TiO_2/竹炭复合材料研究(Ⅰ)制备与表征

以60目竹炭为载体、钛酸四正丁酯为钛源,采用溶胶-凝胶法制备了TiO2/竹炭复合材料。用XRD、SEM、EDX等分析技术对其进行了表征,并就其对罗丹明B的光降解的催化作用进行了研究。结果表明,所制备的TiO2/竹炭复合材料经过500℃绝氧烧结后,其负载的TiO2主要呈锐钛矿型结构,具有较好的紫外光催化活性。     

Growth of crystalline SiC film free of cavities by heating PS/silica sol-gel coatings on Si (111) substrate

Single crystalline 6H-SiC films were prepared by spin-coating silica and polystyrene (PS) sol-gel layers subsequently on Si (111) substrate, and then the sample heated in vacuum (10⁻³ Pa) to temperature above 1000 °C. The films were investigated by Fourier transform infrared absorption (FTIR), transmission electron diffraction (TED), X-ray diffraction (XRD), and scanning electron microscopy (SEM) measurements. Plan-view SEM observations indicated that the silica layer sandwiched by PS and Si substrate can suppress the interface cavity formation. It was proposed that the silica layer acted as a barrier of out-diffused Si atoms, and took the place of the substrate as the reservoir of Si supply to form SiC during the heat treatment.     

载银纳米TiO2抗菌竹炭的制备

以工业TiOSO4为原料,分别通过水解法和胶溶法制备载银纳米TiO2抗菌竹炭.采用XRD和SEM对样品进行了表征,研究了不同载银量、煅烧温度、TiO2/C和竹炭粒径对抗菌率的影响.结果表明,水解法制备的抗菌竹炭的抗菌效果优于胶溶法制备的抗菌竹炭,控制载银量、煅烧温度、TiO2/C、竹炭粒径分别为2%、500℃、2%、200目时,水解法制备的抗菌竹炭抗菌率最佳;控制载银量、煅烧温度、TiO2/C、竹炭粒径分别为3%、500℃、3%、200目时,胶溶法制备的抗菌竹炭抗菌率最佳.     

Influence of Preparation Technology on the Structure and Phase Composition of MoSi_2-Mo_5Si_3 /SiC Multi-coating for Carbon/Carbon Composites

Oxidation protective MoSi 2 -Mo 5 Si 3 /SiC multi-coatings for carbon/carbon composites were prepared by chemical vapor reaction and slurry-sintering method. The influence of preparation technology on the structure and phase composition of the coating was investigated by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) analyses, and then their relationship was discussed. The results indicate that the Si/Mo ratio of the slurry and sintering processing were ...     

Oxidation Protective C/SiC/Si-SiC Multilayer Coating for Carbon/Carbon Composites Applying at 1873 K

A C/SiC/Si-SiC multilayer coating for protecting carbon/carbon(C/C) composites against oxidation was prepared by slurry and pack cementation.X-ray diffraction(XRD) and energy dispersive spectroscopy(EDS) analysis showed that the inner coating obtained from the slurry and pack cementation was a C/SiC gradient layer acting as bonding layer,and the exterior coating formed in the second pack cementation was a Si-SiC double phase coating.Oxidation tests at 1873 K in air showed that the coating exhibited excellen...     

SiC空心球的制备与表征

以炭黑和粉煤灰为原料,通过微波加热碳热还原法制备了SiC空心球.制备工艺为:将粉煤灰与炭黑球模板按n(C)∶n(SiO2)=4.2配料,在1300℃氢气气氛下恒温0.5h.采用扫描电子显微镜、能谱仪、X射线衍射和拉曼光谱对SiC空心球进行了表征,结果表明,SiC空心球球壳由带有缺陷的β-SiC线组成,β-SiC线的直径为50～500nm.     

凝胶注模成型制备纳米复合多孔氮化硅陶瓷

采用凝胶注模成型两步法烧结工艺,利用纳米碳粉增强,成功地制备出了具有高强度、结构比较均匀并有较高气孔率的氮化硅多孔陶瓷。借助X射线衍射(XRD)、扫描电子显微镜(SEM)、X射线能谱(EDS)、Archimedes法和三点弯曲法等方法对多孔氮化硅陶瓷的微观结构和基本力学性能进行了研究。结果表明:在适当工艺条件下可制成平均强度>100 MPa、气孔率>60%的多孔氮化硅陶瓷。SEM照片显示气孔是由长柱状β-Si₃N₄晶搭接而成的,气孔分布均匀。XRD图谱显示有SiC生成。发育良好的柱晶结构、均匀的气孔分布以及反应生成的SiC微晶是获得高性能的主要原因。      

直流电弧等离子体制备纳米SiC及其催化特性

利用工业块体硅为硅源, CH₄为碳源, 在含有H₂和Ar混合气氛中, 采用直流电弧等离子体法制备SiC纳米粒子。CH₄含量影响SiC纳米粒子的化学组成和形貌。结果显示: 产物中含有3C-SiC和6H-SiC两种物相, 而在CH₄压力为0.005 MPa条件下制备的SiC纳米粒子还含有Si/SiC核壳结构。利用制备的SiC纳米颗粒作为催化剂, 在恒光强下光电催化还原脱除2,4-二氯酚中的Cl原子。结果显示在-1.02 V偏压下光电催化180 min后, 对2,4-二氯酚的去除效率达92.5%, SiC纳米粒子的吸附效率为19.6%。因此, SiC纳米颗粒可取代贵金属, 作为低成本光电催化候选材料用于污水处理。     

铜包覆碳化硅复合粉体材料的制备及表征

选用平均粒径约为50～100μm的碳化硅颗粒作为基料,以水合联氨为还原剂、氨水为络合剂,利用非均相成核法制备铜包覆碳化硅复合粉体材料,在温度为83℃时得到了分散效果较好的复合粉体,采用XRD、SEM、EDS对复合粉体进行了表征,结果表明,制备的铜微晶粒径为100nm左右,碳化硅颗粒表面的铜包覆层均匀、连续.     

钢渣/木炭纳微复合物的制备与电磁特性

以钢渣、木炭为原料,采用高性能球磨工艺得到具有磁-电阻复合损耗的钢渣/木炭片状纳微复合物。并用EDS、XRD、SEM、网络矢量分析仪等表征手段研究了钢渣/木炭复合物的组成、物相、形貌以及电磁特性。结果表明,钢渣/木炭复合物的电磁特性对木炭的含量呈现强烈的依赖性。随木炭含量的增大,钢渣/木炭复合物的介电常数实部和虚部显著提高。当木炭含量为50%时,钢渣/木炭复合物因其高的介电损耗和优良的匹配特性而显示最佳的吸波性能,此时最大反射率值为-33.4dB,<-10和-20dB的有效带宽分别为15.2和8.6GHz。     

模板法制备MoSi2/竹炭复合材料及吸波性能

以竹材炭化的多孔竹炭(BC)为模板,金属间化合物二硅化钼(MoSi_2)为吸收剂,采用包埋硅(Si)粉固相烧结工艺制备MoSi_2/BC多孔复合吸波材料。利用XRD、SEM和矢量网络分析仪对MoSi_2/BC复合材料的物相组成、显微结构、介电和吸波性能进行表征。结果表明:在氩气(Ar)保护气氛下,1450℃烧结制备的MoSi_2/BC复合材料主要含物相MoSi_2、SiC及无定型碳。BC基体孔隙内除分布有MoSi_2外,还布满排列无序、尺寸长短不一、相互交叉呈网状的碳化硅晶须(SiC_W),SiC_W的存在可有效提高复合材料电磁波吸收性能。在8.2～12.4GHz频率范围内,与环氧树脂混合后,复合材料反射率随MoSi_2/BC含量增加而逐渐减小。MoSi_2/BC含量为50%(质量分数)时,随试样厚度增加反射率降低,且最小反射率向高频方向移动;在11.87GHz处最低反射率为-13dB,反射损耗小于-10dB带宽约达1.0GHz,具有良好的吸波性能。     

Si(111)衬底上6H-SiC薄膜的低压化学气相外延生长与表征

在Si(111)衬底上,采用SiH4-C3H8-H2气体反应体系,通过低压化学气相沉积(LPCVD)工艺外延出结晶质量良好的SiC薄膜.低温光致发光谱表明该薄膜属于6H-SiC多型体.X射线衍射图表明该薄膜具有高度的择优取向性.扫描电子显微镜图表明该薄膜由片状SiC晶粒组成.拉曼光谱和透射电子衍射谱的结果进一步表明该薄膜具有较高的结晶质量.对Si(111)衬底上6H-SiC薄膜的生长机制进行了初步探讨.     

Study on Mechanical Behavior of CVD-SiC Coated C/SiC Composites under Simulated Space Environments

SiC coating was prepared on the surface of C/SiC composites by chemical vapor deposition (CVD) method, and then mechanical behavior of CVD-SiC coated C/SiC composites under cold and thermal cycling had been investigated. Specimens were thermally cycled between the temperatures of ?100 °C and 100 °C for up to 200 cycles, respectively. The coating was characterized by XRD, SEM and EDS. The results showed that there were no significant changes in the flexural property. CVD-SiC coated C/SiC composites had good mechanical stability in above simulated space environments. While great changes occurred on both elements and structure of the coating, from homogeneous single-phase of SiC into the inner layer of SiC and the outer of C, which caused the change of the bending strength.     

Morphological, structural and optical properties of thin SiC layer growth onto silicon by pulsed laser deposition

Crystalline silicon carbide thin layers were grown on a p-type Si(1 0 0) substrate by pulsed laser deposition (PLD) using KrF excimer laser at λ=248 nm from a 6H-SiC hot-pressed target. The target “SiC” used to elaborate our SiC films is realized from a mixture of 1SiO₂ with 3C (carbon) “1SiO₂+3C” heated in an oven at 2500 °C (the target was a hot-pressed material and supplied by Goodfellow). The morphological, structural and optical properties of SiC layers were investigated by scanning electronic microscopy (SEM), high-resolution X-ray diffraction (XRD), secondary ion mass spectrometry (SIMS) and UV-visible spectrophotometer. XRD analysis of the target showed that this latter is a hexagonal structure (6H-SiC). The XRD pattern shows that a 1.6 μm crystalline SiC layer was formed. In addition, a SIMS analysis gives a ratio Si/C of the thin SiC layer around 1.15 but the ratio Si/C of the target was found equal to 1.06, whereas one should have 1.0. This is due to the degree of the sensitivity of the SIMS technique and due to the higher ionization efficiency of Si compared to C atoms, all these which give different ratios. It is known that the PLD technique reproduces the same macroscopic property (optical, mechanical, structural, etc.) of the target. An optical gap (E_Gap) of the SiC layer of about 2.51 eV was obtained by reflectance measurement. Finally, a crystalline thin SiC layer of 1.6 μm was elaborated using PLD method at low-temperature deposition.     

化学气相反应法制备SiC涂层对C/C复合材料力学性能影响

采用化学气相反应法在C/C复合材料表面制备了SiC涂层,利用X射线衍射仪、扫描电镜及能谱等分析手段研究了涂层的形貌和结构,并采用三点弯曲试验研究了材料的力学性能,讨论了SiC涂层及制备工艺对复合材料断裂行为的影响.结果表明:涂层后材料的弯曲强度和最大断裂位移明显增大.未涂层C/C复合材料的平均弯曲强度为172.4MPa,而涂层后C/C复合材料的平均弯曲强度为239.8MPa,弯曲强度提高了39.1%.涂层试样强度的提高主要与制备过程中部分蒸气扩散渗透反应引起的界面强化及SiC颗粒的增强作用有关.此外,涂层后材料的断裂模式未发生明显转变,断裂过程中试样表现出一定的假塑性和韧性断裂特征.     

竹炭基铈掺杂氧化锌制备及催化降解亚甲基蓝

以竹粉为碳源、ZnCl₂为锌源、六水合硝酸铈(Ⅲ)(Ce(NO₃)₃·6H₂O)为铈源,采用一锅法制备得到新型竹炭负载Ce掺杂ZnO复合材料(Ce-ZnO/BC)。利用XRD、FTIR、SEM、EDS、BET、XPS、紫外-可见光漫反射光谱(DRS)及光致荧光光谱(PL)对所制备复合材料进行全面表征,并对其光催化降解有机染料性能进行了研究。获得了催化材料的最佳制备条件:ZnCl₂与竹粉浸渍比为3∶10,煅烧温度为500℃,Ce(NO₃)₃·6H₂O加入量为ZnCl₂的2.5%。所得材料分别以日光和紫外光为光源,在暗处吸附20 min,光照120 min、亚甲基蓝(MB)溶液50 mL(10 mg·L?1),催化剂用量为40 mg 条件下,对MB降解率分别为92.2%和93.7%。并且研究结果表明,其催化MB降解符合一级反应动力学原理,催化剂具有一定的重复使用性能。      

脉冲电沉积纳米SiC/Ni-Co复合镀层腐蚀特性

采用X射线衍射(XRD)、扫描电镜(SEM)、能谱分析(EDS)研究了脉冲电沉积法制备的纳米晶Ni-Co合金镀层及其纳米 SiC/Ni-Co复合镀层的组织结构、表面形貌和成分。用浸泡法和电化学极化法对比测试了纳米晶Ni-Co合金镀层和纳米 SiC/Ni-Co复合镀层在3.5 wt% NaCl和5 wt% HCl溶液中的腐蚀行为。研究结果表明：通过脉冲电沉积法制备的Ni-Co合金镀层和纳米SiC/Ni-Co复合镀层具有典型的纳米晶结构;随着纳米SiC颗粒的增加,复合镀层的晶粒尺寸减小,硬度增加。所制备的纳米SiC/Ni-Co复合镀层颗粒分散均匀,其在3.5 wt% NaCl和5 wt% HCl溶液中的耐蚀性均优于纳米晶Ni-Co合金镀层。纳米晶Ni-Co合金镀层和纳米SiC/Ni-Co复合镀层在3.5 wt% NaCl溶液中的腐蚀速率极低,表现出极好的耐腐蚀性能,而在5 wt% HCl溶液中的腐蚀形态则表现为点蚀。     

利用晶硅切割废砂浆制备SiC粉体

以光伏产业晶硅切割废砂浆为主要原料,通过真空碳化法制备了 SiC 粉末。在通过物理和化学方法测定废砂浆组分含量的基础上,确定了初始原料 Si/C 配比。随后,利用 XRD 和 SEM 分别研究了真空热处理温度、无机碳源种类等对所制备粉末的物相和组织的影响,产物粉末的粒径分布范围通过激光粒度仪测试。研究表明,在900~1100℃温度范围,随着反应温度的升高,硅粉与活性炭的碳化反应越来越完全,并在1100℃完全生成了 SiC 粉末。继续升温,X 射线衍射峰的强度逐渐升高,SiC 产物粉末的粒度越来越大。此外,不同碳源在相同条件的碳化反应结果表明,活性炭作为碳源比石墨效果更佳。     

单源热蒸发制备有机无机杂化CH3NH3PbI3薄膜及其性能表征

采用全真空单源热蒸发沉积技术直接制备钙钛矿太阳电池用有机无机杂化CH₃NH₃PbI₃薄膜。利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、能量色散谱仪(EDS)和分光光度计对制备的CH₃NH₃PbI₃薄膜微结构、表面形貌、化学成分和光学性能进行表征分析, 并与非真空旋涂法制备的CH₃NH₃PbI₃薄膜性能进行比较。结果表明: 单源热蒸发法制备的CH₃NH₃PbI₃薄膜呈现单一的钙钛矿四方晶体结构, 且与蒸发源材料的晶体结构同源性高, 没有出现杂质相偏析; 对比旋涂法制备的CH₃NH₃PbI₃薄膜表面均匀致密平整, 且薄膜结晶度更高; 单源热蒸发法制备的CH₃NH₃PbI₃薄膜禁带宽度为1.57 eV, 符合钙钛矿太阳电池吸收层光学性能要求。     

Combustion synthesis and microwave absorption property of SiC(Fe) solid solution powder under different reaction time

SiC(Fe) solid solution powders were synthesized via combustion reaction of the Si and C system in a 0.1 MPa nitrogen atmosphere using iron as the dopant and PTFE as the chemical activator, under different reaction time. The microstructures of prepared powders have been characterized by the SEM, EDS, XRD and Raman spectra, respectively. Results indicate that the prepared powders have fine spherical particles and narrow particle size distribution. The electric permittivities of SiC samples were determined in the frequency range of 8.2–12.4 GHz. Results show that the permittivity of SiC decreases with the increasing reaction time. The Fe doped SiC powder with reaction time of 45 min with 2 mm or 2.5 mm thickness exhibit the best microwave absorption properties in the X-band range(8.2–12.4 GHz). A method to predict absorbing property in the other frequency range has been presented.