• Korean Chemical Engineering Research
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• v.57 no.4
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• pp.445-454
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• 2019

Layered double hydroxides (LDHs) nanoparticles have emerged as novel nanomaterials for bio-imaging applications due to its unique layered structure, physicochemical properties, and good biocompatibility. Bio-imaging is one of the most important fields for medical applications in clinical diagnostics and therapeutics of various diseases. Enhanced diagnostic techniques are needed to realize new paradigm for next-generation personalized medicine through nanoscale materials. When nanotechnology is introduced into bio-imaging system, nanoparticle probes can endow imaging techniques with enhanced ability to obtain information about biological system at the molecular level. In this review, we summarize structural features of LDH nanoparticles with current issues of bio-imaging system. LDH nanoparticle probes are also discussed through in vitro as well as in vivo studies in various bio-imaging techniques including fluorescence imaging, magnetic resonance imaging (MRI), positron emission tomography (PET), and computed X-ray tomography (CT), which will have the potential in the development of the advanced nanoparticles with high sensitivity and selectivity.

• Economic and Environmental Geology
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• v.56 no.1
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• pp.23-53
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• 2023

In this review paper, previous studies on layered double hydroxides (LDHs) published in the Korean Citation Index (KCI) were examined to investigate a research trend for LDHs in Korea. Since the first publication in 2002, 160 papers on LDHs have been published until January 2023. Among the 31 academic fields, top 5 fields appeared in the order of chemical engineering, chemistry, materials engineering, environmental engineering, and physics. The chemical engineering shows the highest record of published paper (71 papers) while around 10 papers have been published in the other four fields. All papers were reclassified into 15 research fields based on the industrial and academic purposes of using LDHs. The top 5 in these fields are in order of environmental purification materials, polymer catalyst materials, battery materials, pharmaceutical/medicinal materials, and basic physicochemical properties. These findings suggest that researches on the applications of LDH materials in the academic fields of chemical engineering and chemistry for the improvement of their functions such as environmental purification materials, polymer catalysts, and batteries have been being most actively conducted. The application of LDHs for cosmetic and agricultural purposes and for developing environmental sensors is still at the beginning of research. Considering a market-potential and high-efficiency-eco-friendly trend, however, it will deserve our attention as emerging application fields in the future. All reclassified papers were summarized in our tables and a supplementary file, including information on applied materials, key results, characteristics and synthesis methods of LDHs used. We expect that our findings of overall trends in LDH research in Korea can help design future researches with LDHs and suggest policies for resources and energies as well as environments efficiently.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.31 no.3
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• pp.143-148
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• 2021

Alkaline oxygen evolution reaction (OER) electrocatalysts have been widely studied for improving the efficiency and green hydrogen production through electrochemical water splitting. Transition metal-based electrocatalysts have emerged as promising materials that can significantly reduce the hydrogen production costs. Among the available electrocatalysts, transition metal-based layered double hydroxides (LDHs) have demonstrated outstanding OER performance owing to the abundant active sites and favorable adsorption-desorption energies for OER intermediates. Currently, cobalt doped nickel LDHs (NiCo LDHs) are regarded as the benchmark electrocatalyst for alkaline OER, primarily owing to the physicochemical synergetic effects between Ni and Co. We report effects of heat-treatment of the as-grown NiCo LDH on electrocatalytic activities in a temperature range from 250 to 400℃. Electrocatalytic OER properties were analysed by linear sweep voltammetry (LSV) and electrochemical impedance spectroscopy (EIS). The heat-treatment temperature was found to play a crucial role in catalytic activity. The optimum heat-treatment temperature was discussed with respect to their OER performance.

• Journal of Environmental Science International
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• v.23 no.7
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• pp.1333-1338
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• 2014

LDHs(layered double hydroxides) are of use adsorbent to remove heavy metals, micro-organic pollutants as well as high concentration of phosphorus from wastewater to low concentration of surface water without pH adjustments. This study examined the generation condition of LDHs saturated with phosphorus. Less than 20% regeneration rate was obtained in the absence of alkali and regeneration solution. After the desorption of LDHs with several conditions of acid and alkali solution, more than 60% of regeneration rate could be expected in the case of using $MgCl_2$ as regeneration solution.

• Clean Technology
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• v.28 no.2
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• pp.154-162
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• 2022

Microstructured Al@Al₂O₃ and Al@Ni-Al LDH (LDH = layered double hydroxide) core-shell metal-ceramic composites are prepared by hydrothermal reactions of aluminum (Al) metal substrates. Controlled hydrothermal reactions of Al metal substrates induce the hydrothermal dissolution of Al ions at the Al-substrate/solution interface and reconstruction as porous metal-hydroxides on the Al substrate, thereby constructing unique metal-ceramic core-shell composite structures. The morphology, composition, and crystal structure of the core-shell composites are affected largely by the ions in the hydrothermal solution; therefore, the critical physicochemical and surface properties of these unique metal-ceramic core-shell microstructures can be modulated effectively by varying the solution composition. A Ni/Al@Al₂O₃ catalyst with highly dispersed catalytic Ni nanoparticles on an Al@Al₂O₃ core-shell substrate was prepared by a controlled reduction of an Al@Ni-Al LDH core-shell prepared by hydrothermal reactions of Al in nickel nitrate solution. The reduction of Al@Ni-Al LDH leads to the exolution of Ni ions from the LDH shell, thereby constructing the Ni nanoparticles dispersed on the Al@Al₂O₃. The catalytic properties of the Ni/Al@Al₂O₃ catalyst were investigated for CO₂ methanation reactions. The Ni/Al@Al₂O₃ catalyst exhibited 2 times greater CO₂ conversion than a Ni/Al₂O₃ catalyst prepared by conventional incipient wetness impregnation and showed high structural stability. These results demonstrate the high effectiveness of the design and synthesis methods for the metal-ceramic composite catalysts derived by hydrothermal reactions of Al metal substrates.

• Proceedings of the Korean Vacuum Society Conference
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• 2016.02a
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• pp.371.1-371.1
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• 2016

다양한 물질계의 2차원 나노구조는 그래핀과 함께 그 고유특성으로 최근 광전소자, 전자소자, 센서, 에너지 생성 및 저장과 수소에너지 생성 등의 응용으로 매우 많은 관심을 받고 있다. 특히 층상이중수산화물 (layered-double hydroxide; LDH) 2차원 나노구조는 생성의 용이성과 층상 내 금속 이온의 교환을 통한 특성의 자유로운 제어가 가능하므로 많은 관심을 받고 있다. 층상이중수산화물 화합물은 [Zn(1-x) MIII(x)(OH)2][$An-x/n{\cdot}mH2O$] (MIII = Al, Cr, Ga; An- = CO32-, Cl-, NO3-, CH3COO-) 구조로써, Brucite-type 구조 내에서 3가 양이온의 상태에 따라서 다양한 특성을 제어할 수 있는 장점이 있다. 이러한 장점으로 인해 층상이중수산화물 화합물은 촉매나, 에너지 저장, 음이온 교환 및 흡착, 화학적 촉매, 바이오 소자 등에 응용이 연구되고 있으며, 다양한 금속 산화물을 제조하기 위한 중간자 precursor로써도 연구되고 있다. 하지만, 이러한 대부분의 연구들을 통한 결과물들이 분말 및 수용액 상태로 남게 되며, 이러한 화합물의 특성을 제어하기 어려운 문제점이 있다. 더욱이 이러한 나노구조물들을 다양한 소자로 응용하기 위해서는 상용의 실리콘이나 glass 등의 기판형태의 물질상에 성장시킬 수 있어야 하며, 그러한 기판 위에서의 형상 및 특성 제어가 용이해야 한다. 따라서 본 연구에서는 실리콘 기판을 적용한 Zn기반의 층상이중 수산화물 화합물을 성장하고, 하부물질의 조성제어를 통한 층상이중수산화물 화합물의 형상제어가 가능한 기술에 관한 연구를 보고하고자 한다. 이를 위한 하부물질의 조성은 Zn와 Al을 통해 이루어지며, 기형성된 Al2O3박막을 핵형성층으로 활용한다. 이러한 방법으로 형성된 층상이중수산화물 화합물에 대해 이차전자주사현미경, 투과전자현미경 및 X-ray회절기법을 통해 구조분석을 하고, Raman 및 광발광스펙트럼 분석을 통해 광학적 분석을 시행함으로써, 층상이중수산화물이 기판상에서 형성되는 메커니즘에 관한 규명을 시행하였다. 이러한 분석연구를 통해 핵형성층의 에칭 따라 실리콘 기판상에서 성장하는 층상이 중수산화물 화합물의 형상 및 조성이 제어되는 메커니즘을 구명하였다.

• Economic and Environmental Geology
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• v.57 no.5
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• pp.577-592
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• 2024

This study presents the synthesis and characterization of MgAl-layered double hydroxide (LDH)/rice husk hydrochar (RHH) nanocomposites (MgAl-LDH/RHHs) via an in situ one-pot hydrothermal route at 150 ℃, utilizing Mg:Al molar ratio of 2:1 for arsenic remediation. The formation of MgAl-LDH/RHHs and their physicochemical properties were evaluated under varying hydrothermal aging times systematically. Prolonging the aging period to 12 hrs significantly enhanced the crystallinity and crystal size of the LDHs, resulting in a 3D hierarchical structure with the highest specific surface area (27.98 m²/g) formed on the hydrochar surface. The hexagonal crystal structure (d₀₀₃ = 0.8246 nm) was characterized by a rhombohedral unit cell with lattice parameters a = 0.3049 nm and c = 2.4738 nm, and a high positive charge density of 4.284 e/nm². These properties were found to be favorable for the sorption of arsenic oxyanions. Batch adsorption experiments were conducted to assess the potential of MgAl-LDH/RHHs-12h for the remediation of arsenic-contaminated soils. The original soil sample (CY) was mechanically sieved into fine-grained (CYF, < 75 ㎛) and coarse-grained (CYC, 75 ㎛-2 mm) fractions. When these soil samples were reacted with deionized water, arsenate was identified as the dissolved arsenic species, with concentrations of 2.85 mg/L for CY, 4.02 mg/L for CYF, and 2.55 mg/L for CYC, respectively. Kinetic sorption experiments, conducted at pH 5.0 and 8.0 in the presence and absence of 0.1 M NaCl as a background electrolyte, revealed that arsenic sorption onto MgAl-LDH/RHHs-12h was inhibited at pH 8 in the presence of NaCl. These findings suggest that effective arsenic sorption requires low pH conditions with minimal background electrolytes in soils.

• Journal of the Korean Chemical Society
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• v.39 no.8
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• pp.627-634
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• 1995

Layered double hydroxides ($Mg-Al-CO_3$ systems, LDH), which are hydrotalcite-like anionic clay minerals, having different $Mg^{2+}\;to\;Al^{3+}$ ratio were synthesized by coprecipitation method. The subsequent products were characterized by the following methods; elemental analysis, X-ray powder diffraction, thermal analysis (DSC and TGA), FT-IR and $^{27}$Al-MAS NMR. X-ray powder patterns showed that the products formed were layered structure materials. Two heat absorption peaks were observed around 20 ∼280$^{\circ}C$ (surface water and interlayer water) and 280∼500$^{\circ}C$ (water from lattice hydroxide and carbon dioxide from interlayer carbonate) in DSC diagrams, and they were quantitatively analyzed by TGA diagrams (in case LDH4 16.2% and 28.6% respectively). FT-IR spectra indicate that the interlayer carbonate ions occupied symmetrical sites between two adjacent layers in a parallel direction. $^{27}$Al-MAS NMR spectra show only single resonance (8.6 ppm) of the octahedrally coordinated aluminum similar magnesium. When LDH4 was calcined at 560$^{\circ}C$ for 3 hours in air, its layered structure was destroyed giving a mixed metal oxide. However it readily became rehydrated in aqueous chromate solution to its original structure.

• Bulletin of the Korean Chemical Society
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• v.23 no.1
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• pp.35-40
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• 2002

Photoreaction of guest organic anions in layered organic-inorganic hybrid materials was investigated. The layered hybrids were synthesized by an anion-exchange reaction of $[LiAl_2(OH)_6]Cl{\cdot}yH_2O$ layered double hydroxide with aqueous (Z,Z)- and (E,E)-muconates under inert atmospheric condition, to give new organicinorganic hybrids of $[LiAl_2(OH)_6]_2[(Z,Z)-C_6H_4O_4]{\cdot}zH_2O$ and $[LiAl_2(OH)_6]_2[(E,E)-C_6H_4O_4]{\cdot}H_2O$, respectively. The basal spacings calculated by XRPD of intercalates indicate that muconate anions have almost vertical arrangements against the host $[LiAl_2(OH)_6]^+$ lattices in the interlayer of organic-inorganic hybrid materials. When UV light was irradiated on the suspension of $[LiAl_2(OH)_6]_2[(Z,Z)-C_6H_4O_4]{\cdot}zH_2O$, the (Z,Z)-muconate anions of the gallery space of hybrids were polymerized in the aqueous media while it was isomerized into more stable (E,E)-muconate in the methanollic suspension in the presence of catalytic amount of molecular iodine. All the products were characterized using elemental analysis, TGA, XRPD, FT-IR, $^1H$ NMR and $^{13}C$ CP-MAS NMR.

• Journal of Surface Science and Engineering
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• v.56 no.5
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• pp.299-308
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• 2023

In this study, phosphorus (P)-doped nickel cobaltite (P-NiCo₂O₄) and nickel-cobalt layered double hydroxide (P-NiCo-LDH) were synthesized on nickel (Ni) foam as a conductive support using hydrothermal synthesis. The thermal properties, crystal structure, microscopic surface morphology, chemical distribution, electronic state of the constituent elements on the sample surface, and electrical properties of the synthesized P-NiCo₂O₄ and P-NiCo-LDH samples were analyzed using thermogravimetric analysis-differential scanning calorimetry (TGA-DSC), X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), galvanostatic charge-discharge (GCD), and electrochemical impedance spectroscopy (EIS). The P-NiCo₂O₄ electrode exhibited a specific capacitance of 1,129 Fg^-1 at a current density of 1 Ag^-1, while the P-NiCo-LDH electrode displayed a specific capacitance of 1,012 Fg^-1 at a current density of 1 Ag-1. When assessing capacity changes for 3,000 cycles, the P-NiCo₂O₄ electrode exhibited a capacity retention rate of 54%, whereas the P-NiCo-LDH electrode showed a capacity retention rate of 57%.