Images and maps were measured with a Gemini 1550 SEM (Zeiss, Germany) and an EDX detector Ultim Max 100 (Oxford Instruments, UK) at an acceleration voltage of 10 kV. Samples were coated with 18 nm titanium using a Precision Etching Coating System Model 682 (GATAN, United States) prior to SEM observation and EDX studies.
Model 682
Manufactured by Ametek
Sourced in United States
The Ametek Model 682 is a laboratory equipment device designed for specialized tasks. It offers core functionality to support various applications within a controlled environment. The device specifications and capabilities are tailored to meet the needs of research and testing procedures.
Automatically generated - may contain errors
7 protocols using model 682
1
SEM and EDX Characterization of Coated Samples
2
Analyzing Porous Gel Microstructure via SEM
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Cross-sectional images of the dried-gels were acquired using SEM, following published procedures [8 (link)]. For sample preparation, for imaging of the cross-sections, uniform-sized gels were made and freeze-dried and sputter-coated with gold/palladium (2–3 min) in a sputter coater (Gatan Model 682 Precision etching coating system, Pleasantown, CA, USA) and visualized using SEM (S-4800, Hitachi, Japan) at voltages of 12 kV at varying magnifications. Resultant images obtained were analyzed using Image J to determine their average pore diameter (µm) and its variation across samples.
3
Scanning and Transmission Electron Microscopy Analysis of CNTs
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The surface morphology analysis of the specimens was conducted using scanning electron microscopy (Merlin compact with Gemini-I electron column, Zeisis Pvt. Ltd., Jena, Germany) at room temperature. Before the tests, all samples were coated with gold by a Gatan Model 682 precision etching coating system for about 15 min to improve the electron conductivity of the samples. The cryogenic fracture surface analysis was examined at a voltage of 10.0 kV.
The transmission electron microscopy of the specimens was examined through JOEL JEM 2100. The specimens were prepared by dispersing the CNTs into the ethanol solution with and without PVP. A single drop of this dispersion from both specimens was placed on a carbon-coated copper grid. Then the specimens were dried at room temperature.
The transmission electron microscopy of the specimens was examined through JOEL JEM 2100. The specimens were prepared by dispersing the CNTs into the ethanol solution with and without PVP. A single drop of this dispersion from both specimens was placed on a carbon-coated copper grid. Then the specimens were dried at room temperature.
4
Scaffold Degradation Characterization via SEM
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SEM micrographs were acquired from acellular printed scaffolds at varying time points to study the effects of environmental degradation on the scaffolds. Prior to SEM imaging, samples were lyophilized and sputter-coated with gold/palladium (2–3 min) in a sputter coater (Gatan Model 682 Precision etching coating system, Pleasantown, CA) and visualized using SEM. Average pore diameter of the acellular crosslinked 3D printed scaffolds was measured at Days-0 and -14 by analyzing electron micrographs of cross-sectioned lyophilized samples (S-4800, Hitachi, Japan) at 7 kV voltage and current of 5 μA at varying magnification. Collected images obtained were analyzed using Image J to determine the average sizes of the pores (pore diameter, μm) during each time point studied. A total of at least n = 5 images per sample was assessed for samples evaluated at varying time points.
5
Characterization of Multi-Walled Carbon Nanotubes
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The structure of MWNTs was examined
by scanning electron microscopy
(SEM) using an FEI Quanta FEG 250 SEM from FEI Co. (Hillsboro, OR,
USA). The equipment was operated at ∼20 keV. Prior to imaging,
the sample surface was coated with <50 nm layer of gold and palladium
using a GATAN model 682 precision etching coating system. Thermal
analysis of MWNTs was carried out using a PerkinElmer Thermogravimetric
Analyzer (Waltham, MA, USA) using nitrogen as a carrier gas. The temperature
was gradually increased from 30 to 800 °C using approximately
10 mg of sample. The difference in weight over the temperature gradient
provided the information about the sample. The charge on MWNTs was
measured, using a ZetaPALS analyzer (Brookhaven, NY, USA), through
electrophoretic mobilities of MWNTs at variable pH of the background
solution.
Brunauer, Emmett, and Teller (BET) surface area and
porosity of MWNTs was measured by NOVA 2200e automated gas sorption
system (Quantachrome, FL., USA) using nitrogen gas at 77 K. The data
were analyzed by Quantachrome NOVAWIN data acquisition and reduction
software version 11.02 provided by the manufacturer. The adsorption/desorption
isotherms of N2 were measured at a relative pressure (P/Po), ranging from 0.0001 to
0.99. The BET equation was utilized to determine the specific surface
area.
by scanning electron microscopy
(SEM) using an FEI Quanta FEG 250 SEM from FEI Co. (Hillsboro, OR,
USA). The equipment was operated at ∼20 keV. Prior to imaging,
the sample surface was coated with <50 nm layer of gold and palladium
using a GATAN model 682 precision etching coating system. Thermal
analysis of MWNTs was carried out using a PerkinElmer Thermogravimetric
Analyzer (Waltham, MA, USA) using nitrogen as a carrier gas. The temperature
was gradually increased from 30 to 800 °C using approximately
10 mg of sample. The difference in weight over the temperature gradient
provided the information about the sample. The charge on MWNTs was
measured, using a ZetaPALS analyzer (Brookhaven, NY, USA), through
electrophoretic mobilities of MWNTs at variable pH of the background
solution.
Brunauer, Emmett, and Teller (BET) surface area and
porosity of MWNTs was measured by NOVA 2200e automated gas sorption
system (Quantachrome, FL., USA) using nitrogen gas at 77 K. The data
were analyzed by Quantachrome NOVAWIN data acquisition and reduction
software version 11.02 provided by the manufacturer. The adsorption/desorption
isotherms of N2 were measured at a relative pressure (P/Po), ranging from 0.0001 to
0.99. The BET equation was utilized to determine the specific surface
area.
6
Fabrication of Al2O3 Bicrystal for TEM Analysis
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The Al2O3 bicrystal was fabricated by the thermal diffusion bonding of two high-purity single crystals (>99.99%, Shinkosha Co. Ltd.) at 1500 °C for 30 h in air. For doping Zr, we spattered Zr on the single crystal surface before bonding using an etch-coating system (Model 682, Gatan Inc.). The specimens for TEM observations were prepared as follows. We cut the fabricated bicrystals into small pieces and polished mechanically to a thickness of about 20 μm. They were further thinned to electron transparency by Ar+ ion milling using an ion polishing system (Model 691, Gatan Inc.).
7
Electrochemical Characterization of Pencil Graphite Electrodes
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Electrochemical studies were carried out using a Princeton VersaSTAT MC (VersaSTAT 3, Model RE-1, Princeton Applied Research, AMETEK, USA). The electrochemical study was performed by using a conventional three-electrode system consisting of a bare/modified PGE as working electrode, the counter electrode was a platinum wire, while the reference electrode was Ag/AgCl (saturated KCl). Pencil graphite was available as pencil lead from Rotring Co. Ltd (Germany, S0312670 of type 2B, B, HB, H and 2H). All leads possessed a diameter of 0.5 mm and were used as received.
The pH values of buffer solutions were recorded using a pH meter (Hanna Instruments Brazil, São Paulo, SP, Brazil). All measurements were done at room temperature.
For morphological characterization of prepared NP-modified PGEs, samples were coated with 10 nm thick gold by using a PECS fine grinding and coating device (Gatan, Model 682, UK). Then a scanning electron microscopy (SEM) instrument (JEOL JSM-5400 LV, Oxford, USA) was used.
The pH values of buffer solutions were recorded using a pH meter (Hanna Instruments Brazil, São Paulo, SP, Brazil). All measurements were done at room temperature.
For morphological characterization of prepared NP-modified PGEs, samples were coated with 10 nm thick gold by using a PECS fine grinding and coating device (Gatan, Model 682, UK). Then a scanning electron microscopy (SEM) instrument (JEOL JSM-5400 LV, Oxford, USA) was used.
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