CN105784437A - 从显微样品修改样品表面层的方法 - Google Patents
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Abstract
本发明涉及从显微样品修改样品表面层的方法,方法在真空中执行,方法包括以下步骤:提供附着到操纵器(116)的显微样品(120);提供第一(受控)温度处的第一液体(122A);在第一液体中浸泡样品,从而导致样品表面修改;从第一液体移除样品;提供第二(受控)温度处的第二液体(122B);在第二液体中浸泡样品;以及从第二液体移除样品。这使得能够实现样品原位的湿法处理,从而增加速度和/或避免样品的后续改变/污染(诸如氧化)等。该方法对于在利用(镓)FIB加工薄片之后蚀刻薄片以移除其中发生镓植入或其中晶格被扰乱的表面层而言特别有用。
Description
技术领域
本发明涉及在粒子光学装置中从样品修改样品表面层的方法,该方法在真空中执行。
背景技术
这样的方法从SJRandolph等人的“Capsule-freefluiddeliveryandbeam-inducedelectrodepositioninascanningelectronmicroscope”,RSCAdv.,2013,p20016–23[-1-]是已知的。
Randolph描述了使用液体注射系统(纳米毛细管)来在环境扫描电子显微镜(ESEM)的低真空腔中沉积CuSO4溶液的液滴。液体的毛细流动通过使纳米毛细管与衬底接触来诱导。然后形成并且通过控制就衬底温度(利用Peltier加热/冷却台来冷却衬底)而言的液滴蒸发速率和通过控制注射到真空腔中的H2O蒸汽的压力来稳定化(也就是说:其体积保持大致恒定)显微液滴。聚焦离子束通过压力限制孔而进入液滴使得扫描电子显微镜的电子发射器可以操作在比低真空腔中的真空更好的真空下。通过使用毛细管作为阳极并且ESEM的电子束作为虚拟阴极来实现水相的Cu2+到固态、高纯度、经沉积的Cu的电化学还原,这使得能够实现导电和绝缘衬底二者上的电沉积。
要指出的是,术语“粒子光学装置”用于涵盖电子显微镜(透射电子显微镜、扫描电子显微镜、扫描透射电子显微镜等)、聚焦离子束机器(FIB)及其组合。
本发明意图提供修改样品表面层的改进的且更加通用的方法。
发明内容
为那个目的,本发明的方法包括以下步骤:
·提供附着到操纵器的显微样品,
·提供第一温度处的第一液体,
·在第一液体中浸泡样品,从而导致样品表面修改,
·从第一液体移除样品,
·提供第二温度处的第二液体,
·在第二液体中浸泡样品,以及
·从第二液体移除样品。
发明人认识到,在真空中使用液体不仅仅对使用虚拟阴极的电沉积是有用的,而且当样品浸泡在第一液体中并且然后浸泡在第二液体中时打开了样品表面的湿法处理应用的全新领域。这样的样品表面修改是粗糙度、亲水性、表面电荷、表面能、生物相容性或反应性的修改、官能团的添加、生物材料的添加、样品表面的镀层或样品表面层的移除。
通过在第一液体中浸泡样品,实现(湿法)处理时间的控制,这在Randolph的方法中并未实现。通过在第二液体中浸泡样品,样品可以例如被冲洗,或者可以添加另外的湿法过程步骤。
优选地第一温度和第二温度是受控温度。由于真空中的液体温度强烈地影响其蒸发速率,并且因此强烈地影响液体驻留在其中的真空的劣化。
要指出的是,尽管Randolph公开了在电镀和真空中使用液滴,但是Randolph没有提到在液体中浸泡样品。Randolph也没有提到除镀层之外的其它用途,因为Randolph在样品(表面)上形成液滴并且旨在局部形成其中电子束瞄准的那些定位上的沉积。与此相对,本申请人的发明的目的在于整个样品表面或至少浸没在液体中的整个样品表面的表面修改。
要指出的是,第一和第二液体可以形成在一个表面(“衬底”)上,但是还可以形成在两个不同表面(“衬底”)上。在后一种情况下,表面可以在例如温度(用于控制不同液体的蒸发速率)或组成(示出例如针对不同液体的不同润湿性质)方面不同。
优选地,通过使用射束诱导沉积形成焊接来将样品附着到操纵器,该射束诱导沉积由激光束、电子束或离子束诱导。
在实施例中,样品在任何方向上具有小于10μm的尺寸并且第一液体和第二液体以小于1皮升、更具体地小于1飞升的体积作为液滴沉积。
要指出的是,当液体暴露于真空,发生液体的蒸发。该蒸发使装置的真空劣化并且减少液体的量。通过调整(控制)液滴的温度和通过周围真空的部分压力以及来自液体的施加器(毛细管等)的流动来发生蒸发的控制。需要所有这些因素来稳定化液滴和液滴体积。
要指出的是,尽管在例如通常存在于SEM或FIB中的台的表面上使用液滴是提供液体的一种形式,但是也可以使用其它提供形式。这样的其它形式可以包括:
·在例如台的凹陷中提供小体积的(温度受控的)液体,在使用之后降低液体的温度,并且因此降低蒸发速率,
·提供当未被使用时从真空密封的小体积的液体,
·经由台中的小通道提供液体,
·液滴在表面上的电喷射,
·使用喷墨技术(包括在通道中形成小蒸汽泡或者使用通过使用压电晶体的通道变形将液滴挤出)施加液滴,
·等。
该方法特别适合于修改半导体样品的表面从而将表面蚀刻到所要求的厚度和/或利用薄保护层(诸如铂层)对样品进行镀层。
该方法还非常适合于使用聚焦离子束从工件(例如晶片或生物样品)切除样品,如从例如转让给Hitachi的美国专利No.US5,270,552[-2-]得知的那样。
表面修改的优选实施例是蚀刻、电化学蚀刻、无电式镀层或使用非虚拟阴极的电镀。在这些实施例中,第一液体是蚀刻剂或者镀液。蚀刻移除通过控制蚀刻剂化学品的参数、浸没时间(浸泡时间)、液体浓度和液体温度(以及在电化学蚀刻的情况下的电流)可控制。
同样地,镀层厚度通过控制镀层化学品的参数、浸没时间(浸泡时间)、液体浓度和液体温度(以及在电镀的情况下的电流)可控制。
由此可以实现蚀刻移除或镀层厚度的精细控制,使得该方法非常适合于移除或添加具有小于10nm厚度的表面层,而且用于移除或添加厚得多的层。
在电镀和电蚀刻的情况下,样品关于液体偏置,液体从例如其停留在其上的表面得到其电势。
在优选实施例中,第二液体是冲洗液。冲洗液结束例如蚀刻或镀层的在先步骤,并且还从表面清洗掉存在于第一液体中的任何物质。冲洗可以通过在冲洗液中若干次地浸泡样品或者在不同体积(不同液滴或这样的类似物)的冲洗液中重复浸泡而重复若干次。
在另一实施例中,第一液体包含生物材料,从而将生物材料施加到样品。第二液体可以导致生物材料到表面的键合,或者可以是对生物材料进行固定或染色的固定剂或染色剂。这样的固定剂/染色剂的示例是例如甲醛、戊二醛、四氧化锇、四氧化钌(rutheniumtetroxide)。
在又一实施例中,表面修改包括通过形成通过酶、纳米线或其它纳米结构的沉积导致的活性部位来官能化样品,并且第二液体包括提供材料到所述活性部位。
这些技术对在大气条件下非原位准备生物样品的技术人员而言是已知的。通过现在在真空中原位应用这些技术,在那里的适用性以及其使用的容易性被增强。
在再一实施例中,在一个表面上提供两种液体,操纵器关于所述表面可移动。
该表面可以是样品台的表面。
在优选实施例中,在样品表面层的修改期间和/或之后使用带电粒子束检查样品表面。
在又一实施例中,使用第一液体注射系统和第二液体注射系统来施加液体。
在另外的实施例中,第一液体注射系统和第二液体注射系统集成在一个结构液体注射系统中。
该实施例对于避免两个液体注射系统的定位特别有用,因为这仅涉及一个系统的定位,并且因此节省处理时间。
要指出的是,为了控制蒸发速率,液体的温度必须优选地良好受控。作为示例:在4℃处水的蒸汽压力是8.14hPa并且在20℃处为23.4hPa。两个带电粒子装置的真空系统应当能够处置所述量的蒸发的液体,并且液体的量应当足够大使得液体在整个处理时间期间存在。尽管低温(刚好高于熔点)有利于系统中的压力和液体的蒸发,但是高温造成更高的反应速率。取决于所使用的化学过程和所获得的效果(样品表面粗糙度、亲水性、表面电荷、表面能、生物相容性或反应性的修改、官能团的添加、生物材料的添加、样品表面的镀层或样品表面层的移除),选择最佳温度。
使用聚焦离子束减薄的硅薄片遭受表面上的镓植入以及晶格损坏,参见例如J.Mayer等人的“TEMSamplePreparationandFIB-InducedDamage”,MRSBULLETIN,Vol.32(2007年5月),p.400-407[-3-]。解决方案是从薄片蚀刻小于例如10nm的薄层。应当小心的是,如果样品与操纵器之间的焊接用于连接二者,该处理不造成焊接的完全移除,造成样品与操纵器之间的断开,并且因而造成样品的可能损失。这可以通过使用焊接材料和液体的良好组合或者通过在液体中仅部分地浸泡样品而保持焊接远离液体(要记住的是,液体润湿样品表面,如果适用的话)来实现。而且,由于焊接的厚度典型地为大致1μm,因此如果从样品移除小得多的厚度(例如小于10nm或小于50nm),移除焊接是不太可能的。值得一提的是,典型地为了移除利用聚焦离子束加工的半导体样品的表面层,移除小于10nm的层。
用于修改的化学品强烈地取决于样品材料和修改的类型。作为示例一些蚀刻剂:
表1:用于不同样品材料的蚀刻剂
样品材料 | 蚀刻剂 | 优选温度范围[℃] |
硅 | H2O中的~20% KOH | + 20至100 |
钢 | 4 – 15 % HClO4,乙醇中的2%丁氧基乙醇 | -45至-40 |
钨 | 水中的0.5 - 10 % NaOH | -20至-10 |
铝 | 乙醇中的~10 % HClO4 | 0至20 |
铜 | 乙醇中的H3PO4 | 0至20 |
由于用于这些蚀刻剂的第一液体是不同的(在该示例中为基于乙醇的或基于水的),因此应当相应地选择使用匹配的第二液体(在该示例中用于冲洗)。温度应当选择成匹配修改的要求(例如反应速率)和可允许的蒸发速率。蒸发速率可能受来自液体注射器/供给的最大流动限制(因为在高蒸发速率处还可能发生溶解的化学品的浓度中的改变),或者受带电粒子装置的泵送速度限制。
取决于用途,第一液体和第二液体可以具有相同(受控)温度或不同(受控)温度。
同样地,镀层(化学镀层或电镀)化学品和溶剂对本领域技术人员而言是已知的。
使用具有溶解的生物材料的水或酒精的第一液体,第二材料可以包括将它们自身附着到生物材料的特定部位的例如荧光蛋白、荧光标记物、电子致密标记物(例如具有5与25nm之间直径的银或金粒子)。
要指出的是,如本文所使用的荧光标记物的定义包括有机染料和无机荧光标记物(量子点)。
包括酶、纳米线或其它纳米结构的第一液体可以用于官能化第二液体中的生物材料可以键合到的样品(例如形成样品上的活性部位)。
附图说明
现在使用附图来阐述本发明,其中相同的附图标记指示对应的图。为那个目的:
图1示意性地示出根据本发明的SEM,
图2示意性地示出根据本发明的SEM的细节,
图3示意性地示出根据本发明的SEM的可替换布置的细节。
具体实施方式
图1示意性地示出根据本发明的SEM。
SEM柱100安装在可抽空样品腔130上。SEM柱包括产生具有0.2至20keV之间的可选能量(注:已知使用更高和更低的能量)的能量电子束104的电子发射器102。该电子束由透镜106A、106B、106C操纵并且通过偏转器108A、108B偏转。透镜和偏转器在本质上可以是静电或磁性的,并且透镜和偏转器的数目可以变化。射束穿过隔膜(未示出)中的孔,从而限制射束的直径以及限制气体到SEM柱的真空中的流入。
离开SEM柱的电子束指向SEM的样品台112。台典型地能够在三个方向上平移并且绕两个或三个轴倾斜。在检查样品之前,将附着到操纵器116的远端118的样品120浸泡在第一液体122的液滴中。第一液体的液滴从液体注射器110A获得。同样地,第二液体的液滴可以从液体注射器110B获得。
在将样品浸泡在第一和第二液体中之后,将样品运送至其中电子束与台交叉的定位。当射束撞击样品时,发射例如由Everhart-Thornley检测器114检测的次级电子,从而使得能够实现样品的检查。
为了控制液体的蒸发速率,将Peltier加热器/冷却器124附连到台。冷却液体,最终冻结它,降低液体的蒸汽压力,并且因此降低其蒸发速率(在真空中)。
控制器126控制柱(包括偏转器),充当用于来自检测器114的信号的信号/图像处理器,并且控制操纵器、液体注射器和真空泵(后者未示出)。
要指出的是,液体注射系统对本领域技术人员而言是已知的并且从例如德国罗伊特林根的KleindiekNanotechnikGmbH商业上可得到,参见http://www.nanotechnik.com/mis-em.html[-4-]。其它注射器可以基于经修改的气体注射系统(GISses)或者基于使用从喷墨打印机得到的技术的注射器(例如使用压电逐出器,如转让给RicohCompanyLtd.的美国专利No.US8,919,902[-5-]中所讨论的,或者热学气泡逐出器,如转让给HewlettPackardDevelopmentCompanyL.P.的美国专利No.US8,919,938[-6-]中所讨论的)或者基于来自针的电喷射。
还要指出的是,尽管以上示例仅提到电子束,但是同样地,产生包括离子的带电粒子束的装置是已知的。离子可以例如通过气体放电源、液体金属离子源形成。离子可以是带正电或带负电的离子,并且可以是多电荷或单电荷离子。还可以生成带电集群。
图2示意性地示出根据本发明的SEM的细节。
图2示意性地示出其中形成液体液滴的区域的放大视图。看到将样品118浸泡在液体液滴122A中。这可以通过关于彼此移动样品操纵器116和台112来实现,即通过移动操纵器或台来实现。第一液滴122A的温度通过加热器124来调整,并且不需要等同于第二液滴122B的温度。液滴的体积可以通过分别经由液体注射系统110A和110B对液体的供给、液滴的温度和围绕液滴的真空中的残留气体的组成来调整。
如本领域技术人员清楚的,样品表面的修改速度是液体组成(材料浓度等)、样品浸泡在液体中的温度和时间周期的函数。而且液滴内的样品的移动(从而在样品浸没在液滴中的同时影响靠近样品表面的化学品的浓度)影响过程速度。这可以通过使用例如液滴的(超)声激发(例如通过将液滴放置在谐振压电致动器上,或者作为可替换方案,形成作为振动极端的样品附着到的操纵器的极端,或者将整个操纵器放置在(超)声激发器上)来有利地使用。而且台可以配备成移动液体。
图3示意性地示出另一实施例的细节。
图3示出其中不使用液滴而是使用小容器300A、300B的实施例。为了避免连续蒸发,这些容器可以由通过致动器(未示出)可移动的盖子302A、302B闭合。这些盖子的致动器可以采用压电致动器或其它构件。同样,快速温度控制可以用于避免在液体未被“使用”时的蒸发。
容器的大小(直径)应当足够大使得样品可以浸泡在容器中。
要指出的是,在液体表面从样品台112的表面充分移除的情况下,当蒸汽凝结在通道壁上时,液体的较高温度可以与通道的低温组合,导致降低的蒸发速率。
本领域技术人员将认识到,可以使用多于两种液体,并且在将样品浸泡在液体中之前、期间或之后,样品可以被检查、暴露于气体、暴露于例如BID(射束诱导沉积,使用离子束、电子束或激光束)、暴露于等离子体等。该方法使得能够实现样品原位的湿法处理,从而增加速度(因为样品不需要从真空腔取出)和/或避免样品的后续改变/污染(诸如氧化)等。
该方法对于在利用(镓)FIB加工薄片之后蚀刻薄片以移除其中发生镓植入或其中晶格被扰乱的表面层而言特别有用。
引用文献
[-1-]SJRandolph等人,“Capsule-freefluiddeliveryandbeam-inducedelectrodepositioninascanningelectronmicroscope”,RSCAdv.,2013,p20016–23。
[-2-]转让给Hitachi的美国专利No.5,270,552。
[-3-]J.Mayer等人,“TEMSamplePreparationandFIB-InducedDamage”,MRSBULLETIN,Vol.32(2007年5月),p.400-407。
[-4-]http://www.nanotechnik.com/mis-em.html。
[-5-]转让给RicohCompanyLtd的美国专利No.8,919,902。
[-6-]转让给HewlettPackardDevelopmentCompanyL.P的美国专利No.8,919,938。
Claims (17)
1.在粒子光学装置(100)中从样品(120)修改样品表面层的方法,方法在真空中执行,方法包括以下步骤:
·提供附着到操纵器(116)的显微样品(120),
·提供第一温度处的第一液体(122A),
·在第一液体中浸泡样品,从而导致样品表面修改,
·从第一液体移除样品,
·提供第二温度处的第二液体(122B),
·在第二液体中浸泡样品,以及
·从第二液体移除样品。
2.如权利要求1所述的方法,其中样品表面修改是样品表面粗糙度、亲水性、表面电荷、表面能、生物相容性或反应性的修改、官能团的添加、生物材料的添加、样品表面的镀层或样品表面层的移除。
3.如前述权利要求中任一项所述的方法,其中通过使用射束诱导沉积形成焊接来将样品(120)附着到操纵器(116),射束诱导沉积由激光束、电子束或离子束诱导。
4.如前述权利要求中任一项所述的方法,其中样品(120)在任何方向上具有小于10μm的尺寸并且第一液体(122A)和第二液体(122B)以小于1皮升、更具体地小于1飞升的体积作为液滴沉积。
5.如前述权利要求中任一项所述的方法,其中样品(120)是半导体样品。
6.如前述权利要求中任一项所述的方法,其中提供附着到操纵器(116)的样品(120)的步骤包括以下步骤:
·提供工件,
·将样品(120)附着到操纵器(116),以及
·使用聚焦离子束从工件切除样品。
7.如前述权利要求中任一项所述的方法,其中样品表面修改通过蚀刻、电化学蚀刻、无电式镀层或电镀导致,所述电镀使用非虚拟阴极。
8.如权利要求7所述的方法,其中所移除或添加的样品表面层的厚度小于10nm。
9.如前述权利要求中任一项所述的方法,其中第二液体(122B)是冲洗液,并且在第二流体中浸泡样品冲洗样品(120)。
10.如权利要求9所述的方法,其中样品(120)被重复冲洗。
11.如权利要求10所述的方法,其中每一个冲洗步骤在新鲜的冲洗液中执行。
12.如权利要求1-6中任一项所述的方法,其中第一液体(122A)包含生物材料,样品表面修改包括向样品表面提供生物材料并且第二液体导致生物材料到样品表面的键合。
13.如权利要求1-6中任一项所述的方法,表面修改包括通过形成通过酶、纳米线或其它纳米结构的沉积导致的活性部位来官能化样品(120),并且第二液体(122B)包括提供材料到所述活性部位。
14.如前述权利要求中任一项所述的方法,其中在一个表面上提供两种液体(122A,122B),操纵器(118)关于所述表面可移动。
15.如前述权利要求中任一项所述的方法,其中在样品表面层的修改期间和/或之后使用带电粒子束(104)检查样品表面。
16.如前述权利要求中任一项所述的方法,其中使用第一液体注射系统(110A)和第二液体注射系统(110B)来施加液体。
17.如权利要求16所述的方法,其中第一液体注射系统(110A)和第二液体注射系统(110B)集成在一个结构液体注射系统中。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP15150779.5A EP3043372B1 (en) | 2015-01-12 | 2015-01-12 | Method of modifying a sample surface layer from a microscopic sample |
EP15150779.5 | 2015-01-12 |
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US10105734B2 (en) | 2018-10-23 |
EP3043372A1 (en) | 2016-07-13 |
US20160199878A1 (en) | 2016-07-14 |
CN105784437B (zh) | 2018-08-28 |
JP2016130733A (ja) | 2016-07-21 |
EP3043372B1 (en) | 2017-01-04 |
JP6110519B2 (ja) | 2017-04-05 |
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