• Resources Recycling
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• v.13 no.3
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• pp.37-42
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• 2004

PVC powder was dehydrochlorinated by hydrothermal reaction at reaction time 0∼5 hr, reaction temperature $200∼250^{\circ}C$ in 0∼2M NaOH solution, and shape and structure of the PVC residue was investigated. The shape of the residue was changed largely according to NaOH concentration. Most of the residue was cohered in the aqueous solution, and many pores less than 10 $\mu\textrm{m}$ were formed on the surface. Dense network structure was well developed inside the residue. On the other hand, the residue in the NaOH solution was not cohered and its shape is roughly spherical. In the IR spectrum of the residue both in water and NaOH solution at $250^{\circ}C$, aromatic rings and absorption peak by C=C double bond were observed. From the results, it was observed that aromatic circle reaction and bridge reaction occured inter and intra molecules.

• Proceedings of the Korea Association of Crystal Growth Conference
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• 1996.06b
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• pp.219-222
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• 1996

수열법은 밀폐용기중에서 10$0^{\circ}C$이상의 가열, 가압된 수용액이 반응에 관여하는 것으로써, 수정, CaCO3, AlPO4, GaPO4 등과 같은 단결정의 육성 뿐만 아니라 균일분산계로부터 균일한 결정성의 미립자 합성에도 폭넓게 이용되고 있다. 세라믹분말의 합성에 있어서, 이 방법은 특히 형상, 입자크기의 제어가 용이할 뿐만 아니라 고상법, 졸-겔법, 공침법에서와 같은 열처리, 분쇄과정이 필요없기 때문에 고순도의 초미립자를 얻을 수 있는 장점이 있다. 근년 미국, 일본에서는 수열법을 이용한 유전, 압전체 등 세라믹분말의 일부가 공업적인 규모로 대량 생산되고 있다. 그러나 이에 대한 국내 기술은 아직 초기단계에 이르고 있는 실정이다. 따라서 본 연구실에서는 수열법에 의한 단결정 육성 (예; 자수정, CaCO3, AlPO4, GaPO4, KTP, Emerald 등), 박막제조 (예; GaP, PbTiO3, BaTiO3 등), 정제 (고령토, 장석, 도석 등), 원석처리 (진주, 인공 emerald, 비취 등) 그리고 각종 세라믹분말의 합성 등과 같은 다양한 기반기술의 축적과 동시에 공업화에 대응한 수열장치를 위하여 반응용기의 대형화, 엄밀한 밀폐방식, 실용적인 수열조건 등을 개발해 오고 있다. 본 발표에서는 현재까지의 연구개발 내용 중에서 결정성 미립자에 관련한 세라믹분말의 합성에 대한 일부의 결과들을 보고한다. 일반적으로 수열장치는 전기로, 반응용기, 온도 및 압력제어계 등을 기본으로 하고 있으며 시판용의 대부분이 교반기가 부착된 수직형 (vertical type)이다. 이와 같은 방식에 있어서는 엄밀한 밀폐가 곤란, 반응온도의 한계성 (25$0^{\circ}C$ 이하), 증진율의 한계성 (소량생산) 등과 같은 점이 있기 때문에 본 연구실에서는 개폐식 전기로내에 엄밀한 밀폐가 가능한 수평식(horizontal type)의 반응용기를 채택한 뒤 이를 회전 또는 시이소(seesaw)식으로 움직일 수 있도록 하여 연속공정화, 온도구배의 자율조절 그리고 보다 저온에서도 인위적인 이온의 확산을 효율적으로 유도할 수 있도록 하였다. 이와 같은 방식은 기존의 방식과 비교하여 반응용기 내에 응집현상과 미반응물이 존재하지 않으며 또한 단분산으로 결정성 미립자를 대량적으로 얻을 수 있는 장점이 있었다. 다음은 이상과 같이 본 연구실에서 자체 개발한 수열장치를 이용하여 PbTiO3, (Pb,La)TiO3Mn, BaTiO3, ZnSiO4:Mn, CaWO4 등과 같은 세라믹분말에 대한 합성 실험의 결과이다. 압전성, 초전성이 우수한 PbTiO3 및 (Pb,La)TiO3:Mn 분말의 수열합성은 PbO, TiO2, La2O3 등의 분말을 출발원료로 하여 합성도도 25$0^{\circ}C$부근의 알카리성 용액중에서 결정성 PbTiO3 및 (Pb,La)TiO3:Mn 미립자를 단상으로 얻었으며 입자의 형상 및 크기는 합성온도와 수열용매의 종류에 의존하였다. 유전체로서 폭넓게 응용되고 있는 BaTiO3 분말은 Ba(OH)2.8H2O, TiO2와 같은 최적의 출발원료를 선택함으로써 15$0^{\circ}C$ 부근의 저온영역에서도 용이하게 합성할 수 있었다. 특히 본 연구에서는 수용성인 Ba(OH)2.8H2O를 사용함으로써 host-guest적인 반응을 유도시키는데 있어 물의 가장 실용적이고 효과적인 수열용매임도 알았다. ZnSiO4:Mn, CaWO4, MgWO4와 같은 형광체 분말은 공업적으로 고상반응 또는 습식법에 의해 얻어지고 있으나 이들 방법에 있어서는 분쇄공정으로 인한 형광특성의 저하와 같은 문제점이 있다. 따라서 본 연구에서는 수열법을 이용하여 이들 화합물의 합성을 시도하였으며 그 결과 합성온도 30$0^{\circ}C$ 부근의 알칼리성 용액중에서 수열적으로 얻어짐을 알았다. 여기서의 합성분말을 이용하여 실제 조명램프로 제조한 결과 녹색, 청색 발광용 형광체로서 우수한 형광특성을 나타내었다. 천연에서 소량 산출되고 있는 고가의 (Li,Al)MnO2(OH)2:Co 분말은 도자기의 전사지용 청색안료로써 이용되고 있다. 본 연구실에서는 LiOH.H2O, Al(OH)3, MnO2 등의 분말을 출발원료로 하고 24$0^{\circ}C$ 온도 부근 그리고 물을 수열용매로 하여 천연산에 필적하는 (Li,Al)MnO2(OH)2:Co 분말을 인공적으로 합성하였다.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.4 no.2
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• pp.139-147
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• 1994

Orthophosphate crystals were grown by the hydrothermal method and the properties of grown crystals were investigated by means of X-ray diffraction. Vickers hardness tester, etc. The starting powders of $AIPO_4 and GaPO_4 $were prepared as a single phase by the solid state reaction of stoichiometric mixture of $AI_2O_3 or Ga_2O_3$ and $NH_4H_2PO_4$ and the subsequently by the hydrothermal treatment. The hydrothermal conditions for high growth rates of the orthophosphate crystals are as follows: $AlPO_4$ crystal; temperature ranges, between $170$~$200^{\circ}C$; temperatures difference, $15$~$20^{\circ}C;$, hydrothermal solvent, 4m HCl, $GaPO_4 crystal; temperature ranges, between $210 and 240^{\circ}C;$; temperature difference, $25$~$30^{\circ}C; $, hydrothermal solvent, 4m HCl. Morphologies of grown crystals tended to be bounded by (1010), (1011) and (0111) faces at low temperatures, and grew with well developed (0001) faces by increasing the growth temperature. On the other hand, the properties of orthophosphate crystals $(AlPO_4/GaPO_4)$ were as follows: lattice parameters (nm); a=0.494, c=1.094/a=0.490, c=1.105, density (gcm-3); 2.62/3.56, Vickers hardness (Nm^2); $1.02{\times}10^1^0/7.06{\times}10^9$, refractive indices; $ne=1.529{\pm}0.003, no=1.519{\pm}0.003/ne=1.611{\pm}0.006, no=1.599{\pm}0.006, birefringence; {\pm}0.01/{\pm}0.012$, dielectric constant (Fm-1); 6/7.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.3 no.1
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• pp.12-17
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• 1993

Growth runs of KTP single crystals were carried out by the hydrothermal method. KTP powders used for the crystal growth were prepared as a single phase by the solid state reaction of a stoichiometric mixture of $KH_2PO_4 and TiO_2$ at TEX>$800^{\circ}C$ and subsequently by the hydrothermal treatment at $250^{\circ}C$ 4m KF solution. The most effective solvents for the crystal growth of KTP were KF and K $K_2HPO_4$ solutions. Solubilities of KTP in these solutions were positive over the range $350~450^{\circ}C$.Seed crystals of good quality could be obtained by the horizontal temperature gradient method at temperatures over the range 380~430^{\circ}C$ in these solutions. The hydrothermal conditions for the high growth rates of seed crystals are as follows: growth method; vertical temperature gradient method, solvent; 4m KF or $K_2HPO_4$ solution, temperature region; $400~450^{\circ}C$, pressure region; $1000~1500kg/cm^2$, where solubility of KTP was large enough to proceed the growth. Under such conditions, seed crystals of KTP are grown at a rate of approximately 0.06-0.08mm/day in the direction of the c-axis. Morphologies of grown crystals tended to be bounded by (100), (011) and (201) faces.

• Journal of the Korean Ceramic Society
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• v.39 no.3
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• pp.245-251
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• 2002

We prepared γ-alumina beads using the amorphous alumina, obtained by fast calcination of gibbsite, and its were immersed in aqueous solution of the mixture of 21.87% nitric acid and 28.57% acetic acid. The beads thus were hydrothermaly treated at 200$^{\circ}$C for 3h, and were investigated changes of crystal, pore characteristics, $N_2$ adsorption and desorption isotherms, mechanical strengths and thermal resistance. Acicular platelet crystals of 0.1∼0.3${\mu}$m were transformed into acicular boehmite crystals of 1∼2${\mu}$m having the same crystal structure. Through this changes, we found that reversible phase transformation due to hydrothermal reaction took placed between boehmite and ${\gamma}$-alumina. In comparison to the ${\gamma}$-alumina bead before hydrothermal treatment, $N_2$ adsorption capacity was increased from 450㎖/g to 670㎖/g, and pore volume between 100${\AA}$ and 1000${\AA}$ was increased form 0.15㎖/g to 0.77㎖g, and mechanical strength was increased form 1.4MPa to 2.2MPa. Also, it showed the remarkable thermal resistance which sustained ${\theta}$-alumina crystal structure and pores between 100${\AA}$ and 1000${\AA}$ at 1000$^{\circ}$C in 40vol% steam.

• Journal of the Korean Ceramic Society
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• v.40 no.8
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• pp.758-764
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• 2003

The cylindrical ${\gamma}$-alumina pellets were prepared by forming, hydration, drying and calcination after mixing amorphous alumina and pore generating agent with water. Concentration of Fe(NO$_3$)$_3$ㆍ9$H_2O$ that was catalyst precursor was fixed and made mixing solution that changed concentration of $CH_3$COOH in range of 2.5~20%, and here ${\gamma}$-alumina pellets were immerged and were hydrothermaly treated for 3 h at $200^{\circ}C$. And then we investigated creation and change of crystal, pore characteristics, $N_2$ adsorption and desorption isotherms, changes of acid site and mechanical strengths etc. According to the concentration of $CH_3$COOH, the crystals grew to acicular shape of 0.5~2${\mu}m$ length, and crystal structure showed the pseudo-boehmite structure. When hydrothermaly treated in 10% $CH_3$COOH solution, pore volume between 100~1000 $\AA$ was highest by 0.86 cc/g, and width of hysteresis curved line due to $N_2$ adsorption/desorption appeared as was smallest. When concentration of $CH_3$COOH was in range of 5~15%, new C-H functional groups were formed. Mechanical strength of pellets was highest by 1.35 MPa when $CH_3$COOH concentration was 2.5%.

• Journal of the Korean Ceramic Society
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• v.40 no.7
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• pp.683-689
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• 2003

The cylindrical ${\gamma}$-alumina pellets were prepared using amorphous alumina and pore generating agent. Its were immersed in aqueous solution of the mixture of Fe(NO$_3$)$_3$.9$H_2O$ and $CH_3$COOH, Fe(NO$_3$)$_3$.9$H_2O$ and $CH_3$COOH and HNO$_3$, and Fe(NO$_3$)$_3$.9$H_2O$ and HNO$_3$. The pellets thus were hydrothermally treated at 20$0^{\circ}C$ for 3 h in autoclave, and were investigated morphologies and changes of crystal pore characteristics, $N_2$ adsorption and desorption isotherms, active sites and mechanical strength etc. According to the preparation method, acicular platelet pseudo-boehmite crystals of 0.1~0.3 ${\mu}{\textrm}{m}$ size were transformed into acicular pseudo-boehmite cristals of 0.5~2 ${\mu}{\textrm}{m}$ size having the same crystal structure. When ${\gamma}$-alumina pellets were immersed in aqueous solution of the mixture of Fe(NO$_3$)$_3$.9$H_2O$ and $CH_3$COOH and then were hydrothermally treated, pore volume between 100 $\AA$ and 1000 $\AA$ was increased from 0.34 ㏄/g to 0.86 ㏄/g, and the gap of $N_2$ adsorption and desorption hysteresis loop was decreased due to increasement of pore size. New active site that could adsorb the C-H functional group was created on the catalist. Also, mechanical strength of catalyst was increased from 1.06 ㎫ to 1.36 ㎫.

• Applied Chemistry for Engineering
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• v.20 no.2
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• pp.234-240
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• 2009

$Mg(OH)_2$ particles were prepared by precipitation and a hydrothermal treatment to examine the effect of $MgCl_2$ concentration, alkali type and concentration, temperature, hydrothermal treatment on the formation of $Mg(OH)_2$ particles using full factorial design, as one of DOE (Design of experiment) methods. The primary particle size is similar to the secondary particle size for the samples after the hydrothermal treatment, where the average particle size of $Mg(OH)_2$ increased with increasing the concentration of $MgCl_2$ and hydrothermal temperature and decreasing alkali/Mg molar ratio. On the other hand, for the samples prepared from precipitation, the secondary particle size is larger than the primary particles due to aggregation. The difference in alkaline source is that the particles prepared from $NH_4OH$ exhibit the larger size with better dispersion than those from NaOH. Low density polyethylene and ethylene-co-vinyl acetate (LDPE-EVA) resin composed of the smaller secondary particle size of $Mg(OH)_2$ shows a higher limited oxygen index (LOI) at 50 and 55% loading, but the smaller primary particle size may result in a better grade in UL-94 tests. At the high loading of 60%, all samples with any preparation methods exhibit V-0 grade but the LOI value depends on not only primary particle size but also dispersion state.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2005.07a
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• pp.35-37
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• 2005

100, 200nm 크기의 colloidal silica 각각에 나노 ceria 입자를 수열합성법으로 코팅하였다. Colloidal silica 입자에 ceria를 코팅 시 slurry의 pH조절과 수열처리에 이용하여 silica에 ceria가 코팅됨을 TEM과 zeta-potential을 이용하여 확인하였다. 연마 슬러리의 분산 안정성과 연마효율을 높이기 위하여 슬러리의 pH 는 9로 하였으며, 이때의 zeta-potential 값은 -25 mV이었다. 1 wt%로 제조된 연마슬러리를 이용하여, 4 inch $SiO_2$, $Si_3N_4$ wafer를 압력변화에 따른 연마특성을 관찰 하였다. Ceria coated colloidal silica 100 nm, 200 nm와 commercial한 $CeO_2$입자를 연마압력 6 psi로 oxide film을 연마한 결과 연마율이 각각 2490 ${\AA}/min$, 4200 ${\AA}/min$, 4300 ${\AA}/min$으로 측정되었다. 또한 $SiO_2$, $Si_3N_4$ film의 6 psi압력에서 ceria coated colloidal silica 100 nm, 200 nm와 commercial 한 $CeO_2$입자의 선택비는 3, 3.8, 6.7 이었다. 입자크기가 클수록 연마율이 높으며, Preston equation을 따라 연마 압력과 연마율이 비례하였다.

• Journal of Broadcast Engineering
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• v.4 no.2
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• pp.144-154
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• 1999

The binomial sequences are family of orthogonal sequences that can be generated with remarkable simplicity-no multiplications are necessary. This paper introduces a class of non-recursive multidimensional filters for frequency-selective image processing without multiplication operations. The magnitude responses are narrow-band. approximately gaussian-shaped with center frequencies which can be positioned to yield low-pass. band-pass. or high-pass filtering. Algorithms for the efficient implementation of these filters in software or in hardware are described. Also. we show that the binomial QMFs are the maximally flat magnitude square Perfect Reconstruction paraunitary filters with good compression capability and these are shown to be wavelet filters as well. In wavelet transform the original image is decomposed at different scales using a pyramidal algorithm architecture. The decomposition is along the vertical and horizontal direction and maintains constant the number of pixels required to describe the images. An efficient perfect reconstruction binomial QMF-Wavelet signal decomposition structure is proposed. The technique provides a set of filter solutions with very good amplitude responses and band split. The proposed binomial QMF-filter structure is efficient, simple to implement on VLSl. and suitable for multi-resolution signal decomposition and coding applications.