Structural and mechanical properties of room temperature sputter deposited CrN coatings

Chromium nitride (CrN) thin films were deposited at room temperature on silicon and glass substrates using DC reactive magnetron sputtering in Ar + N-2 plasma. Structure and mechanical properties of these films were examined by using XRD, FESEM and nanoindentation techniques. XRD studies revealed that films are of mixed phase at lower nitrogen partial pressure (P-N2) and single phase at higher (P-N2). Microscopy results show that the films were composed of non-equiaxed columns with nanocrystallite morphology. The hardness and elastic modulus of the films increase with increasing nitrogen partial pressure (P-N2). A maximum hardness of similar to 29 GPa and elastic modulus of 341 GPa were obtained, which make these films useful for several potential applications. (C) 2012 Elsevier Ltd. All rights reserved.

Evaluation of CaO-CeO2-partially stabilized zirconia thermal barrier coatings

Plasma sprayable powders were prepared from ZrO2-CaO-CeO2 system using an organic binder and coated onto stainless steel substrates previously coated by a bond coat (Ni 22Cr 20Al 1.0Y) using plasma spraying. The coatings exhibited good thermal barrier characteristics and excellent resistance to thermal shock at 1000 degrees C under simulated laboratory conditions (90 half hour cycles without failure) and at 1200 degrees C under accelerated burner rig test conditions (500 2 min cycles without failure). No destabilization of cubic/tetragonal ZrO2 phase fraction occured either during the long hours (45 h cumulative) or the large number of thermal shock tests. Growth of a distinct SiO2 rich region within the ceramic was observed in the specimens thermal shock cycled at 1000 degrees C apart from mild oxidation of the bond coat. The specimens tested at 1200 degrees C had a glassy appearance on the top surface and exhibited severe oxidation of the bond coat at the ceramic-bond coat interface. The glassy appearance of the surface is due to the formation of a liquid silicate layer attributable to the impurity phase present in commercial grade ZrO2 powder. These observations are supported by SEM analysis and quantitative EDAX data.

Thermal shock characteristics of plasma sprayed mullite coatings

Commercially available mullite (3Al(2)O(3). 2SiO(2)) powders containing oxides of calcium and iron as impurities, have been made suitable for plasma spraying by using an organic binder. Stainless steel substrates covered with Ni-22Cr-10Al-1.0Y bond coat were spray coated with mullite, The 425 mu m thick coatings were subjected to thermal shock cycling under burner rig conditions between 1000 and 1200 degrees C and less than 200 degrees C with holding times of 1, 5, and 30 min. While the coatings withstood as high as 1000 shock cycles without failure between 1000 and 200 degrees C, spallation occurred early at 120 cycles when shocked from 1200 degrees C, The coatings appeared to go through a process of self erosion at high temperatures resulting in loss of material. Also observed were changes attributable to melting of the silicate grains, which smooth down the surface. Oxidation of the bond coat did not appear to influence the failure, These observations were supported by detailed scanning electron microscopy and quantitative chemical composition analysis, differential thermal analysis, and surface roughness measurements.

Defect-selective photothermal imaging: a sensitive tool for damage mapping in optical coatings

A defect-selective photothermal imaging system for the diagnostics of optical coatings is demonstrated. The instrument has been optimized for pump and probe parameters, detector performance, and signal processing algorithm. The imager is capable of mapping purely optical or thermal defects efficiently in coatings of low damage threshold and low absorbance. Detailed mapping of minor inhomogeneities at low pump power has been achieved through the simultaneous action of a low-noise fiber optic photothermal beam defection sensor and a common-mode-rejection demodulation (CMRD) technique. The linearity and sensitivity of the sensor have been examined theoretically and experimentally, and the signal to noise ratio improvement factor is found to be about 110 compared to a conventional bicell photodiode. The scanner is so designed that mapping of static or shock sensitive samples is possible. In the case of a sample with absolute absorptance of 3.8 x 10(-4), a change in absorptance of about 0.005 x 10(-4) has been detected without ambiguity, ensuring a contrast parameter of 760. This is about 1085% improvement over the conventional approach containing a bicell photodiode, at the same pump power. The merits of the system have been demonstrated by mapping two intentionally created damage sites in a MgF2 coating on fused silica at different excitation powers. Amplitude and phase maps were recorded for thermally thin and thick cases, and the results are compared to demonstrate a case which, in conventional imaging, would lead to a deceptive conclusion regarding the type and location of the damage. Also, a residual damage profile created by long term irradiation with high pump power density has been depicted.

K-Ar ages of biotite and muscovite from Pangong metamorphic complex, Shyok suture zone, India: Implications for the youngest post-collision metamorphic event in Ladakh Himalaya

The garnet-kyanite-staurolite and garnet-biotite-staurolite gneisses were collected from a locality within Lukung area that belongs to the Pangong metamorphic complex in Shyok valley, Ladakh Himalaya. The kyanite-free samples have garnet and staurolite in equilibrium, where garnets show euhedral texture and have flat compositional profile. On the other hand, the kyanite-bearing sample shows equilibrium assemblage of garnet-kyanite-staurolite along with muscovite and biotite. In this case, garnet has an inclusion rich core with a distinct grain boundary, which was later overgrown by inclusion free euhedral garnet. Garnet cores are rich in Mn and Ca, while the rims are poor in Mn and rich in Fe and Mg, suggesting two distinct generations of growth. However, the compositional profiles and textural signature of garnets suggests the same stage of P -T evolution for the formation of the inclusion free euhedral garnets in the kyanite-free gneisses and the inclusion free euhedral garnet rims in the kyanite-bearing gneiss. Muscovites from the four samples have consistent K-Ar ages, suggesting the cooling age (∼ 10 Ma) of the gneisses. These ages make a constraint on the timing of the youngest post-collision metamorphic event that may be closely related to an activation of the Karakoram fault in Pangong metamorphic complex.

High vacuum tribology of polycrystalline diamond coatings

Polycrystalline diamond coatings have been grown on unpolished side of Si(100) wafers by hot filament chemical vapour deposition process. The morphology of the grown coatings has been varied from cauliflower morphology to faceted morphology by manipulation of the growth temperature from 700 degrees C to 900 degrees C and methane gas concentration from 3% to 1.5%. It is found that the coefficient of friction of the coatings under high vacuum of 133.32 x 10(-7) Pa (10(-7) torr) with nanocrystalline grains can be manipulated to 0.35 to enhance tribological behaviour of bare Si substrates.

High efficiency infrared antireflection coatings (ARCs) for space optics

Simple ARC designs for germanium (Ge) optics useful in spaceborne electro-optical systems have been generated. It is seen that the designs which are non-quarterwave in nature are efficient in terms of spectral coverage and residual reflection loss. They have been realised experimentally and the resulting ARCs are found to have very good spectral and durability properties.

Vacuum emissivity meter for thermal emittance measurements of coatings

The problems in measuring thermal emittance by steady?state calorimetric technique have been analyzed. A few suggestions to make it more accurate, simple, and rapid have been discussed and results are presented.

Laser-fused refractory oxides for optical coatings

Laser sintering was carried out using a high power continuous-wave CO2 laser to prepare pellets of zirconia (ZrO2), hafnia (HfO2) and yttria (Y2O3) mixed oxides as starting materials in the deposition of optical coatings. Hardened recrystallized pellets appeared to have been formed during laser treatment. X-ray diffraction analysis revealed a monoclinic-to-tetragonal phase transformation in the binary system while the ternary system was found to have a mixture of two crystalline phases. Cross-sectional scanning electron microscopy showed two isothermal crystalline regions in the ternary system. The optical inhomogeneity was low in the films deposited from the laser-fused pellets, but the absorption at a wavelength of 351 nm increased with increasing HfO2 content. The films deposited from laser-fused pellets were analysed by electron spectroscopy for chemical analysis and found to be stoichiometric and homogeneous.

Nucleophilic attacks of 1,2-diaminoethane on MeCN ligands: synthesis, x-ray structure, and spectral and electrochemical properties of [Ru(.mu.-O)(.mu.-O2CAr)2[NH2CH2CH2NHC(Me)NH]2(PPh3)2](ClO4)2(Ar = C6H4-p-X; X = H, Me, OMe, Cl)

The diruthenium(III) complex [Ru2O(O2CAr)2(MeCN)4(PPh3)2](ClO4)2 (1), on reaction with 1,2-diaminoethane (en) in MeOH at 25-degrees-C, undergoes nucleophilic attacks at the carbon of two facial MeCN ligands to form [(Ru2O)-O-III(O2CAr)2-{NH2CH2CH2NHC(Me)NH}2(PPh3)2](ClO4)2 (2) (Ar = C6H4-p-X, X = H, Me, OMe, Cl) containing two seven-membered amino-amidine chelating ligands. The molecular structure of 2 with Ar = C6H4-p-OMe was determined by X-ray crystallography. Crystal data are as follows: triclinic, P1BAR, a = 13.942 (5) angstrom, b = 14.528 (2) angstrom, c = 21.758 (6) angstrom, alpha = 109.50 (2)-degrees, beta = 92.52 (3)-degrees, gamma = 112.61 (2)-degrees, V = 3759 (2) angstrom 3, and Z = 2. The complex has an {Ru2(mu-O)(mu-O2CAr2)2(2+)} core. The Ru-Ru and average Ru-O(oxo) distances and the Ru-O-Ru angle are 3.280 (2) angstrom, 1.887 [8] angstrom, and 120.7 (4)-degrees, respectively. The amino group of the chelating ligand is trans to the mu-oxo ligand. The nucleophilic attacks take place on the MeCN ligands cis to the mu-oxo ligand. The visible spectra of 2 in CHCl3 display an absorption band at 565 nm. The H-1 NMR spectra of 2 in CDCl3 are indicative of the formation of an amino-amidine ligand. Complex 2 exhibits metal-centered quasireversible one-electron oxidation and reduction processes in the potential ranges +0.9 to +1.0 V and -0.3 to -0.5 V (vs SCE), respectively, involving the Ru(III)2/Ru(III)Ru(IV) and Ru(III)2/Ru(II)Ru(III) redox couples in CH2Cl2 containing 0.1 M TBAP. The mechanistic aspects of the nucleophilic reaction are discussed.

Precursor Dependent Microstructure Evolution and Nonstoichiometry in Nanostructured Cerium Oxide Coatings Using the Solution Precursor Plasma Spray Technique

A solution precursor plasma spray (SPPS) technique has been used for direct deposition of cerium oxide nanoparticles (CNPs) from various cerium salt solutions as precursors. Solution precursors were injected into the hot zone of a plasma plume to deposit CNP coatings. A numerical study of the droplet injection model has been employed for microstructure development during SPPS. The decomposition of each precursor to cerium oxide was analyzed by thermogravimetric-differential thermal analysis and validated by thermodynamic calculations. The presence of the cerium oxide phase in the coatings was confirmed by X-ray diffraction studies. Transmission electron microscopy studies confirmed nanocrystalline (grain size <14 nm) characteristic of the coatings. X-ray photoelectron spectroscopy studies indicated the presence of a high concentration of Ce3+ (up to 0.32) in the coating prepared by SPPS. The processing and microstructure evolution of cerium oxide coatings with high nonstoichiometry are reported.