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1 Jurnal f the Krean Ceramic Sciety Vl. 47, N. 6, pp. 40~4, 010. DOI: /KCERS Phase Stability and Plasma Ersin Resistance f La-Gd-Y Rare-earth Oxide - Al O Ceramics Kyeng-Bem Kim and Sung-Min Lee Engineering Ceramics Center, Krea Institute f Ceramic Engineering and Technlgy, Ichen , Krea (Received Octber 10, 010; Revised Octber 1, 010; Accepted Octber 16, 010) La-Gd-Y m y - ù y üv p ½ Á w» l ( ; ; ) ABSTRACT In this study, we have investigated new plasma resistant materials with less usage f rare-earth xides than Y O which is currently used in the semicnductr industry. We bserved the stability ranges f (Gd Y) O and (La Y)Al O ternary systems, and measured their etch rates under typical flurine plasma. (Gd Y) O system shwed an extensive slid slutin up t 80 ml% gadlinium, but (La Y)Al O shwed a negligible substitutin between rare-earth ins, which can be explained by the differences between the inic radii. The etch rates depended n the ttal amunt f rare-earth xides but nt n the substitutin f the rare-earth ins. When the specimen was examined using XPS after the expsure t flurine plasma, the strng surface flurinatin was bserved with a shift f the binding energy t higher energy. Key wrds : Rare-earth xide, Plasma resistance, Phase stability 1. syƒ œ v œ w j wš ƒ ƒw ƒ š. 1) v œ yw y e w yw k v w w t w jš ƒ w. ) üv w t Al O üv w Y O ƒ k š. -10) Y O ƒ v Al O w ü ƒ p p yw w ƒ š» š. Kim v - p g xr t yƒ j Crrespnding authr : Sung-Min Lee smlee@kicet.re.kr Tel : Fax : w š k p ww. yw ƒ ) ƒ w ƒ, y j rl ƒ û š w p yw ƒ. ) Y O ƒ üv ù wù ³ew ƒ w w ƒ š x r. Y O k m w ù wš m y - ù üv w mw. Y O Al O ƒw ƒ w. ƒ Y O sww ù yw garnet ƒ Y O. yw Y O ù w ù Al O ƒ w š v y ù k ƒ ù ƒ. m y yw üv ) w» w w yw w kw v ƒ. 40

2 La-Gd-Y 희토류계 산화물-알루미나 세라믹스의 상안정화 영역과 내플라즈마 특성 41 Plasma Etching Cnditins Parameter RF pwer, W RF pwer (bias), W CF, SCCM O, SCCM Ar, SCCM Pressure, mtrr Table 1. Cnditin 을 이용하여 분쇄한 분말 원료를 준비하였다. 준비된 분 말을 지름 10 mm의 금속몰드에 충진시키고 저압으로 1 차 성형한 후 냉간정수압성형기(Cld Isstatic Press)를 사 용하여 00 MPa의 압력으로 두께 mm의 성형체를 얻었 다. 성형된 시험편을 대기 분위기하에서 C/min로 1680 C 까지 승온한 후 4시간 소결하고 노냉하여 소결체를 제조 하였다. 소결이 끝난 시험편을 9,, 1 (µm) 단계의 다이 아몬드 페이스트를 사용하여 경면 연마하였으며 아세톤 에서 초음파를 사용하여 세척하였다. 제조한 시험편과 비 교할 시험편으로 (0001)면의 단결정 사파이어(광학연마급, 사파이어 테크놀러지, 한국)와 동일한 조건에서 제조한 이 트리아 소결체 및 쿼츠유리를 사용하였다. 연마한 시험편 표면의 중간 영역을 폭 0. mm만 노출 되도록 켑톤 테이프를 사용하여 마스킹하였다. 내플라즈 마성을 평가할 식각장치로는 ICP (Inductively Cupled Plasma)형의 식각장치(Versaline, UNAXIS C., USA)를 사 용하였다. 식각가스로는 CF 와 O 를 사용하였고 플라즈 마에 노출시킨 시간은 10분씩 6번 총 60분 이었으며 자 세한 식각 조건을 Table 1에 나타내었다. 플라즈마에 노출된 시험편의 화학조성 및 화학결합 상 태를 분석하기 위하여 XPS (PHI 000, Ulvac-phi C., Japan)를 사용하였다. 한편 소결체의 결정상을 분석하기 위하여 고출력 X-선 회절기(D/max-00, Rigaku, Japan)를 이용하여 1 kv, 0 ma의 조건에서 10 /min의 속도로 분 쇄된 소결체의 분말을 스캔하여 회절패턴을 얻었다. 표면 의 미세구조와 성분을 관찰하기 위하여 시험편을 백금으 로 코팅한 후 FE-SEM (JSM-6701F, Jel, Japan)을 이용 하여 분석하였다. 또한 시험편의 식각깊이를 surface prfiler(surfcrder ET000, Ksaka Lab., Japan)를 이용하 여 측정하였다. Fig. 1. Experimental chemical cmpsitins (ml%) f rareearth xide and Al O ceramics : (a) Y-Gd-Al and (b) YLa-A systems. 본 연구에서는 Gd-Y-Al계와 La-Y-Al계의 삼성분계 상 태도에서 가장 희토류 산화물을 적게 사용하면서 안정된 화합물을 만드는 Y Al O 와 LaAl O 에 각각 Y 대신 Gd을 La 대신 Y을 치환하면서 상안정영역을 조사하였다. 제조된 시험편을 불소계 플라즈마에 노출시킨 후 식각율 을 측정하고 표면의 조성을 XPS를 이용하여 분석하였다.. 실험방법 내플라즈마성을 평가하기 위한 시험편을 제조하기 위 하여 고순도 알루미나(AKP-0, Sumitm Chemical C., Japan)와 고순도 이트리아(C-grade, H. C. Starck, Germany), 고순도 가돌륨산화물(99.9%, Kjund Chemical C., Japan), 고순도 란탄산화물(99.9%, Kjund Chemical C., Japan)을 사용하였다. 실험에 사용한 조성을 Fig. 1에 표기하였다 (Gd0-Gd100, La0-La100). 준비된 원료를 무수에탄올을 용 매로 분산제(RE 610, Rhdia C., USA)를 첨가한 뒤, Al O 볼을 사용하여 0시간 동안 밀링하였다. 혼합이 완 료된 슬러리를 핫 플레이트 위에서 교반하며 일차 건조 한 후 80 C의 오븐에서 시간 동안 추가 건조하고 유발 4. 결과 및 토의 Fig. 는 (Gd Y) Al O 와 (La Y)Al O 의 전체 희토류 원소중에서 이트륨의 함량을 0 ml%씩 변화시킴에 따라 발생하는 결정상의 변화를 보여주고 있다. (Gd Y) Al O 는 희토류원소중 Gd의 상대적 함량이 0~80 ml%의 범위 제 47 권 제6호(010)

3 4 ½ Á Fig.. X-ray diffractin patterns fr (a) (Gd Y) O and (b) (La Y)Al O ceramics sintered at 1680 C fr 4 h. garnet ƒ w ƒ Gd w 100 ml%ƒ garnet w š GdAlO Al O ƒ ù y w. w (La Y)Al O m La w 80 ml% garnet crundum ùkùš La w w LaAl O w ƒ La w 0ml% garnet crundum. wr m Y ml% ƒƒ k d w š. y w» w Fig. X z e vj z t wš y ùkü. (Gd Y) O garnet z vj I (), GdAlO I (0), Fig.. Relative fractin f phases frm X-ray peak intensities : (a) Garnet, GdAlO and Al O, and (b) LaAl O, Garnet and Al O. crundum I (104) l ƒ w. ƒ (La Y)Al O crundum vj I (104), garnet I (01), LaAl O I (0) w. w l garnet ƒ (Gd Y) O š ƒ š, (La Y)Al O š ƒ ƒ œ w y w. w š + La +, Gd +, Y j» y ƒw +ƒ +ƒ. Y 0.9 Å, Gd ƒ + Å, La 1.0 Å, Gd Y + 4.4%, La 14.4% j j» ƒ š. Gd + Y ey š ƒ + š, La + š ƒ w. (Gd Y) O (La Y)Al O m Y w 0, 60 ml% d Fig. 4 ùkü. X z w wz

4 La-Gd-Y 희토류계 산화물-알루미나 세라믹스의 상안정화 영역과 내플라즈마 특성 Fig Micrstructures f (a) Gd40 and (b) Gd100 in (Gd Y) Al O ceramics, and (c) La40, and (d) La100 in (La Y)Al O ceramics sintered at 1680 C fr 4 h. Fig. 6. Etch rates under flurine plasma expsure fr 1 h. 에서 예측되는 것과 같이 (Gd Y) Al O 의 경우 Gd가 100 ml% (Gd100) 일 때 밝은 색상의 GdAlO 와 어두운 색상의 Al O 을 확인 할 수 있었다. 이와 비교하여 Gd의 함량이 40 ml% (Gd40)일 때 단일상으로 구성되어 있는 것을 확인할 수 있으며 EDX 분석상으로도 Y : Gd의 원 자비가 약 6 : 으로 출발조성으로부터 예상되는 값과 유사하였다. 따라서 X선 회절 분석결과와 종합하여 보면 (Gd Y) Al O 의 고용체 범위는 희토류 원소중 Gd의 함 량기준 80 ml% 이상인 것으로 판단되었다. 반면에 (La Y)Al O 계의 희토류 원소중 La의 함량이 100 ml% (La100) 일 때 LaAl O 단일상으로 구성되어 있으며, 희토류 원소중 La 의 함량이 40 ml% (La40) 일 때 반사전자이미지를 살펴보면 세 가지 상이 존재하는 것 을 확인할 수 있다. EDX 분석결과 밝은 색은 Y Al O 으 로, 회색은 LaAl O, 검은색은 Al O 로 확인되었다. LaAl O 결정의 Y 고용량과, Y Al O 결정의 La 고용량 Fig.. Tentative isthermal sectins at 1680 C f the ternary phase diagram f (a) Y-Gd-Al and (b) Y-La-Al systems. 제 47 권 제6호(010)

5 44 ½ Á Table. Chemical Cmpsitins Measured frm XPS Analysis Element Selected peak Atmic fractin, % Atmic sensitivity factr fr cmpsitin calculatin Al p La 4d F 1s O 1s C 1s Fig. 7. Phtelectrn spectrum fr Al atms n the LaAl O surface after the expsure t flurine plasma and reference(yalo ) specimen. EDX w w. m j» l w ew. l 1680 C k xk Fig. ùkü. wz w y l yw xk w». xr v k z ƒ d w. w xr q, id, Y O w (Fig. 6). x id ƒ ƒ ƒ r, q.6%, Y O 1.%, (Gd Y) O.8~.8%, (La Y)Al O 8.6~.1% ƒ ùkü. m w ƒ û, m w. š ùkü (Gd Y) O m w Gd w 0~80 ml% yw ƒ r ±1% w. XPS(X-ray phtelectrn spectrscpy) w v t yw w k w. Table LaAl O t ùkü w atmic sensitivity factr»w ùkü. t w y w š,) w y w» w t e XPS vj e 8 ev» Al vj w. m y Al p e 7.8 ev w v w ƒ 1.8 ev w (Fig. 7).» ƒ ƒ xr t ww yw cre level p k» ƒw. t 1) w ƒ vj e yƒ w w š w. y xr t y YF, LaF, GdF ƒ š ƒ w t d ƒ w t d r l w. rl rl y w, YF y 481 kj/ml, LaF 4 kj/ml, GdF 40 kj/ml m y j. m ƒ 14) sw m m w ƒ j w w. 4. m y ù yw ƒ üv p y wš w. m y ù yw m y (Gd Y) O (La Y)Al O kw š ƒ w. (Gd Y) O m Gd š ƒ 0~80 ml%, (La Y)Al O Y La š. w w m w. w ƒƒ w v ƒ d w ƒ m w j w š m ey w j. Acknwledgment ù» y w. w wz

6 La-Gd-Y m y - ù y üv p 4 REFERENCES 1. G. S. May and C. J. Spans, Fundamentals f Semicnductr Manufacturing and Prcess Cntrl, pp , Jhn Wiley & Sns, Inc., New Jersey, A. J. V. Rsmalen, J. A. G. Baggerman, and S. J. H. Brader, Dry Etching fr VLSI, pp. 9-69, Plenum Press, New Yrk and Lndn, D-M. Kim, S-Y. Yn, K-B. Kim, H-S. Kim, Y-S. Oh, and S-M. Lee, Plasma Resistance f Yttria Depsited by EB- PVD Methd (in Krean), J. Kr. Ceram. Sc., 4 [] 707- (008). 4. D-M. Kim, S-M. Lee, S-W. Kim, H-T. Kim, and Y-S. Oh, Micrstructural Changes f the Al O Ceramics during the Expsure t Flurine Plasma (in Krean), J. Kr. Ceram. Sc., 4 [7] (008).. D-M. Kim, K-B. Kim, S-Y. Yn, Y-S. Oh, H-T. Kim, and S-M. Lee, Effects f Artificial Pres and Purity n the Ersin Behavirs f Plycrystalline Al O Ceramics under Flurine Plasma, J. Ceram. Sc. Jpn., 7 [8] (009). 6. K. Mrita, H. Uen, and H. Murayama, Plasma Resistant Articles and Prductin Methd Theref," US Patent 694 (00). 7. A. Miyazaki, K. Mrita, S. Nagasaka, and S. Mriya, Plasma Resistant Member and Plasma Treatment Apparatus Using the Same, US Patent (004). 8. R. J. O Dnnell, J. E. Daugherty, and C. C. Chang, Brn Nitride/ Yttria Cmpsite Cmpnents f Semicnductr Prcessing Equipment and Methd f Manufacturing Theref, US Patent (004). 9. Y. Kbayashi, M. Ichishima, and Y. Ykyama, Plasma Resistant Member, US Patent (006). 10. J. Iwasawa, R. Nishimizu, M. Tkita, M. Kiyhara, and K. Uematsu, Plasma Resistant Dense Yttrium Oxide Film Prepared by Aersl Depsitin Prcess, J. Am. Ceram. Sc., 90 [8] 7- (007).. D-M. Kim, K-B. Kim, S-H. Lee, Kim, J-K. Lee, Y-S. Oh, and S-M. Lee, XPS Study n the Interactin f Yttrium- Aluminum Oxide with Flurine-based Plasma, J. Am. Ceram. Sc., submitted, (010).. K-B. Kim, D-M. Kim, J-K. Lee, Y-S. Oh, H-T. Kim, H-S. Kim, and S-M. Lee, Ersin Behavirs f YAG Ceramics under Flurine Plasma and their XPS Analysis, J. Kr. Ceram. Sc., 46 [] (009). 1. J. C. Vickerman and I. S. Gilmre, Surface Analysis p., nd ed., Wiley, Singapre, R. A. Kent, Mass Spectrmetric Studies f Plutnium Cmpunds at High Temperatures. II. The Enthalpy f Sublimatin f Plutnium(III) Fluride and the Dissciatin Energy f Plutnium(I) Fluride, J. Am. Chem. Sc., 90 [1] 67-9 (1968). 47«6y(010)

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