본 논문에서는 일방향 텅스텐 섬유의 프리프레그 제조공정을 확보하고 가압소결법을 사용하여 텅스텐 연속섬유 강화 텅스텐 기지 복합재료(Wf/Wcomposites)를 제조하여 미세조직, 경도 및 굽힘강도에 대해 평가하였다. 특히, 텅스텐 섬유의 체적율의 변화에 따른 Wf/W 복합재료의 특성을 조사하였다. 또한 텅스텐 섬유의 인장시험을 통하여 강도를 평가하고 Weibull 확률분포와 미세조직 분석을 통하여 고찰하였다. 텅스텐 기지재의 성형을 위하여 평균 입경이 약 0.76 μm인 텅스텐 분말을 사용하였다. 일방향 텅스텐 섬유의 프리프레그는 텅스텐 섬유를 10 vol%, 15 vol%, 20 vol%의 체적율로 일정한 간격으로 배열하고 텅스텐 분말에 PVA(Polyvinyl alcohol)와 PEG(Polyethylene glycol)를 혼합한 액상 슬러리를 사용하여 제조하였다. 즉, 일방향으로 배열된 텅스텐 섬유에 액상슬러리를 함침시키고 건조하여 프리프레그를 제작하였다. Wf/W 복합재료는 사각형상의 흑연 금형에 프리프레그를 일방향으로 적층한 후 1500 ℃의 온도에 가압성형하여 제조하였다. Wf/W 복합재료의 제조에 사용한 텅스텐 섬유의 평균 인장강도는 약 2.65 GPa로서 Weibull 확률분포에 따르면 매우 균질한 성질을 보유하였다. Wf/W 복합재료는 섬유 체적율이 10 vol%인 경우에 Wf/W 복합재료에서 섬유 주위에 기공과 소결 결함들이 상대적으로 적게 관찰되지만, 텅스텐 섬유의 체적율 변화에 관계없이 약 80 %의 비슷한 상대밀도를 나타내었다. 그러나 텅스텐 섬유의 체적율이 증가함에 따라 소결과정에서 사용한 텅스텐 프리프레그 주위에 큰 기공들이 형성하였으며 텅스텐 섬유의 체적율이 20vol%인 경우에 소결 결함이 현저히 나타났다. 텅스텐 섬유의 체적율이 15vol%인 Wf/W 복합재료의 굽힘강도는 230 MPa로서 상대적으로 높은 굽힘강도를 나타내었다. 파단면 관찰 결과에 따르면, 텅스텐 단체재료는 균열에 의해 빠르게 파괴되는 취성적인 파괴형태를 나타내었다. 이에 비해 Wf/W 복합재료는 텅스텐 섬유의 존재에 의해 균열의 굴절을 동반하면서 섬유의 풀 아웃과 계면 박리가 국부적으로 발생하였다. 또한, 섬유 체적율이 10vol%의 경우 텅스텐 기지재와 텅스텐 섬유의 강한 접착에 의한 급속한 파단이 발생하였으며 섬유 체적율이 20 vol%의 경우에는 텅스텐 섬유의 과다한 소성변형에 의해 섬유 자체의 파괴가 발생하였다. 이로 인해 텅스텐 섬유의 체적율이 증가하더라도 Wf/W 복합재료의 굽힘강도는 오히려 감소한 것으로 생각된다. 텅스텐 섬유와 텅스텐 복합재료 기지재의 비커스경도는 각각 약 560 Hv와 871 Hv를 나타내었다. 그러나, 텅스텐 기지재의 경도는 섬유의 체적율에 따른 소결 결함에 의해 산포도가 크게 나타났다. 또한 과다한 섬유 체적율의 첨가는 텅스텐 기지재의 소성유동을 작아지게 함으로서 섬유 자체에 손상을 유발하여 오히려 기계적 특성을 저하시키는 요인으로 생각된다.
In this paper, the tungsten continuous fiber reinforced tungsten matrix composites (Wf/W) were fabricated through the secure ofprepreg manufacturing process of unidirectional tungsten fiber, using the pressure-assisted sintering method. The characteristics of Wf/W composites such as microstructure, hardness and bending strength were evaluated. In particular, the properties of Wf/W composites material were investigated according to the change in the volume ratio of tungsten fibers. The strength of tungsten fibers was also evaluated through a tensile test, based on the detailed analysis of Weibull probability distribution and microstructure. The tungsten powder having an average particle diameter of about 0.76 μm was used for the fabrication of the tungsten matrix material. The uni-directional tungsten fiber prepreg was prepared with a liquid slurry in which PVA (Polyvinyl alcohol), PEG (Polyethylene glycol) and tungsten powder were mixed, after arranging the continuous tungsten fibers at a regular interval. The volume fractions of tungsten fibers were 10 vol%, 15 vol% and 20 vol%, respectively. That is, the tungsten fibers of uni-directional orientation were impregnated with liquid slurry in the rectangular mold and dried to prepare a prepreg. Wf/W composites were fabricated at the temperature of 1500 °C, after laminating the fiber prepregs into the one direction inside a rectangular graphite mold. The tungsten fiber used for the preparation of Wf/W composites possessed the average tensile strength of about 2.65 GPa. It had very homogeneous properties, according to the Weibull probability distribution. Wf/W composites showed a similar relative density of about 80 % regardless of the change in the volume fraction of tungsten fibers, even if there were relatively few pores and sintering defects around the fiber when the fiber volume fraction was 10 vol%. However, as the volume fraction of tungsten fibers increased, large pores were formed around the tungsten fiber prepreg used in the sintering process, and sintering defects were significantly observed at the fiber volume fraction of 20 vol%. Wf/W composites represented the flexural strength of about 230 MPa at the fiber volume fraction of 15 vol%, indicating a relatively high strength level. It was found form the results of fracture surface observation that the monolithic tungsten materials exhibited a brittle fracture pattern, resulted from a rapid propagation of cracks. On the other hand, Wf/W composites locally represented the fiber pull-out and the interfacial delamination, accompanying the crack deflection due to the presence of tungsten fibers. When the fiber volume fraction was 10 vol%, the rapid fracture also occurred due to strong adhesion between tungsten matrix and tungsten fiber. When the fiber volume fraction was 20 vol%, the tungsten fiber itself was destroyed owing to the excessive plastic deformation. It could be thought that the flexural strength of Wf/W composites rather decreased even if the volume fraction of tungsten fibers increased. The Vicker’s hardness of tungsten fiber and tungsten matrix material was about 560 Hv and about 871 Hv, respectively. However, the tungsten matrix material had a large dispersion in the hardness, due to the pore dispersion and the sintering defects according to the volume fractions of tungsten fibers. The excessive addition of fibers can be also considered as a factor causing the damage of the fiber itself and rather lowering the mechanical properties, owing to the reduction of the plastic flow in the tungsten matrix material.
목차
1. 서 론1.1 연구 배경 ··································································································· 11.2 연구 목적 ··································································································· 32. 시험편 제조 및 실험방법2.1 Wf/W 복합재료의 제조 ·················································································· 42.2 단일 섬유의 인장시험 ··················································································· 122.3 소결밀도 측정 ··························································································· 142.4 미세조직 분석 ··························································································· 162.5 굽힘강도 평가 ··························································································· 182.6 비커스 경도 평가 ····················································································· 193. 결과 및 고찰3.1 텅스텐 섬유 인장강도와 경도 ····································································· 213.2 Wf/W 복합재료의 특성 ················································································ 264. 결 론 ················································································································· 45참 고 문 헌 ··········································································································· 46영 문 요 약(Abstract) ······················································································· 51