锌镀层硅酸盐钝化膜的耐腐蚀性能

为了考察锌镀层硅酸盐钝化膜的耐腐蚀性能,通过中性盐雾试验、3%CuSO4点滴试验对比研究了锌镀层、硅酸盐钝化膜及低铬酸盐钝化膜的耐腐蚀性能,并用极化曲线电化学测试方法研究了硅酸盐钝化膜的电化学性能。结果表明:硅酸盐钝化膜明显提高了锌镀层的耐腐蚀性能,其耐蚀性优于低铬酸盐钝化膜;硅酸盐钝化膜也明显提高了锌镀层的自腐蚀电位,有效地控制了其腐蚀的电化学过程,属阳极控制型。锌镀层硅酸盐钝化膜具有较高的耐蚀性能。     

混合稀土-三聚磷酸盐复合钝化膜的组构、耐蚀性能及机理

为了提高无铬钝化膜的性能,对A3钢镀锌后,以混合稀土与三聚磷酸盐为钝化液进行复合钝化,通过中性盐雾、盐水浸泡法考察了复合钝化膜的耐腐蚀性能,分析了其成膜机理;通过X射线光电子能谱测试了复合钝化膜的组成元素。结果表明:复合钝化膜能够有效地提高镀锌层的耐腐蚀性能,且耐腐蚀性能优于低铬酸钝化膜;复合钝化膜主要由稀土元素,P,O组成,其主要组成物为稀土硫酸盐、稀土多磷酸盐。     

高耐腐蚀性三价铬彩色钝化膜制备工艺优化及膜层性能研究

为进一步提高三价铬彩色钝化膜的性能,在无机钝化液中加入有机硅树脂,制备了一种新型高耐蚀性能三价铬彩色钝化液。该钝化液可以在镀锌板表面形成有机-无机复合钝化膜,通过红外光谱仪分析钝化膜结构,采用扫描电镜观察钝化膜微观形貌,用能谱仪分析钝化膜的微观组成,采用电化学试验、中性盐雾试验对钝化膜耐蚀性能进行表征。以正交试验对三价铬彩色钝化液组分进行了优选,以单因素试验研究了钝化温度、钝化液pH值、钝化时间等钝化条件对钝化膜耐腐蚀性能的影响。结果表明:最佳钝化液成分为硫酸铬10.00 g/L,硅树脂12.50 g/L,硝酸钠4.00 g/L,硝酸镍1.25 g/L,氯化钠2.00 g/L;最佳钝化条件为温度30℃,时间150 s,pH值1.8;以最优条件制得的钝化膜色彩鲜艳,耐蚀性能突出,耐中性盐雾腐蚀时间达196 h。     

热浸锌层植酸/硅烷复合钝化膜及其耐蚀性能

为了研制热浸锌层表面高耐蚀、绿色环保的无铬钝化工艺,对热浸锌板进行植酸钝化、硅烷钝化和植酸/硅烷两步复合钝化。采用正交试验和单因素试验对复合钝化工艺进行了优化;采用Tafel曲线、盐雾试验及硫酸铜点滴试验分析复合钝化膜的耐蚀性能,利用场发射扫描电镜(FESEM)观察了钝化膜的表面形貌,通过EDS分析钝化膜的成分,并提出复合钝化膜的结构模型。结果表明:植酸膜与硅烷膜通过"交联-协同作用"在热浸锌表面形成一层致密的保护膜层,较单一钝化膜更致密,耐蚀性能与三价铬钝化膜相当;经植酸/硅烷复合钝化处理后,锌表面生成的钝化膜层阻碍O_2和电子在锌表面和溶液之间的转移和传递,改变了界面反应历程,从而提高了阴极极化,改善了复合钝化膜的耐腐蚀性能。     

碳钢表面铈盐钝化膜和铈盐-硅烷复合钝化膜的耐蚀性能

碳钢常规铈盐钝化膜的耐蚀性不够理想。以硝酸铈和过氧化氢配制钝化液,通过化学浸泡处理,在Q235碳钢表面制备铈盐钝化膜;通过KH-560硅烷偶联剂对铈盐钝化件进行二次封孔处理,制备了铈盐-硅烷复合钝化膜;对2种钝化膜试样进行了NSS,EIS,SEM和EDS测试。试验结果显示,铈盐钝化膜明显提高了基材的耐蚀性能,但是钝化膜表面存在一些微孔和裂缝,对其耐蚀性能造成不利影响;而硅烷膜能够完整覆盖和填充铈盐钝化膜表面的缝隙和微孔,改善了铈盐钝化膜的耐蚀性能。     

Cr(Ⅲ)热浸镀锌钝化液的研究

由于Cr(Ⅵ)对环境有不利影响,因此寻找不合Cr(Ⅵ)的钝化液非常重要.研究在连续热浸镀锌钝化液中以Cr(Ⅲ)、铈、钴替代Cr(Ⅵ),钝化液通过辊涂和烘干处理工艺得到钝化膜.试验通过电化学方法研究钝化膜的抗腐蚀行为.SEM形貌观察发现,所获得的钝化膜较Cr(Ⅵ)钝化膜具有更加致密的表面膜层,SiO2在膜层结构中阻碍了微裂纹的扩展,提高了膜层抗形变性能;电化学极化曲线研究表明,铈、钴抑制了阳极极化腐蚀过程;盐雾试验结果表明,复合钝化膜较传统钝化膜具有更好的抗蚀性能.钝化膜的膜附着量达70-80 mg/m2,试样出现锈蚀的时间可以达到192 h,试验色差为1.5.     

新型奥氏体耐热钢钝化膜的XPS谱研究

为了比较新型耐热钢CHDG-A钝化处理前后的耐腐蚀性能,以及研究钝化膜的组成,采用6％FeCl3溶液浸泡法研究了3种不同表面粗糙度的CHDG-A合金试样的抗点蚀能力,并用X射线光电子能谱(XPS)研究了经硝酸钝化后合金表面钝化膜的主要成分.结果表明:表面粗糙度越大,合金的抗点蚀性能越差,而经过硝酸钝化后耐蚀性能大幅提高;钝化膜表面的主要成分是CrO3、Cr2O3、Fe2O3等氧化物,钝化膜内部主要为Cr2O3 Fe3O4、Cr单质、Fe单质、Ni单质等,Cr、Ni单质的存在有利于提高钝化膜的稳定性.     

稀土铈对镀锌层三价铬彩色钝化膜的影响

为了提高镀锌层三价铬彩色钝化膜的性能,通过单因素试验和对比分析的方法研究了稀土铈盐对三价铬彩色钝化膜的影响。研究发现在三价铬彩色钝化液中添加硫酸铈1.5 g/L时,钝化膜的表面质量及耐腐蚀性能最好。对比三价铬钝化膜及含铈三价铬钝化膜的外观颜色,发现稀土铈盐的添加加深了彩色钝化膜的色泽,提高了钝化膜的亮度及均匀性。从金相显微镜和扫描电镜(SEM)分析可知,2种钝化膜膜层明显,且含铈钝化膜的表面致密度更高。通过能谱仪(EDS)分析可知,稀土铈元素参与了成膜过程。黏着力测试和电化学测试表明,含铈三价铬钝化膜有较好的耐磨性和耐蚀性。初步分析镀锌层三价铬彩色钝化膜的成膜过程可知,成膜反应和溶解膜反应形成了一个动态平衡过程,通过控制钝化浸渍时间和钝化液的p H值,控制钝化膜的溶解,可以提高钝化膜的致密性。     

单晶硅的电化学钝化

常温下,用电化学氧化法在单晶硅表面形成 SiO_2钝化膜,钝化液可为有机溶液或纯水,控制电压能调节钝化膜厚度。测试并比较了钝化膜的基本性能。     

纳米SiO2及无机盐改性丙烯酸树脂-有机硅烷复合钝化膜的耐蚀性能

为了提高丙烯酸树脂类钝化膜的耐蚀性能,以三甲基氯硅烷对纳米SiO2进行表面改性,制成分散液后与硅烷偶联剂KH-563、丙烯酸树脂及无机盐Ni(CH3COO)2等复配成无铬钝化液,对热镀锌板进行复合钝化。采用红外光谱测试了改性纳米SiO2的结构,采用粒度仪分析其粒径;利用扫描电镜和能谱分析了复合钝化膜的微观形貌和成分;采用电化学及中性盐雾试验分析了复合钝化膜的耐蚀性能。结果表明:纳米SiO2改性后,表面能降低,分散性良好;改性纳米SiO2与丙烯酸树脂发生交联作用,形成了网状结构,提高了复合钝化膜的致密性;复合钝化耐蚀性能较丙烯酸树脂钝化膜及热镀锌板显著提高。     

Electrical and optical properties of semi-insulating polycrystalline silicon thin films: the role of microstructure and doping

We have investigated the relationship between microstructure and electrical conductivity in semi-insulating polycrystalline silicon (SIPOS) with oxygen concentrations in the 2–35 at.% range and the effect of doping with boron, phosphorus, arsenic and erbium by ion implantation. SIPOS thin films are mixtures of silicon and silicon oxide phases. The chemical and morphological evolution of these phases upon annealing is emphasized. Electrical conductivity measurements are interpreted in terms of a physical model containing few free parameters related to the material microstructure. A direct extension of this model explains also the conductivity increase in SIPOS doped with elements of the third or the fifth group. In the last part of the paper, data of electroluminescence at 1.54 μm in Er-implanted SIPOS due to intra-4f transitions of the Er³⁺ ion are shown and discussed.     

Silicon surface passivation by hot-wire CVD Si thin films studied by in situ surface spectroscopy

Silicon thin films can provide an excellent surface passivation of crystalline silicon (c-Si) which is of importance for high efficiency heterojunction solar cells or diffused emitter solar cells with well-passivated rear surfaces. Hot-wire chemical vapor deposition (hot-wire CVD) is an attractive method to synthesize Si thin films for these applications as the method is ion-bombardment free yielding good quality films over a wide range of deposition rates. The properties of the interface between hot-wire CVD Si thin films and H-terminated c-Si substrates have been studied during film growth by three complementary in situ techniques. Spectroscopic ellipsometry has been used to determine the optical properties and thickness of the films, whereas information on the H-bonding modes and H-depth profile has been obtained by attenuated total reflection infrared spectroscopy. Second-harmonic generation (SHG), a nonlinear optical technique sensitive to surface and interface states, has been used to probe two-photon resonances related to modified Si-Si bonds at the interface. By correlating the observations with ex situ lifetime spectroscopy experiments the growth and surface passivation mechanism of the Si films are discussed.     

X-ray photoelectron spectroscopic studies of sprayed CdS films

The chemical composition of sprayed CdS films has been evaluated using X-ray photoelectron spectroscopy. The general impurity content in the film is discussed, throwing light on the pyrolysis reaction involved in CdS deposition. Further, the stoichiometry of these films is studied as a function of process parameters such as pyrolysis temperature, Cd/S ratio in the solution, deposition rate and film thickness. A definite correlation is observed between composition and process parameters. The compositional variation appears to be related to the structure of CdS films as well as the growth mechanism. The effects induced by annealing in nitrogen, hydrogen and ambient air are also discussed. Hydrogen and nitrogen annealing is responsible for oxygen desorption from CdS. On the other hand air annealing induces stoichiometric variations along with oxygen intake in the films.     

Effect of oxygen agglomeration in polycrystalline Si (SIPOS) films

IR transmission spectra of SIPOS structures were measured and were investigated by using an approach of deconvolution of the Si–O stretching band into Gauss profiles. It was found that the space distribution of oxygen in SIPOS layers treated at elevated temperatures does not correspond to the prediction of RBM statistics. The oxygen agglomeration was observed. Optical microscopy was also applied to get additional information about the SIPOS films after treatment in HF solution. The peculiarities of the space distribution of oxygen in SIPOS films are explained on the basis of a computer simulation of free Si surface relaxation. A computer model has shown that a disordered phase arises in the Si surface layers at elevated temperatures. This phase is characterized by a large concentration of stressed and dangling bonds. There are lattice nodes with more than one dangling bond that are suitable sites for oxygen agglomeration.     

Evaluation of charge transfer characteristics of metal-free phthalocyanine thin films by displacement current measurement

We have investigated phthalocyanine thin films using displacement current measurement. Two types of samples were prepared by vacuum evaporation method. One is the sample with a passivation film. The other is the sample without a passivation film. The passivation films were prepared by casting toluene solution containing 3 wt.% of polystyrene. The results obtained by measuring the samples elucidate the relation between carrier behavior and ambience. It is clarified that there are many traps in the sample without the passivation film. On the other hand, in the sample with the passivation film, traps are not observed. Therefore, it is concluded that the passivation film provides the constraint of oxygen doping as well as the preservation of carrier transfer system.     

用ECRCVD方法制备优质氮化硅钝化膜

利用电子回旋共振等离子体化学气相沉积(ECR—CVD)技术，以SiH4和N2为反应气体进行了氮化硅钝化薄膜的低温沉积技术的研究。采用原子力显微镜、傅立叶变换红外光谱和椭圆偏振光检测等技术对薄膜的表面形貌、结构、厚度和折射率等性质进行了测量。结果表明，采用ECR—CVD技术能够在较低的衬底温度条件下以较高的沉积速率制备厚度均匀的氮化硅薄膜，薄膜中H含量很低。薄膜沉积速率随微波功率和混合气体中硅烷比例的增加而增大。折射率随微波功率的增大而减小，随混合气体中硅炕比例的增大而增大。在相同气体混合比和微波功率条件下，较高衬底温度条件下制备的薄膜折射率较大。     

Passivation coating on titanium powder surface via SnCl4-Ti gas–solid fluidization reaction

Titanium powder is easily oxidized in the forming and sintering process due to its active chemistry. In this study, a passivation coating is formed on Ti powder surface via SnCl₄-Ti gas–solid fluidization reaction using fluidized bed. It is found that at 200–350 ℃, Ti-Sn-Cl-O passivation layer is formed on Ti powder surface on account of the reaction among SnCl₄, oxide film on powder surface, and Ti matrix. Upon further increasing the temperature to above 500℃, deoxygenation reaction occurs accompanied by the formation of gaseous TiCl_m and TiO_xCl_y escaping from Ti powder matrix, resulting in the decreasing of surface oxygen content. Besides, elemental Sn and Ti-Sn compounds are formed on Ti powder surface, and part of Sn is diffused into titanium matrix. The passivation behavior is mainly consisted of oxygen film destruction and oxygen removal with the fluidization temperature increasing. Overall, the suitable temperature is about 350℃ to form a passivation coating on Ti powder surface, which can achieve oxidation isolation and deoxygenation in subsequent forming and sintering process.     

Nanostructure of pure iron anodically oxidized in borate buffer solution and annealed by infrared radiation

The behavior of oxide film on pure iron passivated in a borate buffer solution and subsequently radiated by infrared light (IR) was investigated in comparing to that by just IR annealing without passivation, and was evaluated by film structure, etc. The effect of thermal annealing over 250 degrees C was observed with gamma-Fe2O3 grain growth and sharp increase in surface roughness, film thickness and oxygen content. An ellipsometric parameter of tan psi was sensitively reflected by annealing effect, and tan psi curve had a shoulder at 150 degrees C for 5 min and a peak of tan psi was shifted from 350 nm to 450 nm in wavelength. This shift was also caused by the formation of gamma-Fe2O3, because the peak was also observed in tan psi of the bulk Fe2O3 family. Passivation effects at 800 mV prior to IR annealing on thickness and oxygen content changed at 150 degrees C, and decreased tan psi at 350 nm and excessive film growth over 250 degrees C, and increased oxygen content under 100 degrees C and surface roughness at 50-250 degrees C. The terrace width with atomic scale flatness was slightly increase by passivation prior to IR annealing at 50-250 degrees C, and the maximum terrace width reached larger than 10 nm by passivation and IR annealing at 100 degrees C for 30 min.     

金刚石膜在多孔硅发光中的应用

采用微波等离子体化学气相沉积（MPCVD）法成功地在多孔硅上沉积出均匀、致密的金刚石膜。光致发光测量表明,金刚石膜可以有效稳定多孔硅的发光波长和发光强度,具有明显的钝化效应。金刚石膜的这个特点再加上高硬度特性使金刚石膜成为多孔硅的一种潜在的钝化膜。