Purification of copper foils driven by single crystallization

High-purity copper(Cu) with excellent thermal and electrical conductivity, is crucial in modern technological applications, including heat exchangers, integrated circuits, and superconducting magnets. The current purification process is mainly based on the zone/electrolytic refining or anion exchange, however, which excessively relies on specific integrated equipment with ultra-high vacuum or chemical solution environment, and is also bothered by external contaminants and energy consumption. Here we report a simple approach to purify the Cu foils from 99.9%(3N) to 99.99%(4N) by a temperature-gradient thermal annealing technique, accompanied by the kinetic evolution of single crystallization of Cu.The success of purification mainly relies on(i) the segregation of elements with low effective distribution coefficient driven by grain-boundary movements and(ii) the high-temperature evaporation of elements with high saturated vapor pressure.The purified Cu foils display higher flexibility(elongation of 70%) and electrical conductivity(104% IACS) than that of the original commercial rolled Cu foils(elongation of 10%, electrical conductivity of ~ 100% IACS). Our results provide an effective strategy to optimize the as-produced metal medium, and therefore will facilitate the potential applications of Cu foils in precision electronic products and high-frequency printed circuit boards.

Oxidation behavior of 4774DD1 Ni-based single-crystal superalloy at 980℃ in air

The oxidation behavior of a novel Ni-based single-crystal 4774DD1 superalloy for industrial gas turbine applications was investigated by the isothermal oxidation at 980℃ and discontinuous oxidation weight gain methods.The phase constitution and morphology of surface oxides and the characteristics of the crosssection oxide film were analyzed by XRD,SEM and EDS.Results show that the oxidation kinetics of the 4774DD1 superalloy follows the cubic law,indicating its weak oxidation resistance at this temperature.As the oxidation time increases,the composition of the oxide film evolves as following:One layer consisting of a bottom Al_(2)O_(3)sublayer and an upper(Al_(2)O_(3)+NiO)mixture sublayer after oxidized for 25 h.Then,two layers composed of an outermost small NiO discontinuous grain layer and an internal layer for 75 h.This internal layer is consisted of the bottom Al_(2)O_(3)sublayer,an intermediate narrow CrTaO_(4)sublayer,and an upper(Al_(2)O_(3)+NiO)mixture sublayer.Also two layers comprising an outermost relative continuous NiO layer with large grain size and an internal layer as the oxidation time increases to 125 h.This internal layer is composed of the upper(Al_(2)O_(3)+NiO)mixture sublayer,an intermediate continuous(CrTaO_(4)+NiWO_(4))mixture sublayer,and a bottom Al_(2)O_(3)sublayer.Finally,three layers consisting of an outermost(NiAl2O_(4)+NiCr2O_(4))mixture layer,an intermediate(CrTaO_(4)+NiWO_(4))mixture layer,and a bottom Al_(2)O_(3)layer for 200 h.

Localization effect in single crystal of RuAs_(2)

We report the magnetotransport and thermal properties of RuAs_(2) single crystal.RuAs_(2) exhibits semiconductor behavior and localization effect.The crossover from normal state to diffusive transport in the weak localization(WL)state and then to variable range hopping(VRH)transport in the strong localization state has been observed.The transitions can be reflected in the measurement of resistivity and Seebeck coefficient.Negative magnetoresistance(NMR)emerges with the appearance of localization effect and is gradually suppressed in high magnetic field.The temperature dependent phase coherence length extracted from the fittings of NMR also indicates the transition from WL to VRH.The measurement of Hall effect reveals an anomaly of temperature dependent carrier concentration caused by localization effect.Our findings show that RuAs_(2) is a suitable platform to study the localized state.

Corrosion behavior of single-and poly-crystalline dual-phase TiAl–Ti3Al alloy in NaCl solution

To clarify the correlation of single-crystalline structure with corrosion performance in high-strength TiAl alloys, electrochemical and surface characterization was performed by comparing Ti–45Al–8Nb dual-phase single crystals with their polycrystalline counterparts in NaCl solution. Polarization curves show a lower corrosion rate and a higher pitting potential of ~280 mV for the dual-phase single crystals. Electrochemical impedance spectroscopy and potentiostatic polarization plots revealed a higher impedance of the charge transfer through the compact passive film. Surface composition analysis indicated a compact film with more content of Nb, as twice as that in the film on the polycrystals.Our results reflect that the dual-phase Ti–45Al–8Nb single crystals possess a higher corrosion resistance in NaCl solution, compared with their polycrystalline counterpart, arising from a more homogeneous microstructure and composition distribution.

Material Removal Characteristics of Single-Crystal 4H-SiC Based on Varied-Load Nanoscratch Tests

Single-crystal silicon carbide(SiC)has been widely applied in the military and civil fields because of its excellent physical and chemical properties.However,as is typical in hard-to-machine materials,the good mechanical properties result in surface defects and subsurface damage during precision or ultraprecision machining.In this study,single-and double-varied-load nanoscratch tests were systematically performed on single-crystal 4H-SiC using a nanoindenter system with a Berkovich indenter.The material removal characteristics and cracks under different planes,indenter directions,normal loading rates,and scratch intervals were analyzed using SEM,FIB,and a 3D profilometer,and the mechanisms of material removal and crack propagation were studied.The results showed that the Si-plane of the single-crystal 4H-SiC and edge forward indenter direction are most suitable for material removal and machining.The normal loading rate had little effect on the scratch depth,but a lower loading rate increased the ductile region and critical depth of transition.Additionally,the crack interaction and fluctuation of the depth-distance curves of the second scratch weakened with an increase in the scratch interval,the status of scratches and chips changed,and the comprehensive effects of the propagation and interaction of the three cracks resulted in material fractures and chip accumulation.The calculated and experimental values of the median crack depth also showed good consistency and relativity.Therefore,this study provides an important reference for the high-efficiency and precision machining of single-crystal SiC to ensure high accuracy and a long service life.

A Comparative Investigation of Single Crystal and Polycrystalline Ni-Rich NCMs as Cathodes for Lithium-Ion Batteries

Nickel-rich LiNi_(1-x-y)Co_(x)Mn_(y)O_(2)(NCM,1-x-y≥0.6)is known as a promising cathode material for lithium-ion batteries since its superiority of high voltage and large capacity.However,polycrystalline Ni-rich NCMs suffer from poor cycle stability,limiting its further application.Herein,single crystal and polycrystalline LiNi_(0.84)Co_(0.07)Mn_(0.09)O_(2)cathode materials are compared to figure out the relation of the morphology and the electrochemical storage performance.According to the Li^(+)diffusion coefficient,the lower capacity of single crystal samples is mainly ascribed to the limited Li+diffusion in the large bulk.In situ XRD illustrates that the polycrystalline and single crystal NCMs show a virtually identical manner and magnitude in lattice contraction and expansion during cycling.Also,the electrochemically active surface area(ECSA)measurement is employed in lithium-ion battery study for the first time,and these two cathodes show huge discrepancy in the ECSA after the initial cycle.These results suggest that the single crystal sample exhibits reduced cracking,surface side reaction,and Ni/Li mixing but suffers the lower Li^(+)diffusion kinetics.This work offers a view of how the morphology of Ni-rich NCM effects the electrochemical performance,which is instructive for developing a promising strategy to achieve good rate performance and excellent cycling stability.

Centimeter-sized Cs_(3)Cu_(2)I_(5)single crystals grown by oleic acid assisted inverse temperature crystallization strategy and their films for high-quality X-ray imaging

Low-dimensional halide perovskites have become the most promising candidates for X-ray imaging,yet the issues of the poor chemical stability of hybrid halide perovskite,the high poisonousness of lead halides and the relatively low detectivity of the lead-free halide perovskites which seriously restrain its commercialization.Here,we developed a solution inverse temperature crystal growth(ITCG)method to bring-up high quality Cs_(3)Cu_(2)I_(5)crystals with large size of centimeter order,in which the oleic acid(OA)is introduced as an antioxidative ligand to inhibit the oxidation of cuprous ions effieiently,as well as to decelerate the crystallization rate remarkalby.Based on these fine crystals,the vapor deposition technique is empolyed to prepare high quality Cs_(3)Cu_(2)I_(5)films for efficient X-ray imaging.Smooth surface morphology,high light yields and short decay time endow the Cs_(3)Cu_(2)I_(5)films with strong radioluminescence,high resolution(12 lp/mm),low detection limits(53 nGyair/s)and desirable stability.Subsequently,the Cs_(3)Cu_(2)I_(5)films have been applied to the practical radiography which exhibit superior X-ray imaging performance.Our work provides a paradigm to fabricate nonpoisonous and chemically stable inorganic halide perovskite for X-ray imaging.

Effects of temperature on critical resolved shear stresses of slip and twining in Mg single crystal via experimental and crystal plasticity modeling

Magnesium(Mg)single crystal specimens with three different orientations were prepared and tested from room temperature to 733 K in order to systematically evaluate effects of temperature on the critical resolved shear stress(CRSS)of slips and twinning in Mg single crystals.The duplex non-basal slip took place in the temperature range from 613 to 733 K when the single crystal samples were stretched along the<0110>direction.In contrast,the single basal slip and prismatic slip were mainly activated in the temperature range from RT to 733 K when the tensile directions were inclined at an angle of 45°with the basal and the prismatic plane,respectively.Viscoplastic self-consistent(VPSC)crystal modeling simulations with genetic algorithm code(GA-code)were carried out to obtain the best fitted CRSSs of major deformation modes,such as basal slip,prismatic slip,pyramidalⅡ,{1012}tensile twinning and{1011}compressive twinning when duplex slips accommodated deformation.Additionally,CRSSs of the basal and the prismatic slip were derived using the Schmid factor(SF)criterion when the single slip mainly accommodated deformation.From the CRSSs of major deformation modes obtained by the VPSC simulations and the SF calculations,the CRSSs for basal slip and{1012}tensile twinning were found to show a weak temperature dependence,whereas those for prismatic,slip and{1011}compressive twinning exhibited a strong temperature dependence.From the comparison of previous results,VPSC-GA modeling was proved to be an effective method to obtain the CRSSs of various deformation modes of Mg and its alloys.

Review of solution growth techniques for 4H-SiC single crystal

Silicon carbide(SiC),a group IV compound and wide-bandgap semiconductor for high-power,high-frequency and high-temperature devices,demonstrates excellent inherent properties for power devices and specialized high-end markets.Solution growth is thermodynamically favorable for producing SiC single crystal ingots with ultra-low dislocation density as the crystallization is driven by the supersaturation of carbon dissolved in Si-metal solvents.Meanwhile,solution growth is conducive to the growth of both N-and P-type SiC,with doping concentrations ranging from 10^(14)to 10^(19)cm^(-3).To date,4-inch 4H-SiC substrates with a thickness of 15 mm produced by solution growth have been unveiled,while substrates of 6 inches and above are still under development.Based on top-seeded solution growth(TSSG),several growth techniques have been developed including solution growth on a concave surface(SGCS),melt-back,accelerated crucible rotation technique(ACRT),two-step growth,and facet growth.Multi-parameters of the solution growth including meniscus,solvent design,flow control,dislocation conversion,facet growth,and structures of graphite components make high-quality single crystal growth possible.In this paper,the solution growth techniques and corresponding parameters involved in SiC bulk growth were reviewed.

Single crystal growth and electronic structure of Rh-doped Sr_(3)Ir_(2)O_(7)

Ruddlesden-Popper iridate Sr_(3)Ir_(2)O_(7)is a spin-orbit coupled Mott insulator.Hole doped Sr_(3)Ir_(2)O_(7)provides an ideal platform to study the exotic quantum phenomena that occur near the metal-insulator transition(MIT)region.Rh substitution of Ir is an effective method to induce hole doping into Sr_(3)Ir_(2)O_(7).However,the highest doping level reported in Sr_(3)(Ir_(1-x)Rh_(x))_(2)O_(7)single crystals was only around 3%,which is far from the MIT region.In this paper,we report the successful growth of single crystals of Sr3(Ir_(1-x)Rh_(x))_(2)O_(7)with a doping level of~9%.The samples have been fully characterized,demonstrating the high quality of the single crystals.Transport measurements have been carried out,confirming the tendency of MIT in these samples.The electronic structure has also been examined by angle-resolved photoemission spectroscopy(ARPES)measurements.Our results establish a platform to investigate the heavily hole doped Sr_(3)Ir_(2)O_(7) compound,which also provide new insights into the MIT with hole doping in this material system.

Understand anisotropy dependence of damage evolution and material removal during nanoscratch of MgF_(2) single crystals

To understand the anisotropy dependence of the damage evolution and material removal during the machining process of MgF_(2) single crystals,nanoscratch tests of MgF_(2) single crystals with different crystal planes and directions were systematically performed,and surface morphologies of the scratched grooves under different conditions were analyzed.The experimental results indicated that anisotropy considerably affected the damage evolution in the machining process of MgF_(2) single crystals.A stress field model induced by the scratch was developed by considering the anisotropy,which indicated that during the loading process,median cracks induced by the tensile stress initiated and propagated at the front of the indenter.Lateral cracks induced by tensile stress initiated and propagated on the subsurface during the unloading process.In addition,surface radial cracks induced by the tensile stress were easily generated during the unloading process.The stress change led to the deflection of the propagation direction of lateral cracks.Therefore,the lateral cracks propagated to the workpiece surface,resulting in brittle removal in the form of chunk chips.The plastic deformation parameter indicated that the more the slip systems were activated,the more easily the plastic deformation occurred.The cleavage fracture parameter indicated that the cracks propagated along the activated cleavage planes,and the brittle chunk removal was owing to the subsurface cleavage cracks propagating to the crystal surface.Under the same processing parameters,the scratch of the(001)crystal plane along the[100]crystal-orientation was found to be the most conducive to achieving plastic machining of MgF_(2) single crystals.The theoretical results agreed well with the experimental results,which will not only enhance the understanding of the anisotropy dependence of the damage evolution and removal process during the machining of MgF_(2) crystals,but also provide a theoretical foundation for achieving the high-efficiency and low-damage processing of anisotropic single crystals.

Stable yellow light emission from lead-free copper halides single crystals for visible light communication

Yellow light-emitting diodes(LEDs) as soft light have attracted abundant attention in lithography room, museum and art gallery. However, the development of efficient yellow LEDs lags behind green and blue LEDs, and the available perovskites yellow LEDs suffer from the instability. Herein, a pressure-assisted cooling method is proposed to grow lead-free CsCu2I3single crystals, which possess uniform surface morphology and enhanced photoluminescence quantum yield(PLQY) stability, with only 10% PLQY losses after being stored in air after 5000 h.Then, the single crystals used for yellow LEDs without encapsulation exhibit a decent Correlated Color Temperature(CCT) of 4290 K, a Commission Internationale de l’Eclairage(CIE) coordinate of(0.38, 0.41), and an excellent 570-h operating stability under heating temperature of 100°C. Finally, the yellow LEDs facilitate the application in wireless visible light communication(VLC), which show a-3 dB bandwidth of 21.5 MHz and a high achievable data rate of 219.2 Mbps by using orthogonal frequency division multiplexing(OFDM) modulation with adaptive bit loading. The present work not only promotes the development of lead-free single crystals, but also inspires the potential of CsCu2I3in the field of yellow illumination and wireless VLC.

THE EFFECT STRESS ON THE MAGNETOSTRICTION IN TWIN- FREE SINGLE CRYSTALS Tb_y Dy_(1-y) (Fe_(1-x) T_x)_2 (T=Al,Mn)

Magnetostriction at room temperature under various conditions of compressive prestress and applied fields in Tb yDy 1-y (Fe 1-x T x) 2 (T=Al,Mn) twin-free single crystals were investigated. The substitution of Al or Mn for Fe lowers the magnetostriction un-der ordinary temperature and pressure, but it also decreases the saturation field, which enables these materials with potential benefits for applications.

Effect of surface recrystallization on the creep rupture property of a single-crystal superalloy

The effect of surface recrystallization by heating after shot-peening on the creep rapture property and fracture behavior of a single-crystal superalloy was investigated. The results show that the creep rupture property of the single-crystal superalloy was greatly influenced by surface recrystallization. A recrystallized surface layer with a depth of 101 ~m resulted in a decrease in creep rupture life by nearly 50%, and an almost linear reduction of creep rupture life was observed with the increase of recrystallization depth. A lower strength of the recrystal- lized layer, inhomogeneous deformation between the recrystallized layer and the matrix, and stress concentration caused by notch effect resuited in the decrease in creep rupture life of the single-crystal superalloy.

Surface recrystallization of a single crystal nickel-base superalloy

The recrystallization behavior of a single crystal nickel-base superalloy was investigated by shot peening and subsequent annealing. Two kinds of recrystallization microstructures, which are intensively dependent on the annealing temperature, are shown in the nickel-base superalloy after shot peening and subsequent annealing. Surface recrystallized grains are obtained when the superalloy is annealed at solution treatment temperature. The nucleation of recrystallization originates from the dendritic core, where rapid dissolution of γ＇ particles occurs. Cellular recrystallization is observed after annealing at lower temperatures. Cellular structures induced by high diffusivity of the moving boundary and more γ＇ particles dissolution led by residual stress are developed from the surface region. Recrystallized kinetics of the shot-peened alloy annealed at 1050°C accords with the Johnson-Mehl-Avrami-Kolmogorov equation. The low Avrami exponent is caused by the inhomogeneous distribution of stored energy, the decreasing of stored energy during recovery, and the strong resistance of boundary migration by γ＇ particles.

Effects of Ru on the microstructure and phase stability of a single crystal superalloy

Two experimental single crystal superalloys, the Ru-free alloy and the Ru-containing alloy with [001 ] orientation, were cast in a directionally solidified furnace, while other alloying element contents were kept unchanged. The effects of Ru on the microstructure and phase stability of the single crystal superalloy were investigated, y＇ directional coarsening and rafting were observed in the Ru-free alloy and Ru-containing alloy after long-term aging at 1070~C for 800 h. Needle-shaped o topologically close packed （TCP） phases precipitated and grew along the fixed direction in both the alloys. The precipitating rate and volume fraction of TCP phases decreased significantly by adding Ru. The compositions ofy and y＇ phases measured using an energy-dispersive X-ray spectroscope （EDS） in transmission electron microscopy （TEM） analysis showed that the addition of Ru lessened the partition ratio of TCP forming elements, Re, W and Mo, and decreased the satu- ration degrees of these elements in y phase, which can enable the Ru-containing alloy to be more resistant to the formation of TCP phases. It is indicated that the addition of Ru to the Ni-based single crystal superalloy with high content of the refractory alloying element can enhance phase stability.

Solidification Simulation of Investment Castings of Single Crystal Hollow Turbine Blade

The three-dimensional solidification simulation of the investment castings of single crystal hollow turbine blade at the withdrawal rates of 2 mm/min, 4.5 mm/min and 7 mm/min has been performed with the finite element thermal analysis. The calculated results are in accordance with the experimental ones. The results show that with the increase of withdrawal rate the concave curvature of the liquidus isotherm is larger and larger, and the temperature gradients of the blades increase. No effects of withdrawal rate on the distribution of the temperature gradients of the starter and helical grain selector of the blades are observed at withdrawal rates of 2 mm/min, 4.5 mm/min and 7 mm/min. The relatively high temperature gradient between 500℃/cm and 1000℃/cm in the starter and helical grain selector is obtained at three withdrawal rates.

Solidification Simulation of Single Crystal Investment Castings

The three dimensional solidification simulation of the single crystal investment castings at withdrawal rates of 2 mm祄in, 4.5 mm祄in and 7 mm祄in was performed with the finite element thermal analysis method. The calculated results were in accordance with the experimental ones. The results showed that with the increase of with-drawal rate the concave curvature of the liquidus isotherm was bigger and bigger and the temperature gradient of the castings decreased. No effects of withdrawal rate on the distribution of the temperature gradient of the starter and helical grain selector of the castings were observed at withdrawal rates of 2 mm祄in, 4.5 mm祄in and 7mm祄in. The relatively high temperature gradient between 500癈礳m and 1000癈礳m in the starter and helical grain selector was obtained at three withdrawal rates. The study indicates the three dimensional solidification simulation by finite element method is a powerful tool for understanding solidification and predicting defects in single crystal investment castings.

Inclusions in large diamond single crystals at different temperatures of synthesis

The inclusions in large diamond single crystals have effects on its ultimate performance, which restricts its industrial applications to a great extent. Therefore, it is necessary to study the inclusions systematically. In this paper, large diamond single crystals with different content values of inclusions are synthesized along the(100) surface by the temperature gradient method(TGM) under 5.6 GPa at different temperatures. With the synthetic temperature changing from 1200?C to 1270?C,the shapes of diamonds change from plate to low tower, to high tower, even to steeple. From the microscopic photographs of the diamond samples, it can be observed that with the shapes of the samples changing at different temperatures, the content values of inclusions in diamonds become zero, a little, much and most, correspondingly. Consequently, with the temperature growing from low to high, the content values of inclusions in crystals increase. The origin of inclusions is explained by the difference in growth rate between diamond crystal and its surface. The content values of inclusions in diamond samples are quantitatively calculated by testing the densities of diamond samples. And the composition and inclusion content are analyzed by energy dispersive spectroscopy(EDS) and x-ray diffraction(XRD). From contrasting scanning electron microscopy(SEM) photographs, it can be found that the more the inclusions in diamond, the more imperfect the diamond surface is.

Multiscale simulation of nanometric cutting of single crystal copper——effect of different cutting speeds

A multiscale simulation has been performed to determine the effect of the cutting speed on the deformation mechanism and cutting forces in nanometric cutting of single crystal copper. The multiscale simulation model, which links the finite element method and the molecular dynamics method, captures the atomistic mechanisms during nanometric cutting from the free surface without the computational cost of full atomistic simulations. Simulation results show the material deformation mechanism of single crystal copper greatly changes when the cutting speed exceeds the material static propagation speed of plastic wave. At such a high cutting speed, the average magnitudes of tangential and normal forces increase rapidly. In addition, the variation of strain energy of work material atoms in different cutting speeds is investigated.