CN110129780A - A kind of superhydrophobic magnesium alloy surfaces preparation method - Google Patents
A kind of superhydrophobic magnesium alloy surfaces preparation method Download PDFInfo
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- CN110129780A CN110129780A CN201910507504.5A CN201910507504A CN110129780A CN 110129780 A CN110129780 A CN 110129780A CN 201910507504 A CN201910507504 A CN 201910507504A CN 110129780 A CN110129780 A CN 110129780A
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- Prior art keywords
- magnesium alloy
- water
- superhydrophobic
- preparation
- phosphonic acids
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 50
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 239000000956 alloy Substances 0.000 claims abstract description 17
- 239000002253 acid Substances 0.000 claims abstract description 12
- 150000003009 phosphonic acids Chemical class 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 5
- -1 phospho Chemical class 0.000 claims abstract description 5
- 238000005498 polishing Methods 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- QLZHNIAADXEJJP-UHFFFAOYSA-N Phenylphosphonic acid Chemical compound OP(O)(=O)C1=CC=CC=C1 QLZHNIAADXEJJP-UHFFFAOYSA-N 0.000 claims description 12
- 244000137852 Petrea volubilis Species 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 3
- 208000011580 syndromic disease Diseases 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 239000007769 metal material Substances 0.000 abstract description 5
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 238000004381 surface treatment Methods 0.000 abstract 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 14
- 238000000034 method Methods 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 8
- 238000000576 coating method Methods 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 7
- 239000007787 solid Substances 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/78—Pretreatment of the material to be coated
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The present patent application belongs to field of metal material surface treatment, specifically discloses a kind of superhydrophobic magnesium alloy surfaces preparation method, comprising the following steps: (1) by magnesium alloy mechanical polishing, clean up it is spare；(2) water-soluble organic phospho acid is dissolved in deionized water, the magnesium alloy materials in step (1) is dipped in 0.01-0.1mol/L phosphonic acids aqueous solution, be heated to 95-100 DEG C, constant temperature 16-24h；(3) magnesium alloy materials in step (2) are taken out from phosphonic acids solution, phosphorated super-hydrophobic coat will be obtained after magnesium alloy cleaning, drying with deionized water.This programme solves the problems, such as that preparing super hydrophobic surface application is limited mainly for the preparation of Mg alloy surface film.
Description
Technical field
The invention belongs to field of material technology, specifically disclose a kind of superhydrophobic magnesium alloy surfaces preparation method.
Background technique
Super hydrophobic surface with good automatically cleaning, corrosion-resistant, fouling resistance, the anti-icing characteristics such as cover is widely used in gold because of it
Belong in material surface research.Traditional super hydrophobic surface preparation is usually two-step method, and two approach realize super hydrophobic surface building.
Approach (1) first step manufactures coarse structure, and second step is in coarse structure surface modification low-surface energy substance (such as silicon fluoride)；On the way
Diameter (2) first step low-surface energy substance surface modification, second step manufacture coarse structure on low-surface energy substance surface.
The method for preparing super hydrophobic surface at present has etching method, template, electrostatic spinning, sol-gel method, anodic oxidation
Method, micro-arc oxidation, ion-exchange, removal alloying etc., these methods have higher requirements to experimental facilities and operate multiple
Miscellaneous cumbersome, there are limitations when production, so that using being restricted.
Summary of the invention
The purpose of the present invention is to provide a kind of superhydrophobic magnesium alloy surfaces preparation methods, prepare super hydrophobic surface with solution
Using limited problem.
In order to achieve the above object, the technical solution of the present invention is as follows: a kind of superhydrophobic magnesium alloy surfaces preparation method, including
Following steps:
(1) by AZ31 magnesium alloy mechanical polishing, clean up it is spare；
(2) water-soluble organic phospho acid is dissolved in deionized water, the magnesium alloy materials in step (1) is dipped in water-soluble phosphine
In acid solution, constant temperature 16-24h；
(3) magnesium alloy materials in step (2) are taken out from phosphonic acids solution, is cleaned magnesium alloy with deionized water, done
Phosphorated super-hydrophobic coat is obtained after dry.
The working principle and beneficial effect of the technical program is:
(1) present invention utilizes the surface-active and interfacial reaction characteristic of metal material, and inventor is during test of many times
It was found that phosphorated superhydrophobic magnesium alloy surfaces can be prepared using one-step method, prepared without two-step method, because phenyl-phosphonic acid has
Double action: can construct coarse structure and drop low-surface-energy；
(2) after phenyl-phosphonic acid loses proton in the solution, become the phenyl-phosphonic acid ion of bear electricity, in magnesium alloy materials table
Face and magnesium ion generate stable chemical bonding and act on, and impart the excellent hydrophobic performance of coating, and coating contact angle is greater than 150 °.
Wherein phenyl-phosphonic acid is reacted with magnesium while constructed coarse structure, and reduces Mg alloy surface energy；
(3) preparation method of the invention is simple and efficient, at low cost, has universality, which has corrosion-resistant, anti-biological
Equal tables/interfacial characteristics are stained, are with a wide range of applications.
Further, magnesium alloy materials pretreatment includes: to cut magnesium alloy materials in step (1), is thrown with SiC sand paper machinery
Light is smooth to surface, then with successively with acetone, dehydrated alcohol, deionized water ultrasonic cleaning 5-10min removal metal watch
Face impurity and greasy dirt, drying.After handling magnesium alloy using the above method, convenient for forming super-hydrophobic coat in Mg alloy surface.
Further, successively using SiC sand paper 400#, 800#, 1200#, 2000# polishing magnesium alloy in step (1).Using upper
The SiC sand paper for stating model successively polishes and Mg alloy surface can be made flat and smooth, convenient for forming super-hydrophobic coat in Mg alloy surface.
Further, water-soluble phosphonic acids is phenyl-phosphonic acid in step (2).Using phosphenylic acid while constructing coarse structure
Low-surface-energy can drop.
Further, water-soluble phosphine acid solution thermostat temperature is 95-100 DEG C in step (2).Use the water solubility of above-mentioned temperature
Phosphonic acids solution can accelerate the phosphorated speed of Mg alloy surface.
Further, the substance withdrawl syndrome of the water-soluble phosphine acid solution of step (2) is 0.01-0.1mol/L.Using above-mentioned
Water-soluble phosphine acid solution in concentration range can form coating in homogeneous thickness in Mg alloy surface.
Detailed description of the invention
Fig. 1 is the surface macrograph of super-hydrophobic magnesium alloy in the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of superhydrophobic magnesium alloy surfaces in the present invention.
Specific embodiment
It is further described below by specific embodiment:
In the present solution, " super-hydrophobic " property for referring to super hydrophobic or forming super hydrophobic, that is, be extremely hard to soak.Make
With the steady contact angle by the droplet formation in solid substrate surface, the quantitative determination of the wetting ability as particular solid it is general
It reads, is also always well known in the industry.Wetting is when making liquid together with the surface of solids since intermolecular interaction produces
The ability raw, liquid maintenance is contacted with the surface of solids.The degree (wettable) of wetting passes through between cohesive force and cohesive force
The balance of power determines.If the steady contact angle of water droplet and substrate surface is greater than 90 °, it is commonly referred to be hydrophobic.For example,
There are the material that drop has high stable contact angle on it, water on such as paraffin, it is about that angle is steadily contacted for which
107°.The hydrophobic coating for the high stable contact angle that many applications need to have greater than 150 °.This type coating is known as super-hydrophobic coat.
A kind of superhydrophobic magnesium alloy surfaces preparation method, using following steps:
(1) magnesium alloy pretreatment is spare；Magnesium alloy materials are cut, the SiC of 400#, 800#, 1200#, 2000# are successively used
It is smooth that sand paper machinery is polished to surface, then with successively with acetone, dehydrated alcohol, deionized water ultrasonic cleaning 5min removal
Metal surface impurity and greasy dirt, drying；
(2) water-soluble organic phospho acid is dissolved in deionized water, water-soluble phosphonic acids is preferably phenyl-phosphonic acid in the present embodiment；
Magnesium alloy materials in step (1) are dipped in water-soluble phosphine acid solution, the substance withdrawl syndrome of water-soluble phosphine acid solution is
0.01-0.1mol/L, preferred concentration 0.1mol/L in the present embodiment, is heated to 95-100 DEG C for water-soluble phosphine acid solution, this reality
Applying heating temperature in example is preferably 100 DEG C, constant temperature 16-24h, and preferred thermostat temperature is for 24 hours in the present embodiment；
(3) magnesium alloy materials in step (2) are taken out from phosphonic acids solution, is cleaned magnesium alloy with deionized water, done
Phosphorated super-hydrophobic coat as depicted in figs. 1 and 2 is obtained after dry.
Embodiment 1
After magnesium alloy materials are cut, light successively is polished to the SiC sand paper machinery of 400#, 800#, 1200#, 2000#
Cunning is smooth, is then successively blown with acetone, dehydrated alcohol, deionized water ultrasonic cleaning 5min removal metal surface impurity and greasy dirt
It is spare after dry；Phenyl-phosphonic acid 0.5269g is weighed, is dissolved in 100ml deionized water, pretreated metal material is dipped in and is prepared
Phenyl-phosphonic acid solution in, take out, dried up after being rinsed well with deionized water, through Contact-angle measurement after 95 DEG C of hydro-thermal reaction 16h
Instrument measurement, coating static contact angle are 151.4 °, and roll angle is 7.6 °.
Embodiment 2
After magnesium alloy materials are cut, light successively is polished to the SiC sand paper machinery of 400#, 800#, 1200#, 2000#
Cunning is smooth, is then successively blown with acetone, dehydrated alcohol, deionized water ultrasonic cleaning 8min removal metal surface impurity and greasy dirt
It is spare after dry；Phenyl-phosphonic acid 0.7905g is weighed, is dissolved in 100ml deionized water, pretreated metal material is dipped in and is prepared
Phenyl-phosphonic acid solution in, take out, dried up after being rinsed well with deionized water, through Contact-angle measurement after 98 DEG C of hydro-thermal reaction 20h
Instrument measurement, coating static contact angle are 154.5 °, and roll angle is 5.4 °.
Embodiment 3
After magnesium alloy materials are cut, light successively is polished to the SiC sand paper machinery of 400#, 800#, 1200#, 2000#
Cunning is smooth, is then successively blown with acetone, dehydrated alcohol, deionized water ultrasonic cleaning 10min removal metal surface impurity and greasy dirt
It is spare after dry；Phenyl-phosphonic acid 1.5809g is weighed, is dissolved in 100ml deionized water, pretreated metal material is dipped in and is prepared
Phenyl-phosphonic acid solution in, 100 DEG C of hydro-thermal reactions are taken out afterwards for 24 hours, dry up after being rinsed well with deionized water, through Contact-angle measurement
Instrument measurement, coating static contact angle are 159.1 °, and roll angle is 2.3 °.
In the present solution, being carried out using coating layer touch angle measuring instrument (German Dataphysics contact angle measurement OCA15EC)
Detection.
What has been described above is only an embodiment of the present invention, and the common sense such as well known specific structure and characteristic are not made herein in scheme
Excessive description.It, without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art
Several modifications and improvements are made, these also should be considered as protection scope of the present invention, these all will not influence what the present invention was implemented
Effect and patent practicability.
Claims (6)
1. a kind of preparation method of superhydrophobic magnesium alloy surfaces, which comprises the following steps:
(1) by AZ31 magnesium alloy mechanical polishing, clean up it is spare；
(2) water-soluble organic phospho acid is dissolved in deionized water, it is molten that the magnesium alloy materials in step (1) are dipped in water-soluble phosphonic acids
In liquid, constant temperature 16-24h；
(3) magnesium alloy materials in step (2) are taken out from phosphonic acids solution, it will be after magnesium alloy cleaning, drying with deionized water
Obtain phosphorated super-hydrophobic coat.
2. a kind of superhydrophobic magnesium alloy surfaces preparation method according to claim 1, which is characterized in that magnesium in step (1)
Alloy material pretreatment includes: to cut magnesium alloy materials, and it is smooth to be polished to surface with SiC sand paper machinery, then with according to
Secondary acetone, dehydrated alcohol, deionized water ultrasonic cleaning 5-10min removal metal surface impurity and greasy dirt, drying.
3. a kind of superhydrophobic magnesium alloy surfaces preparation method according to claim 2, which is characterized in that in step (1) according to
It is secondary to use SiC sand paper 400#, 800#, 1200#, 2000# polishing magnesium alloy.
4. a kind of superhydrophobic magnesium alloy surfaces preparation method according to claim 1, which is characterized in that water in step (2)
Dissolubility phosphonic acids is phenyl-phosphonic acid.
5. a kind of superhydrophobic magnesium alloy surfaces preparation method according to claim 1, which is characterized in that water in step (2)
Dissolubility phosphonic acids solution thermostat temperature is 95-100 DEG C.
6. a kind of superhydrophobic magnesium alloy surfaces preparation method according to claim 1, which is characterized in that the water of step (2)
The substance withdrawl syndrome of dissolubility phosphonic acids solution is 0.01-0.1mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910507504.5A CN110129780A (en) | 2019-06-12 | 2019-06-12 | A kind of superhydrophobic magnesium alloy surfaces preparation method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910507504.5A CN110129780A (en) | 2019-06-12 | 2019-06-12 | A kind of superhydrophobic magnesium alloy surfaces preparation method |
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| CN110129780A true CN110129780A (en) | 2019-08-16 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112775561A (en) * | 2020-12-31 | 2021-05-11 | 华东交通大学 | Pyrolytic carbon mechanical valve leaflet with two-stage pattern on surface and preparation method thereof |
| CN113278956A (en) * | 2021-04-22 | 2021-08-20 | 华东交通大学 | Preparation method of super-hydrophobic copper mercaptan on surface of magnesium alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014012052A1 (en) * | 2012-07-13 | 2014-01-16 | President And Fellows Of Harvard College | Slips surface based on metal-containing compound |
| CN105420788A (en) * | 2015-11-27 | 2016-03-23 | 福州大学 | Pure-magnesium or magnesium alloy surface water repelling micro-arc oxidation coating and preparing method thereof |
| CN105463461A (en) * | 2015-12-03 | 2016-04-06 | 大连理工大学 | Preparing method of three-dimensional network super-hydrophobic surface |
| KR20160037274A (en) * | 2014-09-26 | 2016-04-06 | 경기대학교 산학협력단 | Super-Hydrophobic Particle and Composite having the Same |
-
2019
- 2019-06-12 CN CN201910507504.5A patent/CN110129780A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014012052A1 (en) * | 2012-07-13 | 2014-01-16 | President And Fellows Of Harvard College | Slips surface based on metal-containing compound |
| KR20160037274A (en) * | 2014-09-26 | 2016-04-06 | 경기대학교 산학협력단 | Super-Hydrophobic Particle and Composite having the Same |
| CN105420788A (en) * | 2015-11-27 | 2016-03-23 | 福州大学 | Pure-magnesium or magnesium alloy surface water repelling micro-arc oxidation coating and preparing method thereof |
| CN105463461A (en) * | 2015-12-03 | 2016-04-06 | 大连理工大学 | Preparing method of three-dimensional network super-hydrophobic surface |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112775561A (en) * | 2020-12-31 | 2021-05-11 | 华东交通大学 | Pyrolytic carbon mechanical valve leaflet with two-stage pattern on surface and preparation method thereof |
| CN113278956A (en) * | 2021-04-22 | 2021-08-20 | 华东交通大学 | Preparation method of super-hydrophobic copper mercaptan on surface of magnesium alloy |
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