• Title/Summary/Keyword: Si-N precursor

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Pore-Controlled Synthesis of Mesoporous Silica Particles by Spray Pyrolysis from Aqueous Silicic Acid (규산 수용액으로부터 분무열분해법에 의한 기공 특성이 제어된 메조기공의 다공성 실리카 분말 합성)

  • Chang, Han Kwon;Lee, Jin Woo;Oh, Kyoung Joon;Jang, Hee Dong;Kil, Dae Sup;Choi, Jeong Woo
    • Particle and aerosol research
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    • v.8 no.2
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    • pp.89-95
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    • 2012
  • Spherical mesoporous silica particles, of which main pore diameter was 3.8 nm, were successfully prepared by spray pyrolysis from aqueous silicic acid. The effect of precursor concentration, reaction temperature, and the addition of urea and PEG on the particle diameter and pore properties such as pore diameter, total pore volume, and specific surface area were investigated by using FE-SEM, particle size analyzer, and nitrogen absorption-desorption analysis. With an increase of the precursor concentration from 0.2 M to 0.7 M, the average particle diameter, total pore volume, and specific surface area of the porous silica particles increased from 0.56 to $0.96\;{\mu}m$, 0.434 to $0.486\;cm^3/g$, 467.8 to $610.4\;m^2/g$, respectively. Within the temperature range $(600\;^{\circ}C{\sim}800\;^{\circ}C)$, there was no significant difference in the pore diameter, total pore volume, and specific surface area. In addition, the addition of urea as an expansion aid led to slight increases in particle diameter, pore diameter, and specific surface area. However, when the polyethylene glycol (PEG) as an organic template was used, the total pore volume of porous particles increased dramatically.

Reactivity of aluminosilicate materials and synthesis of geopolymer mortar under ambient and hot curing condition

  • Zafar, Idrees;Tahir, Muhammad Akram;Hameed, Rizwan;Rashid, Khuram;Ju, Minkwan
    • Advances in concrete construction
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    • v.13 no.1
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    • pp.71-81
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    • 2022
  • Aluminosilicate materials as precursors are heterogenous in nature, consisting of inert and partially reactive portion, and have varying proportions depending upon source materials. It is essential to assess the reactivity of precursor prior to synthesize geopolymers. Moreover, reactivity may act as decisive factor for setting molar concentration of NaOH, curing temperature and setting proportion of different precursors. In this experimental work, the reactivities of two precursors, low calcium (fly ash (FA)) and high calcium (ground granulated blast furnace slag (GGBS)), were assessed through the dissolution of aluminosilicate at (i) three molar concentrations (8, 12, and 16 M) of NaOH solution, (ii) 6 to 24 h dissolution time, and (iii) 20-100℃. Based on paratermeters influencing the reactivity, different proportions of ternary binders (two precursors and ordinary cement) were activated by the combined NaOH and Na2SiO3 solutions with two alkaline activators to precursor ratios, to synthesize the geopolymer. Reactivity results revealed that GGBS was 20-30% more reactive than FA at 20℃, at all three molar concentrations, but its reactivity decreased by 32-46% with increasing temperature due to the high calcium content. Setting time of geopolymer paste was reduced by adding GGBS due to its fast reactivity. Both GGBS and cement promoted the formation of all types of gels (i.e., C-S-H, C-A-S-H, and N-A-S-H). As a result, it was found that a specified mixing proportion could be used to improve the compressive strength over 30 MPa at both the ambient and hot curing conditions.

Preparation of Ferroelectric (YbxY1-x)MnO3 Thin Film by Sol-Gel Method (졸-겔법에 의한 (YbxY1-x)MnO3강유전체 박막제조)

  • 강승구;이기호
    • Journal of the Korean Ceramic Society
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    • v.41 no.2
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    • pp.170-175
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    • 2004
  • The ferroelectric (Y $b_{x}$ $Y_{1-x}$)Mn $O_3$ thin films were fabricated by sol-gel method using Y-acetate, Yb-acetate, and Mn-acetate as raw materials. The stable (Y $b_{x}$ $Y_{1-x}$)Mn $O_3$ precursor solution (sol) was prepared through the reflux process with acetylaceton as a catalyst and coated on Si(100) substrate by spin coating. The heat treatment temperature and, Rw ($H_2O$/alkoxide moi ratio) dependence on crystallinity of thin films were studied. The lowest temperature for obtaining YbMn $O_3$phase and the optimum heat-treatment conditions were proved as at 7$50^{\circ}C$ and 80$0^{\circ}C$, respectively. The hexagonal YbMn $O_3$with c-axis preferred orientation could be obtained at Rw=1 condition. The remanent polarization for the thin films of x=0 or 1 was about 200 nC/㎤ while, for the specimens ot 0< x< 1, were 50∼100 nC/$\textrm{cm}^2$.

Low Temperature Preparation of Transparent Glass-Ceramic Using Metal-Alkoxides (1) Synthesis and Properties of Porous Monolithic Gel in Li2O·1.7Al2O3·8.6SiO2 (금속 알콕시드를 이용한 투명 결정화유리의 저온 합성 (1) Li2O·1.7Al2O3·8.6SiO2 다공성 겔체의 합성)

  • Chun, Kyung-Soo;Tak, Joong-Jae
    • Applied Chemistry for Engineering
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    • v.18 no.6
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    • pp.568-574
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    • 2007
  • Crack-free dried gel monoliths of the composition $Li_2O1{\cdot}7Al_2O_3{\cdot}8.6SiO_2$ have been prepared as a precursor of transparent glass-ceramic by the hydrolysis and polycondensation of mixed metal alkoxides in solutions containing N,N-dimethylformamide as the drying control chemical additive, alcohols, and water. It was investigated that activation energy for gelation according to the variation of water concentration ranged from 13 to 14 kcal/mol. Only when the amount of water for gelation was 3 times higher than the stoichiometric amount, monolithic dry gels were successfully prepared after drying at $70{\sim}75^{\circ}C$ and at a rate of 0.1~0.3%/h. The specific surface area, the pore volume, the average pore diameters of dried gel at $180^{\circ}C$ were about $239.40m^2/g$, 0.001~0.03 mL/g, and $145.62{\AA}$, respectively. It showed that the dried monolithic gel had a porous body. The DTA curve had the first exothermic peak around $800^{\circ}C$ and the 2nd peak around $980^{\circ}C$, which may correspond to crystallization of the gel.

Nickel Film Deposition Using Plasma Assisted ALD Equipment and Effect of Nickel Silicide Formation with Ti Capping Layer (Plasma Assisted ALD 장비를 이용한 니켈 박막 증착과 Ti 캡핑 레이어에 의한 니켈 실리사이드 형성 효과)

  • Yun, Sang-Won;Lee, Woo-Young;Yang, Chung-Mo;Ha, Jong-Bong;Na, Kyoung-Il;Cho, Hyun-Ick;Nam, Ki-Hong;Seo, Hwa-Il;Lee, Jung-Hee
    • Journal of the Semiconductor & Display Technology
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    • v.6 no.3
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    • pp.19-23
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    • 2007
  • The NiSi is very promising candidate for the metallization in 45 nm CMOS process such as FUSI(fully silicided) gate and source/drain contact because it exhibits non-size dependent resistance, low silicon consumption and mid-gap workfunction. Ni film was first deposited by using ALD (atomic layer deposition) technique with Bis-Ni precursor and $H_2$ reactant gas at $220^{\circ}C$ with deposition rate of $1.25\;{\AA}/cycle$. The as-deposited Ni film exhibited a sheet resistance of $5\;{\Omega}/{\square}$. RTP (repaid thermal process) was then performed by varying temperature from $400^{\circ}C$ to $900^{\circ}C$ in $N_2$ ambient for the formation of NiSi. The process temperature window for the formation of low-resistance NiSi was estimated from $600^{\circ}C$ to $800^{\circ}C$ and from $700^{\circ}C$ to $800^{\circ}C$ with and without Ti capping layer. The respective sheet resistance of the films was changed to $2.5\;{\Omega}/{\square}$ and $3\;{\Omega}/{\square}$ after silicidation. This is because Ti capping layer increases reaction between Ni and Si and suppresses the oxidation and impurity incorporation into Ni film during silicidation process. The NiSi films were treated by additional thermal stress in a resistively heated furnace for test of thermal stability, showing that the film heat-treated at $800^{\circ}C$ was more stable than that at $700^{\circ}C$ due to better crystallinity.

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Bioinspired superhydrophobic steel surfaces

  • Heo, Eun-Gyu;O, Gyu-Hwan;Lee, Gwang-Ryeol;Mun, Myeong-Un
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.02a
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    • pp.509-509
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    • 2011
  • Superhydrophobic surfaces on alloyed steels were fabricated with a non-conventional method of plasma etching and subsequent water immersion procedure. High aspect ratio nanopatterns of nanoflake or nano-needle were created on the steels with various Cr content in its composition. With CF4 plasma treatment in radio-frequence chemical vapor deposition (r.-f. CVD) method, steel surfaces were etched and fluorinated by CF4 plasma, which induced the nanopattern evolution through the water immersion process. It was found that fluorine ion played a role as a catalyst to form nanopatterns in water elucidated with XPS and TEM analysis. The hierarchical patterns in micro- and nano scale leads to superhydrophobic properties on the surfaces by deposition of a hydrophobic coating with a-C:H:Si:O film deposited with a gas precursor of hexamethlydisiloxane (HMDSO) with its lower surface energy of 24.2 mN/m, similar to that of curticular wax covering lotus surfaces. Since this method is based on plasma dry etching & coating, precise patterning of surface texturing would be potential on steel or metal surfaces. Patterned hydrophobic steel surfaces were demonstrated by mimicking the Robinia pseudoacacia or acacia leaf, on which water was collected from the humid air using a patterned hydrophobicity on the steels. It is expected that this facile, non-toxic and fast technique would accelerate the large-scale production of superhydrophobic engineering materials with industrial applications.

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Synthesis of Periodic Mesoporous Organosilica by Microwave Heating

  • Yoon, Sang-Soon;Son, Won-Jin;Biswas, Kalidas;Ahn, Wha-Seung
    • Bulletin of the Korean Chemical Society
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    • v.29 no.3
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    • pp.609-614
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    • 2008
  • A periodic mesoporous organosilica material was synthesized by microwave heating (PMO-M) using 1,2-bis(trimethoxysilyl)ethane as a precursor in a cationic surfactant solution, and textural properties were compared with those of the product produced by conventional convection heating (PMO-C). These synthesized materials were characterized using XRD, TEM/SEM, N2 adsorption isotherm, 29Si and 13C NMR, and TGA, which confirmed their good structural orders and clear arrangements of uniform 3D-channels. Synthesis time was reduced from 21 h in PMO-C to 2-4 h in PMO-M. PMO-M was made of spherical particles of 1.5-2.2 m m size, whereas PMO-C was made of decaoctahedron-shaped particles of ca. 8.0 m m size. Effect of synthesis temperature, time, and heating mode on the PMO particle morphology was examined. The particle size of PMO-M could be controlled by changing the heating rate by adjusting microwave power level. PMO-M demonstrated improved separation of selected organic compounds compared to PMO-C in a reversed phase HPLC experiment. Ti-grafted PMO-M also resulted in higher conversion in liquid phase cyclohexene epoxidation than by Ti-PMO-C.

HMDS Treatment of Ordered Mesoporous Silica Film for Low Dielectric Application (저유전물질로의 응용을 휘한 규칙성 메조포러스 실리카 박막에의 HMDS 처리)

  • Ha, Tae-Jung;Choi, Sun-Gyu;Yu, Byoung-Gon;Park, Hyung-Ho
    • Journal of the Korean Ceramic Society
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    • v.45 no.1
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    • pp.48-53
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    • 2008
  • In order to reduce signal delay in ULSI, an intermetal material of low dielectric constant is required. Ordered mesoporous silica film is proper to intermetal dielectric due to its low dielectric constant and superior mechanical properties. The ordered mesoporous silica film prepared by TEOS (tetraethoxysilane) / MTES (methyltriethoxysilane) mixed silica precursor and Brij-76 surfactant was surface-modified by HMDS (hexamethyldisilazane) treatment to reduce its dielectric constant. HMDS can substitute $-Si(CH_3)_3$ groups for -OH groups on the surface of silica wall. In order to modify interior silica wall, HMDS was treated by two different processes except the conventional spin coating. One process is that film is dipped and stirred in HMDS/n-hexane solution, and the other process is that film is exposed to evaporated HMDS. Through the investigation with different HMDS treatment, it was concluded that surface modification in evaporated HMDS was more effective to modify interior silica wall of nano-sized pores.

Influence of Deposition Parameters on Film Hardness for Newly Synthesized BON Thin Film by Low Frequency R.F. PEMOCVD

  • G.C. Chen;J.-H. Boo;Kim, Y.J.;J.G. Han
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2001.06a
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    • pp.73-73
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    • 2001
  • Boron-containing materials have several excellent properties, such as superlnardness, insulation and non-Rinear optical property. Recently, oxynitride compounds, such as Si(ON), Ti(ON), became the promising materials applied in diffusion barrier layer and solar cell. With the expectation of obtaining the hybrid property, we have firstly grown the BON thin film by radio frequency (R.F.) plasma enhanced metalorganic chemical vapm deposition (PEMOCVD) with 100 kHz frequency and trimethyl borate precursor. The plasma source gases used in this study were Ar and $H_2$, and two kinds of nhmgen source gases, $N_2$ and <$NH_3$, were also employed. The as-grown films were characterized by XPS, IR, SEM and Knoop microlhardness tester. The relationship between the films hardness and the growth rate indicated that the hardness of the film was dependent on several factors such as nitrogen source gas, substrate temperature and film thickness due to the variation of the composition and the structure of the film. Both nitrogen and carbon content could raise the film hardness, on which nitrogen content did stronger effect than carbon. The smooth morphology and continuous structure was benefit of obtaining high hardness. The maximum hardness of BON film was about 10 GPa.

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Fabrication and Physicochemical Properties of Carbon/Titania/Bentonite Monolith for Architecture

  • Oh, Won-Chun;Choi, Jong-Geun;Song, Da-Ye;Kim, Ha-Rry;Chen, Ming-Liang;Zhang, Feng-Jun;Park, Tong-So
    • Korean Journal of Materials Research
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    • v.20 no.3
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    • pp.167-173
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    • 2010
  • In this study, we used activated carbon (AC) and titanium oxysulfate as a titanium precursor to prepare carbon/titania composites. We then mixed it with bentonite in different ratios to make a carbon/titania/bentonite monolith for use in architecture bricks by using Phenolic rosin (PR) as a bonding agent. The physicochemical properties of the prepared composites were analyzed by BET surface area, scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray analysis (EDX), self-cleaning effect and bactericidal tests. The BET surface areas increased as the ratio of carbon/titania composites increased. The SEM microscopy showed that the $TiO_2$ and bentonite were coated on the surface of the AC. The XRD patterns showed a mixture structure of anatase and rutile of $TiO_2$ with a clear $SiO_2$ structure. The EDX spectra of the carbon/titania/bentonite monolith confirmed the presence of various elements, namely C, O, Ti and Si, as well as other, impure elements. Moreover, to determine the self-cleaning effect of the carbon/titania/bentonite monolith, we used methylene blue (MB, $C_{16}H_{18}N_3S{\cdot}Cl{\cdot}3H_2O$) in an aqueous solution under the irradiation of visible light. Accordingly, all of the samples had excellent degradation of the MB solution. Furthermore, it was observed that the composites with sunlight irradiation had a greater effect on E. coli than any other experimental conditions.