• Bulletin of the Korean Chemical Society
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• 제22권1호
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• pp.30-36
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• 2001

The crystal structures of fully dehydrated $Pd^{2+}$ - and $TI^{+}$ -exchanged zeolite X, $Pd_{18}TI_{56}Si_{100}Al_{92}O_{384}(Pd_{18}TI_{50-}X$, a = $24.935(4)\AA$ and $Pd_{21}TI_{50}Si_{100}Al_{92}O_{384}(Pd_{21}TI_{50-}X$ a = $24.914(4)\AA)$, have been determined by single-crystal X-ray diffraction methods in the cubic space group Fd3 at $21(1)^{\circ}C.$ The crystals were prepared using an exchange solution that had a $Pd(NH_3)_4Cl_2\;:TINO_3$ mole ratio of 50 : 1 and 200 : 1, respectively, with a total concentration of 0.05M for 4 days. After dehydration at $360^{\circ}C$ and 2 ${\times}$$10^{-6}$ Torr in flowing oxygen for 2 days, the crystals were evacuated at $21(1)^{\circ}C$ for 2 hours. They were refined to the final error indices $R_1$ = 0.045 and $R_2$ = 0.038 with 344 reflections for $Pd_{18}Tl_{56-}X$, and $R_1$ = 0.043 and $R_2$ = 0.045 with 280 reflections for $Pd_{21}Tl_{50-}X$; I > $3\sigma(I).$ In the structure of dehydrated $Pd_{18}Tl_{56-}X$, eighteen $Pd^{2+}$ ions and fourteen $TI^{+}$ ions are located at site I'. About twenty-seven $TI^{+}$ ions occupy site II recessed $1.74\AA$ into a supercage from the plane of three oxygens. The remaining fifteen $TI^{+}$ ions are distributed over two non-equivalent III' sites, with occupancies of 11 and 4, respectively. In the structure of $Pd_{21}Tl_{50-}X$, twenty $Pd^{2+}$ and ten $TI^{+}$ ions occupy site I', and one $Pd^{2+}$ ion is at site I. About twenty-three $TI^{+}$ ions occupy site II, and the remaining seventeen $TI^{+}$ ions are distributed over two different III' sites. $Pd^{2+}$ ions show a limit of exchange (ca. 39% and 46%), though their concentration of exchange was much higher than that of $TI^{+}$ ions. $Pd^{2+}$ ions tend to occupy site I', where they fit the double six-ring plane as nearly ideal trigonal planar. $TI^{+}$ ions fill the remaining I' sites, then occupy site II and two different III' sites. The two crystal structures show that approximately two and one-half I' sites per sodalite cage may be occupied by $Pd^{2+}$ ions. The remaining I' sites are occupied by $TI^{+}$ ions with Tl-O bond distance that is shorter than the sum of their ionic radii. The electrostatic repulsion between two large $TI^{+}$ ions and between $TI^{+}$ and $Pd^{2+}$ ions in the same $\beta-cage$ pushes each other to the charged six-ring planes. It causes the Tl-O bond to have some covalent character. However, $TI^{+}$ ions at site II form ionic bonds with three oxygens because the super-cage has the available space to obtain the reliable ionic bonds.

• Korean Chemical Engineering Research
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• 제46권4호
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• pp.806-812
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• 2008

귀금속촉매 존재하에서 암모니아 전환반응은 배가스내의 암모니아를 처리하는데 중요한 기술이다. 과잉용액 함침법을 이용하여 $Pt-Rh/Al_2O_3$, $Pt-Rh/TiO_2$, $Pt-Rh/ZrO_2$, $Pt-Pd/Al_2O_3$, $Pd-Rh/Al_2O_3$, $Pd-Rh/TiO_2$, $Pd-Rh/ZrO_2$, $Pt-Pd-Rh/Al_2O_3$, $Pd/Ga-Al_2O_3$, $Rh/Ga-Al_2O_3$, 그리고 $Ru/Ga-Al_2O_3$의 촉매를 제조하였다. 제조된 촉매는 1/4"의 반응기에 $10,000{\sim}50,000hr^{-1}$의 공간속도 조건하에서 촉매활성능 실험을 수행하였다. 암모니아의 초기농도는 2,000 ppm (나머지는 공기)으로 유지하였다. $T_{50}$는 암모니아 전환율이 50%일 때를 나타내는 온도를, $T_{90}$은 90%의 전환율일 때의 온도를 나타낸다. 알루미나를 담지체로 사용했을때의 $T_{50}$와 $T_{90}$은 다른 담체를 사용했을때의 $T_{50}$와 $T_{90}$보다 훨씬 낮았다. Pd-Rh촉매의 경우 $Al_2O_3$를 담체로 사용하였을 때 $ZrO_2$나 $TiO_2$보다 저온 활성이 우수하게 나타났다. 황산화물의 피독실험 결과 본 연구에서는 최종적으로 $Pt-Rh/Al_2O_3$ 촉매가 다른 촉매에 비하여 우수함을 보였다. 실험결과 Pt-Rh가 암모니아 전환공정에서 유용한 촉매라는 사실을 알 수 있다.

• 분석과학
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• 제19권4호
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• pp.333-341
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• 2006

PVP-protected Ag, Pd and $Pt_{50}-Ru_{50}$ colloids were prepared independently by using ${\gamma}$-irradiation and electron beam (EB) at ambient temperature. UV-visible spectra of these colloids show the characteristic bands of surface resonance and give evidence for the formation of nanoparticles. Transmission electron microscopy (TEM) experiments were used to know the morphology of nanoparticles prepared by ${\gamma}$-irradiation and EB. The size of Ag, Pd, and $Pt_{50}-Ru_{50}$ nanoparticles prepared by ${\gamma}$-irradiation was ca. 13, 2-3, 15 nm, respectively. While, the size of Ag, Pd, and $Pt_{50}-Ru_{50}$ nanoparticles prepared by EB was ca. 10, 6, and 1-3 nm, respectively. Cyclic voltamograms (CV) were recorded for the Au electrodes immobilized with these nanoparticles. CVs indicated the modifications in the surface as a result of immobilization.

• 대한화학회지
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• 제50권5호
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• pp.369-373
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• 2006

Pd(CF3CO2)2-phosphine 및 Pd(CF3CO2)2-sulfide 계를 촉매로 사용하여 styrene의 아릴화반응을 연구하였다. 주 생성물인 trans-stilbene의 수율은 phosphine 치환체의 염기도가 증가할수록 높아졌고 입체장애가 클수록 낮아졌다. arylphosphine에서 styrene으로 aryl 기가 이동하는 현상은 동일한 arylphosphine에 대하여 Pd(CF3CO2)2의 경우가 더 높은 염기도를 가진 Pd(CH3CO2)2의 경우보다 더 많이 나타났으므로 이 반응은 Pd 이온이 먼저 aryl 기에 공격을 하는 친전자성 메커니즘에 의해 진행된다고 본다. 한편 Pd(CF3CO2)2-sulfide보다 Pd(CF3CO2)2-phosphine 계가 더 효과적인 촉매로 작용하였다.

• BMB Reports
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• 제50권11호
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• pp.578-583
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• 2017

Programmed cell death-1 (PD-1) is a coinhibitory molecule and plays a pivotal role in immune regulation. Here, we demonstrate a role for PD-1 in pathogenesis of inflammatory bowel disease (IBD). Wild-type (WT) mice had severe wasting disease during experimentally induced colitis, while mice deficient for PD-1 ($PD-1^{-/-}$) did not develop colon inflammation. Interestingly, $PD-1^{-/-}$ mice cohoused with WT mice became susceptible to colitis, suggesting that resistance of $PD-1^{-/-}$ mice to colitis is dependent on their gut microbiota. 16S rRNA gene-pyrosequencing analysis showed that $PD-1^{-/-}$ mice had altered composition of gut microbiota with significant reduction in Rikenellaceae family. These altered colon bacteria of $PD-1^{-/-}$ mice induced less amount of inflammatory mediators from colon epithelial cells, including interleukin (IL)-6, and inflammatory chemokines. Taken together, our study indicates that PD-1 expression is involved in the resistance to experimental colitis through altered bacterial communities of colon.

• 한국표면공학회지
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• 제50권5호
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• pp.411-420
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• 2017

In this paper, two methods of making the Pd-added $SnO_2$ ($Pd-SnO_2$) powder with pure tetragonal phase by the hydrazine method were suggested and compared in terms of crystal structure, surface morphology, and alcohol gas response. One of the addition methods is to use $PdCl_2$ as a Pd source, the other is to use Pd-based organic with oleylamine (OAM). When Pd concentration was increased from 0 to 5 wt%, the average grain size of $Pd-SnO_2$ made with Pd-OAM were decreased from 32 to 12 nm. In the case of using with $PdCl_2$, grain size of the $PdCl_2$ fell to less than 10 nm. However, agglomerated and extruded surface morphology was observed for the films with Pd addition over 4 wt%. The crack-free $Pd-SnO_2$ thick films were able to successfully fill the $30{\mu}m$ gap of patterned Pt electrodes by optimized ink dropping method. Also, the 2 wt% $Pd-SnO_2$ thick film made with PdCl2 showed gas responses ($R_{air}/R_{gas}$) of 3.7, 5.7 and 9.0 at alcohol concentrations of 10, 50 and 100 ppm, respectively. On the other hand, the prepared 3 wt% $Pd-SnO_2$ thick film with Pd-OAM exhibited very excellent responses of 3.4, 6.8 and 12.2 at the equivalent measurement conditions, respectively. The 3 wt% $Pd-SnO_2$ thick film with Pd-OAM has a specific surface area of $31.39m^2/g$.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2010년도 제39회 하계학술대회 초록집
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• pp.84-84
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• 2010

We present an in-situ study of the interaction of a bimetallic Rh50Pd50 bulk crystal with O2, CO, and NO using ambient pressure x-ray photoelectron spectroscopy and compare it to results for 10 nm nanoparticles with the same overall composition. The surface of the bulk crystal has less Rh present under both oxidizing and reducing conditions than the nanoparticles under identical conditions. Segregation and oxidation/reduction proceeds quicker and at lower temperature for nanoparticles than for the bulk crystal. The near surface of the Rh50Pd50 bulk crystal after high temperature vacuum annealing is ca. 9% Rh measured by XPS. Heating in 0.1 Torr O2 to $350^{\circ}C$ increases the Rh surface composition to ca. 40%. The surface can then be reduced by heating in H2 at $150^{\circ}C$, leading to a reduced surface of 30% Rh. Titration of CO from this Rh-rich surface proceeds at a much lower pressure than on the Rh-deficient starting surface.

• 한국전기화학회:학술대회논문집
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• 한국전기화학회 1999년도 제3회 총회 및 추계학술발표회
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• pp.50-50
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• 1999

• 센서학회지
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• 제29권6호
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• pp.399-406
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• 2020

Pd nanogap hydrogen sensors were developed using an elastomeric substrate and operated through an on-off mechanism. A 10 nm thick Pd thin film was formed on a polydimethylsiloxane (PDMS) substrate, and 50% of the physical strain was applied in the longitudinal direction to fabricated uniform nanogaps. The initial concentration of the hydrogen gas for the PDMS/Pd films was controlled, and subsequently, the on-off switching response was measured. We found that the average nanogap was less than 50 nm, and the Pd nanogap hydrogen sensors operated over a wide range of temperatures. In particular, the sensors work properly even at a very low temperature of -40℃ with a fast response time of 2 s. In addition, we have investigated the relative humidity and annealing effects.

• 한국결정학회지
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• 제1권2호
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• pp.66-75
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• 1990

Pd-Te계의 상평형도를 시차열분석, X선회절분석, 전자현미분석, 반사현미경을 사용해 연구하였다. 본 계의 0-50 at.%Te 부분의 새로운 상관계가 정립되었다. 본 계에는 Pd17Te4, Pd20Te7, Pd8Te3, Pd7Te3, PdgTe4, Pd3Te2, PdTe, PdTe2 등 8개의 화합물이 존재하며 이중 Pd17Te4와 Pd7Te3는 처음 보고되는 신종 화합물이다. Pd17Te4는 등축정계이며 공간군 Fd3r에 속하며 단위포 크기 (a)는 12. 678(5)차이다. PdaTe.4와Pd7Te3의 X선회절분말자료는 사방정계의 단위포 a=12.843(3), b=15.126(3), c=11.304(2)A와 단사 정계의 단위포 a=7.444(1), b=13.918(2), c=8.873 (2)il, β=92.46(2)에 의해 각각 격자지수화가 가능하였다. 본계에 존재하는 합성 화합물의 일부 물리적, 광학적 자료를 새로 보고하였다.