CN104911519A - Method for preparing titanium alloy super-hydrophobic and anti-frost surface by using ultra-short pulse laser - Google Patents
Method for preparing titanium alloy super-hydrophobic and anti-frost surface by using ultra-short pulse laser Download PDFInfo
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Abstract
The present invention relates to a method for preparing a titanium alloy super-hydrophobic and anti-frost surface by using ultra-short pulse laser, and belongs to the technical field of metal substrate surface modification. According to the method, the titanium alloy sample surface is subjected to polishing pretreatment, the polished sample surface is cleaned in an ultrasonic wave cleaning instrument with deionized water, blow drying with cold wind or air drying is performed after the cleaning, a laser processing technology is utilized, an ultra-short pulse laser is used to adjust the relevant process parameters, the sample is subjected to a surface treatment, countless micro structures are processed on the sample surface, and after completing the processing, the processed sample is placed into an electric heating drying box to bake so as to obtain the titanium alloy super-hydrophobic anti-frost surface, wherein the surface has the micron-scale papillary or crack-like structure or nano-scale hole structure and other structures, and further has characteristics of excellent super-hydrophobicity and frost resistance. The preparation method of the present invention has characteristics of simple process, convenient operation, high efficiency, low energy consumption, low cost, green environmental protection, and easy industrial application achieving.
Description
Technical field:
The invention belongs to metallic substrate surface technical field of modification, relate to the preparation method on super-hydrophobic frost resistance surface on titanium alloy substrate, more particularly, the present invention relates to a kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface.
Background technology:
The animals and plants of occurring in nature are through the selection of 1 years and evolution, and have the life style of its uniqueness, super-hydrophobic automatic cleaning surface is exactly wherein a kind of: small and weak insect body surface, owing to possessing super hydrophobic functional, can fly in the rain; Owing to having super-hydrophobic micro-nano structure on the pin of water spider, can on the water surface almost non-resistance creep; The super-drainage structure of lotus leaf surface substantially increases its self-cleaning function; The petal surface of the plants such as Rose just has very outstanding super-hydrophobicity, these performances material antiseptic erosion, anti-oxidant etc. in have application prospect widely, cause the application of metallic surface wetting property in association area thus.Therefore prepare super hydrophobic surface on the metal material more and more to be paid close attention to, people thirst for ultra-hydrophobicity to be applied to industrial production, especially on titanium alloy surface, prepare super-hydrophobic performance.Usual regulation, is greater than 90 ° by water droplet at the contact angle CA on surface and is called hydrophobic surface, when contact angle CA be greater than 150 °, the roll angle TA surface that is less than 10 ° is called super hydrophobic surface.
Ti6Al4V titanium alloy has that density is low, specific tenacity is high, solidity to corrosion is good, thermal conductivity is low, etc. characteristic, be a kind of light-high-strength corrosion resistance structure material, be widely used in machinery industry, medical industry, aerospace industry etc.As one of the primary structural material of aircraft, the application level of titanium alloy is one of important symbol weighing the advanced degree of aircraft selection, is the importance affecting aircraft tactical qualities.With laser technology processing Ti6Al4V titanium alloy surface, make Ti6Al4V titanium alloy surface form the super hydrophobic surface of frost resistance, very there is application prospect.
The wetting property of metallic substance is the very important feature in metallic surface, and the microtexture of material and moiety joint effect the wetting property of material surface.Prepare super-hydrophobic method on the metal material to have a lot, typical method has: anonizing, chemical medicinal liquid etch, electrochemical etching+chemical corrosion method, laser ablation+chemical corrosion method.Anonizing is exactly immerse in the middle of boiling water by porous oxidation alumina gel, then by distillation material and aluminium stone or silica mixing, in order to effectively obtain super hydrophobic surface, also need to carry out necessary modification with low-surface energy substance effects on surface, the efficiency of processing is not high.And additive method all be unable to do without the immersion of chemical medicinal liquid, by putting in chemical reagent by sample bubble, its surface is made to form pit shape microstructure.These methods are comparatively large to the pollution of environment, and operating procedure is complicated.Super hydrophobic surface is prepared on Ti6Al4V titanium alloy material; by a kind of without chemical medicinal liquid, pollution-free laser processing method simple to operate for use; the microstructure that material surface form height is consistent improves titanium alloy surface pattern; realize the requirement of material surface super-hydrophobic automatic cleaning, for raising the efficiency, energy-conservation, protection of the environment etc. is all significant.Application number is the preparation method that patent discloses a kind of aluminium alloy bionic super-hydrophobic surface of 201310079939.7, first with washes of absolute alcohol aluminium alloy, then laser processing is carried out in aluminum alloy surface, the cratering structure of countless microscale is processed at specimen surface, again sample is immersed in chemical etching solution, the shape characteristic of specimen surface is changed, but the method does not break through the process of surface treatment of traditional chemical etching completely, also chemical etching is make use of further after adopting laser processing technology, and the toluene solution that the aluminum alloy specimen after chemical etching is put into containing DTS is modified, the film of low surface energy is formed gradually on its surface, this complex treatment process, and employ high malicious carcinogenic substance toluene, easily cause environmental pollution.Application number is the preparation method that application discloses the super-hydrophobic micro-nano structure of a kind of titanium alloy surface of 201410788477.0, first carries out ultrasonic cleaning with acetone and raw spirit respectively to titanium alloy sample, obtains the titanium alloy sample of surface clean; Then femtosecond laser lithography process is carried out on the titanium alloy sample surface that effects on surface is clean, and a step obtains the titanium alloy sample with grating type or well type or the super-hydrophobic micro-nano structure surface of blind round hole type.Although utilize femto-second laser can process point-device microstructural surfaces, this simple method can not cover femto-second laser inherent defect, as price and costliness thereof, working (machining) efficiency is low, processing environment is harsh defect.Application number be 200910183588.8 patent discloses a kind of bionic metal ultra-wetting trans-scale structure design method and preparation method, the method is by complicated super hydrophilic Design Theory, pending sample is placed in high vacuum chamber, twice sweep is carried out respectively under different angles, final acquisition access expansion biological surface pattern across scale micro-structure, but the method strictly need control various process parameters, and processing cost is too high, be not suitable for industrialization scale operation completely.
In sum, develop a kind of technique simple, preparation efficiency is high, be applicable to commercial application, and do not produce any environmental pollution, disposablely realizing the super-hydrophobic frost resistance performance of metallic substrate surface and without the need to the method through any chemical technology process, is current researcher technical problem urgently to be resolved hurrily.
Summary of the invention
In order to overcome the deficiency that prior art exists, the object of the present invention is to provide a kind of technique simple, preparation efficiency is high, the titanium alloy super-hydrophobic surface preparation method of environmental protection.Method of the present invention can obtain steady in a long-term, contact angle in various size and difform titanium alloy material surface and be greater than 150 °, the roll angle super hydrophobic surface that is less than 10 °, and simultaneously obtained surface also has outstanding frost resistance performance.
Object of the present invention realizes particular by following technical proposals: a kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface, described method comprises the steps:
Step one, carries out polishing pre-treatment by pending titanium alloy surface, obtains the titanium alloy sample after surface finish;
Step 2, is placed on the titanium alloy sample after surface finish described in step one in the ultrasonic washing instrument filling deionized water and cleans, and after cleaning up, to be dried up by described titanium alloy sample surface cold wind or room temperature is dried naturally, obtains clean titanium alloy sample;
Step 3, utilizes laser processing technology, carries out laser scanning process, process countless micro-nano structures at sample surfaces after adopting ultrashort pulse laser to regulate relevant processing parameter to the cleaning titan alloy sample surface obtained described in step 2;
Described laser scanning adopts galvanometer system to carry out beam flying, and the speed of vibration mirror scanning is 0.1mm/s-30m/s, and the break-make of laser and the sweep limit of galvanometer system, track while scan and process velocity control and setting by computer program;
Or described laser scanning adopts polygon prism system to carry out beam flying, the speed of polygon prism scanning is 1m/s-800m/s, and the break-make of laser and the sweep limit of polygon prism system, track while scan and process velocity control and setting by computer program;
Or described laser scanning uses motion platform system to realize, and is fixed by light beam, sample relative beam moves, and the speed of Platform movement is 0.1mm/s-3m/s, and the break-make of laser, Platform movement track and speed control and setting by computer program;
Step 4, puts into fixed temperature and humidity electrically heated drying cabinet by the titanium alloy sample of the surface obtained described in step 3 after laser processing process and toasts, and namely obtains described titanium alloy super-hydrophobic frost resistance surface;
Wherein, the ultrashort pulse laser wavelength described in step 3 is less than 1550nm, and described laser processing parameter is: pulsewidth is greater than 10ps, and single pulse energy is less than 0.08mJ.
Further, the titanium alloy described in technique scheme is preferably Ti6Al4V titanium alloy.
Further, in technique scheme, the repetition rate of ultrashort pulse laser described in step 3 is 200kHz-1MHz, and described pulsewidth is 10ps-10ns.
Further preferably, the wavelength of described ultrashort pulse laser is 1064nm, and the pulsewidth of described ultrashort pulse laser is 80ps-10ns.
Further preferably, described pulsewidth is 80ps, and described single pulse energy is 7.5 μ J-8.5 μ J, and described laser scanning speed is 200mm/s-600mm/s.
Further preferably, described pulsewidth is 10ns, and described single pulse energy is 0.06mJ-0.07mJ, and described laser scanning speed is 1500mm/s-2000mm/s.
Again further preferably, the repetition rate of described ultrashort pulse laser is 200kHz, and described single pulse energy is 8.5 μ J, and described laser scanning speed is 400mm/s.
Further, pressure in electrically heated drying cabinet described in technique scheme step 4 is normal atmospheric pressure, and humidity is 40%-60%RH, and temperature is 100 DEG C-250 DEG C, the time of described sample baking is 2-8 hour, and the temperature error in described electrically heated drying cabinet is ± 1 DEG C.
Still more preferably, the humidity in described fixed temperature and humidity electrically heated drying cabinet is 50%RH, and temperature is 200 DEG C, and the time of baking is 6 hours.
Further, polishing pre-treatment in technique scheme described in step one adopts the pre-grinding test sample of gold phase machine that power is 370W, lap speed is 450 revs/min, lap diameter is 230mm, polishing preprocessing process needs that auxiliary diameter is 200mm, 1000 object SiC waterproof abrasive papers carry out polished finish at described titanium alloy surface, and polishing scope is 100cm
2, polishing time 10 minutes.
Further, in technique scheme, described in step 2, the ultrasonic frequency of ultrasonic cleaning instrument is 40kHz, and described deionized water resistivity is 18.25 megaohms, and titanium alloy sample surface should be flooded by described deionized water, at room temperature continuous wash 30 minutes.
The invention still further relates to a kind of titanium alloy super-hydrophobic frost resistance surface adopting aforesaid method to prepare, described surface has micron-sized papillary or splits striated structure or nano level pore space structure, overshooting shape structure.
Compared with prior art, the inventive method has the following advantages:
(1) the titanium alloy surface maximum contact angle utilizing the inventive method to prepare can reach 172.7 °, and minimum roll angle is 6.3 °, therefore has extraordinary ultra-hydrophobicity.
(2) preparation method's technique of the present invention is simple, easy to operate, efficiency is high, less energy consumption, cost is low, overcomes the defect that tradition uses chemical reagent etching titanium alloy surface or still need to adopt the further modification of surfaces of low-surface energy substance again after laser processing completes completely, environmental protection, do not adopt any chemical reagent coating, and the processing parameter of the inventive method easily controls, be easy to realize industrial application.
(3) the super-hydrophobic titanium alloy surface stable performance adopting the inventive method to prepare, possesses self-cleaning function and excellent frost resistance performance, considerably increases the use range of titanium alloy.
Accompanying drawing explanation
Fig. 1 (a), (b) are respectively contact angle schematic diagram, the roll angle schematic diagram on the titanium alloy super-hydrophobic frost resistance surface that the embodiment of the present invention 1 utilizes ultra-short pulse laser to prepare;
Fig. 2 (c), (d) are respectively contact angle schematic diagram, the roll angle schematic diagram on the titanium alloy super-hydrophobic frost resistance surface that the embodiment of the present invention 2 utilizes ultra-short pulse laser to prepare;
Fig. 3 (e), (f) are respectively contact angle schematic diagram, the roll angle schematic diagram on the titanium alloy super-hydrophobic frost resistance surface that the embodiment of the present invention 3 utilizes ultra-short pulse laser to prepare;
Fig. 4 (g), (h) are respectively contact angle schematic diagram, the roll angle schematic diagram on the titanium alloy super-hydrophobic frost resistance surface that the embodiment of the present invention 4 utilizes ultra-short pulse laser to prepare;
Fig. 5 is the scanning electron microscope (SEM) photograph on the titanium alloy super-hydrophobic frost resistance surface that the embodiment of the present invention 1 utilizes ultra-short pulse laser to prepare;
Fig. 6 is the scanning electron microscope (SEM) photograph on the titanium alloy super-hydrophobic frost resistance surface that the embodiment of the present invention 2 utilizes ultra-short pulse laser to prepare;
Fig. 7 is the scanning electron microscope (SEM) photograph on the titanium alloy super-hydrophobic frost resistance surface that the embodiment of the present invention 3 utilizes ultra-short pulse laser to prepare;
Fig. 8 is the scanning electron microscope (SEM) photograph on the titanium alloy super-hydrophobic frost resistance surface that the embodiment of the present invention 4 utilizes ultra-short pulse laser to prepare.
Fig. 9 (a), (b) are respectively common alloy of titanium surface and the white growing state figure of super-hydrophobic frost resistance titanium alloy surface under-5 DEG C of conditions after 20min that prepare of the embodiment of the present invention 1, wherein: room temperature is 23 DEG C, relative humidity is 50%.
Figure 10 (a), (b) are respectively common alloy of titanium surface and the white growing state figure of super-hydrophobic frost resistance titanium alloy surface under-5 DEG C of conditions after 20min that prepare of the embodiment of the present invention 2, wherein: room temperature is 23 DEG C, relative humidity is 50%.
Figure 11 (a), (b) are respectively common alloy of titanium surface and the white growing state figure of super-hydrophobic frost resistance titanium alloy surface under-5 DEG C of conditions after 20min that prepare of the embodiment of the present invention 3, wherein: room temperature is 23 DEG C, relative humidity is 50%.
Figure 12 (a), (b) are respectively common alloy of titanium surface and the white growing state figure of super-hydrophobic frost resistance titanium alloy surface under-5 DEG C of conditions after 20min that prepare of the embodiment of the present invention 4, wherein: room temperature is 23 DEG C, relative humidity is 50%.
Embodiment
For a better understanding of the present invention, below in conjunction with specific embodiment, technical scheme of the present invention is described in further detail.
The experimental technique used in following embodiment if no special instructions, is ordinary method.
A kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface of the present invention, with reference to nature biotechnology material as design basis, Ti6Al4V titanium alloy surface imitates the constitutional features of nature biotechnology matrix material fine structure distribution, design surface structure.
Embodiment 1
A kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface of the present embodiment, comprises following concrete steps:
Step one, by the polishing of Ti6Al4V titanium alloy, power is selected to be 370W, lap speed is 450 revs/min, lap diameter is the pre-grinding test sample of gold phase machine of 230mm, polishing process needs that auxiliary diameter is 200mm, 1000 object SiC waterproof abrasive papers carry out polished finish at described titanium alloy surface, and polishing scope is 100cm
2, polishing time 10 minutes, obtains the titanium alloy sample after surface finish;
Step 2, titanium alloy sample ultrasonic washing instrument after surface finish described in step one is cleaned, ultrasonic washing instrument ultrasonic frequency is 40kHz, sample surfaces is flooded with the deionized water that resistivity is 18.25 megaohms, at room temperature, continuous wash 30 minutes, after cleaning up, room temperature is dried naturally, obtains clean titanium alloy sample;
Step 3, adopt ultrashort pulse laser, laser wavelength is 1064nm, carries out laser scanning manufacturing, process countless microstructures at sample surfaces to the cleaning titan alloy sample surface obtained described in step 2, described laser apparatus pulsewidth is 80ps, and single pulse energy is 8.5 μ J, and repetition rate is 200kHz, and described laser scanning utilizes X-Y scanning galvanometer system, makes laser beam with the speed of 400mm/s titanium alloy sample surface described in ablation line by line, described galvanometer system is by X-Y optical scanning head, electric drive amplifier, optical reflecting lens and field lens composition, the sweep limit of described galvanometer system and speed, line sweep and Surface scan path are undertaken controlling and setting by computer, the signal that described computer provides is by drive amplification circuit drives optical scanning head, thus the deflection of laser beam is controlled at X-Y plane, sample moves in the x-direction relative to laser beam, by controlling translational speed and laser pulse repetition frequency, its pulse matching degree is made to reach 1%-99%, complete after moving, single step stepping in the y-direction again, by control step distance, its light beam overlap ratio is made to reach 1%-99% in y direction, worktable reverses, described sample work range is 126mm x 126mm,
Step 4, the sample after processing, after step 3 laser processing, is put in electrically heated drying cabinet and is toasted by sample, air pressure be normal atmospheric pressure, humidity is 50%RH, and temperature is that under 200 DEG C of conditions, constant temperature toasts 6 hours, obtains described titanium alloy super-hydrophobic frost resistance surface.
Employing resistivity is the deionized water of 18.25 megaohms, utilize the contact angle on the titanium alloy super-hydrophobic frost resistance surface obtained described in the test of optical contact angle surface interfacial tension survey meter, roll angle: adopt the method that accesses to measure, volume required suspension drop is formed under liquid feeding syringe needle, the Z axis of example platform is regulated to make sample surfaces increase, when sample surfaces is with when contacting bottom the drop hung under liquid feeding syringe needle, drop just transfers to sample surfaces from liquid feeding syringe needle, and then measure by regulating sample table Z axis to make sample surfaces drop to original position, because the titanium alloy surface ultra-hydrophobicity prepared is excellent, the water droplet of 3-8 microlitre cannot adhere to, so drop volume is 9 microlitres, probe temperature is 25.5 DEG C, humidity is 19.5%RH.
Titanium alloy super-hydrophobic frost resistance that the present embodiment prepares surface, its stereoscan photograph as shown in Figure 5, the nano level hole of its surface presentation and overshooting shape structure.
The titanium alloy super-hydrophobic frost resistance surface that the present embodiment prepares and the contact angle schematic diagram of water are as shown in Fig. 1 (a), and roll angle schematic diagram is as shown in Fig. 1 (b).
The titanium alloy super-hydrophobic frost resistance surface that the present embodiment prepares is 172.7 ° with the contact angle of water, and roll angle is 6.3 °, and test result is in table 1.
In addition, be 23 DEG C in room temperature, when relative humidity is 50%, the super-hydrophobic frost resistance titanium alloy undressed common alloy of titanium and the present embodiment prepared is placed on the refrigeration platform of-5 DEG C respectively, observe the frost situation of each titanium alloy surface after 20min, white growing state as shown in Figure 9.As shown in Figure 9, after 20min, undressed titanium alloy surface is obviously covered by ice sheet, and the titanium alloy surface that the present embodiment prepares only has regional area to occur tiny ice crystal, and the titanium alloy surface obtained by visible the present embodiment has good frost resistance performance.
Embodiment 2
A kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface of the present embodiment, comprises following concrete steps:
Step one, by the polishing of Ti6Al4V titanium alloy, power is selected to be 370W, lap speed is 450 revs/min, lap diameter is the pre-grinding test sample of gold phase machine of 230mm, polishing process needs that auxiliary diameter is 200mm, 1000 object SiC waterproof abrasive papers carry out polished finish at described titanium alloy surface, and polishing scope is 100cm
2, polishing time 10 minutes, obtains the titanium alloy sample after surface finish;
Step 2, titanium alloy sample ultrasonic washing instrument after surface finish described in step one is cleaned, ultrasonic washing instrument ultrasonic frequency is 40kHz, sample surfaces is flooded with the deionized water that resistivity is 18.25 megaohms, at room temperature, continuous wash 30 minutes, after cleaning up, dry up with cold wind, obtain clean titanium alloy sample;
Step 3, adopt ultrashort pulse laser, laser wavelength is 1064nm, laser scanning manufacturing is carried out to the cleaning titan alloy sample surface obtained described in step 2, countless microstructures is processed at sample surfaces, described laser apparatus pulsewidth is 80ps, single pulse energy is 7.5 μ J, repetition rate is 200kHz, described laser scanning routing motion workplatform, the cleaning titan alloy sample obtained described in step 2 is fixed on motion workplatform, utilize lens by laser beam focusing on to the sample, make the surface of sample relative to the focusing etching hot spot of described ultrafast laser light beam along x, y, z three-dimensional direction moving, speed is 400mm/s, by titanium alloy sample described in ablation is surperficial line by line, realize the etching of micro-nano structure, described motion platform unit is three-dimensional servo precision mobile platform, and the scope of described platform movement, speed, direction, can along X, Y, Z three-dimensional direction movings by computer control, and sample work range is 150mm x 150mm,
Step 4, the sample after processing, after step 3 laser processing, is put in electrically heated drying cabinet and is toasted by sample, air pressure be normal atmospheric pressure, humidity is 52%RH, and temperature is that under 250 DEG C of conditions, constant temperature toasts 2 hours, obtains described titanium alloy super-hydrophobic frost resistance surface.
Adopt contact angle, the roll angle on the titanium alloy super-hydrophobic frost resistance surface obtained described in the test of above-described embodiment 1 identical testing method.
Titanium alloy super-hydrophobic frost resistance that the present embodiment prepares surface, its stereoscan photograph as shown in Figure 6, the nano level hole of its surface presentation and overshooting shape structure.
The titanium alloy super-hydrophobic frost resistance surface that the present embodiment prepares and the contact angle schematic diagram of water are as shown in Fig. 2 (c), and roll angle schematic diagram is as shown in Fig. 2 (d).
The titanium alloy super-hydrophobic frost resistance surface that the present embodiment prepares is 170.2 ° with the contact angle of water, and roll angle is 9.8 °, and test result is in table 1.
In addition, adopt the identical testing method of above-described embodiment 1 and test condition to test the frost resistance situation of the super-hydrophobic frost resistance titanium alloy that undressed common alloy of titanium and the present embodiment prepare, white growing state as shown in Figure 10.As shown in Figure 10, after 20min, undressed titanium alloy surface is obviously covered by ice sheet, and the titanium alloy surface that the present embodiment prepares only has regional area to occur tiny ice crystal, and the titanium alloy surface obtained by visible the present embodiment has good frost resistance performance.
Embodiment 3
A kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface of the present embodiment, comprises following concrete steps:
Step one, by the polishing of Ti6Al4V titanium alloy, power is selected to be 370W, lap speed is 450 revs/min, lap diameter is the pre-grinding test sample of gold phase machine of 230mm, polishing process needs that auxiliary diameter is 200mm, 1000 object SiC waterproof abrasive papers carry out polished finish at described titanium alloy surface, and polishing scope is 100cm
2, polishing time 10 minutes, obtains the titanium alloy sample after surface finish;
Step 2, titanium alloy sample ultrasonic washing instrument after surface finish described in step one is cleaned, ultrasonic washing instrument ultrasonic frequency is 40kHz, sample surfaces is flooded with the deionized water that resistivity is 18.25 megaohms, at room temperature, continuous wash 30 minutes, after cleaning up, room temperature is dried naturally, obtains clean titanium alloy sample;
Step 3, adopt ultrashort pulse laser, laser wavelength is 1064nm, carry out laser scanning manufacturing to the cleaning titan alloy sample surface obtained described in step 2, process countless microstructures at sample surfaces, the pulsewidth of described laser apparatus is 10ns, single pulse energy is 0.07mJ, repetition rate is 900kHz, and described laser scanning utilizes X-Y scanning galvanometer system, makes laser beam with the speed of 1800mm/s titanium alloy sample surface described in ablation line by line, described galvanometer system is by X-Y optical scanning head, electric drive amplifier, optical reflecting lens and field lens composition, the sweep limit of described galvanometer system and speed, line sweep and Surface scan path are undertaken controlling and setting by computer, the signal that described computer provides is by drive amplification circuit drives optical scanning head, thus the deflection of laser beam is controlled at X-Y plane, sample moves in the x-direction relative to laser beam, by controlling translational speed and laser pulse repetition frequency, its pulse matching degree is made to reach 1%-99%, complete after moving, single step stepping in the y-direction again, by control step distance, its light beam overlap ratio is made to reach 1%-99% in y direction, worktable reverses, described sample work range is 126mm x 126mm,
Step 4, the sample after processing, after step 3 laser processing, is put in electrically heated drying cabinet and is toasted by sample, air pressure be normal atmospheric pressure, humidity is 59%RH, and temperature is that under 100 DEG C of conditions, constant temperature toasts 8 hours, obtains described titanium alloy super-hydrophobic frost resistance surface.
Adopt contact angle, the roll angle on the titanium alloy super-hydrophobic frost resistance surface obtained described in the test of above-described embodiment 1 identical testing method.
Titanium alloy super-hydrophobic frost resistance that the present embodiment prepares surface, its stereoscan photograph as shown in Figure 7, the micron-sized papillary structure of its surface presentation.
The titanium alloy super-hydrophobic frost resistance surface that the present embodiment prepares and the contact angle schematic diagram of water are as shown in Fig. 3 (e), and roll angle schematic diagram is as shown in Fig. 3 (f).
The titanium alloy super-hydrophobic frost resistance surface that the present embodiment prepares is 158.1 ° with the contact angle of water, and roll angle is 7.3 °, and test result is in table 1.
In addition, adopt the identical testing method of above-described embodiment 1 and test condition to test the frost resistance situation of the super-hydrophobic frost resistance titanium alloy that undressed common alloy of titanium and the present embodiment prepare, white growing state as shown in figure 11.As shown in Figure 11, after 20min, undressed titanium alloy surface is obviously covered by ice sheet, and the titanium alloy surface that the present embodiment prepares only has regional area to occur tiny ice crystal, and the titanium alloy surface obtained by visible the present embodiment has good frost resistance performance.
Embodiment 4
A kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface of the present embodiment, comprises following concrete steps:
Step one, by the polishing of Ti6Al4V titanium alloy, polishing selects power to be 370W, lap speed is 450 revs/min, lap diameter is the pre-grinding test sample of gold phase machine of 230mm, polishing process needs that auxiliary diameter is 200mm, 1000 object SiC waterproof abrasive papers carry out polished finish at described titanium alloy surface, and polishing scope is 100cm
2, polishing time 10 minutes, obtains the titanium alloy sample after surface finish;
Step 2, titanium alloy sample ultrasonic washing instrument after surface finish described in step one is cleaned, ultrasonic washing instrument ultrasonic frequency is 40kHz, sample surfaces is flooded with the deionized water that resistivity is 18.25 megaohms, at room temperature, continuous wash 30 minutes, after cleaning up, room temperature is dried naturally, obtains clean titanium alloy sample;
Step 3, adopt ultrashort pulse laser, laser wavelength is 1064nm, carries out laser processing, process countless microstructures at sample surfaces to the cleaning titan alloy sample surface obtained described in step 2, the pulsewidth of described laser apparatus is 10ns, single pulse energy is 0.06mJ, and repetition rate is 900kHz, and described laser scanning utilizes polygon prism system, make laser beam with the speed of 1800mm/s titanium alloy sample surface described in ablation line by line, sample work range is 100cm
2; Described polygon prism system is made up of the polygonal prism of high speed rotating, electric drive amplifier and field lens, the line sweep scope of described polygon prism system and speed are undertaken controlling and setting by computer controller, the signal that described computer controller provides is by described drive amplification circuit drives polygon prism, upwards laser-beam deflection can be realized at one-dimensional square, combine with motion platform simultaneously, realize the movement of other direction; Wherein titanium alloy sample moves in the x-direction relative to laser beam, by controlling translational speed and laser pulse repetition frequency, its pulse matching degree is made to reach 1%-99%, complete after moving, single step stepping in the y-direction again, by control step distance, its light beam overlap ratio is made to reach 1%-99% in y direction;
Step 4, the sample after processing, after step 3 laser processing, is put in electrically heated drying cabinet and is toasted by sample, air pressure be normal atmospheric pressure, humidity is 48%RH, and temperature is that under 200 DEG C of conditions, constant temperature toasts 4 hours, obtains described titanium alloy super-hydrophobic frost resistance surface.
Adopt contact angle, the roll angle on the titanium alloy super-hydrophobic frost resistance surface obtained described in the test of above-described embodiment 1 identical testing method.
The titanium alloy super-hydrophobic frost resistance surface that the present embodiment prepares, its stereoscan photograph as shown in Figure 8.Its surface presentation is micron-sized splits striated structure.
The titanium alloy super-hydrophobic frost resistance surface that the present embodiment prepares and the contact angle schematic diagram of water are as shown in Fig. 4 (g), and roll angle schematic diagram is as shown in Fig. 4 (h).
The titanium alloy super-hydrophobic frost resistance surface that the present embodiment prepares is 159.6 ° with the contact angle of water, and roll angle is 8.4 °, and test result is in table 1.
In addition, adopt the identical testing method of above-described embodiment 1 and test condition to test the frost resistance situation of the super-hydrophobic frost resistance titanium alloy that undressed common alloy of titanium and the present embodiment prepare, white growing state as shown in figure 12.As shown in Figure 12, after 20min, undressed titanium alloy surface is obviously covered by ice sheet, and the titanium alloy surface that the present embodiment prepares only has regional area to occur tiny ice crystal, and the titanium alloy surface obtained by visible the present embodiment has good frost resistance performance.
The contact angle on titanium alloy super-hydrophobic frost resistance surface that table 1 prepares for various embodiments of the present invention, the test result of roll angle.
Table 1
| Embodiment | Contact angle/° | Roll angle/° |
| Embodiment 1 | 172.7 | 6.3 |
| Embodiment 2 | 170.2 | 9.8 |
| Embodiment 3 | 158.1 | 7.3 |
| Embodiment 4 | 159.6 | 8.4 |
The above embodiment of the present invention is only used to clearly demonstrate the citing that the present invention does, and is not the restriction to embodiments of the present invention.Every any amendment of doing in the present invention's spirit and principle, equivalent replacement and improvement etc., within the protection domain that all should be included in the claims in the present invention.
Claims (10)
1. utilize ultra-short pulse laser to prepare the method on titanium alloy super-hydrophobic frost resistance surface, it is characterized in that: described method comprises the steps:
Step one, carries out polishing pre-treatment by pending titanium alloy surface, obtains the titanium alloy sample after surface finish;
Step 2, is placed on the titanium alloy sample after surface finish described in step one in the ultrasonic washing instrument filling deionized water and cleans, and after cleaning up, to be dried up by described titanium alloy sample surface cold wind or room temperature is dried naturally, obtains clean titanium alloy sample;
Step 3, utilizes laser processing technology, carries out laser scanning process, process countless micro-nano structures at sample surfaces after adopting ultrashort pulse laser to regulate relevant processing parameter to the cleaning titan alloy sample surface obtained described in step 2;
Described laser scanning adopts galvanometer system to carry out beam flying, and the speed of vibration mirror scanning is 0.1mm/s-30m/s, and the break-make of laser and the sweep limit of galvanometer system, track while scan and process velocity control and setting by computer program;
Or described laser scanning adopts polygon prism system to carry out beam flying, the speed of polygon prism scanning is 1m/s-800m/s, and the break-make of laser and the sweep limit of polygon prism system, track while scan and process velocity control and setting by computer program;
Or described laser scanning uses motion platform system to realize, and is fixed by light beam, sample relative beam moves, and the speed of Platform movement is 0.1mm/s-3m/s, and the break-make of laser, Platform movement track and speed control and setting by computer program;
Step 4, puts into fixed temperature and humidity electrically heated drying cabinet by the titanium alloy sample of the surface obtained described in step 3 after laser processing process and toasts, and namely obtains described titanium alloy super-hydrophobic frost resistance surface;
Wherein, the ultrashort pulse laser wavelength described in step 3 is less than 1550nm, and described laser processing parameter is: pulsewidth is greater than 10ps, and single pulse energy is less than 0.08mJ.
2. a kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface as claimed in claim 1, is characterized in that: described titanium alloy is Ti6Al4V titanium alloy.
3. a kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface as claimed in claim 1 or 2, is characterized in that: the repetition rate of ultrashort pulse laser described in step 3 is 200kHz-1MHz, and described pulsewidth is 10ps-10ns.
4. a kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface as claimed in claim 3, is characterized in that: the pulsewidth of described ultrashort pulse laser is 80ps-10ns.
5. a kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface as claimed in claim 4, it is characterized in that: the wavelength of described ultrashort pulse laser is 1064nm, described pulsewidth is 80ps, described single pulse energy is 7.5 μ J-8.5 μ J, and described laser scanning speed is 200mm/s-600mm/s.
6. a kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface as claimed in claim 4, it is characterized in that: the wavelength of described ultrashort pulse laser is 1064nm, described pulsewidth is 10ns, described single pulse energy is 0.06mJ-0.07mJ, and described laser scanning speed is 1500mm/s-2000mm/s.
7. a kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface as claimed in claim 5, it is characterized in that: the repetition rate of described ultrashort pulse laser is 200kHz, described single pulse energy is 8.5 μ J, and described laser scanning speed is 400mm/s.
8. a kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface as claimed in claim 1, it is characterized in that: the pressure in electrically heated drying cabinet described in step 4 is normal atmospheric pressure, humidity is 40%-60%RH, temperature is 100 DEG C-250 DEG C, the time of described sample baking is 2-8 hour, and the temperature error in described electrically heated drying cabinet is ± 1 DEG C.
9. a kind of method utilizing ultra-short pulse laser to prepare titanium alloy super-hydrophobic frost resistance surface as claimed in claim 8, it is characterized in that: the humidity in described fixed temperature and humidity electrically heated drying cabinet is 50%RH, temperature is 200 DEG C, and the time of baking is 6 hours.
10. the titanium alloy super-hydrophobic frost resistance surface adopting the method described in any one of claim 1-9 to prepare, described surface has micron-sized papillary or splits striated structure or nano level pore space structure, overshooting shape structure.
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Cited By (4)
| 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 |
| CN108356409A (en) * | 2018-01-26 | 2018-08-03 | 合肥工业大学 | A kind of underwater bubble tuning titanium sheet and its processing method and application method |
| CN109676245A (en) * | 2018-09-30 | 2019-04-26 | 湖北工业大学 | A method of super hydrophilic glass surface is prepared using pulse laser |
| CN113210872A (en) * | 2021-05-24 | 2021-08-06 | 西南交通大学 | Method for rapidly preparing titanium alloy bionic super-hydrophobic surface by femtosecond laser |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101219506A (en) * | 2008-01-07 | 2008-07-16 | 江苏大学 | Laser production method for metal base ultra-hydrophobicity micro-structure surface |
| US7470335B2 (en) * | 2000-06-09 | 2008-12-30 | Lsp Technologies, Inc. | Method of modifying a workpiece following laser shock processing |
| CN101844272A (en) * | 2010-01-27 | 2010-09-29 | 长春理工大学 | Method and system for manufacturing self-cleaning surface structure by adopting laser interference photoetching technology |
| CN103627883A (en) * | 2013-11-07 | 2014-03-12 | 清华大学 | Method of regulating and controlling light absorption property of metal surface by picosecond pulse laser |
-
2015
- 2015-05-28 CN CN201510281693.0A patent/CN104911519B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7470335B2 (en) * | 2000-06-09 | 2008-12-30 | Lsp Technologies, Inc. | Method of modifying a workpiece following laser shock processing |
| CN101219506A (en) * | 2008-01-07 | 2008-07-16 | 江苏大学 | Laser production method for metal base ultra-hydrophobicity micro-structure surface |
| CN101844272A (en) * | 2010-01-27 | 2010-09-29 | 长春理工大学 | Method and system for manufacturing self-cleaning surface structure by adopting laser interference photoetching technology |
| CN103627883A (en) * | 2013-11-07 | 2014-03-12 | 清华大学 | Method of regulating and controlling light absorption property of metal surface by picosecond pulse laser |
Cited By (5)
| 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 |
| CN108356409A (en) * | 2018-01-26 | 2018-08-03 | 合肥工业大学 | A kind of underwater bubble tuning titanium sheet and its processing method and application method |
| CN109676245A (en) * | 2018-09-30 | 2019-04-26 | 湖北工业大学 | A method of super hydrophilic glass surface is prepared using pulse laser |
| CN113210872A (en) * | 2021-05-24 | 2021-08-06 | 西南交通大学 | Method for rapidly preparing titanium alloy bionic super-hydrophobic surface by femtosecond laser |
| CN113210872B (en) * | 2021-05-24 | 2022-07-12 | 西南交通大学 | Method for rapidly preparing titanium alloy bionic super-hydrophobic surface by femtosecond laser |
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