化学镀法制备Fe包覆Al复合粉末

以次亚磷酸钠为还原剂,通过化学镀的方法制取了铁包覆铝的复合粉末,研究了络合剂、pH值、镀覆温度和镀覆时间对包覆效果的影响,采用XRD和SEM对复合粒子的表面形貌和物相结构进行了分析.结果表明铝粉表面包覆的铁层呈团粒状,优化的工艺参数为硫酸亚铁初始质量浓度:8 g/L,次亚磷酸钠质量浓度:30～40 g/L,酒石酸钾钠:16 g/L,柠檬酸:6 g/L,pH值:9.5,镀液温度:78℃,镀覆时间:40 min.     

包裹型Al(OH)3-Y(OH)3/ZrB2复合粉体的合成工艺优化研究

本文采用共沉淀法优化包裹型Al(OH)3-Y(OH)3/ZrB2复合粉体的合成工艺,通过TEM对合成的复合粉体进行形貌分析,得出适宜的包覆工艺参数分别是pH=9、溶液浓度为Al3+=0.017 moL/L和Y3+ =0.01 mol/L、滴定速度为0.05 ml/s、反应时间为60min.通过优化工艺,可以合成出包裹结构较好的包裹型Al(OH)3-Y(OH)3/ZrB2复合粉体,其包裹层厚度约为150 ～ 300 nm,为改善ZrB2基复合材料难于烧结致密化和高温条件下易氧化奠定原料基础.     

化学镀法制备陶瓷-金属复合结合剂的工艺研究

采用化学镀镍包覆陶瓷结合剂粉体的方法制备陶瓷-金属复合结合剂.确定了制备陶瓷-金属复合结合剂的镀液成分及镀覆温度等工艺参数;并用强度测试仪、EDS、SEM等仪器,对其强度等性能以及微观形貌和结构进行表征.结果表明:当镀液温度为60℃,硫酸镍含量为35 g/L,次磷酸钠浓度达到25 g/L时,结合剂增重率最大,增重30;.烧结后结合剂抗弯强度和抗冲击强度也最大,分别比未镀覆的陶瓷结合剂提高76.57;和58.43;;通过形貌观察,发现陶瓷-金属复合结合剂中陶瓷相与金属相的润湿性和结合力良好,镀层金属沿陶瓷晶界均匀分布,陶瓷相和金属相在陶瓷复合结合剂中构成三维网络结构,相互镶嵌交错.     

ZrB2/ZrO2复合粉体的放电等离子烧结行为

以高纯ZrB2粉末和ZrOCl2为原料,应用沉淀法制备了ZrO2包覆ZrB2复合粉体,并通过放电等离子烧结技术(SPS)得到高致密度的ZrB2/ZrO2复合材料.采用TEM、SEM、XRD对粉体及其烧结体进行测试,并对纯ZrB2粉体与包覆式复合粉体的烧结行为进行分析.研究结果表眀:利用沉淀法可以形成包裹结构;包覆式复合粉体的烧结性能大大优于纯ZrB2粉体,在1950℃的烧结温度下,保温10min,得到相对致密度97.8;的ZrB2/ZrO2复合材料.     

Al_2O_3包覆SrSO_4纳米复合粉体的制备与表征

采用直接沉淀-超临界流体干燥方法合成了纳米SrSO4粉体,以溶胶-凝胶法对其表面进行包覆Al(OH)3凝胶的处理,经煅烧后制备出Al2O3包覆SrSO4纳米复合粉体。通过XRD、TEM、SEM等对不同工艺条件下制备的纳米复合粉体的表面形貌和特性进行了研究。研究表明:当Al3+的浓度为0.1 mol/L、pH值为8时,可以获得好的氧化铝前驱体包覆SrSO4纳米复合粉体,经700℃煅烧3 h后获得了均匀、致密的Al2O3包覆SrSO4纳米复合粉体。     

微波水热法制备Al2O3包覆Al复合粉体的研究

用微波水热辅助沉淀法制得氧化铝前驱体/铝复合粉体,再经过1000℃煅烧2 h得到氧化铝/铝复合粉体,用XRD、SEM和EDS对粉体进行了表征.研究表明:相比普通水热法,微波水热法制备时间短,制得的前驱体水合氧化铝结晶度更好.当微波水热反应pH=11、反应时间为120 min、硝酸铝浓度为1 mol/L时,前驱体水合氧化铝的结晶度和煅烧后氧化铝对铝粉的包覆效果均达到最佳.     

高岭土/纳米TiO2复合光催化材料制备及性能研究

以高岭土为载体、钛酸丁酯为钛源,采用溶胶-凝胶法制备出高岭土/纳米TiO2复合光催化材料.采用XRD、SEM、EDS等方法对其物相组成和显微结构进行了表征,以亚甲基蓝(MB)溶液为目标降解物对其光催化性能进行了研究.结果表明:高岭石的粒径明显减小,且晶片表面负载了大量10～30nm的锐钛矿相TiO2晶粒.复合光催化材料对MB分子的去除率随光催化反应时间的延长逐步提高,且受TiO2负载量、投入量、MB溶液浓度的影响;当TiO2负载量为5 mmol/g、投入量为2 g/L、MB溶液为10 mg/L时,暗反应吸附1h、光催化90 min后对MB的去除率可达89.26;,显示出较好的光催化性能和去除效果.随着循环利用次数的增加,复合粉体的光催化性能逐步提高,并具有较高的回收率.     

RE元素对高温自润滑复合镀层性能的影响

通过对超微粉体表面预处理,采用化学复合镀的方法,在0Gr18Ni9Ti试件上得到Ni-Re-P/(人造金刚石粉(C)+CaF2)、Ni-P/(人造金刚石粉(C)+CaF2)两种复合镀层,通过测试性能比较,铼元素的加入后,耐高温自润滑复合镀层的抗氧化能力和耐磨擦磨损的能力都有较大的提高.     

纳米SiO2包覆片状微米h-BN复合粉体的制备与表征

利用St(o)ber法,以氨水为催化剂,通过正硅酸乙酯(TEOS)的水解与缩合反应,在片状微米六方氮化硼(h-BN)表面包覆一层纳米球形二氧化硅(SiO2),制备出一种以h-BN为核、SiO2为壳的h-BN@SiO2核壳结构复合粉体.采用XRD、SEM、EDS和TEM分别对包覆前后粉体进行表征,结果显示由球形纳米SO2组成的包覆层完整、致密,且与h-BN基体结合紧密、牢固.研究了TEOS与氨水添加方式对包覆效果的影响,结果表明先将氨水添加至h-BN的乙醇悬浮液中,然后分次缓慢逐滴向其中添加TEOS,每次滴加完成后间隔一段时间再进行下一次滴加得到的包覆效果最佳.     

三种改性方法对纳米ZnO催化剂粉体的光催化性能的影响

以SnCl4·5H2O、ZnNO3·6H2O、HCl、NaOH、FeCl3·6H2O为原料,采用共沉淀法制备Fe掺杂纳米ZnO、纳米ZnO/SnO2和Fe掺杂纳米ZnO/SnO2三种复合催化剂粉体,以降解甲基橙溶液反应为模型,研究了不同比例的ZnO/SnO2复合、Fe元素掺杂量以及SnO2复合Fe元素掺杂同时作用对纳米ZnO粉体光催化活性的影响,采用X射线衍射(XRD)测试方法对不同量Fe元素掺杂纳米ZnO粉体进行了表征.采用透射电镜对三种改性方法ZnO粉体进行表征.结果表明:随着ZnO/SnO2的物质的量比增加,ZnO/SnO2复合光催化剂的催化活性先增加,然后降低;随着Fe掺杂量的增加,纳米ZnO粉体的光催化活性先增加,然后降低.三种改性方法都能提高纳米ZnO粉体的光催化活性,其中Fe元素掺杂以及SnO2复合改性纳米ZnO粉体的光催化效果最好,物相为ZnO和SnO2,颗粒尺寸为15 ～20 nm,分散性好,比表面积为68.7m2/g.     

CsI-LiCl共晶材料的坩埚下降法生长与闪烁性能研究

本文采用坩埚下降法,在真空密封的石英坩埚中成功生长出CsI-LiCl与CsI-LiCl:Na共晶闪烁体。通过扫描电子显微镜(SEM)观察晶体微结构表明该共晶中LiCl相与CsI相存在周期性的层状排列,CsI相的厚度在5 μm左右。共晶样品的X射线激发发射谱显示在CsI-LiCl和CsI-LiCl:Na共晶样品存在缺陷发光,在CsI-LiCl样品中还观察到了纯CsI的自陷激子(STE)发光。CsI-LiCl样品在α粒子激发下的多道能谱中观察到明显的全能峰,这一结果证明CsI-LiCl共晶可用于热中子探测的潜力。     

静电纺丝法制备CeO2微纳米纤维及其除氟性能

以聚丙烯腈(PAN)为载体,六水合硝酸铈[Ce(NO₃)₃·6H₂O]为原料,采用静电纺丝法制备了Ce(NO₃)₃/PAN纤维,在空气中热处理得到CeO₂微纳米纤维,通过XRD、BET和SEM对CeO₂微纳米纤维进行表征。采用静态吸附实验探讨了CeO₂微纳米纤维去除水溶液中氟离子的性能,考察了溶液pH值、初始氟离子浓度及共存阴离子等对吸附性能的影响。结果表明,pH=3时,CeO₂微纳米纤维对F^-的吸附性能最佳,CeO₂吸附量随着F^-浓度的增大呈上升趋势。CeO₂微纳米纤维对F^-的吸附等温线遵循Langmuir模型,二级动力学模型能很好地描述CeO₂微纳米纤维对F^-的吸附过程。CeO₂微纳米纤维的除氟性能优良,可为其实际应用提供理论参考。     

First-principles coexistence simulations of supercooled liquid silicon

We perform first-principles coexistence simulations of the low-density and the high-density phases of supercooled liquid silicon and find a negative slope for the coexisting line in the temperature-pressure plane. Electron density maps and electron-localization function plots of the two phases of silicon show marked differences. The calculated differences suggest more localized electrons in the low-density liquid compared to the high-density liquid, coming from an increased population of covalent bonds, which further explain the calculated negative slope in the two phase coexistence regime. This is consistent with the presence of a pseudo-gap in low-density liquid silicon, absent in the high-density liquid which shows a metallic behavior.     

Triethyl ammonium salt of O,O′-bis(p-tolyl)dithiophosphate, [Et3NH]+[(4-MeC6H4O)2PS2]−

Triethyl ammonium Salt of O,O′-bis(p-tolyl)dithiophosphate and O,O′-bis(m-tolyl)dithiophosphate have been obtained by reaction of p- and m-cresol, respectively with P₂S₅ in toluene and have been characterized by elemental analysis, IR, ¹H and ³¹P NMR spectroscopy. The molecular structure of O,O′-bis(p-tolyl)dithiophosphate has been determined. Crystal data: [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻: Monoclinic, P2₁/c, a=15.2441(9) ?, b=10.415(2) ?, c=3.9726(9) ?, β=91.709(7)°, V=2217.5(1) ?⁻³, Z=4.Supplementary materials Additional material available from the Cambridge Crystallographic Data Centre (CCDC no. 600927 for [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻ comprises the final atomic coordinates for all atoms, thermal parameters, and a complete listing of bond distances and angles. Copies of this information may be obtained free of charge on application to The Director, 12 Union Road, Cambridge CB2 2EZ, UK (fax: +44-1223-336033; email: deposit@ccdc.cam.ac.uk or www:http://www.ccdc.cam.ac.uk).     

Crystal structures of thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane

Structures of both thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane, ?C₆H₄?CH₂SCH₂?C₆H₁₀?CH₂SCH₂?, have been determined, wherecis andtrans refer to the attachments to the cyclohexane ring. Thecis form crystallizes in the monoclinic space groupP2₁/c witha=8.4299(11)Å,b=21.772(2)Å,c=8.9724(13)Å, β=116.574(11)^o, andZ=4. Thetrans isomer packs into the monoclinic space groupP2₁ witha=8.159(16)Å,b=10.185(5)Å,c=9.558(2)Å, β=112.435(18)^o, andZ=2. The cyclohexane ring of thecis isomer is in the chair conformation, while the cyclohexane of thetrans isomer is found in a twisted boat conformation.     

CTAB与SDBS对碳酸锶粒子生长形态调控及机理研究

以表面活性剂CTAB和SDBS为化学添加剂,采用化学共沉淀法对碳酸锶晶体的生长形态进行调控,成功地制备出了实心的树枝状和花瓣为空心的花状碳酸锶粉体,并用X射线衍射(XRD)、扫描电子显微镜(SEM)和傅里叶变换红外光谱(FT-IR)等分析手段对样品进行了表征;最后重点对化学添加剂可能产生的影响机理进行了初步的探讨.结果表明,CTAB和SDBS在晶体生长的过程中能起到显著的影响作用,两者对粒子分散性能的作用效果相反,而且后者对晶体(013)和(213)晶面表面能降低的贡献明显大于前者.     

Crystal structure of Zn4Na(OH)6SO4Cl·6H2O

The structure of Zn₄Na(OH)₆SO₄Cl·6H₂O, a secondary mineral from Hettstedt, Germany, was determined by single-crystal X-ray diffraction. The crystals are hexagonal,a=8.413(8),c=13.095(24) Å, space group $P\bar 3$ , Z=2. The structure was refined to R=0.0554 and R_w=0.0903 for 970 reflections with I≥3σ(I). The structure can be described as zinc hydroxide layers perpendicular toc, from which sulfates and chlorides extend. The layers are held together by a system of hydrogen bonds involving hexaaquo Na⁺ ions which occupy the interlayer space.     

X-ray analysis of sideroxol from <Emphasis Type="Italic">Sideritis leptoclada</Emphasis>

Sideroxol (1), a kaurane diterpene which has the ent-7α,18-dihydroxy-15β,16β-epoxykaurane structure (MW = 320.47, C₂₀H₃₂O₃) was obtained from the acetone extract of Sideritis leptoclada plant as well as from some other Sideritis species. It crystallizes in the orthorhombic space group P2₁, 2₁, 2₁ with a = 10.967(3), b = 24.555(5), c = 6.372(4) Å, Dc = 1.240 g cm⁻³, Z = 4, and refines to R = 0.065 for 721 independent reflections. The skeleton consists of three fused six-membered rings and a five-membered ring with fused epoxide. The six membered rings exhibited slightly distorted chair conformation. In addition to sideroxol, two kaurane and five kaurene diterpenes were isolated from the hexane and acetone extracts of the studied plant.     

Photoluminescence characteristics of Mg- and Si-doped GaN thin films grown by MOCVD technique

We have studied the optical, structural and surface morphology of doped and undoped GaN thin films. The p- and n-type thin films have been successfully prepared by low-pressure MOCVD technique by doping with Mg and Si, respectively. The different carrier concentrations were obtained in the GaN thin films by varying dopant concentrations. Photoluminescence (PL) studies were carried to find the defect levels in the doped and undoped GaN thin films at low temperature. In the undoped GaN thin films, a low intensity and broad yellow band peak was observed. The donor–acceptor pair (DAP) emission and its phonon replicas were observed in both the Si or Mg lightly doped GaN thin films. The dominance of the blue and the yellow emissions increased in the PL spectra, as the carrier concentration was increased. The XRD and SEM analyses were employed to study the structural and surface morphology of the films, respectively. Both the doped and the undoped films exhibited hexagonal structure and polycrystalline nature. Mg-doped GaN thin films showed columnar structure whereas Si-doped films exhibited spherical shape grains.