Mechanical properties of nanocrystalline and epitaxial TiN films on (100) silicon

2001 ◽  
Vol 16 (9) ◽  
pp. 2733-2738 ◽  
Author(s):  
H. Wang ◽  
A. Sharma ◽  
A. Kvit ◽  
Q. Wei ◽  
X. Zhang ◽  
...  

We investigated mechanical properties of TiN as a function of microstructure varying from nanocrystalline to single crystal TiN films deposited on (100) silicon substrates. By varying the substrate temperature from 25 to 700 °C during pulsed laser deposition, the microstructure of TiN films changed from nanocrystalline (having a uniform grain size of 8 nm) to a single crystal epitaxial film on the silicon (100) substrate. The microstructure and epitaxial nature of these films were investigated using x-ray diffraction and high-resolution transmission electron microscopy. Hardness measurements were made using nanoindentation techniques. The nanocrystalline TiN contained numerous triple junctions without any presence of amorphous regions. The width of the grain boundary remained constant at less than 1 nm as a function of boundary angle. Similarly the grain boundary structure did not change with grain size. The hardness of TiN films decreased with decreasing grain size. This behavior was modeled recently involving grain boundary sliding, which is particularly relevant in the case of hard materials such as TiN.

2001 ◽  
Vol 697 ◽  
Author(s):  
H. Wang ◽  
A. Kvit ◽  
X. Zhang ◽  
C. C. Koch

AbstractHigh-temperature materials such as TiN have been successfully applied as wear corrosion protection, decorative coatings, electrical contacts and diffusion barriers in electronic devices. However the poor toughness and ductility have limited some of these applications. To alleviate some of these problems, reduction of grain size can enhance grain boundary sliding and grain boundary diffusion related creep phenomena. We have investigated mechanical and electrical properties of TiN as a function of microstructure varying from nanocrystalline to single crystal TiN films deposited on (100) silicon substrates. By varying the substrate temperature from 25oC to 700oC during pulsed laser deposition, the microstructure of TiN films changed from nanocrystalline (having uniform grain size of 8 nm) to a single crystal epitaxial film on the silicon (100) substrate. The microstructure and epitaxial nature of these films were investigated using X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). Hardness measurements were made using nanoindentation techniques. Resistivity measurements were performed by van der Pauw method. The nanocrystalline TiN contained numerous triple junctions without any presence of amorphous regions. The width of the grain boundary remained constant 1 nm as a function of boundary angle. Similarly the grain boundary structure did not change with grain size. The hardness of TiN films decreased with decreasing grain size in nanoscale. This behavior has been modeled recently involving grain boundary sliding which is particularly relevant in the case of hard materials such as TiN. The dependence of resistivity of TiN as a function of the substrate temperature is discussed and correlated with hardness results.


2011 ◽  
Vol 683 ◽  
pp. 103-112 ◽  
Author(s):  
B. Yang

The evolution of the microstructure and mechanical properties of electrodeposited nanocrystalline Ni with different annealing procedures was studied systematically. For the annealed specimens hardness decreases with increasing average grain size but the dependence changes at different grain size ranges. The specimens annealed at a low temperature show higher hardness compared to the as-deposited nanocrystalline Ni, despite an increased measured average grain size. In association with this hardening an increase in elastic modulus and a decrease in microstrain was observed after annealing. With increasing annealing temperature both the tensile strength and the fracture strain were observed to decrease, this is companied with a transition from ductile to brittle in the fracture surfaces. These results indicated that the mechanical behaviour of nanocrystalline Ni depends not only on the average grain size but also on the grain boundary structure. A change in the grain boundary state arising from annealing may be responsible for the observed increase in hardness and elastic modulus as well as the deterioration of tensile properties.


2004 ◽  
Vol 449-452 ◽  
pp. 265-268 ◽  
Author(s):  
Tetsuhiko Onda ◽  
H. Yamauchi ◽  
Motozo Hayakawa

The effect of CoO addition into Y-TZP (Yttria doped Tetragonal Zirconia Polycrystals) was studied on the evolution of its sintering ability, grain size, grain boundary structure and mechanical properties. The doping of a small amount of CoO effectively reduced the sintering temperature. A small amount of CoO up to ~ 0.3 mol% was effective for the suppression of grain growth, but the addition of 1.0 mole % resulted in an enhanced grain growth. The hardness and toughness of the CoO doped TZP were about the same as those of undoped TZP. Furthermore, despite the grain refinement, CoO doped TZP did not exhibit improved mechanical properties. This may be suggesting that CoO dopant had weakened the grain boundary strength.


2004 ◽  
Vol 818 ◽  
Author(s):  
R. O. Ritchie ◽  
X.-F. Zhang ◽  
L. C. De Jonghe

AbstractThrough control of the grain-boundary structure, principally in the nature of the nanoscale intergranular films, a silicon carbide with a fracture toughness as high as 9.1 MPa.m1/2 has been developed by hot pressing β-SiC powder with aluminum, boron, and carbon additions (ABC-SiC). Central in this material development has been systematic transmission electron microscopy (TEM) and mechanical characterizations. In particular, atomic-resolution electron microscopy and nanoprobe composition quantification were combined in analyzing grain boundary structure and nanoscale structural features. Elongated SiC grains with 1 nm-wide amorphous intergranular films were believed to be responsible for the in situ toughening of this material, specifically by mechanisms of crack deflection and grain bridging. Two methods were found to be effective in modifying microstructure and optimizing mechanical performance. First, prescribed post-annealing treatments at temperatures between 1100 and 1500°C were seen to cause full crystallization of the amorphous intergranular films and to introduce uniformly dispersed nanoprecipitates within SiC matrix grains; in addition, lattice diffusion of aluminum at elevated temperatures was seen to alter grain-boundary composition. Second, adjusting the nominal content of sintering additives was also observed to change the grain morphology, the grain-boundary structure, and the phase composition of the ABC-SiC. In this regard, the roles of individual additives in developing boundary microstructures were identified; this was demonstrated to be critical in optimizing the mechanical properties, including fracture toughness and fatigue resistance at ambient and elevated temperatures, flexural strength, wear resistance, and creep resistance.


1990 ◽  
Vol 5 (5) ◽  
pp. 919-928 ◽  
Author(s):  
S. E. Babcock ◽  
D. C. Larbalestier

Regular networks of localized grain boundary dislocations (GBDs) have been imaged by means of transmission electron microscopy in three different types of high-angle grain boundaries in YBa2Cu3O7-δ, implying that these boundaries possess ordered structures upon which a significant periodic strain field is superimposed. The occurrence of these GBD networks is shown to be consistent with the GBD/Structural Unit and Coincidence Site Lattice (CSL)/Near CSL descriptions for grain boundary structure. Thus, these dislocations appear to be intrinsic features of the boundary structure. The spacing of the observed GBDs ranged from ∼10 nm to ∼100 nm. These GBDs make the grain boundaries heterogeneous on a scale that approaches the coherence length and may contribute to their weak-link character by producing the “superconducting micro-bridge” microstructure which has been suggested on the basis of detailed electromagnetic measurements on similar samples.


2007 ◽  
Vol 121-123 ◽  
pp. 1241-1244 ◽  
Author(s):  
Dong Seok Seo ◽  
Hwan Kim ◽  
Jong Kook Lee

In this study, it was demonstrated how second phases with small amount, which are hardly detected by XRD analysis, affect grain boundary dissolution and related mechanical properties of HA. All HA disks sintered at 1200 oC for 2 h in air with under moisture protection were phase pure and had Ca/P molar ratio of 1.67. Following certain period of exposure to the distilled water, the surface dissolution initiated at grain boundaries and particle loosening, subsequently resulting in decrease in mechanical properties of HA. In order to understand the dissolution mechanism, grain boundary structure of HA was identified by transmission electron microscopy (TEM) and high resolution TEM observation. From the analysis, it was found that the non-stoichiometric phase as α-tricalcium phosphate (TCP) transformed from β-TCP was existed at grain boundaries and caused surface dissolution of HA. From the XRD analysis, it was found that (211) and (112) planes of hydroxyapatite were susceptible to dissolution, whereas (300) plane was relatively stable.


1995 ◽  
Vol 391 ◽  
Author(s):  
M. Hasunuma ◽  
H. Toyoda ◽  
T. Kawanoue ◽  
S. Ito ◽  
H. Kaneko ◽  
...  

AbstractIn order to clarify the relationship between Al line reliability and film microstructure, especially grain boundary structure and crystal texture, we have tested three kinds of highly textured Al lines, namely, single-crystal Al line, quasi-single-crystal Al line and hypertextured Al line, and two kinds of conventional Al lines deposited on TiN/Ti and on SiO2. Consequently, the empirical relation between the electromigration (EM) lifetime of Al line † and the (111) full width at half maximum (FWHM) value ω is described by † ∝ ω-2 [1]. This improvement of Al line reliability results from as following reasons; firstly, homogeneous microstructure and high activation energy of 1.28eV for the single-crystal Al line (ω=0.18°); secondly, sub-grain boundaries which consisted of dislocation arrays found in the quasi-single-crystal Al line (ω=0.26°) has turned out to be no more effective mass transport paths because dislocation lines are perpendicular to the direction of electron wind. Although there exist plural grain boundary diffusion paths in the newly developed hypertextured Al line (ω=0.5°) formed by using an amorphous Ta-Al underlayer {1], the vacancy flux along the line has been suppressed to the same order of magnitude of single crystal line. It has been clarified that the decrease of FWHM value has promoted the formation of sub-grain boundaries and low-angle boundaries with detailed orientation analysis of individual grains in the hypertextured film. The longer EM lifetime for the hypertextured Al line is considered to be due to the small grain boundary diffusivities for these stable grain boundaries, and this diffusivity reduction resulted in the suppression of void/hillock pair in the Al lines. These results have confirmed that controlling texture and/or grain boundary itself is a promising approach to develop reliable Al lines which withstand higher current densities required in future ULSIs.


2012 ◽  
Vol 18 (S2) ◽  
pp. 346-347
Author(s):  
C. Wade ◽  
M. McLean ◽  
R. Vinci ◽  
M. Watanabe ◽  
L. Giannuzzi

Extended abstract of a paper presented at Microscopy and Microanalysis 2012 in Phoenix, Arizona, USA, July 29 – August 2, 2012.


Author(s):  
D. L. Rohr ◽  
S. S. Hecker ◽  
L. E. Murr

Iridium is a most interesting fee metal with a high melting point (2443°C) and extremely high elastic moduli (Young's modulus of 76 million psi). Single crystals of Ir fail by brittle cleavage and polycrystalline Ir fails by brittle intergranular fracture at temperatures below 1000°C. We have previously shown that both modes of fracture are intrinsic and not impurity related. (1)The present study was undertaken to study the grain boundary structure of Ir by transmission electron microscopy. Sheet specimens of Ir-0.3%W (used in space nuclear power applications) were recrystallized at temperatures above 1300°C. Thin foils were prepared by spark planing and electropolishing with an acidified CaCl2 solution in a jet polisher and were examined in a JEOL 200 B electron microscope operated at 200 kv.We examined a large number of foils and found the most interesting grain boundary features to be ledges (2) (Fig. la).


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