微波水解法制备针形α-Fe2O3纳米粒子

为了研究微波在纳米晶粒形成中的作用, 用 Ｆｅ Ｃｌ_３ 溶液在微波作用下水解, 并在其中掺入 Ｎａ Ｈ_２ Ｐ Ｏ_４ 的方法, 制备了针形的α Ｆｅ_２ Ｏ_３ 纳米粒子结果, 水解速度大大提高, 并且, 通过测试发现, 水解液的酸度、各成分浓度的配比及微波作用时间对晶粒的结构和形貌均有重要影响本文对微波与 Ｈ_２ Ｐ Ｏ^－_４ 在形成针形纳米晶粒中的作用机制也作了阐述.     

掺杂对纳米氧化铁晶化相的影响

用Ｘ射线衍射、透射电镜和穆斯堡尔谱对由掺杂了不同比例Ｓｂ的溶液－凝胶系统制得的α－Ｆｅ２Ｏ３纳米晶的晶粒度和精细结构进行了研究。结果显示，未掺杂时由Ｆｅ（ＯＨ）３非晶相干凝胶晶化而得的α－Ｆｅ２Ｏ３相晶粒较大；掺Ｓｂ后，干凝胶晶化时一部分Ｓｂ参与形成ＦｅＳｂＯ４晶相，另外的Ｓｂ原子进入α－Ｆｅ２Ｏ３晶相中形成间隙式固溶体；系统中掺杂量增多，固溶于α－Ｆｅ２Ｏ３晶相中的Ｓｂ浓度相庆也增大，它们很可能     

钛掺杂的α-Fe2O3-K2O纳米湿敏陶瓷结构与性能研究

采用硬脂酸胶法新工艺在α－Ｆｅ２Ｏ３－Ｋ２Ｏ复合体系中掺入ＴｉＯ２,ＸＲＤ,ＢＥＴ比表面吸附,Ａｒｃｈｉｍｅｄｅ排水法等手段对掺钛α－Ｆｅ２Ｏ３－Ｋ２Ｏ纳米陶瓷分析表征结果表明,适量掺杂ＴｉＯ２,材料仍保持α－Ｆｅ２Ｏ３的刚玉结构,且具有很高的热稳定性,但抑制了主晶相晶粒成长,增大了材料比表面积及孔隙率,电性能及湿敏特生测试结果表明,适量掺杂ＴｉＯ２,降低了材料固有电阻,显著减小了材料湿滞;认为钛     

用高能球磨制备氧化铁/聚氯乙烯纳米复合材料

运用穆斯堡尔谱、ＴＥＭ、ＸＲＤ方法研究了Ｆｅ３Ｏ４／聚氯乙烯（ＰＶＣ）粉末高能球磨产物,发现有超顺磁性α－Ｆｅ２Ｏ３生成,其形成原因可能是聚合物在空气中降解,生成含氧官能团与Ｆｅ３Ｏ４相互作用。     

THERMAL STABILITY OF NANOSTRUCTURED γ-Fe_2O_3 MAGNETIC POWDER

发现纳米γ－Ｆｅ２Ｏ３磁粉的ＤＴＡ曲线上出现了一个不能重现的放热峰Ｘ射线衍射分析证实此放热峰对应于从γ－Ｆｅ２Ｏ３向α－Ｆｅ２Ｏ３的结构相变，主要是结构相变和晶粒长大引起的。对比实验的结果表明，纳米γ－Ｆｅ２Ｏ３磁粉的结构相变明显高于普通的γ－Ｆｅ２Ｏ３磁粉。     

流态化CVD包硅的Fe3O4的氧化行为

采用流态化ＣＶＤ包硅技术制得了表面均匀包覆ＳｉＯ２的Ｆｅ３Ｏ４磁粉,对该包硅Ｆｅ３Ｏ４磁粉的氧化机理和动力学进行了研究,结果表明,氧化反应机理符合三维球对称对散模,氧化反应活化能随包硅量的增加而增加,流化ＣＶＤ包硅能提高Ｆｅ３Ｏ４磁粉的抗氧化作用在于粒子表面形成了均匀的ＳｉＯ２保护层。     

多孔La0.6Sr0.4Co0.2Fe0.8O3-δ的制备及表征

多孔Ｌａ０．６Ｓｒ０．４Ｃｏ０．２Ｆｅ０．８Ｏ３－δ陶瓷具有一定的强度、良好的透气和电传导性能,可用于中温ＳＯＦＣ阴极支撑和氧分离膜活性支撑体。本文用固相反应法制备了多孔Ｌａ０．６Ｓｒ０．４Ｃｏ０．２Ｆｅ０．８Ｏ３－δ陶瓷。考察了烧结条件１成型压力有机添加剂量对孔隙率和孔径的影响,研究发现气体渗透随机孔隙率线性增长,电导率随孔隙率的增大而下降,并满足关系式σ＝σ０（１－Ｐ）＾３．１。     

掺杂聚苯胺磁化率的研究

分别研究了浓Ｈ２ＳＯ４掺杂本征态聚苯胺（ＰＡｎ）、ＨＣｌ掺杂ＰＡｎ以及ＦｅＣｌ３掺杂这两种聚安在地的磁化率。通过研究磁化率的变化曲线,我们得到了一些有意义的结果：浓Ｈ２ＳＯ４掺杂ＰＡａ和ＨＣｌ掺杂ＰＡｎ的磁化率变化规律不同;ＦｅＣｌ３掺杂浓Ｈ２ＳＯ４－ＰＡｎ材料可以获得比ＦｅＣｌ３掺杂ＨＣｌ－ＰＡｎ材料更高的磁化率;ＦｅＣｌ３在掺杂ＨＣｌ－ＰＡｎ材料和浓Ｈ２ＳＯ４－ＰＡｎ材料时,ＦｅＣｌ３在这两种     

ZnxFe3—xO4的制备及性能

采用合适加剂在碱性溶液中制备了ＦｅＺｎ铁氧体，研究了其形成机理及磁性能，提出ＦｅＺｎ铁氧体的形成机理为：Ａｎ＾２＋＋２Ｆｅ＾３＋＋８０Ｈ＾－→ＺｎＦｅ２Ｏ４＋４Ｈ２Ｏ Ｆｅ＾２＋＋２Ｆｅ＾２＋＋８０Ｈ＾－→Ｆｅ３Ｏ４＋４Ｈ２Ｏ。     

一种制备γ－Fe_2O_3薄膜的新方法

采用一种简单的新工艺分别在硅片和氧化铝陶瓷基片上制备了γ－Ｆｅ＿２Ｏ＿３薄膜。该工艺分３步完成：首先利用Ｆｅ（ＮＯ＿３）＿３酒精溶液通过浸渍涂布工艺制备α－Ｆｅ＿２Ｏ＿３薄膜，其次α－Ｆｅ＿２Ｏ＿３薄膜在氢气流中、３２０～３５０℃之间热处理３０ｍｉｎ被还原为Ｆｅ＿３Ｏ＿４薄膜，最后Ｆｅ＿３Ｏ＿４薄膜在空气中２５０℃左右热处理３０ｍｉｎ被氧化为γ－Ｆｅ＿２Ｏ＿３薄膜。ＸＲＤ和ＳＥＭ分析结果表明该γ－Ｆｅ＿２Ｏ＿３薄膜呈尖晶石物相和自由取向，晶粒为针形，具有疏松多孔的微结构。     

Effect of fluoride on apatite formation from Ca4(PO4)2O in 0.1 mol L−1 KH2PO4

The effect of fluoride on the hydrolysis of tetracalcium phosphate (TTCP; Ca4(PO4)2O) was investigated in 0.1 mol l–1KH2PO4 containing 0–83 mol l–1 KF. Characterization of the final apatite phase formed by the hydrolysis was made with X-ray diffraction and SEM. The initial pH was between 4.5 and 5.4, depending on the solutions, and the pH rapidly increased and was kept constant between 7.3 and 6.5. An increase in KF concentration tended to lower the pH in the final stage of hydrolysis. The calcium concentration was considerably lower than the phosphorus concentration throughout the reaction. The fluoride concentration decreased shortly after the start of hydrolysis. The hydrolysis of TTCP in 0.1 mol l–1 KH2PO4 proceeded to form hydroxyapatite via DCPD when the KF concentration was low. The hydrolysis product was a calcium-deficient non-stoichiometric hydroxyapatite with a Ca/P ratio of about 1.5. With an increase in the KF concentration in the 0.1 mol l–1 KH2PO4 solution, TTCP directly transformed into hydroxyapatite containing F- ions or fluorapatite and with improved crystallinity. The addition of fluoride in the solution initially accelerated the formation of apatite. However, the layer of newly formed apatite adhering to the TTCP particles retarded TTCP dissolution; as a result, hydrolysis was delayed. IR analysis showed that the apatite phase contained HPO2–4 ions in the structure. The formula for the hydrolysis product of TTCP in the presence of fluoride can be expressed as follows: Ca10–x(HPO4)x(PO4)10–x(OH)2–x–yFy. © 1998 Chapman & Hall.     

Microwave assisted hydrolysis of aluminium metal and preparation of high surface area <Emphasis Type="Italic">γ</Emphasis> Al<Subscript>2</Subscript>O<Subscript>3</Subscript> powder

Phase pure boehmite particles were prepared by microwave assisted hydrolysis of aluminium sheets. These particles were calcined in air to produce γ Al₂O₃ particles with specific surface area of ~210 m²/g. The alumina particles were characterized by studying X-ray diffraction, transmission electron microscopy and Fourier transform infrared spectroscopy. For comparison, the aluminium hydroxide particles were also prepared by normal hydrolysis of aluminium metal. Normal hydrolysis yielded a mixture of boehmite and bayerite particles whereas microwave assisted hydrolysis produced phase pure boehmite particles. The importance of using microwave radiation for the hydrolysis of aluminium metal is also manifested in a shorter reaction time.     

微波场下纳米Mg-Al-LDHs及PO_4~(3-),P_2O_7~(4-)柱撑Mg-Al层状双氢氧化物的合成

用微波加热反应-变速滴加共沉淀法合成了[Mg-Al-CO3]纳米层状双氢氧化物,并以[Mg-Al-CO3]纳米层状双氢氧化物为前体,用微波加热反应-离子交换法制备了PO43-,P2O74-柱撑Mg-Al层状双氢氧化物。该法合成的[Mg-Al-CO3]纳米层状双氢氧化物的粒径约为10-40nm。讨论了微波和变速滴加碱液的速度对纳米层状双氢氧化物的合成的影响。用FT-IR、TEM与XRD对产物进行了表征,结果表明在微波加热反应的条件下可在短时间内用PO43-,P2O74-彻底交换CO32-。     

The effect of microwave-assisted for photo-catalytic degradation of rhodamine B in aqueous nano TiO2 particles dispersions

The photo-catalytic decomposition of rhodamine B was examined in aqueous nano TiO2 particles dispersions to assess effects of the microwave radiation assisted photo-catalytic process driven by UV radiation. The results of photo-catalytic degradation of rhodamine B showed that the decomposition rate increased with the microwave intensity, UV intensity, TiO2 particle dosages and the circulating fluid velocity. Addition of oxygen gas in the photo-catalytic degradation of rhodamine B increased the reaction rate. The effect of addition of H2O2 was not significant when photo-catalysis was used without additional microwave radiation or when microwave was irradiated without the use of photo-catalysts. When H2O2 was added under simultaneous use of photo-catalysis and microwave irradiation, however, considerably higher degradation reaction rates were observed. This study demonstrates that the microwave irradiation can play a very important role in photo-catalytic degradation.     

磷酸盐基耐高温粘结涂层的性能及功能填料对其性能的影响

本文以Al(OH)3和H3PO4为原料,研究了磷酸盐粘结剂的最佳合成条件,探讨了P/Al配比和反应温度对Al(H2PO4)3的形成以及填料的加入对粘结剂耐热性的影响,利用XRD和TG-DSC对粘结剂晶体结构和涂层热性能进行了分析。结果表明:P/Al比例为3∶1.4,合成温度在120~200℃范围内,可获得性能较好的Al(H2PO4)3粘结剂。填料的加入有利于粘结剂表面吸附水的蒸发和磷酸盐基体分子间结晶水的脱除,提高了涂层的热稳定性和耐高温性能。     

Sintering of MgO and MgO-TiC ceramics by plasma,microwave and conventional heating

The densification of MgO and MgO-TiC ceramics by hollow cathode plasma and microwave sintering techniques was studied. The resultant fractional densities were compared to those of conventionally sintered samples. It was demonstrated that indirect heating and sintering of MgO by microwave radiation was possible. Higher fractional densities were obtained in MgO by microwave sintering in comparison to conventional sintering under the same conditions. In the case of MgO-TiC composites, chemical reaction led to Mg₂TiO₄ formation in all samples. Plasma sintering suppressed this reaction and exhibited reduced sinterability upon TiC addition. On the other hand, small amounts of TiC additions aided the conventional sintering of MgO, resulting in better mechanical properties. Furthermore, commercial grade MgO was sintered to higher densities than relatively pure research grade MgO. Hardness and fracture toughness values are reported.     

低功率微波法合成焦磷酸钛纳米粉体及其机理

以氢氧化钛与H3PO4为原料,采用微波法在400 W功率下辐射5 min得到焦磷酸钛纳米粉体,对合成粉体进行X射线衍射、傅里叶变换红外光谱、扫描电镜和激光粒度分析,探讨焦磷酸钛粉体的微波合成机理。结果表明,焦磷酸钛粉体具有立方体结构,存在P─O、O─P─O和P─O─P键的特征吸收峰;焦磷酸钛粉体为粒度分布较均匀,颗粒粒径为50~100 nm,外形为球状;氢氧化钛与H3PO4反应先生成中间产物Ti(HPO4)2,再进一步脱水生成焦磷酸钛粉体。     

Immobilization of aqueous cadmium by addition of phosphates

In situ immobilization of heavy metals in polluted soils using phosphates leads to formation of products which are highly insoluble and thermodynamically stable over a broad pH and Eh range. In this research effectivity of Cd ions immobilization (initial [Cdaq]-4.800 mM) from aqueous solutions by different phosphorus compounds (K2HPO4, NH4H2PO4 and "Polifoska 15" fertilizer) was compared at pH in the range 4.00-9.00 and for reaction times 2-1440 h. The highest reduction of cadmium concentration (>99%), owing due to the formation of cadmium phosphates, was observed for all used phosphorus sources within pH range of 6.75-9.00. Uptake of cadmium for pH< or =5.00 did not exceed 80% and was lowest in the reaction with "Polifoska 15" fertilizer (28.25%). Identification of phases formed in the reactions using XRD, FTIR and SEM-EDS-EBSD was carried out. It was noticed that crystallinity of formed solid decreased with pH increase. Formation of Cd5H2(PO4)4.4H2O was observed in acidic conditions (pH< or =5.00), at pH approximately 7.00 mixture of following cadmium phosphates Cd(H2PO4)2, Cd3(PO4)2 and Cd5H2(PO4)4.4H2O was formed. Amorphic cadmium phosphates were noticed in alkaline conditions (pH>8.50).     

Raman and infrared spectroscopic investigations on aqueous alkali metal phosphate solutions and density functional theory calculations of phosphate-water clusters

Phosphate (PO(4)(3-)) solutions in water and heavy water have been studied by Raman and infrared spectroscopy over a broad concentration range (0.0091-5.280 mol/L) including a hydrate melt at 23 degrees C. In the low wavenumber range, spectra in R-format have been constructed and the R normalization procedure has been briefly discussed. The vibrational modes of the tetrahedral PO(4)(3-)(aq) (T(d) symmetry) have been assigned and compared to the calculated values derived from the density functional theory (DFT) method for the unhydrated PO(4)(3-)(T(d)) and phosphate-water clusters: PO(4)(3-).H(2)O (C(2v)), PO(4)(3-).2H(2)O (D(2d)), PO(4)(3-).4H(2)O (D(2d)), PO(4)(3-).6H(2)O (T(d)), and PO(4)(3-).12H(2)O (T), a cluster with a complete first hydration sphere of water molecules. A cluster with a second hydration sphere of 12 water molecules and 6 in the first sphere, PO(4)(3-).18H(2)O (T), has also been calculated. Agreement between measured and calculated vibrational modes is best in the case of the PO(4)(3-).12H(2)O cluster and the PO(4)(3-).18H(2)O cluster but far less so in the case of the unhydrated PO(4)(3-) or phosphate-water cluster with a lower number of water molecules than 12. The asymmetric, broad band shape of v(1)(a(1)) PO(4)(3-) in aqueous solutions has been measured as a function of concentration and the asymmetric and broad band shape was explained. However, the same mode in heavy water has only half the full width at half-height compared to the mode in normal water. The PO(4)(3-) is strongly hydrated in aqueous solutions. This has been verified by Raman spectroscopy comparing v(2)(H(2)O), the deformation mode of water, and the stretching modes, the v(1)OH and v(3)OH of water, in K(3)PO(4) solutions as a function of concentration and comparison with the same modes in pure water. A mode at approximately 240 cm(-1) (isotropic R spectrum) has been detected and assigned to the restricted translational mode of the strong hydrogen bonds formed between phosphate and water, P-O...HOH. In very concentrated K(3)PO(4) solutions (C(0) > or = 3.70 mol/L) and in the hydrate melt, formation of contact ion pairs (CIPs) could be detected. The phosphate in the CIPs shows a symmetry lowering of the T(d) symmetry to C(3v). In the less concentrated solutions, PO(4)(3-)(aq) solvent separated ion pairs and doubly solvent separated ion pairs exist, while in very dilute solutions fully hydrated ions are present (C(0) < or = 0.005 mol/L). Quantitative Raman measurements have been carried out to follow the hydrolysis of PO(4)(3-)(aq) over a very broad concentration range. From the hydrolysis data, the pK(3) value for H(3)PO(4) has been determined to be 12.45 at 23 degrees C.