• 한국분말재료학회지
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• 제18권1호
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• pp.35-40
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• 2011

LAS-system ceramic powder, spodumene ($Li_2O{\cdot}Al_2O_3{\cdot}4SiO_2$), was successfully synthesized by a chemical solution technique employing PVA(polyvinyl alcohol) as an organic carrier. The PVA content affected the microstructure of porous precursor gels and the crystalline development. The optimum PVA content contributed to homogeneous distribution of metal ions in the precursor gel and it resulted in the synthesis of glass free $\beta$-spodumene powder having a specific surface area of $7.57\;m^2/g$. The agglomerated $\beta$-spodumene powders were also enough soft to grind to fine powders by a simple ball milling process. The microstructures of the densified powder compacts were strongly dependant on the minor phases of spodumene solid solution and amount of liquid phase, which were formed from the inhomogeneous precursors.

• 한국결정성장학회지
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• 제3권2호
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• pp.162-166
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• 1993

적외선 할로겐 lamp를 열원으로 하는 image furnace을 사용하는 Floating Zone process를 이용하여 Spodumene$(LiAlLi_2O_6)$ 단결정을 성장하였다. 결정의 길이는 50~60mm, 직경 6~8mm였고 dopant에 따라 녹색, 흑색, 연한 녹색의 결정을 얻었다. Spodumene 조성의 고찰을 위해 XRD와 FTIF을 조사하였으며, Laue back reflection pattern을 통해 결정성을 고찰하였다. 결정의 광투과도 측정을 위해 optical transmittance를 측정하였다.

• 한국세라믹학회지
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• 제31권7호
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• pp.784-794
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• 1994

Though spodumene have a law theraml expension and good thermal shock resistance, its sintering temperature is too close to its melting point in the application for industral purpose. Solving the problems, impurities within the silicate minerals act as a frit during firing, so its densification is expected through enlargement of sintering temperature range. By the heat treatment of starting materials, mixtures of silicate mineral, lithium carbonate, if necessary SiO2 or Al2O3 were added for stoichiometric correction, in the range of 1000~125$0^{\circ}C$ for 10 hrs, $\beta$-spodumene single phase was synthesized. Mixtures with sillimanite group minerals, $\beta$-spodumene was formed at 120$0^{\circ}C$ or 125$0^{\circ}C$ via intermediate phases of petalite, Li2SiO3 and LiAlO2. For the case of kaolin group minerals, synthesis were completed at 110$0^{\circ}C$ for Hadon pink kaolin, 120$0^{\circ}C$ for New Zealand white kaolin, When pyrophyllite group minerals were used, those were at the range of 1000~125$0^{\circ}C$. Spodumene was completed at lowest temperature, 100$0^{\circ}C$ from the mixture of Wando pyrophyllite among them. Microstructure of synthesized powders showed the inrregular lump shape such as densed crystallines.

• 한국세라믹학회지
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• 제32권2호
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• pp.171-182
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• 1995

Five eucryptite and ten spodumene compositional powders were syntehsized from three sillimanite group, two kaolin group, and five pyrophyllite group silicate minerals. Those powders were isotatically pressed and fired at 1200~135$0^{\circ}C$ for 2 hrs, and then the sintered bodies were characterized. Silicate minerals with molar ratio of Al2O3 to SiO2 correspond to those of eucryptite and spodumene are kaolin and pyrophyllite group silicate minerals, respectively. Sintering characteristics of eucryptite from kaolin group and spodumene from pyrophyllite group mineral were superior to those from other silicate minerals. Eucryptite sintered bodies with 95~97% relative densities and densified microstructures can be obtained using Hadong pink kaolin as starting materials by sintering over broad temperature zone(1250~135$0^{\circ}C$). The eucryptite sintered bodies which were fired at 130$0^{\circ}C$ for 2hrs, from Hadong pink kaolin had within 3.0wt% microstructural compositional variations compaired with stoichiometric compound, and had good negative thermal expansiion property with -3.55$\times$10-6/$^{\circ}C$ thermal expansion coefficient. Spodumene sintered bodies which were prepared from pyrophyllite group silicate minerals, had dense microstructures and high densities by densification through liquid phase sintering with enlarged temperature range. The specimens which were fired at 130$0^{\circ}C$ for 2 hrs from Gusipyrophillite, had dense microstructure with crystallines mainly, and low thermal expansion property with 0.62$\times$10-6/$^{\circ}C$ thermal expansion coefficient. The porous texture and residual glass phase in LAS system ceramics which were prepared from silicate minerals, tend to increase the thermal expansion properties of sintered bodies to positive direction.

• 한국세라믹학회지
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• 제29권7호
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• pp.533-538
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• 1992

Effect of Li2O.4B2O frit on the microstructural and thermal expansion behaviour of $\beta$-spodumene ceramics was investigated. With 4.0~8.0 wt.% frit addition, sintering temperature range was enlarged and densification was enhanced through liquid phase sintering. As the amount of frit addition was increased, thermal expansion coefficient was increased to 1.72$\times$10-6$^{\circ}C$-1 of its highest value, which indicated that the increment of thermal expansion coefficient due to the second phase was constrained.

• 한국세라믹학회지
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• 제29권8호
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• pp.646-650
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• 1992

Effect of Li2O.4B2O3 frit addition on microstructural and thermal expansion behaviour of the $\beta$-spodumene ceramics made from kaolinite was investigated. With 2.0~4.0 wt% frit addition, the densification by liquid phase sintering caused low water absorption below 3% and enhancement of beding strength. As the amount of frit addition was increased, thermal expansion coefficient was increased to large scale, but in 2 wt% frit addition, its thermal expansion coefficient was constrained to 1.92$\times$10-6$^{\circ}C$-1.

• 한국결정성장학회지
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• 제20권1호
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• pp.53-57
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• 2010

화력 발전소에서 배출된 석탄 바닥재로 L-A-S($Li_2O-Al_2O_3-SiO_2$)계 결정화 유리를 제조함에 있어 수식제인 CaO 첨가가 결정화 온도, 결정상 종류, 미세구조 등의 특성에 미치는 영향을 분석하였다. L-A-S계 유리에 CaO를 첨가하면 DTA 그래프 상의 유리 전이 온도 및 결정화 온도가 함께 높아지고 주 결정상으로 ${\beta}$-spodumene($LiAlSi_2O_6$) 및 eucryptite ($LiAlSiO_4$)가 생성되었으며, 동시에 CaO와 관련된 미지의 상도 약간 생성되었다. 결정화 유리 시편은 표면 및 내부 결정화 거동을 함께 나타냈으며, CaO 첨가량이 증가하면 시편 내부의 결정 크기 및 분율이 높아졌다. 또한 시편의 겉에서 내부 방향으로 성장한 표면 결정은, CaO 첨가에 따라 다양한 형태를 보였으며 CaO 첨가량이 9 wt% 이상이 되면 일부 균열이 관찰되었는데 이는 ${\beta}$-spodumene과 CaO 관련 결정 간에 열팽창계수 차이에 의한 것으로 생각된다.

• 한국세라믹학회지
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• 제28권9호
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• pp.730-738
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• 1991

Machinable ceramics containing ${\beta}$-spodumene crystal was fabricated by melting method using domestic pyrophyllite. Raw materials were batched by molar ratio of 8:2, 7:3, 6:4, and 5:5 for fluorophlogopite and ${\beta}$-spodumene. These compounds were melted at 1450$^{\circ}C$ for 1 hr and formed in graphite mold. Base glasses were heat-treated according to 2-step schedule which was determined from DTA, XRD analysis and SEM observation. Fabricated machinable ceramics have excellent themal, chemical properties and machinability.

• 한국결정성장학회지
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• 제21권5호
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• pp.218-224
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• 2011

저열팽창 특성을 갖는 난소결 물질인 LAS($Li_2O-Al_2O_3-SiO_2$)계를 고상 소결로 제조하였다. LAS계의 ${\beta}$-spodumene($Li_2O-Al_2O_3-4SiO_2$) 조성에 소결 조제로 $CaCO_3$를 첨가하였고, 강도 증가를 위하여 $ZrO_2$를 첨가하였다. 첨가제의 양의 변화와 소결 온도의 변화에 따른 소결 특성, 미세 구조, 기계적 특성 및 열팽창 특성에 대하여 조사하였다. 0.1 mol%의 $CaCO_3$을 첨가하였을 때, 치밀화가 증진됨을 미세구조 관찰에 의해 확인하였으며, $ZrO_2$의 첨가로 강도가 증진됨을 확인하였다. Dilatometer로 측정한 열팽창 계수는 선택된 전 조성에서 값이 $1.2{\sim}1.7{\times}10^6/^{\circ}C$임을 확인하였다.

• 한국결정성장학회지
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• 제22권1호
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• pp.57-63
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• 2012

$Al_2TiO_5$에 LAS(${\beta}$-spodumene)와 $Fe_2O_3$를 첨가하여 고상법으로 세라믹 소결체를 제조하였다. $Al_2TiO_5$에 첨가된 LAS는 액상을 형성하고, $Fe_2O_3$는 입자 성장을 억제시켜 소결체를 치밀화하였다. 첨가제의 양을 변화시켜 소결특성, 기계적 특성 및 열충격 특성에 대하여 조사하였다. $Fe_2O_3$가 20 wt% 첨가된 LAS를 $Al_2TiO_5$에 20 wt% 첨가하였을 때, 꺽임 강도는 120 MPa 이상이었고, 열충격에 대한 저항성은 $1200^{\circ}C$ 이상으로 우수함을 확인하였다.