CN114088981B - Side wall scanning probe and processing method thereof - Google Patents
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Abstract
Description
技术领域technical field
本发明涉及微纳操作技术领域,具体涉及一种侧壁扫描探针及其加工方法。The invention relates to the technical field of micro-nano operation, in particular to a sidewall scanning probe and a processing method thereof.
背景技术Background technique
在过去的几十年里,原子力显微镜(AFM)已成为生命科学、生物、材料科学、半导体工业、微纳米技术等各学科中最重要的测量表征仪器之一。现代半导体和微机电系统器件中,复杂表面表征是必不可少的,如表征光子器件中纳米结构的侧壁粗糙度是一个关键的挑战,对优化诸如波导等纳米光学器件的效率起着重要作用。Over the past few decades, atomic force microscopy (AFM) has become one of the most important measurement and characterization instruments in various disciplines such as life science, biology, material science, semiconductor industry, micro-nano technology, etc. Complex surface characterization is essential in modern semiconductor and MEMS devices, such as characterizing the sidewall roughness of nanostructures in photonic devices is a key challenge and plays an important role in optimizing the efficiency of nano-optical devices such as waveguides .
传统的AFM扫描技术只能采集二维平面高度图,没有垂直测量的能力,同时现有的AFM悬臂探针的设计不能接触的倾斜角度大于针尖边角的表面,缺少对侧壁扫描的能力。针对上述的难点,Florian Krohs等人通过使用聚焦离子束(Focused ion beam,FIB)加工带有侧向尖端的AFM探针结合特定的侧壁扫描模式完成对侧壁形貌的扫描成像(FKrohs,Haenssler O C,Bartenwerfer M,et al.Atomic force microscopy for highresolution sidewall scans[C]International Conference on Manipulation.IEEE,2015)。Traditional AFM scanning technology can only collect two-dimensional plane height maps, without the ability to measure vertically. At the same time, the design of the existing AFM cantilever probe cannot touch the surface with an inclination angle larger than the corner of the needle tip, and lacks the ability to scan the side wall. In response to the above-mentioned difficulties, Florian Krohs et al. used a focused ion beam (Focused ion beam, FIB) to process an AFM probe with a lateral tip combined with a specific sidewall scanning mode to complete scanning imaging of the sidewall morphology (FKrohs, Haenssler O C, Bartenwerfer M, et al. Atomic force microscopy for high resolution sidewall scans [C] International Conference on Manipulation. IEEE, 2015).
然而现有的侧壁扫描探针主要通过聚焦离子束在传统的AFM探针上修饰完成,同时需要对标准的AFM设备和扫描模式进行重大的修改。一方面由于FIB工艺固有的串行性不利于探针大批量的生产,另一方面对标准的AFM设备大量修改也使得扫描方案难以推广。However, the existing sidewall scanning probes are mainly modified on traditional AFM probes by focused ion beams, and significant modifications to standard AFM equipment and scanning modes are required. On the one hand, the inherent seriality of the FIB process is not conducive to the mass production of probes, and on the other hand, a large number of modifications to the standard AFM equipment also make it difficult to promote the scanning scheme.
发明内容Contents of the invention
本发明针对面向原子力显微镜(Atomic Force Microscopy,AFM)的核心部件——侧壁扫描探针,采用微纳加工工艺制作侧壁扫描探针,箭头式的前端使扫描时追踪定位更为精确和方便,悬臂中间薄壁连接部分允许箭头式前端实现一定角度的偏转,配合线圈磁场对磁粒球的偏转控制实现高精度的侧壁扫描成像,悬垂式锥形针尖在针尖偏转时能有效地保护样品,以此实现对样品侧壁的高分辨率形貌成像,为微纳米结构的复杂表面表征提供一种具有高分辨率和高集成化的有力手段。The present invention is aimed at the core component of the atomic force microscope (Atomic Force Microscopy, AFM) - the side wall scanning probe, adopts micro-nano processing technology to make the side wall scanning probe, and the arrow-shaped front end makes the tracking and positioning more accurate and convenient during scanning , the thin-walled connection part in the middle of the cantilever allows the arrow-type front end to achieve a certain angle of deflection, and the deflection control of the magnetic particle ball by the coil magnetic field is used to achieve high-precision sidewall scanning imaging. The suspended tapered needle tip can effectively protect the sample when the needle tip is deflected. , so as to realize high-resolution topographical imaging of the sidewall of the sample, and provide a powerful means with high resolution and high integration for the complex surface characterization of micro-nano structures.
本发明至少通过如下技术方案之一实现。The present invention is realized through at least one of the following technical solutions.
一种侧壁扫描探针,包括悬臂以及与悬臂连接的前端部;所述悬臂上表面设置有金属反射层;所述前端部上表面设有磁粒球,前端部下表面设有针尖结构。A side wall scanning probe comprises a cantilever and a front end connected to the cantilever; the upper surface of the cantilever is provided with a metal reflection layer; the upper surface of the front end is provided with magnetic particles, and the lower surface of the front end is provided with a needle point structure.
优选的,所述针尖结构为锥形针尖结构,所述锥形针尖结构包括锥形针尖以及与前端部连接的棱台,所述锥形针尖通过连接件与棱台连接。Preferably, the needle point structure is a tapered needle point structure, the tapered needle point structure includes a tapered needle point and a prism connected to the front end, and the tapered needle point is connected to the prism through a connecting piece.
优选的,所述锥形针尖的形状为圆锥或者棱锥,长度为1~3μm,与棱台连接的连接件为棱柱,所述棱柱长度为5~10μm。Preferably, the shape of the tapered needle tip is a cone or a pyramid, the length of which is 1-3 μm, and the connecting piece connected to the prism is a prism, and the length of the prism is 5-10 μm.
优选的,所述悬臂侧面通过连接件与前端部侧面连接。Preferably, the side of the cantilever is connected to the side of the front end through a connecting piece.
优选的,与前端部连接的连接件为呈长方体状的薄壁,宽度为0.5~1μm,长度为8~15μm。Preferably, the connecting piece connected to the front end is a thin rectangular parallelepiped with a width of 0.5-1 μm and a length of 8-15 μm.
优选的,所述悬臂呈扁平长方体状,所述悬臂长度150~200μm,宽度30~60μm,厚度1~3μm。Preferably, the cantilever is in the shape of a flat cuboid, the cantilever has a length of 150-200 μm, a width of 30-60 μm, and a thickness of 1-3 μm.
优选的,前端部为箭头式形状,箭头尖端长度10~20μm,箭头尖端俯视呈正三角形。Preferably, the front end is in the shape of an arrow, the length of the tip of the arrow is 10-20 μm, and the tip of the arrow is an equilateral triangle in plan view.
优选的,所述前端部上表面设置有用于定位磁粒球的凹槽。Preferably, the upper surface of the front end part is provided with grooves for positioning magnetic balls.
优选的,所述悬臂的材料为Si3N4材料;所述悬臂、前端部、针尖结构一体成型;Preferably, the material of the cantilever is Si 3 N 4 material; the cantilever, the front end, and the tip structure are integrally formed;
所述金属反射层的材料为Au、Cr、Ni、Ag、Al、Pt、Pd中的一种或多种。The material of the metal reflective layer is one or more of Au, Cr, Ni, Ag, Al, Pt and Pd.
所述的一种侧壁扫描探针的加工方法,包括以下步骤:A method for processing a sidewall scanning probe comprises the following steps:
1)清洗硅基底,在硅基底上制作悬臂和前端部底面掩膜,并采用刻蚀的方法转移悬臂和前端部图形;1) Cleaning the silicon substrate, making a cantilever and front end bottom surface mask on the silicon substrate, and transferring the cantilever and front end graphics by etching;
2)在前端部图形上,采用光刻制作针尖结构掩膜,并采用深刻蚀的方法转移针尖结构图形;2) On the front-end pattern, use photolithography to make a needle-tip structure mask, and use a deep etching method to transfer the needle-tip structure pattern;
3)在步骤2)的针尖结构图形上,采用光刻制作内侧保护层;3) On the needle tip structure pattern in step 2), use photolithography to make the inner protective layer;
4)以内侧保护层为掩膜,采用腐蚀的方法制作锥形针尖;4) Using the inner protective layer as a mask, the tapered needle tip is made by corrosion;
5)采用局部湿法氧化制作多晶硅氧化层作为悬臂底层材料;5) Using partial wet oxidation to make polysilicon oxide layer as the bottom material of the cantilever;
6)通过光刻图形化悬臂图形并刻蚀完成图形转移,采用等离子体增强化学气相沉积方法生成悬臂主体Si3N4层;6) Pattern the cantilever pattern by photolithography and etch to complete the pattern transfer, and use the plasma enhanced chemical vapor deposition method to form the Si 3 N 4 layer of the cantilever main body;
7)采用光刻图形化金属反射层区域,通过电子束蒸发蒸镀Cr/Au反射层,制得金属反射层;7) Patterning the metal reflective layer area by photolithography, and evaporating the Cr/Au reflective layer by electron beam evaporation to prepare the metal reflective layer;
8)采用光刻图形化磁粒球区域,电子束蒸镀磁性材料,随后对磁性材料进行快速热退火处理形成磁粒球;8) Using photolithography to pattern the magnetic particle area, electron beam evaporation of magnetic material, and then performing rapid thermal annealing on the magnetic material to form magnetic particle balls;
9)腐蚀硅基底,完成侧壁扫描探针的释放,制得侧壁扫描探针。9) Etching the silicon substrate to complete the release of the sidewall scanning probes to obtain the sidewall scanning probes.
相对于现有技术,本发明具有如下有益效果:Compared with the prior art, the present invention has the following beneficial effects:
(1)本发明侧壁扫描探针是在普通硅片上进行图形转移,与现有工艺兼容,不需要FIB等其他工艺,有效降低生产成本和工艺复杂度,提高探针生产效率和工艺可靠性。(1) The sidewall scanning probe of the present invention performs pattern transfer on ordinary silicon wafers, is compatible with existing processes, does not require other processes such as FIB, effectively reduces production costs and process complexity, and improves probe production efficiency and process reliability sex.
(2)本发明侧壁扫描探针箭头式前端,遮挡面积小,使视场追踪和定位更加精确和方便。(2) The arrow-type front end of the scanning probe on the side wall of the present invention has a small shielding area, making the field of view tracking and positioning more accurate and convenient.
(3)本发明侧壁扫描探针悬臂薄壁连接和磁力球的设计使箭头式前端能实现侧壁扫描成像,悬垂式锥形针尖在针尖偏转时能有效保护待测样品。(3) The design of the cantilever thin-wall connection and the magnetic ball of the sidewall scanning probe of the present invention enables the arrow-shaped front end to realize sidewall scanning imaging, and the suspended tapered needle tip can effectively protect the sample to be tested when the needle tip is deflected.
附图说明Description of drawings
图1为本发明实施例侧壁扫描探针的结构示意图;1 is a schematic structural view of a sidewall scanning probe according to an embodiment of the present invention;
图2A为本发明实施例刻蚀薄硅基示意图;FIG. 2A is a schematic diagram of etching a thin silicon substrate according to an embodiment of the present invention;
图2B为本发明实施例光刻图形化悬垂棱柱示意图;2B is a schematic diagram of a photolithography patterned overhang prism according to an embodiment of the present invention;
图2C为本发明实施例制作锥形针尖的过程示意图;2C is a schematic diagram of the process of making a tapered needle tip according to an embodiment of the present invention;
图2D为本发明实施例腐蚀的锥形针尖示意图;Figure 2D is a schematic diagram of a tapered needle tip corroded by an embodiment of the present invention;
图2E为本发明实施例多晶硅氧化层示意图;2E is a schematic diagram of a polysilicon oxide layer according to an embodiment of the present invention;
图2F为本发明实施例侧壁扫描探针图形的转移示意图;FIG. 2F is a schematic diagram of the transfer of the pattern of the sidewall scanning probe according to the embodiment of the present invention;
图2G为本发明实施例制得的磁粒球结构示意图;Fig. 2G is a schematic diagram of the structure of magnetic spheres prepared in the embodiment of the present invention;
图2H为本发明实施例制得的侧壁扫描探针结构示意图;FIG. 2H is a schematic structural diagram of a sidewall scanning probe prepared in an embodiment of the present invention;
图3为本发明实施例侧壁扫描探针的扫描模式示意图。FIG. 3 is a schematic diagram of a scanning mode of a sidewall scanning probe according to an embodiment of the present invention.
具体实施方式Detailed ways
为表达的更简洁清晰,在下列描述当中,不详细描述公知的功能和结构,以凸显本发明的优势和特征。为了使本技术领域的人员更好地理解本发明方案,下面结合附图和具体实施方式对本发明作进一步的详细说明。显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。For more concise and clear expression, in the following description, well-known functions and structures are not described in detail, so as to highlight the advantages and features of the present invention. In order to enable those skilled in the art to better understand the solution of the present invention, the present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments. Apparently, the described embodiments are only some of the embodiments of the present invention, but not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
实施例1Example 1
如图1所示,本实施例提供一种侧壁扫描探针,包括悬臂1、磁粒球4和锥形针尖7。As shown in FIG. 1 , this embodiment provides a sidewall scanning probe, which includes a cantilever 1 , a
所述悬臂1的前端5呈三角箭头形,箭头形前端通过薄壁部分3(连接件)和悬臂1连接,悬臂1上表面设置有金属反射层2。所述磁粒球4呈球形,设置于箭头式前端5上部。所述锥形针尖7设置于箭头式前端5下部,且所述锥形针尖通过细长棱柱3和棱台连接,所述棱台和箭头式前端5相连。The front end 5 of the cantilever 1 is in the shape of a triangular arrow, and the arrow-shaped front end is connected to the cantilever 1 through a thin-walled part 3 (connector), and the upper surface of the cantilever 1 is provided with a metal reflective layer 2 . The
本实施例中,所述悬臂1的材料为Si3N4材料。In this embodiment, the material of the cantilever 1 is Si 3 N 4 material.
本实施例中,所述悬臂呈扁平长方体状,所述悬臂长度200μm,宽度35μm,厚度2μm。所述探针薄壁部分呈长方体状,宽度为0.5μm,长度为10μm。所述箭头式尖端长度15μm,俯视呈正三角形。In this embodiment, the cantilever is in the shape of a flat cuboid, the length of the cantilever is 200 μm, the width is 35 μm, and the thickness is 2 μm. The thin-walled portion of the probe is in the shape of a cuboid with a width of 0.5 μm and a length of 10 μm. The length of the arrow-shaped tip is 15 μm, and it is an equilateral triangle when viewed from above.
本实施例中,所述磁粒球的材料为钕铁硼,钕铁硼微粒直径为4μm。In this embodiment, the material of the magnetic balls is NdFeB, and the diameter of NdFeB particles is 4 μm.
本实施例中,锥形针尖形状为棱锥,长度为2μm,连接的棱柱长度为7μm。In this embodiment, the shape of the tapered tip is a pyramid with a length of 2 μm, and the length of the connected prism is 7 μm.
本实施例中,所述金属反射层3的材料为Au、Cr、Ni、Ag、Al、Pt、Pd中的一种或多种。In this embodiment, the material of the metal
实施例2Example 2
本实施例提供一种侧壁扫描探针的精细加工方法。如图2A-2H所示,步骤如下:This embodiment provides a fine processing method for a sidewall scanning probe. As shown in Figure 2A-2H, the steps are as follows:
首先清洗晶向为<100>的薄硅基100,氮气吹干后,采用光刻的方法在光刻胶101上图形化5μm×5μm的正方形,以光刻胶101为掩膜使用感应耦合等离子体(inductivelycoupled plasma,ICP)设备刻蚀薄硅基100转移针尖图形至硅基底,如图2A;First, clean the
将上述样品依次浸入80℃去胶液20min(分钟)、清洗丙酮超声10min和异丙醇30sec(秒),大量去离子水清洗后氮气吹干去除光刻胶101,采用厚胶工艺旋涂8-12μm的光刻胶101,并用光刻的方法图形化悬垂针尖的中间棱柱,以光刻胶101为掩膜使用ICP将棱柱图形转移至硅基100,如图2B;The above samples were immersed in 80°C degumming solution for 20 minutes (minutes), cleaned with acetone for 10 minutes and isopropanol for 30 seconds (seconds), washed with a large amount of deionized water, blown dry with nitrogen to remove
将上述样品依次浸入85℃去胶液30min(分钟)、清洗丙酮超声15min和异丙醇1min,大量去离子水清洗后氮气吹干去除光刻胶101,采用光刻的方法图形化侧壁保护膜,如图2C;随后以光刻胶101为掩膜,使用质量分数为30%KOH溶液在70℃腐蚀硅基100,完成锥形针尖的转移。如图2D;The above samples were immersed in 85°C degumming solution for 30 minutes (minutes), cleaned with acetone and ultrasonically for 15 minutes, and isopropanol for 1 minute. After cleaning with a large amount of deionized water, blow dry with nitrogen to remove the
采用去胶工艺去除光刻胶101,将样品在950℃的环境下湿法氧化15分钟的进行局部氧化。生成多晶硅氧化层102约100nm,如图2E;The
随后,采用光刻的方法在硅基底100上图形化箭头式侧壁扫描探针,采用等离子增强气相沉积(Plasma Enhanced Chemical Vapor Deposition,PECVD)沉积一层2μm的悬臂主体Si3N4层103,采用去胶工艺去除光刻胶和光刻胶上的Si3N4层,完成侧壁扫描探针图形的转移,如图2F;Subsequently, the arrow-shaped sidewall scanning probe is patterned on the
采用光刻的方法在悬臂主体Si3N4层103上图形化金属反射层104所在区域,电子束蒸发蒸镀Cr/Au反射层,厚度为5nm/50nm。使用去胶工艺完成多余金属和光刻胶的剥离,制作出金属反射层。光刻图形化磁粒球区域,电子束蒸发(Electron Beam Evaporation,EB)蒸镀Au/钕铁硼Au层,厚度为10nm/3μm/10nm,采用去胶工艺去除光刻胶和残留得金属层。随后对样品进行快速热退火处理(Rapid Thermal Annealing,RTA)完成磁粒球得制作,如图2G;The area where the metal
将样品置入缓冲层腐蚀液(Buffered Oxide Etch,BOE)溶液去除在硅基表面形成的多晶硅氧化层102以方便下面的释放操作,最后采用质量分数为30%KOH溶液在70℃腐蚀样品5h,完成最后探针样品的释放,即制得侧壁扫描探针,如图2H;The sample was placed in a buffered oxide etch solution (Buffered Oxide Etch, BOE) solution to remove the
实施例3Example 3
与实施例2基本相同,所不同的是:本实施例还提供一种侧壁扫描探针的扫描方法。It is basically the same as Embodiment 2, except that this embodiment also provides a scanning method of a sidewall scanning probe.
使用激光光束发生器11,反射镜12和四象限光电二极管13检测侧壁扫描探针14的挠度,间接测量针尖和样品16的相互作用。利用悬臂梁的挠度信号作为闭环控制器的反馈,通过调整采样高度来保持悬臂梁的施加力或幅值恒定。电磁线圈15来控制探针的偏转角度。如图3所示;The interaction between the tip and the
完成侧壁扫描探针14安装后,对探针和设备进行激光和参数校准,随后将探针移至待测试样品16区域,使用锁定放大器在侧壁扫描探针的共振频率处使探针产生扭转共振,从而使振荡的探针尖端可以轻敲垂直和水平的样品表面,同时对轻敲振幅测量来控制X和Z扫描的运动。After the installation of the
当扫描开始时,侧壁扫描探针14平行于水平面(沿X轴)扫描时接近样品16垂直侧壁。此时探针14尖端振荡幅度由Z轴扫描控制器调节。当探针14尖端位置与样品16侧壁之间的距离等于尖端水平振荡的幅度时,尖端开始敲击样品16垂直壁。随着针尖和样品侧壁距离变小,探针尖端水平振荡的幅度也开始减小,当减小到设定阈值时,Z轴扫描控制器使探针向上移动,同时电磁线圈15控制探针14的偏转角度,将幅度恢复到设定点,完成对侧壁的扫描。When scanning begins, the
以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节,也不限制该发明仅为所述的具体实施方式。显然,根据本说明书的内容,可作很多的修改和变化。本说明书选取并具体描述这些实施例,是为了更好地解释本发明的原理和实际应用,从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。The preferred embodiments of the invention disclosed above are only to help illustrate the invention. The preferred embodiments are not exhaustive in all detail, nor are the inventions limited to specific embodiments described. Obviously, many modifications and variations can be made based on the contents of this specification. This description selects and specifically describes these embodiments in order to better explain the principle and practical application of the present invention, so that those skilled in the art can well understand and utilize the present invention. The invention is to be limited only by the claims, along with their full scope and equivalents.
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