CN113832514A - Method for improving surface hardness and wear resistance of titanium-containing material - Google Patents
Method for improving surface hardness and wear resistance of titanium-containing material Download PDFInfo
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- CN113832514A CN113832514A CN202111145982.XA CN202111145982A CN113832514A CN 113832514 A CN113832514 A CN 113832514A CN 202111145982 A CN202111145982 A CN 202111145982A CN 113832514 A CN113832514 A CN 113832514A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/627—Electroplating characterised by the visual appearance of the layers, e.g. colour, brightness or mat appearance
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- C—CHEMISTRY; METALLURGY
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
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Abstract
The invention discloses a method for improving the surface hardness and the wear resistance of a titanium-containing material, which is characterized by comprising the following steps of: 1) cutting and forming a workpiece containing a titanium material; 2) immersing the formed workpiece into electrolyte, and connecting an anode with the workpiece and a cathode with an inert conductor electrode by using a pulse power supply to form a loop; the inert conductor electrode is stainless steel; 3) applying pulse current with the current density of 10-20A/dm 2, the pulse frequency of 50-200 Hz, the duty ratio of 30%, the temperature of the electrolyte of 35 +/-2 ℃ and the application time of 5-90 minutes to form a coating on the surface of the workpiece; 4) the coating is polished by using a carborundum abrasive disc, and 40-80% of the formed coating is reserved so as to obtain a high-hardness and high-wear-resistance coating. The invention does not need complex pretreatment process, the electrolyte proportion is simpler and more environment-friendly, and B, F and other element components which have higher environmental pollution are not introduced; the conception, the specific structure and the generated technical effect of the invention are further explained by combining the attached drawings so as to fully understand the purposes, the characteristics and the effects of the invention.
Description
Technical Field
The invention relates to the field of medical implant material manufacturing, in particular to a method for improving the surface hardness and the wear resistance of a titanium-containing material.
Background
Titanium and titanium alloy have high specific strength, excellent corrosion resistance, good high-temperature performance and the like, and are widely applied in the fields of aerospace, petroleum, chemical engineering, light industry, metallurgy, automobiles, construction, medicine and the like. However, titanium alloys have lower hardness and inferior wear resistance compared to aluminum-magnesium alloys and steel materials. The hardness of the pure titanium is about 150-200 Hv, and the titanium alloy does not exceed 350Hv generally. Such hardness values do not meet the requirements of practical production applications in many cases.
Increasing attention has been paid to improving the hardness and wear resistance of titanium alloys by surface modification. The method for improving the surface modification of the titanium alloy mainly comprises the following steps: laser cladding surface treatment, surface deposition coating methods (classified into CVD methods and PVD methods), anodic oxidation methods, and micro-arc oxidation methods which have appeared in recent years, and the like. The laser cladding surface treatment has high treatment speed and wide application range, but has rough surface, poor smoothness, low adhesive force and expensive equipment. The CVD method of surface deposition coating can improve the surface property of titanium alloy, but the coating and the body are easy to generate brittle fracture. The PVD method has the advantages of slow film forming speed, low preparation efficiency and high cost. The anodic oxidation method has simpler process, but the formed film has thin thickness and limited hardness improvement. In the micro-arc oxidation technology which appears in recent years, a ceramic film layer grows on the surface of a material under the action of instantaneous high temperature and high pressure generated by arc discharge. The micro-arc oxidation film layer is firmly combined with the body, the structure is compact, the toughness is high, and the film layer generally shows good wear resistance, corrosion resistance and other characteristics.
Application number CN 102199785B discloses a micro-arc oxidation solution of a titanium alloy wear-resistant coating and application thereof. It is characterized in that: KOH, Na2SiO3, NaF, triethanolamine and Na2B4O7 solute are used, and the solvent is deionized water. The concentration of each solute is preferably 3g/L of KOH, 5g/L of Na2SiO3, 3g/L of NaF, triethanolamine: 3g/L, Na2B4O 7: lg/L. The micro-arc oxidation process controls the current density to be 3-5A/dm2, the temperature of the electrolyte is less than 60 ℃, the time is 5-30min, and the thickness of the wear-resistant coating formed on the surface of the titanium alloy after 5-30min is 10-40 um. Elements such as silicon, boron and the like for improving the hardness are introduced into the wear-resistant coating formed by the micro-arc oxidation treatment of the titanium alloy, and the hardness of the coating after the micro-arc oxidation reaches more than HV 700.
Disclosure of Invention
In view of the above-mentioned defects of the prior art, the technical problem to be solved by the present invention is to greatly improve the surface hardness and wear resistance of the titanium-containing material by using an environmentally friendly electrolyte solution.
In order to achieve the above object, the present invention provides a method for improving the surface hardness and wear resistance of a titanium-containing material, which is characterized by comprising the following steps:
1) cutting and forming a workpiece containing a titanium material;
2) immersing the formed workpiece into electrolyte, and connecting an anode with the workpiece and a cathode with an inert conductor electrode by using a pulse power supply to form a loop; the inert conductor electrode is stainless steel;
3) applying pulse current with the current density of 10-20A/dm 2, the pulse frequency of 50-200 Hz, the duty ratio of 30%, the temperature of the electrolyte of 35 +/-2 ℃ and the application time of 5-90 minutes to form a coating on the surface of the workpiece;
4) the coating is polished by using a carborundum abrasive disc, and 40-80% of the formed coating is reserved so as to obtain a high-hardness and high-wear-resistance coating.
Further, the electrolyte includes: 10-30 g/L of sodium phosphate; 1-10 g/L of KOH and 5-30 g/L of sodium aluminate.
Further, during the reaction of step 3): stage one, white light is discharged within 2 minutes; and in the second stage, white light discharge and orange red discharge coexist, and the time is 2 minutes after the reaction starts, and can last for 5-10 minutes.
Further, the reaction process in the step 3) also comprises a third stage, wherein the orange discharge is continuously generated after the second stage, and the duration is more than 30 minutes;
further, the reaction process in the step 3) also comprises a stage four, the arc discharge is eliminated after the stage three, and the reaction can be continued for 10-30 minutes.
Further, the step 2) further comprises the step of fixing the formed workpiece on a fixer, wherein the fixer is made of a titanium wire with the diameter of 2 mm.
Further, the surface of the part of the holder at the electrolyte-air interface and in the electrolyte is covered with an insulating substance.
Furthermore, the pulse frequency is 100-200 Hz, and the application time is 60-90 minutes.
Further, the pulse frequency was 200Hz, and the application time was 90 minutes.
Further, the step 3) comprises that during the reaction, the electrolyte is stirred by using an air compressor.
The invention is mainly different from the prior art in that: complex pretreatment process is not needed, the electrolyte is simpler and more environment-friendly in proportioning, and B, F and other element components which have higher environmental pollution are not introduced; the conception, the specific structure and the generated technical effect of the invention are further explained by combining the attached drawings so as to fully understand the purposes, the characteristics and the effects of the invention.
Drawings
FIG. 1 is a surface micro-topography of a titanium alloy oxide film prepared in a preferred embodiment 1 of the present invention.
Detailed Description
The technical contents of the preferred embodiments of the present invention will be more clearly and easily understood by referring to the drawings attached to the specification. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
In the drawings, structurally identical elements are represented by like reference numerals, and structurally or functionally similar elements are represented by like reference numerals throughout the several views. The size and thickness of each component shown in the drawings are arbitrarily illustrated, and the present invention is not limited to the size and thickness of each component. The thickness of the components may be exaggerated where appropriate in the figures to improve clarity.
The electrolyte includes: 10-30 g/L of sodium phosphate; KOH 1-10 g/L, sodium aluminate 5-30 g/L
The titanium-containing material comprises: pure titanium (TA2, TA3, TA4, etc.), Ti6Al4V alloy (TC2, TC3, TC4, etc.)
The process comprises the following steps:
1) cutting and molding the titanium alloy;
2) immersing the formed workpiece into electrolyte, and connecting an anode with the workpiece and a cathode with an inert conductor electrode by using a pulse power supply to form a loop; the inert conductor electrode is stainless steel;
3) applying pulse current with current density of 10-20A/dm 2, pulse frequency of 50-200 Hz, duty ratio of 30%, electrolyte temperature of 35 +/-2 deg and application time of 5-90 min. The reaction process sequentially comprises the following steps: stage one: white light is discharged within 2 minutes; and a second stage: white light discharge and orange red discharge coexist, the time is 2 minutes after the reaction starts, and the time can last for 5-10 minutes; and a third stage: orange discharge, which continues to occur after stage two and can last for more than 30 minutes; and a fourth stage: after the third stage, the arc discharge disappears, but the reaction can be continued for 10-30 minutes.
4) The coating is polished by using a carborundum abrasive disc, and 40-80% of the formed coating is reserved so as to obtain a high-hardness and high-wear-resistance coating.
The effect is as follows:
the coating with the thickness of 90-110 mu m can be obtained by using the process, the coating with the thickness of more than 50 mu m can be obtained after polishing, the Vickers hardness of the coating can reach 750-1100 Hv, and the coating is greatly superior to the prior art level. Microscopic analysis of the cross section shows that the three layers-the outer layer is light yellow, there are dark blue purple particles, the inner layer is yellow white, and the surface layer at the coating-metal interface is brown yellow.
In the case of the example 1, the following examples are given,
the process comprises the following steps:
1) cutting and molding a titanium alloy Ti6Al4V alloy TC2 to obtain a sample which is a round cake with the diameter of 2.5cm and the thickness of 0.5 cm;
2) pretreatment: the surface of the sample is simply polished by using sand paper, and burrs are removed; no other pretreatment is needed;
3) preparing an electrolyte:
preparing an electrolyte, wherein the electrolyte comprises the following components: 10g/L of sodium phosphate; KOH2g/L, sodium aluminate 5 g/L; mixing uniformly until all the components are dissolved;
4) reaction:
immersing a workpiece into electrolyte, and using a pulse power supply, wherein the anode is connected with the workpiece, and the cathode is connected with an inert conductor electrode to form a loop; the inert conductor electrode is stainless steel; the workpiece holder was made of 2mm diameter titanium wire and the part of the holder in the electrolyte and at the electrolyte-air interface was insulated by a tape made of fluoroplastic film. The adhesive tape is used for eliminating current loss caused by the oxidation of the bracket and avoiding micro-discharge at the interface of electrolyte and air. The holder is in threaded contact with the sample. In the reaction process, the electrolyte is fully stirred by using an air compressor.
Applying pulse current with current density of 10A/dm2, pulse frequency of 50Hz, duty ratio of 30% and electrolyte temperature of 35 + -2 deg.C. The application time was 60 minutes. Measuring the thickness of the coating by using a Quanix 1500 thickness gauge to obtain the coating with the thickness of 50 mu m;
5) the coating was abraded using a carborundum abrasive disc and water mill, leaving a coating thickness of 40 μm and measured for Vickers hardness Hv at a load of 200 grams on a PMT3 apparatus. Diamond pyramids were used as indenters. The vickers hardness of the coating was measured to be 762 Hv.
In the case of the example 2, the following examples are given,
the process comprises the following steps:
1) cutting and molding a titanium alloy Ti6Al4V alloy TC2 to obtain a sample which is a round cake with the diameter of 2.5cm and the thickness of 0.5 cm;
2) pretreatment: the surface of the sample is simply polished by using sand paper, and burrs are removed; no other pretreatment is needed;
3) preparing an electrolyte:
preparing an electrolyte, wherein the electrolyte comprises the following components: 15g/L of sodium phosphate; KOH2g/L, sodium aluminate 15 g/L; mixing uniformly until all the components are dissolved;
4) reaction:
immersing a workpiece into electrolyte, and using a pulse power supply, wherein the anode is connected with the workpiece, and the cathode is connected with an inert conductor electrode to form a loop; the inert conductor electrode is stainless steel; the workpiece holder was made of 2mm diameter titanium wire and the part of the holder in the electrolyte and at the electrolyte-air interface was insulated by a tape made of fluoroplastic film. The adhesive tape is used for eliminating current loss caused by the oxidation of the bracket and avoiding micro-discharge at the interface of electrolyte and air. The holder is in threaded contact with the sample. In the reaction process, the electrolyte is fully stirred by using an air compressor.
Applying pulse current with current density of 15A/dm2, pulse frequency of 50Hz, duty ratio of 30% and electrolyte temperature of 35 + -2 deg.C. The application time was 90 minutes. Measuring the thickness of the coating by using a Quanix 1500 thickness gauge to obtain the coating with the thickness of 115 mu m;
5) the coating was abraded using a carborundum abrasive disc and water mill, leaving a 67 μm thick coating, and the vickers hardness Hv was measured on a PMT3 apparatus at a load of 200 grams. Diamond pyramids were used as indenters. The vickers hardness of the coating was determined to be 824 Hv.
The phase composition was studied on a DRON-3M diffractometer, Nigla Yeff inorganic chemistry institute of Russian academy of sciences, CuK 3 radiation, Ni filters, 2 steps from 5 to 65. The analysis shows that the relative peak intensity I of the aluminum titanate Al2TiO5 is 100, and the relative peak intensity I of the rutile TiO2 is 30.
In the case of the example 3, the following examples are given,
the process comprises the following steps:
1) cutting and molding a titanium alloy Ti6Al4V alloy TC4 to obtain a sample which is a round cake with the diameter of 2.5cm and the thickness of 0.5 cm;
2) pretreatment: the surface of the sample is simply polished by using sand paper, and burrs are removed; no other pretreatment is needed;
3) preparing an electrolyte:
preparing an electrolyte, wherein the electrolyte comprises the following components: 20g/L of sodium phosphate; KOH 4g/L, sodium aluminate 10 g/L; mixing uniformly until all the components are dissolved;
4) reaction:
immersing a workpiece into electrolyte, and using a pulse power supply, wherein the anode is connected with the workpiece, and the cathode is connected with an inert conductor electrode to form a loop; the inert conductor electrode is stainless steel; the workpiece holder was made of 2mm diameter titanium wire and the part of the holder in the electrolyte and at the electrolyte-air interface was insulated by a tape made of fluoroplastic film. The adhesive tape is used for eliminating current loss caused by the oxidation of the bracket and avoiding micro-discharge at the interface of electrolyte and air. The holder is in threaded contact with the sample. In the reaction process, the electrolyte is fully stirred by using an air compressor.
Applying pulse current with current density of 15A/dm2, pulse frequency of 200Hz, duty ratio of 30% and electrolyte temperature of 35 + -2 deg.C. The application time was 90 minutes. Measuring the thickness of the coating by using a Quanix 1500 thickness gauge to obtain the coating with the thickness of 90 mu m;
5) the coating was abraded using a carborundum abrasive disc and water mill, leaving a 83 μm thick coating, and the Vickers hardness Hv was measured on a PMT3 apparatus at a load of 200 grams. Diamond pyramids were used as indenters. The vickers hardness of the coating was determined to be 1094 Hv.
The phase composition was studied on a DRON-3M diffractometer, Nigla Yeff inorganic chemistry institute of Russian academy of sciences, CuK 3 radiation, Ni filters, 2 steps from 5 to 65. The analysis shows that the relative peak intensity I of the aluminum titanate Al2TiO5 is 100, and the relative peak intensity I of the rutile TiO2 is 10.8.
The invention relates to a novel technology for generating a high-hardness wear-resistant film layer on the surface of a titanium alloy through in-situ reaction. Through the matching of electrolyte and corresponding electrical parameters, a series of electrochemical reactions occur on the surface of the titanium alloy material, the reactions include micro-arc oxidation discharge, the thickness of a film layer can reach 90-110 mu m, the coating with the thickness of more than 50 mu m can be obtained after polishing, the Vickers hardness of the coating can reach 750-1100 Hv, and the coating is greatly superior to the prior art level. Microscopic analysis of the cross section shows that the three layers-the outer layer is light yellow, there are dark blue purple particles, the inner layer is yellow white, and the surface layer at the coating-metal interface is brown yellow.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. A method for improving the surface hardness and wear resistance of a titanium-containing material, which is characterized by comprising the following steps:
1) cutting and forming a workpiece containing a titanium material;
2) immersing the formed workpiece into electrolyte, and connecting an anode with the workpiece and a cathode with an inert conductor electrode by using a pulse power supply to form a loop; the inert conductor electrode is stainless steel;
3) applying pulse current with the current density of 10-20A/dm 2, the pulse frequency of 50-200 Hz, the duty ratio of 30%, the temperature of the electrolyte of 35 +/-2 ℃ and the application time of 5-90 minutes to form a coating on the surface of the workpiece;
4) and polishing the coating, and reserving 40-80% of the formed coating to obtain the high-hardness and high-wear-resistance coating.
2. The method of claim 1, wherein the electrolyte comprises: 10-30 g/L of sodium phosphate; 1-10 g/L of KOH and 5-30 g/L of sodium aluminate.
3. The method of claim 1, wherein during the step 3) reaction: stage one, white light is discharged within 2 minutes; and in the second stage, white light discharge and orange red discharge coexist, and the time is 2 minutes after the reaction starts, and can last for 5-10 minutes.
4. The method of claim 3, wherein the reaction process of step 3) further comprises a third stage, wherein the orange discharge continues to occur after the second stage for more than 30 minutes.
5. The method of claim 3, wherein the reaction process of step 3) further comprises a fourth stage, after the third stage, the arc discharge disappears, and the reaction can be continued for 10-30 minutes.
6. The method of claim 1, wherein step 2) further comprises securing the formed workpiece to a holder made of 2mm diameter titanium wire.
7. The method of claim 1, wherein the surface of the holder at the electrolyte-air interface and in-electrolyte interface is covered with an insulating substance.
8. The method of claim 1, wherein the pulse frequency is 100 to 200Hz and the application time is 60 to 90 minutes.
9. The method of claim 1, wherein the pulse frequency is 200Hz and the application time is 90 minutes.
10. The method of claim 1, wherein step 3) comprises stirring the electrolyte using an air compressor during the reaction.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114592227A (en) * | 2022-03-22 | 2022-06-07 | 西比里电机技术(苏州)有限公司 | Method for treating surface of aluminum-titanium-containing alloy |
| CN114606549A (en) * | 2022-03-22 | 2022-06-10 | 西比里电机技术(苏州)有限公司 | Surface treatment method for alloy containing vanadium and titanium |
| CN115976602A (en) * | 2022-12-31 | 2023-04-18 | 诸暨市中俄联合材料实验室 | Titanium-based wear-resistant coating with reticulate pattern structure and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107557840A (en) * | 2017-10-26 | 2018-01-09 | 杨晓艳 | A kind of magnesium alloy differential arc oxidation technique |
| CN109518254A (en) * | 2018-11-27 | 2019-03-26 | 中国船舶重工集团公司第七二五研究所 | A kind of microarc oxidation solution, titanium alloy high rigidity micro-arc oxidation films and preparation and application |
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2021
- 2021-09-28 CN CN202111145982.XA patent/CN113832514A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107557840A (en) * | 2017-10-26 | 2018-01-09 | 杨晓艳 | A kind of magnesium alloy differential arc oxidation technique |
| CN109518254A (en) * | 2018-11-27 | 2019-03-26 | 中国船舶重工集团公司第七二五研究所 | A kind of microarc oxidation solution, titanium alloy high rigidity micro-arc oxidation films and preparation and application |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114592227A (en) * | 2022-03-22 | 2022-06-07 | 西比里电机技术(苏州)有限公司 | Method for treating surface of aluminum-titanium-containing alloy |
| CN114606549A (en) * | 2022-03-22 | 2022-06-10 | 西比里电机技术(苏州)有限公司 | Surface treatment method for alloy containing vanadium and titanium |
| CN115976602A (en) * | 2022-12-31 | 2023-04-18 | 诸暨市中俄联合材料实验室 | Titanium-based wear-resistant coating with reticulate pattern structure and preparation method thereof |
| CN115976602B (en) * | 2022-12-31 | 2023-09-19 | 诸暨市中俄联合材料实验室 | Titanium-based wear-resistant coating with reticulate pattern structure and preparation method thereof |
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