Three-Dimensional Nanoscale Imaging of Polymer Bulk-Heterojunction by Scanning Electrical Potential Microscopy and C<sub>60</sub><sup>+</sup> Cluster Ion Slicing

Yu, Bang-Ying; Lin, Wei–Chun; Huang, Jen-Hsien; Chu, Chih‐Wei; Lin, Yao; Kuo, Chung Yen; Lee, Szu-Hsian; Wong, Ken‐Tsung; Ho, Kuo–Chuan; Shyue, Jing‐Jong

doi:10.1021/ac901588t

Cited by 21 publications

(34 citation statements)

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“…Co‐sputtering with a 10 kV C 60 + and a 0.2 kV Ar + beam is known to preserve the chemical structure of the remaining surface for various organic/polymeric materials . Using the co‐sputtering beam as the ionization source, molecular D‐SIMS spectra were also acquired (Fig.…”

Section: Resultsmentioning

confidence: 99%

“…The apparatus is based on a PHI 5000 VersaProbe (ULVAC‐PHI, Chigasaki, Japan) scanning X‐ray microprobe system operated at a base pressure of <1 × 10 –7 Pa, which was achieved by evacuation using ion getter pumps. The Ar + ion source was operated at 0.2 kV and 300 nA (measured on an Au target) using a floating voltage of 500 V. A voltage setting of 0.2 kV has been previously found to preserve the chemical structure of the remaining surface for various organic/polymeric materials while yielding a more stable sputtering rate . The ray path contained a 1° bend to filter fast Ar atoms.…”

Section: Methodsmentioning

confidence: 99%

“…Throughout the study of these cluster ion sources, buckminsterfullerene (C 60 + ) has received significant attention since it became a commercially available product in 2003 . Using surface analysis techniques and C 60 + ion sputtering, biological/medical and organic electronic materials have been widely studied.…”

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confidence: 99%

“…This was feasible because the auxiliary Ar + beam could suppress the carbon deposition and/or remove graphitized materials through the removal of the top surface . To date, this co‐sputtering technique has only been used as a slicing tool that removes the outermost surface, while the newly exposed surface is analyzed using other means (namely, X‐ray photoelectron spectrometry and scanning probe microscopy). In previous studies, the sputtered materials were not analyzed, making it unclear how the auxiliary Ar + beam affected the mass distribution of secondary ions and whether the co‐sputtering technique could serve as an ionization source for the dynamic SIMS (D‐SIMS) analysis of organic materials.…”

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confidence: 99%

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Molecular dynamic‐secondary ion mass spectrometry (D‐SIMS) ionized by co‐sputtering with C₆₀⁺ and Ar⁺

You

Chang

Lin

et al. 2011

Rapid Comm Mass Spectrometry

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Dynamic secondary ion mass spectrometry (D-SIMS) analysis of poly(ethylene terephthalate) (PET) and poly(methyl methacrylate) (PMMA) was conducted using a quadrupole mass analyzer with various combinations of continuous C(60)(+) and Ar(+) ion sputtering. Individually, the Ar(+) beam failed to generate fragments above m/z 200, and the C(60)(+) beam generated molecular fragments of m/z ~1000. By combining the two beams, the auxiliary Ar(+) beam, which is proposed to suppress carbon deposition due to C(60)(+) bombardment and/or remove graphitized polymer, the sputtering range of the C(60)(+) beam is extended. Another advantage of this technique is that the high sputtering rate and associated high molecular ion intensity of the C(60)(+) beam generate adequate high-mass fragments that mask the damage from the Ar(+) beam. As a result, fragments at m/z ~900 can be clearly observed. As a depth-profiling tool, the single C(60)(+) beam cannot reach a steady state for either PET or PMMA at high ion fluence, and the intensity of the molecular fragments produced by the beam decreases with increasing C(60)(+) fluence. As a result, the single C(60)(+) beam is suitable for profiling surface layers with limited thickness. With C(60)(+)-Ar(+) co-sputtering, although the initial drop in intensity is more significant than with single C(60)(+) ionization because of the damage introduced by the auxiliary Ar(+), the intensity levels indicate that a more steady-state process can be achieved. In addition, the secondary ion intensity at high fluence is higher with co-sputtering. As a result, the sputtered depth is enhanced with co-sputtering and the technique is suitable for profiling thick layers. Furthermore, co-sputtering yields a smoother surface than single C(60)(+) sputtering.

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Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

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confidence: 99%

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confidence: 99%

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Molecular dynamic‐secondary ion mass spectrometry (D‐SIMS) ionized by co‐sputtering with C₆₀⁺ and Ar⁺

You

Chang

Lin

et al. 2011

Rapid Comm Mass Spectrometry

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“…By stacking the images acquired at different sputtering times as in the sputter‐and‐view scheme, the 3D composition was obtained. In previous studies, it has been shown that C 60 + cluster ion beams do not alter the remaining surface of P3HT:PCBM (poly(3‐hexylthiophene‐2,5‐diyl:[6,6]‐phenyl‐C61‐butyric acid methyl ester) blends significantly, and it has been confirmed that C 60 + sputtering can be used to profile organic solar cells and OLEDs . On the other hand, it is known that C 60 + leaves a small amount of residual amorphous carbon on the surface .…”

Section: Methodsmentioning

confidence: 95%

3D In Situ ToF‐SIMS Imaging of Perovskite Films under Controlled Humidity Environmental Conditions

Lin

Chang

Abbasi

et al. 2016

Adv Materials Inter

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Since CH3NH3PbI3 perovskites are discovered as a viable active material for next‐generation photovoltaic devices, their instability in humid environments is a constant challenge. Therefore, understanding the exact spatially resolved degradation process is a crucial need before being able to improve the stability and durability of these exceptional materials. In this work, it is demonstrated that the CH3NH3PbI3 perovskite will eventually degrade irreversibly at high humidity through a slow leaching and vaporization process of CH3NH2. Deuterium oxide (D2O) is used as a humidity source instead of H2O to distinguish the exogenous water diffusing into the perovskite from moisture embedded during sample fabrication. The degradation process of CH3NH3PbI3 perovskite is examined in situ by using time‐of‐flight secondary ion mass spectrometry (ToF‐SIMS) and an argon ion cluster beam for layer‐by‐layer in situ sputtering and then compared to their corresponding solar cell performances. 3D images are constructed from the layer‐by‐layer spatially resolved elemental distribution analysis and the D2O moisture penetration through the sample. It is observed that the H/D exchange on the organic methylammonium ion is the first indication for moisture uptake in a given volume element. The intermediate products of interaction with moisture are also analyzed by ToF‐SIMS and X‐ray photoelectron spectroscopy. The initial products of this deuterium exchange reaction are CH3NH2D, CH3NHD2, and CH3ND3. In the following, the D2O molecule stepwise replaces the methylammonium, which leads to evaporation of the organic molecules and eventually to erosion of the perovskite along with drastic changes in morphology, crystallography, and photovoltaic performance.

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Modeling dynamic cluster SIMS experiments

Garrison

Schiffer

Kennedy

et al. 2012

Surface & Interface Analysis

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The underpinnings of two SIMS experimental findings are elucidated using the power of molecular dynamics to provide insight at the molecular level. First, the improvement of depth resolution for C 60 bombardment of Irganox delta layers and polymer layers using sample rotation is explained by molecular dynamics simulations of the repetitive bombardment of Ag surfaces with 20 keV Au 3 , C 60 , and Ar 872 at grazing angles of incidence with both single azimuthal angle and random azimuthal angles. Single azimuthal angle simulations at grazing angles show the formation of trenches and valleys parallel to the cluster beam form and are elongated with increasing incident angle. Cluster bombardment simulations with random azimuthal angles mimic sample rotation and show that under grazing angles of incidence, the surface is smoother because of the random impact angles preventing trench and valley formation. Second, depth profiles using C 60 at a 70 angle of incidence have been improved by co-bombardment with low energy Ar ions emitted at 33 from the C 60 beam and at a 45 incident angle from the surface. Molecular dynamics simulations of the bombardment of solid benzene with low energy Ar and 15 keV C 60 were used to show the depth of damage created during bombardment. For low kinetic energy (<200 eV), the damage caused by the Ar atom is in the same region as for the C 60 cluster. It is believed that for the experimental conditions used during co-bombardment, the Ar beam is breaking up the ridges created by the grazing C 60 beam.

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Three-Dimensional Nanoscale Imaging of Polymer Bulk-Heterojunction by Scanning Electrical Potential Microscopy and C₆₀⁺ Cluster Ion Slicing

Cited by 21 publications

References 35 publications

Molecular dynamic‐secondary ion mass spectrometry (D‐SIMS) ionized by co‐sputtering with C₆₀⁺ and Ar⁺

Molecular dynamic‐secondary ion mass spectrometry (D‐SIMS) ionized by co‐sputtering with C₆₀⁺ and Ar⁺

3D In Situ ToF‐SIMS Imaging of Perovskite Films under Controlled Humidity Environmental Conditions

Modeling dynamic cluster SIMS experiments

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Three-Dimensional Nanoscale Imaging of Polymer Bulk-Heterojunction by Scanning Electrical Potential Microscopy and C60+ Cluster Ion Slicing

Cited by 21 publications

References 35 publications

Molecular dynamic‐secondary ion mass spectrometry (D‐SIMS) ionized by co‐sputtering with C60+ and Ar+

Molecular dynamic‐secondary ion mass spectrometry (D‐SIMS) ionized by co‐sputtering with C60+ and Ar+

3D In Situ ToF‐SIMS Imaging of Perovskite Films under Controlled Humidity Environmental Conditions

Modeling dynamic cluster SIMS experiments

Contact Info

Product

Resources

About

Three-Dimensional Nanoscale Imaging of Polymer Bulk-Heterojunction by Scanning Electrical Potential Microscopy and C₆₀⁺ Cluster Ion Slicing

Molecular dynamic‐secondary ion mass spectrometry (D‐SIMS) ionized by co‐sputtering with C₆₀⁺ and Ar⁺

Molecular dynamic‐secondary ion mass spectrometry (D‐SIMS) ionized by co‐sputtering with C₆₀⁺ and Ar⁺