• Journal of Hydrogen and New Energy
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• v.7 no.2
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• pp.157-164
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• 1996

The AB5-type metal hydride electrodes using $(LM)Ni_{4.49}Co_{0.1}Mn_{0.205}Al_{0.205}$(LM : Lanthaniumrich Mischmetal) alloy powders(${\leq}200$mesh) which were coated with 25wt% copper in an acidic bath were prepared with or without addition of 10wt% PTFE as a binder. Prior to electrochemical measurements, the electrodes were sintered at $40^{\circ}C$ for 1 and 2hrs in vacuum with Mm(mischmetal) and sponge type Ti getters. The properties such as maximum capacity, cycle life and mechanical strength of the negative electrode have been investigated. The surface analysis of the electrode was also obtained before and after charge-discharge cycling using scanning electron microscope(SEM). From the observations of electrochemical behavior, it was found that the sintered electrode shows a lower maximum discharge capacity compared with non-sintered electrode but it shows a better cycle life. For the both electrodes with or without addition of PTFE binder, the values of mechanical strength were obtained, and their values increased with increasing sintering time. However, there is little difference of discharge capacity for both electrodes.

• Bulletin of the Korean Chemical Society
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• v.14 no.1
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• pp.137-143
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• 1993

The tetranuclear heterometallic complex CpMo$Os_3(CO)_{10}({\mu]-H)2[{\mu}3-{\eta}^2-C(O)CH_2Tol]\;(1,\;Cp={\eta}^5-C_5H_5,\;Tol=p-C_6H_4Me)$ has been examined by variable-temperature $^{13}$C-NMR spectroscopy and by a full three-dimensional X-ray structual analysis. Complex 1 crystallizes in the orthorhombic space group Pna2$_1$ with a = 12.960(1) ${\AA}$, b = 11.255(l) ${\AA}$, c = 38.569(10)${\AA}$, V = 5626(2) ${\AA}^3$ and ${\rho}$(calcd) = 2.71 gcm$^{-3}$ for Z = 8 and molecular weight 1146.9. Diffraction data were collectedon a CAD4 diffractometer, and the structure was refined to $R_F$ = 9.7% and $R_{W^F}$ = 9.9% for 2530 data (MoK${\alpha}$ radiation). There are two essentially equivalent molecules in the crystallographic asymmetric unit. The tetranuclear molecule contains a triangulated rhomboidal arrangement of metal atoms with Os(2) and Mo at the two bridgehead positions. The metal framework is planar; the dihedral angle between Os(l)-Os(2)-Mo and Os(3)-Os(2)-Mo planes is 180$^{\circ}$. A triply bridging (${\mu}_3,\;{\eta}^2$) acyl ligand lies above the Os(l)-Os(2)-Mo plane; the oxygen atom spans the two bridgehead positions, while the carbon atom spans one bridgehead position and an acute apical position. The molecular architecture is completed by an ${\eta}^5$-cyclopentadienyl ligand and a semi-triply bridging carbonyl ligand on the molybdenum atom, and nine terminal carbonyl ligands-four on Os(3), three on Os(l), and two on Os(2). The two hydride ligands are inferred to occupy the Os(l)-Os(2) and Mo-Os(3) edges from structural and NMR data.

• Journal of Hydrogen and New Energy
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• v.28 no.1
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• pp.9-16
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• 2017

Hydrogen forms metal hydrides with some metals and alloys leading to solid-state storage under moderate temperature and pressure that gives them the safety advantage over the gas and liquid storage methods. However, it has disadvantages of slow hydrogen adsorption-desorption time and low thermal conductivity. To improve characteristics of metal hydrides, it is important that activation and thermal conductivity of metal hydrides are improved. In this study, we have been investigated hydrogen storage properties of Hydralloy C among Ti-Mn alloys. Also, the characteristics of activation and thermal conductivity of Hydralloy C were enhanced to improve kinetics of hydrogen adsorption-desorption. As physical activation method, PHEM (planetary high energy mill) was performed in Ar or $H_2$ atmosphere. Hydralloy C was also activated by $TiCl_3$ catalyst. To improve thermal conductivity, various types of ENG (expanded natural graphite) were used. The prepared samples were compacted at pressure of 500 bar. As a result, the activation properties of $H_2$ PHEM treated Hydralloy C was better than the other activation methods. Also, the amounts of hydrogen storage showed up to 1.6 wt%. When flake type ENG was added to Hydralloy C, thermal conductivity and hydrogen storage properties were improved.

• Journal of Powder Materials
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• v.13 no.5 s.58
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• pp.327-335
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• 2006

In the development of new hydrogen absorbing materials for a next generation of metal hydride electrodes for rechargeable batteries, metastable Mg-Ni-based compounds find currently special attention. Amor phous-nanocrystalline $Mg_{63}Ni_{30}Y_7$ and $Mg_{50}Ni_{30}Y_{20}$ alloys were produced by mechanical alloying and melt-spinning and characterized by means of XRD, TEM and DSC. On basis of mechanically alloyed Mg-Ni-Y powders, complex hydride electrodes were fabricated and their electrochemical behaviour in 6M KOH (pH=14,8) was investigated. The electrodes made from $Mg_{63}Ni_{30}Y_7$ powders, which were prepared under use of a SPEX shaker mill, with a major fraction of nanocrystalline phase reveal a higher electrochemical activity far hydrogen reduction and a higher maximum discharge capacity (247 mAh/g) than the electrodes from alloy powder with predominantly amorphous microstructure (216 mAh/g) obtained when using a Retsch planetary ball mill at low temperatures. Those discharge capacities are higher that those fur nanocrystalline $Mg_2Ni$ electrodes. However, the cyclic stability of those alloy powder electrodes was low. Therefore, fundamental stability studies were performed on $Mg_{63}Ni_{30}Y_7$ and $Mg_{50}Ni_{30}Y_{20}$ ribbon samples in the as-quenched state and after cathodic hydrogen charging by means of anodic and cathodic polarisation measurements. Gradual oxidation and dissolution of nickel governs the anodic behaviour before a passive state is attained. A stabilizing effect of higher fractions of yttrium in the alloy on the passivation was detected. During the cathodic hydrogen charging process the alloys exhibit a change in the surface state chemistry, i.e. an enrichment of nickel-species, causing preferential oxidation and dissolution during subsequent anodization. The effect of chemical pre-treatments in 1% HF and in $10\;mg/l\;YCl_3/1%\;H_2O_2$ solution on the surface degradation processes was investigated. A HF treatment can improve their anodic passivation behavior by inhibiting a preferential nickel oxidation-dissolution at low polarisation, whereas a $YCl_3/H_2O_2$ treatment has the opposite effect. Both pre-treatment methods lead to an enhancement of cathodically induced surface degradation processes.

• Applied Chemistry for Engineering
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• v.8 no.4
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• pp.568-574
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• 1997

The effect of microencapsulation of maetal hydride (MH) with copper on the electrode performance of a Ni/MH battery has been investigated. The MH electrodes were prepared with a combination of cold press and paste methods. The discharge capacity of the electrode increased with an addition of small amounts if CMC into the electrode, but decreased when heat-treated in an oxygen-free nitrogen flow. The capacity of a Cu-coated $LaNi_5$ electrode was higher than that of LaNi5electrode. The discharge capacity of the electrode prepared with Cu-coated $LaNi_5$ increased with the increase of copper content in the electrode. It is considered that the increase of copper content enhanced the current density on the electrode surface, leading to the increase of the discharge capacity The MH electrode coated by an acidic electroless plating method showed much higher discharge capacity than that using an alkaline electroless plating method. The discharge capacity of the $LaNi_{4.5}Al_{0.5}$ electrode was higher than that of the $LaNi_5$ electrode. Also, the effect of microencapsulation on the deactivation of $LaNi_5$ was studied using an absorption-desorption cycle in CO-containing hydrogen.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.20 no.1
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• pp.1-6
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• 2010

CuInGaSe(CIGS) mixed-source was prepared by hydride vapor phase epitaxy (HVPE). Each metal was mixed in regular ratio and soaked at $1090^{\circ}C$ for 90 minutes in nitrogen atmosphere. After making the mixed-source to powder state, the pellet was made by the powder. The diameter of pellet is 10 mm. The CIGS thin film was deposited on soda lime glass evaporated Mo layer bye-beam evaporator. To confirm the crystallization, we measured X-ray diffraction (XRD). High intensity X-ray peaks diffracted from (112), (204)/(220), (116)/(312) and (400) of CIGS thin film and from (110) of Mo were confirmed by XRD measurement.

• Journal of Hydrogen and New Energy
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• v.16 no.1
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• pp.92-101
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• 2005

[ $Li_3AlH_6$ ] (5.6wt% theoretical hydrogen storage capacity) powders with and without Ti-containing dopants have been successfully synthesized by mechanochemical reaction near room temperatures from mixtures of LiH and $LiAlH_4$ powders. It has been observed that single phase $Li_3AlH_6$ could be obtained within 2-3 hours of milling, but the addition of reactive $TiCl_2\;or\;TiCl_3$ to the starting mixtures. caused partial decomposition of $LiAlH_4$ into LiCl and free Al with gaseous $H_2$. By addition of these reactive dopants to the as-synthesized $Li_3AlH_6$, this problem could be solved. The addition of 2 mol% $TiCl_2\;or\;TiCl_3\;to\;Li_3AlH_6$ decreased the decomposition start temperature up to 30-50$^{\circ}C$, while that of Ti or $TiH_2$ did not change the thermal decomposition behavior of $Li_3AIH_6$.

• Journal of Hydrogen and New Energy
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• v.22 no.3
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• pp.380-385
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• 2011

$MgH_2$ was synthesized by hydriding chemical vapor deposition (HCVD). In this study, we examined the hydrogen storage property of $MgH_2$ synthesized by HCVD. The results of pressure-composition-temperature (PCT) measurement showed that the HCVDed $MgH_2$ reversibly absorbed hydrogen as much as 6 wt%. Each hydrogenation rate was very greater than the conventional alloy methods. The reason was that the particle size made by HCVD was small as approximately 1 ${\mu}m$. The PCT of $MgH_2$ made by HCVD methode was similar to a commercial $MgH_2$. The ${\Delta}H$ and ${\Delta}S$ value are respectively -76.8 $kJ/mol{\cdot}H_2$ and -137.4 $kJ/mol{\cdot}H_2$. Mg made by HCVD methode was activated easily than commercial Mg. Also the initial reaction rate was faster than that of commercial $MgH_2$. 70% of the total storage were stored during 400s.

• Resources Recycling
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• v.28 no.6
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• pp.18-25
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• 2019

In order to recover the cerium contained in the spent nickel metal hydride batteries (NiMH battery), the recovered rare earth complex precipitates from NIMH were converted into rare earth hydroxides through ion exchange reaction to react with NaOH aqueous solution at a reaction temperature of 70 ℃, for 4 hours. Rare earth hydroxides were oxidized by injecting air at 80 ℃ for 4 hours to oxidize Ce³⁺ to Ce⁴⁺. The oxidation rate of cerium was confirmed to be about 25 % through XPS, and the oxidized powder was separated from the rest of the rare earth using the difference in solubility in dilute sulfuric acid. The finally recovered powder has a crystal phase of cerium hydroxide (Ce(OH)₄). The cerium purity of the final product was about 94.6 %, and the recovery rate was 97.3 %.

• Journal of Powder Materials
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• v.25 no.3
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• pp.213-219
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• 2018

We report a method for preparing rare earth oxides ($Re_xO_y$) from the recycling process for spent Ni-metal hydride (Ni-MH) batteries. This process first involves a leaching of spent Ni-MH powders with sulfuric acid at $90^{\circ}C$, resulting in rare earth precipitates (i.e., $NaRE(SO_4)_2{\cdot}H_2O$, RE = La, Ce, Nd), which are converted into rare earth oxides via two different approaches: i) simple heat treatment in air, and ii) metathesis reaction with NaOH at $70^{\circ}C$. Not only the morphological features but also the crystallographic structures of all products are systematically investigated using field-emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD); their thermal behaviors are also analyzed. In particular, XRD results show that some of the rare earth precipitates are converted into oxide form (such as $La_2O_3$, $Ce_2O_3$, and $Nd_2O_3$) with heat treatment at $1200^{\circ}C$; however, secondary peaks are also observed. On the other hand, rare earth oxides, RExOy can be successfully obtained after metathesis of rare earth precipitates, followed by heat treatment at $1000^{\circ}C$ in air, along with a change of crystallographic structures, i.e., $NaRE(SO_4)_2{\cdot}H_2O{\rightarrow}RE(OH)_3{\rightarrow}RE_xO_y$.