CN1282623C - 小板状压制品 - Google Patents
小板状压制品 Download PDFInfo
- Publication number
- CN1282623C CN1282623C CNB018216048A CN01821604A CN1282623C CN 1282623 C CN1282623 C CN 1282623C CN B018216048 A CNB018216048 A CN B018216048A CN 01821604 A CN01821604 A CN 01821604A CN 1282623 C CN1282623 C CN 1282623C
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- 239000000203 mixture Substances 0.000 claims abstract description 69
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- 238000001354 calcination Methods 0.000 claims description 45
- 229910021536 Zeolite Inorganic materials 0.000 claims description 30
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 30
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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 21
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- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 12
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
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- 125000000914 phenoxymethylpenicillanyl group Chemical group CC1(S[C@H]2N([C@H]1C(=O)*)C([C@H]2NC(COC2=CC=CC=C2)=O)=O)C 0.000 description 1
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
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Classifications
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Abstract
介绍了一种基于无机吸附剂和粘合剂的厚度小于700μm的小板状压制品,其通过由这种无机吸附剂、粘合剂、水和可能的压制助剂组成的混合物,在至少70MPa的压力下压制成型制备,这里混合物中干吸附剂与干粘合剂的重量比为约4和0.7之间,在160℃测定的混合物中水含量为约8%和20%之间;在至少约500℃的温度下将得到的新压制品煅烧至总水含量大大去除。
Description
本发明涉及一种基于无机吸附剂和粘合剂的厚度小于700μm的小板状压制品(压片),其特征为具有高力学强度和很低的脆性,能有效地吸附无机和有机气体或蒸汽。
基于沸石和粘合剂制备压制品,特别是片体的方法已经众所周知。根据JP-A-61 15 5216,沸石片体是通过将沸石、粘合剂和润滑剂混合,然后将混合物挤出而制备。明显地涉及了各维尺寸相同的片体。
从JP-A-56063818中已知用作气体吸附剂的沸石片体的制备方法,其中将粉末状,并在105-110℃干燥的沸石与8.1wt%膨润土粉末混合,并与4%尿素水溶液捏合。将混合物压成片体,干燥,并在510℃煅烧。尿素含量决定着压力强度的提高。
从JP-A-55 16 5144已知将粉末状的用于冷集料的沸石粉末与膨润土和水一起捏合,将混合物挤出,形成直径为0.8-10mm的圆形粒子。
根据JP-A-55 10 4913,Na沸石与25wt%黏土混合,与水捏合,挤出,在650℃煅烧,浸在氯化钙溶液中,洗涤,在110℃干燥,在400℃下活化。片体用作干燥剂。
根据JP-A-4 603 2572,沸石粉末与高岭土和Na-(或NH4-)羟乙基纤维素混合,成型,干燥,在650℃煅烧,以提高沸石片体的强度。
根据JP-A-21 44 121,除臭剂通过沸石粉末或粒子与氯化钙或膨润土和水挤出成型,接着将混合物压成片体,并将片体煅烧。
根据JP-A-63 218 234,干燥剂通过将由微孔粒子(例如石膏、水泥、陶瓷粉末)与一种无机或有机填料,例如CaCl2、LiCl、膨润土、沸石、PVA或其他水溶性聚合物组成的混合物挤出成型制备。将此混合物压成片体,然后硬化。
根据JP-A-60 132 643,用作干燥剂的沸石片体是使用20%海泡石作粘合剂而制备。混合物与水一起捏合,压成片体,在150℃干燥,在550℃煅烧。这种片体与沸石片体相比,具有更好的干燥效果。
按照现有技术制备的片体不适于空间狭窄的情况和有力学应力的情况下使用,因为它们太厚,太重,基于质量和表面的对有害气体和蒸汽的吸附力太小。用按照现有技术中的工艺和混合物得到的压制品太脆,特别在燃烧后碎裂。
众所周知,电致发光仪器只有当使用干燥剂时才会无问题地工作长久。这归因于电极,特别是阴极例如对湿度的灵敏度(阴极由Ca或Mg合金组成)。因此,尽可能将这些仪器在保护气下封闭好。
EP 500 382 A2中介绍在电致发光仪器中使用吸湿剂。其中这种粉末状或小球状干燥剂涂在黑色硅酮树脂涂层上。根据优选的实施方案,将干燥剂装入透气的袋子。
US-A-5 882 761中也介绍了在电致发光仪器中使用干燥剂。优选使用的干燥剂是BaO。
上述文本中已知的吸附剂的缺点是,它们只能吸附水蒸气。但是,阴极上的腐蚀可能是由除了水以外在用于密封作用的环氧树脂固化时生成的其他气体(氨气、挥发性胺)引起的。此外,氧气的作用还导致发光构件不能使用(阴极氧化)。
本发明的主题是,提供一种基于无机吸附剂和无机粘合剂的厚度很小(小于700μm)的小板状压制品(压片),尽管其厚度很小,但是强度很高,从而可以特别嵌入只有有限的空间且可能受到震动的电子构件中(例如汽车和移动电话中的电子显示设备)。
按照本发明这个主题是通过提供基于无机吸附剂和粘合剂的厚度小于700μm的小板状压制品(压片)来解决,其通过将组成为或含有至少一种无机吸附剂,至少一种粘合剂以及还有非必要的水和压制助剂的混合物,在至少70 MPa的压力下压制成型制备,其中混合物中干吸附剂与干粘合剂的重量比为约4和0.7之间,在160℃测定的混合物中水含量为约8%和20%之间;在至少约500℃的温度下将得到的新压制品煅烧至总水含量大大去除。
按本发明的压制品(压片)在很小质量的条件下仍具有高强度、低脆性、高吸附速率和高吸附容量。其热膨胀很小,不磨损,容易通过在制备时加入颜料来染色。
按本发明的压片可以在自动工艺中,单位时间内大量件数地制备。它们容易操作,例如可以借助所谓的“取放”(“pick-and-place”)机器从存储容器中取出,应用于电子仪器中。
按本发明的压片除了水蒸气以外还能吸附其他气体(氨气、胺、氧气)。因为它们具有高的吸附容量,所以装有它们的电子仪器不要求完全气密性密闭,即水蒸气在仪器中的扩散速率可以大于0。此外,简化了对合适的仪器密封材料(例如环氧树脂)的选择,因为直到这种材料必定已经达到最终最低的水蒸气透过率的临界时间还可能会通过使用压片而延长。
无机吸附剂优选是天然或人工合成的沸石。但是,还可以使用其它吸附剂,例如无定形硅酸或氢氧化铝,以及由两种或多种吸附剂组成的混合物。
作为粘合剂,原则上可使用每种在本领域专业人员看来合适的粘合剂。作为粘合剂优选使用近晶型黏土,特别是膨润土。同样可能使用其它的无机粘合剂,例如氧化铝氢氧化物(假勃姆石)。但是,还可以使用基于碳水化合物或蛋白质的有机粘合剂,例如淀粉、纤维素衍生物(如CMC或CEC)、酪蛋白或还有合成高分子如PVA、PVP或多酚或含单宁的粘合剂(白坚木)。还可能使用不同粘合剂的混合物。
惊奇地发现,通过把膨润土掺入沸石中没有减小后者的吸附能力。事实上,确定是一种协同效应,即混合物的水蒸气吸附能力在煅烧后比纯沸石降低的程度相比于纯计算期望的结果小很多。
压片的厚度优选不大于约400μm,特别是约200-400μm。
本发明的内容还有一种特别用于制备上面定义的压制品的工艺,其特征为,将一种组成为或包含至少一种无机吸附剂,至少一种粘合剂,还非必要地含有水和压制助剂的混合物在至少约70MPa的压力下压制,其中混合物中干吸附剂与干粘合剂的重量比为约4-0.7,160℃下测定的混合物中水含量为约8-20%;将得到的新压制品在至少约500℃温度下煅烧,直到总水含量大大去除。
结果发现,按照这种工艺得到了具有非常优良的物理和化学性能的特别有利的压制品。特别有利的压制品在原料混合物中干吸附剂与粘合剂的混合比例为约1.5-1的条件下制备。
期望的混合物水含量可以通过组分(吸附剂、粘合剂)的水含量和/或额外加入水来调节。
作为吸附剂优选使用的沸石A以粉末形式得到,水含量约为10-22%。作为粘合剂优选使用的膨润土以水含量约10-20%的粉末形式得到。所用膨润土中蒙脱土含量优选>80%,基于干态。作为压制助剂优选二价或三价金属的脂肪酸盐,例如硬脂酸钙、硬脂酸镁或硬脂酸铝。
发现在压制混合物成为压制品时,当混合物中不含有较大份额的,即有不多于约15%,优选不多于约8%,特别优选0%的>250μm,优选>200μm,特别优选>150μm的粒子,以及粒子的主要部分,即至少50%,优选至少60%是大于约45μm时可以得到最好的结果。
优选的工艺方案是,将沸石粉末与膨润土粉末按期望比例与水混合,水量应使得混合物可以造粒。对此优选使用强混合器。必须加入的水量取决于沸石与膨润土的混合比例以及每种应用的膨润土的胶体化学特性,可以由专业人员很容易地按常规方法测定。造粒后,将混合物调节或干燥至在160℃下测定的水含量为约8-20%。然后,将混合物按预先规定粉碎至粒度<250μm,优选<200μm,特别优选<150μm。
特别惊奇地发现,在压制混合物成为新压制品时,当混合物粒子至少大部分具有基本球形特征,例如通过喷雾干燥得到时结果最好。因此,特别优选的工艺方案是,将沸石粉末和膨润土粉末在使用高剪切的搅拌设备,例如Ultra-Turrax搅拌器的情况下,在水中悬浮成可抽取的悬浮液,并按照传统方法喷雾干燥。通过相应地控制喷雾干燥工艺可以将混合物的水含量调节至优选数值,约8-20%(水含量在160℃下测定)。粒度分布的调节,以使得上面定义的混合物不含较大份额的>250μm,优选>200μm,特别优选>150μm的粒子,以及粒子中大部分大于约45μm,同样可以通过相应地控制喷雾干燥工艺,如需要还随后进行如在现有技术中已知的工艺步骤,如解聚,筛滤和筛分来实施。
由混合物制备的压制品通过应用至少约70MPa的压力成型。优选的压制压力为约100-1300MPa。混合物的压制可以在专业人员已知结构类型的在商业上可购买的自动压机中进行。
为了保证压制品的顺利生产,成型的压制品没有残余料且容易从压制模具中取出是很重要的。这可以通过选择相应的表面改性的模具(用例如TiN或WC改性的钢),精确调节混合物中的水含量,控制压制过程所在地点的温度和空气湿度得到保证。在混合物中水含量低的情况下,调节到相对较高的绝对空气湿度,例如在约25-35℃下相对湿度为60-80%时是有利的。在混合物中的水含量高的情况下,相对较低的绝对空气湿度,例如在约20-30℃下相对湿度为30-50%是有利的。更有利的可能是,在预定数量的压制周期后,例如每个循环或每两个循环后在压制模具上涂覆“抗粘着剂”,例如硬脂酸镁或硬脂酸钙。由此可以有效避免压制物料粘附在压制模具上。
压制品在约500-900℃,优选在约650℃煅烧,直到达到重量恒定,水含量大大去除。
此外惊奇地发现,在煅烧压制品时形成的拱形或曲面可以通过煅烧步骤中对压制品施加压力而基本得到克服。
按照优选的实施方案,煅烧过程中通过使用一种专门构造的带煅烧仪对压制品施加压力,其中通过皮带将压力进汽冲击施加到压制品上。原则上,煅烧过程中在压制品上的压力进汽冲击可以按任意方式进行,只要通过使用压力一方面极为有效地防止了煅烧过程中压制品的拱形的形成,另一方面此压力不会损坏压制品即可。一般应用的压力为10-30,000Pa,特别是100-5,000Pa。按照另一个优选的可能性,将一定数量的压制品堆积在例如由不锈钢或陶瓷制成的小管道中。优选这些小管道有钻孔,其可以允许煅烧过程中水的逸出。由此可以快速且均匀地干燥。在小管道内的总堆积体承受的压力足够用于克服煅烧过程中拱形或曲面,但是不会导致此工艺步骤中压制品打碎,粘结在一起或熔结。一般压力为约10-30,000Pa,特别是100-5,000Pa。按本发明在压力进汽冲击下煅烧的压片是平的,没有显示出或只显示出最小的拱形或曲面,这是在电致发光仪器中使用的前提条件。
根据另一个优选的实施方案,煅烧温度逐步实施或升高,以防止由于水快速或不均匀逸出而在压制品中形成裂纹和缝隙。
压制品还可在真空下煅烧,冷却,由此它们也能吸附永久气体,例如氧气。
此外,压制品还可以含有用于染色的颜料,例如Fe3O4。
本发明的内容还有,上面定义的压制品作为电子仪器或构件中,例如显示设备中的部件,特别是作为电致发光构件中,例如有机发光二极管(LED)中的部件方面的应用。但是,它们还可以用于对湿度敏感的液晶显示设备(LCD)中。
这种仪器或构件可能会在制备时或使用过程中由于无机或有机气体或蒸汽而功能上受到损坏,基于其结构类型只提供给吸附剂很小的空间。
这种电子仪器或构件(例如机动车和移动电话中的显示设备)经常受到强烈的震动,因此压制品不会被打碎或弄成碎屑是很重要的。基于其强度,不必给压制品加盖透气薄膜,由此简化了电子构件的制备。
相对于BaO而言,可以实现电子构件的体积和成本的明显降低。这种压片在电子构件内,在所需要的温度和湿度范围内对水蒸气具有基于质量更高的吸附容量和吸附速率。此外,使用BaO时还必须考虑在水合反应中材料的体积增加100%;因此,在构件内必须安排额外的体积供给干燥剂膨胀且在BaO与电致发光层之间引入水蒸气透过膜,其防止了膨胀的和可能剥落的干燥剂与层之间的接触。与此相对照,压片在吸附水蒸气时体积没有改变,保持力学稳定,从而可以舍弃在构件内提供额外的膨胀体积以及引入保护膜。
BaO还有一个缺点,其自身和其水合产物具有强碱性;此外在吸附湿气时原位升温很强烈,在与有机化合物直接接触时容易发生自燃。这将用于上述保护膜的聚合物的选择限定在很贵的,例如含氟聚合物上,这样就提高了构件的成本。此外,使用BaO时有清除废料的问题,因为作为损害健康的化学品,使电子构件的单个零件的拆卸、重复使用和清除废料很难。
但是,按本发明的压制品还可能用于其他方面,例如作为药物包装中的部件,因为这里只提供有限的体积用于容纳干燥剂。
压制品可以是任意形状,例如圆形、正方形、三角形或长方形或还含有管道和/或留出空白。按本发明的压制品无尘且耐磨。它们可以在常用的自动压机中单位时间中大量件数地制备。
通过下面的实施例对本发明加以阐述。
实施例1(比较)
将75.2kg沸4A(水含量20%),23.8kg膨润土(水含量12%)和1kg硬脂酸钙在强混合器中混合2分钟。然后,加入水直到粘度强烈上升,再混合4分钟。将混合物在110℃干燥至水含量为12%,然后造粒(Stokes造粒机),筛滤(250μm)。0.22g粒度<250μm的材料用69MPa的压力压制成圆形压片。新压片在650℃煅烧3小时,在排除湿气的条件下冷却,密封包装。压片的厚度在煅烧时减小约15-25%。
产品性能:
厚度: 300±50μm
湿度(煅烧后): <1%
生产时的废品: >90%
落体试验*: 100%破碎,压片边缘破碎
*所谓的落体试验用于作为抗压强度的量度,其中让100个煅烧压制品(直径为27mm的圆片)从高度为1m处平的侧面向下地落体。确定破碎试样的百分比含量。
实施例2(比较)
将57kg沸石4A(水含量20%),42kg膨润土(水含量12%)和1kg硬脂酸钙在强混合器中混合2分钟。然后,加入水直到粘度强烈上升,再混合4分钟。将混合物在110℃干燥至水含量为12%,然后造粒(Stokes造粒机),筛滤(250μm)。0.22g粒度<250μm的材料用69MPa的压力压制成压片。新压片在650℃煅烧3小时,在排除湿气的条件下冷却,密封包装。
产品性能:
厚度: 300±50μm
湿度(煅烧后): <1%
生产时的废品: 75%
落体试验: 80%破碎
实施例3
将57kg沸石4A(水含量20%),42kg膨润土(水含量12%)和1kg硬脂酸钙在强混合器中混合2分钟。然后,加入水直到粘度强烈上升,再混合4分钟。将混合物在110℃干燥至水含量为12%,然后造粒(Stokes造粒机),在250μm筛上筛滤。0.22g粒度<250μm的材料用72MPa的压力压制成压片。新压片按照实施例2进行后处理:
产品性能:
厚度: 300±50μm
湿度(煅烧后): <1%
生产时的废品: <50%
落体试验: 60%破碎
实施例4
将57kg沸石4A(水含量20%),42kg膨润土(水含量12%)和1kg硬脂酸钙在强混合器中混合2分钟。然后,加入水直到粘度强烈上升,再混合4分钟。将混合物在110℃干燥至水含量为12%,然后造粒(Stokes造粒机),在250μm筛上筛滤。0.22g粒度<250μm的材料用350MPa的压力压制成压片。新压片在650℃煅烧3小时,在排除湿气的条件下冷却,包装。
产品性能:
厚度: 300±50μm
湿度(煅烧后): <1%
生产时的废品: <25%
落体试验: 15%破碎
吸附容量* 1小时后: 5.4wt%
5小时后: 7.2wt%
24小时后: 13.0wt%
*对水蒸气的吸附容量在25℃下,空气湿度为10%的气氛中测定。
实施例5
重复实施例4的加工方法,只是新压片的煅烧在真空中进行。煅烧的压片基本上与实施例4的压片具有相同的产品性能,但是另外表现出对氧气的吸附容量约5ml/g(在干燥的氧气气氛中测定)。
实施例6
将56.5kg沸石4A(水含量20%),41.5kg膨润土(水含量12%)和1kg硬脂酸钙和1kg白坚木在强混合器中混合2分钟。然后,加入水直到粘度强烈上升,再混合4分钟。将混合物在110℃干燥至水含量为12%,然后造粒(Stokes造粒机),筛滤(250μm)。0.22g粒度<250μm的材料用200MPa的压力压制成压片。新压片在650℃煅烧3小时,在排除湿气的条件下冷却,包装。
产品性能:
厚度: 300±50μm
湿度(煅烧后): <1%
生产时的废品: <35%
落体试验: 10%破碎
实施例7
重复实施例4的加工方法,只是在压制时使用的压力为1200MPa。落体试验结果为10%破碎。废品为<10%。
实施例8
重复实施例4的加工方法,只是使用54kg沸石4A,40kg膨润土,5kgFe3O4和1kg硬脂酸钙。得到的压片染成了深色,可以在LED显示器中用作对比平面。
实施例9
将110.5kg沸石4A(水含量20%),76.0kg膨润土(水含量12%)和1.9kg硬脂酸钙在使用高剪切搅拌设备(Ultra-Turrax搅拌器)的情况下,在水中悬浮,水的用量使得形成可抽取的悬浮液。这种悬浮液进行喷雾干燥,其方式为形成水含量为9.2%(在160℃干燥测定),粒度分布为有0%>150μm和30%<45μm的粉末。0.17g这种材料用190MPa的压力压制成直径为20mm的压片,其中压制模具的周围空气中水蒸气分压为约30mbar。新压片在650℃加压下煅烧3小时。为此,将各300个新压片在由不锈钢制成的钻通小管(高120mm,内径22mm)中堆积,对此堆积体施加2550Pa压力。煅烧后在排除湿气的条件下冷却,包装。
产品性能:
厚度: 300±50μm
垂直膨胀: <350μm
(厚度+曲率)
湿度: <1%
(煅烧后)
生产时的废品: <5%
落体试验: <1%
实施例10
将110.5kg沸石4A(水含量20%),76.0kg膨润土(水含量12%)和1.9kg硬脂酸钙在使用高剪切搅拌设备(Ultra-Turrax搅拌器)的情况下,在水中悬浮,水的用量使得形成可抽取的悬浮液。这种悬浮液进行喷雾干燥,其方式为形成水含量为12.6%(在160℃干燥测定),粒度分布为有0%>150μm和26%<45μm的粉末。0.17g这种材料用210MPa的压力压制成直径为20mm的压片,其中压制模具的周围空气中水蒸气分压为约17mbar。新压片在650℃加压下煅烧3小时。为此,将各300个新压片在由不锈钢制成的钻通小管(高120mm,内径22mm)中堆积,对此堆积体施加2550Pa压力。煅烧后在排除湿气的条件下冷却,包装。
产品性能:
厚度: 300±50μm
垂直膨胀: <350μm
(厚度+曲率)
湿度: <1%
(煅烧后)
生产时的废品: <5%
落体试验: <1%
实施例11
将110.5kg沸石4A(水含量20%),76.0kg膨润土(水含量12%)和1.9kg硬脂酸钙在使用高剪切的搅拌设备(Ultra-Turrax搅拌器)的情况下,在水中悬浮,水的用量使得形成可抽取的悬浮液。这种悬浮液进行喷雾干燥,其方式为形成水含量为15.5%(在160℃干燥测定),粒度分布为有4%>150μm和有8%<45μm的粉末。0.17g这种材料用195MPa的压力压制成直径为20mm的压片,其中压制模具的周围空气中水蒸气分压为约12mbar,压制模具周期性地用硬脂酸镁喷涂。新压片在650℃加压下煅烧3小时。为此,将各300个新压片在由不锈钢制成的钻通小管(高120mm,内径22mm)中堆积,对此堆积体施加2550Pa压力。煅烧后在排除湿气的条件下冷却,包装。
产品性能:
厚度: 300±50μm
垂直膨胀: <350μm
(厚度+曲率)
湿度: <1%
(煅烧后)
生产时的废品: <5%
落体试验: <1%
实施例12
将57kg沸4A(水含量20%),42kg的50/50由石绒与高岭土形成的混合物(水含量12%)和1kg硬脂酸钙在强混合器中混合2分钟。然后,加入水直到粘度强烈上升,再混合4分钟。将混合物干燥至水含量为12%,然后造粒,在150μm筛上筛滤。0.17g粒度<150μm的材料用200MPa的压力压制成压片。新压片在650℃煅烧3小时,在排除湿气的条件下冷却,包装。
产品性能:
厚度: 300±50μm
湿度(煅烧后): <1%
生产时的废品: 25%
落体试验: 70%破碎
实施例13
一种有机的电致发光构件1(正方形,面积为12.9cm2),如图1所示,使用实施例4的压片(圆形,直径27mm)制备。压片2在构件的后壁3上固定后,借助粘合剂4在构件的玻璃基底5上固定,如果可能就借助粘合剂密封。然后,拍摄构件的发光部分6(由阳极7、发光层8和阴极9组成)的显微镜照片(放大50倍)。这些照片没有显示出表明阴极9上有腐蚀的暗(不发光)斑。
此构件在85℃和相对空气湿度为85%的条件下存放500h。然后,重新拍摄构件1的发光部分6的显微镜照片。两个显微镜照片的比较说明,没有形成表明阴极9上有腐蚀的暗斑。
实施例14(比较)
一种如实施例9的有机电致发光构件1使用BaO制备。作为BaO的覆盖层使用透水性的聚四氟乙烯薄膜,其借助薄的双面胶带固定在构件的后壁3上。调节BaO的量,使得BaO、聚四氟乙烯薄膜和双面胶带的总质量与实施例9中应用的压片的质量完全对应。然后,如实施例9所述,拍摄在85℃和空气湿度为85%的条件下存放500h之前和之后发光部分的放大的照片。两个照片的比较说明,有明显可辨别的表明阴极9上有腐蚀的暗斑的生长。
Claims (51)
1.一种小板状压制品,含有至少一种无机吸附剂和至少一种粘合剂,其厚度小于700μm,其通过将组成为或含有这种无机吸附剂和这种粘合剂的混合物,在100至1300MPa的压力下压制成型制备,这里混合物中干吸附剂与干粘合剂的重量比为4和0.7之间,在160℃测定混合物中水含量为8%和20%之间,其中该混合物另外不包含多于15%的>250μm的粒子;在至少500℃的温度下将得到的新压制品煅烧至在煅烧温度下测定的剩余湿度<2wt%。
2.如权利要求1的压制品,其特征为,向混合物中加入水和/或压制助剂。
3.如权利要求1的压制品,其特征为,无机吸附剂是天然或人工合成的沸石。
4.如权利要求1的压制品,其特征为,粘合剂是近晶型黏土。
5.如权利要求4的压制品,其特征为,近晶型黏土是膨润土。
6.如权利要求1的压制品,其特征为,压制品的厚度为200-400μm。
7.如权利要求1的压制品,其特征为,混合物中干吸附剂与干粘合剂的重量比为1.5-1。
8.如权利要求2的压制品,其特征为,作为压制助剂使用一种2价或3价金属的脂肪酸盐。
9.如权利要求1的压制品,其特征为,它使用一种含单宁的粘合剂压制而成。
10.如权利要求9的压制品,其特征为,所述含单宁的粘合剂是白坚木。
11.如权利要求1的压制品,其特征为,混合物中不含多于8%的>250μm的粒子。
12.如权利要求11的压制品,其特征为,混合物中不含多于0%的>250μm的粒子。
13.如权利要求1的压制品,其特征为,混合物中不含多于15%的>150μm的粒子。
14.如权利要求1的压制品,其特征为,混合物中粒子的大部分,即至少50%大于45μm。
15.如权利要求14的压制品,其特征为,混合物中粒子的至少60%大于45μm。
16.如权利要求1的压制品,其特征为,混合物中含有主要为球形的粒子。
17.如权利要求1的压制品,其特征为,多于50%的粒子基本上为球形。
18.如权利要求17的压制品,其特征为,多于75%的粒子基本上为球形。
19.如权利要求18的压制品,其特征为,多于80%的粒子基本上为球形。
20.如权利要求19的压制品,其特征为,多于98%的粒子基本上为球形。
21.如权利要求1的压制品,其特征为,混合物通过喷雾干燥得到。
22.如权利要求1的压制品,其特征为,将它在真空下煅烧。
23.如权利要求1的压制品,其特征为,煅烧在压制品上有压力进汽冲击的条件下进行。
24.如权利要求1的压制品,其特征为,压制品的煅烧在加压下,在钻通的小管中进行。
25.一种用于制备小板状压制品的工艺,其特征为,将组成为或含有无机吸附剂和干粘合剂的混合物,在100至1300MPa的压力下压制成型,这里混合物中干吸附剂与干粘合剂的重量比为4和0.7之间,在160℃测定的混合物中水含量为8%和20%之间,其中该混合物另外不包含多于15%的>250μm的粒子;在至少500℃的温度下将得到的新压制品煅烧至在煅烧温度下测定的剩余湿度<2wt%。
26.如权利要求25的工艺,其特征为,向混合物中加入水和/或压制助剂。
27.如权利要求25的工艺,其特征为,无机吸附剂是天然或人工合成的沸石。
28.如权利要求25的工艺,其特征为,粘合剂是近晶型黏土。
29.如权利要求28的工艺,其特征为,近晶型黏土是膨润土。
30.如权利要求25的工艺,其特征为,压制品的厚度为200-400μm。
31.如权利要求25的工艺,其特征为,混合物中干吸附剂与干粘合剂的重量比为1.5-1。
32.如权利要求26的工艺,其特征为,作为压制助剂使用一种2价或3价金属的脂肪酸盐。
33.如权利要求25的工艺,其特征为,使用一种含单宁的粘合剂进行压制。
34.如权利要求33的工艺,其特征为,所述含单宁的粘合剂是白坚木。
35.如权利要求25的工艺,其特征为,混合物中不含多于8%的>250μm的粒子。
36.如权利要求35的工艺,其特征为,混合物中不含多于0%的>250μm的粒子。
37.如权利要求25的工艺,其特征为,混合物中不含多于15%的>150μm的粒子。
38.如权利要求25的工艺,其特征为,混合物中粒子的大部分,即至少50%大于45μm。
39.如权利要求38的工艺,其特征为,混合物中粒子的至少60%大于45μm。
40.如权利要求25的工艺,其特征为,混合物中含有主要为球形的粒子。
41.如权利要求25的工艺,其特征为,多于50%的粒子基本上为球形。
42.如权利要求41的工艺,其特征为,多于75%的粒子基本上为球形。
43.如权利要求42的工艺,其特征为,多于80%的粒子基本上为球形。
44.如权利要求43的工艺,其特征为,多于98%的粒子基本上为球形。
45.如权利要求25的工艺,其特征为,混合物通过喷雾干燥得到。
46.如权利要求25的工艺,其特征为,在真空下进行煅烧。
47.如权利要求25的工艺,其特征为,煅烧在压制品上有压力进汽冲击的条件下进行。
48.如权利要求25的工艺,其特征为,压制品的煅烧在加压下,在钻通的小管中进行。
49.如权利要求1的压制品用作电子仪器中的部件方面的用途。
50.如权利要求49的用途,其特征为,用作显示设备中的部件。
51.如权利要求49的用途,其特征为,用作电致发光构件中的部件。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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DE10065946.2 | 2000-12-12 | ||
DE10065946A DE10065946A1 (de) | 2000-12-12 | 2000-12-12 | Plättchenförmige Presskörper |
Publications (2)
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CN1484623A CN1484623A (zh) | 2004-03-24 |
CN1282623C true CN1282623C (zh) | 2006-11-01 |
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Application Number | Title | Priority Date | Filing Date |
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CNB018216048A Expired - Fee Related CN1282623C (zh) | 2000-12-12 | 2001-12-12 | 小板状压制品 |
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EP (1) | EP1341736A2 (zh) |
JP (1) | JP4142951B2 (zh) |
KR (1) | KR100585542B1 (zh) |
CN (1) | CN1282623C (zh) |
AU (1) | AU2002238423A1 (zh) |
DE (1) | DE10065946A1 (zh) |
WO (1) | WO2002048025A2 (zh) |
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DE19959957A1 (de) * | 1999-12-13 | 2001-06-21 | Sued Chemie Ag | Plättchenförmige Preßkörper |
US20050238803A1 (en) * | 2003-11-12 | 2005-10-27 | Tremel James D | Method for adhering getter material to a surface for use in electronic devices |
DE102004024676A1 (de) * | 2004-05-18 | 2005-12-15 | Süd-Chemie AG | Filmförmige sorbenshaltige Zusammensetzungen |
US8173995B2 (en) | 2005-12-23 | 2012-05-08 | E. I. Du Pont De Nemours And Company | Electronic device including an organic active layer and process for forming the electronic device |
KR102666704B1 (ko) * | 2018-12-07 | 2024-05-16 | 엘지디스플레이 주식회사 | Oled 디스플레이 패널 및 그 제조 방법 |
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JPS60129139A (ja) * | 1983-12-16 | 1985-07-10 | Matsushita Electric Ind Co Ltd | ゼオライトフイルム |
JPH03203193A (ja) * | 1989-12-29 | 1991-09-04 | Sharp Corp | 薄膜elパネル |
JP2000268954A (ja) * | 1999-03-17 | 2000-09-29 | Matsushita Electric Ind Co Ltd | 発光素子 |
DE19959957A1 (de) * | 1999-12-13 | 2001-06-21 | Sued Chemie Ag | Plättchenförmige Preßkörper |
-
2000
- 2000-12-12 DE DE10065946A patent/DE10065946A1/de not_active Ceased
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2001
- 2001-12-12 AU AU2002238423A patent/AU2002238423A1/en not_active Abandoned
- 2001-12-12 WO PCT/EP2001/014618 patent/WO2002048025A2/de active IP Right Grant
- 2001-12-12 EP EP01986867A patent/EP1341736A2/de not_active Withdrawn
- 2001-12-12 KR KR1020037007820A patent/KR100585542B1/ko not_active IP Right Cessation
- 2001-12-12 CN CNB018216048A patent/CN1282623C/zh not_active Expired - Fee Related
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EP1341736A2 (de) | 2003-09-10 |
WO2002048025A8 (de) | 2003-01-09 |
KR100585542B1 (ko) | 2006-06-14 |
WO2002048025A2 (de) | 2002-06-20 |
DE10065946A1 (de) | 2002-06-13 |
JP2004515443A (ja) | 2004-05-27 |
AU2002238423A1 (en) | 2002-06-24 |
CN1484623A (zh) | 2004-03-24 |
JP4142951B2 (ja) | 2008-09-03 |
KR20030067700A (ko) | 2003-08-14 |
WO2002048025A3 (de) | 2003-05-30 |
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