纳米CoB/SiO_2/PVP粉体的制备及表征

以SiO2为载体,采用浸渍化学镀法在含聚乙烯吡咯烷酮(PVP)的氯化钴溶液中制备了CoB/SiO2/PVP粉体。通过X射线衍射、扫描电子显微镜、高倍透射电镜、差示扫描量热法和傅里叶变换红外分光光度计等方法对所制备的粉体的物相、组织形貌和热稳定性进行了表征。结果表明,CoB/SiO2/PVP粉体是非晶态合金,具有复杂的网状结构,并表现为不规则形态的团聚体;CoB/SiO2PVP粉体的热稳定性较CoB粉体提高了110°C。     

硼热/碳热还原反应合成ZrB_2-SiC复合粉体及其抗氧化性能

以锆英石、氧化硼和活性炭为原料,通过硼热/碳热还原合成工艺制备Zr B2-Si C复合粉体。用X射线衍射、场发射扫描电子显微镜和透射电子显微镜研究了Zr B2-Si C复合粉体的物相组成和显微结构。用综合热分析仪研究Zr B2-Si C复合粉体的氧化动力学。结果表明:以锆英石为原料,采用硼热/碳热还原反应工艺,1 500℃反应3 h,合成出纯相Zr B2-Si C复合粉体;复合粉体中,Zr B2呈柱状或颗粒状,Si C则呈晶须状。采用Kissinger法和Ozawa法,计算了Zr B2和Si C的表观活化能,其数值分别为369和211 k J/mol。     

钡铁氧体粉体及其复合电纺纤维的制备

通过化学共沉淀法制备了磁铅石型钡铁氧体粉体,采用激光粒度仪、扫描电子显微镜（SEM）和X-射线衍射仪（XRD）等对其进行表征测试,并采用微波网络分析仪对该粉体的吸波性能进行了初步研究。分别将化学共沉淀法制备的钡铁氧体粉体以及粒径为纳米级的钡铁氧体粉体与聚乙烯吡咯烷酮（PVP）共混后静电纺丝,通过调节钡铁氧体粉体的加入方式及其分散状态等条件,探索最佳纺丝状态,制备出了负载钡铁氧体粒子的电纺纤维毡,采用扫描电子显微镜（SEM）观测了纤维形貌。     

聚乙烯吡咯烷酮/羧化壳聚糖水凝胶的制备及其理化性质的测定

本文在室温和酸性条件下,通过聚乙烯吡咯烷酮(PVP)和羧化壳聚糖(CMC)在水溶液中的混合制备了PVP/CMC水凝胶,测定了其溶胀性能。并运用红外(IR)、差示扫描量热法(DSC)、扫描电子显微镜(SEM)等方法表征了PVP/CMC水凝胶的性质。结果表明,PVP/CMC水凝胶有较好的溶胀性能,为对pH和温度敏感的物理吸附水凝胶。     

液相先驱体转化结合溶胶凝胶法合成ZrC-SiC纳米复合粉体

以八水合氧氯化锆为锆源、正硅酸乙酯为硅源、蔗糖为碳源,采用液相先驱体转化结合溶胶凝胶法合成ZrC-SiC纳米复合粉体.借助傅立叶红外光谱仪分析了有机锆先驱体的官能团,借助X射线衍射仪和扫描电子显微镜研究了Si/Zr摩尔比对复合粉体物相组成与显微形貌的影响.研究表明:有机锆先驱体具有链状或网状结构;1450℃烧成并保温2 h,Si/Zr摩尔比0.28时复合粉体中仍存在未反应的m-ZrO2相,Si/Zr摩尔比增加至1.11、2.56、5.88、23.17时均合成了纯相ZrC-SiC纳米复合粉体;随着Si/Zr摩尔比的增加,复合粉体粒径变化不大;Si/Zr摩尔比为2.56时平均粒径仅90 nm,且元素分布均匀.     

双反应室激光诱导气相合成纳米Si/C/N复相粉体及其微波介电特性

用激光诱导气相反应法,以六甲基二硅胺烷(Me3Si)2NH)(MeCH3)为原料,用双反应室激光气相合成纳米粉体装置合成了纳米Si/C/N复相粉体,复相粉体的粒径为20～30nm,纳米粉体的分散性好,无严重团聚.研究了纳米Si/C/N复相粉体在8.2～12.4 GHz的微波介电特性,纳米Si/C/N复相粉体介电常数的实部(ε′)和虚部(ε″)在8.2～12.4 GHz随频率增大而减小,复合材料的ε′和ε″可以通过纳米粉体的含量进行调整,而且介电损耗(tgδ=ε″/ε′)较高,是较为理想的微波吸收材料,计算结果表明经典的有效媒质公式对含纳米Si/C/N复相粉体的复合材料是不适合的.纳米Si/C/N复相粉体中Si,C,N原子周围的化学环境比纯SiC和Si3N4相的混合体要复杂得多,这是导致其性能变化的主要原因.纳米Si/C/N复相粉体中的SiC微晶固溶了大量的N原子,在纳米Si/C/N复相粉体中形成大量的带电缺陷,在电磁场作用下形成极化耗散电流,极化弛豫是其吸收电磁波的主要原因.     

SLS用纳米羟基磷灰石/聚酰胺6复合粉体的制备及粉体性能分析

采用高温高压溶剂沉淀法制备出纳米羟基磷灰石/聚酰胺6(n-HAP/PA6)复合粉体。通过扫描电子显微镜(SEM)、示差扫描量热法(DSC)和X-射线衍射(XRD)对粉体的微观形貌、热性能和结构进行分析;通过对粉体粒径及分布、压缩度和休止角测试,讨论了粉体的流动性能。结果表明:制备出的粉体由蓬松多孔结构变为光滑致密的近球形颗粒;随着n-HAP含量的增加,n-HAP/PA6复合粉体的熔融焓逐渐降低,有助于降低选择性激光烧结(SLS)扫描功率;成功实现了对粉体粒径的控制,当n-HAP含量为10%时粒径达到29.68μm;压缩度和休止角的降低充分表明,复合粉体中n-HAP含量为10%时所制备的粉体流动性最好。     

化学溶液分解法制备硅酸铋粉体及其表征

以正硅酸乙酯和五水硝酸铋为原料,采用化学溶液分解法制备Bi4Si3O12粉体。用X射线衍射仪和扫描电子显微镜分析了粉体的相结构和形貌,研究了正硅酸乙酯的用量对粉体相组成的影响。结果表明,前驱物粉体在650℃下煅烧1小时,得到了单一的Bi4Si3O12的粉体;颗粒大小为3～5μm,由若干个大小为300～500nm的晶粒组成为多孔的网状结构;当铋硅比(摩尔比)的用量为1∶2时,可以制备出相组成完全为Bi4Si3O12的粉体。     

Si掺杂TiO2光催化材料的制备、活性及其机理

采用两步溶胶-凝胶法制备了Si掺杂TiO2(Si:TiO2)粉体,通过X射线衍射、热重-差热分析和X射线光电子能谱表征了Si:TiO2粉体样品的晶相及表面结构,以甲基橙为目标物考察了Si掺杂TiO2的光催化活性.研究发现:Si:TiO2粉体在水中降解有机物时,比纯TiO2粉体具有更高的光催化活性;Si:TiO2粉体具有...     

纳米SiO2/NR复合材料制备工艺的研究

采用乳液共混法,研究了纳米SiO2/NR复合材料的制备工艺以及复合材料的力学性能.结果表明,纳米SiO2改性剂(硅烷偶联剂TESPT)用量为10%,搅拌时间为60min,天然胶乳浓度为20%,纳米SiO2用量为20～30份,可制备出力学性能较好的纳米Si02/NR复合材料.     

Preparation and properties of poly(Nε,Nε-dicarboxymethyl-l-lysine)

A new ampholytic homopolypeptide, $\text{poly}\text{(N}{}^{\mathrm{\epsilon }}\text{,N}{}^{\mathrm{\epsilon }}\text{-}\text{dicarboxy-methyl-}\text{l}\text{-lysine}\text{)}$, which has one tertiary amino and two carboxyl groups in the side chain has been derived from a hydrochloride salt of poly(L-lysine). The polymer in aqueous solution seems to be in the coil form with locally extended structure (LES) at neutral pH. In both the acidic and alkaline regions, the molar ellipticity of the polymer changes as a result of change in net charge on the side chain. The conformational changes may be from the coil with LES to other coiled forms. 5–7 M NaClO₄ and 80% aqueous methanol induce the α-helix in the polymer at neutral pH. Divalent cations, Cu²⁺ and Ca²⁺, do not induce any remarkably ordered structures such as α-helix or β-structure in the polymer in aqueous solution at any pH. Ultraviolet absorption studies show an absorption peak of the polymer-Cu²⁺ complex near 240 nm. Dependence of the peak intensity on pH at various q values ($\text{q =}\text{[}\text{Cu}{}^{\mathrm{2+}}\text{]}\text{[}\text{residue}\text{]}$) indicates the two steps of the complex formation. At q less than 0.64, the formation is described only with the first step. An average coordination number for Cu²⁺ at the first step was calculated to be about 2 by the method of Mandel and Leyte. The association constant of Cu²⁺ with the residue at the step was determined from the absorption data to be far smaller than that for the Cu²⁺-EDTA complex. The second step of the formation occurs in the case of large q but the absorption data for the second step cannot be obtained exactly due to precipitation.     

Wet Milling of Fe/Al/Al2O3 and Fe2O3/Al/Al2O3 Powder Mixtures

Wet milling of Al₂O₃-aluminide alloy (3A) precursor powders in acetone has been investigated by milling Fe/Al/Al₂O₃ and Fe₂O₃/Al/Al₂O₃ powder mixtures. The influence of the milling process on the physical and chemical properties of the milled powders has been studied. Particle refinement and homogenization were found not to play a dominant role, whereas plastic deformation of the metal particles leads to the formation of dislocations and a highly disarranged polycrystalline structure. Although no chemical reactions among the powder components in Fe₂O₃/Al/Al₂O₃ powder mixtures were observed, the formation of a nanocrystalline, ordered intermetallic FeAl phase in Fe/Al/Al₂O₃ powder mixtures caused by mechanical alloying was detected. Chemical reactions of Fe and Al particle surfaces with the atmosphere and the milling media lead to the formation of highly porous hydroxides on the particle surfaces. Hence the specific surface area of the powders increases, while the powder density decreases during milling. The fraction of Fe oxidized during milling was determined to be 0.13. The fraction of Al oxidized during milling strongly depends on the metal content of the powder mixture. It ranges between 0.4 and 0.8.     

Participation of lewis base on vinyl chloride polymerization with Al(C2H5)3CCl4 catalyst system

The polymerization of vinyl chloride has been investigated using an $\text{Al}\text{(}\text{C}{}_2\text{H}{}_5\text{)}{}_3\text{CCl}{}_4$ catalyst system in the presence of various Lewis bases. Effective Lewis bases are γ-butyrolactone, diglyme and diethylenetriamine which are multidentate. The rate of polymerization is dependent not only on the basicity of the Lewis base used but also on a coordination number of one. The latter is the predominant factor. For the effect of polymeric amines, a tentative hypothesis is discussed.     

Sintering of Si3N4-Y2O3-Al2O3

Sintering kinetics of the system Si₃N4-Y2O₃-Al₂O3 were determined from measurements of the linear shrinkage of pressed disks sintered isothermally at 1500° to 1700°C. Amorphous and crystalline Si₃N₄ were studied with additions of 4 to 17 wt% Y₂O₃ and 4 wt% A1₂O₃. Sintering occurs by a liquid-phase mechanism in which the kinetics exhibit the three stages predicted by Kingery's model. However, the rates during the second stage of the process are higher for all compositions than predicted by the model. X-ray data show the presence of several transient phases which, with sufficient heating, disappear leaving mixtures of β ' -Si₃N₄ and glass or β '-Si₃N₄, α '-Si₃N₄, and glass. The compositions and amounts of the residual glassy phases are estimated.     

Synthesis and Characterization of Ti0.33Ta0.33Nb0.33C and Ti0.33Ta0.33Nb0.33CxN1-x Whiskers

Ta_0.33Ti_0.33Nb_0.33C and Ta_0.33Ti_0.33Nb_0.33C _x N_{1− x} whiskers were synthesized via a carbothermal vapor-liquid-solid growth mechanism in the temperature range 900°-1450°C in Ar or N₂. The optimum temperature was 1250°C. Whiskers were obtained in a yield of 70-90 vol%. The whiskers were 0.5–1 µm in diameter and 10–30 µm in length. The starting materials that produced the highest whisker yield were: TiO₂, Ta₂O₅, Nb₂O₅, C, Ni, and NaCl. C was added to reduce the oxides, and Ni to catalyze whisker growth. NaCl was used as a source of Cl for vapor-phase transportation of Ta and Nb oxochlorides and Ti chlorides to the catalyst. The catalyst metal was recycled several times during the synthesis and was transported as NiCl₂( g ) according to thermodynamic calculations. The rate of formation and the chemical composition of the whiskers depended on the synthesis temperature, the choice of catalyst, and the atmosphere. At low temperatures, the whiskers were enriched in Nb and Ta, whereas the Ti content increased with increased synthesis temperature.