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1 Jurnal f the Krean Ceramic Sciety Vl. 45, N. 1, pp. 87~81, 008. Effects f Y O Additin n Densificatin and Thermal Cnductivity f AlN Ceramics During Spark Plasma Sintering Jae Hng Chae*, J Sek Park*, **, Jng Pil Ahn*, Kyung Hun Kim*, and Byung Ha Lee*, ** *Krea Institute f Ceramic Engineering and Technlgy, Seul , Krea **Department f Materials Science and Engineering, Myngji University, Yngin , Krea (Received September 9, 008; Revised Nvember 5, 008; Accepted Nvember 6, 008) Y O ƒƒ AlN v e w y*á *, ** Á v*á½ z*á w*, ** *» ** w œw ( ; ; ) ABSTRACT Spark plasma sintering (SPS) f AlN ceramics were carried ut with Y O as sintering additive at a sintering temperature 1,550 ~ 1,700 C. The effect f Y O additin n sintering behavir and thermal cnductivity f AlN ceramics was studied. Y O added AlN shwed higher densificatin rate than pure AlN nticeably, but the frmatin f yttrium aluminates phases by the slid-state reactin f Y O and Al O existed n AlN surface culd delay the densificatin during the sintering prcess. The thermal cnductivity f AlN specimens was prmted by the additin f Y O up t wt% in spite f the frmatin f YAG secndary phase in AlN grain bundaries because Y O additin culd reduced the xygen cntents in AlN lattice which is primary factr f thermal cnductivity. Hwever, the thermal cnductivity rather decreased ver wt% additin because an immderate frmatin f YAG phases in grain bundary culd decrease thermal cnductivity by a phnn scattering surpassing the cntributin f Y O additin. Key wrds : Aluminum nitride, Ytrria, Thermal cnductivity, Sintering 1. AlN w ( 0 Wm 1 K 1 ),» üyw w g q w š z»q packaging, (heat sink), œ e š. 1-) w AlN w œ w» y ƒ û» m ù e m y ƒw wwš. 4,5) w x w e y k AlN ü w s g k š w w j. AlN Y O ƒ Al O Y O Crrespnding authr : J Sek Park Tel : Fax : yttrium aluminates x w š, û AlN ü w š YAG (Y Al 5 O 1 ), YAP (YAlO ) YAM(Y 4 Al O 9 ) AlN ü ƒ» w j š. 6,7) v (Spark Plasma Sintering) pulse wš w m k w š v š graphite w jule w ww. v 8) p 000 C š ¾ ü ƒ ƒ wš v neck x, t y, y z, y z» w ü y, y, w w. 8,9) Y O ƒ w v 87

2 88 yá Á vá½ zá w w AlN w p p w š w.. x AlN (99.9%, Kjund Chem., Japan) Y O (99.9%, Cerac, USA) w. AlN Y O 1,, 5 wt% ƒw š, k z 4 ww z yw e j k wš» 90 C 4 w yw w. yw graphite mld g v e(s-515s Sumitm Cal mining C., Japan) w»w 40 MPa, 100 C/min 1550 ~ 1700 C 5 z þ w. Archimedes w d w, X- z e(m0xhf, MAC Science. C. Ltd., Japan) w ƒ w w, laser flash e(lfa 47, NETZSCH. Germany) w y d w r w. x (JSM-5900LV, JEOL, Japan) w w.. š Fig. 1 v ùkü v Y O ƒ w ( w Y O ƒ 1Y, Y, 5Y Fig. 1. Relative density f AlN specimens with sintering temperature and sintering additives. Fig.. XRD patterns f AlN pwder, pure and 5 wt% Y O added AlN sintered bdies at 1,700 C. t») 97% š ùk üš ƒw ( w pure t») 1,650 C 97% w š. AlN ù Ht-press ƒw 1,700 C š. w 10-1) x v w m û ƒ š w. w v w. Fig. AlN XRD ùk üš. Y O 5wt% ƒw r z YAG x, Y O ƒ w YAG, YAM, YAP AlN ü w Y O ƒ w. ƒ Y O AlN t w Al O mw x š AlN ü w» w» w x. 6,7,1,14) Fig. v ƒ d w ùkü mw e y w. Y O ƒw w 1,00 C wš. Y O ƒw w z ¾ x v š ùküš, Y O ƒw ƒw e y š w e yƒ w wz

3 YO 첨가가 AlN 세라믹스의 방전 플라즈마 소결 거동 및 열전도도에 미치는 영향 89 소결 조제의 첨가량에 따른 치밀화 거동을 살펴보면 Y O 의 첨가량이 증가할수록 오히려 치밀화 완료 시점이 늦어지고 있으며 과 5 wt%를 첨가한 경우에는 580초 부 근인 약 1,580 C 근처에서 소결 수축이 느려지기 시작하 며 첨가량이 증가하면 더욱 뚜렷이 이러한 경향을 나타 내고 있다. Qia 등의 보고에 따르면 AlN의 소결에 있어 서 Y O 의 첨가 시 Y O 와 Al O 의 고상 반응에 의해 소 결 수축이 느려질 수 있으며 온도가 더 상승하여 액상이 형성되면 액상 소결에 의해 치밀화가 급속히 진행된다. 본 연구에서도 Fig. 에서 XRD 분석 결과와 Y O 의 첨 가량이 증가하면 소결 수축 지연이 더욱 뚜렷이 나타남 을 고려하면 첨가된 Y O 와 Al O 의 고상 반응에 의한 YAG 상의 형성으로 소결 수축의 지연 현상이 나타난 것 으로 사료된다. Fig. 4는 1,700 C에서 소결된 시편들의 미세구조를 보여 주는 SEM 사진으로, Fig. 의 XRD 분석 결과에는 나타 나지 않지만 Y O 1 wt%가 첨가된 경우에도 이차상이 존 재하고 있음을 보여주고 있다. 상압 소결이나 ht-press 소 결인 경우 Y O 가 첨가된 AlN 소결체의 경우 매우 뚜렷 한 입계 파괴를 일반적으로 나타내고 있지만, 이 와는 달리 본 연구에서의 경우에는 입내 파괴와 입계 파 괴가 혼재하여 나타나고 있으는데 pure한 시편의 경우 주 로 입내 파괴 양상을 보이고 있으며, Y O 가 첨가된 시 15) Fig.. Densificatin behavirs f AlN pwders during spark plasma sintering prcess. 다. 이는 AlN의 소결 시 첨가된 Y O 가 AlN 표면의 Al O 와의 반응으로 액상이 형성되기 때문에 치밀화가 급 속히 진행되는 것으로 잘 알려져 있다. 특히 방전플라 즈마 소결의 경우 국부적으로 고온 영역이 형성된다고 알 려져 있는데, 이는 국부적인 영역에서 이러한 액상의 형성을 더욱 촉진하여 소결 조제를 첨가하지 않은 경우 보다 빠른 치밀화 거동을 나타내는 것이라 사료된다. 4,5) 8,9) Fig ,1,14,15) Back-scattered electrn SEM fractured surface images f AlN specimens sintered at 1,700C. 제 45 권 제 1호(008)

4 80 yá Á vá½ zá w Fig. 5. Variatin f thermal cnductivity f AlN specimens with sintering temperature. r YAG w q ƒ ùš y w. v t y w k w, w Áòw w w w w. 8,9) x w š w š w w w» ü q ùkü, w w w» q ùküš. Fig. 5 AlN r d ùkü v. r ƒ ƒ š. ƒ» w. Y O ƒ y r wt% ƒ¾ ƒ ƒ š ù 5wt% ƒ ƒ š. AlN ƒ j w e AlN ü w 1,) Y O ƒ AlN ü w û ƒ ƒw ƒ w š, yttrium aluminates x v w. x w AlN w ƒ û (YAG 1 Wm 1 K 1 ) s j» ww w. Y O ƒ w y wt% ƒ ¾ w w YAG x AlN ü w û z w wz ƒ w, 5 wt% ƒ YAG ƒ w z ƒ ƒ wt% ƒ û š. 4. v w Y O ƒw AlN w m û š w. AlN Y O ƒ ƒw e y AlN t x Al O š w e y e y j z ùkü z YAG x w. AlN Y O ƒ AlN ü w ƒ w ƒ x w w ƒ y w. REFERENCES 1. G. A. Slack, Nnmetallic Crystals with High Thermal Cnductivity, J. Phys. Chem. Slids, (197).. L. M. Sheppard, Aluminum nitride: a versatile but challenging material, Am. Ceram. Sc. Bull., (1990).. Y. Baik and R. A. Drew, Aluminum Nitride: Prcessing and Applicatins, Key Eng. Mater., (1996). 4. K. Kmeya, H. Inue, and A. Tsuge, Effect f Varius Additives n Sintering f Aluminum Nitride, Ygy-Kykaishi, (1985). 5. K. Kmeya, H. Inue, and A. Tsuge, Rle f Y O and SiO Additins in Sintering f AlN, J. Am. Ceram. Sc., (1974). 6. A. V. Virkar, T. B. Jacksn, and R. A. Cutler, Thermdynamic and Kinetic Effects f Oxygen Remval n the Thermal Cnductivity f Aluminum Nitride, J. Am. Ceram. Sc., (1989). 7. T. B. Jacksn, A. V. Virkar, K. L. Mre, R. B. Dinwideie, and R. A. Cutler, High Thermal Cnductivity Aluminum Nitride Ceramics: the Effect f Thermdynamic, Kinetic and Micrstructural Factrs, J. Am. Ceram. Sc., (1997). 8. M. Tkita, Trends in Advanced SPS(Spark Plasma Sintering) Systems and Technlgy, J. Sc. Pwder & Tech. Jpn., (199). 9. M. Omri, Sintering, Cnslidatin, Reactin and Crystal Grwth by the Spark Plasma System (SPS), Mater. Sci & Eng., A (000). 10. G. Pezztti, A. Nakahira, and M. Tajika, Effect f Extended Annealing Cycles n the Thermal Cnductivity f AlN/

5 Y O ƒƒ AlN v e w 81 Y O Ceramics, J. Eur. Ceram. Sc., (000). 11. S. W. Chi, H. C. Lee, J. Rhee, and I. C. Lee, Sintering f Aluminum Nitride (I); Pressureless Sintering, J. Kr. Ceram. Sc., (1991). 1. J. Y. Qiu, Y. Htta, K. Watari, K. Mitsuishi, and M. Yamazaki, Lw-temperature Sintering Behavir f the Nan-sized AlN Pwder Achived by Super-fine Grinding Mill with Y O and CaO Additives, J. Eur. Ceram. Sc., (006). 1. M. Medraj, Y. Baik, W. T. Thmpsn, and R. A. L. Drew, Understanding AlN Sintering Thrugh Cmputatinal Thermdynamics Cmbined with Experimental Investigatin, J. Mater. Prc. Tech., (005). 14. M. Kasri and F. Uen, Thermal Cnductivity Imprvement f YAG Added AlN Ceramics in the Grain Bundary Eliminatin Prcess, J. Eur. Ceram. Sc., (1995). 15. L. Qia, H. Zhu, H. Xue, and S. Wang, Effect f Y O n Lw Temperature Sintering and Thermal Cnductivity f AlN Ceramics, J. Eur. Ceram. Sc., 61-7 (00). 45«1y(008)

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