CN1441854A - 制备超薄保护涂层的方法 - Google Patents

制备超薄保护涂层的方法 Download PDF

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CN1441854A
CN1441854A CN01812313A CN01812313A CN1441854A CN 1441854 A CN1441854 A CN 1441854A CN 01812313 A CN01812313 A CN 01812313A CN 01812313 A CN01812313 A CN 01812313A CN 1441854 A CN1441854 A CN 1441854A
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soccerballene
substrate
described method
fullerene
target
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J·W·戴克斯
J·W·赫恩
J·E·安杰洛
W·D·莫斯利
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Seagate Technology LLC
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Abstract

在真空室中放置一富勒烯靶子和一基底。将具有足够能量可从靶子上发射富勒烯分子，但不足以形成显著量比所述靶子富勒烯更高分子结构的富勒烯的带电粒子束206，即电子束或离子束，投射在靶子208上。富勒烯214就在所述基底212上沉积。不论沉积富勒烯所用的是什么方法，在沉积过程中可以加热所述基底212到高于富勒烯－富勒烯解吸温度的某个温度，形成由大约富勒烯单层组成的涂层。

Description

制备超薄保护涂层的方法
发明领域
本发明涉及用于物件的保护涂层，具体涉及存储和/或检索数据用的磁盘驱动系统中部件的保护涂层，该部件包括例如读/写磁头和存储磁盘。
发明背景
许多技术中的进步已经对各种器件生产中所用的材料提出了很高要求。尤其在提高性能要求的同时，小型化降低了可允许的偏差。涂覆技术已经变得极重要，因为涂层在保持下面基底所需性能的同时，可以用来改变组合物的表面性能。特别是，薄的涂层可以用来保护下面的基底，免受各种侵害。
旋转的磁、光和光磁数据存储器件使用数据存储磁片，带有固定在空气动力滑触头上的磁头，从磁盘读取数据和/或写入数据。滑触头有着面对磁盘表面的空气轴承表面。在使用时，滑触头以一预定的距离“浮动”在飞速旋转的磁盘上面。
数据存储磁盘驱动器可以使用一片或多片具有信息存储介质的磁盘。在磁盘或磁光盘驱动器中，所述介质包括在一非磁性基底上较薄的磁层。数据存储于沿同心数据磁道的一些特定位置上，通常在数据存储区域内。
滑触头和磁盘表面之间的间歇接触会导致磁盘表面和滑触头的磨损。为了保护磁盘表面和/或滑触头免于磨损和腐蚀，在磁盘表面和/或滑触头表面包括磁头的磁性介质上涂上保护层。优选的保护层能降低滑触头和磁盘的磨损、摩擦和氧化，同时能保持在旋转期间以及在开始和停止旋转时，滑触头和磁盘表面之间空气动力的相互作用。在加工和制造过程中，也在磁头和滑触头上使用保护层来保护磁头。
为了在磁盘表面获得更高的存储密度，正日益减小读/写磁头和磁盘表面之间的浮动高度。例如，对于高密度磁盘驱动器来说，要求浮动高度小到大约10纳米(nm)并不鲜见。减小浮动高度能提高磁头和磁盘表面之间的磁性相互作用，结果能相应地达到更高的数据存储密度。因此，保护涂层要足够薄，以免过分增大磁头的磁性转换器和接近磁盘表面的磁性材料之间的有效距离。因此，当要求浮动高度为10nm时，保护涂层应该很薄，宜不大于1nm。
在基底上已经使用碳涂层来形成保护层。但是这种涂层增大了表面和下面基底之间的距离。因此，例如在生产磁盘中，保护涂层等的存在所导致的磁头和磁性介质之间距离增大的作用会抵消减小浮动高度所产生的性能提高。
最近，在磁盘驱动器中已经研究了富勒烯作为磁性器件如磁盘用的潜在涂层材料。例如，美国专利No.5,374,463说明了具有由厚度为30～150埃(3～15nm)的多层富勒烯形成的薄膜涂层的磁盘。但是，所述富勒烯涂层对于目前磁盘驱动器的浮动高度要求来说太厚了。本发明提供一种解决此问题和其它问题的方法，并提供已有技术不具有的其它优点。
发明概述
本发明提供在基底上沉积富勒烯涂层的方法。在一真空室中放置一富勒烯靶子和一基底。将具有足够能量可从靶子上发射富勒烯分子但不与富勒烯反应的带电粒子束即电子或离子束投射在靶子上。使产生的富勒烯沉积在基底上。
在另一实施方式中，将基底加热至高于富勒烯-富勒烯解吸温度的某一温度，将富勒烯沉积在基底上形成由大约富勒烯单层组成的涂层。
本发明的其它特征和优点，可以通过阅读以下详细说明并参考相关附图可以显而易见。
附图简要说明
图1是可应用本发明的磁盘驱动器的透视图。
图2说明形成本发明优选实施方式的富勒烯涂层的设备和方法。
示例性实施方式的详细说明
图1是使用本发明的磁盘驱动器100的透视图。磁盘驱动器100包括带有基座102和顶盖(未显示)的外壳。磁盘驱动器还包括用磁盘夹具108安装在主轴电动机(未显示)上的磁盘组106。磁盘组106包括围绕于中心轴109安装的共同旋转的许多个磁盘107。每个磁盘表面具有相关的磁头-滑触头110，它安装在磁盘驱动器100上，能和面对的磁盘表面传递信息。磁头-滑触头110包括浮动在磁盘组106的单独磁盘的相关磁盘表面上方的滑触头结构和用于从面对磁盘表面上的同心磁道读取数据和写入数据的转换磁头111。在图1所示的例子中，通过连接在执行机构116的磁道存取臂114上的悬架112来支撑磁头-滑触头110。通过音圈电动机(VCM)的驱动，执行机构116与其连接的磁头110绕着驱轴120转动。执行机构116的旋转使磁头沿弓形轨迹122移动，将磁头定位在磁盘内径124和磁盘外径126之间所需的数据磁道上方。音圈电动机118通过装在电路板128上的伺服电子器件，根据磁头-滑触头110的磁头和电脑主机(未显示)提供的信号而驱动。在电路板128上还包括读取和写入的电子器件，根据通过磁头-滑触头110的读取磁头从磁盘组106读取的数据为主计算机提供信号，并向磁头-滑触头110的写入磁头提供写入信号，将数据写入磁盘中。
由主轴电动机带动磁盘107沿箭头132方向的旋转，会在磁盘表面上产生风。滑触头110抗着风的作用以设计距离浮动在相应磁盘的表面上。
上述Dykes等人的申请描述了在洁净金属或半导体基底表面上含有纯化富勒烯材料单层的超薄保护涂层，所述富勒烯牢固地结合在基底表面上。富勒烯-金属/半导体的吸引力比各层之间富勒烯-富勒烯的吸引力要强。优选C60富勒烯作为涂层材料，因为它对基底有很强的附着力，并且比较容易获得。富勒烯是具有开放笼形结构的碳簇分子，所述结构以分子表面上是4～6面的多边形或环形为特征。就其总体形状，C60分子是球形的，有点类似于足球，所以有时称为具有“足球”分子结构。例如，熟知的富勒烯包括也称为“巴奇球”的C60(buckminster富勒烯)、C70、C80和C84。富勒烯分子的直径约为5～10埃(0.5～1.0纳米)。
富勒烯分子对洁净金属和半导体表面呈现极强的附着力，且耐腐蚀，还提供适合的摩擦性质。富勒烯分子对洁净金属或半导体基底所形成的结合/键合比和富勒烯分子之间所形成的更强。
富勒烯分子附着在洁净金属半导体基底上，其强度超过了富勒烯-富勒烯的分子间作用力。富勒烯附着在另一物体上的强度，可以通过富勒烯分子从表面上的凝聚相解吸或蒸发的温度来衡量。所述解吸温度和富勒烯与表面之间的结合/键合的强度有关。更高的解吸温度表示更强的结合/键合，反之亦然。对于有些表面，该表面和富勒烯会在低于解吸的温度下反应，这时该反应温度就为键合强度提供一个下限。
就多层富勒烯涂层而言，它是具有多层富勒烯分子的富勒烯涂层，其开始解吸温度表示富勒烯-富勒烯的分子间键合的强度。富勒烯-富勒烯键合的解吸温度通常为500～570K。而表示富勒烯和金属或半导体表面附着的结合/键合强度的对应于富勒烯-金属/半导体吸引力的解吸温度为625～725K或者更高。
富勒烯可以使用各种方法进行合成，有一些富勒烯已经获得很好的表征。富勒烯可以从各种来源购得，包括SES Research of Houston，TX。富勒烯加以纯化，例如用富勒烯有机分散液进行柱色谱纯化，该色谱可填充二氧化硅或氧化铝。将纯化的富勒烯沉积在清洁的基底上。
可以将富勒烯，宜为纯化形式的富勒烯，沉积在基底表面上形成富勒烯涂层。一种用于沉积富勒烯的方法包括加热富勒烯升华形成富勒烯蒸气。使一表面和所述富勒烯蒸气接触。以下将叙述的使用带电粒子束如电子束或离子束进行的溅射方法能改进对沉积过程的控制。
图2显示一个由真空系统的外壳202形成的真空室200。带电粒子束即电子束或离子束的发生器204将电子束或离子束206投射在由富勒烯-60(C60)形成的富勒烯靶子208，如多层富勒烯-60靶子或者粉末状富勒烯-60的靶子上。具体地说，所述靶子可以是富勒烯簇的粉末或富勒烯的固相或凝聚相。富勒烯可以是结晶状或者是无定形的。富勒烯靶子可以形成在电子束发生器的阳极210上，使来自电子束发生器阴极的电子轰击富勒烯靶子的阳极，使富勒烯分子发射到真空室中。所述从阴极到阳极的带电粒子束可以拦截传输中的富勒烯。
带电粒子束应具有足够低的电压和通量，以避免富勒烯的分解或者相当多的高级富勒烯如C70、C76、C78、C84等的形成。但是，若需要的话，除C60外靶子上还可以包含其它富勒烯。可以使用各种电子束发生器装置来产生电子束。例如，电子束发生器可以是棒料喂送的电子束发生器，在此情况下富勒烯靶子以棒的形式用于发生器。电子束发生器可以例如使用以低于约1千伏，通常约250～25伏的恒定电压提供的30千瓦功率来操作，将电子发射到靶子上。电子束发生器通常以约1～0.01安培，在有些实施方式中以约0.2～0.05安培的发射电流来操作。可以使用一种分子/原子束和电子束或电弧相互作用，使原子或分子流离子化来产生离子束。用来形成离子束的原子/分子优选是惰性的。合适的离子包括例如氩离子。
由于污染物的存在会干扰表面和富勒烯分子之间的牢固附着，所以保持基底212清洁，不受污染是很重要的。例如，基底表面的氧化物会使富勒烯分子和金属或半导体基底之间的结合/键合强度降低。在某些条件下氢可以和碳反应。一种满足清洁沉积环境要求的方法，是在高真空条件下通过如化学或蒸气沉积方法形成基底，或者在高真空条件下用溅射或其它方法清洁基底。在任何情况下，富勒烯的沉积宜在基底表面上或在沉积室的气氛中基本没有污染物的条件下进行，因为污染物会影响牢固附着的富勒烯层的形成。
在优选实施方式中，沉积应在真空，宜在约10-2～10-10乇中进行。在多数情况下，压力应约为10-7乇(torr)或更低。压力的降低可以确保在室中基本不存在氧、氢和水分。具体地说，低压应确保氧、氢和水分的分压在极端真空的条件下，低于约10-9乇。本发明方法也可以在大气压下进行，但是必须注意避免污染物的存在。例如，可以在惰性气体中使氧、水分和氢的分压均低于约10-9乇的条件下进行此方法。
撞击富勒烯靶子208的电子或离子使富勒烯分子从靶子中发射出来。至少有一些富勒烯分子学沿箭头212的方向朝清洁基底214发射，将分子216沉积在基底的表面218上。结果，在基底214的表面218上沉积了富勒烯涂层。
这时并不需要使用任何带电金属板或其它聚焦装置，使富勒烯分子朝基底212聚焦，但是若需要的话也可以进行聚焦。然而，基底212和靶子208之间的距离应尽实际可能的小，以避免富勒烯发射到外壳202周边和室200内其它地方的损失。由于基底较大话，通常其位置距离靶子要稍远些，以获得合理的表面覆盖率，合适的距离可以根据需涂覆表面的大小来确定。因此，在涂覆室中，与靶子的距离，存储磁盘通常应比磁盘驱动器磁头放得远些。
在其上沉积富勒烯的基底材料的选择也取决于涂覆物件的具体用途和性能参数。对于磁头，合适的基底材料包括例如Ni、Co、NiFe、CoFe、CoZrNb、NiFeCr、AlSiFE、NiFeRe以及它们的混合物或者合金。对于磁盘，合适的基底材料包括金属如钴和钴合金，如Co-Ni、Co-Cr、Co-Ni-Fe、Co-Ni-Cr、Co-Pt、Co-Ni-Pt、Co-Cr-Ta、Co-Cr-Pt、Co-Cr-Ni-B、Co-P、Co-Ni-P和其它类似材料，以及它们的混合物和合金。其它金属和合金，包括例如PtMn、Cu、Ru、Rh、Ta、CoPt、CoCuPt、Au等。对于磁光盘，可以包括一种或多种稀土元素和一种或多种过渡金属如TbFeCo、GdFeCo、TbFeCoZr、DyFeCo和GdDyFeCo。
不管在基底表面沉积富勒烯所用的方法如何，沉积的富勒烯可能超过单层。富勒烯多层增加了保护层不需要的附加厚度。而且，由于富勒烯-富勒烯分子间的吸引力明显小于富勒烯与洁净金属或半导体表面之间强的吸引力，所以所述增加的富勒烯层不稳定。
虽然可以控制沉积时间和条件来直接沉积出单层，但是很难控制适于生产单层的沉积条件。若沉积的超过单层，就需要除去附加的富勒烯多层，而留下在洁净金属或半导体表面上牢固附着的单层。为了除去附加的富勒烯，可以将经涂覆基底加热到可以解吸富勒烯多层但同时又不影响单层的温度，这一点在以下将进一步说明。由于相对于富勒烯-富勒烯分子间的键合来说，富勒烯和洁净金属或半导体表面之间的结合/键合更强，使得这种选择性解吸是可能的。
在另一实施方式中，大约单层的富勒烯涂层，可以在用加热器214加热基底到高于富勒烯-富勒烯键合的解吸温度，但又低于富勒烯-基底键合的解吸温度的某个温度(例如约为200～400℃，通常约为225～350℃)的条件下在基底212上沉积富勒烯分子来形成，同时阻止多层富勒烯的形成。因此，所述富勒烯单层的形成可以一步进行到位。在有些实施方式中，可以在整个沉积过程中加热基底。但是，基底也可以仅在沉积过程中的一段时间进行加热，例如使得富勒烯开始凝聚在冷的基底上，再加热基底来完成单层的形成。类似地，也可以在开始进行富勒烯沉积过程之前加热基底。
使用上述溅射方法通过上述Dykes等人申请中的升华方法、旋涂法或者任何其它合适的方法，可以将富勒烯沉积在所述基底上。如本文用于富勒烯涂层的术语“单层”是指具有大约一层富勒烯分子的涂层，但若所述涂层稍微多或者少于单层，其性能不会受到多大影响。而且，虽然富勒烯分子单层通常在基底上积聚成两维结晶结构，但是在单层中具有较小晶格缺陷的富勒烯涂层不会改变富勒烯层所需的性质，可以认为是近似的单层。不管如何，富勒烯单层保护基底免于磨损和水蒸汽的腐蚀，能为满意的润滑性能提供超薄层适用于磁性数据存储部件如读/写磁头、滑触头和磁盘。
在基底上富勒烯分子单层的形成产生了具有厚度小于约1.0纳米的涂层。在要求小的浮动高度如在磁盘驱动器的情况下，这个特征尤其有利。可以在沉积过程中如本文所述加热基底，或者在沉积过程以后除去富勒烯多层，来形成富勒烯单层。例如，可以如上述Dykes等人的申请所述，在形成富勒烯多层之后，加热所述基底，或者往富勒烯多层施涂溶剂，或者用高能射线照射来去除富勒烯多层，上述后两个方法在由Dykes等人与本文同日提交，名为“制备超薄保护层的方法”的申请No.S01.12-0805/STL 9643中有记述。
数据存储磁盘的表面还可以在富勒烯保护层上进一步有一层润滑层。合适的润滑层包括聚合物，例如氟化高聚物，如全氟聚醚及其衍生物。合适的全氟聚醚聚合物，包括例如FomblinZ-60(平均分子量(AMW)＝约60，000原子质量单位(AMU)或道尔顿)，FomblinZ-25(AMW＝约25，000 AMU)和FomblinZ-15(AMW＝约15，000 AMU)。由Montedison(Ausimont)S.P.A.，Milan，Italy制造的Fomblin全氟聚醚的分子式为CF3O(CF2CF2O)n(CF2O)mCF3，式中n和m可以改变来产生具有特定数值平均分子量的特定产品。
在一些特别优选的实施方式中，磁盘驱动器的磁头表面和磁盘表面均具有富勒烯单层。由于富勒烯分子之间的弱相互作用力，有富勒烯涂层的磁头不会强烈地附着在有富勒烯涂覆的磁盘上。对于这些实施方式，磁盘基底表面上是不需要另加润滑层来达到所需磨擦性能的。
在一个实施方式中，换言之，富勒烯-60的靶子(208)与基底(212)置于真空室(200)中。将具有足够能量可以使富勒烯分子从靶子发射出来但同时又不会形成显著比C60更高分子结构的富勒烯的带电粒子束(206)投射到靶子上。产生的富勒烯(214)C60就沉积在基底上。在其它实施方式中，可以使用其它富勒烯。
在一些优选实施方式中，是在操作压力约10-2～10-10乇，宜约10-7～10-9乇的真空室中进行此过程。电子束由发射电压低于1千伏的电子束发生器产生。合适的离子束包括例如氩离子束。
在另一实施方式中，在用一个加热器(214)加热基底至高于富勒烯-富勒烯解吸温度的情况下，将富勒烯在基底上沉积形成大约富勒烯单层组成的涂层。
虽然是就磁性物件，如磁盘或磁光盘驱动器的磁头/滑触头和磁盘所用的保护层说明了本发明，但是本技术领域的技术人员应能意识到，本发明可以用于其它器件上，所述器件包括但不限于用在驱动器的主轴电动机和音圈电动机的轴承上以及使用涂层和润滑技术尤其是需要超薄涂层的其它系统上。
在此应该理解，即使在上述说明中阐述了本发明各种实施方式的许多特征和优点，以及本发明各种实施方式的具体结构和功能，但是这些内容仅仅是说明性的，在具体细节，尤其在涂层的结构和排列、去除多分子层的方式上可以作出改动，而仍保留在本发明权利要求书所表述的广义意思表示的完整范围的原则。例如，在不背离本发明范围和精神的条件下，根据保护层具体的用途可以改变一些具体的细节，而仍基本保持相同的功能。因此，虽然本发明是结合富勒烯涂层进行说明的，但是将多分子层减少成为单分子层的方法可以通过各种不会不利地升高被涂覆物件温度的方法，如机械或化学的方法来完成。虽然本文所述的发明直接涉及获得单层涂层的特定技术，但是应意识到，本领域技术人员在不背离本发明范围和精神的条件下，可以使用本发明所述的技术形成受控的多分子层涂层。

Claims (24)

1.在基底上沉积富勒烯涂层的方法，该方法包括：
a)在一个室中以足以从包含富勒烯的靶子上发射出富勒烯分子，而不会与富勒烯反应的能量，将带电粒子束投射到所述靶子上，将产生的富勒烯沉积在置于该室中的基底表面上。
2.权利要求1所述的方法，其特征在于所述室是在约10-2～10-10乇的压力操作的。
3.权利要求1所述的方法，其特征在于所述带电粒子束为电子束。
4.权利要求1所述的方法，其特征在于所述带电粒子束为离子束。
5.权利要求1所述的方法，其特征在于所述基底是由选自金属和半导体以及它们的混合物的材料形成。
6.权利要求1所述的方法，其特征在于所述基底是由选自Co-Ni、Co-Cr、Co-Ni-Cr、Co-Pt、Co-Ni-Pt、Co-Cr-Ta、Co-Cr-Pt、Co-Cr-Ni-B、Co-P、Co-Ni-P、PtMn、Cu、Ru、Rh、Ta、CoPt、CoCuPt、Au、稀土金属、过渡金属以及它们的混合物和合金的材料形成的。
7.权利要求1所述的方法，其特征在于所述富勒烯分子以相当于富勒烯单层解吸温度至少约为700K的富勒烯-基底键合强度附着在基底上。
8.权利要求1所述的方法，其特征在于所述方法还包括如下步骤：
b)将所述基底加热至高于富勒烯-富勒烯解吸温度某一温度的同时，将富勒烯沉积在基底上。
9.权利要求8所述的方法，其特征在于基底上的富勒烯涂层大约为单层。
10.权利要求1所述的方法，其特征在于所述富勒烯为C60。
11.权利要求1所述的方法，其特征在于所述基底表面包括金属或半导体，该方法还包括如下步骤：
b)在所述室中形成清洁的金属或半导体表面。
12.权利要求1所述的方法，其特征在于所述带电粒子束是以不高于约1千伏的电压投射的电子束。
13.权利要求1所述的方法，其特征在于所述靶子包含富勒烯簇的粉末。
14.权利要求1所述的方法，其特征在于所述靶子包含凝聚的富勒烯层。
15.在金属或半导体基底上形成大约单层富勒烯涂层的方法，该方法包括：
a)在基底上沉积富勒烯一段沉积时间；
b)在所述沉积时间的至少一部分时间内加热所述基底，使其温度高于富勒烯-富勒烯解吸温度，但又低于富勒烯-基底解吸温度。
16.权利要求15所述的方法，其特征在于所述步骤(b)是在约225～350℃的温度进行的。
17.权利要求15所述的方法，其特征在于所述基底是由选自金属和半导体以及它们的混合物的材料形成。
18.权利要求15所述的方法，其特征在于所述基底是由选自Co-Ni、Co-Cr、Co-Ni-Cr、Co-Pt、Co-Ni-Pt、Co-Cr-Ta、Co-Cr-Pt、Co-Cr-Ni-B、Co-P、Co-Ni-P、PtMn、Cu、Ru、Rh、Ta、CoPt、CoCuPt、Au、稀土金属、过渡金属以及它们的混合物和合金的材料形成的。
19.权利要求15所述的方法，其特征在于所述富勒烯分子以相当于富勒烯单层解吸温度至少约为700K的富勒烯-基底键合强度附着在基底上。
20.权利要求15所述的方法，其特征在于所述富勒烯为C60。
21.权利要求15所述的方法，其特征在于富勒烯的沉积是通过升华来进行的。
22.权利要求15所述的方法，其特征在于富勒烯的沉积是通过对富勒烯靶子溅射来进行的。
23.权利要求15所述的方法，其特征在于所述基底在整个沉积时间均在加热。
24.权利要求15所述的方法，其特征是在沉积时间的一部分时间中加热所述基底，在加热基底的同时形成富勒烯单层。
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