ICP—AES法测定陶瓷二氧化铀芯块粉末标准物质中铝,钡,钴,钽,钛和钒

随着大型核电事业的发展,对核纯陶瓷二氧化铀芯块的质量控制、质量保证及对测试方法的校准和确认等方面,迫切需要研制核纯陶瓷二氧化铀芯块的杂质标准物质.测定铀及其化合物中痕量杂质元素,需预先将铀与杂质元素分离,国外大多采用萃取法,国内都采用萃取色谱法.所用萃取剂有TBP、TOPO以及TEHP等.本文用我院合成的237季铵萃取树脂进行分离富集,并用ICP-AES法同时测定陶瓷二氧化铀芯块粉末标准物质中铝、钡、钴、钽、钛和钒.     

特种合金钢系列标准物质研制

介绍了特种合金钢系列标准物质的研制过程。采用合理的冶炼锻轧工艺,选取不同部位的样品进行均匀性检验,确定了15种元素的认定值及扩展不确定度,并进行了线性、一致性考察以及与国内外同类标准物质的比对。结果表明,本套特种合金钢系列标准物质的均匀性良好,定值准确且有良好的梯度分布。     

高性能陶瓷聚合物前驱体研究新进展

含硅聚合物是制备高性能陶瓷的重要前驱体。聚合物前驱体热解转化法在非氧化物陶瓷及其复合材料制备方面具有特别优势。本文主要介绍了含不饱和基团聚硅碳烷、线性和超支化聚硼硅氮烷、含过渡金属聚合物等几类前驱体的结构设计和合成新方法,以及其在电磁波吸收材料、锂电池负极材料、特种陶瓷结构3D打印成型方面应用的新进展。     

开拓创新 精益求精

<正>中国船舶重工集团公司第十二所标准物质研究室是国家冶金标准样品定点研制单位(证书号为:BKRK25-2009)和国家有色标准样品会员单位,拥有独特的金属材料标准物质均匀化制备技术优势,主要研制开发铸造金属材料光谱分析用标准物质和成分分析标准物质,广泛应用于兵器、航空、航天、船舶、冶金、机械等行业。北京、上海、沈阳、武汉、济南等全国各大城市均有代理销售单位。发展目标:成为中国金属材料标准物质制备基地及国防特种合金标准物质研究试验中心。     

快速络合滴定法测定刺梨中单宁含量

刺梨中含有大量维生素C及其它还原性物质,目前国内外报导的几种主要测定单宁方法,用于刺梨中单宁含量的测定都有其不足之处。本工作在文献基础上,探讨了锌沉淀单宁的特性及其动态平衡理论,建立了利用标准滴定曲线或回归直线方程式测定刺梨中单宁含量方法。本法克服了维生素C及其它还原性物质的干扰,提高了精度和准确度,且简便,快速。     

聚合物流变特性标准物质的研制

介绍聚合物流变特性标准物质的研制过程。聚合物流变特性标准物质主要由聚异丁烯和十六烷组成。研制的该标准物质具有良好的均匀性、稳定性。经对测定数据进行统计处理,确定了该标准物质在不同静态剪切速率下粘度和第一法向应力差的标准值并给出了其相对扩展不确定度。     

用CTMAB作沉淀剂叶蜡石中二氧化硅的重量测定法

我国对叶蜡石的应用已有近两千年的历史,由于叶蜡石具有绝缘性、耐酸性、导热导电率低、熔点和比热高等特性,目前已广泛应用于耐火材料、陶瓷、玻纤、白水泥、造纸和橡塑等许多工业领域。陶瓷工业是叶蜡石的主要应用领域,主要用于生产建筑陶瓷、卫生陶瓷、精细美术陶瓷和特种陶瓷。     

透光率计滤光片标准物质的研制

以中性灰玻璃及特种石英玻璃为材料,采用切割、研磨、抛光等工艺,制备了校准透光率计用系列滤光片标准物质,标准物质的均匀性不确定度为0.08%,校准周期内的稳定性不确定度为0.19%,扩展不确定度为0.5%(k=2)。该标准物质可广泛用于校准透光率计,具有携带方便、性能稳定等优点。     

氢化物发生-原子荧光光谱法测定地球化学样品中的锗

样品经硝酸-氢氟酸-硫酸混合酸消解,磷酸提取。通过对溶液的测定介质和介质浓度、KBH4浓度、灯电流等条件的优化及其对共存元素测定影响及其消除,建立了用原子荧光光谱法测定地球化学样品中微量锗的方法,方法检出限为33ng/g,测定范围为0.10~60μg/g,经国家一级标准物质验证,测定结果与标准值吻合;方法精密度好,准确度高。     

氢化物发生-原子荧光光谱法测定地球化学样品中的锗

样品经硝酸-氢氟酸-硫酸混合酸消解,磷酸提取。通过对溶液的测定介质和介质浓度、KBH4浓度、灯电流等条件的优化及其对共存元素测定影响及其消除,建立了用原子荧光光谱法测定地球化学样品中微量锗的方法,方法检出限为33ng/g,测定范围为0.10~60μg/g,经国家一级标准物质验证,测定结果与标准值吻合;方法精密度好,准确度高。     

Comparison of a portable micro-X-ray fluorescence spectrometry with inductively coupled plasma atomic emission spectrometry for the ancient ceramics analysis

Two multielement instrumental methods of analysis, micro X-ray fluorescence spectrometry (micro-XRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were applied for the analysis of 7th and 5th century B.C. ancient ceramic sherds in order to evaluate the above two methods and to assess the potential to use the current compact and portable micro-XRF instrument for the in situ analysis of ancient ceramics. The distinguishing factor of interest is that micro-XRF spectrometry offers the possibility of a nondestructive analysis, an aspect of primary importance in the compositional analysis of cultural objects. Micro-XRF measurements were performed firstly directly on the ceramic sherds with no special pretreatment apart from surface cleaning (micro-XRF on sherds) and secondly on pressed pellet disks which were prepared for each ceramic sherd (micro-XRF on pellet). For the ICP-AES determination of elements, test solutions were prepared by the application of a microwave-assisted decomposition procedure in closed high-pressure PFA vessels. Also, the standard reference material SARM 69 was used for the efficiency calibration of the micro-XRF instrument and was analysed by both methods. In order to verify the calibration, the standard reference materials NCS DC 73332 and SRM620 as well as the reference materials AWI-1 and PRI-1 were analysed by micro-XRF. Elemental concentrations determined by the three analytical procedures (ICP-AES, micro-XRF on sherds and micro-XRF on pellets) were statistically treated by correlation analysis and Student's t-test (at the 95% confidence level).     

硅基聚合物前驱体转化陶瓷微观结构研究进展

聚合物前驱体转化法使得陶瓷材料的制备实现了可分子设计和可聚合物工艺加工,在陶瓷基复合材料、陶瓷纤维、功能涂层、特种胶粘剂等方面具有重要应用价值.不同于传统粉末烧结工艺,该方法涉及有机聚合物至无机陶瓷的转化过程,因此,聚合物前驱体的分子结构以及陶瓷化工艺对所制备陶瓷材料的微观结构和功能特性具有直接影响.本文综述了基于聚合...     

Topical Problems in Elemental Analysis of Advanced Ceramic Materials

Selected prominent problems in the analysis of advanced ceramic materials are surveyed. The importance of reliability of results is discussed in the field of elemental trace- and microanalysis in view of its interaction with economy, power of detection, local resolution and speciation selectivity. Particular problems in the analysis of major constituents, trace components and microlocal distributions are based on the striking propertics of ceramics; they are exemplified. Analytical assistance must start from the beginning of the production processing, in the preparation of the powdered base materials. Determination of the stoichiometry requires high accuracy and differentiation of chemical species in bulk and surface analysis of ceramic base powders. Element trace determination by direct instrumental methods requires standard reference materials for calibration; these are currently inavailable in a sufficient variety. For optimum reliability and power of detection, element traces must be prepared in isolated form in a small excitation volume for analysis. A review on the state-of-the-art of wet-chemical combined procedures is presented. Decomposition position procedures are emphasized, due to their risk of contributing severe systematic error. Combustion in elementary fluorine is presented for decomposition of refractory materials. The performance of some direct procedures is discussed. Very efficient methods are available for element trace determinations in ceramic materials, offering high detection power. Several approaches for high-resolution local microanalysis in non-conductive ceramic materials are identified as the most promising development in the analysis of sintered compact ceramic products and devices.     

Rare-earth-doped transparent glass ceramics

Glass ceramics are a known class of polycrystalline ceramic materials, where, depending on the glass matrix and the particular crystalline phases, one can obtain materials with improved mechanical, thermal, electrical or optical properties. The characteristics and applications of optical glass ceramics are reviewed, with particular emphasis on rare-earth-doped transparent glass ceramics for photonics, including the search for new transparent glass ceramic compositions and the development of suitable methods to process such materials into functional devices.     

结构陶瓷复合材料的现状和发展趋势

本文简要叙述了结构陶瓷高温下强度及硬度高、蠕变小、抗氧化、耐腐蚀、耐磨损等优越性能,同时指出了陶瓷应用于承载结构的致命弱点,即陶瓷的脆性。较详细地综述了克服陶瓷脆性的主要技术方向--开发第二相粒子、纤维(晶须)补强增韧的微米陶瓷复合材料及纳米陶瓷复合材料,并分析了纳米陶瓷的发展前景。     

生物模板法制备木材陶瓷*

生物模板法是一种制备具有生物形貌特点的结构和功能材料的新方法。由于木材组织结构方面的独特性,制备其多级孔结构的木材生态陶瓷在探索特殊微观结构和性能之间的关系方面有着重大的意义。本文总结了生物模板法制备陶瓷材料技术的发展现状,并且指出了各种工艺的优缺点,着重介绍了木材陶瓷的发展历史、制备方法、机理和性能,概述了木材陶瓷在骨移植材料和催化材料方面的应用和发展前景。     

Thermal analysis and the processing of electronic and magnetic ceramics

Control of processing parameters, in both conventional ceramic routes and novel gel processing routes, is vital in the production of electronic and magnetic ceramics. The role of thermal analysis in the provision of basic data for the understanding of both types of processing route is discussed with special emphasis being placed upon the production of 1–2–3 YBCO superconductors and MgO-based soft ferrite materials for TV deflection unit applications.     

Trends in development of calcium phosphate-based ceramic and composite materials for medical applications: Transition to nanoscale

Current status and lines of research were considered for calcium phosphate-based ceramic materials intended for application in new technologies for damaged bone tissue regeneration. The main trend is toward mimicking the composition, structure, and properties of biological bone tissues by ceramic materials. This necessitated developmental efforts on synthesizing polysubstituted, in particular nanocrystalline, biphasic calcium phosphates and on preparing ceramics and composite materials thereof. The progress achieved in this area was reviewed, and certain benefits associated with medical application of these materials were discussed.     

基于环硼氮烷的高陶瓷产率SiBCN先驱体的合成与性能

聚合物先驱体转化法作为制备SiBCN陶瓷及其复合材料的重要途径,具有成型温度低、产物结构和组成可控等优点.设计合成合适的聚合物先驱体是提高陶瓷产率和性能的关键因素之一,本文采用三氯环硼氮烷(TCB)与乙炔基氯化镁进行反应,合成了乙炔基环硼氮烷,进而与二氯硅烷和二氯甲基乙烯基硅烷进行共氨解反应,制备了聚硼硅氮烷先驱体(PBSZ)并进行了高温裂解.采用综合热分析(TG-DSG)对其陶瓷化过程进行了分析,并采用XRD和SEM对陶瓷化产物的结构进行了表征.PBSZ在室温下是液态,易溶于二氯甲烷和氯仿等溶剂,可加工性优良.基于PBSZ先驱体的SiBCN陶瓷产率超过80%;陶瓷化产物在1400℃以下为无定形状态,在1500℃可形成由α-Si3N4,β-Si3N4,h-BN和SiO2晶体结构组成的陶瓷;陶瓷产物表面致密平整且具有优异的热稳定性和氧化性能,表明聚硼硅氮烷(PBSZ)有望成为高陶瓷产率和高性能陶瓷的重要先驱体.     

Use of Sol-Gel or Coacervate Process to Formulate Glassy or Ceramic Phosphates for Coating

Abstract

One of the objectives of present research on glassy and ceramic phosphates for coating materials is the synthesis of new precursors and the formulation of their mixtures. The properties of these materials depend mainly on the relative proportions of their constituents. Being able to varie at will the formulation of the materials the importance of the sol gel to glass or ceramics is dearly shown. This soft process is in a number of cases, preferable to the conventional high-temperature process.