CN1405241A - 混合氧化物型高折射率的涂料及方法 - Google Patents

混合氧化物型高折射率的涂料及方法 Download PDF

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CN1405241A
CN1405241A CN02142951A CN02142951A CN1405241A CN 1405241 A CN1405241 A CN 1405241A CN 02142951 A CN02142951 A CN 02142951A CN 02142951 A CN02142951 A CN 02142951A CN 1405241 A CN1405241 A CN 1405241A
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保罗·G·库姆斯
拉塞尔·E·德郎
夏洛特·R·拉加利
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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    • C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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Abstract

分子式是MNxOy的材料组合物，其中M，N是元素周期表IIIB、IVB和VB族的金属元素；O是氧；x和y的值要使氧与金属的比例和y/(1+x)的比值小于4。这种材料是以单一的氧化物相存在，并只有单一类型的晶体结构而检测不到第二种类型的晶体结构，该材料是低于化学计量的。

Description

混合氧化物型高折射率的涂料及方法
该申请是申请日为1996年5月6日、申请号为96194812.4、发明名称为“混合氧化物型高折射率的涂料及方法”的分案申请。
本发明涉及一种混合氧化物型的具有高折射率的涂料及方法。
美国专利No.3,034,924公开了镧系元素和过渡金属/金属氧化物的混合物。氧化锆是一种市场上可以买得到的高折射率的涂料。然而，这种材料在制作涂层时具有高熔点、高耗能以及不均匀等缺点。同时，氧化钛也可以用作高折射率的涂料。氧化钛涂层通常有不希望的吸收。氧化锆和氧化钛粉末的混合物在市场上也可以买到。然而，这种混合物是多相材料，因此不能产生一种相合的蒸发源。所以需要一种新型的、改进的、克服了这些缺点的混合氧化物型的具有高折射率的涂料。
概括地讲，本发明的一个目的是提供一种特别适用于抗反射涂层的混合氧化物型具有高折射率的涂料。
本发明的另一目的是提供一种能够在较低温度下熔化的具有上述特征的材料及方法。
本发明的再一目的是提供一种使其本身进行电子束蒸发的具有上述特征的材料和方法。
本发明的另一目的是提供可以用氧气活性蒸发以产生化学计量的材料的具有上述特征的材料及方法。
本发明的再一目的是提供一种提供坚硬及粘附的薄膜具有上述特征的材料及方法。
从下面结合附图的描述，本发明的其他目的及特点将会很明显。
图1是说明本发明方法的流程图。
就本发明而言，该材料的组合物的化学式为MNxOy，其中M和N是CAS元素周期表中IIIB、IVB和VB族的金属，其中O是氧，x和y的值的选择要使氧与金属的比例小于4以及y/(1+x)也小于4。更具体地说，M和N金属选自Sc、Y、La、Ce、Pr、Nd、Ac、Th、Pa、U、Ti、Zr、Hf、V、Nb和Ta。落入该类的材料的组成包括下列实例：YTixOy，HfIixOy和ZrNbxOy，因此可以看出：这种材料是由两种金属/金属氧化物组成的。但是，这种材料的组合物可很容易地由三种或更多的金属/金属氧化物组成。
在上述范围内的一种材料的具体组合物为ZrTixOy，其中x＝1.0，y＝2.0～3.9。当y的值在大于0和2.0之间时也可以形成其他材料。然而这些材料将是金属性的，当采用蒸发时，它们是很难生成ZrTiO4薄膜的。当x的值超过1.0时，该混合物中二氧化钛的含量增加，相图将变得更加复杂，这在材料组成低于化学计量时更加显著。当x值小于1.0时，材料开始表现出纯氧化锆的特性并且熔解温度升高，不具备本发明材料的典型优越性。
在本发明的一实施方案中，由重量比为15.6％的Ti、17.4％的TiO2和67.0％的ZrO2制备出一种均相混合物。该粉末状材料如图1中第11步中所示进行彻底混合。由上面的讨论可知，三种组分的重量百分比的选择使这种材料的分子式为ZrTiO2.8。当然，Ti、TiO2和ZrO2的比例可进行变化以给出分子式为ZrTiOy，其中y的范围可以是2.0～3.9。然后，将该粉末进行均相化和压片。
当如第12步所示压片形成后，再用合适的方法如第13步所示将其熔化，如用诱导炉或电子束炉。在熔化过程中，这三种成粉末状的组分反应生成一种单一的氧化物相。可以如第14步所示采用熔化步骤形成适当大小的锭，例如直径为5cm，长度为15～75cm。这种材料可以以这种铸锭形式贮存备用。或者，这些铸锭经压碎或打碎成大小为0.5～5mm的小颗粒，并且优选如图1中第16步所示的大约2mm。如果需要，这种压碎的材料也可以以这种形式贮存备用。
假设我们希望利用这种材料形成一层抗反射涂层，如1995年5月9日提交的共同待审的流水号为08/438,197的申请中所描述。在这一实施方案中，这种材料只有立方型的氧化锆晶体结构而没有检测到ZrTiO4的晶型结构。以颗粒形式存在的压碎的锭可以作为原料供应到传统类型的电子枪蒸发器以形成一层具有高折射率的抗反射涂层，如1995年5月9日提交的共同待审的流水号为08/438,197的申请中描述的那种类型。在材料蒸发过程中，导入过量的氧气进入涂敷装置的真空箱中，使得这种低于化学计量的材料用氧气活性蒸发以生成化学计量的涂层。
可以发现这种以ZrTiO2.8形式存在的压碎的锭状材料在大约1800℃时熔化，比纯的氧化锆熔点低约900℃。这种较低的熔解温度和沉积温度是非常有利的，因为有极少量的热量从热源辐射到基质上。例如，一个在1800℃辐射的热源所释放的热量不超过在2700℃辐射的热源所释放的总能量的1/4。本发明的材料的较低沉积温度可以使得以更快的速度施用涂料，并且可以将涂料施用到更薄的聚合物基质材料上，这是利用辊式涂覆器获得高生产率、低成本的抗反射涂料的明确的好处。与本发明的该实施方案相关的发现是：向这种混合物中加入更多的氧化钛可导致更低的熔解温度，例如该温度比未加入二氧化钛的熔解温度低至少约900℃。
这种材料的折射率大约是2.0。当与那种在1995年5月9日提交的共同待审的流水号为08/438,197的申请中描述的低折射率材料混合时，可以发现所形成的抗反射膜和由以氧化锆作为高折射率材料所制成的膜一样坚硬和粘附。
依照本发明制备的另一种材料的分子式是NbTi0.5O3，这一组成可概括成NbTi0.5Oy，其中y可以是在大于0和3.5之间。这种材料用与ZrTiOy相似的方法生产。从均相的Nb2O5、Ti和TiO2粉末压片后，熔化制成锭，然后压碎作为原料装进电子枪蒸发器。尽管Nb/Ti的比例可以不等于2，但选择NbTi0.5O3是因为它可以用氧气活性蒸发生成化学计量的NbTi0.5O3.5(Nb2TiO7)。这种材料的折光率在约2.0左右。当这种材料被用作抗反射涂层时，它具有理想的较低蒸发温度如1900℃，比Nb2O5的蒸发温度2100℃低200℃。
从前面可以看出，本文提供了一类新型的、改进的混合氧化物型的高折射率的光学涂料以及应用这种具有很多理想特点的涂料的方法。特别是，由于其蒸发所需的较低的温度，这种材料适用于辊涂操作。由于这种材料是单相材料而适用于电子枪蒸发，因此避免了破裂。另外，本文提供了一种坚硬、持久的材料，该材料特别适用于抗反射涂层。

Claims (6)

1.一种在基质表面生产光学涂层的方法，包括：取两种金属/金属氧化物的粉末，将它们混合成均匀混合物，将粉末的均相混合物压片，熔解该片，将熔解的片制成锭，把这些锭粉碎成小颗粒后，用氧气蒸发小颗粒以在基质表面生成一层光学涂层形式的化学计量的材料。
2.如权利要求1所述的方法，其中蒸发步骤是由电子束蒸发完成的。
3.如权利要求1所述的方法，其中蒸发步骤是由热蒸发完成的。
4.如权利要求1所述的方法，其中金属/金属氧化物用的粉末选自元素周期表中IIIB、IVB和VB族。
5.如权利要求1所述的方法，其中均匀混合的粉末压片要在混合物的熔点以上加热。
6.如权利要求1所述的方法，其中小颗粒加热到蒸发温度，并沉积在基质上。
CN02142951A 1995-05-09 2002-09-13 混合氧化物型高折射率的涂料及方法 Pending CN1405241A (zh)

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US08/438,198 US5641719A (en) 1995-05-09 1995-05-09 Mixed oxide high index optical coating material and method
US08/438,198 1995-05-09

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CN1096438C (zh) 2002-12-18
KR100252552B1 (ko) 2000-04-15
DE69611781D1 (de) 2001-03-22
JPH11504987A (ja) 1999-05-11
US5989626A (en) 1999-11-23
DE69611781T2 (de) 2001-05-31
US5641719A (en) 1997-06-24
EP0828696A4 (en) 1999-01-07
CN1187804A (zh) 1998-07-15
ATE199142T1 (de) 2001-02-15
WO1996035650A1 (en) 1996-11-14
KR19990014682A (ko) 1999-02-25
EP0828696B1 (en) 2001-02-14
EP0828696A1 (en) 1998-03-18

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