• Applied Chemistry for Engineering
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• v.5 no.1
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• pp.1-15
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• 1994

Temperature-programmed desorption method is a very useful technique for the research of heterogeneous catalysts. In most cases, the experimental condition is atmospheric. However, recently TPD experiments under vacuum conditions using powder catalysts give lots of very important results that can't be obtained otherwise. In this paper, the interpretation method of TPD results and the experimental technique under vacuum conditions are introduced briefly.

• Bulletin of the Korean Chemical Society
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• v.30 no.6
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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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• v.32 no.5
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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.

• Korean Journal of Materials Research
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• v.29 no.3
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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.

• Journal of the Korean Vacuum Society
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• v.15 no.1
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• pp.73-80
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• 2006

Thermally-driven effusion of inert gases out from Si(100), into which energetic $\~l keV\;He^+,\;Ne^+,\;A^r+,\;and\;Kr^+ ions$ had been implanted at a moderate substrate temperatures of $\~400 K$, was investigated by means of temperature-programmed desorption (TPD) mass spectrometry. While He effused out broadly over $500\~1,100 K$, Ne, Ar, and Kr effusion occurred sharply at 810, 860, and 875 K, respectively. Hydrogen adsorption/desorption analysis for the ion-treated Si(100) surfaces indicated minimal to severe damage by ions with increasing mass from He to Kr. Implications of these results in light of literature reports are discussed.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.08a
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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.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.02a
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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.

• Applied Chemistry for Engineering
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• v.18 no.6
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• pp.592-598
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• 2007

The adsorption capability of cobalt phthalocyanine derivatives was investigated by means of X-ray diffractometor (XRD), FT-IR spectroscopy, scanning electron microscopy (SEM), and temperature programmed desorption (TPD). According to TPD results for ammonia, cobalt phthalocyanine derivatives showed two desorption peaks at low temperature ($100{\sim}150^{\circ}C$) and high temperature ($350{\sim}400^{\circ}C$) indicating that there were two kinds of acidities. Tetracarboxylic cobalt phthalocyanine (Co-TCPC) has a stronger desorption peak (chemical adsorption) at high temperature and a weaker desorption peak (physical adsorption) at low temperature than cobalt phthalocyanine (Co-PC). The specific surface areas of Co-TCPC and Co-PC were 37.5 and $18.4m^2/g$, respectively. The pore volumes of Co-TCPC and Co-PC were 0.17 and $0.10cm^3/g$, respectively. The adsorption capability of triethyl amine calculated by breakthrough curve at 120 ppm of equilibrium concentration was 24.3 mmol/g for Co-TCPC and 0.8 mmol/g for Co-PC. The removal efficiencies of dimethyl sulfide of Co-TCPC and Co-PC in batch experiment of 225 ppm of initial concentration were 92 and 18%, respectively. The removal efficiencies of trimethyl amine of Co-TCPC and Co-PC in batch experiment of 118 ppm of initial concentration were 100 and 17%, respectively.

• Bulletin of the Korean Chemical Society
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• v.30 no.7
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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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• v.57 no.5
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• pp.714-722
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• 2019

Catalysts were prepared by using incipient wetness impregnation method with 17 wt% Ni on a support ($SiO_2-Y_2O_3$, $Al_2O_3$, $SiO_2-ZrO_2$, $SiO_2$, $TiO_2$, MgO) and the catalytic activity in the reductive amination of ethanol with ammonia in the presence of hydrogen was compared and evaluated. The catalysts used before and after the reaction were characterized using X-ray diffraction, nitrogen adsorption, ethanol-temperature programmed desorption (EtOH-TPD), isopropanol-temperature programmed desorption (IPA-TPD), and hydrogen chemisorption etc. In the case of preparing $ZrO_2$ and $Y_2O_3$ supports, the small amount of Si dissolution from the Pyrex reactor surface provoked the formation of mixed oxides $SiO_2-ZrO_2$ and $SiO_2-Y_2O_3$. Among the catalysts used, $Ni/SiO_2-Y_2O_3$ catalyst showed the best activity, and this good activity was closely related to the highest nickel dispersion, and low desorption temperature in EtOH-TPD and IPA-TPD. The low catalytic activity on Ni/MgO catalysts showed low activity due to the formation of NiO-MgO solid-solutions. In the case of $Ni/TiO_2$, the reactivity was low due to the low nickel metal phase due to strong metal-support interaction. In the case of using a support as $SiO_2-Y_2O_3$, $Al_2O_3$, $SiO_2-ZrO_2$, and $SiO_2$, the selectivities of ethylamines and acetonitrile were not significantly different at similar ethanol conversion.