Measurement of thermal residual stresses in ZrB2-SiC composites

Neutron diffraction, Raman spectroscopy, and x-ray diffraction were employed to measure the stresses generated in the ZrB₂ matrix and SiC dispersed particulate phase in ZrB₂-30 vol% SiC composites produced by hot pressing at 1900 °C. Neutron diffraction measurements indicated that stresses begin to accumulate at ∼1400 °C during cooling from the processing temperature and increased to 880 MPa compressive in the SiC phase and 450 MPa tensile in the ZrB₂ phase at room temperature. Stresses measured via Raman spectroscopy revealed the stress in SiC particles on the surface of the composite was ∼390 MPa compressive, which is ∼40% of that measured in the bulk by neutron diffraction. Grazing incidence x-ray diffraction was performed to further characterize the stress state in SiC particles near the surface. Using this technique, an average compressive stress of 350 MPa was measured in the SiC phase, which is in good agreement with that measured by Raman spectroscopy.     

In situ measurement of stresses in diamond-like carbon films

In situ determination of stresses in thin films can be used as an important tool to assist process development as well as to understand the thermodynamics of film formation. A simple technique for the measurement of stresses in growing films is described here. The technique consists of measuring the displacement of a laser beam reflected from the film surface. Displacement is induced by changes in the radius of the curvature of the substrate resulting from stresses in the film. The detector sensitivity at the used wavelength (635 nm) is approximately 12 mV μm⁻¹, for which our experimental set-up is equivalent to 4 mV μrad⁻¹. The actual data collected consist of the reflected beam displacement vs. time, and provides at any instant the value of the average stress. By knowing the deposition rate, time is directly correlated with film thickness, and the local stress can be determined. Examples of measurement of stresses in tetragonally bonded amorphous carbon films prepared by filtered cathodic arc are presented, as well as how this technique can be used to design the deposition process to virtually eliminate intrinsic stresses.     

Investigation of the residual stress in UO2-Mo composites via a neutron diffraction method

UO₂-Mo composites with a core-shell structure have been considered candidates for the thermal conductivity (TC)-enhanced UO₂ pellets and have demonstrated commercial potential for use in novel high-level safety reactors. Nevertheless, UO₂-Mo composites tend to form micro-cracks that are caused by the presence of residual stress (RS) during manufacturing. In this work, neutron diffraction measurements were employed to analyse the RS in UO₂-Mo core-shell structured composites fabricated by spark plasma sintering (SPS) for the first time. It was found that in the UO₂-Mo composites, the RS state present in the UO₂ matrix was tensile in nature. The RS in the UO₂ matrix increased with increaseing Mo content. There was a maximum value of 148 ± 15 MPa in the UO₂-10 vol% Mo composite. The micro-cracks produced in the high-Mo content composites were explained by the results of the neutron diffraction measurements. These results could provide significant guidance for the manufacturing and improvement of the operational performance of UO₂-Mo composites as next-generation fuels.     

Fabrication of modified ultra high-temperature ceramic hybrid powders using in situ grown SiC nanowires

Ultra-high temperature ceramic (UHTC) hybrid powders modified using in situ grown SiC nanowires (SiCNWs) were successfully prepared via a simple catalytic method. The self-produce carbon and silicon source promoted the growth of SiCNWs during the pyrolysis process of ZrB₂ polymer precursors coated ZrB₂-SiC powders. The results showed that the growth of SiCNWs could be explained by a tip-growth model and vapor–liquid–solid (VLS) growth mechanism. The SiCNWs with diameter of 200 nm were single crystalline, and the content could be controlled by changing the catalyst content.     

碳化硅陶瓷的研究进展

碳化硅陶瓷以优异的高温力学性能以及优良的耐化学腐蚀性能得到了越来越广泛的应用,本文重点介绍了碳化硅陶瓷的烧结工艺以及性能特点等。     

Determination of the bulk fraction of spherical non-uniformities in high-density materials

The paper conducts a thorough comparative analysis of several models for assessing the porosity of materials. As in the models under consideration, the main role is given to a geometrical perspective of the problem. The obtained results become applicable to other types of inclusions within the studied volume of an arbitrary material. The theoretical analysis yields a table with a number of parameters for comparing various porosity assessment approaches and the number concentration of pores in the material bulk. The evaluated difference in the outcomes of different methods applied is as high as ~40% based on Al₂O₃−RE:YAG (RE=Ce; Ce + Gd) composite ceramic phosphors taken as model objects. Such a huge variance among the calculated values demonstrates the importance of analyzing each certain porosity assessment approach applied when comparing the experimental data.     

Residual stresses and crystalline quality of heavily boron-doped diamond films analysed by micro-Raman spectroscopy and X-ray diffraction

X-ray diffraction analysis and micro-Raman spectroscopy measurements have been used for stress studies on HFCVD diamond films with different levels of boron doping. The boron incorporation in the film varied in the range 10¹⁸-10²¹ boron/cm³. The grain size, obtained from SEM images, showed grains with 2-4-μm average size, which decreases when the doping level increases. The thickness of the films obtained by SEM cross-section view decreased from 8 to 5 μm as the doping level increased from 0 (undoped film) to 10²¹ boron/cm³. The total residual stress was determined by measuring, for each sample, the (331) diamond Bragg diffraction peak for Ψ-values ranging from −60° to +60°, and applying the sin² ψ method. For the micro-Raman spectroscopy the spectral analysis performed on each sample allowed the determination of the residual stress, from the diamond Raman peak shifts, and also the diamond purity, which decreases from 99 to 75% as the doping level increases. The type and magnitude of the residual stress obtained from X-ray and micro-Raman measurements agreed well only for undoped film, disagreeing when the doping level increased. We attributed this discrepancy to the domain size characteristic of each technique.     

Investigation of novel superhard materials by multi-cycling nanoindentation

Depth sensing nanoindentation is applied to characterize the mechanical properties of new superhard materials such as cubic c-BC_x. Special load–time functions are developed to test the material by repeated loading and unloading processes. These intelligent load functions are applied in multi-cycling indents at the same place on the sample surface. Besides being time-efficient, the data collection method also does not suffer from lateral inhomogeneities of the sample. The hardness of the single phase cubic c-BC_x sample was found to be 78 GPa and its indentation modulus is between 900 and 1000 GPa. Hysteresis loops are observed in the superhard material, which are attributed to the generation of nano-cracks.     

Evaluation of residual stresses during brazing of Al2O3-ZrO2 to cemented tungsten carbide

In the context of the assembly of a cutting tool for wood machining, this article proposes to evaluate the residual stress in a ceramic plate (Al₂O₃-ZrO₂) induced by a brazing step with a cemented tungsten carbide (WC-Co) through a brazing filler (Ag-Cu-Ti). The residual stresses were evaluated using neutron and X-ray diffraction method. Moreover, a mathematical model was used in the case of a three layer assembly, which is based on mechanical properties such as: the thermal coefficient, the Young's modulus, the Poisson's ratio and the thickness of each layer. The observation of the chemical mapping of the brazing filler before and after the assembly, using energy dispersive X-ray spectroscopy (EDX), showed the chemical migration of the titanium to the ceramic oxide and the tungsten carbide. It was estimated that the brazed assembly is under a flexural stress, with a maximum in a compressive stress area near the brazing joint which reaches 85.6 MPa. This stress value reaches 12% of the bending strength allowed by the ceramic (716 MPa). The discussion proposes to highlight the limits of each method. The mathematical model has however shown good accuracy to give a first estimated residual stress in the ceramic plate.     

Microscale computational simulation and experimental measurement of thermal residual stresses in glass–alumina functionally graded materials

Glass–alumina functionally graded materials are new attractive composite materials, that can achieve peculiar mechanical properties due to their gradual compositional variation. Nevertheless, the difference between the coefficients of thermal expansion of the constituent phases may result in significant thermal residual stresses in service or during fabrication. A proper glass formulation can minimize the mismatch in thermo-mechanical properties, thus relevantly reducing the mean value of the resultant thermal stresses. However, it is a crucial requirement to evaluate the effect of microstructural discreteness and randomness on the actual stress distribution in functionally graded materials. With this aim, a computational model which applies the finite element method at the microscale is used. The careful modelling of the real microstructural details enables to accurately predict the local stress values and distribution. In order to verify the reliability of the computational simulations, the residual thermal stresses were also experimentally measured by means of a piezo-spectroscopic technique. The comparison between the numerical and the experimental results validate the microstructure-based model.     

Generation of large residual stresses in injection moldings

Large residual stresses have been generated in injection molded bars by ejecting them prematurely and completing the cooling process by quenching into ice water or liquid nitrogen. The stress distribution formed under these conditions was found to be much closer to parabolic than is the case when the moldings cool conventionally. Limited testing on moldings made in this way indicated significant property enhancement and improved resistance to ultraviolet degradation.     

Improvement of mechanical performances and characteristics of bulk Bi-2212 materials exposed to Au diffusion and stabilization of durable tetragonal phase by Au

This study centers sensitively on the determination of optimum diffusion annealing temperature (650–850 °C) for the electrical, superconducting, crystal structure, and especially mechanical characteristics of Au surface-layered Bi-2212 superconducting materials with the aid of dc electrical resistivity, powder X-ray diffraction and microhardness measurements. The experimental results show that all the characteristic properties (normal state resistivity, critical transition temperatures, degree of broadening, phase fractions, lattice cell parameters, elastic modulus, yield strength, fracture toughness, brittleness index and flexural strength parameters) improve considerably with the increment in the annealing temperature up to 800 °C as a consequence of the decreased local structural distortions, lattice strains, disorders, defects and grain boundary interaction problems in the Cu-O₂ consecutively stacked layers. After the critical annealing temperature value of 800 °C, the parameters immediately recrudesce towards their global minimum points. Similarly, the highest Bi-2223 phase fraction and c-axis length are observed at the 800 °C annealing temperature due to the best crystallinity and crystal plane alignments. Additionally, the optimum value strengthens the mechanical durability and ideal flexural strength as a result of the stabilization of durable tetragonal phase. Thus, the presence of Au impurities increases the critical stress value so that the crack-producing flaws and cracks propagation divert or slow down rapidly. On the other hand, the excess temperature value such as 850 °C leads to the deleterious effect on the mechanical performances of Au surface-layered Bi-2212 compound because of the increased residual porosity and omnipresent flaws (stress raisers and crack initiation sites). Further, it is at least equally important that the crack propagation or dislocation movement more proceeds through the transgranular regions instead of along the intergranular regions with increasing temperature up to the optimum value beyond which the limited number of operable slip systems enhances noticeably and the intergranular fracture becomes more dominant.     

Investigation of relaxation of nanodiamond surface in real and reciprocal spaces

The structure of a nanodiamond powder with an average grain size of 5 nm was investigated using large-Q neutron diffraction. Both Bragg scattering and PDF analysis were employed. The effect of annealing under vacuum at temperatures up to 1200 °C was studied. The studies lead to a tentative model of nanocrystalline diamond, where the core with a perfect diamond lattice is surrounded by a shell of compressed diamond lattice, and this core–shell structure is enveloped in a non-diamond carbon. The non-diamond envelope of nanograins, a “gas-like” carbon, is stable up to 1000 °C and transforms into a graphite phase (an onion-type structure) at about 1200 °C. The amount of non-crystalline carbon in the powder annealed below 1000 °C is about 10%. In the sample annealed at 1200 °C a graphite-type carbon, with a total of about 15% of sp² bonds is formed.     

Analysis of the development of isotropic residual stresses in a bismaleimide/spiro orthocarbonate thermosetting resin for composite materials

In this article, we extend our model of isotropic residual stress development in thermosets to a novel thermosetting resin system: bismaleimide/spiro orthocarbonate. In this system, the cure shrinkage and resulting isotropic residual stresses are reduced through a ring‐opening reaction that occurs independently of the addition reaction. The modeling effort includes a parametric analysis of the effects of various parameters, including the volume changes involved in the reactions, the relative rates and orders of the reactions, the cure history, and the values of the bulk moduli and thermal expansion coefficients. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 227–244, 2003     

Structural transformations of Muscovite at high temperature by X-ray and neutron diffraction

Structural transformations of Muscovite at temperature up to 1095 °C were determined using powder X-ray and neutron diffraction. Data were collected at room temperature from preliminary heated and quenched samples at 650 °C, 980 °C and 1095 °C. X-ray data were interpreted by either Rietveld method and neutron data, which complete the structural information by a better assignation of oxygen positions. With neutron data atom position was refined by fitting Pair Distribution Functions. It was found to be a progressive but continuous microstructural change, with the formation of an increasingly disorganized structure, but the layered organization of muscovite is maintained up to 1095 °C. Rietveld refinements from X-ray confirm the 6 to 5 coordination of Al atoms above 650 °C. It induces some structural changes as the orientation and mutual position of tetrahedrons in silicate layers. Pair Distribution Function refinements show the weakening of the long range structural organization, above 5 Å. At lower distance, a local order is maintained and the preferential alignments of both alumina unit pairs and silica tetrahedron were observed. This residual structural order of high-temperature muscovite is favorable to the achievement of textured ceramics.