) and polished.
On this behalf, the samples were newly embedded in resin and vapor-coated with coal powder which allowed for a better discrimination by backscatter analysis. Photos of the intersections were made at 10 kV (Zeiss Supra 50 VP) and at a magnification of 10.000x. Element analysis was performed from the tubular plugs and – as a control - from intertubule dentin areas.
Imaging was performed by a single operator (BS) who was unaware of the pre-treatment of the specimen. Likewise, the person analyzing the respective images (PS) was blinded to the group allocation.
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5

Characterization of Microcapsule Morphology and Composition

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Scanning electron microscopy (SEM, Zeiss Supra 50VP, Carl Zeiss Microscopy LLC , White Plains, NY, USA) coupled with ImageJ (National Institute of Health) was used to characterize the capsule shell thickness, agglomeration, and average microcapsule size. The SEM samples were sputter coated with platinum, and measurements were made at 5.0 kV accelerating voltage.
Thermogravimetric analysis (TGA, TA Instruments TAQ50, TA Instruments, New Castle, DE, USA) was used to determine MMI-2/PA content within microcapsules [10 (link)]. The amount of encapsulated solution is taken as the mass loss during the TGA run. Capsule specimens were heated at a rate of 5 °C min−1 to 100 °C and held for 30 min to stimulate water loss. This was followed by heating to 180 °C for 30 min and 200 °C for 60 min, which bracketed the boiling point of PA (b.p. 196 °C).
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6

Microstructure Analysis of Pack-Cemented Samples

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In order to study the microstructure pack-cementation and conditioning, samples were hot mounted (Struers Poly Fast, Struers GmbH, Willich, Germany) and ground from 180 grit down to 2000 grit, followed by mechanical polishing with a 3 μm and 1 μm diamond suspension and finished using colloidal silica. The microstructures were investigated using a Zeiss Merlin or Zeiss Supra 50 VP (Carl Zeiss Microscopy, Oberkohen, Germany) scanning electron microscope (SEM). SEM images were typically performed in the backscattered electron (BSE) mode. To determining the diffusion path, electron backscatter diffraction (EBSD) measurements (Oxford Instruments, Bognor Rigis, UK) were performed for phase identification after conditioning. For EBSD, electrons were accelerated using 15 kV and a grit of 517 × 376 pixels with as step size of 0.11 µm was used. For phase identification, the following crystallographic parameters and databases has been used, Table 1.
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7

Surface Morphology Characterization of SERS Substrates

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The surface morphology of the SERS substrates was studied with scanning electron microscopy using the electron microscope Supra 50VP (Zeiss, Oberkochen, Germany) with a resolution of 1.5 nm.
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8

Characterization of PANI Films

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As-deposited and washed PANI films were analyzed by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). FTIR spectra were acquired using a Thermo Nicolet 6700 spectrometer in transmission mode using an MCT/A detector at a resolution of 4 cm−1 and averaged over 128 scans. An FTIR spectrum of aniline monomer was also acquired in attenuated total reflectance (ATR) mode. Top-down SEM images were taken using a Zeiss Supra 50VP with the in lens detector at 15 kV and a working distance of 4 mm. The images, acquired using line integration with 7 repeats, were used to estimate film thicknesses. Prior to SEM imaging, samples were sputtered with Pt for 30 s. XPS analysis was conducted using a Physical Electronics VersaProbe 5000 with a micro-focused monochromatic scanned X-ray beam from an Al Kα X-ray source (1486 eV photons) at a spot size of 100 µm, 25 W, and 15 kV. High resolution C1s, N1s, Cl2p, and Sb3d spectra were recorded with a pass energy of 23.5 eV and an energy step of 0.05 eV for a total of 512, 2048, 256, and 256 scans, respectively.
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9

Characterization of Nanodiamond Morphology

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The morphology of nanodiamond was characterized using a TEM (JEOL JEM-2100, Japan) with an accelerating voltage of 200 kV. The TEM samples were prepared by dispersing powders in ethanol by sonication, depositing several drops of the solution onto a copper grid covered by lacey carbon films, and then drying in air. The particle size distribution of the 0.82 mg mL−1 nanodiamond solution in LiPF6-EC/DEC electrolyte was measured using a Zetasizer Nano ZS (Malvern Instruments) in 173° scattering geometry. The morphology of Li deposits was characterized using a SEM (Zeiss Supra 50VP, Germany), operated at 3.0 kV. The SEM samples were prepared in the glove box. The XRD patterns of Li deposits were recorded by a powder diffractometer (Rigaku Smart Lab, USA) with Cu Kα radiation at an acquisition rate of 0.2° min−1 and 0.5 s dwelling time.
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10

High-Resolution SEM Imaging of Substrates

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SEM images were obtained using the scanning electron microscope Supra 50VP (Zeiss, Germany). The electron optical GEMINI column provided excellent beam brightness with an ultrahigh resolution of 1 nm at the accelerating voltage of 20 kV. Substrate surfaces and profiles were scanned at the accelerating voltage of 10 kV, with an aperture size of 30 µm, at the work distance of 8 mm, and at the chamber pressure of 9 × 10−4 Pa.
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