CN112126264B - Magnesium alloy anticorrosion and wear-resistant coating composition and use method thereof - Google Patents
Magnesium alloy anticorrosion and wear-resistant coating composition and use method thereof Download PDFInfo
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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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
- B05D1/00—Processes for applying liquids or other fluent materials
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- 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
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- 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
- B05D3/02—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 by baking
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- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention relates to the technical field of magnesium alloy surface protection, in particular to a magnesium alloy surface anti-corrosion wear-resistant coating composition and a using method thereof. The magnesium alloy anticorrosion and wear-resistant coating composition comprises the following components in percentage by mass: 0.05-5% of graphene oxide, 0.1-7.5% of modified siloxane, 0.05-1% of surfactant and a dispersing agent: 86.5 to 99.8 percent, and obtaining the anticorrosive and wear-resistant coating after mixing; the modified siloxane is prepared by taking unsaturated fatty acid and mercapto siloxane as main raw materials, adding a photoinitiator, and reacting under the illumination of ultraviolet rays, and when the coating is coated on the surface of the magnesium alloy, the coating not only can obviously improve the adhesive force of the coating and the surface of magnesium and magnesium alloy, but also can improve the corrosion resistance and wear resistance of the surface of the magnesium alloy, and has positive application value.
Description
The technical field is as follows:
the invention relates to the technical field of magnesium alloy surface protection, in particular to a magnesium alloy surface anti-corrosion wear-resistant coating composition and a using method thereof.
Technical background:
the magnesium alloy has a plurality of excellent performances such as light specific gravity, low density, high specific strength/specific stiffness, good biocompatibility, good processability and the like, and has wide application prospects in the fields of electronic industry, automobiles, aerospace, biomedical treatment and the like. However, the chemical activity of magnesium alloy is relatively active, which limits the application of magnesium and its alloy. Magnesium alloy has poor corrosion resistance, and although magnesium can form an oxide film on the surface in air, the oxide film is loose and porous, and the corrosion resistance is not ideal. In addition, because the magnesium alloy has low hardness, the magnesium alloy is easy to scratch and wear in practical use, which severely limits the application and popularization of the magnesium alloy. Therefore, the improvement of corrosion resistance and wear resistance is the key to the improvement of the performance of the magnesium alloy material.
Currently, many methods have been developed to improve the wear resistance of magnesium alloys, including electroplating, electroless plating, micro-arc oxidation, organic/inorganic coating, etc. However, these methods have many disadvantages. Electron beam physical vapor deposition is performed in a vacuum state, large workpieces and complex parts are difficult to process, and industrial scale is difficult to realize. Thermal spraying often requires the use of plasma or laser devices, which can be costly and difficult to maintain. The plating solution used in electroplating and chemical plating is often seriously polluted and is limited to use. Compared with other technologies, the organic/inorganic coating has the advantages of low cost, low toxicity, no pollution, simple operation, uniform coating, strong material adaptability and the like, and is gradually applied to the field of magnesium alloy surface protection. Graphene Oxide (GO) is a typical two-dimensional material with good chemical and physical properties and excellent mechanical properties, making it widely used in anti-corrosion coatings and lubrication. The functional groups on GO (e.g., -OH, epoxy, and-COOH) help to improve the compatibility of GO with other materials. Liang et al [ h.y.liang, y.f.bu, j.y.zhang, z.y.cao, a.m.liang.graphene oxide film as solid solution coating. acs appl.mater.inter.2013,5:6369-6375 ] prepared a GO film on a silicon-based MEMS device by electrophoretic deposition. The results show that: when the GO film is used as a solid lubricating film, the friction and wear resistance of silicon-based MEMS devices are improved. However, in most processes, the bonding of GO on the substrate surface is very weak. The graphene oxide compounded long-chain carbon-chain fatty acid can improve the corrosion resistance of the surface of the magnesium alloy. Chenning et al [ Chenning, Wang Yan Hua et al, graphene/stearic acid super-hydrophobic composite film layer corrosion resistance, materials research report 2017,31(10): 751-. However, the film prepared by the method has the same weak adhesion with the surface of the magnesium alloy. Therefore, it is required to introduce a transition layer having a specific functional group to improve its adhesive strength. It is reported that CN103628050B discloses a coating compounded by graphene oxide and organic siloxane, chemical bond linkage between metal and graphene is realized by siloxane coupling agent, and the bonding force between the substrate and graphene or multi-layer graphene can be improved, but only the research on the corrosion resistance of metal is involved, the wear resistance of the coating to magnesium alloy substrate is not researched, and finally, hydrazine hydrate is also required to be introduced.
Therefore, how to obtain a compact and uniform protective coating which not only has excellent chemical stability, but also is well combined with the surface of the magnesium alloy, and the corrosion resistance and the wear resistance of the surface of the magnesium alloy are obviously improved, which is the technical problem to be solved by the invention.
The invention content is as follows:
in view of the above problems, the present invention provides an organic-inorganic hybrid composition for improving corrosion resistance and wear resistance of magnesium alloy and a method of using the same.
The technical scheme is as follows:
the magnesium alloy anti-corrosion and wear-resistant composition is coated on the surface of a magnesium workpiece and is formed by drying and curing.
The coating forming composition consists of the following components in percentage by mass:
0.05 to 5 percent of graphene oxide
0.1 to 7.5 percent of modified siloxane
0.05 to 1 percent of surfactant
Dispersing agent: 86.5 to 99.8 percent
The graphene oxide is prepared by adopting an improved Hummers method, and functional groups such as hydroxyl, carboxyl, epoxy and the like are introduced into a graphene structure. The graphene oxide is too much in dosage, is not easy to disperse, is easy to settle, and cannot achieve the application effect when being too little. The dosage of the graphene oxide is preferably 0.05% -5%. More preferably 0.5% to 2.5%.
Further, the magnesium alloy anti-corrosion and wear-resistant coating at least contains one modified siloxane; the preparation method of the modified siloxane is characterized in that the modified siloxane is prepared by adopting the unsaturated fatty acid and the siloxane containing sulfydryl as main raw materials and benzoin dimethyl ether as an initiator (1-3% of the mass of the raw materials) and reacting under the illumination of ultraviolet rays.
Wherein the mass ratio of the unsaturated fatty acid to the mercapto siloxane is 1-1.5: 1.
The unsaturated fatty acid is an organic acid having a long carbon chain containing a double bond in the molecular chain, and may be an unsaturated fatty acid having one double bond in the molecular chain, such as cis-5-dodecenoic acid, myristoleic acid, oleic acid, linoleic acid, mesonic acid, or arachidic acid, or an unsaturated fatty acid having a plurality of double bonds in the molecular chain, such as arachidonic acid, eicosapentaenoic acid, or docosahexaenoic acid. Preferably, the unsaturated fatty acid has one double bond in the molecular chain, and more preferably, oleic acid.
Further, the siloxane containing sulfydryl can be one or two of mercaptopropyl trimethoxy silane and mercaptopropyl triethoxy siloxane;
furthermore, from the perspective of improving corrosion resistance and wear resistance of the surface of the magnesium alloy and improving adhesion, the dosage of the modified siloxane is preferably 0.5-7.5%; more preferably 1% to 5%.
The modified siloxane prepared by the invention can be diffused to the surface of graphene oxide or permeate between graphene oxide lamella, so that the aim of preventing water molecules and corrosive anions from permeating into a substrate through nano holes on the surface of the graphene oxide and lamella gaps is fulfilled. The unsaturated fatty acid of the long carbon chain fatty chain improves the surface wear resistance of the magnesium alloy, and more importantly, the modified siloxane can also improve the adhesion between the coating and the surface of the magnesium alloy.
Furthermore, the surfactant in the magnesium alloy surface treatment composition is a nonionic surfactant, and the surfactant not only promotes the dispersion of the graphene oxide and the modified siloxane, but also can improve the wettability of the surfactant on the magnesium alloy substrate and improve the treatment uniformity. Preferably, the surfactants suitable for the present invention are alkyl alcohol polyoxyethylene ethers, alkyl acid ester polyoxyethylene ethers, alkylamine polyoxyethylene ethers; according to a characteristic of the invention, the alkyl radical of the surfactant contains at least 5 to 25 carbon atoms, the alkyl radical may be saturated or unsaturated, and the hydrophilic segment of the surfactant has at least 5 to 15 ethylene oxide repeating units. The surfactant in the composition is preferably an oleate polyoxyethylene ether (e.g. sorbitan monooleate polyoxyethylene ether). The dosage of the surfactant is preferably 0.05% -1%, and more preferably 0.1% -0.5%; if the surface active amount is too high, the water absorption of the coating is improved, the corrosion resistance is reduced, and if the surface active amount is too small, the dispersion assisting effect cannot be achieved.
Furthermore, the dispersing agent is a water-alcohol solvent, on one hand, the dispersing agent can be used as a dispersing carrier of graphene oxide and modified siloxane, on the other hand, the dispersing agent can also adjust the hydrolysis rate of siloxane functional groups, and the stability of the whole treatment process is improved. The carbon chain length of the alcohol solvent is monohydric alcohol, dihydric alcohol or trihydric alcohol with 1-8 carbon atoms; the alcoholic solvent may be one or a mixture of several. Ethanol or isopropanol is preferred from the viewpoint of safety and environmental protection. The amount of organic solvent is preferably 86.5% to 99.8%, more preferably 92% to 98.4%.
In order to improve the curing speed of the coating, acetic acid can be contained in the coating composition in a trace amount as a catalyst. If necessary, the composition can be added with other auxiliary components.
Under the action of a high-speed disperser, uniform and stable dispersion liquid is obtained according to the required components and proportions, namely the magnesium alloy surface anti-corrosion and wear-resistant composition. The use method of the composition comprises the following steps:
(1) grinding, polishing and degreasing the magnesium alloy, then carrying out hydroxylation treatment on the surface of the magnesium alloy by using alkali liquor (6mol/L sodium hydroxide solution), cleaning and drying for later use;
(2) and (2) coating the composition on the magnesium alloy sheet pretreated in the step (1) by adopting a spin-coating method, and drying the magnesium alloy sheet in an oven at 120 ℃ for 2h to form an anticorrosive and wear-resistant coating on the surface of the magnesium alloy.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides an anticorrosive and wear-resistant composition for a magnesium alloy surface and a use method thereof. The composition is prepared by compounding oleic acid modified siloxane and graphene oxide, the corrosion resistance and the wear resistance of the surface of the magnesium alloy can be improved through the synergistic effect of the graphene oxide and long-chain unsaturated fatty acid, and the adhesive force of a coating and the surface of magnesium and magnesium alloy is improved by introducing reactive siloxane groups into unsaturated fatty acid molecules. In addition, the anti-corrosion and wear-resistant composition for the surface of the magnesium alloy is simple to produce and prepare and convenient to construct.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to specific examples, which are provided for illustration only and are not intended to limit the scope of the present invention. The process parameters, modes of operation and methods of detection not mentioned in the examples below are all conventional parameters available to the person skilled in the art using routine limited trials.
Pretreatment of the surface of the magnesium alloy:
a5 cm multiplied by 5cm test piece made of AZ31 magnesium alloy is sequentially polished by 800#, 1400# and 2000# abrasive paper, polished by a polishing machine, the granularity of polishing paste is 2.5M, the polished magnesium alloy is sequentially ultrasonically cleaned by acetone, alcohol and deionized water for 5 minutes and then dried, alkaline washing pretreatment is carried out by 6mol/L NaOH aqueous solution for 6 hours, and drying is carried out for standby.
Example 1
(1) Preparation of modified siloxane:
weighing 56.2g of oleic acid and 39.3g of mercaptopropyl trimethoxysilane, uniformly mixing, and reacting for 2 hours at normal temperature by adopting ultraviolet light by using benzoin dimethyl ether as a photoinitiator to obtain the modified siloxane A.
(2) Preparation of anticorrosive and wear-resistant composition:
0.5g (0.5%) of sorbitan monooleate polyoxyethylene ether, 7.5g (7.5%) of modified siloxane A and 89.5g (89.5%) of ethanol are weighed and mixed uniformly, and 2.5g (2.5%) of graphene oxide (purchased from graphene research institute in south of the Yangtze river) is slowly added to form a uniform dispersion liquid under the condition of high-speed stirring.
(3) Preparing a coating:
and (3) spin-coating the dispersion liquid obtained in the step (2) on the surface of the pretreated magnesium alloy by using a spin-coating instrument, wherein the spin-coating parameters are as follows: the low speed was 500rpm for 10s, the high speed was 1500rpm for 20 s. And putting the spin-coated magnesium alloy sample into an oven to be dried for 2h at 120 ℃ for curing.
Example 2
(1) Preparation of modified siloxane:
modified siloxane A was prepared in the same manner as in example 1.
(2) Preparation of anticorrosive and wear-resistant composition:
0.05g (0.05%) of sorbitan monooleate polyoxyethylene ether, 5g (5.0%) of modified siloxane A and 94.9g (94.9%) of isopropanol are weighed and uniformly mixed, and 0.05g (0.05%) of graphene oxide is slowly added under the condition of high-speed stirring to form uniform dispersion liquid.
(3) Preparing a coating:
and (3) spin-coating the dispersion liquid obtained in the step (2) on the surface of the pretreated magnesium alloy by using a spin-coating instrument, wherein the spin-coating parameters comprise 500rpm at a low speed for 10s, 1500rpm at a high speed for 20 s. And putting the spin-coated magnesium alloy sample into an oven to be dried for 2h at 120 ℃ for curing.
EXAMPLE 3 (best mode)
(1) Preparation of modified siloxane:
weighing 56.2g of oleic acid and 47.7g of mercaptopropyltriethoxysilane, uniformly mixing, and reacting for 2 hours at normal temperature by adopting ultraviolet light by using benzoin dimethyl ether as a photoinitiator to obtain modified siloxane B;
(2) preparation of anticorrosive and wear-resistant composition:
0.1g (0.1%) of sorbitan monooleate polyoxyethylene ether, 0.1% of modified siloxane B1g (1%) and 97.9g (97.9%) of ethanol are weighed and uniformly mixed, and 1g (1%) of graphene oxide is slowly added under the condition of high-speed stirring to form uniform dispersion liquid.
(3) Preparing a coating:
and (3) spin-coating the dispersion liquid obtained in the step (2) on the surface of the pretreated magnesium alloy by using a spin-coating instrument, wherein the spin-coating parameters comprise 500rpm at a low speed for 10s, 1500rpm at a high speed for 20 s. And putting the spin-coated magnesium alloy sample into an oven to be dried for 2h at 120 ℃ for curing.
Example 4
(1) Preparation of modified siloxane:
modified siloxane A was prepared in the same manner as in example 3.
(2) Preparation of anticorrosive and wear-resistant composition:
weighing 1g (1%) of sorbitan monooleate polyoxyethylene ether, 0.1g (0.1%) of modified siloxane A and 93.9g (93.9%) of isopropanol, uniformly mixing, and slowly adding 5g (5%) of graphene oxide under the condition of high-speed stirring to form a uniform dispersion liquid.
(3) Preparing a coating:
and (3) spin-coating the dispersion liquid obtained in the step (2) on the surface of the pretreated magnesium alloy by using a spin-coating instrument, wherein the spin-coating parameters comprise 500rpm at a low speed for 10s, 1500rpm at a high speed for 20 s. And putting the spin-coated magnesium alloy sample into an oven to be dried for 2h at 120 ℃ for curing.
Comparative example 1
The magnesium alloy surface after pretreatment was used as comparative example 1, and the magnesium alloy surface was not coated with the corrosion-resistant and wear-resistant coating.
Comparative example 2
Comparative example 2 is different from example 1 in that: the anticorrosive and wear-resistant dispersion liquid only contains 3g of graphene oxide and 97g of ethanol, and other operations are unchanged.
Comparative example 3
Comparative example 3 is different from example 1 in that: the modified siloxane is replaced by oleic acid in the same mass, and other operations are unchanged.
And (3) testing the performance of the protective coating on the surface of the magnesium alloy:
coating thickness test: the prepared test specimens were cut into a size of 10X 10mm, and the thickness of the coating layer of the sample prepared in example was measured by a scanning electron microscope of JSM-IT 100.
And (3) testing the corrosion resistance of the coating: sealing the prepared sample by using copper powder conductive adhesive and silicon rubber, wherein the electrodes used in the three-electrode method are respectively as follows: the reference electrode is a saturated calomel electrode, the counter electrode is a platinum electrode, and the sample is a working electrode. The medium solution used in the experiment was 3.5% NaCl solution, and the electrochemical performance of the sample was tested using an electrochemical workstation model CS 350.
And (3) testing the wear resistance of the coating: the friction performance of the sample was measured by a UMT-2 type friction machine at a sliding speed of 0.01 m.s-1The force used was 100mN and the time was 30 min.
In combination with the examples, it can be seen that the unmodified graphene oxide coating has limited protection effect on the magnesium alloy substrate. In the invention, the stearic acid is used for modifying the graphene oxide and the graphene oxide is coated on the surface of the magnesium alloy in a spin coating manner, so that the corrosion resistance of the magnesium alloy is greatly improved, and the wear resistance of the magnesium alloy is greatly improved, which shows that the coating has a good protection effect on the magnesium alloy.
TABLE 1
| Thickness of coating | Corrosion voltage (V) | Corrosion current (A/cm)2) | COF | |
| Example 1 | 0.38μm | -1.236 | 1.35×10-6 | 0.09 |
| Example 2 | 0.25μm | -1.127 | 6.21×10-7 | 0.08 |
| Example 3 | 0.2μm | -1.062 | 1.22×10-7 | 0.07 |
| Example 4 | 0.4μm | -1.242 | 2.67×10-6 | 0.08 |
| Comparative example 1 | / | -1.514 | 2.25×10-4 | 0.47 |
| Comparative example 2 | 0.23μm | -1.475 | 4.25×10-5 | 0.2 |
| Comparative example 3 | 0.38μm | -1.427 | 4.36×10-6 | 0.15 |
It can be seen from table 1 that, according to the present invention, after the graphene oxide is modified and is spin-coated on the surface of the magnesium alloy, the corrosion resistance and wear resistance of the magnesium alloy are significantly improved, and the coating prepared in example three has relatively better performance, which indicates that the coating has a better protection effect on the magnesium alloy.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. The magnesium alloy anticorrosion and wear-resistant coating composition is characterized in that: the composite material comprises the following components in percentage by mass: 0.05-5% of graphene oxide, 0.1-7.5% of modified siloxane, 0.05-1% of surfactant and 86.5-99.8% of dispersant; wherein the modified siloxane is prepared by taking unsaturated fatty acid and mercapto siloxane as main raw materials through reaction;
the unsaturated fatty acid is one or more of cis-5-dodecenoic acid, myristoleic acid, oleic acid, linoleic acid, mesonic acid, arachidic acid, arachidonic acid, eicosapentaenoic acid, and docosahexaenoic acid.
2. The magnesium alloy corrosion and wear resistant composition of claim 1, wherein: the unsaturated fatty acid is oleic acid.
3. The magnesium alloy corrosion and wear resistant coating composition of claim 1, wherein: the mercapto-containing siloxane is one or a mixture of mercaptopropyl trimethoxy silane and mercaptopropyl triethoxy siloxane.
4. The magnesium alloy corrosion and wear resistant coating composition of claim 1, wherein: the surfactant is a nonionic surfactant.
5. The magnesium alloy corrosion and wear resistant coating composition of claim 1, wherein: the surfactant is one or more of alkyl alcohol polyoxyethylene ether, alkyl acid ester polyoxyethylene ether and alkylamine polyoxyethylene ether.
6. The magnesium alloy corrosion and wear resistant coating composition of claim 1, wherein: the using amount of the graphene oxide is 0.5-2.5%; the dosage of the modified siloxane is 1 to 5 percent; 0.1 to 0.5 percent of surfactant; the dispersant accounts for 92 to 98.4 percent.
7. The magnesium alloy corrosion and wear resistant coating composition of claim 1, wherein: the surfactant is oleic acid ester polyoxyethylene ether.
8. The magnesium alloy corrosion and wear resistant coating composition of claim 1, wherein: the dispersing agent is ethanol or isopropanol.
9. Use of a magnesium alloy anti-corrosion, wear resistant coating composition according to any of claims 1-8, characterized in that:
(1) grinding, polishing and degreasing the magnesium alloy, then carrying out hydroxylation treatment on the surface of the magnesium alloy by using alkali liquor, cleaning and drying for later use;
(2) and (3) mixing the coating composition, coating the mixture on the magnesium alloy sheet pretreated in the step (1) by adopting a spin coating method, and drying the magnesium alloy sheet in an oven at 120 ℃ to form an anticorrosive and wear-resistant coating on the surface of the magnesium alloy.
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