稀释气体对化学气相沉积SiC涂层生长行为的影响

以CH3SiCl3-H2为反应气体,采用Ar和H2作为稀释气体。在1100℃、负压条件下,由化学气相沉积制备了SiC涂层,研究了稀释气体对涂层沉积速率、形貌以及晶体结构的影响。以Ar为稀释气体时,随着稀释气体流量的增加沉积速率迅速减小;用Ar作稀释气体制备的SiC涂层相对粗糙,随着Ar流量的增加,晶粒簇之间的空隙较大,涂层变得疏松。XRD分析表明：当稀释气体Ar流量超过200ml／min时,涂层中除了β-SiC外,还逐渐出现了少量的α-SiC。以H2为稀释气体时,当H2流量增加到400ml／min时,涂层的沉积速率迅速增大;以H2为稀释气体制备的SiC涂层致密、光滑,沉积的SiC涂层全部是β-SiC,且具有非常强的(111)晶面取向,涂层中无α-SiC出现。     

沉积条件对CVD法SiC涂层形貌和组成成分的影响

采用MTS-H2-Ar体系通过等温化学气相沉积(CVD)在石墨基底表面沉积了SiC涂层。研究了沉积温度、气体总压和气体流量对涂层形貌和组成成分的影响。SEM和AFM观察表明,SiC一次颗粒尺寸在100nm以内。在本实验的沉积条件变化范围内,Ar流量增大使涂层表面变粗糙,温度升高使涂层变厚。X射线衍射和拉曼光谱分析显示沉积物主要为3C型的β-SiC。气体总压和H2流量都增大时易生成游离Si。气体总压较小而H2流量较大时易生成游离C。当气体总压为5kPa,H2流量为500mL·min-1时可得到化学计量比的SiC。     

CVD沉积工艺对SiC涂层结晶度与耐腐蚀性能的影响

通过化学气相沉积(CVD)SiC涂层来提高SiC_f/SiC复合材料的耐腐蚀性能,本文以CH_3SiCl_3(MTS)为源气体,在反应烧结SiC基体上制备SiC涂层,控制沉积温度、炉压及H_2/MTS摩尔比等工艺参数,通过X射线衍射实验(XRD)得到不同工艺条件下生成的碳化硅涂层的物相组成和结晶度,通过高温水腐蚀实验检测涂层的耐腐蚀性,并利用扫描电子显微镜(SEM)观察腐蚀前后的表面形貌。结果表明:当沉积时间为8 h,沉积温度从1050℃到1250℃,β-SiC涂层表面平整性提高,沉积厚度由12.97μm急剧增加至71.10μm, SiC晶粒尺寸逐渐增大,最终呈金字塔状;碳化硅涂层腐蚀60 d后,表面呈现针状结构,1250℃下沉积的SiC涂层耐腐蚀性能较好;β-SiC涂层的晶粒尺寸随沉积炉压的增大而增大,结晶度随沉积炉压增大而减小,在200 Pa以下,获得的β-SiC晶粒的结晶度最高(81.08%)、晶粒尺寸最小(13.7 nm);随着H_2/MTS摩尔比增加,β-SiC晶粒结晶度迅速下降,当H_2/MTS=6.5时,结晶度最高(95.91%)。     

炭纤维表面用化学气相沉积法涂覆碳化硼的研究

以CH4，BCl3，H2为原料气，采用化学气相沉积法(常压CVD)在炭纤维表面连续涂覆B4C，通过正交实验得到最佳涂覆条件；采用IR、TG—DTA、XRD等技术考察了涂层的组成、结构和形貌，并对最佳涂覆条件下炭纤维的拉伸强度进行测试。实验结果表明：当υH2／υBCl3=3．5、υBCl1／υCH4=1．7、气体总流速=160mL／min，沉积温度1100℃，走丝速度5转／min时，涂层表面有明显的一层致密物质，表面较平整，涂层纤维的氧化温度由未涂层时的350℃提高到630℃，纤维的单丝强度由未涂层时的1．93GPa提高到3．15GPa。在炭纤维表面采用化学气相沉积法涂覆B4C不仅装置简单、操作方便，而且可以明显地提高炭纤维的抗热氧化性和单丝强度。     

C/SiC复合材料表面化学气相沉积涂覆SiC涂层及其抗氧化性能

采用化学气相沉积法,在1 100 ℃,在碳纤维增强碳化硅复合材料表面制备SiC涂层,研究了涂层连续沉积和分4次沉积(每次沉积时间为6 h)所制备的SiC涂层的微观结构和涂层样品的氧化性能.结果表明:两种SiC涂层的厚度均约为40 μm,且4次沉积制备的SiC涂层为一个连续的整体.涂层连续沉积时,表面只出现裸露裂纹;分4次沉积制备时,表面出现大量边缘有SiC生长锥的附着裂纹,附着裂纹在高温氧化时易发生自愈合.与连续涂层样品相比,4次涂层能显著提高C/SiC样品的抗氧化性能.4次涂层样品经1 400 ℃,50 h氧化后,质量损失为0.88%,质量损失速率稳定在6.30 × 10-5 g/(cm2?h),且4次涂层样品具有优异的抗热震性能.     

堇青石基体化学气相沉积碳化硅薄膜及其性能表征

采用等温等压化学气相沉积技术,分别以CH3SiCl3-H2和SiCl4-CH4-H2为气源,在沉积温度1100和1000℃、压力101 kPa条件下,制备了SiC薄膜. 利用SEM和XRD、显微拉曼光谱、EDAX元素分析、HRTEM等测试技术对沉积薄膜的结构和组成进行了表征. 结果表明,1100℃时,以CH3SiCl3-H2为气源沉积得到纯净的SiC薄膜,以b-SiC (111)面择优定向生长,由微米级的金字塔锥形结构组成,硅含量随着沉积温度降低而增加;以SiCl4-CH4-H2为气源沉积得到非晶态碳掺杂的SiC薄膜,碳含量随着沉积温度降低而增加. 此外,以CH3SiCl3-H2为气源沉积的SiC颗粒平均粒径均比以SiCl4-CH4-H2为气源的粒径大. 前者SiC薄膜的方块电阻在kW级以上,且随着沉积温度的下降急剧升高;后者1100℃时制备的薄膜的方块电阻在kW级以上,且随着沉积温度的降低而急剧下降,1000℃时降低到W级.     

电泳沉积-烧结两步法制备C/SiC复合材料

采用电泳沉积法在石墨基体上制备厚度可控的Si涂层,考察了电泳沉积参数(电压、沉积时间、固含量及添加剂量)对涂层沉积量的影响。所制备的Si涂层通过烧结与石墨基体发生在位反应形成SiC涂层。涂层成分的XRD分析表明烧结后生成β-SiC。用SEM观察涂层烧结前后的形貌,烧结后Si渗入基体内部。孔径分布数据表明所形成的SiC涂层导致石墨孔径变小。1200℃的抗氧化实验表明涂层起到了良好的防护作用。实验提供了一种制备C/SiC复合材料的新方法。     

氧化铝陶瓷表面化学气相沉积钛涂层的制备及性能

利用卤化物还原原理,以Ti粉和I2粉为反应原料,通过化学气相沉积的方法在Al2O3陶瓷基体上制备了金属Ti涂层。考察了原料配比、加热温度及保温时间等工艺参数对涂层沉积的影响。通过X射线衍射仪分析了涂层的物相组成。利用扫描电子显微镜及能谱仪对涂层的微观组织形貌及成分进行了分析。采用座滴法考察铜与沉积了涂层的氧化铝陶瓷间的润湿性。研究结果表明,化学气相沉积法在氧化铝陶瓷表面制备Ti涂层的适宜工艺参数为:Ti与I2的质量比=1∶3,沉积温度为1 100℃,沉积时间为60min。所获得的Ti涂层纯度较高,具有明显的(110)晶面择优取向性,涂层与陶瓷结合良好。铜与涂层间的润湿角在1 113℃时为57°。     

石墨表面CVD氮化硅涂层的制备与抗氧化研究

采用化学气相沉积法，以SiCl₄-NH₃-H₂为先驱体气体和载气，在等静压石墨表面制备了氮化硅涂层，沉积温度900～1 300℃,沉积压力1 000 Pa,并在600～1 000℃进行了空气气氛静态氧化实验。X射线衍射结果表明，900℃和1 100℃沉积的氮化硅为非结晶态，1 300℃沉积的为结晶的α-Si₃N₄。氧化增重结果表明，900～1 300℃沉积的涂层，对石墨氧化均有明显的防护作用，其中，1 100℃涂层防护效果最好，900℃涂层防护效果最差。采用SEM对氧化前后的涂层表面进行了观察，900℃涂层在800℃或更高温度的空气气氛中发生了明显的氧化现象；1 100℃和1 300℃涂层即使在1 000℃下也未发生明显的氧化现象。基底的氧化由涂层开裂导致，且α-Si₃N₄结晶涂层开裂更显著。     

工艺因素对水热电泳沉积硅酸钇涂层显微结构的影响

采用水热电泳沉积法在C/C-SiC复合材料表面制备了硅酸钇抗氧化外涂层.研究了沉积电流密度和低温热处理对硅酸钇涂层的影响.采用X-射线衍射仪(XRD)和扫描电子显微镜(SEM)对涂层的相组成和显微结构进行了表征.结果表明:采用声化学法制备的硅酸钇微晶颗粒尺寸为25～40nm.随着沉积电流密度增加,硅酸钇涂层均匀性、致密性先逐渐增加后降低.当电流密度超过0.04 A/cm2时会导致涂层表面开裂.进行低温热处理,涂层表面硅酸钇纳米晶出现熔融现象;随热处理温度增加,涂层表面呈现玻璃化趋势.当热处理温度达1200℃时,表面完全熔融,形成致密的硅酸钇玻璃层.涂层在1500℃静态空气中,经过氧化10 h后,失重仍然小于2%.     

Determination of the nitrogen compound balance between the atmosphere and a Norway spruce forest ecosystem

Wet, throughfall and stemflow deposition measurements of nitrogen compounds (NH₄ ⁺- and NO₃ ^–-ions) were carried out in a Norway spruce forest in Hungary, together with direct dry deposition and emission estimates (NH₃, NO, NO₂, HNO₃, N₂O gases, NH₄ ⁺ and NO₃ ^– particles). The total deposition of nitrogen compounds from the atmosphere to the forest ecosystem, estimated as the sum of the wet deposition and the measured dry flux, was 1.9 g N m^–2 yr^–1 for the examined period (1996–1998). The net deposition (difference of the deposition and the emission) was 1.8 g N m^–2 yr^–1. About 61% of the deposition is due to dry deposition processes. Ammonia gas dominates in the dry deposition (48%). Soil emission of nitric oxide (NO) and nitrous oxide (N₂O) constitutes only 5% of the total (wet and dry) deposition. From the comparison of directly measured dry deposition figures and the dry deposition calculated as the difference of the throughfall plus stemflow and wet deposition, it is probable that around 60% of the dry deposited nitrogen compounds (36% of the total, dry and wet deposition) are taken up by stomata, mostly in gaseous form. The remaining part (64%) of the deposited nitrogen compounds is leached to the ground where it is partly taken up by the root system, takes part in the soil mineralisation processes, or leaves the ecosystem by ground or surface water run-off.     

Controllable growth of aluminum nanorods using physical vapor deposition

This letter proposes and experimentally demonstrates that oxygen, through action as a surfactant, enables the growth of aluminum nanorods using physical vapor deposition. Based on the mechanism through which oxygen acts, the authors show that the diameter of aluminum nanorods can be controlled from 50 to 500 nm by varying the amount of oxygen present, through modulating the vacuum level, and by varying the substrate temperature. When grown under medium vacuum, the nanorods are in the form of an aluminum metal - aluminum oxide core-shell. The thickness of the oxide shell is ~2 nm as grown and is stable when maintained in ambient for 30 days or annealed in air at 475 K for 1 day. As annealing temperature is increased, the nanorod morphology remains stable while the ratio of oxide shell to metallic core increases, resulting in a fully aluminum oxide nanorod at 1,475 K.     

热油管道最佳蜡沉积厚度研究

热油管道输送含蜡油在管壁出现蜡沉积时,往往频繁使用清防蜡剂或者清管器清管手段予以清除。但是在管道建设初期和运营后期,实际输量小于设计输量,在管壁形成一定厚度的蜡沉积反而有益于提升输送效益。通过分析热油管道蜡沉积前后总传热系数和轴向温降的变化,给出了蜡沉积前后温降计算、经济效益评估、允许最小输量计算等公式。为定量分析蜡沉积最优厚度提供了理论依据,对不同管道确定蜡沉积厚度具有指导意义。     

电化学方法制备生物活性陶瓷

生物活性陶瓷因其优良的生物相容性,广泛应用于临床医学领域。电化学方法开创制备生物活性磷酸钙陶瓷新途径,由于操作简单、条件可控等多方面的优点日益引起重视。介绍了电化学方法制备生物活性磷酸钙陶瓷的原理、工艺进展;讨论了电化学制备方法的特点、影响因素和发展前景。     

Anodic, cathodic and cyclic voltammetric deposition of ruthenium oxides from aqueous RuCl3 solutions

Anodic, cathodic and cyclic voltammetric (CV) deposition of ruthenium oxides from aqueous RuCl₃ solutions have been investigated using stationary and rotating disk electrodes (RDE) in this work. The CV deposition behavior was examined using a RDE to differentiate the contribution of current from the reactions of ruthenium ions in the electrolyte and ruthenium oxides already adsorbed on the electrode. The results indicate that the CV growth of ruthenium oxides within the potential range of aqueous electrolyte decomposition is attributed to the anodic oxidation of ruthenium ions in the electrolyte. Cathodic deposition occurs only at potential negative than −0.30 V versus saturated calomel electrode (SCE) when H₂ evolves on the electrodes. Anodic deposition of ruthenium oxides can be obtained effectively in the potential range of ca. 0.9-1.1 V versus SCE, depending on the pH value of the electrolyte. The optimum anodic and cathodic deposition potential for maximum deposition efficiency is 1.0 and −0.9 V versus SCE, respectively, in the electrolyte solution of pH 2.     

Fabrication of TiO2‒Ag nanocomposite thin films via one-step gas-phase deposition

In this work, TiO₂‒Ag nanocomposite thin films were fabricated for the first time via simultaneous plasma-enhanced chemical vapor deposition and physical vapor deposition of TiO₂ and Ag nanoparticles in the gas-phase, respectively. The presence of Ag nanoparticles in the prepared nanocomposites has been confirmed using transmission electron microscopy and energy dispersive X-ray spectrometry techniques. The obtained electron microscopy images showed that the average size of TiO₂‒Ag nanoparticles was larger than that of pristine TiO₂. Moreover, the temperature of the anatase transformation into the rutile phase was decreased due to the presence of Ag nanoparticles in the TiO₂ matrix, while the photocatalytic activity of the produced nanocomposite (estimated by studying the degradation of methylene blue aqueous solution under UV irradiation) was 35% greater than that of pristine TiO₂. Therefore, the addition of Ag nanoparticles into the TiO₂ matrix significantly affected the morphology, phase transformation temperature, and photocatalytic performance of the fabricated material.     

等离子体增强化学气相沉积法制备氢化硅膜的自晶化倾向性

为了探寻生长过程中硅膜的自晶化沉积,采用等离子体增强化学气相沉积(PECVD)法沉积了氢化硅薄膜,系统研究了不同沉积阶段所得硅膜微观结构的迁变规律。结果表明,硅膜的显微结构依赖于沉积时间,当沉积时间仅为30min时,所得硅膜的结构为非晶;而当沉积时间延至60min时,硅膜形成微晶颗粒;此后随着沉积时间的增加,晶化程度提高,且非晶区域面积相应减小。另外,硅膜的沉积速率也随沉积时间的增加而增加。在硅膜沉积过程中,随时间不断变化的界面状态可能为其自晶化的主要原因。     

化学沉积纳米晶Co-P合金及其沉积速率影响因素的研究

化学沉积可得到均匀、致密的纳米晶薄膜,是一种较为理想的纳米晶制备方法。采用正交实验优化了化学沉积纳米晶钴磷合金的工艺配方,研究了正交实验5因素如硫酸钴、柠檬酸三钠、硼酸、次磷酸钠和温度及负载因子、沉积时间对沉积速度的影响。研究获得的优化工艺配方和参数为:0 06～0 12mol/LCoSO4·7H2O,0 40～0 55mol/LNaH2PO2·H2O,0 15～0 3mol/LNa3C6H5O7·2H2O,0 3～0 6mol/LH3BO3,50～80℃,负载因子0 4～0 8dm2/L。     

自泳涂料与自泳涂装技术

简要介绍了自泳涂料与自泳涂装技术，分析了自泳涂装的优缺点。     

Role of TiO2 nanoparticles in the dry deposition of NiO micro-sized particles at room temperature

A room-temperature dry-deposition method with TiO₂ powder was used to deposit NiO particles onto a fluorine-doped tin oxide (FTO) substrate. Initially, in the absence of TiO₂ powder, we observed that the NiO particles did not adhere to the substrate; however, the addition of TiO₂ particles facilitated NiO deposition. The volume percentage (vol%) deposition of NiO particles increased with the TiO₂ particle concentration. The inability of the NiO particles to adhere to the FTO substrate was attributed to the absence of deformation and fragmentation in the substrate. This is related to the lower hardness of the FTO substrate, compared with that of the NiO particles. However, the addition of the TiO₂ particles at different vol% during NiO deposition induced deposition, possibly due to the lower hardness of the TiO₂ particles compared with the FTO substrate. The minimum TiO₂ fraction that enabled NiO powder deposition was ~4.8 vol%. Microstructural analysis revealed that TiO₂ powder agglomerates tended to break up as the NiO particles impacted the substrate surface, creating a “deposition complement” from the excess kinetic energy. The deposition mechanism was investigated using microstructural analysis, electron probe microanalysis, and Brunauer–Emmett–Teller (BET) measurements; the results confirmed the influence of the TiO₂ powders on NiO powder deposition, specifically, an improvement in the adhesion and density of the NiO powder and a decrease in the surface roughness of the coating. Therefore, we demonstrated NiO deposition with TiO₂ particles at room temperature, providing potential applications to the supercapacitor and battery industries.