Search results for: recrystallized

Authors: Mousa Bani Baker, Raed Abendeh, Zaidoon Abu Salem, Hesham Ahmad

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This research paper was commissioned to discuss the Jordanian marble, which is a non-foliated metamorphic rock composed of recrystallized carbonate minerals, most commonly calcite or dolomite. Geologists use the term "marble" to refer to metamorphosed limestone; however, stonemasons use the term more broadly to encompass unmetamorphised limestone. Marble is commonly used for sculpture and as a building material. The marble has many uses; one of them is using the white marble that has been prized for its use in sculptures since classical times. This preference has to do with its softness, relative isotropy and homogeneity, and a relative resistance to shattering. Another use of it is the construction marble which is “a stone which is composed of calcite, dolomite or serpentine which is capable of taking a polish” Marble Institute of America. This report focuses most about the marble in Jordan and its properties: rock definition, physical properties, the marble occurrences in Jordan, types of Jordanian marble and their prices and test done on this marble.

Keywords: marble, metamorphic, non-foliated, compressive strength, recrystallized, Moh’s hardness, abrasion, absorption, modulus of rupture, porosity

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Authors: Wen-Hsi Lee, C.G. Kao

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In this study, Cu paste was prepared and printed with narrow line screen printing process on polycrystalline Si solar cell which has already finished the back Al printing and deposition of double anti-reflection coatings (DARCs). Then, two-step firing process was applied to sinter the front electrode and obtain the ohmic contact between front electrode and solar cell. The first step was in air atmosphere. In this process, PbO-based glass frit etched the DARCs and Ag recrystallized at the surface of Si, constructing the preliminary contact. The second step was in reducing atmosphere. In this process, CuO reduced to Cu and sintered. Besides, Ag nanoparticles recrystallized in the glass layer at interface due to the interactions between H2, Ag and PbO-based glass frit and the volatility of Pb, constructing the ohmic contact between electrode and solar cell. By experiment and analysis, reaction mechanism in each stage was surmised, and it was also proven that ohmic contact and good sheet resistance for front electrode could both be obtained by applying newly-invented paste and process.

Keywords: front electrode, solar cell, ohmic contact, screen printing, paste

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Authors: M. Ghosh, A. Miroux, L. A. I. Kestens

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At molecular or micrometre scale, practically all materials are neither homogeneous nor isotropic. The concept of texture is used to identify the structural features that cause the properties of a material to be anisotropic. For metallic materials, the anisotropy of the mechanical behaviour originates from the crystallographic nature of plastic deformation, and is therefore controlled by the crystallographic texture. Anisotropy in mechanical properties often constitutes a disadvantage in the application of materials, as it is often illustrated by the earing phenomena during drawing. However, advantages may also be attained when considering other properties (e.g. optimization of magnetic behaviour to a specific direction) by controlling texture through thermo-mechanical processing). Nevertheless, in order to have better control over the final properties it is essential to relate texture with materials processing route and subsequently optimise their performance. However, up to date, few studies have been reported about the evolution of texture in 6061 aluminium alloy during warm processing (from room temperature to 250ºC). In present investigation, recrystallized 6061 aluminium alloy samples were subjected to tensile and plane strain compression (PSC) at room and warm temperatures. The gradual change of texture following both deformation modes were measured and discussed. Tensile tests demonstrate the mechanism at low strain while PSC does the same at high strain and eventually simulate the condition of rolling. Cube dominated texture of the initial rolled and recrystallized AA6061 sheets were replaced by domination of S and R components after PSC at room temperature, warm temperature (250ºC) though did not reflect any noticeable deviation from room temperature observation. It was also noticed that temperature has no significant effect on the evolution of grain morphology during PSC. The band contrast map revealed that after 30% deformation the substructure inside the grain is mainly made of series of parallel bands. A tendency for decrease of Cube and increase of Goss was noticed after tensile deformation compared to as-received material. Like PSC, texture does not change after deformation at warm temperature though. n-fibre was noticed for all the three textures from Goss to Cube.

Keywords: AA 6061, deformation, temperature, tensile, PSC, texture

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Authors: Seok Hong Min, Tae Kwon Ha

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In the present study, hot-rolled sheets of Mg-xZn alloy s(x=6, 8, and 10 weight percent) were produced by employing casting, homogenization heat treatment, hot rolling, and annealing processes subsequently. Effect of Zn addition on the microstructure and mechanical properties of Mg-Zn alloys were also investigated in each process. Through calculation of phase equilibria of Mg-Zn alloys, solution treatment temperature was decided as temperatures from 350 oC, where supersaturated solid solution can be obtained. After solution treatment, hot rolling was successfully conducted by reduction of 60%. Compression and tension tests were carried out at room temperature on the samples as-cast, solution treated, hot-rolled and recrystallized after rolling.

Keywords: Mg-Zn alloy, heat treatment, microstructure, mechanical properties, hot rolling

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Authors: Veeresham Mokali

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Recrystallization microstructure and grain growth studies of Ta₀.₅Nb₀.₅Hf₀.₅ZrTi₁.₅ refractory high entropy alloy have been explored in the present work. The as-cast Ta₀.₅Nb₀.₅Hf₀.₅ZrTi₁.₅ alloy was cold-rolled to 90% in several passes at room temperature and further subjected to annealing treatment for recrystallization at 800°C, 1000°C, 1250°C, and 1400°C temperatures for one hour. However, the characterization of heavily cold-rolled and annealed condition specimens was done using scanning electron microscopy (SEM-EBSD). The cold-rolled specimens showed the development of an inhomogeneous microstructure. Upon annealing, recrystallized microstructures were achieved; in addition to that, the coarsening of microstructure with raising annealing temperature noticed in the range of 800°C – 1400°C annealed temperatures.

Keywords: refractory high entropy alloys, cold-rolling, recrystallization, microstructure

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Authors: Young Sik Kim, Tae Kwon Ha

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Effect of Zn addition on the microstructure and mechanical properties of Mg-Zn alloys with Zn contents from 6 to 10 weight percent was investigated in this study. Through calculation of phase equilibria of Mg-Zn alloys, carried out by using FactSage® and FTLite database, solution treatment temperature was decided as temperatures from 300 to 400oC, where supersaturated solid solution can be obtained. Solid solution treatment of Mg-Zn alloys was successfully conducted at 380oC and supersaturated microstructure with all beta phase resolved into matrix was obtained. After solution treatment, hot rolling was successfully conducted by reduction of 60%. Compression and tension tests were carried out at room temperature on the samples as-cast, solution treated, hot-rolled and recrystallized after rolling. After solid solution treatment, each alloy was annealed at temperatures of 180 and 200oC for time intervals from 1 min to 48 hrs and hardness of each condition was measured by micro-Vickers method. Peak aging conditions were deduced as at the temperature of 200oC for 10 hrs. By addition of Zn by 10 weight percent, hardness and strength were enhanced.

Keywords: Mg-Zn alloy, heat treatment, microstructure, mechanical properties, hardness

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Authors: Jiří Kubásek, Peter Minárik, Klára Hosová, Stanislav Šašek, Jozef Veselý, Jitka Stráská, Drahomír Dvorský, Dalibor Vojtěch, Miloš Janeček

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Mg-2Y-2Gd-1Ca and Mg-4Y-4Gd-2Ca alloys were processed by extrusion or equal channel angular pressing (ECAP) to analyse the effect of the microstructure on ignition temperature, mechanical properties and corrosion resistance. The alloys are characterized by good mechanical properties and exceptionally high ignition temperature, which is a critical safety measure. The effect of extrusion and ECAP on the microstructure, mechanical properties and ignition temperature was studied. The obtained results indicated a substantial effect of the processing conditions on the average grain size, the recrystallized fraction and texture formation. Both alloys featured a high strength, depending on the composition and processing condition, and a high ignition temperature of ≈1100 °C (Mg-4Y-4Gd-2Ca) and ≈950 °C (Mg-2Y-2Gd-1Ca), which was attributed to the synergic effect of Y, Gd and Ca oxides, with the dominant effect of Y₂O₃. The achieved combination of enhanced mechanical properties and the ignition temperature makes these alloys a prominent candidate for aircraft applications.

Keywords: magnesium alloys, enhanced ignition temperature, mechanical properties, ECAP

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Authors: Linyue Jia, Wenbo Du, Zhaohui Wang, Ke Liu, Shubo Li

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Due to the great potential for weight reduction in aerospace and automotive industries, magnesium-rare earth (Mg-RE) based alloys with outstanding mechanical performance have been widely investigated for decades. However, magnesium alloys are still restricted in engineering applications because of their lower strength and ductility. Hence, there are large spaces and challenges in achieving high-performance Mg alloys. This work reports an Mg-Gd-Er-Zn-Zr alloy with ultrahigh strength and good ductility developed via hot extrusion, pre-deformation, and two-stage aging. The extruded alloy comprises fine dynamically recrystallized (DRXed) grains and coarse worked grains with a large aspect ratio. Pre-deformation has little effect on the microstructure and macro-texture and serves primarily to introduce a large number of dislocations, resulting in strain hardening and higher precipitation strengthening during subsequent aging due to more nucleation sites. As a result, the alloy exhibits a yield strength (YS) of 506 MPa, an ultimate tensile strength (UTS) of 549 MPa, and elongation (EL) of 8.2% at room temperature, showing superior strength-ductility balance than the other wrought Mg-RE alloys previously reported. The current study proposes a combination of pre-deformation and two-stage aging to further improve the mechanical properties of wrought Mg alloys for engineering applications.

Keywords: magnesium alloys, mechanical properties, microstructure, pre-deformation, two-stage aging

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Authors: Saliha Gachi, Mouloud Aissani, Fouad Boubenider

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Friction Stir Welding (FSW) is a solid-state welding technique that can join material without melting the plates to be welded. In this work, we are interested to demonstrate the potentiality of FSW for joining the heat-treatable aluminum alloy 2024-T3 which is reputed as difficult to be welded by fusion techniques. Thereafter, the FSW joint is compared with another one obtained from a conventional fusion process Tungsten Inert Gas (TIG). FSW welds are made up using an FSW tool mounted on a milling machine. Single pass welding was applied to fabricated TIG joint. The comparison between the two processes has been made on the temperature evolution, mechanical and microstructure behavior. The microstructural examination revealed that FSW weld is composed of four zones: Base metal (BM), Heat affected zone (HAZ), Thermo-mechanical affected zone (THAZ) and the nugget zone (NZ). The NZ exhibits a recrystallized equiaxed refined grains that induce better mechanical properties and good ductility compared to TIG joint where the grains have a larger size in the welded region compared with the BM due to the elevated heat input. The microhardness results show that, in FSW weld, the THAZ contains the lowest microhardness values and increase in the NZ; however, in TIG process, the lowest values are localized on the NZ.

Keywords: friction stir welding, tungsten inert gaz, aluminum, microstructure

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Authors: Yebeen Ji, Jimin Yun, Kwonhoo Kim

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Magnesium alloys were limited for industrial applications due to having a limited slip system and high plastic anisotropy. It has been known that specific textures were formed during processing (rolling, etc.), and These textures cause poor formability. To solve these problems, many researchers have studied controlling texture by adding rare-earth elements. However, the high cost limits their use; therefore, alternatives are needed to replace them. Although Pb addition doesn’t directly improve magnesium properties, it has been known to suppress the diffusion of other alloying elements and reduce grain boundary energy. These characteristics are similar to the additions of rare-earth elements, and a similar texture behavior is expected as well. However, there is insufficient research on this. Therefore, this study investigates the behavior of texture and microstructure development after adding Pb to magnesium. This study compared and analyzed AZ61 alloy and Mg-15wt%Pb alloy to determine the effect of adding solute elements. The alloy was hot rolled and annealed to form a single phase and initial texture. Afterward, the specimen was set to contraction and elongate parallel to the rolling surface and the rolling direction and then subjected to high-temperature plane strain compression under the conditions of 723K and 0.05/s. Microstructural analysis and texture measurements were performed by SEM-EBSD. The peak stress in the true strain-stress curve after compression was higher in AZ61, but the shape of the flow curve was similar for both alloys. For both alloys, continuous dynamic recrystallization was confirmed to occur during the compression process. The basal texture developed parallel to the compressed surface, and the pole density was lower in the Mg-15wt%Pb alloy. It is confirmed that this change in behavior is because the orientation distribution of recrystallized grains has a more random orientation compared to the parent grains when Pb is added.

Keywords: Mg, texture, Pb, DRX

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Authors: Da-Wei Wang, Liang Yang, Xuan-Long Peng, Mei-Chuan Kuo, Jen-Taut Yeh

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The tensile retention and waterproof properties of thermoplastic starch (TPS) resins were significantly enhanced by modifying with proper amounts of citric acid (CA) and by melt-blending with poly(lactic acid) (PLA), although no distinguished chemical reaction occurred between CA and starch molecules. As evidenced by Fourier transform infrared spectroscopy and Solid-state 13C Nuclear Magnetic Resonance analyses, disruption of intra and interhydrogen-bondings within starch molecules did occur during the modification processes of CA modified TPS (i.e. TPS100CAx) specimens. The tensile strength (σf) retention values of TPS specimens reduced rapidly from 27.8 to 20.5 and 0.4 MPa, respectively, as the conditioning time at 20°C/50% relative humidity (RH) increased from 0 to 7 and 70 days, respectively. While the elongation at break (εf) retention values of TPS specimens increased rapidly from 5.9 to 6.5 and 34.8%, respectively, as the conditioning time increased from 0 to 7 and 70 days. After conditioning at 20°C/50% RH for 70 days, the σf and εf retention values of the best prepared (TPS100CA0.1)30PLA70 specimen are equivalent to 85% and 167% of its initial σf and εf values, respectively, and are more than 105 times higher but 48% lower than those of TPS specimens conditioned at 20°C/50% RH for the same amount of time. Demarcated diffraction peaks, new melting endotherms of recrystallized starch crystals and distinguished ductile characteristics with drawn debris were found for many conditioned TPS specimens, however, only slight retrogradation effect and much less drawn debris was found for most conditioned TPS100CAx and/or (TPS100CA0.1)xPLAy specimens. The significantly improved water proof, tensile retention properties and relatively unchanged in retrogradation effect found for most conditioned TPS100CAx and/or (TPS100CA0.1)xPLAy specimens are apparently due to the efficient blocking of the moisture-absorbing hydroxyl groups (free or hydrogen bonded) by hydrogen-bonding CA with starch molecules during their modification processes.

Keywords: thermoplastic starch, hydrogen-bonding, water proof, strength retention

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Authors: Muhammad Nawaz, Waqas Ahmad

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Dimension stone is used in construction since prehistoric time; however, its use in the construction has gained significant attention for the last few decades. The present study is designed to investigate the physical and strength properties of volcanic rocks from the Kohistan Island Arc to assess their use as dimension stone. On the basis of the composition, color and texture, five varieties of andesites (MMA, PMA-1, PMA-2, CMA and FMA) and two varieties of agglomerates (AG-1 and AG-2) were identified. These were characterized in terms of their petrography (compositional and textural), physical properties (specific gravity, water absorption, porosity) and strength properties (Unconfined compressive strength and Unconfined tensile strength). Two non-destructive tests (Ultrasonic pulse velocity test and Schmidt Hammer) were conducted and the degree of polishing was evaluated. In addition, correlation analyses were carried out to establish possible relationships among these parameters. The presence of chlorite, epidote, sericite and recrystallized quartz showed the signs of low-grade metamorphism in andesites. The results showed feldspar, amphibole and quartz imparted good physical and strength properties to the samples MMA, CMA, FMA, AG1 and AG2. Whereas, the abundance of alteration products such as chlorite, sericite and epidote in PMA-1 and PMA-2 reduced the physical and strength properties. The unconfined compressive strength showed a strong correlation with ultrasonic pulse velocity, dry density, porosity and water absorption. The values of ultrasonic pulse velocity and Schmidt hammer were considerably affected by the weathering grade. The samples PMA-1 and PMA-2, due to their high water absorption and low strength values, were not recommended for use in load-bearing masonry units and outdoor applications. Whereas, the excellent properties, i.e. high strength and good polishing, the samples, FMA and MMA suggested their use as a decorative and facing stone, in the external pavement, ashlar, rubbles and load-bearing masonry units etc.

Keywords: Physico-mechanical properties, Volcanic rocks, Kohistan Island Arc, Pakistan

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Authors: Soumyajit Koley, Kuladeep Rajamudili, Supriyo Ganguly

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In recent years, iron-based shape-memory alloys have been emerging as an inexpensive alternative to costly Ni-Ti alloy and thus considered suitable for many different applications in civil structures. Fe-17Mn-10Cr-5Si-4Ni-0.5V-0.5C alloy contains 37 wt.% of total solute elements. Such complex multi-component metallurgical system often leads to severe solute segregation and solidification cracking. Wire-arc additive manufacturing (WAAM) of Fe-17Mn-10Cr-5Si-4Ni-0.5V-0.5C alloy was attempted using a cold-wire fed plasma arc torch attached to a 6-axis robot. Self-standing walls were manufactured. However, multiple vertical cracks were observed after deposition of around 15 layers. Microstructural characterization revealed open surfaces of dendrites inside the crack, confirming these cracks as solidification cracks. Machine hammer peening (MHP) process was adopted on each layer to cold work the newly deposited alloy. Effect of MHP traverse speed were varied systematically to attain a window of operation where cracking was completely stopped. Microstructural and textural analysis were carried out further to correlate the peening process to microstructure.MHP helped in many ways. Firstly, a compressive residual stress was induced on each layer which countered the tensile residual stress evolved from solidification process; thus, reducing net tensile stress on the wall along its length. Secondly, significant local plastic deformation from MHP followed by the thermal cycle induced by deposition of next layer resulted into a recovered and recrystallized equiaxed microstructure instead of long columnar grains along the vertical direction. This microstructural change increased the total crack propagation length and thus, the overall toughness. Thirdly, the inter-layer peening significantly reduced the strong cubic {001} crystallographic texture formed along the build direction. Cubic {001} texture promotes easy separation of planes and easy crack propagation. Thus reduction of cubic texture alleviates the chance of cracking.

Keywords: Iron-based shape-memory alloy, wire-arc additive manufacturing, solidification cracking, inter-layer cold working, machine hammer peening

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Authors: Rajkumar Ghosh

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Jhakri Thrust (JT) coeval of Sarahan Thrust (ST) was later considered to be part of Chaura Thrust (CT). The Main Central Thrust (MCT) delimits the southern extreme of Higher Himalaya, whereas the northern boundary defines by South Tibetan Detachment System (STDS). STDS is parallel set of north dipping extensional faults. The activation timing of MCT and STDS. MCT activated in two parts (MCT-L during 15- 0.7 Ma, and MCT-U during 25-14 Ma). Similarly, STDS triggered in two parts (STDS-L during 24-12 Ma, and STDS-U during 19-14 Ma). The activation ages for MBT and MFT. Besides, the MBT occurred during 11-9 Ma, and MFT followed as <2.5 Ma. There are two mylonitised zones (zone of S-C fabric) found under the microscope. Dynamic and bulging recrystallization and sub-grain formation was documented under the optical microscope from samples collected from these zones. The varieties of crenulated schistosity are shown in photomicrographs. In a rare and uncommon case, crenulation cleavage and sigmoid Muscovite were found together side-by-side. Recrystallized quartzo-feldspathic grains exist in between crenulation cleavages. These thin-section studies allow three possible hypotheses for such variations in crenulation cleavages. S/SE verging meso- and micro-scale box folds around Chaura might be a manifestation of some structural upliftment. Near Chaura, kink folds are visible. Prominent asymmetric shear sense indicators in augen mylonite are missing in meso-scale but dominantly present under the microscope. The main foliation became steepest (range of dip ~ 65 – 80 º) at this place. The aim of this section is to characterize the box fold and its signature in the regional geology of Himachal Himalaya. Grain Boundary Migration (GBM) associated temperature range (400–750 ºC) from microstructural studies in grain scale along Jhakri-Wangtu transect documented. Oriented samples were collected from the Jhakri-Chaura transect at a regular interval of ~ 1km for strain analysis. The Higher Himalayan Out-of-Sequence Thrust (OOST) in Himachal Pradesh is documented a decade ago. The OOST in other parts of the Himalayas is represented as a line in between MCTL and MCTU. But In Himachal Pradesh area, OOST activated the MCTL as well as in between a zone located south of MCTU. The expectations for strain variation near the OOST are very obvious. But multiple sets of OOSTs may produce a zigzag pattern of strain accumulation for this area and figure out the overprinting structures for multiple sets of OOSTs.

Keywords: Chaura Thrust, out-of-sequence thrust, Main Central Thrust, Sarahan Thrust

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Authors: Michalina Aniola, Andrzej Katrusiak

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4,4-Bipyridine is an important compound often used in chemical practice and more recently frequently applied for designing new metal organic framework (MoFs). Here we present a systematic high-pressure study of its hydrobromide salt. 4,4-Bipyridine hydrobromide monohydrate, 44biPyHBrH₂O, at ambient-pressure is orthorhombic, space group P212121 (phase a). Its hydrostatic compression shows that it is stable to 1.32 GPa at least. However, the recrystallization above 0.55 GPa reveals a new hidden b-phase (monoclinic, P21/c). Moreover, when the 44biPyHBrH2O is heated to high temperature the chemical reactions of this compound in methanol solution can be observed. High-pressure experiments were performed using a Merrill-Bassett diamond-anvil cell (DAC), modified by mounting the anvils directly on the steel supports, and X-ray diffraction measurements were carried out on a KUMA and Excalibur diffractometer equipped with an EOS CCD detector. At elevated pressure, the crystal of 44biPyHBrH₂O exhibits several striking and unexpected features. No signs of instability of phase a were detected to 1.32 GPa, while phase b becomes stable at above 0.55 GPa, as evidenced by its recrystallizations. Phases a and b of 44biPyHBrH2O are partly isostructural: their unit-cell dimensions and the arrangement of ions and water molecules are similar. In phase b the HOH-Br- chains double the frequency of their zigzag motifs, compared to phase a, and the 44biPyH+ cations change their conformation. Like in all monosalts of 44biPy determined so far, in phase a the pyridine rings are twisted by about 30 degrees about bond C4-C4 and in phase b they assume energy-unfavorable planar conformation. Another unusual feature of 44biPyHBrH2O is that all unit-cell parameters become longer on the transition from phase a to phase b. Thus the volume drop on the transition to high-pressure phase b totally depends on the shear strain of the lattice. Higher temperature triggers chemical reactions of 44biPyHBrH2O with methanol. When the saturated methanol solution compound precipitated at 0.1 GPa and temperature of 423 K was required to dissolve all the sample, the subsequent slow recrystallization at isochoric conditions resulted in disalt 4,4-bipyridinium dibromide. For the 44biPyHBrH2O sample sealed in the DAC at 0.35 GPa, then dissolved at isochoric conditions at 473 K and recrystallized by slow controlled cooling, a reaction of N,N-dimethylation took place. It is characteristic that in both high-pressure reactions of 44biPyHBrH₂O the unsolvated disalt products were formed and that free base 44biPy and H₂O remained in the solution. The observed reactions indicate that high pressure destabilized ambient-pressure salts and favors new products. Further studies on pressure-induced reactions are carried out in order to better understand the structural preferences induced by pressure.

Keywords: conformation, high-pressure, negative area compressibility, polymorphism

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Authors: Nivedita T. Patil, M. T. Patil, M. S. Shashidhar, R. G. Gonnade

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Cyclitols are cycloalkane polyols which have raise attention since they have numerous biological and pharmaceutical properties. Among these, inositols are important cyclitols, which constitute a group of naturally occurring polyhydric alcohols. Myo, scyllo, allo, neo, D-chiro- are naturally occurring structural isomer of inositol while other four isomers (L-chiro, allo, epi-, and cis-inositol) are derived from myo-inositol by chemical synthesis. Myo-inositol, most abundant isomer, plays an important role in signal transduction process and for the treatment of type 2 diabetes, bacterial infections, stimulation of menstruation, ovulation in polycystic ovary syndrome, improvement of osteogenesis, and in treatment of neurological disorders. Considering the vast application of the derivatives, it becomes important to supply these compounds for further studies in quantitative amounts, but the synthesis of suitably protected chiral inositol derivatives is the key intermediates in most of the synthesis which is difficult. Chiral inositol derivatives could also be of interest to synthetic organic chemists as they could serve as potential starting materials for the synthesis of several natural products and their analogs. Thus, obtaining chiral myo-inositol derivatives in a more eco-friendly way is need for current inositol chemistry. Thus, the resolution of nonracemates by preferential crystallization of enantiomers has not been reported as a method for inositol derivatives. We are optimistic that this work might lead to the development of the two tosylate enantiomers as synthetic chiral pool molecules for organic synthesis. Resolution of racemic 4-O-benzyl 6-O-tosyl myo-inositol 1, 3, 5 orthoformate was successfully achieved on multigram scale by preferential crystallization, which is more scalable, eco-friendly method of separation than other reported methods. The separation of the conglomeric mixture of tosylate was achieved by suspending the mixture in ethyl acetate till the level of saturation is obtained. To this saturated clear solution was added seed crystal of the desired enantiomers. The filtration of the precipitated seed was carried out at its filtration window to get enantiomerically enriched tosylate, and the process was repeated alternatively. These enantiomerically enriched samples were recrystallized to get tosylate as pure enantiomers. The configuration of the resolved enantiomers was determined by converting it to previously reported dibenzyl ether myo-inositol, which is an important precursor for mono- and tetraphosphates. We have also developed a convenient and practical method for the preparation of enantiomeric 4-O and 6-O-allyl myo-inositol orthoesters by resolution of diastereomeric allyl dicamphante orthoesters on multigram scale. These allyl ethers can be converted to other chiral protected myo-inositol derivatives using routine synthetic transformations. The chiral allyl ethers can be obtained in gram quantities, and the methods are amenable to further scale-up due to the simple procedures involved. We believe that the work described enhances the pace of research to understand the intricacies of the myo-inositol cycle as the methods described provide efficient access to enantiomeric phosphoinositols, cyclitols, and their derivatives from the abundantly available myo-inositol as a starting material.

Keywords: cyclitols, diastereomers, enantiomers, myo-inositol, preferential crystallization, signal transduction

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Authors: Marcos Perez, Christian Dumont, Olivier Nodin, Sebastien Nouveau

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Nickel superalloys are used to manufacture high-temperature rotary engine parts such as high-pressure disks in gas turbine engines. High strength at high operating temperatures is required due to the levels of stress and heat the disk must withstand. Therefore it is necessary parts made from materials that can maintain mechanical strength at high temperatures whilst remain comparatively low in cost. A manufacturing process referred to as the triple melt process has made the production of cast and wrought (C&W) nickel superalloys possible. This means that the balance of cost and performance at high temperature may be optimized. AD730TM is a newly developed Ni-based superalloy for turbine disk applications, with reported superior service properties around 700°C when compared to Inconel 718 and several other alloys. The cast ingot is converted into billet during either cogging process or open die forging. The semi-finished billet is then further processed into its final geometry by forging, heat treating, and machining. Conventional ingot-to-billet conversion is an expensive and complex operation, requiring a significant amount of steps to break up the coarse as-cast structure and interdendritic regions. Due to the size of conventional ingots, it is difficult to achieve a uniformly high level of strain for recrystallization, resulting in non-recrystallized regions that retain large unrecrystallized grains. Non-uniform grain distributions will also affect the ultrasonic inspectability response, which is used to find defects in the final component. The main aim is to analyze the recrystallization behavior and microstructural evolution of AD730 at subsolvus temperatures from a semi-finished product (billet) under conditions representative of both cogging and hot forging operations. Special attention to the presence of large unrecrystallized grains was paid. Double truncated cones (DTCs) were hot forged at subsolvus temperatures in hydraulic press, followed by air cooling. SEM and EBSD analysis were conducted in the as-received (billet) and the as-forged conditions. AD730 from billet alloy presents a complex microstructure characterized by a mixture of several constituents. Large unrecrystallized grains present a substructure characterized by large misorientation gradients with the formation of medium to high angle boundaries in their interior, especially close to the grain boundaries, denoting inhomogeneous strain distribution. A fine distribution of intragranular precipitates was found in their interior, playing a key role on strain distribution and subsequent recrystallization behaviour during hot forging. Continuous dynamic recrystallization (CDRX) mechanism was found to be operating in the large unrecrystallized grains, promoting the formation intragranular DRX grains and the gradual recrystallization of these grains. Evidences that hetero-epitaxial recrystallization mechanism is operating in AD730 billet material were found. Coherent γ-shells around primary γ’ precipitates were found. However, no significant contribution to the overall recrystallization during hot forging was found. By contrast, strain presents the strongest effect on the microstructural evolution of AD730, increasing the recrystallization fraction and refining the structure. Regions with low level of deformation (ε ≤ 0.6) were translated into large fractions of unrecrystallized structures (strain accumulation). The presence of undissolved secondary γ’ precipitates (pinning effect), prior to hot forging operations, could explain these results.

Keywords: AD730 alloy, continuous dynamic recrystallization, hot forging, γ’ precipitates

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