CN1511122A - 电阻减小的介电组合物 - Google Patents

电阻减小的介电组合物 Download PDF

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CN1511122A
CN1511122A CNA028101081A CN02810108A CN1511122A CN 1511122 A CN1511122 A CN 1511122A CN A028101081 A CNA028101081 A CN A028101081A CN 02810108 A CN02810108 A CN 02810108A CN 1511122 A CN1511122 A CN 1511122A
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weight
conductive oxide
dielectric
dielectric medium
slurry
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CN100379704C (zh
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Rj
R·J·布查德
A
L·-T·A·程
K·W·航
D·H·罗奇
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EIDP Inc
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EI Du Pont de Nemours and Co
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Abstract

本发明提供一种介电组合物，其包含一种电介质和一种导电氧化物，其中所述电介质在约450℃－约550℃范围内的温度下在空气中是可烧结的；所述导电氧化物选自锑掺杂的氧化锡、锡掺杂的氧化铟、具有混合价态或者在约450－约550℃在氮气下烧结后形成混合价态的过渡金属氧化物，以及导电贵金属氧化物如二氧化钌；其中，导电氧化物含量为电介质和导电氧化物总重量的约0.25重量％－约25重量％。介电组合物具有减小的电阻并且用于电子场发射装置中以消除电子发射体附近电介质的充电和静电荷诱导场发射效应。

Description

电阻减小的介电组合物
技术领域
本发明涉及一种电阻减小的介电组合物，其用于电子场发射装置中，以消除电子发射体附近介电体的带电和静电荷诱导的场发射效应。
背景技术
在场发射装置例如场发射显示器的阴极板的某些设计中，阴极表面的布置可能要求发射体导线以电绝缘介电体表面为边界或者紧密靠近电绝缘介电体表面。在场发射过程中，这些相邻的介电体表面被具有浅的入射角(shallow angle of incidence)的高能电子轰击。结果，可能从留下正静电荷的电介质表面发生二次电子发射。这些带正电的表面，距离发射体很近，将对发射体施加一个大的正电场，导致在电介质表面方向上甚至更强的发射。这种效应所以是自增强的并且将支配任何门或阳极控制。由于静电荷随着时间不断累积，不可控制的带电诱导发射甚至在非常低的连续阳极电压下也可能发生。这一问题严重限制了阳极电压。一个解决方案是改变阴极布置，这可能使这种带电效应最小化。一个优选的解决方案是开发单层或多层介电系统，其由于具有低的二次发射特性或者随着电场增大有效耗散电荷而不会充电。
发明内容
本发明提供了一种介电组合物，其包含一种电介质和一种导电氧化物，其中电介质在约450℃-约550℃在空气中是可烧结的，导电氧化物选自锑掺杂的氧化锡、锡掺杂的氧化铟、具有混合价态或者在约450-约550℃在氮气下烧结后形成混合价态的过渡金属氧化物，以及导电贵金属氧化物如二氧化钌。导电氧化物含量为电介质和导电氧化物总重量的约0.25重量％-25重量％，优选约0.5重量％-约15重量％。介电组合物必须能够首先在空气中烧结后在氮气中烧结，以便与形成电子发射体阴极组件中所必需的处理相适应。
本发明还提供一种用于丝网印刷的包含电介质和导电氧化物的介电组合物浆料，其中电介质在约450℃-约550℃的温度下是可在空气中烧结的，导电氧化物选自锑掺杂的氧化锡、锡掺杂的氧化铟、具有混合价态或者在约450-约550℃在氮气氛下烧结后形成混合价态的过渡金属氧化物，以及导电贵金属氧化物如二氧化钌。导电氧化物含量为介电和导电氧化物总重量的约0.25重量％-25重量％，优选约0.5重量％-约15重量％。
这样的介电组合物已经减小了电阻并用于场发射装置中。
还提供了用于本发明介电组合物中的优选的电介质。该电介质是一种固溶体，包含约1-约26重量％SiO2、约0.5-约6重量％Al2O3、约6-约24重量％B2O3、约2-约24重量％ZnO、约0.1-约5重量％Na2O和约20-约75重量％Bi2O3。优选该固溶体包含约1-约9重量％SiO2、约0.6-约6重量％Al2O3、约6-约14重量％B2O3、约2-约13重量％ZnO、约0.1-约2重量％Na2O和约65-约72重量％Bi2O3。更优选该固溶体包含约2重量％SiO2、约3重量％Al2O3、约13重量％B2O3、约9重量％ZnO、约1重量％Na2O和约72重量％Bi2O3。
优选的导电氧化物是锑掺杂的氧化锡。
附图说明
图1是在实施例5-1和对比实验A-C中所用的电子发射体结构的示意图。
图2表示用对比实验A的样品获得的发射结果。
图3表示用实施例5的样品获得的发射结果。
发明详述
本发明通过引入少量半导性或金属材料提供了电阻减小的介电组合物，以减小或消除电介质上的带电。在某种浓度的半导性或金属材料下，电阻将下降到足够低的范围，以允许在高电场下有效进行静电荷耗散并仍然提供要求的绝缘性能，以防止相邻发射体导线或点之间的短路。这样的介电组合物可以用作整个电介质，或也可以用作多层介电系统中的顶层，其提供良好的层的横向(cross)的绝缘和有效的表面电荷耗散。
本发明提供的介电组合物包含在约450℃-约550℃温度下可以烧结的电介质和一种导电氧化物，该导电氧化物选自锑掺杂的氧化锡、锡掺杂的氧化铟、具有混合价态或者在约450-约550℃在氮气氛下烧结后形成混合价态的过渡金属氧化物，以及通常的导电贵金属氧化物如二氧化钌。导电氧化物含量为介电和导电氧化物总重量的约0.25重量％-25重量％，优选约0.5重量％-约15重量％。获得希望电阻率所需的导电氧化物最佳用量随着所用的特定导体及其分散状态而变化。介电组合物的希望电阻率取决于发射体的特定结构，即发射体布线或点的尺寸以及发射体布线或点的分隔。可以针对所用的特定结构调节导电氧化物用量。
用于丝网印刷本发明介电组合物的浆料通常含有电介质粉末、导电氧化物、有机介质、溶剂和表面活性剂。介质和溶剂的作用是在浆料中悬浮和分散微粒组分，即固体，使其具有典型形成图案过程中如丝网印刷所需的合适的流变性。存在许多现有技术中已知的此类介质。可以使用的树脂的实例是纤维素树脂如乙基纤维素和各种分子量的醇酸树脂。丁基卡必醇、乙酸丁基卡必醇酯、二丁基卡必醇、邻苯二甲酸二丁酯和松油醇是有用的溶剂的实例。配制这些和其它溶剂以获得希望的粘度和挥发性要求。表面活性剂可以用来改善颗粒的分散。有机酸如油酸和硬脂酸以及有机磷酸酯如卵磷脂或Gafac磷酸酯是典型的表面活性剂。如果丝网印刷的浆料是用光图案化的(photopatterned)，则浆料中含有光引发剂、可显影粘合剂和可光硬化的单体，例如包括至少一种可加聚的烯键式不饱和化合物，至少一种丝网印刷浆料通常含有电介质熔块和导电氧化物、有机介质、溶剂和表面活性剂。
在丝网印刷电介质浆料中所用的熔块通常是合适的氧化物混合物。正如本领域技术人员熟知的，惰性填料可以加入到熔块中以改进某些性质，例如熔块的流动特性、烧结组合物的强度、膨胀的温度系数等。所有这样的浆料和所得的烧结介电组合物可以含有0-35重量％的无机填料。这样的填料的典型实例是氧化铝、二氧化硅、锆酸钙和锆英石。对于本发明的目的，电介质是指所有的电介质，包括存在的任何填料。
用于丝网印刷本发明介电组合物的浆料中的优选电介质熔块包含约1-约26重量％SiO2、约0.5-约6重量％Al2O3、约6-约24重量％B2O3、约2-约24重量％ZnO、约0.1-约5重量％Na2O和约20-约75重量％Bi2O3。更优选该电介质熔块含约1-约9重量％SiO2、约0.6-约6重量％Al2O3、约6-约14重量％B2O3、约2-约13重量％ZnO、约0.1-约2重量％Na2O和约65-约72重量％Bi2O3。最优选该电介质熔块包含约2重量％SiO2、约3重量％Al2O3、约13重量％B2O3、约9重量％ZnO、约1重量％Na2O和约72重量％Bi2O3。
在烧成后，该浆料提供一种电介质，该电介质是具有以上重量比的SiO2、Al2O3、B2O3、ZnO、Na2O和Bi2O3的固溶体。
实施例
实施例1-4
这些实施例的目的是比较用于介电组合物的各种导电氧化物。
使用铋基电介质熔块和Cr2O3、V2O5、V2O3和SnO2:Sb制备了四种浆料。前三种氧化物是标准的粉末试剂。锑掺杂的氧化锡SnO2:Sb是ZelecECP 3010-XC，其可以得自E.I.du Pont de Nemours andcompany，Wilmington，DE。
在这些实施例中使用的铋基熔块Bi-熔块具有表I所示的组成：
                     表I
            成分                 重量％
            Bi2O3              71.8
            B2O3               13.2
            ZnO                   9.0
            Al2O3                 3.0
            SiO2                  2.0
            Na2O                  1.0
用表II所示组成制备四种浆料：
                    表II
             实施例       实施例       实施例       实施例
             1            2            3.           4
成分        重量％      重量％      重量％      重量％
Bi-熔块      66.0         66.0         66.0         66.0
SnO2:Sb     16.5         无          无           无
Cr2O3     无           16.5         无           无
V2O5      无           无           16.5         无
V2O3      无           无           无           16.5
载体         16.4         16.4         16.4         16.4
表面活性剂   0.6          0.6          0.6          0.6
颜料         0.5          0.5          0.5          0.5
载体是标准厚膜浆料成分，由在β松油醇溶剂中的10％乙基纤维素混合物组成。表面活性剂是一种有机磷酸酯，Gafac RE-610。颜料是标准颜料级铝酸钴。
把四种浆料中的每一种以0.25英寸(0.6cm)×1英寸(2.5cm)的垫形式印刷在载玻片上。每个垫约10微米厚。使用得自E.I.du Pontde Nemours and Company，Wilmington，DE.的银浆组合物7095在每个垫上丝网印刷银电极，以测定电阻。在其间测量电阻的银电极之间的间隙为约1mm。在525℃空气中烧结后然后在510℃氮气中烧结后测量每个样品的电阻。四种烧成后浆料的电性能表示在下表III中：
                       表III
                        空气烧结            氮烧结
        实施例1         1.2MΩ                              0.9MΩ
        实施例2         ＞1GΩ                              ＞1GΩ
        实施例3         540MΩ                              7MΩ
        实施例4         15M                  23MΩ
所有的导电氧化物降低了电介质的电阻。SnO2:Sb在空气中烧结后表现出最大的减小，和在氮气中二次烧结后最小的变化。
实施例5-11，对比实验A-C
这些实施例和对比实验表示各种含量的导电氧化物SnO2:Sb在消除电介质充电和所产生的不希望的电子发射方面的作用。
把实施例1的浆料与具有表IV所示组成的浆料共混：
                    表IV
            成分               重量％
            Bi-熔块             70.0
            SnO2:Sb            无
            载体                29.0
            表面活性剂          0.5
            颜料                0.5
其中Bi-熔块、载体、表面活性剂和颜料与实施例1所用的浆料相同。按浆料总重量计，用0-10重量％的SnO2:Sb含量形成10种不同的浆料。每个实施例和对比实验表示在下表V中：
                       表V
        成分 实施例或          重量％
        对比实施例     SnO2:Sb       电阻     充电
        A                0             ＞200GΩ     大量
        B                2             ＞200GΩ     大量
        C                3             ～200GΩ     一些
        5                3.5           152GΩ        无@3kV
        6                3.75          52GΩ          无@3kV
        7                4             3.3GΩ        无@3kV
        8                4.25          236MΩ        无@3kV
        9                4.5           79MΩ          无@3kV
        10               5             33MΩ          无@3kV
        11               10            136kΩ        无@3kV
如图1所示，把每一个实施例和对比实验中的介电组合物在载玻片2上印成0.75”(1.9cm)方形垫1。然后把介电组合物在空气中在525℃烧结。由15个20密耳(0.51mm)宽和20密耳(0.51mm)间距的条3组成的图案(pattern)被丝网印刷在介电组合物上。银浆组成的条丝网印刷后在空气中在525℃温度下烧结，随后把发射体浆料丝网印刷在银线上面并在氮气中在510℃下烧结。银浆是得自E.I.duPont de Nemours and Company，Wilmington，DE的组合物7095。用于这些实施例的发射体浆料通过混合三种组分制备：一种是含有单壁碳纳米管的悬浮液，一种是含有10％乙基纤维素和90％β-松油醇的一般有机介质，一种是典型的含银浆料。激光烧蚀生长单壁碳纳米管得自Tubes@Rice，Rice University，Houston，TX，是一种用激光烧蚀生产的未提纯粉末。纳米管悬浮液通过超声作用即超声混合一种含有1重量％纳米管粉末和99重量％三甲基苯的混合物来制备。所用的超声混合机是Dukane Model 92196，其具有1/4英寸喇叭形辐射体，在40kHz和20瓦操作。发射体浆料通过把纳米管悬浮液/有机介质/银浆按27/40/33的重量比组合来制备。这种组合在三辊磨机中混合10次，以形成发射体浆料。
如4所示，电连接交替的条。介电组合物的电阻值可以使用用于此特殊线图案的静电计5测定。数据显示当导电氧化物在浆料中的浓度达到～3％时，导电氧化物开始对此结构起作用，电阻下降至～200GΩ。所有实施例和对比实施例的电阻表示在表V中。
使用由两个电极组成的平板发射测量单元对于所有的实施例和对比实验进行场发射，一个作为阳极或集电体，另一个作为阴极。所述阴极由安装在聚四氟乙烯(PTFE)夹具中的铜块组成。该铜块放在PTFE的1英寸×1英寸(2.5cm×2.5cm)的凹入区域中，并把样品基底安装在铜块上，在铜块和样品基底之间利用铜带进行导电连接。把高压引线连接到该铜块上。阳极与样品按一定距离与样品保持平行，该距离可以变化，但是一旦选定，则对于样品的一组测量保持恒定。使用1.25mm的间距。阳极由通过化学气相沉积涂敷氧化铟锡的玻璃板组成。然后涂敷标准ZnS-基磷光体，磷光体P-31，Type 139，得自ElectronicSpace Products International。把电极连接到氧化铟锡涂层。测试设备插入到真空系统，然后把系统抽真空到低于1×10-5乇(1.3×10-3Pa)的基础压力。可以向阴极施加频率为60Hz、典型脉冲宽度为3微秒的负压脉冲，也可以施加恒定的电压。由于发射电流由磷光体发射的图像用照相机记录。
在场发射过程中产生的带电问题和本发明的介电组合物的明显改善可以使用这些样品来证明。作为对比，用脉冲电压和恒定阳极电压研究不含SnO2:Sb填料的对比实施例A的发射体单元。图2a表示在阳极-阴极间隙上以60Hz施加持续3微秒的高压脉冲时的二极管发射图像。在2kV下观察带电诱导发射的开始，其可以在图2a中可以以亮斑形式看到。这些亮斑随时间迅速扩展，并且在其开始数秒内带电诱导的发射变得不可控制。当施加连续的阳极电压时，带电诱导发射在1kV的阳极电压下发生，如图2b所示。图3a和3b证明使用本发明的介电组合物消除场发射过程中的带电现象的效果。当用实施例5的发射体单元进行相同的二极管发射试验，所述发射体单元含有3.5％的SnO2:Sb，在3kV的脉冲阳极电压和1.5kV的连续阳极电压下观察到没有带电诱导的发射，分别如图3a和3b所示。

Claims (21)

1.一种介电组合物，其包含一种电介质和一种导电氧化物，其中所述电介质在约450℃-约550℃范围内的温度下在空气中是可烧结的；所述导电氧化物选自锑掺杂的氧化锡、锡掺杂的氧化铟、具有混合价态或者在约450-约550℃在氮气下烧结后形成混合价态的过渡金属氧化物，以及导电贵金属氧化物如二氧化钌；导电氧化物含量为所述电介质和导电氧化物总重量的约0.25重量％-约25重量％。
2.权利要求1的介电组合物，其在约450℃-约550℃的温度下在空气中烧结，并且随后在约450℃-约55O℃的温度下在氮气中烧结。
3.权利要求1的介电组合物，其中，所述导电氧化物的存在量为所述电介质和所述导电氧化物总重量的约0.5重量％-约15重量％。
4.权利要求1的介电组合物，其中所述导电氧化物是锑掺杂的氧化锡。
5.权利要求1的介电组合物，其中所述电介质是一种固溶体，其包含约1-约26重量％SiO2，约0.5-约6重量％的Al2O3，约6-约24重量％B2O3，约2-约24重量％的ZnO，约0.1-约5重量％的Na2O和约20-约75重量％的Bi2O3。
6.权利要求5的介电组合物，其中，所述电介质是一种固溶体，其包含约1-约9重量％SiO2，约0.6-约6重量％的Al2O3，约6-约14重量％B2O3，约2-约13重量％的ZnO，约0.1-约2重量％的Na2O和约65-约72重量％的Bi2O3。
7.权利要求1-4的任一项的介电组合物，其中，所述电介质是一种固溶体，其包含约2重量％SiO2，约3重量％的Al2O3，约13重量％B2O3，约9重量％的ZnO，约1重量％的Na2O和约72重量％的Bi2O3。
8.一种用于丝网印刷介电组合物的浆料，其包含一种电介质和一种导电氧化物，其中所述电介质在约450℃-约550℃的温度在空气中是可烧结的；所述导电氧化物选自锑掺杂的氧化锡、锡掺杂的氧化铟、具有混合价态或者在约450-约550℃在氮气下烧结后形成混合价态的过渡金属氧化物，以及导电贵金属氧化物如二氧化钌。所述导电氧化物含量为所述电介质和所述导电氧化物总重量的约0.25重量％-25重量％。
9.权利要求8的浆料，其中所述导电氧化物的存在量为所述电介质和所述导电氧化物总重量的约0.5重量％-约15重量％。
10.权利要求8的浆料，其中所述导电氧化物是锑掺杂的氧化锡。
11.权利要求8的浆料，其中所述电介质是一种固溶体，其包含约1-约26重量％SiO2，约0.5-约6重量％的Al2O3，约6-约24重量％B2O3，约2-约24重量％的ZnO，约0.1-约5重量％的Na2O和约20-约75重量％的Bi2O3。
12.权利要求11的浆料，其中，所述电介质是一种固溶体，其包含约1-约9重量％SiO2，约0.6-约6重量％的Al2O3，约6-约14重量％B2O3，约2-约13重量％的ZnO，约0.1-约2重量％的Na2O和约65-约72重量％的Bi2O3。
13.权利要求8-10的任一项的浆料，其中，所述电介质是一种固溶体，其包含约2重量％SiO2，约3重量％的Al2O3，约13重量％B2O3，约9重量％的ZnO，约1重量％的Na2O和约72重量％的Bi2O3。
14.权利要求8-12的任一项的浆料，其中，所述浆料可以用光形成图案。
15.权利要求13的浆料，其中所述浆料可以用光形成图案。
16.一种电子场发射装置，其使用一种介电组合物，该介电组合物包含电介质和导电氧化物，其中所述电介质在约450℃-约550℃的温度在空气中是可烧结的；所述导电氧化物选自锑掺杂的氧化锡、锡掺杂的氧化铟、具有混合价态或者在约450-约550℃在氮气下烧结后形成混合价态的过渡金属氧化物，以及导电贵金属氧化物如二氧化钌；所述导电氧化物含量为所述电介质和所述导电氧化物总重量的约0.25重量％-25重量％。
17.权利要求16的电子场发射装置，其中所述导电氧化物的存在量为所述电介质和所述导电氧化物总重量的约0.5重量％-约15重量％。
18.权利要求16的电子场发射装置，其中所述导电氧化物是锑掺杂的氧化锡。
19.权利要求16的电子场发射装置，其中所述电介质是一种固溶体，其包含约1-约26重量％SiO2，约0.5-约6重量％的Al2O3，约6-约24重量％B2O3，约2-约24重量％的ZnO，约0.1-约5重量％的Na2O和约20-约75重量％的Bi2O3。
20.权利要求19的电子场发射装置，其中，所述电介质是一种固溶体，其包含约1-约9重量％SiO2，约0.6-约6重量％的Al2O3，约6-约14重量％B2O3，约2-约13重量％的ZnO，约0.1-约2重量％的Na2O和约65-约72重量％的Bi2O3。
21.权利要求16-18的任一项的电子场发射装置，其中，所述电介质是一种固溶体，其包含约2重量％SiO2，约3重量％的Al2O3，约13重量％B2O3，约9重量％的ZnO，约1重量％的Na2O和约72重量％的Bi2O3。
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