• 한국세라믹학회지
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• 제41권11호
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• pp.864-871
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• 2004

폐 염화알루미늄(AlCl$_3$) 수용액과 수산화나트륨(NaOH) 용액의 가수분해 반응에 의해 무정형의 수산화알루미늄 겔을 석출시키고, 이를 숙성하여 다공성 유사베마이트(pseudo-boehmite) 겔을 제조하였다 pH를 7.6～11.6 범위로 조절하고 반응온도를 60～10$0^{\circ}C$로 변화시켜 2～24시간 숙성시켰을 때, 겔 침전물의 결정변화, 적외선흡수스펙트럼의 변화, 비표면적 및 기공구조의 변화를 조사하여 최대 기공부피를 갖는 유사베마이트 겔의 제조조건을 확립하였다. pH 7.6～9.6 범위에서 석출된 겔 침전물로부터 250～357 $m^2$/g 정도의 비표면적과 0.4～0.74 cc/g의 기공부피 그리고 58～l14$\AA$의 평균기공크기를 갖는 다공성 유사베마이트가 제조되었으며, pH 10.6～11.6 범위에서 석출된 겔 침전물로부터는 기공이 거의 없는 베이어라이트(bayerite)가 제조되었다.

• 한국세라믹학회지
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• 제31권1호
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• pp.79-87
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• 1994

AIN은 불안정하여 물과 접촉하면 12시간 이내에 172cal/g의 열을 내면서 가수분해되어 알루미나 삼수화물이 생성되었다. AIN의 가수분해 과정은 초기에 비정질 알루미나 수화물이 생성되었으며, 가수분해 조건에 따라 비정질알루미나 수화물의 용해-재석출과정으로 알루미나 삼수화물 특히 bayerite가 생성되었고, 응축과정으로 pseudo-boe-hmite가 AIN 입자표면에 생성되었다. 가수분해 온도 4$0^{\circ}C$ 이하에서는 비정질 알루미나 수화물이, 4$0^{\circ}C$와 6$0^{\circ}C$ 사이에서는 bayerite가 각각 생성되었고, 6$0^{\circ}C$ 이상의 경우는 초기에 pseudo-boehmite의 입자표면에 형성되었다. bayerite는 가수분해 시간이 길수록, 그리고 용액내 pH가 높을수록 잘 생성되었으나 pseudo-boehmite는 가수분해 반응이 급격히 일어날 때와 용액내 ethyl alcohol의 존재로 OH 기의 흡착을 방해하여 가수분해 반응이 억제될 때 잘 생성되었다. 그리고 pH=2.0인 용액에서는 AIN의 가수분해가 거의 일어나지 않았다.

• 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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• 제26권3호
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• pp.445-451
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• 1989

Hydrolysis of aluminum isopropoxide with excess water in the presence of excess isopropyl alcohol resulted in the formation of boehmite in independence of temperature of hydrolysis and aging. Stoichiometric and substoichiometric amount of water hydrolyzed aluminum isopropoxide to pseudo-boehmite and amorphous one, respectively. $\alpha$-Al2O3 with 0.3${\mu}{\textrm}{m}$ in median size was produced by calcination of boehmite, bseudo-boehmite and amorphous boehmite at 125$0^{\circ}C$, 120$0^{\circ}C$, and 115$0^{\circ}C$ for one hour, respectively. Singnificant reduction in particle size was found during transition from $\theta$-Al2O3 to $\alpha$-Al2O3. $\alpha$-Al2O3 produced in this study was relatively uniform spherical and its purity was found to be over 99.9%.

• 한국세라믹학회지
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• 제33권5호
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• pp.547-555
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• 1996

Porous alumina ceramics were fabricated by pseudo-boehmite phydosol-gel process within/without commercial $\alpha$-alumina particles average 1 and 40 micron respectively. The pore characteristics of fired specimens were studied by the measurement of bulk density total porosity thyermal analysis pore volume pore distribution BET area XRD and SEM. with increasing of firing temperature pore volume and BET surface area were decreased and the average pore size was increased to approximately 146$\AA$ upto 80$0^{\circ}C$ by de-watering of [OH] and formation of $\alpha$-alumina. The fired relative density of the alumina-dispersed specimen with average 1 micron particle was increased with the amounts of dispersed particle by bimodal packing theory which is compared to the ones of specimen including of average 40 micron particle. It was confirmed that the percola-tion threshold in porous ceramics with coarser particle (40 micron) has formed between the transformed-alumina from hydrogel and dispersed-alumina of above 50 vol% particle and the total porosity was increased at the threshold point above.

• 한국세라믹학회지
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• 제30권12호
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• pp.1029-1038
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• 1993

The microstructures of aluminas, included of dissolved CaO as $\alpha$-alumina seeded pseudo-boehmite hydrosol was gelled in plaster mold and doped of MgO as dipping of calcines(120$0^{\circ}C$-2h) into Mg-nitrate solution, were compared to the one of which additives are excluded during the gellation. It was formed the boundary layer of 300~350${\mu}{\textrm}{m}$ distance from surface to the inside, containing of approximately 500ppm CaO by dissolved Ca from plaster mold. As the MgO addition to the boundary layer with dissolved CaO, the microstructure of the layer was uniformed and inhibited the grian growth, compared to one of that additives be excluded specimen and of MgO doped-inside region. This result was considered as abnormal grain growth and effect of flat boundary formation be appeared by effects of dissolved CaO, were decreased by MgO co-doping.

• 공업화학
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• 제5권4호
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• pp.597-608
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• 1994

$(NH_4)_2SO_4$와 저품위 bauxite의 황산화 반응에 따라 얻어진 ammonium aluminium sulfate로부터 수열균일침전을 통해 무정형 alumina gel수화물 및 결정형 boehmite를 합성하고 이로 부터 고순도 $Al_2O_3$를 제조하는 새로운 공정 개발을 시도하였다. 이 공정은 ammonium aluminium sulfate용액 중의 Fe 성분을 제거하기 위한 용매추출공정과 정제된 ammonium aluminium sulfate용액으로부터 균일침전에 의한 Al 함유 침전물의 생성에 관한 것으로 이루어져 있다. 추출제 Alamine 336에 의한 적절한 용매추출조건은 shaking time 4분, 수상에 대한 유기상의 비 0.25였다. Urea를 이용한 수열균일 침전반응은 Al 함유용액 중의 Al에 대한 urea의 당량비 6.0의 조건에서 반응온도 $100^{\circ}C$ 이하에서는 무정형 alumina gel 수화물, $120^{\circ}C$ 이상 $150^{\circ}C$ 이하에서는 pseudo boehmite 그리고 $150^{\circ}C$ 이상에서는 결정형 boehmite가 합성되었다. 이 합성된 무정형 alumina gel 수화물은 소성시간 2시간, 소성온도 $1000^{\circ}C$ 이상에서 그리고 결정형 boehnite는 소성시간 2시간, 소성온도 $1250^{\circ}C$ 이상에서 ${\alpha}-Al_2O_3$로 전이되며 얻어진 ${\alpha}-Al_2O_3$의 순도는 99.97%의 고순도였다.

• 한국세라믹학회지
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• 제42권5호
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• pp.338-345
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• 2005

To prepare the complex gel of flux and pseudo-boehmite used in precursor of the flaky ${\alpha}-A1_2O_3$ crystal, aqueous solution of the mixture of sodium carbonate and sodium phosphate was added with stirring in aqueous solution of the mixture of sodium sulfate, potassium sulfate and titanium sulfate. The complex gel was dried at $110^{\circ}C$ and was crystallized above $1,050^{\circ}C$, and then the effect of the amount of titanium sulfate on size, morphology, thickness and crystal size distribution of the flaky ${\alpha}-A1_2O_3$ crystal was investigated. Addition of titanium sulfate was prevented the aggregation and generation of twin crystal, and had an effect on the crystal size and the thickness during crystal growth. When the amount of titanium sulfate was more than 6 g, particle size was decreased but was free from crystal twining and aggregation. On the other hand, when the amount of titanium sulfate was lower than 6 g, crystal size was increased but crystal twinning and aggregation were noticed.

• 한국세라믹학회지
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• 제35권10호
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• pp.1085-1093
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• 1998

Amorphous alumina powder prepared by the fast calcination of aluminum trihydroxide(Al(OH)3 gibbsite) for 0.5 second at 580$^{\circ}C$ was investigated rehydration propeties. Phase composition crystal size and mor-phology surface area pore volume and pore size distribution of pesudo-boehmite and bayerite crystals changed with temperature time water/alumina ratio and particle size when amorphous alumina rehydrated with water. Phase compositions were examined with XRD and DTA and crystal sized morphologies were investigaed with SEM and TEM. Also rehydration properties of amorphous alumina were in-vestigated by measuring the surface area pore volume and pore size distribution.

• 한국세라믹학회지
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• 제40권7호
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• pp.683-689
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• 2003

비정질알루미나와 기공형성제를 물과 혼합하여 원통형으로 성형하고 수화, 건조 및 소성하여 ${\gamma}$-alumina pellet을 제조하였다. 이를 Fe(NO$_3$)$_3$.9$H_2O$와 $CH_3$COOH, HNO$_3$ 또는 $CH_3$COOH와 HNO$_3$의 혼합용액에 침척시켜 20$0^{\circ}C$ 온도로 3시간 수열처리 한 다음 결정의 형태 및 변화, 기공특성, $N_2$ 흡/탈착특성, 산점변화 및 기계적 강도 등을 조사하였다. 제조방법에 따라서 0.1~0.3 $mu extrm{m}$ 크기의 작은 결정이 0.5~2 $\mu\textrm{m}$ 길이의 큰 침상결정으로 형태가 변했고, 결정구조는 의사베마이트 또는 ${\gamma}$-alumina 구조를 나타냈다. ${\gamma}$-alumina pellet에 Fe(NO$_3$)$_3$.9$H_2O$와 $CH_3$COOH 용액을 침적시켜 수열처리 했을 때 촉매와 반응물간의 물질전달이 용이한 100~1000 $\AA$ 사이의 기공부피가 0.34 ㏄/g에서 0.86 ㏄/g으로 크게 증가하였다. 기공크기의 증가로 인해 질소 흡.탈착이 원활히 이루어짐을 알 수 있었으며, C-H 그룹의 관능기를 흡착할 수 있는 새로운 활성점이 형성되었다. 또한 촉매의 기계적 강도도 1.06 ㎫에서 1.36 ㎫로 증가하였다.