A Ni-Ti-B alloy powder prepared by mechanical alloying (MA) of individual Ni, Ti, and B components is examined with the aim of elucidating the phase transitions and crystallization during heat treatment. Ti and B atoms penetrating into the Ni lattice result in a Ni (Ti, B) solid solution and an amorphous phase. Differential thermal analysis (DTA) reveals peaks related to the decomposition of the metastable Ni (Ti, B) solid solution and the separation of equilibrium Ni3Ti, TiB2, and τ-Ni20Ti3B6 phases. The exothermal effects in the DTA curves move to lower temperatures with increasing milling time. The formation of a TiB2 phase by annealing indicates that the mechanochemical reaction of the Ni-Ti-B alloy does not comply with the alloy composition in the ternary phase diagram, and Ti-B bonds are found to be more preferable than Ni-B bonds.
Zn(BH4)2 was prepared by milling ZnCl2 and NaBH4 in a planetary ball mill in an Ar atmosphere, and XRD analysis, SEM observation, FT-IR analysis, DTA, and TGA were performed for synthesized Z (BH4)2 samples. 90 wt% MgH2+ 1.67 wt% Zn(BH4)2(+NaCl)+5 wt% Ni+1.67 wt% Ti+1.67 wt% Fe (named 90MgH2+1.67Zn(BH4) (+NaCl)+5Ni+1.67Ti+1.67Fe) samples were also prepared by milling in a planetary ball mill in an H2 atmosphere. The gas absorption and release properties of the Zn(BH4)2(+NaCl) and 90MgH2+1.67Zn(BH4)2(+NaCl)+5Ni+1.67Ti+1.67Fe samples were investigated. An FT-IR analysis showed that Zn(BH4)2 formed in the Zn(BH4)2(+NaCl) samples prepared by milling ZnCl2 and NaBH4. At the first cycle at 320 oC, 90MgH2+1.67Zn(BH4)2(+NaCl)+5Ni+1.67Ti+1.67Fe absorbed 2.95 wt% H for 2.5 min and 4.93 wt% H for 60 min under 12 bar H2, and released 1.46 wt% H for 10 min and 4.57 wt% H for 60 min under 1.0 bar H2.
Ti-Ni alloys are widely used in numerous biomedical applications (e.g., orthodontics, cardiovascular science, orthopaedics) due to their distinctive thermomechanical and mechanical properties, such as the shape memory effect, superelasticity and low elastic modulus. In order to increase the biocompatibility of Ti-Ni alloys, many surface modification techniques, such as the sol-gel technique, plasma immersion ion implantation (PIII), laser surface melting, plasma spraying, and chemical vapor deposition, have been employed. In this study, a Ti-49.5Ni (at%) alloy was electrochemically etched in 1M H2SO4+ X (1.5, 2.0, 2.5) wt% HF electrolytes to modify the surface morphology. The morphology, element distribution, crystal structure, roughness and energy of the surface were investigated by scanning electron microscopy (SEM), energy-dispersive Xray spectrometry (EDS), X-ray diffractometry (XRD), atomic force microscopy (AFM) and contact angle analysis. Micro-sized pores were formed on the Ti-49.5Ni (at%) alloy surface by electrochemical etching with 1M H2SO4+ X (1.5, 2.0, 2.5) wt% HF. The volume fractions of the pores were increased by increasing the concentration of the HF electrolytes. Depending on the HF concentration, different pore sizes, heights, surface roughness levels, and surface energy levels were obtained. To investigate the osteoblast adhesion of the electrochemically etched Ti-49.5Ni (at%) alloy, a MTT test was performed. The degree of osteoblast adhesion was increased at a high concentration of HF-treated surface structures.
니오븀 금속을 기반으로 하는 Nb56Ti23Ni21 합금 분리막의 수소 투과 특성 및 화학적 안정성에 관한 연구를 수행하였다. 이를 위하여 직경 10 mm, 두께 0.5 mm의 Nb56Ti23Ni21 합금 분리막을 제작하였으며, 2가지 조성(H2 100%, H2 60% + CO2 40%)의 공급가스를 450℃의 온도에서 투과시킬 때 압력에 따른 수소 투과 특성에 관한 실험을 진행하였다. 본 실험에서의 최대 수소 투과량은 순수한 수소를 투과시킬 경우 절대압력 3 bar에서 5.58mL/min/cm2로 나타났다. 또한 공급가스 조성에 따른 각각의 경우 모두 Sievert's law에 잘 부합하였으며, 이산화탄소와의 혼합가스 사용시, 투과량은 수소 분압 감소에 비례하여 감소하였다. 투과 실험 후 XRD 분석을 통하여 Nb56Ti23Ni21 합금 분리막의 이산화탄소에 대한 화학적 안정성에 대한 실험을 수행하였다.
팔라듐이 코팅된 V53Ti26Ni21 합금 분리막을 통해 수소 투과시 혼합가스의 영향에 대해 알아보았다. 순수 수소, 수소, 이산화탄소 및 일산화탄소의 혼합가스를 공급가스로 주입할 때, 450℃, 1-3 bar의 압력에서 팔라듐이 코팅된 V53Ti26Ni21 합금 분리막의 수소 투과 실험을 수행하였다. 수소만을 공급한 투과 실험에서 팔라듐 코팅된 V53Ti26Ni21 합금 분리막(두께: 0.5 mm)의 수소 투과량은 3 bar, 450℃ 조건에서 5.36mL/min/㎠였다. 또한 수소/이산화탄소, 수소/일산화탄소 및 수소/이산화탄소/일산화탄소를 공급한 투과실험에서 V53Ti26Ni21 합금 분리막의 수소 투과량은 각각 4.46, 5.20, 3.91mL/min/㎠였다. 따라서, 수소/이산화탄소, 수소/일산화탄소 및 수소/이산화탄소/일산화탄소 혼합가스를 각각 공급할 때 투과량은 온도와 압력에 상관없이 수소 분압 감소만큼 감소하였고 모든 경우 Sievert 법칙을 잘 만족시켰다. 투과 후 분리막의 XRD 결과로부터 V53Ti26Ni21 합금 분리막은 여러 혼합가스에 대해 안정성과 내구성이 우수하다는 것을 알 수 있었다.
Methods of producing hydrogen include steam reforming, electrochemical decomposition of water, and the SI process. Among these methods, the Sulfur iodine process is one of the most promising processes for hydrogen production. The thermochemical sulfur-iodine (SI) process uses heat from a high-temperature-gas nuclear reactor to produce H2 gas; this process is known for its production of clean energy as it does not emit CO2 from water. But the SI-process takes place in an extremely corrosive environment for the materials. To endure SI environments, the materials for the SI environment will have to have strong corrosion resistance. This work studies the corrosion resistances of the Fe-Si, Ni-Ti and Ni Alloys, which are tested in SI-process environments. Among the SI-process environments, the conditions of boiling sulfuric acid and decomposed sulfuric acid are selected in this study. Before testing in boiling sulfuric acid environments, the specimens of Fe-4.5Si, Fe-6Si, Ni-4.5Si, Ni-Ti-Si-Nb and Ni-Ti-Si-Nb-B are previously given heat treatment at 1000˚C for 48 hrs. The reason for this heat treatment is that those specimens have a passive film on the surface. The specimens are immersed for 3~14 days in 98wt% boiling sulfuric acid. Corrosion rates are measured by using the weight change after immersion. The corrosion rates of the Fe-6Si and Ni-Ti-Si-Nb-B are found to decrease as the time passes. The corrosion rates of Fe-6si and Ni-Ti-Si-Nb-B are measured at 0.056 mm/yr and 0.16 mm/yr, respectively. Hastelloy-X, Alloy 617, Alloy 800H and Haynes 230 are tested in the decomposed sulfuric acid for one day. Alloy 800H was found to show the best corrosion resistance among the materials. The corrosion rate of Alloy 800H is measured at -0.35 mm/yr. In these results, the corrosion resistance of materials depends on the stability of the oxide film formed on the surface. After testing in boiling sulfuric acid and in decomposed sulfuric acid environments, the surfaces and compositions of specimens are analyzed by SEM and EDX.
The amorphization process and the thermal properties of amorphous TiCuNiAl powder during milling by mechanical alloying were examined by X-ray diffractometry (XRD), differential scanning calorimetry (DSC), and transmission electron microscopy (TEM). The chemical composition of the samples was examined by an energy dispersive X-ray spectrometry (EDX) facility attached to the scanning electron microscope (SEM). The as-milled powders showed a broad peak (2 = 42.4) with crystalline size of about 5.0 nm in the XRD patterns. The entire milling process could be divided into three different stages: agglomeration (0 < t 3 h), disintegration (3 h < t 20 h), and homogenization (20 h < t 40 h) (t: milling time). In the DSC experiment, the peak temperature T and crystallization temperature T were 466.9 and 444.3, respectively, and the values of T, and T increased with a heating rate (HR). The activation energies of crystallization for the as-milled powder was 291.5 kJ/mol for T.
The Ti-Ni alloy nanopowders were synthesized by a levitational gas condensation (LGC) by using a micron powder feeding system and their particulate properties were investigated by x-ray diffraction (XRD), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) method. The starting Ti and Ni micron powders were incorporated into the micron powder feeding system. An ingot type of the Ti-Ni ahoy was used as a seed material for the levitation and evaporation reactions. The collected powders were finally passivated by oxidation. The x-ray diffraction experiments have shown that the synthesized powders were completely alloyed with Ti and Ni and comprised of two different cubic and monoclinic crystalline phases. The TEM results showed that the produced powders were very fine and uniform with a spherical particle size of 18 to 32nm. The typical thickness of a passivated oxide layer on the particle surface was about 2 to 3 nm. The specific surface area of the Ti-Ni alloy nanopowders was based on BET method.
급냉응고방식으로 제조한 비정질 Z r62-xN i10C u20A l8 Tix (x=3, 6, 9at%) 합금을 사용하여 열적, 기계적 성질을 조사하였다. 시효온도에 따른 결정화 거동은 Ti 3at%에서는 비정질→비정질+Z r2A l3+Zr+(Ni,Ti)→Z r2Cu+Al+(Ni,Ti)의 결정화 거동을 나타내었으며, Ti 6at%에서는 비정질→비정질+Al→A l2Ti+NiZr+CuTi, Ti 9at%에서는 비정질→비정질+Zr+Al→Zr+A l2Zr+Al Ti3+CuTi의 결정화 거동을 보였다. 시효온도가 증가할수록 비정질 모상에 석출상의 체적율( Vf )이 증가하고 그에 따라 비커스 경도 ( Hv )간이 증가하였다. 파괴인장강도(σf )는 Vf 의 증가에 따라 증가하다가 Z r59A l10N i20C u8 Ti3은 Vf =38%에서 1219MPa의 최대값을 보이고, Z r56A l10N i20C u8 Ti6은 Vf =2%에서 1203MPa의 최대값을 보이고, Z r53A l10N i20C u8 Ti9 Vf =5%에서 1350MPa의 최대값을 나타낸 후 그 이상의 Vf 에서는 급격히 감소하였다. σf 가 급격히 감소하는 Vf 와 연성 파면에서 취성파면으로 천이되는 Vf 가 일치하였다.f/가 일치하였다.
Ti-50Ni(at%) and Ti-40Ni-10Cu(at%) alloy powders have been fabricated by ball milling method, and their microstructure and phase transformation behavior were investigated by means of scanning electron microscopy/energy dispersive spectrometry, differential scanning calorimetry (DSC), X-ray diffractions and transmission electron microscopy. In order to investigate the effect of ball milling conditions on transformation behavior, ball milling speed and time were varied. Ti-50Ni alloy powders fabricated with the milling speed more than 250 rpm were amorphous, while those done with the milling speed of 100rpm were crystalline. In contrast to Ti-50Ni alloy powders, Ti-40Ni-10Cu alloy powders were crystalline, irrespective of ball milling conditions. DSC peaks corresponding to martensitic transformation were almost discernable in alloy powders fabricated with the milling speed more than 250 rpm, while those were seen clearly in alloy powders fabricated with the milling speed of 100 rpm. This was attributed to the fact that a strain energy introduced during ball milling suppressed martensitic transformation.
Ti-45.2at.%Ni-5at.%Cu and Ti-40.2at.%Ni-10atat.%Cu alloy powders were fabricated by gas atomization process. The microstructures, Shape, hardness and phase transformation behaviors of the powders were investigated by means of optical microscopy, scanning electron microscopy, micro-hardness measurement, x-ray diffraction analyses and differential scanning calorimetry. The hardness of the Ti-Ni-XCu alloy powders decreased as Cu-content increased. The x-ray diffraction analyses were carried out for powders without heat treatment, and those that treated at 85 for an hour in a vaccum state( torr) and then quenched into ice water. The intensity of B phase increased with heat treating. The monoclinic B martensite was formed in the Ti-Ni-XCu alloy powders during cooling.