침전법으로 제조한 Alumina 분말의 특성(III) : 소결거동

홍기곤,이홍림 한국세라믹학회 1988 한국세라믹학회지 Vol.25 No.5

Alpha alumina powder with fine particle size and narrow particle size distribution was prepared by precipitation method using Al2(SO4)3.18H2O as a starting material. The alpha alumina powder was prepared by calcining aluminum hydroxide which was formed under various pH values. The sinterabilityof alpha alumina powder and the effect of MgO on the sinterability of alpha alumina powder were investigated. The sinterability of alpha alumina powder was the order of pH=10≒pH11>pH=7≒pH9, and alpha alumina obtained from boehmite which was prepared by precipitation method reached to 97.5% of theoretcal density by the pressureless sintering. The effect of MgO on volume shrinkage of alumina was very slight in the initial sintering stage but remarkable in the final sintering stage. It was also found that MgO controlled effectively the grain growth of alumina.

침전법으로 제조한 $Al_2O_3$-$ZrO_2$계 세라믹스의 미세구조 및 기계적 특성

홍기곤,이홍림 한국세라믹학회 1990 한국세라믹학회지 Vol.27 No.8

A precipitation method, one of the most effective liquid phase reaction methods, was adopted in order to prepare high-tech Al2O3/ZrO2 composite ceramics. Al2(SO4)3.18H2O, ZrOCl2.8H2O and YCl3.6H2O were used as starting materials and NH4OH as a precipitation agent, various types of metal hydroxides were obtained by single precipitation(series A) and co-precipitation(series B) method at the pH condition between 7 and 11. Fine Al2O3-ZrO2 powders were prepared at optimum calcination condition and the effects of ZrO2 on microstructures and mechanical properties of Al2O3 were investigated. The composition of Al2O3/ZrO2 composites wax fixed as Al2O3-15 v/o ZrO2(+3m/o Y2O3). ZrO2 limited the grain growth of Al2O3 and increased grain size homogeneity of Al2O3 more effectively than MgO.Flexural strength values in Al2O3 and Al2O3/ZrO2 composites were 340-430 MPa and 540-820 MPa, respectively, and the effect of strength improvement showed 20-50% by adding ZrO2 to Al2O3. Fracture toughness of Al2O3/ZrO2 composites was improved by stress-induced phase transformation of tetragonal ZrO2 and toughening effect by microcrack was not observed. Also, ZrO2 particles located at Al2O3 grain junction contributed to toughening, while spherical ZrO2 particles located within Al2O3 grain did not contribute to toughening. Weibull moduli of Al2O3 ceramics and Al2O3/ZrO2 composites of series A and series B were 4.34, 5.17 and 9.06, respectively. Above 0.5 of failure probability, strength values in Al2O3 ceramics and Al2O3/ZrO3 composites of series A and series B were above 400 MPa, 700 MPa and 650 MPa, respectively.

침전법으로 제조한 Al2O3-15v/o ZrO2(+3m/o Y2O3)계 세라믹스의 소결거동

홍기곤,이홍림 한국세라믹학회 1989 한국세라믹학회지 Vol.26 No.3

Al2O3/ZrO2 composites were prepared by precipitation method using Al2(SO4)3.18H2O, ZrOCl2.8H2O and YCl3.6H2O as starting materials and NH4OH as a precipitation agent. Al2O3/ZrO2 composites(series A) were prepared by mixing Al2O3 powder obtained by single precipitation method with ZrO2(+3m/o Y2O3) powder obtained by co-predipitation method. Al2O3/ZrO2 composites (series B) were prepared by co-precipitation method using the three starting materials. In all cases, the composition was controlled as Al2O3-15v/o ZrO2(+3m/o Y2O3). The composites of series A showed higher final relative densities than those of series B and tetagonal ZrO2 in all cases was retained to about 95% at room temperature. ZrO2 particles were coalesced more rapidly in grain boundary of Al2O3 than within Al2O3 grain. ZrO2 particles were located at 3-and 4-grain junction of Al2O3 and limited the grain growth of Al2O3. It was observed that MgO contributed to densification of Al2O3 but limited grain growth of Al2O3 by MgO was not remarkable. In all Al2O3/ZrO2 composites, exaggerated grain growth of Al2O3 was not observed and Al2O3/ZrO2 composites were found to have homogeneous microstructures.

침전법으로 제조한 Alumina 분말의 특성(1): 알루미늄 수산\ulcorner루

홍기곤,이홍림 한국세라믹학회 1988 한국세라믹학회지 Vol.25 No.2

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.

불소성 $Al_2O_3-C$질 내화벽돌의 특성에 미치는 첨가물의 영향

홍기곤,채상택 한국세라믹학회 1994 한국세라믹학회지 Vol.31 No.7

The effect of additives on properties of unfired Al2O3-C bricks were investigated. The increase of carbon content and the addition of MgO or spinel improved the resistances against spalling and corrosion of unfired Al2O3-C bricks. Also, the oxidation resistance of unfired Al2O3-C brick was increased by adopting complex metals of Al and Si in spite of the increase of carbon content.

Mechanical Properties and Failure Analysis of $Al_2O_3/ZrO_2$ Composites

홍기곤,한동빈,Hong, Gigon-Hong,Han, Dong-Bin Materials Research Society of Korea 1992 한국재료학회지 Vol.2 No.3

$Al_2O_3/ZrO_2$복합분말에 상릉분말을 침가하여 상압소결법으로 $Al_2O_3/ZrO_2$복합체를 제조한 후, 밀도, 강도, 경도 및 파괴인성등의 물성을 측정하였으며 미세구조 및 파괴단면도 관찰하였다. 상용분말의 침가량이 중량비로 50%이하인 경우에는 평균 꺽임 강도가 640 MPa정도로 거의 변화가 없었으며, 50%이상 첨가된 경우에는 강도가 저하되었는데, 이는 미세조직과 관계가 있는 것으로 생각된다. 또한 파괴인성(4.3-5.3 $Mpam^{1/2}$)값은 상용분말 첨가량에 비례하여 증가하였다. 파괴단면 관찰결과 파괴원인으로는 가공에서 생기는 표면 결함, $ZrO_2$ agglomeration에 의한 crack-like void 및 $Al_2O_3/ZrO_2$ nano복합체 분말과 상용분말간의 소결성 차이에서 생기는 계면 분리등이 관찰되었는데, nano 복합 분말만을 사용한 소결체에서는 가공에 의한 표면 결함만이 파괴원으로 작용하였다. 또한, 파괴형태는 주로 transgranular fracture이었다 $Al_2O_3/ZrO_2$ composites were fabricated by pressureless sintering from commercial powders and/or nano composite powder of $Al_2O_3/ZrO_2$. The Properties of the composites such as density, strength, hardness and fracture toughness were evaluated. Microstructures and fracture surfaces ware also examined. The flexural strength remains unchanged(~640 MPa) as long as the content of commercial powders is not extreamly high, and depends on microstructures of the composites. Fracture toughness(4.3-5.3 $Mpa{\cdot}m^{1/2}$) increases with increasing content of commercial powders. Fractography shows that failure-initiating sources are 1)surface flaws resulting from machining damage, 2)crack-shaped voids formed due to $ZrO_2$ agglomeration, and 3)surface separation caused by inhomogeneous blending and by sinterability difference between nato composite powder and commercial powders of $Al_2O_3/ZrO_2$. Failure mode of the composites was mainly transgranular.

공침법으로 제조한 $ZrO_2$+3m/o $Y_2O_3$계 분체의 특성(I) : 정방정 Zirconia분체의 안정성

홍기곤,이홍림 한국세라믹학회 1990 한국세라믹학회지 Vol.27 No.3

The properties of the powder of ZrO2+3m/o Y2O3 system prepared by co-precipitation method at the pH values of 7, 9, 10 and 11 were investigated. ZrOCl2.8H2O and YCl3.6H2O were used as starting materials and NH4OH as a precipitation agent. Zirconium hydroxide near by Zr(OH)4 structure showed more excellent crystallinity and lower formation temperature of tetragonal ZrO2. In the range of this study, cubic ZrO2 was not formed and stability of tetragonal ZrO2 prepared in the conditiion of pH 7 was most excellent. Average particle sizes and specific surface areas of tetragonal ZrO2 powders, prepared as calcining amorphous zirconium hydroxides at $600^{\circ}C$ for 1h, were 0.6-0.8${\mu}{\textrm}{m}$ and 45-70$m^2$/g, respectively.

직접결합 마그네시아-크로미아질 내화벽돌의 특성에 미치는 $Cr_2O_3$ 함유량의 영향

홍기곤,엄창중 한국세라믹학회 1997 한국세라믹학회지 Vol.34 No.1

The effects of Cr2O3 content on the properties of direct-bonded MgO-Cr2O3 bricks were investigated in the range of 10 to 30 wt% of Cr2O3. Modulus of rupture of bricks was excellent in about 20 wt% of Cr2O3 content. The corrosion resistance of bricks was improved by increasing Cr2O3 content and was directly pro-portional to the amount of secondary spinels. On the other hand, the spalling resistance of bricks depended on the amount of flux rather than Cr2O3 content. 출발원료로서 소결마그네시아 클링커 및 천연크롬철광을 사용하여 Cr2O3의 함유량을 약 10-30 중량%의 범위에서 변화시켜 직접결합 마그네시아-크로미아질 내화벽돌의 특성에 미치는 Cr2O3의 영향을 고찰하였다. 상온 꺾임강도 및 고온 꺽임강도는 Cr2O3의 함유량 및 flux 성분의 함유량과는 상관관계가 성립하지 않았으며, 상온 꺾임강도 및 고온 꺾임강도가 가장 우수한 Cr2O3 함유량의 범위는 20중량% 전후였다. 내식성을 좌우하는 주된 요인은 flux성분의 함유량보다는 2차 spinel의 생성량이었으며, 내식성은 2차 spinel의 생성량 증가에 따라 선형적으로 증가하였다. 또한, 내spalling성은 주로 flux 성분의 함유량에 의존하였으며, flux 함유량이 적을수록 내spalling성이 우수하였다.

공침법으로 제조한 Al2O3-15v/o ZrO2(+3m/o Y2O3)계 분말의 특성

홍기곤,이홍림 한국세라믹학회 1989 한국세라믹학회지 Vol.26 No.2

The properties of the powder of Al2O3-15v/o ZrO2(+3m/o Y2O3) system prepared by co-precipitation method at the pH values of 7, 9, 10 and 11 were investigated. Al2(SO4)3.18H2O, ZrOCl2.8H2O and YCl3.6H2O were used as starting materials and NH4OH as a precipitation agent. Zirconium hydroxide decreased the specific surface area of aluminum hydroxide of AlOOH type, while increased the specific surface area of aluminum hydroxide of Al(OH)3 type, and formed co-network structure of Al-O-Zr type with the aluminum hydroxides. The rate of transition to $\alpha$-Al2O3 from co-precipitated materials occurred in the order of 7≒10, 9 and 11 of pH values. Al2O3 and ZrO2 interacted to bring about coupled grain growth, and the growth of ZrO2 crystallite size rapidly occurred within $\theta$-Al2O3 matrix. Segregation did not occur in the system Al2O3-15v/o ZrO2(+3m/o Y2O3) and Y2O3 acted as a stabilizer to ZrO2. The lattice strain of tetragonal ZrO2 was increased by the constraint effect of Al2O3 matrix.

침전법으로 제조한 Alumina 분말의 특성(II) : 열처리에 따른 Alumina 분말의 특성

홍기곤,이홍림 한국세라믹학회 1988 한국세라믹학회지 Vol.25 No.3

침전법에 의해서 pH가 7, 9, 10, 11인 조건에서 생성된 알루미늄 수산화물을 출발물질로 하여 열처리에 따른 알루미나 분말의 특성을 연구하였다. $600^{\circ}C$에서 2시간 동안 열처리하였을 때 비정질 알루미늄 수산화물의 결정수가 탈수된 후에 생성된 최초의 상은 비정질 알루미나의 비표면적은 감소하였다. 비정질 알루미늄 수산화물을 제외한 나머지 알루미늄 수산화물로부터 결정수의 탈수는 비표면적을 증가시켰으며 AlOOH 형태의 수산화물의 존재비가 클수록 전이 알루미나 존재영역까지는 비표면적이 더 크게 나타났다. $\alpha-Al_2O_3$로의 전이속도는 동일온도에서 pH=7 > pH=10 > pH=9 > pH=11의 순서로 일어났으며, 생성된 $\alpha-Al_2O_3$ 분말의 morphology는 알루미늄 수산화물의 외형을 남긴 형골입자(skeleton particle였다. 또한, 열처리 온도의 증가와 $\alpha-Al_2O_3$로의 전이가 일어남에 따라 비표면적의 감소와 더불어 입자성장이 일어나다. The starting materials were aluminum hydroxide prepared by precipitation method at the conditions of pH values; 7, 9, 10 and 11. The properties of alumina powder on heat-treatment were studied. After dehydrating structural water from amorphous aluminum hydroxide, the first formed phase was amorphous alumina and its specific surface are was decreased. The specific surface area was increased by dehydration of structural water from aluminum hydroxides except amorphous aluminum hydroxide. The specific surface area was increased with increase of the ratio of A1OOH to $A1(OH)_3$ in the region of transition aluminas. The rate of transition from aluminum hydroxide to alpha alumina occurred in the order of 7, 10, 9 and 11 of pH values. The morphology of alpha alumina powders was skeleton particles remaining outer shape of aluminum hydroxide. Both the elevation of heat-treatment temperature and the transition toalpha alumina decreased specific surface area and brought about the growth of particles.