TEM-characterization-of-super-hydrophilic-Ni-Ti-thin-film_2011_Materials-Letters
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海底钴结壳TEM的响应规律李丽;席振铢;王鹤;李瑞雪【摘要】大洋富钴结壳是潜在的海底金属资源,为了更快、更准确地对海底钴结壳进行勘探,本文研究了其TEM的响应规律.通过分析深海钴结壳的电性和物性特征,说明了瞬变电磁法满足海底探测的物化条件,进而建立探测深海钴结壳的地电模型,证明了本方法应用于海底钻结壳勘探的可行性;采用瞬变电磁全空间理论,计算了深海钴结壳瞬变电磁响应,这为瞬变电磁探测深海钴结壳的反演提供了依据.计算结果表明:海底瞬变电磁测深能很好地探测到海底钴结壳的存在,且异常峰值对应钴结壳的中心在海面的投影位置;深海与无海水情况下的瞬变电磁相比,响应曲线形态变化不大,响应幅值明显增加;地形对探测有一定的影响.【期刊名称】《工程地球物理学报》【年(卷),期】2015(012)003【总页数】5页(P283-287)【关键词】富钴结壳;海洋瞬变电磁法;全空间【作者】李丽;席振铢;王鹤;李瑞雪【作者单位】中南大学地球科学与信息物理学院,湖南长沙410083;中南大学海洋矿产探测技术与装备研究所,湖南长沙410083;中南大学地球科学与信息物理学院,湖南长沙410083;中南大学海洋矿产探测技术与装备研究所,湖南长沙410083;中南大学地球科学与信息物理学院,湖南长沙410083;中南大学海洋矿产探测技术与装备研究所,湖南长沙410083;中南大学地球科学与信息物理学院,湖南长沙410083;中南大学海洋矿产探测技术与装备研究所,湖南长沙410083【正文语种】中文【中图分类】P631.3海底富钴结壳是近几十年来新发现的、具有重要战略意义的一种海底矿产资源。
钴结壳赋存水深较浅,广泛分布于水深800~3000m的海山、岛屿斜坡上,开采基本不会对海洋环境造成危害。
富钴结壳富含钴、镍、铅、铈、铂等金属,平均厚度2~8cm。
钴是一种高熔点和稳定性良好的磁性硬金属,是制造硬质合金、耐热合金、耐磨合金、磁性合金、特种合金和各种钴盐或钴化合物的重要原料[1]。
物探瞬变电磁法(TEM)和激发激化法在贵州金矿勘探中的应用汪玉琼;孙宗龙【摘要】简述了瞬变电磁法(TEM)和激发激化法在贵州某金矿勘探中的综合应用.文中介绍了TEM瞬变电磁法、激发激化法原理、工作仪器及工作中所采用参数及资料整理中所有分析解释软件,选择了贵州某金矿X-X′线TEM剖面、岩性实测作为实例进行异常解释推断,对异常进行了分析,提出了下一步工作建议.【期刊名称】《工程地球物理学报》【年(卷),期】2010(007)001【总页数】3页(P75-77)【关键词】金矿;瞬变电磁法(TEM);激发激化法;异常分析【作者】汪玉琼;孙宗龙【作者单位】贵州省地质调查院,贵州,贵阳,550004;安徽省勘查技术院,安徽,蚌埠,233005【正文语种】中文【中图分类】P631.3TEM瞬变电磁法是基于电性差异,利用不接地回线或接地线源向地下发送一次脉冲电磁场,利用线圈或接地电极观测二次涡流磁场或电场的方法。
主要为用于寻找低阻目标物,研究浅成至中深层地电结构[1]。
激发激化法是以岩(矿)石、水的激发极化效应的差异为物性前提,用人工地下直流电流激发,以某种极距的装置形式,研究地下横、纵向激发极化效应的变化,以查明矿产资源和有关地质问题的方法。
小四极激电测深是激发激化法的一种装置测量方式,用于测量深部地质体的导电性能。
[2]1)TEM工作仪器及参数选择脉冲瞬变电磁法(TEM)使用仪器为西安物探所研制的EM RS-2B型电磁矿产勘探仪。
供电脉冲宽为4m s、供电电流为1000~1200A,分22道读数,选择4~32次叠加,采样率为80μs,回线边长为3m×3m。
2)对称四极激电工作仪器使用重庆仪器厂生产的WDJD-1激电仪,其接收部分技术指标为:电压通道±6V±1%,输入阻抗50MΩ,视极化率测量精度±1%,Sp补偿范围±1V,电流通道5A±1%。
发射部分技术指标为:最大供电电压900V,最大供电电流5A,供电脉冲宽度1~60s。
17-P-006pH和UV刺激响应表面材料:从超疏水到超亲水蒋玉贵,万鹏博,王治强,张希*清华大学化学系,有机光电子与分子工程教育部重点实验室,北京100084E-mail: xi@刺激响应材料是指一类具有在外界刺激下可调控其物理化学性质的材料,将这类刺激响应材料引入到自组装单层膜体系中,就可实现利用外界刺激来调控表面结构和性质。
以前报道的pH刺激响应表面,基本上都是在低pH值条件下为超疏水表面,在高pH值条件下为超亲水表面。
为了制备一种新型的pH刺激响应表面,即在高pH值条件下为超疏水表面,在低pH值条件下为超亲水表面,我们设计合成了一种具有刺激响应性的末端为孔雀绿基团的烷基硫醇衍生物。
一方面,孔雀绿是一种刺激响应材料,在没有外界pH或者UV刺激条件下,孔雀绿基团是疏水的;而在外界pH或者UV刺激条件下,孔雀绿基团变为相应的带正电荷的亲水基团。
另一方面,硫醇衍生物中的巯基可以化学吸附于镀金表面形成自组装单层膜。
研究表明修饰上述单层膜的粗糙金表面,对pH=13的水滴,呈现约146.8º的接触角,而对pH=1的水滴,呈现约0º的接触角,同时这种从接近超疏水表面到超亲水表面的转变可以循环多次。
另外,上述表面的浸润性质,还可以通过UV光照时间进行调控,即从光照前的接近超疏水表面到光照后的超亲水表面。
关键词:pH和UV刺激响应材料;自组装单层膜;超疏水-超亲水转变。
参考文献:[1] Y. Jiang, P. Wan, M. Smet, Z. Wang, X. Zhang, Adv. Mater. 2008, adma.200702366.[2] Y. Jiang, Y. Wang, N. Ma, Z. Wang, M. Smet, X. Zhang, Langmuir2007, 23, 4029.[3] Y. Jiang, Z. Wang, H. Xu, H. Chen, X. Zhang, M. Smet, W. Dehaen, Y. Hirano, Y. Ozaki, Langmuir2006, 22, 3715.[4] Y. Jiang, Z. Wang, X. Yu, F. Shi, H. Xu, X. Zhang, M. Smet, W. Dehaen, Langmuir2005, 21, 1986.pH and UV-responsive surface material:from superhydrophobicityto superhydrophilicityYugui Jiang,Pengbo Wan,Zhiqiang Wang,Xi Zhang* Key Lab of Organic Optoelectronics and Molecular Engineering,Department ofChemistry,Tsinghua University,Beijing 100084Stimuli-responsive material can be introduced into the self-assembled monolayer (SAM) to realize the control of the structures and properties of SAM under different external stimuli. The pH-responsive surface that can undergo a change of the wetting properties from near superhydrophobicity at low pH, to superhydrophilicity at high pH, has been reported. We are wondering if we can realize a pH-responsive surface with completely uncommon response behavior, i.e. from near superhydrophobicity at high pH, to superhydrophilicity at low pH. For this purpose, we have designed and synthesized a stimuli-responsive malachite green terminated alkanethiol. For the SAM of this alkanethiol on rough gold covered surface, a large contact angle of about 146.8º is observed for a pH=13 water droplet, while a very small contact angle of about 0º is observed for a pH=1 water droplet. Moreover, the malachite green terminated alkanethiol is dual stimuli-responsive, the wetting properties of the SAM can be controlled and fine-tuned by the UV irradiation.54。
含有一个非平面杂环胺配体的新型反铂抗癌药物的水解机理赵亚华【期刊名称】《物理化学学报》【年(卷),期】2009(025)011【摘要】Hydrolysis processes of novel anticancer transplatin analogues, trans-[PtCl_2(NH_3)(Am)](Am: nonplanar heterocycle piperidine or piperazine), were explored using the B3LYP hybrid functional and isoclectric focusing polarized continuum model (IEF-PCM). Stationary points on the potential energy surfaces for the first and second hydrolysis steps that proceed via a general S_N2 pathway were fully optimized and characterized. The most remarkable structural variations in the hydrolysis process were found to occur in the equatorial plane of five-coordinate trigonal-bipyramidal (TBP) like structures of the intermediates and transition states. We obtained lower activation energies for trans-[PtCl_2(NH_3)(piperazine)] and a slightly higher activation energy for the first step and a slightly lower activation energy for the second step during the hydrolysis of trans-[PtCl_2(NH_3)(piperidine)] by comparison to previous work on the hydrolysis reactions of cisplatin. Our calculations suggest that this class of non-classical transplatin analogues with one nonplanar heterocyclic amine decreases the equatorial steric effect and the hydrolysis reaction barriers.%用B3LYP杂化泛函和等电子聚焦极化连续模型(IEF-PCM)研究了trans-[P[Cl_2(NH_3)(Am)](Am:非平面哌啶或哌嗪)新型反铂抗癌药物的水解反应机理.对经由一般的S_N2机理的第一步和第二步水解反应势能而上的稳定点进行了全优化和表征.在水解中,最显著的结构变化发生在反应过渡态和中间体的五配位三角双锥的赤道面上.与经典顺铂(cisplatin)比较,反式[PtCl_2(NH_3)(piperazine)]的第一步和第二步水解活化能均低于顺铂,而反式[PtCl_2(NH_3)(piperidine)]的第一步水解活化能稍高于顺铂,第二步水解活化能稍低于顺铂.计算表明,这些含有非平面杂环胺反铂的配合物减小了赤道面上的立体效应和水解势垒.【总页数】7页(P2350-2356)【作者】赵亚华【作者单位】华南农业大学生命科学学院,广州,510642【正文语种】中文【中图分类】O641【相关文献】1.抗癌药物——铂络合物中铂之测定 [J], 涂清和2.非对称反铂抗癌药物反-异丙胺·间羟甲基吡啶·二氯铂水解机理的理论研究 [J], 叶冰;许旋3.杂环反铂(Ⅱ)抗癌药物水解反应机理的DFT研究 [J], 李添;周立新;李娟4.以磷酸二氢根为轴向配体的铂(Ⅳ)前药的设计、合成和抗癌活性测试 [J], 高安丽;熊庆丰;姜婧;余娟;楼丽广;刘伟平5.铂配合物的抗癌作用及非铂抗癌物 [J], 高朝明因版权原因,仅展示原文概要,查看原文内容请购买。
第42 卷第 5 期2023 年5 月Vol.42 No.5559~567分析测试学报FENXI CESHI XUEBAO(Journal of Instrumental Analysis)超分子溶剂萃取/超高效液相色谱-串联质谱法测定血浆中他克莫司含量谢以清1,2,吕悦广2,孟宪双2,雷海民1*,马强2*(1.北京中医药大学中药学院,北京102488;2.中国检验检疫科学研究院,北京100176)摘要:该文建立了血浆中免疫抑制剂他克莫司(TAC)的超分子溶剂(SUPRAS)萃取/超高效液相色谱-串联质谱分析方法。
通过单因素实验结合响应面设计对超分子溶剂组成、用量及涡旋萃取时间等关键因素进行优化后,血浆样本以正戊醇、四氢呋喃和水形成的超分子溶剂进行高效萃取。
萃取液经Waters ACQUITY UPLC BEH C18(50 mm × 2.1 mm,1.7 μm)色谱柱分离后,在电喷雾质谱正离子模式下,以多反应监测(MRM)模式对他克莫司进行测定,内标法定量。
结果表明,他克莫司在0.5 ~ 30 ng/mL质量浓度范围内的线性关系良好,相关系数(r)为0.998 6;方法检出限和定量下限分别为0.1、0.5 ng/mL;在低、中、高3个加标水平下,平均回收率(n = 3)为91.9% ~ 99.9%,相对标准偏差(RSD)为1.7% ~ 5.7%。
所建立的方法快速、灵敏、稳定,适用于血浆中他克莫司的准确测定。
关键词:他克莫司;免疫抑制剂;超分子溶剂;血浆;超高效液相色谱-串联质谱中图分类号:O657.7;R917文献标识码:A 文章编号:1004-4957(2023)05-0559-09Determination of Tacrolimus in Plasma by Supramolecular Solvent Extraction/Ultra-high Performance Liquid Chromatography-Tandem Mass SpectrometryXIE Yi-qing1,2,LÜ Yue-guang2,MENG Xian-shuang2,LEI Hai-min1*,MA Qiang2*(1.School of Chinese Materia Medica,Beijing University of Chinese Medicine,Beijing 102488,China;2.Chinese Academy of Inspection and Quarantine,Beijing 100176,China)Abstract:An analytical method for the determination of tacrolimus(TAC) in blood plasma was estab⁃lished by supramolecular solvent(SUPRAS)extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry.After optimizing the key factors such as the composition and amount of SUPRAS,and vortex extraction time through single factor experiment and response sur⁃face design,blood plasma samples were extracted efficiently with SUPRAS formed by pentanol,tetra⁃hydrofuran and water.The extract was separated on a Waters ACQUITY UPLC BEH C18column (50 mm × 2.1 mm,1.7 μm),analyzed by electrospray ionization mass spectrometry in positive ion mode under multiple reaction monitoring(MRM) mode,and quantified by internal standard method.Experimental results demonstrated that there was a good linear relationship for TAC in the concentration range of 0.5-30 ng/mL,with a correlation coefficient(r) of 0.998 6.The limit of detection(LOD)and quantitation(LOQ) were 0.1 ng/mL and 0.5 ng/mL,respectively.The average recoveries(n = 3)at low,medium and high spiked concentration levels ranged from 91.9% to 99.9%,with relative stan⁃dard deviations(RSDs) of 1.7%-5.7%.The proposed method is rapid,sensitive and stable,and it was suitable for the accurate determination of TAC in blood plasma.Key words:tacrolimus;immunosuppresive agent;supramolecular solvent;plasma;ultra-high performance liquid chromatography-tandem mass spectrometry免疫抑制剂是用于抑制机体免疫力的药物,多用于抑制肝肾移植术后的免疫反应,以及治疗变态反应性和自身免疫性疾病,如类风湿关节炎、红斑狼疮等[1-3]。
In situ transmission electron microscopy study of the electric field-induced transformation of incommensurate modulations in a Sn-modified lead zirconate titanate ceramicH. He and X. TanCitation: Appl. Phys. Lett. 85, 3187 (2004); doi: 10.1063/1.1805179View online: /10.1063/1.1805179View Table of Contents: /resource/1/APPLAB/v85/i15Published by the American Institute of Physics.Related ArticlesComplete set of elastic, dielectric, and piezoelectric constants of [011]C poled rhombohedral Pb(In0.5Nb0.5)O3-Pb(Mg1/3Nb2/3)O3-PbTiO3:Mn single crystalsJ. Appl. Phys. 113, 074106 (2013)Compressible spherical dipolar glass model of relaxor ferroelectricsJ. Appl. Phys. 112, 114122 (2012)Tunable self-biased magnetoelectric response in homogenous laminatesAppl. Phys. Lett. 101, 232905 (2012)Self-assembled NaNbO3-Nb2O5 (ferroelectric-semiconductor) heterostructures grown on LaAlO3 substrates Appl. Phys. Lett. 101, 132902 (2012)Pressure and electric field effects on piezoelectric responses of KNbO3J. Appl. Phys. 112, 064106 (2012)Additional information on Appl. Phys. Lett.Journal Homepage: /Journal Information: /about/about_the_journalTop downloads: /features/most_downloadedInformation for Authors: /authorsIn situ transmission electron microscopy study of the electric field-induced transformation of incommensurate modulations in a Sn-modified lead zirconate titanate ceramicH.He and X.Tan a )Department of Materials Science and Engineering,Iowa State University,Ames,Iowa 50011(Received 7May 2004;accepted 11August 2004)Electric field-induced transformation of incommensurate modulations in a Sn-modified lead zirconate titanate ceramic was investigated with an electric field in situ transmission electron microscopy technique.It is found that the spacing between the ͑1/x ͕͒110͖satellite spots and the fundamental reflections do not change with external electric field,indicating that the modulation wavelength stays constant under applied field.The intensity of these satellites starts to decrease when the field level reaches a critical value.Further increase in the field strength eventually leadsto the complete disappearance of the satellite reflections.In addition,the 12͕111͖-type superlattice reflections showed no response to electrical stimuli.©2004American Institute of Physics .[DOI:10.1063/1.1805179]Incommensurate modulations have been observed experimentally with transmission election microscopy (TEM )in many perovskite ferroelectric ceramics,such as PbZrO 3,1Pb ͑Zr 1−x Ti x ͒O 3,2,3Sn-modified Pb ͑Zr 1−x Ti x ͒O 3(PZST ),4–7La-modified Pb ͑Zr 1−x Ti x ͒O 3(PLZT ),8–10Pb ͑Co 1/2W 1/2͒O 3,11,12and Pb ͑Sc 1/2Ta 1/2͒O 3.12,13They are characterized by the satellite reflections in electron diffrac-tion patterns and the regular fringes in image contrast.The modulation wave vector represented by the satellites is along the normal direction of those fringes,and the distance of the satellites to the fundamental reflections in reciprocal space corresponds to the spacing of the fringes in real space.The wave vector is parallel to the ͗110͘direction in most cases and the wavelength lies in the range of 5ϳ20a ,where a is the lattice parameter for the parent paraelectric structure.8Transformation of the intermediate incommensurate phase to other phases can be triggered by external stimuli,such as chemical composition and temperature.6–10Sn-or Ti-content in the PZST system and La content in the PLZT system were utilized before as controlling variables for the phase transformation.8–10In the PZST system,it has been shown that decrease in Sn content or increase in Ti content leads to the incommensurate antiferroelectric-to-ferroelectric phase transformation.In the PLZT system,the modulation wavelength was observed to increase with Ti molar fraction.8Utilizing temperature as the controlled variable in the study of such transformations allows in situ TEM studies,where the evolution of the satellite reflections can be directly observed.6,7The hot-stage in situ TEM observations revealed that the modulation wavelength increases continuously with increasing temperature.Based on these studies,Viehland et al.8suggested that the competing ferroelectric and antiferro-electric ordering in these perovskites are responsible for the presence of incommensurate modulations.However,unam-biguous evidence has yet to be found.In this letter,we report the study of the incommensurate phase transformation trig-gered by controlled electric fields.The evolution of the sat-ellite spots driven by external electrical stimuli is recorded.A hybrid coprecipitation method similar to that used by Yang and Payne 14was followed to prepare the ceramic powder with a chemical formula Pb 0.99Nb 0.02͓͑Zr 0.55Sn 0.45͒0.94Ti 0.06͔0.98O 3(abbreviated as PZST 45/6/2).Pressed cylinders,15mm in diameter by 20mm thick,were formed by cold-isostatic pressing at 350MPa.The preformed pellets were then hot pressed in an Al 2O 3die at 1150°C for 2h in air.Thin slices from the hot-pressed piece were annealed at 1300°C for 2h in an atmosphere containing excess PbO.The annealed slices were then ground,polished,and electroded.Dielectric character-ization was performed with an LCR meter (HP-4284A,Hewlett-Packard )at frequency of 1kHz in conjunction with an environmental chamber.A heating rate of 3°C/min was used during measurement.Electric field-induced polariza-tions were recorded with a standardized ferroelectric test sys-tem (RT-66A,Radiant technologies ).TEM specimens were prepared from ultrasonically cut 3-mm-diam disks.The thickness of these disks was reduced to ϳ150m by grinding and polishing.The center portion was further thinned to ϳ10m by dimpling.The dimpled specimens were then annealed at 300°C for 30min to mini-mize residual stresses.An argon ion mill was used for further thinning until final perforation occurred in the center.Gold electrodes with spacing of 250µm were evaporated to the TEM specimens,and platinum wires were used to connect the electrodes to the electrical contacts on the TEM specimen holder.Figure 1shows the schematic diagram of the TEM specimen configuration.Details of the electric field in situ TEM technique can be found elsewhere.15–18TEM studies were carried out on a Phillips CM-30microscope operating at 300kV .Temperature dependence of the dielectric permittivity of PZST 45/6/2is shown in Fig.2.The dielectric constant peaks with a value of 920at the temperature of 167°C.Electric field-induced polarization measurement showed double hysteresis loops (Fig.3),indicating an electric field-induced antiferroelectric-to-ferroelectric phase transforma-tion at room temperature.These results are consistent with previous observations from other researchers.5–7In order to determine the field level needed for the in situa )Electronic mail:xtan@APPLIED PHYSICS LETTERS VOLUME 85,NUMBER 1511OCTOBER 20040003-6951/2004/85(15)/3187/3/$22.00©2004American Institute of Physics3187TEM study and to assess the sample geometry effect on the field-induced antiferroelectric-to-ferroelectric phase transfor-mation,a dimpled and annealed 3-mm-diam disk specimen was tested for the hysteresis measurement and the result is also plotted in pared to the conventional circular plate sample with electric field applied along the thickness direction,the TEM-specimen-like disk shows a more gradual phase transformation with much broader loops.Furthermore,the backward switch from the induced ferroelectric phase to the antiferroelectric phase is sluggish,and a nonzero remnant polarization is detected.In situ TEM studies were carried out on a disk specimen with a central perforation.Actual electric field in the speci-men is disturbed (intensified in some areas while diluted in others )by the presence of the perforation.Electron transpar-ent areas that are subjected to intensified electric fields in the specimen were located in the TEM and one grain within this area was focused for the successive detailed in situ study.For an ideal circular perforation,the intensification ratio is 2.19The local electric field strength in this grain was thus esti-mated by doubling the nominal field strength.The evolution of the satellite spots in a ͗112͘-zone axis selected area diffraction pattern under static electric fields is shown in Fig.4.Initially,this grain displays one set of in-commensurate modulations.In the electron diffraction pat-tern,one set of the ͑1/x ͕͒110͖satellite spots is evident,as shown in Fig.4(a ).No detectable changes to these satellite spots were observed with applied static electric field up to 40kV/cm.At the field level of 48kV/cm,these satellites become weaker in their intensity [Fig.4(b )].This field level lies in the close vicinity of the E F (the critical field to trigger the antiferroelectric-to-ferroelectric transformation )mea-sured from the bulk sample.However,careful measurement indicates that the modulation wavelength does not change with increasing field strength.When the field strength reached 56kV/cm,most satellite spots disappeared.As shown in Fig.4(c ),only very weak satellites can be barely seen surrounding the three strong fundamental reflections in the left of this micrograph.The field strength was then re-duced to 40kV/cm.The satellites reappeared,with the strongest ones sitting in the upper-left corner of Fig.4(d ).When the field level was raised again to 56kV/cm [Fig.4(e )],all the satellite spots completely disappeared,indicat-ing the complete transformation to the ferroelectric phase.After the electric field was completely removed,no satellite spots were observed to reappear,as shown in Fig.4(f ).The observation confirms the sluggish nature of the backward ferroelectric-to-antiferroelectric transformation that has been noticed by other researchers in a similar composition.20It has been suggested that in PZT-based ferroelectric per-ovskites,the presence of incommensurate modulations in the antiferroelectric phase is a result of the competition between the ferroelectric and antiferroelectric ordering.8The continu-ous increase in the modulation wavelength with increasing temperature is interpreted that there exists a ferroelectric phase within a narrow temperature range just below the paraelectric transition temperature.When temperature is raised close to this temperature range the ferroelectric order-ing is enhanced.The modulation wavelength is thus in-creased.However,our observations on the electric field-induced transformation of the incommensurate modulation show a different scenario.The intensity of the satellite reflec-tions,rather than the modulation wavelength,changes with the applied electric field strength.The wavelength stays con-stant at a value of 2.3nm.Since external electric field is known to enhance the ferroelectric ordering,we suggest that the electric field-induced antiferroelectric (incommensurate )-to-ferroelectric transformation proceeds as following.When the applied electric field reaches E F ,the phase transformation is initiated in some areas of the grain.The transformation is an abrupt one and no intermediate changes in the modulation wavelength takes place.With increasing electric field strength,the fraction of the transformed area increases and the intensity of the satellite diffraction peaks getsweaker.FIG.2.Temperature dependence of dielectric constant at 1kHz in the PZST 45/6/2ceramic.FIG.3.Electric field-induced polarization measurement at 4Hz in a bulk circular plate sample and an unperforated TEMspecimen.FIG.1.Schematic diagram of specimens for the electric field in situ TEM study.Obviously,a mechanism involving the nucleation of ferro-electric phase and the motion of the phase boundary controls the transformation process.Further studies will be focused on these issues.In addition to the ͑1/x ͕͒110͖satellite spots,12͕111͖-type superlattice reflections were also present in the ͗112͘-axis diffraction pattern,as labeled in Fig.4(e ).The structural ori-gin for these superlattice reflections is still under debate.2,5–7,9,21However,the present in situ TEM study pro-vides valuable insight into the physics mechanism for the presence of these superlattice reflections.It is clear in Fig.4that the intensity of the 12͕111͖spots does not change with the applied electric field,implying a mechanism that is quite rigid to external disturbance.This seems to favor the oxygen octohedra tilting model.21To summarize,in situ TEM technique was applied to the study of the electric field-induced antiferroelectric-to-ferroelectric phase transformation in a PZT-based ceramic.Upon application of external electric fields,the wavelength of the incommensurate modulation in the antiferroelectric phase showed no change but the intensity of the satellite reflections decreased when the field exceeds a critical value.This critical strength matches closely to the E F measured in the bulk sample.This work was supported by the Process Science Initia-tive (PSI )program at Ames Laboratory,U.S.DOE (GrantNo.10-501-115612).The authors are grateful to Dr.David Cann for the access to the dielectric characterization instru-ment in his group at Iowa State University.1Z.Xu,X.Dai,D.Viehland,and D.A.Payne,J.Am.Ceram.Soc.78,2220(1995).2J.Ricote,D.L.Corker,R.W.Whatmore,S.A.Impey,A.M.Glazer,J.Dec,and K.Roleder,J.Phys.:Condens.Matter 10,1767(1998).3S.Watanabe and Y .Koyama,Phys.Rev.B 66,134102(2002).4J.S.Speck,M.De Graef,A.P.Wilkinson,A.K.Cheetham,and D.R.Clarke,J.Appl.Phys.73,7261(1993).5D.Viehland,D.Forst,Z.Xu,and J.Li,J.Am.Ceram.Soc.78,2101(1995).6Z.Xu,D.Viehland,P.Yang,and D.A.Payne,J.Appl.Phys.74,3406(1993).7Z.Xu,D.Viehland,and D.A.Payne,J.Mater.Res.10,453(1995).8D.Viehland,X.Dai,J.Li,and Z.Xu,J.Appl.Phys.84,458(1998).9J.Knudsen,D.I.Woodward,and I.Reaney,J.Mater.Res.18,262(2003).10Z.Xu,X.Dai,and D.Viehland,Phys.Rev.B 51,6261(1995).11S.Watanabe and Y .Koyama,Phys.Rev.B 65,064108(2002).12C.A.Randall,S.A.Markgraf,A.S.Bhalla,and K.Baba-Kishi,Phys.Rev.B 40,413(1989).13K.Z.Baba-Kishi and D.J.Barber,J.Appl.Crystallogr.23,43(1990).14P.Yang and D.A.Payne,J.Appl.Phys.71,1361(1992).15Z.Xu,X.Tan,P.Han,and J.K.Shang,Appl.Phys.Lett.76,3732(2000).16X.Tan,Z.Xu,J.K.Shang,and P.Han,Appl.Phys.Lett.77,1529(2000).17X.Tan,Z.Xu,and J.K.Shang,Mater.Sci.Eng.,A 314,157(2001).18X.Tan,and J.K.Shang,Philos.Mag.A 82,1463(2002).19R.M.McMeeking,ZAMP 40,615(1989).20W.Chan,H.Chen,and E.V .Colla,Appl.Phys.Lett.82,2314(2003).21D.Viehland,Z.Xu,and D.A.Payne,J.Appl.Phys.74,7454(1993).FIG.4.Evolution of the ͗112͘selected area diffraction pattern under applied electric fields in PZST 45/6/2.(a )Original state,(b )48,(c )56,(d )40,and (e )56kV/cm,and (f )field removed.。
我们来深入地探讨一下十氢化镧(LaH10)的晶体结构。
十氢化镧是一种重要的储氢材料,具有很高的理论氢存储容量。
在储氢材料领域,对其晶体结构的深入研究对于理解其储氢机理和性能具有重要意义。
在本文中,我们将对十氢化镧的fm-3m相的晶体结构进行全面的评估和探讨。
1. 晶体结构概述十氢化镧的fm-3m相晶体结构属于立方晶系,属于fcc结构类型。
在这种结构中,氢原子占据着八面体间隙位置,并与镧原子形成特定的化学键和相互作用。
这种晶体结构的稳定性对于十氢化镧的氢储存性能具有重要影响。
2. 晶格参数和原子位置根据实验和理论研究,十氢化镧的fm-3m相晶体结构的晶格参数和原子位置已经被确定。
其中,镧原子和氢原子的位置关系及其对晶体结构的影响是十分重要的。
理解晶格参数和原子位置对于设计和改进氢储存材料具有重要意义。
3. 晶体结构稳定性了解十氢化镧的fm-3m相晶体结构的稳定性对于预测其在不同条件下的性能至关重要。
通过理论模拟和实验验证,可以评估晶体结构在不同温度、压力下的稳定性,从而为材料设计和合成提供重要参考。
回顾本文所探讨的内容,我们对十氢化镧的fm-3m相晶体结构进行了全面的评估和探讨。
通过深入了解晶体结构的概况、晶格参数和原子位置以及晶体结构的稳定性,我们可以更好地理解这一重要储氢材料的性能及其在氢能领域的应用前景。
个人观点和理解:在我看来,十氢化镧作为一种重要的储氢材料,其晶体结构的深入理解对于进一步提高其氢存储性能至关重要。
通过对其晶格参数、原子位置和稳定性的研究,可以为其在氢能领域的应用和发展提供重要支持。
未来,我期待能够看到更多关于十氢化镧及其他储氢材料晶体结构的深入研究,以推动氢能技术的发展和应用。
以上是对十氢化镧(fm-3m相)晶体结构的全面评估和探讨,希望能够对您有所帮助。
十氢化镧(LaH10)是一种重要的储氢材料,具有很高的理论氢存储容量,因此对其晶体结构进行深入研究具有非常重要的意义。
PHI AES对科学研究的重要作用关键词:AES、表面分析、纳米尺度、元素鉴定、元素mapping学术期刊是研究人员共享科技成果、加深对科学问题的理解和学习交流的基石。
高质量文章的发表,既离不开让人耳目一新的新思路、新观点,更不乏有效的、可靠的表征技术的支撑。
例如,PHI公司(Physical Electronics)中的俄歇电子能谱(AES)在推动2022年科技的大力发展上功不可没。
回顾2022年,PHI AES仪器帮助相关学者发表了800余篇学术出版物,包括同行评审的文章和书籍,其中不少论文发表在影响力很高的顶级期刊上。
PHI AES设备被应用于诸多高新技术领域,例如高温防腐涂层1、无碳钢2、结构钢3-4、月球地质学5、区域选择性ALD6、环境修复7和燃料电池8等。
例如,KTH皇家理工学院和Sandvik Materials Technology的研究人员借助PHI AES来研究质子交换膜燃料电池(PEMFC)的工作机制,为电动汽车的发展提供了一个有前途的选择,从而有望推动内燃机的替代。
研究表明,对PEM燃料电池中的双极板(BPPs)进行改进,可以在降低成本的同时提高功率密度。
该项工作发表于国际知名期刊《Energy Conversion and Management》8。
PEMFC由许多堆叠膜电极组件(MEA)构成,组件之间通过BPPs分隔氧化剂和还原剂,并传导电流和排出所产生的水,因而BPPs的稳定性对燃料电池的性能影响甚大。
一方面,在研究BPPs的过程中,发现其表面上存在碳-金属氧化物(MOxCy (M = Cr, Fe, Ni)“污渍”。
这种污渍是在激光切割BPPs时产生:激光切割带碳涂层的不锈钢(C-coated 316L)会产生喷射物质并溅在碳涂层上,形成的碳-金属氧化物(被定义为“污渍”,碳来源于碳涂层)直接连接到不锈钢基底上,并且污渍周围的碳涂层上也会覆盖一层与之组分类似的薄膜(见图1)。
超低温高比能全液相锂硫电池多级结构硫正极的构筑及其过渡态演化机制研究To address your question about the construction of hierarchical sulfur cathodes with high energy density for all-liquid lithium-sulfur (Li-S) batteries and the investigation of their transitional state evolution mechanisms at ultra-low temperatures, comprehensive research has been conducted.All-liquid Li-S batteries are regarded as promising candidates for next-generation energy storage devices due to their high theoretical specific capacity, low cost, and environmental friendliness. However, challenges remain in achieving long cycle life and stable performance at low temperatures. To overcome these issues, efforts have been made to design hierarchical sulfur cathodes with enhanced electrochemical activity and stability.Hierarchical structures can be formed by introducing carbon materials or metal oxides/nitrides as functional additives into the sulfur matrix. These additives not only providephysical support but also serve as conductive pathways and catalytic sites for electrochemical reaction kinetics improvement. By constructing multi-layered architectures or integrating nanosized materials within the sulfur cathodes, a large amount of active sites can be exposed to enhancethe diffusion of polysulfide intermediates and mitigate the shuttle effect during charge-discharge processes.Additionally, research on transition state evolution mechanisms is crucial for understanding the degradation process of all-liquid Li-S batteries under ultra-low temperature conditions. Transition state analysis provides insights into intermediate species formation,transformation pathways, and rate-determining steps during battery operation. Various characterization techniques such as in situ X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) have been employed to monitor morphological changes and chemical reactions occurring at different stages of discharge/charge cycles.Furthermore, computational simulations based on densityfunctional theory (DFT) have aided in unraveling the mechanisms governing transition states in all-liquid Li-S batteries. By calculating activation barriers for different reaction steps and analyzing electronic structures of intermediates, researchers are able to propose strategiesfor improving battery performance at ultra-low temperatures.Overall, through the construction of hierarchical sulfur cathodes and investigation of transition state evolution mechanisms, significant progress has been made in understanding and addressing the challenges associated with all-liquid Li-S batteries at ultra-low temperatures. These findings contribute to the development of high-performance energy storage systems that can meet the demands of future applications.对于你提出的关于构建具有高能量密度的多级结构硫正极以应用于全液相锂硫电池,并研究其在超低温高比能工况下的过渡态演化机制的问题,已经进行了全面的研究。
APPLICATIONAZ MIF developers are high contrast, ultra-high purity tetramethyl-ammonium hydroxide (TMAH) based photoresist developers formulated for a wide range of advanced IC and thick photoresist applications. •Surfactant enhanced and surfactant free options •Industry leading normality control •Wide range of normality available•High purity, low particulate formulations•Multiple bulk and non-bulk packaging optionsPROCESSINGGENERAL PROCESSING GUIDELINESAZ MIF developers should be used at room temperature in puddle, spray, or batch immersion processing mode. Variations in develop time, developer temperature, and substrate temperature will result in inconsistent develop uniformity and will affect process repeatability/reproducibility. It is important to monitor and control these variables.When processed in batch immersion mode, MIF developer bath life will be limited by the volume of dissolved photoresist in solution and by carbonate uptake from the fab environment. 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纳米硒的生物医学作用研究进展曹晖;刘红梅【摘要】硒是人体必需微量营养元素,在生命体中有延缓衰老、清除自由基、保护心血管、抗癌等诸多功效.但是,由于传统补硒剂的安全剂量和毒性剂量范围过于接近,导致硒在保健食品和医药品中的应用受到了限制.纳米硒是近些年来发展的一种新颖的硒形态,综述了纳米硒对生物体的毒性、生物医学作用(如抗氧化、抗癌、抗菌)、用作膳食营养补充剂的潜能等方面的研究进展,并对未来的研究进行了展望,以期为纳米硒的生物医学应用和保障人类的健康提供参考.【期刊名称】《生物技术进展》【年(卷),期】2017(007)005【总页数】8页(P518-525)【关键词】硒;纳米硒;抗氧化;抗癌;毒性【作者】曹晖;刘红梅【作者单位】华中科技大学化学与化工学院,武汉430074;华中科技大学化学与化工学院,武汉430074【正文语种】中文硒是人体必需的一种微量营养元素,对人体健康至关重要。
缺硒可导致心血管疾病、癌症、大骨节病、病毒感染性疾病等的发病率显著升高,而补硒则有助于预防这些疾病[1~4]。
一般认为硒主要通过硒蛋白发挥生物学功能。
在硒蛋白中,硒以硒代半胱氨酸(Sec)—第21种天然氨基酸的形式存在。
目前已知人体内有25种硒蛋白,它们在抗氧化防御、细胞信号转导、甲状腺激素水平调节、免疫调节等生命过程中发挥着重要作用[5]。
其中,抗氧化、清除自由基是硒最重要的生物学功能。
例如,硒酶-谷胱甘肽过氧化物酶(GPx)是机体抗氧化防御系统中重要的成员,它们可以催化体内有毒的H2O2和脂质过氧化物(ROOH)变为无毒的水和醇,从而保护蛋白质、DNA和脂类免受氧化损伤。
传统的食物来源或营养补充的硒化合物包括无机硒(常见的有亚硒酸钠、硒酸钠)和有机硒(常见的有硒代蛋氨酸、硒代半胱氨酸)。
但是,硒在生物体内的安全剂量范围非常狭窄,很容易因过量而产生毒性,这限制了传统硒化合物在临床疾病防治方面的广泛应用[1,2,4]。
收稿日期:2020⁃09⁃29。
收修改稿日期:2020⁃12⁃28。
国家自然科学基金(No.21875037,51502036)和国家重点研发计划(No.2016YFB0302303,2019YFC1908203)资助。
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E⁃mail :***************.cn ,***************第37卷第3期2021年3月Vol.37No.3509⁃515无机化学学报CHINESE JOURNAL OF INORGANIC CHEMISTRYp 区金属氧化物Ga 2O 3和Sb 2O 3光催化降解盐酸四环素性能差异毛婧芸1黄毅玮2黄祝泉1刘欣萍1薛珲*,1肖荔人*,3(1福建师范大学环境科学与工程学院,福州350007)(2福建师范大学生命科学学院,福州350007)(3福建师范大学化学与材料学院,福州350007)摘要:对沉淀法合成的p 区金属氧化物Ga 2O 3和Sb 2O 3紫外光光催化降解盐酸四环素的性能进行了研究,讨论了制备条件对光催化性能的影响。
最佳制备条件下得到的Ga 2O 3⁃900和Sb 2O 3⁃500样品光催化性能存在巨大差异,通过X 射线粉末衍射、傅里叶红外光谱、N 2吸附-脱附测试、荧光光谱、拉曼光谱、电化学分析及活性物种捕获实验等对样品进行分析,研究二者光催化降解盐酸四环素的机理,揭示影响光催化性能差异的本质因素。
结果表明,Ga 2O 3和Sb 2O 3光催化性能差异主要归结于二者不同的电子和晶体结构、表面所含羟基数量及光催化降解机理。
关键词:p 区金属;氧化镓;氧化锑;光催化;盐酸四环素中图分类号:O643.36;O614.37+1;O614.53+1文献标识码:A文章编号:1001⁃4861(2021)03⁃0509⁃07DOI :10.11862/CJIC.2021.063Different Photocatalytic Performances for Tetracycline Hydrochloride Degradation of p ‑Block Metal Oxides Ga 2O 3and Sb 2O 3MAO Jing⁃Yun 1HUANG Yi⁃Wei 2HUANG Zhu⁃Quan 1LIU Xin⁃Ping 1XUE Hun *,1XIAO Li⁃Ren *,3(1College of Environmental Science and Engineering,Fujian Normal University,Fuzhou 350007,China )(2College of Life and Science,Fujian Normal University,Fuzhou 350007,China )(3College of Chemistry and Materials Science,Fujian Normal University,Fuzhou 350007,China )Abstract:The UV light photocatalytic performances of p ⁃block metal oxides Ga 2O 3and Sb 2O 3synthesized by a pre⁃cipitation method for the degradation of tetracycline hydrochloride were explored.The effects of synthesis conditions on the photocatalytic activity were discussed.The Ga 2O 3⁃900and Sb 2O 3⁃500samples prepared under optimal condi⁃tions exhibited a remarkable photocatalytic activity difference,which were characterized by X⁃ray diffraction,Fouri⁃er transform infrared spectroscopy,N 2adsorption⁃desorption tests,fluorescence spectrum,Raman spectrum,electro⁃chemical analysis and trapping experiment of active species.The photocatalytic degradation mechanisms of tetracy⁃cline hydrochloride over the photocatalysts were proposed and the essential factors influencing the difference of pho⁃tocatalytic performance were revealed.The results show that the different photocatalytic activities observed for Ga 2O 3and Sb 2O 3can be attributed to their different electronic and crystal structures,the amount of hydroxyl groupin the surface and the photocatalytic degradation mechanisms.Keywords:p ⁃block metal;Ga 2O 3;Sb 2O 3;photocatalysis;tetracycline hydrochloride无机化学学报第37卷0引言盐酸四环素(TC)作为一种四环素类广谱抗生素,被广泛应用于治疗人体疾病及预防畜禽、水产品的细菌性病害,其在世界范围的大量使用致使其在环境中积累[1]。
TEM characterization of super-hydrophilic Ni –Ti thin filmKotekar P.Mohanchandra a ,⁎,Youngjae Chun a ,Sergey V.Prikhodko b ,Gregory P.Carman aa Mechanical and Aerospace Engineering Department,University of California,Los Angeles,CA 90095,USA bMaterials Science and Engineering Department,University of California,Los Angeles,CA 90095,USAa b s t r a c ta r t i c l e i n f o Article history:Received 25August 2010Accepted 15January 2011Available online 25January 2011Keywords:TEMSputter deposition Bio-materialsSuper-hydrophilicA super-hydrophilic Ni –Ti thin film is evaluated using cross-sectional transmission electron microscopy (TEM).Following sputter deposition and annealing,the Ni –Ti thin films are chemically treated with buffered oxide etchant,nitric acid and 30%hydrogen peroxide solution to produce a 100-nm-thick surface oxide layer.The fabricated Ni –Ti thin films show a 10-to 15-nm TiO 2thick layer on its surface with a ~67°wetting angle.For the surface treated sample,a porous oxide 100nm TiO layer is found with a b 5°.It is believed that TiOOH (H 2O)n complex forms on the surface to produce the observed super-hydrophilic behavior.Published by Elsevier B.V.Bulk equiatomic nickel –titanium (Ni –Ti)alloy is used in many biomedical applications,such as endovascular stents,guide-wires and various prosthetic devices because of its biocompatibility [1–3].More recently,researchers have proposed using thin film Ni –Ti in vascular implants [4,5].The biocompatibility of both the bulk and thin film Ni –Ti is attributed to 10-to 15-nm-thick native titanium oxide which forms on the surface.Several researchers studied the composition and structure of the native oxides in both the bulk and thin film Ni –Ti [6–8].A large number of studies con firmed that the native oxide layer consists of TiO 2,while a few studies reveal the presence of both TiO and TiO 2in the surface oxide layer.To improve the biocompatibility,researchers have modi fied the surface oxide layer by electro-polishing,ultraviolet radiation exposure,thermal and chemical [9–12]treatment which provide thicker surface oxide layers and in many instances change the hydrophilic nature of the Ni –Ti surface.In general,hydrophilic surfaces are more desirable in some applications such as biomedical.Transmission electron microscopy (TEM)is a useful technique for evaluating crystallinity and morphology of multiphase structure.TEM studies typically focuses on a planar surface analysis,whereas information concerning thickness variation is absent due to sample preparation dif ficulties.Typically,only cross-sectional studies provide information regarding types,structures and thickness dimensions present through the thickness.Recently,Potapov et ed cross-sectional TEM to characterize native oxide layers on the surface of Ni –Ti tubing and reported the presence of a thin TiO 2film layer [13].In regards to thin film Ni –Ti materials there are relatively few TEM studies on native surface oxides of thin film Ni –Ti [14].Therefore,aneed exists to better understand the native oxide as well as those intentionally produced in thin film Ni –Ti materials.Furthermore,there is an absence of cross-sectional TEM studies on thin film Ni –Ti.The few TEM studies available on thin film Ni –Ti report the presence of TiO 2or a mixture of TiO 2and TiO with an absence of any reporting purely a TiO layer [15].Since different Ti oxides can signi ficantly affect hydrophilic response of Ni –Ti devices their controlled fabrication is a subject of practical importance.In this letter,we report results on cross-sectional TEM character-ization of morphology and crystallinity of thin Ni –Ti film surface after chemical treatment.The chemical treatment of thin film Ni –Ti was previously reported to produce a super-hydrophilic surface with zero wetting angle [16].However,an explanation for this phenomenon was not presented.TEM results indicate that the native oxides produced on Ni –Ti thin film has a 5-to 10-nm-thick rutile TiO 2layer,while the chemical treatment of the thin film Ni –Ti has a 100-nm-thick porous TiO layer.When compared to TiO 2,TiO is capable of forming a complex of TiOOH(H 2O)n which is postulated to lead to the observed super-hydrophilicity.Ni –Ti thin films in this study were produced by a DC sputtering technique coupled with a hot target method using a near equiatomic Ni –Ti alloy target under ultra-high vacuum atmosphere.A 5-μm-thick Ni –Ti film was deposited on a silicon (100)substrate with a 0.5-μm-thick thermal oxide layer.The films were annealed and crystallized on the wafer at 500°C for 1h in a vacuum better than 10−7Torr.More details of the film fabrication method are reported in earlier publications [17].Differential scanning calorimetric measurements were performed to determine phase transformation temperatures of the Ni –Ti films.Measured transformation temperatures were mar-tensite finish M f =−32°C,martensite start M s =−10°C,austenite start A s =12°C and austenite finish A f =36°C.All results reported in this manuscript are for Ni –Ti films in the fully austenite state.Materials Letters 65(2011)1184–1187⁎Corresponding author.Tel.:+13108509014;fax:+13102062302.E-mail address:kpmohan@ (K.P.Mohanchandra).0167-577X/$–see front matter.Published by Elsevier B.V.doi:10.1016/j.matlet.2011.01.037Contents lists available at ScienceDirectMaterials Lettersj o u r na l ho m e p a g e :w w w.e l s ev i e r.c o m /l o c a t e /m a t l e tFollowing sputter deposition and annealing,the Ni –Ti thin films were chemically treated as follows.First,the samples were immersed in buffered oxide etchant (BOE:aqueous NH 4-HF etchant)for 10min to remove the native oxide layer on the film surface.The films were subsequently treated by nitric acid (HNO 3)for 40min to remove excess nickel.Finally,the films were immersed in 30%hydrogen peroxide (H 2O 2)solution for 14h.During the H 2O 2process it was observed that gas evolved and the film surface color changed slowly to a slight yellowish tinge.This chemical treatment process produces a super-hydrophilic surface as described by Chun et al .[16].In this study,hydrophilicity of the samples was determined by measuring the wetting angles produced by water droplet on the film surface.Fig.1shows the wetting angle measurements in either annealed or chemically treated Ni –Ti thin films.The wetting angle for the annealed sample is 67°while for the chemically treated sample it is less than 5°.It has been previously reported that increases in hydrophilicity due to various surface treatments in Ni –Ti are attributed to the attachment of hydroxyl group (―OH)to the surface oxide layer [18].However,little information is available concerning the structure of the surface oxide layer and thus understanding the surface oxide characteristic is a critical concern.Cross-sectional TEM samples are prepared from four different Ni –Ti thin films:1)as annealed Ni –Ti thin film (sample UT),2)after BOE (sample T1),3)after HNO 3(sample T2)and,4)after H 2O 2(sample T3)treatments.Samples were prepared by “lift-out ”method [13,19]using Nova 600dual-beam system (FEI).To protect the samples surface layers from the high energy focused Ga ion beam,a 0.1-μm-thick Pt was deposited on the Ni –Ti thin film by electron beam deposition followed by a 0.9-μm-thick Pt deposited using ion beam.Ion milling produces a thin cross-sectional sample of size 10μm (length)×2μm (width)×7μm (depth)consisting of Ni –Ti/Oxide/Pt.After final milling,the sample is lifted out with a needle-like probe and is subsequently attached to a TEM grid.The sample on the TEM grid is further thinned down from 2μm width to electron transpar-ency,less than 70nm,using a low ion beam current of 30pA.The entire sample preparation procedure was monitored using the secondary electron imaging mode inside Nova 600.Prepared samples were examined using scanning/transmission electron microscope(S/TEM)Titan (FEI)operating at accelerating voltage 300keV coupled with energy dispersive spectrometer (EDS)used for the elemental analysis.The TEM micrographs of the four samples i.e.,annealed (UT)and three chemically treated Ni –Ti thin films (T1,T2and T3),are shown in Fig.2a –d.The Pt surface protection layer is present in all the foursamples and visible on the right side of each image.Selective area electron diffraction (SAED)of the Si substrate was used to orient each sample in the TEM uniformly with the sample surface perpendicular to [100]zone axis.Fig.2a –c is procured at the same magni fication while Fig.2d is at a slightly lower magni fication.Fig.2a shows the high resolution TEM (HRTEM)image of the surface oxide region of the UT sample.Beneath the Pt layer a 10-to 15-nm-thick polycrystalline native oxide layer is observed.The inset in Fig.2a shows the SAED ring pattern obtained from a 50nm diameter circular region containing the native oxide region,the Ni –Ti region,and the Pt coating.The indexed SAED pattern identi fied the oxide layer as rutile TiO 2#1-1292(JCPDS),tetragonal P42/mnm with a =4.58A,b =4.58and C =2.95A.The SAED ring pattern shows fundamental re flections from the {101},{111},{200},{211}and {002}planes in the TiO 2.The SAED pattern also shows fundamental re flections {200}and {220}of Pt and the {100}of parent Ni –Ti.SAED obtained from the parent Ni –Ti grain (not shown here)reveals a B2type structure.The parent Ni –Ti phase observed in all four sample studied (Fig.2a –d)in this paper is identical and is not discussed further.Fig.2b –d represents TEM images of the samples taken after each of the three steps in the surface treatment to produce a super-hydrophilic layer.Fig.2b shows sample T1(following BOE etch to remove the 10-to 15-nm TiO 2)has a 10-nm-thick region directly adjacent to the Pt layer.This region was void of any spots or rings in the SAED indicating an amorphous structure.Based on STEM/EDS results the region closest to the Pt in Fig.2b contains relatively larger amount of Ni compared to the parent phase i.e.the Ni to Ti ratio (at %)changes from 1.22at the top surface (just below Pt)to 1.09at approximately 80nm from the top surface.We attribute this to the native oxide that formed following removal of the TiO 2layer reducing the Ti content.Fig.2c shows a TEM micrograph of sample T2(following HNO 3etch to remove Ni)with three distinct thin layers next to the Pt region.Since the sample T2was exposed to atmosphere following etching,a 2-nm-thick oxide layer forms on the sample.Beneath the oxide layer,one can observe two additional thin layers identi fied by different contrast.The lighter contrast indicates Ti rich region while the darker contrast indicates Ni rich region.Fig.2d shows sample T3(following H 2O 2to grow an oxide layer)has a 100-nm-thick layer next to the Pt region.This region is substantially larger than the surface regions observed in any of the previous TEM micrographs (Fig.2a –c).A closer examination of the region in Fig.2d reveals the presence of TiO as explained below.Fig.3a is a SEM micrograph of the sample T3showing a 100-nm-thick porous layer beneath the Pt layers.Chu et al .[20]attributed submicron pores in bulk Ni –Ti alloy to chemical polish prior to H 2O 2treatment.In contrast,our study shows the submicron pores in the oxide layer formed after H 2O 2treatment on the Ni –Ti thin film i.e.,not due to chemical polishing.HRTEM image of the surface oxide for sample T3is shown in Fig.3b.The image shows fine grains with sizes varying from 2to 5nm.The d-spacing is measured using a Digital-Micrograph software in conjunction with Fast Fourier Transform (FFT)dot patterns acquired at the individual grains along with the FFT ring pattern (inset of Fig.3b)acquired in a 20nm×20nm area.The d-spacing values measured corresponds to JCPDS data (#2-1196)for cubic TiO (space group:Fm3m,a =0.4235nm)as shown in Table 1.In addition,the SAED ring pattern shown in the inset of Fig.3b of this region also shows several diffraction rings.These diffraction rings also correspond to fundamental re flections from {200},{220},{222}and {311}of cubic TiO.The TEM results show that the chemically treated Ni –Ti thin films have a cubic TiO layer on its surface whereas the as annealed Ni –Ti thin films have rutile TiO 2layer.The 0.3026nm spacing between the Ti atoms in the cubic TiO is nearly equal to the lattice spacing of Ni –Ti in the B2phase i.e.,0.3010nm.In contrast the 0.546nm spacing between nearest Ti atoms in rutile TiO 2is much larger than the lattice parameter of the B2phase.Therefore,we believe that the growth of cubic TiO(100)Fig. 1.Wetting angle measurements (a)before treatment,θ~67°,and (b)after treatment,θb 5.1185K.P.Mohanchandra et al./Materials Letters 65(2011)1184–1187lattice parallel to the (100)lattice of B2is energetically more favorable at low temperature due to lattice matching [13].While this is postulated,we were unable to con firm epitaxial growth of TiO on Ni –Ti using HRTEM even though we were able to con firm the presence of TiO.In our study we used H 2O 2as an oxidizing agent to form a TiO layer on the Ni –Ti thin films.The oxidization reaction proceeds by decomposition of H 2O 2into water and oxygen in the presence of Ti on the Ni –Ti thin film surface.The gas that was observed duringtheFig.2.TEM micrographs of (a)UT,(b)T1,(c)T2,and (d)T3samples.Fig.3.(a)SEM micrograph of sample T3.(b)HRTEM micrograph at the porous region.1186K.P.Mohanchandra et al./Materials Letters 65(2011)1184–1187immersion of Ni–Ti thinfilm into the H2O2solution suggests the oxygen production.The oxygen reacting with Ti produces TiO as confirmed with TEM results.It is well established that H2O2reacts with Ti and also forms hydroxyl radicals(OH.).Highly reactive and short lived hydroxyl radicals further decompose the H2O2and produce more oxygen and water.This in turn produces a yellow colored TiOOH(H2O)n(i.e.as observed)complex as an end product and has been suggested previously for H2O2interaction with H2O2 [21].We believe that the yellow colored surface is a TiOOH(H2O)n complex on the Ni–Ti thinfilm surface and that this complex produces a surface exhibiting super-hydrophilic behavior.AcknowledgmentThis work is supported by the National Institutes of Health under award number1RC1HL099445-01.The authors have no conflicts of interest to disclose.References[1]Stoeckel D.Min Invas Ther Allied Technol2000;9:81–8.[2]Gil FJ,Planell JA.Proceedings of the Institution of Mechanical Engineers,Part H.JEng Med1998;212:473–88.[3]Danilov A,Tuukkanen T,Tuukkanen J,JämsäT.J Biomed Mater Res A2007;82:810–919.[4]Barras CDJ,Myers KA.Eur J Vasc Endovasc Surg2000;19:564–9.[5]Shabalovskaya SA.Biomed Mater Eng2002;12:60–109.[6]Michiardi A,Aparicio C,Planell JA,Gil FJ.J Biomed Mater Res Part B2006;77B:249–56.[7]Miyauchi M,Kieda N,Hishita S,Mitsuhashi T,Nakajima A,Watanabe T,et al.SurfSci2002;511:401–7.[8]Maitz FM,Pham M,Wieser E,Tsyganov I.J Biomater Appl2003;17:303–18.[9]Wu W,Liu X,Han H,Yang D,Lu S.J Mater Sci 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H.Biomaterials1989;10:166–75.Table1d-spacing and(h k l)indices from both FFT and SAED patterns.d-spacing,nm (FFT)d-spacing,nm(JCPDS:#2-1196)(h k l)from FFT(dot pattern)(h k l)from FFTring pattern(h k l)from SAEDpattern0.245±0.0030.245(111)0.212±0.0020.212(200)(200)(200) 0.150±0.0040.150(220)(220)(220) 0.128±0.0020.128(311)(311) 0.122±0.0030.122(222)(222)1187K.P.Mohanchandra et al./Materials Letters65(2011)1184–1187。