介孔铝酸钴的溶胶－凝胶法合成与表征

采用嵌段聚合物P123为表面活性剂，以氯化铝和氯化钴为无机先驱物，采用溶胶－凝胶法合成介孔铝酸钴纳米粒子。X射线衍射（XRD）表明样品具有单一的尖晶石型结构，利用氮气吸附－脱附比表面测定仪测得不同焙烧温度样品的比表面积，发现700℃焙样品比表面积最大，其比表面积为59．3E／g，孔径为10．8nm。紫外可见光谱仪测示表...     

碳包覆氧化亚钴纳米颗粒的制备与性能研究

采用直流电弧放电等离子体技术成功制备了碳包覆氧化亚钴纳米颗粒,并对样品的形貌、晶体结构、粒度、比表面积和孔结构采用高分辨透射电子显微镜(HRTEM)、X射线衍射(XRD)、X射线能量色散光谱(XEDS)、拉曼散射光谱(Raman)和N_2吸-脱附等测试手段进行了分析。HRTEM表明该方法制备的碳包覆氧化亚钴纳米颗粒具有典型的核壳结构,颗粒形貌主要为球形或椭球结构,粒度均匀,分散性良好,粒径分布在20~60nm,平均粒径为40nm,外壳碳层的厚度为5nm。XRD证明样品的内核为面心立方结构的氧化亚钴纳米颗粒,外壳为碳层。XEDS图谱表明样品中主要存在Co、O和C元素的特征峰。Raman光谱说明样品中碳外包覆层的石墨化程度较低,发生了红移现象。样品的N_2吸附-脱附等温曲线属Ⅳ型,BET比表面积为33m~2/g,BJH脱附累积总孔孔容和脱附平均孔径分别为0.078cm~3/g和11nm。当量粒径为43nm,与TEM和XRD测得的结果基本一致。     

纳米TiO2光催化剂的电化学法制备及其表征

采用有机电解-溶胶-凝胶法制备了纳米TiO2光催化剂,通过XRD、TEM、TG-DTA、激光粒度分析法等对纳米TiO2的结构相变、表面形貌、颗粒大小等进行了表征.实验表明:当热处理温度低于350℃时,TiO2的晶相结构均为锐钛型,颗粒大小在25nm以下,样品的比表面积大于65m2*g-1;热处理温度为400℃时,TiO2的晶相结构出现锐钛型和金红石型混合相,颗粒大小在35nm以下,样品比表面积为46.43m2*g-1,实验制备的粉体样品属于纳米级水平;实验测试了各焙烧温度下粉体样品的光催化活性.     

无模板剂法合成介孔NiAl_(10)O_(16)纳米粉及表征

不添加模板剂或者有机表面活性剂,通过摩尔比为1∶10的镍和铝硝酸盐水溶液与碳酸铵溶液水解的方法制备了高比表面积的介孔NiAl_(10)O_(16)纳米粉体。研究了焙烧温度对介孔NiAl_(10)O_(16)纳米粉体的比表面积和镍物种的影响。采用热重差热分析(TGDSC)、X射线粉末衍射(XRD)、氢气程序升温还原(H2-TPR)扫描电镜(SEM)、透射电镜(TEM)及N2吸附-脱附等手段表征。结果表明,制备的NiAl_(10)O_(16)纳米粉具有虫孔状介孔结构,比表面积在123~402m~2/g,孔径集中在2.9~6.6nm,孔容为0.20~0.29cm~3/g。随着焙烧温度的增加,样品的比表面积减小,孔径增加。样品中出现的表面铝酸镍和骨架铝酸镍,能够满足不同催化反应对镍物种的需求。     

纳米CexGd1-xO2-δ复合氧化物的制备及表征

采用柠檬酸溶胶-凝胶法(Sol-Gel),以Ce(NO_3)_3·6H_2O、Gd_2O_3、柠檬酸为原料,制备纳米级Ce_xGd_(1-x)O_(2-δ)复合氧化物,对制得的样品进行X射线衍射、比表面、扫描电镜及能谱和透射电镜表征,研究样品的组成、晶粒大小、比表面积和样品形貌特征。结果表明,Ce_xGd_(1-x)O_(2-δ)复合氧化物在600℃和800℃焙烧后均形成均匀的面心立方CeO_2基固溶体和/或体心立方Gd_2O_3基固溶体。单组分Gd_2 O_3样品在800℃焙烧后形成具有体心立方的Gd_2O_3物相,经600℃焙烧后还同时含有43%(质量分数)的六方Gd_2O_2CO_3晶型。对于同一Gd~(3+)掺杂比例样品,焙烧温度越高,晶粒越大,比表面积越小;同一焙烧温度样品的晶粒尺寸随Gd~(3+)掺杂量增大先减小后增大,但均小于单组分CeO_2和Gd_2O_3,且Ce_(0.5)Gd_(0.5)O_(2-δ)样品晶粒最小。表明复合氧化物的形成提高了抗烧结能力,形成更多孔隙结构,使样品晶粒变小,比表面积变大,并且x=0.5为形成最小纳米级样品的最佳比例。     

Co3O4纳米颗粒的制备及表征

以脱脂棉为碳源,硝酸钴为前驱物,采用碳辅助法焙烧制备了粒径为50nm Co3O4纳米颗粒。用X射线衍射(XRD)对不同焙烧温度(200~600℃)下样品的物相、晶粒度进行了研究,并结合傅立叶红外光谱(FT-IR)对Co3O4物相演变进行了分析,确定中间产物前躯体是CoCO3;通过扫描电镜(SEM)和透射电镜(TEM)对制备的Co3O4样品的形貌、粒径进行了分析;同时,X射线能谱(EDS)和氮气吸附-脱附曲线测试等表明制备的Co3O4表面存在碳元素和孔结构,具有较大的比表面积,有利于提升其光解水制氢能力。     

银纳米粉的比表面积研究

采用阳极弧放电等离子体方法制备了高纯银纳米粉末.利用X射线衍射(XRD)、透射电子显微镜(TEM)对样品的形貌、晶体结构、粒度进行性能表征.利用静态表面吸附仪依据BET多层吸附原理,在液氮温度下(78K)和气体饱和蒸气压力范围内测试样品对N2的吸附-脱附等温线,用图解法根据吸附等温线求出单层吸附容量,由BET吸附公式计算出纳米粉末比表面积.结果表明:银纳米粉末的晶体结构为fcc结构,粒径范围在10～50nm,平均粒径为26nm,比表面积为23.81 m2/g.     

碳包覆NiO纳米颗粒的制备与性能

采用直流电弧放电等离子体技术成功制备了碳包覆NiO(NiO@C)纳米颗粒,并对样品的形貌、晶体结构、粒度、比表面积和孔结构采用高分辨透射电子显微镜、X射线衍射、X射线能量色散分析谱仪、拉曼散射光谱和N_2吸-脱附等测试手段进行了分析。实验结果表明:直流电弧等离子体技术制备的NiO@C纳米颗粒具有典型的核壳结构,内核为面心立方结构的NiO纳米颗粒,外壳为碳层。颗粒形貌主要为立方体结构,粒度均匀,分散性良好,粒径分布在30~70nm范围,平均粒径为50nm,外壳碳层的厚度为5nm。NiO@C纳米颗粒BET比表面积为28m~2/g,等效直径为46nm,与TEM和XRD测得的结果基本一致。Raman光谱说明样品中碳包覆层的石墨化程度较低,发生了红移现象。     

制备条件对溶胶-凝胶法合成氧化锰八面体分子筛的影响

以高锰酸钾和马来酸为原料采用溶胶-凝胶法合成了氧化锰八面体分子筛,详细考察了制备参数如焙烧条件、陈化条件、水热处理对合成材料的晶型和比表面积的影响,焙烧温度影响制备材料的晶型,焙烧时间对比表面积有较大影响,而适当的水热处理则可以增加材料的比表面积.较为合适的制备条件为70℃水热处理,在450℃焙烧2h,得到的样品具有较好的晶型和较大的表面积.     

镍纳米粉的阳极弧等离子体制备与粒度研究

采用阳极弧放电等离子体方法成功制备了高纯镍纳米粉体并对其粒度进行表征.采用X射线衍射(XRD)测试样品的物相和结构,并用Scherrer公式计算晶粒粒度;采用透射电子显微镜(TEM)分析样品的形貌、结构和粒度分布;采用表面吸附仪测定样品的N2吸附-脱附等温线,并由BET理论模型计算出样品的比表面积和颗粒粒度.实验结果表明:本法所制备的镍纳米的晶体结构与相应的块体材料基本相同,为fcc结构的晶态,呈规则的球形链状分布,比表面积为14.23m2/g,粒径范围分布在(20～70) nm,平均粒径为47 nm,三种方法测得的结果基本一致.     

铝酸钴对软聚氯乙烯阻燃热降解性影响

通过活性炭模板法制备出尖晶石型铝酸钴阻燃剂。将其应用于软聚氯乙烯(PVC)的阻燃研究。当添加10 g铝酸钴时,软PVC的阻燃、消烟和力学性能最佳。通过热重-红外和扫描电镜对阻燃前后的热降解过程进行研究,表明,阻燃处理后,软PVC样品的初始降解温度提前,高温时的剩炭量增加;降解过程中释放HCl和-CH_3气体碎片的最大释放峰温度提前,并且气体的释放量减少,降解过程中形成稳定的炭层,阻止了内部可燃气体与外部的氧气接触,达到良好的阻燃消烟性能。     

铝酸酯偶联剂表面改性微晶白云母/PVC复合材料的制备及力学性能

以中国川西地区发现的一种新型矿物资源微晶白云母为原料,以铝酸酯偶联剂F-1为改性剂,对微晶白云母进行改性研究,并将表面改性后的微晶白云母加入聚氯乙烯(PVC)中制得微晶白云母/PVC复合材料。测试了改性粉体与石蜡体系的黏度及复合材料的力学性能,并采用扫描电子显微镜表征了其微观结构。结果表明,铝酸酯偶联剂F-1能有效改善微晶白云母表面与有机物质的界面结合,并且将经铝酸酯偶联剂F-1改性的微晶白云母加入PVC基体中能提高微晶白云母/PVC复合材料的力学性能,当铝酸酯偶联剂的用量为1.0%(质量分数,下同)、微晶白云母用量为15%时,微晶白云母/PVC复合材料的力学性能最好。     

Synthesis of nano grade hollow silica sphere via a soft template method

The nano grade hollow silica sphere (HSS) was synthesized by a novel soft template method. We found that the precipitate of aluminate had a porous structure that could be the soft template for HSS. After mixing the colloidal silica with the aluminate precipitate, the bubble trapped in this porous structure could form the nano grade HSS. The aluminate precipitate was removed by adjusting the pH of the slurry to approximately 1. The outside diameter, the specific surface, and the mean pore size diameter of the forming HSS were 60-90 nm, 571 m2/g, and 3 nm, respectively. The formed HSS was collected by modifying the surface with Si(OCH3)3CHCH2 (VTMO) and then filtrating the precipitated gel in the n-butanol and ethanol solvent system.     

Synthesis and characterization of lithium aluminate nanoparticles

In this work, we report the synthesis of lithium aluminate nanoparticles using simple coprecipitation method in various aqueous surfactant solutions and microemulsion systems. The particles have also been synthesized by coprecipitation without surfactants and sol–gel methods for comparison purpose. Nanocrystalline powders of lithium aluminate with spherical shape were obtained upon calcination. The resultant powders were characterized by XRD, SEM, TGA and BET techniques. As per the results from X-ray diffraction (XRD), the powder prepared by coprecipitation in the presence of Tween 80 and sol–gel showed purer γ-phase when it was calcined at 950 °C. Scanning electron microscopy (SEM) results show that the type of surfactant used has a distinct effect on the size of the lithium aluminate particles. The sample prepared by microemulsion technique shows smaller average particle size of 30 nm and high surface area (70 m²/g).     

高效温和制备纳米片状β-Co(OH)2用于超级电容器电极

以水合氯化钴为原料,氢氧化钠和水合肼为碱性沉淀剂,在不添加任何分散剂的情况下采用化学沉淀法制备出呈六边形的片状β-Co(OH)_2。采用X射线衍射和透射电子显微镜表征所制样品的结构和形貌,采用循环伏安和恒电流充放电等测试方法对其电化学性能进行初步研究。结果表明,六边形片状β-Co(OH)_2边长为100~200nm,厚度为几十纳米,且随氯化钴溶液浓度的降低,单晶片的厚度逐渐减小。其表现出一定的电化学性能,电流密度为1A/g时,比电容可达到83.3F/g,且性能稳定。     

C–Co Nanocomposite Materials

The formation of cobalt particles on the surface of graphite supports via salt thermolysis is studied by x-ray diffraction, electron microscopy, Auger electron spectroscopy, and secondary ion mass spectrometry. The results demonstrate that each step in the fabrication of graphite–cobalt composites causes changes in the particle size, phase composition, and morphology of the deposit. The process involves the formation of a thin, fine-grained salt film on the surface of thermally expanded graphite particles as a result of impregnation; thermal decomposition of the salt, leading to the formation of crystalline cobalt oxide particles 50 to 100 nm in size, uniformly distributed over the surface of thermally expanded graphite; and the formation of Co particles on the graphite surface. The Co particles are 60–70 to 150 nm in size and form aggregates up to 400 nm in size.     

Polymer-Mediated Synthesis of Fine-Sized Cobalt Particles

A novel method to synthesize monodisperse, fine-sized cobalt particles (average particle size 200 nm) by a polymer matrix (not commonly known for chemical chelation)-mediated sodium borohydride reduction of cobalt chloride has been demonstrated and discussed. As against the conventional concept of using a supramolecule as a growth Poisson during the crystallization of inorganic salt from solution, the present procedure adopts the path very similar to biomineralization. The polymer matrix chelates the cobalt ions by a combined process of physical entrapment and chemical chelation. The process leads to a controlled nucleation and ordered growth of cobalt salt in polymer matrix. Orderly grown cobalt salt on reduction yields monodisperse cobalt particles having uniform size and morphology.     

Tuning of magnetic parameters in cobalt-polystyrene nanocomposites by reduction cycling

Cobalt nanoparticles were prepared by a reduction process inside polymer pores using CoSO₄·7H₂O and NaBH₄. A porous polymer network (sulphonated polystyrene) was chosen, as the template for the synthesis of elementary cobalt as high surface area cobalt nanoparticles are prone to oxidation. The preliminary studies reveal that the cobalt is first formed with an oxide protective layer outside and upon repeating the reduction cycles, inner pores of the polymers are opened which enhanced the yield of metallic cobalt. These high surface area cobalt nanoparticles embedded in a polymer are ideal for the synthesis of carbon nanotubes as cobalt can act as a catalyst for the nanotube synthesis. The concentration of cobalt can be tuned in this technique by repeating the cycling process.     

Effect of calcium lignosulfonate on tricalcium aluminate and its hydration products

In the tricalcium aluminate—calcium lignosulfonate—water system, evidence has been obtained for the formation of a complex and precipitation of a highly basic calcium lignosulfonate. The hexagonal calcium aluminate hydrate as well as the cubic aluminate hydrate irreversibly adsorb calcium lignosulfonate. Adsorption results in changes of surface area, morphology, thermal behaviour and rate of interconversions.     

纳米介孔分子筛的合成、表征与催化性能的研究

以硅酸钠为硅源、偏铝酸钠为铝源、十六烷基三甲基溴化铵为模板剂,两步水热法合成出了有序性好、热稳定性与水热稳定性高的介孔分子筛.XRD、AFM、TG、RT-IR、BET比表面和孔径测定以及热稳定性和水热稳定性研究表明:制得了粒径为30～50nm的纳米级介孔分子筛,并且所制备介孔分子筛的比表面积大于800m2/g;在1123K以上热稳定性好;100℃水热处理10天后有序性、孔径和比表面都没有明显的变化.负载Pt样品对苯加氢反应的催化性能研究表明,反应温度250℃、3.0MPa下,载Pt样品的苯加氢活性和选择性都接近100%,连续反应30h催化活性没有明显的降低.