柔性ZnO/PI/PET复合薄膜的制备工艺及其阻隔性能研究

目的 解决物理溅射沉积法制备的无机氧化物类高阻隔包装材料柔韧性不足,使用过程中易脆裂的问题。方法 采用射频磁控溅射技术（RF）,以氧化锌（ZnO）、聚酰亚胺（PI）为靶材,在PET塑料表面同时沉积制备ZnO/PI/PET复合薄膜。详细分析PI的引入对ZnO阻隔层微观结构以及性能的影响,优化ZnO/PI/PET的溅射制备工艺。结果 沉积层微观形貌及包装性能受溅射功率密度比（PZnO/PPI）的影响较大。随着PZnO/PPI的降低,沉积层PI含量增加,阻隔层纳米颗粒由燕麦形状向球形转变,球径呈降低趋势。沉积层柔韧性提升明显,经过100次折叠后,没有明显裂纹产生（PZnO/PPI≤2）。在PZnO/PPI为2,氩气流量为40 mL/min,沉积时间为30 min,工作气压为0.5 Pa的条件下,ZnO/PI/PET复合阻隔薄膜对水蒸气、氧气的阻隔能力最为理想,水蒸气透过率为0.342 g/(m2?d),氧气透过率为0.365 mL/(m2?d)。结论 适量PI片段的引入可以有效提升无机氧化物阻隔层的柔韧性及耐折叠能力,还可进一步提升复合沉积膜对水蒸气、氧气等气体小分子的阻隔能力。     

ZnO/SiO2复合薄膜的制备及其阻隔性能研究

目的为了进一步提高氧化锌(ZnO)沉积复合薄膜对氧气的阻隔能力,探索其应用于食品和药品包装材料的可行性。方法采用射频磁控溅射技术(RF),以ZnO和二氧化硅(SiO2)为靶材,在PET塑料表面同时沉积,制备ZnO/SiO2复合薄膜包装材料,并详细分析SiO2的引入对ZnO沉积膜微观结构和阻隔能力的影响,优化ZnO/SiO2的制备工艺。结果SiO2的引入,使ZnO纳米颗粒的形状由片状燕麦变成了球形,当功率密度比PSiO2/PZnO为0.67,氩气流量为20 mL/min,沉积时间为20 min,工作气压为0.5 Pa时,ZnO/SiO2复合薄膜的氧气透过率降低为0.462 mL/(m^2·d),水蒸气透过率有所增加,为0.367 g/(m^2·d)。结论引入合适比例的SiO2,可有效提升ZnO沉积层对氧气渗入的阻隔能力,但SiO2引入量过高时,会加剧纳米裂纹,对复合薄膜的阻隔能力不利。     

脉冲微波表面波PECVD在有机PET表面沉积DLC薄膜的阻隔性研究

目的 探讨使用脉冲微波表面波等离子体辅助化学气相沉积技术在聚对苯二甲酸乙二醇酯（PET）材料表面沉积类金刚石薄膜作为阻隔层的可行性。方法 以C2H2为单体,氩（Ar）为放电气体,采用脉冲微波表面波等离子体化学气相沉积（PECVD）技术在有机PET材料表面沉积类金刚石（Diamond-like Carbon, DLC）薄膜。研究工艺参数,如脉冲微波放电功率、工作气压、单体与工作气体的体积比等,对DLC薄膜沉积速率和阻隔性能的影响。通过傅里叶变换红外光谱（FT-IR）、原子力显微镜（AFM）、氧气和水蒸气透过率测试仪等对薄膜结构与性能进行表征。结果 DLC薄膜的结构和成分随着等离子体放电工艺参数的变化而改变,造成其阻隔性能也随之发生变化。PET表面沉积纳米级DLC薄膜后,氧气透过率和水蒸气透过率可以分别降至0.58 mL/(m2?d)和2.5 g/(m2?d)。结论 DLC薄膜对氧气和水蒸气都表现出良好的阻隔性,可以应用于食品、药品的阻隔包装。     

SiOx/PET复合薄膜的力学性能及阻隔性能

目的基于氧化硅(SiO_x)镀层优异的性能,研究不同厚度的SiO_x层对SiO_x/PET复合薄膜力学性能和阻隔性能的影响,以期得到性能较优的SiO_x/PET复合薄膜。方法以自制的聚对苯二甲酸乙二醇酯(PET)薄膜为基材,采用等离子体增强化学气相沉积法沉积得到SiO_x层厚度分别为40,150,230,320 nm的SiO_x/PET复合薄膜,并进行傅里叶变换红外线光谱分析、力学性能和阻隔性能测试,以及薄膜表观形貌分析。结果沉积SiO_x层后,SiO_x/PET复合薄膜拉伸强度和断裂伸长率随SiO_x层厚度的增大先增大后减小,氧气透过率和水蒸气透过率则出现明显衰减而后逐渐平缓的趋势。SiO_x层厚度达150~230 nm时,复合薄膜的力学性能和阻隔性能表现较优,拉伸强度、断裂伸长率、氧气透过率以及水蒸气透过率分别提高了约25.0%,20.9%,79.3%,77.3%。结论适宜厚度的SiO_x层可以使得SiO_x/PET复合薄膜同时具备较优的力学性能和阻隔性能。     

ITO上磁控溅射ZnO薄膜及其光电性质

在ITO(In2O3:Sn)衬底上射频溅射ZnO薄膜,研究了射频溅射功率对ZnO薄膜的晶体结构,表面形貌及光学透过率的影响.结果表明,随着射频功率的提高,沿(002)方向生长的ZnO薄膜的结晶度显著增强,薄膜的表面颗粒略有减小,表面粗糙度由13.13 nm降低到5.06 nm.在300～400 nm波长范围内薄膜的光学透过率随着射频功率的增加而降低.在双层薄膜中空间内建电场的存在有助于光生电子和空穴有效地分离,使ZnO/ITO双层薄膜具有较强的光电响应能力,光电流达14μA.     

射频功率对筒状聚酯内壁类金刚石薄膜结构与性能的影响研究

利用偏压/射频耦合等离子体增强化学气相沉积技术在聚对苯二甲酸乙二醇酯(简称聚酯,PET)筒内壁制备了类金刚石薄膜(DLC)。采用X射线光电子能谱、扫描电子显微镜、三维表面轮廓仪、紫外/可见光分光光度计和气体渗透率测试仪考察了射频功率对类金刚石薄膜的结构、沉积速率、表面形貌、光学透过率和气体阻隔性能的影响。结果表明,膜层沉积可有效阻挡近紫外区域的光线,同时对O2,CO2的阻隔能力明显提高,这是由于DLC膜层的致密性质以及PET表面原有缺陷的覆盖。与未镀膜PET相比,150 W时制备的DLC膜的气体透过率分别从58.5,61.7cm3m-2atm-1d-1降低至0.7,1.5 cm3m-2.atm-1d-1,相应的对O2,CO2的阻隔率分别可以提高80倍和40倍。     

磁控溅射制备大面积ZnO薄膜性能的研究

通过磁控溅射氧化锌陶瓷靶材的方法在玻璃基片上制备ZnO薄膜,研究了溅射功率、溅射气压以及基片温度对ZnO薄膜相结构、禁带宽度及光学性能的影响.使用X射线衍射仪(XRD)分析了薄膜相结构,使用台阶仪测试薄膜厚度,采用薄膜测试仪测试薄膜的透过率,采用扫描电镜(SEM)观察薄膜表面形貌.结果表明:不同制备条件下均形成具有(0...     

等离子体增强原子层沉积增透阻隔膜的研究

高阻隔高透光率的柔性复合材料在包装和电子封装领域具有很高的应用价值。本文采用等离子增强原子层沉积技术在PET基体上制备了多层结构的增透阻隔膜,研究了等离子增强原子层沉积制备氧化硅和氮化硅的工艺参数,利用光学模拟软件设计出所需透过率的膜层结构。结果表明:等离子体增强原子层沉积制备的薄膜原子力显微镜表面形貌晶粒分布均匀,薄膜致密,红外光谱显示制备的薄膜为高纯度的SiO_2和Si_3N_4,薄膜的透水率降低了2个数量级,可见光范围透过率可达到94%。     

沉积气压对电弧离子镀制备ZnO薄膜的结构和性能影响

采用阴极真空电弧离子镀技术在玻璃衬底上制备出了具有择优取向的透明ZnO薄膜. 利用X射线衍射仪、扫描电子显微镜及紫外-可见吸收光谱仪分别对ZnO薄膜的结构、表面形貌及可见光透过率进行了分析.XRD结果表明,所制备的ZnO薄膜具有六角纤锌矿结构的(002)和(101)两种取向,在沉积气压＞1.0Pa时所制备的ZnO薄膜具有(002)择优取向,并且非常稳定.SEM图表明,ZnO晶粒大小较为均匀,晶粒尺寸随着气压升高而变小.在400～1000nm范围内,ZnO薄膜的可见光透过率超过80%,吸收边在370nm附近,所对应的光学带隙约为3.33～3.40eV,并随着沉积气压上升而变大.     

射频磁控溅射对PET基材制备铝薄膜的性能影响

针对传统制铝技术,为提高膜层结合力、阻隔性,采用射频磁控溅射镀铝工艺,制备纯铝高阻隔性膜层,在PET塑料薄膜表面沉积纯铝的实验。通过对射频电源功率和溅射气压等参数的改变,探究射频功率、溅射气压对薄膜结合力、阻隔性的影响。结果表明:薄膜沉积过程中的射频功率和溅射气压对磁控镀铝薄膜性能影响较大,在一定的溅射压力下,膜层的结合力随射频功率的增大而逐渐增大,膜层的阻隔性随射频功率的增大,先提高后降低,射频功率为85W时,氧气透过率最小为1.11cm3/(m2·day·atm);在射频功率相同的情况下,结合力随着溅射气压的增大,先增大后降低,膜层的阻隔性随着溅射气压的增大而逐渐降低,溅射气压为0.5Pa时,结合力最高为1.68N/mm。较传统铝膜结合力提高2倍,阻隔性提高5倍。     

PET纤维基AZO透明导电薄膜溅射工艺参数的优化

室温下,结合正交实验表,用射频磁控溅射在涤纶(PET)非织造布基材上生长AZO(Al2O3:ZnO)纳米结构薄膜.采用四探针测量仪测试AZO薄膜的方块电阻,用原子力显微镜(AFM)分析薄膜微结构;通过正交分析法对实验L9(33)AZO薄膜的性能指标进行分析.实验结果表明:溅射厚度对AZO薄膜导电性能起主导作用,其次为氩气压强和溅射功率;同时,得出制备AZO薄膜的最佳工艺为:溅射功率150W、厚度100m和气压0.2Pa,该参数下样品的方块电阻为1.633×103Ω,AZO纳米颗粒的平均直径约为69.4nm.     

Growth and characterization of high resistivity c-axis oriented ZnO films on different substrates by RF magnetron sputtering for MEMS applications

In the present work, we report the deposition of high resistivity c-axis oriented ZnO films by RF magnetron sputtering. The deposition parameters such as RF power, target-to-substrate spacing, substrate temperature, and sputtering gas composition affect the crystallographic properties of ZnO films, which were evaluated using XRD analysis. The self-heating of the substrate in plasma during film deposition was investigated and we report that highly “c-axis oriented” ZnO thin films can be prepared on different substrates without any external heating under optimized deposition parameters. The post-deposition annealing of the film at 900 °C for 1 h in air ambient increases the intensity of (002) peak corresponding to c-axis orientation in addition with the decrease in full width at half maxima (FWHM). Bond formation of ZnO was confirmed by FTIR analysis. Grains distribution and surface roughness have been analyzed using SEM and AFM. The DC resistivity of the films prepared under different deposition conditions was measured using MIS/MIM structures and was found to be in the range of 10¹¹–10¹² Ω cm at low electric field of 10⁴ V/cm. The ZnO film of 1 μm thickness has transmittance of over 85% in the visible region. Applications of these films in MEMS devices are discussed.     

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。     

Effect of ZnO buffer layer on AZO film properties and photovoltaic applications

Aluminum-doped ZnO (AZO) transparent conducting films were deposited on glass substrates with and without intrinsic ZnO (i-ZnO) buffer layers by a home made and low cost radio-frequency (RF) magnetron sputtering system at room temperature in pure argon ambient and under a low vacuum level. The films were examined and characterized for electrical, optical, and structural properties for the application of CIGS solar cells. The influence of sputter power, deposition pressure, film thickness and residual pressure on electrical and optical properties of layered films of AZO, i-ZnO and AZO/i-ZnO was investigated. The optimization of coating process parameters (RF power, sputtering pressure, thickness) was carried out. The effects of i-ZnO buffer layer on AZO films were investigated. By inserting thin i-ZnO layers with a thickness not greater than 125 nm under the AZO layers, both the carrier concentration and Hall mobility were increased. The resistivity of these layered films was lower than that of single layered AZO films. The related mechanisms and plasma physics were discussed. Copper indium gallium selenide (CIGS) thin film solar cells were fabricated by incorporating bi-layer ZnO films on CdS/CIGS/Mo/glass substrates. Efficiencies of the order of 7–8% were achieved for the manufactured CIGS solar cells (4–5 cm² in size) without antireflective films. The results demonstrated that RF sputtered layered AZO/i-ZnO films are suitable for application in low cost CIGS solar cells as transparent conductive electrodes.     

铝/改性氟塑料复合薄膜的制备

采用射频磁控溅射技术在改性氟塑料表面沉积铝层,制备了金属/氟化高聚物复合薄膜.利用场发射扫描电镜(FESEM)及能量散射谱(EDS)分析仪对沉积的铝层进行了表面形貌的表征和化学组分的分析.初步探讨了溅射功率、气压和时间等不同溅射参数对铝层结构和铝层在氟塑料表面附着情况的影响.结果表明:溅射功率是决定复合薄膜质量的重要因素,功率过低得不到致密的铝层结构,而且铝层容易从氟塑料表面脱离,功率过高则会产生很强的热效应而使复合薄膜弯曲.溅射气压和时间分别影响铝层在氟塑料表面的沉积速率和生长厚度.     

磁控溅射制备硅铝阻隔膜的研究

采用磁控溅射技术以10%Si～90%Al合金为靶材,通入O2将Si氧化成SiO2,Al氧化成Al2O3,在普通PET薄膜表面制备具有高阻隔性无机阻隔薄膜层,以增加其阻隔性.传统的磁控溅射法制备SiO2膜工艺,大多采用射频溅射法,但其成本较高,效率较低,无法充分满足大面积工业化镀膜生产的需要.而采用10%Si～90%Al合金不仅可以实现直流溅射工艺,而且测量结果表明,薄膜的阻隔性得到大幅度提高.     

Influence of RF power on structural,morphology, electrical,composition and optical properties of Al-doped ZnO films deposited by RF magnetron sputtering

In this study, influence of RF power on the structural, morphology, electrical, composition and optical properties of Al-doped ZnO (ZnO:Al) films deposited by RF magnetron sputtering have been investigated. Films were systematically and carefully investigated by using variety of characterization techniques such as low angle X-ray diffraction, UV–visible spectroscopy, Raman spectroscopy, Hall measurement, X-ray photoelectron spectroscopy, field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy etc. Low angle X-ray diffraction analysis showed that the films are polycrystalline with hexagonal wurtzite structure and which was further confirmed by Raman spectroscopy analysis. Its preferred orientation shifts from (102) to (002) with increase in RF power. The average grain size was found in the range of 15–21 nm over the entire range of RF power studied. The FE-SEM analysis showed that grain size and surface roughness of ZnO:Al films increase in with increase in RF power. The UV–visible spectroscopy analysis revealed that all films exhibit transmittance >85 % in the visible region. The optical band gap increases from 3.37 to 3.85 eV when RF power increased from 75 to 225 W. Hall measurements showed that the minimum resistivity has been achieved for the film deposited at 200 W. The improvement in the electrical properties may attribute to increase in the carrier concentration and Hall mobility. Based on the experimental results, the RF power of 200 W appears to be an optimum sputtering power for the growth of ZnO:Al films. At this optimum sputtering power ZnO:Al films having minimum resistivity (8.61 × 10^?4 Ω-cm), highly optically transparent (~87 %) were obtained at low substrate temperature (60 °C) at moderately high deposition rate (22.5 nm/min). These films can be suitable for the application in the flexible electronic devices such as TCO layer on LEDs, solar cells, TFT-LCDs and touch panels.     

CoFe合金薄膜的制备及原子力表征

室温下采用射频磁控溅射技术在涤纶纺粘非织造布表面沉积钴铁(CoFe)合金薄膜.通过原子力显微镜(AFM)观察了CoFe合金薄膜在无纺织布表面沉积的微观结构,并较为系统地分析了溅射时间、溅射压强及溅射功率对CoFe合金薄膜微观结构的影响.结果表明,磁控溅射的工艺参数配置对CoFe合金薄膜表面形貌的影响很大,溅射时间的长短、溅射功率的大小对成膜的均匀性有很大影响,在一定的溅射压强(0.5Pa)时合金颗粒将会因团聚而急速增大.     

Estimation of moisture barrier ability of thin SiNx single layer on polymer substrates prepared by Cat-CVD method

The SiNx films with the thickness of 50 nm were prepared by Cat-CVD method on the cyclic olefin copolymer (COC) and the polyethylene terephthalate (PET) substrates, and their moisture barrier abilities were evaluated. MOCON measurement method and Ca degradation test showed the moisture permeation results of 0.02 g/(m² day) for PET substrate and 0.006 g/(m² day) for COC substrate after SiNx deposition. Applying the simple model of gas barrier property, it was estimated that the Cat-CVD method achieves the high coverage ratio of over 99% for SiNx film on these substrates, and the moisture permeation rate of single SiNx film with the thickness of 50 nm was estimated to be 0.0045 g/(m² day).