Kα spectrometer

Raman studies were carried out using a Renishaw 1000 spectrometer equipped with a He-Ne laser (λ = 633 nm) and coupled to a microscope with a 50× objective. The Raman system was calibrated using a silicon reference. Acquisition time was 10 s. Raman scattering spectra were recorded in the range of 150–2000 cm⁻¹. X-ray diffraction (XRD) analysis was carried out using a Bruker AXS D8 (Lynxeye XE) diffractometer with a monochromated copper X-ray source (Kα₁, λ = 1.54 Å) under a glancing incident angle (θ) of 1°. UV–Vis spectroscopy was performed using a Perkin Elmer Lambda 950 UV/Vis/NIR Spectrophotometer. A Labsphere reflectance standard was used as a reference. X-Ray photoelectron spectroscopy (XPS) was performed using a Thermo K-α spectrometer with monochromated aluminium Kα radiation, a dual beam charge compensation system and constant pass energy of 50 eV. Survey scans were collected in the range of 0–1200 eV. High-resolution peaks were used for the principal peaks of Ti 2p, O 2p and C 1s. The peaks were modelled using sensitivity factors to calculate the film composition. The area underneath these bands is an indication of the element concentration within the region of analysis (spot size: 400 µm).

The following samples were prepared for antimicrobial testing: control polyurethane polymer samples (solvent treated only), glutaraldehyde‐impregnated samples (biocidal swelling solution treated), and glutaraldehyde‐coated samples (biocidal solution treated only). The infrared absorbance spectra of the polyurethane polymer samples were measured using a Bruker Platinum ATR, within the range 4000–400 cm⁻¹ with an accumulation of 15 scans per sample. X‐ray photoelectron spectroscopy (XPS) analysis of the solvent‐treated and glutaraldehyde‐impregnated polyurethane polymer samples was carried out using a Thermo Scientific, (United Kingdom) K‐α spectrometer to classify the different elements present as a function of polymer depth. All binding energies were calibrated to the C 1s peak at 284.5 eV.

XPS was performed
on a Thermo Fisher Scientific K-α+ spectrometer. Samples were
analyzed using a microfocused monochromatic Al X-ray source (72 W)
over an area of ∼400 μm. Data were recorded at pass energies
of 150 eV for survey scans and 40 eV for high-resolution scans with
1 and 0.1 eV step sizes, respectively. Charge neutralization of the
sample was achieved through a combination of both low-energy electrons
and argon ions. Three well-separated areas were selected on each sample
for analysis to examine any surface heterogeneity. Data analysis was
performed in CasaXPS using a Shirley-type background and Scofield
cross sections, with an energy dependence of −0.6.

The morphology of the synthesized materials was examined using scanning electron microscopy (SEM, VERIOS 460, FEI) operating at 10 kV and high-resolution transmission electron microscope (HR-TEM, ARM300, JEOL) operating at 300 kV. Elemental mapping was attained using energy-dispersive X-ray spectroscopy (EDX) equipped with the SEM and TEM. The crystal structure analysis was performed using an X-ray diffractometer (XRD, D/Max2000, Rigaku) with Cu-Ka radiation. Surface chemistry was analyzed using X-ray photoelectron spectroscopy (XPS, Thermo Scientific Kα spectrometer, 1486.6 eV)

Field-emission scanning electron microscopy. Two Ti implants from each surface group were removed from the sterile packs with plastic tweezers and fixed with carbon tape to SEM stubs, taking care to not to damage or contaminate the surfaces. Both the lateral and flat surfaces of the implants were imaged non-coated at an accelerating voltage of 5 keV and increasing magnifications (up to 50,000×) by FE-SEM (Hitachi S-5200, Japan).
X-ray photoelectron spectroscopy. Implants were analyzed by XPS using a Thermo Fisher Scientific K_α spectrometer (E. Grinstead, UK). A monochromatic Al K_α X-ray source was used with a nominal 400 µm spot size. Survey spectra were obtained (200 eV pass energy (PE)) followed by an examination at 150 eV PE of spectral regions of interest from which the relative atomic percentage composition was obtained. High-resolution spectra (25 eV PE) were also obtained for the Ti envelope. Charge compensation was applied for all spectra using a combined e/Ar + floodgun, and the energy scale was shifted to place the C1s peak at 284.6 eV. All data processing was performed using the Avantage 5.926 software supplied by the manufacturer.