CN102677127A - Magnesium alloy microarc oxidation-electrophoresis composite coating and preparation method thereof - Google Patents
Magnesium alloy microarc oxidation-electrophoresis composite coating and preparation method thereof Download PDFInfo
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Abstract
The invention provides a magnesium alloy microarc oxidation-electrophoresis composite coating which consists of a ceramic layer and a deposition layer. The ceramic layer is covered on the surface of magnesium alloy through microarc oxidation treatment and the deposition layer deposits on the surface of the ceramic layer through electrophoresis treatment. The thickness of the ceramic layer is 15micrometers-35 micrometers, the surface roughness Ra is 2.0 micrometer -4.5 micrometer and the porosity factor is 15%-40%. The thickness of the deposition layer is 20 micrometers -45micrometers. The invention further provides a preparation method of the composite coating, which includes the following steps: firstly, carrying out microarc oxidation treatment on the magnesium alloy to obtain the ceramic layer on the magnesium alloy surface; and secondly, carrying out electrophoresis treatment on the magnesium alloy which is coated with the ceramic layer on the surface to obtain the microarc oxidation-electrophoresis composite coating. The magnesium alloy microarc oxidation- electrophoresis composite coating has excellent comprehensive performances and can fully satisfy the requirements for corrosion resistance and resistances to heat, humidity and the like of magnesium alloy coatings in China national defense military industry and aviation fields.
Description
Technical field
The invention belongs to technical field of magnesium alloy surface treatment, be specifically related to a kind of magnesium alloy differential arc oxidation-electrophoresis compound coating and preparation method thereof.
Background technology
Magnesiumalloy has advantages such as density is little, specific tenacity is high, specific rigidity is high, damping performance is good, capability of electromagnetic shielding is good; Have significant advantage at aspects such as reducing energy consumption, minimizing environmental pollution, realization lightweight, therefore be widely used in fields such as automobile, electronics, weaponry, defence and military, aerospace.
Yet; The standard potential of magnesiumalloy is extremely negative, and its solidity to corrosion is very poor, and the sull that the surface forms behind natural oxidation in atmosphere is loose porous; Basically do not possess provide protection; Therefore magnesiumalloy is easy to receive corrosion failure, and especially in particular surroundings such as high humidity, high-temperature, highly-saline complicated severe environment, dense corrosive environment can cause serious corrosion to magnesiumalloy.
The surface treatment method of magnesiumalloy mainly contains anodic oxidation, chemical oxidation, differential arc oxidation and electrophoresis phosphatization etc. in the industrial production at present.
Magnesiumalloy after anodic oxidation or chemical oxidation treatment records its anti-corrosion time≤100h through neutral salt spray corrosion test, far below the conventional protection against corrosion requirement more than the 500h.
Differential arc oxidation is that on anodize technology basis, grow up a kind of is matrix with valve metals such as aluminium, magnesium, titanium or its alloy, in the novel method of its surface preparation ceramic layer.The surface in situ that the moment high temperature sintering of this method through microcell acts on matrix grows one deck oxide ceramic layer; This ceramic layer and matrix combine excellent propertys such as firm, its solidity to corrosion and wear resistance, can satisfy the solidity to corrosion requirement in the general environment, but in particular surroundings such as hot and humid, its solidity to corrosion and needs of production also have bigger gap.
The electrophoresis phosphating process can make the solidity to corrosion of magnesiumalloy significantly improve." Zinc phosphating of Mg alloy surface and ability cathode electrophoresis " that " the Jiangsu University's journal " of 2007 the 1st phases delivered by people such as connecting construction discloses a kind of elder generation and prepared one deck zinc phosphating film at Mg alloy surface; On phosphatize phosphate coat, carry out the method for ability cathode electrophoresis Processing of Preparation compound coating then, utilize the salt air corrosion of the compound coating ability 1000h of this method preparation.But this electrophoresis phosphating process process is complicated, and wastewater discharge is big, and environmental pollution is serious.
Discover, substitute the electrophoresis phosphating process with micro-arc oxidation process, can improve the solidity to corrosion of magnesiumalloy, the oxide ceramic layer of differential arc oxidation and electrophoretic deposition layer have very high bonding force, and can simplify the operation of electrophoresis process.
" microtexture and the corrosion resistance of magnesium alloy differential arc electrophoresis composite film " delivered by people such as Yang Wei in 2009 the 4th phases " investigation of materials journal " discloses and a kind of magnesiumalloy carried out the method that differential arc oxidation-electrophoretic process prepares composite film.The bonding force of ceramic layer and electrophoretic deposition layer is high in the composite film of this method preparation, the salt air corrosion of ability 800h; But its over-all properties is not as good as the compound coating of electrophoresis phosphating process preparation, and do not relate to for performances such as humidity resistance that improves magnesiumalloy and endurance empty oil immersion bubbles.
Publication number is the method that the Chinese patent of CN101376973A provides workpiece such as a kind of vacuum sputtering and electrophoresis combined coating processing micro-arc oxidation aluminium, magnesium, titanium.This method is carried out differential arc oxidation to workpiece such as aluminium, magnesium, titaniums earlier and is obtained ceramic layer; Carrying out vacuum splashing and plating then handles; Make the ceramic layer surface obtain electroconductive coating, and adopt the electrophoretic paint of different colours to carry out electrophoretic process, make workpiece have coloured appearance; Have ceramic effect concurrently and pass through color effect, have stronger metal-like; But this invention does not relate to for performances such as solidity to corrosion that improves workpiece such as aluminium, magnesium, titanium and humidity resistances.
Publication number is that the Chinese patent of CN101376974A provides a kind of micro-arc oxidation workpiece vacuum splashing and plating thin-film against electromagnetic interference electrophoresis combined coating method for processing.This method is handled through vacuum splashing and plating, but obtains to prevent the coating of EMI property and electroconductibility at the arc differential oxide ceramic coatingsurface, again this coating is carried out electrophoretic painting and handles, and makes workpiece such as aluminium, magnesium, titanium have pottery concurrently, passes through color and anti-EMI effect; But this invention does not relate to for performances such as solidity to corrosion that improves workpiece such as aluminium, magnesium, titanium and humidity resistances.
Notification number is the method that the Chinese patent of CN100588755C provides a kind of magnesium alloy differential arc electrophoresis composite surface to handle.It is that electrolytic solution carries out the differential arc oxidation processing that this method at first places silicate with pending magnesium alloy workpiece; After treating that magnesium alloy work-piece surface forms ceramic layer; Again workpiece is immersed in the deionized water; Clean with ultrasonic cleaner, at last workpiece is carried out electrophoretic process, finally form compound coating.The operation of conventional electrophoresis process has been simplified in this invention, has reduced environmental pollution, the salt spray corrosion test of the compound coating ability 700h of preparation.But its over-all properties is not as good as the compound coating of phosphatization rear electrophoresis; And this invention does not relate to for performances such as moisture-proof heat that improves magnesiumalloy and endurance empty oil immersion bubbles.
Summary of the invention
Technical problem to be solved by this invention is the deficiency to above-mentioned prior art, provides that a kind of preparation technology is simple, low production cost, is suitable for the magnesium alloy differential arc oxidation-electrophoresis compound coating of large-scale industrial production.This compound coating has the excellent comprehensive performance, can satisfy fully that fields such as present China's national defense military project, aerospace, weaponry are corrosion-resistant to magnesium alloy coating, moisture-proof is warm, performance demands such as endurance empty oil immersion bubble, shock-resistant and bonding strength.
For solving the problems of the technologies described above; The technical scheme that the present invention adopts is: a kind of magnesium alloy differential arc oxidation-electrophoresis compound coating; Form by being overlying on the ceramic layer of Mg alloy surface after handling through differential arc oxidation and after electrophoretic process, being deposited on the surperficial settled layer of said ceramic layer, it is characterized in that the thickness of said ceramic layer is 15 μ m~35 μ m; Surface roughness Ra is 2.0 μ m~4.5 μ m, and porosity is 15%~40%; The thickness of said settled layer is 20 μ m~45 μ m.
Above-mentioned a kind of magnesium alloy differential arc oxidation-electrophoresis compound coating, the thickness of said ceramic layer are 20 μ m~30 μ m, and surface roughness Ra is 2.5 μ m~3.5 μ m, and porosity is 20%~30%; The thickness of said settled layer is 30 μ m~40 μ m.
Above-mentioned a kind of magnesium alloy differential arc oxidation-electrophoresis compound coating, the thickness of said ceramic layer are 25 μ m, and surface roughness Ra is 3.0 μ m, and porosity is 25%; The thickness of said settled layer is 35 μ m.
In addition, the present invention also provides a kind of method for preparing above-mentioned magnesium alloy differential arc oxidation-electrophoresis compound coating, it is characterized in that this method may further comprise the steps:
Step 1, with magnesiumalloy after organic solvent or washed with de-ionized water are clean; Placing differential arc oxidation electrolytic solution, is anode with the magnesiumalloy, is negative electrode with the stainless steel; The temperature of keeping differential arc oxidation electrolytic solution is 20 ℃~40 ℃; Adopting the pulse power, is that 400V~650V, frequency are that 100Hz~300Hz, dutycycle are that differential arc oxidation is handled 20min~40min under 20%~45% the condition at voltage, obtains ceramic layer at Mg alloy surface; Said differential arc oxidation electrolytic solution is that silicate is electrolytic solution or aluminate-series electrolytic solution;
Step 2, the magnesiumalloy that surface in the step 1 is covered with ceramic layer place electrophoresis liquid; The magnesiumalloy that is covered with ceramic layer with the surface is a negative electrode; With the stainless steel is anode, and the temperature of keeping electrophoresis liquid is 15 ℃~30 ℃, adopts the pulse power; At voltage is that 180V~300V, frequency are that 100Hz~600Hz, dutycycle are electrophoretic process 2min~5min under 10%~20% the condition, obtains settled layer on the ceramic layer surface; Said electrophoresis liquid is a cationic cataphoresis liquid;
Step 3, the magnesiumalloy that surface in the step 2 is covered with ceramic layer and settled layer are cured processing, obtain magnesium alloy differential arc oxidation-electrophoresis compound coating at Mg alloy surface behind the naturally cooling.
Above-mentioned method, organic solvent described in the step 1 are acetone or ETHYLE ACETATE.
Above-mentioned method, silicate described in the step 1 are that electrolytic solution is formulated by water glass, additive and deionized water; Said silicate is that the mass concentration of electrolytic solution mesosilicic acid sodium is 7g/L~28g/L, and the mass concentration of additive is 0.5g/L~4g/L; Said additive is Sodium Fluoride, Potassium monofluoride, tsp or Sodium hexametaphosphate 99.
Above-mentioned method, silicate described in the step 1 are that electrolytic solution is formulated by water glass and deionized water; Said silicate is that the mass concentration of electrolytic solution mesosilicic acid sodium is 7g/L~28g/L.
Above-mentioned method, the electrolytic solution of aluminate-series described in the step 1 is formulated by sodium aluminate, additive and deionized water; The mass concentration of sodium aluminate is 8g/L~12g/L in the said aluminate-series electrolytic solution, and the mass concentration of additive is 2g/L~6g/L; Said additive is Sodium Fluoride, Potassium monofluoride, tsp or Sodium hexametaphosphate 99.
Above-mentioned method, the liquid of cationic cataphoresis described in the step 2 prepares by following method: with cationic epoxy electrocoating paint and colorant by volume 3~5: 1 mix after, be scattered in equably in the deionized water, obtain cationic cataphoresis liquid; The percent by volume of deionized water is 50%~70% in the said cationic cataphoresis liquid.
Above-mentioned method, the temperature of solidification treatment described in the step 3 are 180 ℃~185 ℃, and the time of solidification treatment is 20min~25min.
The present invention compared with prior art has the following advantages:
(1) raw material sources of the present invention are extensive, and preparation technology is simple, and low production cost is suitable for large-scale industrial production;
(2) the present invention at first carries out the differential arc oxidation processing to magnesiumalloy; After treating that Mg alloy surface forms ceramic layer; Utilize the growth in situ of this ceramic layer, the good and surface irregularity porous characteristics with matrix bond; Directly be placed on and carry out depositing treatment in the electrophoresis liquid, make the electrophoresis organism be deposited on the ceramic layer surface smoothly, equably, finally form magnesium alloy differential arc oxidation-electrophoresis compound coating; The ceramic layer in the magnesium alloy differential arc oxidation-electrophoresis compound coating of employing the present invention preparation and the bonding force of settled layer are high, have guaranteed that its over-all properties is significantly improved;
(3) the present invention need not the magnesiumalloy that the surface is covered with ceramic layer is carried out the conductive processing before the electrophoresis; Directly be placed on and carry out depositing treatment in the electrophoresis liquid; Simplified the operation of electrophoresis process greatly; Reduce production cost, significantly improved the over-all properties of magnesium alloy differential arc oxidation-electrophoresis compound coating, can satisfy the application request of performances such as magnesiumalloy in the particular surroundings such as hot and humid is corrosion-resistant, moisture-proof heat fully;
(4) the present invention is through carrying out the screening of component and the optimization of proportioning to differential arc oxidation electrolytic solution and electrophoresis liquid; Avoid the use of and contain the component that Cr6+ etc. works the mischief to human body and environment; Avoid the use of instability, be prone to decomposition components, make that preparation technology of the present invention is simple, controlled, easy handling;
(5) magnesium alloy differential arc oxidation of the present invention-electrophoresis compound coating, the time of pressing its anti-neutral salt spray corrosion test of GB/T 10125-1997 test surpasses 2400h, and sample after corrosion test and test specimen are rated 9 grades by GB/T 6461-2002; In temperature be under 60 ℃ the condition time of hot resistance test surpass no wrinkling, foaming or obscission behind the 240h; In temperature be under 130 ℃ the condition time of endurance empty oil immersion bubble test surpass not have behind the 1200h and bubble, come off or other defect; Bonding strength between this compound coating and the magnesiumalloy is greater than 25MPa; The sticking power of electrophoretic deposition layer is assessed as 1 grade by the GB/T1720-79 test; Simultaneously, this compound coating also has advantages such as impact strength height and controllable thickness; In a word; Magnesium alloy differential arc oxidation of the present invention-electrophoresis compound coating has the excellent comprehensive performance, can satisfy fully that fields such as present China's national defense military project, aerospace, weaponry are corrosion-resistant to magnesium alloy coating, moisture-proof is warm, performance demands such as endurance empty oil immersion bubble, shock-resistant magnesiumalloy and bonding strength.
Below in conjunction with accompanying drawing and embodiment the present invention is done further explain.
Description of drawings
Fig. 1 is the cross section pattern SEM photo of magnesium alloy differential arc oxidation-electrophoresis compound coating after cold edge is handled of the embodiment of the invention 1 preparation.
Fig. 2 is the surface topography SEM photo of the magnesium alloy differential arc oxidation-electrophoresis compound coating of the embodiment of the invention 1 preparation.
Fig. 3 is the surface topography SEM photo of ceramic layer in the magnesium alloy differential arc oxidation-electrophoresis compound coating of the embodiment of the invention 1 preparation.
Embodiment
Embodiment 1
The magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating is formed by being overlying on the ceramic layer of Mg alloy surface after handling through differential arc oxidation and after electrophoretic process, being deposited on the surperficial settled layer of said ceramic layer; The thickness of said ceramic layer is 25 μ m; Surface roughness Ra is 3.0 μ m, and porosity is 25%; The thickness of said settled layer is 35 μ m.
The preparation method of the magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating may further comprise the steps:
Step 1, with the AZ91D magnesiumalloy after washed with de-ionized water is clean; Placing differential arc oxidation electrolytic solution, is anode with the magnesiumalloy, is negative electrode with the stainless steel; The temperature of keeping differential arc oxidation electrolytic solution is 20 ℃~40 ℃; Adopting the pulse power, is that 550V, frequency are that 150Hz, dutycycle are that differential arc oxidation is handled 30min under 25% the condition at voltage, obtains ceramic layer at Mg alloy surface; Said differential arc oxidation electrolytic solution is that silicate is electrolytic solution; Preferred silicate is that electrolytic solution is formulated by water glass, Sodium Fluoride and deionized water, and wherein the mass concentration of water glass is 21g/L, and the mass concentration of Sodium Fluoride is 0.5g/L;
Step 2, the magnesiumalloy that surface in the step 1 is covered with ceramic layer place cationic cataphoresis liquid; The magnesiumalloy that is covered with ceramic layer with the surface is a negative electrode; With the stainless steel is anode, and the temperature of keeping electrophoresis liquid is 15 ℃~30 ℃, adopts the pulse power; At voltage is that 220V, frequency are that 100Hz, dutycycle are electrophoretic process 3min under 10% the condition, obtains settled layer on the ceramic layer surface; Preferred cation type electrophoresis liquid obtains by following method preparation: after cationic epoxy electrocoating paint and colorant were mixed in 4.5: 1 by volume; Be scattered in the deionized water equably; Obtain cationic cataphoresis liquid, the percent by volume of deionized water is 50% in this cationic cataphoresis liquid;
Step 3, the magnesiumalloy that surface in the step 2 is covered with ceramic layer and settled layer are solidification treatment 23min under 183 ℃ the condition in temperature, obtain magnesium alloy differential arc oxidation-electrophoresis compound coating at Mg alloy surface behind the naturally cooling.
The cross section pattern SEM photo of magnesium alloy differential arc oxidation-electrophoresis compound coating after cold edge is handled of present embodiment preparation is as shown in Figure 1.The I district is cold edge material layer among the figure, the settled layer of II district for obtaining through electrophoretic process, and the III district is for handling the ceramic layer that obtains through differential arc oxidation, and the IV district is a magnesiumalloy.Visible by Fig. 1, settled layer is fine and close, evenly, ceramic layer is vesicular structure but does not have tangible communicating pores and exist that settled layer is partially submerged in the hole of ceramic layer, combining between settled layer and the ceramic layer, between ceramic layer and the magnesiumalloy is firm.
The surface topography SEM photo of the magnesium alloy differential arc oxidation-electrophoresis compound coating of present embodiment preparation is as shown in Figure 2.By the surface compact of visible this compound coating of Fig. 2, even, smooth.
The surface topography SEM photo of ceramic layer is as shown in Figure 3 in the magnesium alloy differential arc oxidation-electrophoresis compound coating of present embodiment preparation.The ceramic layer surface irregularity porous that after differential arc oxidation is handled, obtains among the figure, roughness Ra is 3.0 μ m, porosity is 25%, the diameter of largest hole opening part is about 39 μ m.
Embodiment 2
The magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating is formed by being overlying on the ceramic layer of Mg alloy surface after handling through differential arc oxidation and after electrophoretic process, being deposited on the surperficial settled layer of said ceramic layer; The thickness of said ceramic layer is 35 μ m; Surface roughness Ra is 4.5 μ m, and porosity is 40%; The thickness of said settled layer is 45 μ m.
The preparation method of the magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating may further comprise the steps:
Step 1, with the MB15 magnesiumalloy after acetone is clean; Placing differential arc oxidation electrolytic solution, is anode with the magnesiumalloy, is negative electrode with the stainless steel; The temperature of keeping differential arc oxidation electrolytic solution is 20 ℃~40 ℃; Adopting the pulse power, is that 650V, frequency are that 300Hz, dutycycle are that differential arc oxidation is handled 40min under 45% the condition at voltage, obtains ceramic layer at Mg alloy surface; Said differential arc oxidation electrolytic solution is that silicate is electrolytic solution, and preferred silicate is that electrolytic solution is formulated by water glass, Potassium monofluoride and deionized water, and wherein the mass concentration of water glass is 14g/L, and the mass concentration of Potassium monofluoride is 0.5g/L;
Step 2, the magnesiumalloy that surface in the step 1 is covered with ceramic layer place cationic cataphoresis liquid; The magnesiumalloy that is covered with ceramic layer with the surface is a negative electrode; With the stainless steel is anode, and keeping the electrophoresis liquid temperature is 15 ℃~30 ℃, adopts the pulse power; At voltage is that 300V, frequency are that 600Hz, dutycycle are electrophoretic process 5min under 20% the condition, obtains settled layer on the ceramic layer surface; Preferred cation type electrophoresis liquid is prepared by following method: after cationic epoxy electrocoating paint and colorant were mixed in 5: 1 by volume; Be scattered in the deionized water equably; Obtain cationic cataphoresis liquid, the percent by volume of deionized water is 70% in this cationic cataphoresis liquid;
Step 3, the magnesiumalloy that surface in the step 2 is covered with ceramic layer and settled layer are solidification treatment 20min under 185 ℃ the condition in temperature, obtain magnesium alloy differential arc oxidation-electrophoresis compound coating at Mg alloy surface behind the naturally cooling.
Embodiment 3
The magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating is formed by being overlying on the ceramic layer of Mg alloy surface after handling through differential arc oxidation and after electrophoretic process, being deposited on the surperficial settled layer of said ceramic layer; The thickness of said ceramic layer is 18 μ m; Surface roughness Ra is 3.27 μ m, and porosity is 29.5%; The thickness of said settled layer is 31 μ m.
The preparation method of the magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating may further comprise the steps:
Step 1, with the ZM6 magnesiumalloy after ETHYLE ACETATE cleans up; Placing differential arc oxidation electrolytic solution, is anode with the magnesiumalloy, is negative electrode with the stainless steel; Keeping the differential arc oxidation electrolyte temperature is 20 ℃~40 ℃; Adopting the pulse power, is that 450V, frequency are that 300Hz, dutycycle are that differential arc oxidation is handled 20min under 20% the condition at voltage, obtains ceramic layer at Mg alloy surface; Said differential arc oxidation electrolytic solution is that silicate is electrolytic solution, and preferred silicate is that electrolytic solution is formulated by water glass, tsp and deionized water, and wherein the mass concentration of water glass is 28g/L, and the mass concentration of tsp is 4g/L;
Step 2, the magnesiumalloy that surface in the step 1 is covered with ceramic layer place cationic cataphoresis liquid; The magnesiumalloy that is covered with ceramic layer with the surface is a negative electrode; With the stainless steel is anode, and keeping the electrophoresis liquid temperature is 15 ℃~30 ℃, adopts the pulse power; At voltage is that 180V, frequency are that 100Hz, dutycycle are electrophoretic process 4min under 15% the condition, obtains settled layer on the ceramic layer surface; Preferred cation type electrophoresis liquid is prepared by following method: after cationic epoxy electrocoating paint and colorant were mixed in 4: 1 by volume; Be scattered in the deionized water equably; Obtain cationic cataphoresis liquid, the percent by volume of deionized water is 50% in this cationic cataphoresis liquid;
Step 3, the magnesiumalloy that surface in the step 2 is covered with ceramic layer and settled layer are solidification treatment 20min under 185 ℃ the condition in temperature, obtain magnesium alloy differential arc oxidation-electrophoresis compound coating at Mg alloy surface behind the naturally cooling.
Embodiment 4
The magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating is formed by being overlying on the ceramic layer of Mg alloy surface after handling through differential arc oxidation and after electrophoretic process, being deposited on the surperficial settled layer of said ceramic layer; The thickness of said ceramic layer is 15 μ m; Surface roughness Ra is 2.0 μ m, and porosity is 15%; The thickness of said settled layer is 20 μ m.
The preparation method of the magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating may further comprise the steps:
Step 1, with the AZ91D magnesiumalloy after washed with de-ionized water is clean; Placing differential arc oxidation electrolytic solution, is anode with the magnesiumalloy, is negative electrode with the stainless steel; The temperature of keeping differential arc oxidation electrolytic solution is 20 ℃~40 ℃; Adopting the pulse power, is that 400V, frequency are that 200Hz, dutycycle are that differential arc oxidation is handled 25min under 30% the condition at voltage, obtains ceramic layer at Mg alloy surface; Said differential arc oxidation electrolytic solution is that silicate is electrolytic solution; Preferred silicate is that electrolytic solution is formulated by water glass, Sodium hexametaphosphate 99 and deionized water, and wherein the mass concentration of water glass is 7g/L, and the mass concentration of Sodium hexametaphosphate 99 is 4g/L;
Step 2, the magnesiumalloy that surface in the step 1 is covered with ceramic layer place cationic cataphoresis liquid; The magnesiumalloy that is covered with ceramic layer with the surface is a negative electrode; With the stainless steel is anode, and keeping the electrophoresis liquid temperature is 15 ℃~30 ℃, adopts the pulse power; At voltage is that 280V, frequency are that 400Hz, dutycycle are electrophoretic process 4.5min under 18% the condition, obtains settled layer on the ceramic layer surface; Preferred cation type electrophoresis liquid is prepared by following method: after cationic epoxy electrocoating paint and colorant were mixed in 3: 1 by volume; Be scattered in the deionized water equably; Obtain cationic cataphoresis liquid, the percent by volume of deionized water is 60% in this cationic cataphoresis liquid;
Step 3, the magnesiumalloy that surface in the step 2 is covered with ceramic layer and settled layer are solidification treatment 23min under 182 ℃ the condition in temperature, obtain magnesium alloy differential arc oxidation-electrophoresis compound coating at Mg alloy surface behind the naturally cooling.
Embodiment 5
The magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating is formed by being overlying on the ceramic layer of Mg alloy surface after handling through differential arc oxidation and after electrophoretic process, being deposited on the surperficial settled layer of said ceramic layer; The thickness of said ceramic layer is 27 μ m; Surface roughness Ra is 3.2 μ m, and porosity is 34.2%; The thickness of said settled layer is 20 μ m~33 μ m.
The preparation method of the magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating may further comprise the steps:
Step 1, with the ZM6 magnesiumalloy after organic solvent cleans up; Placing differential arc oxidation electrolytic solution, is anode with the magnesiumalloy, is negative electrode with the stainless steel; Keeping the differential arc oxidation electrolyte temperature is 20 ℃~40 ℃; Adopting the pulse power, is that 480V, frequency are that 250Hz, dutycycle are that differential arc oxidation is handled 35min under 20% the condition at voltage, obtains ceramic layer at Mg alloy surface; Said differential arc oxidation electrolytic solution is that silicate is electrolytic solution, and preferred silicate is that electrolytic solution is formulated by water glass and deionized water, and wherein the mass concentration of water glass is 25g/L; Said organic solvent is preferably acetone or ETHYLE ACETATE;
Step 2, the magnesiumalloy that surface in the step 1 is covered with ceramic layer place cationic cataphoresis liquid; The magnesiumalloy that is covered with ceramic layer with the surface is a negative electrode; With the stainless steel is anode, and keeping the electrophoresis liquid temperature is 15 ℃~30 ℃, adopts the pulse power; At voltage is that 240V, frequency are that 600Hz, dutycycle are electrophoretic process 2min under 20% the condition, obtains settled layer on the ceramic layer surface; Preferred cation type electrophoresis liquid is prepared by following method: after cationic epoxy electrocoating paint and colorant were mixed in 3: 1 by volume; Be scattered in the deionized water equably; Obtain cationic cataphoresis liquid, the percent by volume of deionized water is 58% in this cationic cataphoresis liquid;
Step 3, the magnesiumalloy that surface in the step 2 is covered with ceramic layer and settled layer are solidification treatment 20min under 185 ℃ the condition in temperature, obtain magnesium alloy differential arc oxidation-electrophoresis compound coating at Mg alloy surface behind the naturally cooling.
Embodiment 6
The magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating is formed by being overlying on the ceramic layer of Mg alloy surface after handling through differential arc oxidation and after electrophoretic process, being deposited on the surperficial settled layer of said ceramic layer; The thickness of said ceramic layer is 28 μ m; Surface roughness Ra is 4.1 μ m, and porosity is 39%; The thickness of said settled layer is 41 μ m.
The preparation method of the magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating may further comprise the steps:
Step 1, with the AZ91D magnesiumalloy after washed with de-ionized water is clean; Placing differential arc oxidation electrolytic solution, is anode with the magnesiumalloy, is negative electrode with the stainless steel; Keeping the differential arc oxidation electrolyte temperature is 20 ℃~40 ℃; Adopting the pulse power, is that 650V, frequency are that 100Hz, dutycycle are that differential arc oxidation is handled 40min under 20% the condition at voltage, obtains ceramic layer at Mg alloy surface; Said differential arc oxidation electrolytic solution is aluminate-series electrolytic solution; Preferred aluminate-series electrolytic solution is formulated by sodium aluminate, Potassium monofluoride and deionized water, and wherein the mass concentration of sodium aluminate is 8g/L, and the mass concentration of Potassium monofluoride is 1g/L;
Step 2, the magnesiumalloy that surface in the step 1 is covered with ceramic layer place cationic cataphoresis liquid; The magnesiumalloy that is covered with ceramic layer with the surface is a negative electrode; With the stainless steel is anode, and keeping the electrophoresis liquid temperature is 15 ℃~30 ℃, adopts the pulse power; At voltage is that 260V, frequency are that 550Hz, dutycycle are electrophoretic process 4.5min under 10% the condition, obtains settled layer on the ceramic layer surface; Preferred cation type electrophoresis liquid is prepared by following method: after cationic epoxy electrocoating paint and colorant were mixed in 4.5: 1 by volume; Be scattered in the deionized water equably; Obtain cationic cataphoresis liquid, the percent by volume of deionized water is 62.5% in this cationic cataphoresis liquid;
Step 3, the magnesiumalloy that surface in the step 2 is covered with ceramic layer and settled layer are solidification treatment 25min under 180 ℃ the condition in temperature, obtain magnesium alloy differential arc oxidation-electrophoresis compound coating at Mg alloy surface behind the naturally cooling.
Embodiment 7
The magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating is formed by being overlying on the ceramic layer of Mg alloy surface after handling through differential arc oxidation and after electrophoretic process, being deposited on the surperficial settled layer of said ceramic layer; The thickness of said ceramic layer is 24 μ m; Surface roughness Ra is 3.8 μ m, and porosity is 35%; The thickness of said settled layer is 36 μ m.
The preparation method of the magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating may further comprise the steps:
Step 1, with the AZ91D magnesiumalloy after acetone is clean; Placing differential arc oxidation electrolytic solution, is anode with the magnesiumalloy, is negative electrode with the stainless steel; Keeping the differential arc oxidation electrolyte temperature is 20 ℃~40 ℃; Adopting the pulse power, is that 550V, frequency are that 300Hz, dutycycle are that differential arc oxidation is handled 30min under 26% the condition at voltage, obtains ceramic layer at Mg alloy surface; Said differential arc oxidation electrolytic solution is aluminate-series electrolytic solution; Preferred aluminate-series electrolytic solution is formulated by sodium aluminate, Sodium hexametaphosphate 99 and deionized water, and wherein the mass concentration of sodium aluminate is 12g/L, and the mass concentration of Sodium hexametaphosphate 99 is 6g/L;
Step 2, the magnesiumalloy that surface in the step 1 is covered with ceramic layer place cationic cataphoresis liquid; The magnesiumalloy that is covered with ceramic layer with the surface is a negative electrode; With the stainless steel is anode, and keeping the electrophoresis liquid temperature is 15 ℃~30 ℃, adopts the pulse power; At voltage is that 300V, frequency are that 450Hz, dutycycle are electrophoretic process 3.5min under 20% the condition, obtains settled layer on the ceramic layer surface; Preferred cation type electrophoresis liquid is prepared by following method: after cationic epoxy electrocoating paint and colorant were mixed in 3.5: 1 by volume; Be scattered in the deionized water equably; Obtain cationic cataphoresis liquid, the percent by volume of deionized water is 50% in this cationic cataphoresis liquid;
Step 3, the magnesiumalloy that surface in the step 2 is covered with ceramic layer and settled layer are solidification treatment 23min under 185 ℃ the condition in temperature, obtain magnesium alloy differential arc oxidation-electrophoresis compound coating at Mg alloy surface behind the naturally cooling.
Embodiment 8
The magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating is formed by being overlying on the ceramic layer of Mg alloy surface after handling through differential arc oxidation and after electrophoretic process, being deposited on the surperficial settled layer of said ceramic layer; The thickness of said ceramic layer is 19 μ m; Surface roughness Ra is 3.9 μ m, and porosity is 32%; The thickness of said settled layer is 34 μ m.
The preparation method of the magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating may further comprise the steps:
Step 1, with the MB15 magnesiumalloy after ETHYLE ACETATE cleans up; Placing differential arc oxidation electrolytic solution, is anode with the magnesiumalloy, is negative electrode with the stainless steel; Keeping the differential arc oxidation electrolyte temperature is 20 ℃~40 ℃; Adopting the pulse power, is that 550V, frequency are that 100Hz, dutycycle are that differential arc oxidation is handled 30min under 40% the condition at voltage, obtains ceramic layer at Mg alloy surface; Said differential arc oxidation electrolytic solution is aluminate-series electrolytic solution, and preferred aluminate-series electrolytic solution is formulated by sodium aluminate, tsp and deionized water, and wherein the mass concentration of sodium aluminate is 10g/L, and the mass concentration of tsp is 4g/L;
Step 2, the magnesiumalloy that surface in the step 1 is covered with ceramic layer place cationic cataphoresis liquid; The magnesiumalloy that is covered with ceramic layer with the surface is a negative electrode; With the stainless steel is anode, and keeping the electrophoresis liquid temperature is 15 ℃~30 ℃, adopts the pulse power; At voltage is that 280V, frequency are that 600Hz, dutycycle are electrophoretic process 4min under 15% the condition, obtains settled layer at ceramic layer; Preferred cation type electrophoresis liquid is prepared by following method: after cationic epoxy electrocoating paint and colorant were mixed in 5: 1 by volume; Be scattered in the deionized water equably; Obtain cationic cataphoresis liquid, the percent by volume of deionized water is 70% in this cationic cataphoresis liquid;
Step 3, the magnesiumalloy that surface in the step 2 is covered with ceramic layer and settled layer are solidification treatment 20min under 185 ℃ the condition in temperature, obtain magnesium alloy differential arc oxidation-electrophoresis compound coating at Mg alloy surface behind the naturally cooling.
Embodiment 9
The magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating is formed by being overlying on the ceramic layer of Mg alloy surface after handling through differential arc oxidation and after electrophoretic process, being deposited on the surperficial settled layer of said ceramic layer; The thickness of said ceramic layer is 30 μ m; Surface roughness Ra is 2.5 μ m, and porosity is 20%; The thickness of said settled layer is 40 μ m.
The preparation method of the magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating may further comprise the steps:
Step 1, with the MB15 magnesiumalloy after organic solvent cleans up; Placing differential arc oxidation electrolytic solution, is anode with the magnesiumalloy, is negative electrode with the stainless steel; Keeping the differential arc oxidation electrolyte temperature is 20 ℃~40 ℃; Adopting the pulse power, is that 600V, frequency are that 100Hz, dutycycle are that differential arc oxidation is handled 20min under 30% the condition at voltage, obtains ceramic layer at Mg alloy surface; Said differential arc oxidation electrolytic solution is aluminate-series electrolytic solution, and preferred aluminate-series electrolytic solution is formulated by sodium aluminate, Sodium Fluoride and deionized water, and wherein the mass concentration of sodium aluminate is 9g/L, and the mass concentration of Sodium Fluoride is 3g/L; Said organic solvent is preferably acetone or ETHYLE ACETATE;
Step 2, the magnesiumalloy that surface in the step 1 is covered with ceramic layer place cationic cataphoresis liquid; The magnesiumalloy that is covered with ceramic layer with the surface is a negative electrode; With the stainless steel is anode, and keeping the electrophoresis liquid temperature is 15 ℃~30 ℃, adopts the pulse power; At voltage is that 200V, frequency are that 600Hz, dutycycle are electrophoretic process 2min under 10% the condition, obtains settled layer on the ceramic layer surface; Preferred cation type electrophoresis liquid is prepared by following method: after cationic epoxy electrocoating paint and colorant were mixed in 4: 1 by volume; Be scattered in the deionized water equably; Obtain cationic cataphoresis liquid, the percent by volume of deionized water is 70% in this cationic cataphoresis liquid;
Step 3, the magnesiumalloy that surface in the step 2 is covered with ceramic layer and settled layer are solidification treatment 20min under 180 ℃ the condition in temperature, obtain magnesium alloy differential arc oxidation-electrophoresis compound coating at Mg alloy surface behind the naturally cooling.
Embodiment 10
The magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating is formed by being overlying on the ceramic layer of Mg alloy surface after handling through differential arc oxidation and after electrophoretic process, being deposited on the surperficial settled layer of said ceramic layer; The thickness of said ceramic layer is 20 μ m; Surface roughness Ra is 3.5 μ m, and porosity is 30%; The thickness of said settled layer is 30 μ m.
The preparation method of the magnesium alloy differential arc oxidation of present embodiment-electrophoresis compound coating may further comprise the steps:
Step 1, with the AZ91D magnesiumalloy after organic solvent or washed with de-ionized water are clean; Placing differential arc oxidation electrolytic solution, is anode with the magnesiumalloy, is negative electrode with the stainless steel; The temperature of keeping differential arc oxidation electrolytic solution is 20 ℃~40 ℃; Adopting the pulse power, is that 580V, frequency are that 100Hz, dutycycle are that differential arc oxidation is handled 25min under 20% the condition at voltage, obtains ceramic layer at Mg alloy surface; Said differential arc oxidation electrolytic solution is aluminate-series electrolytic solution; Preferred aluminate-series electrolytic solution is formulated by sodium aluminate, tsp and deionized water, and wherein the mass concentration of sodium aluminate is 11g/L, and the mass concentration of tsp is 2g/L; Said organic solvent is preferably acetone or ETHYLE ACETATE;
Step 2, the magnesiumalloy that surface in the step 1 is covered with ceramic layer place cationic cataphoresis liquid; The magnesiumalloy that is covered with ceramic layer with the surface is a negative electrode; With the stainless steel is anode, and keeping the electrophoresis liquid temperature is 15 ℃~30 ℃, adopts the pulse power; At voltage is that 240V, frequency are that 100Hz, dutycycle are electrophoretic process 4min under 20% the condition, obtains settled layer on the ceramic layer surface; Preferred cation type electrophoresis liquid is prepared by following method: after cationic epoxy electrocoating paint and colorant were mixed in 4.8: 1 by volume; Be scattered in the deionized water equably; Obtain cationic cataphoresis liquid, the percent by volume of deionized water is 70% in this cationic cataphoresis liquid;
Step 3, the magnesiumalloy that surface in the step 2 is covered with ceramic layer and settled layer are solidification treatment 23min under 185 ℃ the condition in temperature, obtain magnesium alloy differential arc oxidation-electrophoresis compound coating at Mg alloy surface behind the naturally cooling.
Cationic epoxy electrocoating paint of the present invention is the cationic epoxy electrocoating paint of the commercially available general type that is easy to get.
The above only is preferred embodiment of the present invention, is not that the present invention is done any restriction.Every according to inventing technical spirit to any simple modification, change and equivalence variation that above embodiment did, all still belong in the protection domain of technical scheme of the present invention.
Claims (10)
1. magnesium alloy differential arc oxidation-electrophoresis compound coating; Form by being overlying on the ceramic layer of Mg alloy surface after handling through differential arc oxidation and after electrophoretic process, being deposited on the surperficial settled layer of said ceramic layer; It is characterized in that; The thickness of said ceramic layer is 15 μ m~35 μ m, and surface roughness Ra is 2.0 μ m~4.5 μ m, and porosity is 15%~40%; The thickness of said settled layer is 20 μ m~45 μ m.
2. according to a kind of magnesium alloy differential arc oxidation-electrophoresis compound coating described in the claim 1, it is characterized in that the thickness of said ceramic layer is 20 μ m~30 μ m, surface roughness Ra is 2.5 μ m~3.5 μ m, and porosity is 20%~30%; The thickness of said settled layer is 30 μ m~40 μ m.
3. according to a kind of magnesium alloy differential arc oxidation-electrophoresis compound coating described in the claim 2, it is characterized in that the thickness of said ceramic layer is 25 μ m, surface roughness Ra is 3.0 μ m, and porosity is 25%; The thickness of said settled layer is 35 μ m.
4. method for preparing like claim 1, magnesium alloy differential arc oxidation described in 2 or 3-electrophoresis compound coating is characterized in that this method may further comprise the steps:
Step 1, with magnesiumalloy after organic solvent or washed with de-ionized water are clean; Placing differential arc oxidation electrolytic solution, is anode with the magnesiumalloy, is negative electrode with the stainless steel; The temperature of keeping differential arc oxidation electrolytic solution is 20 ℃~40 ℃; Adopting the pulse power, is that 400V~650V, frequency are that 100Hz~300Hz, dutycycle are that differential arc oxidation is handled 20min~40min under 20%~45% the condition at voltage, obtains ceramic layer at Mg alloy surface; Said differential arc oxidation electrolytic solution is that silicate is electrolytic solution or aluminate-series electrolytic solution;
Step 2, the magnesiumalloy that surface in the step 1 is covered with ceramic layer place electrophoresis liquid; The magnesiumalloy that is covered with ceramic layer with the surface is a negative electrode; With the stainless steel is anode, and the temperature of keeping electrophoresis liquid is 15 ℃~30 ℃, adopts the pulse power; At voltage is that 180V~300V, frequency are that 100Hz~600Hz, dutycycle are electrophoretic process 2min~5min under 10%~20% the condition, obtains settled layer on the ceramic layer surface; Said electrophoresis liquid is a cationic cataphoresis liquid;
Step 3, the magnesiumalloy that surface in the step 2 is covered with ceramic layer and settled layer are cured processing, obtain magnesium alloy differential arc oxidation-electrophoresis compound coating at Mg alloy surface behind the naturally cooling.
5. method according to claim 4 is characterized in that, organic solvent described in the step 1 is acetone or ETHYLE ACETATE.
6. method according to claim 4 is characterized in that, silicate described in the step 1 is that electrolytic solution is formulated by water glass, additive and deionized water; Said silicate is that the mass concentration of electrolytic solution mesosilicic acid sodium is 7g/L~28g/L, and the mass concentration of additive is 0.5g/L~4g/L; Said additive is Sodium Fluoride, Potassium monofluoride, tsp or Sodium hexametaphosphate 99.
7. method according to claim 4 is characterized in that, silicate described in the step 1 is that electrolytic solution is formulated by water glass and deionized water; Said silicate is that the mass concentration of electrolytic solution mesosilicic acid sodium is 7g/L~28g/L.
8. method according to claim 4 is characterized in that, the electrolytic solution of aluminate-series described in the step 1 is formulated by sodium aluminate, additive and deionized water; The mass concentration of sodium aluminate is 8g/L~12g/L in the said aluminate-series electrolytic solution, and the mass concentration of additive is 2g/L~6g/L; Said additive is Sodium Fluoride, Potassium monofluoride, tsp or Sodium hexametaphosphate 99.
9. method according to claim 4; It is characterized in that; The liquid of cationic cataphoresis described in the step 2 prepares by following method: with cationic epoxy electrocoating paint and colorant by volume 3~5: 1 mix after, be scattered in equably in the deionized water, obtain cationic cataphoresis liquid; The percent by volume of deionized water is 50%~70% in the said cationic cataphoresis liquid.
10. method according to claim 4 is characterized in that, the temperature of solidification treatment described in the step 3 is 180 ℃~185 ℃, and the time of solidification treatment is 20min~25min.
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