CN109504280A - A kind of preparation method of Mg alloy surface sial complex sol coating - Google Patents
A kind of preparation method of Mg alloy surface sial complex sol coating Download PDFInfo
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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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- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
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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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- 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
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- 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
- C23C22/22—Orthophosphates containing alkaline earth metal cations
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Abstract
The invention discloses a kind of methods of Mg alloy surface sial complex sol coating, belong to material surface modifying technology field.This method comprises the concrete steps that: (1) preparing magnesium alloy pretreatment liquid: calcium nitrate, tertiary sodium phosphate are added in a certain amount of distilled water, nitric acid strong stirring, which is added, makes sediment dissolve to obtain clear mixed solution, is eventually adding nitric acid and sodium hydroxide adjusts pH value；(2) magnesium alloy pre-treatment obtains Ca-P layers: after the polishing of magnesium alloy sand paper, ultrasonic cleaning, immersing and deposits Ca-P layers in above-mentioned pretreatment solution；(3) preparation of aluminium silica solution composite coating: the magnesium alloy after obtaining Ca-P layers is immersed in sial complex sol-trimethyl oxysilane mixed solution, immersion-drying 1-3 times is repeated, then solidification obtains.Preparation method of the invention is fairly simple, and the degradation speed of preparation-obtained silicon-aluminum sol composite coating is low, and the magnesium alloy with the coating has preferable corrosion resistance.
Description
Technical field
The invention belongs to material surface modifying technology fields, and in particular to a kind of Mg alloy surface sial complex sol coating
Preparation method.
Background technique
Magnesium alloy can play its superior performance with its excellent performance, in industry and medical domain.However, by
Active in the property of magnesium, corrosion resistance of magnesium alloy energy difference is a great weakness, largely limits magnesium alloy
Using.It is often at high cost with regard to the purity of raising magnesium alloy from the point of view of current technology or the novel magnesium alloy for developing high corrosion resistance
And effect is limited, and the core emphasis of magnesium alloy anticorrosion should be the interface for changing magnesium alloy and surrounding medium, therefore anti-
Only magnesium and Corrosion Behaviors of Magnesium Alloys is most effective, the simplest method is to carry out surface coated treatment to it.Surface covering it is economic and environment-friendly,
And efficiently feasibility has obtained the extensive approval of people, surface-coating technology mainly has chemical conversion, anodic oxidation, differential of the arc oxygen
Change, vapor deposition, ion implanting, chemical plating and plating and sol-gel technique, and with the development of technology, the kind of coating
Class is also being continuously increased, and composite coating technology is also applied to the anti-corrosion of magnesium alloy by people, and composite coating refers to two kinds or two kinds
The above coating often can achieve single coating and be unable to reach protecting effect as magnesium alloy protective coating, composite coating.
Summary of the invention
The purpose of the present invention is to solve magnesium alloy in the prior art, corrosion resistance is low when in use, and degradation speed is fast
Disadvantage provides a kind of preparation method of simple sial complex sol coating of step, the composite coating good corrosion resistance prepared.
The present invention adopts the following technical scheme: a kind of method that Mg alloy surface prepares aluminium silica solution composite coating, including
Following steps:
(1) it configures magnesium alloy pretreatment liquid: calcium nitrate, tertiary sodium phosphate being added in distilled water, nitric acid strong stirring is added
Make sediment dissolve to obtain clear mixed solution, is eventually adding nitric acid and sodium hydroxide adjusts pH value to 3-4, obtain pre-treatment
Liquid.
The molar concentration of the calcium nitrate is 0.02-0.15mol/L, and the molar concentration of tertiary sodium phosphate is 0.003-
0.15mol/L。
(2) pre-treatment of magnesium alloy obtains Ca-P layers: taking the magnesium alloy of sheet to use sand paper to polish first, after ultrasonic cleaning
It is immersed in the pretreatment liquid that step (1) obtains and impregnates 15min-24h；By the cleaning of post-depositional magnesium alloy, drying.
(3) preparation of aluminium silica solution composite coating: the aluminium silicon composite sol of equivalent and trimethyl oxysilane are added and burnt
In cup, is stirred 6 hours in 30 DEG C, obtain uniform mixed solution；Step (2) pre-treatment is obtained Ca-P layers of magnesium alloy sample
It is put into above-mentioned mixed solution and impregnates, take out after complete wetting to be put into dry in resistance furnace and take out, then repeat to impregnate,
Drying is three times；Final curing obtains the magnesium alloy with aluminium silica solution composite coating.
Further, the concentration of nitric acid in the step (1) is 65-68%.
Further, the concentration of the sodium hydroxide in the step (1) is 1mol/L.
Further, the solid content of aluminium silicon composite sol is 20-30%, PH 3-4 in the step (3).
Further, temperature is controlled by the way of with heating water bath when stirring in the step (3).
Further, step (3) drying temperature is 60-80 DEG C, drying time 15-30min.
Further, step (3) solidification temperature is 120-220 DEG C, curing time 15-30min.
The principles of science of the present invention:
Since the standard electrode potential of magnesium alloy is lower and is easily corroded, the appropriate to the occasion generation of silylation layer is prepared in Mg alloy surface
The binding force of corrosion reaction, magnesium alloy substrate and silylation layer is poor, and destruction can occur to early in the later period.In addition single silicon
Alkane thickness degree is only tens nanometers, and there are micropores, and corrosion resistance is limited, and wear-resisting property is lower.The present invention is used to magnesium alloy
Surface carries out Ca-P layers of pre-treatment, using Ca-P layers as transition zone, is placed on silane and contacts with the direct of magnesium alloy, improve silane
The binding force of layer and magnesium alloy substrate；The compactness for improving silylation layer using aluminium silicon composite sol simultaneously, so that it is anti-corrosion to improve its
Property and wearability.
Compared with prior art, the present invention has following technical effect that
1, it is added by Ca-P transition zone, the surface compact of aluminium silicon composite sol coating, the presence of pore-free and micro-crack.
2, the corrosion current of silicon-aluminum sol composite coating is far below the corrosion current of preprocessing layer and magnesium alloy, corrosion
Current potential reduces simultaneously, and the results are shown in Table 1.
The corrosion current and corrosion potential of table 1, different coating
3, after pre-treatment silicon-aluminum sol composite coating hydrogen desorption capacity be far below magnesium alloy hydrogen desorption capacity, Ca-P transition zone
Addition the corrosion resistance of magnesium alloy can be improved, its prolonged erosion of the silicon-aluminum sol coating of non-pre-treatment is even lower than magnesium alloy
Matrix.
4, the silicon-aluminum sol composite coating after pre-treatment is still fine and close in 7 days rear surfaces of Hank ' S immersion, corrosion-free product
Occur, the corrosion resistance of silicon-aluminum sol composite coating is higher than the Ca-P coating after single pre-treatment.
5, preparation method of the invention is fairly simple, and the degradation speed of preparation-obtained silicon-aluminum sol composite coating is low,
Magnesium alloy with the coating has preferable corrosion resistance.
Detailed description of the invention
Fig. 1 is the stereoscan photograph for the silicon-aluminum sol composite coating that embodiment 1 obtains；
As shown in Figure 1, the coating is uniform and compact, non-microcracked and hole presence.
Fig. 2 be the Ca-P coating after the obtained pre-treatment of embodiment 1, the silicon-aluminum sol composite coating after pre-treatment and
The polarization curve of magnesium alloy；
What Mg was indicated in figure is magnesium alloy substrate, and Ca-P indicates that the coating after magnesium alloy pre-treatment, MTMS indicate that sial is molten
Glue composite coating.Table 1 is the corrosion current density and corrosion potential that Fig. 2 is fitted, and as known from Table 1, silicon-aluminum sol is compound
The corrosion current of coating is 4.82x10-6A, far below the corrosion current (1.9x10 of the Ca-P coating after pre-treatment-5) and magnesium A
Corrosion current (the 3.16x10 of alloy substrate-4A)。
Fig. 3 be the Ca-P coating after the obtained pre-treatment of embodiment 1, the silicon-aluminum sol composite coating after pre-treatment and
The electrochemical impedance figure that magnesium alloy measures in 3.5% sodium chloride solution；
Abscissa is the real part of resistance in figure, and ordinate is resistance imaginary part, it can be seen that the processing of silicon-aluminum sol composite coating
Capacitive reactance arc radius afterwards is obviously bigger than the capacitive reactance arc radius of Ca-P coating after magnesium alloy substrate and pre-treatment more, illustrates to apply
Layer has good protective capability to magnesium alloy base.
Fig. 4 is the stereoscan photograph for the silicon-aluminum sol composite coating that embodiment 2 obtains；
The coating is uniform and compact, non-microcracked and hole presence.
Fig. 5 be embodiment 2 obtain magnesium alloy, non-pre-treatment silicon-aluminum sol coating and sial after pre-treatment it is molten
Hydrogen desorption capacity of the glue composite coating in Hank ' S solution.
Since the hydrogen desorption capacity of the silicon-aluminum sol coating of non-pre-treatment has been more than measurement range two days later, in Fig. 5 only its two
It hydrogen desorption capacity.Fig. 5 can be seen that the silicon-aluminum sol coating protection effect of non-pre-treatment is poor, only in a few days ago effective, the later period
Its corrosion resistance is even lower than magnesium alloy substrate；The hydrogen desorption capacity of silicon-aluminum sol composite coating is substantially less than magnesium alloy substrate, illustrates
The corrosion resistance of magnesium alloy can be improved in the addition for crossing layer.
Fig. 6 be the Ca-P coating after the obtained pre-treatment of embodiment 2, the silicon-aluminum sol composite coating after pre-treatment and
Magnesium alloy impregnated 7 days in Hank ' S solution after pattern.
As shown in fig. 6, the silicon-aluminum sol composite coating after pre-treatment impregnates 7 days rear surfaces in Hank ' S and still causes
Close, only the Ca-P coating surface after pre-treatment has the appearance of point corrosion pit and white corrosion product, and magnesium alloy matrix surface is a large amount of
Corrosion product.Illustrate that the corrosion resistance of silicon-aluminum sol composite coating is higher than the Ca-P coating of single pre-treatment.
Specific embodiment
In order to which technical characteristic of the invention, purpose and beneficial effect are more clearly understood, now to skill of the invention
Art scheme carries out described further below, but should not be understood as that limiting the scope of the invention.
Embodiment 1
1.43g four water-calcium nitrate is added first in the distilled water of 180ml, after stirring makes it completely dissolved, is then added
The tertiary sodium phosphate of 0.19g obtains turbid solution, and adding nitric acid stirring clarifies turbid solution, adds distilled water, and use nitric acid
With sodium hydroxide adjust pH value be 4.0, adjustings solution total capacity be 200ml, obtain 0.03mol/l calcium nitrate,
0.0025mol/l tertiary sodium phosphate pretreatment liquid.Magnesium alloy plate is successively used to alcohol, acetone ultrasonic cleaning 10min, then closes magnesium
Gold plaque immerses in the deposition liquid of heating water bath to 40 degrees Celsius for 24 hours, then takes out distilled water cleaning, finally in an oven, 60 DEG C
Dry 1h.By the MTMS (trimethyl oxysilane) of the Si-Al complex sol of 20g and 20g, stirring 6 is small in 30 DEG C in beaker
When, the solution that is uniformly mixed.Magnesium alloy sample after pre-treatment is put into mixed solution and is impregnated, is taken after complete wetting
It is put into resistance furnace and dries out, 80 DEG C of drying temperature, soaking time 30min, take out；Then repeat to impregnate, impregnate three times.
Last 200 DEG C of solidifications, curing time 30min.Obtain the magnesium alloy with aluminium silica solution composite coating.
Embodiment 2
4.723g four water-calcium nitrate is added first in the distilled water of 180ml, after stirring makes it completely dissolved, is then added
The tertiary sodium phosphate of 7.762g obtains turbid solution, and adding nitric acid stirring clarifies turbid solution, adds distilled water, and use nitric acid
Adjusting pH value with sodium hydroxide is 4.0, and adjusting solution total capacity is 200ml, obtains calcium nitrate, the 0.1mol/l phosphorus of 0.1mol/l
Sour trisodium pretreatment liquid.Magnesium alloy plate is successively used to alcohol, acetone ultrasonic cleaning 10min, magnesium alloy plate is then immersed into water-bath
It is heated to 30min in 40 degrees Celsius of deposition liquid, then takes out distilled water cleaning, finally in an oven, 60 DEG C of drying 1h.It will
The Si-Al complex sol of 20g and the MTMS (trimethyl oxysilane) of 20g are stirred 6 hours in 30 DEG C in beaker, are obtained uniformly
Mixed solution.Magnesium alloy sample after pre-treatment is put into mixed solution and is impregnated, is taken out after complete wetting and is put into resistance
It dries, 80 DEG C of drying temperature, soaking time 30min, takes out in furnace；Then repeat to impregnate, dry three times.Last 180 DEG C
Solidification, curing time 30min.Obtain the magnesium alloy with aluminium silica solution composite coating.
Embodiment 3
1.43g four water-calcium nitrate is added first in the distilled water of 180ml, after stirring makes it completely dissolved, is then added
The tertiary sodium phosphate of 0.19g obtains turbid solution, and adding nitric acid stirring clarifies turbid solution, adds distilled water, and use nitric acid
With sodium hydroxide adjust pH value be 4.0, adjustings solution total capacity be 200ml, obtain 0.03mol/l calcium nitrate,
0.0025mol/l tertiary sodium phosphate pretreatment liquid.Magnesium alloy plate is successively used to alcohol, acetone ultrasonic cleaning 10min, then closes magnesium
Gold plaque immerses 8h in the deposition liquid of heating water bath to 40 degrees Celsius, then takes out distilled water cleaning, finally in an oven, 60 DEG C of bakings
Dry 1h.The MTMS (trimethyl oxysilane) of the Si-Al complex sol of 20g and 20g are stirred 6 hours in 30 DEG C in beaker,
The solution being uniformly mixed.Magnesium alloy sample after pre-treatment is put into mixed solution and is impregnated, is taken out after complete wetting
It is put into resistance furnace and dries, 80 DEG C of drying temperature, soaking time 30min, take out；Last 220 DEG C of solidifications, curing time 30min.
Obtain the magnesium alloy with aluminium silica solution composite coating.
Claims (7)
1. a kind of preparation method of Mg alloy surface sial complex sol coating, it is characterised in that the following steps are included:
(1) it configures magnesium alloy pretreatment liquid: calcium nitrate, tertiary sodium phosphate is added in distilled water, nitric acid strong stirring, which is added, to be made to sink
Starch dissolves to obtain clear mixed solution, is eventually adding nitric acid and sodium hydroxide adjusts pH value to 3-4, obtain pretreatment liquid；
The molar concentration of the calcium nitrate is 0.02-0.15mol/L, and the molar concentration of tertiary sodium phosphate is 0.003-0.15mol/L；
(2) pre-treatment of magnesium alloy obtains Ca-P layers: taking the magnesium alloy of sheet to use sand paper to polish first, immerses after ultrasonic cleaning
15min-24h is impregnated in the pretreatment liquid obtained to step (1)；By the cleaning of post-depositional magnesium alloy, drying；
(3) preparation of aluminium silica solution composite coating: the aluminium silicon composite sol of equivalent and trimethyl oxysilane are added in beaker,
It is stirred 6 hours in 30 DEG C, obtains uniform mixed solution；The magnesium alloy sample that step (2) pre-treatment obtains Ca-P layers is put into
It is impregnated in above-mentioned mixed solution, takes out to be put into dry in resistance furnace after complete wetting and take out, then repeat immersion, drying
Three times；Final curing obtains the magnesium alloy with aluminium silica solution composite coating.
2. the preparation method of Mg alloy surface sial complex sol composite coating as described in claim 1, which is characterized in that institute
Stating the concentration of nitric acid in step (1) is 65-68%.
3. the preparation method of Mg alloy surface sial complex sol composite coating as described in claim 1, which is characterized in that institute
The concentration for stating the sodium hydroxide in step (1) is 1mol/L.
4. the preparation method of Mg alloy surface sial complex sol composite coating as described in claim 1, which is characterized in that institute
The solid content for stating aluminium silicon composite sol in step (3) is 20-30%, PH 3-4.
5. the preparation method of Mg alloy surface sial complex sol composite coating as described in claim 1, which is characterized in that institute
Temperature is controlled by the way of with heating water bath when stating stirring in step (3).
6. the preparation method of Mg alloy surface sial complex sol composite coating as described in claim 1, which is characterized in that institute
Stating step (3) drying temperature is 60-80 DEG C, drying time 15-30min.
7. the preparation method of Mg alloy surface sial complex sol composite coating as described in claim 1, which is characterized in that institute
Stating step (3) solidification temperature is 120-220 DEG C, curing time 15-30min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116656230A (en) * | 2022-02-19 | 2023-08-29 | 湖北唯吾新材料科技有限公司 | Preparation method of water-based normal-temperature self-drying organic silicon multi-hybrid resin |
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| CN1900360A (en) * | 2006-07-14 | 2007-01-24 | 西南大学 | Process for preparing magnesium alloy surface function gradient film |
| CN102886073A (en) * | 2012-10-09 | 2013-01-23 | 天津大学 | Biological glass coat for medical magnesium alloy surface and preparation method of biological glass coat |
| CN103933611A (en) * | 2014-03-27 | 2014-07-23 | 同济大学 | Preparation method of hydroxyapatite/polylactic acid composite coating on surface of medical magnesium alloy |
| CN104404480A (en) * | 2014-11-19 | 2015-03-11 | 无锡光旭新材料科技有限公司 | Method for preparing hydroxyapatite and bone collagen composite coating on surface of magnesium alloy |
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2018
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| CN1900360A (en) * | 2006-07-14 | 2007-01-24 | 西南大学 | Process for preparing magnesium alloy surface function gradient film |
| CN102886073A (en) * | 2012-10-09 | 2013-01-23 | 天津大学 | Biological glass coat for medical magnesium alloy surface and preparation method of biological glass coat |
| CN103933611A (en) * | 2014-03-27 | 2014-07-23 | 同济大学 | Preparation method of hydroxyapatite/polylactic acid composite coating on surface of medical magnesium alloy |
| CN104404480A (en) * | 2014-11-19 | 2015-03-11 | 无锡光旭新材料科技有限公司 | Method for preparing hydroxyapatite and bone collagen composite coating on surface of magnesium alloy |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116656230A (en) * | 2022-02-19 | 2023-08-29 | 湖北唯吾新材料科技有限公司 | Preparation method of water-based normal-temperature self-drying organic silicon multi-hybrid resin |
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Effective date of registration: 20230831 Address after: 230000 B-2705, wo Yuan Garden, 81 Ganquan Road, Shushan District, Hefei, Anhui. Patentee after: HEFEI LONGZHIYUN PHARMACEUTICAL TECHNOLOGY Co.,Ltd. Address before: 230000 floor 1, building 2, phase I, e-commerce Park, Jinggang Road, Shushan Economic Development Zone, Hefei City, Anhui Province Patentee before: Dragon totem Technology (Hefei) Co.,Ltd. Effective date of registration: 20230831 Address after: 230000 floor 1, building 2, phase I, e-commerce Park, Jinggang Road, Shushan Economic Development Zone, Hefei City, Anhui Province Patentee after: Dragon totem Technology (Hefei) Co.,Ltd. Address before: 243002 59 Hudong Middle Road, Huashan District, Ma'anshan, Anhui Patentee before: ANHUI University OF TECHNOLOGY |