Supra 50vp

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.

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).

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.

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.

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.

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.

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.