CN105081488A - Quick controllable manufacturing method of large-area micron/nanometer texture on metal material surface - Google Patents

Quick controllable manufacturing method of large-area micron/nanometer texture on metal material surface Download PDF

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CN105081488A
CN105081488A CN201510513351.7A CN201510513351A CN105081488A CN 105081488 A CN105081488 A CN 105081488A CN 201510513351 A CN201510513351 A CN 201510513351A CN 105081488 A CN105081488 A CN 105081488A
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substrate
exposure
micro
textures
nano
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贺海东
曲宁松
曾永彬
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23HWORKING OF METAL BY THE ACTION OF A HIGH CONCENTRATION OF ELECTRIC CURRENT ON A WORKPIECE USING AN ELECTRODE WHICH TAKES THE PLACE OF A TOOL; SUCH WORKING COMBINED WITH OTHER FORMS OF WORKING OF METAL
    • B23H5/00Combined machining
    • B23H5/06Electrochemical machining combined with mechanical working, e.g. grinding or honing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23HWORKING OF METAL BY THE ACTION OF A HIGH CONCENTRATION OF ELECTRIC CURRENT ON A WORKPIECE USING AN ELECTRODE WHICH TAKES THE PLACE OF A TOOL; SUCH WORKING COMBINED WITH OTHER FORMS OF WORKING OF METAL
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Abstract

本发明提供了一种金属材料表面大面积微/纳米织构的快速可控制造方法,结合了激光干涉光刻和微细电解加工均可以达到亚微米、纳米级的分辨率的特点,同时利用激光干涉光刻容易实现大面积曝光,而微细电解加工能够加工几乎所有的导电材料的特性,实现了在金属表面以低成本高效率,从简单到复杂、大面积的、尺寸可控的微/纳米结构的制备。不仅能够降低加工成本,大大缩短了加工周期,而且对研究织构化表面的摩擦学特性具有重要的意义。

The invention provides a fast and controllable manufacturing method of large-area micro/nano texture on the surface of metal materials, which combines the characteristics of laser interference lithography and micro electrolytic processing that can achieve submicron and nanometer resolution, and uses laser Interference lithography is easy to achieve large-area exposure, while micro-electrolytic processing can process almost all the characteristics of conductive materials, and realizes micro/nano micro-/nano-electrode on the metal surface at low cost and high efficiency, from simple to complex, large-area, and size-controllable Preparation of structures. It can not only reduce the processing cost and greatly shorten the processing cycle, but also has important significance for the study of the tribological properties of the textured surface.

Description

金属材料表面大面积微/纳米织构的快速可控制造方法Rapid and controllable fabrication of large-area micro/nanotextures on metallic surfaces

技术领域 technical field

本发明涉及光刻/微细电化学加工领域,具体是一种金属材料表面大面积微/纳米织构的快速可控制造方法。 The invention relates to the field of photolithography/micro-electrochemical processing, in particular to a rapid and controllable manufacturing method for large-area micro/nano textures on the surface of metal materials.

背景技术 Background technique

零件的摩擦磨损是影响机械系统性能和可靠性的主要因素。据调查统计,大约有80%的零件失效是由各种形式的机械摩擦和磨损引起的。因此,保证机械系统功能和使用寿命的关键在于如何降低构件间的摩擦磨损问题。经研究发现,表面织构化技术是改善材料表面摩擦学特性的一种有效手段。随着机械系统的不断微型化,对于表面织构特征尺寸的需求逐渐缩小至微米、亚微米甚至纳米尺度。而在机械系统中,大部分器件是由金属材料制成。因此,针对金属材料表面的微织构化技术的研究具有十分重要的意义。目前,常采用的方法主要包括:微细铣削、激光加工、磨料气射流和电火花加工等。然而,以上方法均存在一定的局限性,例如:(1)微细铣削存在加工应力和表面残余应力,且很难实现对难加工材料表面的织构化处理;(2)激光加工和电火花加工表面均存在热影响区,表面粗糙度较差;(3)磨料气射流仅适用于对脆性材料的加工等。另外,这些方法所加工出的织构的特征尺寸一般在几十到几百微米之间,很难实现数微米或更小尺寸织构的制备。 The friction and wear of parts is the main factor affecting the performance and reliability of mechanical systems. According to survey statistics, about 80% of component failures are caused by various forms of mechanical friction and wear. Therefore, the key to ensuring the function and service life of the mechanical system is how to reduce the friction and wear between components. The research found that surface texturing technology is an effective means to improve the tribological properties of the material surface. With the continuous miniaturization of mechanical systems, the demand for surface texture feature size is gradually reduced to micron, submicron and even nanoscale. In mechanical systems, most devices are made of metallic materials. Therefore, the research on micro-texturing technology for the surface of metal materials is of great significance. At present, the commonly used methods mainly include: micro-milling, laser processing, abrasive gas jet and EDM. However, the above methods all have certain limitations, for example: (1) micro-milling has processing stress and surface residual stress, and it is difficult to achieve texture treatment on the surface of difficult-to-machine materials; (2) laser processing and EDM There are heat-affected zones on the surface, and the surface roughness is poor; (3) Abrasive air jet is only suitable for processing brittle materials. In addition, the characteristic size of the textures processed by these methods is generally between tens to hundreds of microns, and it is difficult to realize the preparation of textures with a size of several microns or smaller.

电解加工(ECM)是一种基于电化学阳极溶解原理的减材制造方法,加工过程中工件材料以“离子”的形式去除。而“离子”的大小处于纳米量级,因此,ECM在制备微/纳米尺度结构方面具有原理上的优势。同时,ECM还具有可成型范围广(可加工几乎所有的导电材料)、表面质量好(无毛刺、微裂纹、再铸层和热影响区)、工具无损耗和生产效率高等特点。掩模电解加工(TMECM)是ECM的一种特殊形式,其原理是首先将阳极表面经光刻处理后再进行电解加工。该技术结合了光刻技术的高分辨率和ECM的高效率,也是金属材料表面织构制备的常用方法之一。对于TMECM来说,前期掩模板的制作十分重要,它对最终织构的特征参数起着决定性作用。目前,掩模的制作方法主要有照相精缩法、电子束直写法和聚焦离子束直写法等。但这些方法均存在价格昂贵、制作周期长和掩模板面积小等缺点。而这些问题在制备特征尺寸为亚微米、纳米尺度的掩模板时显的尤为突出。此外,织构的类型、尺寸和疏密程度在不同环境下对材料表面摩擦学特性影响很大。当所需织构的特征参数需要改变时,如果采用传统的TMECM工艺,掩模板则必须重新制作,这不仅造成了材料的浪费,而且将大大延长工艺周期。 Electrolytic machining (ECM) is a subtractive manufacturing method based on the principle of electrochemical anodic dissolution, in which workpiece material is removed in the form of "ions" during machining. However, the size of "ions" is on the nanometer scale, so ECM has a theoretical advantage in preparing micro/nano-scale structures. At the same time, ECM also has the characteristics of wide range of formability (machining almost all conductive materials), good surface quality (no burrs, microcracks, recasting layer and heat-affected zone), no loss of tools and high production efficiency. Mask electrolytic machining (TMECM) is a special form of ECM, and its principle is to firstly process the anode surface by photolithography and then perform electrolytic machining. This technology combines the high resolution of photolithography and the high efficiency of ECM, and is also one of the commonly used methods for surface texture preparation of metal materials. For TMECM, the preparation of the mask in the early stage is very important, and it plays a decisive role in the characteristic parameters of the final texture. At present, the manufacturing methods of masks mainly include photoreduction method, electron beam direct writing method and focused ion beam direct writing method. However, these methods all have disadvantages such as high price, long production cycle and small mask area. These problems are particularly prominent when preparing masks with submicron and nanoscale feature sizes. In addition, the type, size and density of the texture have a great influence on the tribological properties of the material surface under different environments. When the characteristic parameters of the required texture need to be changed, if the traditional TMECM process is used, the mask plate must be remade, which not only causes waste of materials, but also greatly prolongs the process cycle.

激光干涉光刻(LIL)是一种新兴的光刻技术,其不需要昂贵的光学镜头和掩膜板,用现有的光源和抗蚀剂就容易在大的曝光场范围内得到精细的结构。同时,LIL还具有以下优点:(1)易于实现不同类型周期性结构的制备。通过改变参与曝光光束的数量,可以得到不同类型的结构,例如:条纹结构-双光束干涉曝光、呈三角形排列的孔阵列结构-三光束干涉曝光、呈矩形排列的孔阵列结构-四光束干涉曝光等;(2)容易实现亚微米、纳米尺度结构的制备,其最小分辨率可达激光波长的1/4倍。(3)结构的特征尺寸可实现动态调控。通过调节干涉光束的入射角度,可以改变织构的排布周期,即疏密度;通过改变曝光剂量,可以实现对结构占空比的控制。综上所述,LIL技术能够以低成本高效率,实现从简单到复杂、大面积的、尺寸可控的微/纳米结构的制备。 Laser interference lithography (LIL) is an emerging lithography technology, which does not require expensive optical lenses and masks, and can easily obtain fine structures in a large exposure field range with existing light sources and resists . At the same time, LIL also has the following advantages: (1) It is easy to realize the preparation of different types of periodic structures. By changing the number of exposure beams, different types of structures can be obtained, such as: stripe structure-two-beam interference exposure, triangular array of holes-three-beam interference exposure, rectangular array of holes-four-beam interference exposure etc.; (2) It is easy to realize the preparation of submicron and nanoscale structures, and its minimum resolution can reach 1/4 times of the laser wavelength. (3) The characteristic size of the structure can be dynamically adjusted. By adjusting the incident angle of the interference beam, the arrangement period of the texture, that is, the density, can be changed; by changing the exposure dose, the duty cycle of the structure can be controlled. In summary, LIL technology can realize the preparation of simple to complex, large-area, and size-controllable micro/nanostructures at low cost and high efficiency.

激光干涉光刻和微细电解加工均有各自的优缺点,若能将两种工艺进行结合,更易于实现在金属表面大面积亚微米、纳米尺度织构的制备。 Both laser interference lithography and micro-electrolytic machining have their own advantages and disadvantages. If the two processes can be combined, it will be easier to realize the preparation of large-area submicron and nanoscale textures on metal surfaces.

发明内容 Contents of the invention

本发明为了解决现有技术的问题,提供了一种金属材料表面大面积微/纳米织构的快速可控制造方法,将激光干涉光刻和微细电解加工工艺进行结合,易于实现在金属表面大面积亚微米、纳米尺度织构的制备,并且降低了加工成本,大大缩短了加工周期。 In order to solve the problems of the prior art, the present invention provides a rapid and controllable manufacturing method of large-area micro/nano textures on the surface of metal materials, which combines laser interference lithography and micro-electrolytic processing technology, and is easy to realize large-scale micro/nano textures on the metal surface. The preparation of sub-micron and nano-scale textures reduces the processing cost and greatly shortens the processing cycle.

本发明提供了一种金属材料表面大面积微/纳米织构的快速可控制造方法,包括以下步骤: The invention provides a rapid and controllable manufacturing method of a large-area micro/nano texture on the surface of a metal material, comprising the following steps:

1)将基片表面分别用丙酮、酒精和去离子水进行超声清洗,以除去表面的污渍。之后,在真空干燥箱中进行烘烤,确保基片表面的绝对干燥。 1) The surface of the substrate is ultrasonically cleaned with acetone, alcohol and deionized water, respectively, to remove surface stains. After that, it is baked in a vacuum drying oven to ensure the absolute dryness of the substrate surface.

2)将光刻胶均匀的涂覆在基片表面,对其进行前烘处理;光刻胶包括正性光刻胶和负性光刻胶。 2) Coating the photoresist evenly on the surface of the substrate, and performing pre-baking treatment; the photoresist includes positive photoresist and negative photoresist.

按照所需织构的特征参数,选择合适的曝光方式,调节光束的入射角度为0-90°,光阑孔的大小为1-150mm,设定曝光量,对基片进行干涉曝光;通过改变曝光方式,得到不同类型的织构;改变光束的入射角得到不同周期的织构,所需织构的周期为0.1-10μm;改变光阑孔径的大小,实现对曝光面积的调节;改变曝光量,得到不同占空比的织构,所需占空比为10-80%。所述的干涉曝光方式包括双光束曝光、三光束曝光和四光束曝光。 According to the characteristic parameters of the required texture, select the appropriate exposure method, adjust the incident angle of the beam to 0-90°, the size of the aperture hole to 1-150mm, set the exposure amount, and perform interference exposure on the substrate; by changing Different types of textures can be obtained by means of exposure; textures of different periods can be obtained by changing the incident angle of the beam, and the required texture period is 0.1-10 μm; changing the size of the diaphragm aperture can realize the adjustment of the exposure area; changing the exposure amount , to obtain textures with different duty ratios, the required duty ratio is 10-80%. The interference exposure method includes two-beam exposure, three-beam exposure and four-beam exposure.

4)将经步骤3)曝光处理后的基片放入显影液池中进行超声显影,显影结束后,立即用去离子水冲洗掉基片表面残留的显影液,对基片进行硬烘烤,也称为坚膜,以防止后续微细电解加工过程中光刻胶膜从基片表面脱落。 4) Put the substrate after the exposure treatment in step 3) into the developer pool for ultrasonic development. After the development, immediately rinse off the residual developer on the surface of the substrate with deionized water, and hard bake the substrate. Also known as hard film, to prevent the photoresist film from falling off the surface of the substrate during the subsequent micro-electrolytic processing.

5)待基片自然冷却后,将其固定于微细电解加工系统中的阳极夹具内,并与超短脉冲电源的正极相连,进行电解加工;电解加工使用超短脉冲电源,加工时电压为1-20V,周期为0.1-10μs,脉宽为10-1000ns。加工过程中,电解液从加工间隙内高速流过,以带走电解产物、氢气泡和反应热等。通过控制加工时间,实现不同深度织构的制备。 5) After the substrate is naturally cooled, fix it in the anode fixture in the micro electrolytic machining system, and connect it to the positive pole of the ultrashort pulse power supply for electrolytic machining; the electrolytic machining uses an ultrashort pulse power supply, and the voltage during processing is 1 -20V, period is 0.1-10μs, pulse width is 10-1000ns. During the processing, the electrolyte flows through the processing gap at high speed to take away the electrolysis products, hydrogen bubbles and reaction heat. By controlling the processing time, the preparation of different depth textures can be realized.

6)电解加工完毕后,将基片置于去胶液池中,除去表面剩余的光刻胶膜后,利用酒精和去离子水进行反复超声清洗,整个加工工艺过程结束。 6) After the electrolytic processing is completed, the substrate is placed in the glue removal pool, and after removing the remaining photoresist film on the surface, it is cleaned repeatedly with alcohol and deionized water, and the entire processing process is completed.

本发明有益效果在于: The beneficial effects of the present invention are:

1、本发明提出了一种基于激光干涉光刻和微细电解加工的复合制造方法,激光干涉光刻和微细电解加工均可以达到亚微米、纳米级的分辨率。同时,激光干涉光刻容易实现大面积曝光,而微细电解加工能够加工几乎所有的导电材料。由此可见,该方法易于实现在金属表面大面积亚微米、纳米尺度织构的制备。 1. The present invention proposes a composite manufacturing method based on laser interference lithography and micro-electrolytic machining. Both laser interference lithography and micro-electrolytic machining can achieve submicron and nanoscale resolution. At the same time, laser interference lithography is easy to achieve large-area exposure, and micro-electrolytic machining can process almost all conductive materials. It can be seen that this method is easy to realize the preparation of large-area submicron and nanoscale textures on metal surfaces.

2、在整个工艺过程中,该方法无需使用掩模,从而避免了价格昂贵、制作工艺复杂的掩模的制作。这不仅降低了加工成本,而且大大缩短了加工周期。 2. In the whole process, the method does not need to use a mask, thereby avoiding the manufacture of an expensive and complicated mask. This not only reduces the processing cost, but also greatly shortens the processing cycle.

3、改变曝光工艺的相关参数,就可实现对织构类型、疏密程度、占空比的调节,这对研究织构化表面的摩擦学特性具有重要的意义。 3. Changing the relevant parameters of the exposure process can realize the adjustment of the texture type, density and duty cycle, which is of great significance to the study of the tribological properties of the textured surface.

附图说明 Description of drawings

图1为本发明提供的加工方法的工艺流程图。 Fig. 1 is the process flow diagram of the processing method provided by the present invention.

图2(a)为双光束曝光显影后基片表面的光刻胶膜图样示意图。 Fig. 2(a) is a schematic diagram of the photoresist film pattern on the surface of the substrate after double-beam exposure and development.

图2(b)为三光束曝光显影后基片表面的光刻胶膜图样示意图。 Fig. 2(b) is a schematic diagram of the pattern of the photoresist film on the surface of the substrate after three-beam exposure and development.

图2(c)为四光束曝光显影后基片表面的光刻胶膜图样示意图。 Fig. 2(c) is a schematic diagram of the photoresist film pattern on the surface of the substrate after four-beam exposure and development.

具体实施方式 Detailed ways

下面结合附图对本发明作进一步说明。 The present invention will be further described below in conjunction with accompanying drawing.

实施例1 Example 1

本发明一种金属材料表面大面积微织构的可控制造方法,如图1所示,可分为激光干涉光刻和微细电解加工两部分,具体包括以下步骤。 A controllable manufacturing method of a large-area micro-texture on the surface of a metal material of the present invention, as shown in Figure 1, can be divided into two parts: laser interference lithography and micro-electrolytic processing, and specifically includes the following steps.

(1)基片前处理。基片1的材料选用304不锈钢,将其分别在丙酮、酒精和去离子水中超声清洗5分钟,以除去其表面的油污和其他粉尘杂质。然后,置于150℃的真空干燥箱中烘烤10min,确保其表面相对干燥,这样有益于光刻胶2和基片1表面更好的结合。 (1) Substrate pretreatment. The material of the substrate 1 is 304 stainless steel, which is ultrasonically cleaned in acetone, alcohol and deionized water for 5 minutes to remove oil stains and other dust impurities on the surface. Then, place it in a vacuum drying oven at 150° C. and bake for 10 minutes to ensure that its surface is relatively dry, which is beneficial to better bonding of the photoresist 2 and the surface of the substrate 1 .

(2)涂胶和前烘。选用型号为AR-P3740的正性光刻胶,利用高速匀胶机,将光刻胶2以4000rpm的转速均匀的涂覆在基片1表面,得到的胶膜厚度为1.4μm。然后,将基片1置于100℃的热板上前烘1min。 (2) Gluing and pre-baking. The positive photoresist model AR-P3740 was selected, and the photoresist 2 was uniformly coated on the surface of the substrate 1 at a speed of 4000 rpm by using a high-speed coater, and the thickness of the obtained film was 1.4 μm. Then, the substrate 1 was pre-baked on a hot plate at 100° C. for 1 min.

(3)干涉曝光。激光器选用波长为365nm的紫外激光,调节入射角为20°,设置曝光量为55mJ/cm2,将基片1固定于双光束激光干涉系统中的样品台上进行曝光,显影后基片表面的光刻胶膜图样示意图如图2(a)所示。 (3) Interference exposure. The laser is an ultraviolet laser with a wavelength of 365nm, the incident angle is adjusted to 20°, and the exposure amount is set to 55mJ/cm 2 . The substrate 1 is fixed on the sample stage in the double-beam laser interference system for exposure. The schematic diagram of photoresist film pattern is shown in Fig. 2(a).

(4)显影与坚膜(硬烘烤)。将曝光后的基片1在型号为AR300-47的显影液中超声显影60s。接着,将基片1置于115℃的热板上硬烘烤1min,以防止后续微细电解工艺中光刻胶膜2从基片1表面脱落。 (4) Development and hard film (hard baking). The exposed substrate 1 was ultrasonically developed for 60 s in a developing solution of model AR300-47. Next, place the substrate 1 on a hot plate at 115° C. for hard baking for 1 min, so as to prevent the photoresist film 2 from falling off from the surface of the substrate 1 in the subsequent micro-electrolysis process.

(5)微细电解加工。待基片1自然冷却后,将其固定在微细电解系统中的工件夹具内,并与超短脉冲电源8的正极相连。阴极6采用与基片大小相同的钨片,电解液7为10g/L的HCl溶液,加工电压为6V,脉冲宽度为60ns,周期为8μs。接通电源,进行微细电解加工。加工过程中,电解液7从加工间隙5内高速流过,带走电解产物、氢气泡及加工热,以保证加工精度和稳定性。 (5) Micro electrolytic machining. After the substrate 1 is naturally cooled, it is fixed in the workpiece holder in the micro-electrolysis system and connected to the positive pole of the ultrashort pulse power supply 8 . The cathode 6 is a tungsten sheet with the same size as the substrate, the electrolyte 7 is 10g/L HCl solution, the processing voltage is 6V, the pulse width is 60ns, and the period is 8μs. Turn on the power and perform micro electrolytic machining. During the processing, the electrolyte 7 flows through the processing gap 5 at high speed, taking away the electrolysis products, hydrogen bubbles and processing heat, so as to ensure the processing accuracy and stability.

(6)去除胶膜。将电解加工后的基片1置于型号为AR300-70的去胶液中30min,除去基片1表面的光刻胶2膜。然后,用丙酮、酒精和去离子水反复冲洗。整个加工工艺流程结束。 (6) Remove the film. The electrolytically processed substrate 1 was placed in AR300-70 degumming solution for 30 minutes to remove the photoresist 2 film on the surface of the substrate 1 . Then, rinse repeatedly with acetone, alcohol, and deionized water. The whole processing process is finished.

实施例2 Example 2

(1)基片前处理。基片1的材料选用TC1钛合金,将其分别在丙酮、酒精和去离子水中超声清洗5分钟,以除去其表面的油污和其他粉尘杂质。然后,置于150℃的真空干燥箱中烘烤10min,确保其表面相对干燥,这样有益于光刻胶2和基片1表面更好的结合。 (1) Substrate pretreatment. The material of the substrate 1 is TC1 titanium alloy, which is ultrasonically cleaned in acetone, alcohol and deionized water for 5 minutes to remove oil stains and other dust impurities on the surface. Then, place it in a vacuum drying oven at 150° C. and bake for 10 minutes to ensure that its surface is relatively dry, which is beneficial to better bonding of the photoresist 2 and the surface of the substrate 1 .

(2)涂胶和前烘。选用型号为AR-P3740的正性光刻胶,利用高速匀胶机,将光刻胶2以4000rpm的转速均匀的涂覆在基片1表面,得到的胶膜厚度为1.4μm。然后,将基片1置于100℃的热板上前烘1min。 (2) Gluing and pre-baking. The positive photoresist model AR-P3740 was selected, and the photoresist 2 was uniformly coated on the surface of the substrate 1 at a speed of 4000 rpm by using a high-speed coater, and the thickness of the obtained film was 1.4 μm. Then, the substrate 1 was pre-baked on a hot plate at 100° C. for 1 min.

(3)干涉曝光。激光器选用波长为365nm的紫外激光,调节入射角为30°,设置曝光量为80mJ/cm2,将基片1固定于三光束激光干涉系统中的样品台上进行曝光,显影后基片表面的光刻胶膜图样示意图如图2(b)所示。 (3) Interference exposure. The laser is an ultraviolet laser with a wavelength of 365nm, the incident angle is adjusted to 30°, and the exposure amount is set to 80mJ/cm 2 . The substrate 1 is fixed on the sample stage in the three-beam laser interference system for exposure. The schematic diagram of photoresist film pattern is shown in Fig. 2(b).

(4)显影与坚膜(硬烘烤)。将曝光后的基片1在型号为AR300-47的显影液中超声显影60s。接着,将基片1置于115℃的热板上硬烘烤1min,以防止后续微细电解工艺中光刻胶膜2从基片1表面脱落。 (4) Development and hard film (hard baking). The exposed substrate 1 was ultrasonically developed for 60 s in a developing solution of model AR300-47. Next, place the substrate 1 on a hot plate at 115° C. for hard baking for 1 min, so as to prevent the photoresist film 2 from falling off from the surface of the substrate 1 in the subsequent micro-electrolysis process.

(5)微细电解加工。待基片1自然冷却后,将其固定在微细电解系统中的工件夹具内,并与超短脉冲电源8的正极相连。阴极6采用与基片大小相同的钨片,电解液7为1.0%NaCl+1.0%NaNO3的混合溶液,加工电压为15V,脉冲宽度为100ns,周期为10μs。接通电源,进行微细电解加工。加工过程中,电解液7从加工间隙5内高速流过,带走电解产物、氢气泡及加工热,以保证加工精度和稳定性。 (5) Micro electrolytic machining. After the substrate 1 is naturally cooled, it is fixed in the workpiece holder in the micro-electrolysis system, and connected to the positive pole of the ultrashort pulse power supply 8 . The cathode 6 uses a tungsten sheet with the same size as the substrate, the electrolyte 7 is a mixed solution of 1.0%NaCl+1.0%NaNO 3 , the processing voltage is 15V, the pulse width is 100ns, and the period is 10μs. Turn on the power and perform micro electrolytic machining. During the processing, the electrolyte 7 flows through the processing gap 5 at high speed, taking away the electrolysis products, hydrogen bubbles and processing heat, so as to ensure the processing accuracy and stability.

(6)去除胶膜。将电解加工后的基片1置于型号为AR300-70的去胶液中30min,除去基片1表面的光刻胶2膜。然后,用丙酮、酒精和去离子水反复冲洗。整个加工工艺流程结束。 (6) Remove the film. The electrolytically processed substrate 1 was placed in AR300-70 degumming solution for 30 minutes to remove the photoresist 2 film on the surface of the substrate 1 . Then, rinse repeatedly with acetone, alcohol, and deionized water. The whole processing process is finished.

实施例3 Example 3

制备步骤与实施例2相同,步骤3)中将三光束激光替换为四光束激光,显影后基片表面的光刻胶膜图样示意图如图2(c)所示。 The preparation steps are the same as in Example 2. In step 3), the three-beam laser is replaced by the four-beam laser. The photoresist film pattern on the surface of the substrate after development is shown in FIG. 2(c).

本发明具体应用途径很多,以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以作出若干改进,这些改进也应视为本发明的保护范围。 There are many specific application approaches of the present invention, and the above description is only a preferred embodiment of the present invention. It should be pointed out that for those of ordinary skill in the art, some improvements can also be made without departing from the principles of the present invention. Improvements should also be regarded as the protection scope of the present invention.

Claims (8)

1.一种金属材料表面大面积微/纳米织构的快速可控制造方法,其特征在于包括以下步骤: 1. A fast and controllable manufacturing method of large-area micro/nano texture on the surface of a metal material, characterized in that it comprises the following steps: 1)将基片进行清洗预处理; 1) The substrate is cleaned and pretreated; 2)将光刻胶均匀的涂覆在基片表面,对其进行前烘处理; 2) uniformly coating the photoresist on the surface of the substrate, and pre-baking it; 3)按照所需织构的特征参数,选择合适的曝光方式,调节光束的入射角度为0-90°,光阑孔的大小为1-150mm,设定曝光量,对基片进行干涉曝光; 3) Select an appropriate exposure method according to the characteristic parameters of the required texture, adjust the incident angle of the light beam to 0-90°, the size of the aperture hole to 1-150mm, set the exposure amount, and perform interference exposure on the substrate; 4)将经步骤3)曝光处理后的基片放入显影液池中进行超声显影,显影结束后,立即用去离子水冲洗掉基片表面残留的显影液,对基片进行硬烘烤; 4) putting the substrate after the exposure treatment in step 3) into the developer pool for ultrasonic development, after the development, immediately rinse off the remaining developer on the surface of the substrate with deionized water, and hard bake the substrate; 5)待基片自然冷却后,将其固定于微细电解加工系统中的阳极夹具内,并与超短脉冲电源的正极相连,进行电解加工; 5) After the substrate is naturally cooled, fix it in the anode fixture in the micro electrolytic machining system, and connect it to the positive electrode of the ultrashort pulse power supply for electrolytic machining; 6)电解加工完毕后,将基片置于去胶液池中,除去表面剩余的光刻胶膜后,进行清洗。 6) After the electrolytic processing is completed, the substrate is placed in a glue removal pool, and the remaining photoresist film on the surface is removed, and then cleaned. 2.根据权利要求1所述的金属材料表面大面积微/纳米织构的快速可控制造方法,其特征在于:步骤1)所述的清洗预处理过程为将基片表面分别用丙酮、酒精和去离子水进行超声清洗,之后,在真空干燥箱中进行烘烤。 2. The rapid and controllable manufacturing method of large-area micro/nano textures on the surface of metal materials according to claim 1, characterized in that: the cleaning pretreatment process described in step 1) is to use acetone and alcohol respectively on the surface of the substrate Ultrasonic cleaning with deionized water, followed by baking in a vacuum oven. 3.根据权利要求1所述的金属材料表面大面积微/纳米织构的快速可控制造方法,其特征在于:步骤2)所述的光刻胶包括正性光刻胶和负性光刻胶。 3. The rapid and controllable manufacturing method of large-area micro/nano textures on the surface of metal materials according to claim 1, characterized in that: the photoresist in step 2) includes positive photoresist and negative photoresist glue. 4.根据权利要求1所述的金属材料表面大面积微/纳米织构的快速可控制造方法,其特征在于:所述的步骤3)中,通过改变曝光方式,得到不同类型的织构;改变光束的入射角得到不同周期的织构;改变光阑孔径的大小,实现对曝光面积的调节;改变曝光量,得到不同占空比的织构。 4. The rapid and controllable manufacturing method of large-area micro/nano textures on the surface of metal materials according to claim 1, characterized in that: in the step 3), different types of textures are obtained by changing the exposure method; Change the incident angle of the light beam to obtain textures with different periods; change the size of the aperture to realize the adjustment of the exposure area; change the exposure amount to obtain textures with different duty ratios. 5.根据权利要求4所述的金属材料表面大面积微/纳米织构的快速可控制造方法,其特征在于:所述的干涉曝光方式包括双光束曝光、三光束曝光和四光束曝光。 5. The rapid and controllable manufacturing method of large-area micro/nano textures on the surface of metal materials according to claim 4, characterized in that: said interference exposure methods include double-beam exposure, three-beam exposure and four-beam exposure. 6.根据权利要求4所述的金属材料表面大面积微/纳米织构的快速可控制造方法,其特征在于:所述的织构的周期为0.1-10μm,占空比为10-80%。 6. The rapid and controllable manufacturing method of large-area micro/nano textures on the surface of metal materials according to claim 4, characterized in that: the period of the texture is 0.1-10 μm, and the duty ratio is 10-80% . 7.根据权利要求1所述的金属材料表面大面积微/纳米织构的快速可控制造方法,其特征在于:步骤5)所述的电解加工使用超短脉冲电源,加工时电压为1-20V,周期为0.1-10μs,脉宽为10-1000ns。 7. The rapid and controllable manufacturing method of large-area micro/nano textures on the surface of metal materials according to claim 1, characterized in that: the electrolytic processing in step 5) uses an ultra-short pulse power supply, and the voltage during processing is 1- 20V, period is 0.1-10μs, pulse width is 10-1000ns. 8.根据权利要求1所述的金属材料表面大面积微/纳米织构的快速可控制造方法,其特征在于:步骤6)所述的清洗过程包括利用酒精和去离子水进行超声清洗。 8. The rapid and controllable manufacturing method of large-area micro/nano textures on the surface of metal materials according to claim 1, characterized in that: the cleaning process in step 6) includes ultrasonic cleaning with alcohol and deionized water.
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