Ultim max 65

An inverted fluorescence microscope (ECLIPSE, Ti-S, Nikon, Co., Ltd.) with an oil immersion objective (100×, Plan Flour, Nikon) was used. Movies of the sample were taken while moving the viewing field, and the number of clusters having various m values was counted. Approximately 1000 clusters were counted in the total for PS samples. For the titania sample, more than 50 clusters were counted because most of the particles formed large aggregates.
Large aggregates of titania samples were observed using a confocal laser scanning microscope (type C2, Nikon) and an all-in-one microscope (BZ-X800, KEYENCE, Osaka, Japan) equipped with an optical sectioning module (BZ-H4XF, KEYENCE, Osaka, Japan).
The particles’ surface structure and elemental analysis were performed using a transmission electron microscope (type S-4800, Hitachi, Tokyo) and a EDS/EDX detector (ULTIM MAX65, Oxford Instruments, Tokyo, Japan) at the Analysis Center, Nagoya City University.

Scanning electron microscope (SEM)—Tescan MIRA3 Brno, The Czech Republic—and optical microscope (OM)—Opta-Tech 40LAB, Warsaw, Poland—were used to investigate the surface conditions of the worn samples.
SEM investigations was conducted in contrast to the secondary electron (SE) and backscattered electrons (BSE). The BSE contrast is beneficial because it gives information about chemical composition diversity. The areas that contain light elements are dark, whereas heavy elements are bright. Additionally, sample surfaces were analyzed by the EDS method. The microanalyzer (Ultim^® Max 65, Oxford Instruments, High Wycombe, UK) was used to detect the elements appearing on the surface of the sample. Calcium, fluorine, nickel, chromium, and oxygen were analyzed. The results of the EDS analysis were shown in one color-element concentration map and in twelve color-scale maps. In this investigation, the accelerating voltage equal to 12 kV was used because the interaction volume has to be limited.

The worn surfaces of sintered materials and counter-specimens as well as wear products were observed after the tests using SEM (Mira 3, Tescan, the Czech Republic) equipped with EDS (Ultim Max 65, Oxford Instruments, Abingdon, UK). In order to limit the excitation zone, an accelerating voltage of 12 kV was used. Quantitative tests of chemical composition of the surface of sintered materials and wear products were carried out. The element concentrations were also distributed in the form of EDS maps by means of a color scale. In the color scale, the colors corresponded to the concentration of the selected element. The intensive color pixels indicated the highest concentration of the element, and the darker areas corresponded to the concentration near to zero. Numerical values on these maps correspond to the number of counts. The phase composition tests were carried out on sinter surfaces after the frictional tests using an X-ray diffractometer (Empyrean, PANalytical, the Netherlands) equipped with a copper lamp (X-ray wavelength λ = 1.54060 Å) and an X’Celerator detector. XRD patterns were recorded at room temperature, in the angular range 25–100° 2theta, in steps of 0.017° 2theta. The phase analysis of the obtained diffractograms was performed in the HighScore program equipped with the PDF-4 database.

The morphology of the film surfaces was observed using SEM (Tescan Mira3, Tescan, Brno, Czech Republic) equipped with EDS (Oxford Instruments Ultim Max 65). An accelerating voltage of 12 kV was applied. Prior to SEM observation, the sheet surface of selected films was cleaned with methanol and dried for 220 min at 60 °C. All samples were sputtered coated with an amorphous layer of carbon with a thickness of approximately 20 nm. The Jeol JEE 4B vacuum evaporator (Peabody, MA, USA) was used. The contents of elements such as Mg were analyzed. Due to the low atomic number of carbon, its content was not measured. The distribution of element concentrations in the form of EDS patterns maps were performed.

For EDX measurements, a cross-section of the monolith was polished with an ion cross-section polisher (JEOL, SM-09010) in order to obtain a plane surface. To increase the conductivity of the surface, gold was sputtered onto it. The microstructure and chemical composition of the catalyst were then analyzed by means of a scanning electron microscope (SEM) (Zeiss, Gemini SEM300) equipped with an EDX-detector (UltimMax 65, Oxford instruments). The images were acquired at 20 kV with a scan time of 2 ms/pixel. The EDX data were then processed by AZtec software (V. 5.1, Oxford Instruments).

SEM investigation was performed on a Sigma VP (Zeiss, Germany) at low acceleration voltage (0.7 kV) and detected with an in-lens detector. The CSS was coated by sputter deposition with a 4.0 nm layer of a platinum/palladium alloy (80/20), while the AC—CSS were analyzed without coating.
The energy-dispersive X-ray spectroscopy (EDX) signal was detected with an Ultim^® Max 65 (Oxford Instruments, Abingdon, UK) at 5.5 kV. The signal was further processed and evaluated in AZtecLive software.