纳米CuO/Bi2O3粉体的制备及催化性能

以Cu(NO3)2，Bi(NO3)3和CO(NH2)2为原料，用水解法并掺加添加剂直接制备出纳米CuO／Bi203粉体。用FI-IR，XRD和TEM对其组成、粒子大小、表面形貌进行表征。结果表明，CuO／Bi：0，为类球形纳米粉体，粒度均匀，粒径20nm～4nm。实验结果证明CuO／Bi2O3对合成丁炔二醇具有良好的催化活性和选择性。     

水热合成微孔纳米羟基磷灰石

以Ca(NO3)2·4H2O、P2O5为原料,水-乙醇为溶剂,在碱性介质中,采用水热法合成微孔纳米羟基磷灰石晶体(HAP),研究了水-乙醇的体积比对产物组成、晶体结构的影响. 利用X射线衍射(XRD)、红外光谱(FTIR)、热分析(TG/DTA)、透射电镜(TEM)等检测技术对HAP的晶相、化学组成和形貌进行了表征和分析. 结果表明,当V(水):V(乙醇)=1:1时,可得到晶体发育完整、晶体表面孔洞分布均匀(孔密度约为3×109个/cm2)和孔径约为1～2 nm的六方柱状纳米羟基磷灰石晶体(60 nm×100 nm).     

ZnO粉体的两种不同制备途径

本文用沉淀法和气相沉积法两种方法制备了ZnO粉体，对所得样品用粉末X射线衍射(XRD)、透射电镜(TEM)和红外吸收光谱(IR)进行了鉴定和表征，初步探讨了气相沉积法制备的ZnO微粒的生长机理，并对所用的两种制备方法作了简要的比较。     

超级电容器纳米氧化锰电极材料的合成与表征

以聚乙二醇为分散剂 ,利用高锰酸钾和醋酸锰溶液之间的化学共沉淀法制备纳米水合氧化锰 .借助SEM ,TEM ,FT IR ,XRD和BET分析手段对样品结构及性能进行表征 .研究结果表明 ,SEM和TEM显示所得粉体为纳米粉体 ,粒径大约为10～ 3 0nm左右 ,XRD分析表明该粉体为无定型α MnO2 ·nH2 O ,FT IR分析表明获得的粉体为水合物 ,BET测试比表面积达160 7m2 /g .以氧化锰为研究电极 ,饱和甘汞电极 (SCE)为参比电极 ,铂片为辅助电极的三电极体系中 ,以 1mol/L的Na2 SO4溶液为电解液 ,通过循环伏安法研究其电化学行为 .实验结果表明 ,纳米氧化锰是理想的超级电容器电极材料 ,在电位窗口为 -0 2～ 0 9V (vs .SCE)范围内 ,扫描速度为 4mV/s ,其比电容达到 2 0 3 4F/g .     

超声辐射沉淀法纳米ZnO的制备与表征

以草酸盐为沉淀剂,采用超声辐射沉淀法制备出纳米ZnO粉体,并通过XRD、TG－DTA－DTG、IR和TEM等技术研究了纳米ZnO的合成过程及粉体性能。结果表明,将超声辐射引入了普通沉淀法,可显著提高粉体性能,所得纳米ZnO粒子外貌的球形,粒度分布均匀,分散性好,平均晶粒尺寸为26nm。     

纳米晶氧化锡的水热合成与表征

以水热法合成了高比表面积的纳米晶SnO_2粉体，运用FT-IR，XRD，BET，TEM 等手段对粉体的晶化过程进行了分析表征。FT-IR显示120 ℃水热得到的粉体即实 现水合锡化合物的晶化。XRD分析表明所得粉体均匀数纳米，且随水热温度的提高 ，晶粒长大。水热粉体均具有很高的比表面积。TEM显示粉体呈单分散状态。将水 热粉体进行热处理，粉体则长大较快，比表面积降低，分散性能出现反常改善。     

微孔纳米羟基磷灰石的水热合成与结构表征

以Ca(NO3)2.4H2O,P2O5为原料,水-乙醇体系为溶剂,在碱性介质中,采用水热法合成微孔羟基磷灰石,并考察了水热温度、时间对晶体结构的影响。通过X-射线衍射(XRD)、红外光谱(FTIR)、热分析(TG/DTA)、透射电镜(TEM)等检测手段对HAP的晶相、化学组成和形貌进行了表征和分析,结果表明:160℃下水热8小时,可得到粒径为70×167nm的六方柱状微孔纳米HAP晶体,晶体表面孔径大约为1~2nm,孔密度大约为3×109个/cm2。     

纳米级β-磷酸钙的合成

通过Ca(OH)2/H3PO4/H2O体系合成了一系列的纳米级β-磷酸钙,研究了反应物浓度、反应时间对β-磷酸钙中Ca/P比的影响,应用IR,TEM,XRD对其形态和组成进行了表征并和Ca(NO3),4H2O/(NH4)2HPO4/H2O体系所制得的β-磷酸钙进行了比较.研究表明:两种方法都可以直接制备纳米级β-磷酸钙,烧结后晶体结构更完善.     

化学共沉淀法制备镱掺杂二氧化锡纳米粉体

采用化学共沉淀法,以Yb(NO3)3·6H2O和SnCl4·5H2O为原料,氨水为沉淀剂,在掺杂浓度为nSn∶nYb=9∶1的条件下,合成了分散均匀的镱掺杂二氧化锡纳米粉体。利用SEM、XRD、TG-DTA、IR等分析方法对粉体的形貌、物相、结构等进行了表征。实验结果表明,当前驱体在600℃下煅烧3h时,可以获得晶化良好、四方晶相的镱掺杂二氧化锡纳米粉体。     

溶胶-凝胶法制备BTN陶瓷材料及其性能研究

采用溶胶0凝胶法制备BTN前躯体，用XRD，IR和TEM等方法对粉体的结构和形貌进行了表征，采用等静压工艺将粉体成型，进行常压烧结，结果表明，粉体含有的团聚较少，粒径在30nm左右，至800℃时，晶体结构已经完全形成，主晶相为Nd2Ti2O7，与固相法相比，其成瓷范围宽（1270－1410℃），介电常数（ε）稳定，介质损耗(tgδ)小。     

尿素共沉淀法制备纤维状羟基磷灰石/壳聚糖复合粉料

尿素共沉淀法制备纤维状羟基磷灰石/壳聚糖复合粉料;壳聚糖; 羟基磷酸钙; 尿素共沉淀     

不同条件下合成的纳米羟基磷灰石晶体的性能研究

用磷酸钠和硝酸钙为原料,在8种不同条件下制备了纳米羟基磷灰石(n-HA)晶体,研究了不同条件下制备的n-HA晶体的形态、组成、Ca/P摩尔比和结晶度。运用透射电镜((TEM)、红外光谱(IR)和X射线衍射(XRD)分析和表征了不同条件下得到的纳米羟基磷石灰晶体的形貌、组成和结晶度。用化学方法分析了纳米羟基磷灰石晶体的Ca/P摩尔比。结果表明,不同条件下合成的纳米磷灰石晶体均为含有HPO42-和CO32-的弱结晶结构,与自然骨磷灰石类似。     

Surface modification of calcium hydroxyapatite with pyrophosphoric acid

The surface of synthetic colloidal calcium hydroxyapatite (Ca(10)(PO(4))(6)(OH)(2); CaHap) was treated with pyrophosphoric acid (H(4)P(2)O(7); PP) in acetone and the materials were characterized by XRD, thermal analysis, N(2) adsorption, TEM, and FTIR. No remarkable change in XRD patterns or in particle morphology by the modification was observed. The additional amount of PO(4) of CaHap was increased with an increase in PP concentration. The Ca/P molar ratio of CaHap was decreased from 1.62 to 1.35 by the modification. IR results indicated that the PP reacts with surface P-OH groups of CaHap to form additional surface P-OH groups as follows: surface P-OH+H(4)P(2)O(7)--> surface P-O-PO(OH)(2) + H(3)PO(4). When the modified CaHap with Ca/P molar ratio less than 1.50 was treated at 850 degrees C in air, the materials transformed into beta-Ca(3)(PO(4))(2).     

Comparative study of particle size analysis of hydroxyapatite-based nanomaterials

The purpose of this work was to compare hydroxyapatite (HAP) and composites of HAP, HAP with chitosan (CS), and HAP with poly(vinyl pyrrolidone) (PVP), in terms of their particle size and morphology, using different methods, such as Coulter counter analysis, X-ray diffraction (XRD), and transmission electron microscopy (TEM). Although many researchers have studied HAP and CS/HAP and PVP/HAP composites extensively, there is no evidence of a comparative study of their particle sizes. For this reason, different complementary methods have been used so as to provide a more complete image of final product properties — particle size — from the perspective of possible applications. The syntheses of HAP and HAP with polymer nanoparticles were carried out employing a precipitation method. Variation in particle size with synthesis time and influence of the reactants’ concentration on the materials’ preparation were systematically explored. Crystallite size calculated from XRD data revealed nanosized particles of HAP, CS/HAP, and PVP/HAP materials in the range of 2.5–9.2 nm. Coulter counter analysis revealed mean particle sizes of one thousand orders of magnitude larger, confirming that this technique measures agglomerates, not individual particles. In addition, the particles’ morphology and an assessment of their binding mode were completed by TEM measurements.     

Hydroxyapatite Hierarchically Nanostructured Porous Hollow Microspheres: Rapid,Sustainable Microwave‐Hydrothermal Synthesis by Using Creatine Phosphate as an Organic Phosphorus Source and Application in Drug Delivery and Protein Adsorption

Hierarchically nanostructured porous hollow microspheres of hydroxyapatite (HAP) are a promising biomaterial, owing to their excellent biocompatibility and porous hollow structure. Traditionally, synthetic hydroxyapatite is prepared by using an inorganic phosphorus source. Herein, we report a new strategy for the rapid, sustainable synthesis of HAP hierarchically nanostructured porous hollow microspheres by using creatine phosphate disodium salt as an organic phosphorus source in aqueous solution through a microwave‐assisted hydrothermal method. The as‐obtained products are characterized by powder X‐ray diffraction (XRD), Fourier‐transform IR (FTIR) spectroscopy, SEM, TEM, Brunauer–Emmett–Teller (BET) nitrogen sorptometry, dynamic light scattering (DLS), and thermogravimetric analysis (TGA). SEM and TEM micrographs show that HAP hierarchically nanostructured porous hollow microspheres consist of HAP nanosheets or nanorods as the building blocks and DLS measurements show that the diameters of HAP hollow microspheres are within the range 0.8–1.5 μm. The specific surface area and average pore size of the HAP porous hollow microspheres are 87.3 m²g^?1 and 20.6 nm, respectively. The important role of creatine phosphate disodium salt and the influence of the experimental conditions on the products were systematically investigated. This method is facile, rapid, surfactant‐free and environmentally friendly. The as‐prepared HAP porous hollow microspheres show a relatively high drug‐loading capacity and protein‐adsorption ability, as well as sustained drug and protein release, by using ibuprofen as a model drug and hemoglobin (Hb) as a model protein, respectively. These experiments indicate that the as‐prepared HAP porous hollow microspheres are promising for applications in biomedical fields, such as drug delivery and protein adsorption.     

PW_(11)/SBA-15介孔杂化材料的直接合成与表征

采用三嵌段共聚物EO20PO70EO20(P123)为模板剂,正硅酸乙酯(TEOS)和缺位Keggin型多金属氧酸盐Na7PW11O39(PW11)为无机前驱体,由共缩合法一步合成了PW11/SBA-15介孔杂化材料.通过红外(IR)光谱、紫外-可见漫反射光谱(UV-Vis/DRS)、X射线衍射(XRD)、低温N2吸附、透射电子显微镜(TEM)等手段对杂化材料和合成过程进行了表征.结果表明:杂化材料中不仅多金属氧酸盐的Keggin单元保留完整,且共价键联于介孔孔道内部,而且样品基本具有规整有序的六方介孔结构.TEOS预水解时间的长短对有序结构的构筑有明显影响,随预水解时间延长,样品的介观有序性增加.这是因为多金属氧酸盐对模板剂P123有盐析作用,其作用大小与多金属氧酸盐前驱物的溶解度有关.     

Sorption of tartrate ions to lanthanum (III)-modified calcium fluor- and hydroxyapatite

The present article details the formation of lanthanum-modified apatites and the binding process of tartrate ions with these obtained apatites. Chemical analyses, FT-IR and (31)P NMR spectroscopies, XRD powder, TGA, and TEM analyses were employed for studying the reaction between Ca(10)(PO(4))(6)(OH)(2) (HAp) or Ca(10)(PO(4))(6)(F)(2) (FAp) and LaCl(3). The reaction was found to take place mainly through partial dissolution of the apatite followed by precipitation of a new phase containing lanthanum phosphate. When La(3+) was introduced in the presence of L(+)-tartaric acid (TAH(2)), no fundamental changes were observed in the HAp or FAp structures. However, there did occur a formation of a new phase of Ca or/and La tartrate salt.     

以大蓟髓芯为模板制备复合孔生物活性玻璃及其体外成骨性能

以天然植物大蓟髓芯为大孔模板,以嵌段共聚物为介孔软模板,制备了孔径为60～100μm、孔壁为介孔相的高度有序多级复合孔生物活性玻璃.用扫描电子显微镜(SEM)、粉末X射线衍射仪(XRD)、高分辨率透射电镜(HRTEM)及N2吸附-脱附等测试手段对合成的样品进行了表征.结果表明,合成的材料精确地复制了植物模板的形貌,同时具有较高的比表面积和较大的孔容.通过体外模拟生理体液测试表明,这种复合孔生物活性玻璃可诱导羟基磷灰石晶体在其表面形成,具有良好的体外成骨性能,因而在骨组织修复方面具有潜在应用前景.     

羟基磷灰石/丝素蛋白复合纤维的制备及其矿化研究

在以静电纺丝法制备羟基磷灰石(HAP)/丝素蛋白(SF)复合纤维的前提下, 采用同轴共纺法获得了以HAP为“芯”、SF为“皮”的双组分电纺纤维(电纺膜), 并通过扫描和透射电镜、红外光谱以及X射线衍射等手段对电纺纤维进行了表征. 结果表明, HAP均存在于上述两种方法制备的纳米纤维中, 但同轴共纺法不仅可以避免HAP/SF共混电纺时pH值对丝素蛋白结构的影响, 并且能大大提高电纺膜中HAP的含量. 同时, 我们还分别以SF纤维、HAP/SF复合纤维和HAP/SF“皮-芯”纤维作为有机基质, 对羟基磷灰石在其上的矿化过程进行了探索, 结果表明含较多羟基磷灰石的HAP/SF“皮-芯”纤维更有利于矿化的进行.     

明胶/羟基磷灰石复合物微球中明胶对无机相影响的研究

在油包水的乳液体系中,通过原位合成的方法使羟基磷灰石(HAP)在明胶链上化学沉积,改变明胶溶液的浓度,制得了一系列的明胶/HAP复合物微球.采用X射线衍射仪(XRD)、傅里叶变换红外光谱仪(FTIR)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和热失重分析仪(TGA)等对产物的组成、形貌以及热失重情况进行了表征.结果表明,明胶用量对复合物微球中HAP的形成具有重要影响.在明胶溶液浓度为0.025 g/mL时,明胶分子链提供的结合位点恰好与溶液中游离的Ca2+、PO43-等离子达到平衡状态,复合物微球中无机相含量达40%,这是明胶与HAP以化学键合的形式结合所能得到的最大值.