11 月22,欧洲专利局( European Patent Office ,EPO) 决定撤销编号为 1449238 的 欧洲专利(以下简称 EP-238) 。该专利是 有机电致发光(OLED)技术领域 的一份有关金属有机磷光材料的核心专利。 撤销EP-238的一项主要依据是原吉林大学 马於光 等人(Yuguang Ma,Houyu Zhang, Jiacong Shen,Chiming Che)于1998年发表在合成金属(Synthetic Metals, 94,1998, 245-248)杂志上的一篇文章, Electroluminescence from triplet metal-ligand charge-transfer excited state of transition metal complexes。 请求撤销EP-238的是三家著名公司:默克(Merck),巴斯夫(BASF)和住友化学(Sumitomo Chemicals)。这三家公司都看好OLED技术和材料,并为此投入巨资。 Merck 两年前还在南韩,最近又在台湾设立OLED材料研发中心。BASF将在2014年在南韩设立OLED材料研发实验室。 OLED 照明和显示器件由两个电极及位于两电极之间的多层有机和金属有机材料组成。当在电极上加上一个适当的电压时,来自阳极的空穴与来自阴极的电子就会在发光层中结合,产生发光。按照材料的不同种类,OLED器件也就分成了基于小分子和基于高分子的两大类。基于小分子的OLED器件由蒸镀工艺实现多层结构,而基于高分子的OLED器件由各种溶液过程完成制作。 由于其高效率的三线态发光,金属有机磷光材料一直是过去十几年间OLED领域的一个研究和开发热点。目前红绿光材料在 Samsang 的 Galaxy S 和 Galaxy Note 系列手机显示屏上已开始应用。拥有磷光材料的核心专利的UDC在2013年通过材料销售和专利许可获得的收入估计将超过一亿四千万 美圆 。但UDC的 EP-238 的专利覆盖面太大,严重制约其它公司在 金属有机磷光材料领域进行开发,并通过对新材料开发从OLED这一钱途无量的新技术而获利。更令 上述三家公司不爽的是,这一制约其发展的关键专利根本就不具有可申请专利的基本资格(patentability)。EP-238于2006年11月2日获欧洲专利局授权, 对该项专利的无效请求始于2007年,由 默克,巴斯夫和住友化学分别提出。 马於光 等人先于该专利申请在Syn. Met.上 首次 发表的三线态磷光材料电致发光工作成为这三家公司挑战EP-238的主要依据之一。 EP-238 有30项权利。这30项权利可分为两组,其一为权利1-15,其二为权利16-30。这两组的上位权利如下: Claim 1. An electroluminescent layer comprising an emissive layer including an emissive molecule that is a phosphorescent organometallic iridium compound or a phosphorescent organometallic osmium compound ; and Claim 16. An organic light emitting device comprising a heterostructure containing an emissive layer that produces luminescent emission when a voltage is applied across the heterostructure, wherein the emissive layer includes a molecule that is a phosphorescent organometallic iridium compound or a phosphorescent organometallic osmium compound. 马於光 等人的工作以及其它几篇文章使得三家公司的律师( Lowe Hauptman Ham 专利与知识产权律师事务所)得出以下EP-238不应获得专利权的理由并分别就其进行了非常专业的论证, 最终导致欧洲专利局做出撤销全部已授专利权利的决定: 1. UDC did not invent an electroluminescent layer separate and apart from an OLED 2. UDC did not invent OLEDs or any component of an OLED 3. UDC did not invent iridium or luminescent organometallic iridium compounds a) UDC did not invent iridium or its usein an OLED b) UDC did not invent an iridium compound c) UDC did not invent Ir(ppy)3 d) UDC did not invent an emissive layer that includes an iridium compound 4. UDC did not invent phosphorescence 5. UDC did not invent organometallic phosphorescent iridium devices 6. UDC did not invent an OLED containing phosphorescent compounds 目前, UDC还有权上诉。但笔者认为,搬回局面的可能很小。 这是一起少有的在重大技术领域进行知识产权维权而引用的中国原创研究结果。也许大家会提出以下问题。 1. 吉林大学或 马於光现在的华南理工 知道这事吗? 2. 杂志Synthetic Metals的影响影子有多高? 3. 马於光 等人(Yuguang Ma,Houyu Zhang, Jiacong Shen,Chiming Che)首次报导了三线态磷光材料用于OLED器件,但他们为啥不申请专利?是因为那几个金属配位(有机)化合物性能不好嘛? 4. 如果他们申请专利,能获得EP-238那样宽的保护范围吗? 5. 仅就他们Syn. Met.文章中的数据和结果,获得的专利能有用吗? 6. UDC 会受很大影响吗? 7. 那三家公司攻破欧洲专利局后,还会转战其它国家并获得撤销UDC在其它国家申请的相同专利的胜利吗? 8. 那三家公司和其它包括中国在内的企业能由此得到好处吗? 9. 蓝光磷光材料的瓶颈是否会由于清除了一个专利障碍而引来更多的淘金者并最终得到解决?
据美国CEN周刊2011年4月18日报道,加拿大多伦多大学同时又是云南大学物理系的LU Zheng-hong教授领导的研究小组,成功的研制出一种有机发光二极管(OLEDs)氯化电极材料,在传统OLED(有机发光二极管)的电极材料上涂上一层氯原子涂层,不但可提高OLED的发光效率,还能大幅简化生产工序,降低生产成本,将加速OLED在主流平板显示和其他发光技术上的应用。CEN的介绍如下,但是LU教授等人的原始研究论文于2011年4月14日在 Science网站公布( DOI: 10.1126/science.1202992 )。 据负责该项研究的加拿大多伦多大学有关研究人员介绍,这项技术的应用极为简便,只需在现有标准工业化OLED的电极材料氧化铟锡(ITO,也称掺锡氧化铟)上增加一层一个原子厚的氯元素涂层即可。新技术不但能够提高传统OLED的电气性能,还能省去在传统OLED上大量应用的多种昂贵涂层。在氧化铟锡上涂上一层一个原子厚的氯并非难事,他们已经开发出了一种通过紫外线辅助氯化技术,可以免去使用氯气过程,从而使整个生产过程更为安全可靠。长期以来OLED都以高效闻名,但在提高亮度的情况下其效能就会出现显著的快速下降。为了对新型OLED的发光效能进行验证,研究人员将这种氯化OLED(Cl-OLED)与传统的OLED进行了对比测试。结果发现,具有氯原子涂层的OLED在提高亮度后可以避免效能下降,在发光亮度非常高的情况下,工作效率可提高一倍多。更多信息请浏览原文。 Chlorination Improves Organic Electronics Materials: Treatment could simplify manufacturing, reduce costs Jyllian N. Kemsley Chlorinating a common electrode material for organic light-emitting diodes (OLEDs) could make devices easier and less expensive to manufacture, researchers report ( Science, DOI: 10.1126/science.1202992 ). In a typical OLED, electrons move from an organic, light-emitting material to indium tin oxide. But the energy of the electrons removed from the light-emitting material is higher than the oxide can accept. Consequently, layers of other materials—for example, copper phthalocyanine—are used to bridge the gap and facilitate electron flow. The additional layers, however, add cost and complexity to manufacturing and reduce the electrical efficiency of electronic devices. In an effort to do without those extra layers, a research group led by materials science and engineering graduate students Michael G. Helander and Zhibin Wang and professor Zhenghong Lu at the University of Toronto chlorinated the electrodes by exposing the material to o -dichlorobenzene and ultraviolet light. The treatment causes chlorine radicals from the solvent to displace oxygen and bind to indium on the electrode surface. The resulting layer of polar In–Cl bonds increases the electrostatic potential just above the electrode’s surface. That change in potential increases the electron energy that the electrode can accept and closes the energy gap between the electrode and light-emitting materials, such as a phosphorescent iridium complex doped into 4,4- N,N -dicarbazole biphenyl. Electrons can then directly transfer between the light-emitting layer and the chlorinated electrode, making electronic devices easier to manufacture and more efficient to operate. The prototype devices made by the Toronto group show a substantial improvement in operating voltages and efficiency, says Franky So , a materials science and engineering professor at the University of Florida . “This approach might lead to a paradigm shift in OLED technology.”
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