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At least 829 records · Page 46

Structure and particle size analysis of LaFeO{sub 3} nanoparticles

Particle size analysis of LaFeO{sub 3} nanoparticles has been done through different methods. A simple low temperature syntheses of LaFeO{sub 3}-NPs were carried out via PVA based sol-gel method. The role of PVA in this method is complexing agent. The product were characterized with the help of X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), and Transmission Electron Microscopy (TEM). The Rietveld refinement on X-ray diffraction peaks have been done in order to calculate various structural parameters. The Scherrer method was applied to calculate the crystallite size. Further, the crystallite size and associated lattice strain of LaFeO{sub 3}-NPs were studied using Williamson-Hallmethod. The FESEM image shows the presence of spherical morphology. The formation of LaFeO{sub 3} nanoscale particles, with their size, has been confirmed by TEM characterization.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Green Synthesis and Antioxidant Study of Silver Nanoparticles of Root Extract of Sageretia thea and Its Role in Oxidation Protection Technology

Development of environmentally friendly synthesis of nanoparticles is one of the important areas of research in nanotechnology. In present study silver naopartticles (AgNPs) of root extract of Sageretia thea (S. thea) were synthesized at room temperature. The synthesized AgNPs were characterized by UV. Visible spectroscopy (UV), scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive spectroscopy (EDX), transmission electron microscopy (TEM), dynamic light scattering (DLS) and Fourier transform infrared (FT-IR) spectroscopy. Formation of AgNPs was confirmed by visual examination the colour change from yellow to brick red due to surface Plasmon resonance band at 435 nm. SEM and TEM analysis of synthesized AgNPs revealed spherical morphology with average particle size 25 nm. Crystalline nature of the AgNPs in face centered cubic structure is evident from the selected area electron diffraction (SAED) and XRD pattern. The presence of elemental Ag was confirmed by EDX analysis at 3kv. Different functional groups which responsible for reduction and stabilization of reaction medium was confirmed by FTIR spectroscopy. The biosynthesized AgNPs showed strong DPPH and dye protection radical scavenging assay while modest hydrogen peroxide radical scavenging assay as compare to crude extract. The present investigations suggest that biosynthesized nanoparticles have a high potential for use in the preparation of drugs used against various diseases and also a promising candidate for many medical applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Thermal and Mechanical Properties of Eco-friendly Poly(Vinyl Alcohol) Films with Surface Treated Bagasse Fibers

Bagasse fibers reinforced poly(vinyl alcohol) (PVA) composite films were successfully prepared by solution casting method. To enhance the dispersing effect of the fillers, alkali treatment of the plant fibers was adopted before the fabrication of composites. The structure and properties of the resulting composites were characterized by scanning electron microscopy (SEM), X-ray diffraction, differential scanning calorimetry, mechanical tests, water uptake and thermal stability in detail. The results showed that bagasse fibers after surface modification exhibited good compatibility with PVA matrix. The increased polarity as well as the roughness would be beneficial to the interaction and mechanical interlocking between the fiber and matrix. Acting as the heterogeneous nucleation agents, the fibers could enhance the degree of crystallization and decrease the supercooling degrees of PVA matrix. The fibers exhibited dramatically reinforcing effect in the matrix, and with the increase of fiber, the Young’s modulus and tensile yield stress increased. The Young’s modulus and tensile yield stress of composites with 8% filler would be 3 and 2 times compared with neat PVA films. The thermal stability decreased a little and the water uptake increased with the increase of filler content. These composite films would find wide applications in green packaging areas for their fine mechanical and thermal properties.

36 MATERIALS SCIENCE↗

Electrochemical Corrosion Behavior of Plasma-Sprayed FeCrNiMoCBSi Amorphous/Nanocrystalline Coatings in Simulated Seawater Medium

A novel FeCrNiMoCBSi coating was fabricated on F22 marine steel by plasma spraying. The coating microstructure and composition were characterized by scanning electron microscope, transmission electron microscope, x-ray diffraction, differential scanning calorimetry, and x-ray photoelectron spectroscopy. The results showed that the coating consisted of amorphous and nanocrystalline phases. Additionally, the corrosion resistance in simulated seawater was evaluated by electrochemical corrosion methods. It was found that the coating exhibited an excellent resistance to pitting corrosion. For long-time immersion tests, the corrosion resistance was gradually decreased with the increasing through-porosity due to the permeation of the corrosive solution into the coating. The coating lost its efficacy through three stages, namely the protection stage, the permeation stage, and the failure stage.

36 MATERIALS SCIENCE↗

Microstructural characterization of limestone exposed to heat with XRD, SEM and TG-DSC

Highlights: • The microstructure of limestone (25 °C–800 °C) was analyzed by XRD, SEM and TG-DSC. • The microstructural properties of the crystal are anisotropic in different crystal plane directions. • Microstructure controls the macroscopic properties of limestone. - Abstract: Limestone is a common rock used in many buildings and found in underground engineering projects. After exposure to heat, for example, the occurrence of fires, the stability of limestone structures is mostly affected, which may have safety repercussions. Therefore, the impact of thermal effects on the microstructure of limestone is investigated in this study, in which 8 groups of limestone samples are exposed to different temperatures (25 °C, 100 °C, 200 °C, 300 °C, 500 °C, 600 °C, 700 °C and 800 °C), after which X-ray diffraction, differential scanning calorimetry and scanning electron microscopy are carried out. The mineral composition and the microstructure of the samples are numerically modeled, in which the diffraction peaks, full width at half maximum, integral breadth, microstrain, average domain size and dislocation density are analyzed. The macroscopic properties obtained from the results in other works in the literature including porosity, compressive strength, damage coefficients and modulus of elasticity are also compared with the parameters above. The changes in the crystal structure of two minerals, calcite and dolomite, are found to be anisotropic in the different crystal plane directions. It is also found that the limestone microstructure affects the macroscopic properties. A temperature between 200 °C to 300 °C is the critical temperature at which both the macroscopic properties and macrostructure demonstrate significant changes.

36 MATERIALS SCIENCE↗

A study on tensile properties of Alloy 709 at various temperatures

In recent years, there have been several advancements in energy production from both fossil fuels and the alternate “clean” sources such as nuclear fission. These advancements are fueled by the need for more efficient systems that will optimize the use of the depleting fossil fuel reserves and shift the focus to cleaner sources of energy. The efficiency of any power generation cycle is dependent on the ability of the structural material to withstand increased peak operating temperatures. Advanced austenitic stainless steels have been in the focus as structural material for the next generation nuclear power plants, due to their strength, corrosion resistance, weldability and the wide range of temperatures at which the austenite phase is stable. Alloy 709, a recently developed advanced austenitic stainless steel, is being investigated in this paper. Here in this study, tensile tests were conducted on dog-bone samples of Alloy 709 in an in-situ scanning electron microscope (SEM) loading and heating stage, equipped with electron backscatter diffraction (EBSD), at various temperatures. The in-situ experiments indicated that the material primarily accommodated deformation by slip at lower temperatures. Void formation and coalescence at grain boundaries preceded slip at higher temperatures. Although crack initiation at all elevated temperatures was intergranular, the crack propagation through the material and the final fracture was transgranular ductile. Additionally, tensile tests were conducted on larger cylindrical samples at 550, 650 and 750 °C in air. The results of tests conducted in air and in-situ were found to be in agreement, at these temperatures.

36 MATERIALS SCIENCE↗

Importance of Martensite Spatial Distribution at Large Volume Fractions in Imparting Ductility in High-Strength Dual-Phase Steel

Controlled austenite decomposition in a cold-rolled steel was carried out in a hot-dip process simulator with different inter-critical annealing process parameters to produce dual-phase steel consisting of martensite phase fraction above 50%. The evolving microstructure was characterized by using scanning electron microscope and electron backscattered diffraction techniques. Macro- and micro-texture was characterized by using x-ray diffraction and electron backscattered diffraction techniques, respectively. Uniaxial tensile deformation showed a very good combination of ultra-high strength above 900 MPa with uniform elongation of above 7%. An anomalous increase in ductility was observed for steel with high martensite volume fraction of 62.2% compared to that of lower fraction of 52.3%, indicating the influence of size and spatial distribution arrangement of ferrite and martensite phases. The enhancement in the ductility with high strength was attributed to the improved plastic deformability of hard fine martensite phase along with fine ferrite surrounding it. The nature of micro- and macro-texture was also found to affect strain partitioning compatibility between ferrite and martensite in this study.

36 MATERIALS SCIENCE↗

Calcium-Substituted Y{sub 3}Ba{sub 5}Cu{sub 8}O{sub 18} Ceramics Synthesized via Thermal Treatment Method: Structural and Superconducting Properties

In this work, Y{sub 3}(Ba{sub 1−x}Ca{sub x}){sub 5}Cu{sub 8}O{sub 18} compounds with x = 0.00, 0.01, 0.02, 0.03 and 0.05 were synthesized by thermal treatment of aqueous solution of metal nitrates and polyvinylpyrrolidone (PVP). The effects of Ca substitution on the crystal structure, electrical resistance and the microstructure of samples were investigated using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), four-point probe measurement and AC susceptibility. FESEM analysis showed that there was an increase in the grain size and compactness. The zero-resistance critical temperature decreased from 92 K for the pure sample to 83 K for sample x = 0.05. From AC susceptibility result, the intra- and inter-granular loss peaks shifted toward lower temperature and become wider and broader with the increase of Ca substitution due to the weakening of grain coupling. On the other hand, the inter-granular critical current density (J{sub cm}) was found to increase with Ca substitution and has the highest value J{sub cm} = 35 A cm{sup − 2} at x = 0.05, indicating that the Ca substitution was associated with the formation of pinning centres in the Y-358 matrix.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of TiN Addition on 3Y-TZP Ceramics with Emphasis on Making EDM-Able Bodies

In this study, to produce electrically conductive ceramics, rapid hot press (RHP) sintering of 3 mol.% yttria-stabilized tetragonal zirconia polycrystal (3Y-TZP) and 3Y-TZP/TiN composites with TiN amounts of 25, 35, and 45 vol.% was performed at 1300, 1350, and 1400 °C. Interestingly, the toughness and hardness were improved in the presence of TiN up to 35 vol.% and maximum fracture toughness and hardness of 5.40 ± 0.05 MPa m{sup 1/2} and 14.50 ± 0.06 GPa, respectively, were obtained. However, the bending strength was decreased which could be attributed to the rather weak interfaces of nitride and oxide phases. Regarding the zirconia matrix, the effect of grain size on fracture toughness of the samples has been studied using x-ray diffraction and field emission scanning electron microscope (FESEM) analysis. It was also found that electrical resistivity decreased to the value of 6.88 × 10{sup −6} Ω m at 45 vol.% of TiN. It seems the TiN grains form a network to impose conductivity on the ZrO{sub 2} body; however, below 35 vol.% TiN, due to lack of percolation effect, this conductivity could not be maintained according to FESEM studies. Finally, electrically conductive samples were successfully machined by electrical discharge machining (EDM).

36 MATERIALS SCIENCE↗

Analysis of integrity and microstructure of linear friction welded Waspaloy

Nickel-base superalloy, Waspaloy, was linear friction welded (LFWed) under different axial shortening conditions of 2.0, 3.4, and 4.6 mm. The tensile properties and microhardness of the weldments were investigated in the as-LFWed condition and compared with those in the post-weld heat treated (PWHTed) condition. Mechanical properties were related to microstructures following examination by optical microscopy, high resolution scanning electron microscopy, and electron backscatter diffraction (EBSD). Analyses of the EBSD results in terms of the misorientation angle distribution, which represents the stored energy, were performed. In the as-LFWed condition, the yield strength (YS) and ultimate tensile strength (UTS) increased with axial shortening due to greater expulsion of the softened interfacial material toward the periphery as flash. In contrast, with increasing axial shortening the total elongation initially remained constant and then decreased. This was also related to the expulsion of the softened interfacial material into the bifurcated flash. Extensive dissolution of the strengthening phase (γ′) in the weld area during linear friction welding (LFW) contributed to the lower YS and UTS in the as-welded condition compared to the PWHTed condition where the γ′ particles were recovered. After performing post-weld heat treatment (PWHT), the total elongation improved due to the relaxation of stored energy and grain growth in the thermomechanically affected zone (TMAZ). - Highlights: • Tensile property and microstructure in Waspaloy linear friction welds were studied. • Yield strength and ultimate tensile strength increased with axial shortening. • Elongation initially remained constant and then decreased with axial shortening. • Post-weld heat treat recovered dissolved γ′ particles and increased weld strength. • Stored energy relaxation during post-weld heat treatment improved weld elongation.

36 MATERIALS SCIENCE↗

Development of nano-Y2O3 dispersed Zr alloys synthesized by mechanical alloying and consolidated by pulse plasma sintering

Highlights: • Zr-Fe-Cr-Cu-Ti-1.0wt% nano-Y{sub 2}O{sub 3} dispersed alloys are fabricated by mechanical alloying and pulse plasma sintering. • These alloys record extremely high compressive strength, Young’s modulus, and hardness. • These mechanical properties are superior as compared to other commercially available Zr based alloys. • Dispersion of nanometric FeZr{sub 2}, Y{sub 2}Ti{sub 2}O{sub 7}, Fe{sub 2}Ti, ZrCu, Cr{sub 2}Zr, Y{sub 2}O{sub 3} leads to grain boundary pinning at elevated temperature. - Abstract: In this paper, Zr alloys are synthesized with nominal compositions: 50Zr-30Fe-10Cr-5Cu-5Ti (alloy A), and 49Zr-30Fe-10Cr-5Cu-5Ti-1Y{sub 2}O{sub 3} (alloy B), 45Zr-30Fe-10Cr-10Cu-5Ti (alloy C), 44Zr-30Fe-10Cr-10Cu-5Ti-1Y{sub 2}O{sub 3} (alloy D) (all in wt%) by mechanical alloying and consolidated by pulse plasma sintering at 1173 K (900 °C), 1223 K (950 °C) and 1273 K (1000 °C) using 75 MPa uniaxial pressure applied for 5 min and 70 kA pulsed current at 3 Hz pulse frequency. The microstructure and phase evolution during mechanical alloying and sintering has been characterized by X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM & TEM) and energy dispersive spectroscopy (EDS). Mechanical properties i.e. hardness and compressive strength were determined by using nano-indentation unit and universal testing machine. The produced alloys recorded very high levels of compressive strength (1359–2456 MPa), and hardness (7.05–10.05 GPa) which measures 1.5–2.0 times more than that of other Zr alloys (2 O{sub 3}) particles which can contribute to grain boundary pinning, and improved creep and oxidation resistance at elevated temperature.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Effect of gadolinium addition on microstructural evolution and solidification characteristics of Al-15%Mg2Si in-situ composite

Highlights: • The Al{sub 3}Gd is the heterogeneous nucleation of primary Mg{sub 2}Si in Al-15%Mg{sub 2}Si composite. • Addition of Gd to Al-15%Mg{sub 2}Si resulted in the formation of Al{sub 2}Si{sub 2}Gd and AlSiGd intermetallic compounds. • Absorption of Gd atoms preferentially on {100} facets of Mg{sub 2}Si crystals changed its growth manners. • Primary Mg{sub 2}Si transformed from coarse-dendritic to perfect truncated octahedral shape after treating with 1.0 wt% Gd. • Gd addition increased the nucleation and growth temperatures of primary Mg{sub 2}Si. - Abstract: The current study investigated the effects of gadolinium (Gd) addition (0, 0.3, 0.5, 1.0, and 2.0 wt%) on microstructural development and solidification characteristics of hypereutectic Al-15%Mg{sub 2}Si in-situ composite. Microstructural examinations were carried out via optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and electron backscattered diffraction (EBSD). The results showed that an addition of 1.0 wt% Gd, changed the morphology of primary Mg{sub 2}Si from coarse dendritic to fine truncated octahedral shape. Furthermore, the average size of primary Mg{sub 2}Si particles decreased from 40 μm to 20 μm and density increased from 495 to 1167 particles/mm{sup 2}. Besides that, cooling curve thermal analysis (CCTA) technique revealed that Gd addition increased nucleation and growth temperatures of primary Mg{sub 2}Si phase. It is proposed that modification and refinement mechanism of Gd addition are mainly attributed to formation of tiny Al{sub 3}Gd particles as the heterogeneous nucleation substrates for primary Mg{sub 2}Si, which results in a refined distribution of these particles and poisoning effect by adsorbing Gd atoms, preferentially on {100} facets of Mg{sub 2}Si crystals. Moreover, it is believed that formation of Gd intermetallic compounds is responsible for refinement of primary Mg{sub 2}Si particles.

36 MATERIALS SCIENCE↗

Development of a fast framing detector for electron microscopy

A high frame rate detector system is described that enables fast real-time data analysis of scanning diffraction experiments in scanning transmission electron microscopy (STEM). This is an end-to-end development that encompasses the data producing detector, data transportation, and real-time processing of data. The detector will consist of a central pixel sensor that is surrounded by annular silicon diodes. Both components of the detector system will synchronously capture data at almost 100 kHz frame rate, which produces an approximately 400 Gb/s data stream. Low-level preprocessing will be implemented in firmware before the data is streamed from the National Center for Electron Microscopy (NCEM) to the National Energy Research Scientific Computing Center (NERSC). Live data processing, before it lands on disk, will happen on the Cori supercomputer and aims to present scientists with prompt experimental feedback. This online analysis will provide rough information of the sample that can be utilized for sample alignment, sample monitoring and verification that the experiment is set up correctly. Only a compressed version of the relevant data is then selected for more in-depth processing.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Practical aspects of diffractive imaging using an atomic-scale coherent electron probe

Four-dimensional scanning transmission electron microscopy (4D-STEM) is a technique where a full two-dimensional convergent beam electron diffraction (CBED) pattern is acquired at every STEM pixel scanned. Capturing the full diffraction pattern provides a rich dataset that potentially contains more information about the specimen than is contained in conventional imaging modes using conventional integrating detectors. In this work, using 4D datasets in STEM from two specimens, monolayer MoS 2 and bulk SrTiO 3 , we demonstrate multiple STEM imaging modes on a quantitative absolute intensity scale, including phase reconstruction of the transmission function via differential phase contrast imaging. Finally, practical issues about sampling (i.e. number of detector pixels), signal-to-noise enhancement and data reduction of large 4D-STEM datasets are emphasized.

36 MATERIALS SCIENCE↗

The Structural and Magnetic Characteristics of Nanocrystalline Co{sub 82}Zr{sub 18} Alloy

In the present study, the structural and magnetic characteristics of nanocrystalline Co{sub 82}Zr{sub 18} alloy with different structure and crystallite sizes were investigated. In this regard, the nanocrystalline Co{sub 82}Zr{sub 18} sample with different structure and crystallite sizes were prepared using a copper boat vacuum induction melting plus melt spinning and subsequent annealing processes. The prepared samples were characterized using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), differential scanning calorimetry (DSC), and vibrating scanning magnetometer (VSM). According to achieved results, single-phase structure of Zr{sub 2}Co{sub 11} can successfully form by means of melt spinning process at wheel speed of 40 m/s. The melt-spun ribbons exhibit hard magnetic properties with the coercivity and saturation of magnetization in the range of 2.3 kOe and 58 emu/g, respectively. The highest value of coercivity in Co{sub 82}Zr{sub 18} alloy was estimated to be about 3 kOe in annealed sample at 500{sup ∘}C for 1 h.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Ruthenium oxide nanostring clusters anchored Graphene oxide nanocomposites for high-performance supercapacitors application

Highlights: • GO-RuO{sub 2} nanocomposites were synthesized by simple hydrothermal method. • GO-RuO{sub 2} nanocomposites were characterized by XRD, SEM, TEM and EDS. • GO-RuO{sub 2} nanostring composite has shown a maximum specific capacitance of 859 Fg{sup −1} at the scan rate of 5 mVs{sup −1}. • GO-RuO{sub 2} nanostring composite electrode exhibits tremendous cyclic stability. - Abstract: Here, we report simple hydrothermal method for the preparation of Graphene oxide (GO) is embellished with nanostring clusters of ruthenium oxide (GO-RuO{sub 2}). The structure of the nanocomposite material was ascertained using X-ray diffraction (XRD), Raman spectroscopy, Scanning electron spectroscopy (SEM), Energy dispersive spectroscopy (EDS) and Transmission spectroscopy (TEM). The supercapacitor performance of the nanocomposites was investigated in acidic electrolyte, 1.0 M H{sub 2}SO{sub 4}, in a three-electrode setup. GO-RuO{sub 2} nanostring composite has shown a maximum specific capacitance of 859 Fg{sup −1} at the scan rate of 5 mVs{sup −1} using Cyclic voltammetry (CV) and by using Chronopotentiometry (CP) the specific capacitance towered up to 512 Fg{sup −1} at a current density of 2.5 Ag{sup −1}. Further, the material also possesses a high energy density of 246 Wh kg{sup -1}with a maximum power density of 1028 W kg{sup -1}. GO-RuO{sub 2} nanostring composite electrode exhibits tremendous cyclic stability with the specific capacitance retention of nearly 99% of the initial capacitance.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Process-Structure-Property Relations for As-Deposited Solid-State Additively Manufactured High-Strength Aluminum Alloy

Solid-state additive manufacturing methods provide innovative solutions to circumvent problems associated with materials susceptible to hot cracking by avoiding liquid solid phase transformations. In this work, the process parameter influence on microstructural evolution and mechanical response of a fully dense aluminum alloy 7050 (AA7050) component manufactured via a rapid, solid-state additive manufacturing process known as Additive Friction Stir Deposition (AFS-D) was quantified for the first time. Three sections (starting dwell, transient, crossover of roads) of the deposition that exhibit differing thermomechanical processing histories were evaluated for the resulting microstructure and mechanical response. The microstructural characterization was performed on the as-deposited AA7050 via Electron Backscatter Diffraction (EBSD), TEM, optical microscopy, and Scanning Electron Microscopy (SEM). The microstructural characterization revealed refined constituent particles and grains throughout the as-deposited AA7050 microstructure. Furthermore, quasi-static tensile experiments were conducted in both the build and transverse directions, in order to quantify the orientation influence on tensile properties of the as-deposited AA7050 build. Spatially dependent tensile properties were observed in the material due to heat input variation coarsening of secondary phases towards the initial layers of the AFS-D build. Post-mortem analysis revealed that voids nucleated and coalesced from the overgrowth of the strengthening precipitates present in the material, resulting in fracture.

36 MATERIALS SCIENCE↗

The influence of reduced graphene oxide on electrical conductivity of LiFePO{sub 4}-based composite as cathode material

LiFePO{sub 4} is fascinating cathode active materials for Li-ion batteries application because of their high electrochemical performance such as a stable voltage at 3.45 V and high specific capacity at 170 mAh.g{sup −1}. However, their low intrinsic electronic conductivity and low ionic diffusion are still the hindrance for their further application on Li-ion batteries. Therefore, the efforts to improve their conductivity are very important to elevate their prospecting application as cathode materials. Herein, we reported preparation of additional of reduced Graphene Oxide (rGO) into LiFePO{sub 4}-based composite via hydrothermal method and the influence of rGO on electrical conductivity of LiFePO{sub 4}−based composite by varying mass of rGO in composition. Vibration of LiFePO{sub 4}-based composite was detected on Fourier Transform Infrared Spectroscopy (FTIR) spectra, while single phase of LiFePO{sub 4} nanocrystal was observed on X-Ray Diffraction (XRD) pattern, it furthermore, Scanning Electron Microscopy (SEM) images showed that rGO was distributed around LiFePO4-based composite. Finally, the 4-point probe measurement result confirmed that the optimum electrical conductivity is in additional 2 wt% rGO for range 1 to 2 wt% rGO.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗