CN100558940C - 涂布的基片及其制备方法 - Google Patents
涂布的基片及其制备方法 Download PDFInfo
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- CN100558940C CN100558940C CNB2005800259424A CN200580025942A CN100558940C CN 100558940 C CN100558940 C CN 100558940C CN B2005800259424 A CNB2005800259424 A CN B2005800259424A CN 200580025942 A CN200580025942 A CN 200580025942A CN 100558940 C CN100558940 C CN 100558940C
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- titanium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
- H01L21/02126—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material containing Si, O, and at least one of H, N, C, F, or other non-metal elements, e.g. SiOC, SiOC:H or SiONC
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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Abstract
一种涂布的基片,其含有包括密度为至少1.6g/cm3的氢化碳氧化硅的至少一层阻挡层,和至少一层选自铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛的阻挡层。
Description
相关申请的交叉参考
[0001]无
发明领域
[0002]本发明涉及涂布的基片,和更特别地涉及如下的涂布的基片,其含有包括密度为至少1.6g/cm3的氢化碳氧化硅的至少一层阻挡层和选自铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛中的至少一层阻挡层。
发明背景
[0003]阻挡涂层通过保护敏感材料避免空气、湿气和其它环境元素从而在宽范围的应用中起到重要的作用,其中所述应用包括电子包装、食品包装和表面处理。结果,这种涂层增加许多消费产品的可靠度和可用寿命。
[0004]适合于用作层间电介质或者环境阻挡层的氢化碳氧化硅膜和生产这种膜的方法是本领域已知的。例如,Loboda等人的美国专利No.6159871公开了一种生产氢化碳氧化硅膜的化学气相沉积方法,该方法包括将包括含甲基的硅烷和提供氧的气体的反应性气体混合物引入到含有基片的沉积腔室内,并在25℃-500℃的温度下诱导含甲基的硅烷和提供氧的气体之间的反应;其中在反应过程中存在控制量的氧气,以便在基片上提供介电常数小于或等于3.6的含氢、硅、碳和氧的膜。
[0005]Loboda的国际申请公布No.WO02/054484公开了一种集成电路,其包括形成由半导体材料制成的基片的固态器件的组件、连接该固态器件的金属布线和在至少该金属布线上形成的扩散阻挡层,其中所述扩散阻挡层是组成为SiwCxOyHz的合金膜,其中w的值为10-33,x的值为1-66,y的值为1-66,z的值为0.1-60,和w+x+y+z=100原子%。
[0006]Loboda等人的美国专利No.6593655公开了一种半导体器件,在其上具有通过引入包括含甲基的硅烷和提供氧的气体的反应性气体混合物到含有半导体器件的沉积腔室内并在25℃-500℃的温度下诱导所述含甲基的硅烷与提供氧的气体之间的反应而产生的膜;其中在反应过程中存在控制量的氧气,以便在半导体器件上提供介电常数小于或等于3.6的含氢、硅、碳和氧的膜。
[0007]Cerny等人的美国专利No.6667553公开了选自液晶器件、发光二极管显示器和有机发光二极管显示器的基片,在其上具有通过引入包括含甲基的硅烷和提供氧的气体的反应性气体混合物到含有基片的沉积腔室内并在25℃-500℃的温度下诱导所述含甲基的硅烷与提供氧的气体之间的反应而产生的膜;其中在反应过程中存在控制量的氧气,以便在基片上提供介电常数小于或等于3.6的含氢、硅、碳和氧的膜,和以产生对于波长范围为400nm-800nm的光来说透光率大于或等于95%的膜。
[0008]尽管前述参考文献公开了具有良好介电和阻挡性能的氢化碳氧化硅的涂层,但仍需要对环境元素,尤其是水蒸气和氧气,具有优异抗性的介电涂层。
发明概述
[0009]本发明涉及涂布的基片,其包括:
基片;
在基片上的第一阻挡层,其中第一阻挡层包括密度为至少1.6g/cm3的氢化碳氧化硅;和
在第一阻挡层上的至少两层交替的缓冲层和阻挡层,其中每一交替的缓冲层包括密度小于1.6g/cm3的氢化碳氧化硅,和每一交替的阻挡层独立地选自密度为至少1.6g/cm3的氢化碳氧化硅、铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛,条件是至少一层交替的阻挡层选自铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛。
[0010]本发明还涉及一种涂布的基片,其包括:
基片;
在基片上的第一缓冲层,其中第一缓冲层包括密度小于1.6g/cm3的氢化碳氧化硅;和
在第一缓冲层上的至少三层交替的阻挡层和缓冲层,其中每一交替的阻挡层独立地选自密度为至少1.6g/cm3的氢化碳氧化硅、铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛,和每一交替的缓冲层包括密度小于1.6g/cm3的氢化碳氧化硅,条件是至少一层交替的阻挡层是密度为至少1.6g/cm3的氢化碳氧化硅,和至少一层交替的阻挡层选自铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛。
[0011]所述涂布的基片中的阻挡层具有低的水蒸气传输速率,典型地为10-1-10-3g/m2/天。此外,阻挡层对氧气和金属离子,例如铜和铝,具有低的渗透性。此外,阻挡层具有高的抗龟裂性和低的压缩应力。进一步地,与常规的碳氧化硅膜相比,含氢化碳氧化硅的阻挡层具有更高的密度和更低的孔隙率。
[0012]可使用常规的设备和技术进行本发明的方法。例如,可分别使用化学气相沉积和双频化学气相沉积,来沉积缓冲和阻挡层中的氢化碳氧化硅。此外,可使用常规的物理气相沉积技术,例如蒸发(热和电子束)、RF溅射和DC磁控管溅射,来沉积铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛的阻挡层。
[0013]本发明的阻挡层可用作许多器件中的层间电介质和/或对湿气和氧气的阻挡层,其中所述器件包括半导体器件、液晶、发光二极管、有机发光二极管、光电器件、光学器件、光生伏打电池、薄膜电池和太阳能电池。
附图简述
[0014]图1示出了本发明的涂布的基片的第一实施方案的截面视图。
[0015]图2示出了本发明的涂布的基片的第二实施方案的截面视图。
发明详述
[0016]如图1所示,本发明的涂布的基片的第一实施方案包括基片100;在基片100上的第一阻挡层102,其中第一阻挡层102包括密度为至少1.6g/cm3的氢化碳氧化硅;和在第一阻挡层102上的至少两层(示出了四层)交替的缓冲层104和阻挡层106,其中每一交替的缓冲层104包括密度小于1.6g/cm3的氢化碳氧化硅,且每一交替的阻挡层106独立地选自密度为至少1.6g/cm3的氢化碳氧化硅、铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛,条件是至少一层交替的阻挡层106选自铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛。涂布的基片的第一实施方案典型地包括在第一阻挡层上的2-16或者4-10层交替的缓冲层和阻挡层。
[0017]基片可以是具有平面、复杂或不规则轮廓的刚性或挠性材料。此外,基片可以透过或者不透过电磁光谱中可见光区域内的光(~400到~700nm)。此处所使用的术语“透过”是指对于电磁光谱中可见区域内的光来说,基片的透光率为至少30%,或者至少60%,或者至少80%。此外,术语“不透过”是指对于电磁光谱中可见区域内的光来说,基片的透光率小于30%。
[0018]基片的实例包括但不限于:半导体材料,例如硅、具有二氧化硅表面层的硅,和砷化镓;石英;熔凝石英;氧化铝;陶瓷;玻璃;金属箔;聚烯烃,例如聚乙烯、聚丙烯、聚苯乙烯、聚对苯二甲酸乙二酯(PET)和聚萘二甲酸乙二酯;氟烃聚合物,例如聚四氟乙烯和聚氟乙烯;聚酰胺,例如尼龙;聚酰亚胺;聚酯,例如聚(甲基丙烯酸甲酯);环氧树脂;聚醚;聚碳酸酯;聚砜;和聚醚砜。基片可以是单一的材料或者是含两种或更多种不同材料的复合材料。
[0019]第一阻挡层包括典型地在25℃下密度为至少1.6g/cm3,或者至少1.7g/cm3,或者至少1.8g/cm3的氢化碳氧化硅。典型地,阻挡层中的氢化碳氧化硅在25℃下的密度为1.7-2.5g/cm3,或者1.7-2.0g/cm3,或者1.8-2.0g/cm3。可通过测量沉积物的质量、厚度和表面积来容易地测定氢化碳氧化硅的密度。
[0020]第一阻挡层中的氢化碳氧化硅含有硅、氧、碳和氢。例如,氢化碳氧化硅可用通式SimOnCpHq表示,其中m的值为10-33原子%,或者18-25原子%;n的值为1-66原子%,或者10-20原子%;p的值为1-66原子%,或者15-38原子%;q的值为0.1-60原子%,或者25-40原子%,和m+n+p+q=100原子%。
[0021]第一阻挡层的厚度典型地为0.2-10微米,或者0.2-5微米,或者0.2-2微米。当第一阻挡层的厚度小于0.2微米时,该层的水蒸气传输速率典型地增加。当第一阻挡层的厚度大于10微米时,该层可易于龟裂。
[0022]对电磁光谱中可见光区域内的光(~400到~700nm)来说,第一阻挡层的透光率典型地为至少30%,或者至少50%,或者至少70%。例如,在厚度为150微米的聚对苯二甲酸乙二酯上的厚度为1微米的阻挡层典型地为至少70%。
[0023]可通过将包括含硅化合物、氩气和氧气的反应性气体混合物引入到含基片的沉积腔室内,其中含硅化合物选自至少一种硅烷,至少一种硅氧烷及其混合物,氩气的流量与含硅化合物的流量之比为10-30,氧气的流量与含硅化合物的流量之比为0.15-1.0,基片温度为20-80℃,和压力为1.33-60Pa;施加RF功率到所述气体混合物上,生成等离子体,其中RF功率为300-1000W;和施加LF功率到基片上,其中LF功率为50-120W,以便在基片上沉积包含密度为至少1.6g/cm3的氢化碳氧化硅的第一阻挡层,从而沉积第一阻挡层。
[0024]在本发明方法的第一步中,包括含硅化合物、氩气和氧气的反应性气体混合物引入到含基片的沉积腔室内,其中含硅化合物选自至少一种硅烷,至少一种硅氧烷及其混合物,氩气的流量与含硅化合物的流量之比为10-30,氧气的流量与含硅化合物的流量之比为0.15-1.0,基片温度为20-80℃,和压力为1.33-60Pa。
[0025]所述反应性气体混合物中的含硅化合物选自至少一种硅烷、至少一种硅氧烷及其混合物。硅烷的实例包括但不限于:含甲基的硅烷,例如甲基硅烷、二甲基硅烷、三甲基硅烷和四甲基硅烷;和烷氧基硅烷,例如二甲氧基二甲基硅烷、三甲氧基甲基硅烷、四甲氧基硅烷、三乙氧基甲基硅烷、二乙氧基二甲基硅烷、三乙氧基甲基硅烷、三乙氧基乙烯基硅烷、四乙氧基硅烷、二甲氧基甲基苯基硅烷、三甲氧基苯基硅烷、3-环氧丙氧丙基三甲氧基硅烷、3-甲基丙烯酰氧基丙基三甲氧基硅烷、二乙氧基甲基苯基硅烷、三(2-甲氧基乙氧基)乙烯基硅烷、三乙氧基苯基硅烷和二甲氧基二苯基硅烷。硅氧烷的实例包括但不限于:四甲基二硅氧烷、六甲基二硅氧烷和四乙氧基硅烷。含硅化合物可以是单一的硅烷,两种或更多种不同硅烷的混合物,单一的硅氧烷,两种或更多种不同的硅氧烷的混合物,或者至少一种硅烷和至少一种硅氧烷的混合物。
[0026]可使用在双频模式下操作的常规平行板化学气相沉积系统,来进行本发明的方法。在这一系统中,沉积腔室含有与射频(RF)功率源相连的顶电极,典型地为喷头,和与低频(LF)功率源相连的底电极,典型地为基片座。RF功率源在1-20MHz的频率下典型地提供10-1000W的功率。在CVD体系中通常使用13.56MHz的RF频率。LF功率源在325-375KHz的频率下典型地提供10-1200W的功率。此外,典型地使用滤波,以最小化两个信号之间的相互作用。例如,典型地使用感应器和电容器,使所述顶电极和底电极分别接地。
[0027]含硅化合物的流量典型地为20-150sccm(标准立方厘米/分钟),或者30-120sccm,或者30-80sccm。
[0028]氩气的流量典型地为200-1500sccm,或者300-1200sccm,或者300-800sccm。
[0029]氧气的流量典型地为5-100sccm,或者5-60sccm,或者5-40sccm。
[0030]氩气的流量与含硅化合物的流量之比典型地为10-30,或者10-20,或者10-15。当氩气的流量与含硅化合物的流量之比大于30sccm时,可能出现基片温度的显著增加。
[0031]氧气的流量与含硅化合物的流量之比典型地为0.15-1.0,或者0.5-1.0,或者0.5-0.8。当氧气的流量与含硅化合物的流量之比小于0.15时,阻挡层可能主要包括碳化硅。当氧气的流量与含硅化合物的流量之比大于1.0时,该层的水蒸气的传输速率典型地增加。
[0032]基片温度典型地为20-80℃,或者25-50℃,或者25-40℃。
[0033]沉积压力典型地为1.33-60Pa,或者1.33-25Pa,或者1.33-15Pa。当压力大于60Pa时,该层的水蒸气的传输速率典型地增加。
[0034]在本发明方法的第二步中,施加RF功率到气体混合物中,以产生等离子体,其中RF功率为300-1000W。或者,RF功率为400-800W或者400-600W。
[0035]在本发明方法的第三步中,施加LF功率到基片上,其中LF功率为50-120W,以在基片上产生密度为至少1.6g/cm3的第一阻挡层。或者,LF功率为60-100W或者65-85W。
[0036]每一交替的缓冲层包括典型地在25℃下密度小于1.6g/cm3或者小于1.4g/cm3的氢化碳氧化硅。典型地,交替的缓冲层中的氢化碳氧化硅的密度在25℃下为1.0-1.5g/cm3,或者1.1-1.5g/cm3,或者1.2-1.5g/cm3。可通过测量沉积物的质量、厚度和表面积,来容易地确定氢化碳氧化硅的密度。
[0037]除了其阻挡性能以外,交替的缓冲层还提供交替的阻挡层可沉积在其上的光滑的表面。此外,交替的缓冲层降低涂布的基片的压缩应力。
[0038]交替的缓冲层中的氢化碳氧化硅含有硅、氧、碳和氢,且可用以上对于第一阻挡层中的氢化碳氧化硅给出的通式表示。
[0039]交替的缓冲层的厚度典型地为0.2-10微米,或者0.2-5微米,或者0.2-2微米。当交替的缓冲层的厚度小于0.2微米时,缓冲层不可能提供充分覆盖底下的阻挡层。当交替的缓冲层的厚度大于10微米时,该层易于龟裂。
[0040]对于电磁光谱中的可见区域内的光(~400到~700nm)来说,交替的缓冲层的透光率典型地为至少60%,或者至少70%,或者至少80%。例如,在厚度为150微米的聚对苯二甲酸乙二酯基片上的厚度为1微米的缓冲层的透光率典型地为至少80%。
[0041]沉积密度小于1.6g/cm3的氢化碳氧化硅的交替缓冲层的方法是本领域已知的,如在Loboda等人的美国专利No.6159871、Loboda的WO02/054484A2、Hu等人的美国专利No.5718967和Thomas等人的美国专利No.5378510中所例举的。例如,可通过如美国专利No.6159871中所述的化学气相沉积方法,来沉积密度最高约为1.4g/cm3的氢化碳氧化硅膜。简而言之,这一方法牵涉将包括含甲基的硅烷和提供氧的气体的反应性气体混合物引入到含基片的沉积腔室内,并在25-500℃的温度下诱导所述含甲基的硅烷和提供氧的气体之间的反应;其中在反应过程中存在控制量的氧气,以便在基片上提供介电常数为小于或等于3.6的含氢、硅、碳和氧的膜。含甲基的硅烷的实例包括甲基硅烷、二甲基硅烷、三甲基硅烷和四甲基硅烷。提供氧的气体的实例包括但不限于:空气、臭氧、氧气、一氧化二氮和一氧化一氮。
[0042]可通过选择提供氧的气体的类型和/或用量,来控制在沉积工艺过程中存在的氧的含量。以1体积份含甲基的硅烷计,提供氧的气体的浓度典型地小于5体积份,或者0.1-4.5体积份。当氧的浓度太高时,该工艺将形成化学计量接近于SiO2的氧化硅膜。当氧的浓度太低时,该工艺将形成化学计量接近于SiC的碳化硅膜。可通过常规试验容易地确定对于特定的应用来说含氧气体的最佳浓度。
[0043]可通过将包括含硅化合物、氩气和氧气的反应性气体混合物引入到含有具有阻挡层的基片的沉积腔室内,从而制备密度介于1.4至1.6g/cm3的氢化碳氧化硅膜,其中含硅化合物选自至少一种硅烷、至少一种硅氧烷及其混合物,氩气的流量与含硅化合物的流量之比为1-10,氧气的流量与含硅化合物的流量之比为0.5-2.0,基片温度为25-50℃,和压力为5-40Pa;施加RF功率到气体混合物上,以生成等离子体,其中RF功率为150-300W;和施加LF功率到基片上,其中LF功率为15-30W。
[0044]每一交替的阻挡层独立地选自密度为至少1.6g/cm3的氢化碳氧化硅,铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛,条件是至少一层交替的阻挡层选自铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛。此处所使用的术语“交替的阻挡层”是指密度为至少1.6g/cm3的氢化碳氧化硅的单一层;铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛或氮氧化钛的单一层;或者两层或更多层不同的层,其中各层选自铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛。
[0045]交替的阻挡层的厚度典型地为0.2-10微米,或者0.2-5微米,或者0.2-2微米。当交替的阻挡层的厚度小于0.2微米时,该层的水蒸气传输速率典型地增加。当交替的阻挡层的厚度大于10微米时,该层易于龟裂。
[0046]氢化碳氧化硅的交替的阻挡层及其沉积方法如上述对于第一阻挡层所述。铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛的单独的层的厚度典型地为0.2-3微米,或者0.2-2微米,或者0.2-1微米。可使用常规方法,例如热蒸发、共蒸发、RF溅射和DC磁控管溅射,来沉积这些金属、合金和氧化物的阻挡层。
[0047]如图2所示,本发明的涂布的基片的第二实施方案包括基片200;在基片200上的第一缓冲层202,其中第一缓冲层202包括密度小于1.6g/cm3的氢化碳氧化硅;和在第一缓冲层202上的至少三层(示出了四层)交替的阻挡层204和缓冲层206,其中每一交替的阻挡层204独立地选自密度为至少1.6g/cm3的氢化碳氧化硅、铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛,和每一交替的缓冲层206包括密度小于1.6g/cm3的氢化碳氧化硅,条件是至少一层交替的阻挡层204是密度为至少1.6g/cm3的氢化碳氧化硅,和至少一层交替的阻挡层204选自铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛。
[0048]涂布的基片的第二实施方案典型地包括在第一缓冲层上的3-10或者3-5层交替的阻挡层和缓冲层。除了它们的阻挡性能以外,第一缓冲层和交替的缓冲层提供交替的阻挡层可沉积在其上的光滑的表面。此外,第一缓冲层和交替的缓冲层降低涂布的基片的压缩应力。
[0049]每一交替的阻挡层和每一交替的缓冲层如以上对于涂布的基片的第一实施方案所述。此外,第一缓冲层如以上对于第一实施方案中的交替的缓冲层所述。此外,可使用以上对于第一实施方案所述的那些方法来沉积第二实施方案中的阻挡层和缓冲层。
[0050]涂布的基片的阻挡层具有低的水蒸气传输速率,典型地为10-1-10-3g/m2/天。此外,阻挡层对氧气和金属离子,例如铜和铝,具有低的渗透率。此外,阻挡层具有高的抗龟裂性和低的压缩应力。进一步地,与常规的碳氧化硅膜相比,包含氢化碳氧化硅的阻挡层具有更高的密度和更低的孔隙率。
[0051]可使用常规的设备和技术进行本发明的方法。例如,可分别使用化学气相沉积和双频化学气相沉积,来沉积缓冲和阻挡层中的氢化碳氧化硅。此外,可使用常规的物理气相沉积技术,例如热蒸发、RF溅射和DC磁控管溅射,来沉积铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛的阻挡层。
[0052]本发明的阻挡层可用作许多器件中的层间电介质和/或对湿气和氧气的阻挡层,其中所述器件包括半导体器件、液晶、发光二极管、有机发光二极管、光电器件、光学器件、光生伏打电池、薄膜电池和太阳能电池。
实施例
[0053]提供下述实施例以更好地阐述本发明的涂布的基片和方法,但不被视为限制所附权利要求书描述的本发明的范围。
[0054]使用在25℃的基片温度和0.09Torr(12.0Pa)的压力下在双频模式下操作的获自Applied Process Technologies(Tucson,Az)的Model No.2212 HDP平行板化学气相沉积系统,与顶电极(喷头)相连的RF功率源和与底电极(基片座)相连的LF功率源,来沉积实施例中的包含氢化碳氧化硅的缓冲层和阻挡层。
[0055]在制备每一涂布的基片之前,通过使用在40Pa的压力下由CF4和O2生成的等离子体,500sccm的CF4流量,100sccm的O2流量,40W的LF功率和500W的RF功率,首先等离子体蚀刻腔室的内表面5-10分钟,来彻底清洁沉积腔室。在等离子体蚀刻之后,用异丙醇擦拭腔室壁。
[0056]通过DC磁控管溅射,以约0.02-0.05μm/min的速度来沉积实施例中的包含钛、铝和氮化钛的阻挡层。
[0057]在12.0Pa的压力下,500sccm的氩气流量、40W的LF功率和300W的RF功率下,用氩气等离子体处理实施例中的(涂布和未涂布的)聚对苯二甲酸乙二酯(PET)基片30秒。
[0058]使用MOCON PERMATRAN-W Permeation Test System,在37.8℃的温度和90%的相对湿度下,测定涂布和未涂布的PET基片的水蒸气传输速率(WVTR)。在扩散池内夹紧涂布的PET试样,然后用不含湿气的氮气(10sccm)吹扫,直到建立稳定的水蒸气传输速率。
[0059]使用Tencor FLX-2320(KLA Tencor,Milpitas,CA)ThinFilm Stress Measurement System,在氮气氛围下,在18-22℃的温度下,测量涂布的PET基片的压缩应力。
[0060]通过测量在直径为10.2cm的圆形基片上沉积的膜的质量、厚度和表面积,来测定包含氢化碳氧化硅的缓冲层和阻挡层的密度。通过在环境条件(25℃,101.3kPa)下,使用精度为1×10-5g的分析天平来测量层的质量。
[0061]使用在环境条件下操作的Spectroscopic Ellipsometer(J.A.Woollam Co.,Inc.,Lincoln,NE),来测定膜的厚度和折射指数。通过在直径为10.2cm和电阻率大于5Ω·cm的p-Si晶片上沉积膜,从而制备试样。
实施例1-3
[0062]在实施例1和2的每一个中,使用表1所示的工艺条件,制备具有下述多层结构的涂布的基片:
实施例1:PET/缓冲层/阻挡层A/缓冲层/阻挡层A/缓冲层/阻挡层B/缓冲层
实施例2:PET/缓冲层/阻挡层A/缓冲层/阻挡层A/缓冲层/阻挡层C/缓冲层
其中PET是指直径为20cm和厚度为175微米的等离子体处理的聚对苯二甲酸乙二酯的圆形片材(参见上面),缓冲层是指密度为1.5g/cm3的氢化碳氧化硅的缓冲层;阻挡层A是指密度为1.9g/cm3的氢化碳氧化硅的阻挡层;阻挡层B是指由在底下的缓冲层上的钛层(~300nm)和在钛层上的铝层(~300nm)组成的阻挡层;和阻挡层C是指由在底下的缓冲层上的氮化钛层(~300nm)和在氮化钛层上的铝层(~300nm)组成的阻挡层。在实施例3中,测量直径为10cm和厚度为175微米的未涂布的等离子体处理的基片的水蒸气传输速率(WVTR),并与实施例1和2的涂布的基片相比较。表1中示出了涂布的基片的缓冲层和阻挡层的性能,和表2示出了未涂布和涂布的基片的性能。
表1
TMS是三甲基硅烷,LF是低频,RF是射频,DR是沉积速率,T是平均厚度,RI是折射指数,应力是指压缩应力,和d是密度。
表2
WVTR是水蒸气传输速率,涂层厚度是指缓冲层和阻挡层结合的总厚度,和未涂布是指未涂布的PET基片。
Claims (10)
1.一种涂布的基片,其包括:
基片;
在基片上的第一阻挡层,其中第一阻挡层由密度为至少1.6g/cm3的氢化碳氧化硅组成;和
在第一阻挡层上的至少两层交替的缓冲层和阻挡层,其中每一交替的缓冲层由密度小于1.6g/cm3的氢化碳氧化硅组成,和每一交替的阻挡层独立地选自密度为至少1.6g/cm3的氢化碳氧化硅、铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛,条件是至少一层交替的阻挡层选自铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛。
2.权利要求1的涂布的基片,其中涂布的基片包括在第一阻挡层上的2-16层交替的缓冲层和阻挡层。
3.权利要求1的涂布的基片,其中第一阻挡层和交替的阻挡层中的氢化碳氧化硅的密度为1.7-2.5g/cm3。
4.权利要求1的涂布的基片,其中第一阻挡层以及交替的缓冲层和阻挡层各自的厚度为0.2-10微米。
5.权利要求1的涂布的基片,其中交替的缓冲层中的氢化碳氧化硅的密度为1.0-1.5g/cm3。
6.一种涂布的基片,其包括:
基片;
在基片上的第一缓冲层,其中第一缓冲层由密度小于1.6g/cm3的氢化碳氧化硅组成;和
在第一缓冲层上的至少三层交替的阻挡层和缓冲层,其中每一交替的阻挡层独立地选自密度为至少1.6g/cm3的氢化碳氧化硅、铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛,和每一交替的缓冲层由密度小于1.6g/cm3的氢化碳氧化硅组成,条件是至少一层交替的阻挡层是密度为至少1.6g/cm3的氢化碳氧化硅,和至少一层交替的阻挡层选自铝、氧化铝、氮化铝、氮氧化铝、钛、氧化钛、氮化钛和氮氧化钛。
7.权利要求7的涂布的基片,其中涂布的基片包括在第一缓冲层上的3-10层交替的阻挡层和缓冲层。
8.权利要求7的涂布的基片,其中第一缓冲层和交替的缓冲层中的氢化碳氧化硅的密度为1.0-1.5g/cm3。
9.权利要求7的涂布的基片,其中第一缓冲层以及交替的阻挡层和缓冲层各自的厚度为0.2-10微米。
10.权利要求1的涂布的基片,其中交替的阻挡层中的氢化碳氧化硅的密度为1.7-2.5g/cm3。
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EP (2) | EP1799883A2 (zh) |
JP (1) | JP4987717B2 (zh) |
KR (1) | KR101210859B1 (zh) |
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