To examine the change of chemical components on the plasma-treated PTFE surface, angular-dependent X-rayphotoelectron spectroscopy (XPS) measurements were conducted by using a Quantum 2000 instrument (ULVAC-PHI) attached to an Al-Kα source with take-off angles of 15, 45, and 75°. The area of X-ray irradiation was Φ = 100 μm, the pass energy was 23.50 eV, and the step size was 0.05 eV. The C1s-XPS spectra were collected between 280 and 296 eV. The cumulative numbers of the measurement were three. During the XPS measurement, the low-speed electron beam and the Ar ion beam were irradiated for the measured samples to neutralize the charges of them. The binding energies of as-received and plasma-treated PTFE were referenced to the peak indexed to −CF2− at 292.5 eV and 291.8 eV, respectively20 (link), 25 (link).
Quantum 2000
Manufactured by Physical Electronics
Sourced in Japan, United States
The Quantum 2000 is an advanced analytical instrument designed for surface analysis. It utilizes a combination of X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES) techniques to provide detailed information about the chemical composition and electronic structure of a material's surface. The Quantum 2000 is capable of performing high-resolution, quantitative analysis of elemental concentrations, chemical states, and depth profiles of a wide range of materials.
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Lab products found in correlation
Jsm 7001f, by JEOL (2 mentions)
Icpe 9000, by Shimadzu (2 mentions)
Multipak software, by Physical Electronics (1 mentions)
Epma 1610, by Shimadzu (1 mentions)
S 4800, by Hitachi (1 mentions)
Xplora, by Horiba (1 mentions)
Jsm 7500fa, by JEOL (1 mentions)
Jem 1200 ex 2 microscope, by JEOL (1 mentions)
D8 discover, by Bruker (1 mentions)
Jem 2100f, by JEOL (1 mentions)
Asap 2020 hd analyser, by Micrometrics (1 mentions)
X pert pro powder diffractometer, by Malvern Panalytical (1 mentions)
Ultra plus 55, by Zeiss (1 mentions)
19 protocols using quantum 2000
1
Plasma-treated PTFE Surface Analysis
2
Surface Analysis of Ti-sputtered YSZ
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The Ti-sputtered YSZ surface was analyzed using X-ray photoelectron spectroscopy (XPS; Quantum 2000, ULVAC, Kanagawa, Japan) at 24 W before and after heat treatment to identify the chemical constituents and elemental states of the YSZ disks. The binding energies were calibrated by the C1s hydrocarbon peak at 285.0 eV. The XPS profiles were analyzed using the MultiPak software (ULVAC).
Secondary electron images (SEIs) were obtained using an electron probe microanalyzer (EPMA-1610, Shimadzu, Kyoto, Japan; EPMA) to observe the morphological characteristics of the fracture surface of the YSZ disks. Elemental mapping was performed on the fracture surfaces of the YSZ disks in the Au and Ti sputtering groups using EPMA.
For EPMA line analysis of the treated surface, a specimen in the Ti sputtering group was diagonally cut and polished, and its cross section was analyzed using EPMA at a voltage of 15 kV and a measurement time of 1.3 h.
Secondary electron images (SEIs) were obtained using an electron probe microanalyzer (EPMA-1610, Shimadzu, Kyoto, Japan; EPMA) to observe the morphological characteristics of the fracture surface of the YSZ disks. Elemental mapping was performed on the fracture surfaces of the YSZ disks in the Au and Ti sputtering groups using EPMA.
For EPMA line analysis of the treated surface, a specimen in the Ti sputtering group was diagonally cut and polished, and its cross section was analyzed using EPMA at a voltage of 15 kV and a measurement time of 1.3 h.
3
Nanoscale Surface Characterization of SiC Substrates
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A nanoindenter (ENT-2100, ELIONIX Inc.) was used to form some indents on the specimen, which were used as a reference in AFM observations. The maximum load applied for indentation was 100 mN. A total of 400 indents (20 × 20) separated by a distance of 10 μm were formed. The surface morphology of the polished SiC substrates was measured by AFM (SPA-400, SII Nanotechnology) in the tapping mode. For each specimen, 100 points that were uniformly distributed over the polished area were observed. The surface composition of the SiC substrates polished with pad rotation speeds of 500 rpm and 2500 rpm was determined by XPS (Quantum 2000, ULVAC-PHI) with AlKα radiation (1486.6 eV). To centralize the XPS observation to the top surface, the stage on which the specimen was located was tilted with a very low takeoff angle of 10°. Before the XPS measurements, to remove the organic contaminants on the specimen, cleaning in a sulfuric acid (H2SO4) and hydrogen peroxide (H2O2) mixture (SPM) was conducted for 10 min followed by cleaning in pure water for 10 min. The concentration of the SPM solution was H2SO4 (97 wt%): H2O2 (30 wt%) = 4:1. For each specimen, five points uniformly distributed over the polished area were observed to exclude any area dependence.
4
XPS Analysis of Plasma-Treated PTFE and SUS304
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XPS (Quantum2000, ULVAC-PHI, Chigasaki, Kanagawa, Japan) was used to investigate the change in the chemical-bonding state of the surfaces of PTFE and SUS304 samples before and after plasma treatment. The cumulative number, pass energy, and step size were 3, 25.00 eV, and 0.05 eV, respectively. XPS measurements were conducted at an X-ray take-off angle of 45°. Both low-speed EB and low-speed Ar ion irradiation were used to avoid surface charging during XPS measurements. The measured XPS data were analyzed using data analysis software (MultiPak V8.2C, 2007-9-04). The peaks were indexed to CF2 at 292.5 [12 (link)] and 291.8 eV for the as-received PTFE and plasma-treated PTFE samples, respectively [38 (link),39 (link)], and to C–C (C–H) at 284.6 eV for the SUS304 samples [38 (link)].
5
Characterization of Pd Nanoparticles on Substrates
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All the obtained samples were characterized by scanning electron microscopy (SEM), inductively coupled plasma atomic emission spectroscopy (ICP-AES), and X-ray photoelectron spectroscopy (XPS). The surfaces of the irradiated samples were observed by SEM-EDX (JSM-7001F, JEOL, Tokyo, Japan). Prior to the SEM observations, the surfaces of the polymer plates were coated with Os (OPC60A, Filgen, Aichi, Japan). SEM observations were performed at an acceleration voltage of 10–15 kV. The amount of Pd immobilized on the substrates was analyzed by ICP-AES (ICPE-9000, Shimadzu, Kyoto, Japan). The substrate surfaces (50 mm × 50 mm) were treated with 2 mL of aqua regia (HCl:HNO3 = 3:1) to dissolve the Pd nanoparticles. The surface chemical state was analyzed by XPS (Quantum 2000, ULVAC-PHI, Kanagawa, Japan) using an Al Kα X-ray source operating at 15 kV. A C1s level of 284.6 eV was used as an internal standard to correct for the peak drift. All high-resolution XPS peaks were fitted using XPSPEAK41 software.
6
X-ray Photoelectron Spectroscopy Protocol
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XPS measurements were performed using a scanning XPS spectrometer (Quantum-2000, Ulvac-Phi) with a monochromated Al-Kα source. All the XPS spectra were obtained below 5 × 10−6 Pa. The photoelectron take-off angle was 45°, and the X-ray irradiation area was Ø100 μm. Narrow scan XPS spectra of Si2p, C1s, O1s, and F1s were collected at 95–115 eV, 275–300 eV, 525–545 eV, and 680–700 eV, respectively, with a pass energy of 23.50 eV and a step size of 0.05 eV. The cumulative number of measurements was three. During an XPS measurement, the samples were irradiated with a low-speed electron beam and an Ar ion beam to achieve charge neutralization. The obtained XPS spectra of the PDMS samples were referenced to the peak indexed to C–Si–O–Si and/or C–H at 284.6 eV36 (link),37 (link), and the obtained XPS spectra of as-received and HAP-treated PTFE samples were referenced to peaks indexed to –CF2– at 292.5 eV34 (link),35 (link) and 291.8 eV13 ,38 (link), respectively. The main peak of –CF2– in the C1s-XPS spectra shifted toward lower binding energy for plasma-treated PTFE due to surface charging13 ,40 (link).
7
XPS Analysis of AP-PCVM-etched Surfaces
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To examine the difference in the chemical components on AP-PCVM-etched surfaces for different oxygen fractions, angular-dependent X-ray photoelectron spectroscopy (XPS) measurements were conducted using a Quantum 2000 instrument (ULVAC-PHI) with Al-Kα excitation (1486.6 eV) and a take-off angle of 30°. The area of X-ray irradiation was Φ = 100 μm, the pass energy was 23.50 eV and the step size was 0.05 eV. Si2p-XPS spectra were collected between 95 and 115 eV. The number of cumulative measurements was three. During the XPS measurement, a low-speed electron beam and an Ar ion beam were irradiated on the measured samples to neutralize their charges. All spectra were charge-compensated to C1s at 284.6 eV, which corresponds to hydrocarbons and a shoulder component, probably from oxidized hydrocarbons28 (link).
8
XPS Analysis of Plasma-Treated Polymer Surfaces
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The chemical composition of a polymer's surface changes upon plasma treatment. XPS was conducted using an XPS spectrometer (Quantum 2000, ULVAC-PHI, Japan) attached to an Al-Kα X-ray source. The X-ray irradiation area was ø 100 μm, and the take-off angle was 45°. During the XPS measurement, the sample was irradiated by a low-speed electron beam and an Ar ion beam to achieve charge neutralization. A narrow-scan XPS spectrum of C1s was recorded at 275–300 eV with a pass energy of 23.50 eV and a step size of 0.05 eV. Three measurements were performed for each PTFE sample before and after HAP treatment. The spectra were referenced to peaks indexed to –CF2– at 292.5 eV for as-received PTFE31,32 (link) and 291.8 eV for plasma-treated PTFE.33,34 (link)
9
Chemical Bonding Analysis of PTFE Surfaces
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XPS (Quantum2000, ULVAC-PHI, Japan) was applied to investigate the variations in the chemical bonding state of the pure-PTFE and GC-PTFE surfaces before and after HAP treatment. Additionally, it was used to investigate the chemical bonding state of peeled surface of Cu/pure-PTFE and Cu/GC-PTFE. The cumulative number, pass energy, and step size were 3, 25.00 eV, and 0.05 eV, respectively. The X-ray take-off angle was 45°, and surface charging was avoided using low-speed EB and low-speed Ar-ion beam during XPS measurement. The measured XPS data were analyzed using data analysis software (MultiPak V8.2C, 2007-9-04). As reported, the peak corresponding to the CF2 of PTFE was observed at 292.5 eV.25,26 (link) Therefore, the measured XPS data were calibrated using this reference positions.
10
Pd Nanoparticle Characterization Protocols
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The amount of Pd immobilized on the substrates was analyzed by ICP-AES (ICPE-9000, Shimadzu, Kyoto, Japan). The surfaces of the substrates were washed with aqua regia (HCl:HNO3 = 3:1) to dissolve the Pd nanoparticles. The surfaces of the irradiated samples were characterized by SEM-EDX (JSM-7001F, JEOL Ltd., Tokyo, Japan) and XPS (Quantum 2000, ULVAC-PHI, Kanagawa, Japan). Prior to the SEM observation, the surfaces of the resin plates were coated with Os (OPC60A, Filgen, Aichi, Japan). The surface chemical state was analyzed via XPS using an Al Kα X-ray source operating at 15 kV. A C1s level of 284.6 eV was used as an internal standard to correct for the peak drift. All high-resolution XPS peaks were fitted using the XPSPEAK41 software.
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