CN104907697B - A kind of method that utilization ultrafast laser prepares titanium alloy super-hydrophobic frost resistance surface - Google Patents
A kind of method that utilization ultrafast laser prepares titanium alloy super-hydrophobic frost resistance surface Download PDFInfo
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- CN104907697B CN104907697B CN201510279894.7A CN201510279894A CN104907697B CN 104907697 B CN104907697 B CN 104907697B CN 201510279894 A CN201510279894 A CN 201510279894A CN 104907697 B CN104907697 B CN 104907697B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/352—Working by laser beam, e.g. welding, cutting or boring for surface treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/08—Non-ferrous metals or alloys
- B23K2103/14—Titanium or alloys thereof
Abstract
The present invention relates to a kind of method that utilization ultrafast laser prepares titanium alloy super-hydrophobic frost resistance surface, belong to metallic substrate surface technical field of modification.Titanium alloy sample is polished pretreatment by this method first, then deionized water cleaning sample surface in ultrasonic washing instrument is utilized, after cleaning up, cold wind is dried up or dried, recycle laser processing technology, sample is surface-treated after regulating the technological parameter of correlation using ultrafast laser, countless micro-structurals are processed in sample surfaces, after machining, sample after processing is put into electrically heated drying cabinet and toasted, obtain the titanium alloy super-hydrophobic frost resistance surface, the surface has nano level papillary structure or gully shape structure, the surface possesses excellent ultra-hydrophobicity, also there is outstanding resistancet of rost energy simultaneously.The preparation method technique of the present invention is simple, and easy to operate, efficiency high, less energy consumption, cost is low, environmental protection, it is easy to accomplish commercial Application.
Description
Technical field：
The invention belongs to metallic substrate surface technical field of modification, it is related to super-hydrophobic frost resistance surface on titanium alloy substrate
Preparation method, it is more particularly related to which a kind of utilization ultrafast laser prepares the side on titanium alloy super-hydrophobic frost resistance surface
Method.
Background technology：
Animals and plants in nature pass through the selection and evolution of 1 years, possess its unique life style, it is super-hydrophobic from
Clean surface is exactly one of which：Small and weak insect body surface, due to possessing super hydrophobic functional, can fly in the rain
OK；, can almost non-resistance be creeped on the water surface due to super-hydrophobic micro-nano structure on the pin of water spider；Lotus leaf table
The super-drainage structure in face substantially increases its self-cleaning function；The petal surface of the plants such as rose just has what is protruded very much to surpass
Hydrophobicity, these performances are lost in material antiseptic, it is anti-oxidant in terms of have application prospect widely, thus cause metal watch
Application of the face wellability in association area.Therefore super hydrophobic surface is prepared on the metal material to get growing concern for,
People thirst for super-hydrophobicity can apply to industrial production, and super-hydrophobic performance is especially prepared in titanium alloy surface.Generally
Regulation, by water droplet surface contact angle CA be more than 90 ° be referred to as hydrophobic surfaces, when contact angle CA be more than 150 °, roll angle TA it is small
It is referred to as super hydrophobic surface in 10 ° of surface.
Ti6Al4V titanium alloys have that density is low, specific strength is high, corrosion resistance good, the low characteristic of thermal conductivity, are that a kind of lightweight is high
Intensity corrosion resistance structure material, is widely used in machinery industry, medical industry, Aero-Space industry etc..It is used as the master of aircraft
One of structural material is wanted, the application level of titanium alloy is to weigh one of important symbol of the advanced degree of aircraft selection, be that influence flies
One importance of machine tactical qualities.Ti6Al4V titanium alloy surfaces are processed with laser technology, make Ti6Al4V titanium alloy surfaces
The super hydrophobic surface of automatically cleaning frost resistance is formed, very with application prospect.
The wellability of metal material is a critically important feature of metal surface, the microstructure and constituent of material
Joint effect the wellability of material surface.Preparing super-hydrophobic method on the metal material has a lot, and typical method has：
Anodizing, chemical medicinal liquid etch, electrochemical etching+chemical corrosion method, laser ablation+chemical corrosion method.Anodic oxidation
Method is exactly to immerse porous oxidation alumina gel among boiling water, is then mixed the material of distillation and aluminium stone or silica, in order to have
Effect ground obtains super hydrophobic surface, in addition it is also necessary to necessary modification is carried out to surface with low-surface energy substance, the efficiency of processing is not high.
And other method all be unable to do without the immersion of chemical medicinal liquid, by the way that sample bubble is put in chemical reagent, its surface is set to form pit
Shape micro-structural.Pollution of these methods to environment is larger, and operating procedure is complicated.For being prepared on Ti6Al4V titanium alloy materials
Go out super hydrophobic surface, using it is a kind of without chemical medicinal liquid, pollution-free laser processing method simple to operate, material surface form height
In consistent micro-structural improve titanium alloy surface pattern, realize the requirement of material surface super-hydrophobic automatic cleaning, for improve efficiency,
Energy-conservation, environmental protection etc. are all significant.The patent of Application No. 201310079939.7 discloses a kind of aluminium alloy and imitated
The preparation method of raw super hydrophobic surface, first with washes of absolute alcohol aluminium alloy, is then laser machined in aluminum alloy surface,
The cratering structure of countless minute yardsticks is processed in specimen surface, then sample is immersed in chemical etching solution, makes specimen surface
Shape characteristic change, but this method completely break through traditional chemical etching process of surface treatment, using Laser Processing
Chemical etching is also further make use of after technique, and the aluminum alloy specimen after chemical etching is put into the toluene containing DTS
Modified in solution, the film of low-surface-energy is gradually formed on its surface, the complex treatment process, and used high poison carcinogenic
Material toluene, easily causes environmental pollution.The patent of Application No. 201410657627.4 discloses a kind of ultra-hydrophobic high sticking
Metal surface and preparation method thereof, class rose surface microscopic knot is prepared by high power psec or femtosecond laser in metal surface
The periodicity micro nano structure of structure, then by the surface modification of low free energy material, realize ultra-hydrophobic high sticking metal surface
Preparation, this method carries out necessary modification using low-surface energy substance to surface, and processing efficiency is low；Application No.
200910183588.8 patent disclose a kind of bionic metal ultra-wetting trans-scale structure design method and preparation method, the party
Pending sample is placed in high vacuum chamber by complicated super hydrophilic Theoretical Design, carries out two under different angles respectively by method
Secondary scanning, it is final obtain access expansion biological surface pattern across scale micro-structure, but this method need to strictly control every work
Skill parameter, processing cost is too high, is completely unsuitable for industrialization large-scale production.
In summary, a kind of technique is developed simple, preparation efficiency is high, it is adaptable to commercial application, and does not produce any
Environmental pollution, disposably realizes that the super-hydrophobic resistancet of rost of metallic substrate surface can be without the side by the processing of any chemical technology
Method, is current researcher technical problem urgently to be resolved hurrily.
The content of the invention
It is simple it is an object of the invention to provide a kind of technique in order to overcome the shortcomings of that prior art is present, preparation efficiency
The high, preparation method on the titanium alloy super-hydrophobic frost resistance surface of environmental protection.The method of the present invention can be in various sizes and difference
The titanium alloy material surface of shape obtain steady in a long-term, contact angle be more than 150 °, roll angle be less than 10 ° of super hydrophobic surface,
Obtained surface also has outstanding resistancet of rost energy simultaneously.
The purpose of the present invention is realized particular by following technical proposals：One kind prepares titanium alloy using ultrafast laser and surpassed
The method on hydrophobic frost resistance surface, methods described comprises the following steps：
Step one, pending titanium alloy surface is polished pretreatment, obtains the titanium alloy sample after the polishing of surface；
Step 2, the titanium alloy sample after surface polishing described in step one is placed on the ultrasonic wave cleaning for filling deionized water
Cleaned in instrument, after cleaning up, the drying of titanium alloy sample surface cold wind or room temperature are dried naturally, the titanium of cleaning is obtained
Alloy sample；
Step 3, using laser processing technology, is regulated after the technological parameter of correlation to step 2 using ultrafast laser
The obtained clean titanium alloy sample surface carries out laser scanning processing, and countless micro-structurals are processed in sample surfaces；
The laser scanning carries out light beam scanning using galvanometer system, and the speed of vibration mirror scanning is 0.1mm/s-30m/s, is swashed
The break-make of light and the scanning range of galvanometer system, scanning track and process velocity are by computer program control and setting；
Or the laser scanning is realized using motion platform system, and light beam is fixed, the motion of sample relative beam, platform fortune
Dynamic speed is 0.1mm/s-3m/s, and break-make, platform movement locus and the speed of laser are by computer program control and setting；
Step 4, is put into constant temperature permanent by titanium alloy sample of the surface obtained described in step 3 after Laser Processing is handled
Toasted in wet electrically heated drying cabinet, that is, obtain the titanium alloy super-hydrophobic frost resistance surface；
Wherein, the ultrafast laser wavelength described in step 3 is less than 1000nm, and the laser processing parameter is：Pulsewidth is more than
30fs, single pulse energy is less than 0.1mJ.
Further, the titanium alloy described in above-mentioned technical proposal is preferably Ti6Al4V titanium alloys.
Further, the repetition rate of ultrafast laser described in step 3 is 10kHz-200kHz in above-mentioned technical proposal,
The pulsewidth is 30fs-10ps.
It is further preferred that the pulsewidth of the ultrafast laser is 80fs-800fs.
It is further preferred that the wavelength of the ultrafast laser is 800nm, the pulsewidth of the ultrafast laser is 90fs-
550fs。
It is further preferred that the pulsewidth is 90fs, the single pulse energy is 50 μ J-66 μ J, the laser scanning
Speed is 20mm/s-60mm/s.
It is further preferred that the pulsewidth is 550fs, the single pulse energy is 50 μ J-66 μ J, the laser scanning
Speed is 20mm/s-60mm/s.
Further, the pressure described in above-mentioned technical proposal step 4 in electrically heated drying cabinet is normal atmospheric pressure, humidity
It it is 100 DEG C -250 DEG C for 40%-60%RH, temperature, the time of the sample baking is in 2-8 hours, the electrically heated drying cabinet
Temperature error be ± 1 DEG C.
It is further preferred that the humidity in the constant temperature and humidity electrically heated drying cabinet is 50%RH, temperature is 200 DEG C, is dried
The roasting time is 6 hours.
Further, the polishing pretreatment in above-mentioned technical proposal described in step one uses power to turn for 370W, abrasive disk
The pre-grinding test sample of gold phase machine that speed is 450 revs/min, lap diameter is 230mm, polishing preprocessing process needs auxiliary a diameter of
200mm, the SiC waterproof abrasive papers of 1000 mesh, polishing scope is 100cm2, polishing time 10 minutes.
Further, in above-mentioned technical proposal described in step 2 be cleaned by ultrasonic instrument supersonic frequency be 40kHz, it is described go from
Sub- water resistance rate is 18.25 megaohms, and the deionized water should flood titanium alloy sample surface, at room temperature 30 points of continuous wash
Clock.
The invention further relates to the titanium alloy super-hydrophobic frost resistance surface that a kind of use above method is prepared, the surface
With nano level papillary structure or gully shape structure.
Compared with prior art, the inventive method has advantages below：
(1) the titanium alloy surface Maximum Contact angle prepared using the inventive method is up to 170.5 °, minimum roll angle
For 3.8 °, therefore with extraordinary ultra-hydrophobicity.
(2) preparation method technique of the invention is simple, and easy to operate, efficiency high, less energy consumption, cost is low, overcomes completely
Tradition etches titanium alloy surface using chemical reagent or still needs to enter one using low-surface energy substance again after the completion of Laser Processing
The defect of modification of surfaces is walked, environmental protection does not use any chemical reagent coating, and the technological parameter of the inventive method is easily controlled
System, it is easy to accomplish commercial Application.
(3) the super-hydrophobic titanium alloy metal surface performance stabilization prepared using the inventive method, possesses self-cleaning
Function and excellent resistancet of rost energy, considerably increase the use scope of titanium alloy.
Brief description of the drawings
Fig. 1 (a), (b) are respectively the titanium alloy super-hydrophobic frost resistance that the embodiment of the present invention 1 is prepared using ultrafast laser
Contact angle schematic diagram, the roll angle schematic diagram on surface；
Fig. 2 (c), (d) are respectively the titanium alloy super-hydrophobic frost resistance that the embodiment of the present invention 2 is prepared using ultrafast laser
Contact angle schematic diagram, the roll angle schematic diagram on surface；
Fig. 3 (e), (f) are respectively the titanium alloy super-hydrophobic frost resistance that the embodiment of the present invention 3 is prepared using ultrafast laser
Contact angle schematic diagram, the roll angle schematic diagram on surface；
Fig. 4 (g), (h) are respectively the titanium alloy super-hydrophobic frost resistance that the embodiment of the present invention 4 is prepared using ultrafast laser
Contact angle schematic diagram, the roll angle schematic diagram on surface；
Fig. 5 is the scanning on the titanium alloy super-hydrophobic frost resistance surface that the embodiment of the present invention 1 is prepared using ultrafast laser
Electron microscope；
Fig. 6 is the scanning on the titanium alloy super-hydrophobic frost resistance surface that the embodiment of the present invention 2 is prepared using ultrafast laser
Electron microscope；
Fig. 7 is the scanning on the titanium alloy super-hydrophobic frost resistance surface that the embodiment of the present invention 3 is prepared using ultrafast laser
Electron microscope；
Fig. 8 is the scanning on the titanium alloy super-hydrophobic frost resistance surface that the embodiment of the present invention 4 is prepared using ultrafast laser
Electron microscope.
Fig. 9 (a), (b) are respectively the super-hydrophobic frost resistance titanium that common alloy of titanium surface and the embodiment of the present invention 1 are prepared
White growing state figure of the alloy surface after 20min under the conditions of -5 DEG C, wherein：Room temperature is 23 DEG C, and relative humidity is 50%.
Figure 10 (a), (b) are respectively the super-hydrophobic frost resistance that common alloy of titanium surface and the embodiment of the present invention 2 are prepared
White growing state figure of the titanium alloy surface after 20min under the conditions of -5 DEG C, wherein：Room temperature is 23 DEG C, and relative humidity is 50%.
Figure 11 (a), (b) are respectively the super-hydrophobic frost resistance that common alloy of titanium surface and the embodiment of the present invention 3 are prepared
White growing state figure of the titanium alloy surface after 20min under the conditions of -5 DEG C, wherein：Room temperature is 23 DEG C, and relative humidity is 50%.
Figure 12 (a), (b) are respectively the super-hydrophobic frost resistance that common alloy of titanium surface and the embodiment of the present invention 4 are prepared
White growing state figure of the titanium alloy surface after 20min under the conditions of -5 DEG C, wherein：Room temperature is 23 DEG C, and relative humidity is 50%.
Embodiment
In order to be better understood from the present invention, technical scheme is done further in detail below in conjunction with specific embodiment
Introduce.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The method that a kind of utilization ultrafast laser of the present invention prepares titanium alloy super-hydrophobic frost resistance surface, with reference to nature
Boundary's biomaterial is as design basis, the natural imitation circle Biocomposite material fine structure point on Ti6Al4V titanium alloy surfaces
The architectural feature of cloth, design surface structure.
Embodiment 1
The method that a kind of utilization ultrafast laser of the present embodiment prepares titanium alloy super-hydrophobic frost resistance surface, including following tool
Body step：
Step one, Ti6Al4V titanium alloys are polished, is 370W from power, lap speed is 450 revs/min, abrasive disk
A diameter of 230mm pre-grinding test sample of gold phase machine, polishing process needs the SiC waterproof abrasive papers for aiding in a diameter of 200mm, 1000 mesh in institute
State titanium alloy surface to be processed by shot blasting, polishing scope is 100cm2, polishing time is 10 minutes, obtains the titanium after the polishing of surface
Alloy sample；
Step 2, the titanium alloy sample after surface polishing described in step one is cleaned with ultrasonic washing instrument, ultrasonic wave is clear
Instrument ultrasonic frequency is washed for 40kHz, sample surfaces are flooded with resistivity for 18.25 megaohms of deionized water, at room temperature, continuously
Cleaning 30 minutes, after cleaning up, room temperature is dried naturally, obtains the titanium alloy sample of cleaning；
Step 3, using ultrafast laser, laser wavelength is 800nm, to the clean titanium alloy obtained described in step 2
Sample surfaces carry out laser scanning manufacturing, and countless micro-structurals are processed in sample surfaces；The laser pulsewidth is 90fs, single
Pulse energy be 66 μ J, repetition rate is 10kHz, the laser scanning utilize X-Y scanning galvanometer systems, make laser beam with
Titanium alloy sample surface described in the ablation line by line of 44.2mm/s speed；The galvanometer system is by X-Y optical scanning heads, electronics
Driving amplifier, optical reflecting lens and field lens composition, the scanning range and speed of the galvanometer system, line are scanned and Surface scan
Path is controlled and set by computer, the signal that the computer is provided by drive amplification circuit drives optical scanning head,
So as to control the deflection of laser beam in X-Y plane, sample is moved in the x-direction relative to laser beam, by controlling translational speed
And laser pulse repetition frequency, its pulse matching degree is reached 1%-99%, complete after movement, then single step stepping in the y-direction, lead to
Control step distance is crossed, its light beam registration is reached 1%-99%, workbench reversion, the sample range of work in y directions
For 126mm x 126mm；
Sample after processing is put into electrically heated drying cabinet and dried after step 3 is laser machined by step 4, sample
It is roasting, depressed in air pressure for normal atmospheric, humidity is 44%RH, temperature is toasted 4 hours for constant temperature under the conditions of 200 DEG C, obtain described
Titanium alloy super-hydrophobic frost resistance surface.
Use resistivity for 18.25 megaohms of deionized water, tested using optical contact angle surface interfacial tension measuring instrument
The contact angle on the obtained titanium alloy super-hydrophobic frost resistance surface, roll angle：Measured using the method that accesses, the shape under liquid feeding syringe needle
Into the suspension drop of required volume, the Z axis of regulation example platform rises sample surfaces, when outstanding under sample surfaces and liquid feeding syringe needle
During the drop bottom contact of extension, drop is just transferred to sample surfaces from liquid feeding syringe needle, then makes sample by adjusting sample stage Z axis again
Product surface drops to original position and measured, because the titanium alloy surface ultra-hydrophobicity prepared is excellent, 3-8 microlitres
Water droplet can not adhere to, so drop volume be 9 microlitres, test temperature be 25.5 DEG C, humidity is 19.5%RH.
The titanium alloy super-hydrophobic frost resistance surface that the present embodiment is prepared, its stereoscan photograph is as shown in figure 5, its table
Nano level papillary structure is presented in face.
Titanium alloy super-hydrophobic frost resistance surface and the contact angle schematic diagram of water such as Fig. 1 (a) institutes that the present embodiment is prepared
Show, shown in roll angle schematic diagram such as Fig. 1 (b).
The titanium alloy super-hydrophobic frost resistance surface and the contact angle of water that the present embodiment is prepared are 169.1 °, and roll angle is
6.2 °, test result is shown in Table 1.
In addition, being 23 DEG C in room temperature, when relative humidity is 50%, by undressed common alloy of titanium and the present embodiment system
Standby obtained super-hydrophobic frost resistance titanium alloy is respectively placed on -5 DEG C of refrigeration platform, and the frost of each titanium alloy surface is observed after 20min
Jelly situation, white growing state is as shown in Figure 9.As shown in Figure 9, after 20min, undressed titanium alloy surface is substantially by ice sheet
Covering, and the titanium alloy surface that the present embodiment is prepared only has regional area tiny ice crystal occur, it is seen that the present embodiment institute
Obtained titanium alloy surface has good resistancet of rost energy.
Embodiment 2
The method that a kind of utilization ultrafast laser of the present embodiment prepares titanium alloy super-hydrophobic frost resistance surface, including following tool
Body step：
Step one, Ti6Al4V titanium alloys are polished, is 370W from power, lap speed is 450 revs/min, abrasive disk
A diameter of 230mm pre-grinding test sample of gold phase machine, polishing process needs the SiC waterproof abrasive papers for aiding in a diameter of 200mm, 1000 mesh in institute
State titanium alloy surface to be processed by shot blasting, polishing scope is 100cm2, polishing time 10 minutes, obtain surface polishing after titanium close
Golden sample；
Step 2, the titanium alloy sample after surface polishing described in step one is cleaned with ultrasonic washing instrument, ultrasonic wave is clear
Instrument ultrasonic frequency is washed for 40kHz, sample surfaces are flooded with resistivity for 18.25 megaohms of deionized water, at room temperature, continuously
Cleaning 30 minutes, after cleaning up, is dried up with cold wind, obtains the titanium alloy sample of cleaning；
Step 3, using ultrafast laser, laser wavelength is 800nm, to the clean titanium alloy obtained described in step 2
Sample surfaces carry out laser scanning manufacturing, countless micro-structurals are processed in sample surfaces, the laser pulsewidth is 90fs, single
Pulse energy is 50 μ J, and repetition rate is 10kHz, the laser scanning routing motion workbench, will be obtained described in step 2
Clean titanium alloy sample be fixed on motion workbench on, using lens by laser beam focusing on to the sample, make sample
Focusing of the surface of product relative to the ultrafast laser light beam etches hot spot along x, y, z three-dimensional direction moving, and speed is
44.2mm/s, by titanium alloy sample surface described in ablation line by line, realizes the etching of micro-nano structure；The motion platform list
Member is three-dimensional servo precision mobile platform, and the scope of the platform movement, speed, direction, can be along X, Y, Z by computer control
Three-dimensional direction moving, the sample range of work is 150mm x 150mm；
Sample after processing is put into electrically heated drying cabinet and dried after step 3 is laser machined by step 4, sample
It is roasting, depressed in air pressure for normal atmospheric, humidity is 41%RH, temperature is toasted 8 hours for constant temperature under the conditions of 100 DEG C, obtain described
Titanium alloy super-hydrophobic frost resistance surface.
Use resistivity for 18.25 megaohms of deionized water, tested using optical contact angle surface interfacial tension measuring instrument
The contact angle on the obtained titanium alloy super-hydrophobic frost resistance surface, roll angle, because the titanium alloy surface prepared is super thin
Water excellent performance, 3-8 microlitres of water droplet can not adhere to, so drop volume is 9 microlitres, test temperature is 25.5 DEG C, and humidity is
19.5%RH.
The titanium alloy super-hydrophobic frost resistance surface that the present embodiment is prepared, its stereoscan photograph is as shown in fig. 6, its table
Nano level gully shape structure is presented in face.
Titanium alloy super-hydrophobic frost resistance surface and the contact angle schematic diagram of water such as Fig. 2 (c) institutes that the present embodiment is prepared
Show, shown in roll angle schematic diagram such as Fig. 2 (d).
The titanium alloy super-hydrophobic frost resistance surface and the contact angle of water that the present embodiment is prepared are 165.4 °, and roll angle is
7.6 °, test result is shown in Table 1.
In addition, testing undressed common alloy of titanium using the identical method of testing of above-described embodiment 1 and test condition
The frost resistance situation of the super-hydrophobic frost resistance titanium alloy prepared with the present embodiment, white growing state is as shown in Figure 10.By scheming
10 understand that after 20min, undressed titanium alloy surface is substantially covered by ice sheet, and the titanium that the present embodiment is prepared is closed
Gold surface only has regional area tiny ice crystal occur, it is seen that the titanium alloy surface obtained by the present embodiment has well frost-resistant
Freeze performance.
Embodiment 3
The method that a kind of utilization ultrafast laser of the present embodiment prepares titanium alloy super-hydrophobic frost resistance surface, including following tool
Body step：
Step one, Ti6Al4V titanium alloys are polished, is 370W from power, lap speed is 450 revs/min, abrasive disk
A diameter of 230mm pre-grinding test sample of gold phase machine, polishing process needs the SiC waterproof abrasive papers for aiding in a diameter of 200mm, 1000 mesh in institute
State titanium alloy surface to be processed by shot blasting, polishing scope is 100cm2, polishing time 10 minutes, obtain surface polishing after titanium close
Golden sample；
Step 2, the titanium alloy sample after surface polishing described in step one is cleaned with ultrasonic washing instrument, ultrasonic wave is clear
Instrument ultrasonic frequency is washed for 40kHz, sample surfaces are flooded with resistivity for 18.25 megaohms of deionized water, at room temperature, continuously
Cleaning 30 minutes, after cleaning up, room temperature is dried naturally, obtains the titanium alloy sample of cleaning；
Step 3, using ultrafast laser, laser wavelength is 800nm, to the clean titanium alloy obtained described in step 2
Sample surfaces carry out laser scanning manufacturing, countless micro-structurals are processed in sample surfaces, the pulsewidth of the laser is
550fs, single pulse energy is 66 μ J, and repetition rate is 10kHz, and the laser scanning utilizes X-Y scanning galvanometer systems, makes laser
Beam is with titanium alloy sample surface described in the ablation line by line of 44.2mm/s speed；The galvanometer system by X-Y optical scanning heads,
Electric drive amplifier, optical reflecting lens and field lens composition, the scanning range and speed of the galvanometer system, line are scanned and face
Scanning pattern is controlled and set by computer, and the signal that the computer is provided passes through drive amplification circuit drives optical scanner
Head, so as to control the deflection of laser beam in X-Y plane, sample is moved in the x-direction relative to laser beam, by controlling mobile speed
Degree and laser pulse repetition frequency, make its pulse matching degree reach 1%-99%, complete after movement, then single step stepping in the y-direction,
By controlling step distance, its light beam registration is set to reach 1%-99% in y directions, workbench reversion, the sample processes model
Enclose for 126mm x 126mm；
Sample after processing is put into electrically heated drying cabinet and dried after step 3 is laser machined by step 4, sample
It is roasting, depressed in air pressure for normal atmospheric, humidity is 56%RH, temperature is toasted 2 hours for constant temperature under the conditions of 250 DEG C, obtain described
Titanium alloy super-hydrophobic frost resistance surface.
Use resistivity for 18.25 megaohms of deionized water, tested using optical contact angle surface interfacial tension measuring instrument
The contact angle on the obtained titanium alloy super-hydrophobic frost resistance surface, roll angle, because the titanium alloy surface prepared is super thin
Water excellent performance, 3-8 microlitres of water droplet can not adhere to, so drop volume is 9 microlitres, test temperature is 25.5 DEG C, and humidity is
19.5%RH.
The titanium alloy super-hydrophobic frost resistance surface that the present embodiment is prepared, its stereoscan photograph is as shown in fig. 7, its table
Face has nano level papillary structure.
Titanium alloy super-hydrophobic frost resistance surface and the contact angle schematic diagram of water such as Fig. 3 (e) institutes that the present embodiment is prepared
Show, shown in roll angle schematic diagram such as Fig. 3 (f).
The titanium alloy super-hydrophobic frost resistance surface and the contact angle of water that the present embodiment is prepared are 164.4 °, and roll angle is
4.7 °, test result is shown in Table 1.
In addition, testing undressed common alloy of titanium using the identical method of testing of above-described embodiment 1 and test condition
The frost resistance situation of the super-hydrophobic frost resistance titanium alloy prepared with the present embodiment, white growing state is as shown in figure 11.By scheming
11 understand that after 20min, undressed titanium alloy surface is substantially covered by ice sheet, and the titanium that the present embodiment is prepared is closed
Gold surface only has regional area tiny ice crystal occur, it is seen that the titanium alloy surface obtained by the present embodiment has well frost-resistant
Freeze performance.
Embodiment 4
The method that a kind of utilization ultrafast laser of the present embodiment prepares titanium alloy super-hydrophobic frost resistance surface, including following tool
Body step：
Step one, Ti6Al4V titanium alloys are polished, polishing is 370W from power, lap speed is 450 revs/min, is ground
Grinding wheel diameter is 230mm pre-grinding test sample of gold phase machine, and polishing process needs to aid in the SiC waterproof abrasive papers of a diameter of 200mm, 1000 mesh
It is processed by shot blasting in the titanium alloy surface, polishing scope is 100cm2, polishing time 10 minutes, obtain surface polishing after
Titanium alloy sample；
Step 2, the titanium alloy sample after surface polishing described in step one is cleaned with ultrasonic washing instrument, ultrasonic wave is clear
Instrument ultrasonic frequency is washed for 40kHz, sample surfaces are flooded with resistivity for 18.25 megaohms of deionized water, at room temperature, continuously
Cleaning 30 minutes, after cleaning up, room temperature is dried naturally, obtains the titanium alloy sample of cleaning；
Step 3, using ultrafast laser, laser wavelength is 800nm, to the clean titanium alloy obtained described in step 2
Sample surfaces are laser machined, and countless micro-structurals are processed in sample surfaces, the pulsewidth of the laser is 550fs, single
Pulse energy is 50 μ J, and repetition rate is 10kHz, the laser scanning routing motion workbench, will be obtained described in step 2
Clean titanium alloy sample be fixed on motion workbench on, using lens by laser beam focusing on to the sample, make sample
Focusing of the surface of product relative to the ultrafast laser light beam etches hot spot along x, y, z three-dimensional direction moving, and speed is
44.2mm/s, by titanium alloy sample surface described in ablation line by line, realizes the etching of micro-nano structure；The motion platform list
Member is three-dimensional servo precision mobile platform, and the scope of the platform movement, speed, direction, can be along X, Y, Z by computer control
Three-dimensional direction moving, the sample range of work is 150mm x 150mm；
Sample after processing is put into electrically heated drying cabinet and dried after step 3 is laser machined by step 4, sample
It is roasting, depressed in air pressure for normal atmospheric, humidity is 50%RH, temperature is toasted 6 hours for constant temperature under the conditions of 200 DEG C, obtain described
Titanium alloy super-hydrophobic frost resistance surface.
Use resistivity for 18.25 megaohms of deionized water, tested using optical contact angle surface interfacial tension measuring instrument
The contact angle on the obtained titanium alloy super-hydrophobic frost resistance surface, roll angle, because the titanium alloy surface prepared is super thin
Water excellent performance, 3-8 microlitres of water droplet can not adhere to, so drop volume is 9 microlitres, test temperature is 25.5 DEG C, and humidity is
19.5%RH.
The titanium alloy super-hydrophobic frost resistance surface that the present embodiment is prepared, its stereoscan photograph is as shown in Figure 8.Its table
Nano level gully shape structure is presented in face.
Titanium alloy super-hydrophobic frost resistance surface and the contact angle schematic diagram of water such as Fig. 4 (g) institutes that the present embodiment is prepared
Show, shown in roll angle schematic diagram such as Fig. 4 (h).
The titanium alloy super-hydrophobic frost resistance surface and the contact angle of water that the present embodiment is prepared are 170.5 °, and roll angle is
3.8 °, test result is shown in Table 1.
In addition, testing undressed common alloy of titanium using the identical method of testing of above-described embodiment 1 and test condition
The frost resistance situation of the super-hydrophobic frost resistance titanium alloy prepared with the present embodiment, white growing state is as shown in figure 12.By scheming
12 understand that after 20min, undressed titanium alloy surface is substantially covered by ice sheet, and the titanium that the present embodiment is prepared is closed
Gold surface only has regional area tiny ice crystal occur, it is seen that the titanium alloy surface obtained by the present embodiment has well frost-resistant
Freeze performance.
Table 1 is the contact angle on the titanium alloy super-hydrophobic frost resistance surface that various embodiments of the present invention are prepared, roll angle
Test result.
Table 1
| Embodiment | Contact angle/° | Roll angle/° |
| Embodiment 1 | 169.1 | 6.2 |
| Embodiment 2 | 165.4 | 7.6 |
| Embodiment 3 | 164.4 | 4.7 |
| Embodiment 4 | 170.5 | 3.8 |
The above embodiment of the present invention is not to the present invention just for the sake of clearly illustrating examples of the invention
Embodiment restriction.Every any modification made in spirit of the invention and principle, equivalent substitution and improvement etc. all should
Within the protection domain of the claims in the present invention.
Claims (9)
1. a kind of method that utilization ultrafast laser prepares titanium alloy super-hydrophobic frost resistance surface, it is characterised in that：Methods described bag
Include following steps：
Step one, pending titanium alloy surface is polished pretreatment, obtains the titanium alloy sample after the polishing of surface；
Step 2, the titanium alloy sample after surface polishing described in step one is placed in the ultrasonic washing instrument for filling deionized water
Cleaning, after cleaning up, the drying of titanium alloy sample surface cold wind or room temperature is dried naturally, the titanium alloy of cleaning is obtained
Sample；
Step 3, using laser processing technology, is regulated after the technological parameter of correlation to described in step 2 using ultrafast laser
Obtained clean titanium alloy sample surface carries out laser scanning processing, and countless micro-structurals are processed in sample surfaces；
The laser scanning carries out light beam scanning using galvanometer system, and the speed of vibration mirror scanning is 0.1mm/s-30m/s, laser
Break-make and the scanning range of galvanometer system, scanning track and process velocity are by computer program control and setting；
Or the laser scanning is realized using motion platform system, and light beam is fixed, the motion of sample relative beam, platform motion
Speed is 0.1mm/s-3m/s, and break-make, platform movement locus and the speed of laser are by computer program control and setting；
Step 4, constant temperature and humidity electricity is put into by titanium alloy sample of the surface obtained described in step 3 after Laser Processing is handled
Toasted in heated drying case, that is, obtain the titanium alloy super-hydrophobic frost resistance surface；
Wherein, the ultrafast laser wavelength described in step 3 is less than 1000nm, and the laser processing parameter is：Pulsewidth is more than
30fs, single pulse energy is less than 0.1mJ；
Pressure described in step 4 in electrically heated drying cabinet is normal atmospheric pressure, humidity be 40%-60%RH, temperature be 100 DEG C-
250 DEG C, the time that the sample is toasted is that the temperature error in 2-8 hours, the electrically heated drying cabinet is ± 1 DEG C.
2. the method that a kind of utilization ultrafast laser as claimed in claim 1 prepares titanium alloy super-hydrophobic frost resistance surface, it is special
Levy and be：Described titanium alloy is Ti6Al4V titanium alloys.
3. the method that a kind of utilization ultrafast laser as claimed in claim 1 or 2 prepares titanium alloy super-hydrophobic frost resistance surface, its
It is characterised by：The repetition rate of ultrafast laser described in step 3 is 10kHz-200kHz, and the pulsewidth is 30fs-10ps.
4. the method that a kind of utilization ultrafast laser as claimed in claim 3 prepares titanium alloy super-hydrophobic frost resistance surface, it is special
Levy and be：The pulsewidth of the ultrafast laser is 80fs-800fs.
5. the method that a kind of utilization ultrafast laser as claimed in claim 4 prepares titanium alloy super-hydrophobic frost resistance surface, it is special
Levy and be：The wavelength of the ultrafast laser is 800nm, and the pulsewidth of the ultrafast laser is 90fs-550fs.
6. the method that a kind of utilization ultrafast laser as claimed in claim 5 prepares titanium alloy super-hydrophobic frost resistance surface, it is special
Levy and be：The pulsewidth is 90fs, and the single pulse energy is 50 μ J-66 μ J, and laser scanning speed is 20mm/s-60mm/s.
7. the method that a kind of utilization ultrafast laser as claimed in claim 5 prepares titanium alloy super-hydrophobic frost resistance surface, it is special
Levy and be：The pulsewidth is 550fs, and the single pulse energy is 50 μ J-66 μ J, and laser scanning speed is 20mm/s-60mm/s.
8. the method that a kind of utilization ultrafast laser as claimed in claim 1 prepares titanium alloy super-hydrophobic frost resistance surface, it is special
Levy and be：Humidity in the constant temperature and humidity electrically heated drying cabinet is 50%RH, and temperature is 200 DEG C, and the time of baking is 6 hours.
9. the titanium alloy super-hydrophobic frost resistance surface that a kind of method described in use claim any one of 1-8 is prepared, institute
Stating surface has nano level papillary structure or gully shape structure.
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| CN107096998A (en) * | 2017-05-08 | 2017-08-29 | 英诺激光科技股份有限公司 | It is a kind of to carry out anticorrosive beating calibration method using ultrafast laser |
| CN111830605A (en) * | 2019-04-18 | 2020-10-27 | 上旸光学股份有限公司 | Optical lens with laser-induced periodic surface microstructure |
| CN110480282A (en) * | 2019-05-20 | 2019-11-22 | 长春理工大学 | A kind of copper-based material surface delay icing structure and preparation method thereof |
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| CN113199148B (en) * | 2021-05-06 | 2022-02-15 | 大连理工大学 | Processing method of transverse cake-shaped bouncing super-hydrophobic inclined column array of liquid drops |
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