CN102186789B - 形成基于干玻璃的玻璃料的方法 - Google Patents
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- C—CHEMISTRY; METALLURGY
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/08—Frit compositions, i.e. in a powdered or comminuted form containing phosphorus
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
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- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
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- C03C3/21—Silica-free oxide glass compositions containing phosphorus containing titanium, zirconium, vanadium, tungsten or molybdenum
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- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
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Abstract
揭示了一种基于干玻璃的玻璃料以及制备干玻璃的玻璃料的方法。在一个实施方式中,干玻璃的玻璃料包含钒、磷和金属卤化物。该卤化物可以是例如氟化物或氯化物。在另一个实施方式中,制备干玻璃的玻璃料的方法包括煅烧用于玻璃料的批料,然后在诸如氮气气氛的惰性气氛中使所述批料熔融。在又一个实施方式中,一种制备干玻璃的玻璃料的方法包括煅烧用于玻璃料的批料,然后在诸如氮气气氛的空气气氛中使所述批料熔融。
Description
相关申请的交叉参考
本申请要求2008年10月20日提交的美国临时专利申请序列号第61/106730号以及2009年7月16日提交的美国专利申请第12/504276号的优先权的权益,所述专利申请内容是本文的依据并且全文参考结合入本文中。
技术领域
本发明涉及用于形成基于无机玻璃的干玻璃料的方法。更具体说,本发明涉及用于形成适合用作玻璃封装的密封介质的基于干无机玻璃的玻璃料的方法。
背景技术
通常采用大的玻璃母片,在单次组装中通过形成多个器件来制造电致发光(EL)器件,例如有机发光二极管器件。也就是说,将器件包封在两大片玻璃或玻璃板之间以形成复合组件,然后从复合组件上切割得到各个器件。复合组件中的每个器件包括围绕各个器件的有机发光二极管的密封,该密封将顶板和底板密封在一起并保护置于其中的有机发光二极管,因为一些器件,尤其是有机发光二极管,在环境气氛中的氧气和水分的存在下会发生劣化。EL器件可采用粘合剂如环氧树脂粘合剂进行密封,或者新近采用玻璃料,加热该玻璃料使其熔融并在两块板之间形成密封。
玻璃料密封的器件表现出优于粘合剂密封器件的某些优点,其中尤其是优异的气密性而不需要在器件内用吸气器密封来清除污染物。因此,玻璃料密封的器件能够提供比用粘合剂密封更长寿命的器件。然而,已发现由于玻璃料内包含的水分以及在密封工艺期间由玻璃料释放到容纳有机发光材料的空腔中的水分,玻璃料密封的器件可能易于发生劣化。
发明内容
揭示了形成基于干玻璃的玻璃料的方法,所述玻璃料适用于密封电子器件,尤其是包含有机材料的电子器件,例如有机发光二极管显示器、有机发光二极管照明面板和某些类型的基于有机材料的光伏器件。
在一个实施方式中,揭示了一种形成干玻璃的玻璃料的方法,该方法包括:形成包含钒和磷的批料;在调节步骤中将所述批料加热至约450-550℃保持至少约1小时;在所述调节步骤之后使所述批料熔融以形成玻璃熔体;冷却所述玻璃熔体以形成玻璃;其中,直接***探针的质谱法测得,所述玻璃的OH含量等于或小于约20ppm。
在另一个实施方式中,揭示了一种用于形成基于玻璃的玻璃料的玻璃粉末,其中,所述玻璃粉末包含钒、磷和金属卤化物。
在另一个实施方式中,揭示了一种用于形成基于玻璃的玻璃料的玻璃粉末,其中,所述玻璃粉末包含V2O5、P2O5和金属卤化物。
在又一个实施方式中,揭示了一种形成玻璃料的方法,该方法包括:形成包含V2O5、P2O5和金属卤化物的批料;在调节步骤中将所述批料加热至约450-550℃保持至少约1小时;在所述调节步骤之后使所述批料熔融以形成玻璃熔体;冷却所述玻璃熔体以形成玻璃;其中,所述玻璃的OH含量等于或小于约20ppm。
参见附图,通过以下说明性的描述能够更容易理解本发明,同时更清楚地了解本发明的其它目的、特征、细节和优点,以下描述不是限制性的。本发明人的意图是所有这些另外的体系、方法特征和优点都包括在该描述之内,包括在本发明的范围之内,并受到所附权利要求书的保护。
附图说明
图1是包含有机材料的示例性玻璃封装的截面图。
图2是透射率百分数与波数的关系图,图示了β-OH的典型测量结果。
图3是用于测量放气的水蒸汽的DIP-MS设备的示意图。
图4是根据本发明实施方式的标准加热程序的图形表示。
图5是根据本发明实施方式的压缩加热程序的图形表示。
图6显示了对玻璃料组合物C1的粗的手工研磨样品进行的DIP-MS测量的结果,显示了对水提取的离子色谱图。
图7显示了按图6中进行的但不含样品的对照DIP-MS测量的结果,表明图6所示现象(尖峰)与400-700℃升温期间结构水物质的放气有关。
图8显示了在对照(非干)玻璃料组合物C1的粗的手工研磨样品上进行的DIP-MS测量的结果,显示了与无峰样品C2的结果相比,400-700℃升温期间结构水物质的放气。
图9的照片显示了485℃煅烧(左图)和600℃煅烧(右图)之后对照批料组合物的熔融石英坩埚。
具体实施方式
在以下的详述中,为了说明而非限制,给出了说明具体细节的示例性实施方式,以提供对本发明的透彻理解。但是,对于本领域普通技术人员显而易见的是,在从本说明书获益后,可以以不同于本文详述的其它实施方式实施本发明。另外,本文会省去对于熟知的器件、方法和材料的描述,以免使得本发明的描述难以理解。最后,在任何可适用的情况下,相同的编号表示相同的元件。
气密密封的玻璃封装可用于各种应用,包括象光学显示器(例如平板电视、手机显示器、相机显示器)和光伏器件(例如太阳能电池)这样的光子器件。虽然对于某些部件,例如液晶显示器(LCD),已广泛使用环氧树脂密封,但新近的研究针对可用于类似目的的包封的有机材料。例如,有机发光二极管可用于显示器和照明。某些有机材料也可用于光电领域,其中有机太阳能电池有前途。
虽然有机材料提供某些益处,但包含有机材料的器件易受高温、氧气和水分接触的影响。也就是说,如果暴露于超过约100℃的温度、或接触氧气或水分,有机材料会快速劣化。为此,必须非常小心以确保采用有机材料的器件是气密密封的。一种这样的方法包括将有机材料密封在两块玻璃板之间。只有无机玻璃适合作为容纳有机材料的容器。无机玻璃基本上环境稳定,对于水分和氧气的扩散是高度不可渗透的。然而,所得封装仅仅与在两块板之间形成密封的材料一样好。
现有技术的器件常常采用环氧树脂粘合剂作为玻璃板之间的密封介质。LCD显示器的制造是一个这样的例子。然而,板之间的玻璃密封更好地满足了适用于电子器件,例如前述显示器、照明面板和光伏器件的某些有机材料所要求的长期气密性程度。因此,使用基于无机玻璃的玻璃料已成为用于有机电子器件的密封介质的选择。
例如(非限制性),用于有机发光二极管显示器10(图1)的示例性玻璃料密封方法可包括在第一(底板)玻璃基板14上形成光电元件12。光电元件12通常包括阳极和阴极(未示出)以及位于两个电极之间的一层或多层光电材料(例如有机发光材料)。玻璃料16设置在底板基板和第二玻璃(覆盖)基板18之间。例如,可先将玻璃料分配到覆盖基板上。在一些实施方式中,先将作为糊料的玻璃料分配到覆盖基板18上,然后加热烧结玻璃料并且使其粘附于覆盖基板。烧结可以在炉中进行。然后,将覆盖基板18设置成与底板基板至少部分重叠对齐,辐射源20(例如发射激光束22的激光器20)加热玻璃料以使其软化并在覆盖基板和底板基板之间形成气密密封,从而形成包含OLED的气密玻璃封装。
通常,玻璃中存在的水可分为两大类:结构水,其中水的原子(通常以羟基或OH离子存在)在熔融工艺期间连接到形成玻璃的多面体分子结构上并成为玻璃网络的基本部分;以及表面水,其中,例如在研磨期间在玻璃球磨以制备玻璃料期间存在的水分子本身连接到由断键形成的玻璃料颗粒表面上未饱和的价态位点上。通常,表面水可通过简单的干燥工艺,例如通过加热玻璃料的玻璃而去除,而结构水的结合要强得多,在任何干燥步骤期间仍可保留在玻璃中。
虽然玻璃中水的存在不一定会使玻璃性质劣化(除了Mid-IR吸光度增加之外),在玻璃料密封工艺中的随后加热期间水的释放(放气)可能牵涉到玻璃的商业应用。受到水放气影响的一种具体应用涉及用于密封OLED器件的玻璃料的用途,其极易受到甚至是ppm级的水的影响。本发明所用的水可以是气相的形式(例如,放气期间,或者作为羟离子,OH)。
在典型的玻璃料制造工艺中,由常规玻璃形成方法,例如溶胶-凝胶法或者通过加热颗粒状批料(沙)形成玻璃。然后将所得玻璃熔融,制成薄带,然后球磨成所需的粒度。例如,3μm的平均粒度适用于制造OLED器件。球磨之后,将粉末状的玻璃料的玻璃与填料掺混得到玻璃料掺混物预定的热膨胀系数。例如,具有合适的热膨胀系数的填料是β-锂霞石。一旦制得掺混物并预先干燥(例如在炉中加热掺混物),将玻璃料的玻璃(或掺混的玻璃料,视情况而定)与有机载体(例如Texanol)、有机粘合剂(例如乙基纤维素)以及需要的各种分散剂和表面活性剂混合来制备糊料。然后将玻璃料糊料在玻璃基板上分配成特定的图案(例如环或框架状图案),空气中加热以烧掉有机物,然后在N2中随后加热至400℃,以预烧结(presenter)玻璃料。如该术语所包含的,预烧结步骤使得玻璃料固结并使玻璃料粘附于(覆盖)基板)。将一个或多个OLED器件的预烧结基板与匹配的基板(底板基板)激光密封通常采用激光来实现,激光穿过固结的玻璃料,加热并软化该玻璃料,随后当玻璃料冷却和固化时在覆盖基板和底板基板之间形成密封。激光密封期间,在400℃以上将玻璃料密封加热至少十分之几秒,导致玻璃料中的结构水(即OH)释放,可能使OLED劣化。
在随后的玻璃料加热至700℃期间消除玻璃中水放气的工作集中在降低玻璃的OH含量。采用了两种方法:(1.)改变玻璃组成,和(2)物理上改变熔融过程。根据以下两种方法测量水量:测量β-OH(主要测量OH-离子的Mid-IR吸收峰,和DIP-MS(直接***探针质谱法)。根据本发明,干玻璃(和所得干玻璃料)定义为直接***探针质谱法测量时,β-OH值等于或小于约0.3mm-1,或者OH含量等于或小于约20ppm。优选地,直接***探针质谱法测量时,玻璃包含的β-OH的值等于或小于约0.3mm-1,OH含量等于或小于约20ppm。优选地,所述玻璃显示,以粗的手工研磨粉末,或者以细的(3μm)球磨粉末的形式重新加热至700℃时,DIP-MS未能检测到水放气。
对经过研磨然后磨光至厚度0.1-0.4mm的玻璃退火片进行β-OH测量。β-OH测量提供了关于玻璃中羟离子,而不仅仅是在特定温度区域内解吸的那些羟基的总浓度的数据。如图2和下式1所示,β-OH是基线透射率与OH-吸收峰处透射率之比,对于组成相同、或者非常类似的玻璃,该值与羟离子浓度成正比。
β-OH=log(ref%T/OH%T)/(thk) 1
式中,ref%T是无-OH吸收区域附近的透射率水平,OH%T是OH峰基线处的透射率水平(~3380cm-1),thk是样品厚度(mm)。
对于组成相同、或者非常类似的玻璃,β-OH与羟离子浓度成正比。β-OH测量提供了玻璃中所有羟离子,而不仅仅是在特定温度区域内解吸的那些羟基的相对羟基(OH)吸收系数。可采用任何常规红外光谱技术进行测量,例如傅里叶变换红外光谱法。
对粗的手工研磨的粉末(-200M/+100M,或约75-150μm)或细的球磨粉末(平均粒度等于或小于3μm)进行DIP-MS测量。DIP-MS配置与许多标准质谱研究中采用的真空炉质谱技术不同,前者的示意图如图3所示,DIP-MS配置利用包含直接置于质谱仪34的电离区域(电子冲击电离器32)内的待测样品30的加热探针28。除了上述部件之外,如3所示示例性的DIP-MS配置还包括四极离子分析器36和检测器38。波浪线40代表从样品30到检测器38的离子路径。与真空炉质谱测量不同,无需石英转移管,并且不存在相关的化学物质沉积或者石英转移管在高温下渗透性的问题。因此,DIP-MS适用于更可靠地定量分析化学物质。
DIP-MS测量采用两种不同的加热程序:a)标准循环(图4),其中,将样品加热至400℃,保持5小时以去除任何表面水,然后以10℃/分钟的速率加热至700℃,和b)压缩程序(图5),该程序使用与标准程序相同的使样品升温至400℃,但在400℃保持时间较短(2小时),并且采用较快加热升温至700℃(50℃/分钟)。所有样品在整个DIP-MS运行期间在真空中加热。
图6显示了对适用于激光密封OLED器件的玻璃料玻璃组合物的粗的手工研磨样品进行的DIP-MS测量结果,显示了对水提取的离子色谱(并对纳-安培与分钟表示的时间关系作图)。以标准程序运行。在将样品加热至400℃时,在运行最初的几分钟内记录来自表面水的少量水放气。在400℃保持4小时的过程中(从20分钟到260分钟),未记录到额外的水放气现象,证实最初的水放气与表面水有关。在样品加热再继续后,在约550℃开始观察到一些与水放气相关的离散现象。
注意在进行无样品的对照测量时未观察到这些离散现象(图7),进一步说明这些现象与400-700℃的升温期间结构水物质的放气有关。对照测量期间仅观察到作为仪器一般背景信号所特有的宽的模糊的浅峰。
如表I所示,发现使用卤化物对于减少结构水含量尤其有效,由以下两个方面得到说明:含卤化物的组合物中β-OH含量显著降低,并且DIP-MS测量检测显示在400-700℃加热升温期间根本不能检测出水放气。表I总结了4种组合物(C2-C4)以及不含卤化物的对照组合物(C1)的结果。图8显示了对不含卤化物的C1样品,以及所有Al2O3被AlF3代替的基本相同的C2样品进行DIP-MS扫描的高温部分的比较。两种材料均为粗的手工研磨的玻璃粉末。曲线42表示对含氟玻璃(C2)的扫描,显示无特征图形并且无独特现象。相反,曲线44表示的对C1样品的扫描显示,在约550-650℃的范围内发生一些离散的水放气现象。C5样品的β-OH值比预计的要高,与其它卤化物的结果不一致,认为这是样品制备差的结果(因为β-OH测量对样品的表面清洁度敏感)。未进行样品C3和C4的DIP-MS测量。
表I
除了在玻璃料中加入卤化物,还进行与卤化物加入无关的其它试验,其中,改良熔化工艺以制备具有低β-OH值的玻璃,并且在随后的DIP-MS分析期间不显示结构水放气。
表II显示了各种工艺改变实验和测量的结构水含量(β-OH)和/或放出的结构水的量(DIP-MS)。如表所示,这些不同实验包括确定熔融期间热循环的作用(实验1),批料空气煅烧和N2熔融(实验2),批料空气煅烧(485℃或600℃)然后是批料的空气熔融(实验3和4);使所有除V2O5之外的基本玻璃组分熔融,然后使V2O5再熔融(实验5);和在感应电炉中使标准碎玻璃再熔融并在再熔融期间使O2或N2/O2鼓泡通过熔体(实验6和7)。与标准工艺相比,这些方法中的大多数导致β-OH值显著降低和/或DIP-MS测量未检测到结构水放气,例外情况是熔融期间的高-低-高的热循环(实验1);和600℃煅烧加标准1000℃熔融(实验5)。
表II
该结果有趣的特征是煅烧温度的影响。选择煅烧作为降低结构水的可能的方式,因为这能使玻璃料掺混物的任何原料中作为组成成分存在的水在被接纳到熔体结构中之前从批料逸出。有趣的是,485℃空气-煅烧/1000℃空气-熔融(实验3)在降低结构水的量方面具有显著效果(β-OH=0.205),但600℃空气-煅烧/1000℃空气-熔融(实验5)相对无效果(β-OH=0.433)。一种可能的解释由图9提供,图9显示了分别在485℃煅烧和600℃煅烧之后对照批料组合物的熔融石英坩埚46和48。煅烧的485℃批料基本上是疏松、多孔、未固结的粉末,而600℃煅烧的批料发生显著熔融,因为关键批料组分之一(五氧化二磷)的熔点为563℃。一种可能的解释是,与较低温度485℃煅烧相比,600℃产生的液相封闭了水放气的许多逃逸通道,导致熔体结构中包含的水较多。485℃空气-煅烧/1000℃N2-熔融的组合(实验2)在所有方法中产生最低的β-OH。认为这是因为485℃空气-煅烧的作用与N2吹扫通过玻璃熔体并带走水物质的能力相结合而造成的。在实验6和7中也观察到N2的有益作用,其中常规熔融的碎玻璃在N2气氛中再熔融,同时使O2或N2/O2鼓泡通过熔体。
在完成表II的物理实验之后,选择三种方法重复测试以确定不含水的结果的重现性。这些方法是:用卤化物代替Al2O3(例如AlF3);485℃空气煅烧2小时,然后在1000℃空气中熔融;和485℃空气煅烧2小时然后在1000℃N2气氛中熔融。表III显示了这些技术在β-OH和水放气结果方面的比较。在初始实验中产生干玻璃的三种方法可以重复工作来制得干玻璃。
表III
表IV所提供的DIP-MS结果表明,对于精细研磨(粒度等于或小于约3μm)的球磨粉末以及由在400℃预烧结处理之后精细研磨的粉末制成的玻璃料掺混物糊料也可看到上述一些方法所显示的不存在结构水放气的现象。
表IV
用于制备干玻璃和玻璃料的上述一些技术看来似乎一般与含钒和磷酸盐的玻璃有关,而不是仅仅与目前用于OLED玻璃料密封的Sb2O3磷酸钒玻璃有关。下表V显示了根据本发明的一个实施方式,不含Sb的Fe2O3-V2O5-P2O5玻璃的β-OH值。
表V
应当强调,本发明上述实施方式、特别是任意“优选的”实施方式仅仅是可能实现的实施例,仅仅为了清楚地理解本发明的原理而提出的。可以在基本上不偏离本发明的精神和原理的情况下,对本发明的上述实施方式进行许多的改变和调整。所有这些调整和改变都包括在本文中,包括在本发明和说明书的范围之内,并受到所附权利要求书的保护。
Claims (15)
1.一种形成玻璃料的方法,包括:
形成包含钒和磷的批料;
在调节步骤中将所述批料加热至450-550℃保持至少1小时,形成疏松、多孔、未固结的批料粉末;
在所述调节步骤之后使所述批料粉末熔融以形成玻璃熔体;
冷却所述玻璃熔体以形成不含锑的玻璃;
研磨所述玻璃以形成玻璃颗粒;和
其中,所述玻璃的OH含量等于或小于20ppm。
2.如权利要求1所述的方法,其特征在于,所述玻璃包含的β-OH等于或小于0.3mm-1。
3.如权利要求1所述的方法,该方法还包括将所述玻璃颗粒与降低热膨胀系数的填料掺混。
4.如权利要求1所述的方法,其特征在于,在所述调节步骤中将所述批料加热至少2小时的时间。
5.如权利要求1所述的方法,其特征在于,所述熔融步骤在氮气气氛中进行。
6.如权利要求1所述的方法,其特征在于,所述熔融步骤包括将所述批料粉末加热到至少1000℃的温度以使所述批料粉末熔融。
7.如权利要求1所述的方法,其特征在于,在加热批料之后立即熔融批料粉末。
8.一种形成玻璃料的方法,包括:
形成包含V2O5、P2O5和金属卤化物的批料;
在调节步骤中将所述批料加热至450-550℃保持至少1小时,形成疏松、多孔、未固结的批料粉末;
在所述调节步骤之后使所述批料粉末熔融以形成玻璃熔体;
冷却所述玻璃熔体以形成玻璃;
其中,所述玻璃的OH含量等于或小于20ppm。
9.如权利要求8所述的方法,其特征在于,所述金属卤化物的金属选自:铁、钒和铝。
10.如权利要求9所述的方法,其特征在于,所述金属卤化物包括AlCl3或AlF3。
11.如权利要求8所述的方法,其特征在于,所述批料进一步包括Fe2O3和TiO2。
12.如权利要求8所述的方法,其特征在于,所述玻璃不含锑。
13.如权利要求8所述的方法,其特征在于,在所述调节步骤中将所述批料加热至少2小时的时间。
14.如权利要求9所述的方法,该方法还包括将所述玻璃颗粒与降低热膨胀系数的填料掺混。
15.如权利要求8所述的方法,其特征在于,在加热批料之后立即熔融批料粉末。
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