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1 Jurnal f the Krean Ceramic Sciety Vl. 46, N. 5, pp. 505~509, 009. DOI: /KCERS Wear Prperties f Silicn Nitride Nan-Ceramics Jae-Hee Kim, Venkata Manj Kumar B, Wn-Sik Kim, and Seng-Hyen Hng*, Department f Materials Science and Engineering, Seul Natinal University, Seul , Krea *Department f Materials Science and Engineering and Research Institute f Advanced Materials (RIAM), Seul , Krea (Received July 0, 009; Revised August 6, 009; Accepted August 9, 009) ù y³ ü p ½ ÁVenkata Manj Kumar BÁ½ Áy x*, w œw * œ (RIAM) ( ; ; ) ABSTRACT In this study, bulk nan-crystalline Si ceramics were fabricated by spark plasma sintering (SPS) and their mechanical prperties, in particular wear, were investigated. A wide range f grain sizes, frm 80 nm and 50 nm were btained by varying sintering cnditins (1550 C-5 min t 1650 C-0 min). The elastic mdulus f btained ceramics was ~50 GPa and hardness was in the range f 1~14 GPa. The indentatin fracture tughness increased frm.58 MPa m 1/ t.4 MPa m 1/ with increasing sintering temperature pssibly due t the elngated grains. Sliding wear tests revealed at least an rder magnitude imprvement in wear resistance with grain refinement. Micrstructure analysis indicated that nan-si specimens wrn mainly thrugh delaminatin and micrcracking, while that f carser specimens revealed severe wear with grain debnding and fracture. Key wrds : Nan-Si, Spark plasma sintering, Grain size, Wear prperties, Mechanical prperties l ù ƒ» p w ƒ. j»ƒ» p w šƒ ù» w». t Schuh 1) ù ƒ w z» p sƒw p w š šw. p š,, š ù ü p yw ƒ j y³ (Si ) t turbine ù gas turbine ƒ - š œ t š, ù mw», p ü p w jš w ƒ w š., Dgan ) 00 nm 5µm w s³ ƒ y³ ƒƒ w» p sƒw Crrespnding authr : Seng-Hyen Hng shhng@snu.ac.kr Tel : Fax : ü p w š šw. w s ³ j» 100 nm w» p š w w ƒ š. w ƒ ù ƒ š ww ù ƒ w w 100 nm w s³ ƒ ù w w». ù tw-step sintering, micrwave sintering, š spark plasma sintering (SPS) mw 100 nm w s³ ƒ ù w šƒ. -5) Ht isstatic pressing (HIP), spark plasma sintering (SPS), š ht pressing (HP) ù y³ w» w ù, j» 00 nm j»¾ w.,6-8) Li y³ ù š w w ù y w w 160 nm s³ ƒ w. e y š 100 nm w s³ ƒ ù y³ w ƒ. š ù SPS 505

2 506 ½ ÁVenkata Manj Kumar BÁ½ Áy x w 5,9) Y O ƒw wš tw-step sinteringw ). ƒ ƒ w SPS tw-step sintering w w mw ù j» y³ w w., w e y ù y³ s³ ü p š wš w. w, m y (SPS), œ» y k y³ w ü p d w.. x x 6wt% Y O wt% Al O (PCT6YA, Plasma and Ceramic Technlgy, Salaspils, Latvia)ƒ sw. t 70m /g, s³ 0 nm. ù œ» y, z ƒ d w 4.8% ƒ w. ) q w 10 mm» xw, x» w 150 MPa xw. r m y (SPS) w» w, 10 mm ü ƒ graphite die š, ~1500 A ~0 MPa ƒw œ w. 100 C/min, ƒƒ 1550~1650 C, 5 ~0 w w j» w. r j d w š, q r z O -CF 4 gas (80:0 in vl.) w v ew r, field emissin scanning electrn micrscpe (FESEM 7401F, JEOL, Japan) w w. s³ linear intercept methd Image Pr sftware (Media Cybernetics, Image-Pr Plus, USA) w d w. k (E, elastic mdulus) ultrasnic pulse-ech tester (Tektrnix TDS 0, Panametrics, Mdel 5800, Krea) w d. Vickers indenter (Mituyt, Japan) w d w. 1 kg w 15 w, 10 kg w 15 w Anstis s frmular k crack length d w w. 10) w ball-n-disc tribmeter w ü p d w» k. (0±5 C and 45±5% RH). ü p sƒ r cunterbdy Si balls (SBB Tech. C., Suwn, Krea) 6.5 mm. Si ball r ü p sƒ q» m w. Si balls x» ball hlder š 6mm wear track ü p sƒ 1500 rpm r z j m/s 44 m j j z w. x 5N w ƒw x w w w š x. 11) x, n-line (COF) w w». ƒƒ x z ww, s³» w. ü p wear track s y w» w, ƒ ù t SEM (JSM 5600, JEOL, Japan) FE-SEM w w. Wear track ¾ d w» w alphastep prfilmeter (Mdel N. 500, TENCOR, Germany) w. Wear track s ¾ w v w. wear vlume (mm )=π track radius track width wear depth (1) wear rate (mm /Nm) =wear vlume/ (nrmal lad sliding distance) (). š Fig. 1 w y³ r XRD. w Si N O swwš» s w ù. ) y³ Table 1» w, Fig. 1. XRD diffractin patterns f plished surfaces fr develped Si N O-cntained silicn nitride nanceramics; (a) 1550 C, 5 min, (b) 1600 C, 5 min, (c) 1650 C, 5 min, and (d)1650 C, 0 min. w wz

3 나노 질화규소 세라믹스의 내마모 특성 Characterizatin f the Tested Ceramic Materials Grain size (nm) Relative density (%) Cnditins [Density] Linear Diameter ( C-min) (g/cm ) Intercept (mean) [.05] [.06] [.06] [.07] Table 1. mdulus Aspect rati Elastic(GPa) HV (GPa) K (MPa m ) IC 1/ 있다. 이 결과는 이전 SPS를 사용하여 나노 세라믹스를 제조하는데 성공한 보고들 에서 볼 수 있듯이 SPS가 소 결 시간, 소결 온도를 줄여 입자성장을 억제하는데 효과 가 있음을 다시 한 번 확인할 수 있었다. Fig. (b)는 소 결 온도가 증가함에 따라 나노 입자로 구성된 모체 사이 에 길게 늘어난 β-si N 입자들의 수가 점점 증가하는 동 시에 평균입도도 증가한 것을 알 수 있다. Fig. (d)는 1650 C에서 0분 동안 소결된 시편의 미세구조를 나타내 고 있다. 파단면과 연마면에서 볼 수 있듯이 질화규소의 전형적인 미세구조인 이중미세구조(duplex micrstructure) 가 나타난 것을 확인할 수 있으며, 길게 늘어난 입자의 경우 ~1.8 µm까지 늘어난 입자도 보인다. 이렇게 늘어난 입자의 aspect rati는 최대 ~7 정도의 값을 보여주기도 하 였다. 그러나 여전히 늘어나지 않은 나노 크기의 equiaxed 입자들이 모체로써 상당 수 존재하여 평균입도는 ~50 nm 로 측정되었다 (Table 1). 제조된 질화규소 세라믹스의 탄성계수는 ~50 GPa 값 을 나타내었다 (Table 1). 경도는 입자크기 감소에 따라 1에서 14 GPa로 소폭 상승한 반면, 인성의 경우.에서.5 MPam 로 소폭 감소하였다. 이 값들은 마이크론/서브 마이크론의 질화규소 세라믹스에서 일반적으로 보고되는 가지는 기계적 특성 값과 거의 일치하는 값이며, 대략적 인 값으로 탄성계수는 50~00 GPa, 경도는 14~16 GPa 그 리고 파괴인성은 ~6 MPam 정도이다. 질화규소 세라믹스의 마찰 거동은 마모 시험 중에 생긴 마찰력을 계속적으로 측정한 값에 의존하여 평가하였다. 모든 시편은 시간에 따라 거의 동일한 마찰계수 거동을 나타내었으며, 평균 마찰계수는 0.47~0.54 사이의 값을 가 진다는 것을 확인하였으며, 입자크기의 영향력은 미미하 지만 그 크기가 줄어들수록 마찰계수 값이 ~10% 정도 소 폭 감소했음을 알 수 있다(Fig. (a)). 제조된 질화규소 세라믹스의 마모율 변화를 Fig. (b)에 나타내었다. 마모율 은 10 ~10 mm /Nm의 값을 가졌으며, 입자크기가 작아질 수록 마모율이 10배 가량 감소하였다. 입자크기가 큰 1650 C, 5분과 0분 시편(~190 nm, ~50 nm)에서는 ~10 mm /Nm 정도의 값을 나타내었고 입자크기가 작은 1550 C, 5분 시 편(~80 nm)에서는 mm /Nm 정도의 값을 보여주 며 최소값으로 측정되었다. 입자크기와 마모율의 관계(Hall 5,9) 4 1/ 1/ Fig.. FESEM micrgraphs f fractured and etched surface (a) sintered at 1550 C, 5 min, (b) 1600 C, 5 min, (c) 1650 C, 5 min, and (d) 1650 C, 0 min. 이론 밀도의 ~94%에 이르렀으나 더 이상의 밀도 증가는 나타나지 않았다. 이론 밀도가.6으로 계산되었는데 이 는 시편 내에 Si N O 이차상이 없을 때 사용 가능한 값 이다. 그러나 제조된 시편 내에는 많은 양의 Si N O 이차 상이 존재하고 있기 때문에 상대밀도 값이 실제의 값보 다 떨어진 것이라 여겨진다. 좀 더 정확한 밀도 값을 알 기 위해서는 추가적인 실험이 요구된다. Fig. (a)는 1550 C에서 소결한 시편의 파단면과 연마면을 나타낸 미 세조직이며 Table 1에 기재한 것처럼 평균입도는 ~80 nm 정도인 나노 크기의 입자로 이루어져 있음을 확인할 수 1) 1) 제 46 권 제 5호(009)

4 김재희 Venkata Manj Kumar B 김원식 홍성현 508 Fig. 4. Fig.. (a) Average COF and (b) wear rate with sintering cnditins in the develped SiNO phase-cntained silicn nitride nan-ceramics. Petch-type relatin)는 길게 늘어난 입자들 때문에 이 실험 에서는 정량적으로는 다루기는 어렵지만, 적어도 질화규 소 세라믹스의 내마모성이 입자크기가 감소함에 따라 크 게 향상될 수 있다는 것은 명확히 말할 수 있겠다. 제조 된 질화규소 세라믹스를 가지고 마모 시험 중 재료에서 일어난 마모 기구를 파악하기 위해 SEM 분석을 실시하 여 Fig. 4에 나타내었다. Equiaxed 모양의 나노 입자로 이 루어진 1550 C 시편의 마모된 표면을 살펴보면 주로 여 러 층으로 덮여있음을 확인할 수 있다. 이 층들은 시편 표면이 변형되어 생성된 것이며 micrcracks이 자주 발견 되는 것을 알 수 있다(Fig. 4(a)). 남겨져 있는 debris 입자 들은 대부분 0.1~1 µm 지름을 가지는 둥글며 길쭉한 형 태이다. 그러나 소결 온도가 증가함에 따라 입자 크기가 증가한 1600 C 이상의 시편에서는 그 마모된 표면의 모 양이 눈에 띄게 변화되고 있음을 알 수 있다. 즉, wear track 내에서 부분적으로 이전보다 더욱 심한 균열이 일 어나는 비율이 점점 크게 증가하고 있다는 것을 의미한 다 (Fig. 4(b)). Cracking과 grain debnding의 정도는 소 결 온도가 증가함에 따라 같이 증가하여 마모의 정도가 점점 심해지는 것을 알 수 있다 (Figs. 4(c)와 (d)). 게다가 한국세라믹학회지 SEM micrgraphs f wrn surface fr SiNO phasecntained silicn nitride nan-ceramics; (a) sintered at 1550C, 5 min, (b) 1600C, 5 min, (c) 1650C, 5 min, (d), (e), and (f) 1650C, 0 min. Fig. 4(b)의 부분확대사진(오른쪽 상단)에서 볼 수 있듯이, 표면 밑부분까지도 마모가 일어나 표면 아래 부분이 드 러난 것을 알 수 있다. 이러한 현상은 1600 C 시편에서는 부분적으로 일어난 것에 그쳤지만, 1650 C, 5분과 0분의 시편에서는 위와 같은 정도의 마모가 지배적으로 일어났 음을 나타내고 있다. 이러한 사실은 마모 시험이 같은 조 건에서 행해졌음에도 불구하고 균열의 전파가 훨씬 빠르 고 많이 일어날 때 생기는 lateral cracking 현상에 의해 설 명될 수 있다. Lateral cracking이 일어남에 따라 grain debnding과 mechanical fracture 등의 현상이 더 넓은 지 역에서 급격하게 가속화되어 마모가 심하게 나타난 것으 로 여겨진다 (Fig. 4(c) 오른쪽 상단). Fig. 4(e)와 (f)는 마 모가 계속적으로 일어남에 따라 생겨난 많은 양의 debris 가 서로 뭉쳐 하나의 층(cmpacted layers)을 형성하고 있 으며 이 층이 wear track 곳곳을 광범위하게 덮고 있어 마 모가 굉장히 심하게 일어난 것을 알 수 있다. 입자크기 변화에 대한 마모기구를 정리하면, equiaxed 형태의 나노 미세구조를 가지는 시편에서는 delaminatin 현상이 주로 나타나 상대적으로 마모가 심하지 않았으며, 입자가 더 커지고 이중미세구조를 가지는 시편에서는 fracture가 지 배적으로 나타나 마모가 더욱 심하게 일어나는 양상을 나 타내었다고 할 수 있다. 이러한 마모 기구의 변화는 14-18)

5 ù y³ ü p 509 Fig. (b) y ew. 4. β-si -6 wt%, Y O - wt%, Al O yw SPS 1550 C-5 min 1650 C-0 min¾ w w. e y y³ Si N O w ƒƒ 80 nm 50 nm¾ w j» s³ ƒ. β-si w y ü p sƒ w. j»ƒ w w ~10% ùkü š, j» mm /Nm¾ j., j»ƒ ù j» 10 w ü p j w. w» w j j» ù ƒ (duplex micrstructure) y³ grain debnding transgranular fracture w ƒ ù debrisƒ x. ƒ w ù ew, equiaxed xk ù» w» delaminatin micrcracks ù y w. m w ù ƒ ù ü p. Acknwledgment This study was supprted by a grant frm the Fundamental R&D Prgram fr Cre Technlgy f Materials funded by the Ministry f Knwledge Ecnmy, Republic f Krea. REFERENCES 1. C. A. Schuh, T. G. Nieh, and H. Iwasaki, The Effect f Slid Slutin W Additins n the Mechanical Prperties f Nancrystalline Ni, Acta Mater., 51 [] 41-4 (00).. C. P. Dgan and J. A. Hawk, Micrstructure and Abrasive Wear in Silicn Nitride Ceramics, Wear, 50 [1-1] 56-6 (001).. H. D. Kim, Y. J. Park, B. D. Han, M. W. Park, W. T. Bae, Y. W. Kim, H. T. Lin, and P. F. Becher, Fabricatin f Dense Bulk Nan-Si Ceramics withut Secndary Crystalline Phase, Script. Mater., 54 [4] (006). 4. J. Lu, K. Zhang, G. Wang, and W. Han, Fabricatin f Fine-Grained Si -Si N O Cmpsites by Sintering Amrphus Nan-Sized Silicn Nitride Pwders, J. Wuhan Univ. Tech. - Mater. Sci. Ed., 1 [00] 97-9 (006). 5. X. Xu, T. Nishimura, N. Hirsaki, R. J. Xie, and H. Tanaka, Fabricatin f a Nan-Si /Nan-C Cmpsite by High- Energy Ball Milling and Spark Plasma Sintering, J. Am. Ceram. Sc., 90 [4] (007). 6. T. Nishimura, M. Mitm, H. Hirtsuru, and M. Kawahara, Fabricatin f Silicn Nitride Nan-Ceramics by Spark Plasma Sintering, J. Mater. Sci. Lett., 14 [15] (1995). 7. I. Tanaka, G. Pezztti, T. Okamt, Y. Miyamt, and M. Kizumi, Ht Isstatic Press Sintering and Prperties f Silicn Nitride withut Additives, J. Am. Ceram. Sc., 7 [9] (1989). 8. Y. L. Li, Y. Liang, F. Zheng, X. F. Ma, and S. J. Cui, Sintering f Nanpwders f Amrphus Silicn Nitride under Ultrahigh Pressure, J. Mater. Res., 15 [4] (000). 9. X. Xu, T. Nishimura, N. Hirsaki, R. J. Xie, Y. Zhu, Y. Yamamt, and H. Tanaka, New Strategies fr Preparing Nansized Silicn Nitride Ceramics, J. Am. Ceram. Sc., 88 [4] 94-7 (005). 10. G. R. Anstis, P. Chantikul, B. R. Lawn, and D. B. Marshall, A Critical Evaluatin f Indentatin Techniques fr Measuring Fracture Tughness: I, Direct Crack Measurements, Eng. Fract. Mech., (197). 11. D. S. Lim, J. W. An, and H. J. Lee, Effect f Carbn Nantube Additin n the Triblgical Behavir f Carbn/Carbn Cmpsites, Wear, 5 [5-6] (00). 1. G. Petzw and M. Herrmann, Silicn Nitride Ceramics, Struct. Bnd., 10 [5] (00). 1. D. H. Jeng, F. Gnzalez, G. Palumb, K. T. Aust, and U. Erb, The Effect f Grain Size n the Wear Prperties f Electrdepsited Nancrystalline Nickel Catings, Script. Mater., 44 [] (001). 14. N. P. Suh, Delaminatin Thery f Wear, 5 [1] (197). 15. O. Desa and S. Bahadur, Material Remval and Subsurface Damage Studies in Dry and Lubricated Single-Pint Scratch Tests n Alumina and Silicn Nitride, Wear, (1999). 16. D. C. Cranmer, Frictin and Wear Prperties f Mnlithic Silicn-Based Ceramics, J. Mater. Sci., 0 [6] 09-7 (1985). 17. Y. Wang and S. M. Hsu, Wear and Wear Transitin Mechanisms f Ceramics, Wear, 195 [1-] 11- (1996). 18. T. E. Fischer and H. Tmizawa, Interactin f Tribchemistry and Micrfracture in the Frictin and Wear f Silicn Nitride, Wear, (1985). 46«5y(009)

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