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).     

银掺杂纳米羟基磷灰石抗菌粉体的水热合成及结构表征

采用水热法,以硝酸钙(Ca(NO3)2 4H2O)、硝酸银(AgNO3)和磷酸氢二铵((NH4)2HPO4)为主要原料,制备纳米级银掺杂羟基磷灰石(Ag-HA)抗菌粉体.考察了硝酸银加入量、反应温度、反应时间对产物结构和形貌的影响.XRD分析结果显示Ag-HA与HA具有相同的晶体结构.EDS和XRF分析结果说明Ag+取代Ca2+在HA晶体中的位置,生成AgxCa10-x(PO4)6(OH)2.抗菌试验结果表明,所制备的Ag-HA抗菌粉体具有良好的抗菌性能,最小抑菌浓度MIC值≤50μg/mL(对大肠杆菌、黄色葡萄球菌).     

羟基磷灰石合成工艺研究

羟基磷灰石 [Ｃａ10 (ＰＯ4 ) 6(ＯＨ) 2 ,简称ＨＡＰ]是80年代发展起来的新型牙科、骨科材料 ,其成份接近生物体骨质的无机成份 ,能诱发新骨生长 ,具有良好的生物相容性。ＨＡＰ的制备方法较多 ,有溶胶 凝胶法[1,2 ] 、沉淀法、电化学合成法[3 ,4 ] 等。1　实验1 1　试剂与仪器所用试剂除磷酸三丁酯为化学纯外 ,其它都是分析纯。美国尼高力公司 (ＮＩＣＯＬＥＴ)傅里叶变换红外光谱仪 (ＭＡＧＮＡ 5 5 0 (Ⅱ ) )。1 2　ＨＡＰ的制备1 2 1　溶胶 凝胶法合成ＨＡＰ　我们以不同原料制备了ＨＡＰ。第一种方法是以Ｃａ(ＮＯ3)2 与磷酸三丁…     

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。     

水热法合成羟基磷灰石的结构和形貌

羟基磷灰石是一种微溶于水的弱碱性磷酸钙盐 (Ｃａ10 (ＰＯ4 ) 6 (ＯＨ) 2 ,ＨＡ) [1] ,多用于人体硬组织(骨、牙 )的修复替换[2 ] 。与人类骨骼相比 ,致密羟基磷灰石仍然表现出较低的力学性能[3] 。由于针棒状的晶体具有较低的位错密度 ,较高的抗拉性能[4 ] 。近年来 ,针状或棒状羟基磷灰石的合成已引起广泛关注。合成ＨＡ的方法有固态反应法[5] 、液相沉淀法[6 ] 、溶胶 凝胶法[7,8] 及溅射法[9] 等 ,但只有少数几种方法能够对产物的形貌进行控制。虽然采用水热法在 2 0 0℃和 2ＭＰａ下合成了羟基磷灰石晶须[10 ] ,但实验步骤较为复杂 ,…     

超临界水中含碳酸根羟基磷灰石的快速连续合成

Carbonated hydroxyapatites(CHA) were rapidly and continuously synthesized in supercritical water by using a tubular reactor. The effects of reaction time and the ratio of PO₄^3-/CO₃^2- on the apatite structure were investigated by using XRD, FTIR and TEM. Results showed that 30 seconds were enough to produce fully crystalline CHA nano-rods, ca. 20×70 nm in size, at 380 ℃ and 24 MPa. When the ratio of PO₄^3-/CO₃^2- was not less than 1, the CO₃^2- ions mainly substituted for PO₄^3- in apatite structure; but CO₃^2- ions could react with Ca²⁺ to form CaCO₃ phase when the ratio of PO₄^3-/CO₃^2- was less than 1.     

纳米羟基磷灰石的合成方法研究进展

羟基磷灰石(Hydroxyapatite,HAP)是一种重要的生物、医药、重金属污染土壤/水体修复材料,本文总结了HAP的结构、组成、发展历程及应用,并从干法、湿法两个大方面系统总结了羟基磷灰石的合成方法及各种方法的优劣,对HAP合成方法的改进方向及应用前景进行了展望.     

含硅羟基磷灰石的水热合成与结构表征

以Ca(NO₃)₂、(NH₄)₃PO₄、Si(OCH₂CH₃)₄(TEOS)为原料，在200 ℃下水热处理8 h制得含硅羟基磷灰石(Si-HA)粉体。通过X-射线荧光光谱(XRF)、X-射线衍射(XRD)、红外光谱(FTIR)、透射电镜(TEM)、差示扫描量热仪(DSC)对Si-HA的晶相、化学组成、形貌和热稳定性进行了分析。结果表     

纳米羟基磷灰石/溶菌酶复合体的原位合成及酶活性研究

利用一种新的溶菌酶的组装方法, 湿法合成原位组装了羟基磷灰石/溶菌酶复合体, 对组装体进行多种表征并与浸渍组装的方法进行了对比.     

不同钙源的羟基磷灰石的合成及表征

通过比较法研究了不同钙源在水热条件下合成羟基磷灰石的方法。SEM,XRD和FT-IR的测试结果表明,蛋壳不仅可以成为有效钙源,而且多孔结构还可充当硬模板,在磷酸二氢钠缓慢腐蚀CaCO_3的同时提供PO_4~(3-)诱导生成花状羟基磷灰石。研究表明,磷酸肌酸钠水热缓慢分解释放磷酸根在合成高纯度羟基磷灰石方面有着广阔的应用前景。     

水热重结晶法制备羟基磷灰石纳米棒

本文以Ca(NO₃)₂和(NH₄)₂HPO₄为原料，采用重结晶法，在水热条件下制备了羟基磷灰石(HA)纳米棒；利用X-射线衍射(XRD)、透射电镜(TEM)、高分辨透射电镜(HRTEM)、红外光谱(FTIR)等分析测试手段，研究了pH值和晶化时间对HA组成和结构的影响。实验结果表明，室温混合pH值为7.5的沉淀物和pH值为10.5的清液，于180 ℃下水热处理10 h重结晶制得的HA纳米棒的平均长径比最长(约为28)；采用不同pH值的清液，体系的单体浓度(即化学势)改变时，得到的HA纳米棒的长径比不同；随着晶化时间延长，纳米棒的长径比先增大后减小。     

水热电沉积羟基磷灰石/Ti复合涂层的研究

在水热电沉积羟基磷灰石（Hydroxyapatite，简称HA）涂层的电解液中加入Ti粉，制备了HA/Ti复合涂层，探讨了Ti粉的加入对涂层结合强度和生物活性的影响，并研究了涂层的热稳定性。结果表明，500 ℃焙烧2 h后，HA/Ti复合涂层的结合强度为18.4 MPa，明显高于纯HA涂层的11.2 MPa；模拟体液浸泡7 d后，涂层表层形成一层碳磷灰石。Ti粉的加入明显提高了涂层的结合强度，又不降低涂层的生物活性。500 ℃焙烧不改变涂层的相组成，焙烧温度高于600 ℃时，HA部分发生分解，Ti氧化为金     

水热法制备核—壳结构勃姆石超细粉体

以硫酸铝水溶液和尿素为原料,两亲嵌段共聚物聚苯乙烯-嵌段-聚丙烯酸-2-羟基乙酯(P(St)-b-P(HEA))为结构引导剂,通过水热法合成了核壳状勃姆石超细粉体。使用X-射线衍射技术(XRD),透射电子显微镜(TEM)和扫描电子显微镜(SEM)对产物进行了表征。并在试验的基础上,对可能的形成机理进行了讨论。     

Microwave-Assisted Hydrothermal Rapid Synthesis of Ultralong Hydroxyapatite Nanowires Using Adenosine 5′-Triphosphate

Ultralong hydroxyapatite (HAP) nanowires are promising for various biomedical applications owing to their chemical similarity to the inorganic constituent of bone, high biocompatibility, good flexibility, excellent mechanical properties, etc. However, it is still challenging to control the formation of ultralong HAP nanowires because of the presence of free PO₄³⁻ ions in the reaction system containing the inorganic phosphate source. In addition, it takes a long period of time (usually tens of hours) for the synthetic process of ultralong HAP nanowires. Herein, for the first time, we have developed an eco-friendly calcium oleate precursor microwave hydrothermal method using biocompatible adenosine 5′-triphosphate (ATP) as a bio-phosphorus source and water as the only solvent for the rapid synthesis of ultralong HAP nanowires. The controllable hydrolysis of ATP can avoid the premature formation of calcium phosphate nuclei and uncontrollable crystal growth. Microwave heating can significantly shorten the synthetic time from tens of hours required by the traditional heating to 1 h, thus achieving high efficiency, energy saving and low cost. The as-prepared ultralong HAP nanowires with high flexibility have lengths of several hundred micrometers and diameters of 10~20 nm, and they usually self-assemble into nanowire bundles along their longitudinal direction. The as-prepared ultralong HAP nanowire/chitosan porous scaffold has excellent bioactivity, good biodegradation and cytocompatibility owing to the bioactive adenosine adsorbed on the surface of ultralong HAP nanowires. It is expected that ultralong HAP nanowires will be promising for various applications in the biomedical fields, such as bone defect repair, skin wound healing, and as a drug nanocarrier.     

Hydrothermal Synthesis and Characterization of Per ovskite PbTiOs3Powders from Different Precursors

Perovskite-type of PbTiO₃ fine powders which are homogeneous in physic-chemical properties has been hydrothermally synthesized from the different precursors. The borderline reaction conditions, such as temperature and time, for the formation of PbTiO₃ were established and the effect of the precursor on the particle properties was investigated. As a precursor, Pb-Tialko-carbonate xerogel dispersed in 2-methoxyethanol was found to be effective for the synthesis of the PbTiO₃ powders with a lower agglomeration and a simple mode of particle-size.     

Hydrothermal Synthesis and Characterization of Perovskite PbTiO_3 Powders from Different Precursors

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较为宽松条件下水热合成铁酸铋粉体

Bismuth ferrite(BiFeO₃) powders were hydrothermally synthesized by using FeCl₃·6H₂O and BiCl₃ as staring materials, NaOH as a mineralizer and NH₄Cl as an additive. The results show that pure BiFeO₃ powders can be synthesized under loose hydrothermal conditions of reaction temperature ranging from 140 to 230 ℃ and NaOH concentration ranging from 2 mol·L^-1 to 5 mol·L^-1. Moreover, the morphologies of the products can be controlled by changing the hydrothermal conditions.     

水热合成微晶菱镁矿研究

菱镁矿主要成份是MgCO3,菱镁矿是制取镁砂的重要原料,世界每年以菱镁矿为原料制取的镁砂达数百万吨。受天然品位限制,由菱镁矿不易制取高纯镁砂,转变成可溶性盐再精制又要增加成本。以可溶盐硫酸镁、氯化镁、硝酸镁等直接热解制取镁砂会放出强酸性腐蚀气体。化学合成无水纯MgCO3比较困难,通常先制水合盐,水合盐一般需要在CO2气流中干燥或在50℃以下长时间干燥才得无水MgCO3犤1犦。作者认为合成纯MgCO3的关键条件是控制pH值,不致生成可溶性的碳酸氢镁,也不致让氢氧化镁共结晶。本文选择脲做沉淀剂,实现适宜的pH值。理论上,还可选择与…