• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2002.11a
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• pp.63-63
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• 2002

현재 기계적 합금화법에서는 주로 합금을 구성하는 성분원소 분말을 불활성분위기에서 볼밀처리 함으로써 함금화를 시키거나 모합금에 산화물을 분산시켜 복합화시키는 공정을 통하여 각종 화합물, 비정질상 및 과포화고용체등의 준안정상의 합성 뿐만이 아니라 초미세조직의 생성에 관한 폭 넓은 분야의 연구가 행하여지고 있다. 한편 MA에서는 볼멀처리중 기계적 에너지의 투여에 의하여 실제 반응온도보다 낮은 온도에서 발생하는 특이한 화학반응 즉 Mechanochemical 반응을 일으키 기도 한다. 본 연구에서는 헤마타이트($Fe_20_3$)와 금속윈소인 Ti의 MA처리에 의하여 고상환원반응 을 유기시켜 $Fe-TiO_2$계 nanocomposite 분말재료를 제조하고자 한다. 특히 MA 공정에 있어서 자기 물성의 변화와 X선 회절을 통하여 고상환원반응에 의한 복합분말의 생성과정을 조사하였다. 출발원료는 $Fe_20_3$(고순도화학제,99.9%, 평균입경 0.1$\mu\textrm{m}$)와 금속원소인 Ti(99.9%, 명균업경 150$\mu\textrm{m}$)을 몰비 2:3의 조성이 되도록 하여 MA를 실시하였다. 볼멀은 고에너지 유성형 볼밀장치(독일 제, Fritsch P-5)를 이용하였으며 진공치환형 용기에 원료분말을 장입하여 2회정도 진공배기한 후 아르곤 가스를 충전하여 볼밀을 행하였다. 얻어진 분말시료에 대하여 x-선 회절장치, 전자현미경 (SEM) 및 진동시료형자력계(VSM)를 통하여 결정구조, 미셰조직 빛 자기특성을 조사하였다. $Fe_2O_3-Ti$ 혼합분말의 MA처리 에 의하여 초기단계부터 환원반응과 함께 $Fe_3TIO_{lO}$ 중간상이 관찰 되었으나 30hrs의 MA처리 후 Fe와 산화물 $TiO_2$로 모두 환원되어 $Fe-TiO_2$계 나노복합분말이 얻어짐을 알 수 있었다. 이 때 X션 회절피크의 line broadening으로부터 복합분말의 Fe 명균 결정립 크기는 24nm로 초미세 결정럽의 분말합금이었다. 포화자화값은 볼밀처리에 따라 점점 증가하여 MA 30시간에는 20.3emu/g로 포화됨을 알 수 있었다. 또한 보자력 Hc는 MA초기단계에 350e로 매우 낮으나 30시간 후에는 Hc값이 2600e로 매우 큰 값을 나타내었다. 이것은 환원반응결과 초기에 생성된 Fe의 결정립이 비교적 크고 결정결함이 적으나 볼밀처리를 30시간까지 행하면 Fe 결정렵의 미세화 빛 strain 증가로 magnetic hardening이 일어나기 때문인 것으로 사료된다.

• Textile Coloration and Finishing
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• v.25 no.2
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• pp.118-125
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• 2013

Poly(vinyl alcohol) (PVA)/titanium dioxide ($TiO_2$) composite nanofibers were produced at different $TiO_2$ concentrations (0.5, 1 and 1.5 wt.%) using the electrospinning method. The parameters of electrospinning including polymer contents, voltage and tip-to-collector distance (TCD) were optimized for fabrication process. The study showed that 7.5 wt.% PVA, 15 kV applied voltage and 15 cm TCD are the best condition to obtain uniform PVA/$TiO_2$ nanofibers. $TiO_2$ nanoparticles give significant effect in fiber morphology. $TiO_2$ content increases the diameter of the fibers and roughen the fiber surfaces. The PVA/$TiO_2$ nanofibers were characterized by scanning electron microscope (SEM), transmission electron microscope (TEM) and X-ray diffraction (XRD).

• Bulletin of the Korean Chemical Society
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• v.19 no.11
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• pp.1185-1188
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• 1998

Layered nanocomposite, SiO2/TiO2 sol pillared clay, has been prepared by the ion exchange reaction of Na' ion in montmorillonite with positively charged mixed SiO2/TiO2 sol. The nanosized sol particles were synthesized by mixing SiO2 sol solution with TiO2 one, which is obtained by acidic hydrolysis of TEOS and TiCl4, respectively. From powder XRD, the basal spacing (d001) of the sample calcined at 400 ℃ was found to be ca. 60 Å, due to the multistacking of nanosized SiO2 and TiO2 sol particles, which was confirmed by the pore size analysis from 129Xe NMR and micropore analysis calculated from nitrogen adsorption. The BET specific surface area shows the value of 684 m2g-1 (Langmuir 1115 m2g-1), which is the highest among various pillared clays ever reported previously, and the total porosity is found to be 0.51 mlg-1, and the pores are mainly composed of micropore with a size of ca. 11.8 Å. This result agrees with the adsorption capacity obtained from water adsorption. According to diffuse reflectance ultraviolet-visible spectroscopy, it is found that the TiO2 particles stabilized in the interlayer space of montmorillonite are quantum-sized of ca. 20 Å.

• Bulletin of the Korean Chemical Society
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• v.32 no.8
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• pp.2584-2592
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• 2011

Nickel nanoparticle-poly(N-vinyl-2-pyrrolidone)/$TiO_2-ZrO_2$ composite (Ni-PVP/$TiO_2-ZrO_2$) was prepared by in situ polymerization method. The physical and chemical properties of Ni-PVP/$TiO_2-ZrO_2$ were investigated by XRD, FT-IR, BET, TGA, SEM and TEM techniques. The catalytic performance of this novel heterogeneous catalyst was determined for the Suzuki-Miyaura cross-coupling reaction between aryl halides and phenylboronic acid in the presence of methanol-water mixture as solvent. The effects of reaction temperature, the amount of catalyst, amount of support, solvent, and amount of metal for the synthesis of Ni-PVP/$TiO_2-ZrO_2$, were investigated as well as recyclability of the heterogeneous composite. The catalyst used for this synthetically useful transformation showed considerable level of reusability besides very good activity.

• Bulletin of the Korean Chemical Society
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• v.33 no.5
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• pp.1753-1758
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• 2012

A novel, efficient and controlled protocol for the synthesis and enhanced photocatalytic activity of $Au@TiO_2$ nanocomposite is developed. $TiO_2$ (P25) was pretreated by employing UV light (${\lambda}$ = 254 nm) and the pretreated $TiO_2$ was uniformly decorated by gold nanoparticles (AuNPs) in presence of sodium citrate and UV light. UV pretreatment makes the $TiO_2$ activated, as electrons were accumulated within the $TiO_2$ in the conduction band. These accumulated electrons facilitate the formation of AuNPs which were of very small size (2-5 nm), similar morphology and uniformly deposited at $TiO_2$ surface. It leads to formation of stable and crystalline $Au@TiO_2$ nanocomposites. The rapidity (13 hours), monodispersity, smaller nanocomposites and easy separation make this protocol highly significant in the area of nanocomposites syntheses. As-synthesized nanocomposites were characterized by TEM, HRTEM, TEM-EDX, SAED, XRD, UV-visible spectrophotometer and zeta potential. Dye degradation experiments of methyl orange show that type I ($Au@TiO_2$ nanocomposites in which $TiO_2$ was pretreated with UV light) has enhanced photocatalytic activity in comparison to type II ($Au@TiO_2$ nanocomposites in which $TiO_2$ was not pretreated with UV light) and $TiO_2$ (P25). This shows that pretreatment of $TiO_2$ provides type I a better catalytic activity.

• Journal of Powder Materials
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• v.11 no.3
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• pp.247-252
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• 2004

Recently, it has been found that mechanical alloying (MA) facilitates the nanocomposites formation of metal-metal oxide systems through solid-state reduction during ball milling. In this work, we studied the MA effect of Fe$_{3}$O$_{4}$-M (M = Al, Ti) systems, where pure metals are used as reducing agents. It is found that composite powders in which $Al_{2}$O$_{3}$ and TiO$_{2}$ are dispersed in $\alpha$-Fe matrix with nano-sized grains are obtained by mechanical alloying of Fe$_{3}$O$_{4}$ with Al and Ti for 25 and 75 hours, respectively. It is suggested that the large negative heat associated with the chemical reduction of magnetite by aluminum is responsible for the shorter MA time for composite powder formation in Fe$_{3}$O$_{4}$-Al system. X-ray diffraction results show that the reduction of magnetite by Al and Ti if a relatively simple reaction, involving one intermediate phase of FeAl$_{2}$O$_{4}$ or Fe$_{3}$Ti$_{3}$O$_{10}$. The average grain size of $\alpha$-Fe in Fe-TiO$_{2}$ composite powders is in the range of 30 nm. From magnetic measurement, we can also obtain indirect information about the details of the solid-state reduction process during MA.

• Textile Coloration and Finishing
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• v.26 no.3
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• pp.195-200
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• 2014

Poly(vinyl alcohol)(PVA)/pullulan/titanium dioxide($TiO_2$) composite nanofibers were produced at different $TiO_2$ concentrations(1 and 3 wt.%) using the electrospinning method. The parameters of electrospinning including polymer contents, voltage and tip-to-collector distance(TCD) were optimized for fabrication process. The study showed that the best condition to make PVA/pullulan nanofiber and effect of $TiO_2$ nanoparticles. The PVA/pullulan/$TiO_2$ nanofibers were characterized by scanning electron microscope(SEM), transmission electron microscope(TEM), Thermogravimetric analysis (TGA) and X-ray diffraction(XRD).

• Korean Journal of Metals and Materials
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• v.56 no.12
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• pp.900-909
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• 2018

A $ZnO/TiO_2$ photocatalyst decorated with PbS quantum dots (QDs) was synthesized to achieve high photocatalytic efficiency for the decomposition of dye in aqueous media. A $TiO_2$ porous layer, as a precursor photocatalyst, was fabricated using micro-arc oxidation, and exhibited irregular porous cells with anatase and rutile crystalline structures. Then, a ZnO-deposited $TiO_2$ catalyst was fabricated using a zinc acetate solution, and PbS QDs were uniformly deposited on the surface of the $ZnO/TiO_2$ photocatalyst using the successive ionic layer adsorption and reaction (SILAR) technique. For the PbS $QDs/ZnO/TiO_2$ photocatalyst, ZnO and PbS nanoparticles are uniformly precipitated on the $TiO_2$ surface. However, the diameters of the PbS particles were very fine, and their shape and distribution were relatively more homogeneous compared to the ZnO particles on the $TiO_2$ surface. The PbS QDs on the $TiO_2$ surface can induce changes in band gap energy due to the quantum confinement effect. The effective band gap of the PbS QDs was calculated to be 1.43 eV. To evaluate their photocatalytic properties, Aniline blue decomposition tests were performed. The presence of ZnO and PbS nanoparticles on the $TiO_2$ catalysts enhanced photoactivity by improving the absorption of visible light. The PbS $QDs/ZnO/TiO_2$ heterojunction photocatalyst showed a higher Aniline blue decomposition rate and photocatalytic activity, due to the quantum size effect of the PbS nanoparticles, and the more efficient transport of charge carriers.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2009.11a
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• pp.150-150
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• 2009

In this paper, various kinds of epoxy based nanocomposites were made and AC breakdown properties of nano-$TiO_2$ and micro-silica filler mixture of epoxy based composites were studied by sphere to sphere electrode. Moreover, nano- and micro-filler combinations were adopted as an approach toward practical application of nanocomposite insulating materials. AC breakdown test was performed at room temperature $(25^{\circ}C)$, $80^{\circ}C$ and $100^{\circ}C$. The result shows breakdown strength about non-filled, nano-scale $TiO_2$, micro-scale silica and nano-$TiO_2$, micro-silica filled epoxy composites.

• Journal of Powder Materials
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• v.10 no.6
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• pp.443-447
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• 2003

Nano-sized $TiB_2$ was in situ synthesized in copper matrix through self-propagating high temperature synthesis (SHS) with high-energy ball milled Ti-B-Cu elemental mixtures as powder precursors. The size of $TiB_2$ particles in the product of SHS reaction decreases with time of preliminary mechanical treatment ranging from 1 in untreated mixture to 0.1 in mixtures milled for 3 min. Subsequent mechanical treatment of the product of SHS reaction allowed the $TiB_2$ particles to be reduced down to 30-50 nm. Microstructural change of $TiB_2$-Cu nanocomposite during spark plasma sintering (SPS) was also investigated. Under simultaneous action of pressure, temperature and electric current, titanium diboride nanoparticles distributed in copper matrix move, agglomerate and form a interpenetrating phase composite with a fine-grained skeleton.