溅射辅助微波等离子体化学气相沉积SiCN晶体

在微波等离子体化学气相沉积系统中,利用脉冲氮离子束溅射二氰二氨靶产生的碳氮粒子作为合成前驱物,在石英玻璃基片上研究了SiCN晶体的合成。用扫描电子显微镜(SEM)、X射线能谱(EDX)、X射线衍射(XRD)和X射线光电子能谱(XPS)研究了基片温度对薄膜的形貌、成分和结构的影响。结果表明:随着基片温度的降低,沉积物由截面为六方形的结晶良好的SiCN晶体(800℃)变成发育不完全的聚片状晶体(700℃),直到变成颗粒细小的无定形碳氮薄膜(550℃)。衍射峰的强度以及晶胞参数a和c的值随温度的降低而减小。薄膜为C原子部分取代Si3N4中的Si原子位置而形成的SiCN晶体,其中N原子主要与Si原子结合,C原子以sp3C—N、sp2CN和sp2CC键的形式存在。降低基片温度有利于提高薄膜中的C含量和sp3C—N键的含量。     

SiCN扩散阻挡层薄膜的制备及特性研究

采用磁控溅射法在单晶硅衬底上制备了SiCN及Cu/SiCN薄膜,并对试样进行了退火处理.利用原子力显微镜(AFM)、X射线衍射(XRD)、四探针测试仪(FPP)研究了SiCN薄膜的表面形貌、物相结构及在Cu/SiCN/Si结构中SiCN薄膜对铜与硅的阻挡性能.结果表明,沉积态SiCN薄膜为无定型的非晶结构,晶化温度在1000℃以上;SiCN薄膜作为Cu的扩散阻挡层有较好的热稳定性及阻挡性,阻挡失效温度在600℃左右.     

Si和C的存在形态对TiSiCN薄膜微观结构与性能的影响

为扩展Ti Al N和Ti CN薄膜的应用,以适应高速切削和绿色干式切削加工技术发展趋势和要求,采用工业化多弧离子镀在工业用钢H13表面制备Ti SiCN硬质薄膜,以改善H13钢的力学和摩擦学性能。借助扫描电子显微镜、X射线衍射仪、X射线光电子能谱仪、维氏显微硬度计、摩擦磨损仪研究了Si和C的存在形态及其对Ti SiCN薄膜的微观形貌、微观结构、硬度和摩擦磨损性能的影响。结果表明:Ti Si CN薄膜组织致密,具有纳米晶Ti(CN)与非晶相(SiC、Si3N4和C);薄膜中C原子固溶于Ti(CN)中,随着C含量的增加,Ti(CN)固溶度增加;部分C以非晶态的形式存在,起到阻碍Ti Si CN纳米晶粒生长作用; Si以非晶SiC和Si3N4相的形式存在,并包裹Ti CN纳米晶,抑制薄膜晶粒的长大;高Si含量Ti Si CN-No.2薄膜和高C含量Ti Si CN-No.3薄膜表现出高硬度和耐磨减摩特性。     

添加H2对SiH4/N2/Ar等离子体淀积的氮化硅电学和光学特性的影响

研究了加H2对SiH4/N2/Ar高密度、低离子能量的等离子体淀积的氮化硅薄膜(淀积的衬底温度为400℃)电学和光学性能的影响。实验结果表明,加入H2使氮化硅薄膜的光学带隙增加,其折射率以及在氢氟酸缓冲液中腐蚀速率减小,而XPS测试的N、Si原子比没有改变,均为1.3。FTIR测量表明,样品中Si-H键的密度低于仪器检测限,而添加H2的样品中N-H键密度稍增加。此外,由淀积的氮化硅膜构成的MIS结构的高频C-V测试(1 MHz)显示,当氢气流量从零增加到8sccm时,高频C-V的回滞幅度从(0.40±0.05)V降低到(0.10±0.01)V。基于这些实验结果和理论分析,表明了加适量H2能够促进弱的Si-Si键以及Si和N的悬挂键向Si-N键转化。     

添加H2对SiH4/N2/Ar等离子体淀积的氮化硅电学和光学特性的影响

研究了加H2对SiH4/N2/Ar高密度、低离子能量的等离子体淀积的氮化硅薄膜(淀积的衬底温度为400℃)电学和光学性能的影响。实验结果表明,加入H2使氮化硅薄膜的光学带隙增加,其折射率以及在氢氟酸缓冲液中腐蚀速率减小,而XPS测试的N、Si原子比没有改变,均为1.3。FTIR测量表明,样品中Si-H键的密度低于仪器检测限,而添加H2的样品中N-H键密度稍增加。此外,由淀积的氮化硅膜构成的MIS结构的高频C-V测试(1 MHz)显示,当氢气流量从零增加到8sccm时,高频C-V的回滞幅度从(0.40±0.05)V降低到(0.10±0.01)V。基于这些实验结果和理论分析,表明了加适量H2能够促进弱的Si-Si键以及Si和N的悬挂键向Si-N键转化。     

气体流量比对反应溅射Si3N4薄膜的影响

利用射频磁控反应溅射法,以高纯Si为靶材,高纯N2气为反应气体,在Si衬底上制备出了Si3N4薄膜,研究了气体流量比对薄膜质量的影响.结果表明,薄膜的沉积速率主要与气体的流量比有关,随着气体流量比的增加,沉积速率下降,靶面的溅射由金属模式过渡到氮化物模式;薄膜中N/Si的原子比增加;红外吸收谱的Si-N键的振动峰向标准峰逼近.     

DBD-PECVD法制备CN薄膜的结构及性能研究

使用自行设计的真空系统,采用介质阻挡放电等离子体增强化学气相沉积(DBD-PECVD)法,分别以CH4/N2、C2H2/N2、C2H4/N2混合气体作为反应气体,在单晶硅片上成功制备了CN薄膜.FTIR结果证实了薄膜中碳氮原子结合成化学键,Raman结果说明薄膜中含有类金刚石结构,AFM结果表明薄膜粗糙度随放电气压的升高而逐渐增大.三种混合气体沉积的CN薄膜,以CH4/N2的沉积速度最慢,薄膜表面粗糙度最小,含H量最少;C2H2/N2的沉积速度最快,薄膜表面粗糙度最大.     

ZrO2-SiO2薄膜对离子交换增强玻璃的光学和力学性能影响

采用溶胶-凝胶法在玻璃表面制备出ZrO₂-SiO₂薄膜, 然后通过离子交换形成镀膜增强玻璃, 研究了薄膜组成对离子交换增强玻璃的力学和光学性能的影响。利用紫外可见分光光度计、激光椭偏仪、纳米压痕、三点抗弯和能谱(EDX)分析了薄膜结构及性能。结果表明: 所有薄膜均连续均匀, 纯ZrO₂薄膜为四方相结构, 含Si薄膜为无定形结构; 薄膜具有较高弹性恢复率(>60%)以及H/E比(>0.1), 有利于强度增强; 随Si含量增加, 可见光透过率增大, 但表面硬度和杨氏模量随之降低; 0.5ZrO₂-0.5SiO₂薄膜综合性能最佳: 表面硬度为18 GPa, 抗弯强度为393 MPa, 厚度~45 nm时可见光透过率大于85%。     

热丝CVD生长SiCN薄膜的研究

在HFCVD系统中采用SiH₄/CH₄/H₂/N₂混合气体成功的制备了SiCN薄膜.SEM照片显示制备的SiCN薄膜由棒状结构构成,而在HRTEM下发现这些棒状结构是由生长在无定型SiCN基体当中的纳米晶粒组成的.进一步的SAED和XRD分析说明SiCN纳米晶粒具有类似于α-Si₃N₄的结构.XPS和FTIR分析表明薄膜中含有Si、C、N和O几种元素以及C=N、Si-N和C-N等共价键,但是并没有观察到C-Si的存在.由实验得出结论,SiCN晶体的生长包括两个步骤:α-Si₃N₄团簇的生长和C取代其中Si的过程.     

钯钌原子比对碳载Pd-Ru催化剂催化H2O2电还原性能影响

利用化学还原法制备了不同原子比的碳载Pd-Ru催化剂,考察了钯钌原子比对碳载Pd-Ru催化剂催化H2O2电还原反应性能的影响。研究结果表明,随着Ru元素的增加,碳载Pd-Ru催化剂的粒径逐渐减小,各催化剂上H2O2电还原反应的起始还原电势稳定在0.82V,电流密度先增大后减小。当Pd∶Ru=1∶1时,PdRu/C催化剂表现了最好的催化性能。     

Conversion of a plasma enhanced chemical vapor deposited silicon-carbon-nitride thin film at ultra-low temperature by oxygen plasma

In this work we present an ultra-low temperature method for the oxidation of an amorphous silicon-carbide-nitride (SiCN) material. The SiCN is deposited on silicon substrates by plasma enhanced chemical vapor deposition using CH₄, SiH₄, and N₂ chemistry. The physical and chemical properties are characterized for the as-deposited SiCN and post-oxidized films are discussed. The SiCN film is exposed to oxygen plasma, where it undergoes a chemical transformation into a binary SiO₂ material system. A 1.7 nm/min oxidation rate is typical for this process and compares favorably to oxidation methods utilizing much higher temperatures. The substrate temperature remains extremely low throughout the oxidation process, T_s < 200 °C. Changes in film stress, optical constants, film thickness, surface roughness, and film density are measured. Chemical analysis by X-ray photoelectron spectroscopy is reported for both the as-deposited and oxidized film and confirms the resultant film to be the chemical equivalent of thermally grown SiO₂. We discuss applications specifically targeted to the conversion of SiCN to SiO₂.     

蓝宝石衬底上制备SiO2薄膜的研究

采用射频磁控反应溅射法,以高纯Si为靶材,高纯O2为反应气体,成功地在蓝宝石基片上制备出了二氧化硅(SiO2)薄膜,并对薄膜的沉积速率、成分、结构及红外光学性能进行了研究.结果表明,制备的SiO2薄膜与蓝宝石衬底结合牢固;和其它镀膜技术相比,射频磁控反应溅射法可以在较低的温度下制备出SiO2薄膜;制备出的SiO2薄膜在3～5μm波段对蓝宝石衬底有明显的增透效果.     

The photoluminescence of SiCN thin films prepared by C implantation into α-SiNx:H

SiCN thin films were prepared by high-dosage (2 × 10¹⁷ cm^− 2) C⁺ ion implantation into α-SiN_x:H films. The prepared films were then processed by thermal annealing for 2 h at 800 °C, 1000 °C and 1200 °C respectively. The composition and bond structure of SiCN were analyzed by X-ray photoemission spectroscopy, Auger electron spectroscopy, Raman spectroscopy and X-ray diffraction, and photoluminescence. Ternary structure with N bridging C and Si of the film annealed at 800 °C was found. The luminescent properties of SiCN have also been studied by synchrotron radiation at 20 K. Four emission bands were observed, corresponding to 2.95, 2.58, 2.29 and 2.12 eV at 20 K, respectively. In this paper, we report the experimental results and try to explain them.     

白宝石上生长SiO2薄膜的工艺

用射频磁控反应溅射法,以高纯Si为靶材,高纯O2为反应气体,在白宝石上制备SiO2薄膜。对影响薄膜生长的工艺参数进行了分析,测试了薄膜的成分,并研究了薄膜的红外光学性能。结果表明,制备的薄膜中Si和O形成SiO2化学键,计算出的O与Si的原子比接近2:1,采用射频磁控反应溅射法在白宝石上能够沉积出SiO2薄膜。制备出的SiO2薄膜对白宝石衬底有较好的增透作用。     

Analyses of interface adhesion between porous SiOCH low-k film and SiCN layers by nanoindentation and nanoscratch tests

In this study, an Si/PEOX/SiCN/SiOCH/SiCN multilayered film stack has been prepared by chemical vapor deposition. The bonding configurations between porous SiOCH film and SiCN etch stop layers have been analyzed by X-ray photoelectron spectroscopy, and the interface adhesion has been investigated by nanoindentation and nanoscratch tests. Elements of Si, C, N, and O constructed an interlayer region of about 10 nm with mixing bonds of Si to C, Si to N and Si to O at the interface between the porous SiOCH film and SiCN layers. During nanoindentation and nanoscratch tests, interface delamination occurred between SiOCH and SiCN layers due to the accumulation of sufficient shear stresses around the indented regions. The interface adhesion energy was accordingly measured as 1.68 J/m² by nanoindentation test with an applied load of 30 mN. With higher applied loads, the measured interface adhesion energy decreased. By the nanoscratch test, the interface adhesion energy was measured as about 0.91 J/m², lower than that obtained by nanoindentation test due to the mode mixity effect.     

Evaluation of corrosion resistance of SiCN films deposited by HWCVD using organic liquid materials

SiCN films were obtained at a substrate temperature of 250 °C by hot wire chemical vapor deposition (HWCVD) using hexamethyldisilazane which is non-explosion organic liquid source instead of SiH₄. The SiCN films were immersed into 10% H₂SO₄ for 1 week to investigate a corrosion resistance of SiCN films. The film thicknesses of these samples were measured by ellipsometry using a He-Ne laser at 632.8 nm. No SiCN film thickness was changed at all for 1 week in 10% H₂SO₄. We confirmed that SiCN films showed high corrosion resistance for 10% H₂SO₄.     

H2O+ O2气氛下电子束蒸镀制备MgO介质保护膜特性研究

采用电子束蒸镀法在H2O+ O2气氛下制备了MgO介质保护膜,通过扫描电镜、X射线衍射(XRD)等方法分析了MgO薄膜的表面、截面形貌与晶体结构,研究了不同H2O流量下得到的MgO薄膜对等离子屏放电特性的影响。结果表明:MgO薄膜呈柱状结构,随H2O流量增加MgO晶粒尺寸变大、晶界减少;XRD分析结果显示H2O+ O2气氛下,MgO薄膜除(111)晶面择优取向外,还出现了(220)晶面取向;H2O气氛的通入降低了等离子屏的维持电压、改善了放电裕度,同时缩短了寻址放电延迟时间,有利于等离子屏节能降耗和实现快速寻址。     

Effect of electron beam irradiation on structure and properties of SiCN thin films prepared by plasma assisted radio frequency magnetron sputtering

Silicon carbon nitride thin films were deposited on Si (100) substrate at room temperature by plasma assisted radio frequency magnetron sputtering. The bonding structure and properties of SiCN films irradiated by pulsed electron beams were studied by means of X-ray photoelectron spectroscopy and nano-indentation. The results showed that electron beam irradiation had a great effect on the structure and property of the films. Under sputtering gas pressure of 3.7 Pa, a transition from the (Si,C)N_x bonded structure to the (Si,C)₃N₄ bonded structure was found in the SiCN thin film with electron beam irradiation. At sputtering gas pressure of 6.5 Pa, the enhancement of hardness in the SiCN film after treatment with electron beam irradiation resulted from the promotion of the sp³-hybridization of carbons bonds.     

Sputtered FeCoN soft magnetic thin films with high resistivity

Fe/sub 70/Co/sub 30/N thin films with thickness from 20 to 1100 /spl Aring/ were prepared by radio- frequency reactive sputtering in an N/sub 2/--Ar mixture. The FeCoN films prepared in a low nitrogen flow rate percentage (<6%) and sputtering pressure (<8 mTorr) have a high B/sub s/ of about 24.0 kG, but a moderate hard-axis coercivity H/sub ch/ of 5-30 Oe. With further increase in N/sub 2/ percentage or sputtering pressure, films become significantly softer, with H/sub ch/ of about 0.1-0.6 Oe, and have a higher resistivity of up to about 160 /spl mu//spl Omega//spl middot/cm. The change in the magnetic properties with nitrogen flow rate percentage and sputtering pressure can be attributed to the formation of an ultrafine grain size nanocrystalline FeCoN thin film as observed by high-resolution transmission electron microscope. The soft properties of FeCoN films with nano-sized crystallites remain stable even after being annealed at 270/spl deg/C.     

探索MOCVD法制备TiO2薄膜的最佳反应条件

用低压金属有机化合物化学气相沉积 (MOCVD法 ),以四异丙纯钛 (TTIP)为源物质,高纯氮气作为载气,氧气为反应气体,制备出了 TiO2薄膜。分析出了沉积温度、氧气流量等因素对沉积速率的影响。发现在不同反应条件下 TiO2薄膜生长行为受动力学控制或受扩散控制,为制备优质 TiO2薄膜提供了依据。