CN102650048A - Method for preparing hydroxyapatite composite gradient coating on surface of titanium alloy - Google Patents
Method for preparing hydroxyapatite composite gradient coating on surface of titanium alloy Download PDFInfo
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- CN102650048A CN102650048A CN2012101601891A CN201210160189A CN102650048A CN 102650048 A CN102650048 A CN 102650048A CN 2012101601891 A CN2012101601891 A CN 2012101601891A CN 201210160189 A CN201210160189 A CN 201210160189A CN 102650048 A CN102650048 A CN 102650048A
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Abstract
The invention discloses a method for preparing a hydroxyapatite composite gradient coating on the surface of titanium alloy. The method comprises the steps as follows: polishing the surface of the titanium alloy to be prepared so as to remove a surface oxidation layer, cleaning and drying; preparing a layer of pure metal Ni on the surface of the titanium alloy; and mixing absolute ethanol with HAp powder according to a mass ratio of 2 to 1 so as to prepare slurry, uniformly coating the slurry onto the surface of the titanium alloy with the Ni layer by a coating thickness of 0.1-0.3 mm, drying, placing into a vacuum furnace, stepwise heating to be 1050 DEG C at a speed of 10 DEG C/min, insulating for 1 h, and carrying out furnace cooling. According to the method, the coating preparation process is simplified, the cost is reduced and the efficiency is improved.
Description
Technical field
The present invention relates to a kind of method for preparing complex gradient coating at titanium alloy surface.
Background technology
Titanium alloy is widely used in field of biomedical materials as bone alternate material, and the gordian technique that limits its use is that biological activity is lower, and Young's modulus is higher than people's flexible bone modulus, thereby after implantation, causes the stress shielding effect.(Hydroxyapatite, HAp) coating is to improve one of its bioactive main method to prepare Win 40350 at titanium alloy surface.And the main method that solves the stress shielding effect is the preparation complex gradient coating.
At present; The method for preparing the HAp coating at titanium alloy surface is a lot; Major part need be accomplished under comparatively high temps, because thermal expansion coefficient difference is bigger between titanium alloy and the Win 40350, thereby in temperature-fall period, causes the bigger residual thermal stress of appearance between coating and the substrate; Cause the bonding strength between the two lower, implant the back coating and be prone to peel off.
Document " unrelieved stress of plasma spraying bio-active gradient coating and bonding strength, Wang Yingjun, Ning Chengyun; Chen Kai etc.; Journal of Inorganic Materials, 1998,13 (4): 529-534. " proposes the bioactivity glass of 40%, 20%, 0% content is joined among the HAp; Divide and adopt for 3 times plasma spraying method to spray to titanium alloy surface, realize the Gradient distribution of composition.Document " preparation and the Interface Study thereof of light cladding titanium base bioceramic coating, Zheng Min, Fan Ding; Li Xiukun; Zhang Jianbin, Liu Qibin. Rare Metals Materials and engineering .2009,38 (11) " will contain 80%, 40%, the mixed powder of 0%Ti powder divides and is coated in the substrate for three times; Respectively it is carried out laser melting coating and prepare coating, obtain having the coating of component gradient.Above method is the representative thinking for preparing complex gradient coating at titanium alloy surface; Promptly at first prepare composite powder with gradient composition; At first prefabricated one deck coating is at titanium alloy-based basal surface; And make this composite powder and substrate form metallurgical binding at a certain temperature, carry out the preparation of the second layer, the 3rd layer of coating again, thereby realize the component gradient of coating.Utilize this thinking repeatedly to prepare just and can obtain complex gradient coating, increased preparation cost on the one hand, on the other hand coating section transitions and inhomogeneous.
Summary of the invention
In order to overcome the deficiency of prior art, the present invention provides a kind of and prepares the method for Win 40350 complex gradient coating at titanium alloy surface, adopts transient liquid phase method one step preparation complex gradient coating, simplifies preparation technology of coating, reduces cost, raises the efficiency.
The technical solution adopted for the present invention to solve the technical problems may further comprise the steps:
(a) titanium alloy surface to be prepared is polished with the removal surface oxide layer, and clean, dry;
(b) prepare one deck pure metal Ni at titanium alloy surface, for tabular titanium alloy, can Ni paper tinsel (thickness 0.05-0.3mm) be placed on the titanium alloy plate, adopt diffusion welding method at 900 ℃, 4MPa pressure is incubated 1 hour down; For special-shaped titanium alloy, can adopt electro-plating method to introduce the Ni layer at titanium alloy surface, the Ni layer thickness is 0.005-0.08mm;
(c) use mass ratio to mix with the HAp powder as the absolute ethyl alcohol of 2:1; Adopt ultrasonic or whisking appliance is mixed and made into slurry, evenly be coated in the prefabricated titanium alloy surface that has prepared the Ni layer, coat thickness reaches 0.1-0.3mm; Put into vacuum oven after the drying; Speed with 10 ° of C/min is warming up to 1050 ℃ stage by stage, is incubated after 1 hour, and stove is cold.
The invention has the beneficial effects as follows: the present invention adopts the transient liquid phase method; Utilize the metal Ti atom at its eutectic point (942 ℃) mutual diffusion mutually to take place with metal Ni atom; In the extremely short time, form liquid phase; Soak into the HAp powder, form metallurgical binding with the titanium alloy-based end, the complex gradient coating of formation and the bonding strength at the titanium alloy-based end have been brought up to 40-88MPa.
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Description of drawings
Fig. 1 is that the Ni paper tinsel links synoptic diagram with the diffusion of the titanium alloy-based end.
Among Fig. 1,1-titanium alloy, 2-seaming chuck, the heat insulation solder mask of 3-, 4-nickel foil, 5-pedestal, 6-web member.
Fig. 2 is special-shaped titanium alloy electroplated Ni layer synoptic diagram.
Among Fig. 2,1-abnormity titanium alloy, 2-coating spare, 3-prefab.
Embodiment
With reference to accompanying drawing.
Embodiment 1: at plate shaped Ti-6Al-4V substrate surface preparation HA complex gradient coating.
Choose plate shaped Ti-6Al-4V titanium alloy 1, titanium alloy 1 (on mill the groove that dark 1mm, length and width are 50mm,,, behind acetone, alcohol ultrasonic cleaning 20min, rinse well to remove surface oxide layer with sand papering, and oven dry with redistilled water.Choose the nickel foil 4 that is of a size of 0.1mm * 50mm * 50mm, it is tiled in the groove of titanium alloy 1, place between seaming chuck 2, heat insulation solder mask 3 and the pedestal 5, in the diffusion brazier 900 ℃, 4MPa down insulation spread connection in 1 hour, obtained web member 6.The absolute ethyl alcohol that with mass ratio is 2:1 mixes with the HA powder, adopts ultrasonic or whisking appliance is mixed and made into slurry, evenly is painted on the nickel foil surface of web member 6, and coat thickness reaches 0.1-0.3mm, obtains prefab.This prefab is placed vacuum oven, be warming up to 1050 ℃ stage by stage, be incubated furnace cooling after 1 hour with the speed of 10 ° of C/min.
Through test, prepared composite gradient cladding composition is HA/Ti
2Ni, mean thickness are 0.25mm, and compound coating and titanium alloy surface form the chemical combination key, and the bonding strength that on average stretches reaches 88MPa.
Embodiment 2: at special-shaped Ti-6Al-4V substrate surface preparation HA complex gradient coating.
For special-shaped Ti-6Al-4V titanium alloy 1,,, behind acetone, alcohol ultrasonic cleaning 20min, rinse well to remove surface oxide layer with sand papering with redistilled water, and oven dry.Place plating tank as negative electrode titanium alloy 1, carry out electronickelling, obtain coating spare 2.The absolute ethyl alcohol that with mass ratio is 2:1 mixes with the HA powder, adopts ultrasonic or whisking appliance is mixed and made into slurry, evenly is painted on coating spare 2 surfaces, and coat thickness reaches 0.05-0.2mm, obtains prefab 3.This prefab 3 is placed vacuum oven, be warming up to 1050 ℃ stage by stage, be incubated furnace cooling after 1 hour with the speed of 10 ° of C/min.
Through test, prepared composite gradient cladding composition is HA/Ti
2Ni, mean thickness are 0.13mm, and compound coating and titanium alloy surface form the chemical combination key, and the bonding strength that on average stretches reaches 50MPa.
Embodiment 3: at plate shaped Ti-4Al-2.5Fe substrate surface preparation HA complex gradient coating.
Choose plate shaped Ti-4Al-2.5Fe titanium alloy 1, titanium alloy 1 (on mill the groove that dark 1mm, length and width are 50mm,,, behind acetone, alcohol ultrasonic cleaning 20min, rinse well to remove surface oxide layer with sand papering, and oven dry with redistilled water.Choose the nickel foil 4 that is of a size of 0.1mm * 50mm * 50mm, it is tiled in the groove of titanium alloy 1, place between seaming chuck 2, heat insulation solder mask 3 and the pedestal 5, in the diffusion brazier 900 ℃, 4MPa down insulation spread connection in 1 hour, obtained web member 6.The absolute ethyl alcohol that with mass ratio is 2:1 mixes with the HA powder, adopts ultrasonic or whisking appliance is mixed and made into slurry, evenly is painted on the nickel foil surface of web member 6, and coat thickness reaches 0.1-0.3mm, obtains prefab.This prefab is placed vacuum oven, be warming up to 1050 ℃ stage by stage, be incubated furnace cooling after 1 hour with the speed of 10 ° of C/min.
Through test, prepared composite gradient cladding composition is HA/Ti
2Ni, mean thickness are 0.28mm, and compound coating and titanium alloy surface form the chemical combination key, and the bonding strength that on average stretches reaches 54MPa.
Embodiment 4: at special-shaped Ti-4Al-2.5Fe substrate surface preparation HA complex gradient coating.
For special-shaped Ti-4Al-2.5Fe titanium alloy 1,,, behind acetone, alcohol ultrasonic cleaning 20min, rinse well to remove surface oxide layer with sand papering with redistilled water, and oven dry.Place plating tank as negative electrode titanium alloy 1, carry out electronickelling, obtain coating spare 2.The absolute ethyl alcohol that with mass ratio is 2:1 mixes with the HA powder, adopts ultrasonic or whisking appliance is mixed and made into slurry, evenly is painted on coating spare 2 surfaces, and coat thickness reaches 0.05-0.2mm, obtains prefab 3.This prefab 3 is placed vacuum oven, be warming up to 1050 ℃ stage by stage, be incubated furnace cooling after 1 hour with the speed of 10 ° of C/min.
Through test, prepared composite gradient cladding composition is HA/Ti
2Ni, mean thickness are 0.09mm, and compound coating and titanium alloy surface form the chemical combination key, and the bonding strength that on average stretches reaches 40MPa.
Embodiment 5: at plate shaped Ti-6Al-7Nb substrate surface preparation HA complex gradient coating.
Choose plate shaped Ti-6Al-7Nb titanium alloy 1, titanium alloy 1 (on mill the groove that dark 1mm, length and width are 50mm,,, behind acetone, alcohol ultrasonic cleaning 20min, rinse well to remove surface oxide layer with sand papering, and oven dry with redistilled water.Choose the nickel foil 4 that is of a size of 0.1mm * 50mm * 50mm, it is tiled in the groove of titanium alloy 1, place between seaming chuck 2, heat insulation solder mask 3 and the pedestal 5, in the diffusion brazier 900 ℃, 4MPa down insulation spread connection in 1 hour, obtained web member 6.The absolute ethyl alcohol that with mass ratio is 2:1 mixes with the HA powder, adopts ultrasonic or whisking appliance is mixed and made into slurry, evenly is painted on the nickel foil surface of web member 6, and coat thickness reaches 0.1-0.3mm, obtains prefab.This prefab is placed vacuum oven, be warming up to 1050 ℃ stage by stage, be incubated furnace cooling after 1 hour with the speed of 10 ° of C/min.
Through test, prepared composite gradient cladding composition is HA/Ti
2Ni, mean thickness are 0.3mm, and compound coating and titanium alloy surface form the chemical combination key, and the bonding strength that on average stretches reaches 74MPa.
Embodiment 4: at special-shaped Ti-6Al-7Nb substrate surface preparation HA complex gradient coating.
For special-shaped Ti-6Al-7Nb titanium alloy 1,,, behind acetone, alcohol ultrasonic cleaning 20min, rinse well to remove surface oxide layer with sand papering with redistilled water, and oven dry.Place plating tank as negative electrode titanium alloy 1, carry out electronickelling, obtain coating spare 2.The absolute ethyl alcohol that with mass ratio is 2:1 mixes with the HA powder, adopts ultrasonic or whisking appliance is mixed and made into slurry, evenly is painted on coating spare 2 surfaces, and coat thickness reaches 0.05-0.2mm, obtains prefab 3.This prefab 3 is placed vacuum oven, be warming up to 1050 ℃ stage by stage, be incubated furnace cooling after 1 hour with the speed of 10 ° of C/min.
Through test, prepared composite gradient cladding composition is HA/Ti
2Ni, mean thickness are 0.1mm, and compound coating and titanium alloy surface form the chemical combination key, and the bonding strength that on average stretches reaches 53MPa.
Claims (3)
1. one kind prepares the method for Win 40350 complex gradient coating at titanium alloy surface, it is characterized in that comprising the steps:
(a) titanium alloy surface to be prepared is polished with the removal surface oxide layer, and clean, dry;
(b) prepare one deck pure metal Ni at titanium alloy surface;
(c) use mass ratio to be mixed and made into slurry as absolute ethyl alcohol and the HAp powder of 2:1, evenly be coated in the titanium alloy surface that has prepared the Ni layer, coat thickness reaches 0.1-0.3mm; Put into vacuum oven after the drying; Speed with 10 ° of C/min is warming up to 1050 ℃ stage by stage, is incubated after 1 hour, and stove is cold.
2. the method for preparing the Win 40350 complex gradient coating at titanium alloy surface according to claim 1; It is characterized in that: described step (2) is that the Ni paper tinsel of 0.05-0.3mm places on the titanium alloy plate with thickness, adopts diffusion welding method to be incubated 1 hour down at 900 ℃, 4MPa pressure.
3. according to claim 1ly prepare the method for Win 40350 complex gradient coating at titanium alloy surface, it is characterized in that: described step (2) adopts electro-plating method to introduce the Ni layer at titanium alloy surface, and the Ni layer thickness is 0.005-0.08mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106132596A (en) * | 2014-01-15 | 2016-11-16 | 西门子能源公司 | The material utilizing powder and paper tinsel deposits |
| CN106947970A (en) * | 2017-03-23 | 2017-07-14 | 华东理工大学 | A kind of titanium or titanium alloy surface prepares fine grain Ti3The method and apparatus of Al/TiN gradient coatings |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1629364A (en) * | 2003-12-17 | 2005-06-22 | 中南大学 | Preparation method of hydroxyapatite/titanium oxide gradient coating |
| CN101327337A (en) * | 2008-07-17 | 2008-12-24 | 西北工业大学 | Method for preparing titanium alloy/hydroxylapatite gradient composite coating |
| CN101352772A (en) * | 2008-08-13 | 2009-01-28 | 西北工业大学 | Diffusion welding method of TiAl/Nb based alloy and Ni based high-temperature alloy |
-
2012
- 2012-05-22 CN CN2012101601891A patent/CN102650048A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1629364A (en) * | 2003-12-17 | 2005-06-22 | 中南大学 | Preparation method of hydroxyapatite/titanium oxide gradient coating |
| CN101327337A (en) * | 2008-07-17 | 2008-12-24 | 西北工业大学 | Method for preparing titanium alloy/hydroxylapatite gradient composite coating |
| CN101352772A (en) * | 2008-08-13 | 2009-01-28 | 西北工业大学 | Diffusion welding method of TiAl/Nb based alloy and Ni based high-temperature alloy |
Non-Patent Citations (1)
| Title |
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| 李亚鹏等: "医用金属表面羟基磷灰石复合涂层研究进展", 《材料导报》, vol. 25, no. 4, 30 April 2011 (2011-04-30), pages 80 - 84 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106132596A (en) * | 2014-01-15 | 2016-11-16 | 西门子能源公司 | The material utilizing powder and paper tinsel deposits |
| CN106947970A (en) * | 2017-03-23 | 2017-07-14 | 华东理工大学 | A kind of titanium or titanium alloy surface prepares fine grain Ti3The method and apparatus of Al/TiN gradient coatings |
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Application publication date: 20120829 |