利用球磨六角氮化硼制备立方氮化硼的研究

首先对六角氮化硼(hBN)进行了不同时间的球磨,并以球磨后的hBN作为初始原料研究了在高温高压条件下其对立方氮化硼(cBN)制备的影响.利用X-射线衍射、Rman光谱、XPS测试手段对球磨后的六角氮化硼进行了测试分析.结果表明,球磨不仅破坏了六角氮化硼的有序度,还改变了其表面成分和相对含量.     

高能球磨合成铁酸钙粉体的形貌及物相分析

以CaCO3、Fe2O3为原料,采用高能球磨结合热处理的工艺,制备了Ca2Fe2 O5粉体.借助X射线衍射分析、扫描电子显微镜测试手段,分析了球磨时间与热处理条件等工艺因素对合成Ca2 Fe2 O5粉体物相及形貌的影响.同时根据球磨3h原料差热曲线分析结果,得到了材料合成温度及温度范围与实验结果相符合,并探讨了高能球磨对产物合成的影响机理.结果表明:高能球磨能够降低铁酸钙粉体的合成温度,在球磨3h,800℃热处理24h的条件下,可以得到高纯度的Ca2 Fe2 O5粉体,同时球磨时间对热处理后粉体的颗粒形貌也有影响.     

立方氮化硼单晶生长界面层的精细结构

以Li3N为触媒、六方氮化硼(hBN)为原料,采用静态高温高压法合成立方氮化硼(cBN)单晶.为探讨cBN合成机理,利用扫描电镜观察了cBN单晶生长界面层形貌,利用俄歇电子能谱和X射线光电子能谱对界面层精细结构进行了表征.结果表明,cBN单晶被合成后的触媒粉末所包裹,界面层中B、N元素相对比例基本保持不变,且随着距离cBN单晶越来越近,B、N元素的sp2杂化态逐渐减少,sp3杂化态逐渐增多,这说明hBN含量逐渐减少,而cBN含量逐渐增多.由于Li元素非常活泼,在高温高压体系中的电子结构极不稳定,故可以作为电子转移的桥梁,完成电子由N向B的转移.据此认为在cBN单晶生长界面层中,B、N元素的sp2杂化态逐渐转变成了sp3杂化态.以上结果说明hBN在触媒催化作用下可直接转变为cBN.     

NH4F含量及煅烧工艺对氧化铝相变及α-Al2O3微观形貌的影响

为研究NH4F含量及煅烧工艺对氧化铝相变及α-Al2O3微观形貌的影响,向Al(OH)3粉体中引入不同质量分数的NH4F,经不同条件煅烧后获得Al2 O3粉体样品.采用X射线衍射仪和扫描电子显微镜进行物相分析和晶相形貌观察.结果表明,NH4F的引入可以显著降低Al2 O3的相变温度,含量5.0; NH4F的Al(OH)3在900℃保温2.5h全部转变为α-Al2O3,这比传统的转变温度低200～ 250℃.同时,随着NH4F含量的增加,α-Al2O3晶粒形貌由颗粒状变为平面六角片状.但是平面六角片状α-Al2 O3在1200℃是不稳定的,长时间煅烧时,α-Al2O3晶体又"熔解"为小颗粒晶粒.     

BaTiO3包覆羰基铁吸波剂的制备及其吸波性能研究

为了进一步改善羰基铁低频吸波性能,本文采用溶胶凝胶法和高能球磨法制备了BaTiO3表面改性羰基铁的复合吸波剂,并通过X射线衍射仪、SEM、EDS和矢量网络分析仪等手段对复合吸波剂的微观形貌,结构组成和吸波性能进行了分析和研究.结果表明:随球磨时间的增加,BaTiO3与羰基铁的结合形式由混合变为表面吸附,介电常数显著增大,磁导率略微增加,低频段阻抗匹配性能及电磁波衰减能力得到提升.当球磨时间为2h复合吸波剂在3.2 GHz处反射率达到-15.5 dB.通过BaTiO3对羰基铁表面改性能够调节介电常数并显著提升材料的低频吸波性能.     

Ni-MoS2/γ-Al2O3催化剂的制备及其光催化性能研究

采用共沉淀结合水热合成方法,以γ-Al2O3为载体,制备出Ni-MoS2/γ-Al2O3复合催化剂.采用X射线粉末衍射仪(XRD)、扫描电子显微镜(SEM)等方法对样品的结构与形貌进行表征.研究了MoS2负载量、煅烧温度对Ni-MoS2/γ-Al2O3复合催化剂光催化降解罗丹明B性能的影响,并考察了催化剂的循环使用性能.结果表明:负载量为30wt;,煅烧温度为300℃的复合催化剂Ni-MoS2/γ-Al2O3表面的MoS2纳米片兼具有良好的结晶度和均匀分散性,其纳米片尺寸约为200nm.可见光下,Ni-MoS2/γ-Al2O3(MoS2 30wt;/Ni 5wt;)复合催化剂对罗丹明B的降解效率能达到100;,且循环使用5次后,对罗丹明B的降解效率仍能够达到88.9;.     

超声波辅助固液反应球磨制备ZnFe2O4纳米晶的研究

以α-Fe2O3和ZnO粉体为原料,在超声波辅助高能球磨作用下通过诱发固液相反应,并在低温下烧结合成了ZnFe2O4纳米晶粉末.采用X射线、透射电镜(TEM)对前驱体和烧结产物进行了表征,分析了球磨过程对粉体晶粒尺寸的影响和znFe2O4的形成过程.实验结果表明:超声波辅助固液球磨能在低温下烧结合成ZnFe2O4纳米晶,纳米晶的晶粒尺寸为15～25 nm;相比无超声波辅助下的固液球磨,超声波球磨降低znFe2O4烧结温度约50℃;同一烧结温度下,球磨时间越长,ZnFe2O4转化率越高,晶粒尺寸越小.     

In掺杂量对ZnO薄膜微结构和光学性质的影响

采用溶胶-凝胶法分别制备未掺杂和In掺杂ZnO薄膜,用X射线衍射仪、扫描电镜和紫外可见分光光度计测试分析薄膜的微结构、表面形貌和光学性质.结果表明:In掺杂ZnO薄膜仍为六角纤锌矿结构,但In的掺入抑制ZnO薄膜的结晶,使得薄膜的结晶度降低.In掺杂ZnO薄膜表面呈网络状结构,随着In掺杂量的增加,表面起伏程度减小,空隙减少,表面平整,致密度提高.In掺杂ZnO薄膜的光学带宽Eg值均小于未掺杂ZnO薄膜,且随In掺杂量的增加先增大后减小,并用Burstein-Moss效应和缺陷浓度变化对光学带宽变化进行了解释.     

Nb掺杂下CaTi2O4(OH)2片状结构的溶剂热制备及光催化性能研究

利用无水氯化钙-钛酸四正丁酯-无水乙醇体系,通过掺杂Nb用溶剂热法制备了CaTi2O4(OH)2片状结构.利用X射线衍射(XRD),扫描电子显微镜(SEM)和比表面积测试仪(BET)对样品的显微结构和比表面积进行检测分析,并用紫外-可见吸收光度计分析了样品对光的吸收特性,研究掺人不同Nb量对CaTi2O4(OH)2样品的物相结构、微观形貌以及其光催化性能的影响,并考察了不同光源对所制备样品性能的影响.实验结果表明:随着Nb掺杂量的增加,样品的结晶度逐渐增加,当Nb掺杂量为6;时,CaTi2O4(OH)2片状结构结晶度达到最大值75.92;,此时在光源250 nm照射下光催化性能达到最优,进一步增加Nb掺杂量8;,光催化性能随之降低.这主要是样品的结晶度、能级和比表面积减小成为主导因素.     

B掺杂量对TiO2纳米粉体的结构与光催化性能影响研究

采用溶胶凝胶法制备了不同量B掺杂TiO2纳米粉体,采用X射线衍射(XRD)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、傅里叶变换红外吸收光谱(FT-IR)及紫外-可见漫反射光谱(UV-Vis)等技术对催化剂进行了表征.结果表明:B部分掺入到TiO2晶格间隙中形成B-O-Ti键,部分以B2O3的形式存在,随着B掺杂量的增加,进入晶格的B比例减少;B掺杂有效抑制了TiO2由锐钛矿相向金红石相的转变,掺杂样品经650℃煅烧后仍为锐钛矿结构,随B掺杂量的增加,其晶粒变小;B掺杂使得TiO2表面羟基量显著增加,且掺杂量越大表面羟基量越多;各掺杂样品的吸收边带没有明显红移,光吸收强度较未掺杂TiO2稍弱,且随着B掺杂量的增加,光吸收能力呈递减趋势.可见光催化降解亚甲基蓝结果表明,B掺杂大大提高了TiO2的光催化活性,这与掺B后晶粒变小,表面羟基量显著增加有关;当B掺杂质量百分数为1.0;时,B/TiO2可见光催化活性最高,达93.40;.     

Mechanical amorphization in the Ni---Zr system investigated by positron lifetime spectroscopy

The process of solid-state amorphization induced by high-energy ball milling of binary mixture of crystalline elemental powders is investigated by positron lifetime spectroscopy along with X-ray diffraction and differential scanning calorimetry. The experiments are performed on compacted samples of powders mechanically alloyed over a wide composition range (state range) at different milling times (state times) and intensities. The positron lifetime spectra is decomposed into two components. The short-lived component is composition and milling-time dependent. The second lifetime component, found during the initial stages of the milling process, appears to be due to annihilation from states trapped at crystalline interface joints. The results indicate that the solid-state reactions during ball milling involve the transformation and disappearance of the crystalline interface joints in the powder particles.     

Structure and properties of nanocrystalline Cu70Fe18Co12 obtained by mechanical alloying

Cu₇₀Fe₁₈Co₁₂ alloy is prepared by mechanical alloying of pure Cu, Fe, Co powder using a high energy ball mill, with increasing milling time ranging from 4 to 8, 24, 36 and 54 h. The variation of the morphology and the elemental distribution were measured at these different stages on various grains of the alloy using a scanning electron microscope with a dispersive energy analyzer. Atomic clusters of iron were observed on some grains after 8 h of milling, confirming the non-homogenisation of the powder at this stage. Beyond 12 h, the homogenisation is ensured over a volume of one cube micron. Microstructural changes during the mechanical alloying have been studied by X-ray diffractometry (XRD) and Mössbauer spectroscopy. X-ray diffraction measurements confirm the dissolution of iron and cobalt phases in the FCC matrix of copper after 24 h of milling with increase of the structural parameter. This same dissolution was also measured by Mössbauer spectroscopy, confirming that after 4 h of milling the CuFe phase begins to form and iron dissolution is incomplete with partial amount of alpha Fe phase surviving after 36 h of milling.     

Synthesis of highly ordered hBN in presence of group I/IIA carbonates by solid state reaction

This comprehensive study declares experimentally the effects of IA/IIA metal carbonates on the formation of hexagonal boron nitride (hBN) with the aid of the available experimental methods as regards Fourier transform infrared spectroscopy (FT‐IR), powder X‐ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (TEM). hBN is synthesized in the existence of the metal carbonates at the low temperature by modified O'Connor method. The experimental findings of FT‐IR and XRD investigations show that the addition of metal carbonates affects considerably the crystallization of hBN powder during the synthesis process. The presence of the high concentration level of the additions improves harshly the crystallinity. In this respect, the graphitization index deduced from the XRD patterns reduces with the enhancement in the amount of the dopant content. At the same time, the differentiation between the products is analyzed by the SEM surveys. According to the results, the materials synthesized by the Li₂CO₃ powder exhibit both the tubular form and rod‐like while the other samples prepared by the CaCO₃ chemical dopant display the homogeneous plates. Even, the TEM images confirm the nanowires and nanotubes structures such as multi‐walled cylindrical, bamboo nanotubes in all the materials studied in this work.     

海洋电场传感器低噪声Ag/AgCl电极的制备及性能

分别通过研磨法、球磨法、液相沉淀法和微反应器法制备了Ag/AgCl电极所用的AgCl前驱粉体,对其进行了形貌和成分分析,并对电极短期稳定性、电化学噪声的水平进行了测试。结果表明:相比之下,球磨法所制备的Ag/AgCl电极一致性好,同种电极之间的极差电位小于0.11125 mV。该电极具有良好的短期稳定性能,电位差漂移量不超过0.01906 mV/24 h,电极电压噪声密度在1 Hz处可降低至19.16 nV/Hz1/2。     

Structure and magnetic properties of bulk amorphous Fe60Co10Ni10Zr7B13 alloy formed by mechanical synthesis and hot pressing

Formation and magnetic properties of the bulk amorphous Fe₆₀Co₁₀Ni₁₀Zr₇B₁₃ alloy are described. The amorphous powder was prepared by high-energy ball milling of the amorphous ribbon and then was pressed under high pressure and temperature to obtain a bulk alloy in the form of a disc 5 mm in diameter and 2.5 mm thick. The compacted discs are fully amorphous as confirmed by X-ray diffraction and Mössbauer spectroscopy measurements. Differential scanning calorimetry curve recorded for the amorphous ribbon shows two exothermal peaks related to two stages of crystallization. Similar thermal behavior is observed for the powder samples. Hysteresis loops obtained for the amorphous ribbon, as-milled and compacted powders reveal their soft magnetic properties.     

纤蛇纹石的水热生长机制研究

以氧化镁和二氧化硅为原料,采用水热法在不同反应时间下合成了一系列纤蛇纹石纳米管.利用X-射线衍射(XRD)、红外光谱(IR)、扫描电镜(SEM)、高分辨透射电镜(TEM)等手段研究了纤蛇纹石晶体生长和晶体结构随反应时间的变化过程.X-射线衍射和红外光谱分析表明:随着反应时间的增加所得到的纤蛇纹石样品结晶逐渐完善、卷曲程度逐渐增大;电镜分析表明:获得的纳米管的外径和内径分别为15～40 nm和6～9 nm,长度为50～300 nm,出现了双层管式结构.根据实验结果,结合负离子多面体配位生长理论对纤蛇纹石的生长机理研究表明,纤蛇纹石是由片状逐渐卷曲成管状的.     

Study of ion transport behavior in a mechanochemically synthesized silver halide mixed composite system: [0.75 AgI:0.25 AgCl]

Ion transport behavior in a mechanochemically synthesized silver halide mixed composite has been investigated. AgI and AgCl, in 75: 25 mol. wt. (%) ratio, has been prepared by high energy ball milling for different milling times viz. 5, 10, 20, 30, 40, and 50 h as well as by simple physical mixing (referred to as zero hour milling). The room temperature conductivity has been evaluated as a function of milling time. The conductivity increased initially with increasing milling time, then decreased. The increase in conductivity has been attributed to the increased degree of amorphosity in the sample as a consequence of high energy ball milling. The 30-hour milled sample exhibited highest conductivity with an enhancement of more an order of magnitude from that of zero hour milled sample. To explain the ion transport mechanism in the optimum conducting sample, other basic ionic parameters viz. ionic mobility (μ), mobile ion concentration (n), ionic transference number (t_ion) etc. have also been determined. The materials and structural properties have been characterized using XRD, FTIR, and DSC techniques. Using the optimum conducting sample as electrolyte, all-solid-state battery has been fabricated having cell configuration: Ag (anode) // (0.75 AgI:0.25AgCl) // C + I₂ + Electrolyte (cathode), and the cell performance has been studied under varying load conditions.     

Comparison of glass formation by mechanical alloying and solid-state interdiffusion in Ni---Zr composites

The amorphization process in mechanically alloyed Ni---Zr powders has been investigated by optical microscopy, scanning and transmission electron microscopy, X-ray diffraction, differential scanning calorimetry and saturation magnetization measurements. Starting from elemental crystalline Ni and Zr powders, ball milling first produces a characteristically layered microstructure. Further milling leads to an ultrafine composite in which amorphization by solid-state reaction sets in between 4 and 16 h milling time. Longer milling results in fully homogeneous amorphous material. The obtained results corroborate the similarity of the amorphization process during mechanical alloying with the solid-state interdiffusion reaction in artificially modulated multilayer composites. In particular, mechanical alloying prevents intermetallic phase formation during the interdiffusion reaction because of extremely thin starting layers, thus resulting in a wider glass-forming range than obtained by other preparation techniques based on solid-state interdiffusion.     

固相合成YAG微晶粉体的XRD研究

以高纯Al_2O_3和Y_2O_3超微粉为原料,通过高能球磨和固相反应法制备了Y_3Al_5O_(12)(YAG)微晶;采用X射线衍射法(XRD)研究了球磨时间、煅烧温度、保温时间等对合成YAG微晶相组成的影响.结果表明:原料粉体的粒度随研磨时间延长而降低;随煅烧温度的提高,产物的物相由Y_4Al_2O_9和YAlO_5 逐渐向YAG相转变;延长保温时间有利于Y~(3+)和Al~(3+)的扩散以及Al_2O_3和Y_2O_3的固相反应.当Al_2O_3和Y_2O_3的摩尔比为5 ∶ 3,混合粉体经过15 h的机械球磨并于1300 ℃煅烧40 min即可得到单一物相的YAG微晶粉末.