• Korean Journal of Materials Research
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• v.33 no.11
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• pp.465-474
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• 2023

The effects of La³⁺ substitution for Sr²⁺-site on the crystal structure and the dielectric properties of (Ba_0.7Sr_0.3-3x/2La_x) (Ti_0.9Zr_0.1)O₃ (BSLTZ) (0.005 ≤ x ≤ 0.02) ceramics were investigated. The structural characteristics of the BSLTZ ceramics were quantitatively evaluated using the Rietveld refinement method from X-ray diffraction (XRD) data. For the specimens sintered at 1,550 ℃ for 6 h, a single phase with a perovskite structure and homogeneous microstructure were observed for the entire range of compositions. With increasing La³⁺ substitution (x), the unit cell volume decreased because the ionic size of La³⁺ (1.36 Å) ions is smaller than that of Sr²⁺ (1.44 Å) ions. With increasing La³⁺ substitution (x), the tetragonal phase fraction increased due to the A-site cation size mismatch effect. Dielectric constant (ε_r) increased with the La³⁺ substitution (x) due to the increase in tetragonality (c/a) and the average B-site bond valence of the ABO₃ perovskite. The BSLTZ ceramics showed a higher dielectric loss due to the smaller grain size than that of (Ba_0.7Sr_0.3)(Ti_0.9Zr_0.1)O₃ ceramics. BSLTZ (x = 0.02) ceramics met the X7R specification proposed by the Electronic Industries Association (EIA).

• Composites Research
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• v.36 no.5
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• pp.289-296
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• 2023

In this study, we investigated the electromagnetic properties and microwave absorption characteristics of M-type hexagonal ferrites, which are known as millimeter-wave absorbing materials, according to their calcination temperature. The M-type ferrites synthesized using a molten salt-based sol-gel method exhibited a single-phase M-type crystal structure at calcination temperatures above 850℃. The synthesized particle size increased as well with the calcination temperature. Saturation magnetization increased gradually with increasing calcination temperature, but coercivity reached a maximum at 1050℃ and then rapidly decreased. After preparing a thermoplastic polyurethane (TPU) composite containing 70 wt% of M-type ferrites, we measured the complex permittivity and permeability in the Q-band (33-50 GHz) and V-band (50-75 GHz) frequency ranges, where ferromagnetic resonance occurred. Strong magnetic loss from ferromagnetic resonance occurred in the 50 GHz band for all composite samples. Based on the measured results, we calculated the reflection loss of the TPU/M-type ferrite composite. By calculating the reflection loss of the M-type ferrite composite, the M-type ferrite calcined at 1250℃ showed excellent electromagnetic wave absorption performance of more than -20 dB at 52 GHz with a thickness of about 0.5 mm.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.37 no.3
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• pp.297-303
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• 2024

In this study, KTN heterolayer thin films were fabricated by alternately stacking films of K(Ta_0.70Nb_0.30)O₃ and K(Ta_0.55Nb_0.45)O₃ synthesized using the sol-gel method. The sintering temperature and time were 750℃ and 1 hour, respectively. All specimens exhibited a polycrystalline pseudo-cubic crystal structure, with a lattice constant of approximately 0.398 nm. The average grain size was around 130~150 nm, indicating relatively uniform sizes regardless of the number of coatings. The average thickness of a single-coated film was approximately 70 nm. The phase transition temperature of the KTN heterolayer films was found to be approximately 8~12℃. Moreover, the 6-coated KTN heterolayer film displayed an excellent dielectric constant of about 11,000. As the number of coatings increased, and consequently the film thickness, the remanent polarization increased, while the coercive field decreased. The 6-coated KTN heterolayer film exhibited a remanent polarization and coercive field of 11.4 μC/cm² and 69.3 kV/cm at room temperature, respectively. ΔT showed the highest value at a temperature slightly above the Curie temperature, and for the 6-coated KTN heterolayer film, the ΔT and ΔT/ΔE were approximately 1.93 K and 0.128×10^-6 K·m/V around 40℃, respectively.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.37 no.2
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• pp.208-214
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• 2024

This reports the electrical properties of single-crystal β-gallium oxide (β-Ga₂O₃) vertical Schottky barrier diodes (SBDs) with a different guard ring structure. The vertical Schottky barrier diodes (V-SBDs) were fabricated with two types guard ring structures, one is with metal deposited on the Al₂O₃ passivation layer (film guard ring: FGR) and the other is with vias formed in the Al₂O₃ passivation layer to allow the metal to contact the Ga₂O₃ surface (metal guard ring: MGR). The forward current values of FGR and MGR V-SBD are 955 mA and 666 mA at 9 V, respectively, and the specific on-resistance (R_on,sp) is 5.9 mΩ·cm² and 29 mΩ·cm². The series resistance (R_s) in the nonlinear section extracted using Cheung's formula was 6 Ω, 4.8 Ω for FGR V-SBD, 10.7 Ω, 6.7 Ω for MGR V-SBD, respectively, and the breakdown voltage was 528 V for FGR V-SBD and 358 V for MGR V-SBD. Degradation of electrical characteristics of the MGR V-SBD can be attributed to the increased reverse leakage current caused by the guard ring structure, and it is expected that the electrical performance can be improved by preventing premature leakage current when an appropriate reverse voltage is applied to the guard ring area. On the other hand, FGR V-SBD shows overall better electrical properties than MGR V-SBD because Al₂O₃ was widely deposited on the Ga₂O₃ surface, which prevent leakage current on the Ga₂O₃ surface.

• Clean Technology
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• v.30 no.1
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• pp.28-36
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• 2024

As demand for electric vehicles increases, the market for lithium-ion batteries is also rapidly increasing. The battery life of lithium-ion batteries is limited, so waste lithium-ion batteries are inevitably generated. Accordingly, lithium was selectively preleached from waste lithium iron phosphate (LiFePO₄, hereafter referred to as the LFP) cathode material powder among lithium ion batteries, and iron phosphate (FePO₄) powder was recovered. The recovered iron phosphate powder was mixed with alkaline sodium carbonate (Na₂CO₃) powder and heat treated to confirm its crystalline phase. The heat treatment temperature was set as a variable, and then the leaching rate and powder characteristics of each ingredient were compared after water leaching using Di-water. In this study, lithium showed a leaching rate of approximately 100%, and in the case of powder heat-treated at 800 ℃, phosphorus was leached by approximately 99%, and the leaching residue was confirmed to be a single crystal phase of Fe₂O₃. Therefore, in this study, lithium, phosphorus, and iron components were individually separated and recovered from waste LFP powder.

• The Journal of the Petrological Society of Korea
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• v.10 no.3
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• pp.179-189
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• 2001

The determination of trace concentration of U, Th and Pb was carried out for chemical dating of zircon and monazite by electron microprobe. Detection limit and error range should be considered to measure characteristic X-rays of M-line from those minerals, which are low in the ionization of atom and low peak intensity in the spectrum. The element of U, Th and Pb were simultaneously measured with 3 spectrometers equipped with PET crystal to reduce a total counting time and error due to drift of instrumental operating condition. Detection limit could be improved from increase of the peak/background ratio through adjusting pulse height analyzer about 1000 mv baseline. Under permissible maximum analytical conditions, theoretical detection limit of U, Th and Pb is down to 30 ppm (99% confidence level). The analytical result was maintained at a relative error $\pm$10% ($2{\sigma}$) in 800 ppm Pb, $\pm$5% ($2{\sigma}$) in 2330 ppm U and $\pm$10% ($2{\sigma}$) in dating from a single measurement of zircon at 15 keV and 100 nA. However, for the precise dating of zircon and monazite, if it is considered a 3 $\mu\textrm{m}$ spatial resolution, <100 ppm ($3{\sigma}$) detection limit and <$\pm$10% ($2{\sigma}$) relative error, optimum analytical conditions are given as 15~20 keV accelerating voltage, 100~200 nA beam current and 300~1200 sec total counting time. To reduce material damage by high current, there is need to be up to 3~5 $\mu\textrm{m}$ of electron beam diameter, or to use arithmetic average of multiple measuring at a shorter counting time. A younger or relatively low concentration rocks can be dated chemically by lower detection limit and improved precision resulted from increase of current and measuring time.

• Applied Microscopy
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• v.9 no.1
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• pp.57-69
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• 1979

The ultrastructural changes of embryo and endosperm cells were observed during the green fruit with embryo about $250{\mu}$ long to germination. 1. In the embryo cells of green fruit with embryo about $250{\mu}$ long, mitochondrial cristae and plastid are undifferentiated and dictyosome are occasionally observed. There are electron-opaque globoids in the vacuole and a lot of spherosomes in the outer layer of smooth endoplasmic reticulum. Endosperm is filled with spherosomes and electron-opaque protein bodies surrounded by spherosomes, and due to these, other organelle are not observed. 2. In the embryo cells of seeds with red seed coat, mitochondrial cristae are well developed, electron-opaque globoids increased, and vacuoles are enlarged. In the endosperm, however, spherosomes increased, protein bodies are enlarged, and electron-opaque globoidal crystals are dispersed within them. 3. In the procambium and epicotyl cells of dehiscent seed, Golgi vacuoles and vesicles are well developed, and mitochondrial cristae are also well differentiated. Spherosomes are numerously present and radicle cells, peripheral cells of hypocotyl, and vacuoles of cotyledon are well differentiated. Endosperm is filled with spherosomes containing electron-opaque granules and protein bodies are surrounded by a single membrane. There are acid phosphatase around globoids and spherosomes. 4. At the time of seeding, spherosomes markedly increased in the outer layer of cotyledon and protein bodies are also observed. Cell organelles are differentiated and plastids containing starch are also present. 5. In the outer $2{\sim}3$ layers of cotyledons, radicle cells, and peripheral cells of hypocotyl during post-seeding to germination, spherosomes and plastids with starch increased, and mitochondria and microbodies are also found around the nucleus of embryo cells. With approaching, the germination stage, in the endosperm contacting with embryo, vacuoles are well differentiated but spherosomes decreased. There increased electron-opaque materials within vacuoles. In other endosperm, with the decrease of spherosome, mitochondria increased and electro n-opaque globular bodies are formed and gradually increased. The outer layer of protein bodies are reduced while electron-transparent portions are enlarged and fused together to occupy the outer layer where small particles are formed. 6. In the endosperm of germination stage, spherosomes decreased while protein bodies, are fused together to form 2 or 3 within a cell.

• Journal of the Korean Chemical Society
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• v.45 no.3
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• pp.242-246
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• 2001

The quaternary thiophosphates, $A_2NiP_2S_6$ (A=Rb, Cs), have been synthesized with halide fluxes and structurally characterized by single-crystal X-ray diffraction technique. These compounds crystallize in the space group $C_{2h}^5-P2_1/n$ of the monoclinic system with two formula units in a cell of dimensions a=5.960(2), b=12.323(4), $c=7.491(3)\AA$, $\beta=97.05(3)^{\circ}$, and $V=546.0(3)\AA^3$ for Rb2NiP2S6 and a=5.957(4), b=12.696(7), $c=7.679(4)\AA$, $b=93.60(5)^{\circ}$, and $V=579.7(5)\AA^3$ for $Cs_2NiP_2S_6.$ These compounds are isostructural. The structure of $Cs_2NiP_2S_6$ is made up of one-dimensional $_\infty^1[NiP_2S_6^{2-}]$ chains along the a axis and these chains are isolated by $Cs^+$ ions. The Ni atom is octahedrally coordinated by six S atoms. These Ni$S_6$ octahedral units are linked by sharing three m-S atoms of the $[P_2S_6^{4-}]$ anions to form the infinite one-dimensional $_\infty^1[NiP_2S_6^{2-}]$ chain. For $Cs_2NiP_2S_6$, the magnetic susceptibility reveals an antiferromagnetic exchange interaction below 8K,which corresponds to the Neel temperature ($T_N$). Above $T_N$, this compound obeys Curie-Weiss law. The magnetic moment, C, and ${\theta}forCs_2NiP_2S_6$ are 2.77 B.M., 0.9593 K, and -19.02 K, respectively. The effective magnetic moment obtained from the magnetic data is agreed with the spin-only value of $Ni^{2+}d^8$(2.83 B.M.) system.

• Korean Journal of Materials Research
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• v.11 no.5
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• pp.427-430
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• 2001

We prepared 10cm-diameter Si(100)/500 $\AA$-Si$_3$N$_4$/Si(100) wafer Pairs adopting 500 $\AA$ -thick Si$_3$N$_4$layer as insulating layer between single crystal Si wafers. Si3N, is superior to conventional SiO$_2$ in insulating. We premated a p-type(100) Si wafer and 500 $\AA$ -thick LPCVD Si$_3$N$_4$∥Si (100) wafer in a class 100 clean room. The cremated wafers are separated in two groups. One group is treated to have hydrophobic surface and the other to have hydrophilic. We employed a FLA(fast linear annealing) bonder to enhance the bond strength of cremated wafers at the scan velocity of 0.1mm/sec with varying the heat input at the range of 400~1125W. We measured bonded area using a infrared camera and bonding strength by the razor blade crack opening method. We used high resolution transmission electron microscopy(HRTEM) to probe cross sectional view of bonded wafers. The bonded area of two groups was about 75%. The bonding strength of samples which have hydrophobic surface increased with heat input up to 1577mJ/$m^2$ However, bonding strength of samples which have hydrophilic surface was above 2000mJ/$m^2$regardless of heat input. The HRTEM results showed that the hydrophilic samples have about 25 $\AA$ -thick SiO layer between Si and Si$_3$N$_4$/Si and that maybe lead to increase of bonding strength.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2008.06a
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• pp.239-240
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• 2008

As semiconductor devices are scaled down for better performance and more functionality, the Cu-based interconnects suffer from the increase of the resistivity of the Cu wires. The resistivity increase, which is attributed to the electron scattering from grain boundaries and interfaces, needs to be addressed in order to further scale down semiconductor devices [1]. The increase in the resistivity of the interconnect can be alleviated by increasing the grain size of electroplating (EP)-Cu or by modifying the Cu surface [1]. Another possible solution is to maximize the portion of the EP-Cu volume in the vias or damascene structures with the conformal diffusion barrier and seed layer by optimizing their deposition processes during Cu interconnect fabrication, which are currently ionized physical vapor deposition (IPVD)-based Ta/TaN bilayer and IPVD-Cu, respectively. The use of in-situ etching, during IPVD of the barrier or the seed layer, has been effective in enlarging the trench volume where the Cu is filled, resulting in improved reliability and performance of the Cu-based interconnect. However, the application of IPVD technology is expected to be limited eventually because of poor sidewall step coverage and the narrow top part of the damascene structures. Recently, Ru has been suggested as a diffusion barrier that is compatible with the direct plating of Cu [2-3]. A single-layer diffusion barrier for the direct plating of Cu is desirable to optimize the resistance of the Cu interconnects because it eliminates the Cu-seed layer. However, previous studies have shown that the Ru by itself is not a suitable diffusion barrier for Cu metallization [4-6]. Thus, the diffusion barrier performance of the Ru film should be improved in order for it to be successfully incorporated as a seed layer/barrier layer for the direct plating of Cu. The improvement of its barrier performance, by modifying the Ru microstructure from columnar to amorphous (by incorporating the N into Ru during PVD), has been previously reported [7]. Another approach for improving the barrier performance of the Ru film is to use Ru as a just seed layer and combine it with superior materials to function as a diffusion barrier against the Cu. A RulTaN bilayer prepared by PVD has recently been suggested as a seed layer/diffusion barrier for Cu. This bilayer was stable between the Cu and Si after annealing at $700^{\circ}C$ for I min [8]. Although these reports dealt with the possible applications of Ru for Cu metallization, cases where the Ru film was prepared by atomic layer deposition (ALD) have not been identified. These are important because of ALD's excellent conformality. In this study, a bilayer diffusion barrier of Ru/TaCN prepared by ALD was investigated. As the addition of the third element into the transition metal nitride disrupts the crystal lattice and leads to the formation of a stable ternary amorphous material, as indicated by Nicolet [9], ALD-TaCN is expected to improve the diffusion barrier performance of the ALD-Ru against Cu. Ru was deposited by a sequential supply of bis(ethylcyclopentadienyl)ruthenium [Ru$(EtCp)_2$] and $NH_3$plasma and TaCN by a sequential supply of $(NEt_2)_3Ta=Nbu^t$ (tert-butylimido-trisdiethylamido-tantalum, TBTDET) and $H_2$ plasma. Sheet resistance measurements, X-ray diffractometry (XRD), and Auger electron spectroscopy (AES) analysis showed that the bilayer diffusion barriers of ALD-Ru (12 nm)/ALD-TaCN (2 nm) and ALD-Ru (4nm)/ALD-TaCN (2 nm) prevented the Cu diffusion up to annealing temperatures of 600 and $550^{\circ}C$ for 30 min, respectively. This is found to be due to the excellent diffusion barrier performance of the ALD-TaCN film against the Cu, due to it having an amorphous structure. A 5-nm-thick ALD-TaCN film was even stable up to annealing at $650^{\circ}C$ between Cu and Si. Transmission electron microscopy (TEM) investigation combined with energy dispersive spectroscopy (EDS) analysis revealed that the ALD-Ru/ALD-TaCN diffusion barrier failed by the Cu diffusion through the bilayer into the Si substrate. This is due to the ALD-TaCN interlayer preventing the interfacial reaction between the Ru and Si.