Dynamic analysis of preferential orientation of arasonite crystals in nacre from mollusk shell

Based on the scanning electron microscope （SEM） observations, it is confirmed that the nacre is composed of aragonite crystals and organic matrix with interlaced arrangement, showing ordered ＂brick-mortar＂ structure. The dynamic analysis of preferential orientation of aragonite crystals in the nacre from the abalone （Haliotis diverscolor supertexta） with different shell ages is systematically investigated using X-ray diffraction （XRD） and high resolution transmission electron microscope （HRTEM）. Experiments reveal that, in the nacre from the juvenile mollusk shell, there exist three kinds of orientations of aragonite crystals： （113）, （002） and （012）. However, along with the growing of the mollusk shell, the intensity of （012） and （113） becomes weak, and the （002） becomes the preferred crystal orientation of aragonite in the nacre from the adult mollusk shell, which means that the c axis of aragonite crystals is perpendicular to the nacreous layers. The results obtained show that the nacre possesses a highly ordered structure at the micrometer/nanometer mulUscale levels.     

贝壳中文石晶体择优取向的XRD分析

贝壳珍珠层独特的结构是其优异力学性能的重要原因.采用X射线衍射法(XRD)对贝壳珍珠层及柱状晶的晶体结构及择优取向进行了详细的探讨.结果表明:珍珠层中文石晶体在沿珍珠层面上存在两种定向排列,即(002)和(012),具有择优取向性,柱状晶层结构的无序性比珍珠层大.     

The relationship between nacreous layer color and CaCO3 crystal orientation

The pearl or nacreous layer of mollusk shell is composed of CaCO₃ aragonite crystals. The factors affecting their color are very complex, such as metal elements, chromoprotein, and nucleation materials, we analyzed the crystal orientation of nacreous layers with different color prepared from fresh water clamsHyriopsis cumingii Lea by X-ray diffraction. The results show that the crystal CaCO₃ orientation on specific plane is responsible for the color of pearl and nacreous pearl color. Supported by National Natural Science Foundation of China and Morning Sunlight Program of Wuhan City Government. Jiang Xinnong: born in 1970, Lecturer     

贝壳韧带微结构的高分辨扫描电镜研究

采用高分辨SEM及XRD对合浦珠母贝韧带进行了研究,结果表明,合浦珠母贝韧带无机相主要由文石组成.韧带具有明显的层状结构,同一生长层及相隔生长层中文石纤维呈一致定向排列,而相邻生长层文石纤维的定向明显不同,呈“交叉棱柱层”结构样式.合浦珠母贝韧带中文石纤维的直径为80~90 nm,具有典型的2D光子晶体结构特征.     

贝壳珍珠层动态的文石板片厚度及其新结构模型

利用扫描电镜对大珠母贝、合浦珠母贝及三角帆蚌壳中区珍珠层自然断面微结构进行了系统的研究,首次发现贝壳珍珠层纵向文石板片厚度在不同部位具有明显的差异,大珠母贝、合浦珠母贝及三角帆蚌珍珠层从内层面到外层面文石板片最大厚度差分别达到462、246、26nm;并根据SEM观察结果初步建立了一种新的连续可变厚度型珍珠层结构模型,这对生物矿物学、物理光学及仿生材料学方面的相关研究具有重要指导意义.     

珍珠母堆垛微结构的力学性能和热稳定性

一直以来,软体动物贝壳内的珍珠母因为其由文石片和片间有机基质薄层堆垛而成的微结构及其卓越的力学行为而广受关注,但对贝壳珍珠母的多级结构,尤其是其中的两级有机基质结构的力学功能研究甚少.本文通过机械载荷和温度载荷组合来研究皱纹盘鲍（Haliotis Discus Hannai）贝壳内的珍珠母的结构和力学特性关联.发现文石片层间的有机基质的热解有效降低了珍珠母堆垛微结构的强度和韧性,并在250℃时使珍珠母的层叠堆垛结构完全崩溃,此时有机基质的热解量约为1.7wt%,仅为有机基质总量的40%.而力学性能试验比较发现,珍珠母堆垛微结构的热稳定远低于其基本组成单元——文石片纳米复合结构.另外,尽管有机基质薄层的黏着作用对珍珠母的力学性能具有积极意义,但珍珠母微结构本身的逐层交错堆垛设计机制是影响其刚度的决定性因素.     

Extraction and Purification of Matrix Protein from the Nacre of Pearl Oyster Pinctada fucata

A soluble matrix protein P14 with an apparent molecular mass of 14.5 kDa was isolated from fragmented nacre of pearl oysters （Pinctada fucata） treated with 10% NaOH solution to investigate the nacre matrix proteins and their effect on the CaCO3 crystal. The protein was characterized by gel exclusion chromatography and reversed-phase high performance liquid chromatography after demineralization by 10% acetic acid. The X-ray diffraction pattern of P14 crystals indicates that P14 plays an important role in nacre biomineralization. P14 can induce aragonite formation, stimulate CaCO3 crystal formation, and accelerate aragonite precipitation. Heating of the acid insoluble nacre residue, which was named conchiolin, in 10% sodium dodecyl sulfate solution supplemented with 10% β-mercaptoethanol solution for 10-20 min at about 100℃ gave two other soluble proteins having molecular masses of 19.4 kDa and 25.0 kDa. The present study suggests that these two proteins are linked to the insoluble organic matrix by disulfide bridges because the extraction yield increases when β-mercaptoethanol is added to the medium.     

高白填料氢氧化铝的微观结构

不同分解工艺生产的高白填料,其氢氧化铝晶体生长形态不同.采用扫描电镜、X射线衍射和拉曼光谱等分析手段研究了碳分和种分氢氧化铝高白填料产品的微观结构,揭示了它们晶体发育的变化.结果表明,高白填料氢氧化铝晶体属单斜晶系,空间群P21/n,择优生长晶面均为(002)晶面;种分氢氧化铝晶体比碳分氢氧化铝晶体的(002)晶面择优取向因子值小,为多晶面生长;种分氢氧化铝晶体晶格参数比碳分氢氧化铝晶体晶格参数和拉曼光谱特征峰半高宽数值小,因此,种分高白填料氢氧化铝晶体中杂质和晶格缺陷比较少,晶体结晶度明显好于碳分高白填料产品.     

不同取向贝壳材料力学性能的压痕法研究

天然生物材料的组织结构特征及其与性能间的关系研究对于材料的仿生设计有重要意义.利用压痕法压研究了贝壳材料的硬度,断裂韧性及脆性指标,并结合SEM技术研究了贝壳珍珠层压痕形貌,探讨了珍珠层的增韧机制.结果表明,无论是珍珠层和还是柱状晶生长纹对其性能影响较小,珍珠层在平行于片层方向上与垂直于片层方向的性能差别较大,珍珠层明显的各向异性主要来自于其独特的组织特征.珍珠层其成分和独特的微观结构特点决定了其在应力场中是一种能量耗散结构,裂纹在扩展过程中,裂纹偏转,有机物桥联,纤维拔出等多种增韧机制在协同作用于材料韧性.     

Al_2O_3-ZrO_2复相陶瓷的超塑压缩变形织构

为了验证Al2O3-ZrO2复相陶瓷压缩变形后是否出现织构,采用X射线衍射（XRD）、极图和扫描电镜（SEM）对Al2O3-ZrO2复相陶瓷超塑压缩变形后的组织进行了分析。结果表明：复相陶瓷压缩变形后,Al2O3晶粒在（110）、（113）和（300）晶面出现择优取向,织构强度高达6.21,而ZrO2取向不明显。     

Bone indentation recovery time correlates with bond reforming time.

Despite centuries of work, dating back to Galileo, the molecular basis of bone's toughness and strength remains largely a mystery. A great deal is known about bone microsctructure and the microcracks that are precursors to its fracture, but little is known about the basic mechanism for dissipating the energy of an impact to keep the bone from fracturing. Bone is a nanocomposite of hydroxyapatite crystals and an organic matrix. Because rigid crystals such as the hydroxyapatite crystals cannot dissipate much energy, the organic matrix, which is mainly collagen, must be involved. A reduction in the number of collagen cross links has been associated with reduced bone strength and collagen is molecularly elongated ('pulled') when bovine tendon is strained. Using an atomic force microscope, a molecular mechanistic origin for the remarkable toughness of another biocomposite material, abalone nacre, has been found. Here we report that bone, like abalone nacre, contains polymers with 'sacrificial bonds' that both protect the polymer backbone and dissipate energy. The time needed for these sacrificial bonds to reform after pulling correlates with the time needed for bone to recover its toughness as measured by atomic force microscope indentation testing. We suggest that the sacrificial bonds found within or between collagen molecules may be partially responsible for the toughness of bone.     

PAH模板调控六棱片状碳酸铈形成机理的研究

以聚烯丙基氯化铵(PAH)为模板剂,(NH_4)_2CO_3为沉淀剂,采用液相法合成了特殊形貌的碳酸铈晶体.利用激光共聚焦显微镜、扫描电镜、红外光谱(FT-IR)及X射线衍射(XRD)等技术研究了不同反应时间碳酸铈形貌的变化,并对碳酸铈晶体的形貌和结构进行了表征.结果表明:在模板剂PAH的作用下,碳酸铈的形貌由最初的棒状逐渐向六棱片状转化,这一过程与PAH对碳酸铈晶体不同晶面的取向吸附有关.采用材料模拟软件Material Studio对PAH与碳酸铈晶面的静电吸附过程进行了模拟,从而揭示了PAH模板调控碳酸铈形貌的机理.     

海水养殖金色珍珠独特的吸收光谱及其微结构

通过紫外-可见(ultraviolet-visible, UV-VIS)吸收光谱、场发射扫描电镜(field emissionscanning electron microscope, FE-SEM)与傅里叶变换红外(Fourier transform infrared,FTIR)光谱对海水养殖金色珍珠(golden seawater cultured pearl, gold CP)的微结构及其吸收光谱特征进行了较系统的研究. 结果表明: 海水养殖金色珍珠外表面珍珠层“叠瓦状”结构的疏密程度在其表面的不同区域存在不同, 该特征可能是导致金色珍珠不同区域的紫外-可见吸收光谱存在差异的因素之一; 在由内向外的方向上, 接近珍珠核心处的珍珠层中未见单一的文石板片或棱柱结构, 而在珍珠层的中部及外侧区域均为文石板片结构; 珍珠层的外表面由多级结构构成, 其中单个珍珠层微米级的文石板片由纳米级文石小颗粒组成.     

CoAPO-5沸石晶体的合成及表征

利用水热方法,生长出了不同掺Co2+摩尔比的AlPO4-5沸石晶体(CoAPO-5)。X射线粉末衍射(XRD)和傅立叶红外吸收(FTIR)分析了晶体的结构,结果表明,Co2+离子的引入并没有显著改变AlPO4-5晶体的晶格结构;光学显微镜和扫描电子显微镜(SEM)观测了CoAPO-5晶体的光学质量和表观尺寸,结果显示,合成出的晶体形貌完整、透明,尺寸达到45 mμ×45μm×300μm;X射线荧光分析(XRF)测试了CoA-PO-5晶体的化学成分,结果表明,当Co2+离子进入AlPO4-5晶格中取代了Al3+离子,使晶体晶格带负电性,且由此导致Brφnsted酸位的产生。     

水／乙二醇混合溶剂中微波辅助合成碳酸钙

在水/乙二醇混合溶剂中,通过微波辅助加热的方法,研究溶液过饱和度对碳酸钙成核生长的影响。分别采用扫描电子显微镜(SEM)、X-射线粉末衍射(XRD)对所得的样品进行了表征。结果表明,过饱和度的改变对碳酸钙形貌和晶型具有非常明显的影响,分别获得了菱面体状方解石、纤维捆扎状文石、松树枝状球霰石为主体的碳酸钙晶体。     

溶胶-凝胶法制备ZnO及Fe掺杂ZnO薄膜及其表征

采用溶胶-凝胶法在玻璃基体上制备了ZnO和Fe掺杂ZnO薄膜,并通过扫描电子显微镜、原子力显微镜、X射线衍射仪和紫外-可见分光光度计对所制备薄膜的表面形貌、结构和光学性能进行分析。结果表明,2种薄膜均表面光滑,为沿(101)晶面取向的纤锌矿结构;与ZnO薄膜相比,Fe掺杂ZnO薄膜表面更光滑,且晶粒尺寸从58.512nm减小到36.460nm;另外,Fe掺杂后,沿(101)晶面的取向程度减弱,且禁带宽度由3.1eV增大到3.4eV。     

电化学自组装法制备透明ZnO薄膜及性能研究

以低浓度的Zn(NO3)2为电解液、KCl为支持电解质,采用电沉积自组装法在氧化铟锡(ITO)玻璃基片上成功制备了尺寸可控、性能优异、具有强的C轴择优取向生长的纳米柱ZnO薄膜;并进一步获得了六方晶体纳米结构的ZnO薄膜的优化沉积工艺.同时,结合X射线衍射(XRD)、扫描电镜测试(SEM)、透射电镜(TEM)、紫外吸收光谱(UV-vis)等测试手段对薄膜的形貌、晶形及光学性能进行了系统表征.结果表明,制备的ZnO薄膜为六方纤锌矿结构,且沿[002]方向的择优生长趋势明显、物相纯正;该薄膜的透射率最大值可达75%,禁带宽度接近于3.28 eV.     

Cu_2ZnSnS_4纳米晶的合成和表征

用乙酰丙酮铜、二水醋酸锌、氯化亚锡和高纯硫分别作为反应的铜源、锌源、锡源和硫源,油胺充当反应溶剂和活性剂,采用热注入法在不同的温度和反应时间下合成出了Cu_2ZnSnS_4纳米晶体.然后,使用X射线衍射、紫外-可见分光光度计、扫描电子显微镜和透射电子显微镜等手段分别对Cu_2ZnSnS_4纳米晶体的晶格结构、吸收谱线和表面形貌进行了表征.通过对比发现,在270℃时合成出的纳米晶体比较纯净,纳米晶体颗粒的尺寸在一定反应时间内随反应时间的延长而增大.得到的产物在有机溶剂甲苯中分散性良好.这样的"墨汁"溶液在后期制备薄膜太阳能电池更有利.     

乌龟卵壳结构的研究

本文对乌龟卵壳在扫描电镜下的微观结构进行了研究.乌龟卵壳主要由钙质层与壳膜组成.钙质层由霰石状态的碳酸钙晶体组成,可分为许多个壳单位,每个壳单位由同一中心辐射出来的针状晶体构成.卵壳的外表面具有一定的饰纹,有些部位还分布有纵横交错的有机纤维和块状的有机物质.壳膜由多层网状纤维组成,没有内、外壳膜之分.龟卵在孵化过程中不形成气室.同时对孵化前后龟卵壳的结构进行了对比研究.     

Microstructure controlling of Ti／N particles dissipated energy to superficial layer of titanium nitride film

The titanium nitride (TiNx) thin film with a controllable surface structure was fabricated by the dc-reactive magnetron sputtering technique, and the variation of microstructure in the surface layer with the energy of condensed adatom was investigated through X-ray diffraction (XRD) pattern and transmission electron microscope(TEM). It was found that the lattice parameters and the full width at half maximum (fwhm) of XRD peak on the top layers in the preferred orientation of (111) and (002) were closely correlated to the impacting induced phase composition, compressive strain, crystallite size and the fault density of the thin films. In the theory, a new means was used to model the atomistic process of per condensed adatom. The average energy at least in the minimum energy state of the incorporate adatom on TiN surface layer was statistically formulized through a careful consideration of dynamical process, which properly interpreted the experimental observations.