CN113774457A - Method for manufacturing medical titanium-containing material with micro-porous structure surface - Google Patents
Method for manufacturing medical titanium-containing material with micro-porous structure surface Download PDFInfo
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- CN113774457A CN113774457A CN202111144986.6A CN202111144986A CN113774457A CN 113774457 A CN113774457 A CN 113774457A CN 202111144986 A CN202111144986 A CN 202111144986A CN 113774457 A CN113774457 A CN 113774457A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- 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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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- 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
- C25D11/36—Phosphatising
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
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- C—CHEMISTRY; METALLURGY
- 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
- C25D5/18—Electroplating using modulated, pulsed or reversing current
Abstract
The invention discloses a method for manufacturing a medical titanium-containing material with a micro-porous structure surface, which is characterized by comprising the following steps: 1) cutting and forming a workpiece containing a titanium material; 2) immersing the formed workpiece into an electrolyte containing sodium phosphate, 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; 3) applying pulse current with the current density of 10-15A/dm 2, the pulse frequency of 50-200 Hz, the duty ratio of 20-35%, and the application time of 5-20 minutes. The invention is a process method for directly forming a bioactive film layer with a porous structure by carrying out one-step reaction on a titanium alloy in electrolyte by using a pulse power supply, and complex pre-treatment and post-treatment are not required to be carried out on the alloy material; the process is greatly simplified; the reaction time is greatly shortened; the surface of the obtained product has a unique crater-shaped porous structure, and has obvious effects on inducing the growth of bone cells and healing tissues; the electrolyte has simple components, is easy to prepare and is environment-friendly.
Description
Technical Field
The invention relates to the field of medical implant materials, in particular to a method for manufacturing a medical titanium-containing material with a micro-porous structure surface.
Background
The titanium alloy is an alloy material widely applied in the field of medical implant materials at present. However, the untreated titanium alloy has limited biocompatibility with human tissues, is difficult to be tightly combined with biological tissues after being implanted into a body, is difficult to induce wound healing, and is easy to cause inflammatory reaction.
In recent years, a great deal of research shows that a coating with a micro-porous structure close to the surface pore morphology of human skeleton is prepared in the field of medical implant materials, so that the biocompatibility can be improved, and the wound healing can be promoted.
The prior art uses anode oxidation, acid etching, plasma spraying and other processes to treat medical metal materials, but the processes all have obvious defects: anodic oxidation is difficult to control the microstructure and the crystallization component of the film layer, the coating is thin (below 10 microns), the coating is mainly used for physical protection and coloring of titanium and magnesium alloy, and the improvement on the biocompatibility is limited. The surface of the film layer formed by acid etching is a concave-convex surface, which is mainly used for improving the corrosion resistance and has no obvious improvement on the biocompatibility. The plasma spraying process can form a surface coating with certain roughness, but the bonding force between the coating and the substrate metal is weak, and the coating is easy to fall off due to the action of external force during and after an operation when an organism is implanted, so that serious medical accidents are caused.
The existing titanium alloy micro-arc oxidation method (CN 103911644B) in electrolyte comprises pretreatment, micro-arc oxidation and post-treatment, and is characterized in that phytic acid or phytate electrolyte is used as the electrolyte, a 100 Hz-3000 Hz pulse power supply is used, the current density is 10-80 mA/cm2, and the prepared oxide film is black and contains calcium phytate components. The process has the problems that the components of the phytic acid double-salt electrolyte are complex, the microstructure of an oxide film is not controlled, the frequency of a pulse power supply is high, and the direct reaction of power frequency alternating current is not facilitated.
A preparation method (CN 103088348B) of a low-elasticity-modulus bioactive ceramic membrane with a titanium surface porous structure layer is provided, and the process comprises three steps of powder metallurgy, micro-arc oxidation and electrodeposition. The process has the problems that the process steps are complicated, the principle of realizing the biological activity is to play a role through a hydroxyapatite coating, and the total thickness of the coating is thick, so that the application occasions are limited.
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 generate a micro-porous structure surface of a titanium-containing material by a simple electrolyte and a simple process.
In order to achieve the aim, the invention provides a method for manufacturing a medical titanium-containing material with a micro-porous structure surface, which is characterized by comprising the following steps:
1) cutting and forming a workpiece containing a titanium material;
2) immersing the formed workpiece into an electrolyte containing sodium phosphate, 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;
3) applying pulse current with the current density of 10-15A/dm 2, the pulse frequency of 50-200 Hz, the duty ratio of 20-35%, and the application time of 5-20 minutes.
Further, the electrolyte includes: 10-30 g/L of sodium phosphate.
Further, the sodium phosphate is 20-30 g/L.
Further, the sodium phosphate is 30 g/L.
Further, the pulse power supply is a direct current pulse power supply.
Further, the titanium-containing material comprises:
pure titanium or Ti6Al4V alloy;
the pure titanium comprises at least one of TA2, TA3 and TA 4;
the Ti6Al4V alloy comprises at least one of TC2, TC3 and TC 4.
Further, the step 1) comprises the steps of uniformly stirring the mixture by using deionized water to prepare electrolyte mainly containing sodium phosphate, and simply polishing the surface of the titanium-containing material after cutting and forming by using sand paper to remove burrs.
Preferably, the temperature range of the electrolyte is 10-40 ℃, the pulse frequency is 50-100 Hz, the duty ratio is 25-35%, and the application time is 8-15 minutes.
Preferably, the temperature range of the electrolyte is 20-40 ℃, the pulse frequency is 50Hz, the duty ratio is 30-35%, and the application time is 8-10 minutes.
Preferably, the temperature range of the electrolyte is 30-40 ℃, the pulse frequency is 50Hz, the duty ratio is 30%, and the application time is 10 minutes.
Preferably, said step 3) occurs during the 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.
Preferably, the reaction process in the step 3) further comprises a third stage, wherein orange discharge is continuously generated after the second stage, and the duration is more than 30 minutes;
preferably, the reaction process in the step 3) further comprises a fourth stage, wherein after the third stage, the arc discharge disappears, and the reaction can be continued for 10-30 minutes.
The invention relates to a process method for directly forming a bioactive film layer with a porous structure by one-step reaction of titanium alloy in electrolyte by using a pulse power supply. It is characterized in that: complex pre-treatment and post-treatment of the alloy material are not needed; the reaction process is one-step reaction, and the process is greatly simplified; the reaction time is greatly shortened; the surface of the obtained product has a unique crater-shaped porous structure, and has obvious effects on inducing the growth of bone cells and healing tissues; the electrolyte has simple components, is easy to prepare and is environment-friendly.
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
Drawings
FIG. 1 is a surface micro-topography of a titanium alloy oxide film prepared according to a preferred embodiment 1 of the present invention;
FIG. 2 is a surface micro-topography of a titanium alloy oxide film prepared according to a preferred embodiment 2 of the present invention;
FIG. 3 is a surface micro-topography of a titanium alloy oxide film prepared according to a preferred embodiment 3 of the present invention;
FIG. 4 is a surface micro-topography of a titanium alloy oxide film prepared in accordance with a preferred embodiment 4 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 process comprises the following steps:
the electrolyte includes: 10-30 g/L of sodium phosphate. Only sodium phosphate was contained. (Key feature other electrolytes may be added selectively, but not to play a significant role)
The raw materials comprise: pure titanium (TA 2, TA3, TA4, etc.), Ti6Al4V alloy (TC 2, 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 the current density of 10-15A/dm 2, the pulse frequency of 50-200 Hz, the duty ratio of 20-35%, and the application time of 5-20 minutes.
Step 3) occurs during the 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.
Step 3), the reaction process also comprises a third stage, wherein orange discharge is continuously generated after the second stage, and the reaction can last for more than 30 minutes;
and step 3), the reaction process also comprises a stage four, the arc discharge is generated after the stage three, and the reaction can be continued for 10-30 minutes.
Example 1
20g/L sodium phosphate, uniformly stirring with deionized water to prepare electrolyte, selecting TA2 as a pure titanium sample, simply polishing the surface with sand paper to remove burrs, and carrying out micro-arc oxidation in the electrolyte by using a direct current pulse power supply by using the titanium sample as an anode and a stainless steel barrel as a cathode to obtain the porous coating.
The micro-arc oxidation process is controlled to be 25%, the positive current density is constant to be 10A/dm2, the negative current density is constant to be 10A/dm2, the pulse frequency is 50Hz, the temperature of the electrolyte is 10-20 ℃, the time is 8min, a porous coating is formed on the surface of the micro-arc oxidized titanium sample, and the titanium sample is cleaned by clear water and then naturally dried.
After the TA2 sample is subjected to micro-arc oxidation, a porous coating is obtained, and the thickness of the coating is 9 microns by testing through an Elcometer456 eddy current thickness gauge.
After the TA2 sample is subjected to micro-arc oxidation, a porous coating is obtained, and the surface roughness is 1.2 microns by testing with a surface roughness tester.
After the micro-arc oxidation of the above TA2 sample, a porous coating was obtained, and it can be seen from the SEM image of FIG. 1 that the coating has a porous structure.
Example 2
20g/L sodium phosphate, uniformly stirring with deionized water to prepare electrolyte, selecting TA3 as a pure titanium sample, simply polishing the surface with sand paper to remove burrs, and carrying out micro-arc oxidation in the electrolyte by using a direct current pulse power supply by using the titanium sample as an anode and a stainless steel barrel as a cathode to obtain the porous coating.
The micro-arc oxidation process controls the duty ratio to be 20%, the positive current density to be 12A/dm2, the negative current density to be 12A/dm2, the pulse frequency to be 50Hz, the electrolyte temperature to be 10-30 ℃, the time to be 10min, the surface of the titanium sample after micro-arc oxidation forms a porous coating, and the titanium sample is cleaned by clear water and then naturally dried.
After the TA3 sample is subjected to micro-arc oxidation, a porous coating is obtained, and the thickness of the coating is 10 microns by testing through an Elcometer456 eddy current thickness gauge.
After the TA3 sample is subjected to micro-arc oxidation, a porous coating is obtained, and the surface roughness of the porous coating is 1.2 microns by testing with a surface roughness meter
After the above TA3 sample was micro-arc oxidized, a porous coating was obtained, and the coating was seen to have a porous structure in the SEM image of FIG. 2.
Example 3
30g/L sodium phosphate is uniformly stirred by deionized water to prepare electrolyte, a pure titanium sample is TA4, the surface of the pure titanium sample is simply polished by abrasive paper to remove burrs, the titanium sample is used as an anode, a stainless steel barrel is used as a cathode, and a direct current pulse power supply is adopted to perform micro-arc oxidation in the electrolyte to obtain the porous coating.
The micro-arc oxidation process controls the duty ratio to be 30%, the positive current density to be 10A/dm2, the negative current density to be 15A/dm2, the pulse frequency to be 100Hz, the electrolyte temperature to be 10-40 ℃, the time to be 10min, the surface of the titanium sample after micro-arc oxidation forms a porous coating, and the titanium sample is cleaned by clear water and then naturally dried.
After the TA4 sample is subjected to micro-arc oxidation, a porous coating is obtained, and the thickness of the coating is 12 mu m by testing through an Elcometer456 eddy current thickness gauge.
After the TA4 sample is subjected to micro-arc oxidation, a porous coating is obtained, and the surface roughness is 1.5 microns by testing through a surface roughness meter
After the above TA4 sample was micro-arc oxidized, a porous coating was obtained, and the coating was seen to have a porous structure in the SEM image of FIG. 3.
Example 4
30g/L sodium phosphate is uniformly stirred by deionized water to prepare electrolyte, a titanium alloy sample is Ti6Al4V with the label TC4, the surface of the titanium alloy sample is deoiled by acetone, ultrasonically cleaned by ethanol, and subjected to micro-arc oxidation in the electrolyte by using a direct current pulse power supply to obtain the porous coating by using a titanium sample as an anode and a stainless steel barrel as a cathode.
The micro-arc oxidation process is controlled to have the duty ratio of 35%, the positive current density is constant at 15A/dm2, the negative current density is constant at 10A/dm2, the pulse frequency is 200Hz, the temperature of the electrolyte is 10-30 ℃, the time is 15min, a porous coating is formed on the surface of the titanium alloy sample after micro-arc oxidation, and the titanium alloy sample is cleaned by clear water and then naturally dried.
The Ti6Al4V sample is subjected to micro-arc oxidation to obtain a porous coating, and the thickness of the porous coating is 15 microns through an Elcometer456 eddy current thickness gauge.
The Ti6Al4V sample is subjected to micro-arc oxidation to obtain a porous coating, and the surface roughness of the porous coating is 1.8 microns by testing with a surface roughness meter
The above Ti6Al4V sample was micro-arc oxidized to obtain a porous coating, and the coating has a porous structure as can be seen from FIG. 4 and SEM image.
The invention relates to a process method for directly forming a bioactive film layer with a porous structure by one-step reaction of titanium alloy in electrolyte by using a pulse power supply. It is characterized in that: complex pre-treatment and post-treatment of the alloy material are not needed; the reaction process is one-step reaction, and the process is greatly simplified; the reaction time is greatly shortened; the surface of the obtained product has a unique crater-shaped porous structure, and has obvious effects on inducing the growth of bone cells and healing tissues; the electrolyte has simple components, is easy to prepare and is environment-friendly.
1. The thickness of the film layer is about 9-11 microns, and the surface roughness is 1.25 microns (characteristic value), or 1.2-2 microns (range value);
2. the film layer is observed by using SEM to see a volcano-crater-shaped porous structure which is uniformly distributed. Relevant studies show that the porous structure can effectively induce the attachment and growth of bone cells.
3. The film layer only contains three elements of titanium, oxygen and phosphorus, so that the introduction of other elements is reduced, and the stress reaction risk is avoided; the content of the phosphorus element reaches more than 10 percent, which is beneficial to improving the biocompatibility.
4. The reaction electrolyte can reach the domestic wastewater discharge standard after simple precipitation and sand filtration.
A titanium sample placed in an electrolytic solution quickly forms a very thin titanium oxide ceramic layer at the moment of electrification, a weak area in the titanium oxide ceramic layer is simultaneously broken down to form a discharge channel under the action of a strong electric field generated by voltage, the electrolytic solution is injected into the discharge channel and is subjected to high temperature, molten titanium is separated from a matrix and also enters the discharge channel, then plasma chemical reaction occurs in the channel, and a product Ti02 in the reaction is deposited on the inner wall of the discharge channel and the surface near the channel opening, so that the porous titanium oxide ceramic layer is formed and gradually thickened.
The invention relates to a process method for directly forming a bioactive film layer with a porous structure by one-step reaction of titanium alloy in electrolyte by using a pulse power supply. It is characterized in that: complex pre-treatment and post-treatment of the alloy material are not needed; the reaction process is one-step reaction, and the process is greatly simplified; the reaction time is greatly shortened; the surface of the obtained product has a unique crater-shaped porous structure, and has obvious effects on inducing the growth of bone cells and healing tissues; the electrolyte has simple components, is easy to prepare and is environment-friendly.
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 (12)
1. A method for manufacturing a medical titanium-containing material with a micro-porous structure surface is characterized by comprising the following steps:
1) cutting and forming a workpiece containing a titanium material;
2) immersing the formed workpiece into an electrolyte containing sodium phosphate, 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;
3) applying pulse current with the current density of 10-15A/dm 2, the pulse frequency of 50-200 Hz, the duty ratio of 20-35%, and the application time of 5-80 minutes.
2. The method of claim 1, wherein the electrolyte comprises: 10-30 g/L of sodium phosphate.
3. The method of claim 2, wherein the amount of sodium phosphate is 20-30 g/L.
4. The method of claim 2, wherein the sodium phosphate is 30 g/L.
5. The method of claim 1, wherein the pulsed power supply is a dc pulsed power supply.
6. The method of claim 1, wherein the titanium-containing material comprises:
pure titanium or Ti6Al4V alloy;
the pure titanium comprises at least one of TA2, TA3 and TA 4;
the Ti6Al4V alloy comprises at least one of TC2, TC3 and TC 4.
7. The method of claim 1, wherein step 1) comprises uniformly stirring with deionized water to prepare an electrolyte mainly containing sodium phosphate, and the surface of the titanium-containing material after cutting is simply sanded to remove burrs.
8. The method of claim 1, wherein the temperature of the electrolyte is in the range of 10 to 40 ℃, the pulse frequency is 50 to 100Hz, the duty cycle is 25 to 35%, and the application time is 8 to 15 minutes.
9. The method of claim 1, wherein the temperature of the electrolyte is in the range of 20 to 40 ℃, the pulse frequency is 50Hz, the duty cycle is 30 to 35%, and the application time is 8 to 10 minutes.
10. The method of claim 1, wherein the electrolyte has a temperature in the range of 30 to 40 ℃, a pulse frequency of 50Hz, a duty cycle of 30% and an application time of 10 minutes.
11. 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.
12. The method of claim 11, 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;
the method of claim 11, 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 to 30 minutes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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2021
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