• Title/Summary/Keyword: Sintering densification

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Synthesis of Polycrystalline YAG Ceramics by Milling-precipitation (분쇄-침전을 이용한 다결정 YAG 세라믹스의 합성)

  • 홍석범;정현기;심수만
    • Journal of the Korean Ceramic Society
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    • v.40 no.11
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    • pp.1120-1126
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    • 2003
  • Yttrium Aluminum Garnet (YAG) powders were prepared by precipitation of Y hydroxides during milling of alumina powders. The powder calcined at 1200$^{\circ}C$ for 4 h contained a small amount of Yttrium Aluminum Monoclinic (YAM) in addition to YAG. However, phase-pure YAG was obtained in the compact of the milled powder with an average particle size of 0.57 ${\mu}$m at 1300$^{\circ}C$, which is much lower than those (l500∼1600$^{\circ}C$) for a mixed oxide method. The powder was found to exhibit an excellent sinterability regardless of the addition of a sintering aid, SiO$_2$(350 ppm Si). The undoped sample were sintered to a relative density of 98% at l600$^{\circ}C$. In contrast, the addition of SiO$_2$ caused a considerable densification to occur at 1500$^{\circ}C$ and the relative density reached 97.7%. But the sintering aid had little effect on the densification at 1600$^{\circ}C$, showing a similar relative density to the undoped sample.

In-Situ Fabrication of TCP/Al2O3 and Fluorapatite/Al2O3 Composites by Normal Sintering of Hydroxyapatite and Al2O3 Powder Mixtures (Hydroxyapatite와 Al2O3 혼합분말의 상압소결에 의한 TCP/Al2O3 및 Fluorapatite/Al2O3 복합재료의 In-Situ 제조)

  • Ha, Jung-Soo;Han, Yoo-Jeong
    • Korean Journal of Materials Research
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    • v.29 no.2
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    • pp.129-135
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    • 2019
  • A powder mixture of 70 wt% $Al_2O_3$ and 30 wt% hydroxyapatite (HA) is sintered at $1300^{\circ}C$ or $1350^{\circ}C$ for 2 h at normal pressure. An $MgF_2$-added composition to make HA into fluorapatite (FA) is also prepared for comparison. The samples without $MgF_2$ show ${\alpha}$ & ${\beta}$-tricalcium phosphates (TCPs) and $Al_2O_3$ phases with no HA at either of the sintering temperatures. In the case of $1,350^{\circ}C$, a $CaAl_4O_7$ phase is also found. Densification values are 69 and 78 %, and strengths are 156 and 104 MPa for 1,300 and $1,350^{\circ}C$, respectively. Because the decomposition of HA produces a $H_2O$ vapor, fewer large pores of $5-6{\mu}m$ form at $1,300^{\circ}C$. The $MgF_2$-added samples show FA and $Al_2O_3$ phases with no TCP. Densification values are 79 and 87 %, and strengths are 104 and 143 MPa for 1,300 and $1,350^{\circ}C$, respectively. No large pores are observed, and the grain size of FA ($1-2{\mu}m$) is bigger than that of TCP ($0.7{\mu}m{\geq}$) in the samples without $MgF_2$. The resulting $TCP/Al_2O_3$ and $FA/Al_2O_3$ composites fabricated in situ exhibit strengths 6-10 times higher than monolithic TCP and HA.

A Study of Post Electrode Formation by Microwave Sintering in LTCC Substrate (마이크로파 소결법을 이용한 LTCC 기판 Post 전극 형성에 관한 연구)

  • Kim, Yong-Suk;Lee, Taek-Jung;Yoo, Won-Hee;Chang, Byeung-Gyu;Park, Sung-Yeol;Oh, Yong-Soo
    • Journal of the Microelectronics and Packaging Society
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    • v.14 no.4
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    • pp.43-48
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    • 2007
  • This study is focused on the effect of the surface properties for the post electrode, which is used in pad formation consisted of SMT such as IC, passive component, combined with fired LTCC substrate, We carried out the surface microstructure of sintered electrode and the basic reliability evaluations with sample fired by microwave sintering to solve the problems occurred in post electrode by electric sintering. We evaluated surface densification status of post electrode according to various conditions of microwave sintering. In additions, it is obtained strong effect on blister improvement of post electrode because of over-sintering and the insufficient out gas in bum out process. As a result of adhesion strength, we confirmed $44.3N/mm^2$ in microwave sintering and $34.5N/mm^2$ in electric sintering, respectively. This result will be used for the basic reliability test. Finally, microwave sintering seems to be economic in process time with 30 min compared to electric sintering with 10 hr. In terms of Mass production and efficiency, microwave sintering are excepted to be higher than electric sintering.

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Effects of $Nb_2O_5$, and Oxygen Potential on Sintering Behavior of $UO_2$ Fuel Pellets

  • Song, Kun-Woo;Kim, Keon-Sik;Kang, Ki-Won;Jung, Youn-Ho
    • Nuclear Engineering and Technology
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    • v.31 no.3
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    • pp.335-343
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    • 1999
  • The effects of N $b_2$ $O_{5}$ and oxygen potential on the densification and grain growth of U $O_2$ fuel have been investigated.0.3 wt% N $b_2$ $O_{5}$ -doped U $O_2$fuel pellets were sintered at 1$700^{\circ}C$ for 4 hours in sintering atmospheres which have various ratios of $H_2O$ to $H_2$ gas. Compared with those of undoped U $O_2$ pellets, the sintered density and grain size of the 0.3 wt% N $b_2$ $O_{5}$ -doped U $O_2$ pellet increase under the $H_2O$/ $H_2$ gas ratio of 5.0$\times$10$^{-3}$ to 1.0$\times$10$^{-2}$ and under the $H_2O$/ $H_2$gas ratio of 5.0$\times$10$^{-3}$ to $1.5\times$10$^{-2}$ , respectively. The sintering of U $O_2$fuel pellets containing 0.1 wt% to 0.5 wt% N $b_2$ $O_{5}$ was carried out at 168$0^{\circ}C$ for 4 hours. The enhancing effect of N $b_2$ $O_{5}$ on the sintered density and grain size becomes larger as the N $b_2$ $O_{5}$ content increases. The solubility limit of N $b_2$ $O_{5}$ in U $O_{2}$ seems to be between 0.3 wt% and 0.5 wt%, and beyond the solubility limit the second phase whose composition corresponds near to N $b_2$U $O_{6}$ is precipitated on grain boundary. The enhancement of densification and grain growth in U $O_2$ is attributed to the increased concentration of a uranium vacancy which is formed by the interstitial N $b^{4+}$ ion in the U $O_2$ lattice.

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Influence of Additives on Densification of Low-Temperature PZT Ceramics (저온소성용 PZT 세라믹스의 치밀화에 미치는 첨가제의 영향)

  • Park, Yong-Kap
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.8 no.5
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    • pp.995-999
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    • 2007
  • The lead zirconate titanate (PZT) powders were synthesized to make the piezoelectric ceramics in low temperature as low as $900^{\circ}C$. To investigate the influence of additives on sintering of PZT, two kinds of sintering aids were made as follows; $wB_2O_3-xBi_2O_3-zCuO$and LiBiO2-CuO. The sintering aid, $1{\sim}3$ wt.% $LiBiO_2-CuO$, was added into these PZT powders and the specimens were fired at temperature in the range of $800{\sim}1200^{\circ}C$. The highest density was shown in the specimen with 1 wt.% $LiBiO_2-CuO$ as additive at temperature of $900^{\circ}C$. The sintered specimen were analyzed by X-ray diffraction(XRD) and scanning electron microscopy (SEM) was utilized to observe the microstructure, especially the densified morphology of specimens. In the XRD pattern, the well-crystallized PZT phase could be obtained in consequence of firing at $900^{\circ}C$. The scanning electron microscopy(SEM) was utilized to observe the structure of specimens after firing at $900^{\circ}C$. The densified perovskite structure of $PbZrTiO_3$ could be obtained by sintering at temperature as low as $900^{\circ}C$. The high sinterability of PZT ceramics was attributed to the low formation temperature of the liquid phase of additives.

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Mechanical Properties of Bulk Amorphous Ti50Cu20Ni20Al10 Fabricated by High-energy Ball Milling and Spark-plasma Sintering

  • Nguyen, H.V.;Kim, J.C.;Kim, J.S.;Kwon, Y.J.;Kwon, Y.S.
    • Journal of Powder Materials
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    • v.16 no.5
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    • pp.358-362
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    • 2009
  • Ti$_{50}$Cu$_{20}$Ni$_{20}$Al$_{10}$ quaternary amorphous alloy was prepared by high-energy ball milling process. A complete amorphization was confirmed for the composition of Ti$_{50}$Cu$_{20}$Ni$_{20}$Al$_{10}$ after milling for 30hrs. Differential scanning calorimetry showed a large super-cooled liquid region ($\Delta$T$_x$ = T$_x$ T$_g$, T$_g$ and T$_x$: glass transition and crystallization onset temperatures, respectively) of 80 K. Prepared amorphous powders of Ti$_{50}$Cu$_{20}$Ni$_{20}$Al$_{10}$ were consolidated by spark-plasma sintering. Densification behavior and microstructure changes were investigated. Samples sintered at higher temperature of 713 K had a nearly full density. With increasing the sintering temperature, the compressive strength increased to fracture strength of 756 MPa in the case of sintering at 733 K, which showed a 'transparticle' fracture. The samples sintered at above 693 K showed the elongation maximum above 2%.

The Study on Fabrication of LAS System Ceramics for Thermal Shock Resistance from Silicate Minerals (III) Sintering Characteristics of Eucryptite and Spodumene (실리케이트 광물을 이용한 내열충격성 LAS계 세라믹스의 제조에 관한 연구 (III) Eucryptite와 Spondumene 소결특성)

  • 박한수;조경식;문종수
    • Journal of the Korean Ceramic Society
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    • v.32 no.2
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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.

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Effect of Sintering Atmosphere and Carbon Addition on Sintered Density of M3/2 Grade High Speed Steel Powder (M3/2계 고속도 공구강 분말의 소결분위기와 탄소첨가가 소결밀도에 미치는 영향)

  • Ahn, Jin-Hwan;Heo, Jong-Seo;Joo, Dong-Won;Jung, Eun;Sung, Jang-Hyun
    • Journal of Powder Materials
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    • v.5 no.4
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    • pp.265-272
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    • 1998
  • For the purpose of investigating the effect of sintering atmosphere and carbon addition on sintered density and microstructural characteristics, the M3/2 grade high speed steel powders with the addition of carbon are sintered in vacuum and $20%H_2/79%N_2/l%CH_4$ gas atmosphere. With the addition of 0 wt%C, 0.45wt%C and 1.15 wt%C the optimum sintering temperatures decrease down to $1260^{\circ}C$, $1210^{\circ}C$ and $1150^{\circ}C$ respectively for the vacuum sintered specimen, and also decrease down to $1130^{\circ}C$, $1120^{\circ}C$ and $1115^{\circ}C$ for the gas sintered specimen. The threshold temperatures for full densification decrease steeply with increasing carbon content of the sintered specimen, while this temperatures are slowly decreased at high carbon content. The vacuum sintered specimen shows the primary carbides of MC and $M_6C$ type at the optimum sintering temperature, and eutectic carbides of $M_2C$ and Fe-Cr type are produced in the oversintered specimen. The gas sintered specimen exhibits M6C and Fe-Cr type primary carbides at the optimum sintering temperature. The eutectic carbides of $M_6C$ and Fe-Cr type and MX type carbonitride are shown for the oversintered specimen in the gas atmosphere. The hardness of gas sintered specimen shows high value of 830-860 Hv due to the increment of carbide precipitation.

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The Characteristic of Agglomerate and Sintering of Y-PSZ Powders Prepared by Different Processes (제조방법에 따른 Y-PSZ 분말의 응집 및 소결특성)

  • Lee, Jong-Kook;Kim, Hwan;Hwang, Kyu-Hong
    • Journal of the Korean Ceramic Society
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    • v.22 no.5
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    • pp.9-16
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    • 1985
  • Agglomeration of Y-PSZ and its related properties were studied. The ultrafine $ZrO_2$ powder containg 3 mol% $Y_2O_3$ was prepared by 1) coprecipitation method b) hot petroleum drying method c) sol-gel method and the characteristics of calcined powders and the microstructures of sintered body were observed. Powder prepared by the coprecipitation method was about 125$\AA$ in crystallite size and 0.1~1.0${\mu}{\textrm}{m}$ of intra-agglomerate pore size when calcined at $600^{\circ}C$ for 1 hour. because of small crystallite size and weak agglo merate strength resultant densification of sintered body was high. But above the temperature of 130$0^{\circ}C$ efflorescent phenomena due to anions attached to powder surface was observed. Powder prepared by hot petroleum drying method was 65$\AA$ in crystallite size and 1~10${\mu}{\textrm}{m}$ of intraagglome-rate pore size and it was observed that the agglemerates were formed during the calcining process. In this case despite of small crystallite size the rate of sintering was slow and the existing lenticular interagglomerate pore was not eliminated to the final stage of sintering. Powder prepared by sol-gel method showed solid agglomertes due to rapi dhydrolysis reaction. In this powder which involves strong solid agglomerates overall sintering rate was determined by the sintering between the agglomerates and therefore sinterability of powders made by sol-gel method was very poor.

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Sintering of Alumina in the Presence of Oxynitride Additives (Oxynitride의 첨가에 의한 알루미나의 소결)

  • Bae, Won-Tae;Kim, Hae-Du
    • 연구논문집
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    • s.30
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    • pp.111-119
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    • 2000
  • Sintering of alumina powder was studied in the presence of Y-Si oxide and oxynitride additives. The main crystalline phase of the sintering aids pre-reacted at $1400^{\circ}C$ was $\alpha$ - $Y_2$$SiO_2$>$O_7$. Y-N apatite was co-existed in the Si-40N sintering aid because of its high content of N. During the sintering process, liquid phases were formed by the reaction between additives and alumina, and these liquid phases promote the densification of alumina. SEM micrographs showed that uniform grain growth occurred in the system with oxide additive(Si-0N). In the case of oxynitride additive system(Si-20N and Si-40N), bimodal microstructure was observed due to the exaggerated grain growth, As the nitrogen content in the additive system increased the exaggerated grain growth occurred extensively. Bloating, which seemed to be originated by the liberation of $N_2$ gas, occurred un the Si-40N oxynitride additive system.