Stopping the clock on proteomic degradation by heat treatment at the point of tissue excision

The effectiveness of rapid and controlled heating of intact tissue to inactivate native enzymatic activity and prevent proteome degradation has been evaluated. Mouse brains were bisected immediately following excision, with one hemisphere being heat treated followed by snap freezing in liquid nitrogen while the other hemisphere was snap frozen immediately. Sections were cut by cryostatic microtome and analyzed by MALDI-MS imaging and minimal label 2-D DIGE, to monitor time-dependent relative changes in intensities of protein and peptide signals. Analysis by MALDI-MS imaging demonstrated that the relative intensities of markers varied across a time course (0-5 min) when the tissues were not stabilized by heat treatment. However, the same markers were seen to be stabilized when the tissues were heat treated before snap freezing. Intensity profiles for proteins indicative of both degradation and stabilization were generated when samples of treated and nontreated tissues were analyzed by 2-D DIGE, with protein extracted before and after a 10-min warming of samples. Thus, heat treatment of tissues at the time of excision is shown to prevent subsequent uncontrolled degradation of tissues at the proteomic level before any quantitative analysis, and to be compatible with downstream proteomic analysis.

The effect of heat treatment on mechanical properties of pulsed Nd:YAG welded thin Ti6Al4V

Pulsed Nd:YAG has been adopted successfully in welding process of thin (0.7 mm) Ti6Al4V. Laser welding of such thin sheet requires a small focal spot, good laser beam quality and fast travel speed, since too much heat generation can cause distortion for thin sheet weld. The microstructures of Ti6Al4V were complex and strongly affected the mechanical properties. These structures include: a´ martensite, metastable ß, Widmanstätten, bimodal, lamellar and equiaxed microstructure. Bimodal and Widmanstätten structures exhibit a good-balance between strength and ductility. The microstructure of pulsed Nd:YAG welded Ti6Al4V was primarily a´ martensite, which showed the lowest ductility but not significantly high strength. A heat treatment at 950 followed by furnace cooling can transform the microstructure in the weld from a´ martensite structure into Widmanstätten structure.

An examination of the production, heat treatment and mechanical properties of a new wrought magnesium alloy containing 6% Zn. and 1.2% Mn.

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Fatigue behaviour of C-Mn-B steels:effects of heat treatment prestrain and residual stress

The fatigue-crack propagation and threshold behaviour of a C-Mn steel containing boron has been investigated at a range of strength levels suitable for mining chain applications. The heat-treatment variables examined include two austenitizing temperatures (900 degree C and 1250 degree C) and a range of tempering treatments from the as-quenched condition to tempering at 400 degree C. In mining applications the haulage chains undergo a 'calibration' process which has the effect of imposing a tensile prestrain on the chain links before they go into service. Prestrain is shown to reduce threshold values in these steels and this behaviour is related to its effects on the residual stress distribution in the test specimens.

Decomposition of the B2-type matrix

The microstructural stability of aluminide diffusion coatings, prepared by means of a two-stage pack-aluminization treatment on single-crystal nickel-base superalloy substrates, is considered in this article. Edge-on specimens of coated superalloy are studied using transmission electron microscopy (TEM). The effects of coating thickness and post-coating heat treatment (duration, temperature, and atmosphere) on coating microstructure are examined. The article discusses the partial transformation of the matrix of the coating, from a B2-type phase (nominally NiAl) to a L12 phase (nominally Ni3(Al, Ti)), during exposure at temperatures of 850 °C and 950 °C in air and in vacuum for up to 138 hours. Three possible processes that can account for decom- position of the coating matrix are investigated, namely, interdiffusion between the coating and the substrate, oxidation of the coating surface, and aging of the coating. Of these processes, aging of the coating is shown to be the predominant factor in the coating transformation under the conditions considered. © 1992 The Minerals, Metals and Materials Society, and ASM International.

Development and evaluation of a non-destructive adhesion test

The object of this work was to further develop the idea introduced by Muaddi et al (1981) which enables some of the disadvantages of earlier destructive adhesion test methods to be overcome. The test is non-destructive in nature but it does need to be calibrated against a destructive method. Adhesion is determined by measuring the effect of plating on internal friction. This is achieved by determining the damping of vibrations of a resonating specimen before and after plating. The level of adhesion was considered by the above authors to influence the degree of damping. In the major portion of the research work the electrodeposited metal was Watt's nickel, which is ductile in nature and is therefore suitable for peel adhesion testing. The base metals chosen were aluminium alloys S1C and HE9 as it is relatively easy to produce varying levels of adhesion between the substrate and electrodeposited coating by choosing the appropriate process sequence. S1C alloy is the commercially pure aluminium and was used to produce good adhesion. HE9 aluminium alloy is a more difficult to plate alloy and was chosen to produce poorer adhesion. The "Modal Testing" method used for studying vibrations was investigated as a possible means of evaluating adhesion but was not successful and so research was concentrated on the "Q" meter. The method based on the use of a "Q" meter involves the principle of exciting vibrations in a sample, interrupting the driving signal and counting the number of oscillations of the freely decaying vibrations between two known preselected amplitudes of oscillations. It was not possible to reconstruct a working instrument using Muaddi's thesis (1982) as it had either a serious error or the information was incomplete. Hence a modified "Q" meter had to be designed and constructed but it was then difficult to resonate non-magnetic materials, such as aluminium, therefore, a comparison before and after plating could not be made. A new "Q" meter was then developed based on an Impulse Technique. A regulated miniature hammer was used to excite the test piece at the fundamental mode instead of an electronic hammer and test pieces were supported at the two predetermined nodal points using nylon threads. This instrument developed was not very successful at detecting changes due to good and poor pretreatments given before plating, however, it was more sensitive to changes at the surface such as room temperature oxidation. Statistical analysis of test results from untreated aluminium alloys show that the instrument is not always consistent, the variation was even bigger when readings were taken on different days. Although aluminium is said to form protective oxides at room temperature there was evidence that the aluminium surface changes continuously due to film formation, growth and breakdown. Nickel plated and zinc alloy immersion coated samples also showed variation in Q with time. In order to prove that the variations in Q were mainly due to surface oxidation, aluminium samples were lacquered and anodised Such treatments enveloped the active surfaces reacting with the environment and the Q variation with time was almost eliminated especially after hard anodising. This instrument detected major differences between different untreated aluminium substrates.Also Q values decreased progressively as coating thicknesses were increased. This instrument was also able to detect changes in Q due to heat-treatment of aluminium alloys.

Valence-tautomeric RbMnFe Prussian blue analogues:composition and time stability investigation

Three different stoichiometric forms of RbMn[Fe(CN) ]y·zHO [x = 0.96, y = 0.98, z = 0.75 (1); x = 0.94, y = 0.88, z = 2.17 (2); x = 0.61, y = 0.86, z = 2.71 (3)] Prussian blue analogues were synthesized and investigated by magnetic, calorimetric, Raman spectroscopic, X-ray diffraction, and Fe Mössbauer spectroscopic methods. Compounds 1 and 2 show a hysteresis loop between the high-temperature (HT) Fe(S = 1/2)-CN-Mn(S = 5/2) and the low-temperature (LT) Fe(S = 0)-CN-Mn(S = 2) forms of 61 and 135 K width centered at 273 and 215 K, respectively, whereas the third compound remains in the HT phase down to 5 K. The splitting of the quadrupolar doublets in the Fe Mössbauer spectra reveal the electron-transfer-active centers. Refinement of the X-ray powder diffraction profiles shows that electron-transfer-active materials have the majority of the Rb ions on only one of the two possible interstitial sites, whereas nonelectron-transfer-active materials have the Rb ions equally distributed. Moreover, the stability of the compounds with time and following heat treatment is also discussed. © Wiley-VCH Verlag GmbH & Co. KGaA, 2009.

Femtosecond laser writing of buried waveguides in erbium III-Doped oxyfluoride glasses and nano-glass-ceramics

Femtosecond-pulsed laser writing of waveguides, a few mm long, is demonstrated; waveguides were written orthogonally to the writing beam inside the bulk of ErIII-doped oxyfluoride glasses at a depth of 160 mum. The writing beam was 795 nm wavelength, 54 fs pulse duration and 11 MHz repetition rate. Tracks were written at pulse energies of 13.1 nJ to 26.1 nJ and sample translational velocity of 10 mmmiddot.s-1 to 28 mmmiddots-1. The influence of translational velocity and pulse energy on the cross-sectional shape and integrity of the written tracks is reported. Tracks tend to be narrower as the pulse energy is lowered or translational velocity decreased. Above 22.9 nJ, pulse energy, tracks tend to crack. The estimated refractive index profile of one track has a maximum increase of refractive index of 0.003 at the centre. These glasses normally form nano-glass-ceramics on heat treatment just above the glass transformation temperature (Tg). Here, a post-fs-writing heat-treatment just above Tg causes nano-ceramming of the glass sample and removes a light-guiding peripheral region of the fs-written tracks suggesting that this region may have been fs-modified by stress alone. Waveguiding at 651 nm and 973 nm wavelengths, and upconversion, are demonstrated in optimally written tracks.

Autocatalytic deposition of composite coatings

The deposition and properties of electroless nickel composite coatings containing graphite, PTFE and chromium were investigated. Solutions were developed for the codeposition of graphite and chromium with electroless nickel. Solutions for the deposition of graphite contained heavy metal ions for stability, with non-ionic and anionic surfactants to provide wetting and dispersion of the particles. Stability for the codeposition of chromium particles was achieved by oxidation of the chromium. Thin oxide layers of 200 nm thick prevented initiation of the electroless reaction onto the chromium. A mechanism for the formation of electroless composite coatings was considered based on the physical adsorption of particles and as a function of the adsorption of charged surfactants and metal cations from solution. The influence of variables such as particle concentration in solution, particle size, temperature, pH, and agitation on the volume percentage of particles codeposited was studied. The volume percentage of graphite codeposited was found to increase with concentration in solution and playing rate. An increase in particle size and agitation reduced the volume percentage codeposited. The hardness of nickel-graphite deposits was found to decrease with graphite content in the as-deposited and heat treated condition. The frictional and wear properties of electroless nickel-graphite were studied and compared to those of electroless nickel-PTFE. The self-lubricating nature of both coatings was found to be dependent on the ratio of coated area to uncoated area, the size and content of lubricating material in the deposit, and the load between contacting surfaces. The mechanism of self-lubrication was considered, concluding that graphite only produced an initial lubricating surface due to the orientation of flakes, unlike PTFE, which produced true self-lubrication throughout the coating life. Heat treatment of electroless nickel chromium deposits at 850oC for 8 and 16 hours produced nickel-iron-chromium alloy deposits with a phosphorus rich surface of high hardness. Coefficients of friction and wear rates were intially moderate for the phosphorus rich layer but increased for the nickel-iron-chromium region of the coating.

The behaviour of antioxidants in polyolefins under conditions of U.V. exposure

The effects of antioxidants and stabilizers on the oxidative degradation of polyolefins (low density polyethylene [LDPE] and polypropylene [PPJ have been studied after subjecting to prior high temperature processing treatments. The changes in the both chemical and physical properties of unstabilized polymers occurring during processing were found to be strongly dependent on the amount of oxygen present in the mixer. Subsequent thermal and photo-oxidation showed very similar characteristics and the chromophore primarily responsible for:both thermo and photooxidative degradation of unstabilized polymers was found to be hydroperoxide formed during processing. Removal of hydroperoxide by heat treatment in an inert atmosphere although increasing ketonic carbonyl concentration, markedly decreased the rate of photo-oxidation, introducing an induction period similar to that of an unprocessed sample. It was concluded that hydroperoxides are the most important initiators in normally processed polymers during the early stages of photo-oxidation. Antioxidants such as metal dithiocarbamates which act by destroying peroxides into non-radica1 products were found to be efficient melt stabilizers for polyolefins and effective UV stabilizers during the initial photo-oxidation stage, whilst a phenolic antioxidant, n-octadecyl-3-(3',5'-di-terbutyl 4'hydroxypheny1) propionate (Irganox 1076) retarded photo-oxidation rate in the later stages. A typical 'UV absorber' 2-hydroxy-4-octyloxy-benzophenone (HOBP) has a minor thermal antioxidant action but retarded photo-oxidation at all stages. A substituated piperidine derivative, Bis [2.2.6.6-tetramethylpiperidlnyl-4] sebacate (Tinuvin 770) behaved as an pro-oxidant during thermal oxidation of polyolefins but was an effective stabilizer against UV light. The UV absorber, HOBP synergised effectively with both peroxide decomposing antioxidants (metal dithiocarbamates) and a chain-breaking antioxidant (Irganox 1076) during photo-oxidation of the poymers studed whereas the combined effect was additive during thermal oxidation. By contrast, the peroxide decornposers and chain-breaking antioxidant (Irganox 1076) which were effective synergists during thermal oxidation of LDPE· were antagonistic during photo-oxidation. The mechanisms of these processes are discussed.

The behaviour of polymer quenchants

The internationally accepted Wolfson Heat Treatment Centre Engineering Group test was used to evaluate the cooling characteristics of the most popular commercial polymer quenchants: polyalkylene glycols, polyvinylpyrrolidones and polyacrylates. Prototype solutions containing poly(ethyloxazoline) were also examined. Each class of polymer was capable of providing a wide range of cooling rates depending on the product formulation, concentration, temperature, agitation, ageing and contamination. Cooling rates for synthetic quenchants were generally intermediate between those of water and oil. Control techniques, drag-out losses and response to quenching in terms of hardness and residual stress for a plain carbon steel, were also considered. A laboratory scale method for providing a controllable level of forced convection was developed. Test reproducibility was improved by positioning the preheated Wolfson probe 25mm above the geometric centre of a 25mm diameter orifice through which the quenchant was pumped at a velocity of 0.5m/s. On examination, all polymer quenchants were found to operate by the same fundamental mechanism associated with their viscosity and ability to form an insulating polymer-rich-film. The nature of this film, which formed at the vapour/liquid interface during boiling, was dependent on the polymer's solubility characteristics. High molecular weight polymers and high concentration solutions produced thicker, more stable insulating films. Agitation produced thinner more uniform films. Higher molecular weight polymers were more susceptible to degradation, and increased cooling rates, with usage. Polyvinylpyrrolidones can be cross-linked resulting in erratic performance, whilst the anionic character of polyacrylates can lead to control problems. Volatile contaminants tend to decrease the rate of cooling and salts to increase it. Drag-out increases upon raising the molecular weight of the polymer and its solution viscosity. Kinematic viscosity measurements are more effective than refractometer readings for concentration control, although a quench test is the most satisfactory process control method.

The preparation of carbon fibres: a study of the physics and chemistry of the preparation of carbon fibres from acrylic precursors

High strength, high modulus carbon fibres are becoming increasingly important as high performance engineering materials. This thesis describes how they may be prepared by heat treatment from filaments spun from polyacrylonitrile and its copolymers. The chemistry of the first stages of heat treatment is very important in controlling the mechanical properties of the carbonised product. A cyclisation reaction has been found to be responsible for the relatively high thermal stability of pyrolysed polyacrylonitrile, but without oxidation the fibres degrade and fuse. An initial oxidation stage is, therefore, essential to the preparation of fibre of high orientation. The cyclised product of pyrolysis is probably a poly 1,4 dihydropiridine and oxidation converts this to aromatic structures, and cyclised structures containing carbonyl and other oxygenated groups. Oxidation is found to assist the carbon fibre preparation process, by producing a product which condenses at an earlier stage of heat treatment, before fusion can occur. Carbon fibre strength and modulus are dependent upon producing a highly oriented crystal structure. While oxidation of the polymer stabilises the fibre so as to prevent disorientation, further large increases in orientation, with a commensurate improvement in strength and modulus, can be obtained by stretching at temperatures above 1,700 °C. This process is analogous to the way fibre orientation is increased by the stretching of the precursor. A lamellar graphite structure can be created in high temperature fibre, by carefully controlling the degree of oxidation. This type of graphite can produce very high values of Young's modulus. More often, however, graphite fibre has a fibrillar fine structure, which is explicable in terms of continuous graphite ribbons. A ribbon model is the most satisfactory representation of the structure of carbon fibre, as it explains the mechanism of the development of long range order and the variation of Young's modulus with crystalline preferred orientation.

Study of the deposition, properties and applications of electroless deposits containing particles

The deposition efficiencies of a number of electroless nickel and cobalt plating solutions were studied and in the case of nickel compared with a commercial plating solution Nifoss 80. At the optimum plating conditions (92ºC and pH 4.5) Nifoss 80 produced nickel layers most efficiently, the alkaline cobalt solution operated most efficiently at 90ºC and pH 9. The methods of producing compostte layers containing 2-3 µm carbide particles and chromium powder is described. Nickel and cobalt layers containing approximately 27% carbide particles, or 40% (Ni) and 30% (Co) chromium particles by volume were obtained. This value is independent of the particle concentration in the plating solution within the range (20~200 g/l). Hardness of the nickel. as deposited was 515 Hv, this was increased to a maximum of 1155 Hv by heat treatment at 200ºC for 5 hours in vacuum. Incorporation. of .chromium carbide particles resulted in a maximum hardness of 1225 Hv after heating at 500ºC for 5 hours in vacuum and chromium particles resulted in a maximum hardness of 16S0 Hv after heat treatment at 400ºC for 2 hours in vacuum. Similarly the hardness of cobalt as deposited was 600 Hv, this was increased to a maximum of 1300 Hv after heat treatment at 400ºC for 1 hour. Incorporation of chromium carbide particles resulted jn a maximum hardness of 1405 Hv after heating at 400ºC for 5 hours in vacuum and chromium particles resulted in a maximum hardness of 1440 Hv after. heat treating for 2 hours at 400ºC in vacuum. The structure of the deposits was studied by optical and scanning electron microscopy. The wear rate and coefficient of friction was determined by a pin and disc method. Wear rate and coefficient of friction decreased with increase in hardness. The wear resistance of the materials was also determined using a simulated forging test. Dies made of standard die steel were coated and the wear rates of the layers as deposited and after heat treatment were compared with those of uncoated tools. The wear resistance generally increased with hardness, it was 50-75% more than the uncoated die steel. Acetic acid salt spray test and outdoor exposure for six months was used to study the corrosion behaviour of the deposits and potentiodynamic curves plotted to find their corrosion potential. Nickel deposit exhibited less staining than carbide composite deposits and nickel-chromium deposits had the most noble corrosion potential.

Wear of abrasion resisting materials

The wear behaviour of a series of chromium containing white irons has been investigated under conditions of high stress grinding abrasion using a specimen on track abrasion testing machine. The measured abrasion resistance of the irons has been explained in terms of microstructure and hardness and with respect to the wear damage observed at and beneath abraded surfaces. During abrasion material removal occurred by cracking and detachment from the matrix of eutectic carbides as well as by penetration and micromachining effects of the abrasive grits being crushed at the wearing surface. Under the particular test conditions used martensitic matrix structures gave higher resistance to abrasion than austenitic or pearlitic. However, no simple relationship was found between general hardness or matrix microhardness at wear surfaces and abrasion resistance, and the test yielded pessimistic results for austenitic irons. The fine structures of the 15% Cr and 30% Cr alloys were studied by thin foil transmission electron microscopy. It was found that both the matrix and carbide constituents could be thinned for examination at 100 Kv using conventional dishing followed by ion beam thinning. Flany of the rodlike eutectic N7C3 carbides were seen to consist of clusters of scalier rods with individual 117C3 crystals quite often containing central cores of matrix constituent. 3oth eutectic and secondary N7C3 carbides were found to contain stacking faults on planes normal to the basal plane. In the eutectic carbides in the 30A Cr iron there was evidence of an in-situ PI7C3 C. transition which had taken place during the hardening heat treatment of this alloy. In the as-cast austenitic matrix iron strain induced martensite was produced at the wear surface contributing to work hardening. The significance of these findings have been discussed in relation to wear performance.