CN1792929A - 用于生产高折射率层的汽相沉积材料 - Google Patents
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Abstract
本发明涉及包含Ta2Ox，其中x＝4.81～4.88的汽相沉积材料，这种汽相沉积材料的制备方法，以及该材料在生产高折射率层方面的应用。
Description
本发明涉及包含Ta2Ox、其中x＝4.81～4.88的汽相沉积材料，制备这种汽相沉积材料的方法以及该材料在生产高折射率层中的应用。
为了保护表面或者为了获得特定的光学性质，光学元件通常被镀覆薄膜。此类光学元件是，例如，光学透镜、眼镜片、照相机镜头、双目望远镜或用于其他光学器件的光束分离器、棱镜、镜子、窗玻璃等。涂层主要是处理所述表面，通过硬化和/或提高耐化学品性来降低成防止因机械、化学或环境影响所带来的损害，但是经常地也被用来实现低反射，后者特别是用于眼镜片和照相机镜头的情况。
在这一点上，氧化钽(V)(Ta2O5)是一种已知并经常被用来生产高折射率层的材料。通常通过真空蒸发来涂覆Ta2O5层。在该方法中，首先将需要涂覆的基底和含有Ta2O5的容器放置在适当的高真空汽相沉积设备中，随后将该设备抽真空，并通过加热和/或电子束轰击导致汽相沉积物质蒸发，伴有汽相沉积材料沉淀在基底表面上而形成薄层。相应的设备和工艺都是常规的现有技术。
上述方法中的缺点在于Ta2O5在熔化和蒸发时释放出较大量的氧气。这通常发生直到形成分子式为Ta2O5-x，其中x＝0.2～0.4的组成为止。确切的组成主要取决于蒸发过程中物质的温度。氧气的释放引起汽相沉积单元的压力升高，这会极大地依赖反应条件并会导致蒸发终止。
为防止蒸发过程中压力的这种升高，通常在预处理步骤中将Ta2O5预熔化。为了这一目的，将一定量的Ta2O5放置在容器中，Ta2O5在减压下熔化，并允许熔化物冷却。接着，同样为了用上述处理步骤进行预熔化，进一步将Ta2O5放置在容器中。反复进行该步骤，直到获得所需数量的用于蒸发过程的熔化材料。根据熔化温度和熔化持续的时间，所得汽相沉积材料具有的组成为Ta2O4.6～Ta2O4.8。预熔化是一个昂贵且持续很久的过程，因而不适合供应相对大量的汽相沉积材料。
US4156622公开了在太阳能电池上的Ta2O5和元素钽混合物的电子束蒸发能获得分子式为Ta2Oy的钽的低价氧化物，其中y＝2.5～4.8，优选y＝3.3～4.5。但是，由于混合物中的局部非均一性导致各种组成的钽的低价氧化物的沉积，如果要获得均一组成的层—如果可行的话，证明上述方法是不利的。因此，采用上述方法不能实现层组成的特定控制。
JP04-325669描述了一种Ta比例在4～55％重量百分比的Ta2O5和Ta的烧结混合物。这相当于分子式为Ta2O2～Ta2O4.6的钽的低价氧化物。获得的钽的低价氧化物通过电子束蒸发应用于基底上。JP62-207937公开了Ta2O5与Ta的比为9∶1的Ta2O5/Ta烧结混合物。这相当于根据分子式Ta2O4.73的组成。
但是，由于其汽相沉积层经常在光谱的可见区表现出吸收，采用上述组成的钽的低价氧化物被证明是不利的。这一效果是不希望的并且只能通过在400℃左右的空气中进行后续的涂覆加热来消除。这意味着需要消耗能量进行额外的步骤，并且这还会延长所需层的生产过程。另一个避免形成吸收层的方法是采用包括在其中形成电离氧的离子或等离子支持的汽相沉积过程。所需的这些特殊方法和设备是非常复杂且昂贵的，并且为得到所需结果还需要精确的过程控制。因而这些方法不适宜大规模的工业应用。
大量研究表明提高汽相沉积材料中的氧含量有利于形成非吸收层。相反，过高的氧含量导致上述不希望的压力升高。因而，本发明的目的是提供能够克服这一矛盾而又无需改变现行蒸发过程的汽相沉积材料。
利用本发明的汽相沉积材料，可以创造性地实现本发明的目的。本发明因此涉及包含x＝4.81～4.88的Ta2Ox汽相沉积材料。本发明还涉及可通过混合Ta2O5和按混合物重量计1.9～3.1％的Ta、压实或悬浮、成型以及随后在减压下烧结混合物而获得的包含x＝4.81～4.88的Ta2Ox的汽相沉积材料。
本发明还涉及一种制备本发明汽相沉积材料的方法，其中Ta2O5与按混合物重量计1.9～3.1％的Ta混合，将混合物压实或悬浮、成型并随后在减压下烧结。
本发明同样涉及本发明的汽相沉积材料在生产高折射率层方面的应用。
本发明的汽相沉积材料在很多方面占有优势。用来制备汽相沉积材料的Ta2O5和Ta的混合物在形成均匀而致密的熔体的熔化过程中表现出很好的性能。要获得均匀的涂层并且涂层的组成不发生变化，这一点尤为重要。使用本发明的汽相沉积材料，采用电子束蒸发，不需要经过其他的后处理获得了非吸收层。同时，在汽相沉积材料的蒸发中仅观察到少许的压力升高，也就是仅有少量的氧释放出来并且能简单而改善地控制和保持所需的工艺参数。在本发明的汽相沉积材料中，钽与氧的特定比例使得结合上述优点完全成为可能，因而对本发明是必要的。
本发明的汽相沉积材料包含Ta2Ox，其中x＝4.81～4.88；该汽相沉积材料优选包括Ta2O4.82。后者可通过将Ta2O5和按混合物重量计3％的Ta混合、压实或悬浮、成型及随后在减压下烧结混合物而得到。令人惊奇地发现，这种组成的汽相沉积材料特别适合生产高折射率的非吸收层。
在根据本发明制备上述汽相沉积材料的方法中，Ta2O5和按混合物重量计1.9～3.1％的Ta混合，混合物经压实或悬浮、成型及随后在减压下烧结。为制备包含Ta2O4.82的优选方案，Ta2O5和按混合物重量计3％的Ta混合，混合物经压实或悬浮、成型及随后在减压下烧结。
上述Ta2O5和Ta的混合物通过本身已知的适当压实措施压制和成型。但是，在适当的载体介质中制备混合组分的悬浮体也是可行的，该悬浮体被成型并随之被干燥。适当的载体介质为，例如水，如果需要，向其中加入诸如聚乙烯醇、甲基纤维素或聚乙二醇之类的粘合剂(binder)，及加入任选的诸如例如润湿剂或消泡剂之类的助剂。之后，将悬浮体成型。在此，可以使用各种已知技术，如挤压、注塑或喷雾干燥。将所得成型物干燥并脱除粘合剂，例如烧尽。为了便于混合物更好的可操作性和可计量性而采用该方法。所以对混合物的形状没有要求。适宜的形状是所有那些利于简单操作和良好计量的形状，这一点特别重要，尤其是采用本发明的汽相沉积材料对基底进行连续涂覆时，为此需要补足(topping-up)工序。优选的形状是各种片状、丸、盘、截头圆锥、细粒或颗粒、棒或者还有球。
随后烧结成型的混合物。烧结过程在1300～1800℃下减压进行，并且残余压力低于1Pa，优选的温度在1400～1700℃。
烧结好的成型制品在存储、运输及输送到蒸发设备的过程中形状保持不变并且其组成在随后的熔化和蒸发过程是稳定的。
本发明同样涉及汽相沉积材料在生产高折射率层方面的应用。可将本发明的汽相沉积材料涂覆在任何适当的基底上，特别是盘、棱柱、薄膜状基底，诸如由已知适当材料如各种玻璃或塑料组成的光学透镜、眼镜片和物镜及类似物。只要能将基底输送到真空设备中并且在通常的温度和压力环境下保持稳定，应用本发明的汽相沉积材料就根本不受待涂覆的基底性质、尺寸、形状、材料和表面条件方面的任何限制。但是，为提高涂覆层的密度，已经证明有利的措施是在涂覆前和涂覆过程中加热基底，以使汽相沉积材料碰撞预热的基底。根据其性质，将所用基底加热到最高300℃。而这种方法本身是已知的。
所用的汽相沉积过程通常是一个高真空的汽相沉积过程，其中装在适当容器(也称为蒸发坩埚或蒸发舟皿)中的汽相沉积材料与需涂覆的基底一起送至真空设备中。
随后，将设备抽真空，进行加热和/或电子束轰击，引起汽相沉积材料的蒸发。在这一过程中，汽相沉积材料以薄层的形式沉淀在基底上。
使用本发明的汽相沉积材料无需采用复杂的涂覆方法，例如离子轰击(离子辅助沉积，等离子辅助沉积)。这降低了设备的复杂度，从而在获得优质高折射率层的同时降低了涂覆成本。
下面的实施例意在更详细地解释本发明，而不对其进行限制。
实施例
实施例1：汽相沉积材料的制备
将97wt％的氧化钽(Ta2O5)和3wt％的Ta金属粉末加水后在球磨机中强力混合。之后，将混合物干燥并转化为粒径为1～4mm的颗粒。在压力低于1×10-4mbar的真空下以1K/min的加热速率将颗粒在高温真空炉中加热到1650℃，并保温32小时。随后，以5K/min的速率冷却该材料。当冷却至25℃后，将真空炉充满空气，并移出该材料。所得汽相沉积材料由成分为Ta2O4.82的硬质深黑色颗粒组成。
实施例2：汽相沉积材料在生产高折射率层方面的应用
在可从商业获得的汽相沉积装置(来自Leybold的L560)中装入清洁的石英基底。将实施例1的汽相沉积材料加入电子束蒸发装置的水冷铜制坩埚中。将汽相沉积装置抽真空至压力为1×10-5mbar。然后将基底加热温度设定在200℃。1小时后，基底达到约160℃的均匀温度。随后，通过控制阀向装置中通入氧气直至压力达到2×10-4mbar。然后将汽相沉积材料在屏蔽下熔化并加热至蒸发温度。在熔化和蒸发过程中，压力未升高且未出现熔化微滴的飞溅。随后打开屏蔽。用振动石英层厚度测量仪将沉积速率调整到0.2nm/s。之后，物质以此汽相沉积速率蒸发，直至层厚达到230nm。然后结束蒸发。
汽相沉积材料涂覆层在500nm的折射率为2.05。涂层均匀，即整个层厚上折射率是常数。涂层在波长大于350nm的可见光区不发生吸收。吸收仅在从约300nm至紫外光区急剧增加。
Claims (11)
1、汽相沉积材料，包含Ta2Ox，其中x＝4.81～4.88。
2、汽相沉积材料，包含Ta2O4.82。
3、根据权利要求1的汽相沉积材料，可通过混合Ta2O5和按混合物重量计1.9～3.1％的Ta，压实或悬浮、成型并随之减压烧结混合物而获得。
4、根据权利要求2的汽相沉积材料，可通过混合Ta2O5和按混合物重量计3％的Ta，压实或悬浮、成型并随之减压烧结混合物而获得。
5、根据权利要求1至4的汽相沉积材料，其特征在于其为片、丸、盘、截头圆锥、细粒、颗粒、棒或者球状。
6、制备根据权利要求1的汽相沉积材料的方法，其特征在于将Ta2O5和按混合物重量计1.9～3.1％的Ta混合，将混合物压实或悬浮、成型并随之进行减压烧结。
7、根据制备权利要求2的汽相沉积材料的方法，其特征在于将Ta2O5和按混合物重量计3％的Ta混合，将混合物压实或悬浮、成型并随之进行减压烧结。
8、根据权利要求6和7的制备方法，其中烧结在1300～1800℃温度下减压进行。
9、根据权利要求6至8的制备方法，其中烧结在1400～1700℃温度下减压进行。
10、根据权利要求6至9的制备方法，其中将混合物成型为片、丸、盘、截头圆锥、细粒、颗粒、棒或者球状。
11、根据权利要求1至5之一的汽相沉积材料在生产高折射率层方面的应用。
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| DE102004049996A DE102004049996A1 (de) | 2004-10-14 | 2004-10-14 | Aufdampfmaterial zur Herstellung hochbrechender Schichten |
| DE102004049996.9 | 2004-10-14 |
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| CN110468378A (zh) * | 2019-09-12 | 2019-11-19 | 西安邮电大学 | 一种致密五氧化二钽薄膜的制备方法 |
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| DE102006036711B3 (de) * | 2006-08-05 | 2008-02-21 | Gfe Metalle Und Materialien Gmbh | Verfahren zur Herstellung oxidischer Beschichtungswerkstoffe auf der Basis von Refraktärmetallen |
| JP5284821B2 (ja) * | 2008-03-03 | 2013-09-11 | 東邦チタニウム株式会社 | 金属酸化物蒸着材、その製造方法、および金属酸化物蒸着膜の製造方法 |
| JP5284822B2 (ja) * | 2008-03-03 | 2013-09-11 | 東邦チタニウム株式会社 | 酸化タンタル蒸着材、その製造方法、および酸化タンタル蒸着膜の製造方法 |
| JP5426136B2 (ja) * | 2008-10-16 | 2014-02-26 | 東邦チタニウム株式会社 | 酸化タンタル蒸着材、その製造方法、および酸化タンタル蒸着膜の製造方法 |
| CN107015297A (zh) | 2012-09-28 | 2017-08-04 | Hoya株式会社 | 眼镜镜片 |
| US11529230B2 (en) | 2019-04-05 | 2022-12-20 | Amo Groningen B.V. | Systems and methods for correcting power of an intraocular lens using refractive index writing |
| US11583389B2 (en) | 2019-04-05 | 2023-02-21 | Amo Groningen B.V. | Systems and methods for correcting photic phenomenon from an intraocular lens and using refractive index writing |
| US11583388B2 (en) | 2019-04-05 | 2023-02-21 | Amo Groningen B.V. | Systems and methods for spectacle independence using refractive index writing with an intraocular lens |
| US11678975B2 (en) | 2019-04-05 | 2023-06-20 | Amo Groningen B.V. | Systems and methods for treating ocular disease with an intraocular lens and refractive index writing |
| US11944574B2 (en) | 2019-04-05 | 2024-04-02 | Amo Groningen B.V. | Systems and methods for multiple layer intraocular lens and using refractive index writing |
| US11564839B2 (en) | 2019-04-05 | 2023-01-31 | Amo Groningen B.V. | Systems and methods for vergence matching of an intraocular lens with refractive index writing |
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| US4156622A (en) | 1976-11-10 | 1979-05-29 | Solarex Corporation | Tantalum oxide antireflective coating and method of forming same |
| JP3160309B2 (ja) | 1991-04-25 | 2001-04-25 | キヤノン株式会社 | 薄膜形成方法 |
| EP0852266B1 (en) * | 1995-08-23 | 2004-10-13 | Asahi Glass Ceramics Co., Ltd. | Target, process for production thereof, and method of forming highly refractive film |
| WO2000039039A2 (en) * | 1998-12-30 | 2000-07-06 | Corning Incorporated | Tantala doped optical waveguide and method of manufacture |
| JP4298067B2 (ja) * | 1999-06-23 | 2009-07-15 | キヤノンオプトロン株式会社 | 光学薄膜の成膜方法 |
| JP2002121048A (ja) * | 2000-10-11 | 2002-04-23 | Nippon Sheet Glass Co Ltd | 屈折率分布型レンズ用母材ガラス組成物 |
| TW200500311A (en) * | 2003-01-28 | 2005-01-01 | Koninkl Philips Electronics Nv | Transparent zirconium oxide-tantalum and/or tantalum oxide coating |
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| EP1648034B9 (de) | 2010-07-14 |
| CA2523327A1 (en) | 2006-04-14 |
| EP1648034A1 (de) | 2006-04-19 |
| DE102004049996A1 (de) | 2006-04-20 |
| JP5138881B2 (ja) | 2013-02-06 |
| US7598196B2 (en) | 2009-10-06 |
| EP1648034B1 (de) | 2009-12-30 |
| US20060088466A1 (en) | 2006-04-27 |
| TW200626734A (en) | 2006-08-01 |
| JP2006111974A (ja) | 2006-04-27 |
| KR20060054000A (ko) | 2006-05-22 |
| ATE453929T1 (de) | 2010-01-15 |
| DE502005008772D1 (de) | 2010-02-11 |
| KR101256659B1 (ko) | 2013-04-19 |
| CN1792929B (zh) | 2012-03-28 |
| ES2338663T3 (es) | 2010-05-11 |
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