CN112391625B - Method for preparing titanium alloy high-temperature oxidation-resistant coating through laser alloying composite micro-arc oxidation - Google Patents
Method for preparing titanium alloy high-temperature oxidation-resistant coating through laser alloying composite micro-arc oxidation Download PDFInfo
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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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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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Abstract
The invention discloses a method for preparing a titanium alloy high-temperature oxidation-resistant coating by laser alloying composite micro-arc oxidation, which mainly utilizes laser alloying and micro-arc oxidation to treat the surface of the titanium alloy so as to solve the problem that the surface of the titanium alloy in high-temperature service is easy to oxidize to cause the overall performance reduction of a workpiece; the main creativity of the invention is as follows: the method breaks through the limitation of the traditional immersion micro-arc oxidation on the size of the workpiece, and can be used for the integral/local treatment of large-size titanium alloy workpieces; the thickness of a coating required to be prepared by laser alloying is reduced by introducing a micro-arc oxidation technology, the damage of laser treatment to a substrate is reduced, the service performance of the treated material is improved, and the service life of the treated material is prolonged; meanwhile, the quality and the density of the micro-arc oxidation film can be improved by regulating and controlling the components of the alloying layer, and the problem that the performance of the micro-arc oxidation coating is limited due to the porous property is solved.
Description
Technical Field
The invention discloses a method for preparing a titanium alloy high-temperature oxidation-resistant coating by laser alloying composite micro-arc oxidation, relates to laser alloying and micro-arc oxidation technologies, and is used for improving the high-temperature oxidation resistance of the surface of a titanium alloy.
Background
Titanium and titanium alloy are light metal structural materials with small density and high strength, and are widely applied to the fields of aerospace, chemical engineering, ships and the like. For example, parts such as a pressure air disk, a blade, a casing and the like of the aircraft engine made of titanium alloy can improve the thrust-weight ratio of the aircraft engine and the maneuvering performance of the aircraft. As the use ratio of titanium alloys in high performance aircraft increases, naturally higher requirements are placed on the service temperatures. However, under high-temperature service, the surface of the titanium alloy is very easy to oxidize and oxygen embrittlement, particularly, the high-temperature oxidation resistance of the alloy is in a sharp decline trend at the temperature of over 600 ℃, and the development of the titanium alloy to higher temperature is seriously limited. Therefore, the high-temperature oxidation resistance of the titanium alloy outer layer can be enhanced by adopting a proper surface treatment technology from the surface of the material, so that the surface of the titanium alloy outer layer can bear a harsher environment without influencing the internal performance of the titanium alloy outer layer, and the application field of the titanium alloy is further expanded.
The laser surface alloying is a method for local modification treatment of metal material surface, and the added alloy element and base material surface are melted and mixed under the action of high-energy density laser beam, and a surface alloying coating layer whose thickness is about 0.01-2mm can be formed in a short time so as to improve the property of metal material. The method can effectively improve the high-temperature oxidation resistance of the titanium alloy by adding a certain anti-oxidation compound element, and the depth and the width of the modified layer are controllable.
The micro-arc oxidation technology is a surface treatment method developed from an anodic oxidation process. The method is a new technology for protecting a substrate by raising interelectrode voltage from a common anodic oxidation Faraday area to a high-voltage discharge area to generate micro-arc plasma spark discharge and growing a ceramic film layer on the surface of valve metal in situ by utilizing the instantaneous sintering action of electric arc. Due to the in-situ growth characteristic, the ceramic coating prepared on the surface of the titanium alloy by the method does not influence the original performance characteristic of the titanium alloy, and can improve the high-temperature oxidation resistance of the titanium alloy.
Although the two technologies improve the high-temperature oxidation resistance of the titanium alloy to a certain extent, the single treatment obviously cannot meet higher requirements. Therefore, the invention provides a method for preparing a titanium alloy high-temperature oxidation-resistant coating by micro-arc oxidation in a laser alloying composite selected area based on the two technologies.
Disclosure of Invention
The invention aims to provide a method for preparing a titanium alloy high-temperature oxidation-resistant coating by laser alloying composite micro-arc oxidation. Firstly, an alloying layer with good high-temperature oxidation resistance is prepared on the surface of a titanium alloy by using a laser alloying technology, and then a ceramic film layer containing a high-temperature oxidation resistant phase is prepared on the surface of the alloying layer by using a micro-arc oxidation technology, so that the high-temperature oxidation resistance of the alloying layer is further improved (as shown in figure 1).
The technical scheme of the invention is as follows:
a method for preparing a titanium alloy high-temperature oxidation-resistant coating by laser alloying composite micro-arc oxidation comprises the following steps:
(1) Polishing, cleaning and air-drying the surface of the titanium alloy to be treated for later use;
the titanium alloy is, for example: a TC4 alloy;
preferably, the surface of the titanium alloy is polished to Ra 1.6 μm;
(2) Presetting alloy paint on the surface of the titanium alloy prepared in the step (1), and carrying out laser alloying treatment after the titanium alloy is completely air-dried and a laser processing technology is set;
the alloy coating consists of alloy components, a solvent and a binder; wherein the alloy comprises the following components: 50-80wt.%, si:15-25wt.%, nb:5-25wt.%; the solvent is absolute ethyl alcohol; the adhesive is lac; and the mass ratio of the alloy components, the solvent and the binder is 5:12:1;
the thickness of the preset alloy coating layer is 0.2-0.8mm;
the conditions of the laser processing technology are as follows: the diameter of a laser spot is 0.24mm, the control mode of laser motion is galvanometer scanning, the laser power is 500-1000W, the scanning speed is 200-1000mm/s, and the scanning interval is 0.04-0.08mm;
(3) Polishing, degreasing and cleaning the titanium alloy surface subjected to the laser alloying treatment in the step (2) for later use;
further, it is preferable that the roughness of the surface after the polishing treatment is Ra 0.8-1.6 μm;
(4) Preparing electrolyte, and performing micro-arc oxidation on the titanium alloy prepared in the step (3) to prepare a surface high-temperature oxidation-resistant coating;
the electrolyte comprises the following components: naAlO 2 4-15g/L、Na 2 SiO 3 4-8g/L、ZrO 2 2-5g/L, and the solvent is deionized water;
in the micro-arc oxidation process, the stainless steel pipe is used as a cathode, the titanium alloy is used as an anode, the electrolyte is directly sprayed to the surface of the anode through the stainless steel pipe, and the distance between the stainless steel pipe and the titanium alloy is the electrode spacing;
the electrical technological parameters of the micro-arc oxidation are as follows: constant current mode, pulse power supply current density 3-9A/dm 2 The pulse frequency is 500-1000Hz, and the duty ratio is 10-30%; the electrode spacing is 10-15mm; the flow rate of the electrolyte is 0.5-1.5mm/s; the moving speed of the cathode is 3-5mm/min; the overlapping rate of the film layer is 20-40%.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention combines two surface modification technologies of laser alloying and micro-arc oxidation, can overcome the defects of the two technologies in performance during single treatment, greatly improves the high-temperature oxidation resistance of the surface of the titanium alloy, and realizes the effect of 1+1 > 2. Meanwhile, the method breaks through the limitation of the traditional immersion micro-arc oxidation on the size of the workpiece, and can be used for the integral/local treatment of large-size titanium alloy workpieces.
(2) Compared with single laser alloying treatment, the method can reduce the thickness of the coating required to be prepared by laser alloying by introducing the micro-arc oxidation technology, which is beneficial to improving the quality of the alloying layer, reducing the damage of the laser treatment to the substrate, improving the service performance and prolonging the service life of the treated material.
(3) Compared with single micro-arc oxidation treatment, the micro-arc oxidation coating can improve the quality and the density of the micro-arc oxidation coating through the regulation and control of the components of the alloying layer, and solve the problem that the performance improvement of the micro-arc oxidation coating is limited due to the porous property.
Drawings
FIG. 1 is a schematic diagram of a method for preparing a titanium alloy high-temperature oxidation-resistant coating by laser alloying composite selected area micro-arc oxidation;
1-laser, 2-alloy powder, 3-titanium alloy, 4-stainless steel cathode tube, 5-electrolyte and 6-laser alloying coating.
FIG. 2 is a comparison of the surface oxidation weight increase of a substrate, micro-arc oxidation, laser alloying and laser alloying/micro-arc oxidation sample after 100h of high-temperature oxidation at 900 ℃.
Detailed Description
The present invention is further illustrated by the following specific examples, but the scope of the invention is not limited thereto.
In the following examples, the titanium alloy material used was a TC4 alloy, and the sample size was 50X 20X 5mm;
the diameter of a laser spot is 0.24mm, and the control mode of laser motion is galvanometer scanning;
the diameter of the stainless steel pipe adopted by the micro-arc oxidation is 8mm, and the pipe diameter is 5mm.
Example 1
1) The titanium alloy is pretreated by polishing, cleaning and drying.
2) The alloy coating is pre-arranged on the surface of a material, the thickness of a control layer is 0.5mm, and the alloy components in the alloy coating are as follows: al:80wt.%, si:15wt.%, nb:5wt.%, after it has completely air dried, the next step can be carried out.
3) Setting a laser alloying processing technology: carrying out laser alloying treatment on the sample with the laser power of 1000W, the scanning speed of 1000mm/s and the scanning distance of 0.04 mm;
4) Polishing the surface of the sample subjected to laser alloying treatment to Ra 0.8 mu m;
5) Preparing an electrolyte: naAlO 2 15g/L、Na 2 SiO 3 4g/L、ZrO 2 2g/L；
6) Set micro-arc oxidation chemicalTechnological pulse power supply current density 9A/dm 2 Carrying out micro-arc oxidation treatment with the pulse frequency of 500Hz, the duty ratio of 30%, the electrode spacing of 10mm, the electrolyte flow rate of 0.5mm/s, the cathode moving speed of 3mm/min and the film layer overlapping rate of 40%;
the prepared coating surface is detected, and the coating surface has good quality and no defect.
After the high-temperature oxidation at 900 ℃ for 100 hours, the oxidation weight gain of the matrix is 27.92mg/cm 2 The oxidation weight gain of the sample subjected to single laser alloying treatment is 10.31mg/cm 2 The oxidation weight gain of a single micro-arc oxidation treatment sample is 23.25mg/cm 2 The oxidation weight gain of the laser alloying composite micro-arc oxidation treatment sample is 5.32mg/cm 2 The oxidation weight of the matrix is 0.19, and the high-temperature oxidation resistance is obviously improved.
Example 2
The alloy coating comprises the following alloy components: al:50wt.%, si:25wt.%, nb:25wt.%, controlling the layer thickness at 0.5mm.
Setting a laser alloying processing technology: the laser power is 1000W, the scanning speed is 1000mm/s, and the scanning distance is 0.04mm.
The surface of the sample after the laser alloying treatment is polished to Ra 0.8 mu m
Preparing an electrolyte: naAlO 2 4g/L、Na 2 SiO 3 8g/L、ZrO 2 5g/L。
Setting the current density of the micro-arc oxidation process pulse power supply to be 9A/dm 2 The pulse frequency is 500Hz, the duty ratio is 30 percent, the electrode spacing is 10mm, the electrolyte flow rate is 0.5mm/s, the cathode moving speed is 3mm/min, and the film layer overlapping rate is 40 percent.
The other process steps were as in example 1.
The prepared coating surface is detected, and the coating surface has good quality and no defect.
After the high-temperature oxidation at 900 ℃ for 100 hours, the oxidation weight gain of the matrix is 27.92mg/cm 2 The oxidation weight gain of the sample subjected to single laser alloying treatment is 12.45mg/cm 2 The oxidation weight gain of a single micro-arc oxidation treatment sample is 25.67mg/cm 2 The oxidation weight of the laser alloying composite micro-arc oxidation treatment sample is3.68mg/cm 2 The oxidation weight of the matrix is 0.13, and the high-temperature oxidation resistance is obviously improved.
Example 3
The alloy coating comprises the following alloy components: al:80wt.%, si:15wt.%, nb:5wt.%, controlling the layer thickness at 0.2.
Setting a laser alloying processing technology: the laser power is 500W, the scanning speed is 200mm/s, and the scanning interval is 0.08mm.
The surface of the sample after the laser alloying treatment is polished to Ra 1.6 mu m
Preparing an electrolyte: naAlO 2 15g/L、Na 2 SiO 3 4g/L、ZrO 2 2g/L。
Setting the current density of a pulse power supply of 3A/dm in the micro-arc oxidation process 2 The pulse frequency is 1000Hz, the duty ratio is 10 percent, the electrode distance is 15mm, the flow rate of the electrolyte is 1.5mm/s, the moving speed of the cathode is 5mm/min, and the overlapping rate of the film layer is 20 percent.
The other process steps were as in example 1.
The prepared coating surface is detected, and the coating surface has good quality and no defect.
After the high-temperature oxidation at 900 ℃ for 100 hours, the oxidation weight gain of the matrix is 27.92mg/cm 2 The oxidation weight gain of the sample subjected to single laser alloying treatment is 14.32mg/cm 2 The oxidation weight gain of the single micro-arc oxidation treatment sample is 21.79mg/cm 2 The oxidation weight gain of the laser alloying composite micro-arc oxidation treatment sample is 7.89mg/cm 2 The oxidation weight of the matrix is 0.28, and the high-temperature oxidation resistance is obviously improved.
Example 4
The alloy coating comprises the following alloy components: al:65wt.%, si:20wt.%, nb:15wt.%, control layer thickness at 0.3mm.
Setting a laser alloying processing technology: laser power 750W, scanning speed 600mm/s, scanning interval 0.06mm.
The surface of the sample after the laser alloying treatment is polished to Ra 0.8 mu m
Preparing an electrolyte: naAlO 2 10g/L、Na 2 SiO 3 6g/L、ZrO 2 3g/L。
Setting the current density of a pulse power supply of 6A/dm in the micro-arc oxidation process 2 The pulse frequency is 750Hz, the duty ratio is 25%, the electrode distance is 10mm, the flow rate of the electrolyte is 1mm/s, the moving speed of the cathode is 4mm/min, and the overlapping rate of the film layer is 30%.
The other process steps were as in example 1.
The prepared coating surface is detected, and the coating surface has good quality and no defect.
After the high-temperature oxidation at 900 ℃ for 100 hours, the oxidation weight gain of the matrix is 27.92mg/cm 2 The oxidation weight gain of the sample subjected to single laser alloying treatment is 11.78mg/cm 2 The oxidation weight gain of the single micro-arc oxidation treatment sample is 24.31mg/cm 2 The oxidation weight gain of the laser alloying composite micro-arc oxidation treatment sample is 1.85mg/cm 2 。
The composite coating prepared by the invention has good high-temperature oxidation resistance, and shows better performance improvement than single laser alloying or micro-arc oxidation treatment, and the oxidation weight gain of the surface of the treated material is 0.06 of the oxidation weight gain of the matrix, as shown in figure 2.
The foregoing description has described specific embodiments of the present invention. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (3)
1. A method for preparing a titanium alloy high-temperature oxidation-resistant coating by laser alloying composite micro-arc oxidation is characterized by comprising the following steps:
(1) Polishing, cleaning and air-drying the surface of the titanium alloy to be treated for later use;
(2) Presetting an alloy coating on the surface of the titanium alloy prepared in the step (1), and performing laser alloying treatment after the titanium alloy is completely air-dried and a laser processing process is set;
the alloy coating consists of alloy components, a solvent and a binder; wherein the alloy comprises the following components: 50-80wt.%, si:15-25wt.%, nb:5-25wt.%; the solvent is absolute ethyl alcohol; the adhesive is lac; and the mass ratio of the alloy components, the solvent and the binder is 5:12:1; the thickness of the preset alloy coating layer is 0.2-0.8mm;
the conditions of the laser processing technology are as follows: the diameter of a laser spot is 0.24mm, the control mode of laser motion is galvanometer scanning, the laser power is 500-1000W, the scanning speed is 200-1000mm/s, and the scanning interval is 0.04-0.08mm;
(3) Polishing, degreasing and cleaning the titanium alloy surface subjected to the laser alloying treatment in the step (2) for later use; the roughness of the surface after polishing treatment is Ra 0.8-1.6 μm;
(4) Preparing electrolyte, and performing micro-arc oxidation on the titanium alloy prepared in the step (3) to prepare a surface high-temperature oxidation-resistant coating;
the electrolyte comprises the following components: naAlO 2 4-15 g/L、Na 2 SiO 3 4-8 g/L、ZrO 2 2-5g/L, and the solvent is deionized water;
in the micro-arc oxidation process, the stainless steel pipe is used as a cathode, the titanium alloy is used as an anode, the electrolyte is directly sprayed to the surface of the anode through the stainless steel pipe, and the distance between the stainless steel pipe and the titanium alloy is the electrode spacing;
the electrical technological parameters of the micro-arc oxidation are as follows: constant current mode, pulse power supply current density 3-9A/dm 2 The pulse frequency is 500-1000Hz, and the duty ratio is 10-30%; the electrode spacing is 10-15mm; the flow rate of the electrolyte is 0.5-1.5mm/s; the moving speed of the cathode is 3-5mm/min; the overlapping rate of the film layer is 20-40%.
2. The method for preparing the titanium alloy high-temperature oxidation resistant coating through laser alloying composite micro-arc oxidation as claimed in claim 1, wherein in the step (1), the titanium alloy is TC4 alloy.
3. The method for preparing the titanium alloy high-temperature oxidation-resistant coating by laser alloying composite micro-arc oxidation as claimed in claim 1, wherein in the step (1), the surface of the titanium alloy is polished to Ra 1.6 μm.
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| CN105714244A (en) * | 2016-03-30 | 2016-06-29 | 青岛滨海学院 | Titanium alloy surface ceramic/metal gradient high-temperature composite coating and preparing method thereof |
| CN107653475A (en) * | 2017-09-12 | 2018-02-02 | 西安庄信新材料科技有限公司 | A kind of method that titanium alloy surface prepares high temperature composite coating using microarc oxidation solution |
| CN107675170A (en) * | 2017-10-24 | 2018-02-09 | 常州大学 | A kind of preparation method of offshore platform steel surface laser cladding differential arc oxidation coating |
| CN110904485A (en) * | 2019-12-25 | 2020-03-24 | 浙江工业大学 | Scanning type laser-assisted micro-arc oxidation device and method |
| CN111020571A (en) * | 2020-01-15 | 2020-04-17 | 中北大学 | Alloy powder for laser cladding of stainless steel surface and application thereof |
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| DE102004033342A1 (en) * | 2004-07-09 | 2006-02-02 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Process for producing wear-resistant and fatigue-resistant edge layers in titanium alloys and components produced therewith |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105714244A (en) * | 2016-03-30 | 2016-06-29 | 青岛滨海学院 | Titanium alloy surface ceramic/metal gradient high-temperature composite coating and preparing method thereof |
| CN107653475A (en) * | 2017-09-12 | 2018-02-02 | 西安庄信新材料科技有限公司 | A kind of method that titanium alloy surface prepares high temperature composite coating using microarc oxidation solution |
| CN107675170A (en) * | 2017-10-24 | 2018-02-09 | 常州大学 | A kind of preparation method of offshore platform steel surface laser cladding differential arc oxidation coating |
| CN110904485A (en) * | 2019-12-25 | 2020-03-24 | 浙江工业大学 | Scanning type laser-assisted micro-arc oxidation device and method |
| CN111020571A (en) * | 2020-01-15 | 2020-04-17 | 中北大学 | Alloy powder for laser cladding of stainless steel surface and application thereof |
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