CN107556865A - The preparation method of Mg alloy surface selfreparing erosion shield - Google Patents

The preparation method of Mg alloy surface selfreparing erosion shield Download PDF

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CN107556865A
CN107556865A CN201710726007.5A CN201710726007A CN107556865A CN 107556865 A CN107556865 A CN 107556865A CN 201710726007 A CN201710726007 A CN 201710726007A CN 107556865 A CN107556865 A CN 107556865A
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zro
corrosion inhibiter
preparation
carrier
solution
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王桂香
韩昕辰
何津萌
李泽源
吴倩
张晓红
张丽丽
吴春喜
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Harbin Engineering University
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Harbin Engineering University
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Abstract

The present invention is to provide a kind of preparation method of Mg alloy surface selfreparing erosion shield.Corrosion inhibiter is loaded into the ZrO with meso-hole structure2In carrier, then mix with epoxy resin adhesive liquid, mixed glue solution is finally coated on magnesium alloy matrix surface, the corrosion inhibiter is one or more of compoundings in BTA, hexamethylenetetramine, 2 mercaptobenzothiazolers or sodium molybdate.The ZrO of corrosion inhibiter will be loaded2Mixed with epoxy resin adhesive liquid and be coated on magnesium alloy matrix surface, carry out cold curing, you can obtain corrosion inhibiter ZrO2/ epoxy coating.This new coating has anti-corrosion, the function of selfreparing;The coating is green, nontoxic, and has simple preparation technology and relatively low production cost.

Description

The preparation method of Mg alloy surface selfreparing erosion shield
Technical field
It is specifically a kind of the present invention relates to a kind of preparation method of Mg alloy surface selfreparing erosion shield Mg alloy surface corrosion inhibiter-ZrO2The preparation method of/epoxy coating.
Background technology
Corrosion is because there occurs the effect such as electrochemistry, chemistry and physics, gold between metal material and the medium of surrounding Some changes occur for the state of category, so as to cause the destruction of metal material.Within this time after the industrial revolution, machine Tool equipment is widely used in worldwide, and therefore, the phenomenon of corrosion suffers from occurring in the every field of production and living. Metal erosion coverage is wider, caused by economic loss it is larger.In some key areas, such as offshore oil chemical industry, aviation Space flight, the main line of communication is first-class, and hardware can have longer service life used by being intended to.Once there is some play The structure of key effect has the generation of corrosion phenomenon, it will causes the damage and paralysis of structural device, causes serious accident, enter And trigger great economic loss, or even life-threatening.Statistics shows that corrosion can be caused in 3% or so total output value Loss.Traditional magnesium alloy has the advantages that the machinability and castability that density is low, specific strength is big, good, in traffic, building All had a wide range of applications Deng field, it is more active yet with magnesium elements itself chemism, cause magnesium system alloy be easy to Oxygen in air, water reaction, so as to be corroded, and then destroys its material itself, thus have impact on the further of magnesium alloy Using.The characteristic easily corroded for magnesium alloy under normal circumstances, people can be in its surface construction protective layers, so as to completely cut off Magnesium alloy contact with oxygen gas and water and other corrosive mediums in air.It is contemplated that the service life of protective layer, when its quilt When destroying or failing, magnesium alloy will be exposed among surrounding environment, can face the danger being damaged by corrosion again.
Certainly will be the waste to manpower and materials if periodically repaired to Mg alloy surface protective layer.And review one's lessons by oneself overcoating The it is proposed of layer, a new road is opened for the solution of this problem.Selfreparing (also crying self-healing) refers to not outer In the presence of power, when coating is destroyed, coating sample can carry out all or part of self-regeneration to impaired error area, from And reach the purpose for delaying corrosion.During prepares coating, it is that coating sample obtains self-healing to add corrosion inhibiter thereto The effective ways of function, but into coating sample, directly addition corrosion inhibiter can cause corrosion inhibiter to inactivate and reduce the stabilization of coated film Property, so that the etch resistant properties of coating reduce.
Compared with common nano-particle, hallow nanoparticles typically exhibit a series of special properties, such as than surface Product is high, and pore volume is big, and density is small, nontoxicity etc., while corrosion inhibiter is added in organic coating after nano container encapsulates, pole It is big to improve the integrality of coating and realize the controlled release of corrosion inhibiter, just because of with these advantages so that hollow Application of the nano-particle in corrosion-resistant field receives more and more attention.When containing this kind of corrosion inhibiter nano-particle of having loaded When coating is destroyed, the change of some properties (such as pH value, mechanical damage, temperature, potential) of surrounding environment at crack The change of nano container Surface Permeability can be caused by changing, so as to discharge corrosion inhibiter, the characteristics of coating shows self-healing, to gold Category plays slow releasing function.But on preparing ZrO using the precipitation method2Mesoporous material, and pore filling corrosion inhibiter, are disperseed Into epoxy resin adhesive liquid and Mg alloy surface is coated on, realizes that coating protection and the releasable report of corrosion inhibiter intelligence are also seldom See.
The content of the invention
Physical shielding effect and the corrosion inhibiter protection at destruction are had concurrently it is an object of the invention to provide a kind of, are magnesium alloy The preparation method of the Mg alloy surface selfreparing erosion shield of intelligent protection is provided.
The object of the present invention is achieved like this:
Corrosion inhibiter is loaded into the ZrO with meso-hole structure2In carrier, then mix with epoxy resin adhesive liquid, finally will be mixed Rubber alloy liquid is coated on magnesium alloy matrix surface, and the corrosion inhibiter is BTA, hexamethylenetetramine, 2-mercaptobenzothiazole Or one or more of compoundings in sodium molybdate.
The present invention can also include:
1st, the ZrO with meso-hole structure2Carrier is prepared using the precipitation method, is specifically included:By 10~13g ZrOCl2·8H2O solids are dissolved in the zirconium oxychloride solution for obtaining that concentration is 1.0~1.3mol/L in 40mL distilled water, by 0.13~ 0.15g cetyl trimethylammonium bromides are dissolved in the cetyl for obtaining that concentration is 0.01~0.02mol/L in 40mL distilled water Trimethylammonium bromide solution, compound concentration is 1.0~4.0mol/L ammonia spirit, then by zirconium oxychloride solution and hexadecane Stirred after the mixing of base trimethylammonium bromide solution and control temperature to be not higher than 50 DEG C, ammonia spirit is added dropwise to basic zirconium chloride 70 DEG C are heated to after ammonia spirit and stir to having precipitated with the mixed solution of cetyl trimethylammonium bromide, dripping Entirely, separated with centrifuge, precipitation is dried, is calcined, grinding.
2nd, it is described that corrosion inhibiter is loaded into the ZrO with meso-hole structure2Specifically included in carrier:First corrosion inhibiter is dissolved, Then by the ZrO with meso-hole structure2Carrier is added in corrosion inhibitor solution, stirring dipping 12 hours, centrifuge separation, precipitation warp Washing, dry, obtain being loaded with the ZrO of corrosion inhibiter2
3rd, there is the ZrO of meso-hole structure2In the preparation process of carrier, the drying process temperature of precipitation is 110 DEG C, when drying Between be 8~12h;Sintering temperature is 500 DEG C, roasting time 4h.
4th, corrosion inhibiter is loaded into the ZrO with meso-hole structure2In carrier, the washing times of precipitation is twice;Precipitation Drying means is:60 DEG C, vacuum drying chamber, 4 hours.
5th, it is loaded with the ZrO of corrosion inhibiter2Amount be weight resin 3~6%, the ZrO of corrosion inhibiter will be loaded with2With resin After mixing, 1h is stirred;651 curing agent are added, stir 1h;It is ultrasonically treated 5min;Stewing process 10min.
6th, the coating number that mixed glue solution is coated on to magnesium alloy matrix surface is 3 times, and curing is:Suspension is solid Change;Solidification temperature is room temperature;Hardening time is 24~72h.
During magnesium alloy matrix surface prepares coating, it is that coating obtains self-healing function to add corrosion inhibiter thereto Effective ways, but into coating directly addition corrosion inhibiter can cause corrosion inhibiter inactivate and reduce coated film stability, so as to Make the etch resistant properties of coating reduce.The introducing of hollow Nano capsule of the present invention successfully solves this problem, i.e.,:First by inhibition Agent is packaged with nano-particle, then the nano-particle after encapsulation is added in resin adhesive liquid.
The invention provides a kind of Mg alloy surface corrosion inhibiter-ZrO2The preparation method of/epoxy coating, has physics concurrently Screen effect is protected with the corrosion inhibiter at destruction, is a kind of corrosion-inhibiting coating that intelligent protection is provided for magnesium alloy.The present invention provides A kind of ZrO2The new approaches of carrier, utilize ZrO2The all relatively good oxide of this heat-and corrosion-resistant performance is and right as carrier Relatively low in equipment requirement, purity is higher.Mg alloy surface corrosion inhibiter-the ZrO of the present invention2The preparation method of/epoxy coating Simply, it is easily operated, reduce the dosage of corrosion inhibiter and possible pollution on the environment.
In the preparation method of the Mg alloy surface corrosion inhibiter-ZrO2/ epoxy coatings of the present invention, there is meso-hole structure Zirconium dioxide is as carrier, there is provided the storage area of corrosion inhibiter, corrosion inhibiter is added in mesoporous supports, then will load corrosion inhibiter ZrO afterwards2Mixed with epoxy resin, finally by magnesium alloy substrate and corrosion inhibiter-ZrO2/ epoxy resin selfreparing erosion shield With reference to.
Mg alloy surface corrosion inhibiter-ZrO provided by the invention2The preparation method of/epoxy coating, preparation process are: Filling encapsulation → corrosion inhibiter-ZrO of preparation → corrosion inhibiter of mesoporous ZrO 2 carrier2→ magnesium conjunction is mixed with epoxy resin adhesive liquid Auri body and corrosion inhibiter-ZrO2/ epoxy resin adhesive liquid is combined and solidified.Concrete technology is as follows:
It is prepared by the first step, mesoporous ZrO 2:Certain density zirconium oxychloride solution, ammonia spirit, 16 are prepared respectively Alkyl trimethyl ammonium bromide (CTAB) solution;The CTAB solution of certain volume is mixed with zirconium oxychloride solution;Treat that solution mixes Uniformly, then the ammonia spirit of certain volume is added dropwise in CTAB and zirconium oxychloride solution by constant pressure funnel; While being stirred continuously, the flocculent deposit of white occurs in solution, completely after precipitation, precipitation is separated with centrifuge;Will Drying is precipitated, is calcined, grinding, ZrO is made2Carrier is stand-by;
Second step, the filling encapsulation of corrosion inhibiter:First corrosion inhibiter is dissolved respectively;Then a certain amount of carrier is added to inhibition In agent solution, stirring;Separated, precipitated using centrifuge after a period of time, washed, dry, obtain loading corrosion inhibiter ZrO2Carrier;
3rd step, load the mixing of the zirconia carrier and epoxy resin of corrosion inhibiter:Weigh epoxy resin, by resin and Solvent is proportionally mixed, and is stirred;The zirconium dioxide of corrosion inhibiter will be loaded with, high-speed stirred is added to asphalt mixtures modified by epoxy resin In fat glue, a certain amount of curing agent uniformly is added after mixing, is stirred to being well mixed, ultrasound simultaneously stands de-bubble;
4th step, magnesium alloy substrate and corrosion inhibiter-ZrO2/ epoxy resin adhesive liquid combines:Magnesium alloy matrix surface is passed through A series of processing expose fresh matrix to remove surface film oxide;Then by corrosion inhibiter-ZrO2/ epoxy resin adhesive liquid uniformly coats In Mg alloy surface, cold curing.
It is of the invention that successively there is intelligent antiseptic effect using the precipitation method, solvent evaporated method, mechanical mixing method, cladding process preparation Composite coating.Obtained mesoporous ZrO 2 carrier contrast conventional carriers have to the more preferable adaptability of epoxy resin.Meanwhile The loose structure of zirconia carrier, enough spaces are provided for the filling of corrosion inhibiter, a kind of novel corrosion inhibitor has been opened up and has filled out Fill method.The release of traditional corrosion inhibiter is all that will be directly acted on for it in corrosive environment, and it is substantial amounts of not only to cause corrosion inhibiter Waste, also environment is polluted.Corrosion inhibiter and coating protection are combined into one by the present invention, and coating can not only provide conventional guarantor Shield, the position that appropriate corrosion inhibiter protection destroys can also be effectively discharged at scuffing or in corrosive medium, realizes intelligent protection.
The present invention devises a kind of Mg alloy surface corrosion inhibiter-ZrO2The preparation method of/epoxy coating.First, with The precipitation method of the chlorine hydrate zirconium oxide in ammonia spirit, it is prepared for the white powder of Nanosized Zircomea Particles with meso-hole structure End;Then using the method for infiltration and solvent evaporation, corrosion inhibiter is added in loose structure;Again by after load corrosion inhibiter ZrO2Mixed with epoxy resin;Finally by magnesium alloy substrate be immersed in load corrosion inhibiter after ZrO2With in epoxy resin mixed liquor, Carry out room temperature suspension solidification.Compared with traditional corrosion-inhibiting coating, this new coating not only has the anti-corrosion shielding action of conventional coatings, And corrosion inhibiter can be discharged after coating is by external force breakage, corrosion inhibiter adsorbed film is formed in metal surface, makes metallic matrix Retrieve protection.Mesoporous ZrO 2 carrier in the method is a kind of smaller and hot with high molten boiling point, thermal conductivity factor The coefficient of expansion is larger, excellent wear-resisting property, a kind of exsertile inorganic non-metallic material of corrosion resistance, thus has to resin More preferable adaptability.And this method uses all relatively good oxide of this heat-and corrosion-resistant performance of zirconium dioxide as load Body, relatively low for equipment requirement, purity is also higher.Compounded using one or more corrosion inhibiter in the present invention, had to magnesium alloy Good antiseptic effect.
Using CHI660C type electrochemical workstations, 3.5%wt NaCl solution, auxiliary electrode is platinum electrode, reference electrode For calomel electrode, the sample of preparation is tested, and equivalent circuit plan is carried out to electrochemical impedance using ZSimpWin softwares Close analysis.Corrosion inhibiter-ZrO2/ epoxy coating still works in the 2nd day coating impedance of immersion, and coating serves selfreparing after breakage Performance.This programme method is novel, and simple to operate, cost is cheap, and energy consumption is small, is adapted to practical application large-scale production.
To sum up advantage and positive effect of the invention are:
1st, the mesoporous ZrO 2 carrier contrast conventional carriers prepared have to the more preferable adaptability of resin.
2nd, the method for preparing mesoporous ZrO 2 carrier is relatively low for equipment requirement, and purity is also higher.
3rd, the anti-corrosion method of one or more corrosion inhibiter compoundings is proposed.
4th, propose a kind of novel corrosion inhibiter in mesoporous ZrO2In method for packing.
5th, after coating is corroded, coating can provide intelligence to matrix and repair.
6th, method of the invention is green, and technique is simple, works well.
Brief description of the drawings
Fig. 1 is ZrO2The N of mesoporous material2Adsorption desorption figure;
Fig. 2 a- Fig. 2 b are ZrO2The BJH adsorption desorption graph of pore diameter distribution of mesoporous material.ZrO2The specific surface area of mesoporous material is 47.465m2/ g, single-point average pore radius 14.48nm.
Fig. 3 is corrosion inhibiter -5%ZrO2The Bode mould figure of/epoxy coating in 3.5%NaCl solution.In Bode mould figures, Soaked 1 day in 3.5%NaCl solution, impedance magnitude becomes big, corrosion inhibiter-ZrO2/ epoxy coating has certain self-healing.
Corrosion inhibiter-the ZrO of Fig. 4 different contents2The Bode mould figure of/epoxy coating in 3.5%NaCl solution.
Embodiment
Illustrate below for a more detailed description to the present invention.
Embodiment 1
The first step, the preparation of mesoporous ZrO 2 carrier:By 11g ZrOCl2·8H2O solids are dissolved in 40mL distilled water, Concentration is 1.0mol/L;The preparation of CTAB solution:0.13g CTAB are dissolved in 40mL distilled water, concentration is 0.01mol/L's CTAB solution;Compound concentration is 1.0mol/L ammonia spirit;Then stirred after basic zirconium chloride is mixed with CTAB solution, temperature Not higher than 50 DEG C;The ammonia spirit prepared is added dropwise in basic zirconium chloride and CTAB mixed solutions by dropping funel; PH=9.5 is adjusted, more than 70 DEG C are heated to after dripping ammonia spirit, the flocculent deposit of white occurs in solution, it is completely heavy Behind shallow lake, the separation of precipitation centrifuge is drawn;Gained precipitation is placed in beaker, and 10h is dried in 110 DEG C, is smashed Afterwards in 500 DEG C of Muffle kiln roastings 4 hours, it is stand-by that sample is made.
Second step, the filling encapsulation of corrosion inhibiter:20mL ethanol solutions are measured, corrosion inhibiter powder is added, is placed on magnetic agitation It is stirred continuously on device, until solution saturation.Then, 1g ZrO is weighed2Carrier, it is added in corrosion inhibiter-ethanol solution of saturation, Stir about 12 hours.Separated, precipitated with centrifuge again, then with distillation washing twice, be put into 60 DEG C of vacuum drying chamber, do Dry 4 hours, obtain loading the ZrO of corrosion inhibiter2Carrier.
3rd step, load the mixing of the zirconia carrier and epoxy resin of corrosion inhibiter:Epoxy resin E44 is weighed, according to The ratio of resin/solvent=5/2 (solvent is mixed solvent, n-butanol/dimethylbenzene=7/3) is mixed, and is stirred;So Afterwards according to the amount of resin, 1% zirconium dioxide for being loaded with corrosion inhibiter is weighed, the uniform 1h of high-speed stirred, adds curing agent afterwards, then For secondary stirring 1h to being well mixed, ultrasonic 5min simultaneously stands 10min.
4th step, magnesium alloy substrate and corrosion inhibiter-ZrO2/ combine:By corrosion inhibiter-ZrO2/ epoxy resin adhesive liquid uniformly coats In Mg alloy surface, after coating 3 times repeatedly, room temperature suspension solidification 72 hours is carried out.
Embodiment 2
The first step, the preparation of mesoporous ZrO 2 carrier:By 11g ZrOCl2·8H2O solids are dissolved in 40mL distilled water, Concentration is 1.0mol/L;The preparation of CTAB solution:0.13g CTAB are dissolved in 40mL distilled water, concentration is 0.01mol/L's CTAB solution;Compound concentration is 1.0mol/L ammonia spirit;Then stirred after basic zirconium chloride is mixed with CTAB solution, temperature Not higher than 50 DEG C;The ammonia spirit prepared is added dropwise in basic zirconium chloride and CTAB mixed solutions by dropping funel; PH=9.5 is adjusted, more than 70 DEG C are heated to after dripping ammonia spirit, the flocculent deposit of white occurs in solution, it is completely heavy Behind shallow lake, the separation of precipitation centrifuge is drawn;Gained precipitation is placed in beaker, and 10h is dried in 110 DEG C, is smashed Afterwards in 500 DEG C of Muffle kiln roastings 4 hours, it is stand-by that sample is made.
Second step, the filling encapsulation of corrosion inhibiter:20mL ethanol solutions are measured, corrosion inhibiter powder is added, is placed on magnetic agitation It is stirred continuously on device, until solution saturation.Then, 1g ZrO is weighed2Carrier, it is added in corrosion inhibiter-ethanol solution of saturation, Stir about 12 hours.Separated, precipitated with centrifuge again, then with distillation washing twice, be put into 60 DEG C of vacuum drying chamber, do Dry 4 hours, obtain loading the ZrO of corrosion inhibiter2Carrier.
3rd step, load the mixing of the zirconia carrier and epoxy resin of corrosion inhibiter:Epoxy resin E44 is weighed, according to The ratio of resin/solvent=5/2 (solvent is mixed solvent, n-butanol/dimethylbenzene=7/3) is mixed, and is stirred;So Afterwards according to the amount of resin, 3% zirconium dioxide for being loaded with corrosion inhibiter is weighed, the uniform 1h of high-speed stirred, adds curing agent afterwards, then For secondary stirring 1h to being well mixed, ultrasonic 5min simultaneously stands 10min.
4th step, magnesium alloy substrate and corrosion inhibiter-ZrO2/ combine:By corrosion inhibiter-ZrO2/ epoxy resin adhesive liquid uniformly coats In Mg alloy surface, after coating 3 times repeatedly, room temperature suspension solidification 72 hours is carried out.
Embodiment 3
The first step, the preparation of mesoporous ZrO 2 carrier:By 11g ZrOCl2·8H2O solids are dissolved in 40mL distilled water, Concentration is 1.0mol/L;The preparation of CTAB solution:0.13g CTAB are dissolved in 40mL distilled water, concentration is 0.01mol/L's CTAB solution;Compound concentration is 1.0mol/L ammonia spirit;Then stirred after basic zirconium chloride is mixed with CTAB solution, temperature Not higher than 50 DEG C;The ammonia spirit prepared is added dropwise in basic zirconium chloride and CTAB mixed solutions by dropping funel; PH=9.5 is adjusted, more than 70 DEG C are heated to after dripping ammonia spirit, the flocculent deposit of white occurs in solution, it is completely heavy Behind shallow lake, the separation of precipitation centrifuge is drawn;Gained precipitation is placed in beaker, and 10h is dried in 110 DEG C, is smashed Afterwards in 500 DEG C of Muffle kiln roastings 4 hours, it is stand-by that sample is made.
Second step, the filling encapsulation of corrosion inhibiter:20mL ethanol solutions are measured, corrosion inhibiter powder is added, is placed on magnetic agitation It is stirred continuously on device, until solution saturation.Then, 1g ZrO is weighed2Carrier, it is added in corrosion inhibiter-ethanol solution of saturation, Stir about 12 hours.Separated, precipitated with centrifuge again, then with distillation washing twice, be put into 60 DEG C of vacuum drying chamber, do Dry 4 hours, obtain loading the ZrO of corrosion inhibiter2Carrier.
3rd step, load the mixing of the zirconia carrier and epoxy resin of corrosion inhibiter:Epoxy resin E44 is weighed, according to The ratio of resin/solvent=5/2 (solvent is mixed solvent, n-butanol/dimethylbenzene=7/3) is mixed, and is stirred;So Afterwards according to the amount of resin, 5% zirconium dioxide for being loaded with corrosion inhibiter is weighed, the uniform 1h of high-speed stirred, adds curing agent afterwards, then For secondary stirring 1h to being well mixed, ultrasonic 5min simultaneously stands 10min.
4th step, magnesium alloy substrate and corrosion inhibiter-ZrO2/ combine:By corrosion inhibiter-ZrO2/ epoxy resin adhesive liquid uniformly coats In Mg alloy surface, after coating 3 times repeatedly, room temperature suspension solidification 72 hours is carried out.
It by CTAB is activating agent that mesoporous ZrO 2 carrier prepared by the present invention, which is, ZrOCl2·8H2O and ammonia precipitation process Method prepare.The data such as comparative surface area, aperture of zirconia carrier are measured by nitrogen adsorption desorption test (BET) (Fig. 1, Fig. 2 a- Fig. 2 b), deduction cavernous structure are slit type, and are mesoporous material.Using CHI660C type electrochemistry works Stand, 3.5%wt NaCl solution, auxiliary electrode is platinum electrode, and reference electrode is calomel electrode, and the sample of preparation is surveyed Examination, and Equivalent Circuit Fitting analysis (Fig. 3, Fig. 4) is carried out to electrochemical impedance using ZSimpWin softwares.And simulated by software Go out equivalent circuit, contrast the ZrO of different etching time and different content load corrosion inhibiter2Epoxy resin selfreparing anticorrosion applies Layer research corrosion behavior.
Above-mentioned specific embodiment is to illustrate the features of the present invention, and case study on implementation describes inventive concept, experiment The dosage and operating method of time of reaction, temperature and reagent, but the claim of the present invention can not be defined, its It is any to be included within protection scope of the present invention without departing from technical scheme.

Claims (7)

1. a kind of preparation method of Mg alloy surface selfreparing erosion shield, it is characterized in that:Corrosion inhibiter is loaded to Jie The ZrO of pore structure2In carrier, then mix with epoxy resin adhesive liquid, mixed glue solution is finally coated on magnesium alloy matrix surface, institute Corrosion inhibiter is stated as one or more of compoundings in BTA, hexamethylenetetramine, 2-mercaptobenzothiazole or sodium molybdate.
2. the preparation method of Mg alloy surface selfreparing erosion shield according to claim 1, it is characterized in that, the tool There is the ZrO of meso-hole structure2Carrier is prepared using the precipitation method, is specifically included:By 10~13g ZrOCl2·8H2O solids are dissolved in The zirconium oxychloride solution that concentration is 1.0~1.3mol/L is obtained in 40mL distilled water, by 0.13~0.15g cetyl trimethyls Ammonium bromide is dissolved in the cetyl trimethylammonium bromide solution for obtaining that concentration is 0.01~0.02mol/L in 40mL distilled water, matches somebody with somebody Concentration processed is 1.0~4.0mol/L ammonia spirit, then by zirconium oxychloride solution and cetyl trimethylammonium bromide solution Stirred after mixing and control temperature to be not higher than 50 DEG C, ammonia spirit is added dropwise to basic zirconium chloride and cetyl trimethyl bromine In the mixed solution for changing ammonium, it is heated to 70 DEG C after dripping ammonia spirit and stirs to precipitating completely, separated with centrifuge, will be heavy Form sediment and dry, be calcined, grinding.
3. the preparation method of Mg alloy surface selfreparing erosion shield according to claim 2, it is characterized in that, it is described to incite somebody to action Corrosion inhibiter loads to the ZrO with meso-hole structure2Specifically included in carrier:First corrosion inhibiter is dissolved, then there will be mesoporous knot The ZrO of structure2Carrier is added in corrosion inhibitor solution, stirring dipping 12 hours, centrifuge separation, is precipitated through washing, is dried, born It is loaded with the ZrO of corrosion inhibiter2
4. the preparation method of Mg alloy surface selfreparing erosion shield according to claim 3, it is characterized in that with Jie The ZrO of pore structure2In the preparation process of carrier, the drying process temperature of precipitation is 110 DEG C, and drying time is 8~12h;Roasting Temperature is 500 DEG C, roasting time 4h.
5. the preparation method of Mg alloy surface selfreparing erosion shield according to claim 4, it is characterized in that by inhibition Agent loads to the ZrO with meso-hole structure2In carrier, the washing times of precipitation is twice;The drying means of precipitation is:60 DEG C, Vacuum drying chamber, 4 hours.
6. the preparation method of Mg alloy surface selfreparing erosion shield according to claim 5, it is characterized in that being loaded with The ZrO of corrosion inhibiter2Amount be weight resin 3~6%, the ZrO of corrosion inhibiter will be loaded with2After being mixed with resin, 1h is stirred;Add Add 651 curing agent, stir 1h;It is ultrasonically treated 5min;Stewing process 10min.
7. the preparation method of Mg alloy surface selfreparing erosion shield according to claim 6, it is characterized in that described will Coating number of the mixed glue solution coated on magnesium alloy matrix surface is 3 times, and curing is:Suspension solidification;Solidification temperature is room Temperature;Hardening time is 24~72h.
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CN115584501A (en) * 2022-10-26 2023-01-10 中国航发沈阳黎明航空发动机有限责任公司 Corrosive for showing macroscopic crystal defects of nickel-based superalloy single crystal blade and application thereof
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CN116004086A (en) * 2023-01-10 2023-04-25 烟台大学 Preparation method of self-repairing anti-corrosion coating based on ZIFs
CN117567892A (en) * 2024-01-16 2024-02-20 东北大学 Magnesium alloy anticorrosive paint and preparation method and application thereof

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CN113564607A (en) * 2021-07-08 2021-10-29 哈尔滨工程大学 Preparation method of magnesium alloy surface MBT/phytic acid self-repairing system
CN113564607B (en) * 2021-07-08 2023-07-21 哈尔滨工程大学 Preparation method of MBT/phytic acid self-repairing system on magnesium alloy surface
CN115418156A (en) * 2022-09-21 2022-12-02 哈尔滨工程大学 Benzothiazole modified polyaspartate polyurea antifouling paint and preparation method and application thereof
CN115584501A (en) * 2022-10-26 2023-01-10 中国航发沈阳黎明航空发动机有限责任公司 Corrosive for showing macroscopic crystal defects of nickel-based superalloy single crystal blade and application thereof
CN115584501B (en) * 2022-10-26 2024-04-19 中国航发沈阳黎明航空发动机有限责任公司 Macroscopic crystal defect display corrosive agent for nickel-based superalloy single crystal blade and application thereof
CN115820019A (en) * 2022-12-26 2023-03-21 河南大学 Low-porosity low-thickness magnesium alloy composite coating and preparation method and application thereof
CN115820019B (en) * 2022-12-26 2024-02-09 河南大学 Low-porosity low-thickness magnesium alloy composite coating and preparation method and application thereof
CN116004086A (en) * 2023-01-10 2023-04-25 烟台大学 Preparation method of self-repairing anti-corrosion coating based on ZIFs
CN117567892A (en) * 2024-01-16 2024-02-20 东北大学 Magnesium alloy anticorrosive paint and preparation method and application thereof

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Application publication date: 20180109