• Title/Summary/Keyword: Vacuum Sintering

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Effect of Sintering Temperature on the Thermoelectric Properties of Bismuth Antimony Telluride Prepared by Spark Plasma Sintering (방전플라즈마 소결법으로 제조된 Bismuth Antimony Telluride의 소결온도에 따른 열전특성)

  • Lee, Kyoung-Seok;Seo, Sung-Ho;Jin, Sang-Hyun;Yoo, Bong-Young;Jeong, Young-Keun
    • Korean Journal of Materials Research
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    • v.22 no.6
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    • pp.280-284
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    • 2012
  • Bismuth antimony telluride (BiSbTe) thermoelectric materials were successfully prepared by a spark plasma sintering process. Crystalline BiSbTe ingots were crushed into small pieces and then attrition milled into fine powders of about 300 nm ~ 2${\mu}m$ size under argon gas. Spark plasma sintering was applied on the BiSbTe powders at 240, 320, and $380^{\circ}C$, respectively, under a pressure of 40 MPa in vacuum. The heating rate was $50^{\circ}C$/min and the holding time at the sintering temperature was 10 min. At all sintering temperatures, high density bulk BiSbTe was successfully obtained. The XRD patterns verify that all samples were well matched with the $Bi_{0.5}Sb_{1.5}Te_{3}$. Seebeck coefficient (S), electric conductivity (${\sigma}$) and thermal conductivity (k) were evaluated in a temperature range of $25{\sim}300^{\circ}C$. The thermoelectric properties of BiSbTe were evaluated by the thermoelectric figure of merit, ZT (ZT = $S^2{\sigma}T$/k). The grain size and electric conductivity of sintered BiSbTe increased as the sintering temperature increased but the thermal conductivity was similar at all sintering temperatures. Grain growth reduced the carrier concentration, because grain growth reduced the grain boundaries, which serve as acceptors. Meanwhile, the carrier mobility was greatly increased and the electric conductivity was also improved. Consequentially, the grains grew with increasing sintering temperature and the figure of merit was improved.

A Study on Atomosphere Sintering to affect the Abnormal Expansion in Solid-Solid Reaction of $BaTiO_3$ (Barium Titanate를 고상반응으로 합성할 때 팽창에 영향을 주는 분위기조성에 관한 연구)

  • 이은상;임대영
    • Journal of the Korean Ceramic Society
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    • v.23 no.4
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    • pp.41-46
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    • 1986
  • When barium titanate was synthesized in solid-solid reaction the abnormal expansion occurred from 90$0^{\circ}C$ to 110$0^{\circ}C$. The equi molecular mixture of $BaCo_3$ and $TiO_2$ was sintered from 90$0^{\circ}C$ to 130$0^{\circ}C$ on the condition of air vacuum and $CO_2$ atomosphere. After that the specimens were tested closely with XDR Dilatometer and SEM The result indicated that: 1, Volume expansion to be synthesized barium titanate in solid-solid reaction was affected by atomosphere sintering. 2. The solid reaction ot fiorm barium titanate in vacuum atomosphere occurred faster than that in air atomosphere. In vacuum atomosphere the maxium volume expansion was about 30% at 90$0^{\circ}C$ for 2hrs, 3. The solid reaction to form barium titanate in 4CO_2$ atomosphere occurred slower than that in air atomosphere. In $CO_2$ atomosphere the maximum volume expansion was 13% at 100$0^{\circ}C$ for 2 hrs. 4. According to the result of x-ray the expanison was caused by the reaction to form $BaTiO_3$ and change $Ba_2TiO_4$ into 4BaTiO_3$.

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Technology of High Purity Powder Sintering by Ti Scrap Recycling (티타늄 스크랩 재활용에 의한 고순도 분말 소결 기술)

  • Choi, Jung-Chul;Chang, Se-Hun;Cha, Young-Hoon;Oh, Ik-Hyun
    • Korean Journal of Materials Research
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    • v.19 no.7
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    • pp.397-402
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    • 2009
  • In this study, Ti powder was fabricated from Ti scrap by the Hydrogenation-Dehydrogenation (HDH) method. Hydrogenation reactions of Ti scrap occurred at near 450 $^{\circ}C$ with a sudden increase in the reaction temperature and the decreasing pressure of hydrogen gas during the hydrogenation process in the furnace. The dehydrogenation process was also carried out at 750 $^{\circ}C$ for 2hrs in a vacuum of $10^{-4}$ torr. After the HDH process, a deoxidation treatment was carried out with the Ca(purity: 99.5) at 700 $^{\circ}C$ for 2hrs in the vacuum system. It was found that the oxidation content of Ti powder that was deoxidized with Ca showed noticeably lower values, compared to the content obtained by HDH process. In order to fabricate Ti compacts, Ti powder was sintered at $1100\sim1400^{\circ}C$ for 2hrs under a vacuum of $10^{-4}$ torr. The relative density of compact was 94.9% at 1300 $^{\circ}C$. After sintering, all of the Ti compacts showed brittle fracture behavior, which occurred in an elastic range with short plastic yielding up to a peak stress.

Sintering Characterization of Ti Powder Prepared by HDH Process (HDH공정에 의한 티타늄 분말제조 및 소결특성)

  • Choi, Jung-Chul;Chang, Se-Hun;Cha, Young-Hoon;Oh, Ik-Hyun
    • Korean Journal of Materials Research
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    • v.19 no.2
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    • pp.55-60
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    • 2009
  • In this study, Ti powder was fabricated from Ti scrap by a hydrogenation-dehydrogenation (HDH) method. The Ti powders were compacted by Spark plasma sintering (SPS) and the microstructure and mechanical properties of the powders were investigated. A hydrogenation reaction of Ti scrap occurred at temperatures near $450^{\circ}C$ with a sudden increase in the reaction temperature and a decrease in the pressure of the hydrogen gas as measured in a furnace during the hydrogenation process. In addition, a dehydrogenation process was carried out at $750^{\circ}C$ for 2hrs in a vacuum of $10^{-4}torr$. The Ti powder sizes obtained by hydrogenation-dehydrogenation and mechanical milling processes were in the range of $1{\sim}90{\mu}m$ and $1{\sim}100{\mu}m$, respectively. To fabricate Ti compacts, Ti powders were sintered under an applied uniaxial punch pressure of 40 MPa at in a range of $900{\sim}1200^{\circ}C$ for 5 min. The relative density of a SPSed compact was 99.6% at $1100^{\circ}C$, and the tensile strength decreased with an increase in the sintering temperature. However, the hardness increased as the sintering temperature increased.

Transparent Ceramics for Visible/IR Windows: Processing, Materials and Characterization

  • Jung, Wook Ki;Ma, Ho Jin;Kim, Ha-Neul;Kim, Do Kyung
    • Korean Journal of Materials Research
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    • v.28 no.10
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    • pp.551-563
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    • 2018
  • Visible and IR windows require a combination of high optical transparency and superior thermal and mechanical properties. Materials, fabrication and characterization of transparent ceramics for visible/IR windows are discussed in this review. The transparent polycrystalline $Y_2O_3$, $Y_2O_3-MgO$ nanocomposites and $MgAl_2O_4$ spinel ceramics are fabricated by advanced ceramic processing and the use of special sintering technologies. Ceramic processing conditions for achieveing fully densified transparent ceramics are strongly dependent on the initial powder characteristics. In addition, appropriate use of sintering technologies, including vacuum sintering, hot-pressing and spark plasama sintering methods, results in outstanding thermal and mechanical properties as well as high optical transparency of the final products. Specifically, the elimination of light scattering factors, including residual pores, second phases and grain boundaries, is a key technique for improving the characteristics of the transparent ceramics. This paper discusses the current research issues related to synthesis methods and sintering processes for yttria-based transparent ceramics and $MgAl_2O_4$ spinel.

Synthesis and Densification of $Ti_5Si_3$-base Intermetallic Compounds by Reactive Sintering and Electro-Pressure Sintering (반응소결법 및 통전가압소결법에 의한 $Ti_5Si_3$계 금속간화합물의 합성 및 치밀화)

  • 유호준
    • Journal of Powder Materials
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    • v.4 no.4
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    • pp.283-290
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    • 1997
  • $Ti_5Si_3$ intermetallics containing 0-6 wt% of Cu were made by reactive sintering (RS) under vacuum using elemental powder mixtures (Process 1), electro-pressure sintering (EPS) using RS'ed materials (Process2), and EPS using elemental powder mixtures (Process 3). Relatively low dense titanium silicides were gained by process 1, in which porosity decreased with increasing Cu content. For example, porosity changed from 42 to 19.4% with the increase in Cu content from 0 to 6 wt%, indicating that Cu is a useful sintering aid. The titanium silicides fabricated by Process 2 had a higher density than those by Process 1 at given composition, and porosity decreased with increasing Cu content. For example, porosity decreased from 38 to 6.8% with the change in Cu content from 0 to 6 wt%. A high dense titanium silicides were obtained by Process 3. In this Process, porosity decreased a little by Cu addition, and was almost insensitive to Cu content. Namely, about 9 or 7% of porosity was shown in 0 or 1-6 wt% Cu containing silicides, respectively. The hardeness increased by Cu addition, and was not changed markedly with Cu content for the silicides fabricated by Process 3. This tendency was considered to be resulted from porosity, hardening of grain interior by Cu addition, and softening of grain boundary by Cu-base segregates. All these results suggested that EPS using elemental powder mixtures (Process 3) is an effective processing method to achieve satisfactorily dense titanium silicides.

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Manufacturing of Cu-26.7Zn-4.05Al(wt.%) Shape Memory Alloy Using Spark Plasma Sintering (Spark Plasma Sintering을 이용한 Cu-26.7Zn-4.05Al(wt.%) 형상기억합금의 제조)

  • Park, No-Jin;Lee, In-Sung;Cho, Kyeong-Sik;Kim, Sung-Jin
    • Korean Journal of Materials Research
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    • v.13 no.6
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    • pp.352-359
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    • 2003
  • In order to control the grain size, the spark plasma sintering technique is applied for the manufacturing of Cu-26.7Al-4.05AI(wt.%) shape memory alloy with pure Cu, Zn, and Al element powders. The sintering processes were carried out under different atmospheres. The sintered bodies were denser under Ar or Ar+4%$H_2$gas atmosphere than under vacuum. With use of small-sized powders, a very small average grain size of 2∼3 $\mu\textrm{m}$ was obtained, but the single phase was not formed. With the large-sized powders the single austenitic phase was observed with the average grain size of $70∼72\mu\textrm{m}$. When the different size of raw powders was mixed, it is confirmed that the average grain size of the manufactured alloys was 15 $\mu\textrm{m}$ with single austenitic phase, but the distribution of grain size was not uniform.

A Study on the Degradation Mechanism of ZnO Ceramic Varistor Manufactured by Ambient Sintering-Process (분위기 소결공정에 의해 제조된 ZnO 세라믹 바리스터의 열화기구 연구)

  • 소순진;김영진;박춘배
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.13 no.5
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    • pp.383-389
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    • 2000
  • The relationship between the DC degradation characteristics of the ZnO varistor and the ambient sintering-process is investigated in this study. ZnO varistors made o matsuoka’s composition were fabricated by standard ceramic techniques. The ambient sintering-process is performed at the extraordinary electrical-furnace which is equipped with the vacuum system. Gases used in sintering process were oxygen nitrogen argon and air. Using XRD and SEM the phase and microstructure of samples were analyzed respectively. The conditions of DC degradation tests were conducted at 115$\pm$2$^{\circ}C$ for 13 h. Current-voltage analysis is used to determine nonlinear coefficients($\alpha$). Frequency analysis are performed to understand electrical properties as DC degradation test. From above analysis it is found that the ZnO varistor sintered in oxygen atmosphere showed superior properties at the DC degradation test and degradation phenomenon of ZnO varistor is caused by the change of electrical properties in grain boundary. These results are in accordance with Gupta’s degradation model.

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Ball Milling and Sintering Behavior of High Speed Steel Powders Containing VC and Co (VC 및 Co함유 고속도공구강 분말의 볼밀링 및 소결거동)

  • 김용진
    • Journal of Powder Materials
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    • v.3 no.3
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    • pp.181-187
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    • 1996
  • Cobalt and VC powders were ball milled with M2 grade high speed steel powders under various ball to powder ratios. The powders milled under higher ball to powder ratio become finer, more irregular and have a broader size distribution, and thus possess a lower compressibility and a better sinterability regarding densification. Increasing the ball to powder ratio lowered the sintering temperature to obtain the density level necessary to isolate all the pores. Lowering the sintering temperature is very critical to maintain fine microstructure since grain and carbide coarsening are accelerated by higher sintering temperature due to more liquid phase formation. The powders obtained by ball milling at 20 to 1 ratio has the lowest compressibility but has the best sinterability, almost compatible to unmilled pure M2 powders. A sintered body over 97% theoretical density with fine microstructures having average grain size of ~10 microns was obtained from the powder by sintering at 1260 $^{\circ}C$ for 1 hour in vacuum. XRD results indicate that two types of carbides are mainly present in the sintered structure, MC and $M_{6}C$ type. The MC type carbides are more or less round shaped and mainly located at the grain boundaries whereas the $M_{6}C$ type are angular shaped and mainly located inside the grains.

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Preparation and Performance of Aluminosilicate Fibrous Porous Ceramics Via Vacuum Suction Filtration

  • Qingqing Wang;Shaofeng Zhu;Zhenfan Chen;Tong Zhang
    • Korean Journal of Materials Research
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    • v.34 no.1
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    • pp.12-20
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    • 2024
  • This study successfully prepared high-porosity aluminosilicate fibrous porous ceramics through vacuum suction filtration using aluminosilicate fiber as the primary raw material and glass powder as binder, with the appropriate incorporation of glass fiber. The effects of the composition of raw materials and sintering process on the structure and properties of the material were studied. The results show that when the content of glass powder reached 20 wt% and the samples were sintered at the temperature of 1,000 ℃, strong bonds were formed between the binder phase and fibers, resulting in a compressive strength of 0.63 MPa. When the sintering temperatures were increased from 1,000 ℃ to 1,200, the open porosity of the samples decreased from 89.08 % to 82.38 %, while the linear shrinkage increased from 1.13 % to 10.17 %. Meanwhile, during the sintering process, a large amount of cristobalite and mullite were precipitated from the aluminosilicate fibers, which reduced the performance of the aluminosilicate fibers and hindered the comprehensive improvement in sample performance. Based on these conditions, after adding 30 wt% glass fiber and being sintered at 1,000 ℃, the sample exhibited higher compressive strength (1.34 MPa), higher open porosity (89.13 %), and lower linear shrinkage (5.26 %). The aluminosilicate fibrous porous ceramic samples exhibited excellent permeability performance due to their high porosity and interconnected three-dimensional pore structures. When the samples were filtered at a flow rate of 150 mL/min, the measured pressure drop and permeability were 0.56 KPa and 0.77 × 10-6 m2 respectively.