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1 J. Kor. Powd. Met. Inst., Vol. 19, No. 5, 2012 DOI: /KPMI pk gqd p d e x w y ûá Á½x a Á x b Á» w œw, a sw w, b w» Effects of Powder Morphology and Powder Preheating on the Properties and Deposition Behavior of Titanium Coating Layer Manufactured by Cold Spraying Jae-Nam Hwang, Myeong-Ju Lee, Hyung-Jun Kim a, Ik-Hyun Oh b and Kee-Ahn Lee School of Advanced Mater. Eng., Andong National University, Andong , Korea a RIST, Pohang , Korea b KITECH, Gwangju , Korea (Received July 23, 2012; Revised August 7, 2012; Accepted August 16, 2012) Abstract Cold spray deposition using Titanium powder was carried out to investigate the effects of powder morphology and powder preheating on the coating properties such as porosity and hardness. The in-flight particle velocity of Ti powder in cold spray process was directly measured using the PIV (particle image velocimetry) equipment. Two types of powders (spherical and irregular ones) were used to manufacture cold sprayed coating layer. The results showed that the irregular morphology particle appeared higher in-flight particle velocity than that of the spherical one under the same process condition. The coating layer using irregular morphology powder represented lower porosity level and higher hardness. Two different preheating conditions (no preheating and preheating at 500 o C) were used in the process of cold spraying. The porosity decreased and the hardness increased by conducting preheating at 500 o C. It was found that the coating properties using different preheating conditions were dependent not on the particle velocity but on the deformation temperature of particle. The deposition mechanism of particles in cold spray process was also discussed based on the experimental results of in flight-particle velocity. Keywords: Cold spraying, Titanium, Coating, Porosity, Hardness, Microstructure, In-flight particle velocity 1. pk w ü» p» w wœ,, yw,,, sd t w t š [1-3]. w pk ƒ ù w. wì (hexagonal closed packed) p x š, w š p w w z v w [4]. w ey ƒ pk p w œ»» w œ j w š [5]. pk p w w œ š ƒ w w x t w w» š [1,6,7]. pk œ y w wù, gq w» š. *Corresponding Author : Kee-Ahn Lee, TEL: , FAX: , keeahn@andong.ac.kr 348

2 저온 분사 티타늄 코팅층의 특성 및 적층 거동에 미치는 분말 형상과 분말 예열의 영향 분사 코팅(Cold Spray Deposition)은 보통 1~50 µm의 입 도를 가지는 분말 소재를 초음속 제트 속도로 가속시켜 모재와 충돌시켜 분말 소재의 소성변형에 의해 고상 상태 에서 치밀한 코팅층을 형성하는 신 제조 공정 기술이다[8,9]. 특히 이 공정은 저온에서 코팅 공정이 이루어지므로 제조 도중 산화에 의한 상 변화 및 특성 저하 등의 단점을 극 복할 수 있고 높은 밀도, 높은 순도를 가지는 코팅층 형성 에 유용한 방법으로 관심이 집중되고 있다. 저온 분사 코 팅 공정은 산소와 반응성이 높은 티타늄 소재 분말 등에 쓰이기 적합하며 그 외에 나노 분말이나 비정질 분말 등 열적으로 민감한 소재에도 적용이 용이하다[10-12]. 그러나 저온 분사 코팅 공정에 의한 금속 분말의 적층 기구는 아직 명확하게 규명되고 있지 않은 실정이다. 현재 까지 많이 인용되고 있는 적층 기구의 대부분은 현상학적 접근 방법에 의한 것이다. 즉 초음속의 속도를 가진 입자 가 모재와 충돌하여 심한 소성변형을 일으키며 금속간의 결합을 하고 이후 계속되는 입자의 충돌이 먼저 형성된 코팅층을 더욱 치밀하게 하며 연속적 입자의 적층이 가능 하다고 알려져 있다[13,14]. 그리고 분말 입자의 비행 속 도에 의한 충돌 시 운동 에너지가 가장 중요한 요소로 작 용하며, 주로 분말 소재의 입자 크기와 형상, 공정 가스의 종류와 압력, 온도, 노즐의 형상 등에 크게 영향을 받는 것 으로 보고되고 있다[15,16]. 그러나 저온 분사 공정을 이 용한 금속 분말의 코팅층 제조에서 티타늄 소재의 경우는 구리(Cu)나 알루미늄(Al) 등 소재에 비하여 치밀하고 우수 한 특성의 코팅층을 얻기가 어렵다[17]. 이와 관련하여 저 온 분사 코팅 공정 중에 공정 조건이 티타늄 분말의 적층 거동과 코팅 특성에 어떠한 영향을 미치는지 먼저 제시되 349 어야 하지만 현재까지 연구가 부족한 실정이며 특히 티타 늄 코팅층의 특성을 분말의 입자 비행 거동과 연관하여 해석한 경우는 제시된 바 없다. 본 연구에서는 티타늄 분말이 저온 분사 코팅 공정을 통 하여 코팅층을 형성하는데 있어서 분말의 형상 및 분말의 예열 온도가 적층 거동과 코팅 특성에 어떠한 영향을 미 치는지 조사하였다. 이와 함께 저온 분사 코팅 공정 중 분 말 입자 속도를 직접 측정하여 미세조직 및 특성과 연계 하여 저온 분사 티타늄 코팅층의 적층 거동을 규명해보고 자 하였다. 2. 실험방법 본 연구에서는 Hydride-dehydride(HDH) 공정과 Plasma atomization(pa) 공정으로 제조된 두 종류의 순수 티타늄 분말을 사용하였다. 그림 1은 광학 현미경과 주사전자현 미경(SEM)을 이용하여 관찰한 두 분말 입자의 형상과 단 면 미세조직 관찰 결과이다. (a)와 (d)는 SEM을 이용하여 각 분말의 표면 형상을 관찰한 결과이며, (b)와 (c), (e)와 (f)는 분말 단면 조직의 에칭 전, 후 미세조직을 각각 나타 낸 것이다. P 분말(Pyungkwang 사 제조, HDH 공정 사용, 이 후 P 분말로 명명)의 경우((a), (b), (c))는 불규칙 형상을 가지고 있으며 내부에 기공이 존재하는 스폰지 형태의 조 직을 나타내었다. 이에 반해 R 분말(Raymor 사 제조, PA 공정 사용, 이후 R 분말로 명명)은 구상의 형상을 가지며 기공이 거의 없는 상대적으로 조밀한 조직을 나타내었다. 티타늄 분말들의 입자 크기 분포를 측정한 결과, P 분말 의 입자 크기는 2~90 µm(평균 입자 크기 28 µm), R 분말 Fig. 1. Morphology and cross-sectional microstructure of the feedstock powders; (a) SEM image, (b) cross-sectional, (c) etched cross-sectional microstructures of P Ti powders, (d) SEM image, (e) cross-sectional, and (f) etched cross-sectional microstructures of R Ti powders. Vol. 19, No. 5, 2012

3 350 y ûá Á½x Á xá» Table 1. Processing parameters of cold spraying used in this study Cold spraying equipment High pressure (DPD-725 model) Coating material P type Ti powder R type Ti powder Standoff distance (mm) 30 Powder feed rate (kg/h) Pressure (bar) 28 Gas temperature ( o C) 600 Powder temperature ( o C) (RT) 500 Traverse speed (mm/s) 40 Propellant gas type N 2 Substrate Al6061 (no blasting) Nozzle model MOC230LC30 j» 3~80 µm(s³ j» 32 µm) ùk û. P R, ƒƒ 0.49%, 0.14% w wš. w ƒƒ 164 H v (P ) 165 H v (R ) œ w ùkü. gqd (P R ƒ ) DPD-72S š e w ww. w œ ƒ d e w» w R w 500 o C w gqd w. gqd w ƒ w x ww, k œ t 1 w. gqd Al 6061 q w 30 mm š w š ƒ (N 2 ) w. r d w» w, q(mounting)w r w w t w z Ÿw x w w.»œ Ÿwx v w 10 d w z s³ ü w. Vickers» w w 300 g r gq gq, t 3 ù ƒ 10 d w s³ ü. ƒ r e z 85 ml distilled water+10 ml HF+5 ml HNO 3 w 5~10 k z Ÿw x w w. wr gq œ ww, s, s³ d w» w š CCD e (Spray Watch camera), (illumination) w e(hi- Watch laser) d (Spray Watch system, Oseir Ltd.) w w w. l k d e ful w v w w s s³ w. w d l 30 mm ( ƒ d» ) 20 mm 20 mm 1 mm d w.» w d e 2 ùkü. 3. x š 3.1. pk x gqd p d 3 P ( ³ex) R ( x) w Fig. 2. Schematic illustration and experimental set up for the in-flight particle velocity measurement during cold spraying. Journal of Korean Powder Metallurgy Institute (J. Kor. Powd. Met. Inst.)

4 pk gqd p d e x w 351 Fig. 3. The cross-sectional microstructures of the Ti coating layers manufactured using different powder morphologies of (a) P Ti angular powder and (b) R Ti spherical powder. Fig. 4. Porosity and hardness measurement results of cold sprayed coating layers with different powder morphology. Fig. 5. Etched cross-sectional optical micrographs of Ti coating layers with different powder morphologies of (a) P Ti powder and (b) R Ti powder. w œ (t 1) gqd w z w. gqd 3 mm Ì gqd. w P w gqd((a)) R w gqd ((b)) w š w d y w. P R w w gqd»œ d 4 v w.»œ ƒ gqd t»œ w û ùküš gqd t ùküš. w Vol. 19, No. 5, 2012

5 352 y ûá Á½x Á xá» gq œ ƒ y» x w d z, ƒ d w (peening)z» w [17].»œ d w P gqd ƒ R gqd û»œ ( ) ùküš. P gqd(s³ Hv) R gqd(s³ H v ) d. 5 P ((a)) R ((b)) w w gqd e z ùk ü. gq d z w x ù. ù x ( ³ex(P ) x(r )) ƒ x P gqd w x ùkü d.»œ r, P gqd R gqd w j»»œ swš. pk œ s³ w w s d 6 ùkü. P R w s ƒ s(gaussian distribution) š P sƒ w. P R s³ w ƒƒ m/s, m/s P s³ w ƒ 20 m/s ùkû. Raletz [18] œ p v (one-dimensional isentropic theory) ƒ w (1) tx š w. = V p M a γrt C D A p ρ g x m p» V p, M a ƒ w (Mach number), g ƒ (heat capacity), R», C D w (drag coefficient), A p, ρ g ƒ, x, m p ùk ü. œ w» w w C D A p, m p w. Fukanuma [19] x w w x ~1.0 w ƒ ³ex x w ƒ š w w. wr w ( ) ƒ x x ƒ ƒ. w ƒ š ƒ w ³ex w ƒ. j w ƒ ³e x w œ ƒ w. œ p w (critical velocity) j ƒ d gqd x w» w š. ³ex P x R w œ s³ ƒ š y. ³ex P g qd w d v w ƒ ƒ ƒ. ³ex d j w š x w w w gqd ƒ (1) Fig. 6. In-flight particle velocity measurement results of Ti powder particle (with different powder morphology) by Spray Watch system. Journal of Korean Powder Metallurgy Institute (J. Kor. Powd. Met. Inst.)

6 pk gqd p d e x w 353 Fig. 7. The cross-sectional microstructures of the R Ti coating layers manufactured using different powder preheating conditions of (a) no powder preheating and (b) Ti powder preheating at 500 o C. Fig. 8. Porosity and hardness measurement results of cold sprayed coating layers with different powder preheating conditions. Fig. 9. Etched cross-sectional optical micrographs of Ti coating layers with different powder preheating conditions of (a) no preheating and (b) preheating at 500 o C. q. ùkù»œ w š û»œ ùkü ƒ x w. 3.2 pk gqd p d 7 pk (R, x) œ 30 o C(,, (a)) 500 o C((b)) w gqd Ÿwx w. gqd w 500 o C ww gqd»œ j»ƒ w ùkû. 8» gqd»œ t w. gqd Vol. 19, No. 5, 2012

7 354 y ûá Á½x Á xá» Fig. 10. In-flight particle velocity measurement results of Ti powder (with different powder preheating condition) by Spray Watch system. (, ü, t ) 500 o C w, gqd»œ wš ƒw w š. 9 r e z ùküš. w w gqd ((a)) d» xk w w š 500 o C ww ((b)) d wù wùƒ x ùkü gqd x wš y w. w x 500 o C w gqd»œ ƒ w»œ j» w. œ w s³ w s d 10 ùkü.» w m/s, 500 o C w m/s s³ ƒ w s w w ùkû. œ w ù s w w e ùkû. œ 500 o C ww d ƒ j x»œ ƒ wš ƒ ƒw ùkü ( 7~9). ù d x ƒ œ ww w ( 10)., w ww ƒ d ( w ) x ƒw š e w gqd x»œ, p w q. 4. gq œ w gqd x, gq p wš w d, w pk gqd d w w. x x R ³ex P w»œ, gq p w, P ³ex R x 20 m/s s ³ w ùkü. ³ex x w w. ³ex» w d x j ùkù w, û»œ, w gqd p ùkû. R x 500 o C w gqd»œ w ƒw. w d w s³ w s ùkü. w s w d x w w d j x ùkü gqd p w Journal of Korean Powder Metallurgy Institute (J. Kor. Powd. Met. Inst.)

8 pk gqd p d e x w 355 ƒ.» w. š x [1] Y. T. Lee: Machine & Mat., 21 (2009) 74. (Korean) [2] J. Villafuerte: Metal Fishing, 108 (2010) 37. [3] W. Wong: Adv. Mater. Res., 89 (2010) 639. [4] ASM Handbook 10th ed., ASM Inter. (1992) 610. [5] G. Lutjering and J. C. Williams: Springer-Verlag Berlin Heidelberg, Germany (2003) 57. [6] F. H. Froes, V. S. Moxson and V. A. Duz: 2004 Inter. Conf. on PM, Chicago, USA (2004) 178. [7] F. H. Froes, S. J. Mashl, V. Moxson, J. C. Hebeison and V. A. Duz: JOM., 11 (2004) 46. [8] A. Parapin, V. Kosarev, S. Klinkov, A. Alkimov and A. Fomin: Cold spray technology, Elsevier (2001) 1. [9] T. H. V. Steenkiste: Key Eng. Mater., 197 (2001) 59. [10] R. C. McCone: 2003 International Thermal Spray Conference, ASM International, U.S.A. (2003) 63. [11] H. J. Kim, C. Lee and S. Y. Hwang: Mater. Sci. Eng. A, 391 (2005) 243. [12] H. Choi, S. Yoon, S. Uhm and C. Lee: Surf. Coat. Technology., 192 (2005) 374. [13] T. Schmidt, F. Gäertner and H. Kreye: J. Therm. Spray Technol., 15 (2006) 488. [14] H. J. Kim, J. H. Jang, D. H. Jung and C. Lee: J. Kor. Inst. Met. & Mater., 44 (2006) 697. (Korean) [15] T. Schmidt, F. Gäertner and H. Kreye: J. Therm. Spray Technol., 15 (2006) 488. [16] T. V. Steenkiste and J. R. Smith: J. Therm. Spray Technol., 12 (2004) 274. [17] J. S. Yu, H. J. Kim, I. H. Oh and K. A. Lee: J. Kor. Powd. Met. Inst., 19 (2012) 110. (Korean) [18] F. Raletz, M. Vardelle and D. Ezo o: Suf. and Coat. Tech., 201 (2006) (Korean) [19] H. Fukanuma, N. Ohno, B. Sun and R. Huang: Suf. and Coat. Tech., 201 (2006) Vol. 19, No. 5, 2012

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