CN108602668A - 提高氢气加载比率的方法 - Google Patents

提高氢气加载比率的方法 Download PDF

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CN108602668A
CN108602668A CN201780007749.0A CN201780007749A CN108602668A CN 108602668 A CN108602668 A CN 108602668A CN 201780007749 A CN201780007749 A CN 201780007749A CN 108602668 A CN108602668 A CN 108602668A
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transition metal
hydrogen
film
desorption
metal
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D·R·伯吉斯
M·R·格林沃尔德
B·W·巴比
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Abstract

本发明公开了提高过渡金属中氢气的加载比率的方法和设备。阻塞金属结构表面上的解吸位点增加了吸收和解吸过程达到平衡时氢/氘分压。阻塞的解吸位点的数量越多，可以达到越高的平衡压力以获得更高的氢加载比率。此外，由于在晶界处发生氢解吸，因此减少晶界有利于降低氢解吸速率。还公开了增加晶粒尺寸以减小晶界的方法和设备。

Description

提高氢气加载比率的方法
优先权声明
本申请要求2016年1月21日提交的题为“提高氢(氘)气加载到过渡金属中的方法”的美国临时申请号62/281,392，以及2016年6月1日提交的题为“提高氢(氘)气加载的方法”的美国临时申请号62/344,009的优先权，其内容通过引用并入本文。
技术领域
本发明涉及将氢/氘气加载到过渡金属中。
背景技术
大多数过渡金属具有吸附大量氢气并将氢气储存在金属晶格中的能力。所述吸附过程分为两步，首先吸附，然后吸收。在吸附过程中，氢分子吸附到过渡金属的表面。吸附后，每个吸附的氢分子解离成两个氢原子。然后，解离的氢原子被吸收到金属晶格的主体(bulk)中。
几种过渡金属，例如钯、镍等已经广泛用于储存氢的工业应用中。在正常条件下，钯或镍可以吸收氢气达到一定的限度。例如，钯可以达到0.7-0.8(氢原子/金属原子)的加载比率。
通常，一块金属中的气体加载比率可以通过金属的质量变化或气体中的压力变化来确定。为了使氢加载超过0.8的比率或达到超过1.0的加载比率，需要特殊的条件或需要特别长的时间。例如，仅在10,000千帕斯卡的压力下，钯可以达到0.9的加载比率。
发明内容
本申请公开了用于实现高氢气加载比率(例如高于0.9)的方法和设备，而不需要借助特别高的压力或温度。
本公开内容涉及提高氢气加载到过渡金属中。本文中术语“氢气”是指包含一种或多种氢同位素的气体或气体混合物，例如氕、氘或氚。
在一些实施方案中，通过预处理金属表面可以在一块过渡金属中实现提高氢加载比率。因为氢原子即使在吸收之后也可以从金属晶格中逸出，因此减少吸收的氢原子可以逸出的表面积能够提高氢加载比率。在一些实施方案中，通过使解吸位点失活来减少过渡金属表面上的解吸面积。例如，可以通过在过渡金属的表面上沉积薄膜来使解吸位点失活。具有沉积薄膜的过渡金属具有减少的解吸面积，并且减少的解吸面积降低了氢气的解吸速率。薄膜可以是金属或半金属的。在一个实施方案中，薄膜的厚度为1至5个单层厚。单层是一个分子厚的层。
在一些实施方案中，提高过渡金属中氢气的加载比率的方法包括通过在过渡金属的表面上沉积薄膜来减少解吸面积。沉积在过渡金属表面上的薄膜使所述表面上的解吸位点失活。
在一些实施方案中，可通过降低过渡金属中的总晶界(total grain boundaries)来减少过渡金属表面上的解吸面积。例如，通过增加过渡金属中的平均晶粒尺寸可以减小过渡金属中的总晶界。因此，提高过渡金属中氢气的加载比率的另一种方法是增加过渡金属中的晶粒尺寸。
在一个实施方案中，通过在一块玻璃上沉积过渡金属的薄膜，可以增加过渡金属中的平均晶粒尺寸。沉积方法用于制造金属涂层或薄膜。沉积方法的实例包括物理气相沉积(PVD)、化学气相沉积(CVD)等。在PVD中，一块金属线或板通过物理过程(比如溅射)转化成蒸汽。在溅射沉积工艺中，惰性气体(比如氩)的离子以足够的能量朝向金属板(溅射靶)加速以从板逐出金属原子。逐出的金属原子或离子在力场下加速到达基底并沉积在基底上。在一个实施方案中，通过在预定压力和预定温度下退火过渡金属来增加过渡金属中的平均晶粒尺寸。在另一个实施方案中，通过在预定温度和预定压力下将过渡金属的定向金属薄膜蒸发到定向基底上来增加过渡金属中的平均晶粒尺寸。金属薄膜中的定向晶粒的面内尺寸优选大于所述薄膜的厚度。在一个实施方案中，预定压力为0.1至1帕斯卡，预定温度为200℃至1000℃。在另一个实施方案中，预定压力为1×10-4至1×10-6帕斯卡，预定温度为150℃至250℃。在一些实施方案中，退火是增加晶粒尺寸的优选方法。退火引发晶粒生长。当晶粒尺寸增长时，晶粒较少，因此总晶界较小，这导致可用于解吸加载氢的表面积减小。在一些实施方案中，可以组合溅射沉积和退火的方法。过渡金属中的平均晶粒尺寸由于退火而增加，并且过渡金属的解吸面积由于溅射沉积而降低。在一些实施方案中，为了改善过渡金属中氢气的加载比率，将定向金属薄膜在150℃至250℃的预定温度和1×10-4至1×10-6帕斯卡的预定压力下蒸发到定向基底上。所述定向基底可以是定向银基底。基底上的金属薄膜包括定向的晶粒，其面内尺寸(in-plane dimension)大于所述薄膜的厚度。在一个实施方案中，所述薄膜可以是一至五个单层厚。在一些实施方案中，过渡金属可以是钯。在一些实施方案中，可以实现1.0或更高的氢加载比率。在一些实施方案中，金属薄膜在0.1至1帕斯卡的预定压力和200℃至1000℃的预定温度下进一步退火。
再次注意，在本公开内容中，术语“氢”可以指任何氢同位素，氕、氘或氚，或它们的混合物。
附图简述
图1示出了加载氢的示例性金属晶格。
图2示出了金属晶格中的示例性氢吸附和吸收过程。
图3示出了金属晶格中的示例性氢解吸过程。
图4示出了金属薄膜中不同的晶粒尺寸。
图5示出了用于提高金属晶格中的氢加载比率的示例性方法。
具体实施方式
在图1中所示的示例性过渡金属晶胞100中，金属原子形成面心立方(fcc)晶胞。包括水平分割晶胞的一组虚线作为视觉辅助。所述晶胞包括14个金属原子104，其位于所述晶胞的八个角和每个面的中心。所述fcc晶胞100加载有氢原子102，其位于晶格中的八面体间隙位置。在晶胞结构100中，氢加载比率为4个氢原子对4个金属原子，使用常规计数法(角原子的1/8，边缘中心原子的1/4，面心原子的1/2等等)。换言之，金属晶胞100中的氢加载比率已达到1.0，这在正常条件下很难实现。
在正常条件下，金属或金属结构只能达到约0.7或0.8的氢加载比率。图2示出了氢加载过程。所述加载过程解释了为什么在正常条件下难以使一块金属达到高于0.7或0.8的氢加载比率。在图2中，金属或金属晶格200部分地加载氢。在晶格200的表面202上，氢分子首先解离成氢原子102。氢原子102在表面202上的加载过程也称为吸附，并且氢原子102加载到晶格200的主体中的过程称为吸收。在氢气加载期间，两个竞争过程吸收和解吸同时发生。在吸收过程中，晶格200外部的氢原子扩散到晶格200中并被吸收到晶格200中。在解吸过程中，晶格200内的氢原子扩散到晶格200的表面，然后保留在表面或返回到气相。在氢加载过程开始时，扩散到晶格200中的氢原子比扩散出晶格200的氢原子更多，并且吸收速率超过解吸速率。随着更多的氢原子吸收到晶格200中，解吸速率逐渐增加。最终，吸收和解吸过程达到平衡状态，其中在晶格200中吸收的氢原子102的数量保持恒定，并且氢加载比率不随着时间推移而变化。
在解吸过程中，氢原子通过晶格200的表面202上的解吸位点从晶格200逸出。图3示出了一些解吸位点302。解吸位点302是吸附的氢原子102可以从晶格200逸出的位点，并且解吸过程的速率与表面上的解吸位点302的数量成正比。因此，减少解吸位点302的数量会降低解吸速率或减慢解吸过程。在较慢的解吸速率下，在较长时间内吸收速率持续高于解吸速率，直到两个竞争过程再次达到平衡。在达到平衡之前的较长时间内，吸收了更多的氢原子，从而提高氢加载比率。
在许多工业应用中，希望实现高的氢加载比率，例如高于1.0。研究表明，高压或超高压，例如高于10,000千帕斯卡，有助于获得1.2的氢加载比率。研究还表明，各种温度和压力循环有助于实现高的氢加载比率。用于在金属结构中实现氢加载比率的其它技术包括电解共沉积、离子注入和使用纳米颗粒。一些调查进一步表明，强磁场、高电压、高电解电流等可用于实现高于1.0的氢加载比率。
本公开内容教导了用于增加金属结构中的氢加载比率而不需要超过200kPa的氢压力的有利的方法和设备。在本公开内容中，金属结构是指金属或金属晶格或合金晶格。
合适的金属或金属结构选自一组过渡金属，包括钯、铱、镍、铂、铜、银、金、锌、钛、锆、铪、铬、钒、铌、钽、钼、钨、铁、钌、铑、铝、铟、锡、铅及它们的混合物。在一些实施方案中，优选钯。在一些实施方案中，实现了1.0或更高的氢加载比率。在一些实施方案中，实现了1.0至1.8之间的氢加载比率。
在一些实施方案中，金属结构(例如钯晶格)表面上的一部分氢解吸位点通过沉积在金属结构表面上的金属或半金属薄膜失活。可以使用以下元素中的一种或多种来制造所述薄膜：钛(Ti)、锆(Zr)、铪(Hf)、钒(V)、铌(Nb)、钽(Ta)、铬(Cr)、钼(Mo)、钨(Ta)、铁(Fe)、铝(Al)、镓(Ga)、铟(In)、硅(Si)、锗(Ge)和锡(Sn)。在一些实施方案中，薄膜的厚度范围为1至5个单层厚，并且通过溅射单金属靶，或不同金属的多个靶，或合金靶来沉积所述薄膜。使用先前沉积的薄膜的横截面透射电子显微镜校准用于产生仅一至五个单层的薄膜的沉积条件。在一些实施方案中，薄膜可以覆盖10至99％的表面积。在一个实施方案中，厚度为1至5个单层的薄膜覆盖超过表面积的一半。在另一个实施方案中，薄膜覆盖不到一半的表面积。计算表明，阻塞10％的解吸位点导致未阻塞位点的氢(氘)分压增加1.2倍，而阻塞99％的解吸位点导致氢(氘)分压增加10,000倍。
在一些实施方案中，通过溅射一个金属靶或多个金属靶来沉积薄膜。在一些实施方案中，通过溅射单金属靶、不同金属的多个靶或合金靶来沉积薄膜。金属靶的溅射产率是溅射沉积条件的函数。溅射产率定义为当被溅射离子撞击时从靶释放的原子数。特定金属的溅射产率取决于溅射离子所需的能量。例如，需要具有300电子伏特(eV)能量的氩离子来溅射一个镍原子。相比之下，需要能量为400eV的氙离子来溅射一个镍原子。
解吸位点是吸附的氢原子逸出晶格200的位置。如图3所示，一些解吸位点302位于晶格200的表面202上。一些解吸位点位于晶格200的晶界上(图3中未示出)。晶粒是指金属结构的一部分，其中晶体排列是不间断的。晶界是连续晶体结构中的中断，并且基本上表现为金属结构中的内表面。减少金属结构中的晶界减少了总表面积。结果，减少了解吸位点的数量，从而减慢了解吸速率。
在一些实施方案中，通过增加晶粒尺寸来实现晶界的减少。图4a-4d示出了在不同条件下(例如温度和压力)制备(例如退火)的四种示例性金属结构。由于退火条件不同，四种示例性金属结构中的每一种的平均晶粒尺寸是不同的。例如，在图4a中，金属结构中的平均晶粒尺寸最大，约为50-60nm。在图4b中，平均晶粒尺寸为30至40nm。在图4c和图4d中，金属结构在很大程度上破碎了，并且晶粒尺寸小于图4a或图4b中的晶粒尺寸。图4c中的平均晶粒尺寸落在20至30nm的范围内，并且图4d中的平均晶粒尺寸落在20至10nm的范围内。如图4a-4d所示，晶粒尺寸越大，晶界的总面积变得越小。因此，增加晶粒尺寸可以减小晶界，从而可以降低氢解吸速率。
以下是一些实施方案，其说明了可用于增加金属结构中的平均晶粒尺寸的方法和/或系统。在一些实施方案中，出于说明目的，使用特定的金属或材料(例如，钯或玻璃)作为示例。应注意，本文公开的方法和系统可适合于处理或制备其它金属或合金或具有类似性质的任何材料。
在一个实施方案中，过渡金属样品，例如钯，在真空下在0.1至0.001帕斯卡的压力和200至1000℃的温度下退火10至60分钟以诱导晶粒生长。增加金属样品的平均晶粒尺寸会降低样品中的总晶界，这会降低氢解吸的潜在面积。
在一个实施方案中，退火用于增加钯样品中的晶粒尺寸。样品在惰性气体中在标称100千帕斯卡的压力下在200℃至1000℃的温度下退火。退火过程持续约10至60分钟以诱导晶粒生长。惰性气体(溅射气体)可以是氩气或任何气体，比如氮气、二氧化碳或在退火条件下不形成化合物或扩散到钯样品中的其它惰性气体。在一些实施方案中，优选氩气。
如上所述，通过增加金属结构中的平均晶粒尺寸可以减少总晶界。在一些实施方案中，采用改进的溅射沉积工艺来产生金属薄膜，其中薄膜中的平均晶粒尺寸与所述薄膜的厚度一样大。在一个实施方案中，将5至200nm的钯薄膜以0.1至1帕斯卡的总压力在100至1000W的功率下在惰性气体中溅射沉积在一片玻璃上。当钯薄膜中的晶粒尺寸约为，例如，或者变得大于或等于所述薄膜的厚度，平均氢原子扩散距离通过薄膜的厚度比穿过晶界更短，因此使通过晶界的解吸最小化。
在另一个实施方案中，将5至200nm厚的钯薄膜以0.1至1帕斯卡的总压力在100至1000W的功率下在惰性气体中溅射沉积在一片石英玻璃上。在适当的退火条件下对薄膜进行退火直到晶粒尺寸大于薄膜的厚度。例如，钯薄膜在惰性气体存在下在标称100千帕斯卡的压力和200℃至1000℃的温度下退火。退火过程持续约10至60分钟。再例如，将钯薄膜在真空下在0.1至0.001Pa的压力下在200℃至1000℃的温度下退火10至60分钟以诱导晶粒生长。
在一些实施方案中，溅射沉积中使用的基底是定向的银基底。
在一些实施方案中，将25至50nm(100)定向的钯薄膜在1×10-4至1×10-6Pa的压力下和150℃至250℃的基底温度下蒸发到(100)定向的银(Ag)基底上，产生具有面内尺寸大于50nm的(100)定向的晶粒。应注意，(100)定向是指米勒指数100的平面，即，切割x轴但平行于y轴和z轴的平面。这些是两种薄膜的例子，其中所有晶粒具有相同的定向。当使用定向薄膜时，晶粒将比随机定向的晶粒更容易聚结形成更大的晶粒。其中所有晶粒具有大致相同定向的任何薄膜具有这种有利的行为并且可以用于本文公开的方法和装置中。没有特定的平面或平面范围更合适或更优选。
在一些实施方案中，将25至50nm(111)定向的钯薄膜在1×10-4至1×10-6帕斯卡和150℃至250℃温度下蒸发到(111)定向的Ag基底上，得到面内尺寸大于50nm的(11l)定向的晶粒。注意，(111)定向是指切割通过晶胞面的对角线和对立顶点的111平面。这些是两种薄膜的例子，其中基本上所有的晶粒将具有大致相同的定向。
在上述一些实施方案中，可以实现1.0或更高的氢加载比率。在一些实施方案中，氢加载比率优选为1.0至1.8。
图5是描绘用于提高金属材料中的氢加载的示例性过程的流程图。图5中所示的示例性过程是预处理的一个实施方案，其可以用于减少金属材料的解吸面积。通过减少金属材料表面上的解吸位点的数量或增加金属材料中的平均晶粒尺寸，可以实现解吸面积的减少。图5示出了用于增加金属材料中的平均晶粒尺寸的示例性方法。在示例性方法500中，首先将过渡金属膜溅射沉积在一块玻璃上(步骤502)。所述薄膜在0.1至1帕斯卡的预定压力和200℃至1000℃的预定温度下退火。
提高过渡金属中氢气加载比率的另一种方法包括：(i)提供过渡金属作为基底，(ii)提供溅射靶，(iii)提供溅射气体，(iv)用溅射气体溅射所述溅射靶以从溅射靶中逐出金属原子或离子，和(v)在基底上沉积逐出的金属原子或离子。
在不脱离本发明的范围和基本特征的情况下，本发明可以以不同于本文所述的其它特定方式实施。因此，本发明的实施方案在所有方面都被认为是说明性的而非限制性的，并且落入所附权利要求的含义和等同范围内的所有改变都旨在包含在其中。

Claims (19)

1.一种提高过渡金属中氢气加载比率的方法，包括：
在过渡金属表面上沉积薄膜；
通过沉积薄膜使所述过渡金属表面上的解吸位点失活；其中由于解吸位点失活，过渡金属的解吸面积减小；
其中减小的解吸面积降低了氢气的解吸速率并提高了氢气的加载比率。
2.根据权利要求1所述的方法，其中所述薄膜是金属的。
3.根据权利要求1所述的方法，其中所述薄膜是半金属的。
4.根据前述权利要求中任一项所述的方法，其中所述薄膜为1至5个单层厚。
5.根据权利要求1-3中任一项所述的方法，其中所述薄膜包括以下元素中的一种或多种：钛、锆，铪、钒、铌、钽、铬、钼、钨、铁、铝、镓、铟、硅、锗和锡。
6.根据权利要求1-3中任一项所述的方法，其中所述过渡金属是钯、铱、镍、铂、铜、银、金、锌、钛、锆、铪、铬、钒、铌、钽、钼、钨、铁、钌、铑、铝、铟、锡、铅，或它们的混合物，优选钯。
7.根据权利要求1-3中任一项所述的方法，其中提高的氢加载比率为0.9或更高。
8.一种提高过渡金属中氢气加载比率的方法，包括：
在基底上溅射沉积过渡金属的薄膜；和
在0.1至1.0帕斯卡的预定压力和200℃至1000℃的预定温度下使所述过渡金属退火，
其中所述过渡金属中的平均晶粒尺寸增加，且所述过渡金属的解吸面积减少；以及其中过渡金属中氢气的加载比率提高。
9.根据权利要求8所述的方法，其中所述过渡金属是钯。
10.根据权利要求8或9所述的方法，其中所述基底是定向的银基底。
11.根据权利要求8或9所述的方法，其中所述基底是玻璃。
12.根据权利要求8或9所述的方法，其中所述氢加载比率为0.9或更高。
13.根据权利要求8或9所述的方法，其中所述薄膜为1至5个单层厚。
14.一种提高过渡金属中氢气加载比率的方法，包括：
蒸发过渡金属；
沉积蒸发的过渡金属以在定向的基底上形成过渡金属的定向金属薄膜，其中所述定向的金属薄膜的沉积在150℃至250℃的预定温度和1×10-4至1×10-6帕斯卡的预定压力下进行；
其中所述基底上的金属薄膜包括面内尺寸大于所述薄膜的厚度的定向的晶粒。
15.根据权利要求14所述的方法，其中所述过渡金属是钯。
16.根据权利要求14或15所述的方法，其中所述基底是定向的银基底。
17.根据权利要求14或15所述的方法，其中所述氢加载比率为1.0或更高。
18.根据权利要求14或15所述的方法，其中所述薄膜为1至5个单层厚。
19.根据权利要求14所述的方法，还包括在0.1至1帕斯卡的预定压力和200℃至1000℃的预定温度下使所述过渡金属退火。
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