• Korean Journal of Chemical Engineering
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• 제35권12호
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• pp.2365-2378
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• 2018

We investigated the correlation between vanadium surface density and VOx structure species in the selective catalytic reduction of NOx by $NH_3$. The properties of the $VOx/TiO_2$ catalysts were investigated using physicochemical measurements, including BET, XRD, Raman spectroscopy, FE-TEM, UV-visible DRS, $NH_3-TPD$, $H_2-TPR$, $O_2-On/Off$. Catalysts were prepared using the wet impregnation method by supporting 1.0-3.0 wt% vanadium on $TiO_2$ thermally treated at various calcination temperatures. Through the above analysis, we found that VOx surface density was $3.4VOx/nm^2$, and the optimal V loading amounts were 2.0-2.5 wt% and the specific surface area was $65-80m^2/g$. In addition, it was confirmed that the optimal VOx surface density and formation of vanadium structure species correlated with the reaction activity depending on the V loading amounts and the specific surface area size.

• 한국수소및신에너지학회논문집
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• 제21권1호
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• pp.26-34
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• 2010

The electrocatalystic prperties of Pt-Co and Pt-Ni with heteropolyacids (HPAs) entrapped in covalently cross-linked sulfonated poly(ether ether ketone) (CL-SPEEK)/HPA membranes were investigated for water electrolysis. The HP As, including molybdophosphoric acid (MoPA), and tungstophosphoric acid (TPA) were both used as membrane additives and electrocatalysts. The membrane electrode assembly (MEA) was prepared by a nonequilibrium impregnation-reduction (I-R) method. $Pt(NH_3)_4Cl_2$, $NiCl_2$ and $CoCl_2$ as electrocatalytic materials and $NaBH_4$ as reducing agent were used. I order to enhance electrocatalytic activity, the catalyst layer prepared above was electrodeposited (Dep) with HP A. Surface morphologies and physico-chemical properties of MEA were investigated by means of SEM, EDX and XRD. The electrocatalytic properties of composite membranes such as the cell voltage and coulombic charge in CV were in the order of magnitude: CL-SPEEK/MoPA40 (wt%) > CL-SPEEK/TPA30 > Nafion117. In the optimum cell applications for water electrolysis, the cell voltage of Pt/CL-SPEEK-MoPA40/Pt-Co (Dep-MoPA) and Pt/CL-SPEEK-TPA30/Pt-Co (Dep-TPA) was 1.75 Vat $80^{\circ}C$ and $1\;A/cm^2$ and voltage efficiency was 87.1%. Also, the observed activity of Pt-Co (84:16 atomic ratio by EDX) is a little higher than that of Pt-Ni (86: 14). The current density peak of electrodeposited electrodes were better a little than those of unactivated electrodes based on the same membranes.

• 한국수소및신에너지학회논문집
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• 제18권4호
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• pp.391-398
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• 2007

The covalently cross-linked sulfonated polyetheretherketone (CL-SPEEK) membrane was prepared by four-step synthesis of sulfonation-sulfochlorination, partial reduction, lithiation, and cross-linking, and its electrochemical and mechanical properties were investigated for water electrolysis application. The prepared ion exchange membranes showed good electrochemical and mechanical properties; proton conductivity of 0.116 S/cm at $80^{\circ}C$, water uptake of 44.6%, ion exchange capacity of 1.75 meq/g-dry-memb., tensile strength of 64.25 MPa and elongation of 61.11%. The membrane electrode assembly (MEA) with homemade membranes were prepared by non-equilibrium impregnation-reduction (I-R) method. Especially, the electrochemical surface area (ESA) and roughness factor of CL-SPEEK electrolyte by cyclic voltammetry method were 23.46 $m^2/g$ and 307.3 $cm^2-Pt/cm^2$, respectively. The prepared MEA was used in the unit cell of water electrolysis and the cell voltage was 1.81 V at 1 A/$cm^2$ and $80^{\circ}C$, with platinum loadings of 1.31 mg/$cm^2$.

• 청정기술
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• 제24권3호
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• pp.198-205
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• 2018

본 연구는 $Co-CeO_2$ 촉매의 $N_2O$ 분해 반응에서 촉매의 제조 방법이 활성에 미치는 영향을 고찰하였다. $Co-CeO_2$ 촉매는 공침법(Co-precipitation)과 함침법(Incipient wetness impregnation)으로 제조하였다. 제조된 촉매의 성능을 평가하기 위하여 $N_2O$ 직접 촉매 분해(Direct catalytic $N_2O$ decomposition) 반응을 $250{\sim}375^{\circ}C$에서 실시하였다. 그 결과 공침법으로 제조된 촉매(CoCe-CP)는 $O_2$ 및/또는 $H_2O$의 존재 하에서도 $N_2O$ 분해 반응에서 향상된 성능을 보인 반면에 함침법으로 제조된 촉매(CoCe-IM)는 그렇지 못하였다. 이러한 촉매 활성의 차이를 조사하기 위하여 XRD, BET, TEM, $H_2-TPR$, $O_2-TPD$ 그리고 XPS와 같은 촉매 특성 분석들을 진행하였다. 촉매의 제조 방법에 따라서 입자의 크기 및 표면적이 변화하는 것을 확인하였고 합성 과정이 촉매의 물리적 특성에 영향을 미치는 것을 알 수 있었다. 공침법으로 제조된 촉매의 활성 증가는 $Co^{3+}{\rightarrow}Co^{2+}$의 향상된 환원 특성 및 산소 탈착 속도 향상에 기인한 것으로 여겨진다. 하지만, $N_2O$ 분해와 관련이 있는 촉매의 표면 전하 상태 및 결합에너지는 제조 방법에 따라서 변하지 않는 것을 확인하였다.

• Bulletin of the Korean Chemical Society
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• 제33권5호
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• pp.1643-1646
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• 2012

Three Ni-based catalysts with different clay as support were prepared and tested in the hydrogenation of maleic anhydride, among which Ni/clay1 showed best activity and selectivity. Over Ni/clay1 catalyst prepared by impregnation method, 97.14% conversion of maleic anhydride and 99.55% selectivity to succinic anhydride were obtained at $180^{\circ}C$ under a pressure of 1 MPa. Catalytic activity was greatly influenced by the temperature and weighted hourly space velocity. Catalyst deactivation studies showed that this catalyst have a long life time, the yield of MA still higher than 90% even after a reaction time of 60 h. X-ray diffraction (XRD) and $H_2$ temperature programmed reduction (TPR) were use to investigate the properties of the catalyst. XRD and TPR studies showed that Ni was present as $Ni^{2+}$ on the support, which indicated that there was no elemental nickel ($Ni^0$) and $Ni_2O_3$ in the unreduced samples. The formation of Ni was strong impact on catalytic activity.

• 한국수소및신에너지학회논문집
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• 제6권2호
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• pp.75-84
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• 1995

SPE-composites which was prepared with impregnation-reduction method for hydroen production were investigated with morphological and electrochemical analysis. As Pt reagent's concentration increased, Pt loadings increased. However, reductant's concentration had a little effect on Pt loadings. By the morphological analysis, it was found that Pt was deposited inside of SPE. Furthermore, with electrochemical analysis, we found that Pt loading, electricity, roughness factor and active surface area were $2.05mg/cm^2$, 14.20 mC, 21.55, $10.51cm^2/mg$ respectively at reducing agent concentration 0.05 mol/L. Therefore, we found the deposited Pt inside of SPE would give an effect on electrical characteristics of SPE-composites.

• 한국전기전자재료학회논문지
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• 제20권8호
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• pp.671-679
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• 2007

[ $SrAl_2O_4:Eu^{2+},\;Dy^{3+}$ ] phosphor was synthesized using the impregnation method, and its photoluminescence and long-afterglow properties were investigated, A mixture of $Sr(NO_3)_2,\;Al(NO_3)_2\;9H_2O,\;EuCl_3\;6H_2O,\;DyCl_3\;6H_2O,\;NdCl_3\;6H_2O$ salts were dissolved in distilled water and impregnating into the polymer precursor. After drying, the impregnated mixture was heat treated at $900-1400^{\circ}C$ for 2h in a $N_2-H_2$ reduction atmosphere. The microstructure and crystal structure of the $SrAl_2O_4:Eu^{2+},\;Dy^{3+}$ powders were examined by scanning electron microscopy and X-ray diffraction, respectively. The photoluminescence spectra showed an excitation band along over wide wavelength of 250-450nm, and a broaden emission with a maxima peak at 360nm. In addition, the spectra also showed a good long after glow that decayed over a 1000sec period after 10 min excitation illumination.

• 공업화학
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• 제7권5호
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• pp.999-1005
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• 1996

Carbon 표면에 작용기를 도입하기 위해 산화처리한 후, $H^+$과 Pt 양이온을 교환시키는 이온교환법과 백금용액을 계면활성제가 들어있는 메탄올로 환원을 시켜 carbon에 백금을 담지하는 메탄올 환원법으로 촉매를 제조하여 이미 널리 쓰이고 있는 colloid 방법으로 제조한 촉매와 비교하였다. 메탄올 환원법에서 계면활성제는 carbon과 백금입자의 분산효과를 높이고, 안정한 백금 colloid 용액의 유지를 위해 첨가하였다. 각 담지방법에 의해 담지된 백금입자가 $30{\sim}50{\AA}$의 크기로 분산되어 담지된 것을 TEM과 XRD를 통해 확인하였고, 담지방법에 따른 백금의 담지율은 모두 100%에 가까웠고, 그 중 이온교환법의 담지율이 DCP 측정으로는 99.92%, 연소법으로는 99.87%였다. 각 촉매의 활성을 전기화학적으로 비교하기 위하여 산소환원전류밀도를 측정한 결과, 초기에는(60시간 이내) colloid 방법에 의해 제조된 촉매로 제작한 산소극이 0.7V(vs. RHE)에서 $460mA/cm^2$로 이온교환법, 메탄올 환원법에 의해 제조된 촉매보다 더 우수한 전극성능을 나타냈지만, 장시간(약 100시간 이후) 운전시에 전극성능 감소율은 colloid 방법으로 제조한 촉매로 제작한 전극이 가장 높게 증가하였으며, 메탄올 환원법으로 제조한 전극이 가장 안정된 특성을 보였다.

• 청정기술
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• 제24권1호
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• pp.35-40
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• 2018

$N_2O$ 촉매 분해 반응을 위한 $Co_3O_4$ 촉매는 공침법을 이용하여 제조하였으며, 조촉매로서 Ce 및 Zr의 양을 (Ce 또는 Zr)/Co = 0.05의 몰비로 고정하여 제조하였다. 또한 K가 촉매에 미치는 영향을 조사하기 위해 1 wt%의 $K_2CO_3$를 함침하여 촉매를 제조하였다. 제조된 촉매의 특성은 BET, SEM, XRD, $H_2-TPR$, XPS를 통해 분석하였다. $Co_3O_4$ 촉매는 스피넬 결정상을 나타냈으며, 조촉매의 첨가는 입자 크기와 결정 크기를 감소시켜 비표면적을 증가시키는 것으로 나타났다. K의 도핑은 촉매 활성 물질인 Co의 활성 종인 $Co^{2+}$의 농도를 증가시켜 촉매 활성을 향상시키는 것으로 확인되었다. $N_2O$ 분해 반응 테스트는 $GHSV=45,000h^{-1}$, $250{\sim}375^{\circ}C$에서 수행되었으며 $Co_3O_4$ 촉매에 조촉매를 첨가하였을 때도 반응성이 증가하였지만, K를 함침하면 활성이 더욱 크게 증가하는 것으로 나타났다. K의 도핑이 활성 종인 $Co^{2+}$의 농도를 증가시키며, 환원온도를 낮춰 주어 활성에 큰 영향을 주는 것으로 확인하였다.

• 공업화학
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• 제23권2호
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• pp.190-194
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• 2012

다양한 상용 $TiO_2$ 담체를 이용한 10 wt%의 Mn계 촉매를 습윤함침법으로 제조하여 $NH_3$에 의한 NO의 저온 선택적 촉매환원법(SCR) 반응 특성을 연구하였다. 촉매의 특성은 BET, XRD, XPS 그리고 TPR과 같은 물리화학적 분석을 통해 수행되었다. MnOx/$TiO_2$ 촉매의 MnOx 표면밀도는 비표면적에 영향을 받는다. 고분산된 망간산화물에 의한 낮은 MnOx surface density로 저온 SCR 활성이 증가하고 망간산화물의 $MnO_2$에서 $Mn_2O_3$로 환원되는 온도가 감소되었다. 우수한 SCR활성을 위해서는 망간산화물을 높은 비표면적을 가진 $TiO_2$에 담지되어야 하고 고분산된 비정질종이 존재해야 한다.