scholarly journals Highly-Conductive and Well-Adhered Cu Thin Film Fabricated on Quartz Glass by Heat Treatment of a Precursor Film Obtained Via Spray-Coating of an Aqueous Solution Involving Cu(II) Complexes

Coatings ◽  
2018 ◽  
Vol 8 (10) ◽  
pp. 352 ◽  
Author(s):  
Philipus Hishimone ◽  
Hiroki Nagai ◽  
Masato Morita ◽  
Tetsuo Sakamoto ◽  
Mitsunobu Sato

A Cu thin film on a quartz glass substrate was fabricated by a wet process involving heat-treatment of a precursor film spray-coated with an aqueous ammonia solution containing Cu(HCOO)2∙4H2O and Cu(II) complex of ethylenediamine-N,N,N′N′-tetraacetic acid. The precursor film that formed on the substrate at 180 °C in air was heat-treated at 350 °C and post annealed at 400 °C by placing an identical-sized glass on top, under Ar gas flow in a tubular furnace. X-ray diffraction pattern of the resultant film showed only peaks of Cu. The resultant film of 100 nm thickness has an adhesion strength and electrical resistivity of 37(7) MPa and 3.8(6) × 10−5 Ω cm, respectively. The images of atomic force and field-emission scanning-electron microscopies revealed a film of well-connected Cu grains with an average surface roughness of 11 nm. The reflectance of the thin film is more than 90% in the far-infrared region. The film’s chemical composition was also examined by using Auger electron spectroscopy.

Coatings ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 97 ◽  
Author(s):  
Philipus N. Hishimone ◽  
Kenta Watarai ◽  
Hiroki Nagai ◽  
Mitsunobu Sato

A LiCoO2 thin film on a quartz glass substrate was fabricated by a wet process involving heat treatment of a precursor film spray-coated with an aqueous ammonia solution containing LiCH3COO and Co(CH3COO)2. The precursor film formed onto the substrate at 180 °C in air, and was heat treated at 500 °C in air for 0.5 h. The obtained film was spin-coated further with an ethanol-based precursor solution containing identical metal acetates, and heat treated at 500 °C in air for 0.5 h. The X-ray diffraction pattern of the resultant film showed only peaks assignable to the layered-rock-salt LiCoO2. Raman spectroscopy measurements revealed vibrational modes assignable to layered rock salt LiCoO2, with minor content of less than 5 mol% of spinel-type Co3O4. The field emission scanning electron microscopy images indicated that the resultant film was 0.21 μm thick, had no voids, and was a combination of small rounded grains measuring 18 nm in diameter and hexagonal grains larger than 0.2 μm in length. The Hall effect measurements indicated that the resultant thin film was a p-type semiconductor with electrical resistivity of 35(2) Ω·cm and a carrier concentration and carrier mobility of 8(2) × 1016 cm−3 and 2(1) cm2·V−1·s−1, respectively.


Nanomaterials ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 1348
Author(s):  
Hiroki Nagai ◽  
Naoki Ogawa ◽  
Mitsunobu Sato

Deep-ultraviolet (DUV) light-transparent conductive composite thin films, consisting of dispersed multiwalled carbon nanotubes (MWCNTs) and SiO2 matrix composites, were fabricated on a quartz glass substrate. Transparent and well-adhered amorphous thin films, with a thickness of 220 nm, were obtained by weak ultraviolet (UV) irradiation (4 mW cm−2 at 254 nm) for more than 6 h at 20−40 °C onto the precursor films, which were obtained by spin coating with a mixed solution of MWCNT in water and Si(IV) complex in ethanol. The electrical resistivity of MWCNT/SiO2 composite thin film is 0.7 Ω·cm, and transmittance in the wavelength region from DUV to visible light is higher than 80%. The MWCNT/SiO2 composite thin film showed scratch resistance at pencil hardness of 8H. Importantly, the resistivity of the MWCNT/SiO2 composite thin film was maintained at the original level even after heat treatment at 500 °C for 1 h. It was observed that the heat treatment of the composite thin film improved durability against both aqueous solutions involving a strong acid (HCl) and a strong base (NaOH).


2021 ◽  
Vol 14 (02) ◽  
pp. 2151012
Author(s):  
Natangue Heita Shafudah ◽  
Hiroki Nagai ◽  
Mitsunobu Sato

Cubic or tetragonal zirconia thin films of transparent and 100 nm thickness were selectively formed on a quartz glass substrate by heat-treating the molecular precursor films involving Zr(IV) complexes of nitrilotriacetic acid, at 500[Formula: see text]C in air for 1 h. A precursor solution was prepared by a reaction of the ligand and zirconium tetrabutoxide in alcohol under the presence of butylamine. By the addition of H2O2 or H2O into the solution, the spin-coated precursor films were converted to cubic zirconia thin films by the abovementioned procedure. Further, the identical phase was produced also in the case of the electro-sprayed precursor film which was formed by an addition of H2O2 into the solution. On the other hand, the tetragonal zirconia thin film was obtained from a precursor film formed by using a solution dissolving the original Zr(IV) complex of the ligand, without H2O2 nor H2O. The crystal structure of all thin films was determined by using both the X-ray diffraction (XRD) patterns and Raman spectra. Thus, the zirconia thin films of both crystals could be facilely and selectively obtained with no use of hetero-metal ion stabilizers. The XPS spectra of the thin films show that the O/Zr ratio of the cubic phase is 1.37 and slightly larger than tetragonal one (1.29), and also demonstrate that the nitrogen atoms, which may contribute to stabilize these metastable phases at room temperature, of about 5−7 atomic% was remained in the resultant thin films. The adhesion strengths of cubic zirconia thin film onto the quartz glass substrate was 68 MPa and larger than that of tetragonal one, when the precursor films were formed via a spin coating process. The optical and surface properties of the thin films were also examined in relation to the crystal systems.


2020 ◽  
Vol 13 (03) ◽  
pp. 2051012
Author(s):  
Alina Uusiku ◽  
Hiroki Nagai ◽  
Mitsunobu Sato

A conductive Cu thin film with a thickness of 170[Formula: see text]nm, electrical resistivity of 8.9(2) [Formula: see text][Formula: see text]cm and adhesion strength of 12(7) MPa was fabricated at 180∘C in air. The spray solutions were prepared by electrolyzing Cu electrodes in an aqueous solution of ammonium formate, and then by adding ethylenediamine-N, N, N[Formula: see text], N[Formula: see text]-tetraacetic acid (EDTA). The surface morphology image of resultant Cu thin film, observed by a field emission scanning electron microscope, revealed Cu grains with particle sizes of ca. [Formula: see text][Formula: see text]nm. It was indicated that the Cu complex containing EDTA ligand in the spray solution plays important roles to (1) provide enough amount of carbon atoms as a reducing agent for phase transition of its coordinated Cu[Formula: see text] to crystalline Cu0 and (2) prevent the product from oxidation under atmospheric O2 during spray coating.


Nanomaterials ◽  
2021 ◽  
Vol 11 (12) ◽  
pp. 3352
Author(s):  
Yutaka Suwazono ◽  
Takuro Murayoshi ◽  
Hiroki Nagai ◽  
Mitsunobu Sato

A single-walled carbon nanotube/anatase (SWCNT/anatase) composite thin film with a transmittance of over 70% in the visible-light region was fabricated on a quartz glass substrate by heat treating a precursor film at 500 °C in air. The precursor film was formed by spin coating a mixed solution of the titania molecular precursor and well-dispersed SWCNTs (0.075 mass%) in ethanol. The anatase crystals and Ti3+ ions in the composite thin films were determined by X-ray diffraction and X-ray photoelectron spectroscopy, respectively. The effect of the heating process on the SWCNTs was analyzed using Raman spectroscopy. The composite film showed an even surface with a scratch resistance of 4H pencil hardness, as observed using field-emission scanning electron microscopy and atomic force microscopy. The electrical resistivity and optical bandgap energy of the composite thin film with a thickness of 100 nm were 6.6 × 10−2 Ω cm and 3.4 eV, respectively, when the SWCNT content in the composite thin film was 2.9 mass%. An anodic photocurrent density of 4.2 μA cm−2 was observed under ultraviolet light irradiation (16 mW cm−2 at 365 nm) onto the composite thin film, thus showing excellent properties as a photoelectrode without conductive substrates.


Shinku ◽  
1996 ◽  
Vol 39 (1) ◽  
pp. 7-10 ◽  
Author(s):  
Satoru IWAMORI ◽  
Takehiro MIYASHITA ◽  
Shin FUKUDA ◽  
Nobuhiro FUKUDA ◽  
Kazufuyu SUDOH

2010 ◽  
Vol 58 (18) ◽  
pp. 6064-6071 ◽  
Author(s):  
M. Tomozawa ◽  
H.Y. Kim ◽  
A. Yamamoto ◽  
S. Hiromoto ◽  
S. Miyazaki

2013 ◽  
Vol 750-752 ◽  
pp. 1879-1882
Author(s):  
An Na Yue ◽  
Kun Peng ◽  
Ling Ping Zhou ◽  
Jia Jun Zhu ◽  
De Yi Li

Titanium and aluminum films were deposited on oxygen-free copper substrates by electron beam evaporation method to obtain Al/Cu and Al/Ti/Cu layer composites. Evolution of microstructure and properties of Al/Cu and Al/Ti/Cu thin film during heat treatment processes were investigated by XRD, SEM and electrical properties analysis. The introduce of Ti layer can prevent the formation of Cu-Al intermetallic compounds, and has no obvious influence on the electrical resistivity of Al/Cu thin film, which can be used as a pad in microelectronic package and devices.


2010 ◽  
Vol 25 (5) ◽  
pp. 972-975 ◽  
Author(s):  
Kai-Jheng Wang ◽  
Yung-Chi Lin ◽  
Jenq-Gong Duh ◽  
Ching-Yuan Cheng ◽  
Jey-Jau Lee

In situ investigation of the interfacial reaction in the Sn/Cu thin film during aging, and reflow was carried out by synchrotron radiation with high intensity and high resolution of x-ray. With this technique, the phase transformation and evolution of the Sn/Cu thin film during heat treatment can be directly and continuously investigated. Moreover, the information for coefficient of thermal expansion in intermetallic compounds was also evaluated by this approach.


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