A 1.8 μm thick polycrystalline diamond (PCD) thin film layer is prepared on a Si(100) substrate using hot-filament chemical vapor deposition. Thereafter, its thermal conductivity is measured using the conventional laser flash analysis (LFA) method, a LaserPIT-M2 instrument, and the newly proposed light source thermal analysis (LSTA) method. The LSTA method measures the thermal conductivity of the prepared PCD thin film layer using an ultraviolet (UV) lamp with a wavelength of 395 nm as the heat source and a thermocouple installed at a specific distance. In addition, the microstructure and quality of the prepared PCD thin films are evaluated using an optical microscope, a field emission scanning electron microscope, and a micro-Raman spectroscope. The LFA, LaserPIT-M2, and LSTA determine the thermal conductivities of the PCD thin films, which are 1.7, 1430, and 213.43 W/(m·K), respectively, indicating that the LFA method and LaserPIT-M2 are prone to errors. Considering the grain size of PCD, we conclude that the LSTA method is the most reliable one for determining the thermal conductivity of the fabricated PCD thin film layers. Therefore, the proposed LSTA method presents significant potential for the accurate and reliable measurement of the thermal conductivity of PCD thin films.
Various surface colors are predicted and implemented using the interference color generated by controlling the thickness of nano-level diamond like carbon (DLC) thin film. Samples having thicknesses of up to 385 nm and various interference colors are prepared using a single crystal silicon (100) substrate with changing processing times at low temperature by plasma-enhanced chemical vapor deposition. The thickness, surface roughness, color, phases, and anti-scratch performance under each condition are analyzed using a scanning electron microscope, colorimeter, micro-Raman device, and scratch tester. Coating with the same uniformity as the surface roughness of the substrate is possible over the entire experimental thickness range, and more than five different colors are implemented at this time. The color matched with the color predicted by the model, assuming only the reflection mode of the thin film. All the DLC thin films show constant D/G peak fraction without significant change, and have anti-scratch values of about 19 N. The results indicate the possibility that nano-level DLC thin films with various interference colors can be applied to exterior materials of actual mobile devices.
We confirm whether Zr powders can restrain a rapid nitrification reaction and offer a stable oxidation reaction according to temperatures in nitrogen gas purification. A pellet-type, porous Zr getter is prepared (diameter: 10 and thickness: 3 mm) using Zr powder with an average particle size of 45 μm. While maintaining the whole system, the Zr getter reaction is confirmed with an increase in temperature from 150 to 550 oC at increments of 100 oC under 99.999 % purity nitrogen atmosphere comprising of 10 ppm of impurity. Surface color, pore size, stabilized layer, and phase change are confirmed with optical microscopy, SEM-EDS, Micro-Raman, and X-ray diffraction (XRD) according to the Zr getter temperature. The surface color of the Zr getter changes from metallic silver to dark gray as temperature increases. In the EDS results, the nitrogen component is not observed, and oxygen content increases from each surface at elevated temperatures. The Raman and XRD results show the oxidation layer as a result of 350 oC annealing. Therefore, the Zr getter can be applied as a nitrogen getter under 5-nine purity nitrogen atmosphere after appropriate oxidized pre-stabilization process to prevent rapid nitrification reaction.
The photovoltaic properties of perovskite solar cells (PSCs) with a carbon electrode fabricated using different annealing processes are investigated. Perovskite formation (50 oC, 60 min) using a hot-plate and an oven is carried out on cells with a glass/fluorine doped TiO2/TiO2/ZrO2/carbon structure, and the photovoltaic properties of the PSCs are analyzed using a solar simulator. The microstructures of the PSCs are characterized using an optical microscope, a field emission scanning electron microscope, and an electron probe micro-analyzer (EPMA). Photovoltaic analysis shows that the energy conversion efficiency of the samples fabricated using the hot-plate and the oven processes are 2.08% and 6.90%, respectively. Based on the microstructure of the samples and the results of the EPMA, perovskite is formed locally on the carbon electrode surface as the γ-butyrolactone (GBL) solvent evaporates and moves to the top of the carbon electrode due to heat from the bottom of the sample during the hot plate process. When the oven process is used, perovskite forms evenly inside the carbon electrode, as the GBL solvent evaporates extremely slowly because heat is supplied from all directions. The importance of the even formation of perovskite inside the carbon electrode is emphasized, and the feasibility of oven annealing is confirmed for PSCs with carbon electrodes.
We propose a novel stripping solution containing acids (HCl and HNO3), an oxidant [(NH4)2S2O8], and complexing agents (NaCl and citric acid) to remove surface passivation layers from 14K gold alloys fabricated using an investment casting process. The optimized solution employing only HCl acid is determined by varying molar fractions of HCl and HNO3 on 14K yellow gold samples. Stripping properties are also identified for red and white gold alloy samples under the optimized stripping conditions. The removal of passivation layers, weight loss, and microstructure evolution are characterized using Raman spectroscopy, a precision scale, and optical microscopy. The proposed stripping solution effectively removes passivation layers more rapidly than conventional cyanide stripping. Weight loss increases linearly for up to 5 min for all 14K gold alloys. Red gold exhibits the greatest weight loss, followed by yellow gold and white gold. The results of microstructural analysis reveal that the conformal stripping occurs according to time. These results imply that the proposed oxidative chloride stripping might replace conventional cyanide stripping.
The photovoltaic properties of TiO2 used for the electron transport layer in perovskite solar cells(PSCs) are compared according to the particle size. The PSCs are fabricated and prepared by employing 20 nm and 30 nm TiO2 as well as a 1:1 mixture of these particles. To analyze the microstructure and pores of each TiO2 layer, a field emission scanning electron microscope and the Brunauer–Emmett–Teller(BET) method are used. The absorbance and photovoltaic characteristic of the PSC device are examined over time using ultraviolet-visible-near-infrared spectroscopy and a solar simulator. The microstructural analysis shows that the TiO2 shape and layer thicknesses are all similar, and the BET analysis results demonstrate that the size of TiO2 and in surface pore size is very small. The results of the photovoltaic characterization show that the mean absorbance is similar, in a range of about 400-800 nm. However, the device employing 30 nm TiO2 demonstrates the highest energy conversion efficiency(ECE) of 15.07 %. Furthermore, it is determined that all the ECEs decrease over time for the devices employing the respective types of TiO2. Such differences in ECE based on particle size are due to differences in fill factor, which changes because of changes in interfacial resistance during electron movement owing to differences in the TiO2 particle size, which is explained by a one-dimensional model of the electron path through various TiO2 particles.
To produce carbon electrodes for use in perovskite solar cells, electrode samples are prepared by mixing various weight ratios of 35 nm nano carbon(NC) and 1 μm graphite flakes(GF), GF/(NC+GF) = 0, 0.5, 0.7, and 1, in chlorobenzene(CB) solvent with a ZrO2 binder. The carbon electrodes are fabricated as glass/FTO/carbon electrode devices for microstructure characterization using transmission electron microscopy, optical microscopy, and a field emission scanning electron microscopy. The electrical characterization is performed with a four-point probe and a multi tester. The microstructure characterization shows that an electrode with excellent attachment to the substrate and no surface cracks at weight ratios above 0.5. The electrical characterization results show that the sheet resistance is < 70 Ω/sq and the interface resistance is < 70 Ω at weight ratios of 0.5 and 0.7. Therefore, a carbon paste electrode with microstructure and electrical properties similar to those of commercial carbon electrodes is proposed with an appropriate mixing ratio of NC and GF containing a CB solvent and ZrO2.
We propose a speedy two-step deposit process to form an Au electrode on hole transport layer(HTL) without any damage using a general thermal evaporator in a perovskite solar cell(PSC). An Au electrode with a thickness of 70 nm was prepared with one-step and two-step processes using a general thermal evaporator with a 30 cm source-substrate distance and 6.0 × 10−6 torr vacuum. The one-step process deposits the Au film with the desirable thickness through a source power of 60 and 100 W at a time. The two-step process deposits a 7 nm-thick buffer layer with source power of 60, 70, and 80 W, and then deposits the remaining film thickness at higher source power of 80, 90, and 100W. The photovoltaic properties and microstructure of these PSC devices with a glass/FTO/TiO2/perovskite/ HTL/Au electrode were measured by a solar simulator and field emission scanning electron microscope. The one-step process showed a low depo-temperature of 88.5 oC with a long deposition time of 90 minutes at 60 W. It showed a high depo-temperature of 135.4 oC with a short deposition time of 8 minutes at 100 W. All the samples showed an ECE lower than 2.8% due to damage on the HTL. The two-step process offered an ECE higher than 6.25% without HTL damage through a deposition temperature lower than 88 oC and a short deposition time within 20 minutes in general. Therefore, the proposed two-step process is favorable to produce an Au electrode layer for the PSC device with a general thermal evaporator.
The property changes of 18, 14, and 8K green gold alloys for jewelry are observed by adding 0.0, 3.0, and 5.0 wt% of indium (In), respectively. To check the composition of the alloys, an energy dispersive spectroscopy (EDS) analysis is conducted. Color and microstructure analysis is executed through bare-eye, macro camera, UV-VIS-NIR-colormeter, and optical microscope. The melting point, wetting angle, and hardness are measured using TGA-DTA, a wetting angle tester, and a Vickers hardness tester. The EDS analysis result demonstrates that each of the green gold alloys was manufactured with purposed contents. The color analysis result shows that the color of the alloys is similar to the color of the conventional 4 wt%- Cd 18K green gold, and the green color improves as the In content increases. The micro structure analysis result demonstrates that grain refinement improves as the amount of In increases. Enhancements in the melting point, wettability, and Vickers hardness changes appear as the In content increases and Au content decreases. The hardness is up to 260, which implies good durability. Therefore, the results suggest that the proposed 18, 14, and 8K In-added green gold alloys enhance the properties of jewelry products with regard to the green color, castability, and durability.
The properties of 18 K red gold solder alloys were investigated by changing the content of In up to 10.0 wt% in order to replace the hazardous Cd element. Cupellation and energy dispersive X-ray spectroscopy (EDS) were used to check the composition of each alloy, and FE-SEM and UV-VIS-NIR-Colormeter were employed for microstructure and color characterization. The melting temperature, hardness, and wetting angle of the samples were determined by TGA-DTA, the Vickers hardness tester, and the Wetting angle tester. The cupellation result confirmed that all the samples had 18K above 75.0wt%-Au. EDS results showed that Cu and In elements were alloyed with the intended composition without segregation. The microstructure results showed that the amount of In increased, and the grain size became smaller. The color analysis revealed that the proposed solders up to 10.0 wt% In showed a color similar to the reference 18 K substrate like the 10.0 wt% Cd solder with a color difference of less than 7.50. TGA-DTA results confirmed that when more than 5.0 wt% of In was added, the melting temperature decreased enough for the soldering process. The Vickers hardness result revealed that more than 5.0 wt% In solder alloys had greater hardness than 10.0 wt% Cd solder, which suggested that it was more favorable in making a wire type solder. Moreover, all the In solders showed a lower wetting angle than the 10.0 wt% Cd solder. Our results suggested that the In alloyed 18 K red gold solders might replace the conventional 10.0 wt% Cd solder with appropriate properties for red gold jewelry soldering.
Using a customized diffusion bonder, we executed diffusion bonding for ring shaped white gold and red gold samples (inner, outer diameter, and thickness were 15.7, 18.7, and 3.0 mm, respectively) at a temperature of 780 °C and applied pressure of 2300 N in a vacuum of 5 × 10−2 torr for 180 seconds. Optical microscopy, field emission scanning electron microscopy (FE-SEM), and energy-dispersive X-ray spectroscopy (EDS) were used to investigate the microstructure and compositional changes. The mechanical properties were confirmed by Vickers hardness and shear strength tests. Optical microscopy and FE-SEM confirmed the uniform bonding interface, which was without defects such as micro pores. EDS mapping analysis confirmed that each gold alloy was 14K with the intended composition; Ni and Cu was included as coloring metals in the white and red gold alloys, respectively. The effective diffusion coefficient was estimated based on EDS line scanning. Individual values of Ni and Cu were 5.0 × 10−8 cm2/s and 8.9 × 10−8 cm2/s, respectively. These values were as large as those of the melting points due to the accelerated diffusion in this customized diffusion bonder. Vickers hardness results showed that the hardness values of white gold and red gold were 127.83 and 103.04, respectively, due to solid solution strengthening. In addition, the value at the interface indicated no formation of intermetallic compound around the bonding interface. From the shear strength test, the sample was found not to be destroyed at up to 100,000 gf due to the high bonding strength. Therefore, these results confirm the successful diffusion bonding of 14K white-red golds with a diffusion bonder at a low temperature of 780 °C and a short processing time of 180 seconds.
In order to replace 14K white gold alloys, the properties of 5K white gold alloys (Au20-Ag80) were investigated by changing the contents of In (0.0-10.0 wt%). Energy dispersive X-ray spectroscopy (EDS) was used to determine the precise content of alloys. Properties of the alloys such as hardness, melting point, color difference, and corrosion resistance were determined using Vickers Hardness test, TGA-DTA, UV-VIS-NIR-colorimetry, and salt-spray tests, respectively. Wetting angle analysis was performed to determine the wettability of the alloys on plaster. The results of the EDS analysis confirmed that the Au-Ag-In alloys had been fabricated with the intended composition. The results of the Vickers hardness test revealed that each Au-Ag-In alloy had higher mechanical hardness than that of 14K white gold. TGA-DTA analysis showed that the melting point decreased with an increase in the In content. In particular, the alloy containing 10.0 wt% In showed a lower melting temperature (> 70 °C) than the other alloys, which implied that alloys containing 10.0 wt% In can be used as soldering materials for Au-Ag-In alloys. Color difference analysis also revealed that all the Au-Ag-In alloys showed a color difference of less than 6.51 with respect to 14K white gold, which implied a white metallic color. A 72-h salt-spray test confirmed that the Au-Ag- In alloys showed better corrosion resistance than 14K white gold alloys. All Au-Ag-In alloys showed wetting angle similar to that of 14K white gold alloys. It was observed that the 10.0 wt% In alloy had a very small wetting angle, further confirming it as a good soldering material for white metals. Our results show that white 5K Au-Ag-In alloys with appropriate properties might be successful substitutes for 14K white gold alloys.
Dinickel-silicide (Ni2Si)/glass was employed as a counter electrode for a dye-sensitized solar cell (DSSC) device. Ni2Si was formed by rapid thermal annealing (RTA) at 700 oC for 15 seconds of a 50 nm-Ni/50 nm-Si/glass structure. For comparison, Ni2Si on quartz was also prepared through conventional electric furnace annealing (CEA) at 800 oC for 30 minutes. XRD, XPS, and EDS line scanning of TEM were used to confirm the formation of Ni2Si. TEM and CV were employed to confirm the microstructure and catalytic activity. Photovoltaic properties were examined using a solar simulator and potentiostat. XRD, XPS, and EDS line scanning results showed that both CEA and RTA successfully led to tne formation of nano thick- Ni2Si phase. The catalytic activity of CEA-Ni2Si and RTA-Ni2Si with respect to Pt were 68 % and 56 %. Energy conversion efficiencies (ECEs) of DSSCs with CEA-Ni2Si and RTA-Ni2Si catalysts were 3.66 % and 3.16 %, respectively. Our results imply that nano-thick Ni2Si may be used to replace Pt as a reduction catalytic layer for a DSSCs. Moreover, we show that nanothick Ni2Si can be made available on a low-cost glass substrate via the RTA process.
We improve the energy conversion efficiency (ECE) of a dye sensitized solar cell (DSSC) by preparing a working electrode (WE) with localized surface plasmon resonance (LSPR) by inducing Au thin films with thickness of 0.0 to 5.0 nm, deposited via sputtering. Field emission scanning electron microscopy and atomic force microscopy were used to characterize the microstructure of the blocking layer (BL) of the Au thin films. Micro-Raman measurement was employed to confirm the LSPR effect, and a solar simulator and potentiostat were used to evaluate the photovoltaic properties, including the impedance and the I-V of the DSSC of the Au thin films. The results of the microstructural analysis confirmed that nano-sized Au agglomerates were present at certain thicknesses. The photovoltaic results show that the ECE reached a value of 5.34% with a 1-nm thick-Au thin film compared to the value of 5.15 % without the Au thin film. This improvement was a result of the increase in the LSPR of the TiO2 layer that resulted from the Au thin film coating. Our results imply that the ECE of a DSSC may be improved by coating with a proper thickness of Au thin film on the BL.
The cobalt silicides were investigated for employment as a catalytic layer for a DSSC. Using an E-gun evaporation process, we prepared a sample of 100 nm-thick cobalt on a p-type Si (100) wafer. To form cobalt silicides, the samples were annealed at temperatures of 300 oC, 500 oC, and 700 oC for 30 minutes in a vacuum. Four-point probe, XRD, FE-SEM, and CV analyses were used to determine the sheet resistance, phase, microstructure, and catalytic activity of the cobalt silicides. To confirm the corrosion stability, we also checked the microstructure change of the cobalt silicides after dipping into iodide electrolyte. Through the sheet resistance and XRD results, we determined that Co2Si, CoSi, and CoSi2 were formed successfully by annealing at 300 oC, 500 oC, and 700 oC, respectively. The microstructure analysis results showed that all the cobalt silicides were formed uniformly, and CoSi and CoSi2 layers were very stable even after dipping in the iodide electrolyte. The CV result showed that CoSi and CoSi2 exhibit catalytic activities 67 % and 54 % that of Pt. Our results for Co2Si, CoSi, and CoSi2 revealed that CoSi and CoSi2 could be employed as catalyst for a DSSC.
We prepared polymethyl methacrylate (PMMA) beads with a particle size of 80 nm to improve the energy conversion efficiency (ECE) by increasing the effective surface area and the dye absorption ability of the working electrodes (WEs) in a dye sensitized solar cell (DSSC). We prepared the TiO2 layer with PMMA beads of 0.0~1.0 wt%; then, finally, a DSSC with 0.45 cm2 active area was obtained. Optical microscopy, transmission electron microscopy, field emission scanning electron microscopy, and atomic force microscopy were used to characterize the microstructure of the TiO2 layer with PMMA. UV-VIS-NIR was used to determine the optical absorbance of the WEs with PMMA. A solar simulator and a potentiostat were used to determine the photovoltaic properties of the PMMA-added DSSC. Analysis of the microstructure showed that pores of 200 nm were formed by the decomposition of PMMA. Also, root mean square values linearly increased as more PMMA was added. The absorbance in the visible light regime was found to increase as the degree of PMMA dispersion increased. The ECE increased from 4.91% to 5.35% when the amount of PMMA beads added was increased from 0.0 to 0.4 wt%. However, the ECE decreased when more than 0.6 wt% of PMMA was added. Thus, adding a proper amount of PMMA to the TiO2 layer was determined to be an effective method for improving the ECE of a DSSC.
To alloy high melting point elements such as boron, ruthenium, and iridium with copper, heat treatment was performed using metal oxides of B2O3, RuO2, and IrO2 at the temperature of 1200 oC in vacuum for 30 minutes. The microstructure analysis of the alloyed sample was confirmed using an optical microscope and FE-SEM. Hardness and trace element analyses were performed using Vickers hardness and WD-XRF, respectively. Diffusion profile analysis was performed using D-SIMS. From the microstructure analysis results, crystal grains were found to have formed with sizes of 2.97 mm. For the copper alloys formed using metal oxides of B2O3, RuO2, and IrO2 the sizes of the crystal grains were 1.24, 1.77, and 2.23 mm, respectively, while these sizes were smaller than pure copper. From the Vickers hardness results, the hardness of the Ir-copper alloy was found to have increased by a maximum of 2.2 times compared to pure copper. From the trace element analysis, the copper alloy was fabricated with the expected composition. From the diffusion profile analysis results, it can be seen that 0.059 wt%, 0.030 wt%, and 0.114 wt% of B, Ru, and Ir, respectively, were alloyed in the copper, and it led to change the hardness. Therefore, we verified that alloying of high melting point elements is possible at the low temperature of 1200 oC.
We prepared 8 samples of non-silver and silver-added master alloys containing silicon to confirm the existence of nickel-silicides. We then prepared products made of 14K and 18K white gold by using the prepared master alloys containing 0.25, 0.35, and 0.50 wt% silicon to check for nickel release. We then employed the EN 1811 testing standard to investigate the nickel release of the white gold products, and we also confirmed the color of the white gold products with an UV-VISNIR- color meter. We observed NiSix residue in all master alloys containing more than 0.50 wt% Si with EDS-nitric acid etching. For the white gold products, we could not confirm the existence of NiSix through XRD after aqua regia etching. In the EN 1811 test, only the white gold products with 0.25 wt% silicon master alloys successfully passed the nickel release regulations. Moreover, we confirmed that our white gold products showed excellent Lab indices as compared to those of commercial white gold ones, and the silver-added master alloys offered a larger L index. Our results indicate that employing 0.25 wt% silicon master alloys might be suitable for white gold products without nickel-silicide defects and nickel release problems.