• 공업화학
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• 제17권2호
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• pp.188-193
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• 2006

용액의 pH, 주입방법, 온도, 유량의 변화를 주면서 질산알루미늄($Al_{3}(NO_{3})_3{\cdot}9H_{2}O$)을 암모니아수($NH_{4}OH$)로 침전시켜 베마이트(Boehmite)를 합성하였다. 베마이트 상이 형성되는 pH 범위와 입자의 형상과 기공특성에 미치는 합성 조건의 영향을 조사하였다. 베마이트는 반응 용액의 pH가 7.5~9일 때 형성되었고, P2jet 주입방법은 침전이 일어나는 동안 pH를 일정하게 유지할 수 있어 용액내의 반응에 참여하는 이온의 농도가 일정하게 유지되어 균일한 크기의 입자와 기공을 형성할 수 있게 하였다. 따라서 비표면적과 기공부피 두 가지 동시에 향상되었다. 온도가 올라갈수록, 유량이 감소할수록 비표면적과 기공부피가 증가함을 보이고, $60^{\circ}C$ 이상에서는 미세섬유모양의 입자를 얻을 수 있었다. 최적의 조건은 pH 9에서 P2jet 방법으로 주입하고 반응온도 $90^{\circ}C$와 유량 2.5 mL/min을 유지하였을 경우로 비표면적은 $385.46m^2/g$이고 기공 부피는 1.0252 mL/g을 가지는 평균 10 nm의 기공이 형성된 다공성 베마이트를 얻을 수 있었다.

• 한국세라믹학회지
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• 제43권9호
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• pp.564-568
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• 2006

AlO(OH) nano gel is used in precursor of ceramic material, coating material and catalyst. For use of these, not only physiochemical control for particle morphology, pore characteristic and peptization but also studies of synthetic method for preparation of advanced application products were required. In this study, AlO(OH) nano gel was prepared through the aging and drying process of aluminum hydroxides gel precipitated by the hydrolysis reaction of dilute NaOH solution and aluminum sulfate solution. In this process, optimum synthetic condition of AlO(OH) nano gel having excellent pore volume as studying the effect of water and aluminum sulfate mole ratio on gel precipitates has been studied. Water and aluminum sulfate mole ratio brought about numerous changes on crystal morphology, surface area, pore volume and pore size. Physiochemical properties were investigated as using XRD, TEM, TG/DTA, FT-IR, and $N_2$ BET method.

• 대한화학회지
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• 제13권2호
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• pp.149-156
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• 1969

$NaAl(OH)_2CO_3$was synthesized using colloidal earth (Allophane) as the starting material and some of its were studied in detail. It was found that Dawsonite was formed in the pH range (pH 12.5~12.0) that the concentration of $HCO_3^-$ was just begun to increase and the presence of $HCO_3^-$ in the product was clarified from the infrared absorption spectrum. The chemical formular of Dawsonite was therefore presumed as $NaAlO (OH) HCO_3$. From toahhe results of X-ray powder diffraction, both peaks at 5.7 $\AA$ and 2.8 $\AA$ were observed, and fibrous crystalline structure was observed from electron micrograph and also found from the microscopic electron diffraction at 5.7 $\AA.$ Therefore the fibrous axis was considered as =Al=O2=Al=O2=Al=(*image) direction. True specific gravity of Dawsonite was 2.44 and its porosity was 91.4%. It was practically insoluble in water, but decomposed in the boiling water to form Pseudo Boehmite. Stable pH range of Dawsonite was about 4.5~11.5. From the results of D.T.A. and T.G.A., it was observed that $CO_2$was liberated at $350^{\circ}C$, and $H_2O$ at $650^{\circ}C$, and converted into strongly hygroscopic $NaAlO_2$, which was easily decomposed in water into $\beta-Al(OH)_3(Bayerite)$ and NaOH.

• 한국재료학회지
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• 제11권11호
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• pp.978-985
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• 2001

The amorphous alumina was obtained by flash calcination of Bayer gibbsite[$Al(OH)_3$aluminum trihydroxide]. Rehydration and pore characteristics of $r-A1_2O_3$ prepared from rehydrated amorphous alumina were investigated. Crystal phases of pseudo-boehmite and bayerite were changed when amorphous alumina was hydrated at various conditions such as time, the ratio of water/alumina and pH. Specific surface areas and pore volumes of $r- A1_{2O}_3$ were influenced by the reaction time, water/alumina and PH of rehydration. The total pore volume of $r-A1_{2O}_3$increases with increasing the reaction time and ratio of water/alumina. Especially, the pure pseudo-boehmite of single phase could be prepared, when amorphous alumina was hydrated in the range of pH 6.5-8.0 in water/alumina= 10 at $90^{\circ}C$ for 7hr. The $r-Al_{2O}_3$, obtained by calcination of the prepared pseudo-boehmite at $500^{\circ}C$ for 2hrs, is characterized by the specific surface area of $265m^2$/g, total pore volume of $0.75cm^3$/g.

• 한국세라믹학회지
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• 제43권9호
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• pp.575-581
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• 2006

To precipitate the complex gel of flux and aluminum hydroxides gel, aqueous solution of the mixture of $Na_2CO_3\;and\;Na_2PO_4{\cdot}12H_2O$ was added with stirring in aqueous solution of the mixture of $Al_2(SO_4)_3{\cdot}14{\sim}18H_2O,\;Na_2SO_4$, and then the complex gel was aged in $0{\sim}30h\;at\;90^{\circ}C$. As aging time passed, the aluminum hydroxides was grown into the acicular AlO(OH) gel. Also, aging time had an effect on physical properties of the AlO(OH) gel and on crystal growth of the flaky ${\alpha}-Al_2O_3$ prepared by molten-salt precipitation. In this study, the complex gel was crystallized in temperature range of $400{\sim}1,200^{\circ}C$ after drying at $110^{\circ}C$, and then it was investigated to effect of aging time on precipitation temperature, size, thickness, morphology and particle size distribution of the flaky ${\alpha}-Al_2O_3$ crystal. As aging time passed, the flaky a${\alpha}-Al_2O_3$ crystal showed a tendency toward an increase in size and thickness as result from an increase in BET surface area and pore volume of the acicular AlO(OH) gel.

• 한국세라믹학회지
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• 제25권2호
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• pp.111-116
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• 1988

Aluminum hydrates were prepared by precipitation method using Al2(SO4)3$.$18H2O as a starting material and NH4OH as precipitation agent. The phases of aluminum hydrate were changed from amorphous aluminum hydrate to pseudo-boehmite of AlOOH form and bayerite, gibbsite, hydragillite and norstrandite of Al(OH)3 form with increasing pH. As pH increased, agglomeration phenomena were reduced. Aluminum hydrates of AlOOH and Al(OH)3 form represented dehydration of structural water near 175$^{\circ}C$ and 385$^{\circ}C$, and 280$^{\circ}C$, respectively. As the ratio of Al(OH)3 to AlOOH increased, specific surface area was reduced.

• 대한화학회지
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• 제13권2호
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• pp.157-164
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• 1969

Aoolphane was treated with 30% Hydrochloric acid at $18^{\circ}C$ for two hows with stirring in order to obtain the insoluble form of SiO2 gel and to extract quantitatively both $Al_2O_3$as and $Fe_2O_3AlCl_3{\cdot}6H_2O Fe$ and $Cl_3{\cdot}6H_2O$ forms, respectively, at the same time. $SiO_2$ gel was filtered and to the filterate Ammonia was added to precipitate $Al(OH)_3[Fe(OH)_3 Contaminated ]$ The precipitate was separated by filteration and the filterate was recovered as the form of $NH_4Cl$. The precipitate was treated with 200g (NaOH)/l Concentration of NaOH a little excessively to the equivalent at $65~70^{\circ}C$ as $Fe(OH)_3$ formed was insoluble, it was filtered of and to the filterate containing $NaAl(OH)_4(OH_2)_2$Carbon dioxide gas was bubbled at $50^{\circ}C~90^{\circ}C$ to obtain the precipitate with excellent filterability and crystallinity. The product was certified to be Dawsonite $(NaAl(OH)_2CO_3)$ by X-Ray diffraction analysis at below $40^{\circ}C$, when $CO_2$ gas was bubbled into the relatively lower concentration of $NaAl(OH)_4(OH_2)_2$ solution, the precipitate of very fine particles was formed, which was hard to filter and with the Composition of $\alpha-Al_2O_3-H_2O$ (Boehmite).

• 한국광물학회지
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• 제20권3호
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• pp.147-153
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• 2007

비정질 $SiO_2$과 $Al(OH)_3$를 출발물질로 이용하여 $230^{\circ}C,\;30 kg/cm^2$에서 결정성이 우수한 캐올리나이트를 수열합성하였다. 실험범위는 pH $0.3{\sim}9.5$, 화학조성($Al_2O_3/SiO_2 = 0.5{\sim}0.37$), 온도 $180{\sim}280^{\circ}C$, 압력 $10{\sim}60kg/cm^2$이었다. 비정질 $SiO_2$와 $Al(OH)_3$를 화학양론적 조성으로 혼합하면 캐올리나이트와 함께 보에마이트가 미량으로 공존하였으며 $Al_2O_3/SiO_2$ 몰비가 0.45일 때, 캐올리나이트가 단일상으로 합성되었다. $200^{\circ}C$ 이하에서는 240시간의 반응 후에도 보에마이트만 관찰되었지만 $230^{\circ}C$에서는 20시간 반응 후에 캐올리나이트가 안정상으로 합성되었다. 그리고 pH는 캐올리나이트 합성에 중요한 인자로서 pH $2{\sim}6$ 범위에서 결정성이 양호한 합성상이 관찰되었다. 합성된 캐올리나이트의 분말 X-선 회절패턴은 자연산 캐올리나이트와 일치하였고 (001) 회절선들이 잘 발달되어 있었다. 캐올리나이트는 직경 ${\sim}3{\mu}m$의 균질한 구형 결정군집 (clusters)들로 이루어져 있었다.

• Korean Chemical Engineering Research
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• 제46권3호
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• pp.545-549
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• 2008

${\gamma}-AlO$(OH) 졸 입자 뿐만 아니라 소성처리된 ${\gamma}-Al_2O_3$ 입자의 표면특성을 ${\gamma}-AlO$(OH) 졸 제조시 숙성단계에 의하여 조절하였다. 연구결과, ${\gamma}-AlO$(OH) 졸 입자의 등전점은 숙성 증가에 따라 pH 9.25에서 pH 8.70까지 감소하였으며 ${\gamma}-Al_2O_3$ 입자의 경우는 pH 9.90에서 pH 8.86까지 감소하였다. 숙성에 따른 ${\gamma}-Al_2O_3$ 입자의 산, 염기 특성을 고찰한 결과, ${\gamma}-Al_2O_3$ 입자의 산량은 숙성시간의 증가에 따라 0.1367 mmol/g에서 0.0783 mmol/g까지 감소하였으며, Hammett 산성도함수 $H_o$는 4.8 이상의 산세기를 보였다. 한편 ${\gamma}-Al_2O_3$ 입자의 염기량은 숙성시간의 증가에 따라 0.4399 mmol/g에서 0.3074 mmol/g 까지 감소하였다. 따라서 졸-겔법에 의한 ${\gamma}-Al_2O_3$ 제조시 숙성공정이 산, 염기점의 양을 포함한 표면특성을 조절할 수 있는 중요 공정변수임을 제시하였다.

• 한국광물학회지
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• 제22권3호
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• pp.241-248
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• 2009

비정질 $SiO_2$와 $Al(OH)_3{\cdot}xH_{2}O$를 출발물질로 하여 $250^{\circ}C$, $30\;kg/cm^2$의 조건에서 반응시간을 2~36시간까지 변화시키면서 캐올리나이트를 수열합성하였다. 합성된 캐올리나이트에 대하여 XRD, IR, TG-DTA, TEM 및 EDS를 사용하여 특성분석을 실시하였으며, 이로부터 합성된 캐올리나이트의 반응 시간별 광물학적 특성변화를 규명하고자 하였다. X선 회절 분석결과, 반응시간 2시간에 비정질 출발물질에서부터 뵈마이트가 결정화되었으며 2시간 이상 반응시키면, 뵈마이트 피크가 소멸되거나 혹은 감소하였다. 캐올리나이트는 반응 10시간 이후 생성되기 시작하였으며 반응시간의 증가에 따라 결정도가 점차 증가하였다. TGA 분석결과, 반응시간 36시간 이후에 약 13 wt%의 총중량손실이 관찰되었으며 DTA 분석결과 $258^{\circ}C$에서 관찰된 뵈마이트에 의한 발열피크는 서서히 감소되어 반응시간 10시간 이후에 관찰되지 않았고 스피넬상으로의 전이를 나타내는 발열피크는 반응시간 5시간 이후에 관찰되기 시작하여 반응시간 증가에 따라 피크강도가 증가되었다. FT-IR 분석 결과, 합성 캐올리나이트의 Al-OH 신축진동 밴드인 $3696\;cm^{-1}$과 $3620\;cm^{-1}$사이에서 $3670\;cm^{-1}$과 $3653\;cm^{-1}$의 두개의 작은 피크 분리 및 $940\;cm^{-1}$과 $915\;cm^{-1}$에서 관찰된 캐올리나이트의 특징적인 흡수띠의 관찰은 비교적 질서도가 우수한 캐올리나이트가 합성된 것을 지시하였다. TEM 분석결과, 반응시간 15시간 후에서야 비로소 (001)면의 성장으로 판상형의 캐올리나이트가 형성되었다. 반응시간 36시간 후 합성 캐올리나이트는 단순 판상형에서 육각외형의 판상형으로 변화됨을 확인되었다.