• Title/Summary/Keyword: Ti precursor

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Study on crystallization of $PbTiO_3$ thin films by the Sol-Gel method (Sol-Gel법을 이용한 $PbTiO_3$ 박막의 결정화에 관한 연구)

  • Kyu Seog Hwang;Byung Wan Yoo;Byung Hoon Kim
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.4 no.2
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    • pp.199-209
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    • 1994
  • $PbTiO_3$ thin films were prepared on soda-lime-silica slide glasses, Si-wafer and sapphire substrate by the dip-coating of precursor solution. As starting materials, titanium tetra iso-propoxide and lead acetate trihydrate were used. Then acetylacetone was added to prepare stable sol. The effect of the parameters such as viscosity and composition of sol were investigated. The optical transmittance at visible range, refractive index, IR spectra were measured in varying compositions, thickness and heat treatment temperature. The crystallization of $PbTiO_3$ films were measured by using XRD and SEM. Diffusion of compositions from slide glass to thin film were investigated by using EDX, too. These sols not precipitated for 20 days. Transmittance of $PbTiO_3$ films at visible range were decreased with the increase of thickness and heat treatment temperatures, and were exhibited flat spectra. Pyrochlore type appeared in the films on slide glass and perovskite type appeared in the films on Si-wafer or sapphire at $600^{\circ}C$. Perovskite crystals transformed to $PbTi_3O_7$ phase at $800^{\circ}C$.

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Effect of air-contaminated TiN on the deposition characteristics of Cu film by MOCVD (공기 중에 노출된 MOCVD TiN 기판이 MOCVD Cu 증착에 미치는 효과)

  • Choe, Jeong-Hwan;Byeon, In-Jae;Yang, Hui-Jeong;Lee, Won-Hui;Lee, Jae-Gap
    • Korean Journal of Materials Research
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    • v.10 no.7
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    • pp.482-488
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    • 2000
  • The deposition characteristics of Cu film by MOCVD using (hfac)Cu(1,5-COD)(1,1,1,5,5,5-hexafluro-2,4-pentadionato Cu(I) 1,5-cryclooctadiene) as a precursor have been investigated in terms of substrate conditions. Two different substrates such as air-exposed TiN and non-contaminated TiN were used for the MOCVD of Cu. MOCVD of Cu on the air-exposed TiN affected the nucleation rate of Cu as well as its growth, resulting in the Cu films having poor interconnection between particles with relatively small grains. On the other hand, in-situ MOCVD of Cu led to the Cu films having a significantly improved interconnection between particles with larger grains, indicating the resistivity as low as $2.0{\mu}{\Omega}-cm$ for the films having more than 1900$\AA$ thickness. Moreover, better adhesion of Cu films to the TiN by using in-situ MOCVD has been obtained. Finally, initial coalescence mechanism of Cu was suggested in this paper in terms of different substrate conditions by observing the surface morphology of the Cu films deposited by MOCVD.

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Low Temperature Synthesis and Characterization of Sol-gel TiO2 Layers

  • Jin, Sook-Young;Reddy, A.S.;Park, Jong-Hyurk;Park, Jeong-Young
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.353-353
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    • 2011
  • Titanium dioxide is a suitable material for industrial use at present and in the future because titanium dioxide has efficient photoactivity, good stability and low cost [1]. Among the three phases (anatase, rutile, brookite) of titanium dioxide, the anatase form is particularly photocatalytically active under ultraviolet (UV) light. In fabrication of photocatalytic devices based on catalytic nanodiodes [2], it is challenging to obtain a photocatalytically active TiO2 thin film that can be prepared at low temperature (< 200$^{\circ}C$). Here, we present the synthesis of a titanium dioxide film using TiO2 nanoparticles and sol-gel methods. Titanium tetra-isopropoxide was used as the precursor and alcohol as the solvent. Titanium dioxide thin films were made using spin coating. The change of atomic structure was monitored after heating the thin film at 200$^{\circ}C$ and at 350$^{\circ}C$. The prepared samples have been characterized by X-ray diffraction (XRD), scanning electron microcopy, X-ray photoelectron spectroscopy, transmission electron microscopy, ultraviolet-visible spectroscopy (UV-vis), and ellipsometry. XRD spectra show an anatase phase at low temperature, 200$^{\circ}C$. UV-vis confirms the anatase phase band gap energy (3.2 eV) when using the photocatalyst. TEM images reveal crystallization of the titanium dioxide at 200$^{\circ}C$. We will discuss the switching behavior of the Pt /sol-gel TiO2 /Pt layers that can be a new type of resistive random-access memory.

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Microstructural Characterization of MOCVD RuOx Thin Films and Effects of Annealing Gas Ambient (MOCVD RuOx 박막의 미세구조 특성평가와 열처리 가스환경 영향)

  • Kim, Gyeong-Won;Kim, Nam-Su;Choe, Il-Sang;Kim, Ho-Jeong;Park, Ju-Cheol
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.51 no.9
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    • pp.423-429
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    • 2002
  • RuOx thin films were fabricated by the method of liquid delivery MOCVD using Ru(C$_{8}$ $H_{13}$ $O_2$)$_3$ as the precursor and their thermal effects and conductivity were investigated. Ru films deposited at 25$0^{\circ}C$ were annealed at $650^{\circ}C$ for 1min with Ar, $N_2$ or N $H_3$ ambient. The changes of the micro-structure, the surface morphology and the electrical resistivity of the Ru films after annealing were studied. Ar gas was more effective than $N_2$ and N $H_3$ gases as an ambient gas for the post annealing of the Ru films, because of smaller resistivity and denser grains. The X-ray diffraction and X-ray photoelectron spectroscopy results indicate that the Ru $O_2$ phase and the silicidation are not observed regardless of the ambient gases. The minimum resistivity of the Ru film is found to have the value of 26.35 $\mu$Ω-cm in Ar ambient. Voids were formed at Ru/TiN interface of the Ru layer after annea1ing in $N_2$ ambient. The $N_2$ gas generated due to the oxidation of the TiN layer accumulated at the Ru/TiN interface, forming bubbles; consequently, the stacked film may peel off the Ru/TiN interface.e.

The Effect of Nb-doped TiO2 Coating for Improving Stability of NiCrAl Alloy Foam (NiCrAl 합금 폼의 안정성 향상을 위해 코팅된 Nb-doped TiO2의 효과)

  • Jo, Hyun-Gi;Shin, Dong-Yo;Ahn, Hyo-Jin
    • Korean Journal of Materials Research
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    • v.29 no.5
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    • pp.328-335
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    • 2019
  • Nb-doped $TiO_2$(NTO) coated NiCrAl alloy foam for hydrogen production is prepared using ultrasonic spray pyrolysis deposition(USPD) method. To optimize the size and distribution of NTO particles based on good physical and chemical stability, we synthesize particles by adjusting the weight ratio of the Nb precursor solution(5 wt%, 10 wt% and 15 wt%). The morphological, chemical bonding, and structural properties of the NTO coated NiCrAl alloy foam are investigated by X-ray diffraction(XRD), X-ray photo-electron spectroscopy(XPS), and Field-Emission Scanning Electron Microscopy(FESEM). As a result, the samples of controlled Nb weight ratio exhibit a common diffraction pattern at ${\sim}25.3^{\circ}$, corresponding to the(101) plane, and have chemical bonding(O-Nb=O) at 534 eV. The NTO particles with the optimum weight ratio of N (10 wt%) show a uniform distribution with a size of ~18.2-21.0 nm. In addition, they exhibit the highest corrosion resistance even in the electrochemical stability estimation. As a result, the introduction of NTO coated NiCrAl alloy foam by USPD improves the chemical stability of the NiCrAl alloy foam by protecting the direct electrochemical reaction between the foam and the electrolyte. Thus, the optimized NTO coating can be proposed for excellent protection of NiCrAl alloy foam for hydrocarbon-based steam methane reforming(SMR).

Synthesis of Porous $TiO_2$ Thin Films Using PVC-g-PSSA Graft Copolymer and Their Use in Dye-sensitized Solar Cells (PVC-g-PSSA 가지형 공중합체를 이용한 다공성 $TiO_2$ 박막의 합성 및 염료감응 태양전지 응용)

  • Byun, Su-Jin;Seo, Jin-Ah;Chi, Won-Seok;Shul, Yong-Gun;Kim, Jong-Hak
    • Membrane Journal
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    • v.21 no.2
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    • pp.193-200
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    • 2011
  • An amphiphilic graft copolymer comprising a poly(vinyl chloride) (PVC) backbone and poly (styrene sulfonic acid) (PSSA) side chains (PVC-g-PSSA) was synthesized via atom transfer radical polymerization (ATRP). Mesoporous titanium dioxide $(TiO_2)$ films with crystalline anatase phase were synthesized via a sol-gel process by templating PVC-g-PSSA graft copolymer. Titanium isopropoxide (TTIP), a $TiO_2$ precursor was selectively incorporated into the hydrophilic PSSA domains of the graft copolymer and grew to form mesoporous $TiO_2$ films, as confirmed by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. The performances of dye-sensitized solar cell (DSSC) were systematically investigated by varying spin coating times and the amounts of P25 nanoparticies. The energy conversion efficiency reached up to 2.7% at 100 mW/$cm^2$ upon using quasi-solid-state polymer electrolyte.

Effect of compliance current on resistive switching characteristics of solution-processed HfOx-based resistive switching RAM (ReRAM)

  • Jeong, Ha-Dong;Jo, Won-Ju
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.255-255
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    • 2016
  • Resistive random access memory (ReRAM)는 낮은 동작 전압, 빠른 동작 속도, 고집적화 등의 장점으로 인해 차세대 비휘발성 메모리 소자로써 많은 관심을 받고 있다. 최근에 ReRAM 절연막으로 NiOx, TiOx, AlOx TaOx, HfOx와 같은 binary metal oxide 물질들을 적용하는 연구가 활발히 진행되고 있다. 특히, HfOx는 안정적인 동작 특성을 나타낸다는 점에서 ReRAM 절연막 물질로 적합하다고 보고되고 있다. ReRAM 절연막을 형성할 때, 물리 기상 증착 방법 (PVD)이나 화학 기상 증착법 (CVD)과 같은 방법이 많이 이용된다. 이러한 증착 방법들은 고품질의 박막을 형성시킬 수 있는 장점이 있다. 하지만, 높은 온도에서의 공정과 고가의 진공 장비가 이용되기 때문에 경제적인 문제가 있으며, 기판 또는 금속에 플라즈마 손상으로 인한 문제가 발생할 수 있다. 따라서 이러한 문제점들을 개선하기 위해 용액 공정이 많은 관심을 받고 있다. 용액 공정은 공정과정이 간단할 뿐만 아니라 소자의 대면적화가 가능하고 공정온도가 낮으며 고가의 진공장비가 필요하지 않은 장점을 가진다. 따라서 본 연구에서는, 용액공정을 이용하여 HfOx 기반의 ReRAM 제작하였고 $25^{\circ}C$$85^{\circ}C$에서 ReRAM의 동작특성에 미치는 compliance current의 영향을 평가하였다. 실험 방법으로는, hafnium chloride (0.1 M)를 2-methoxyethanol에 충분히 용해시켜서 precursor를 제작하였다. 이후, p-type Si 기판 위에 습식산화를 통하여 300 nm 두께의 SiO2 절연층을 성장시킨 후, 하부전극을 형성하기 위해 electron beam evaporation을 이용하여 10/100 nm 두께의 Ti/Pt 전극을 증착하였다. 순차적으로, 제작된 산화물 precursor를 이용하여 Pt 위에 spin coating 방법으로 1000 rpm 10 초, 6000 rpm 30초의 조건으로 두께 35 nm의 HfOx 막을 증착하였다. 최종적으로, solvent 및 불순물을 제거하기 위해 $180^{\circ}C$의 온도에서 10 분 동안 열처리를 진행하였으며, 상부 전극을 형성하기 위해 electron beam evaporation을 이용하여 Ti와 Al을 각각 50 nm, 100 nm의 두께로 증착하였다. ReRAM 동작에서 compliance current가 미치는 영향을 평가하기 위하여 compliance current를 10mA에서 1mA까지 변화시키면서 측정한 결과, $25^{\circ}C$에서는 compliance current의 크기와 상관없이 일정한 메모리 윈도우와 우수한 endurance 특성을 얻는 것을 확인하였다. 한편, $85^{\circ}C$의 고온에서 측정한 경우에는 1mA의 compliance current를 적용하였을 때, $25^{\circ}C$에서 측정된 메모리 윈도우 크기를 비슷하게 유지하면서 더 우수한 endurance 특성을 얻는 것을 확인하였다. 결과적으로, 용액공정 방법으로 제작된 ReRAM을 측정하는데 있어서 compliance current를 줄이면 보다 우수한 endurance 특성을 얻을 수 있으며, ReRAM 소자의 전력소비감소에 효과적이라고 기대된다.

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Morphology of Lead Titanate Prepared by Wet Chemical Methods (습식화학법으로 제조된 티탄산 납의 형상)

  • 최병철;이문호
    • Korean Journal of Crystallography
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    • v.3 no.1
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    • pp.1-8
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    • 1992
  • The morphology of lead titanate powders prepared by sol-gel and coprecipitation techniques was investigated as a function of firing temperature and soaking time. PbTiO3 precursor powders were derived from a mixed solution of lead nitrate and titanium tetrachloride at 40℃ to 43℃ and pH of 9.0 to 9.7, and fired at temperatures 350-1000℃ for 1-10h in air. An increase of particle size and agglomeration with increasing calcination temperature and duration could be observed. By annealing sol-gel derived powder at 700℃, the tially-formed acicular(and/or prismatic) primary particles transformed to polyhedral shape with soaking time, and further soaking caused coarsening the polyhedral particles with rounded edges. However, the morphology of the coprecipitated powders was not varied during crystallization.

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Synthesis of Ni-based Metallic Glass Composite Fabricated by Spark Plasma Sintering (방전플라즈마소결을 이용한 Ni계 비정질 복합재의 제조)

  • Kim, Song Yi;Guem, Bo Kyeong;Lee, Min Ha;Kim, Bum Sung
    • Journal of Powder Materials
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    • v.20 no.1
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    • pp.33-36
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    • 2013
  • A bulk metallic glass-forming alloy, $Ni_{59}Zr_{20}Ti_{16}Si_2Sn_3$ metallic glass powders was used for good commercial availability and good formability in supercooled liquid region. In this study, the Ni-based metallic glass was synthesized using by high pressure gas atomized metallic glass powders. In order to create a bulk metallic glass sample, the $Ni_{59}Zr_{20}Ti_{16}Si_2Sn_3$ metallic glass powders with ball-milled Ni-based amorphous powder with 40%vol brass powder and Cu powder for 20 hours. The composite specimens were prepared by Spark Plasma Sintering for the precursor. The SPS was performed at supercooled liquid region of Ni-based metallic glass. The amorphous structure of the final sample was characterized by SEM, X-ray diffraction and DSC analysis.

Excimer laser annealing of sol-gel derived PZT thin films

  • Do, Young-Ho;Kang, Min-Gyu;Oh, Seung-Min;Kang, Chong-Yun;Yoon, Seok-Jin
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2010.06a
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    • pp.20-20
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    • 2010
  • The effect of excimer laser annealing on the structural and dielectric behaviors of $PbZr_{0.52}Ti_{0.48}O_3$ (PZT) thin films has been investigated. The amorphous PZT thin films were prepared on Pt/Ti/$SiO_2$/Si substrates by a sol-gel method. The PZT precursor was prepared from lead acetate, zirconium acetylacetonate, and titanium isopropoxide. The starting materials were dissolved in n-propanol and 1,3-propanediol. After, the amorphous PZT thin films were laser-annealed (using KrF excimer laser) as a function of the laser energy density and the number of laser pulse. Structural properties of PZT thin films are characterized by using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The dielectric characterization was done on a RT66A test system and a Agilent 4294A impedance analyzer. The PZT thin films show that excimer laser irradiation drastically improved the crystallization and dielectric properties of the PZT thin films, depending on the energy density and the pulse number.

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