Synthesis of the single phase CIGS particle by solvothermal method for solar cell application

Gu, Sin-Il,Shin, Hyo-Soon,Yeo, Dong-Hun,Hong, Youn-Woo,Nahm, Sahn Elsevier 2011 Current Applied Physics Vol.11 No.1

<P><B>Abstract</B></P><P>Uniform CIGS powder synthesis is required more these days to produce CIGS solar cell using thick film process. Solvothermal CIGS powder synthesis method, among other synthesis methods, is mainly used because it is simple and easy for mass production. But all CIGS synthesis result reported up to now are mixed with CIS, CIGS and CGS, and there was no result that reported single phase CIGS synthesis. Especially, comparable single phase CIGS was synthesized in the CIGS powder synthesis using metal source, but small amount of CIS powder were still remained. In this study, we examined the CIGS synthesis paths in solvothermal method, and synthesize single phase CIGS. CGS seed was synthesized using Cu, In, GaCl<SUB>3</SUB>, Se sources by keeping 12 h at 180 °C, and we were able to synthesize single phase CIGS by keeping it for 24 h at raised temperature of 230 °C. The synthesized CIGS formed uniform particles with its size of less than 100 nm, and was shown in strong agglomeration.</P> <P><B>Highlights</B></P><P>► CIGS powder synthesis is required more these days to produce CIGS solar cell using thick film process. ► The CIGS synthesis paths in solvothermal method, and synthesize single phase CIGS. ► The CIGS formed uniform particles with its size of less than 100 nm.</P>

Synthesis of metal-organic frameworks: A mini review

안화승,Yu-Ri Lee,Jun Kim 한국화학공학회 2013 Korean Journal of Chemical Engineering Vol.30 No.9

Metal organic frameworks (MOFs) are porous crystalline materials of one-, two-, or three-dimensional networks constructed from metal ions/clusters and multidentate organic linkers via coordination bonding, which are emerging as an important group of materials for energy storage, CO2 adsorption, alkane/alkene separation, and catalysis. To introduce newcomers in chemical engineering discipline to the rapidly expanding MOF research works, this review presents a brief introduction to the currently available MOFs synthesis methods. Starting from the conventional solvothermal/hydrothermal synthesis, microwave-assisted, sonochemical, electrochemical, mechanochemical, ionothermal, drygel conversion, and microfluidic synthesis methods will be presented. Examples will be limited to those representative MOF structures that can be synthesized using common organic ligands of 1,4-benzenedicarboxylic acid (and its functionalized forms) and 1,3,5-benzenetricarboxylic acid, in conjunction with metal nodes of Zn2+, Cu2+, Cr3+, Al3+,Fe3+ and Zr4+. Synthesis of widely-investigated zeolitic imidazolate framework (ZIF) structure, ZIF-8 is also included.

Control of particle morphology and size of yttria powder prepared by hydro(solvo)thermal synthesis

오복현,이상진 한국세라믹학회 2022 한국세라믹학회지 Vol.59 No.4

Yttria (Y 2 O 3 ) is a representative material having excellent plasma resistance, and yttria powder, applied to semiconductor components and thermal spray coating, requires excellent sinterability and fl owability, for which particle shape and size are important factors. In the present study, to synthesize yttria powder having various shape applicable to many industrial areas, the morphology of yttria particles was controlled through hydro(solvo)thermal synthesis. The yttria powder was synthesized using deionized water, ethylene glycol and glycerol as solvents. The precursor concentrations and the synthesis conditions such as synthesis temperature and time were examined. The particle shape and size of the yttria powder were adjusted to plate-type, rod-type and spherical-type depending on the applied solvent, precipitant and synthesis temperature. The thermal treatment following the hydro(solvo)thermal synthesis did not have a signifi cant eff ect on the shape of the yttria particles. Cubic single-phase yttria was observed at a calcination temperature of 450 °C or higher, and the crystal phase further devel- oped as the thermal treatment temperature increased. In the powder synthesized using deionized water, the crystal phase developed mostly on the [222] direction depending on the temperature during oriented attachment. On the other hand, in the powder synthesized using ethylene glycol and glycerol as a solvent, the crystal phase developed homogeneously in all crystalline directions.

Effect of solvents on the microstructure of CaWO4 prepared by a solvothermal synthesis

Sulawan Kaowphong,Titipun Thongtem,Somchai Thongtem 한양대학교 세라믹연구소 2010 Journal of Ceramic Processing Research Vol.11 No.4

Different sizes of nanostructured CaWO4 have been prepared by a simple solvothermal synthesis at a low temperature of 160 °C for 6 h through the reaction between Ca(NO3)2·4H2O and Na2WO4·2H2O using various solvents as the reaction medium. The products, characterized by X-ray diffraction (XRD), were specified as pure CaWO4 with the scheelite structure. Scanning electron microscope (SEM) and transmission electron microscope (TEM) analysis showed that the particle sizes are mainly related to the physical and chemical properties of the solvents used in the solvothermal synthesis. Photoluminescence properties were also investigated.

분체공학,유동층,고분자,재료(무기,유기) : 에틸렌디아민을 이용하여 Solvothermal Synthesis로 Y2O3:Eu3+ 나노 입자의 제조

신수철 ( Sin Su Cheol ),조태환 ( Jo Tae Hwan ) 한국화학공학회 2003 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.41 No.5

Eu doped Y₂O₃ nanoparticles were prepared with the solvothemal synthesis using ethylenediamine solvent at 200℃ for 1-5 h and then annealed in air at from 1,000℃ to 1,400 for 2 4 h. The X-ray diffraction pattern of the crystals annealed at 1,000℃ for 2 h could be indexed as pure cubic cell of Y₂O₃ with the lattice parameter a=10.6029 Å which is very close to the reported value (JCPDS Card File 41-1105, a=10.6041 Å). Average sizes of prepared phosphor particles had about 100 nm, size and spherical morphology. The phosphor panicle size decreased and the emission intensity increased as the annealing temperature increased. Through PL spectrum analysis, the 3% Eu doped Y_(2-x)O₃:Eu_(x)^(3+)(x=0.06) phosphor showed the excitation spectrum at 250 nm wavelength and the maximum emission spectrum appeared at 611nm wavelength.

2-메톡시에탄올을 사용한 용매열 합성법에 의해 합성되어진 (Y_l-xGd_x)₂O₃:Eu³⁺ 형광체입자

신수철,조태환,Shin, Su-Cheol,Cho, Tae-Hwan 한국재료학회 2003 한국재료학회지 Vol.13 No.8

($Y_{l-x}$ $Gd_{x}$ )$O_2$$_3$: $Eu^{ 3+}$ red phosphors were prepared with the solvothermal synthesis using the 2-methoxy-ethanol solvents and the emission intensity was investigated that applied with the 254 nm wavelength and the maximum excitation wavelength for energy source. The used solvents for the solvothermal synthesis were made of nitrate salt solutions of Y, Gd and Eu. These solutions dropped in autoclave have be reacted with the solvothermal synthesis at $200^{\circ}C$ for 5hrs and the red phosphors prepared here in were showed the pure cubic phase after annealing at $1000∼1200^{\circ}C$. The brightness of ($Y_{l-x}$ $Gd_{x}$)$_2$$O_3$: $Eu^{3+}$ phosphors particles was increased as an increase of Gd ratio. The maximum excitation wavelengths of ($Y_{l-x}$ $Gd_{x}$ )$_2$$O_3$: $Eu^{3+}$ / phosphors particles were increased according to increasing Gd ratio from 253 nm to 259 nm wavelength. The maximum emission intensity of $Gd_2$$O_3$: $Eu^{3+}$ (Y/Gd = 1/0) phosphors particles under UV 259 nm was found to be higher than the commercial product of $Y_2$$O_3$: $Eu^{3+}$ phosphors.

Solvothermal Synthesis of PtNi Nanoparticle Thin Film Cathode with Superior Thermal Stability for Low Temperature Solid Oxide Fuel Cells

Jiyoon Shin,Kittiwat Kamlungsua,Hao-Yang Li,Pei-Chen Su 한국정밀공학회 2024 International Journal of Precision Engineering and Vol.11 No.4

This work adopts solvothermal synthesis to fabricate PtNi nanoparticles as thin film cathodes with superior resistance against thermally driven agglomeration for low temperature solid oxide fuel cells (LT-SOFCs) operating at 450 ºC. Metal-based porous electrodes are common choices for thin film LT-SOFCs, but pure metals with high density nanoscale porosities are vulnerable to thermal agglomeration, which imposes challenges to maintaining high performance with long-term stability. Typical Pt-based thin film cathodes are previously reported to sustain a record high 600 ºC of thermal annealing with acceptable morphological stability, but the temperature is still too low for practical LT-SOFC application. In this work, the solvothermal synthesized PtNi nanoparticle thin films show superior thermal stability, sustaining 10 h of annealing at 800 ºC without significant agglomeration observed. By controlling the length of synthesis time, the particle sizes and Pt loading ratio can be varied. The cost-effective solvothermal synthesis process for the fabrication of PtNi thin film cathode is a promising way for LT-SOFC manufacturing in scale as it involves no vacuum process like typical sputtering.

Solvothermal Synthesis of TiO2/CNFs Heterostructures with Photocatalytic Activity

Dandan Yu,Jie Bai,Yulong Gu,Chunping Li 성균관대학교(자연과학캠퍼스) 성균나노과학기술원 2015 NANO Vol.10 No.6

Titanium dioxide nanoparticles (TiO2 NPs) embedded carbon nanofibers (CNFs) have been successfully prepared by electrospinning technique, solvothermal synthesis and high-temperature calcination processes. The as-obtained products were characterized by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), UV-Vis diffuse reflectance spectra (DRS) and Fourier transform infrared (FTIR) spectra. The results of characterization revealed that solvothermal treatment and high-temperature calcination were beneficial to the synthesis of anatase TiO2. Compared to the as-fabricated TiO2 powder, TiO2 NPs contained in the TiO2/CNFs were successfully grown on the surface of CNFs without aggregation. The photocatalytic activities of the TiO2/CNFs heterostructures were evaluated by the degradation of methyl orange (MO) under UV light irradiation for 14 h. The TiO2/CNFs exhibited higher photocatalytic activities than pure TiO2 powder, which were attributed to the small size of TiO2 NPs, electron transfer, high adsorption properties of CNFs and the formation of heterostructures between TiO2 and CNFs. Moreover, in aqueous solution, the as-prepared TiO2/CNFs could be easily recycled for the application of CNFs.

용매열반응법으로 합성된 탄소양자점의 합성온도에 따른 형광특성 변화 연구

홍우태,양현경 한국물리학회 2021 새물리 Vol.71 No.3

Carbon dots (CDs) originating from sucrose were synthesized by using a solvothermal method. The morphological, structural and luminescent properties of those CDs were analyzed to investigate the effect of the synthesis temperature on the CDs. TEM images of the CDs showed that increasing the synthesis temperature caused an increase in the particle size and aggregation of the CDs. The FT-IR and XPS spectra of the prepared CDs indicated that an increase in the synthesis temperature eliminated the surface functionalized ligands and the defects in CDs fabricated using the solvothermal reduction. Under 400-nm excitation, the PL spectra of the CDs exhibited a blue emission band with a maximum at 477 nm. When the synthesis temperature was 220 ◦C, the maximum emission intensity of the CDs was the highest. When the synthesis temperature was 250 ◦C, the dominant emission wavelength and emission intensity decreased due to the removed of defect states in the bandgap. The results in this study, clearly show that the synthesis temperature can be used to control the morphological, structural, luminescent properties of CDs. 수크로스 (Sucrose) 기반의 탄소양자점을 용매열반응법을 사용하여 합성하였으며, 합성온도에 따른탄소양자점의 구조, 입자크기 및 표면형상, 형광특성의 변화를 분석하였다. 투과전자현미경 사진을통해, 탄소양자점의 합성온도가 증가함에 따라 크기와 응집도가 증가함을 확인하였다. 탄소양자점의 합성온도에 따른 푸리에 변환 적외선 흡수스펙트럼과 X-선 광전자 분광스펙트럼을 측정하여 합성온도가증가함에 따라 표면 개질 및 불순물에 의한 화학적 결합특성이 줄어들고, 탄소원자간의 sp2 결합특성이증가함을 확인하였다. 탄소양자점의 합성온도에 따른 형광스펙트럼을 측정한 결과, 220 ◦C에서 합성된탄소양자점의 형광세기가 최대가 되고 400 nm으로 여기할 때, 477 nm에서 주 발광파장을 가지는것을 확인하였다. 탄소양자점의 합성온도가 250 ◦C일 때, 탄소양자점의 sp2 결합특성에 대한 결정성이증가하고, 결함 (defect) 과 표면개질특성이 사라지게 되어 형광세기가 감소되고 발광파장이 440 nm로이동되었음을 확인하였다. 이러한 결과를 바탕으로 탄소양자점의 합성온도 변화를 통해 화학결합, 구조, 표면형상 및 형광특성을 조절할 수 있음을 확인하였다.

습식 환원법에 의한 Cu 나노입자의 합성 동향

신용무,지상수,이종현,Shin, Yong Moo,Chee, Sang-Soo,Lee, Jong-Hyun 한국마이크로전자및패키징학회 2013 마이크로전자 및 패키징학회지 Vol.20 No.3

Interest in copper nanoparticles has increased as an alternative for substituting silver nanoparticles because of its lower cost and less electromigration effect than silver. In this paper, the recent research trends and main results in wet-chemical synthesis of sub-100 nm Cu nanoparticles were summarized. The characteristics of synthesis were discussed with a classification such as modified polyol synthesis, modified hydrothermal synthesis, solvothermal synthesis, and the others, focussing on effects of capping agents, reductants, and pH. Information on the oxidation of synthesized copper nanoparticles were additionally commented.