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Methodology for Mechanical Property Testing on Fuel Cladding Using an Expanded Plug Wedge Test

To determine the tensile properties of irradiated fuel cladding in a hot cell, a simple test was developed at ORNL and is described fully in US Patent Application 20060070455, Expanded plug method for developing circumferential mechanical properties of tubular materials. This method is designed for testing fuel rod cladding ductility in a hot cell utilizing an expandable plug to stretch a small ring of irradiated cladding material. The specimen strain is determined using the measured diametrical expansion of the ring. This method removes many complexities associated with specimen preparation and testing. The advantages are the simplicity of measuring the test component assembly in the hot cell and the direct measurement of specimen strain. It was also found that cladding strength could be determined from the test results. The basic approach of this test method is to apply an axial compressive load to a cylindrical plug of polyurethane (or other materials) fitted inside a short ring of the test material to achieve radial expansion of the specimen. The diameter increase of the specimen is used to calculate the circumferential strain accrued during the test. The other two basic measurements are total applied load and amount of plug compression (extension). A simple procedure is used to convert the load circumferential strain data from the ring tests into material pseudo-stress-strain curves. However, several deficiencies exist in this expanded-plug loading ring test, which will impact accuracy of test results and introduce potential shear failure of the specimen due to inherited large axial compressive stress from the expansion plug test. First of all, the highly non-uniform stress and strain distribution resulted in the gage section of the clad. To ensure reliable testing and test repeatability, the potential for highly non-uniform stress distribution or displacement/strain deformation has to be eliminated at the gage section of the specimen. Second, significant compressive stresses were induced by clad bending deformation due to a clad bulging effect (or the barreling effect). The barreling effect caused very large localized shear stress in the clad and left testing material at a high risk of shear failure. The above combined effects will result in highly non-conservative predictions both in strength and ductility of the tested clad, and the associated mechanical properties as well. To overcome/mitigate the mentioned deficiencies associated with the current expansion plug test, systematic studies have been conducted. Through detailed parameter investigation on specific geometry designs, careful filtering of material for the expansion plug, as well as adding newly designed parts to the testing system, a method to reconcile the potential non-conservatism embedded in the expansion plug test system has been discovered. A modified expansion plug testing protocol has been developed based on the method. In order to closely resemble thin-wall theory, a general procedure was also developed to determine the hoop stress $\sigma_\theta$ in the tested ring specimen. A scaling factor called $\chi$-factor is defined to correlate the ring load F ring into hoop stress $\sigma_\theta$, and written as $\sigma_\theta = \chi \frac{F_{ring}} {tl}$. The generated stress-strain curve agrees very well with tensile test data in both the elastic and plastic regions.

expansion plug test↗

High pressure structural study of {beta}-Ti{sub 3}O{sub 5}: X-ray diffraction and Raman spectroscopy

The structural stability of {beta}-Ti{sub 3}O{sub 5} (C2/m) has been investigated by X-ray diffraction and Raman spectroscopy with diamond anvil cells. {beta}-Ti{sub 3}O{sub 5} is stable up to about 26 GPa at room temperature. Isothermal pressure-volume relationship of {beta}-Ti{sub 3}O{sub 5} is well presented by the third-order Birch-Murnaghan equation of state with V{sub 0}=348.6(8) A{sup 3} and B{sub 0}=216(9) GPa. Axial compressibility presents obvious anisotropy. The a-axis and c-axis are more compressible than b-axis due to the different crystal structure arrangement of {beta}-Ti{sub 3}O{sub 5} along b-axis and perpendicular to b-axis direction. The Grueneisen parameters of thirteen observed Raman modes are 0.79-1.74, whose mean is 1.32. - Graphical abstract: The crystal structure of {beta}-Ti{sub 3}O{sub 5}: the projection of {beta}-Ti{sub 3}O{sub 5} along b-axis (Left) and the projection of {beta}-Ti{sub 3}O{sub 5} along c-axis (Right). Highlights: Black-Right-Pointing-Pointer High pressure structural stability of {beta}-Ti{sub 3}O{sub 5} was investigated. Black-Right-Pointing-Pointer {beta}-Ti{sub 3}O{sub 5} is stable up to about 26 GPa. Black-Right-Pointing-Pointer Axial compressibility presents obvious anisotropy. Black-Right-Pointing-Pointer Pressure-volume relationship is well presented by Birch-Murnaghan equation of state. Black-Right-Pointing-Pointer The Grueneisen parameters are 0.79-1.74.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High pressure structure studies of 6H-SrIrO{sub 3} and the octahedral tilting in 3C-SrIrO{sub 3} towards a post-perovskite

The high pressure behaviors of the two perovskite structures (hexagonal 6H-SrIrO{sub 3} and orthorhombic 3C-SrIrO{sub 3}) have been studied in diamond anvil cells to 43 and 60 GPa, respectively, using synchrotron powder X-ray diffraction. 6H-SrIrO{sub 3} was first synthesized at ambient pressure and subsequently transformed into 3C-SrIrO{sub 3} in a large volume press at 8.8 GPa and 1000 °C. Both polymorphs were found to retain the initial symmetry up to the highest pressures measured, but in the case of 6H-SrIrO{sub 3}, two anomalies were identified: a change in the axial compressibilities at 24 GPa and a change in both the axial and volume compressibilities at 32 GPa. Fitting a 3rd order Birch-Murnaghan equation of state to the obtained P-V data yielded bulk moduli of K{sub 0}=151.5(12) GPa (fitted range 0<P<30 GPa) for 6H-SrIrO{sub 3} and K{sub 0}=187.1(9) GPa for 3C-SrIrO{sub 3}. Analysis of the structural parameters for 6H-SrIrO{sub 3} aided by F-f plots suggests the anomalies are caused by changes in the compression mechanism. Comparison of the two polymorphs reveals that 6H-SrIrO{sub 3} becomes less compressible than 3C-SrIrO{sub 3} above 32 GPa as a result of the mechanistic change, and a crossing of their P-V curves is avoided. For 3C-SrIrO{sub 3}, analysis of the octahedral tilt angles shows that these increase monotonically from the ambient value of 7.23(6) to 23.0(2)° at 60 GPa suggesting that a transition to a post-perovskite is approached. - Graphical abstract: The structure of 3C-SrIrO{sub 3} synthesized at high pressure has been studied in a diamond anvil cell and is found to maintain its orthorhombic structure up to 60 GPa but distorts drastically due to octahedral tilting, strongly suggesting that a post-perovskite transition is possible. The compression is compared to 6H-SrIrO{sub 3} synthesized at ambient pressure, which is initially found to be more compressible but undergoes changes in its compression mechanism and 3C remains denser throughout compression. Display Omitted - Highlights: • Structures of 6H- and 3C-SrIrO{sub 3} were studied to pressures of 43 and 60 GPa, respectively. • Both structures maintain the initial symmetry up to the highest pressures measured. • 6H-SrIrO{sub 3} is initially more compressible than 3C-SrIrO{sub 3}. • Due to changes in the compression mechanism in 6H-SrIrO{sub 3} the 3C-SrIrO{sub 3} remains denser throughout. • 3C-SrIrO{sub 3} show large octahedral tilting, strongly suggesting a post-perovskite transition is imminent.

36 MATERIALS SCIENCE↗

Negative linear compressibility in common materials

Negative linear compressibility (NLC) is still considered an exotic property, only observed in a few obscure crystals. The vast majority of materials compress axially in all directions when loaded in hydrostatic compression. However, a few materials have been observed which expand in one or two directions under hydrostatic compression. At present, the list of materials demonstrating this unusual behaviour is confined to a small number of relatively rare crystal phases, biological materials, and designed structures, and the lack of widespread availability hinders promising technological applications. Using improved representations of elastic properties, this study revisits existing databases of elastic constants and identifies several crystals missed by previous reviews. More importantly, several common materials-drawn polymers, certain types of paper and wood, and carbon fibre laminates-are found to display NLC. We show that NLC in these materials originates from the misalignment of polymers/fibres. Using a beam model, we propose that maximum NLC is obtained for misalignment of 26°. The existence of such widely available materials increases significantly the prospects for applications of NLC.

36 MATERIALS SCIENCE↗

High-pressure structural, elastic, and thermodynamic properties of zircon-type HoPO 4 and TmPO 4

Zircon-type holmium phosphate (HoPO 4 ) and thulium phosphate (TmPO 4 ) have been studied by single-crystal x-ray diffraction and ab initio calculations. We report on the influence of pressure on the crystal structure, and on the elastic and thermodynamic properties. The equation of state for both compounds is accurately determined. We have also obtained information on the polyhedral compressibility which is used to explain the anisotropic axial compressibility and the bulk compressibility. Both compounds are ductile and more resistive to volume compression than to shear deformation at all pressures. Furthermore, the elastic anisotropy is enhanced upon compression. Finally, the calculations indicate that the possible causes that make the zircon structure unstable are mechanical instabilities and the softening of a silent B 1u mode.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Fracture, failure and compression behaviour of a 3D interconnected carbon aerogel (Aerographite) epoxy composite

Aerographite (AG) is a mechanically robust, lightweight synthetic cellular material, which consists of a 3D interconnected network of tubular carbon [1]. The presence of open channels in AG aids to infiltrate them with polymer matrices, thereby yielding an electrical conducting and lightweight composite. Aerographite produced with densities in the range of 7–15 mg/cm 3 was infiltrated with a low viscous epoxy resin by means of vacuum infiltration technique. Detailed morphological and structural investigations on synthesized AG and AG/epoxy composite were performed by scanning electron microscopic techniques. Our present study investigates the fracture and failure of AG/epoxy composites and its energy absorption capacity under compression. The composites displayed an extended plateau region when uni-axially compressed, which led to an increase in energy absorption of ~133% per unit volume for 1.5 wt% of AG, when compared to pure epoxy. Preliminary results on fracture toughness showed an enhancement of ~19% in K IC for AG/epoxy composites with 0.45 wt% of AG. Furthermore, our observations of fractured surfaces under scanning electron microscope gives evidence of pull-out of arms of AG tetrapod, interface and inter-graphite failure as the dominating mechanism for the toughness improvement in these composites. These observations were consistent with the results obtained from photoelasticity experiments on a thin film AG/epoxy model composite.

36 MATERIALS SCIENCE↗

Investigation of Mild Steel Thin-Wall Tubes in Unfilled and Foam-Filled Triangle, Square, and Hexagonal Cross Sections Under Compression Load

This study has examined proposed structures with mild steel-reinforced LM30 aluminum (Al) alloy having diversely unfilled and 10 wt.% SiCp composite foam-filled tubes for improving axial compression performance. This class of material has novel physical, mechanical, and electrical properties along with low density. In the present experiment, Al alloy foams were prepared by the melt route technique using metal hydride powder as a foaming agent. Crash energy phenomena for diverse unfilled and foam-filled in mild steel thin-wall tubes (triangular, square and hexagonal) were studied as well. Compression deformation investigation was conducted at strain rates of 0.001-0.1/s for evaluating specific energy absorption (SEA) under axial loading conditions. The results were examined to measure plateau stress, maximum densification strain, and deformation mechanism of the materials. Specific energy absorption and total energy absorption capacities of the unfilled and filled sections were determined from the compressive stress–strain curves, which were then compared with each other.

36 MATERIALS SCIENCE↗

Experimental and numerical analysis of pre-compressed masonry walls in two-way-bending with second order effects

The buckling behavior of slender unreinforced masonry (URM) walls subjected to axial compression and out-of-plane lateral loads is investigated through a combined experimental and numerical homogenizedapproach. After a preliminary analysis performed on a unit cell meshed by means of elastic FEs and non-linear interfaces, macroscopic moment-curvature diagrams so obtained are implemented at a structural level, discretizing masonry by means of rigid triangular elements and non-linear interfaces. The non-linear incremental response of the structure is accounted for a specific quadratic programming routine. In parallel, a wide experimental campaign is conducted on walls in two way bending, with the double aim of both validating the numerical model and investigating the behavior of walls that may not be reduced to simple cantilevers or simply supported beams. Panels investigated are dry-joint in scale square walls simply supported at the base and on a vertical edge, exhibiting the classical Rondelet’s mechanism. The results obtained are compared with those provided by the numerical model.

42 ENGINEERING↗

Residual Stresses in SAVY 4000 and Hagan Container Bodies

Chloride-induced stress corrosion cracking (SCC) has been investigated as a potential failure mechanism for the SAVY 4000 and the Hagan containers used to store plutonium-bearing materials at Los Alamos National Laboratory. This report discusses the regions of the container bodies most susceptible to SCC and the magnitude of the residual stresses in those regions. Boiling MgCl2 testing indicated that for both containers the region near the top weld was most susceptible to SCC. The Hagan showed through wall cracking after 22-24 hours of exposure both parallel (axial stresses) and perpendicular (hoop stresses) to the weld. The SAVY 4000 container showed significant cracking above and below the weld after 47 hours of exposure but there was no visual evidence of a through wall crack and the cracks did not leak water. Two through wall holes formed in the bottom of the SAVY 4000 container after 44-46 hours of exposure. For both containers, average “through wall” residual stresses were determined from hole drilling data 4 mm below the weld. In the Hagan body, average tensile hoop stresses were 194 MPa and average compressive axial stresses were -120 MPa. In the SAVY 4000 body, average compressive hoop stresses were 11 MPa and average tensile axial stresses were 25 MPa. Results suggest that because the Hagan container exhibited through wall cracking in a shorter time in boiling MgCl2 and had the higher average tensile stress, 194 MPa hoop stress, it is more susceptible to SCC than the SAVY 4000 container.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

[Cu(aq)] 2+ is structurally plastic and the axially elongated octahedron goes missing

High resolution (k = 18 Å –1 or k = 17 Å –1 ) copper K-edge EXAFS and MXAN (Minuit X-ray Absorption Near Edge) analyses have been used to investigate the structure of dissolved [Cu(aq)] 2+ in 1,3-propanediol (1,3-P) or 1,5-pentanediol (1,5-P) aqueous frozen glasses. EXAFS analysis invariably found a single axially asymmetric 6-coordinate (CN6) site, with 4×O eq = 1.97 Å, O ax1 = 2.22 Å, and O ax2 = 2.34 Å, plus a second-shell of 4×O water = 3.6 Å. However, MXAN analysis revealed that [Cu(aq)] 2+ occupies both square pyramidal (CN5) and axially asymmetric CN6 structures. The square pyramid included 4×H 2 O = 1.95 Å and 1×H 2 O = 2.23 Å. The CN6 sites included either a capped, near perfect, square pyramid with 5×H 2 O = 1.94 ± 0.04 Å and H 2 O ax = 2.22 Å (in 1,3-P) or a split axial configuration with 4×H 2 O = 1.94, H 2 O ax1 = 2.14 Å, and H 2 O ax2 = 2.28 Å (in 1,5-P). The CN6 sites also included an 8-H 2 O second-shell near 3.7 Å, which was undetectable about the strictly pyramidal sites. Equatorial angles averaging 94° ± 5° indicated significant departures from tetragonal planarity. MXAN assessment of the solution structure of [Cu(aq)] 2+ in 1,5-P prior to freezing revealed the same structures as previously found in aqueous 1M HClO 4 , which have become axially compressed in the frozen glasses. [Cu(aq)] 2+ in liquid and frozen solutions is dominated by a 5-coordinate square pyramid, but with split axial CN6 appearing in the frozen glasses. Among these phases, the Cu–O axial distances vary across 1 Å, and the equatorial angles depart significantly from the square plane. Although all these structures remove the d x 2 –y 2 , d z 2 degeneracy, no structure can be described as a Jahn-Teller (JT) axially elongated octahedron. The JT-octahedral description for dissolved [Cu(aq)] 2+ should thus be abandoned in favor of square pyramidal [Cu(H 2 O) 5 ] 2+ . The revised ligand environments have bearing on questions of the Cu(i)/Cu(ii) self-exchange rate and on the mechanism for ligand exchange with bulk water. In conclusion, the plasticity of dissolved Cu(ii) complex ions falsifies the foundational assumption of the rack-induced bonding theory of blue copper proteins and obviates any need for a thermodynamically implausible protein constraint.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The Development of DYNA3D Material Model 67 - Hyperelastic Elastomeric Foam With Viscoelasticity

A strain energy potential is developed to represent isotropic, medium-density, elastomeric foams under predominately compressive volumetric states. The potential is proven to be polyconvex and coercive, and is thus stable for all admissible loadings. The potential includes terms that capture the increase in hydrostatic and deviatoric stiffnesses as the relative volume decreases to and slightly beyond full consolidation, i.e., the phenomenon commonly called “lock-up”. The model is shown to accurately replicate the axial compressive stress and secant shear modulus from combined uni-axial stress/torsion experiments. An appropriate viscoelastic formulation for the potential is summarized. The potential and viscoelastic option are implemented in the explicit finite element code DYNA3D (Zywicz and Lin, 2014) as material model 67.

42 ENGINEERING↗

Multistage Axial Hydro-Forging Sequence: A New Forming Approach for Manufacturing of Double-Stepped Tubes

To manufacture the large-expansion-ratio double-stepped tube without thinning, a new approach known as multistage axial hydro-forging sequence has been proposed in this study. The whole forming process is divided into five stages. Compared with traditional tube hydroforming, the thickness can be increased by axial compression deformation to reduce the thinning ratio and enhance the forming capacity of the tube in hydro-forging stage and double-stepped hydro-forging stage, respectively. The proposed multistage axial hydro-forging sequence process was implemented by experiments along with the finite element simulation to validate its feasibility. The suitable loading path to prevent defects such as wrinkle and thinning was discussed. The results showed that double-stepped tube with large expansion ratio can be produced successfully with movable dies’ design. There is no thinning in the final tube, particularly in all stepped area, and a better thickness distribution could be achieved. As a result, the proposed multistage axial hydro-forging sequence can be a feasible forming approach for the fabrication of large-expansion-ratio double-stepped tubes with high reliability.

36 MATERIALS SCIENCE↗

Discrepancy in the Critical State Void Ratio of Poorly Graded Sand due to Shear Strain Localization

The critical state (CS) concept is a theoretical framework that models the constitutive behavior of soils, including sand and other granular materials. It supports the notion of a unique postfailure state, where the soil ultimately experiences continuous shearing with no change in the plastic volumetric strain. However, the published literature has frequently noted the nonconvergence of sand specimens with different initial densities to a unique CS in the compression plane due to many factors such as specimen fabric, particle morphology, breakage, and grain size distribution. This paper examines the CS for poorly graded (uniform) glass beads and 3 different types of silica sands using 50 conventional triaxial compression (CTC) experiments, 12 oedometer tests, and in situ synchrotron microcomputed tomography (SMT) scans for 10 CTC experiments. The results of the 50 CTC experiments revealed a diffused CS zone in the compression plane, which was further examined using the in situ SMT scans. A thorough three-dimensional image analysis of the SMT scans accurately quantified the evolution of the local void ratio (elocal) versus axial compression within zones of intensive shearing toward the center of the specimen. The evolution of the void ratio was also measured using the entire volume of the specimen (eglobal). At the CS, the elocal/eglobal ratio was assessed to be ~1.25 when a single shear band developed within the scanned specimens and ~1.1-1.15 for specimens that failed via external bulging that was internally manifested by the development of multiple shear bands. This finding suggests that the CS zone in the compression plane can be attributed to the common wrong consideration of eglobal evolution in lieu of elocal within the developing shear bands. Furthermore, the lack of shear band development in uniaxial compression has made the results of the oedometer test reliable in quantifying the CS parameters in the compression plane.

58 GEOSCIENCES↗

Structural Modifications of Single-Crystal Aragonite CaCO 3 Beginning at ~15 GPa: In Situ Vibrational Spectroscopy and X-Ray Diffraction Evidence

The structural chemistry of carbonates under mantle conditions facilitates our understanding of carbon recycling pathways in the earth’s interior. It also has impacts on the dynamics of mantle–slab interactions. Aragonite is a common calcium carbonate mineral in pelagic marine sediments. The structural chemistry of single-crystal aragonite during successive compression and the behavior of a structural H+ have been investigated by micro-vibrational spectroscopy and synchrotron X-ray diffraction techniques in diamond anvil cells. We describe a reduction of the b-axial compressibility beginning at ~15 GPa, and the related discontinuities in the first-order derivatives of the vibrational modes. The structural modifications of aragonite are manifested by mutations occurring in the pressure relations of the wavenumbers of the O-C-O bending modes, and of the bandwidth and band intensities of the measured internal and external modes. These anomalies are indicative of changes occurring in the force constant of the C-O bonds, and possibly a second-order phase transition. Besides, the [CaO 9 ] polyhedra begin to deform, possibly with some Ca-O bonds becoming elongated and the others shortening. An increase in the co-ordination number for the Ca 2+ sites could be expected under higher pressures. Additionally, the weakening of the OH modes may imply H + -loss from the aragonite lattice above 11.5 GPa.

58 GEOSCIENCES↗

Uniaxial compression of [001]-oriented CaFe 2 As 2 single crystals:the effects of microstructure and temperature on superelasticity Part I: Experimental observations

Micropillar compression experiments on [001]-oriented CaFe 2 As 2 single crystals have recently revealed the existence of superelasticity with a remarkably high elastic limit of over 10%. The collapsed tetragonal phase transition, which is a uni-axial contraction process in which As-As bonds are formed across an intervening Ca-plane, is the main mechanism of superelasticity. Usually, superelasticity and the related structural transitions are affected strongly by both the microstructure and the temperature. As such, in this study, we investigated how the microstructure and temperature affect the superelasticity of [001]-oriented CaFe 2 As 2 micropillars cut from solution-grown single crystals, by performing a combination of in-situ cryogenic micromechanical testing and transmission electron microscopy studies. Our results show that the microstructure of CaFe 2 As 2 is influenced strongly by the crystal growth conditions and by subsequent heat treatment. The presence of Ca and As vacancies and FeAs nanoprecipitates affect the mechanical behavior significantly. In addition, the onset stress for the collapsed tetragonal transition decreases gradually as the temperature decreases. These experimental results are discussed primarily in terms of the formation of As-As bonds, which is the essential feature of this mechanism for superelasticity. Our research outcomes provide a more fundamental understanding of the superelasticity exhibited by CaFe 2 As 2 under uni-axial compression.

36 MATERIALS SCIENCE↗

Anomalous anisotropic compression behavior of superconducting CrAs under high pressure

CrAs was observed to possess the bulk superconductivity under high-pressure conditions. To understand the superconducting mechanism and explore the correlation between the structure and superconductivity, the high-pressure structural evolution of CrAs was investigated using the angle-dispersive X-ray diffraction (XRD) method. The structure of CrAs remains stable up to 1.8 GPa, whereas the lattice parameters exhibit anomalous compression behaviors. With increasing pressure, the lattice parameters a and c both demonstrate a nonmonotonic change, and the lattice parameter b undergoes a rapid contraction at ~0.18–0.35 GPa, which suggests that a pressure-induced isostructural phase transition occurs in CrAs. Above the phase transition pressure, the axial compressibilities of CrAs present remarkable anisotropy. A schematic band model was used to address the anomalous compression behavior of CrAs. Lastly, the present results shed light on the structural and related electronic responses to high pressure, which play a key role toward understanding the superconductivity of CrAs.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Multiferroic CuCrO₂ under high pressure: In situ X-ray diffraction and Raman spectroscopic studies

The compression behavior of delafossite compound CuCrO₂ has been investigated by in situ x-ray diffraction (XRD) and Raman spectroscopic measurements up to 23.2 and 34 GPa, respectively. X-ray diffraction data show the stability of ambient rhombohedral structure up to ~23 GPa. Material shows large anisotropy in axial compression with c-axis compressibility, κ{sub c} = 1.26 × 10⁻³(1) GPa⁻¹ and a-axis compressibility, κ{sub a} = 8.90 × 10⁻³(6) GPa⁻¹. Our XRD data show an irreversible broadening of diffraction peaks. Pressure volume data when fitted to 3rd order Birch-Murnaghan equation of state give the value of bulk modulus, B₀ = 156.7(2.8) GPa with its pressure derivative, B₀{sup ’} as 5.3(0.5). All the observed vibrational modes in Raman measurements show hardening with pressure. Appearance of a new mode at ~24 GPa indicates the structural phase transition in the compound. Our XRD and Raman results indicate that CuCrO{sub 2} may be transforming to an ordered rocksalt type structure under compression.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗