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 PDFInfo
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23H—WORKING 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
- B23H5/00—Combined machining
- B23H5/06—Electrochemical machining combined with mechanical working, e.g. grinding or honing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23H—WORKING 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
The invention provides a quick controllable manufacturing method of a large-area micron/nanometer texture on a metal material surface; and the method realizes the preparation of simple-complex, large-area and controllable-size micron/nanometer structures on metal surfaces with low cost and high efficiency through combining with the characteristic that the laser interference photoetching and the micro electrolytic machining both can reach submicron-level and nanometer-level resolutions and by using the characteristics that the laser interference photoetching is easy to realize large-area exposure and the micro electrolytic machining can machine all electric conducting materials. The method can reduce the machining cost and largely shorten the machining period, and has significant meaning on the research of tribological properties of textured surfaces.
Description
Technical field
The present invention relates to photoetching/PET microfiber field, specifically a kind of quick controlled manufacture method of metal material surface large area micro-/ nano texture.
Background technology
The fretting wear of part is the principal element affecting mechanical system Performance And Reliability.Add up according to investigations, the part failure of nearly 80% is caused by various forms of mechanical friction and wearing and tearing.Therefore, ensure that mechanical system function and the key in service life are the fretting wear problem how reduced between component.Find after deliberation, surface texturing techniques is a kind of effective means improving material surface tribological property.Along with the continuous microminiaturization of mechanical system, the demand for surface texture characteristic size is contracted to micron, sub-micron even nanoscale gradually.And in mechanical system, most of device is made up of metal material.Therefore, the research tool for micro-texturing techniques of metal material surface is of great significance.At present, the normal method adopted mainly comprises: minuteness milling, Laser Processing, abrasive air jet and spark machined etc.But above method all has some limitations, such as: (1) minuteness milling exists machining stress and surface residual stress, and be difficult to realize texturing process to difficult-to-machine material surface; (2) all there is heat affected area in Laser Processing and surface machined by EDM, and surface roughness is poor; (3) abrasive air jet is only applicable to the processing etc. to fragile material.In addition, the characteristic size of the texture that these methods process, generally between tens to hundreds of micron, is difficult to the preparation realizing several microns or smaller szie texture.
Electrolyzed Processing (ECM) a kind ofly subtracts material manufacture method based on Anodic solution principle, and in process, workpiece material is removed with the form of " ion ".And the size of " ion " is in nanometer scale, therefore, ECM is preparing the advantage had in micro-/ nano mesostructure in principle.Meanwhile, ECM also has plastic scope wide (can process nearly all conductive material), surface quality good (impulse-free robustness, micro-crack, recast layer and heat affected area), instrument is lossless and production efficiency high.Mask Electrolyzed Processing (TMECM) is a kind of special shape of ECM, and its principle first anode surface is carried out Electrolyzed Processing again after photoetching treatment.This combine with technique high-resolution of photoetching technique and the high efficiency of ECM are also one of common methods of preparing of metal material surface texture.For TMECM, early stage, the making of mask plate was very important, and it plays decisive role to the characteristic parameter of final texture.At present, the preparation method of mask mainly contains photograph final minification method, electron-beam direct writing method and the straight literary style of FIB etc.But all there is the shortcomings such as the long and mask plate area of expensive, fabrication cycle is little in these methods.And these problems prepare characteristic size be sub-micron, nanoscale mask plate time aobvious particularly outstanding.In addition, the type of texture, size and density degree are very large on the impact of material surface tribological property under various circumstances.When the characteristic parameter of required texture needs to change, if adopt traditional TMECM technique, mask plate then must make again, and this not only causes the waste of material, and greatly will extend process cycle.
Laser interference lithography (LIL) is a kind of emerging photoetching technique, and it does not need expensive optical lens and mask plate, obtains meticulous structure with existing light source and resist with regard to easy within the scope of large exposure field.Meanwhile, LIL also has the following advantages: (1) is easy to the preparation realizing dissimilar periodic structure.By changing the quantity participating in exposing light beam, dissimilar structure can be obtained, such as: hole array structure-four beam interference exposure etc. of striated structure-two-beam interference exposure, the hole array structure-three-beam interference exposure be triangularly arranged, rectangular arrangement; (2) easily realize the preparation of sub-micron, nano-scale structures, its minimum resolution can reach 1/4 times of optical maser wavelength.(3) characteristic size of structure can realize dynamic regulation.By regulating the incident angle of interfering beam, the arrangement cycle of texture can be changed, i.e. density; By changing exposure dose, the control to structure dutycycle can be realized.In sum, LIL technology with low-cost high-efficiency, can realize the preparation from simple to complicated, large-area, that size is controlled micro/nano structure.
Laser interference lithography and electrochemical micromachining all have respective pluses and minuses, if two kinds of techniques can be combined, are easier to realize the preparation in metal surface large-area submicron, nanoscale texture.
Summary of the invention
The present invention is in order to solve the problem of prior art, provide a kind of quick controlled manufacture method of metal material surface large area micro-/ nano texture, laser interference lithography and electrochemical micromachining technique are combined, be easy to realize the preparation in metal surface large-area submicron, nanoscale texture, and reduce processing cost, substantially reduce the process-cycle.
The invention provides a kind of quick controlled manufacture method of metal material surface large area micro-/ nano texture, comprise the following steps:
1) substrate surface is carried out ultrasonic cleaning by acetone, alcohol and deionized water respectively, to remove the spot on surface.Afterwards, toast in vacuum drying chamber, guarantee the adiabatic drying of substrate surface.
2) photoresist is coated in substrate surface uniformly, front baking process is carried out to it; Photoresist comprises positive photoresist and negative photoresist.
According to the characteristic parameter of required texture, select suitable Exposure mode, the incident angle regulating light beam is 0-90 °, and the size of aperture is 1-150mm, setting light exposure, carries out interference exposure to substrate; By changing Exposure mode, obtain dissimilar texture; The incidence angle changing light beam obtains the texture of different cycles, and the cycle of required texture is 0.1-10 μm; Change the size of the aperture of the diaphragm, realize the adjustment to exposure area; Change light exposure, obtain the texture of different duty, required dutycycle is 10-80%.Described interference Exposure mode comprises dual-beam exposure, three beam exposure and four beam exposure.
4) by through step 3) substrate after exposure-processed puts into development liquid pool and carries out ultrasonic development, after development terminates, the residual developer solution of substrate surface is fallen immediately with deionized water rinsing, substrate is toasted firmly, also referred to as post bake, come off from substrate surface to prevent photoresist film in follow-up electrochemical micromachining process.
5) after substrate cools naturally, be fixed in the anode clamp in electrochemical micromachining system, and be connected with the positive pole of ultra short pulses, carry out Electrolyzed Processing; Electrolyzed Processing uses ultra short pulses, and adding man-hour voltage is 1-20V, and the cycle is 0.1-10 μ s, and pulsewidth is 10-1000ns.In process, electrolyte flows through, to take away electrolysate, bubble hydrogen and reaction heat etc. at a high speed in machining gap.By the controlled working time, realize the preparation of different depth texture.
6) after Electrolyzed Processing, substrate is placed in the liquid pool that removes photoresist, after the photoresist film of removing surface residual, utilize alcohol and deionized water to carry out ultrasonic cleaning repeatedly, whole machining process terminates.
Beneficial effect of the present invention is:
1, the present invention proposes a kind of composite manufacturing method based on laser interference lithography and electrochemical micromachining, laser interference lithography and electrochemical micromachining all can reach sub-micron, nano level resolution ratio.Meanwhile, laser interference lithography easily realizes large area exposure, and electrochemical micromachining can process nearly all conductive material.As can be seen here, the method is easy to realize the preparation in metal surface large-area submicron, nanoscale texture.
2, in whole technical process, the method without the need to using mask, thus avoids the making of the mask of expensive, complex manufacturing technology.This not only lowers processing cost, and substantially reduce the process-cycle.
3, change the relevant parameter of exposure technology, just can realize the adjustment to texture type, density degree, dutycycle, this has great importance to the tribological property of research textured surfaces.
Accompanying drawing explanation
Fig. 1 is the process chart of processing method provided by the invention.
The photoresist film pattern schematic diagram that Fig. 2 (a) is dual-beam exposure imaging meron surface.
Fig. 2 (b) is the photoresist film pattern schematic diagram on three beam exposure development meron surfaces.
Fig. 2 (c) is the photoresist film pattern schematic diagram on four beam exposure development meron surfaces.
Detailed description of the invention
Below in conjunction with accompanying drawing, the invention will be further described.
Embodiment 1
The controlled manufacture method of the micro-texture of a kind of metal material surface of the present invention large area, as shown in Figure 1, can be divided into laser interference lithography and electrochemical micromachining two parts, specifically comprise the following steps.
(1) substrate pre-treatment.Material selection 304 stainless steel of substrate 1, cleans 5 minutes in acetone, alcohol and deionized water for ultrasonic respectively by it, to remove greasy dirt and other dust impurities on its surface.Then, the vacuum drying chamber being placed in 150 DEG C toasts 10min, guarantees its surperficial relatively dry, is of value to photoresist 2 and the better combination of substrate 1 surface like this.
(2) gluing and front baking.Select model to be the positive photoresist of AR-P3740, utilize high speed sol evenning machine, photoresist 2 is coated in substrate 1 surface uniformly with the rotating speed of 4000rpm, and the film thickness obtained is 1.4 μm.Then, front baking 1min on hot plate substrate 1 being placed in 100 DEG C.
(3) exposure is interfered.Laser instrument selects wavelength to be the Ultra-Violet Laser of 365nm, and regulate incidence angle to be 20 °, arranging light exposure is 55mJ/cm
2, be fixed on by substrate 1 on the sample stage in double light beam laser interference system and expose, the photoresist film pattern schematic diagram on development meron surface as shown in Figure 2 (a) shows.
(4) development and post bake (firmly toasting).Be ultrasonic development 60s in the developer solution of AR300-47 in model by the substrate 1 after exposure.Then, hot plate substrate 1 being placed in 115 DEG C toasts 1min firmly, comes off from substrate 1 surface to prevent photoresist film 2 in follow-up micro-electrochemical machining technique.
(5) electrochemical micromachining.After substrate 1 cools naturally, be fixed in the work piece holder in micro-electrochemical machining system, and be connected with the positive pole of ultra short pulses 8.Negative electrode 6 adopts the leaf identical with substrate size, and electrolyte 7 is the HCl solution of 10g/L, and machining voltage is 6V, and pulse width is 60ns, and the cycle is 8 μ s.Switch on power, carry out electrochemical micromachining.In process, electrolyte 7 flows through at a high speed in machining gap 5, takes away electrolysate, bubble hydrogen and processing heat, to ensure machining accuracy and stability.
(6) glued membrane is removed.Substrate 1 after Electrolyzed Processing is placed in the liquid 30min that removes photoresist that model is AR300-70, photoresist 2 film on removing substrate 1 surface.Then, repeatedly rinse by acetone, alcohol and deionized water.Whole processing process terminates.
Embodiment 2
(1) substrate pre-treatment.The material selection TC1 titanium alloy of substrate 1, cleans 5 minutes in acetone, alcohol and deionized water for ultrasonic respectively by it, to remove greasy dirt and other dust impurities on its surface.Then, the vacuum drying chamber being placed in 150 DEG C toasts 10min, guarantees its surperficial relatively dry, is of value to photoresist 2 and the better combination of substrate 1 surface like this.
(2) gluing and front baking.Select model to be the positive photoresist of AR-P3740, utilize high speed sol evenning machine, photoresist 2 is coated in substrate 1 surface uniformly with the rotating speed of 4000rpm, and the film thickness obtained is 1.4 μm.Then, front baking 1min on hot plate substrate 1 being placed in 100 DEG C.
(3) exposure is interfered.Laser instrument selects wavelength to be the Ultra-Violet Laser of 365nm, and regulate incidence angle to be 30 °, arranging light exposure is 80mJ/cm
2, be fixed on by substrate 1 on the sample stage in three beam laser interference systems and expose, the photoresist film pattern schematic diagram on development meron surface is as shown in Fig. 2 (b).
(4) development and post bake (firmly toasting).Be ultrasonic development 60s in the developer solution of AR300-47 in model by the substrate 1 after exposure.Then, hot plate substrate 1 being placed in 115 DEG C toasts 1min firmly, comes off from substrate 1 surface to prevent photoresist film 2 in follow-up micro-electrochemical machining technique.
(5) electrochemical micromachining.After substrate 1 cools naturally, be fixed in the work piece holder in micro-electrochemical machining system, and be connected with the positive pole of ultra short pulses 8.Negative electrode 6 adopts the leaf identical with substrate size, and electrolyte 7 is 1.0%NaCl+1.0%NaNO
3mixed solution, machining voltage is 15V, and pulse width is 100ns, and the cycle is 10 μ s.Switch on power, carry out electrochemical micromachining.In process, electrolyte 7 flows through at a high speed in machining gap 5, takes away electrolysate, bubble hydrogen and processing heat, to ensure machining accuracy and stability.
(6) glued membrane is removed.Substrate 1 after Electrolyzed Processing is placed in the liquid 30min that removes photoresist that model is AR300-70, photoresist 2 film on removing substrate 1 surface.Then, repeatedly rinse by acetone, alcohol and deionized water.Whole processing process terminates.
Embodiment 3
Preparation process is identical with embodiment 2, in step 3), three beam lasers is replaced with four beam lasers, and the photoresist film pattern schematic diagram on development meron surface as shown in Figure 2 (c).
Embody rule approach of the present invention is a lot, and the above is only the preferred embodiment of the present invention, should be understood that; for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvement, these improvement also should be considered as protection scope of the present invention.
Claims (8)
1. a quick controlled manufacture method for metal material surface large area micro-/ nano texture, is characterized in that comprising the following steps:
1) substrate is carried out cleaning pretreatment;
2) photoresist is coated in substrate surface uniformly, front baking process is carried out to it;
3) according to the characteristic parameter of required texture, select suitable Exposure mode, the incident angle regulating light beam is 0-90 °, and the size of aperture is 1-150mm, setting light exposure, carries out interference exposure to substrate;
4) by through step 3) substrate after exposure-processed puts into development liquid pool and carries out ultrasonic development, after development terminates, fall the residual developer solution of substrate surface immediately, firmly toast substrate with deionized water rinsing;
5) after substrate cools naturally, be fixed in the anode clamp in electrochemical micromachining system, and be connected with the positive pole of ultra short pulses, carry out Electrolyzed Processing;
6) after Electrolyzed Processing, substrate is placed in the liquid pool that removes photoresist, after the photoresist film of removing surface residual, cleans.
2. the quick controlled manufacture method of metal material surface large area micro-/ nano texture according to claim 1, it is characterized in that: the cleaning preprocessing process described in step 1) is for carry out ultrasonic cleaning by acetone, alcohol and deionized water respectively by substrate surface, afterwards, toast in vacuum drying chamber.
3. the quick controlled manufacture method of metal material surface large area micro-/ nano texture according to claim 1, is characterized in that: step 2) described in photoresist comprise positive photoresist and negative photoresist.
4. the quick controlled manufacture method of metal material surface large area micro-/ nano texture according to claim 1, is characterized in that: in described step 3), by changing Exposure mode, obtains dissimilar texture; The incidence angle changing light beam obtains the texture of different cycles; Change the size of the aperture of the diaphragm, realize the adjustment to exposure area; Change light exposure, obtain the texture of different duty.
5. the quick controlled manufacture method of metal material surface large area micro-/ nano texture according to claim 4, is characterized in that: described interference Exposure mode comprises dual-beam exposure, three beam exposure and four beam exposure.
6. the quick controlled manufacture method of metal material surface large area micro-/ nano texture according to claim 4, is characterized in that: the cycle of described texture is 0.1-10 μm, and dutycycle is 10-80%.
7. the quick controlled manufacture method of metal material surface large area micro-/ nano texture according to claim 1, it is characterized in that: the Electrolyzed Processing described in step 5) uses ultra short pulses, adding man-hour voltage is 1-20V, and the cycle is 0.1-10 μ s, and pulsewidth is 10-1000ns.
8. the quick controlled manufacture method of metal material surface large area micro-/ nano texture according to claim 1, is characterized in that: the cleaning process described in step 6) comprises and utilizes alcohol and deionized water to carry out ultrasonic cleaning.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106842822A (en) * | 2017-01-18 | 2017-06-13 | 长春理工大学 | The laser interference nanometer lithography system of one step texturing modified titanium alloy implant surface |
| CN107557852A (en) * | 2017-09-26 | 2018-01-09 | 西北农林科技大学 | A kind of processing method of high polymer material mechanical seal end surface Surface Texture |
| CN105583525B (en) * | 2016-01-27 | 2018-06-12 | 北京航空航天大学 | One kind is used for polymer/metal mixed structure median surface micro-structure new method for processing |
| CN108857050A (en) * | 2018-06-21 | 2018-11-23 | 西安理工大学 | A kind of preparation method of metal surface rule dimple texture array |
| CN109108403A (en) * | 2018-07-24 | 2019-01-01 | 杭州电子科技大学 | Metal surface dimple-structures manufacturing method and device based on contact adherency removing |
| US20220339725A1 (en) * | 2020-11-17 | 2022-10-27 | Soochow University | A method for preparing a cross-size micro-nano structure array |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105583525B (en) * | 2016-01-27 | 2018-06-12 | 北京航空航天大学 | One kind is used for polymer/metal mixed structure median surface micro-structure new method for processing |
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| CN108857050A (en) * | 2018-06-21 | 2018-11-23 | 西安理工大学 | A kind of preparation method of metal surface rule dimple texture array |
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| US20220339725A1 (en) * | 2020-11-17 | 2022-10-27 | Soochow University | A method for preparing a cross-size micro-nano structure array |
| US11992889B2 (en) * | 2020-11-17 | 2024-05-28 | Soochow University | Method for preparing a cross-size micro-nano structure array |
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