CN110923781A - Surface treatment method for reducing galvanic current of titanium and titanium alloy - Google Patents
Surface treatment method for reducing galvanic current of titanium and titanium alloy Download PDFInfo
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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
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- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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- C25D11/04—Anodisation of aluminium or alloys based thereon
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- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
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Abstract
The invention provides a surface treatment method for reducing galvanic current of titanium and titanium alloy, which comprises the following steps: step 1) pretreatment: cleaning the surface of a titanium or titanium alloy workpiece; step 2) micro-arc oxidation: immersing the pretreated workpiece into micro-arc oxidation electrolyte for micro-arc oxidation; step 3), heating and oxidizing: placing the workpiece subjected to micro-arc oxidation into a heating furnace in an atmospheric atmosphere for heating, and further oxidizing the surface of the workpiece; step 4) silanization treatment: putting the workpiece treated in the step 3) into a silane coupling agent aqueous solution, soaking, taking out and air-drying; step 5) curing treatment: and curing the air-dried workpiece. The surface treatment method for reducing the galvanic current of the titanium and the titanium alloy provided by the invention not only can achieve the aim of reducing the galvanic current of the titanium and the titanium alloy, but also can meet the corrosion resistance requirement when the titanium alloy workpiece is contacted with other metals in the marine environment.
Description
Technical Field
The invention relates to the technical field of titanium and titanium alloy surface treatment, in particular to a surface treatment method for reducing galvanic current of titanium and titanium alloy.
Background
Titanium and titanium alloy have high specific strength, excellent sea water corrosion resistance, no magnetism, high sound transmission coefficient, good formability and weldability and other characteristics, have excellent corrosion resistance in sea water, sea atmosphere and tidal environment, are called as 'marine metal', and are mainly applied to the fields of marine thermoelectric power generation, sea water desalination, oil and gas exploitation, ships, aquaculture and the like.
Although the titanium alloy has excellent corrosion resistance and does not generally need to be subjected to corrosion resistant surface treatment, in a seawater and ocean atmospheric corrosion environment, due to the fact that the titanium alloy is high in potential and is usually at a cathode, galvanic corrosion can occur when the titanium alloy is in contact with dissimilar metals for use, and the surface of the dissimilar metal with low potential can undergo anodic oxidation reaction, so that corrosion damage of the dissimilar metal is accelerated. The common method for preventing galvanic corrosion is to adopt a surface treatment method to prepare an insulating coating on the titanium surface, reduce galvanic current and achieve the purpose of reducing galvanic effect.
Micro-arc oxidation (MAO) is a process of growing a ceramic oxide film in situ on the surface of a material by applying high voltage (direct current, alternating current or pulse) in an electrolyte solution (generally a weak alkaline solution), and the process is a result of the synergistic effect of physical discharge, electrochemical oxidation and plasma oxidation. The micro-arc oxidation is to further increase the voltage on the basis of the common anodic oxidation technology to achieve the purpose of the attack of the oxide filmWhen voltage is applied, spark discharge occurs at the anode, and a ceramic oxide film is formed in situ on the surface of the material, so that the plasma oxide film has the high performance of the ceramic film and maintains the binding force between the anode oxide film and the matrix. TiO formed by micro-arc oxidation2The ceramic layer has good insulating property and can reduce the galvanic couple current of titanium and titanium alloy. However, based on the micro-arc oxidation mechanism, the generated oxide film layer has certain pores, if the pores are sealed, the insulation performance of the film layer can be further improved, and particularly in the marine environment, the galvanic corrosion problem of titanium alloy and dissimilar metal in seawater can be better solved. However, the sealing technology of the micro-arc oxidation film layer pores of the titanium alloy is always a difficult problem in the industry.
Patent CN 102703892B proposes a micro-arc oxidation coating silanization treatment fluid and a hole sealing method, the method provides a hole sealing method applying the micro-arc oxidation coating silanization treatment fluid, and researches the electrochemical impedance of the coating after the hole sealing treatment by the method. However, this method does not allow complete closure of the relatively large gaps.
Therefore, there is a need for a new surface treatment method for reducing galvanic current in titanium and titanium alloys.
Disclosure of Invention
The invention aims to provide a surface treatment method for reducing galvanic current of titanium and titanium alloy, which can not only achieve the aim of reducing galvanic current of titanium and titanium alloy, but also meet the requirement of corrosion resistance when a titanium alloy workpiece is contacted with other metals in a marine environment.
In order to achieve the above object, the present invention provides a surface treatment method for reducing galvanic current of titanium and titanium alloy, comprising the following steps:
step 1) pretreatment: cleaning the surface of a titanium or titanium alloy workpiece;
step 2) micro-arc oxidation: immersing the pretreated workpiece into micro-arc oxidation electrolyte for micro-arc oxidation;
step 3), heating and oxidizing: heating the workpiece after micro-arc oxidation to further oxidize the surface of the workpiece;
step 4) silanization treatment: immersing the workpiece treated in the step 3) into a silane coupling agent aqueous solution, taking out after immersion, and carrying out air drying treatment;
step 5) curing treatment: and curing the air-dried workpiece.
Further, in the step 1), the pretreatment specifically comprises: firstly, deoiling a workpiece in an acetone solution, and then ultrasonically cleaning the workpiece for 0.5-1 h by using ethanol.
Further, the micro-arc oxidation electrolyte in the step 2) comprises sodium silicate, sodium polyphosphate and sodium carbonate; the concentration of sodium silicate in the micro-arc oxidation electrolyte is 15-55g/L, the concentration of sodium polyphosphate is 5-25g/L, the concentration of sodium carbonate is 2-15/L, and the solvent is water.
Further, a sinusoidal constant current power supply is adopted in the step 2) to perform micro-arc oxidation treatment on the workpiece; the parameters during the micro-arc oxidation treatment are as follows: the current density is 3-30A/dm2The frequency is 600-1000Hz, the stop voltage is 300-600V, and the micro-arc oxidation treatment time is 5-30 min.
Further, the specific process of step 3) is as follows: putting the workpiece treated in the step 2) into a heating furnace, and carrying out heating oxidation in the atmosphere, wherein the heating temperature is 300-600 ℃, the heating time is 3-6h, and the heating mode is furnace temperature rise.
Further, the aqueous solution of the silane coupling agent in the step 4) is a hydrolysis solution prepared from a silane coupling agent, alcohols and water; the volume ratio of water, alcohol and the silane coupling agent in the silane coupling agent aqueous solution is 4-10: 1: 1.
further, the preparation method of the silane coupling agent aqueous solution comprises the following steps: after alcohol and water are uniformly mixed, adding a silane coupling agent into the alcohol-water mixture, and fully stirring to uniformly mix the solution; preferably, the silane coupling agent is an alkyl coupling agent, and the alcohol is ethanol.
Further, the specific process of step 4) is as follows: and (3) soaking the workpiece treated in the step 3) in a silane coupling agent aqueous solution for 1-3min, taking out, air-drying, soaking in the solution again, and repeating for multiple times.
Further, the specific process in the step 5) is as follows: and (3) heating the silanized workpiece at the temperature of 150-200 ℃, and curing the film layer after heating for 30-60 min.
Further, the step 2) also comprises post-treatment of the micro-arc oxidized workpiece; the method comprises the following steps: and cleaning the workpiece subjected to micro-arc oxidation treatment by using clean water, drying the workpiece by blowing, and drying the dried workpiece at the temperature of 50-150 ℃ for 10-20 min.
The invention has the following beneficial effects:
the invention provides a surface treatment method for reducing galvanic current of titanium and titanium alloy, which is mainly used for sequentially carrying out micro-arc oxidation, heating oxidation and silanization treatment on the surfaces of the titanium and the titanium alloy, so that a compact and uniform closed micro-arc oxidation film can be generated on the surfaces of the titanium and the titanium alloy. Firstly, a sinusoidal constant current power supply is adopted for micro-arc oxidation treatment; the parameters of the micro-arc oxidation are as follows: the current density is 3A/dm2-30A/dm2The frequency is 600Hz-1000Hz, the final voltage is maintained between 300V-600V, the titanium alloy after deoiling and cleaning is used as an anode, a stainless steel electrolytic tank is used as a cathode, a titanium alloy sample is fixed and placed in an electrolyte, the electrolyte is a sodium phosphate-sodium silicate system, the electrolysis parameters are set, the treatment time is 5min-30min, and a micro-arc oxidation ceramic layer with high hardness, good wear resistance and strong corrosion resistance can be generated on the surface. Then further heating and oxidizing at high temperature of the atmosphere, and heating for 3-6h along with the furnace in the atmosphere of 300-600 ℃; and finally, performing silanization treatment, specifically adding an alcohol solvent and water to prepare a water-soluble liquid on the basis of a silane coupling agent, and performing silanization treatment on the micro-arc oxidation film layer by dipping and curing the titanium and the titanium alloy subjected to micro-arc oxidation and heating oxidation, so that the treatment not only can achieve the purpose of reducing galvanic couple current of the titanium and the titanium alloy, but also can meet the corrosion resistance requirement when the titanium alloy workpiece is contacted with other metals in a marine environment.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below with reference to the drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows the surface topography of a sample treated by the method of comparative example 1 under a scanning electron microscope of 1000 times;
FIG. 2 is a surface topography under a scanning electron microscope of 1000 times for a sample treated by the method of comparative example 2;
FIG. 3 shows the surface topography of a sample treated by the method of example 1 under a scanning electron microscope of 1000 times.
Detailed Description
Embodiments of the invention will be described in detail below with reference to the drawings, but the invention can be implemented in many different ways, which are defined and covered by the claims.
Example 1:
the sample is TC4 in a rolled state, the specification is 225mm multiplied by 120mm multiplied by 3mm, and the specific operation steps are as follows:
1) pretreatment:
and cleaning the rolled TC4 blank by using an acetone solution, removing oil stains on the surface, and then ultrasonically cleaning for 1h by using ethanol.
2) Micro-arc oxidation:
and (3) immersing the pretreated TC4 sample into the micro-arc oxidation electrolyte, adjusting electrolysis parameters, and performing micro-arc oxidation. The micro-arc oxidation electrolyte comprises: the micro-arc oxidation electrolyte comprises sodium silicate, sodium polyphosphate and sodium carbonate, wherein the concentration of the sodium silicate in the micro-arc oxidation electrolyte is 40g/L, the concentration of the sodium polyphosphate is 12g/L, the concentration of the sodium carbonate is 9g/L, and a solvent is water. Carrying out micro-arc oxidation treatment by adopting a sinusoidal constant current power supply; the micro-arc oxidation electrical parameters are as follows: the current density is 3A/dm2-30A/dm2The frequency is 600Hz-1000Hz, the oxidation time is 6 minutes, the termination voltage is 400V, and the solution temperature is controlled to be 30 ℃ in the micro-arc oxidation process. The surface titanium alloy sample after the micro-arc oxidation treatment forms an oxide film layer with the thickness of 4.5 μm, light gray color, porous micro-morphology and smooth surface.
The method also comprises simple post-treatment after the micro-arc oxidation treatment, and specifically comprises the following steps: cleaning the sample subjected to micro-arc oxidation treatment with distilled water, washing away residual liquid medicine on the surface, and drying the surface with high-pressure air; and (3) drying the blow-dried workpiece in a drying furnace at the temperature of 100 ℃ for 15 min.
3) Heating and oxidizing:
and (3) placing the sample subjected to micro-arc oxidation treatment into a heating furnace, heating to 450 ℃ along with the furnace in an atmospheric atmosphere, preserving the temperature for 5 hours, and then discharging from the furnace for air cooling.
4) Silanization treatment:
and (3) putting the titanium alloy sample treated in the step 3) into a silane coupling agent aqueous solution, and soaking and air-drying for multiple times. Specifically, the method comprises the following steps: based on a silane coupling agent SCA-K02W (1, 2-bis (trimethoxysilyl) ethane), ethanol is used as a cosolvent to hydrolyze the silane coupling agent. The hydrolysis mode is as follows: adding 100ml of ethanol into 500ml of deionized water, stirring uniformly, adding 100ml of silane coupling agent, and stirring uniformly. And (3) uniformly mixing the solution by ultrasonic oscillation for 30min, and standing the solution at room temperature for 24h to prepare 700ml of hydrolysis solution with the silane coupling agent concentration of 14%.
Placing the titanium alloy sample subjected to micro-arc oxidation and heating oxidation into the silane coupling agent aqueous solution for dipping for 2min, taking out and air-drying; this was repeated three times.
5) Curing treatment:
and putting the air-dried sample into a stable oven at 150 ℃ for heating for 0.5h to cure the silane film.
Comparative example 1:
the sample is TC4 in a rolled state, the specification is 225mm multiplied by 120mm multiplied by 3mm, and the specific operation steps are as follows:
the TC4 sample is subjected to pretreatment, micro-arc oxidation and simple post-treatment after micro-arc oxidation treatment, heating oxidation treatment, silanization treatment and curing treatment are omitted, and other process parameters are the same as those in example 1.
Comparative example 2:
the sample is TC4 in a rolled state, the specification is 225mm multiplied by 120mm multiplied by 3mm, and the specific operation steps are as follows:
only the TC4 sample is subjected to pretreatment, micro-arc oxidation and simple post-treatment after micro-arc oxidation treatment, and then the silylation treatment and the curing treatment are directly carried out without heating oxidation treatment, and other process parameters are the same as those in example 1.
The samples treated by the methods of comparative example 1, comparative example 2 and example 1 are photographed under a scanning electron microscope of 1000 times, and the detailed surface topography is shown in fig. 1-3. As can be seen from the figure, the shape of the micro-arc oxidation film layer obtained by only carrying out pretreatment, micro-arc oxidation and simple post-treatment after the micro-arc oxidation is shown in figure 1, and the surface has more micropores with different sizes. The shape of the obtained micro-arc oxidation film layer is shown in figure 2, the surface of the micro-arc oxidation film layer is relatively flat after silanization treatment, and most micropores are sealed. The shape of the micro-arc oxidation film obtained after the micro-arc oxidation, the heating oxidation and the silanization treatment by the method is shown in figure 3, the film gap is completely sealed, and a layer of compact and uniform closed micro-arc oxidation film is generated on the surface of titanium and titanium alloy.
In summary, the surface treatment method for reducing galvanic current of titanium and titanium alloy provided by the invention mainly comprises the steps of sequentially carrying out micro-arc oxidation, heating oxidation and silanization on the surfaces of titanium and titanium alloy, so that a compact and uniform closed micro-arc oxidation film can be generated on the surfaces of titanium and titanium alloy. Firstly, a sinusoidal constant current power supply is adopted for micro-arc oxidation treatment; the parameters of the micro-arc oxidation are as follows: the current density is 3A/dm2-30A/dm2The frequency is 600Hz-1000Hz, the termination voltage is maintained between 300V and 600V, the titanium alloy after oil removal and cleaning is used as an anode, a stainless steel electrolytic cell is used as a cathode, a titanium alloy sample is fixed and placed in an electrolyte, the electrolyte is a sodium phosphate-sodium silicate system, the electrolysis parameters are set, the treatment time is 5min-30min, and a micro-arc oxidation ceramic layer with high hardness, good wear resistance and strong corrosion resistance can be generated on the surface. Then is atFurther heating and oxidizing at high atmospheric temperature, and heating for 3-6h in 300-600 ℃ atmospheric atmosphere along with the furnace; and finally, performing silanization treatment, specifically adding an alcohol solvent and water to prepare a water-soluble liquid on the basis of a silane coupling agent, and performing silanization treatment on the micro-arc oxidation film layer by dipping and curing the titanium and the titanium alloy subjected to micro-arc oxidation and heating oxidation, so that the treatment not only can achieve the purpose of reducing galvanic couple current of the titanium and the titanium alloy, but also can meet the corrosion resistance requirement when the titanium alloy workpiece is contacted with other metals in a marine environment.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A surface treatment method for reducing galvanic current of titanium and titanium alloy is characterized by comprising the following steps:
step 1) pretreatment: cleaning the surface of a titanium or titanium alloy workpiece;
step 2) micro-arc oxidation: immersing the pretreated workpiece into micro-arc oxidation electrolyte for micro-arc oxidation;
step 3), heating and oxidizing: heating the workpiece after micro-arc oxidation to further oxidize the surface of the workpiece;
step 4) silanization treatment: immersing the workpiece treated in the step 3) into a silane coupling agent aqueous solution, taking out after immersion, and carrying out air drying treatment;
step 5) curing treatment: and curing the air-dried workpiece.
2. The surface treatment method for reducing galvanic current of titanium and titanium alloys according to claim 1, wherein the pretreatment in step 1) comprises the following steps: firstly, deoiling a workpiece in an acetone solution, and then ultrasonically cleaning the workpiece for 0.5-1 h by using ethanol.
3. The surface treatment method for reducing galvanic current of titanium and titanium alloys according to claim 1, wherein said micro-arc oxidation electrolyte of step 2) comprises sodium silicate, sodium polyphosphate and sodium carbonate; the concentration of sodium silicate in the micro-arc oxidation electrolyte is 15-55g/L, the concentration of sodium polyphosphate is 5-25g/L, the concentration of sodium carbonate is 2-15g/L, and the solvent is water.
4. The surface treatment method for reducing galvanic current of titanium and titanium alloys according to claim 1, wherein the micro-arc oxidation treatment is performed on the workpiece by using a sinusoidal constant current power supply in step 2); the parameters during the micro-arc oxidation treatment are as follows: the current density is 3-30A/dm2The frequency is 600-1000Hz, the stop voltage is 300-600V, and the micro-arc oxidation treatment time is 5-30 min.
5. The surface treatment method for reducing galvanic current of titanium and titanium alloys according to claim 1, wherein the specific process of step 3) is as follows: putting the workpiece treated in the step 2) into a heating furnace, and carrying out heating oxidation in the atmosphere, wherein the heating temperature is 300-600 ℃, the heating time is 3-6h, and the heating mode is furnace temperature rise.
6. The surface treatment method for reducing galvanic current of titanium and titanium alloys according to claim 1, wherein the aqueous solution of silane coupling agent in step 4) is a hydrolyzed solution prepared from silane coupling agent, alcohol and water; the volume ratio of water, alcohol and the silane coupling agent in the silane coupling agent aqueous solution is 4-10: 1: 1.
7. the surface treatment method for reducing galvanic current of titanium and titanium alloys according to claim 6, wherein the silane coupling agent aqueous solution is prepared by: after alcohol and water are uniformly mixed, adding a silane coupling agent into the alcohol-water mixture, and fully stirring to uniformly mix the solution; preferably, the silane coupling agent is an alkyl coupling agent, and the alcohol is ethanol.
8. The surface treatment method for reducing galvanic current of titanium and titanium alloys according to claim 1, wherein the specific process of step 4) is as follows: and (3) soaking the workpiece treated in the step 3) in a silane coupling agent aqueous solution for 1-3min, taking out, air-drying, soaking in the solution again, and repeating for multiple times.
9. The surface treatment method for reducing galvanic current of titanium and titanium alloys according to claim 1, wherein the specific process in step 5) is as follows: and (3) heating the silanized workpiece at the temperature of 150-200 ℃, and curing the film layer after heating for 30-60 min.
10. The surface treatment method for reducing galvanic current of titanium and titanium alloys according to any one of claims 1 to 9, wherein the step 2) further comprises post-treatment of the micro-arc oxidized workpiece; the method comprises the following steps: and cleaning the workpiece subjected to micro-arc oxidation treatment by using clean water, drying the workpiece by blowing, and drying the dried workpiece at the temperature of 50-150 ℃ for 10-20 min.
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