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CN114924098A - A flexible edgeless super-lubricating slider and its preparation method and application - Google Patents

A flexible edgeless super-lubricating slider and its preparation method and application Download PDF

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CN114924098A
CN114924098A CN202210556944.1A CN202210556944A CN114924098A CN 114924098 A CN114924098 A CN 114924098A CN 202210556944 A CN202210556944 A CN 202210556944A CN 114924098 A CN114924098 A CN 114924098A
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flexible
edgeless
microspheres
super
lubricating
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王稳
唐娇
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Southwest Jiaotong University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01QSCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q60/00Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/24AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
    • G01Q60/38Probes, their manufacture, or their related instrumentation, e.g. holders
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01QSCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q60/00Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/24AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
    • G01Q60/38Probes, their manufacture, or their related instrumentation, e.g. holders
    • G01Q60/42Functionalisation

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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Radiology & Medical Imaging (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

The invention discloses a flexible edge-free super-lubricating sliding block and a preparation method and application thereof, wherein the preparation method comprises the following steps: coating a layer of liquid ultraviolet curing glue on the top of the tip of the carrier; adhering the microspheres to the top of the tip of the carrier, and then irradiating the microspheres by using an ultraviolet lamp until the microspheres are cured; the microspheres on the carrier are scratched by sticky flexible polymer liquid drops to prepare flexible non-edge microspheres; and adhering a lubricating layer on the lower surface of the flexible edgeless microsphere to prepare the flexible edgeless super-lubricating slider. The method provided by the invention is simple and convenient, and when the method is applied to the detection of the interface interaction force, the problem of damage under the action of a sudden change load can be avoided due to the buffer action of the flexible macromolecules outside the microspheres. In addition, the microsphere is spherical and has no edge, the boundary friction is small, and the edge-free super-lubrication is in a real sense. The edge-free super-lubrication slider has extremely low abrasion, can effectively prolong the service life of the super-lubrication slider, and has wide adaptability.

Description

一种柔性无边缘超润滑滑块及其制备方法和应用A flexible edgeless super-lubricating slider and its preparation method and application

技术领域technical field

本发明涉及固体超润滑领域,具体涉及一种柔性无边缘超润滑滑块及其制备方法和应用。The invention relates to the field of solid superlubrication, in particular to a flexible edgeless superlubricating slider and a preparation method and application thereof.

背景技术Background technique

从20世纪80年代以来,表面探测技术在物理、化学、材料、生命以及工程等许多领域都有很重要的应用,其基本原理是利用带针尖的微悬臂探测针尖与样品相互作用,样品的大小和性质会随着针尖与样品间距离的变化而变化,从而可以获得样品的不同信息,实现检测目的。然而,目前的原子力显微镜(AFM)使用的探针结构存在一定的缺陷,如何制备理想的探针结构仍是一个挑战,例如,在直接化学气相沉积生长法制备石墨烯涂层探针的过程中,探针很容易被高温损坏;在使用液相剥离石墨烯涂层、模具辅助或PMMA辅助转移方法制备石墨烯涂层探针时,形成的层状异质结不可避免地存在污染,从而导致超润滑性失效;在石墨烯包裹探针的制造过程中,通过热辅助机械剥离或摩擦作用将多层石墨烯纳米薄片转移到探针上,尽管污染可以有效避免,在长时间的滑动测试后,多层石墨烯纳米薄片很容易从探针上脱落;用光刻法制造石墨岛的过程比较复杂,不适合原子力显微镜(AFM)的测量,总之,现有的实验使用的探针多少会对测量结果产生误差,故需要一种超润滑的柔性滑块规避这些问题。Since the 1980s, surface detection technology has had important applications in many fields such as physics, chemistry, materials, life, and engineering. And the properties will change with the distance between the needle tip and the sample, so that different information of the sample can be obtained to achieve the purpose of detection. However, the current probe structures used by atomic force microscopy (AFM) have certain defects, and how to prepare ideal probe structures is still a challenge, for example, in the process of preparing graphene-coated probes by direct chemical vapor deposition growth method , the probes are easily damaged by high temperature; when graphene-coated probes are prepared using liquid-phase exfoliation graphene coating, mold-assisted or PMMA-assisted transfer methods, the formed layered heterojunctions inevitably suffer from contamination, resulting in Superlubricity failure; multilayer graphene nanoflakes are transferred to the probe by thermally assisted mechanical exfoliation or friction during the fabrication of graphene-wrapped probes, although contamination can be effectively avoided, after prolonged sliding tests , the multi-layer graphene nanosheets are easily detached from the probes; the process of fabricating graphite islands by photolithography is complicated and is not suitable for the measurement of atomic force microscopy (AFM). The measurement results produce errors, so a super-lubricated flexible slider is needed to avoid these problems.

发明内容SUMMARY OF THE INVENTION

为了解决上述技术问题,本发明的目的是提供一种柔性无边缘超润滑滑块及其制备方法和应用,以解决现有技术中探针石墨烯涂层容易失效,在突变载荷下超润滑失效和超润滑使用寿命短的问题。In order to solve the above-mentioned technical problems, the purpose of the present invention is to provide a kind of flexible edgeless super-lubricating slider and its preparation method and application, so as to solve the problem that the probe graphene coating in the prior art is easy to fail, and the super-lubrication fails under sudden load. And the problem of short service life of ultra-lubrication.

本发明解决上述技术问题的技术方案如下:提供一种柔性无边缘超润滑滑块的制备方法,包括以下步骤:The technical solution of the present invention to solve the above-mentioned technical problems is as follows: a preparation method of a flexible edgeless super-lubricating slider is provided, comprising the following steps:

S1:在载体尖端的顶部涂覆一层液态的紫外固化胶;S1: Apply a layer of liquid UV-curable glue on the top of the carrier tip;

S2:将微球黏附于步骤S1所得的载体尖端的顶部,然后用紫外灯照射至固化;S2: Adhering the microspheres to the top of the tip of the carrier obtained in step S1, and then irradiating it with an ultraviolet lamp to cure;

S3:将步骤S2所得的载体尖端上的微球划过具有粘性的柔性高分子液滴,制得柔性无边缘微球;S3: Scratch the microspheres on the tip of the carrier obtained in step S2 across the viscous flexible polymer droplets to prepare flexible edgeless microspheres;

S4:在柔性无边缘微球下表面粘附润滑层,制得柔性无边缘超润滑滑块。S4: Adhering a lubricating layer on the lower surface of the flexible edgeless microspheres to obtain a flexible edgeless superlubricating slider.

本发明的有益效果为:本发明通过在载体尖端的微球上包裹具有粘性的柔性高分子液滴,得到表面光滑且无较明显孔洞的微球,然后再利用高分子材料的粘性粘附润滑层,制得柔性无边缘超润滑滑块,本发明提出的制备方法简单、便捷,将制得的柔性无边缘超润滑滑块应用原子力显微镜探针的检测样品时,针尖未与润滑层直接接触,在一定程度上保护了针尖,防止针尖的磨损,同时,球形的结构使其对冲击力和应力有很好的分散作用,再加上柔性的高分子材料,可避免载体尖端冲击应力变强时,由载体传递到润滑层的振动,导致最终扫图的不准确,以及样品在载体的来回扫描过程中损坏的问题。此外,本发明滑块整体形状为球形,减小了边界摩擦,在扫描过程中,滑块与样品之间点与面的接触形式实现了超润滑,无边缘的磨损能够有效提高超滑滑块的使用寿命,并且具有广泛适应性。The beneficial effects of the present invention are as follows: the present invention wraps viscous, flexible polymer droplets on the microspheres at the tip of the carrier to obtain microspheres with smooth surfaces and no obvious holes, and then utilizes the viscous adhesion of the polymer material to lubricate A flexible edgeless super-lubricating slider is prepared. The preparation method proposed by the invention is simple and convenient. When the prepared flexible edgeless ultra-lubricating slider is applied to the detection sample of an atomic force microscope probe, the needle tip is not in direct contact with the lubricating layer. , to a certain extent, protect the needle tip and prevent the needle tip from wearing. At the same time, the spherical structure makes it have a good dispersion effect on the impact force and stress. Coupled with the flexible polymer material, it can avoid the impact stress of the carrier tip becoming stronger. At the same time, the vibration transmitted from the carrier to the lubricating layer leads to the inaccuracy of the final scan and the problem that the sample is damaged during the back and forth scanning of the carrier. In addition, the overall shape of the slider of the present invention is spherical, which reduces the boundary friction. During the scanning process, the point-to-surface contact form between the slider and the sample realizes super lubrication, and no edge wear can effectively improve the ultra-slippery slider. long service life and wide adaptability.

在上述技术方案的基础上,本发明还可以做如下改进:On the basis of above-mentioned technical scheme, the present invention can also do following improvement:

进一步,步骤S1中载体为钨丝、ZnO纳米棒、二氧化硅丝或铜丝。Further, in step S1, the carrier is tungsten wire, ZnO nanorod, silicon dioxide wire or copper wire.

进一步,步骤S1中载体的直径为0.1-0.5mm。Further, the diameter of the carrier in step S1 is 0.1-0.5 mm.

进一步,步骤S1中载体尖端通过以下方法制得:利用电化学腐蚀在载体端部腐蚀出曲率半径为10-40μm的锥形,制得载体尖端。Further, in step S1, the carrier tip is prepared by the following method: using electrochemical etching to etch a cone with a curvature radius of 10-40 μm at the end of the carrier to prepare the carrier tip.

进一步,步骤S2中微球的直径为0.1-500μm。Further, the diameter of the microspheres in step S2 is 0.1-500 μm.

进一步,步骤S2中微球为二氧化硅微球、聚甲基丙烯酸甲酯微球或聚苯乙烯微球。Further, the microspheres in step S2 are silica microspheres, polymethyl methacrylate microspheres or polystyrene microspheres.

采用上述进一步技术方案的有益效果为:采用球形的微球是为了最终滑块的整体造型,球形的结构使其对冲击力和应力有很好的分散作用,球形的滑块在做层间相互作用力的实验中,能够减小滑块和样品的接触面积,进而减少界面之间的相互作用力,实现点对面的相对超润滑。The beneficial effects of adopting the above-mentioned further technical solutions are: the spherical microspheres are used for the overall shape of the final slider, the spherical structure makes it have a good dispersion effect on the impact force and stress, and the spherical sliders interact with each other between the layers. In the force experiment, the contact area between the slider and the sample can be reduced, thereby reducing the interaction force between the interfaces and realizing the relative superlubrication of the point-to-point surface.

进一步,步骤S3中具有粘性的柔性高分子液滴具体为PPC液滴、PC液滴、PCL液滴、PMMA液滴或PE液滴。Further, the viscous flexible polymer droplets in step S3 are specifically PPC droplets, PC droplets, PCL droplets, PMMA droplets or PE droplets.

采用上述进一步技术方案的有益效果为:柔性的高分子液滴在微球表面形成一道高分子膜,这层膜与微球组成的结构可以减缓通过载体前端传来的振动与应力,同时高分子膜与润滑层之间的相互作用力较强,可以将润滑层更加牢固的黏着在表面。The beneficial effects of the above-mentioned further technical solutions are: the flexible polymer droplets form a polymer film on the surface of the microspheres, and the structure composed of the film and the microspheres can slow down the vibration and stress transmitted through the front end of the carrier, and at the same time the polymer film The interaction force between the film and the lubricating layer is strong, and the lubricating layer can be more firmly adhered to the surface.

进一步,步骤S3中润滑层为均为层状的石墨烯、六方氮化硼或二硫化物。Further, in step S3, the lubricating layer is all layered graphene, hexagonal boron nitride or disulfide.

进一步,润滑层宽度为10-20μm。Further, the width of the lubricating layer is 10-20 μm.

进一步,层状的石墨烯是通过机械剥离法制得。Further, the layered graphene is prepared by mechanical exfoliation.

本发明还提供上述的柔性无边缘超润滑滑块的制备方法制得的柔性无边缘超润滑滑块。The present invention also provides a flexible edgeless superlubricating slider prepared by the above-mentioned preparation method of the flexible edgeless superlubricating slider.

进一步,柔性无边缘超润滑滑块的直径为15-25μm。Further, the diameter of the flexible edgeless superlubricating slider is 15-25 μm.

本发明还提供上述的柔性无边缘超润滑滑块在微纳米器件上的应用。The present invention also provides the application of the above-mentioned flexible edgeless super-lubricating slider on micro-nano devices.

上述紫外固化胶的型号为Permabond UV645或Permabond UV649。The model of the above UV curing adhesive is Permabond UV645 or Permabond UV649.

本发明具有以下有益效果:The present invention has the following beneficial effects:

1、本发明制备的柔性无边缘超润滑滑块使探针针尖与石墨烯并没有直接接触,在接触扫描过程中,针尖尖端不会因为接触而产生磨损,也不会在扫描过程中破坏样品,有效的提高了针尖的使用寿命。1. The flexible edgeless ultra-lubricating slider prepared by the present invention makes the probe tip not in direct contact with graphene. During the contact scanning process, the tip of the needle tip will not be worn due to contact, nor will the sample be damaged during the scanning process. , effectively improve the service life of the needle tip.

2、本发明引入的球形结构,在一定程度上对冲击力和应力有很好的分散作用。2. The spherical structure introduced by the present invention has a good dispersion effect on impact force and stress to a certain extent.

3、本发明通过引入柔性衬底,可以减小在接触扫描过程探针针尖产生的振动,以及由于载体前端冲击载荷突变时导致的超润滑失效。3. By introducing a flexible substrate, the present invention can reduce the vibration generated by the probe tip during the contact scanning process and the super-lubrication failure caused by the sudden change of the impact load at the front end of the carrier.

4、本发明提出的柔性滑块实现点对面的超润滑,球形的滑块减少了接触面积,减弱了边界摩擦的影响,最终减小了由于外界因素带来的误差。4. The flexible slider proposed by the present invention realizes the super-lubrication of the point-to-point surface, and the spherical slider reduces the contact area, weakens the influence of boundary friction, and finally reduces the error caused by external factors.

5、本发明提出的柔性无边缘超润滑滑块的制备方法简单、便捷,容易操作,并无固定的润滑层,可以是石墨烯或其他纳米层,且制备过程使用的材料也较宽泛,具有广泛的适用性。5. The preparation method of the flexible edgeless super-lubricating slider proposed by the present invention is simple, convenient, easy to operate, and has no fixed lubricating layer, which can be graphene or other nano-layers, and the materials used in the preparation process are also wide, with Broad applicability.

附图说明Description of drawings

图1为柔性无边缘超润滑滑块的制备过程示意图。Figure 1 is a schematic diagram of the preparation process of the flexible edgeless superlubricating slider.

其中,1、载体尖端;2、紫外固化胶;3、微球;4、具有粘性的柔性高分子液滴;5、润滑层。Among them, 1. carrier tip; 2. UV curing glue; 3. microspheres; 4. flexible polymer droplets with viscosity; 5. lubricating layer.

具体实施方式Detailed ways

以下结合附图对本发明的原理和特征进行描述,所举实例只用于解释本发明,并非用于限定本发明的范围。实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。The principles and features of the present invention will be described below with reference to the accompanying drawings. The examples are only used to explain the present invention, but not to limit the scope of the present invention. If the specific conditions are not indicated in the examples, it is carried out according to the conventional conditions or the conditions suggested by the manufacturer. The reagents or instruments used without the manufacturer's indication are conventional products that can be purchased from the market.

以下所用到的紫外固化胶的型号为Permabond UV645或Permabond UV649。The type of UV curing adhesive used below is Permabond UV645 or Permabond UV649.

实施例1:Example 1:

一种柔性无边缘超润滑滑块,其制备方法包括以下步骤(制备过程示意图见图1):A flexible edgeless super-lubricating slider, the preparation method of which includes the following steps (see Figure 1 for a schematic diagram of the preparation process):

S1:将试纸用IPA(异丙醇)浸湿,然后擦拭载玻片,用牙签蘸取少量二氧化硅微球薄涂在载玻片上,在显微镜下寻找直径为20μm的二氧化硅微球;S1: Wet the test paper with IPA (isopropyl alcohol), then wipe the glass slide, dip a small amount of silica microspheres on the glass slide with a toothpick, and look for silica microspheres with a diameter of 20 μm under the microscope ;

S2:将直径为0.2mm的钨丝,利用电化学腐蚀在钨丝端部腐蚀出曲率半径为30μm的锥形,制得钨丝尖端,在钨丝尖端的顶部涂覆一层液态的紫外固化胶,然后将钨丝安装在微纳米机械操作臂上,在原子力显微镜下确认单个二氧化硅微球的位置,将钨丝尖端对准目标微球,慢慢向下直至二氧化硅微球黏附在钨丝尖端的顶部,再用紫外灯照射至紫外固化胶固化;S2: Etch a tungsten wire with a diameter of 0.2 mm into a cone with a radius of curvature of 30 μm at the end of the tungsten wire by electrochemical etching to obtain the tip of the tungsten wire, and coat a layer of liquid UV curing on the top of the tip of the tungsten wire Then install the tungsten wire on the micro-nano mechanical manipulator, confirm the position of a single silica microsphere under the atomic force microscope, align the tip of the tungsten wire with the target microsphere, and slowly descend until the silica microsphere adheres On the top of the tip of the tungsten wire, irradiate it with a UV lamp until the UV curing glue is cured;

S3:另取一个载玻片,将试纸用IPA浸湿,擦拭载玻片,在载玻片表面滴一滴PPC液滴,将步骤S2固化后钨丝上的微球划过PPC液滴,制得柔性无边缘微球;S3: Take another glass slide, wet the test paper with IPA, wipe the glass slide, drop a drop of PPC droplet on the surface of the slide glass, and scratch the microspheres on the tungsten wire after curing in step S2 across the PPC droplet to make to obtain flexible edgeless microspheres;

S4:通过微纳米机械臂操作步骤S3得到的钨丝,在显微镜下寻找宽度为15μm的单层石墨烯层状材料(通过机械剥离法制得),将钨丝尖端对准、缓慢调整机械臂,直至接触,然后迅速抬起,在柔性无边缘微球下表面粘附一层石墨烯润滑层,制得柔性无边缘超润滑滑块。S4: The tungsten wire obtained in step S3 is operated by the micro-nano manipulator, look for a single-layer graphene layered material with a width of 15 μm (made by mechanical exfoliation method) under the microscope, align the tip of the tungsten wire, and slowly adjust the manipulator, Until contact, and then lifted quickly, a layer of graphene lubricating layer is adhered to the lower surface of the flexible edgeless microspheres to obtain a flexible edgeless ultra-lubricating slider.

实施例2:Example 2:

一种柔性无边缘超润滑滑块,其制备方法包括以下步骤:A flexible edgeless super-lubricating slider, the preparation method of which comprises the following steps:

S1:将试纸用IPA(异丙醇)浸湿,然后擦拭载玻片,用牙签蘸取少量的直径为0.1μm的聚甲基丙烯酸甲酯微球薄涂在载玻片上;S1: Wet the test paper with IPA (isopropyl alcohol), then wipe the glass slide, dip a small amount of polymethyl methacrylate microspheres with a diameter of 0.1 μm with a toothpick and thinly coat it on the glass slide;

S2:将直径为0.1mm的铜丝,利用电化学腐蚀在钨丝端部腐蚀出曲率半径为10μm的锥形,制得铜丝尖端,在铜丝尖端的顶部涂覆一层液态的紫外固化胶,然后将铜丝安装在微纳米机械操作臂上,在原子力显微镜下确认单个聚甲基丙烯酸甲酯微球的位置,将铜丝尖端对准目标微球,慢慢向下直至聚甲基丙烯酸甲酯微球黏附在铜丝尖端的顶部,再用紫外灯照射至紫外固化胶固化;S2: The copper wire with a diameter of 0.1 mm is etched into a cone with a curvature radius of 10 μm at the end of the tungsten wire by electrochemical etching to obtain a copper wire tip, and a layer of liquid UV curing is applied on the top of the copper wire tip Then install the copper wire on the micro-nano mechanical manipulator, confirm the position of a single polymethyl methacrylate microsphere under an atomic force microscope, align the tip of the copper wire with the target microsphere, and slowly go down until the polymethyl methacrylate The methyl acrylate microspheres are adhered to the top of the tip of the copper wire, and then irradiated with a UV lamp until the UV curing glue is cured;

S3:另取一个载玻片,将试纸用IPA浸湿,擦拭载玻片,在载玻片表面滴一滴PC液滴,将步骤S2固化后钨丝上的微球划过PC液滴,制得柔性无边缘微球;S3: Take another glass slide, wet the test paper with IPA, wipe the glass slide, drop a PC droplet on the surface of the slide glass, and scratch the microspheres on the tungsten wire after curing in step S2 across the PC droplet to make a to obtain flexible edgeless microspheres;

S4:通过微纳米机械臂操作步骤S3得到的铜丝,在显微镜下寻找宽度为10μm的单层六方氮化硼层状材料,将铜丝尖端对准、缓慢调整机械臂,直至接触,然后迅速抬起,在柔性无边缘微球下表面粘附一层六方氮化硼润滑层,制得柔性无边缘超润滑滑块。S4: Use the micro-nano manipulator to operate the copper wire obtained in step S3, look for a single-layer hexagonal boron nitride layered material with a width of 10 μm under the microscope, align the tip of the copper wire, slowly adjust the manipulator until contact, and then quickly Lifting, a layer of hexagonal boron nitride lubricating layer is adhered on the lower surface of the flexible edgeless microspheres to obtain a flexible edgeless super-lubricating slider.

实施例3:Example 3:

一种柔性无边缘超润滑滑块,其制备方法包括以下步骤:A flexible edgeless super-lubricating slider, the preparation method of which comprises the following steps:

S1:将试纸用IPA(异丙醇)浸湿,然后擦拭载玻片,用牙签蘸取少量的直径为500μm的聚苯乙烯微球薄涂在载玻片上;S1: Wet the test paper with IPA (isopropyl alcohol), then wipe the glass slide, dip a small amount of polystyrene microspheres with a diameter of 500 μm with a toothpick and thinly coat it on the glass slide;

S2:将直径为0.5mm二氧化硅丝,利用电化学腐蚀在钨丝端部腐蚀出曲率半径为40μm的锥形,制得二氧化硅丝尖端,在二氧化硅丝尖端的顶部涂覆一层液态的紫外固化胶,然后将二氧化硅丝安装在微纳米机械操作臂上,在原子力显微镜下确认单个聚苯乙烯微球的位置,将二氧化硅丝尖端对准目标微球,慢慢向下直至聚苯乙烯微球黏附在二氧化硅丝尖端的顶部,再用紫外灯照射至紫外固化胶固化;S2: The silicon dioxide wire with a diameter of 0.5mm is etched into a cone with a curvature radius of 40 μm at the end of the tungsten wire by electrochemical etching to obtain the tip of the silicon dioxide wire, and the top of the tip of the silicon dioxide wire is coated with a Layer the liquid UV-curable glue, then install the silica wire on the micro-nano mechanical manipulator, confirm the position of a single polystyrene microsphere under the atomic force microscope, align the tip of the silica wire to the target microsphere, and slowly Go down until the polystyrene microspheres adhere to the top of the tip of the silica wire, and then irradiate it with a UV lamp until the UV curing glue is cured;

S3:另取一个载玻片,将试纸用IPA浸湿,擦拭载玻片,在载玻片表面滴一滴PE液滴,将步骤S2固化后二氧化硅丝上的微球划过PE液滴,制得柔性无边缘微球;S3: Take another slide, soak the test paper with IPA, wipe the slide, drop a drop of PE on the surface of the slide, and scratch the microspheres on the silica wire after curing in step S2 across the PE drop , to prepare flexible edgeless microspheres;

S4:通过微纳米机械臂操作步骤S3得到的二氧化硅丝,在显微镜下寻找宽度为20μm的单层二硫化物层状材料,将二氧化硅丝尖端对准、缓慢调整机械臂,直至接触,然后迅速抬起,在柔性无边缘微球下表面粘附一层二硫化物润滑层,制得柔性无边缘超润滑滑块。S4: Use the micro-nano manipulator to operate the silicon dioxide wire obtained in step S3, look for a single-layer disulfide layered material with a width of 20 μm under the microscope, align the tip of the silicon dioxide wire, and slowly adjust the manipulator until contact , and then lifted quickly, a layer of disulfide lubricating layer was adhered to the lower surface of the flexible edgeless microspheres to obtain a flexible edgeless ultra-lubricating slider.

对比例1:Comparative Example 1:

一种石墨烯包裹尖端的探针,其制备方法包括以下步骤:A graphene-wrapped tip probe, the preparation method comprising the following steps:

S1:将石墨烯置于二氧化硅基底上,原子力显微镜的环境室中,将针尖向上提起50μm,并以1℃/s的速率,将石墨烯从25℃快速升温至200℃;S1: Place the graphene on the silica substrate, in the environmental chamber of the atomic force microscope, lift the needle tip upward by 50 μm, and rapidly heat the graphene from 25 °C to 200 °C at a rate of 1 °C/s;

S2:在加热过程中,让针尖撞击石墨烯,导致针尖在顶点附近断裂,断裂后,针尖出现平台。S2: During the heating process, let the needle tip hit the graphene, causing the needle tip to break near the apex, and after the break, a platform appears on the needle tip.

S3:在500N的载荷下,使用断裂的针尖扫描含阶梯边缘的同一区域,在接触式扫描过程中,断裂尖端与石墨烯之间的粘附力将大大增加,石墨烯会从边缘卷起,从基底剥落,然后逐渐转移并包裹住针尖尖端,加热可以赶走吸附在尖端和石墨烯表面的水,并促进断裂尖端与石墨烯的黏附,制得石墨烯包裹尖端的探针。S3: Under the load of 500N, use the broken tip to scan the same area with the stepped edge, during the contact scanning process, the adhesion between the broken tip and the graphene will be greatly increased, and the graphene will roll up from the edge, The tip is peeled off from the substrate, and then gradually transferred and wrapped around the tip of the needle tip. Heating can drive off the water adsorbed on the tip and graphene surface, and promote the adhesion of the fractured tip to the graphene, resulting in a graphene-wrapped tip probe.

试验例Test example

一、将实施例1-3及对比例1制得的探针放于AFM扫描仪上实验,具体方法为:在相同条件下对石墨烯基面进行往复摩擦测量,将实验过后的探针放在原子力显微镜下观察针尖磨损情况。1. Put the probes prepared in Examples 1-3 and Comparative Example 1 on the AFM scanner for experiment. The specific method is: under the same conditions, the reciprocating friction measurement is carried out on the graphene basal plane, and the probe after the experiment is placed on the AFM scanner. The tip wear was observed under an atomic force microscope.

结果为:对比例1在扫描结束后,尖端直径明显增大,这是由于针尖尖端在滑动过程中与基底间会产生横向力,在横向力的作用下,叶尖会产生磨损,在初始接触应力的作用下,尖端表面的润滑层会迅速适应剪切条件,并紧密结合到表面,促使纳米级摩擦层的形成,随着滑动的持续进行,尖端表面的润滑层发生无序变化,润滑层会随着扫描运动的进行,而逐渐向尖端边缘运动,从而增大尖端的直径;而实施例1-3制得的柔性无边缘超滑滑块在实验之后尖端直径并无明显变化,且针尖也无磨损。The results are: the diameter of the tip of the comparative example 1 increases significantly after the scanning is completed. This is due to the lateral force between the tip of the needle tip and the base during the sliding process. Under the action of stress, the lubricating layer on the surface of the tip will quickly adapt to the shearing conditions and be closely bonded to the surface, promoting the formation of a nano-scale friction layer. As the scanning movement progresses, it gradually moves to the edge of the tip, thereby increasing the diameter of the tip; while the flexible edgeless super-smooth sliders prepared in Examples 1-3 have no significant change in the tip diameter after the experiment, and the needle tip Also no wear.

以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection of the present invention. within the range.

Claims (10)

1.一种柔性无边缘超润滑滑块的制备方法,其特征在于,包括以下步骤:1. a preparation method of a flexible edgeless super-lubricating slider, is characterized in that, comprises the following steps: S1:在载体尖端(1)的顶部涂覆一层液态的紫外固化胶(2);S1: apply a layer of liquid UV-curable glue (2) on top of the carrier tip (1); S2:将微球(3)黏附于步骤S1所得的载体尖端的顶部,然后用紫外灯照射至固化;S2: Adhering the microspheres (3) to the top of the tip of the carrier obtained in step S1, and then irradiating it with an ultraviolet lamp to cure; S3:将步骤S2所得的载体尖端(1)上的微球(3)划过具有粘性的柔性高分子液滴(4),制得柔性无边缘微球;S3: Scratch the microspheres (3) on the carrier tip (1) obtained in step S2 across the viscous flexible polymer droplets (4) to prepare flexible edgeless microspheres; S4:在柔性无边缘微球下表面粘附润滑层(5),制得柔性无边缘超润滑滑块。S4: Adhering the lubricating layer (5) on the lower surface of the flexible edgeless microspheres to obtain a flexible edgeless super-lubricating slider. 2.根据权利要求1所述的柔性无边缘超润滑滑块的制备方法,其特征在于,步骤S1中载体为钨丝、ZnO纳米棒、二氧化硅丝或铜丝。2 . The method for preparing a flexible edgeless super-lubricating slider according to claim 1 , wherein in step S1 , the carrier is a tungsten wire, a ZnO nanorod, a silicon dioxide wire or a copper wire. 3 . 3.根据权利要求1所述的柔性无边缘超润滑滑块的制备方法,其特征在于,步骤S1中载体的直径为0.1-0.5mm。3 . The method for preparing a flexible edgeless super-lubricating slider according to claim 1 , wherein the diameter of the carrier in step S1 is 0.1-0.5 mm. 4 . 4.根据权利要求1所述的柔性无边缘超润滑滑块的制备方法,其特征在于,步骤S1中载体尖端(1)通过以下方法制得:利用电化学腐蚀在载体端部腐蚀出曲率半径为10-40μm的锥形,制得载体尖端(1)。4. The preparation method of the flexible edgeless super-lubricating slider according to claim 1, characterized in that, in step S1, the carrier tip (1) is obtained by the following method: utilizing electrochemical corrosion to etch a radius of curvature at the carrier end The carrier tip (1) is made into a 10-40 [mu]m cone. 5.根据权利要求1所述的柔性无边缘超润滑滑块的制备方法,其特征在于,步骤S2中微球(3)的直径为0.1-500μm。5 . The method for preparing a flexible edgeless super-lubricating slider according to claim 1 , wherein the diameter of the microspheres ( 3 ) in step S2 is 0.1-500 μm. 6 . 6.根据权利要求1或5所述的柔性无边缘超润滑滑块的制备方法,其特征在于,步骤S2中微球(3)为二氧化硅微球、聚甲基丙烯酸甲酯微球或聚苯乙烯微球。6. The preparation method of the flexible edgeless super-lubricating slider according to claim 1 or 5, characterized in that in step S2, the microspheres (3) are silicon dioxide microspheres, polymethyl methacrylate microspheres or polystyrene microspheres. 7.根据权利要求1所述的柔性无边缘超润滑滑块的制备方法,其特征在于,步骤S3中具有粘性的柔性高分子液滴(4)为PPC液滴、PC液滴、PCL液滴、PMMA液滴或PE液滴。7. The method for preparing a flexible edgeless super-lubricating slider according to claim 1, wherein the viscous flexible polymer droplets (4) in step S3 are PPC droplets, PC droplets, and PCL droplets , PMMA droplets or PE droplets. 8.根据权利要求1所述的柔性无边缘超润滑滑块的制备方法,其特征在于,步骤S3中润滑层(5)为均为层状的石墨烯、六方氮化硼或二硫化物。8 . The method for preparing a flexible edgeless super-lubricating slider according to claim 1 , wherein the lubricating layer ( 5 ) in step S3 is layered graphene, hexagonal boron nitride or disulfide. 9 . 9.根据权利要求1-8任一项所述的柔性无边缘超润滑滑块的制备方法制得的柔性无边缘超润滑滑块。9. A flexible edgeless super-lubricating slider prepared by the method for preparing a flexible edgeless super-lubricating slider according to any one of claims 1-8. 10.权利要求9所述的柔性无边缘超润滑滑块在微纳米器件上的应用。10. Application of the flexible edgeless superlubricating slider of claim 9 in micro-nano devices.
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Application publication date: 20220819