CN101327337B - Method for preparing titanium alloy/hydroxylapatite gradient composite coating - Google Patents
Method for preparing titanium alloy/hydroxylapatite gradient composite coating Download PDFInfo
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- CN101327337B CN101327337B CN2008101503680A CN200810150368A CN101327337B CN 101327337 B CN101327337 B CN 101327337B CN 2008101503680 A CN2008101503680 A CN 2008101503680A CN 200810150368 A CN200810150368 A CN 200810150368A CN 101327337 B CN101327337 B CN 101327337B
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Abstract
The present invention discloses a gradient compound coating of a titanium alloy/hydroxyapatite and a preparation method thereof. The surface of the titanium alloy to be made is polished, cleaned and baked; 2 to 10 perforated flutes of 2mm multiplied by 2mm to 4 mm multiplied by 4mm are processed on the surface of the titanium alloy every 12mm; all the flutes are parallel to each other and are filled with powder; the titanium alloy filled with powder is placed on a tool with a heating device and is fixed and clamped; the titanium alloy is stirred by friction under the conditions that the room temperature rises to 350 DEG C to 500 DEG C, the rotation speed of a stirrer head ranges from 450 r / min to 850 r / min; the horizontal speed ranges from 28 mm/min to 90 mm/min, with an angle of inclination of 2.5 DEG. The rear area of a stirring area is provided with a cooling device, with the machining parts protected by argon gas. By a stirring method, the HA powder is stirred on the surface of the titanium alloy, thus forming viscoplasticity, speeding up the atom proliferation between the titanium alloy and the HA nano powder, and generating a chemical bond. The tensile-bonding strength is raised from24.8MPa in the prior art to ranging from 65 MPa to 103MPa.
Description
Technical field
The present invention relates to a kind of method that on titanium alloy, prepares composite coating.
Background technology
Titanium alloy is widely used in field of biomedical materials as bone alternate material, the key technology that limits its use is the biological activity height, (Hydroxyapatite, HA) coating is to improve one of its bioactive main method to prepare hydroxyapatite at titanium alloy surface.
The HA coating performance has material impact to the implantation effect and the life-span of titanium alloy.Bond strength between its floating coat and the matrix is even more important.If coating and matrix bond defective tightness, implant cause coating to separate with metallic matrix in human body easily and cause graft failure.Great majority are improved one's methods and are started with from technology itself, have proposed to improve the method for anchoring strength of coating, but the interior complex environment of receptor influences after implanting human body, and coating easily comes off, degrades, absorbs, and loses efficacy thereby cause to implant.Its reason is because the chemical compatibility of titanium alloy surface and HA coating is lower, cause key and very weak between HA molecule and the titanium alloy surface metallic atom, therefore, fundamentally improve Bond Strength of Coating, will start with to the affinity of HA from improving titanium alloy surface.
Transition gradient composite bed is the transition composite bed for preparing titanium alloy and HA at titanium alloy surface, it is changed by close matrix one lateral surface in gradient in structure and composition thickness direction, form the structure gradient and the component gradient of coating, thereby titanium alloy surface character is changed in gradient, improved the bond strength at the titanium alloy-based end.
Summary of the invention
In order to overcome the low deficiency of prior art stretching bond strength, the invention provides the preparation method of a kind of titanium alloy/alloy/hydroxylapatite gradient composite coating, this method adopts the agitating friction method, the stirring of HA powder is entered the titanium alloy top layer, at high temperature form the visco-plasticity state, quicken the atom diffusion between titanium alloy and the HA, and generate chemical bond, can improve the stretching bond strength between HA and the titanium alloy.
The technical solution adopted for the present invention to solve the technical problems: the preparation method of a kind of titanium alloy/alloy/hydroxylapatite gradient composite coating is characterized in may further comprise the steps:
(a) titanium alloy surface to be prepared is polished, and clean, dry;
(b) process the perforation groove of 2～10 4 * 4mm at titanium alloy surface every 12mm, each groove is parallel to each other, and fills powder body in groove;
(c) will more than be filled with powder body titanium alloy be positioned on the frock of band heater, fixing and clamp;
(d) titanium alloy is risen to 350～500 ℃ by room temperature, the rotating speed of stirring-head is 450～850r/min, horizontal translational speed 28～90mm/min, and agitating friction processing is carried out at 2.5 ° at inclination angle, and the stirring area rear is provided with chiller, and uses the argon shield working position;
(e) on the preparation basis of step (a)～(d), open the groove of 3 * 3mm once more, the HA nano powder of filling quality percentage composition 50% and 50% titanium alloy mixed-powder in groove, stirring-head rotating speed 650r/min, horizontal translational speed 45mm/min, the processing of two passage agitating frictions is carried out at 2.5 ° at inclination angle;
(f) on the preparation basis of step (e), open the groove of 2 * 2mm once more, stirring-head rotating speed 600r/min, horizontal translational speed 40mm/min, 2.5 ° at inclination angle, the HA nano powder of filling quality percentage composition 80% and 20% titanium alloy mixed-powder in groove carry out last one agitating friction processing; The titanium alloy-based end, keep 350～500 ℃ of temperature in the agitating friction process, and use the argon shield working position.
Description of drawings
The invention has the beneficial effects as follows: the present invention adopts the agitating friction method, the stirring of HA powder is entered the titanium alloy top layer, at high temperature form the visco-plasticity state, quicken the atom diffusion between titanium alloy and the HA, and generation chemical bond, improved the stretching bond strength between HA and the titanium alloy, the stretching bond strength between HA and the titanium alloy is brought up to 65～103MPa by the 24.8MPa of prior art.
Below in conjunction with drawings and Examples the present invention is elaborated.
The specific embodiment
Fig. 1 is the preparation method preparation process sketch map of titanium alloy of the present invention/alloy/hydroxylapatite gradient composite coating.
Among the figure, 1-titanium alloy, 2-groove, 3-stirring-head, 4-stirring-head shoulder.
With reference to accompanying drawing.Embodiment 1: prepare the HA gradient composite coating at the Ti-6Al-4V surface stirring friction.
Choose Ti-6Al-4V titanium alloy 1, through sand papering, the buffing machine polishing behind acetone, the ethanol ultrasonic waves for cleaning 20min, is rinsed well with redistilled water, and oven dry.12mm opens the groove 2 of two dark 2mm, wide 3mm at interval on titanium alloy 1, and fills the HA micropowder in groove 2, and its micropowder particle diameter is 3 μ m.Stirring-head 3 is selected the tungsten-rhenium alloy for use, its mixing needle end diameter Φ 3.5mm, high 4mm, stirring-head shoulder 4 diameter of phi 12mm.Stirring-head 3 rotating speed 850r/min, horizontal translational speed 36mm/min, agitating friction is carried out to the Ti-6Al-4V groove 2 that is filled with the HA micropowder in 2.5 ° at inclination angle.Titanium alloy 1 usefulness heating tape is heated to 350 ℃ in the agitating friction process, and uses the argon shield working position.
After tested, prepared titanium alloy/HA gradient composite coating thickness is 716 μ m, and HA and titanium alloy surface form chemical combination key, stretching bond strength 68MPa.
Embodiment 2:Ti-6Al-4V surface multi-pass agitating friction prepares blended HA nano powder of different proportion and titanium alloy powder gradient composite coating.
Choose Ti-6Al-4V titanium alloy 1, through sand papering, the buffing machine polishing behind acetone, the ethanol ultrasonic waves for cleaning 20min, is rinsed well with redistilled water, and oven dry.At interval 12mm opens ten grooves 2 of opening dark 4mm, wide 4mm on titanium alloy 1, at first the HA nano powder of filling quality percentage composition 20% and 80% titanium alloy mixed-powder in groove.Stirring-head 3 is selected the tungsten-rhenium alloy for use, its mixing needle end diameter Ф 3.5mm, high 4mm, stirring-head shoulder 4 diameter Ф 12mm.Stirring-head 3 rotating speed 700r/min, horizontal translational speed 90mm/min, a time agitating friction is carried out with the Ti-6Al-4V groove 2 that fills mixed-powder in 2.5 ° at inclination angle.Open the groove of dark 3mm, wide 3mm on this basis once more, the HA nano powder of filling quality percentage composition 50% and 50% titanium alloy mixed-powder in groove, stirring-head 3 rotating speed 650r/min, laterally translational speed 45mm/min, the processing of two passage agitating frictions is carried out at 2.5 ° at inclination angle; The last groove of opening dark 2mm, wide 2mm on this basis, stirring-head 3 rotating speed 600r/min, horizontal translational speed 40mm/min, 2.5 ° at inclination angle, the HA nano powder of filling quality percentage composition 80% and 20% titanium alloy mixed-powder in groove carry out last one agitating friction processing.The titanium alloy-based end, be heated to 400 ℃ with the heating tape in the agitating friction process, and use the argon shield working position.
After tested, prepared titanium alloy surface gradient composite bed thickness is 3820 μ m, and HA and titanium alloy surface form chemical combination key, stretching bond strength 101MPa.
1: 1 blended Ti-6Al-4V nano powder+HA nano powder gradient composite coating of embodiment 3:Ti-6Al-4V surface stirring friction volume ratio.
Choose Ti-6Al-4V titanium alloy 1, through sand papering, the buffing machine polishing behind acetone, the ethanol ultrasonic waves for cleaning 20min, is rinsed well with redistilled water, and oven dry.At interval 12mm opens a plurality of grooves 2 of opening dark 2mm, wide 4mm on titanium alloy 1, and in groove packing volume than 1: 1 blended Ti-6Al-4V nano powder+HA nano powder.Stirring-head 3 is selected the tungsten-rhenium alloy for use, its mixing needle end diameter Ф 3.5mm, high 4mm, stirring-head shoulder 4 diameter Ф 12mm.Stirring-head 3 rotating speed 450r/min, horizontal translational speed 28mm/min, agitating friction is carried out with filling the Ti-6Al-4V groove 2 that mixes nano powder in 2.5 ° at inclination angle.The titanium alloy-based end, be heated to 450 ℃ with the heating tape in the agitating friction process, and use the argon shield working position.
After tested, prepared titanium alloy surface gradient composite bed thickness is 950 μ m, and HA and titanium alloy surface form chemical combination key, stretching bond strength 65MPa.
Embodiment 4: the medical TLE alloy of β type (Ti-(3～6) Zr (2～4) Mo (24～27) Nb) surface stirring friction HA micropowder gradient composite coating.
Choose TLE titanium alloy alloy 1, through sand papering, the buffing machine polishing behind acetone, the ethanol ultrasonic waves for cleaning 20min, is rinsed well with redistilled water, and oven dry.12mm opens a plurality of grooves 2 of opening dark 2mm, wide 4mm at interval on titanium alloy 1, and fills the HA micropowder in groove, and its micropowder particle diameter is 3 μ m.Stirring-head 3 is selected the tungsten-rhenium alloy for use, its mixing needle end diameter Ф 3.5, high 4mm, stirring-head shoulder 4 diameter Ф 12mm.Stirring-head 3 rotating speed 850r/min, horizontal translational speed 36mm/min, agitating friction is carried out with the TLE alloy groove 2 that fills the HA micropowder in 2.5 ° at inclination angle.The titanium alloy-based end, be heated to 500 ℃ with the heating tape in the agitating friction process, and use the argon shield working position.
After tested, prepared titanium alloy surface gradient composite bed thickness is 690 μ m, and HA and titanium alloy surface form chemical combination key, stretching bond strength 66MPa.
Embodiment 5: the medical TLE alloy of β type (Ti-(3～6) Zr (2～4) Mo (24～27) Nb) surface stirring friction HA nano powder gradient composite coating.
Choose TLE titanium alloy alloy 1, through sand papering, the buffing machine polishing behind acetone, the ethanol ultrasonic waves for cleaning 20min, is rinsed well with redistilled water, and oven dry.12mm opens a plurality of grooves 2 of opening dark 2mm, wide 4mm at interval on titanium alloy 1, and fills the HA nano powder in groove.Stirring-head 3 is selected the tungsten-rhenium alloy for use, its mixing needle end diameter Ф 3.5mm, high 4mm, stirring-head shoulder 4 diameter Ф 12mm.Stirring-head 3 rotating speed 450r/min, horizontal translational speed 28mm/min, agitating friction is carried out with the TLE alloy groove 2 that fills the HA nano powder in 2.5 ° at inclination angle.The titanium alloy-based end, be heated to 500 ℃ with the heating tape in the agitating friction process, and use the argon shield working position.
After tested, prepared titanium alloy surface gradient composite bed thickness is 805 μ m, and HA and titanium alloy surface form chemical combination key, stretching bond strength 76MPa.
Embodiment 6: 1: 1 blended medical TLE titanium alloy nano powder+HA nano powder gradient composite coating of the medical TLE alloy of β type (Ti-(3～6) Zr (2～4) Mo (24～27) Nb) surface stirring friction volume ratio.
Choose TLE titanium alloy alloy 1, through sand papering, the buffing machine polishing behind acetone, the ethanol ultrasonic waves for cleaning 20min, is rinsed well with redistilled water, and oven dry.At interval 12mm opens a plurality of grooves 2 of opening dark 2mm, wide 4mm on titanium alloy 1, and in groove packing volume than 1: 1 blended medical TLE titanium alloy nano powder+HA nano powder.Stirring-head 3 is selected the tungsten-rhenium alloy for use, its mixing needle end diameter Ф 3.5mm, high 4mm, stirring-head shoulder 4 diameter Ф 12mm.Stirring-head 3 rotating speed 450r/min, horizontal translational speed 28mm/min, agitating friction is carried out with filling the TLE alloy groove 2 that mixes nano powder in 2.5 ° at inclination angle.The titanium alloy-based end, be heated to 450 ℃ with the heating tape in the agitating friction process, and use the argon shield working position.
After tested, prepared titanium alloy surface gradient composite bed thickness is 905 μ m, and HA and titanium alloy surface form chemical combination key, stretching bond strength 79MPa.
Embodiment 7:Ti-29Nb-13Ta-4.6Zr titanium alloy surface multi-pass blended HA nano powder of agitating friction different proportion and titanium alloy powder gradient composite coating.
Choose Ti-29Nb-13Ta-4.6Zr titanium alloy 1, through sand papering, the buffing machine polishing behind acetone, the ethanol ultrasonic waves for cleaning 20min, is rinsed well with redistilled water, and oven dry.At interval 12mm opens a plurality of grooves 2 of opening dark 4mm, wide 4mm on titanium alloy 1, at first the HA nano powder of filling quality percentage composition 20% and 80% titanium alloy mixed-powder in groove.Stirring-head 3 is selected the tungsten-rhenium alloy for use, its mixing needle end diameter Ф 3.5mm, high 4mm, stirring-head shoulder 4 diameter Ф 12mm.Stirring-head 3 rotating speed 450r/min, horizontal translational speed 28mm/min, a time agitating friction is carried out with the Ti-29Nb-13Ta-4.6Zr groove 2 that fills mixed-powder in 2.5 ° at inclination angle.Open the groove of dark 3mm, wide 3mm on this basis once more, the HA nano powder of filling quality percentage composition 50% and 50% titanium alloy mixed-powder in groove, and carry out the processing of two passage agitating frictions; The last groove of opening dark 2mm, wide 2mm on this basis, the HA nano powder of filling quality percentage composition 80% and 20% titanium alloy mixed-powder carry out last one agitating friction and process in groove.The titanium alloy-based end, be heated to 400 ℃ with the heating tape in the agitating friction process, and use the argon shield working position.
After tested, prepared titanium alloy surface gradient composite bed thickness is 3440 μ m, and HA and titanium alloy surface form chemical combination key, stretching bond strength 99MPa.
Embodiment 8: nearly blended HA nano powder of the surperficial multi-pass agitating friction of beta-titanium alloy Ti-3Zr-2Sn-3Mo-15Nb (TLM) different proportion and titanium alloy powder gradient composite coating.
Choose Ti-3Zr-2Sn-3Mo-15Nb (TLM) titanium alloy titanium alloy 1, through sand papering, the buffing machine polishing behind acetone, the ethanol ultrasonic waves for cleaning 20min, is rinsed well with redistilled water, and oven dry.At interval 12mm opens a plurality of grooves 2 of opening dark 4mm, wide 4mm on titanium alloy 1, at first the HA nano powder of filling quality percentage composition 20% and 80% titanium alloy mixed-powder in groove.Stirring-head 3 is selected the tungsten-rhenium alloy for use, its mixing needle end diameter Ф 3.5mm, high 4mm, stirring-head shoulder 4 diameter Ф 12mm.Stirring-head 3 rotating speed 450r/min, horizontal translational speed 28mm/min, a time agitating friction is carried out with Ti-3Zr-2Sn-3Mo-15Nb (TLM) groove 2 that fills mixed-powder in 2.5 ° at inclination angle.Open the groove of dark 3mm, wide 3mm on this basis once more, the HA nano powder of filling quality percentage composition 50% and 50% titanium alloy mixed-powder in groove, and carry out the processing of two passage agitating frictions; The last groove of opening dark 2mm, wide 2mm on this basis, the HA nano powder of filling quality percentage composition 80% and 20% titanium alloy mixed-powder carry out last one agitating friction and process in groove.The titanium alloy-based end, be heated to 350 ℃ with the heating tape in the agitating friction process, and use the argon shield working position.
After tested, prepared titanium alloy surface gradient composite bed thickness is 3520 μ m, and HA and titanium alloy surface form chemical combination key, stretching bond strength 103MPa.
Claims (2)
1. the preparation method of titanium alloy/alloy/hydroxylapatite gradient composite coating is characterized in that may further comprise the steps:
(a) titanium alloy surface to be prepared is polished, and clean, dry;
(b) process the perforation groove of 2～10 4 * 4mm at titanium alloy surface every 12mm, each groove is parallel to each other, and fills powder body in groove;
(c) will more than be filled with powder body titanium alloy be positioned on the frock of band heater, fixing and clamp;
(d) titanium alloy is risen to 350～500 ℃ by room temperature, the rotating speed of stirring-head is 450～850r/min, horizontal translational speed 28～90mm/min, and agitating friction processing is carried out at 2.5 ° at inclination angle, and the stirring area rear is provided with chiller, and uses the argon shield working position;
(e) on the preparation basis of step (a)～(d), open the groove of 3 * 3mm once more, the HA nano powder of filling quality percentage composition 50% and 50% titanium alloy mixed-powder in groove, stirring-head rotating speed 650r/min, horizontal translational speed 45mm/min, the processing of two passage agitating frictions is carried out at 2.5 ° at inclination angle;
(f) on the preparation basis of step (e), open the groove of 2 * 2mm once more, stirring-head rotating speed 600r/min, horizontal translational speed 40mm/min, 2.5 ° at inclination angle, the HA nano powder of filling quality percentage composition 80% and 20% titanium alloy mixed-powder in groove carry out last one agitating friction processing; The titanium alloy-based end, keep 350～500 ℃ of temperature in the agitating friction process, and use the argon shield working position.
2. the preparation method of titanium alloy according to claim 1/alloy/hydroxylapatite gradient composite coating is characterized in that: described powder body is the mixed powder of HA powder body or HA powder body and titanium alloy powder body.
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| CN102650048A (en) * | 2012-05-22 | 2012-08-29 | 西北工业大学 | Method for preparing hydroxyapatite composite gradient coating on surface of titanium alloy |
| CN108103546B (en) * | 2018-01-15 | 2019-07-30 | 郑州大学 | A kind of controlled degradation magnesium-based functionally graded material and preparation method thereof |
| CN111531266B (en) * | 2020-05-07 | 2021-08-31 | 广东省科学院中乌焊接研究所 | Friction stir welding equipment and method for particle-reinforced gradient composite material |
| CN113088958B (en) * | 2021-03-09 | 2021-12-28 | 中南大学 | Gradient composite bioactive ceramic coating material and preparation method thereof |
| CN114850598A (en) * | 2022-04-21 | 2022-08-05 | 西安优耐特容器制造有限公司 | Preparation method of surface metal-based composite gradient material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1629364A (en) * | 2003-12-17 | 2005-06-22 | 中南大学 | Process for preparing hydroxy apatite / titanium oxide gradient coating |
| CN1712076A (en) * | 2004-06-15 | 2005-12-28 | 中国科学院金属研究所 | Surface treatment for improving bioactivity and wear-resistant ability of titanium alloy surfaces |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1629364A (en) * | 2003-12-17 | 2005-06-22 | 中南大学 | Process for preparing hydroxy apatite / titanium oxide gradient coating |
| CN1712076A (en) * | 2004-06-15 | 2005-12-28 | 中国科学院金属研究所 | Surface treatment for improving bioactivity and wear-resistant ability of titanium alloy surfaces |
Non-Patent Citations (1)
| Title |
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| 李永华，檀雯，郑洁，齐广霞，王忠堂.医用钛合金羟基磷灰石涂层的研究动态.《金属功能材料》.2008,第15卷(第2期),45-48. * |
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