CN108374153A - 一种磁控溅射生长大面积、高度有序纳米颗粒的方法 - Google Patents
一种磁控溅射生长大面积、高度有序纳米颗粒的方法 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5873—Removal of material
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Abstract
磁控溅射生长大面积、高度有序纳米颗粒的方法,对衬底进行清洗处理;亲水处理;将聚甲基丙烯酸支撑的多孔氧化铝薄膜模板(PMMA/AAO)转移至丙酮溶液中去除超薄多孔氧化铝的PMMA支撑层;将去除了PMMA支撑层的超薄多孔氧化铝转移至过氧化氢溶液中室温浸泡2至10小时进行亲水处理;将亲水处理后的超薄多孔氧化铝转移至丙酮溶液中,在丙酮溶液中将超薄多孔氧化铝转移至经亲水处理的衬底上并室温风干;将覆盖有多孔氧化铝的衬底固定于平行对着磁控溅射溅射源的衬底托上;采用磁控溅射生长相应材料;蒸镀完金属后,采用聚酰亚胺高温胶带揭除或采用5~10%的NaOH去除多孔氧化铝,获得大面积、高度有序纳米颗粒。
Description
一、技术领域
本发明具体涉及一种超薄多孔氧化铝辅助磁控溅射生长大面积高度有序金属、半导体、绝缘体、超导体纳米颗粒的方法,属于纳米材料制备技术领域。
二、背景技术
随着微加工技术的发展,纳米材料在诸多领域发挥着越来越重要的作用。金属纳米材料(金、银、铝、铜等)因其表面等离激元特性,在纳米光电集成、光学成像、生物传感、数据存储等领域获得了广泛应用;半导体纳米材料(如量子点、量子线和超晶格)具有许多奇异的光、电、敏感、催化等特性。
传统top-down制备图形化纳米结构技术纳米压印、电子束光刻、全息激光干涉法等在大面积制备纳米阵列上具有时间长、成本高等缺点,限制了诸多材料的产业化应用。因此需要在适当衬底上自组装所需要的结构与纳米材料阵列。多孔氧化铝模板是通过高纯铝片经一步或两步阳极氧化腐蚀制备的。模版孔径均匀,孔的直径可依据腐蚀电压的不同在5~500nm之间变化且易于大面积制备。有的研究者以多孔氧化铝为模板,采用EBE,PLD,CVD等方式生长纳米颗粒,或以生长的颗粒为掩膜,采用刻蚀的方式获得所需的纳米颗粒。这些方法工艺复杂且不利于大面积制备。磁控溅射技术则可制备大面积金属、半导体、绝缘体薄膜。
三、发明内容
本发明的目的是:提出一种磁控溅射生长大面积、高度有序纳米颗粒的方法,尤其是超薄多孔氧化铝辅助磁控溅射生长大面积高度有序金属、半导体、绝缘体、超导体纳米颗粒。
本发明的技术解决方案:一种磁控溅射生长大面积、高度有序纳米颗粒的方法,
依次采用丙酮、酒精、去离子水对衬底进行清洗;采用小功率氧气等离子体,或采用氢氟酸溶液浸泡,或采用紫外光表面处理机对清洗干净的衬底进行亲水处理;将PMMA/AAO(多孔氧化铝)转移至丙酮溶液中去除超薄多孔氧化铝的PMMA支撑层;将去除了PMMA支撑层的超薄多孔氧化铝转移至过氧化氢溶液(30wt%)中室温浸泡2至10小时以提高多孔氧化铝的亲水性;将亲水处理后的超薄多孔氧化铝转移至丙酮溶液中,在丙酮溶液中将超薄多孔氧化铝转移至经亲水处理的衬底上并室温风干;将覆盖有多孔氧化铝的衬底固定于平行对着磁控溅射溅射源的衬底托上;采用磁控溅射生长相应材料;蒸镀完金属后,采用聚酰亚胺高温胶带(kapton高温胶带)揭除或采用5~10wt%的NaOH去除多孔氧化铝,获得大面积、高度有序纳米颗粒。
所述多孔氧化铝的孔直径与膜厚比例为1:3~1:6;
所制备的纳米颗粒很好地继承了超薄多孔氧化铝模版的规律,纳米颗粒具有均匀的尺寸和距离分布。
所制备的纳米颗粒间隔在1nm至500nm之间。
尤其是所制备的纳米颗粒高度在1nm至30nm之间。
所制备的纳米颗粒包括金属和合金纳米颗粒(氮化钛、镍、钛、锌、铬、镁、铌、锡、铝、铟、铁、锆铝、钛铝、锆、铝硅、铜、钽、锗、银、钴、金、钆、镧、钇、铈、钨、不锈钢、镍铬、铪、钼、铁镍等)。
所制备的纳米颗粒包括半导体纳米颗粒(硅、碳化硅、氮化硅、氧化锌、硫化锌、碲化锌、锌镁氧、氧化镓、二氧化钛等)。
所制备的纳米颗粒包括金属氧化物绝缘体纳米颗粒(氧化铝、二氧化硅等)。
纳米颗粒可包括超导体纳米颗粒(二硒化碳、铁碲锡等)。
本发明的有益效果:本发明用多孔氧化铝模板与衬底经过各自的亲水处理后可以获得较强的结合力。这样制备的纳米颗粒很好地继承了超薄多孔氧化铝模版的规律,纳米颗粒具有均匀的尺寸和距离分布。所制备的纳米颗粒直径在10nm至500nm之间。或所制备的纳米颗粒间隔在10nm至400nm之间。或所制备的纳米颗粒高度在1nm至30nm之间。
多孔氧化铝大面积制备的可行性和磁控溅射的生长大面积薄膜材料的广泛应用使得超薄多孔氧化铝辅助磁控溅射生长大面积高度有序金属、半导体、绝缘体、超导体纳米颗粒成为可能。所制备的大面积高度有序亚波长金属纳米颗粒因其局域表面等离激元共振特性在光伏、光探测、光催化、表面增强拉曼散射等重多领域具有潜在应用。
四、附图说明
图1是本发明所述的超薄多孔氧化铝辅助磁控溅射生长大面积高度有序纳米颗粒的工艺示意图。包括三个步骤:(a)将亲水处理后的超薄多孔氧化铝转移至亲水处理后衬底,(b)磁控溅射生长材料,(c)多孔氧化铝模板的去除。
图2所示是采用不同孔径(a)孔径280nm,周期450nm,(b)孔径80nm,周期125nm多孔氧化铝模板辅助生长的TiN纳米颗粒的AFM结果。
图3所示(a)是采用孔径80nm,周期125nm多孔氧化铝模板辅助生长的TiN纳米颗粒的可见-近红外透射光谱,透射光谱显示了中心位于1145nm的透射谷,插图为采用FDTD模拟获得的TiN纳米颗粒的透射结果;(b)为理论模拟的TiN纳米颗粒表面及底部的电场分布情况,纳米颗粒间因局域表面等离激元共振产生较强的场增强。
五、具体实施方式
本发明提出了一种超薄多孔氧化铝辅助磁控溅射生长大面积、高度有序金属、半导体、绝缘体、超导体纳米颗粒的方法,下面通过具体工艺步骤进一步描述本发明:
(1)依次采用丙酮、酒精、去离子水对衬底进行清洗;衬底材料为硅片陶瓷或玻璃等;
(2)采用小功率氧气等离子体,或采用氢氟酸(不能用于玻璃)溶液浸泡,或采用紫外光表面处理机对清洗干净的衬底进行亲水处理;
(3)将PMMA/AAO(多孔氧化铝)转移至丙酮溶液中去除超薄多孔氧化铝的PMMA支撑层;
(4)将去除了PMMA支撑层的超薄多孔氧化铝转移至过氧化氢溶液(30wt%)中室温浸泡2至10小时以提高多孔氧化铝的亲水性;
(5)将亲水处理后的超薄多孔氧化铝转移至丙酮溶液中,在丙酮溶液中将超薄多孔氧化铝转移至经亲水处理的衬底上并室温风干;
(6)将覆盖有多孔氧化铝的衬底固定于平行对着磁控溅射溅射源的衬底托上;
(7)采用磁控溅射生长TiN纳米颗粒材料;磁控溅射采用Ti靶材,采用氮气气氛下蒸镀;如果采用其它材料制备,则是采用相应靶材,如钛,如果镍、钛、锌、铬、镁材料,但控制蒸镀的温度不同,物理热蒸镀是比较成熟的技术,此处不多述。
(8)蒸镀完金属后,采用聚酰亚胺高温胶带(kapton高温胶带)揭除多孔氧化铝模版,获得大面积、高度有序纳米颗粒。
本发明提出的超薄多孔氧化铝辅助磁控溅射生长大面积、高度有序金属、半导体、绝缘体、超导体纳米颗粒的方法,与传统top-down制备图形化纳米结构技术纳米压印、电子束光刻、全息激光干涉法等相比,采用超薄多孔氧化铝辅助磁控溅射生长大面积、高度有序金属、半导体、绝缘体、超导体纳米颗粒的方法具有制备工艺更为简单、制备周期更短、制备难度更低、制备成本更低等优点。
以上内容是结合具体的实施方式对本发明所作的进一步详细说明。本发明并不局限于上述实施方式,如果这些改动和变形属于本发明的权利要求和等同技术范围之内,则本发明也意图包含这些改动和变形。
Claims (7)
1.一种磁控溅射生长大面积、高度有序纳米颗粒的方法,其特征是步骤如下:对衬底进行清洗处理;亲水处理;将聚甲基丙烯酸支撑的多孔氧化铝薄膜模板(PMMA/AAO)转移至丙酮溶液中去除超薄多孔氧化铝的PMMA支撑层;将去除了PMMA支撑层的超薄多孔氧化铝转移至过氧化氢溶液中室温浸泡2至10小时进行亲水处理;将亲水处理后的超薄多孔氧化铝转移至丙酮溶液中,在丙酮溶液中将超薄多孔氧化铝转移至经亲水处理的衬底上并室温风干;将覆盖有多孔氧化铝的衬底固定于平行对着磁控溅射溅射源的衬底托上;采用磁控溅射生长相应材料;蒸镀完金属后,采用聚酰亚胺高温胶带揭除或采用5~10wt%的NaOH去除多孔氧化铝,获得大面积、高度有序纳米颗粒。
2.根据权利1的方法,其特征是衬底进行清洗处理指依次采用丙酮、酒精、去离子水对衬底进行清洗;对衬底采用小功率氧气等离子体,或采用氢氟酸溶液浸泡,或采用紫外光表面处理机对清洗干净的衬底进行亲水处理。
3.根据权利1的方法,其特征是将去除了PMMA支撑层的超薄多孔氧化铝转移至30wt%过氧化氢溶液中室温浸泡2至10小时进行亲水处理。
4.根据权利1的方法,其特征是所述多孔氧化铝的孔直径与膜厚比例为1:3~1:6。
5.根据权利1的方法,其特征是制备的纳米颗粒间隔在1nm至500nm之间。
6.根据权利5的方法,其特征是制备的纳米颗粒高度在1nm至30nm之间。
7.根据权利1的方法,其特征是所制备的纳米颗粒包括金属和合金纳米颗粒,即包括氮化钛、镍、钛、锌、铬、镁、铌、锡、铝、铟、铁、锆铝、钛铝、锆、铝硅、铜、钽、锗、银、钴、金、钆、镧、钇、铈、钨、不锈钢、镍铬、铪、钼、铁镍;
所制备的纳米颗粒还包括半导体纳米颗粒,即包括硅、碳化硅、氮化硅、氧化锌、硫化锌、碲化锌、锌镁氧、氧化镓、二氧化钛;
所制备的纳米颗粒包括金属氧化物绝缘体纳米颗粒,即包括氧化铝、二氧化硅;
或包括超导体纳米颗粒、即包括二硒化碳、铁碲锡。
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