CN101223108A - 含钨的纳米材料及相关纳米技术 - Google Patents
含钨的纳米材料及相关纳米技术 Download PDFInfo
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- CN101223108A CN101223108A CNA200680024351XA CN200680024351A CN101223108A CN 101223108 A CN101223108 A CN 101223108A CN A200680024351X A CNA200680024351X A CN A200680024351XA CN 200680024351 A CN200680024351 A CN 200680024351A CN 101223108 A CN101223108 A CN 101223108A
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Abstract
本发明提供含钨的纳米颗粒、制备含钨的纳米颗粒的方法以及含钨的纳米颗粒的用途，如用于电子器件、光学装置、光子器件、用于精细化学合成的试剂、颜料和催化剂。
Description
相关专利申请的交叉引用
本申请为2003年10月6日提交的美国专利申请10/679,611的部分继续，此申请全文通过引用结合到本文中。本申请也为2002年12月10日提交的美国专利申请10/315,272的部分继续，此申请全文通过引用结合到本文中。本申请要求2004年5月10日提交的临时申请60/569,689的权益，此申请全文通过引用结合到本文中。
发明领域
本发明一般涉及制备含钨的亚微米和纳米粉末的方法和此粉末的用途。
相关背景
通常，尤其纳米粉末和亚微米粉末为新一系列材料，其区别特征是，它们的畴大小是如此之小，以致于大小限制效应成为材料性能的重要决定因素。因此，此限制效应可产生宽范围工业重要性能。因此，纳米粉末为宽范围装置和不同用途产品的设计、研发和工业化带来了特别的机会。此外，由于在常规粗粒物理化学机制不适用时它们代表全新系列的材料前体，这些材料给予独特的性能组合，使不匹配性能的新型多功能组件成为可能。亚微米和纳米大小粉末的一些应用由Yadav等人教授于美国专利6,344,271和同时待审及普通转让的美国专利申请09/638,977、10/004,387、10/071,027、10/113,315和10/292,263中。
发明概述
简单地讲，本发明涉及制备含钨纳米粉末的方法及其用途。
在一些实施方案中，本发明提供掺杂或未掺杂氧化钨的纳米颗粒。
在一些实施方案中，本发明提供制备含钨的掺杂或未掺杂金属氧化物的方法。
在一些实施方案中，本发明提供包含掺杂或未掺杂钨的氧化物复合材料及涂料。
在一些实施方案中，本发明提供包含掺杂或未掺杂氧化钨的粉末的用途。
在一些实施方案中，本发明提供用于多种用途的催化剂。
在一些实施方案中，本发明提供用于多种用途的添加剂。
在一些实施方案中，本发明提供用于光学、传感、热、生物医学、结构、超导、能量和安全用途及其他用途的材料及装置。
在一些实施方案中，本发明提供以大量、低成本和可再现品质制备含钨的新的纳米粉末的方法。
附图简述
图1显示制备本发明的亚微米和纳米粉末的总体示例方法。
发明详述
本发明一般涉及含钨(W)的极细粉末。教授的范围包括高纯度粉末。本文讨论的粉末具有小于1微米的平均晶粒大小，在某些实施方案中小于100纳米。本发明也概括以大量、低成本和可再现品质制备和利用此类粉末的方法。
定义
为了清楚起见，提供以下定义帮助理解本文提供的说明和具体实施例。在对一个具体变量提供一定范围数值时，此范围的上限和下限均包括在所述定义之内。
本文所用“细粉末”是指同时满足以下标准的粉末：
(1)平均大小小于10微米的颗粒；和
(2)长宽比为1至1,000,000的颗粒。
例如，在一些实施方案中，细粉末为具有小于5微米平均畴大小和1至1,000,000长宽比的颗粒的粉末。
本文所用“亚微米粉末”是指具有小于1微米平均大小的细粉末。例如，在一些实施方案中，亚微米粉末为具有小于500纳米平均畴大小和1至1,000,000长宽比的颗粒的粉末。
术语“纳米粉末”、“纳米大小粉末”、“纳米颗粒”和“纳米级粉末”在本文中可互换使用，并且指具有小于250纳米平均大小的细粉末。例如，在一些实施方案中，纳米粉末为具有小于100纳米平均畴大小和1至1,000,000长宽比的颗粒的粉末。
本文所用术语“纯粉末”为具有以金属计至少99.9％组成纯度的粉末。例如，在一些实施方案中，纯度为99.99％。
本文所用术语“纳米材料”是在任何尺寸形式具有小于100纳米畴大小的材料。
本文所用术语“畴大小”是指特定材料形态学的最小尺寸。在粉末的情况下，畴大小为晶粒大小。在晶须和纤维的情况下，畴大小为直径。在片和薄膜的情况下，畴大小为厚度。
术语“粉末”、“颗粒”和“晶粒”在本文中可互换使用，并且包括氧化物、碳化物、氮化物、硼化物、硫属化物、卤化物、金属、金属间化物、陶瓷、聚合物、合金及其组合。这些术语包括单一金属、多金属和复杂组合物。这些术语还包括空心、致密、多孔性、半多孔、涂覆、未涂覆、多层、层压、简单、复杂、枝状、无机、有机、元素、非元素、复合、掺杂、未掺杂、球形、非球形、表面功能化、表面未功能化、化学计量和非化学计量形式或物质。此外，术语粉末在其一般意义上包括一维材料(纤维、管等)、二维材料(小片、薄膜、层压材料、平面等)和三维材料(球、锥体、卵形、圆柱形、立方体、单斜、parallelolipids、哑铃形、六角形、截角十二面体、不规则形状结构等)。
本文所用术语“长宽比”是指颗粒最大尺寸与最小尺寸之比。
本文所用术语“前体”包括可转变成相同或不同组成的粉末的任何未加工物质，在某些实施方案中，前体为液体。术语“前体”包括但不限于有机金属、有机物、无机物、溶液、分散体、熔体、溶胶、凝胶、乳液或混合物。
本文所用术语“粉末”包括氧化物、碳化物、氮化物、硫属化物、金属、合金及其组合。该术语包括空心、致密、多孔性、半多孔、涂覆、未涂覆、多层、层压、简单、复杂、枝状、无机、有机、元素、非元素、分散、复合、掺杂、未掺杂、球形、非球形、表面功能化、表面未功能化、化学计量和非化学计量形式或物质。
本文所用术语“涂层”(或“薄膜”或“层压材料”或“层”)包括任何包含亚微米和纳米粉末的沉积。该术语在其范围内包括空心、致密、多孔性、半多孔、涂覆、未涂覆、简单、复杂、枝状、无机、有机、复合、掺杂、未掺杂、均匀、不均匀、表面功能化、表面未功能化、薄、厚、经预处理、经后处理、化学计量或非化学计量形式或形态学的基质、表面、沉积或其组合。
本文所用术语“分散体”包括油墨、糊、膏、洗剂、牛顿、非牛顿、均匀、不均匀、透明、半透明、不透明、白色、黑色、有色、乳化、具有添加剂、没有添加剂、水基、极性溶剂基或非极性溶剂基的任何流体或类流体态的粉末的混合物。
在一些实施方案中，本发明涉及包含掺杂或未掺杂氧化钨的亚微米和纳米粉末。假定地壳中钨量较为丰富并且目前提纯技术的限制，预料很多工业制备的材料都有天然存在的钨杂质。预料这些杂质低于100ppm，并且在大多数情况下浓度类似于其他元素杂质。除去这些杂质并不实质影响所关注应用的性质。按照本发明意图，从本发明范围排除其中钨以类似于其他元素杂质的浓度存在的含钨杂质的粉末。然而，要强调的是，在一种或多种物质的掺杂或未掺杂组合物中，可有意将钨作为掺杂剂以100ppm或更少浓度引入粉末中，并且这些包括在本发明的范围内。
在一般意义上，本发明教授纳米粉末，在更一般意义上，教授亚微米粉末，所述粉末包含至少100ppp重量钨(W)，在一些实施方案中，以金属计大于1％重量的钨(W)，在其他实施方案中，以金属计大于10％重量的钨(W)。
尽管本发明公开制备含钨的纳米和亚微米粉末的数个实施方案，但按照本发明意图，纳米或亚微米粉末可由任何方法制备或者可作为来自任何方法的副产物得到。
图1显示一般制备亚微米粉末和尤其制备纳米粉末的总体示例方法。图1所示方法始于含钨的原料(例如但不限于粗氧化物粉末、金属粉末、盐、浆、废产物、有机化合物或无机化合物)。图1显示制备本发明的纳米和亚微米粉末的系统的一个实施方案。
图1所示的方法在100始于含钨金属的前体，如乳液、流体、含颗粒的流体悬浮体或水溶性盐。前体可以为蒸发的钨金属蒸气、蒸发的合金蒸气、气体、单相液体、多相液体、熔体、溶胶、溶液、流体混合物、固体悬浮体或其组合。含金属的前体包括在流体相中具有至少某部分的化学计量或非化学计量金属组合物。流体前体用于本发明的某些实施方案。通常，流体更易于输送、蒸发和热处理，从而产生更均匀的产物。
在本发明的一个实施方案中，前体为环境良性、安全、易得、高金属负荷、较低成本的流体材料。含金属钨的前体的实例包括但不限于金属乙酸盐、金属羧酸盐、金属乙酸盐(ethanoate)、金属醇盐、金属辛酸盐、金属螯合物、金属有机化合物、金属卤化物、金属叠氮化物、金属硝酸盐、金属硫酸盐、金属氢氧化物、可溶于有机物或水的金属盐、金属的化合物(包括金属(包括钠/钾/锂)的铵化合物)及含金属的乳液。
在另一个实施方案中，如果需要复合纳米-纳米级和亚微米粉末，可将多种金属前体混合。例如，可混合钨前体和碱(或碱土)金属前体，以制备用于颜色和电陶瓷应用的钠钨氧化物粉末。作为另一个实例，可以合适比例混合钨前体、钒前体和钛前体，以制备用于催化剂应用的高纯度、高表面积、混合氧化物粉末。在另一个实例中，可将钡前体(和/或锌前体)和钨前体混合，以制备用于颜料用途的粉末。此类复合纳米和亚微米粉末可帮助制备具有令人惊讶且独特性质的材料，这种材料不能通过相应单一金属氧化物或由物理共混不同组成的粉末形成的简单纳米复合材料得到。
合乎需要使用较高纯度的前体以制备所需纯度的纳米或亚微米粉末。例如，如果需要大于x％(基于金属重量)的纯度，则被混合和使用的一种或多种前体可具有大于或等于x％(基于金属重量)的纯度。
继续参考图1，将含金属的前体100(含一种或含金属前体的混合物)送入高温处理106，例如，可用高温反应器进行。在一些实施方案中，在加入反应器106时，可将合成助剂(如反应性流体108)与前体100一起加入。此类反应性流体的实例包括但不限于氢气、氨、卤化物、碳氧化物、甲烷、氧气和空气。
虽然本文中的讨论教授制备氧化物的纳米和亚微米粉末的方法，但可很容易以类似方式将这些教授扩展到其他组合物，如碳化物、氮化物、硼化物、碳氮化物和硫属化物。制备这些组合物可利用这些组合物的微米大小粉末前体，或者利用提供这些含钨组合物中所需成分的反应性流体。在一些实施方案中，可使用高温处理。然而，也可使用本发明的方法，用适度温度处理或低/冷冻温度处理制备纳米和亚微米粉末。
前体100可在任何热处理之前以一些其他方式预处理。例如，可调节pH以保证前体稳定性。或者，可用选择性溶液化学形成溶胶或其他态物质，如在有或没有表面活性剂或其他合成助剂存在下沉淀。可在热处理之前预处理前体100或使前体部分燃烧。
可以轴向、径向、切向或在任何其他角度将前体100注入高温区域106。如上所述，前体100可与其他试剂预混合或扩散混合。可通过层流、抛物线、湍流、脉冲、剪切或旋流模式或任何其他流模式将前体100加入热处理反应器。此外，可从反应器106中的一个或多个孔将一种或多种含金属的前体100注入。进料喷射系统可产生包围热源的进料模式，或者，热源可包围进料，或者利用对此的不同组合。在一些实施方案中，喷雾以提高热转移效率、质量转移效率、动量转移效率和反应效率的方式雾化和喷射。反应器形状可以为圆筒形、球形、锥形或任何其他形状。可利用很多方法和设备，如美国专利5,788,738、5,851,507和5,984,997中教授的这些(各专利全文通过引用结合到本文中)。
继续参考图1，在前体100已加入反应器106后，可在高温处理以形成粉末产物。在其他实施方案中，可在较低温度进行热处理以形成粉末产物。为了制备具有所需孔隙率、密度、形态、分散、表面积和组成的产物(如粉末)，可在气体环境进行热处理。此步骤产生副产物，如气体。为了降低成本，可使这些气体循环、质量/热结合或用于制备所述过程所需的纯气流。
在利用高温热处理的实施方案中，可在高于1500K的温度在步骤106(图1)进行高温处理，在一些实施方案中高于2500K，在一些实施方案中高于3000K，在一些实施方案中高于4000K。此温度可用多种方法达到，包括但不限于等离子方法，在空气中燃烧、在纯化的氧或富氧气体中燃烧、利用氧化剂燃烧、热解、在适合反应器中电弧及其组合。等离子可提供反应气体，或者可提供清洁的热源。
在106高温热处理产生在一个相或多个相中包含金属的蒸气。在热处理后，在步骤110使此蒸气冷却，以使亚微米粉末(在某些实施方案中纳米粉末)成核。在某些实施方案中，在步骤110的冷却温度保持足够高以防止水分冷凝。由于方法中的热动力学条件，形成分散粒子。通过设计方法条件，如压力、停留时间、过饱和及成核速率、气体速率、流速、物质浓度、加入稀释剂、混合度、动量转移、质量转移和热转移，可调整纳米和亚微米粉末的形态。重要的是应注意到，本方法的焦点在于制备一种在满足最终应用需求和用户需要方面优良的粉末产物。
在某些实施方案中，在步骤116的冷却到较低温度后将纳米粉末淬火，以最低化并且防止凝聚或晶粒生长。适合淬火方法包括但不限于美国专利5,788,738中教示的方法。在某些实施方案中，可利用声波或超声波淬火。在其他实施方案中，可利用冷却剂气体、水、溶剂、冷表面或低温流体。在某些实施方案中，可利用能够防止粉末在传送壁沉积的淬火方法。适合方法包括但不限于静电方法、用气体覆盖、使用较高流速、机械方法、化学方法、电化学方法或对壁的声波振荡/振动。
在一些实施方案中，高温处理系统包括可能有助于过程品质控制的仪器和软件。此外，在某些实施方案中，对高温处理区域106进行操作以制备细粉末120，在某些实施方案中制备亚微米粉末，在某些实施方案中制备纳米粉末。可监控此过程气体产物的组成、温度和其他变量以保证在步骤112的品质(图1)。在纳米和亚微米粉末120已形成时，可使气体产物循环用于过程108或用作有价值原料，或者可对它们进行处理以除去环境污染物(如果有)。在淬火步骤116后，可将纳米和亚微米粉末进一步在步骤118冷却，然后在步骤120收获。
纳米和亚微米粉末产物120可由任何方法收集。适合收集方法包括但不限于袋过滤、静电分离、膜过滤、旋风分离器、冲击过滤、离心、水力旋流分离器、热泳、磁分离及其组合。
可修改在步骤116的淬火以能够制备涂层。在此实施方案中，可在包含气流的淬火粉末通道中提供基材(分批或连续方式)。通过设计基材温度和粉末温度，可形成包含亚微米粉末和纳米粉末的涂层。
在一些实施方案中，通过使细纳米粉末分散，然后应用各种已知方法，也可制备涂层、薄膜或组件，所述方法如但不限于电泳沉积、磁泳沉积、旋涂、浸涂、喷、刷、丝网印刷、喷墨印刷、色剂印刷和烧结。纳米粉末可在此步骤之前经热处理或反应，以增强其电、光、光子、催化、热、磁、结构、电子、发射、加工或成形性能。
应注意到，在本文所述方法或基于本领域的技术人员修改的类似方法的任何阶段的中间体或产物可直接用作进料前体，以便由本文教授方法和其他方法制备纳米或细粉末。其他适合方法包括但不限于共同拥有的美国专利5,788,738、5,851,507和5,984,997和同时待审的美国专利申请09/638,977及60/310,967中教授的方法，所有这些专利全文通过引用结合到本文中。例如，可将溶胶与燃料共混，然后作为进料前体混合物用于高于2500K的热处理，以制备简单或复杂纳米粉末。
概括地讲，制备粉末的一个实施方案包括(a)制备包含至少100ppm重量钨元素的前体；(b)将前体加入在高于1500K温度操作的高温反应器，在某些实施方案中高于2500K，在某些实施方案中高于3000K，在某些实施方案中高于4000K；(c)其中在高温反应器，在惰性或反应性气氛在具有高于0.25马赫速率的处理流中，前体转化成含稀土金属的蒸气；(d)使蒸气冷却，以使亚微米或纳米粉末成核；(e)使粉末在高气体速率淬火，以防止凝聚和生长；及(f)从气体过滤经淬火的粉末。
制备含钨的纳米粉末的另一个实施方案包括(a)制备包含两种或多种金属的流体前体，其中至少一种金属为高于100ppm重量浓度的钨；(b)将所述前体加入在惰性或反应性气氛中高于1500K温度操作的高温反应器，在一些实施方案中高于2500K，在一些实施方案中高于3000K，在一些实施方案中高于4000K；(c)其中在所述高温反应器，所述前体转化成含钨蒸气；(d)使蒸气冷却，以使亚微米或纳米粉末成核；(e)使粉末在超过0.1马赫的气体速率淬火，以防止凝聚和生长；及(f)从气体分离经淬火的粉末。在某些实施方案中，流体前体可包括合成助剂，如表面活性剂(已知为分散剂、封端剂、乳化剂等)，以控制形态或使过程经济和/或产物性能达到最佳。
制备涂层的一个实施方案包括(a)制备包含一种或多种金属的流体前体，其中一种金属为钨；(b)将所述前体加入在惰性或反应性气氛中高于1500K温度操作的高温反应器，在一些实施方案中高于2500K，在一些实施方案中高于3000K，在一些实施方案中高于4000K；(c)其中在高温反应器中，所述前体转化成含钨的蒸气；(d)使蒸气冷却，以使亚微米或纳米粉末成核；(e)使粉末在基材上淬火，以在基材上形成含钨的涂层。
由本文教授制备的粉末可由后处理改性，如共同拥有的美国专利申请10/113,315所教授，此中请全文通过引用结合到本文中。
纳米颗粒引入产物的方法
亚微米和纳米粉末可由任何方法引入复合结构。一些非限制示例方法教授于共同拥有的美国专利6,228,904，此专利全文通过引用结合到本文中。
可由任何方法将本文教授的亚微米和纳米粉末引入塑料。在一个实施方案中，所述方法包括(a)由任何方法制备含钨的纳米或亚微米粉末，如利用流体前体和超过1500K峰处理温度的方法；(b)提供一种或多种塑料的粉末；(c)将纳米或亚微米粉末与塑料的粉末混合；和(d)在高于塑料粉末软化温度但低于塑料粉末降解温度的温度将经混合的粉末共挤成所需形状。在另一个实施方案中，制备一种塑料粉末的母料，所述母料包含含钨的纳米或亚微米粉末。这些母料以后可由本领域技术人员所熟悉的技术加工成有用产物。在另一个实施方案中，预处理含钨金属的纳米或亚微米粉末，以便涂覆粉末表面，从而易于分散并且保证均匀性。在另一个实施方案中，利用注塑包含纳米粉末和塑料粉末的混合粉末制备有用的产物。
将纳米或亚微米粉末引入塑料的一个实施方案包括(a)由任何方法制备含钨的纳米或亚微米粉末，例如利用流体前体和超过1500K峰处理温度的方法；(b)提供一种或多种塑料的薄膜，其中所述薄膜可经过层压、挤出、吹塑、流延或模塑；和(c)将纳米或亚微米粉末由多种技术涂覆于塑料薄膜上，如旋涂、浸涂、喷涂、离子束涂覆、溅射。在另一个实施方案中，由多种技术使纳米结构涂层直接形成于薄膜上，如本文所教授的那些技术。在一些实施方案中，涂层的晶粒大小小于200nm，在一些实施方案中小于75nm，在一些实施方案中小于25nm。
可由任何方法将亚微米和纳米粉末引入玻璃中。在一个实施方案中，将钨纳米颗粒引入玻璃是通过(a)由任何方法制备含钨的纳米或亚微米粉末，如在惰性或反应性气氛中利用流体前体和超过1500K温度的方法；(b)提供玻璃粉末或熔体；(c)将纳米或亚微米粉末与玻璃粉末或熔体混合；和(d)将包含纳米颗粒的玻璃加工成所需形状和大小的制品。
可由任何方法将亚微米和纳米粉末引入纸中。在一个实施方案中，所述方法包括(a)制备含钨的纳米或亚微米粉末；(b)提供纸浆；(c)将纳米或亚微米粉末与纸浆混合；和(d)将混合的粉末加工成纸，如模压、伏辊挤压和压光。在另一个实施方案中，预处理含钨金属的纳米或亚微米粉末，以便涂覆粉末表面，从而易于分散并且保证均匀性。在另一个实施方案中，将纳米颗粒直接涂覆在制成的纸或纸基产物上；纳米颗粒的小尺寸使它们能够穿透纸结构或停留在纸的表面上，从而使纸功能化。
可由任何方法将本文教授的亚微米和纳米粉末引入皮革、纤维或织物。在一个实施方案中，所述方法包括(a)由任何方法制备含钨的纳米或亚微米粉末，如包括高于1000K操作的步骤的方法；(b)提供皮革、纤维或织物；(c)使纳米或亚微米粉末与皮革、纤维或织物结合；和(d)将经结合的皮革、纤维或织物加工成产品。在另一个实施方案中，预处理含钨金属的纳米或亚微米粉末，以便涂覆粉末表面或使粉末表面功能化，从而易于结合或分散或保证均匀性。在另一个实施方案中，将纳米颗粒直接涂覆在基于皮革、纤维或织物的制成产品上；纳米颗粒的小尺寸使它们能够粘合到或穿透皮革、纤维(聚合物、羊毛、棉、亚麻、来源于动物、来源于农业)或织物，从而使皮革、纤维或织物功能化。
可由任何方法将亚微米和纳米粉末引入膏或油墨中。在一个实施方案中，所述方法包括(a)由任何方法制备含钨的纳米或亚微米粉末，如利用流体前体和高于1500K的峰处理温度的方法；(b)提供膏或油墨的制剂；和(c)使纳米或亚微米粉末与膏或油墨混合。在另一个实施方案中，预处理含钨的纳米或亚微米粉末，以便涂覆粉末表面或使其功能化，从而易于分散并且保证均匀性。在另一个实施方案中，将膏或油墨的预存在制剂与纳米或亚微米粉末混合，以使膏或油墨功能化。
含钨的纳米颗粒可能难以分散于水、溶剂、塑料、橡胶、玻璃、纸等。在某些实施方案中，纳米颗粒的分散性可通过处理氧化钨粉末或其他含钨的纳米颗粒的表面来增强。在某些实施方案中，处理步骤可产生物理结合。在其他实施方案中，处理步骤可使合乎需要的官能团化学结合到纳米颗粒的表面上。例如，为了增强表面相容性，可将脂肪酸(例如，丙酸、硬脂酸和油)或含硅的有机金属化合物或含钛的有机金属化合物应用到纳米颗粒。如果粉末具有酸性表面，可将氨、季盐或铵盐涂覆到表面，以达到所需表面pH。在其他情况下，可用乙酸清洗来达到所需表面状态。可施加磷酸三烷基酯和磷酸以减小起尘和化学活性。在其他情况下，可热处理粉末以改善粉末的分散性。
含钨的纳米颗粒和亚微米粉末的应用
颜料
包含多种金属氧化物的含钨纳米颗粒提供一些作为颜料令人惊讶并且独特的益处。与晶粒大小比可见波长(400-700nm)大得多的颗粒比较，纳米颗粒比可见光波长小，使可见波长以独特方式与纳米颗粒相互作用。纳米颗粒的小尺寸也可产生更均匀分散。在某些实施方案中，重要的是，纳米颗粒不附聚(即，没有烧结的颈形成或硬附聚)。在一些实施方案中，纳米颗粒具有未功能化(即干净)表面；在其他实施方案中，使表面改性或功能化，以便能够与其中需要分散它们的基质结合。
制备无机颜料的突出方法挑战之一是保证复杂多金属制剂中元素的均匀点阵水平混合的能力。本文所述方法的特征之一是以所需的均匀度制备复杂组合物的能力。因此，本文所示教授理想适于用含钨的纳米颗粒产生颜色，并且制备出色表现的颜料。
含钨颜料的一些非限制实例为氧化钨钡、氧化钨锌、氧化钨钙、掺锡的氧化钨、钨青铜、磷钨钼酸和非化学计量的含钨物质。
在一个实施方案中，制备着色产物的方法包括(a)制备含钨的纳米或亚微米粉末；(b)提供一种或多种塑料的粉末；(c)将纳米或亚微米粉末与塑料粉末混合；和(d)将混合的粉末加工成产物。在另一个实施方案中，预处理含钨的纳米或亚微米粉末，以便涂覆粉末表面，从而易于分散并且保证均匀性。在另一个实施方案中，可利用挤出或注塑包含纳米粉末和塑料粉末的混合粉末制备有用产物。
添加剂
含钨的纳米物质为有用的润滑添加剂。非限制实例为二硫化钨纳米颗粒。在某些实施方案中，二硫化钨纳米颗粒的小尺寸使得能够以降低的成本制造较高性能的较薄薄膜。在某些较佳实施方案中，此类润滑纳米颗粒给予使力更均匀分布的能力。在某些实施方案中，如高精确度，紧密间隙移动表面，可将润滑添加剂加入到润滑流体或油中以改善寿命或发动机或引擎。使润滑纳米颗粒添加剂有用的独特特征是，纳米技术能够使颗粒大小小于自然出现的特征粗糙度大小。纳米颗粒进入和缓冲(或停留)于裂缝、槽中，从而降低内部破坏压力、力和无效的热效应。这些添加剂能够分散于现有或新润滑制剂中，并因此以容易的方式结合纳米技术益处。二硫化钨、二硫化钼、硫化钨钼和此类无机或有机纳米颗粒组合物也为其他场合的有用润滑添加剂，例如剃须刀和任何需要最小化不利摩擦效应的表面。
生物化学分析剂
氧化钨钠纳米颗粒，在某些实施方案中为高纯度形式，可用于生物化学分析。含钨纳米颗粒的高表面积，尤其在平均颗粒大小小于100nm时，使它们可用于这些应用。
硫和碳分析促进剂
钨纳米颗粒，在某些实施方案中为金属形式，可通过在感应炉中燃烧用于碳和硫的分析。含钨的纳米颗粒的高表面积和表面活性，尤其在平均颗粒大小小于100纳米时，使它们可用于这些应用。
电和照明应用
含钨的纳米材料作为电子发射剂提供多种独特有益效果。这些有益效果是由于(a)纳米颗粒的小尺寸能够使薄膜装置很薄，(b)高表面积能够降低烧结温度并且减少烧结时间(times)，(c)钨金属的固有低蒸气压，即使在高温，和(d)独特的量子限域和晶界效应。可利用这些性质制备改善的电子发射装置和电接触。复印机、传真机、激光打印机和空气净化器都可得益于由含钨纳米材料制成的充电线(charger wire)。可由含钨纳米粉末制成的其他纳米装置包括电极、化学传感器、生物医学传感器、磷光体和抗静电涂层。含钨纳米材料也提供用于化学机械抛光应用的新组合物。
由于上述原因，在某些实施方案中，含钨的纳米材料尤其用于阴极射线管中的直接加热阴极或间接加热阴极的加热线圈、显示器、x-射线管、速调管、微波炉用的磁控管和电子管。含钨的多金属纳米材料组合物包括用于高强度放电灯和焊接电极的基于稀土和氧化钍的那些材料。X-射线装置阳极也可得益于含钨纳米材料的低蒸气压和热导率。
蒸气压、电导率和电子性能的独特组合使含钨的纳米材料组合物用作高功率半导体整流装置、高电压断路器(例如W-Cu、W-Ag接触)的基片。在其他实施方案中，不同形式含钨的渗透纳米复合材料用于这些应用。高温炉部件，如加热线圈、反射器、热电偶，也可得益于含钨纳米材料的量子受限和低蒸气压性质。
由于同样以上讨论的独特性质组合，含钨纳米材料用于照明应用(如白炽灯)。示例应用包括家用电灯、汽车灯和泛光或投影应用的反光灯。特种灯也可得益于本文教授的纳米技术用于多种应用，例如但不限于音频-视频投影器、光纤系统、摄影机灯、机场跑道标志、影印机、医学和科学仪器以及舞台或演播室系统。在照明产品和应用的某些实施方案中，含钨材料的合金和分散增强形式很有用。
电子应用
在某些实施方案中，含钨纳米材料用作磷光体和电子材料。这些有益效果是由于(a)纳米颗粒的小尺寸能够使薄膜装置很薄，(b)高表面积能够降低烧结温度并且减少烧结时间，(c)钨金属的固有低蒸气压，即使在高温，(d)显著的热导率和电导率，和(e)独特的量子限域和晶界效应。可利用这些性质制备用于x-射线的改善的磷光体(例如，氧化钨钙、氧化钨镁)。改善且更成本有效的基于含钨和铜的除热组件的散热器可由纳米材料制成。含钨的纳米材料油墨(水、溶剂或紫外固化)、粘合剂和糊可用于开发用于陶瓷电路板和其他应用的电极和导体。
对于硅基半导体装置，钨纳米材料给予严格的热膨胀系数。与上述其他有用性质结合，钨和含钨的复杂组合物提供这样的材料，该材料可有助于取得类似于包含微电子技术中所用硅和金属的组合物的热膨胀系数。可利用这些性质制造改善的微电子组件。含钨的纳米材料油墨和糊可用于制备改良的DRAM芯片、其他硅装置和液晶显示器产品。
可用任何方法在所教授的电子装置中利用含钨的纳米颗粒。在一个实施方案中，在微型电池中利用含钨的纳米颗粒的方法包括(a)制备含钨的纳米或亚微米粉末；(b)用粉末制备油墨(水基、溶剂基或紫外可固化单体基油墨)或粘合剂或糊；和(c)利用油墨或粘合剂或糊制备电子装置。
催化剂
含钨纳米颗粒，如氧化物、硫化物和杂多络合物，为多种化学反应的有用催化剂。例如，它们可用于水合、脱水、羟基化和环氧化反应作为催化剂或助催化剂。在一个实施方案中，制备催化剂或助催化剂的方法包括(a)制备含钨的纳米粉末，使得所述粉末的表面积大于25平方米/克，在一些实施方案中大于75平方米/克，在一些实施方案中大于150平方米/克；和(b)在还原环境将粉末还原(或以任何其他方式使粉末活化)，然后在包含掺杂或未掺杂钨化合物的纳米粉末存在下进行化学反应。在一些实施方案中，可在化学反应进行前，利用在溶剂中分散纳米粉末，然后由所述分散体使这些粉末沉积于基质上的其他步骤。
可将上述催化剂粉末与沸石和其他明确的多孔材料混合以增强有用化学反应的选择性和收率。
光学和磷光体
含钨的非化学计量纳米颗粒提供作为磷光体和用于探测器应用的多种独特有益效果。这些有益效果是由于一个或多个以下特征(a)小尺寸，(b)高表面积，(c)在各种介质、油墨和固体基质中的分散性，(e)密度、蒸气压、功函数和带隙的独特和复杂组合。包含含钨纳米颗粒的磷光体和探测器的优点是(a)每英寸高点数密度，(b)形成均匀产物的能力，和(c)制备极薄薄膜，从而减少相同或优良性能所需原料的能力。为了提供所需亮度水平、衰减时间及其他性质，也可对纳米颗粒进行后处理(煅烧、烧结)，以使晶粒生长到最佳大小。
在某些实施方案中使用含钨的多金属组合物(二、三、四或更多种金属)。荧光组合物的具体实例为钨酸钙。这些磷光纳米粉末可用于闪烁计数器、显示器应用、电灯、荧光灯、发光装置、标志、保密(security)颜料、织物颜料、发光漆、玩具、特殊效果等。
含钨的纳米颗粒可用于形成含钨的薄膜，该薄膜在亮光中失去氧，从而变成带蓝色并且滤光；这些薄膜在黑暗中重新氧化，从而变成透明。含钨的纳米材料的很多有用性质之一是钨易失去氧的能力(例如，WO3-W20O58转变)。
间隙化合物
含钨的间隙化合物(例如，碳化物、氮化物、硼化物、硅化物)在硬、耐火应用提供多种独特有益效果。这些有益效果是由于一个或多个以下特征(a)尺寸，(b)硬度，(c)尺寸限制，(e)密度、蒸气压和物理性质的独特和复杂组合。为了提供其他所需性能，也可对纳米颗粒进行后处理(煅烧、烧结)，以使晶粒生长到最佳大小。含钨(和其他金属)的间隙纳米材料组合物用于切削工具、窑的结构元件、涡轮机、引擎、喷砂嘴、保护性涂层等。
合成用的试剂和原料
含钨(如氧化钨)的纳米颗粒和含钨的多金属氧化物纳米颗粒为制备含钨的纳米颗粒其他组合物的有用试剂和前体。在一般意义上，含钨的纳米颗粒与另一种物质即试剂反应，试剂如但不限于酸、碱、有机物、单体、氨，还原流体、氧化流体、卤素、磷化合物、硫属化物、生物材料、气体、蒸气或溶剂；纳米颗粒的高表面积促进反应，由此反应得到的产物也为纳米颗粒。试剂可采取任何合适形式，并且可包含氮、卤素、氢、碳或氧。
这些纳米颗粒产物然后可适用于或用于催化或作为试剂制备宽范围应用的其他精细化学品。利用含钨纳米颗粒的几个非限制实例如下。这些教授可扩展到多金属氧化物及其他组合物，如钨间隙化合物和基于钨的有机金属。在某些实施方案中，可在使用前在不同温度、压力、装料或环境组合下处理或功能化或活化纳米颗粒。
钨：使氧化钨纳米颗粒与碳或与包含氢的还原气体在高于450℃温度反应，以制备钨的纳米颗粒。在某些实施方案中，可利用较低温度。如果是其他实施方案，则可利用在真空或环境压力或更高压力在如800K、1200K等的温度加热纳米晶体。钨金属纳米颗粒用于很多应用(如形成灯丝等的钨金属线)，并且作为前体用于形成含钨物质的其他组合物。
制备含钨纳米颗粒的一个实施方案包括(a)制备包含氧化钨的纳米粉末，(b)使纳米粉末与还原化合物或环境反应；和(c)收集得到的含钨纳米颗粒。含钨纳米材料的较高表面积令人惊讶地使转化在较低温度和较少时间进行。在某些实施方案中，加工温度和时间降低至少10％。在某些实施方案中，加工温度和时间降低至少30％。在某些实施方案中，加工温度和时间降低至少50％。在某些实施方案中，加工温度和时间降低至少70％。
卤化钨：使含钨纳米颗粒与含卤素化合物反应，以生成含卤化钨的化合物。作为说明但不限制，使钨纳米颗粒氯化以制备蓝黑色结晶WCl6固体纳米颗粒。在一个实施方案中，氯化在高于400℃和100-1000托进行(在其他实施方案中可使用其他T和P的组合)。在某些实施方案中，提供过大体积要注意体积膨胀与相变换。通过在氯化期间加入氧或水分，可生成钨的氯氧化物。在一个实施方案中，通过使氟与钨纳米颗粒反应制备氟化钨。在某些实施方案中，通过交换反应生成溴化钨WBr6，例如在BBr3与WCl6纳米颗粒之间的交换反应。在另一个实施方案中，通过使溴蒸气与钨纳米颗粒在高于350℃反应制备WBr5。氟氧化物(例如WOF4)，为极端吸湿性，可通过氧-氟混合物与钨金属纳米颗粒反应来生成。在其他实施方案中，混合钨、氧化钨和过量碘随后在高于300℃反应产生二碘氧化钨(WO2I2)。
低氧化钨：可使氧化钨(WO3黄色)纳米颗粒与还原化合物如氢反应，以制备低氧化钨(例如WO1.63-2.99)的纳米颗粒。低氧化物具有不同于化学计量三氧化物形式的颜色(例如绿、黄、蓝、棕)。进一步还原产生浅灰色W3O，并且提供氧化物和金属化合物两者的性质。
钨青铜：钨青铜纳米颗粒可由通式M1-xWO3表示。在此通式中，M可以为碱金属(Na、K、Cs)或其他金属。通式中的x可以为0或大于0且小于1的任何数。钨青铜纳米颗粒可通过氧化钨纳米颗粒与任何M的化合物反应制备。在一些实施方案中，它为金属M的氧化物、M的氢氧化物或金属M。在其他实施方案中，可利用其他组合物。反应可由高温、真空、高压、气体环境(如氢或含碳物质或氧或惰性气体)辅助。制备钨青铜纳米颗粒的其他方法包括电解还原、熔化、固态反应、共缩、气相沉积、溅射等。在一些实施方案中，不同组成的纳米颗粒使以均匀性质成本有效地制备成为可能。
钨青铜纳米颗粒给予独特的性质。作为说明而非限制，钠钨青铜在x＞xc时提供正电阻温度系数，而在x＜xc时提供负电阻温度系数。xc取决于颗粒大小、缺氧和其他纳米颗粒性质。例如，在某些实施方案中xc为0.3，在其他实施方案中为0.6，而在其他实施方案中可为另一个数值。
含钠钨青铜的纳米颗粒依Na1-xWO3中x的值提供具有金属光泽的强色。可将这些及其他含钨纳米颗粒与云母或其他小片混合以提供特殊效果颜料。钨青铜的纳米颗粒也可作为催化剂用于氧化反应和燃料电池应用。
混合金属钨化合物：可使钨金属纳米颗粒或氧化钨纳米颗粒与其他含金属的纳米颗粒反应，以制备含钨的混合金属化合物的纳米颗粒。此类化合物的实例包括但不限于BaWO4、CdWO4、CaWO4、SrWO4、PbWO4、Na2WO4、Ce2(WO4)3等。或者，如前面讨论，也可直接从前体制备混合金属组合物，如这些钨酸盐。钨酸盐纳米颗粒为光学、电子、催化剂、颜料和其他应用的有用材料。陶瓷、抗腐蚀和阻燃制剂也可得益于钨酸盐纳米材料的独特表面活性、小尺寸及其他性质。
多钨酸盐化合物：在某些调配条件如pH改变时，如上讨论的钨酸盐显示形成独特多钨酸盐纳米簇的性质。通过调节pH、在有机酸中混合、单体等，可制备偏钨酸盐、仲钨酸盐、杂多阴离子、同多阴离子等。杂多钨酸盐纳米颗粒，如包含K、Co、P、Ce、稀土和大阳离子的那些纳米颗粒，可用作催化剂、金属和合金的钝化，并且作为沉淀剂用于有色色淀、调色剂和染料制备。
实施例1-2：氧化钨粉末
将钨酸铵前体溶于50∶50水和异丙醇混合物。利用约150标准升/分钟氧气，将此混合物以约100毫升/分钟速率喷入本文所述的DC热等离子反应器。热等离子反应器中的峰温度高于3000K。使蒸气冷却以使纳米颗粒成核，然后由Joule-Thompson膨胀淬火。收集的粉末用X-射线衍射(Warren-Averbach分析法)和BET分析。经发现，粉末具有小于100nm的微晶大小和大于10m2/gm的比表面积。也发现，该纳米粉末易分散于水、极性溶剂、非极性溶剂和紫外可固化单体中，证明能够容易地用这些纳米粉末制备油墨。
下一步，在单独的试验中使用相同方法，利用约150标准升/分钟氧气，将所述混合物以约75毫升/分钟速率喷入。热等离子反应器中的峰温度高于3000K。使蒸气冷却，然后由Joule-Thompson膨胀淬火。收集的粉末用X-射线衍射(Warren-Averbach分析法)和BET分析。经发现，粉末具有小于75nm的微晶大小和大于15m2/gm的比表面积。
这些实施例显示可以制备含钨的纳米颗粒，并且氧化钨粉末的性质可随方法变化而改变。
实施例3：氧化锡钨粉末
利用高于2000K的峰温度，在热淬火反应器中处理含偏钨酸铵和锡有机金属化合物的混合物。使蒸气冷却，然后由Joule-Thompson膨胀淬火。经发现，粉末具有小于40nm的平均微晶大小。经观察，粉末为漂亮的蓝色。此实施例显示，可用热等离子方法产生蓝色纳米颜料。
通过研究本文公开的本发明的说明或实施方案，本发明的其他实施方案对本领域技术人员显而易见。因此，希望将这些说明和实施例仅作为示例考虑，本发明的真实范围和精神由以下权利要求指明。
Claims (18)
1.一种物质的纳米材料组合物，所述组合物包含：
(a)钨；和
(b)至少一种不同于钨的金属，
其中所述物质的组合物为纳米颜料。
2.权利要求1的物质的纳米材料组合物，其中所述至少一种不同于钨的金属为钠。
3.权利要求1的物质的纳米材料组合物，其中所述组合物包含钨青铜。
4.一种物质的纳米材料组合物，所述组合物由含钨的纳米颗粒与试剂反应制备。
5.一种电子或光学装置，所述装置包含权利要求4的纳米材料。
6.一种制备物质的组合物的方法，所述方法包括：
(a)提供包含含钨纳米颗粒的第一组合物；和
(b)使第一组合物的纳米颗粒与试剂反应，
其中所述反应生成不同于第一组合物的第二组合物。
7.权利要求6的方法，其中所述第一组合物包含具有大于1的长宽比的颗粒。
8.权利要求6的方法，其中所述第一组合物包含氧。
9.权利要求6的方法，其中所述试剂包含氮。
10.权利要求6的方法，其中所述试剂包含卤素。
11.权利要求6的方法，其中所述试剂为酸或碱。
12.权利要求6的方法，其中所述试剂包含氢。
13.权利要求6的方法，其中所述试剂包含氧。
14.权利要求6的方法，其中所述试剂包含碳。
15.权利要求6的方法，其中所述反应在具有高于450℃的温度的环境进行。
16.权利要求6的方法，其中所述第一组合物包含两种或多种金属。
17.一种产物，所述产物包含用权利要求6的方法制备的物质的组合物。
18.一种油墨，所述油墨包含用权利要求6的方法制备的物质的组合物。
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| US11/125,316 | 2005-05-10 | ||
| US11/125,316 US7708974B2 (en) | 2002-12-10 | 2005-05-10 | Tungsten comprising nanomaterials and related nanotechnology |
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| CNA200680024351XA Pending CN101223108A (zh) | 2005-05-10 | 2006-05-10 | 含钨的纳米材料及相关纳米技术 |
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| US (2) | US7708974B2 (zh) |
| EP (1) | EP1888465A4 (zh) |
| JP (2) | JP2008545020A (zh) |
| KR (1) | KR20080026097A (zh) |
| CN (1) | CN101223108A (zh) |
| WO (1) | WO2007092030A2 (zh) |
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-
2005
- 2005-05-10 US US11/125,316 patent/US7708974B2/en not_active Expired - Fee Related
-
2006
- 2006-05-10 EP EP06849773A patent/EP1888465A4/en not_active Withdrawn
- 2006-05-10 JP JP2008511285A patent/JP2008545020A/ja active Pending
- 2006-05-10 CN CNA200680024351XA patent/CN101223108A/zh active Pending
- 2006-05-10 KR KR1020077028519A patent/KR20080026097A/ko not_active Application Discontinuation
- 2006-05-10 WO PCT/US2006/017965 patent/WO2007092030A2/en active Application Filing
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2010
- 2010-04-27 US US12/768,020 patent/US20100210450A1/en not_active Abandoned
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2012
- 2012-08-07 JP JP2012174731A patent/JP2012255163A/ja active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105263857A (zh) * | 2013-03-14 | 2016-01-20 | 麻省理工学院 | 烧结纳米晶合金 |
| US10407757B2 (en) | 2013-03-14 | 2019-09-10 | Massachusetts Institute Of Technology | Sintered nanocrystalline alloys |
| US11634797B2 (en) | 2013-03-14 | 2023-04-25 | Massachusetts Institute Of Technology | Sintered nanocrystalline alloys |
| US11674205B2 (en) | 2013-03-14 | 2023-06-13 | Massachusetts Institute Of Technology | Alloys comprising chromium and second metal material |
| CN104445419A (zh) * | 2014-12-02 | 2015-03-25 | 湖南省华京粉体材料有限公司 | 一种碳刷用二硫化钨复合材料的制备方法 |
| CN104445419B (zh) * | 2014-12-02 | 2016-08-17 | 湖南省华京粉体材料有限公司 | 一种碳刷用二硫化钨复合材料的制备方法 |
| US11644288B2 (en) | 2015-09-17 | 2023-05-09 | Massachusetts Institute Of Technology | Nanocrystalline alloy penetrators |
| CN111498906A (zh) * | 2019-07-17 | 2020-08-07 | 中国科学院上海硅酸盐研究所 | 透明遮热材料、透明遮热微粒子分散体及其制法及用途 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1888465A2 (en) | 2008-02-20 |
| US20050271566A1 (en) | 2005-12-08 |
| US20100210450A1 (en) | 2010-08-19 |
| KR20080026097A (ko) | 2008-03-24 |
| WO2007092030A3 (en) | 2008-01-17 |
| WO2007092030A2 (en) | 2007-08-16 |
| US7708974B2 (en) | 2010-05-04 |
| JP2012255163A (ja) | 2012-12-27 |
| EP1888465A4 (en) | 2010-12-29 |
| JP2008545020A (ja) | 2008-12-11 |
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