CN110747453A - Magnesium workpiece surface spraying liquid and application thereof - Google Patents
Magnesium workpiece surface spraying liquid and application thereof Download PDFInfo
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- CN110747453A CN110747453A CN201911128570.8A CN201911128570A CN110747453A CN 110747453 A CN110747453 A CN 110747453A CN 201911128570 A CN201911128570 A CN 201911128570A CN 110747453 A CN110747453 A CN 110747453A
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- 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
- C23C22/06—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 using aqueous acidic solutions with pH less than 6
- C23C22/07—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 using aqueous acidic solutions with pH less than 6 containing phosphates
- C23C22/08—Orthophosphates
- C23C22/20—Orthophosphates containing aluminium cations
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- 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
- C23C22/73—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 characterised by the process
- C23C22/76—Applying the liquid by spraying
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Abstract
The invention provides a magnesium workpiece surface spraying liquid and a method for preparing a durable super-amphiphobic surface of a magnesium workpiece by using the spraying liquid. The magnesium workpiece surface spraying liquid does not contain fluorine, silicon, rubber, resin and various micro/nano fillers, is environment-friendly in components and does not cause the problem of compatibility; the spraying liquid is uniformly sprayed on the surface of a clean magnesium workpiece, and then the durable super-amphiphobic surface of the magnesium workpiece can be obtained through proper curing treatment. The magnesium workpiece prepared by the method has good super-amphiphobic surface durability, can be subjected to various severe tests such as friction and abrasion, ultraviolet radiation, high-pressure water column impact, strong acid and strong base, organic solvent soaking, strong corrosive medium soaking and the like, and is expected to greatly widen the application field of magnesium materials. The method is suitable for processing magnesium and magnesium alloy workpieces with various sizes and shapes. The method has the characteristics of simple process, convenient operation, environmental protection, easy large-scale industrial treatment and the like.
Description
Technical Field
The invention belongs to the technical field of surface engineering, and particularly relates to magnesium workpiece surface spraying liquid and a method for preparing a durable super-amphiphobic surface of a magnesium workpiece by using the same.
Background
The magnesium material has the advantages of high specific strength and specific rigidity, good damping property, machinability, thermal conductivity, strong electromagnetic shielding capability and the like, is known as a green engineering material with the most development potential and future in the 21 st century, and has wide application prospect in a plurality of fields. However, the magnesium alloy is very active in chemical property, and the natural oxide film on the surface of the magnesium alloy is loose and porous and basically has no protection effect, so that the magnesium alloy is promoted to be widely applied only by improving the durability of the surface of the magnesium alloy through proper surface treatment.
Due to the special wettability of both super-hydrophobic and super-oleophobic surfaces, compared with a single super-hydrophobic surface, the super-amphiphobic surface has more excellent capabilities of self-cleaning, corrosion prevention, stain resistance, drag reduction and the like, and has attracted extensive attention in recent years. At present, great progress is made in preparing super-amphiphobic surfaces on materials such as glass, ceramics, wood, cement, building exterior walls, paper products, plastics, various textiles and the like. For metallic materials, however, it is relatively difficult to prepare a super-amphiphobic surface because of their generally active chemical properties. Through a great deal of research and study, at present, for oil pipelines/pipelines and zinc, copper and aluminum which are relatively stable metal materials, a small amount of invention patents for preparing the super-amphiphobic surface exist, for example, a preparation method of the durable super-amphiphobic surface of the high-strength aluminum alloy ZL201711106428.4 provides a method for preparing the durable super-amphiphobic surface on the Al-Zn-Mg-Cu series high-strength aluminum alloy.
However, magnesium materials are more chemically active than oil pipelines/lines, metals such as zinc, copper, aluminum, etc., which greatly increases the difficulty of preparing durable super-amphiphobic surfaces thereon. In addition, the preparation of the existing super-amphiphobic surface usually needs substances with large pollution such as fluorine, silicon, rubber, resin and the like, and inorganic/organic nano particles, nano fiber micro-polymers, nano fillers, submicron particles, microspheres and the like are added to increase the roughness or a specific micro/nano structure is constructed in a single step to increase the roughness, so that the preparation process is complicated and has large pollution, and the problems of poor binding force of a surface film layer, poor compatibility, easy cracking and the like are often caused, and the durability of the surface is seriously influenced. Therefore, the research and development of the durable super-amphiphobic surface preparation technology aiming at the magnesium material is simple, convenient, efficient and environment-friendly and has great significance for promoting the wide application of the magnesium alloy.
Disclosure of Invention
Aiming at the difficulties and problems in the prior art, the invention aims to provide a magnesium workpiece surface spraying liquid and a method for preparing a durable super-amphiphobic surface of a magnesium workpiece based on the spraying liquid.
The invention adopts the following technical scheme:
the preparation method of the magnesium workpiece surface spraying liquid comprises the following steps:
① diluting 500-750 ml of concentrated phosphoric acid to 1L, then ultrasonically dispersing 150-250 g of aluminum hydroxide in the concentrated phosphoric acid, and stirring for 3-5 hours at 85-100 ℃ to obtain a solution A;
② adding 10-30 ml of nonanoic acid and 70-90 ml of nonanol into 900ml of absolute ethyl alcohol, and stirring for 1-2 hours at normal temperature to obtain a solution B;
③ mixing 400ml of the solution A with 600ml of the solution B, and stirring for 0.5-1.5 hours at normal temperature to obtain the magnesium workpiece surface spraying liquid.
Furthermore, the invention also provides application of the magnesium workpiece surface spraying liquid, and the spraying liquid is used for preparing the durable super-amphiphobic surface of the magnesium workpiece.
Further, the method for preparing the durable super-amphiphobic surface of the magnesium workpiece comprises the following steps:
1, spray coating treatment: and uniformly spraying the spraying liquid on the surface of a clean magnesium workpiece, wherein the ratio of the volume of the spraying liquid to the area of the treated part of the magnesium workpiece is 1L: 20 to 30m2；
②, curing the sprayed magnesium workpiece at 120-150 ℃ for 1-2 hours, and further heating to 240-300 ℃ for continuous curing for 0.5-1 hour to obtain the durable super-amphiphobic surface of the magnesium workpiece.
The magnesium workpiece is pure magnesium or various magnesium alloys and is not limited by shape and size.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the preparation method of the magnesium workpiece surface spraying liquid, concentrated phosphoric acid, aluminum hydroxide, pelargonic acid, nonanol and absolute ethyl alcohol are used as basic raw materials, fluorine, silicon, rubber, resin and various micro/nano fillers are not contained, the components are environment-friendly, and the compatibility problem is not caused; the preparation process is simple, the operation is convenient, and special experimental conditions such as high voltage, electrification and the like are not needed; is easy for industrialized production.
2. The invention skillfully utilizes the extremely active chemical activity of the magnesium material, and the magnesium material and the components in the spraying liquid are subjected to chemical reaction during curing to form firm chemical bonds, and meanwhile, the product has a specific micro/nano structure, thereby meeting the requirement of roughness required for preparing the super-amphiphobic surface and overcoming the problems of poor compatibility, easy cracking, non-durability and the like of a film layer caused by the increased roughness of inorganic/organic nano particles, nano fiber micro-polymers, nano fillers, submicron particles, microspheres and the like used in the existing super-amphiphobic coating. In addition, the specific micro/nano structure is constructed and the surface energy is reduced synchronously in the process of preparing the super-amphiphobic surface by the method, so that the problems of complicated preparation process, large pollution and the like caused by the fact that the specific micro/nano structure is constructed in a single step to increase the roughness in the preparation of the super-amphiphobic surface by a plurality of patent technologies at present are solved.
3. The magnesium workpiece prepared by the method has good super-amphiphobic surface durability, can be subjected to various severe tests such as friction and abrasion, ultraviolet radiation, high-pressure water column impact, strong acid and strong base, organic solvent soaking, strong corrosive medium soaking and the like, and is expected to greatly widen the application field of magnesium materials. The method is suitable for processing magnesium and magnesium alloy workpieces with various sizes and shapes, and has the characteristics of simple process, convenience in operation, greenness, environmental friendliness, easiness in large-scale industrial processing and the like.
Drawings
FIG. 1 is SEM scanning electron microscope image of specific micro/nano structure generated on the surface of magnesium material of the invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
It should be noted that these examples are only for illustrating the present invention, and not for limiting the present invention, and the simple modification of the method based on the idea of the present invention is within the protection scope of the present invention.
Processing pure magnesium or different magnesium alloys into magnesium workpieces with different sizes and shapes according to requirements, sequentially polishing the magnesium workpieces with 180#, 400# and 800# abrasive paper until the surfaces are smooth and flat, washing the magnesium workpieces with pure water, ultrasonically cleaning the magnesium workpieces in absolute ethyl alcohol for 5 minutes, taking the magnesium workpieces out, and drying the magnesium workpieces with cold air to obtain the workpieces with clean surfaces.
Example 1:
the preparation method of the surface spraying liquid of the pure magnesium workpiece (a wafer with the diameter of 20mm and the thickness of 5.0 mm) comprises the following specific steps:
① diluting 500ml concentrated phosphoric acid to 1L, then dispersing 150g aluminium hydroxide in it by ultrasonic wave, stirring 4 hours at 85 deg.C to get solution A;
② adding 10ml pelargonic acid and 90ml pelargonic alcohol into 900ml absolute ethyl alcohol, stirring for 2 hours at normal temperature to obtain solution B;
③ mixing 400ml of the solution A with 600ml of the solution B, and stirring for 0.5 hour at normal temperature to obtain the magnesium workpiece surface spraying solution.
The spray coating liquid is applied to prepare the durable super-amphiphobic surface of the pure magnesium workpiece, and the method comprises the following specific steps:
① spraying, namely uniformly spraying the spraying liquid on the surface of a clean pure magnesium workpiece, wherein the ratio of the volume of the spraying liquid to the area of the treated part of the pure magnesium workpiece is 1L: 30m2；
②, curing the sprayed pure magnesium workpiece at 150 ℃ for 1 hour, and further heating to 240 ℃ for continuous curing for 1 hour to obtain the durable super-amphiphobic surface of the pure magnesium workpiece.
The procedure for testing the durable super-amphiphobic surface was as follows (same for the other examples):
a. super-amphiphobic function test static contact angles and rolling angles of 2 mu L of water drops (pure water) and oil drops (n-hexane) on the surface of a magnesium workpiece are measured by a German Dataphysics OCA20 video optical contact angle measuring instrument to evaluate the hydrophobic and oleophobic functions of the magnesium workpiece, the surface with the static contact angle larger than 150 degrees and the rolling angle smaller than 10 degrees is considered as a super-hydrophobic surface, and the larger the static contact angle is, the smaller the rolling angle is, the better the super-hydrophobic effect is.
b. The durability test adopts a friction wear test, an ultraviolet light radiation test, a high-pressure water column impact test, a strong acid and strong base test, an organic medium soaking test and a strong corrosive medium soaking test to test the durability of the super-amphiphobic surface of the magnesium workpiece, the changes of the static contact angle and the rolling angle of water and oil on the surface of the workpiece before and after the test are tested, if the changes are less than 10 degrees, the durability of the super-amphiphobic surface of the magnesium workpiece is excellent, and the smaller the change is, the better the durability is.
The specific detection method comprises the following steps:
(1) friction and wear test: spreading No. 200 metallographic abrasive paper on a table, contacting one surface of the magnesium workpiece treated by the method with abrasive paper (the surface is a working surface), applying a fixed pressure of 1.0kPa, a dragging distance of 2 meters and a dragging speed of 5mms-1And dragging the workpiece horizontally and longitudinally for 50 times respectively to test the changes of the static contact angle and the rolling angle of water and oil on the surface of the workpiece before and after the friction and wear test.
(2) Ultraviolet radiation test: the magnesium workpiece treated by the method is subjected to ultraviolet radiation, the wavelength of an ultraviolet light source is 254nm, the power is 10W, the workpiece is placed 2cm away from the light source, the radiation time is 28 days, and the changes of the static contact angle and the rolling angle of water and oil on the surface of the workpiece before and after an ultraviolet radiation test are tested.
(3) The magnesium workpiece treated by the method is subjected to high-pressure water column impact test, the water pressure is 300kPa, the release height is 2 meters, the high-pressure water column impact test is continuously carried out for 10 hours, and the changes of the static contact angle and the rolling angle of water and oil on the surface of the workpiece before and after the high-pressure water column impact test are tested.
(4) Strong acid and strong base test: the magnesium workpiece treated by the method of the invention is respectively immersed in 1.0mol/L nitric acid solution (pH is 1) and 1.0mol/L sodium hydroxide solution (pH is 14) for 48 hours, and the changes of the static contact angle and the rolling angle of water and oil on the surface of the workpiece before and after the strong acid and strong base test are tested.
(5) In the organic solvent soaking test, the magnesium workpiece treated by the method is respectively immersed in ethanol, acetone and n-hexane for 480 hours at room temperature, and the changes of the static contact angle and the rolling angle of water and oil on the surface of the workpiece before and after the organic solvent soaking test are tested.
(6) In the strong corrosion medium immersion test, the magnesium workpiece treated by the method is immersed in 3.5 wt% sodium chloride corrosion medium with the pH value of 3.2 +/-0.1 (adjusted by glacial acetic acid) at 35 +/-2 ℃ for 960 hours, and the changes of the static contact angle and the rolling angle of water and oil on the surface of the workpiece before and after the strong corrosion medium immersion test are tested.
The test result of the super-amphiphobic function and the durability thereof shows that: the surface of the pure magnesium workpiece treated by the method is a super-amphiphobic surface: the static contact angle and the rolling angle of the water drop on the surface are respectively 158 degrees and 1 degree, and the static contact angle and the rolling angle of the oil drop on the surface are respectively 155 degrees and 2 degrees; the changes of the static contact angle and the rolling angle of water and oil on the surface of the workpiece before and after a friction wear test, an ultraviolet light radiation test, a high-pressure water column impact test, a strong acid and strong base test, an organic medium soaking test and a strong corrosion medium soaking test are all less than 3 degrees, and the excellent durability is shown.
The invention skillfully utilizes the extremely active chemical activity of the magnesium material, and the magnesium material and the components in the spraying liquid are subjected to chemical reaction during curing to form firm chemical bonds, and meanwhile, the product has a specific micro/nano structure (shown as an attached figure 1), so that the roughness required for preparing the super-amphiphobic surface is met, and the problems of poor compatibility, easy cracking, non-durability and the like of a film layer caused by the fact that inorganic/organic nano particles, nano fiber micro-polymers, nano fillers, submicron particles, microspheres and the like are used for increasing the roughness in the existing super-amphiphobic coating are solved. In addition, the specific micro/nano structure is constructed and the surface energy is reduced synchronously in the process of preparing the super-amphiphobic surface by the method, so that the problems of complicated preparation process, large pollution and the like caused by the fact that the specific micro/nano structure is constructed in a single step to increase the roughness in the preparation of the super-amphiphobic surface by a plurality of patent technologies at present are solved.
Example 2:
the preparation method of the surface spraying liquid of the AZ31 magnesium alloy workpiece (a rectangular plate with the thickness of 1.0m multiplied by 0.5m multiplied by 3.0 mm) comprises the following specific steps:
① diluting 750ml concentrated phosphoric acid to 1L, then dispersing 250g aluminium hydroxide in it by ultrasonic wave, stirring 5 hours at 100 deg.C to get solution A;
② adding 30ml pelargonic acid and 70ml pelargonic alcohol into 900ml absolute ethyl alcohol, stirring for 1 hour at normal temperature to obtain solution B;
③ mixing 400ml of the solution A with 600ml of the solution B, and stirring for 1.5 hours at normal temperature to obtain the magnesium workpiece surface spraying solution.
The spray coating liquid is applied to prepare the durable super-amphiphobic surface of the AZ31 magnesium alloy workpiece, and the method comprises the following specific steps:
① spraying, namely uniformly spraying the spraying liquid on the surface of a clean AZ31 magnesium alloy workpiece, wherein the ratio of the volume of the spraying liquid to the area of the processed part of the AZ31 magnesium alloy workpiece is 1L: 20m2；
②, curing the AZ31 magnesium alloy workpiece after spraying treatment at 120 ℃ for 2 hours, and further heating to 300 ℃ for continuous curing treatment for 0.5 hour to obtain the durable super-amphiphobic surface of the AZ31 magnesium alloy workpiece.
The test result of the super-amphiphobic function and the durability thereof shows that: the surface of the AZ31 magnesium alloy workpiece treated by the method is a super-amphiphobic surface: the static contact angle and the rolling angle of the water drop on the surface are respectively 156 degrees and 2 degrees, and the static contact angle and the rolling angle of the oil drop on the surface are respectively 153 degrees and 3 degrees; the changes of the static contact angle and the rolling angle of water and oil on the surface of the workpiece before and after a friction wear test, an ultraviolet light radiation test, a high-pressure water column impact test, a strong acid and strong base test, an organic medium soaking test and a strong corrosion medium soaking test are all less than 5 degrees, and the excellent durability is shown.
Example 3:
the preparation method of the surface spraying liquid of the AZ61 magnesium alloy workpiece (a square plate with the thickness of 20cm multiplied by 4.0 mm) comprises the following specific steps:
① diluting 600ml concentrated phosphoric acid to 1L, then dispersing 200g aluminium hydroxide in it by ultrasonic wave, stirring for 3 hours at 90 deg.C to obtain solution A;
② adding 20ml pelargonic acid and 80ml pelargonic alcohol into 900ml absolute ethyl alcohol, stirring for 1.5 hours at normal temperature to obtain solution B;
③ mixing 400ml of the solution A with 600ml of the solution B, and stirring for 1.0 hour at normal temperature to obtain the magnesium workpiece surface spraying solution.
The spray coating liquid is applied to prepare the durable super-amphiphobic surface of the AZ61 magnesium alloy workpiece, and the method comprises the following specific steps:
① spraying, namely uniformly spraying the spraying liquid on the surface of a clean AZ61 magnesium alloy workpiece, wherein the ratio of the volume of the spraying liquid to the area of the processed part of the AZ61 magnesium alloy workpiece is 1L: 25m2；
②, curing the AZ61 magnesium alloy workpiece after spraying treatment at 130 ℃ for 1.5 hours, and further heating to 270 ℃ to continue curing for 1 hour to obtain the durable super-amphiphobic surface of the AZ61 magnesium alloy workpiece.
The test result of the super-amphiphobic function and the durability thereof shows that: the surface of the AZ61 magnesium alloy workpiece treated by the method is a super-amphiphobic surface: the static contact angle and the rolling angle of the water drop on the surface are 157 degrees and 2 degrees respectively, and the static contact angle and the rolling angle of the oil drop on the surface are 154 degrees and 2 degrees respectively; the changes of the static contact angle and the rolling angle of water and oil on the surface of the workpiece before and after a friction wear test, an ultraviolet light radiation test, a high-pressure water column impact test, a strong acid and strong base test, an organic medium soaking test and a strong corrosion medium soaking test are all less than 4 degrees, and the excellent durability is shown.
Claims (4)
1. The magnesium workpiece surface spraying liquid is characterized in that the preparation method comprises the following steps:
① diluting 500-750 ml of concentrated phosphoric acid to 1L, then ultrasonically dispersing 150-250 g of aluminum hydroxide in the concentrated phosphoric acid, and stirring for 3-5 hours at 85-100 ℃ to obtain a solution A;
② adding 10-30 ml of nonanoic acid and 70-90 ml of nonanol into 900ml of absolute ethyl alcohol, and stirring for 1-2 hours at normal temperature to obtain a solution B;
③ mixing 400ml of the solution A with 600ml of the solution B, and stirring for 0.5-1.5 hours at normal temperature to obtain the magnesium workpiece surface spraying liquid.
2. Use of the spray coating solution according to claim 1 for the preparation of durable super-amphiphobic surfaces of magnesium workpieces.
3. The use of the magnesium workpiece surface spray coating solution according to claim 1, wherein the method for preparing the durable super-amphiphobic surface of the magnesium workpiece comprises the following steps:
① spraying, namely uniformly spraying the spraying liquid obtained in the claim 1 on the surface of a clean magnesium workpiece, wherein the ratio of the volume of the spraying liquid to the area of the treated part of the magnesium workpiece is 1L: 20-30 m2；
②, curing, namely curing the magnesium workpiece sprayed in the step ① at 120-150 ℃ for 1-2 hours, and further heating to 240-300 ℃ for continuous curing for 0.5-1 hour to obtain the durable super-amphiphobic surface of the magnesium workpiece.
4. The use of the magnesium workpiece surface spray coating solution according to claim 3, wherein the magnesium workpiece is pure magnesium or various magnesium alloys and is not limited by shape and size.
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| JP2015004136A (en) * | 2007-12-14 | 2015-01-08 | 株式会社ネオス | Method for forming a corrosion resistant film on a zinc metal surface |
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| CN102418098A (en) * | 2011-09-16 | 2012-04-18 | 东南大学 | Low-damage preparation method of super-hydrophobic surface of industrial aluminum foil |
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