• Corrosion Science and Technology
• /
• v.6 no.5
• /
• pp.257-260
• /
• 2007

In order to further improve the corrosion resistance and wear resistance of the Ni-P coatings of electroless plating, electroless Ni-P/n-$Al_2O_3$ composite deposits were prepared by adding some nano $Al_2O_3$ Particles in Ni-P plating bath. The bath composition and proproties were studied in this paper. The orthogonal test was applied in order to get the new composite solution, taking the initial stable potential as evaluation standard and considering the elements correlation at the same time. The processing parameters have been optimized by single factor experiment in which the depositing speed was chosen as the evaluation standard. The results showed that the process is stable and the composite Ni-P/n-$Al_2O_3$ deposits werebright and smooth, whose hardness and corrosion resistance are much better than simple Ni-P coatings. Furthermore the surface appearance and structure of the composite Ni-P/n-$Al_2O_3$ coating were investigated by SEM and XRD method. It was proved that the coating surface is typical cystiform cells and its structure is amorphous. All test results ofcomposite coating showed that all various physical coating properties had been improved by adding nano-particles. The hardness of optimal coating is more than 600HV and increases to 1000HV after heat-treating, and its hardness is 20~50% higher than Ni-P coating. The rust points appeared in 200 hour by immersing the coating into the 10%HCl solution and the corrosive speed is $3{\times}10^{-3}mg/(cm^2{\cdot}h)$which was obtained after 300 hour. In the same condition Ni-P coating is $5.6{\times}10^{-3}mg/(cm^2{\cdot}h)$. The salt spray resistance of the layers can exceed 600h with the thickness $20{\mu}m$.

• Korean Journal of Materials Research
• /
• v.8 no.12
• /
• pp.1158-1164
• /
• 1998

Aluminium sulfate solution was prepared by sulfuric acid treatment from gibbsite. Aluminium sulfate hydrate [$Al_2(SO_4)_3$ · $nH_2O$] was precipitated from aluminium sulfate solution by adding it into ethylalcohol. From XRD analysis as-prepared $Al_2(SO_4)_3$ · $nH_2O$ was confirmed to have mixed-crystalization water(n=18, 16, 12, 6). The average water of crystalization calculated from thermogravimetry(TG) was 14.7. Aluminium sulfate hydrate [$Al_2(SO_4)_3$ · $nH_2O$] was thermally decomposed and converted to $Al_2(SO_4)_3$ at $800^{\circ}C$, $\gamma-Al_2O_3$ at $900-1000^{\circ}C$, and $\alpha-Al_2O_3$ at $1200^{\circ}C$. Ni-doped $\gamma-Al_2O_3$, was synthesized from the slurry of as-prepared $\gamma-Al_2O_3$, with the ratio of [Ni]/[Al]=0.5. The reaction conditions of synthesis were determined as initial pH 9.0 and temperature $80^{\circ}C$ The basicity(pH) of slurry was controlled by using urea and $NH_4OH$ solution. Urea was also used for deposition-precipitation. For determining termination of reaction, the data acquisition was performed by oxidation reduction potential(ORP), conductivity and pH value in the process of reaction. Termination of the reaction was decided by observing the reaction steps and rapid decrease in conductivity. On the other hand, BET(Brunauer, Emmett and Teller) and thermal diffusity of Ni- doped $\gamma-Al_2O_3$, with various content of Ni were measured and compared. Thermal stability of Ni- doped $\gamma-Al_2O_3$ at $1250^{\circ}C$ was confirmed from BET and XRD analysis. The surface state of Ni-doped $\gamma-Al_2O_3$ was investigated by X-ray photoelectron spectroscopy(XPS). The binding energy at $Ni2P_{3/2}$ increased with increasing the formation of $NiAl_2O_4$ phase.

• Advances in Energy Research
• /
• v.8 no.4
• /
• pp.223-231
• /
• 2022

An ex-situ gravitational fixed bed pyrolysis reactor was used over Al₂O₃ supported Ni₂P based catalyst with various Ni/P molar ratios (0.5-2.0) and constant nickel loading of 5.37 mmol/g Al₂O₃ to determine the hydrodeoxygenation of rubberwood sawdust (RWS) at atmospheric pressure. The 3D catalysts formed were characterized structurally as well as acidic properties were determined by hydrogen-temperature programmed reduction (TPR). The Ni₂P phase formed completely on Al₂O₃ for 1.5 Ni/P ratio, although lesser crystallite sizes of Ni₂P were seen at Ni/P ratios less than 1.5. Additionally, it was shown that when nickel loading level increased, acidity increased and specific surface area dropped, probably because nickel phosphate is not easily converted to Ni₂P. When Ni/P ratio was 1.5, Ni₂P phase fully formed on Al₂O₃. The catalytic activity was explained in terms of impacts of reaction temperature and Ni/P molar ratio. At relatively high temperature of 450℃, the high-value deoxygenated produce was predominantly composed of n-alkanes. Based on the findings, it was suggested that hydrogenolysis, hydrodeoxygenation, dehydration, decarbonylation, and hydrogenation are all part of mechanism underlying hydrotreatment of RWS. In conclusion, the synthesized Ni₂P/ Al₂O₃ catalyst was capable of deoxygenating RWS with ease at atmospheric pressure, primarily resulting in long chained (C₉-C₂₄) hydrocarbons and acetic acid.

• Applied Chemistry for Engineering
• /
• v.27 no.3
• /
• pp.313-318
• /
• 2016

In this study, an amorphous silica was functionalized with aminosilane, N-[(3-trimethoxysilyl)propyl]ethylenediamine (2NS) and the late transition metal catalysts including ($(DME)NiBr_2$ and $PdCl_2$(COD)) were subsequently immobilized on the functionalized amorphous silica for norbornene polymerization. Effects of the polymerization temperature, polymerization time, Al/Ni molar ratio, and type of co-catalyst on norbornene polymerization were investigated. Unsupported late transition metal catalysts did not show any activities for norbornene polymerization. However, the $SiO_2$/2NS/Ni catayst with MAO system, with increasing polymerization temperature, increased the polymerization activity and decreased the molecular weight of the polynorbornene (PNB). Furthermore, the catalyst when increasing polymerization temperature caused the decrease in both the polymerization activity and molecular weight of PNB. This confirmed that the stability of $SiO_2$/2NS/Ni at a high temperature was greater than that of $SiO_2$/2NS/Pd. Also the longer polymerization time resulted in the higher conversion of norbornene for both catalysts. When the Al : Ni molar ratio was 1000 : 1, the highest activity (15.3 kg-PNB/($({\mu}mol-Ni^*hr$)) but lowest molecular weight ($M_n$ = 124,000 g/mol) of PNB were achieved. Also $SiO_2$/2NS/Ni catalyst with borate/TEAL resulted in diminishing the polymerization activity and molecular weight of PNB with increasing the polymerization temperature.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
• /
• 2004.07a
• /
• pp.138-141
• /
• 2004

[ $MnO_2$ ]가 첨가된 $0.9Pb(Zr_{0.5}Ti_{0.5})O_3-0.2Pb[(Zn_{0.8}Ni_{0.2})_{1/3}Nb_{2/3}]O_3$(0.8PZT-0.2PZNN) 세라믹스는 그 압전특성과 유전특성이 뛰어나지만 $1000^{\circ}C$ 이하의 낮은 소결 온도에서는 소결되지 않는다. $1000^{\circ}C$이하의 낮은 소결온도에서 소결하기 위해 CuO를 첨가한 결과, 소결온도 $920^{\circ}C$에서 소결성은 우수하였으나 그 압전 특성의 저하가 두드러졌다. 이는 XRD에서 확인한 결과에 따르면 CuO의 첨가가 우수한 MPB 조성으로 판명된 $MnO_2$ 가 첨가된 0.8PZT-0.2PZNN 세라믹스의 결정구조를 Rhombohedral 구조로 바꾸기 때문인 것으로 보였으며 이러한 문제는 PZNN의 비율을 조절하여 0.875PZT-0.125PZNN 세라믹스를 선택함으로 인해 해결할 수 있었다. 그러나 여전히 낮은 $Q_m$값을 높이기 위해서 $Al_2O_3$를 첨가하였고 그 결과 시편의 tetragonality 감소와 $Q_m$값의 증가를 확인할 수 있었으나 그 첨가량이 0.2wt% 이상일 경우에는 밀도의 감소로 인한 압전특성의 저하가 나타났다. 밀도의 향상을 위해 Zn and Ni excess 조성을 선택하였고 그 결과 0.5wt% $MnO_2$와 0.2wt% CuO 그리고 0.3wt% $Al_2O_3$를 첨가한 0.875PZT-0.125PZNN 세라믹스(Zn and Ni excess 조성)를 $920^{\circ}C$에서 소결한 경우 $k_p=0.581,\;Q_m=809,\;d_{33}=345\;pC/N\;and\;{\varepsilon}_{33}/{\varepsilon}_0=1345$의 빼어난 압전 및 유전특성과 $330^{\circ}C$의 높은 $T_c$를 보였고 그 조성의 vibration velocity는 약4.5 m/s로 나타났다.

• Proceedings of the Korean Vacuum Society Conference
• /
• 2011.08a
• /
• pp.249-249
• /
• 2011

투명전도성산화물(transparent conducting oxides, TCOs) 박막은 전기 전도성과 광투과성이 우수하여 유기발광다이오드(organic light-emitting diode, OLED), 태양전지(solar cell), 발광다이오드(LED) 등의 광전자 소자에 널리 응용되고 있다. 특히 LED에서 p-GaN층에서 전류가 층안에서 충분하게 확산되지 않기 때문에, TCO는 균일하게 전류를 흘려보내기 위해서 전류확산층(current spreading layer)으로 사용된다. 그 중 널리 쓰이는 산화인듐주석(indium tin oxide, ITO)은 고가의 indium가격과 인체에 유해한 독성 등이 문제점으로 지적되고 있다. 따라서 indium의 함량을 저감하거나 함유하지 않은 새로운 조성의 친환경적 대체 TCO 개발에 대한 연구가 많이 진행되고 있다. 이러한 반도체 재료 중 하나인 AZO (Al-doped zinc oxide, Al2O3 : 2wt.%)는 3.3 eV의 넓은 에너지 밴드갭을 가지며, 가시광선 및 근적외선 파장영역에서 높은 투과율을 나타낸다. 따라서 본 연구에서는 GaN기반 LED 응용을 위한 전류확산층으로 ITO 대신 AZO의 특성을 연구하였다. 박막 증착율이 높고, 제작과정의 조정이 용이한 RF magnetron 스퍼터를 이용하여 glass기판 위에 AZO, Ni/AZO, NiOx/AZO를 증착하였다. 이어서 $N_2$ 분위기에서 다양한 온도 조건에서 열처리(rapid thermal annealing, RTA)하여 전기적 광학적 특성에 대하여 비교 분석하였다.

• Proceedings of the Korean Vacuum Society Conference
• /
• 2010.08a
• /
• pp.211-212
• /
• 2010

GaN 기반의 상부발광형 LED는 동작되는 동안 생기는 전기적 단락, 그리고 칩 위의 p-형 전극과 n-형 전극 사이에 생기는 누설전류 및 신뢰성 확보를 위하여 칩 표면에 passivation 층을 형성하게 된다. SiO2, Si3N4와 같은 passivation layers는 일반적으로 PECVD (Plasma Enhanced Chemical Vapor Deposition)공정을 이용한다, 하지만 이는 공정 특성상 plasma로 인한 damage가 유발되기 때문에 표면 누설 전류가 증가 한다. 이로 인해 forward voltage와 reverse leakage current의 특성이 저하된다. 본 실험에서는 원자층 단위의 박막 증착으로 인해 PECVD보다 단차 피복성이 매우 우수한 PEALD(Plasma Enhanced Atomic Layer Deposition)공정을 이용하여 Al2O3 passivation layer를 증착한 후, 표면 누설전류와 빛의 출력 특성에 대해서 조사해 보았다. PSS (patterned sapphire substrate) 위에 성장된 LED 에피구조를 사용하였고, TCP(Trancformer Copled Plasma)장비를 사용하여 에칭 공정을 진행하였다. 이때 투명전극을 증착하기 위해 e-beam evaporator를 사용하여 Ni/Au를 각각 $50\;{\AA}$씩 증착한 후 오믹 특성을 향상시키기 위하여 $500^{\circ}C$에서 열처리를 해주었다. 그리고 Ti/Au($300/4000{\AA}$) 메탈을 사용하여 p-전극과 n-전극을 형성하였다. Passivation을 하지 않은 경우에는 reverse leakage current가 -5V 에서 $-1.9{\times}10-8$ A 로 측정되었고, SiO2와 Si3N4을 passivation으로 이용한 경우에는 각각 $8.7{\times}10-9$과 $-2.2{\times}10-9$로 측정되었다. Fig. 1 에서 보면 알 수 있듯이 5 nm의 Al2O3 film을 passivation layer로 이용할 경우 passivation을 하지 않은 경우를 제외한 다른 passivation 경우보다 reverse leakage current가 약 2 order ($-3.46{\times}10-11$ A) 정도 낮게 측정되었다. 그 이유는 CVD 공정보다 짧은 ALD의 공정시간과 더 낮은 RF Power로 인해 plasma damage를 덜 입게 되어 나타난 것으로 생각된다. Fig. 2 에서는 Al2O3로 passivation을 한 소자의 forward voltage가 SiO2와 Si3N4로 passivation을 한 소자보다 각각 0.07 V와 0.25 V씩 낮아지는 것을 확인할 수 있었다. 또한 Fig. 3 에서는 Al2O3로 passivation을 한 소자의 output power가 SiO2와 Si3N4로 passivation을 한 소자보다 각각 2.7%와 24.6%씩 증가한 것을 볼 수 있다. Output power가 증가된 원인으로는 향상된 forward voltage 및 reverse에서의 leakage 특성과 공기보다 높은 Al2O3의 굴절률이 광출력 효율을 증가시켰기 때문인 것으로 판단된다.

• Proceedings of the Korean Vacuum Society Conference
• /
• 1999.07a
• /
• pp.115-115
• /
• 1999

GaN는 직접천이형 wide band gap(3.4eV) 반도체로서 청색/자외선 발광소자 및 고출력 전자장비등에의 응용성 때문에 폭넓게 연구되고 있다. 이러한 넓은 분야의 응용을 위해서는 열 적으로 안정된 Ohmic contact을 반드시 실현되어야 한다. n-type GaN의 경우에는 GaN계면에서의 N vacancy가 n-type carrier로 작용하기 때문에 Ti, Al, 같은 금속을 접합하여 nitride를 형성함에 의해서 낮은 접촉저항을 갖는 Ohmic contact을 하기가 쉽다. 그러나 p-type의 경우에는 일 함수가 크고 n-type와 다르게 nitride가 형성되지 않는 금속이 Ohmic contact을 할 가능성이 많다. 시료는 HF(HF:H2O=1:1)에서 10분간 초음파 세척을 한 후 깨끗한 물에 충분히 헹구었다. 그런 후에 고순도 Ar 가스로 건조시켰다. Pd와 Ni은 열적 증착법(thermal evaporation)을 사용하여 p-GaN에 상온에서 증착하였다. 현 연구에서는 열처리에 의한 Pd의 clustering을 줄이기 위해서 wetting이 좋은 Ni을 Pd 증착 전과 후에 삽입하였으며, monchromatic XPS(x-ray photoelectron spectroscopy) 와 SAM(scanning Auger microscopy)을 사용하여 열처리 전과 40$0^{\circ}C$, 52$0^{\circ}C$ 그리고 695$0^{\circ}C$에서 3분간 열처리 후의 온도에 따른 morphology 변화, 계면반응(interfacial reaction) 및 벤드 휨(band bending)을 비교 연구하였다. Nls core level peak를 사용한 band bending에서 Schottky barrier height는 Pd/Ni bi-layer 접합시 2.1eV를, Ni/Pd bi-layer의 경우에 2.01eV를 얻었으며, 이는 Pd와 Ni의 이상적인 Schottky barrier height 값 2.38eV, 2.35eV와 비교해 볼 때 매우 유사한 값임을 알 수 있다. 시료를 후열처리함에 의해 52$0^{\circ}C$까지는 barrier height는 큰 변화가 없으나, $650^{\circ}C$에서 3분 열처리 후에 0.36eV, 0.28eV 만큼 band가 더 ？을 알 수 있었다. Pd/Ni 및 Ni/Pd 접합시 $650^{\circ}C$까지 후 열 처리 과정에서 계면에서 matallic Ga은 온도에 비례하여 많은 양이 형성되어 표면으로 편석(segregation)되어지나, In-situ SAM을 이용한 depth profile을 통해서 Ni/Pd, Pd/Ni는 증착시 uniform하게 성장함을 알 수 있었으며, 후열처리 함에 의해서 점차적으로 morphology 의 변화가 일어나기 시작함을 볼 수 있었다. 이는 $650^{\circ}C$에서 열처리 한후의 ex-situ AFM을 통해서 재확인 할 수 있었다. 이상의 결과로부터 GaN에 Pd를 접합 시 심한 clustering이 형성되어 Ohoic contact에 문제가 있으나 Pd/Ni 혹은 Ni/Pd bi-layer를 사용함에 의해서 clustering의 크기를 줄일 수 있었다. Clustering의 크기는 Ni/Pd bi-layer의 경우가 작았으며, $650^{\circ}C$ 열처리 후에 barrier height는 Pd/Ni bi-layer의 경우에도 Ni의 영향을 받음을 알 수 있었다.

• Journal of Korean Society for Atmospheric Environment
• /
• v.13 no.5
• /
• pp.371-381
• /
• 1997

Precipitation sampls were collected in Chonju-city during October 1994 to September 1995 and were analysed for major ions (N $a^{+}$, $K^{+}$, $Ca^{2+}$, $Mg^{2+}$, C $l^{[-10]}$ , NO/$_3$, S $O_4$$^{2-}$) and trace metals (Al, Cd, Ni, Pb, Sr, Zn) in addition to pH, in order to understand the chemical characteristics of acid rain and to estimate the origin of the determined ions. Most rain showed a neutral or alkaline character, and only 35% had a pH lower than 5.6. S $O_4$$^{2-}$ and N $O_3$$^{[-10]}$ are identified as the primary contributors to precipitation acidity in this region. Neutralization of precipitation acidity occurs as a result of the dissolution of alkaline compounds containing $Ca^{2+}$, $Mg^{2+}$ and $K^{+}$. S $O_4$$^{2-}$ and N $O_3$$^{[-10]}$ precipitation concentrations exhibit a seasonal pattern in which higher concentrations are observed during spring months and lower concentrations during summer months. However, the seasonal behavior of $H^{+}$ concentrations differs from this pattern, in that the highest concentrations occur during autumn months, owing to the different influence of neutralization processes. In all rain, S $O_4$$^{2-}$ concentration exceeded NO/$_3$$^{[-10]}$ concentration. The contribution of maritime sources to the total S $O_4$$^{2-}$ concentration was very low or negligible. For rain strongly affacted by yellow sand, $Ca^{2+}$, $Mg^{2+}$ and $K^{+}$ ions show a sharp increase in concentration, reflecting the increased amount of dust and soil suspended in atmosphere. At the same time, S $O_4$$^{2-}$ and N $O_3$$^{[-10]}$ concentrations are at their highest levels while $H^{+}$ values are not comparably elevated, presumably beacause much of the acidity has been neutralized by alkaline substances. The seasonal variance of trace metal concentrations in rainwater is similar to that of major cations. The annual wet flux of acidic pollutants and trace metals wat calculated to be as follows: N $O_3$$^{[-10]}$ ; 2.32 g/$m^2$, S $O_4$$^{2-}$, 5.34 g/$m^2$, Al; 6.30 mg/$m^2$, Cd; 0.62 mg/$m^2$, Ni; 4.08 mg/$m^2$, Pb: 9.76 mg/$m^2$, Sr; 5.94 mg/$m^2$, Zn; 111 mg/$m^2$./$m^2$.

• Asian Pacific Journal of Cancer Prevention
• /
• v.17 no.10
• /
• pp.4761-4767
• /
• 2016

Objective: The use of Shamma (smokeless tobacco) by certain groups is giving rise to health problems, including cancer, in parts of Saudi Arabia. Our objective was to determine metals levels in Shamma using inductively coupled plasma mass spectrometry (ICP-MS). Methods: Thirty-three samples of Shamma (smokeless tobacco) were collected, comprising four types: brown Shamma (n = 14.0), red Shamma (n = 9.0), white Shamma (n = 4.0), and yellow Shamma (n = 6.0). All samples were collected randomly from Shamma users in the city of Najran. Levels of 11 elements (Al, As, Cd, Co, Cr, Cu, Li, Mn, Ni, Pb, and Zn) were determined by ICP-MS. Results: A mixed standard (20 ppb) of all elements was used for quality control, and average recoveries ranged from 74.7% to 112.2%. The highest average concentrations were found in the following order: Al ($598.8-812.2{\mu}g/g$), Mn ($51.0-80.6{\mu}g/g$), and Ni ($23.2-53.3{\mu}g/g$) in all four Shamma types. The lowest concentrations were for As ($0.7-1.0{\mu}g/g$) and Cd ($0.0-0.06{\mu}g/g$). Conclusions: The colour of each Shamma type reflects additives mixed into the tobacco. Cr and Cu were showed significant differences (P < 0.05) among Shamma types. Moreover, Pb levels are higher in red and yellow Shamma, which could be due to use (PbCrO4) as yellow colouring agent and lead tetroxide, Pb3O4 as a red colouring agent. The findings from this study can be used to raise public awareness about the safety and health effects of Shamma, which is clearly a source of oral exposure to metals.