• 공업화학
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• 제5권1호
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• pp.1-15
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• 1994

승온열탈착기술(temperature-programmed desorption, TPD)은 촉매의 특성을 연구하는데 매우 유용한 실험방법이다. 일반적으로 상압하에서 수행되는 것이 대부분인데, 근래에 진공조건에서 분말상의 촉매에 대한 TPD실험을 통하여 매우 중요한 결과들이 많이 발표되고 있다. 본 논문에서는 진공하에서의 TPD실험결과의 해석 및 실험법이 간략하게 소개된다.

• Bulletin of the Korean Chemical Society
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• 제30권6호
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• pp.1349-1352
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• 2009

We report the results of the surface chemistry of deuterized ethanol exposed Zircaloy-4 (Zry-4) surfaces with various amount of $C_2D_5$OD exposures at 190 K. This system was examined with Auger electron spectroscopy (AES) and temperature programmed desorption (TPD) techniques. In TPD study, $D_2$ was evolved at two different desorption temperature regions accompanying with broad desorption background. The lower temperature feature at around 520 K showed first-order desorption kinetics. The high temperature desorption peak at around 650 K shifted to lower desorption temperature as the exposure of $C_2D_5$OD increased. The Zr(MNV) Auger peak shifted about 2.5 eV from 147 eV to lower electron energy followed by 300 L of $C_2D_5$OD dosing. This implies metallic zirconium was oxidized by deuterized ethanol adsorption. After stepwise annealing of the oxidized Zry-4 sample up to 843 K, the shifted Zr(MNV) peak was gradually shifted back to metallic zirconium peak position. After the sample was heated to 843 K, the oxygen content near the Zry-4 surface was recovered to clean surface level. The concentration of carbon, however, was not recovered by annealing the sample.

• Bulletin of the Korean Chemical Society
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• 제32권5호
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• pp.1559-1563
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• 2011

Thermal hydrogenation of phenylacetylene (PA, $C_8H_6$) to styrene ($C_8H_8$) on pre-$C_xH_y$- and C-covered Cu(111) single crystal substrates has been studied using temperature-programmed desorption (TPD) mass spectrometry. Chemisorbed PA with an acetylene group has been proved to be associated with hydrogen of pre-adsorbed $C_xH_y$ to form styrene (104 amu) on Cu surface. For the parent (PA) mass (102 amu) TPD profile, the TPD peaks at 360 K and 410 K are assigned to chemisorbed vertically aligned PA and flat-lying cross-bridged PA, respectively (J. Phys. Chem. C 2007, 111, 5101). The relative $I_{360K}/I_{410K}$ TPD ratio dramatically increases with increasing pre-adsorbed $C_xH_y$ before dosing PA, while the ratio does not increase for pre-C-covered surface. For PA on pre-$C_xH_y$-covered Cu(111) surface, styrene desorption is enhanced relative to the parent PA desorption, while styrene formation is dramatically quenched on pre-C-covered (lack of adsorbed hydrogen nearby) surface. It appears that only cross-bridged PA associates with adsorbed hydrogen to form styrene that promptly desorbs at 410 K, while vertically aligned PA is less likely to participate in forming styrene.

• 한국재료학회지
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• 제29권3호
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• pp.143-149
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• 2019

To develop flexible adsorbents for compact volatile organic compound (VOC) air purifiers, flexible as-spun zeolite fibers are prepared by an electrospinning method, and then zeolite particles are exposed as active sites for VOC (toluene) adsorption on the surface of the fibers by a thermal surface partial etching process. The breakthrough curves for the adsorption and temperature programmed desorption (TPD) curves of toluene over the flexible zeolite fibers is investigated as a function of the thermal etching temperature by gas chromatography (GC), and the adsorption/desorption characteristics improves with an increase in the thermal surface etching temperature. The effect of acidity on the flexible zeolite fibers for the removal of toluene is investigated as a function of the $SiO_2/Al_2O_3$ ratios of zeolites. The acidity of the flexible zeolite fibers with different $SiO_2/Al_2O_3$ ratios is measured by ammonia-temperature-programmed desorption ($NH_3-TPD$), and the adsorption/desorption characteristics are investigated by GC. The results of the toluene adsorption/desorption experiments confirm that a higher $SiO_2/Al_2O_3$ ratio of the flexible zeolite fibers creates a better toluene adsorption/desorption performance.

• 한국진공학회지
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• 제15권1호
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• pp.73-80
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• 2006

Si(100)에 주입된 불활성 기체 이온들의 열적 방출 특성을 열탈착(temperature-programmed desorption; TPD) 질량분석법으로 고찰하였다. 약 400K의 표면 온도 조건에서 1keV 비온빔에 시료를 노출시켜 주었을 때, He은 $500\~1100 K$의 넓은 온도 범위에서 Si(100)결정 밖으로 분출되어 나온 반면, Ne, Ar, 및 Kr은 각각 810, 860, 875 K 근처에서 매우 좁은 온도 범위에서 TPD 피크를 나타내며 급격하게 방출되었다. He+ 이온으로 처리된 Si(100)은 표면 원자 구조의 손상이 상대적으로 최소한으로 일어났지만, $Ne^+,\;Ar^+,\;Kr^+$ 등의 이온들로 처리된 경우는 질량이 클수록 표면이 원자 스케일로 더 심하게 손상되었음이 수소 흡탈착 분석 결과로 밝혀졌다. 이온빔에 의한 결정 내부의 결함 생성과 관련하여 이러한 실험적 결과가 시사하는 점들을 논의하였다

• 한국진공학회:학술대회논문집
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• 한국진공학회 2012년도 제43회 하계 정기 학술대회 초록집
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• pp.216-216
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• 2012

The interaction of hydrogen with ZnO single crystal surfaces, ZnO (0001), ZnO (000-1), and ZnO (10-10) has been investigated using temperature programmed desorption (TPD) and X-ray photoelectron Spectroscopy (XPS) techniques. When the ZnO single crystal surfaces are exposed to atomic hydrogen at 200 K, all three surfaces show hydrogen desorption at 450 K. ZnO (0001) surface shows hydrogen desorption feature at ~260 K as the hydrogen exposure is increased. The ZnO (10-10) surface shows low-temperature desorption feature first and the high-temperature desorption feature appears as the hydrogen exposure increases. The ZnO (000-1) surface does not show any lower temperature hydrogen desorption. We will report the adsorption configuration of hydrogen atoms on ZnO single crystal surfaces with different surfaces structures.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2012년도 제42회 동계 정기 학술대회 초록집
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• pp.268-268
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• 2012

Adsorption and desorption of toluene from bare and $TiO_2$-coated silica with a mean pore size of 15 nm was studied using breakthrough curves and temperature programmed desorption. Thicknesses of $TiO_2$ films prepared by atomic layer deposition on silica were < 2 nm, and ~ 5 nm, respectively. For toluene adsorption, both dry and humid conditions were used. $TiO_2$-thin film significantly improved toluene adsorption capacity of silica under dry condition, whereas desorption of toluene from the surface as a consequence of displacement by water vapor was more pronounced for $TiO_2$-coated samples with respect to the result of bare ones. In the TPD experiments, silica with a thinner $TiO_2$ film (thickness < 2 nm) showed the highest reactivity for toluene oxidation to $CO_2$ in the absence and presence of water. We show that the toluene adsorption and oxidation reactivity of silica can be controlled by varying thickness of $TiO_2$ thin films.

• 공업화학
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• 제18권6호
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• pp.592-598
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• 2007

Temperature programmed desorption (TPD), XRD, SEM 및 FT-IR를 이용하여 코발트 프탈로시아닌 유도체의 황과 아민화합물에 대한 흡착효율을 조사하였다. 코발트 프탈로시아닌 유도체의 암모니아에 대한 TPD 측정결과, 산도가 낮은 온도($100{\sim}150^{\circ}C$)와 높은 온도($350{\sim}400^{\circ}C$)에서 두개의 탈착피크가 나타났다. 테트라카르복실 코발트프탈로시아닌(Co-TCPC)은 코발트 프탈로시아닌(Co-PC)보다 낮은 온도(물리적 흡착)에서 탈착피크가 약했지만 높은 온도(화학적 흡착)에서 강한 탈착피크가 나타났다. Co-TCPC와 Co-PC의 비표면적은 각각 37.5와 $18.4m^2/g$이었다. Co-TCPC와 Co-PC의 기공부피는 각각 0.17과 $0.10cm^3/g$이었다. 파과곡선으로부터 흡착용량을 계산하였더니 트리에틸 아민 가스 120 ppm의 평형농도에서 Co-TCPC의 흡착용량은 24.3 mmol/g, Co-PC의 흡착용량은 0.8 mmol/g로 나타났다. Co-TCPC와 Co-PC로 디메틸 술파이드 제거효율은 디메틸 술파이드 초기농도 225 ppm에서 각각 92와 18% 제거효율을 보였다. Co-TCPC와 Co-PC로 트리메틸아민 제거효율은 트리메틸아민 초기농도 118 ppm에서 각각 100.0%와 17.0% 제거효율을 보였다.

• Bulletin of the Korean Chemical Society
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• 제30권7호
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• pp.1470-1474
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• 2009

Thermal and photochemistry of methyl iodide ($CH_3I)\;adsorbed\;on\;D_2O$ ice film on Cu(111) at 100 K were studied using temperature-programmed desorption (TPD) time-of-flight mass spectrometry (TOF-MS), X-ray and ultraviolet photoelectron spectroscopies. On the basis of TPD, multilayer and monolayer $CH_3I$ molecules desorb from $D_2O$ ice layer at 120 and 130 K, respectively. Photo-irradiation at 100 K exhibits dramatic changes in the TPD and I $3d_{5/2}\;XPS\;of\;CH_3I$ on ice film, due to a dramatic dissociation of $CH_3I$. The dissociation is likely activated by solvated electrons transferred from the metal substrate during photo-irradiation. No other photo-initiated reaction products were found within our instrumental detection limit. During photo-irradiation, the $CH_3I$, $CH_3$ and I could be trapped (or solvated) in ice film by rearrangement (and self-diffusion) of water molecules. A newly appeared parent molecular desorption peak at 145 K is attributed to trapped $CH_3I$. In addition, the $CH_3$ and I may diffuse through ice and chemisorb on Cu(111), indicated by TPD and I $d_{5/2}$ XPS taken with photo-irradiation time, respectively. No molecular ejection was found during photo-irradiation at 100 K. The work functions for $CH_3I/Cu(111),\;D_2O/Cu(111)\;and\;CH_3I/D_2$O/Cu(111) were all measured to be about 3.9 eV, 1.0 eV downward shift from that of clean Cu(111).

• Korean Chemical Engineering Research
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• 제57권5호
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• pp.714-722
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• 2019

산 염기성질이 다양하게 존재하는 담체($SiO_2-Y_2O_3$, $Al_2O_3$, $SiO_2-ZrO_2$, $SiO_2$, $TiO_2$, MgO) 상에 17 wt% Ni을 고정한 상태에서 함침법을 사용하여 촉매를 제조하여 수소 존재 하에 에탄올과 암모니아의 환원성 아민화 반응에 대한 촉매활성을 비교 평가하였다. 반응 전후에 있어 사용된 촉매는 X-선 회절, 질소 흡착, 에탄올-승온탈착(EtOH-TPD), 이소프로판올-승온탈착(IPA-TPD), 수소 화학흡착을 사용하여 특성분석을 수행하였다. pH 9.5 이상에서 침전법을 사용하여 $ZrO_2$와 $Y_2O_3$ 담체 제조 시 파이렉스 반응기에서 미량의 Si 용융으로 인해 $SiO_2-ZrO_2$와 $SiO_2-Y_2O_3$ 복합 산화물이 각각 생성되었다. 사용된 촉매 중에서 $Ni/SiO_2-Y_2O_3$ 촉매가 가장 좋은 활성을 보였으며 이는 높은 니켈 분산도와 EtOH-TPD와 IPA-TPD에서의 낮은 탈착온도 등과 밀접한 관련이 있었다. Ni/MgO 촉매상에서의 낮은 촉매 활성은 NiO-MgO 고형물 형성에 기인한 것으로 보이며, $Ni/TiO_2$ 경우에서는 담체-금속 간의 강한 상호 작용으로 인해 낮은 니켈 금속 상 존재로 인해 반응성이 낮게 나왔다. $TiO_2$와 MgO 이외의 담체를 사용한 경우에 있어서 유사한 에탄올 전환율에서의 에틸아민류와 아세토니트릴 선택도는 큰 차이를 보이지 않았다.