CN106733564A - The preparation method of the resistance to corrosive magnesium alloy super-hydrophobic surface of biological fluid - Google Patents

The preparation method of the resistance to corrosive magnesium alloy super-hydrophobic surface of biological fluid Download PDF

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Publication number
CN106733564A
CN106733564A CN201611046209.7A CN201611046209A CN106733564A CN 106733564 A CN106733564 A CN 106733564A CN 201611046209 A CN201611046209 A CN 201611046209A CN 106733564 A CN106733564 A CN 106733564A
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magnesium alloy
resistance
nano
biological fluid
preparation
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张倩倩
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Dalian University
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Dalian University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/002—Pretreatement
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • 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
    • B23K26/36—Removing material
    • B23K26/361—Removing material for deburring or mechanical trimming
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2504/00—Epoxy polymers

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Plasma & Fusion (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

The preparation method of the resistance to corrosive magnesium alloy super-hydrophobic surface of biological fluid, the method is comprised the following steps：S1 prepares micron order coarse structure on magnesium alloy sample surface；S2 prepares epoxy resin solution and SiO2Nano dispersion fluid, obtains micro-/ nano surface；Perfluoroalkyl triethoxysilane ethanol solution is spun on sample micro-/ nano composite structure surface by S3, is dried, and obtains super hydrophobic surface.The method that the present invention is constructed using Laser Processing with reference to nanostructured and low surface mass is coated, superhydrophobic surface structure has been obtained, ultra-hydrophobicity is preferable, and with sufficient stability, corrosion resistance in simulated body fluid is effectively improved, and alloy surface has preferable resistance to biological fluid corrosive nature.The inventive method is simple, easy to operate, low cost, time-consuming short, substantially increases production efficiency, and a practicable approach is provided to improve corrosive nature of the magnesium alloy in biological fluid.

Description

The preparation method of the resistance to corrosive magnesium alloy super-hydrophobic surface of biological fluid
Technical field
The invention belongs to technical field of material surface treatment, it is related to a kind of processing method of corrosion proof super hydrophobic surface.
Background technology
Magnesium alloy is used as a kind of light metal material, it is considered to be the green engineering material of 21 century.Because it has specific strength It is high, specific stiffness is high, thermal fatigue property is good, biocompatibility is good, capability of electromagnetic shielding is excellent, thermal conductivity ability strong, antidetonation Property it is good and recyclable the advantages of, had a wide range of applications in fields such as communications and transportation, biomedicine, Aero-Space and national defense industry Prospect.In recent years, magnesium alloy is by spies such as its good biocompatibility, low-density and the close elastic modelling quantity of skeleton Point, as most potential medical metal material now, with very strong development prospect.
Magnesium alloy compared with the existing medical metal material for coming into Clinical practice, has as medical embedded material Advantage following prominent:1. good biocompatibility and biodegradability；2. good mechanical compatibility；3. can drop completely Xie Xing；4. low cost.But so far, magnesium alloy is huge anti-as still existing between the application potential and reality of biomaterial Difference, the poor corrosion resistance of magnesium alloy is to restrict the bottleneck that magnesium alloy elicits latent faculties.Biological magnesium alloy is degraded speed in physiological environment Spend soon, and mostly local corrosion, premature failure during being easily caused fixing device under arms.Closed to solve biologic medical magnesium The subject matter of gold, researcher proposes many methods, wherein, process for modifying surface is that one kind can both improve bio-compatible Property, the effective ways of corrosion resistance of surface can be improved again, and magnesium alloy substrate is lost as the advantage of bio-medical material again, Therefore, process for modifying surface just turns into one of key method of solution medical magnesium alloy development.
Super hydrophobic surface refers to static contact angle surface more than 150 ° of the base material to water, is such as deposited extensively in nature Nelumbo section blade face, the leg of water skipper, dragonfly wing etc., they are respectively provided with super-hydrophobicity and automatical cleaning ability.By to material Surface is modified, and makes it have superhydrophobic characteristic, can effectively reduce the surface free energy of base material, improves and control material Wetting, stick together, lubricate and polishing machine, there is huge application potential in material modification and application aspect.In material substrate Building super-hydrophobic coat has good anticorrosive, fluid drag-reduction and self-cleaning surface performance, in the side such as medical magnesium alloy component Mask has wide practical use.
Research to super-hydrophobic lotus leaf shows：Surface is micro-/receive binary coarse structure and low-surface energy substance is that lotus leaf has The main cause of super-hydrophobic automatic cleaning effect.Although the preparation method of super hydrophobic surface is existing a lot, such as using plasma, chemistry The method that the technologies such as lithographic technique, plating are combined with coating low-surface energy substance, or using the method for chemical conversion, can make It is standby go out super hydrophobic surface, but these methods or apparatus expensive, or have pollution to environment, or manufacturing cycle is long etc., Remain in room for improvement.
The content of the invention
It is rotten the invention provides a kind of simple and easy to do, with low cost and resistance to biological fluid to solve the deficiencies in the prior art The preparation method of the magnesium alloy super-hydrophobic surface of corrosion.Inventor is based on research of the forefathers to magnesium alloy super-hydrophobic material property, Give full play to the advantage of super hydrophobic surface, it is proposed that improve setting for biological medical magnesium alloy performance based on super hydrophobic surface is built Think, by reducing the tackness of test specimen and the contact area, reduction test specimen and liquid of liquid, raising magnesium alloy is in biotic environment Corrosion resistance.
To achieve the above object, the technical solution adopted by the present invention is：
S1 prepares micron order coarse structure on magnesium alloy sample surface；
S2 prepares epoxy resin solution and SiO2Nano dispersion fluid, the sample table after processing is applied to by epoxy resin solution Face, then coats SiO to surface2Nano dispersion fluid, dries, and obtains micro-/ nano surface；
Perfluoroalkyl triethoxysilane ethanol solution is spun on sample micro-/ nano composite structure surface by S3, is dried, and is obtained Obtain super hydrophobic surface.
Preferably, the step S1 obtains coarse micro-scale surface using laser marking machine on magnesium alloy sample surface, Laser marking machine uses point-like pattern, 50~70 μm of lattice distance, 12~15A of electric current.
Surface Machining is carried out using laser marking machine, parameter adjustment is convenient, simple to operate, Laser Processing spacing can change Can be deposited in melting splash on rat by the roughness of micron order coarse structure, small lattice distance；Processing electric current Input energy is determined, input current is big, than increasing, rat highly increases h/d.Two parameter phases of lattice distance and electric current With reference to joint effect surface micrometre-grade coarse structure.
Preferably, step S1 also includes pre-processing magnesium alloy sample, specially：To be closed by the magnesium after polishing, polishing Golden sample, is cleaned by ultrasonic in acetone, ethanol and distilled water successively, then dries up.
Preferably, with acetone as solvent, epoxy resin is 1 with the volume ratio of acetone to the step S2 epoxy resin solutions： 10, the curing agent of the epoxy resin is 2,4,6- tri- (dimethylamino methyl) phenol, and curing agent is polyamide.
Preferably, SiO in the step S22Nano dispersion fluid includes Nano-meter SiO_22Particle, absolute ethyl alcohol and silane coupled Agent, the SiO2The concentration of nano dispersion fluid is 10-20g/L.Its concentration is Nano-meter SiO_22Concentration of the particle in absolute ethyl alcohol, SiO2Through experimental study, when concentration is more than 20g/L, contact angle is not significantly increased the concentration of nano dispersion fluid, and roll angle Become big, super-hydrophobicity is deteriorated.
Further, per 1g Nano-meter SiO_2s2Particle adds 0.5mL silane couplers.
Nano-meter SiO_22There are a large amount of residual bonds and the hydroxyl of different bond styles and can occur with silane coupler in the surface of particle Reaction, improves the cluster of nano particle.SiO2Nano dispersion fluid has synergy with epoxy resin, and both are by coupling Agent, makes Nano-meter SiO_22Particle participates in the solidification process of epoxy resin, by SiO2Nano particle is cured to the micron order after Laser Processing Rough surface.
Preferably, the perfluoroalkyl triethoxysilane volumes of aqueous ethanol concentration is 0.05~0.15%.
Present invention selection epoxy resin is based on its architectural characteristic, epoxy resin and SiO2Coupling agent in dispersion liquid occurs Reaction, in its surface grafting organosilan chain, by SiO after solidification2It is implanted to laser-textured surface.The remaining hydroxyl of epoxy resin Base can also be reacted with perfluoroalkyl triethoxysilane, and fluorine carbon long-chain structure fine and close in order is formed in its surface grafting. In addition, raising of the methyl in epoxy resin to super-hydrophobicity also has certain effect.And other solvents can not be played and ring Oxygen tree fat identical effect.
Beneficial effects of the present invention：
(1) present invention obtains micron scale construction using laser marking machine, and equipment simple operations are convenient, and process velocity is fast, plus Work parameter adjustment is accurate, and process stabilization, even structure shows as the lattice structure of rule, can guarantee that its surface property everywhere Can be homogeneous.
(2) Laser Processing is without electrolyte, it is to avoid actual bodily harm of the solution to environment and operating personnel.
(3) low-surface energy substance perfluoroalkyl triethoxysilane and curing nano SiO2Hydroxyl in the epoxy resin of particle There is condensation reaction in base, fluorine carbon long-chain structure fine and close in order is formed in its surface grafting, make low-surface energy substance with substrate Adhesion is coated better than machinery.
(4) super-hydrophobic magnesium alloy of the invention has carried out the corrosion test in biological fluid is simulated, and its corrosion resistance is better than The corrosion resistance of magnesium alloy substrate, the method can be used for the research and application of Biological magnesium alloy.
In a word, the method that the present invention is constructed using Laser Processing with reference to nanostructured and low surface mass is coated, is obtained Superhydrophobic surface structure, ultra-hydrophobicity is preferable, and with sufficient stability, the corrosion resistance in simulated body fluid is obtained effectively Ground is improved, and alloy surface has preferable resistance to biological fluid corrosive nature.The method is simple, easy to operate, low cost, time-consuming short, Production efficiency is substantially increased, a practicable way is provided to improve corrosive nature of the magnesium alloy in biological fluid Footpath.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph on the AZ91D magnesium alloy samples surface after the processing of the laser marking of embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of the super hydrophobic surface sample modified by nano-particle coating and low-surface energy substance；
Fig. 3 is the Static water contact angular measurement comparison diagram of undressed magnesium alloy substrate and super-hydrophobic magnesium alloy sample； Wherein A is undressed magnesium alloy substrate, and B is the magnesium alloy sample of the inventive method treatment；
After Fig. 4 places 3 months at room temperature for super-hydrophobic magnesium alloy sample, the measurement result figure of Static water contact angles；
Fig. 5 is the electricity of undressed magnesium alloy substrate and super-hydrophobic magnesium alloy sample in Hank ' s simulation biological fluids Chemical impedance spectrogram.
Specific embodiment
Below by embodiment, technical scheme to be protected of the invention is described in detail, but limit never in any form The system present invention.In following embodiments unless otherwise specified, the experimental technique for being used is conventional method, material therefor, reagent Deng can be bought from commercial channel.
Embodiment 1
By the polishing of AZ91D magnesium alloy samples, polishing, with being dried up after ultrasonic cleaning in acetone, ethanol and distilled water, laser is beaten Mark machine uses point-like pattern, 50 μm of lattice distance, electric current 12A to obtain coarse micron order table on AZ91D magnesium alloy samples surface Face, as shown in figure 1, by after Laser Processing, surface forms micron-sized coarse structure.
Embodiment 2
Prepare epoxy resin solution and SiO2Nano dispersion fluid：
Epoxy resin solution：With acetone as solvent, epoxy resin is 1 with the volume ratio of acetone to epoxy resin solution：10.Institute The curing agent of epoxy resin is stated for 2,4,6- tri- (dimethylamino methyl) phenol, curing agent is polyamide.
SiO2Nano dispersion fluid：By Nano-meter SiO_22Particle 1.5g, 0.1L absolute ethyl alcohol and silane coupler 0.75L mix, and obtain It is 15g/L SiO to concentration2Nano dispersion fluid.
It is uniform with ultrasonic vibration, epoxy resin solution is first applied to the sample after being laser machined in embodiment 1 with sol evenning machine Surface, uses high-purity N2Drying, then coats SiO to specimen surface2Nano dispersion fluid, is placed in 3h in drying box, obtains micro-/ nano Surface.
Prepare perfluoroalkyl triethoxysilane ethanol solution：0.1mL perfluoroalkyl triethoxysilanes are dissolved in 0.1L Absolute ethyl alcohol, ultrasonic disperse 30min is sufficiently mixed uniformly, obtains the perfluoroalkyl triethoxysilane that volumetric concentration is 0.1% Ethanol solution.
Perfluoroalkyl triethoxysilane ethanol solution is uniformly applied to micro-/ nano composite structure surface with sol evenning machine, is put The 1h in drying box, obtains super hydrophobic surface.As shown in Fig. 2 the specimen surface after treatment is coarse, there is substantial amounts of micron order Grain, uniformly dispersing nanometer particle thereon.
Embodiment 3
SiO is differed only in embodiment 22Nano dispersion fluid concentration is different.The present embodiment SiO2Nano dispersion fluid concentration It is 10g/L.
Embodiment 4
SiO is differed only in embodiment 22Nano dispersion fluid concentration is different.The present embodiment SiO2Nano dispersion fluid concentration It is 20g/L.
Embodiment 5
Super-hydrophobic magnesium alloy sample after undressed magnesium alloy substrate and embodiment 2 are processed carries out Static water contact Angular measurement is contrasted, and is measured using intravenous infusion contact angle/interfacial tension measuring instrument, the μ L of water-carrying capacity 0.5.From Fig. 3 B, through super After hydrophobic treatment, the static contact angle on magnesium alloy sample surface is increased considerably, and is increased to by 64.9 ° of matrix (Fig. 3 A) 161.1 °, minimum roll angle is 2.109 °.
Embodiment 6
Determine the stability of the inventive method gained magnesium alloy super-hydrophobic surface.The magnesium alloy air that embodiment 2 is processed Static water contact angles test is carried out again after being placed 3 months under middle normal temperature, as shown in Figure 4, was not had an impact magnesium by 3 months and is closed The ultra-hydrophobicity of gold.Static contact angle is more than 150 °, illustrates the stabilization of magnesium alloy super-hydrophobic surface prepared by the inventive method Property is preferable.
Embodiment 7
Determine the corrosion resisting property of the inventive method gained magnesium alloy super-hydrophobic surface.
Magnesium alloy prepared by the inventive method is placed on through the magnesium alloy substrate sample after No. 1000 abrasive paper for metallograph polishings Electro-chemical test is carried out in Hank ' s simulated body fluid media.Test uses three electrode test systems of standard, and reference electrode is full The calomel electrode (SCE) of sum, is platinum electrode to electrode, and working electrode is test sample, and test area is 1cm2。
As seen from Figure 5, matrix, surface super hydrophobic alloy table are significantly greater than through the capacitive reactance arc radius of the sample of super-hydrophobic treatment The impedance value of face corrosion film layer is big, and the protectiveness to sample is good, i.e., the corrosion resisting property of super-hydrophobic sample is greatly improved.

Claims (7)

1. the preparation method of the corrosive magnesium alloy super-hydrophobic surface of resistance to biological fluid, it is characterised in that comprise the following steps：
S1 prepares micron order coarse structure on magnesium alloy sample surface；
S2 prepares epoxy resin solution and SiO2Nano dispersion fluid, is applied to the specimen surface after processing, then by epoxy resin solution SiO is coated to surface2Nano dispersion fluid, dries, and obtains micro-/ nano surface；
Perfluoroalkyl triethoxysilane ethanol solution is spun on sample micro-/ nano composite structure surface by S3, is dried, and is surpassed Hydrophobic surface.
2. the preparation method of the corrosive magnesium alloy super-hydrophobic surface of resistance to biological fluid according to claim 1, its feature It is that the step S1 obtains coarse micro-scale surface, laser marking machine using laser marking machine on magnesium alloy sample surface Using point-like pattern, 50~70 μm of lattice distance, 12~15A of electric current.
3. the preparation method of the corrosive magnesium alloy super-hydrophobic surface of resistance to biological fluid according to claim 1, its feature It is that step S1 also includes pre-processing magnesium alloy sample, specially：By by polishing, polishing after magnesium alloy sample, successively It is cleaned by ultrasonic in acetone, ethanol and distilled water, then dries up.
4. the preparation method of the corrosive magnesium alloy super-hydrophobic surface of resistance to biological fluid according to claim 1, its feature It is that with acetone as solvent, epoxy resin is 1 with the volume ratio of acetone to the step S2 epoxy resin solutions：10, the epoxy The curing agent of resin is 2,4,6- tri- (dimethylamino methyl) phenol, and curing agent is polyamide.
5. the preparation method of the corrosive magnesium alloy super-hydrophobic surface of resistance to biological fluid according to claim 1, its feature It is, SiO in the step S22Nano dispersion fluid includes Nano-meter SiO_22Particle, absolute ethyl alcohol and silane coupler, the SiO2 The concentration of nano dispersion fluid is 10-20g/L.
6. the preparation method of the corrosive magnesium alloy super-hydrophobic surface of resistance to biological fluid according to claim 5, its feature It is, per 1g Nano-meter SiO_2s2Particle adds 0.5mL silane couplers.
7. the preparation method of the corrosive magnesium alloy super-hydrophobic surface of resistance to biological fluid according to claim 1, its feature It is that the perfluoroalkyl triethoxysilane volumes of aqueous ethanol concentration is 0.05~0.15%.
CN201611046209.7A 2016-11-22 2016-11-22 The preparation method of the resistance to corrosive magnesium alloy super-hydrophobic surface of biological fluid Pending CN106733564A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107916421A (en) * 2017-11-13 2018-04-17 常州麒通国际贸易有限公司 A kind of preparation method of corrosion resistance magnesium alloy super-hydrophobic surface
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
CN110055524A (en) * 2019-04-25 2019-07-26 西南交通大学 A kind of bio-medical mg-based material surface can bioid hydrophobically modified layer preparation method
CN110079285A (en) * 2019-04-29 2019-08-02 同济大学 A kind of super-hydrophobic particle and preparation method thereof for underwater leak stopping
CN111299104A (en) * 2020-03-17 2020-06-19 陕西科技大学 Super-hydrophobic composite coating and preparation method thereof
CN113145418A (en) * 2020-01-07 2021-07-23 中国石油天然气集团有限公司 Preparation method of super-hydrophobic material and super-hydrophobic material

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107916421A (en) * 2017-11-13 2018-04-17 常州麒通国际贸易有限公司 A kind of preparation method of corrosion resistance magnesium alloy super-hydrophobic surface
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
CN110055524A (en) * 2019-04-25 2019-07-26 西南交通大学 A kind of bio-medical mg-based material surface can bioid hydrophobically modified layer preparation method
CN110055524B (en) * 2019-04-25 2020-10-30 西南交通大学 Preparation method of bio-medical hydrophobic modified layer on magnesium-based material surface
CN110079285A (en) * 2019-04-29 2019-08-02 同济大学 A kind of super-hydrophobic particle and preparation method thereof for underwater leak stopping
CN113145418A (en) * 2020-01-07 2021-07-23 中国石油天然气集团有限公司 Preparation method of super-hydrophobic material and super-hydrophobic material
CN111299104A (en) * 2020-03-17 2020-06-19 陕西科技大学 Super-hydrophobic composite coating and preparation method thereof
CN111299104B (en) * 2020-03-17 2022-08-26 陕西科技大学 Super-hydrophobic composite coating and preparation method thereof

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