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나노 복합 분말로 소결된 Fe-TiB2의 마모 특성 평가

Assessment of Wear Characteristics of Fe-TiB₂ Sintered from Nanocomposite Mixtures

Journal of the Korean Society for Precision Engineering 2018;35(10):1001-1006.
Published online: October 1, 2018

1 울산대학교 기계공학부

2 울산대학교 첨단소재공학부

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#E-mail: khchung@ulsan.ac.kr, TEL: +82-52-259-2744
• Received: November 26, 2017   • Revised: June 27, 2018   • Accepted: July 4, 2018

Copyright © The Korean Society for Precision Engineering

This is an Open-Access article distributed under the terms of the Creative Commons Attribution Non-Commercial License (http://creativecommons.org/licenses/by-nc/3.0) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

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  • The objective of this study was to investigate wear characteristics of Fe-TiB2 composites prepared by pressureless sintering (PLS) and spark plasma sintering (SPS) using nanocomposite mixtures. Prior to wear test, micro-structures and mechanical properties of specimens were examined. Wear characteristics of these specimens slid against SiC were assessed using ball-on-disk tribo-tester. Results showed that PLS specimen had significantly large TiB2 particles in the Fe matrix than SPS specimen. The relatively large TiB2 particles in PLS specimen might be due to grain growth and coarsening during sintering process. Hardness of SPS specimen was substantially larger than that of PLS specimen. Furthermore, SPS specimen exhibited significantly larger wear resistance than PLS specimen. These differences in hardness and wear resistance between specimens might be associated with differences in their micro-structures. Results of this study provide better understanding of wear characteristics of Fe-TiB2 composites.
TiB2 (Titanium Diboride)는 상대적으로 높은 열 전도와 전기 전도도를 가지고 있을 뿐만 아니라, 우수한 기계적 물성을 가지고 있어,1 Cu, Al, Fe, Ti 등과 같은 다양한 금속 소재를 위한 강화재(Reinforcement)로 사용될 수 있는 것으로 제시되고 있다.2-4 최근에는, TiB2가 액상의 Fe에서 화학적으로 안정된 상태를 유지할 수 있을 뿐만 아니라, 우수한 소결성을 가지는 것으로 보고됨에 따라, Fe-TiB2 복합재의 합성, 기계적 물성, 마모 특성 평가 등에 관한 연구가 활발히 진행되고 있다,5,6 특히, 기지재(Matrix)로 사용되는 Fe의 물성은 가공방법 및 첨가물에 따라 다양하게 변화시킬 수 있으므로, Fe-TiB2 복합재는 절삭 공구, 다이 등과 같이, 높은 내열성 및 마모 저항성이 요구되는 다양한 응용분야에 활용될 수 있는 것으로 기대되고 있다.
Fe-TiB2 복합재의 합성 및 제작을 위해서 많은 방법이 제시되고 있으나, Fe 기지재 내 포함된 TiB2 입자 크기 및 분포의 균일성을 위해서 Self-Propagating High Temperature Synthesis,2,5 Laser Cladding,7 그리고, Plasma Transferred Arc Technique8,9과 같은 In-Situ 합성 방법이 선호되고 있다. 복합재 소결 방법 및 조건은 소재의 구조에 직접적 영향을 미치므로, 기계적 물성 및 표면 특성을 결정할 뿐만 아니라, 나아가 마찰 및 마모 특성에 크게 영향을 미친다. 그러므로, 우수한 특성을 가지는 Fe-TiB2 복합재의 개발을 위해서는, 제작 조건 및 방법에 따른 복합재의 구조적 차이를 먼저 이해하고, 기계적 물성 및 표면 특성, 그리고, 마찰 및 마모 특성을 체계적으로 평가하는 것이 요구된다.
본 연구에서는, Fe-TiB2 나노 복합 분말을 이용하여 소결된 Fe-TiB2 복합재의 내마모 특성을 실험적으로 평가하고 이해하고자 하였다. 실험에 사용된 Fe-TiB2 복합재 시편은 경제적 우수성을 가지는 상압 소결(Pressure Less Sintering, PLS)과 미세한 입자를 빠르고 균일하게 소결할 수 있는 방전 플라즈마 소결(Spark Plasma Sintering, SPS)10 방법으로 준비되었다. 각 시편의 표면 특성과 기계적 성질을 이해하기 위해서, 공초점 현미경(Confocal Microscope), 주사전자현미경(Scanning Electron Microscope, SEM), 마이크로 비커스(Micro-Vickers) 경도계 등을 활용하였으며, Ball-on-Disk Tribo-Tester를 이용한 마모 실험을 수행하였다. 마모 실험 후 시편의 표면을 관찰하고, 마모 입자 분석 등을 수행하여, Fe-TiB2 복합재의 내마모 특성을 이해하고자 하였다.
2.1 실험 시편
FeB와 TiH2 입자들을 이용하여 제작된 Fe-TiB2 나노 복합 분말11을 소결하여 Fe-TiB2 복합재 시편을 제작하였다. 앞서 언급한 바와 같이 Fe-TiB2 복합재 시편은, PLS및 SPS 방법으로 소결되었으며, 디스크 형태로 제작되었다. 일관성 있는 분석을 위하여, 소결된 시편들은 같은 조건(하중 및 시간)에서 연마되었다. Fig. 1은 PLS 및 SPS 방법으로 소결된 시편들의 연마 전 사진, 연마 후의 공초점 현미경 이미지 및 SEM 이미지를 나타낸다. Fig. 1(a)에 제시된 SEM 이미지로부터 알 수 있듯이, PLS 시편에는 Fe 기지 내에 수 μm 크기의 TiB2 입자들이 비교적 고르게 분포되어 있는 것을 알 수 있다. 시편 제작에 사용된 Fe-TiB2 복합 분말에는 나노미터 단위의 TiB2 입자가 형성되어 있음11을 고려할 때, 상대적으로 높은 온도에서 소결되는 PLS 과정에서 TiB2 입자의 성장(Grain Growth), 또는 조대화(Coarsening)가 발생한 것으로 예상된다. 그러나, Fig. 1(b)에 제시된 SEM 이미지로부터, 상대적으로 낮은 온도에서 소결된 SPS시편의 경우에는, 매우 작은 TiB2입자가 형성되어 있음을 알 수 있다. 연마후 두 시편의 표면은 매우 평평하였으나, Fig. 1에 제시된 공초점 현미경 이미지와 같이, PLS 시편의 표면 거칠기가 SPS 시편보다 큰 것으로 나타났다. 서로 다른 5곳의 위치에서 얻은 공초점 현미경 데이터로부터, PLS 및 SPS시편의 표면 거칠기는 각각 1.2 ± 0.1 μm, 0.37 ± 0.02 μm인 것으로 계산되었다. 두 시편의 연마가 같은 조건에서 수행되었음에도 불구하고, 표면 거칠기 차이가 비교적 크게 발생한 것은 두 시편의 연마성(Polishability)이 서로 다른 것을 의미한다. 또한, 마이크로 비커스 경도계를 이용하여 측정한 PLS와 SPS 시편의 경도는 각각 800 HV와 1,500 HV로 나타났다. 이와 같은 연마성 및 기계적 물성의 차이는, 소결 방법에 따라 다르게 형성되는 소재의 미시적 구조 차이(예: TiB2 입자의 크기)에 기인하는 것으로 생각되며, 이러한 결과로부터 두 시편의 마모 특성도 다르게 전개될 것임을 예상할 수 있다.
Fig. 1

Photographs, SEM images, and 3D topographic images of Fe-TiB2 specimens prepared by (a) PLS and (b) SPS

KSPE_2018_v35n10_1001_f001.jpg
2.2 실험 방법
Fe-TiB2 복합재의 마모 특성 평가를 위해서는 Fig. 2에 제시된 바와 같이, Pin-on-Disk Tribo-Tester를 이용하였다. Fe-TiB2 복합재의 경도가 높은 점을 고려하여, 상대재료로써 4 mm의 직경을 가지는 SiC 구를 선택하였다. 마모 실험은 건식 윤활(Dry Lubrication) 상태에서, 5 N의 수직하중 및 60 rpm의 회전 속도에서 수행되었다. 60 rpm의 회전 속도에서 Ball과 시편의 선형 상대 운동 속도는 15 mm/s이었으며, 마모 실험은 17,100 사이클 동안 진행되었다. 이와 같은 실험 조건은 Fe-TiB2 복합재 시편의 마모를 관찰할 수 있도록 예비실험을 통하여 선정되었다. 실험 후 마모가 발생한 SiC 구와 Fe-TiB2 시편의 표면은 공초점 현미경과 SEM 등을 이용하여 관찰하였다. 특히, 마모 특성을 정량적으로 평가하기 위하여, 공초점 현미경 데이터로부터 마모 트랙의 평균 단면 프로파일12을 얻어 비교하였으며, 마모 입자 특성을 파악하기 위해 Energy-Dispersive X-Ray Spectroscopy (EDX)를 이용한 화학적 성분 분석을 수행하였다.
Fig. 2

Photograph of pin-on-disk tribo-tester

KSPE_2018_v35n10_1001_f002.jpg
Fig. 3은 실험후 Fe-TiB2 복합재 표면에 형성된 마모 흔적의 공초점 현미경 이미지, 단면 프로파일, 그리고 3차원 표면 형상 이미지를 나타낸다. Fig. 3에 제시된 데이터로부터, PLS 및 SPS 시편들에 약 400 - 500 μm 정도의 폭을 가지는 마모 흔적이 미끄럼 운동 방향을 따라 형성되어 있음을 명확하게 관찰할 수 있다. 그러나, 단면 프로파일과 3차원 표면 형상 이미지로부터, PLS 및 SPS 시편에 형성된 마모 흔적의 높이가 주변에 비하여 2 - 3 μm 정도 높은 것을 알 수 있다. 이와 같은 결과로부터, 상대운동에 의하여 발생한 마모 입자가 쌓여 마모 흔적을 형성하고 있는 것을 유추할 수 있었다.
Fig. 3

Confocal microscope images, cross-sectional profiles, and 3D topographic images of (a) PLS and (b) SPS specimens after the experiments

KSPE_2018_v35n10_1001_f003.jpg
마모 흔적의 발생 경로를 확인하기 위하여, 마모 흔적을 SEM으로 관찰하고, EDX를 이용한 화학 성분 분석을 수행하여 Fig. 4에 제시하였다. Fig. 4에 제시된 SEM 이미지로부터, 마모 입자들에 의하여 마모 흔적이 형성되어 있음을 확인할 수 있다. 또한, 마모 입자로부터 얻은 EDX 분석 결과에서, 실험에 사용된 복합재 시편으로부터 얻어진 Fe와 Ti 가 검출되었음을 확인할 수 있다. 또한, 다른 주된 성분으로 Si가 관찰되었는데, 이는 실험에 사용된 SiC 구로부터 발생한 것으로 생각된다. 또 다른 주된 입자로 O가 검출되었으며, 이는 Fe가 실험 중 산화된 것으로 여겨진다. Fig. 4에 제시된 결과로부터, Fe-TiB2 복합재 시편의 표면에 형성된 마멸 흔적에는 마멸 입자가 쌓여 있고, 마멸 입자에는 SiC 구로부터 발생한 마모 입자가 포함되어 있는 것을 알 수 있었다. 이러한 결과를 보다 명확하게 확인하기 위하여, 실험 후 SiC 구의 마모 정도를 공초점 현미경으로 관찰하였으며, 공초점 현미경 데이터로부터 얻은 구의 단면 프로파일을 Fig. 5에 제시하였다. Fig. 5에 제시된 바와 같이, SiC 구의 경도가 상대적으로 높음에도 불구하고, 실험에 사용된 Fe-TiB2 복합재 시편과의 상대 운동에 의하여 마모가 심하게 발생하였으며, 이에 따라 구의 끝이 평평해졌음을 알 수 있다. 특히, SiC 구의 양 끝단에도 마모 입자가 쌓여 있는 것도 알 수 있다. 또한, SiC 구의 마모는 PLS 시편과의 상대 운동에 의하여 보다 많이 발생한 것을 알 수 있었다. Figs. 45에 제시한 결과들은 SiC 구에서 발생한 마모 입자들이Fe-TiB2 복합재 시편의 표면으로 전이되어 쌓여 있음을 명확하게 나타낸다.
Fig. 4

SEM images and EDX spectra of wear debris formed on (a) PLS and (b) SPS specimens

KSPE_2018_v35n10_1001_f004.jpg
Fig. 5

Cross-sectional profiles of balls after experiments s

KSPE_2018_v35n10_1001_f005.jpg
Fe-TiB2 복합재 시편의 마모 정도를 평가하게 위하여, 시편들을 초음파 세척(Sonication)하여 마모 입자를 최대한 제거하고자 하였다. 초음파 세척후, PLS 시편의 마모 발생은 비교적 명확하게 관찰할 수 있었으며, 보다 정확한 마모 측정을 위하여 고배율로 얻은 공초점 현미경 데이터를 Fig. 6(a)와 에 제시하였다. Fig. 6(a)에 제시한 단면 프로파일 및 3차원 표면 형상을 분석 결과부터, PLS 시편의 표면에는 최대 0.7 μm 깊이의 마모 트랙이 형성되어 있음을 알 수 있었으며, 마모 트랙의 단면적은 약 50 μm2임을 알 수 있었다. 이러한 데이터로부터, SiC 구와의 상대운동에 의하여 발생한 PLS 시편의 마모율은 약 3 × 10-9mm3/(N·Cycle)로 계산되었다. 초음파 세척으로 마모 입자가 완벽하게 제거되지 않았을 수 있으므로, 해당 마모율은 주어진 실험 조건에서의 최소값으로 여겨지는 것이 타당하다.
Fig. 6

Confocal microscope images, cross-sectional profiles, and 3D topographic images of (a) PLS and (b) SPS specimens after sonication

KSPE_2018_v35n10_1001_f006.jpg
Fig. 6(b)는 세척 후 SPS 시편의 표면을 나타내는 공초점 현미경 이미지, 단면 프로파일, 그리고 3차원 표면 형상을 나타낸다. Fig. 6(b)에 제시된 바와 같이, SPS 시편의 경우에는 세척후에도 상대적으로 많은 양의 마모 입자가 남아 있었다. 그러나, 3차원 표면 형상에서 명확하게 알 수 있듯이, 마모 입자들로 형성된 마모 흔적 사이에서도, 정량적으로 분석 가능한 SPS 시편의 마모는 관찰되지 않았다. 이러한 결과로부터, SPS 시편의 마모 저항성은 PLS 시편에 비하여 훨씬 큼을 알 수 있었다. 이러한 마모 특성의 차이는 두 시편의 구조적 차이에 기인한, 기계적 성질의 차이에 의한 것으로 생각된다.
복합재의 미시 조직, 기계적 물성, 내마모성 등은 제조 또는 소결 방법과 조건에 따라 다르므로, 본 연구를 통하여 얻어진 결과를 모든 Fe-TiB2 복합재로 일반화 시킬 수는 없다. 또한, Fe-TiB2 복합재의 마모 특성을 보다 효과적으로 분석하기 위해서는 다이아몬드와 같이 더욱 경한 소재를 상대재료로 활용하는 것이 요구될 것이다. 그러나, 본 연구를 통하여, 복합재의 미시적 구조에 따라 기계적 물성 및 마모 특성이 영향을 받음을 확인할 수 있었을 뿐만 아니라, 나노 복합재를 이용하여 소결된 Fe-TiB2 복합재의 마모율은 10-9mm3/(N·Cycle) 정도로써 매우 높은 마모 저항성을 가지고 있음을 알 수 있다. 이러한 결과는 Fe-TiB2 복합재의 트라이볼로지적 응용분야를 더욱 확대하는데 기여할 수 있을 것으로 기대된다.
본 연구에서는 Fe-TiB2 나노 복합재 분말을 이용하여, 소결된 Fe-TiB2 시편의 표면 특성, 기계적 성질 및 마모 특성을 평가하였다. 소결 방법으로는 경제적으로 우수한 방법으로 제시되고 있는 PLS와 미세한 입자구조를 빠르고 균일하게 소결을 할 수 있다는 장점을 가지고 있는 SPS 방법을 이용하였다. 예상한 바와 같이, 소결 방법에 따라 Fe-TiB2 시편의 미시적 구조가 다르게 나타났으며, 특히, PLS 공정의 경우, SPS 공정에 비하여 상대적으로 큰 TiB2 입자가 형성되었음을 알 수 있었다. 마이크로 비커스 경도 측정과 마모 시험 결과, 나노 복합재를 이용하여 소결된 Fe-TiB2 복합재의 경도와 내마모성은 매우 우수한 것으로 나타났다. 그러나, 공정에 따른 시편의 미시적 구조의 차이는 기계적 물성과 내마모성의 차이를 유발하는 것으로 나타났다. 즉, 상대적으로 큰 TiB2 입자가 형성되어 있는 PLS 시편의 경도는 800 HV 정도로 SPS 시편의 경도(1500 HV)에 비하여 작은 것으로 나타났다. 또한, Ball-on-Disk Tribo-Tester를 이용한 마모 실험 결과, SiC와의 상대 운동에 의하여 발생하는 PLS 시편의 마모율은 10-9mm3/(N·Cycle)로 계산된 반면, SPS 시편의 마모율은 측정하기 힘들 정도로 작은 것으로 나타났다. 이와 같은 연구는 Fe-TiB2 복합재를 효과적으로 제작하고 응용분야를 더욱 넓히는데 기여할 수 있을 것으로 기대된다.
이 논문은 2017년도 정부(미래창조과학부)의 재원으로 한국연구재단의 지원을 받아 수행된 기초연구사업임(과제번호: NRF-2017R1A2B4009651).
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Hak-Rae Cho
Master’s degree received from the School of Mechanical Engineering, University of Ulsan. Currently, he has graduated. His research interest is precision engineering, tribology and surface engineering.
Ji-Soon Kim
KSPE_2018_v35n10_1001_bf002.jpg
Professor in the School of Material Science and Engineering, University of Ulsan. His research interest is Nanocomposite Materials and Powder Metallurgy.
Koo-Hyun Chung
KSPE_2018_v35n10_1001_bf003.jpg
Professor in the School of Mechanical Engineering, University of Ulsan. His research interest is tribology and surface engineering.

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Assessment of Wear Characteristics of Fe-TiB₂ Sintered from Nanocomposite Mixtures
J. Korean Soc. Precis. Eng.. 2018;35(10):1001-1006.   Published online October 1, 2018
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Assessment of Wear Characteristics of Fe-TiB₂ Sintered from Nanocomposite Mixtures
J. Korean Soc. Precis. Eng.. 2018;35(10):1001-1006.   Published online October 1, 2018
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Assessment of Wear Characteristics of Fe-TiB₂ Sintered from Nanocomposite Mixtures
Image Image Image Image Image Image
Fig. 1 Photographs, SEM images, and 3D topographic images of Fe-TiB2 specimens prepared by (a) PLS and (b) SPS
Fig. 2 Photograph of pin-on-disk tribo-tester
Fig. 3 Confocal microscope images, cross-sectional profiles, and 3D topographic images of (a) PLS and (b) SPS specimens after the experiments
Fig. 4 SEM images and EDX spectra of wear debris formed on (a) PLS and (b) SPS specimens
Fig. 5 Cross-sectional profiles of balls after experiments s
Fig. 6 Confocal microscope images, cross-sectional profiles, and 3D topographic images of (a) PLS and (b) SPS specimens after sonication
Assessment of Wear Characteristics of Fe-TiB₂ Sintered from Nanocomposite Mixtures