Depth profiling of thin plasma-polymerized amine films using GDOES in an Ar-O2 plasma

Kovač, Janez; Ekar, Jernej; Čekada, Miha; Zajı́čková, Lenka; Nečas, David; Blahová, Lucie; Wang, Jiang Yong; Mozetič, Miran

doi:10.1016/j.apsusc.2021.152292

Cited by 8 publications

(5 citation statements)

References 36 publications

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“…The morphological features of polyaniline films electrodeposited with or without surfactant on FTO planar electrodes were first studied using SEM microscopy. SEM pictures show that the PANI film electrodeposited in a surfactant-free HCl solution has a sponge-like morphology (Figure 4A) similar to the one generally observed (Kovac et al, 2022). PANI/HCl + SDS (Figure 4B) and PANI/HCl + CTAB (Figure 4D) films have a similar but even more spongy structure while the structure of PANI/HCl + Tritonx100 (Figure 4C) is different, possibly due to the larger size of the surfactant or the use of a non-ionic surfactant, which leads to the absence of repulsive interactions inside the film (Figure 4).…”

Section: Morphological Features Of the Electrodeposited Polyaniline F...supporting

confidence: 69%

Influence of surfactant on conductivity, capacitance and doping of electrodeposited polyaniline films

Kayishaer,

Magnenet,

Pavel

et al. 2024

Front. Mater.

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The electrodeposition of polyaniline films is usually carried out in acid solutions such as hydrochloric acid, perchloric acid or sulfuric acid, and more rarely in organic acids such as camphorsulfonic acid (CSA). In this study, the impact of the presence of a surfactant in the electrolytic solution based on hydrochloric acid or CSA was evaluated by successively using anionic (sodium dodecyl sulfate, SDS), cationic (cetyltrimethylammonium bromide, CTAB), and non-ionic (Tritonx100) surfactants. Whatever the surfactant and the acid used, the electrochemical oxidation of aniline has successfully led to the formation of a thick polyaniline (PANI) film through a quasi-reversible reaction controlled by the diffusion of aniline monomers. The nature of the surfactant was shown to affect physico-chemical properties of the film, in particular its morphological features (morphology, thickness, roughness), electrochemical activity, specific capacitance, and conductivity. For example, PANI films containing SDS had a spongy morphology when PANI films containing Tritonx100 had a more fibrous and compact structure. Glow Discharge Optical Emission Spectroscopy (GDOES) experiments also highlighted differences depending on the acid used since chloride anions, from HCl, were present only on the top surface of the PANI films when camphorsulfonate anions were present everywhere throughout the polymer film, which impacts the doping process and electrochemical activity of the films. Moreover, the specific capacitance of the PANI/CSA films is higher and more sensitive to current density variation than the one of PANI/HCl films. Finally, electrochemical impedance experiments evidenced that the conductivity of PANI films electrodeposited from CSA solutions was much higher than the one of PANI films prepared from HCl solutions, and highly dependent on the nature of the surfactant, the most conductive films being obtained in the presence of SDS and Tritonx100. Therefore, the originality of this work comes from the possibility of modulating the conductivity, capacitance and electroactivity of electrodeposited polyaniline films using surfactants of different polarity, and from the determination of the distribution of ions in the films using the GDOES technique, which is rarely used to characterise organic films.

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Section: Morphological Features Of the Electrodeposited Polyaniline F...supporting

confidence: 69%

Influence of surfactant on conductivity, capacitance and doping of electrodeposited polyaniline films

Kayishaer,

Magnenet,

Pavel

et al. 2024

Front. Mater.

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“…% of oxygen may be beneficial. 30 Specifically, oxygen will add to the etching efficiency through chemical etching (sometimes referred to as reactive ion etching). Other gases may be added to the noble gas for a particular application, but the addition of reactive gases will often cause unpredictable changes in plasma parameters, particularly, the electron temperature and energy; radiation from the sputtered atoms depends on these parameters.…”

Section: B Plasma Gases Pressures and Flowsmentioning

confidence: 99%

“…This is only a rough estimation because the forward power is spent on other reactions, including the surface neutralization of Ar ions on the anode. A valuable estimation of the surface temperature upon probing samples by GDOES was reported by Kovač et al 30 Excessive heating of samples upon probing by GDOES is avoided using pulsed HF generators. The heat is dissipated on the sample's surface during the pulse of gaseous discharge and cooled during the off-time.…”

Section: E Thermal Effectsmentioning

confidence: 99%

Fundamentals of thin film depth profiling by glow discharge optical emission spectroscopy

Vesel

Zaplotnik

Primc

et al. 2023

Journal of Vacuum Science &Amp; Technology A

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Glow discharge optical emission spectroscopy (GDOES) is a useful technique for qualitative plasma characterization. It also enables depth profiling of solid materials upon exposure of samples to energetic positively charged ions from gaseous plasma, providing specifics of both surface- and gas-phase collision phenomena that are considered. The early stages of developing GDOES useful for the determination of surface composition and depth profiling of solid materials are reviewed and analyzed, stressing the contribution of early authors. The advantages as well as drawbacks of the GDOES technique are presented and discussed. The recent applications of this technique for depth profiling of various materials are presented, and the directions for constructing a laboratory-scale device are provided.

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“…Ion sputtering is the main process taking place during an analysis based on secondary ion mass spectrometry (SIMS) . It is also an essential process for depth profiling, combined with X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). − All three methods employ ion guns for sputtering, although the sputtering process itself is also present in the case of glow-discharge optical emission spectroscopy (GDOES) or glow-discharge mass spectrometry (GDMS). ,− The main difference is the characteristic of the GDOES or GDMS processes, as ions are intrinsic to the plasma that flows toward the cathode, causing its surface to be sputtered away. , These methods are used in many areas of research, for example, during the analysis of oxide layers, while studying corrosion properties, polymer films, mono- and multilayers, biomaterials, microelectronics, , power-storage materials, solar cells, , and catalysts . However, regardless of the exact process used for the ion sputtering, the ion beam generated by the ion gun or the plasma flow, some damage caused by the ion bombardment is always present. − The accumulation of damage is observed as surface roughening, which is most commonly determined with atomic force microscopy (AFM). , This technique is especially suitable for the characterization of nanostructures formed on the surface since it is optimized to achieve molecular and atomic resolutions. − However, AFM can also be used to study many other topographical characteristics of the sample, its conductivity at the nano level, and different forces using its spectroscopy mode. − …”

Section: Introductionmentioning

confidence: 99%

“… 2 − 4 All three methods employ ion guns for sputtering, although the sputtering process itself is also present in the case of glow-discharge optical emission spectroscopy (GDOES) or glow-discharge mass spectrometry (GDMS). 3 , 5 − 7 The main difference is the characteristic of the GDOES or GDMS processes, as ions are intrinsic to the plasma that flows toward the cathode, causing its surface to be sputtered away. 6 , 8 These methods are used in many areas of research, for example, during the analysis of oxide layers, 9 while studying corrosion properties, 10 polymer films, 11 mono- and multilayers, 12 biomaterials, 13 microelectronics, 14 , 15 power-storage materials, 16 solar cells, 17 , 18 and catalysts.…”

Section: Introductionmentioning

confidence: 99%

AFM Study of Roughness Development during ToF-SIMS Depth Profiling of Multilayers with a Cs⁺ Ion Beam in a H₂ Atmosphere

Ekar

Kovač

2022

Langmuir

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The influence of H2 flooding on the development of surface roughness during time-of-flight secondary ion mass spectrometry (ToF-SIMS) depth profiling was studied to evaluate the different aspects of a H2 atmosphere in comparison to an ultrahigh vacuum (UHV) environment. Multilayer samples, consisting of different combinations of metal, metal oxide, and alloy layers of different elements, were bombarded with 1 and 2 keV Cs+ ion beams in UHV and a H2 atmosphere of 7 × 10–7 mbar. The surface roughness S a was measured with atomic force microscopy (AFM) on the initial surface and in the craters formed while sputtering, either in the middle of the layers or at the interfaces. We found that the roughness after Cs+ sputtering depends on the chemical composition/structure of the individual layers, and it increases with the sputtering depth. However, the increase in the roughness was, in specific cases, approximately a few tens of percent lower when sputtering in the H2 atmosphere compared to the UHV. In the other cases, the average surface roughness was generally still lower when H2 flooding was applied, but the differences were statistically insignificant. Additionally, we observed that for the initially rough surfaces with an S a of about 5 nm, sputtering with the 1 keV Cs+ beam might have a smoothing effect, thereby reducing the initial roughness. Our observations also indicate that Cs+ sputtering with ion energies of 1 and 2 keV has a similar effect on roughness development, except for the cases with initially very smooth samples. The results show the beneficial effect of H2 flooding on surface roughness development during the ToF-SIMS depth profiling in addition to a reduction of the matrix effect and an improved identification of thin layers.

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Depth profiling of thin plasma-polymerized amine films using GDOES in an Ar-O2 plasma

Cited by 8 publications

References 36 publications

Influence of surfactant on conductivity, capacitance and doping of electrodeposited polyaniline films

Influence of surfactant on conductivity, capacitance and doping of electrodeposited polyaniline films

Fundamentals of thin film depth profiling by glow discharge optical emission spectroscopy

AFM Study of Roughness Development during ToF-SIMS Depth Profiling of Multilayers with a Cs⁺ Ion Beam in a H₂ Atmosphere

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Depth profiling of thin plasma-polymerized amine films using GDOES in an Ar-O2 plasma

Cited by 8 publications

References 36 publications

Influence of surfactant on conductivity, capacitance and doping of electrodeposited polyaniline films

Influence of surfactant on conductivity, capacitance and doping of electrodeposited polyaniline films

Fundamentals of thin film depth profiling by glow discharge optical emission spectroscopy

AFM Study of Roughness Development during ToF-SIMS Depth Profiling of Multilayers with a Cs+ Ion Beam in a H2 Atmosphere

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AFM Study of Roughness Development during ToF-SIMS Depth Profiling of Multilayers with a Cs⁺ Ion Beam in a H₂ Atmosphere