这项研究得到了捷克共和国赠款机构 (项目号 15-34632L) 和 CEITEC 纳米 + 项目的财政支持, 02.1. 01/0.0/0.0/16 013/0001728。在 CEITEC 纳米研究基础设施 (ID LM2015041, MEYS CR, 2016-2019) 中进行了样品制作和 LTEM 测量。Meena Dhankhar 获得了布尔诺博士学位奖学金的支持。

我们演示了一种制备 TEM 和 MTXM 样品的方法。坡莫合金 nanodiscs 直径范围从 250-4000 毫微米和厚度在 20-100 毫微米之间在30毫微米厚的罪孽膜被制造为 TEM 和200毫微米厚的罪孽膜为 MTXM。图 1显示了罪恶膜的照片。
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/57817/57817fig1.jpg"> 图 1: 用作 MTXM (左) 和 TEM (右) 样品的基片的罪恶膜的照片.图像显示标尺的大小比较。MTXM 框架是一个 5 x 5 毫米矩形与窗口厚度200毫微米和 TEM 框架适合一个3毫米圆直径与窗口厚度30毫微米。<a href="/files/ftp_upload/57817/57817fig1large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
1. 透射电镜样品的制作
注: 在本节中, 我们描述了用于观测磁涡流17的成核过程的 TEM 样品的制作。膜被选择为基材, 因为它们为磁性结构的 lithographical 制造提供了坚实的支持。一个重要的参数是膜的窗口厚度。较高的加速电压允许穿透较厚的样品, 但任何不必要的厚度将导致信号损失19。因此, 我们使用我们的供应商提供的最薄的薄膜 (30 nm)。
<ol><li>
衬底制备和自旋涂层 注: 自旋涂层是一种广泛使用的工艺, 以获得理想的抗膜在基板上。少量的抵抗被丢弃在基板上, 然后以非常高的速度旋转以获得所需的涂层厚度。TEM 膜的自旋涂层是相当奇特的, 因为以下原因: (i) 如果膜是纺在旋转涂布机的轴, 抵抗不会是统一的, 由于膜的小直径和 (ii) 真空支架不能使用, 因为他们可以打破膜。为此, 我们设计了3D 打印适配器 (见图 2), 它保持膜离轴, 不需要真空来保存样品。<ol>
<li>焙在180摄氏度的热板上的罪孽膜, 以去除任何湿气。</li>
		<li>在旋转涂布机上插入适配器, 然后将膜置于适配器中。</li>
		<li>自旋涂层 950 K PMMA (聚甲基丙烯酸甲酯) 抵抗在3000转每分钟1分钟, 以产生大约 200 nm 的薄膜厚度。</li>
		<li>后烘烤的热板上的样品在180°c 3 分钟硬化 PMMA 层。</li>
	</ol>
</li>
</ol><img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/57817/57817fig2.jpg"> 图 2: 3D 打印适配器的照片, 用于在自旋涂层中保持 TEM 膜离轴.多膜可同时涂覆。<a href="/files/ftp_upload/57817/57817fig2large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<ol start="2"><li>
电子束光刻 (EBL)
	<ol>
<li>绘制图形数据库系统 (GDS) 格式的光盘所需的图案, 并将其上载到电子束 (电子束) 光刻系统。</li>
		<li>将样品加载到电子束写入器系统中, 设置舞台和光束。</li>
		<li>将光盘区域暴露在20凯文的光束能量为260µC/厘米2的电子剂量。 注: 博览会过程的合适参数为 250 pA 的光束电流, 步长为 10 nm。与大块基底相比, 这种剂量约为 30%, 因为膜上的背向散射高度降低。</li>
	</ol>
</li>
	<li>
化学发展
	<ol>
<li>暴露后, 在甲基异丁基酮 (MIBK) 的开发者中开发样品2分钟. 用异丙醇 (IPA) 在三十年代停止发展。</li>
		<li>三十年代把每个样品洗去去离子水, 用氮气吹干, 同时拿着镊子。</li>
		<li>使用光学显微镜在低放大倍数 (使用5X 目标), 然后在高放大倍数 (使用100X 目标) 检查样品的发展;图 3显示了一个被开发的样本的光学显微镜图像。</li>
	</ol>
</li>
	<li>
电子束蒸发 注: 电子束蒸发20是一种物理气相沉积形式, 在高真空下由带电钨灯丝产生的高能电子束轰击目标阳极。电子束使原子从目标转变成气态相。这些原子沉淀成固体形式, 将真空室中的所有东西都涂上薄薄的靶材层。最好是使用电子束蒸发系统的升降目的, 因为它给了一个很好的边缘的光盘, 而不存入任何额外的材料光盘的边界。<ol>
<li>将膜小心地用聚 oxydiphenylene pyromellitimide (如Kapton) 贴在支架上, 并通过负载锁将其转移到电子束蒸发器的沉积室中。</li>
		<li>使用电子束蒸发系统将薄层的坡莫合金 (镍80Fe20) 沉积, 其厚度范围从20到 100 nm, 沉积速率约为 1 Aͦ/秒. 使用 8 kV 的加速度电压和光束电流大约 120 mA。</li>
	</ol>
</li>
	<li>
升降
	<ol>
<li>用丙酮 (至少99.5% 纯度) 将1小时的膜放入烧杯中。</li>
		<li>现在用丙酮喷雾膜, 同时用镊子, 直到多余的金属被除去。</li>
		<li>如果多余的金属残留在样品上, 请将膜放回烧杯中, 然后重复该过程。 注: 可选择使用兆声浴来辅助升降过程。请注意, 它是不可能使用经典的超声波浴, 因为它打破了膜。</li>
		<li>用扫描电子显微镜 (SEM) 在5伏的加速电压和 100 pA 的束流中进行最终检查, 将最终的磁片阵列图像。图 3b显示了100,000X 放大倍数的图像。</li>
	</ol>
</li>
	<li>
LTEM 成像
	<ol>
<li>将样品装入 TEM 样品架中, 并将其插入显微镜中。</li>
		<li>使用显微镜的标准程序, 校正样品高度并将洛仑兹模式的显微镜对准所需的加速电压 (在我们的案例中为 300 kV)。</li>
		<li>引入磁信号, 将洛仑兹透镜离焦。</li>
		<li>继续做实验。倾斜样品, 以引入平面场组件 (例如, 合适的角度是 30°, 检查持有人的规格最大倾角)。</li>
		<li>应用磁场刺激物镜 (通常在洛仑兹模式下关闭)。 注: 现场校准曲线应由 TEM 制造商提供。</li>
		<li>对样品进行饱和, 通过 deexciting 物镜, 在相机上捕捉图像, 逐渐减小磁场。示例结果如图 3c所示。</li>
	</ol>
</li>
</ol><img alt="Figure 3" class="xfigimg" src="/files/ftp_upload/57817/57817fig3.jpg"> 图 3: 由光学和电子镜成像的最终样本.(a) 该面板显示了氮化硅膜窗口, 其阵列中的圆盘在电子束曝光后抵抗发展。(b) 本小组展示了扫描电镜所成像的磁片的最终阵列. (c) 此面板显示磁性 nanodiscs 阵列中磁性涡核态的 LTEM 图像。<a href="/files/ftp_upload/57817/57817fig3large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
2. MTXM 样品的制作
注: 在 MTXM 测量中, 我们可以利用该技术的时间分辨率。为了引入高频励磁涡旋, 在第一步制造一个金波导, 然后在第二光刻步骤中将磁片放在波导的顶部。整个结构是捏造的 200 nm 厚的罪恶膜, 这是透明足够的软 x 射线21。详细步骤将在下面的文本中描述, 流程的示意图如图 4所示。MTXM 样品的制作过程贯穿上述的所有步骤, 为 TEM 样品制作, 但需要额外的光刻步骤, 以制造波导。
<img alt="Figure 4" class="xfigimg" src="/files/ftp_upload/57817/57817fig4.jpg"> 图 4: 在 MTXM 时间分辨实验中, 在氮化硅膜上使用圆盘和波导的样品的制备步骤的示意图.它涉及两步光刻, 以获得最终的结构。<a href="/files/ftp_upload/57817/57817fig4large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<ol><li>样品制备和自旋涂层 注: MTXM 膜为 5 x 5 毫米2帧, 具有 3 x 3 毫米2宽和 200 nm 厚的中央窗口。膜不能放在旋转涂布机真空卡盘, 因为它会打破膜。在这种情况下, 我们胶合膜到一个 10 x 10 毫米2硅片, 使其易于使用。<ol>
<li>焙180摄氏度的热板上的罪孽样品, 以去除样品中的水分。</li>
		<li>自旋涂层正面抵抗凯撒在3000转每分钟1分钟;产生的薄膜厚度约为500纳米。 注意: 这种类型的抵抗被选择为其更高的灵敏度, 导致更快的写作时间。在抵抗数据表上可以找到厚度-自旋速度依赖性。</li>
		<li>在热板上烘烤样品在150°c 1 分钟硬化抵抗层。</li>
	</ol></li>
	<li>波导电子束光刻
	<ol>
<li>以 GDS 格式创建所需的波导和对准标记 (用于第二光刻步骤) 的模式, 并将其上载到电子束光刻系统。</li>
		<li>将样品加载到电子束写入器系统中, 设置舞台和光束。</li>
		<li>将光盘区域暴露在20凯文的光束能量为65µC/厘米2的电子剂量, 一个 10 nA 的光束电流, 和一个台阶尺寸 200 nm。 注: 我们使用凯撒正面抵抗公开波导和对准标记。这种抗性比 PMMA 具有更高的灵敏度, 电子剂量的65微机/cm2在光束能量20凯文, 因此, 有利于加快博览会。</li>
	</ol></li>
	<li>化学发展
	<ol>
<li>曝光后, 开发的样品在开发商为1分钟, 并遵循这一塞子 (IPA) 三十年代。</li>
		<li>三十年代把样品洗去去离子水, 用镊子把它们吹干, 用氮气把它们擦干。</li>
	</ol></li>
	<li>电子束蒸发
	<ol>
<li>使用电子束蒸发器将 Ti (3 nm)/Au (100 nm) 双层沉积在波导和对准标记上。</li>
		<li>以 10 rpm 的速度连续旋转样品以增加层的均匀性。 注: 钛层的 3-5 nm, 使胶粘剂接触之间的罪孽样品和 Au 层。金层的厚度通常介于 80-120 nm 之间。这范围的厚度是适合的电线粘合的样品到定制印制电路板, 我们用来注入电流脉冲到波导。</li>
		<li>使用 0.5-0.7 Aͦ/秒的 Ti 的沉积率和 2.5 Aͦ/秒的 Au. 保持电子束系统的基本压力在大约 10-7毫巴或更好。</li>
		<li>或者, 用铜代替 Au 来制作波导, 以提高软 x 射线的透明度。</li>
	</ol></li>
	<li>升降
	<ol>
<li>钛/金薄膜沉积后, 将样品放入丙酮中1小时。</li>
		<li>现在, 用丙酮喷雾膜, 直到多余的金属被除去。</li>
		<li>如果多余的金属残留在样品上, 将它们放回烧杯中丙酮, 然后重复该过程。 注: 可以选择使用兆声浴来支持升降过程。样品与钛/金波导结构, 并与对准标记再次通过相同的光刻步骤, 以制作的磁光盘在波导上。</li>
	</ol></li>
	<li>2沉积
	<ol>
<li>将样品与波导和对准标记插入原子层沉积系统, 并将2层沉积 20 nm, 使波导和圆盘之间的绝缘层。</li>
		<li>用钛前体四 (dimethylamido) 钛 (TDMAT) 和 H2O 为2的氧等离子体沉积, 并以 0.51 Aͦ/周期的速率生长。</li>
	</ol></li>
	<li>样品的自旋涂层 注: 我们使用双层的抵抗, 以提高光盘的边缘质量。在电子束照射的过程中, 底部的抵抗是过量的, 在开发之后, 它提供了一个精致的切边。<ol>
<li>焙在热板上的样品在180°c 15 分钟, 以消除水分。</li>
		<li>自旋涂层共聚物抵抗在4000转每分钟1分钟。 注: 所产生的薄膜厚度约为30纳米。</li>
		<li>后烘烤的热板上的样品在180°c 3 分钟硬化抵抗。</li>
		<li>自旋涂层 PMMA 950K 抵抗在4000转每分钟1分钟。产生的薄膜厚度约为270纳米。</li>
		<li>后烘烤样品在180°c 3 分钟硬化抵抗。</li>
	</ol></li>
	<li>圆盘电子束光刻
	<ol>
<li>创建第二个 lithographical 模式的光盘的 GDS 格式, 并上传到电子束光刻系统。</li>
		<li>使用全局标记将 UV 协调系统与示例对齐。</li>
		<li>使用本地标记对齐写字段, 以便校准写字段的大小、旋转和移位, 以确保光盘在波导上的正确位置。</li>
		<li>将光盘区域暴露在20凯文的光束能量的电子剂量为220µC/厘米2 。使用 200-300 pA 的光束电流和一步大小为 10 nm 以暴露图案。</li>
	</ol></li>
	<li>化学发展
	<ol>
<li>在一个以 MIBK 为基础的开发人员中开发1分钟的样品, 并在三十年代用塞子 (IPA)。</li>
		<li>然后冲洗样品在去离子水三十年代和吹干他们与氮气, 同时拿着镊子。</li>
	</ol></li>
	<li>离子束溅射沉积
	<ol>
<li>将样品插入离子束溅射系统。</li>
		<li>根据溅射材料的方向倾斜试样持有者, 以便通过阴影效应使圆盘锥度变细。 注: 锥度用于控制涡旋环流11的开关。</li>
		<li>在大约 0.50.7毫巴的工作压力下, 用 10--5 Aͦ/秒的沉积速率将 20-50 nm 厚的坡莫合金 (镍80Fe20) 层存入。 注: 基本压力应为 10-7毫巴或更好。</li>
	</ol></li>
	<li>升降
	<ol>
<li>把样品放在丙酮中1小时。</li>
		<li>现在, 用丙酮喷雾膜, 同时把它们放在镊子中, 直到去除多余的金属。</li>
		<li>如果多余的金属残留在样品上, 请将样品放回烧杯中丙酮, 然后重复该过程。 注: 可以选择使用兆声浴来支持升降过程。我们得到了坡莫合金光盘的最终结构在一个钛/Au 波导上的罪恶膜, 如图 5所示。</li>
	</ol></li>
</ol><img alt="Figure 5" class="xfigimg" src="/files/ftp_upload/57817/57817fig5.jpg"> 图 5: 扫描电镜图像的最终结构30毫微米厚和2µm 宽坡莫合金光盘上的黄金波导与对准标记.这些样品进一步用于时间分辨的 MTXM 实验。<a href="/files/ftp_upload/57817/57817fig5large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>

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Y., Ivanov, B. A., Novosad, V., Otani, Y., Shima, H., Fukamichi, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Eigenfrequencies+of+vortex+state+excitations+in+magnetic+submicron-size+disks.">Eigenfrequencies of vortex state excitations in magnetic submicron-size disks.</a> Journal of Applied Physics. 91 (10), 813-823 (2002).</li><li>Urb&#225;nek, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dynamics+and+efficiency+of+magnetic+vortex+circulation+reversal.">Dynamics and efficiency of magnetic vortex circulation reversal.</a> Physical Review B. 91, 094415 (2015).</li><li>Uhl&#237;&#345;, V., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dynamics+switching+of+the+spin+circulation+in+tapered+magnetic+nanodisks.">Dynamics switching of the spin circulation in tapered magnetic nanodisks.</a> Nature Nanotechnology. 8 (5), 341-346 (2013).</li><li>Jung, H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Logic+operations+based+on+magnetic-vortex-state+networks.">Logic operations based on magnetic-vortex-state networks.</a> ACS Nano. 6 (5), 3712-3717 (2012).</li><li>Hasegawa, N., Sugimoto, S., Fujimori, H., Kondou, K., Niimi, Y., Otani, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Selective+mode+excitation+in+three-chained+magnetic+vortices.">Selective mode excitation in three-chained magnetic vortices.</a> Applied Physics Express. 8 (6), 063005 (2015).</li><li>Wintz, S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Magnetic+vortex+cores+as+tunable+spin-wave+emitters.">Magnetic vortex cores as tunable spin-wave emitters.</a> Nature Nanotechnology. 11, 948-953 (2016).</li><li>Hopster, H., Oepen, H. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Magnetic Microscopy of Nanostructures. , (2005).</li><li>Fischer, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Magnetic+imaging+with+polarized+soft+x-rays.">Magnetic imaging with polarized soft x-rays.</a> Journal of Physics D: Applied Physics. 50 (31), 313002 (2017).</li><li>Vanatka, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Magnetic+vortex+nucleation+modes+in+static+magnetic+fields.">Magnetic vortex nucleation modes in static magnetic fields.</a> AIP Advances. 7 (10), 105103 (2017).</li><li>Constancias, C., Landis, S., Manakli, S., Martin, L., Pain, L., Rio, D., Landis, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electron+beam+lithography.">Electron beam lithography.</a> Lithography. , (2013).</li><li>Williams, D. B., Carter, C. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Transmission Electron Microscopy. A Textbook for Materials Science. , (2009).</li><li>Seshan, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Handbook of Thin-film Deposition Processes and Techniques. , (2002).</li></ol>

作者没有什么可透露的。

我们已经展示了 LTEM 和 MTXM 磁性镜样品的制作。这些样品需要在薄的罪孽膜上制作, 这样, 在 LTEM 的情况下, 和软 x 射线的电子, 在 MTXM 的情况下, 可以穿透样品。这些样品可以制造 1) 正面抵抗光刻或 2) 消极抵抗光刻。
我们使用了正面抗光刻技术, 因为它需要更少的样品准备和更少的制造步骤, 并允许更容易的处理。它还允许研究员使用的阴影效果, 我们用于精确的圆盘形状控制 (圆盘一侧的渐狭)。该形状用于控制在核10,11的磁性涡旋的循环。
这种技术的缺点是复杂的升降过程, 因为薄膜材料有时沉积在抗力边缘上, 不能通过升降来去除。我们使用双抗层来解决这个问题。这稍微限制了 lithographical 过程的分辨率 (约 20 nm), 但仍足以用于磁性成像。
消极抵抗光刻技术提供一个更高的决议作为结构以决议下来到7毫微米可以被写入抵抗。然后用湿蚀刻或离子束蚀刻将材料蚀刻掉。这种方法的问题是, 在蚀刻后, 抵抗很难去除。在薄坡莫合金结构的情况下, 通常使用的氧等离子体抗剥离是不可能的, 因为它们很容易氧化。这一事实, 连同使用隐藏技术的需要, 有利于在整个工作中使用的正光刻过程。
我们使用本文所述方法制备的样品, 用于观察 MTXM10、11和不同核态17的循环切换过程中的磁涡动力学..这可以扩展到更多的实验类型, 需要 lithographically 制备的膜结构。

近两年来, 随着技术走向小型化, 纳米结构的磁性得到了深入的研究。随着结构的横向尺寸变小, 铁磁结构的磁性特性也开始受结构几何的影响, 除了磁性材料的性质外。从散装材料到显微组织的不同磁性元素的行为被详细审查 (例如,休伯特和赫尔穆特·舍费尔)1。非平凡磁化地面状态最著名的例子之一是磁性涡旋-卷曲磁化结构发生在微米和亚微米大小的薄磁盘和多边形。这里的磁化是在平面上绕出平面涡核2,3。磁涡的磁化反转在静态4、5、6和动态7、8、9、10中得到了广泛的研究。政权。磁涡的可能的应用是,例如,多比特记忆细胞11, 逻辑电路12, 射频设备13, 或自旋波发射器14。
为了成像磁涡, 特别是涡核, 显微技术的空间分辨率应尽可能接近基本的磁性长度刻度 (低于 10 nm)。洛仑兹透射电镜15 (LTEM) 和磁透射 x 射线显微镜16 (MTXM) 是磁涡流成像的理想候选者, 因为它们提供了高空间分辨率, 而且 MTXM 也提供了高的时间磁化动力学研究的决议。这些技术的缺点是复杂的样品准备, 这是本文的主题。
这里介绍的过程解释了用 TEM17和 MTXM10,11制作成像磁涡的样品。这两种技术都具有传输特性, 因此, 在薄膜上制造结构是必要的。膜通常由氮化硅制成, 其厚度范围从纳米到几上百纳米。这两种方法中的每一个都需要不同的支持框架几何图形。在 MTXM 的情况下, 框架是 5 x 5 毫米2和窗口是大的, 2 x 2 毫米2。在 TEM 的情况下, 框架几何是一个直径为3毫米的圆圈, 其大小取决于实验的窗口尺寸, 通常为 250 x 250 µm2。膜带来了更多的挑战, 更困难的样品处理, 有打破窗口在所有的光刻过程的风险。
样品的制作可以通过正负抗光刻技术进行18。正抗光刻工艺采用正面抗蚀;化学结构的抵抗变化后, 辐照和暴露的部分将成为可溶性在化工开发商。暴露的区域将会冲走, 而未曝光的区域将留在基板上。在负阻光刻过程中, 辐照硬化了抗性, 暴露的区域将保留在基体上, 而未曝光区域将在化学显影中冲洗掉。这两种技术都可以用于样品的制作, 但是我们更喜欢正面抗光刻, 因为与负阻光刻技术相比, 它需要较少的制造步骤。它也更容易处理, 更快, 并经常提供更好的结果。

<table>
	<tbody>
		<tr>
			<td>SiN Membrane - TEM</td>
			<td>Silson</td>
			<td>SiRN-TEM-200-0.25-500</td>
			<td>TEM membrane</td>
		</tr>
		<tr>
			<td>SiN Membrane - MTXM</td>
			<td>Silson</td>
			<td>SiRN-5.0-200-3.0-200</td>
			<td>MTXM membrane</td>
		</tr>
		<tr>
			<td>3D adapter for spin coating</td>
			<td></td>
			<td></td>
			<td>The model of the adapter for 3D printing can be downloaded at: https://www.thingiverse.com/thing:2808368</td>
		</tr>
		<tr>
			<td>PMMA 950k electron beam resist</td>
			<td>Allresist</td>
			<td>AR-P 679.04</td>
			<td>used for TEM sample</td>
		</tr>
		<tr>
			<td>Electron beam resist developer</td>
			<td>Allresist</td>
			<td>AR 600-56</td>
			<td>used for TEM sample</td>
		</tr>
		<tr>
			<td>High-contrast electron beam resist</td>
			<td>Allresist</td>
			<td>AR-P 6200.13</td>
			<td>used for the waveguide on the MTXM sample</td>
		</tr>
		<tr>
			<td>High-contrast electron beam resist developer</td>
			<td>Allresist</td>
			<td>AR-600-546</td>
			<td>used for the waveguide on the MTXM sample</td>
		</tr>
		<tr>
			<td>Tetrakis(dimethylamido)titanium(IV)</td>
			<td>Sigma Aldrich</td>
			<td>669008 Aldrich&#160;</td>
			<td>used for TiO2 thin film deposition by ALD&#160;</td>
		</tr>
		<tr>
			<td>Electron beam resist for nanometer lithography</td>
			<td>Allresist</td>
			<td>AR-P 617.02</td>
			<td>used as the bottom layer of bilayer resist for easier lift-off procedure</td>
		</tr>
		<tr>
			<td>PMMA 950k electron beam resist</td>
			<td>Allresist</td>
			<td>AR-P 679.04</td>
			<td>used as the top layer of bilayer resist for easier lift-off procedure</td>
		</tr>
		<tr>
			<td>Electron beam resist developer</td>
			<td>Allresist</td>
			<td>AR 600-56</td>
			<td>used for development of the disks on waveguide</td>
		</tr>
		<tr>
			<td>Permalloy pellets</td>
			<td>Kurt J Lesker</td>
			<td>EVMPERMQXQ-D</td>
			<td>used for the deposition of the magnetic layers</td>
		</tr>
		<tr>
			<td>Titanium pellets</td>
			<td>Kurt J Lesker</td>
			<td>EVMTI45QXQD</td>
			<td>used as adhesive layer for the gold waveguide</td>
		</tr>
		<tr>
			<td>Gold pellets</td>
			<td>Kurt J Lesker</td>
			<td>EVMAUXX40G</td>
			<td>used for the deposition of the waveguide</td>
		</tr>
	</tbody>
</table>

fabrication of magnetic nanostructures on silicon nitride membranes for magnetic vortex studies using transmission microscopy techniques

电子和 x 射线磁性镜允许高分辨率的磁性成像向下到十纳米。然而, 样品需要在透明的膜上制备, 这些薄膜非常脆弱且难于操作。我们提出了制造样品的过程, 磁性微-和纳米结构的旋转构型形成磁涡, 适用于洛伦兹透射电镜和磁性透射 x 射线显微学研究。样品是在氮化硅膜上制备的, 其制备过程包括自旋涂层、紫外和电子束光刻、抗化学发展、磁性材料的蒸发, 然后是形成最后的磁性结构。洛仑兹透射电子显微术的样品包括在单光刻步骤中制备的磁性 nanodiscs。用磁性 x 射线透射显微镜样品进行时间分辨磁化动态实验, 将磁 nanodiscs 放在波导上, 用于产生可重复的磁场脉冲, 通过电电流通过波导。波导是在额外的光刻步骤中创建的。

图 1显示了用于 MTXM 和 LTEM 镜的罪恶框架和膜的照片。图 2显示了在自旋涂层过程中, 3 维打印适配器的设计, 用于将 TEM 膜脱离轴。图 3显示了 LTEM 样品准备的各个步骤 (在抵抗发展之后和起飞过程之后) 和 LTEM 观察到的最终图像。图 4显示了在 MTXM 时间分辨实验中, 为制作圆盘和在 SiN 膜上的波导而准备步骤的示意图。图 5 显示了包含放在波导上的光盘的最终 MTXM 样本。

Watch this Scientific Journal Video about Fabrication of Magnetic Nanostructures on Silicon Nitride Membranes for Magnetic Vortex Studies Using Transmission Microscopy Techniques at JoVE.com

Fabrication of Magnetic Nanostructures on Silicon Nitride Membranes for Magnetic Vortex Studies Using Transmission Microscopy Techniques

提出了一种适用于透射电镜 (TEM) 和磁透射 x 射线显微术 (MTXM) 研究的磁涡流成形磁性微纳米结构的制备方法。

用透射显微技术制备氮化硅薄膜磁性纳米结构的研究

Electron and x-ray magnetic microscopies allow for high-resolution magnetic imaging down to tens of nanometers. However, the samples need to be prepared ...

fabrication-magnetic-nanostructures-on-silicon-nitride-membranes-for

Research

JoVE Journal

Engineering

8.0K 次观看.  Brno University of Technology. 提出了一种适用于透射电镜 (TEM) 和磁透射 x 射线显微术 (MTXM) 研究的磁涡流成形磁性微纳米结构的制备方法。

视频: Fabrication of Magnetic Nanostructures on Silicon Nitride Membranes for Magnetic Vortex Studies Using Transmission Microscopy Techniques

Fabrication of Uniform Nanoscale Cavities via Silicon Direct Wafer Bonding

Measurements of the heat capacity and superfluid fraction of confined 4He have been performed near the lambda transition using lithographically patterned and bonded silicon wafers. Unlike confinements in porous materials often used for these types of experiments3, bonded wafers provide predesigned uniform spaces for confinement. The geometry of each cell is well known, which removes a large source of ambiguity in the interpretation of data.
Exceptionally flat, 5 cm diameter, 375 &#181;m thick Si wafers with about 1 &#181;m variation over the entire wafer can be obtained commercially (from Semiconductor Processing Company, for example). Thermal oxide is grown on the wafers to define the confinement dimension in the z-direction. A pattern is then etched in the oxide using lithographic techniques so as to create a desired enclosure upon bonding. A hole is drilled in one of the wafers (the top) to allow for the introduction of the liquid to be measured. The wafers are cleaned2 in RCA solutions and then put in a microclean chamber where they are rinsed with deionized water4. The wafers are bonded at RT and then annealed at ~1,100 &#176;C. This forms a strong and permanent bond. This process can be used to make uniform enclosures for measuring thermal and hydrodynamic properties of confined liquids from the nanometer to the micrometer scale.

A method for permanently bonding two silicon wafers so as to realize a uniform enclosure is described. This includes wafer preparation, cleaning, RT bonding, and annealing processes. The resulting bonded wafers (cells) have uniformity of enclosure ~1%1,2. The resulting geometry allows for measurements of confined liquids and gasses.

通过硅直接晶圆粘接制造均匀纳米级腔

Measurements of the heat capacity and superfluid fraction of confined 4He have been performed near the lambda transition using lithographically patterned ...

科研

工程学

Fabrication of Gate-tunable Graphene Devices for Scanning Tunneling Microscopy Studies with Coulomb Impurities

Owing to its relativistic low-energy charge carriers, the interaction between graphene and various impurities leads to a wealth of new physics and degrees of freedom to control electronic devices. In particular, the behavior of graphene&#8217;s charge carriers in response to potentials from charged Coulomb impurities is predicted to differ significantly from that of most materials. Scanning tunneling microscopy (STM) and scanning tunneling spectroscopy (STS) can provide detailed information on both the spatial and energy dependence of graphene&#39;s electronic structure in the presence of a charged impurity.&#160;The design of a hybrid impurity-graphene device, fabricated using controlled deposition of impurities onto a back-gated graphene surface, has enabled several novel methods for controllably tuning graphene&#8217;s electronic properties.1-8 Electrostatic gating enables control of the charge carrier density in graphene and the ability to reversibly tune the charge2 and/or molecular5 states of an impurity. This paper outlines the process of fabricating a gate-tunable graphene device decorated with individual Coulomb impurities for combined STM/STS studies.2-5 These studies provide valuable insights into the underlying physics, as well as signposts for designing hybrid graphene devices.

This paper details the fabrication process of a gate-tunable graphene device, decorated with Coulomb impurities for scanning tunneling microscopy studies. Mapping the spatially dependent electronic structure of graphene in the presence of charged impurities unveils the unique behavior of its relativistic charge carriers in response to a local Coulomb potential.

对于扫描隧道显微学与库仑杂质制造门可调谐石墨烯器件

Owing to its relativistic low-energy charge carriers, the interaction between graphene and various impurities leads to a wealth of new physics and degrees ...

Phase Diagram Characterization Using Magnetic Beads as Liquid Carriers

Magnetic beads with ~1.9 &#181;m average diameter were used to transport microliter volumes of liquids between contiguous liquid segments with a tube for the purpose of investigating phase change of those liquid segments. The magnetic beads were externally controlled using a magnet, allowing for the beads to bridge the air valve between the adjacent liquid segments. A hydrophobic coating was applied to the inner surface of the tube to enhance the separation between two liquid segments. The applied magnetic field formed an aggregate cluster of magnetic beads, capturing a certain liquid amount within the cluster that is referred to as carry-over volume. A fluorescent dye was added to one liquid segment, followed by a series of liquid transfers, which then changed the fluorescence intensity in the neighboring liquid segment. Based on the numerical analysis of the measured fluorescence intensity change, the carry-over volume per mass of magnetic beads has been found to be ~2 to 3 &#181;l/mg. This small amount of liquid allowed for the use of comparatively small liquid segments of a couple hundred microliters, enhancing the feasibility of the device for a lab-in-tube approach. This technique of applying small compositional variation in a liquid volume was applied to analyzing the binary phase diagram between water and the surfactant C12E5 (pentaethylene glycol monododecyl ether), leading to quicker analysis with smaller sample volumes than conventional methods.

Here, we present a protocol to investigate multi-component phase diagrams using externally controlled magnetic beads as liquid carriers in a lab-in-tube approach. This approach can aid in applications that seek to gather further information on phase change in complex liquid systems.

相图表征使用磁珠用作液体载体

Magnetic beads with ~1.9 &#181;m average diameter were used to transport microliter volumes of liquids between contiguous liquid segments with a tube for ...

Ohmic Contact Fabrication Using a Focused-ion Beam Technique and Electrical Characterization for Layer Semiconductor Nanostructures

Layer semiconductors with easily processed two-dimensional (2D) structures exhibit indirect-to-direct bandgap transitions and superior transistor performance, which suggest a new direction for the development of next-generation ultrathin and flexible photonic and electronic devices. Enhanced luminescence quantum efficiency has been widely observed in these atomically thin 2D crystals. However, dimension effects beyond quantum confinement thicknesses or even at the micrometer scale are not expected and have rarely been observed. In this study, molybdenum diselenide (MoSe2) layer crystals with a thickness range of 6-2,700 nm were fabricated as two- or four-terminal devices. Ohmic contact formation was successfully achieved by the focused-ion beam (FIB) deposition method using platinum (Pt) as a contact metal. Layer crystals with various thicknesses were prepared through simple mechanical exfoliation by using dicing tape. Current-voltage curve measurements were performed to determine the conductivity value of the layer nanocrystals. In addition, high-resolution transmission electron microscopy, selected-area electron diffractometry, and energy-dispersive X-ray spectroscopy were used to characterize the interface of the metal&#8211;semiconductor contact of the FIB-fabricated MoSe2 devices. After applying the approaches, the substantial thickness-dependent electrical conductivity in a wide thickness range for the MoSe2-layer semiconductor was observed. The conductivity increased by over two orders of magnitude from 4.6 to 1,500 &#937;&#8722;1 cm&#8722;1, with a decrease in the thickness from 2,700 to 6 nm. In addition, the temperature-dependent conductivity indicated that the thin MoSe2 multilayers exhibited considerably weak semiconducting behavior with activation energies of 3.5-8.5 meV, which are considerably smaller than those (36-38 meV) of the bulk. Probable surface-dominant transport properties and the presence of a high surface electron concentration in MoSe2 are proposed. Similar results can be obtained for other layer semiconductor materials such as MoS2 and WS2.

We describe the approaches for the device fabrication and electrical characterization of molybdenum diselenide (MoSe2) layer semiconductor nanostructures with different thicknesses. In addition, the fabrication of ohmic contacts for MoSe2-layer nanocrystals by the focused-ion beam deposition method using platinum (Pt) as a contact metal is described.

欧姆接触制造用聚焦离子束技术和电气特性的半导体层的纳米结构

Layer semiconductors with easily processed two-dimensional (2D) structures exhibit indirect-to-direct bandgap transitions and superior transistor ...

Integration of Light Trapping Silver Nanostructures in Hydrogenated Microcrystalline Silicon Solar Cells by Transfer Printing

One of the potential applications of metal nanostructures is light trapping in solar cells, where unique optical properties of nanosized metals, commonly known as plasmonic effects, play an important role. Research in this field has, however, been impeded owing to the difficulty of fabricating devices containing the desired functional metal nanostructures. In order to provide a viable strategy to this issue, we herein show a transfer printing-based approach that allows the quick and low-cost integration of designed metal nanostructures with a variety of device architectures, including solar cells. Nanopillar poly(dimethylsiloxane) (PDMS) stamps were fabricated from a commercially available nanohole plastic film as a master mold. On this nanopatterned PDMS stamps, Ag films were deposited, which were then transfer-printed onto block copolymer (binding layer)-coated hydrogenated microcrystalline Si (&#181;c-Si:H) surface to afford ordered Ag nanodisk structures. It was confirmed that the resulting Ag nanodisk-incorporated &#181;c-Si:H solar cells show higher performances compared to a cell without the transfer-printed Ag nanodisks, thanks to plasmonic light trapping effect derived from the Ag nanodisks. Because of the simplicity and versatility, further device application would also be feasible thorough this approach.

A viable transfer printing-based methodology to introduce plasmonic metal nanostructures in solar cells is described. Using nanopillar poly(dimethylsiloxane) stamps, an Ag-based ordered nanodisk array was integrated with standard hydrogenated microcrystalline Si solar cells, which led to improved device performances due to plasmonic light trapping.

灯光诱杀银纳米结构通过转移印花在氢化微晶硅太阳能电池集成

One of the potential applications of metal nanostructures is light trapping in solar cells, where unique optical properties of nanosized metals, commonly ...

Use of a Multi-compartment Dynamic Single Enzyme Phantom for Studies of Hyperpolarized Magnetic Resonance Agents

Imaging of hyperpolarized substrates by magnetic resonance shows great clinical promise for assessment of critical biochemical processes in real time. Due to fundamental constraints imposed by the hyperpolarized state, exotic imaging and reconstruction techniques are commonly used. A practical system for characterization of dynamic, multi-spectral imaging methods is critically needed. Such a system must reproducibly recapitulate the relevant chemical dynamics of normal and pathological tissues. The most widely utilized substrate to date is hyperpolarized [1-13C]-pyruvate for assessment of cancer metabolism. We describe an enzyme-based phantom system that mediates the conversion of pyruvate to lactate. The reaction is initiated by injection of the hyperpolarized agent into multiple chambers within the phantom, each of which contains varying concentrations of reagents that control the reaction rate. Multiple compartments are necessary to ensure that imaging sequences faithfully capture the spatial and metabolic heterogeneity of tissue. This system will aid the development and validation of advanced imaging strategies by providing chemical dynamics that are not available from conventional phantoms, as well as control and reproducibility that is not possible in vivo.

A multi-compartment dynamic phantom is used to simulate some biology of interest for metabolic studies using hyperpolarized magnet resonance agents.

一个多腔动态单一酶幻影超极化磁共振剂研究的用途

Imaging of hyperpolarized substrates by magnetic resonance shows great clinical promise for assessment of critical biochemical processes in real time. Due ...

Frequency Mixing Magnetic Detection Scanner for Imaging Magnetic Particles in Planar Samples

The setup of a planar Frequency Mixing Magnetic Detection (p-FMMD) scanner for performing Magnetic Particles Imaging (MPI) of flat samples is presented. It consists of two magnetic measurement heads on both sides of the sample mounted on the legs of a u-shaped support. The sample is locally exposed to a magnetic excitation field consisting of two distinct frequencies, a stronger component at about 77 kHz and a weaker field at 61 Hz. The nonlinear magnetization characteristics of superparamagnetic particles give rise to the generation of intermodulation products. A selected sum-frequency component of the high and low frequency magnetic field incident on the magnetically nonlinear particles is recorded by a demodulation electronics. In contrast to a conventional MPI scanner, p-FMMD does not require the application of a strong magnetic field to the whole sample because mixing of the two frequencies occurs locally. Thus, the lateral dimensions of the sample are just limited by the scanning range and the supports. However, the sample height determines the spatial resolution. In the current setup it is limited to 2 mm. As examples, we present two 20 mm &#215; 25 mm p-FMMD images acquired from samples with 1 &#181;m diameter maghemite particles in silanol matrix and with 50 nm magnetite particles in aminosilane matrix. The results show that the novel MPI scanner can be applied for analysis of thin biological samples and for medical diagnostic purposes.

A scanner for imaging magnetic particles in planar samples was developed using the planar frequency mixing magnetic detection technique. The magnetic intermodulation product response from the nonlinear nonhysteretic magnetization of the particles is recorded upon a two-frequency excitation. It can be used to take 2D images of thin biological samples.

混频磁探测仪在平面样品成像磁性微粒

The setup of a planar Frequency Mixing Magnetic Detection (p-FMMD) scanner for performing Magnetic Particles Imaging (MPI) of flat samples is presented. ...

Studying Dynamic Processes of Nano-sized Objects in Liquid using Scanning Transmission Electron Microscopy

Samples fully embedded in liquid can be studied at a nanoscale spatial resolution with Scanning Transmission Electron Microscopy (STEM) using a microfluidic chamber assembled in the specimen holder for Transmission Electron Microscopy (TEM) and STEM. The microfluidic system consists of two silicon microchips supporting thin Silicon Nitride (SiN) membrane windows. This article describes the basic steps of sample loading and data acquisition. Most important of all is to ensure that the liquid compartment is correctly assembled, thus providing a thin liquid layer and a vacuum seal. This protocol also includes a number of tests necessary to perform during sample loading in order to ensure correct assembly. Once the sample is loaded in the electron microscope, the liquid thickness needs to be measured. Incorrect assembly may result in a too-thick liquid, while a too-thin liquid may indicate the absence of liquid, such as when a bubble is formed. Finally, the protocol explains how images are taken and how dynamic processes can be studied. A sample containing AuNPs is imaged both in pure water and in saline.

This protocol describes the operation of a liquid flow specimen holder for scanning transmission electron microscopy of AuNPs in water, as used for the observation of nanoscale dynamic processes.

使用扫描透射电子显微镜研究纳米大小的物体的动态过程中的液体

Samples fully embedded in liquid can be studied at a nanoscale spatial resolution with Scanning Transmission Electron Microscopy (STEM) using a ...

Fabrication of 1-D Photonic Crystal Cavity on a Nanofiber Using Femtosecond Laser-induced Ablation

We present a protocol for fabricating 1-D Photonic Crystal (PhC) cavities on subwavelength-diameter tapered optical fibers, optical nanofibers, using femtosecond laser-induced ablation. We show that thousands of periodic nano-craters are fabricated on an optical nanofiber by irradiating with just a single femtosecond laser pulse. For a typical sample, periodic nano-craters with a period of 350 nm and with diameter gradually varying from 50 - 250 nm over a length of 1 mm are fabricated on a nanofiber with diameter around 450 - 550 nm. A key aspect of such a nanofabrication is that the nanofiber itself acts as a cylindrical lens and focuses the femtosecond laser beam on its shadow surface. Moreover, the single-shot fabrication makes it immune to mechanical instabilities and other fabrication imperfections. Such periodic nano-craters on nanofiber, act as a 1-D PhC and enable strong and broadband reflection while maintaining the high transmission out of the stopband. We also present a method to control the profile of the nano-crater array to fabricate apodized and defect-induced PhC cavities on the nanofiber. The strong confinement of the field, both transverse and longitudinal, in the nanofiber-based PhC cavities and the efficient integration to the fiber networks, may open new possibilities for nanophotonic applications and quantum information science.

We present a protocol for fabricating 1-D photonic crystal cavities on subwavelength diameter silica fibers (optical nanofibers) using femtosecond laser-induced ablation.

1-D光子晶体空穴对纳米纤维使用飞秒激光诱导消融制造

We present a protocol for fabricating 1-D Photonic Crystal (PhC) cavities on subwavelength-diameter tapered optical fibers, optical nanofibers, using ...

Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and nanocrystalline materials. The traditional techniques associated with scanning electron microscopy (SEM), such as electron backscatter diffraction (EBSD), do not possess the required spatial resolution due to the large interaction volume between the electrons from the beam and the atoms of the material. Transmission electron microscopy (TEM) has the required spatial resolution. However, due to a lack of automation in the analysis system, the rate of data acquisition is slow which limits the area of the specimen that can be characterized. This paper presents a new characterization technique, Transmission Kikuchi Diffraction (TKD), which enables the analysis of the microstructure of UFG and nanocrystalline materials using an SEM equipped with a standard EBSD system. The spatial resolution of this technique can reach 2 nm. This technique can be applied to a large range of materials that would be difficult to analyze using traditional EBSD. After presenting the experimental set up and describing the different steps necessary to realize a TKD analysis, examples of its use on metal alloys and minerals are shown to illustrate the resolution of the technique and its flexibility in term of material to be characterized.

This paper provides a detailed method to characterize the microstructure of ultra-fine grained and nanocrystalline materials using a scanning electron microscope equipped with a standard electron backscatter diffraction system. Metal alloys and minerals presenting refined microstructures are analyzed using this technique, showing the diversity of its possible applications.