爆轰合成碳包覆钴、镍磁性纳米颗粒的探索

 介绍了爆轰法合成碳包覆钴、镍纳米磁性颗粒研究的初步结果。以黑索今炸药为主体,加入钴、镍金属硝酸盐与有机碳源材料,在爆炸容器中氮气保护下用导爆管雷管引爆,成功地合成了碳包覆钴、镍纳米磁性颗粒。为了探求爆轰固体产物的形貌特征及性能,分别采用了TEM、XRD、VSM等测试手段对其进行表征。实验结果表明,爆轰产物中主要含有碳包覆纳米钴、纳米镍磁性颗粒,成球体或者椭球体,具有完好的核壳结构形貌。合成的碳包覆钴颗粒分布在30~50 nm之间,碳包覆的镍颗粒分布在25~60 nm之间,外层碳壳层主要由无定形碳和石墨构成。磁性测试表明,所得碳包金属钴、镍颗粒在室温下具有良好的软磁特性。     

气相/凝聚炸药爆轰合成的碳包铜纳米颗粒特征

采用凝聚炸药爆轰和气相爆轰分别制备碳包铜纳米颗粒,并利用XRD,Raman和TEM等方法对合成纳米产物进行对比分析。其中凝聚炸药爆轰法以柠檬酸铜干凝胶、油酸和黑索金为原料按照一定比例配成爆炸源,在氮气的保护氛围中引爆；而气相爆轰法以乙酰丙酮铜为原料,分别以H2和O2,H2和空气为爆炸源,在负氧条件下引爆。通过XRD,Raman和TEM分析结果表明,两类爆轰法均可得到分散性良好的碳包覆铜纳米颗粒,碳壳石墨化程度较高。气相爆轰可以合成10 nm以下的纳米晶粒,而凝聚炸药爆轰合成的晶粒尺寸在20~40 nm,且存在较多空壳结构；气相爆轰产物其碳壳尺寸在2~3 nm,凝聚炸药爆轰产物其碳壳尺寸在2~5 nm。     

碳包覆铁纳米颗粒的气相爆轰合成（英文）

以粉末状与气态二茂铁为原料,以氢气和氧气混合气体为爆轰能源,采用气相爆轰法进行了合成碳包覆铁纳米颗粒实验。XRD和TEM实验结果表明,采用两种不同状态的二茂铁,均得到了纳米碳包覆铁颗粒。该包覆颗粒的组成核为铁或铁碳化合物,外层壳主要由石墨碳组成,大部分球形纳米颗粒尺寸分布于5~30 nm之间。通过对比发现,采用气态二茂铁爆轰时,所得到的碳包铁粒度分布较为集中,壳层厚度比较均匀,且粒子具有较好的球形状。最后结合铁碳合金相图,从热处理角度对气相爆轰合成碳包覆铁纳米颗粒的机理进行了分析,得出产物中α-Fe与Fe_3C的形成过程。分析了碳包覆铁纳米颗粒的磁滞回线,其表现出硬磁性与顺磁性双重性质。     

碳包覆铁纳米颗粒的气相爆轰合成北大核心CSCD

以粉末状与气态二茂铁为原料,以氢气和氧气混合气体为爆轰能源,采用气相爆轰法进行了合成碳包覆铁纳米颗粒实验。XRD和TEM实验结果表明,采用两种不同状态的二茂铁,均得到了纳米碳包覆铁颗粒。该包覆颗粒的组成核为铁或铁碳化合物,外层壳主要由石墨碳组成,大部分球形纳米颗粒尺寸分布于5-30 nm之间。通过对比发现,采用气态二茂铁爆轰时,所得到的碳包铁粒度分布较为集中,壳层厚度比较均匀,且粒子具有较好的球形状。最后结合铁碳合金相图,从热处理角度对气相爆轰合成碳包覆铁纳米颗粒的机理进行了分析,得出产物中α-Fe与Fe_3C的形成过程。分析了碳包覆铁纳米颗粒的磁滞回线,其表现出硬磁性与顺磁性双重性质。     

爆轰合成氧化亚铁掺杂的二氧化硅包覆铁纳米颗粒

用一定比例的硝酸铁盐、硅酸钠盐、无水乙醇与黑索金混合制成塑性炸药。在密闭容器中以氩气为保护气,通过爆轰合成氧化亚铁掺杂的二氧化硅包覆铁纳米颗粒。采用X射线衍射(XRD)、透射电镜(TEM)及振动样品磁强计(VSM)对爆轰产物的组成成分、形态结构以及磁性进行测试。实验结果表明,爆轰产物以金属颗粒为核、二氧化硅为包覆层的壳/核结构形式出现,颗粒尺寸在60nm左右。通过分析爆轰产物的磁性曲线可知,在室温下爆轰产物具有较高的剩磁比和矫顽力,表现出弱的铁磁性,是优良的储磁材料。     

初始温度及碳源对碳纳米管气相爆轰法合成的影响

改变初始温度以及分别使用甲烷和乙炔气体作碳源时气相爆轰合成碳纳米管,研究了初始温度与不同碳源对碳纳米管的影响。利用X射线衍射(XRD)、透射电镜(TEM)、拉曼(Raman)光谱等对碳纳米管进行表征。结果表明,随着初始温度的升高,所合成的碳纳米管的产量减少且石墨化程度降低,但管壁会变得光滑且管径有所增加。当使用乙炔时,所合成的产物中没有碳纳米管,而是合成了石墨化程度较高的无定形碳,随着催化剂量的增加,产物中碳包覆颗粒增多且包覆层清晰可见,但存在结构缺陷。当初始温度在110~130 ℃时,使用甲烷气体运用气相爆轰的手段是合成碳纳米管的较佳方案。     

二茂铁质量对气相爆轰法合成碳纳米管的影响

以甲烷和氧气作为爆源,二茂铁为前驱体,探究了不同前驱体质量对所合成的碳纳米管的影响。利用X射线衍射(XRD)、透射电子显微镜(TEM)、高分辨透射电子显微镜(HRTEM)等手段对碳纳米管的形貌和结构进行表征,结果发现:当二茂铁量较少时,只有碳包覆铁纳米颗粒存在;随着二茂铁质量的增加,逐渐有碳纳米管生成,其管径大多分布在10~50nm之间,为多壁碳纳米短管。随着前驱体质量的增加,碳纳米管的石墨化程度提高,结构缺陷也变少。通过对合成产物的热重分析可得,气相爆轰法所制备的碳纳米管具有强烈吸氧性,所得样品中碳纳米管的质量分数为26%左右。     

炸药爆轰法制备纳米石墨粉及其在高压合成金刚石中的应用

介绍了一种制备纳米石墨粉的新方法——负氧平衡炸药爆轰法. 对合成的黑粉产物进行x射线衍射分析，确认其为石墨结构，平均晶粒度为2.58 nm. 透射电子显微分析的结果表明，炸药爆轰法制备的黑粉为六方结构的纳米石墨粉，颗粒呈球形或椭球形. 用小角x射线散射法测定纳米石墨粉的粒度分布在1—50 nm，有92.6wt%的粉末粒度小于16 nm. 平均粒径为8.9 nm. 纳米石墨粉的比表面积约为500—650 m²/g. 在六面顶压机中用纳米石墨粉在Fe粉触媒的作用下进行金刚石的高压合成实验 关键词： 纳米石墨粉 爆轰 金刚石 合成     

氧气浓度对气相爆轰合成纳米碳球的影响

以氧气和苯为反应物,采用气相爆轰法制备纳米碳球是一种新兴的碳纳米材料的制备方法,通过X射线衍射(XRD)进行物相分析,并通过透射电镜(TEM)进行形貌分析,观察了产物的晶粒大小。结果表明,纳米碳球的尺寸在30~50nm之间,随着氧气浓度的增加,产物晶粒尺寸变小,分散性也变好,团聚程度降低。同时发现,反应物的初始浓度对气相爆轰合成纳米材料有重要影响。此外,还对气相爆轰合成纳米碳球的形成机理进行了讨论。     

气相爆轰法合成含铁多壁碳纳米管

以甲烷和氧气为前驱体,二茂铁为催化剂,采用气相爆轰法在密闭反应管中合成多壁碳纳米管。运用X射线衍射(XRD)、透射电子显微镜、Raman光谱等手段对多壁碳纳米管进行形貌表征和物相、成分分析。结果表明:所制备的多壁碳纳米管呈弯曲缠绕状,管径分布在20~50nm,长度达数微米,具有优异的管状结构,并且石墨化程度较高;碳纳米管中除含碳元素外,还包含少量纳米铁颗粒,且产物中含有少量碳化铁。XRD分析表明,爆轰反应发生后催化剂被分解、还原为金属单质。根据实验结果和理论分析,提出了气相爆轰法合成碳纳米管的机理。     

炸药爆轰法制备的纳米石墨粉的拉曼光谱

负氧平衡炸药爆轰法合成的纳米石墨粉,是一种新型的具有良好实用前景的纳米粉体材料。采用负氧平衡炸药梯恩梯(TNT),在分别充有氮气、氩气、二氧化碳等保护性气体、压力为0.25～2 atm的密闭容器内爆轰制备了纳米石墨粉。用激光拉曼光谱对制备的样品进行了测试,结果表明样品为石墨结构。纳米石墨粉的Raman峰与块体石墨相比,其峰位向高波数方向偏移了约5 cm-1。纳米石墨粉Raman峰的半高宽约为22 cm-1,由此可计算出纳米石墨粉的颗粒大小为2.97～3.97 nm。与高纯石墨Raman峰相比,纳米石墨粉的Raman峰由于尺寸效应出现了蓝移现象, 并对此现象进行了讨论。用X射线衍射仪(XRD)和透射电子显微镜(TEM)测定了纳米石墨粉的物相,并对其颗粒粒径进行了估算,其结果为2.58 nm(酸处理前)和1.86 nm(酸处理后),与Raman光谱的结果基本吻合。     

Synthesis and Characterization of Ag@TiO2 Core-shell Nanoparticles and TiO2 Nanobubbles

Ag@TiO₂ core-shell structured particles of nano-size dimensions have been successfully prepared via a one-step way, which has proved quite effective in procuring stable colloids. Transmission electron microscopy (TEM) was employed to characterize the core size and the shell thickness, which typically were 20~40 nm and ~2 nm, respectively. X-ray diffraction (XRD) indicated the existence of silver. Optical absorption dependence on core size and synthetic temperature has been explored by UV–Vis absorption spectroscopy. Finally, the interesting titanium dioxide nanobubbles with silver core leached out by a unique means, were studied, which consequently proved the core-shell structure of the prepared nanoparticles, confirming the TEM observation.     

Preparation and magnetic property of the composite of nitrogen-doped carbon nanotubes decorated with nickel nanoparticles

A magnetic composite of nitrogen-doped carbon nanotubes (CN_x) decorated with nickel nanoparticles was synthesized by a chemical precipitation and deoxidization method. The decorated CN_x were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). The XRD pattern showed that CN_x, nickel nanoparticles and little nickel oxides coexisted in the composite, TEM observation indicated that nickel nanoparticles were highly dispersed on the outer walls of CN_x, Magnetic measurements by VSM demonstrated that the saturated magnetization and remanence of CN_x were improved, while the coercivity was lowered after decorating with nickel nanoparticles.     

不同前驱体相对摩尔量对气相爆燃制备纳米SiO2的影响

 以SiCl₄为前驱体,以空气和氢气的混合气体为爆源,通过改变前驱体的相对摩尔量,考察前驱体的相对摩尔量对产物的影响。通过X射线荧光谱（XRF）、透射电子显微镜（TEM）和X射线衍射（XRD）等测试手段对纳米SiO₂粉体进行表征及分析。通过XRF对产物进行成分分析,测得实验所得产物主要由SiO₂组成,且纯度达到99.9%以上;由XRD分析得知,生成的SiO₂产物属于典型的非晶态结构;由TEM图像可以看出,随着前驱体相对摩尔量的增加,所得到的产物粒子逐渐出现粘结,分散性下降,前驱体相对摩尔比应该控制在1.5以内。     

One-pot synthesis of one-dimensional array Pt nanoparticles on carbon nanotubes via a facile microwave polyol method

High-density attachment and one-dimensional array Pt nanoparticles (NPs) on carbon nanotubes (CNTs) to generate Pt/CNTs heterostructures are obtained via one-pot microwave polyol method. The morphology, composition of as-obtained Pt/CNTs heterostructures is characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD). The Raman spectrum and Fourier transform infrared (FTIR) spectrum show the introduction of defects or functional groups on CNTs surface, which are crucial factors to assist the nucleation and growth of Pt NPs along the skeleton of CNTs.     

Surfactant assisted surface studies of zinc sulfide nanoparticles

We report a simple soft chemical method for the synthesis of ZnS nanoparticles using varying concentration of cationic surfactant CTAB and examine its surface properties. Powder X-ray diffraction, UV-vis spectroscopy, photoluminescence spectroscopy, selective area electron diffraction, and transmission electron microscopy are used to characterize the as prepared ZnS nanoparticles. XRD and TEM measurements show the size of polydispersed ZnS nanoparticles is in the range of 2-5 nm with cubic phase structure. The photoluminescence spectrum of ZnS nanoparticles exhibits four fluorescence emission peaks centered at 387 nm, 412 nm, 489 nm and 528 nm showing the application potential for the optical devices. In Raman spectra of ZnS nanoparticles, the modes around 320, 615 and 700 cm⁻¹ are observed.     

Facile synthesis and photocatalytic activity of hierarchical WO3 core–shell microspheres

In this work, we present a facile template-free precipitation method for the large-scale preparation of hierarchical WO₃ core–shell microspheres in which the core was composed of aggregated nanoparticles encapsulated by a hierarchical shell layer self-assembled by ultrafine nanoplates with a thickness of about 15 nm. The products are characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), differential scanning calorimetry and thermogravimetry (TG/DSC). The experimental parameters affecting the morphology were discussed in detail. We found that the concentration of citric acid and pH value of the reaction solution had profound effects on the morphology of the products. In addition, a formation mechanism was proposed for producing hierarchical WO₃ core–shell microspheres. Furthermore, the obtained hierarchical WO₃ core–shell microspheres showed superior photocatalytic activities for the degradation of rhodamine B (RhB) under visible light irradiation.     

Functional multi-walled carbon nanotube/polysiloxane composite films as supports of PtNi alloy nanoparticles for methanol electro-oxidation

We demonstrate the use of molecular monolayers to enhance the nucleation of electrocatalytically active PtNi alloy nanoparticles onto the multi-walled carbon nanotubes (MWCNTs). After the siloxane was polymerized on the nanotube surfaces, the carbon nanotubes were embedded within the polysiloxane shell with a hydrophilic amino group situated outside. Subsequent deposition of PtNi nanoparticles led to high density of 3-10 nm diameter PtNi alloy nanoparticles uniformly deposited along the length of the carbon nanotubes. The presence of MWCNTs and PtNi in the composite films was confirmed by transmission electron microscopy (TEM), X-ray diffraction (XRD) and energy dispersion X-ray spectra analysis (EDS). The electrocatalytic activity of the PtNi-modified MWCNT/polysiloxane (PtNi/Si-MWCNT) composite electrode for electro-oxidation of methanol was investigated by cyclic voltammetry (CV), and excellent electrocatalytic activity can be observed.