• Title/Summary/Keyword: Cu-free precursor

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New MOD solution for the preparation of high $J_c$ REBCO superconducting films (고특성 REBCO 초전도 박막 제조를 위한 새로운 MOD 전구 용액 제조)

  • Kim, Byeong-Joo;Hong, Gye-Won;Lee, Hee-Gyoun
    • Proceedings of the KIEE Conference
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    • 2005.07c
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    • pp.2001-2003
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    • 2005
  • Various organic acid were used in order to prepare new metalorganic deposition solution for high quality $REBa_2Cu_3O_{7-{\delta}}$ (RE=Y, Eu, Gd) films. Prepared fluorine free MO precursor solution was coated on single crystal (001) $LaAlO_3$ (LAO) by dip coating method. Processing parameters such as oxygen partial pressure, water vapor, ramping rate and pyrolysis temperature etc havebeen controlled in order to make high $J_c$ films with a good epitaxial relationship with substrate. 0.5 micron-thick film was obtained by single coating and no crack appeared after calcination. Oxygen partial pressure was varied in the range of $100{\sim}1,000 ppm$ and conversion heat treatment was carried out at the temperature of $725{\sim}765^{\circ}C$. A critical transition temperature $(T_{c0})$ of 90K and a critical transport current density $(J_c)$ of $>0.5MA/cm^2$ (77K and self-field) were demonstrated for the YBCO film on (001) oriented LAO substrates with a thickness of 0.5 micron. $I_c$ was determined by utilizing a transport measurement. SEM and XRD investigations confirmed that films were grown epitaxially onto the LAO single crystal substrate. It is thought that fluorine free new MOD solutionis promising for high quality REBCO films.

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Hydrogen and Ethanol Gas Sensing Properties of Mesoporous P-Type CuO

  • Choi, Yun-Hyuk;Han, Hyun-Soo;Shin, Sun;Shin, Seong-Sik;Hong, Kug-Sun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.222-222
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    • 2012
  • Metal oxide gas sensors based on semiconductor type have attracted a great deal of attention due to their low cost, flexible production and simple usability. However, most works have been focused on n-type oxides, while the characteristics of p-type oxide gas sensors have been barely studied. An investigation on p-type oxides is very important in that the use of them makes possible the novel sensors such as p-n diode and tandem devices. Monoclinic cupric oxide (CuO) is p-type semiconductor with narrow band gap (~1.2 eV). This is composed of abundant, nontoxic elements on earth, and thus low-cost, environment-friendly devices can be realized. However, gas sensing properties of neat CuO were rarely explored and the mechanism still remains unclear. In this work, the neat CuO layers with highly ordered mesoporous structures were prepared by a template-free, one-pot solution-based method using novel ink solutions, formulated with copper formate tetrahydrate, hexylamine and ethyl cellulose. The shear viscosity of the formulated solutions was 5.79 Pa s at a shear rate of 1 s-1. The solutions were coated on SiO2/Si substrates by spin-coating (ink) and calcined for 1 h at the temperature of $200{\sim}600^{\circ}C$ in air. The surface and cross-sectional morphologies of the formed CuO layers were observed by a focused ion beam scanning electron microscopy (FIB-SEM) and porosity was determined by image analysis using simple computer-programming. XRD analysis showed phase evolutions of the layers, depending on the calcination temperature, and thermal decompositions of the neat precursor and the formulated ink were investigated by TGA and DSC. As a result, the formation of the porous structures was attributed to the vaporization of ethyl cellulose contained in the solutions. Mesoporous CuO, formed with the ink solution, consisted of grains and pores with nano-meter size. All of them were strongly dependent on calcination temperature. Sensing properties toward H2 and C2H5OH gases were examined as a function of operating temperature. High and fast responses toward H2 and C2H5OH gases were discussed in terms of crystallinity, nonstoichiometry and morphological factors such as porosity, grain size and surface-to-volume ratio. To our knowledge, the responses toward H2 and C2H5OH gases of these CuO gas sensors are comparable to previously reported values.

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Solution-Processed Nontoxic and Abundant $Cu_2ZnSnS_4$ for Thin-Film Solar Cells

  • Mun, Ju-Ho
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2012.05a
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    • pp.65-65
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    • 2012
  • Copper zinc tin sulfide ($Cu_2ZnSnS_4$, CZTS) is a very promising material as a low cost absorber alternative to other chalcopyrite-type semiconductors based on Ga or In because of the abundant and economical elements. In addition, CZTS has a band-gap energy of 1.4~1.5eV and large absorption coefficient over ${\sim}10^4cm^{-1}$, which is similar to those of $Cu(In,Ga)Se_2$(CIGS) regarded as one of the most successful absorber materials for high efficient solar cell. Most previous works on the fabrication of CZTS thin films were based on the vacuum deposition such as thermal evaporation and RF magnetron sputtering. Although the vacuum deposition has been widely adopted, it is quite expensive and complicated. In this regard, the solution processes such as sol-gel method, nanocrystal dispersion and hybrid slurry method have been developed for easy and cost-effective fabrication of CZTS film. Among these methods, the hybrid slurry method is favorable to make high crystalline and dense absorber layer. However, this method has the demerit using the toxic and explosive hydrazine solvent, which has severe limitation for common use. With these considerations, it is highly desirable to develop a robust, easily scalable and relatively safe solution-based process for the fabrication of a high quality CZTS absorber layer. Here, we demonstrate the fabrication of a high quality CZTS absorber layer with a thickness of 1.5~2.0 ${\mu}m$ and micrometer-scaled grains using two different non-vacuum approaches. The first solution-processing approach includes air-stable non-toxic solvent-based inks in which the commercially available precursor nanoparticles are dispersed in ethanol. Our readily achievable air-stable precursor ink, without the involvement of complex particle synthesis, high toxic solvents, or organic additives, facilitates a convenient method to fabricate a high quality CZTS absorber layer with uniform surface composition and across the film depth when annealed at $530^{\circ}C$. The conversion efficiency and fill factor for the non-toxic ink based solar cells are 5.14% and 52.8%, respectively. The other method is based on the nanocrystal dispersions that are a key ingredient in the deposition of thermally annealed absorber layers. We report a facile synthetic method to produce phase-pure CZTS nanocrystals capped with less toxic and more easily removable ligands. The resulting CZTS nanoparticle dispersion enables us to fabricate uniform, crack-free absorber layer onto Mo-coated soda-lime glass at $500^{\circ}C$, which exhibits a robust and reproducible photovoltaic response. Our simple and less-toxic approach for the fabrication of CZTS layer, reported here, will be the first step in realizing the low-cost solution-processed CZTS solar cell with high efficiency.

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Changes in Chemical Components of Red Ginseng Extract Solution and Physicochemical Properties of Precipitates Formed During Pterilization and Storage (홍삼 Ext 수용액의 살균과 저장 중 성분의 변화와 생성된 침전물의 이화학적 특성)

  • 김나미;이종태;양재원
    • Journal of Ginseng Research
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    • v.20 no.1
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    • pp.54-59
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    • 1996
  • Red Ginseng extracts sol'n was sterilized at 85f for 20 mins and/or stored at 4$0^{\circ}C$ for 6 months and centrifuged for 20 mins at 8,500xg in order to investigate the changes in chemical components of supernatants and the properties of precipitates. Contents of crude saponin and ginsenoside-$Rb_1$, -$Rg_1$, -Re were partially decreased during heating and storage. Starch contents were decreased from 26.81% in red ginseng extracts to 17.50-8.81% in supernatants, whereas free sugar contents were increased from 15.50% to 20.29~21.35% by heating and storage. The contents of protein and minerals in supernatants were decreased, but acidic polysaccharides and polyphenol compounds were not changed. pH values of supernatants and precipitates were decreased. The absorbances of brown color precursor and brown pigment in precipitates, detected at 285 nm and 440 nm were remarkably increased. The Overa11 data suggest that precipitates in red ginseng extracts sol'n formed during steilization and storage are provably the brown pigments resulting from Maillard reaction of amino compounds with reducing sugar which could be released from starch and protein matrix and $Cu^+$, $Ca^{2+}$ and $Fe^{3+}$ ions are implicated with the reaction incorporated.

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Total pressure dependence of YBCO films in MOD method (MOD 공정에 의해 제조된 YBCO 박막의 압력 의존성)

  • Yoo, Jai-Moo;Chung, Kook-Chae;Ko, Jae-Woong;Kim, Young-Kuk;Wang, Xiao Lin;Dou, Shi Xue
    • Progress in Superconductivity and Cryogenics
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    • v.8 no.1
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    • pp.5-8
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    • 2006
  • The growth properties of MOD-YBCO films were investigated. To enhance the growth rate of YBCO layer and inhibit the build-up of HF gas during the annealing process in TFA-MOD for YBCO coated conductors the method of low pressure annealing was employed. Total pressure was changed from 700Torr to 1Torr and its effect on growth of YBCO films was compared with atmospheric one. The lower Pressure was effective to control of the pore size in MOD method . Surface morphology of YBCO films processed at low total pres sure was rough and composed of random YBCO (103) grains. But large pores, usually observed at atmospheric process in MOD disappeared and also the number of pores was reduced at low pressure annealing. Also discussed ate the effects of Fluorine-free Y and Cu precursor solution on the development of microstructure. Dense surface me phology and with less and small pores can be provided through controlling Fluorine content.

Effect of water partial pressure on the texture and the morphology of MOD-YBCO films on buffered metal tapes

  • Chung, Kook-Chae;Yoo, Jai-Moo;Ko, Jae-Woong;Kim, Young-Kuk;Wang, X.L.;Dou, S.X.
    • Progress in Superconductivity and Cryogenics
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    • v.9 no.2
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    • pp.23-26
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    • 2007
  • The influence of water partial pressure in Metal-organic Deposition (MOD) method was investigated on the texture and the morphology of $YBa_2Cu_3O_{7-x}$ (YBCO) films grown on the buffered metal tapes. The water partial pressure was varied from 4.2% up to 10.0% with the other process variables, such as annealing temperature and oxygen partial pressure, kept constant. In this work, the fluorine-free Y & Cu precursor solution added with Sm was synthesized and coated by the continuous slot-die coating & calcination step. The next annealing step of the YBCO films was done by the reel-to-reel method with the gas flowed vertically down. From the x-ray diffraction analysis, the un-reacted phase like $BaF_2$ peak was found at the water partial pressure of 4.2%, but $BaF_2$ peak intensity is much reduced as the water partial pressure is increased. However, the higher water partial pressure of about 10% in this experiment leads to the poor crystallinity of YBCO films. The morphologies of the YBCO films were not different from each other when the water partial pressure was varied in this work. The maximum critical current density of 3.8MA/$cm^2$ was obtained at the water partial pressure of 6.2% with the annealing temperature of 780$^{\circ}C$ and oxygen partial pressure of 500ppm.

Hexagonal Boron Nitride Monolayer Growth without Aminoborane Nanoparticles by Chemical Vapor Deposition

  • Han, Jaehyu;Yeo, Jong-Souk
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.409-409
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    • 2014
  • Recently hexagonal boron nitride (h-BN), III-V compound of boron and nitrogen with strong covalent $sp^2$ bond, is a 2 dimensional insulating material with a large direct band gap up to 6 eV. Its outstanding properties such as strong mechanical strength, high thermal conductivity, and chemical stability have been reported to be similar or superior to graphene. Because of these excellent properties, h-BN can potentially be used for variety of applications such as dielectric layer, deep UV optoelectronic device, and protective transparent substrate. Ultra flat and charge impurity-free surface of h-BN is also an ideal substrate to maintain electrical properties of 2 dimensional materials such as graphene. To synthesize a single or a few layered h-BN, chemical vapor deposition method (CVD) has been widely used by using an ammonia borane as a precursor. Ammonia borane decomposes into hydrogen (gas), monomeric aminoborane (solid), and borazine (gas) that is used for growing h-BN layer. However, very active monomeric aminoborane forms polymeric aminoborane nanoparticles that are white non-crystalline BN nanoparticles of 50~100 nm in diameter. The presence of these BN nanoparticles following the synthesis has been hampering the implementation of h-BN to various applications. Therefore, it is quite important to grow a clean and high quality h-BN layer free of BN particles without having to introduce complicated process steps. We have demonstrated a synthesis of a high quality h-BN monolayer free of BN nanoparticles in wafer-scale size of $7{\times}7cm^2$ by using CVD method incorporating a simple filter system. The measured results have shown that the filter can effectively remove BN nanoparticles by restricting them from reaching to Cu substrate. Layer thickness of about 0.48 nm measured by AFM, a Raman shift of $1,371{\sim}1,372cm^{-1}$ measured by micro Raman spectroscopy along with optical band gap of 6.06 eV estimated from UV-Vis Spectrophotometer confirm the formation of monolayer h-BN. Quantitative XPS analysis for the ratio of boron and nitrogen and CS-corrected HRTEM image of atomic resolution hexagonal lattices indicate a high quality stoichiometric h-BN. The method presented here provides a promising technique for the synthesis of high quality monolayer h-BN free of BN nanoparticles.

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