Faculty Profiles - SAITO, Nagahiro

Papers - SAITO, Nagahiro

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Principle in imaging contrast in scanning electron microscopy for binary microstructures composed of organosilane self-assembled monolayers

Saito N., Wu Y., Hayashi K., Sugimura H., Takai O.

Journal of Physical Chemistry B Vol. 107 ( 3 ) page： 664 - 667 2003.1

Language：English Publishing type：Research paper (scientific journal) Publisher：Journal of Physical Chemistry B

Field-emission electron microscopy (FE-SEM) was applied to observe coplanar microstructures composed of two different types of organosilane self-assembled monolayers (SAMs). These binary microstructures were prepared on silicon substrates covered with native oxide by a lithographic technique. Four types of organosilane precursors, they are n-octadecyltrimethoxysilane (ODS), heptadecafluoro-1,1,2,2-tetrahydro-decyl-1-trimethoxysilane (a type of fluoroalkylsilane, FAS), n-(6-aminohexyl)aminopropyltrimethoxysilane (AHAPS), and 4-(chloromethyl)phenyltrimethoxysilane (CMPhS), were used in this study. Micropatterns composed of the SAMs were clearly imaged by FE-SEM at low acceleration voltages, around 0.6 kV. The brightness order of the SAMs in FE-SEM was ODS > AHAPS > CMPhS > FAS. Through ab initio molecular orbital calculations, the origin of this FE-SEM contrast was ascribed to the electron affinity between the SAMs, which governed the FE-SEM image contrast. It has been successfully demonstrated that FE-SEM could provide us chemical information on organic films with a monomolecular thickness on a solid support.

DOI： 10.1021/jp021362r

Imaging micropatterned organosilane self-assembled monolayers on silicon by means of scanning electron microscopy and Kelvin probe force microscopy

Wu Y., Hayashi K., Saito N., Sugimura H., Takai O.

Surface and Interface Analysis Vol. 35 ( 1 ) page： 94 - 98 2003.1

Language：English Publishing type：Research paper (scientific journal) Publisher：Surface and Interface Analysis

Field-emission scanning electron microscopy (FE-SEM) and surface potentiometry based on scanning probe microscopy, i.e. Kelvin probe force microscopy (KFM), have been applied to study microstructures consisting of organosilane self-assembled monolayers (SAMs) terminated with -CH3 or -CF3 groups. Onto cleaned Si substrates covered with a thin oxide layer of 2 nm thick, SAMs were formed by chemical vapour deposition using n-octadecyltrimethoxysilane (CH3(CH2)17Si(OCH3)3, ODS) or fluoroalkylsilane (CF3(CF2)7(CH2)2Si (OCH3)3, FAS) as a precursor. Through a photolithographic technique employing vacuum ultraviolet light at 172 nm, microstructures composed of ODS, FAS or both were fabricated. Micropatterns of the SAMs on SiO2/Si substrates were clearly imaged by FE-SEM at an acceleration voltage of the electron beam below 1 kV, but image contrasts became faint with an increase in the acceleration voltage. At a voltage of 5 kV there was almost no detectable contrast. An FE-SEM image of the ODS-FAS microstructure acquired at an acceleration voltage of 0.8 kV clearly demonstrated that the region covered with ODS was brighter and thus, emitted secondary electrons more efficiently than the region covered with FAS. Furthermore, as indicated in a KFM image, the region covered with FAS had a surface potential ∼180 mV lower than that of the region covered with ODS. The origin of these image contrasts between ODS- and FAS-SAMs was the large difference in electronic states between ODS and FAS owing to the electron negativity of fluorine atoms.

DOI： 10.1002/sia.1501

Scanning probe surface modification: Chemical conversion of terminal functional groups on organosilane self-assembled monolayers

Sugimura, H; Saito, N; Hayashi, K; Maeda, N; Takai, O

SCANNING TUNNELING MICROSCOPY/SPECTROSCOPY AND RELATED TECHNIQUES Vol. 696 page： 150 - 157 2003

Alkyl self-assembled monolayer prepared on hydrogen-terminated Si(111) through reduced pressure chemical vapor deposition: Chemical resistivities in HF and NH<inf>4</inf>F solutions

Saito N., Youda S., Hayashi K., Sugimura H., Takai O.

Chemistry Letters ( 12 ) page： 1194 - 1195 2002.12

Regulation of the surface potential of silicon substrates in micrometer scale with organosilane self-assembled monolayers

Hayashi K., Saito N., Sugimura H., Takai O., Nakagiri N.

Langmuir Vol. 18 ( 20 ) page： 7469 - 7472 2002.10

Language：English Publishing type：Research paper (scientific journal) Publisher：Langmuir

Microstructures composed of two types of organosilane self-assembled monolayers (SAMs) terminated with different functional groups have been constructed on silicon substrates covered with native oxide. Surface potential images of these microstructures were acquired by Kelvin-probe force microscopy (KFM). By chemical vapor deposition (CVD), the SAMs were fabricated from n-octadecyltrimethoxysilane (ODS) [H3C(CH2)17Si(OCH3)3], fluoroalkylsilane (FAS), that is, heptadecafluoro-1,1,2,2-tetrahydro-decyl-1-trimethoxysilane [F3C(CF2)7(CH2)2Si(OCH 3)3], and n-(6-aminohexyl)aminopropyltrimethoxysilane (AHAPS) [H2N(CH2)6NH(CH2)3Si(OCH 3)3]. Through a photolithographic technique, binary microstructures consisting of ODS/FAS and ODS/AHAPS were constructed. A surface potential contrast of the two SAMs in each of the binary microstructures was clearly detected by KFM. The surface potential of the FAS-terminated region was ca. 180 mV lower than that of the ODS-terminated region, while the potential of the AHAPS-terminated region was ca. 50 Mv higher. These results agree with surface potentials of the SAMs predicted from dipole moments of the corresponding precursor organosilane molecules as estimated by ab initio molecular orbital (MO) calculations. Moreover, by applying the surface potential contrasts experimentally acquired by KFM to surface potential contrast occupied area with single molecule curves theoretically derived by MO calculations, packing densities of the SAMs prepared by CVD were confirmed ta be smaller than those of Langmuir-Blodgett monolayers.

DOI： 10.1021/la011707h

The decomposition mechanism of p-chloromethylphenyltrimethoxysiloxane self-assembled monolayers on vacuum ultraviolet irradiation

Saito N., Hayashi K., Sugimura H., Takai O.

Journal of Materials Chemistry Vol. 12 ( 9 ) page： 2684 - 2687 2002.9

Language：English Publishing type：Research paper (scientific journal) Publisher：Journal of Materials Chemistry

The decomposition mechanism of p-chloromethylphenyltrimethoxysiloxane (CMPS) self-assembled monolayers (SAMs) due to vacuum ultraviolet (VUV) irradiation at a wavelength of 172 nm has been studied based on water repellency, X-ray photoelectron spectroscopy (XPS) and Kelvin probe force microscopy (KPFM). The CMPS-SAMs were prepared through chemical vapor deposition at 100°C. The water contact angle increased dramatically within the first 30 min, reaching a plateau at this point. The saturated water contact angle was 76°. Next, the CMPS-SAMs were irradiated at under 10 Pa from 0 to 30 min. The CMPS-SAMs irradiated for 15 and 30 min were covered with carboxylated hydrocarbon fragments and silanol groups, respectively. KPFM measurements for micro-patterned SAMs, i.e. CMPS/CO2H and CMPS/SiOH, showed that the surface potential of the carboxylated and silanol regions were -16 and +19 mV vs. CMPS-SAM, respectively. The former negative surface potential difference originated in the electronegativity of the CO2H fragments. These results provide us with a route to prepare an organic template for various fields such as bio-sensors, chemical sensors and electrolytes.

DOI： 10.1039/b203643f

Surface potential contrasts between silicon surfaces covered and uncovered with an organosilane self-assembled monolayer

Hayashi K., Saito N., Sugimura H., Takai O., Nakagiri N.

Ultramicroscopy Vol. 91 ( 1-4 ) page： 151 - 156 2002.8

Language：English Publishing type：Research paper (scientific journal) Publisher：Ultramicroscopy

Surface potentials of Si substrates covered with a organosilane self-assembled monolayers (SAMs) were measured with reference to the substrate uncovered with the SAM using Kelvin probe force microscopy. Based on a photolithographic technique, the reference surface was prepared in a micrometer scale on each of the samples. SAMs were prepared from n-octadecyltrimethoxysilane [ODS: CH3(CH2)17Si(OCH3)3], 3,3,3-trifluoropropyltrimethoxysilane [FAS3: CF3(CH2)2Si(OCH3)3], heptadecafluoro-1,1,2,2-tetrahydro-decyl-1-trimethoxysilane [FAS17: CF3(CF2)7(CH2)2Si (OCH3)3] or n-(6-aminohexyl) aminopropyltrimethoxysilane [AHAPS: H2N(CH2)6NH(CH2)3Si (OCH3)3) by chemical vapor deposition. Potentials of the surfaces covered with ODS-, FAS3- and FAS17-SAMs became more negative than the uncovered Si substrate, while the surface covered with AHAPS-SAM showed a more positive surface potential than the reference. The potential contrasts of these SAMs to the reference were -25, -170, -225 and +50mV for ODS-, FAS3-, FAS17- and AHAPS-SAMs, respectively. These results almost agreed with potentials expected from the dipole moments of the corresponding precursor molecules estimated by ab initio molecular orbital calculation, except for FAS3-SAM. Despite FAS3 molecule having a larger dipole moment than FAS17 molecule, the surface potential contrast of FAS3-SAM was smaller than that of FAS17-SAM, since surface coverage of FAS3-SAM was relatively incomplete compared with the other SAMs. © 2002 Elsevier Science B.V. All rights reserved.

DOI： 10.1016/S0304-3991(02)00094-3

Surface potential images of self-assembled monolayers patterned by organosilanes: Ab initio molecular orbital calculations

Saito N., Hayashi K., Sugimura H., Takai O., Nakagiri N.

Surface and Interface Analysis Vol. 34 ( 1 ) page： 601 - 605 2002.8

Language：English Publishing type：Research paper (scientific journal) Publisher：Surface and Interface Analysis

Self-assembled monolayers (SAMs) with different function terminal groups were prepared on substrates of n-type silicon by chemical vapour deposition (CVD) from n-octadecyltrimethoxysilane (ODS: H3C(CH2)17Si(OCH3)3), heptadecafluoro-1,1,2,2-tetrahydro-decyl-1-trimethoxysilane (FAS: F3C(CF2)7 (CH2)2Si(OCH3)3), n-(6-aminohexyl)aminopropyltrimethoxysilane (AHAPS: H2N(CH2)6NH(CH2)3 Si(OCH3)3) and 4-(chloromethyl)phenyltrimethoxysilane [CMPS: H2ClC(C6H4)Si(OCH3)3]. The sample surfaces covered with ODS-SAM were irradiated under a reduced pressure of 10 Pa with vacuum ultraviolet (VUV) light through a photomask. Then, the irradiated areas with the ODS-SAM removed were covered with another SAM by CVD. Surface potential images of the patterned areas were measured by Kelvin probe force microscopy (KPFM) and explained by ab initio molecular orbital (MO) calculations. The KPFM measurements showed that the surface potential contrasts of the FAS-, AHAPS- and CMPS-SAMs against the ODS-SAM were about -170, +50 and -30 mV, respectively. The surface potentials as a function of area occupied by a molecule were predicted using the respective dipole moments perpendicular to substrates, which were obtained by the ab initio MO calculations. The predicted surface potentials of the FAS-, CMPS- and AHAPS-SAMs approximately agreed with the measured values at areas of about 1.5, 1.6 and 0.6 nm2 per molecule. The ab initio MO calculations also showed differences in surface potentials appearing due to the differences in Fermi levels of the respective SAMs.

DOI： 10.1002/sia.1369

Surface potential microscopy for organized molecular systems

Sugimura H., Hayashi K., Saito N., Nakagiri N., Takai O.

Applied Surface Science Vol. 188 ( 3-4 ) page： 403 - 410 2002.3

Language：English Publishing type：Research paper (scientific journal) Publisher：Applied Surface Science

Surface potentials of organosilane self-assembled monolayers (SAMs) formed on silicon substrates were measured using Kelvin-probe force microscopy (KFM) employing a SAM formed from n-octadecyltrimethoxysilane [ODS: CH 3 (CH 2 ) 17 Si(OCH 3 ) 3 ] as a reference. The reference ODS surface was prepared in a micrometer scale on each of the samples based on a photolithographic technique using vacuum ultra-violet light at 172 nm. Another SAM was prepared on the same sample surface from heptadecafluoro-1,1,2,2-tetrahydro-decyl-1-trimethoxysilane (fluoroalkylsilane with 17 fluorine atoms, FAS17), 3,3,3-trifluoropropyltrimethoxysilane (fluoroalkylsilane with three fluorine atoms, FAS3), n-(6-aminohexyl)aminopropyltrimethoxysilane (AHAPS) or (chloromethyl)phenyltrimethoxysilane (CMPS). Potentials of the surfaces covered with FAS17-SAM, FAS3-SAM and CMPS-SAM became more negative than ODS-SAM, while the surface covered with AHAPS-SAM showed a more positive surface potential than the reference. The acquired potential contrasts of the regions covered with FAS17, FAS3, AHAPS and CMPS with reference to ODS were -180, -150, +50 and -30 mV, respectively. These results almost agreed with potentials expected from the dipole moments of the corresponding precursor molecules estimated by ab initio molecular orbital calculation. © 2002 Elsevier Science B.V. All rights reserved.

DOI： 10.1016/S0169-4332(01)00958-8

Carbon Nitrides

Takai O., Lee K., Ohta R., Saito N.

Seimitsu Kogaku Kaishi/Journal of the Japan Society for Precision Engineering Vol. 68 ( 12 ) page： 1526 - 1529 2002

Surface potentials of patterned organosilane self-assembled monolayers acquired by Kelvin probe force microscopy and ab initio molecular calculation

Saito N., Hayashi K., Sugimura H., Takai O., Nakagiri N.

Chemical Physics Letters Vol. 349 ( 3-4 ) page： 172 - 177 2001.11

Language：English Publishing type：Research paper (scientific journal) Publisher：Chemical Physics Letters

This study aimed experimentally and theoretically to reveal the surface potentials of organosilane self-assembled monolayers (SAMs) using Kelvin probe force microscopy (KPFM) and ab initio molecular orbital (MO) calculations, and to distinguish among the surface domains of the SAMs. We prepared the patterned SAMs of n-octadecyltrimethoxysilane [ODS: H3C(CH2)17Si(OCH3)3], heptadecafluoro-1,1,2,2-tetrahydro-decyl-1-trimethoxysilane [FAS: F3C(CF2)7(CH2) 2Si(OCH3)3] and n-(6-aminohexyl)aminopropyltrimethoxysilane [AHAPS: H2N(CH2)6NH(CH2) 3Si(OCH3)3] by chemical vapor deposition (CVD). The surface potentials for FAS-SAM and AHAPS-SAM vs. ODS-SAM in the atmosphere were -170 and +50 mV, respectively. The experimental surface potentials agreed with the calculated ones at the surface area occupied by a molecule of 1.1-1.5nm2molecule-1. © 2001 Elsevier Science B.V.

DOI： 10.1016/S0009-2614(01)01097-1

Kelvin probe force microscopy images of microstructured organosilane self-assembled monolayers

Sugimura H., Hayashi K., Saito N., Takai O., Nakagiri N.

Japanese Journal of Applied Physics, Part 1: Regular Papers and Short Notes and Review Papers Vol. 40 ( 6 B ) page： 4373 - 4377 2001.6

Language：English Publishing type：Research paper (scientific journal) Publisher：Japanese Journal of Applied Physics, Part 1: Regular Papers and Short Notes and Review Papers

A difference in surface potentials between organosilane self-assembled monolayers (SAMs) was measured by means of Kelvin probe force microscopy (KFM). The SAMs were deposited on a single Si substrate from alkylsilane, that is, octadecyltrimethoxysilane (ODS)[H3C(CH2)17Si(OCH3) 3], and fluoroalkylsilane (FAS), that is, heptadecafluoro-1,1,2,2-tetrahydrodecyl-1-trimethoxysilane [F3C(CF2)7(CH2)2 Si(OCH3)3]. The locations of these SAMs on the substrate were defined by means of a photolithographic technique. The regions terminated with ODS and FAS were clearly distinguished by KFM with the surface potential difference between the ODS- and FAS-terminated surfaces under optimized imaging conditions. The surface potential of the FAS-terminated region was 170 ∼ 180 mV lower than the potential of the ODS-terminated surface. The origin of such a low surface potential of FAS-SAM was ascribed to the larger dipole moment of the FAS molecule induced by the electron negativity of F atoms as estimated from a molecular orbital calculation.

DOI： 10.1143/jjap.40.4373

Surface potential images of microstructured organosilane self-assembled monolayers acquired by Kelvin probe force microscopy

Sugimura, H; Hayashi, K; Saito, N; Takai, O; Nakagiri, N

JAPANESE JOURNAL OF APPLIED PHYSICS PART 2-LETTERS & EXPRESS LETTERS Vol. 40 ( 2B ) page： L174 - L176 2001.2

Catalytic effects of copper on dibenzo-p-dioxin and polychlorinated dibenzo-p-dioxin generations using ab initio molecular orbital method

Hirota M., Kato J., Saito N., Fuwa A.

Toxicological and Environmental Chemistry Vol. 81 ( 3-4 ) page： 133 - 146 2001

Language：English Publishing type：Research paper (scientific journal) Publisher：Toxicological and Environmental Chemistry

The roles played by copper in dibenzo-p-dioxin formation from the precursor phenol have been investigated using ab initio molecular orbital calculation, and the following catalytic roles of copper has been identified: (i) stabilization of the total energy owing to the absorption of phenol, (ii) reduction of oxygen-hydrogen bond strength in phenol, and (iii) reduction of steric effect of hydrogen atom in pre-dioxin. The catalytic effect of copper has been shown in terms of the smaller apparent activation energy. In the case of polychlorinated dibenzo-p-dioxins generation from precursor polychlorinated phenols, the catalytic roles (i), i.e., the stabilization of the total energy of precursor, would become even stronger. On the other hand, the catalytic roles (ii) and (iii) are unchangeable regardless of the existence of substituted chlorine atom.

DOI： 10.1080/02772240109359026

Behavior of Cu-In-Te electrodeposition from acid solution

Ishizaki T., Saito N., Yata D., Fuwa A.

Proceedings of the Second International Conference on Processing Materials for Properties page： 281 - 284 2000.12

Language：English Publishing type：Research paper (scientific journal) Publisher：Proceedings of the Second International Conference on Processing Materials for Properties

Ternary compound-semiconductor, CuInTe2, film was deposited cathodically under potentiostatic conditions on titanium substrate from aqueous solution containing CuCl2, InCl3, TeO2 and HCl in this study. The deposition parameters such as electrolytic solution composition, potential and temperature were optimized for electrodeposition of CuInTe2. Structural characterization of the deposited film was also carried out using XRD and SEM. Electrodeposited films were prepared and analyzed for their chemical composition using ICP. The ICP analyses showed that the stoichiometry of the films could be controlled by (1) the deposition potential and/or by (2) the electrolytic bath composition.

Preparation of YSZ thin films by RF plasma-enhanced metal organic chemical vapor depodition

Nishimura T., Ichikawa T., Saito N., Fuwa A.

Proceedings of the Second International Conference on Processing Materials for Properties page： 267 - 270 2000.12

Language：English Publishing type：Research paper (scientific journal) Publisher：Proceedings of the Second International Conference on Processing Materials for Properties

Yttria-stabilized zirconia (YSZ) has high potential to be used as solid-oxide fuel cell (SOFC) electrolyte. However, the high efficiency of SOFC has not been yet achieved due to the high internal resistance of bulk electrolyte. The resistance becomes lower with the decrease in the electrolyte thickness. Thus, the decrease in electrolyte thickness leads to lower internal resistance. The aim of this study is as follows: (a) to prepare the thin films of YSZ by inductively-coupled RF plasma-enhanced metal organic chemical vapor deposition (PEMOCVD) process using Zr(t-OC4H9)4, Y(DPM)3 and oxygen, and (b) to reveal the relationship between the structural characterizations and the process parameters.

The roles of metallic compounds on dioxins generation-decomposition behavior from thermodynamics and quantum chemistry

Saito N., Hirota M., Ishizaki T., Fuwa A.

Proceedings of the Second International Conference on Processing Materials for Properties page： 727 - 732 2000.12

Language：English Publishing type：Research paper (scientific journal) Publisher：Proceedings of the Second International Conference on Processing Materials for Properties

Owing to their extremely high toxicity in the environment, the dioxins have been attracting social, technical and scientific attention in recent years. The authors theoretically had predicted the thermodynamics properties of all the dioxins via quantum chemistry and statistical thermodynamics and elucidated the generation-decomposition behavior of dioxins in the equilibrium calculation of C-H-O-Cl system. In actual combustion processes, it is said that metallic compounds have much influence on the dioxins behavior. The aim of this study is to reveal the roles of metallic compounds the generation-decomposition behavior of dioxins is revealed from the viewpoints of quantum chemistry. Especially, the catalytic effect of copper has been investigated for the reaction, 2HCl(g)→H2(g)+Cl2(g) and for the etherification reaction from precursors, which is Phenol(g) here, to dioxins. The catalytic role of Cu is shown to have much influence on the generation -decomposition of dioxins.

Kinetics of SiHCl<inf>3</inf> and SiCl<inf>4</inf> evolution in Si(s)-HCl(g) system simulated by ab-initio MO

Saito N., Ishizaki T., Fuwa A.

Materials Transactions, JIM Vol. 41 ( 3 ) page： 383 - 392 2000.3

Language：English Publishing type：Research paper (scientific journal) Publisher：Materials Transactions, JIM

A reaction model for a HCl(g)-Si(s) system is proposed in this study as follows: first, SiCl2(g) and H2(g) are produced by a heterogeneous surface reaction, and then SiHCl3(g) and SiH2Cl2(g) are produced by the homogeneous reaction between SiCl2(g) and HCl(g) and between SiCl2(g) and H2(g), respectively; finally, SiCl4(g) and SiHCl3(g) are produced by the homogeneous reaction between SiHCl3(g) and HCl(g) and between SiH2Cl2(g) and HCl(g), respectively. The mechanism in the first heterogeneous surface reaction step has been studied extensively in the past. However, the detail of the subsequent homogeneous reactions has not yet been understood. It is important to get information of the chemical kinetics of the reactions derived from the reaction intermediate of SiCl2(g) in the SiCl2(g)-HCl(g)-H2(g) system, so the most plausible elementary reactions of reversible unimolecular fission and chain reaction are proposed here. The structures of the molecules formed in these reactions are optimized using the minimization principle of energy calculated by ab-initio molecular orbital method and also their rate constants are calculated by conventional transition state theory. Using these rate constants, the ordinary differential equations are solved on mass balance, and the time dependent concentration profile of respective chemical species and the prior reaction paths are discussed in this study.

DOI： 10.2320/matertrans1989.41.383

Prediction for thermodynamic function of dioxins for gas phase using semi-empirical molecular orbital method with PM3 Hamiltonian

Saito N., Fuwa A.

Chemosphere Vol. 40 ( 2 ) page： 131 - 145 2000.1

Language：English Publishing type：Research paper (scientific journal) Publisher：Chemosphere

In this investigation, respective thermodynamic parameters of heats of formation, standard entropy and specific heat capacity at constant pressure for PCDDs, PCDFs, Co-PCB and PCBs as well as polychlorinated-benzenes and poly-chlorinated-phenols have been evaluated by quantum chemical calculation using a semi-empirical molecular orbital method with the PM3 Hamiltonian and statistical thermodynamic correlation.

DOI： 10.1016/S0045-6535(99)00215-5

Gas phase equilibria for dibenzo-p-dioxin, dibenzo-p-furan and biphenyl in the C-H-O system

Saito N., Ishizaki T., Fuwa A.

Toxicological and Environmental Chemistry Vol. 74 ( 3-4 ) page： 165 - 177 2000

Language：English Publishing type：Research paper (scientific journal) Publisher：Toxicological and Environmental Chemistry

The gas phase equilibrium calculation for the C-H-O system at atmospheric pressure and temperature from 773 to 1773 K at intervals of 250 K was performed to understand the generation and decomposition behavior of dibenzo-p-dioxin (DD), dibenzo-p-furan (DF) and biphenyl (BP) in relation to the existing oxygen potential. It is possible to categorize these results into three regions from the viewpoint of this potential: region (A), region (B) and region (C) are that of the higher, modest and lower oxygen potential, respectively. In region (A), the equilibrium amounts of DD, DF and BP are nearly zero. In region (B), they increase once and then decrease with rise in temperature. In the most characteristic region (C), they increase uniformly with rise in temperature.

DOI： 10.1080/02772240009358879

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