CN103146892B - Femtosecond laser surface pretreatment method for improving bonding state of layer base or film base - Google Patents
Femtosecond laser surface pretreatment method for improving bonding state of layer base or film base Download PDFInfo
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- CN103146892B CN103146892B CN201310072592.3A CN201310072592A CN103146892B CN 103146892 B CN103146892 B CN 103146892B CN 201310072592 A CN201310072592 A CN 201310072592A CN 103146892 B CN103146892 B CN 103146892B
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Abstract
The invention belongs to the field of application of femtosecond laser technology, and particularly relates to a material surface femtosecond laser pretreatment method. According to the invention, a femtosecond laser is utilized to carry out irradiation pretreatment on the base which needs a layer or film on the surface, thereby obtaining a self-assembly-growth long-range nano microstructure on the surface. The chemical plating experiment on the micro/nano surface formed after the femtosecond laser treatment indicates that compared with the traditional chemical plating, the method provided by the invention saves the pretreatment steps of acid washing, alkali washing, activating and the like, and the bonding strength of the plated film and the base is higher than that of the surface which is not subjected to femtosecond laser pretreatment. The technique provided by the invention is simple, convenient, practical and pollution-free, can effectively substitute the pretreatment technique for a layer or membrane preparation technique, improves the bonding state of the layer base or film base, and enhances the bonding strength of the layer base or film base.
Description
Technical field
The invention belongs to femtosecond laser technology Application Areas, particularly a kind of pretreated method of material surface femtosecond laser.
Background technology
Surface Engineering is that surface is after pre-treatment, by surface-coated, surface modification or kinds of surface technology Combined Processing, change form, chemical composition, weave construction and the stress state of solid metal surface or nonmetallic surface, to obtain the systems engineering of surperficial desired properties.Because it can obtain on cheap core surface, there is wear-resisting, anti-corrosion, antifatigue, the coating of the property such as high strength, resistance to punching press, high temperature thermal barrier, there is the feature of " low input; high production ", thereby be used widely in the various fields such as ferrous materials, oceanographic engineering, aerospace field, automobile manufacturing field, oilfield chemical, instrument, biomedicine.Conventional acquisition surface is coated with, coating, and the technology of film and modified layer comprises: thermospray, built-up welding, plating, electroless plating, electrochemical deposition, vapour deposition and application techniques, thermospray, heat expand ooze, laser beam surface modification, e-book surface modification and Ion Beam Surface Modification etc.
As everyone knows, interface is microstructure very important in matrix material, and it has reacted the adherence situation of layer and matrix, is the primary index that determines the over-all properties performance of matrix material.No matter be at matrix surface prepared layer or film, in preparation process, all to need to keep certain bonding force between layer or film and matrix.For some body material, if it not done to pre-treatment, be difficult to guarantee bonding strength between the two, so the pre-treatment of matrix surface all has a great impact the quality of layer or film and life-span.
Although the preconditioning technique using in above-mentioned sufacing is widely applied, still there are many problems.For instance, the pre-treatment of Electroless Plating of Ceramics is chemical roughen, its essence is ceramic surface is carried out to etching, make surface form countless grooves, micropore, cause surface microscopic coarse to increase the surface-area of matrix, guarantee the needed snap close effect of electroless plating, thereby improve the bonding strength of coating and matrix; Chemical roughen also can be removed greasy dirt and oxide compound and other adhesion or the adsorptive on matrix, makes matrix expose fresh activation tissue, improves the wetting property to activation solution, forms as far as possible many catalytic active centers being evenly distributed while being conducive to activate.In this pretreatment process, relate to alligatoring chemical solution proportioning, Coarsening Temperature control etc., program is complicated, operation inconvenience.In addition, there is pollution to human body and environment in coarsening solution, needs subsequent disposal, and the bonding strength of coating and matrix also needs further to be improved.For another example, galvanic deposit medical magnesium alloy will carry out supersaturation Ca (OH) to magnesium alloy before preparing bio-ceramic coating
2solution and anodic oxidation pre-treatment, need to carry out bonderizing etc. before automobile making application.These pretreatment processs all relate to the preparation of solution, the operation of utility appliance and wastewater treatment.
Femtosecond laser, due to its uniqueness, can obtain micro nano structure at material surface.Correlative study has patent report.Application number is that 200810152327.5 patent has been announced a kind of femtosecond laser that utilizes and at metal material surface, prepared the method for micro-/micro-nano structure, at Ti-Ni alloy surface, has made micro-nano structure.The patent No. is that 200810037730.3 patent has been announced a kind of femtosecond laser in the method for plane of crystal self-organizing growth of fine-nano-structure, at tin zinc plane of crystal, make long-range nanostructure, at crystal surface of ZnO, made the nanometer grating with periodic structure.Application number is that 201110302853.7 patent has been announced a kind of femtosecond laser and on synthetic glass surface, prepared the method for hydrophobic micro-structure, can make on synthetic glass surface the hydrophobic micro-structure of different size and pattern, the width of fringe of this periodicity linear array microstructure is 10-30 μ m, and the distance between striped is 10-30 μ m.But above-mentioned three kinds of methods all do not relate to the means using femtosecond laser as pretreatment.
Summary of the invention
The object of the invention is the deficiency existing in above-mentioned pretreatment process, the method for simple, convenient and practical, the free of contamination femtosecond laser pre-treatment of a kind of technique matrix surface is provided, replace the pretreatment process using in current preparative layer and film-forming process.
The device of implementing the inventive method comprises femto-second laser and Controlling System, worktable and computer programming system.Implement different subsequent disposal and adopt respectively different equipment.
Technical solution of the present invention is: utilize femtosecond laser to carrying out irradiation pre-treatment at the matrix of its surperficial prepared layer or film, obtain the long-range nano-micro structure of self-organizing growth on its surface.
Wherein irradiation pre-treatment step is as follows:
(1) tentatively polished with sand paper in pending surface;
(2) pending sample is placed on worktable, opens femto-second laser, according to pre-set programs, carry out surface irradiation pre-treatment;
(3) its concrete technology parameter is as follows:
Femtosecond laser wavelength is 1045nm
Spot size is 30-50 μ m
Pulse width is 500fs
Repetition rate is 500-1000kHz
Pulse energy is 2-8 μ J
Light distribution is Gaussian distribution
Sweep velocity is 120-2400mm/s
Multiple scanning number of times is 30-1200 time.
The described long-range micro nano structure that utilizes self-organizing growth prepared by femtosecond laser comprises the micron projection circle peak consisting of substantially parallel nano-structure or has the parallel micron streak of periodic structure.
Advantage of the present invention is:
1. utilize femto-second laser can obtain micro nano structure to carrying out pre-treatment at the sample of its surperficial masking or preparative layer.Thereby give full play to small-size effect, surface effects and the interfacial effect of nanostructure, thereby improve adsorption rate, catalytic rate and the diffusivity of coating, coating and film preparation process Atom.
2. with respect to the pretreatment process using in traditional masking or preparative layer technology, as the pickling in electroless plating, alkali cleaning and activating process, the method technique is simple, convenient and practical and pollution-free, can effectively substitute the pretreatment technology of preparative layer or filming technology.
3. this pretreatment process can improve layer base or film base bonding state, improves layer base or film substrate bond strength.
Accompanying drawing explanation
Fig. 1 is without after the pretreated laser deposition 4340 steel chemical Ni-P platings of femtosecond laser, the microstructure of film base junction cross section.(a) before tested for hardness, (b) after tested for hardness.
Fig. 2 (a) and (b) be laser deposition 4340 steel through the microstructure of femtosecond laser pretreatment layer, Fig. 2 (c) is the microstructure of pre-treatment tunic base junction cross section after hardness test.Treatment process parameter is: laser repetition rate 1000kHz, pulse energy 8 μ J, sweep velocity 480mm/s, multiple scanning number of times 120 times.
Fig. 3 (a) and (b) be laser deposition 4340 steel through the microstructure of femtosecond laser pretreatment layer, Fig. 3 (c) is the microstructure of pre-treatment tunic base junction cross section after hardness test.Treatment process parameter is: laser repetition rate 1000kHz, pulse energy 8 μ J, sweep velocity 1200mm/s, multiple scanning number of times 300 times.
Fig. 4 (a) and (b) be laser deposition 4340 steel through the microstructure of femtosecond laser pretreatment layer, Fig. 4 (c) is the microstructure of pre-treatment tunic base junction cross section after hardness test.Treatment process parameter is: laser repetition rate 500kHz, pulse energy 2 μ J, sweep velocity 120mm/s, multiple scanning number of times 180 times.
Embodiment
Below in conjunction with Fig. 1-Fig. 4, describe performance of the present invention in detail.
Embodiment mono-:
With tentatively polish 4340 steel of laser direct deposition of sand paper; Open femto-second laser laser apparatus, pre-treatment is carried out in 4340 steel surfaces.Concrete technology parameter is as follows: laser repetition rate 1000kHz, pulse energy 8 μ J, sweep velocity 480mm/s, multiple scanning number of times 120 times.
Then without any other pre-treatment, pretreated 4340 steel of femtosecond laser are carried out to chemical Ni-P plating experiment.After metallographic sample preparation, observe after pre-treatment and electroless plating after its cross section in conjunction with situation, as shown in Figure 2.For ease of relatively, undressed 4340 steel are carried out to electroless plating and do control sample, cross section is shown in Fig. 1 in conjunction with situation.Visible, undressed 4340 steel chemical platings are combined situation with matrix discontinuous, and some region is combination completely.Process, after hardness test, film base occurs separated.Fig. 2 (a) and (b) shown in 4340 steel after femtosecond laser pre-treatment, the micron order of the size inequality that the intimate parallel stripes that it is 279.5nm by width average that surface has formed a lot forms is justified peak.After this processing layer electroless plating, after the hardness test identical with unprocessed sample, film base is not separated, illustrates that film substrate bond strength is improved.
Embodiment bis-:
With tentatively polish 4340 steel of laser direct deposition of sand paper; Open femto-second laser laser apparatus, pre-treatment is carried out in 4340 steel surfaces.Concrete technology parameter is as follows: laser repetition rate 1000kHz, pulse energy 8 μ J, sweep velocity 1200mm/s, multiple scanning number of times 300 times.
Then without any other pre-treatment, pretreated 4340 steel of femtosecond laser are carried out to chemical Ni-P plating experiment.After metallographic sample preparation, observe after pre-treatment and electroless plating after its cross section in conjunction with situation, as shown in Figure 3.For ease of relatively, undressed 4340 steel are carried out to electroless plating and do control sample, cross section is shown in Fig. 1 in conjunction with situation.Visible, undressed 4340 steel chemical platings are combined situation with matrix discontinuous, and some region is combination completely.Process, after hardness test, film base occurs separated.Fig. 3 (a) and (b) shown in 4340 steel after femtosecond laser pre-treatment, the micron order circle peak that the intimate parallel stripes that it is 370.2nm by width average that surface has formed a lot forms, and it is not too large to justify peak size difference.After this processing layer electroless plating, after the hardness test identical with unprocessed sample, film base is not separated, illustrates that film substrate bond strength is improved.
Embodiment tri-:
With tentatively polish 4340 steel of laser direct deposition of sand paper; Open femto-second laser laser apparatus, pre-treatment is carried out in 4340 steel surfaces.Concrete technology parameter is as follows: laser repetition rate 500kHz, pulse energy 2 μ J, sweep velocity 120mm/s, multiple scanning number of times 180 times.
Then without any other pre-treatment, pretreated 4340 steel of femtosecond laser are carried out to chemical Ni-P plating experiment.After metallographic sample preparation, observe after pre-treatment and electroless plating after its cross section in conjunction with situation, as shown in Figure 4.For ease of relatively, undressed 4340 steel are carried out to electroless plating and do control sample, cross section is shown in Fig. 1 in conjunction with situation.Visible, undressed 4340 steel chemical platings are combined situation with matrix discontinuous, and some region is combination completely.Process, after hardness test, film base occurs separated.Fig. 4 (a) and (b) shown in 4340 steel after femtosecond laser pre-treatment, the micron order dimpling circle peak that the intimate parallel stripes that it is 579.2nm by width average that surface has formed a lot forms, and it is not too large to justify peak size difference, convexity is also lower.After this processing layer electroless plating, after the hardness test identical with unprocessed sample, film base is not separated, illustrates that film substrate bond strength is improved.
Claims (1)
1. a femtosecond laser process for surface preparation of improving layer base or film base bonding state, it is characterized in that utilizing femtosecond laser to carrying out irradiation pre-treatment at the matrix of its surperficial prepared layer or film, on its surface, obtain the long-range nano-micro structure of self-organizing growth; Described irradiation pre-treatment step is: tentatively polished with sand paper in pending surface, afterwards the sample after polishing is placed on worktable, open femto-second laser, utilize femtosecond laser to carry out irradiation to specimen surface; Described femtosecond laser wavelength is 1045nm, and pulse width is 500fs, and spot size is 30-50 μ m, repetition rate is 500-1000kHz, and pulse energy is 2-8 μ J, and light distribution is Gaussian distribution, sweep velocity is 120-2400mm/s, and multiple scanning number of times is 30-1200 time; The described long-range micro nano structure that utilizes self-organizing growth prepared by femtosecond laser comprises the micron projection circle peak consisting of substantially parallel nano-structure or has the parallel micron streak of periodic structure.
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| CN103624402B (en) * | 2013-11-14 | 2015-05-13 | 中国科学院上海光学精密机械研究所 | Method for improving laser preprocessing efficiency of optical element small light spot scanning |
| CN103725858B (en) * | 2013-12-24 | 2015-08-05 | 江苏大学 | Photochemical in-situ preparation method of patterned uniform chromium oxide film |
| CN104083802B (en) * | 2014-07-23 | 2015-08-05 | 江苏大学 | Improve the method for medical magnesium alloy surface medical bio anchoring strength of coating |
| CN104928607B (en) * | 2015-07-02 | 2017-12-05 | 江苏大学 | A kind of coating production for improving thermal barrier coating and basal body binding force |
| CN104928674B (en) * | 2015-07-02 | 2017-09-29 | 江苏大学 | Bury and cover the coating production that Combined Processing improves thermal barrier coating and basal body binding force |
| CN106676449A (en) * | 2015-11-04 | 2017-05-17 | 中国人民解放军装甲兵工程学院 | Method for improving bonding strength of coating |
| CN105798463A (en) * | 2016-05-31 | 2016-07-27 | 山东大学 | Pre-treatment technology used before coating of hard alloy cutter |
| CN109136802B (en) * | 2018-08-15 | 2020-05-29 | 沈阳工业大学 | Laser pretreatment corrosion-resistant strengthening process for aluminum alloy |
| CN109079446A (en) * | 2018-09-20 | 2018-12-25 | 北京航空航天大学 | A method of preparing antimicrobial surface on the medical instrument |
| CN110643807A (en) * | 2019-09-12 | 2020-01-03 | 广东工业大学 | Preparation method of micro-nano texture coating |
| CN111958113B (en) * | 2020-09-17 | 2022-04-22 | 哈尔滨工业大学（威海） | Aluminum/steel laser welding method under Cu element-surface microtexture composite regulation and control action |
| CN113387723B (en) * | 2021-06-01 | 2022-08-19 | 广东工业大学 | Diamond coating of ceramic cutter and preparation method and application thereof |
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| CN101264550A (en) * | 2008-04-25 | 2008-09-17 | 河北工业大学 | Application of femtosecond laser in titanium or titanium alloy implantation material surface treatment |
| CN101319347A (en) * | 2008-05-20 | 2008-12-10 | 上海大学 | Method for crystal surface self-organizing growth of fine-nano-structure with femtosecond laser |
| CN101380693A (en) * | 2008-10-14 | 2009-03-11 | 南开大学 | Micro-nano structure preparation method on metallic material surface using femtosecond laser |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101264550A (en) * | 2008-04-25 | 2008-09-17 | 河北工业大学 | Application of femtosecond laser in titanium or titanium alloy implantation material surface treatment |
| CN101319347A (en) * | 2008-05-20 | 2008-12-10 | 上海大学 | Method for crystal surface self-organizing growth of fine-nano-structure with femtosecond laser |
| CN101380693A (en) * | 2008-10-14 | 2009-03-11 | 南开大学 | Micro-nano structure preparation method on metallic material surface using femtosecond laser |
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