CN108785750B - Hydroxyapatite gradient structure coating and preparation method thereof - Google Patents
Hydroxyapatite gradient structure coating and preparation method thereof Download PDFInfo
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- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
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- C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
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Abstract
A hydroxyapatite gradient structure coating and a preparation method thereof relate to the relevant field of biomedical material artificial implants. The invention discloses a hydroxyapatite gradient structure coating, which comprises: a base layer in contact with the substrate and a surface layer overlying the base layer. The preparation steps of the gradient structure coating are that an atmospheric plasma spraying device is adopted to prepare a hydroxyapatite coating on the bottom layer on a preheated substrate and prepare a surface layer on the bottom layer. The gradient structure coating prepared by the method has better biological property and mechanical property, and the coating and the matrix have higher bonding strength.
Description
The technical field is as follows:
the invention relates to the field of biomedical material artificial implants, in particular to a hydroxyapatite coating with a gradient structure and a preparation method thereof.
Background art:
the hydroxyapatite coating is prepared on the surface of the titanium alloy matrix by adopting the atmospheric plasma spraying technology, can give full play to the respective advantages of the metal matrix and the HA biological ceramic material, HAs good biocompatibility and good mechanical property, and is widely applied to the field of biomedical artificial implants.
However, the problem that the requirements of mechanical property and biological property are mutually contradictory exists in the practical application process of the plasma spraying HA coating. After being implanted into a human body, the HA coating is required to induce the growth of bone tissues as soon as possible, and the surface of the coating is expected to have a loose and porous structure and contain a certain amorphous metastable phase, so that the HA coating can be quickly dissolved after being implanted to induce the growth of osteoblasts. Meanwhile, in order to meet the requirement of certain mechanical property, the coating has a compact structure, good bonding property with a matrix and high crystallinity, so that the coating can be kept stable for a long time in service. Therefore, the coating with a single structure is difficult to solve the contradiction between the mechanical property and the biological property.
Meanwhile, the selection of the coating with a loose structure is difficult in the actual preparation process, and the coating with the loose structure needs particles with a lower melting state, but the mechanical property of the coating is influenced. The preparation of the coating with a compact structure requires that the particles are fully melted, but excessive decomposition phases and amorphous phases are generated in the coating, so that the long-term service stability of the coating is reduced.
While much research has focused on the incorporation of tough second phases, such as TiO, into hydroxyapatite powders2、ZrO2And preparing a composite or functionally gradient coating to balance the mechanical property and the biological property of the coating. However, although such a gradient coating HAs a certain disadvantage in that the mechanical properties of the coating can be improved to a certain extent, when the coating is peeled off after a long-term service, the particles as the composite component cannot be decomposed and absorbed in vivo like the HA coating, which may affect the health of the human body.
Therefore, the invention balances the contradiction between the requirements by preparing the gradient structure coating on the surface of the implant, namely the coating has compact bottom layer structure, high crystallinity and loose surface layer structure and has certain amorphous phase content. The crystallinity and the bonding strength of the coating are obviously improved by adjusting the spraying process parameters and the matrix temperature, and the requirements on the biological performance and the mechanical performance of the coating under the actual service condition can be further met.
The invention content is as follows:
the invention aims to provide a hydroxyapatite gradient structure coating and a preparation method thereof, so as to meet the requirements on the biological performance and the mechanical performance of the coating under the actual service condition.
The invention provides a hydroxyapatite gradient structure coating, which comprises a bottom layer (1) connected with a substrate and a surface layer (2) on the bottom layer (1); wherein, the bottom layer (1) is a hydroxyapatite coating with the porosity of 0.98-1.31% and the crystallinity of 63.42-71.43%; the surface layer (2) is a hydroxyapatite coating with the porosity of 8.21-8.82% and the amorphous phase content of 10.12-14.35%; the thickness of the bottom layer (1) is 140-160 μm; the thickness of the surface layer (2) is 40-60 μm, and the bonding strength of the gradient structure coating is not lower than 30 MPa.
The preparation method of the hydroxyapatite gradient structure coating provided by the invention comprises the following steps:
1) hydroxyapatite with the particle size range of 15-63 mu m and the purity of more than 99.5 percent is selected as spraying powder, and the powder is dried in an oven for 2 hours at the temperature of 90 ℃ before spraying. The base material is TC4 alloy, the surface of the base material is cleaned by absolute ethyl alcohol before spraying, the surface of the base material is subjected to sand blasting coarsening treatment by 16-22 meshes of brown corundum under the pressure of 0.5MPa, and then the surface is cleaned by the absolute ethyl alcohol.
2) Spraying of the bottom layer (1): spraying the spraying powder in the step 1) onto the preheated substrate by adopting atmospheric plasma spraying equipment, wherein the spraying process parameters are as follows: the working current is 400A, the working voltage is 60V, the argon flow is 28-30L/min, the spraying distance is 110mm, the temperature of the substrate before spraying is 300-;
3) spraying of the surface layer (2): spraying the spraying powder in the step 1) onto the preheated bottom layer (1) by adopting atmospheric plasma spraying equipment, wherein the spraying process parameters are as follows: the working current is 400A, the working voltage is 40V, the argon flow is 40-42L/min, the spraying distance is 110mm, the temperature of the substrate before spraying is 300-.
The invention has the following beneficial effects:
compared with a hydroxyapatite coating with a single structure, the prepared gradient structure coating has better biological property and mechanical property, can better promote the growth of bone tissues after being implanted into a human body, and has better stability in long-term service. Compared with a composite coating added with a second phase, the composite coating has higher safety to human body under the condition of similar performance. In addition, the method provided by the invention has higher powder utilization rate in the process of preparing the coating.
Description of the drawings:
FIG. 1 is a schematic view of the coating structure, wherein s is a substrate, 1 is a bottom layer, and 2 is a surface layer.
FIG. 2 is a gradient structure coating of example 1.
The specific implementation mode is as follows:
the technical solution of the present invention will be described in detail with reference to specific embodiments.
The hydroxyapatite powder used in the following examples is commercially available. The particle size of the hydroxyapatite powder is 15-63 μm, and the purity is 99.5%; drying in an oven at 90 ℃ for 2h before spraying. The base material is TC4 alloy, the surface of the base material is cleaned by absolute ethyl alcohol before spraying, the surface of the base material is subjected to sand blasting coarsening treatment by 16-22 meshes of brown corundum under the pressure of 0.5MPa, and then the surface is cleaned by the absolute ethyl alcohol. When the matrix is preheated, the matrix is preheated by using a resistance furnace, and the temperature of the matrix is monitored by using an infrared thermometer.
Example 1:
(1) bottom layer spraying: spraying hydroxyapatite powder on the preheated substrate by adopting atmospheric plasma spraying equipment, wherein the spraying process parameters are as follows: the working current is 400A, the working voltage is 60V, the argon flow is 28L/min, the spraying distance is 110mm, the temperature of the substrate before spraying is 500 ℃, the powder feeding rate is 20g/min, the gun swing speed is 500mm/s, the step is 4mm, the thickness of the obtained coating is 160 mu m, the porosity is 0.98%, and the crystallinity is 71.43%.
(2) Surface layer spraying: spraying hydroxyapatite powder on the preheated bottom layer (1) by adopting an atmosphere plasma spraying device, wherein the spraying process parameters are as follows: the working current is 400A, the working voltage is 40V, the argon flow is 42L/min, the spraying distance is 110mm, the temperature of the substrate is 500 ℃ before spraying, the powder feeding rate is 20g/min, the gun swing speed is 500mm/s, the step is 4mm, the thickness of the obtained coating is 40 mu m, the porosity is 8.82%, and the content of the amorphous phase is 10.12%.
The bonding strength of the gradient structure coating reaches 36.23 MPa.
Example 2:
(1) bottom layer spraying: spraying hydroxyapatite powder on the preheated substrate by adopting atmospheric plasma spraying equipment, wherein the spraying process parameters are as follows: the working current is 400A, the working voltage is 60V, the argon flow is 30L/min, the spraying distance is 110mm, the temperature of the base body before spraying is 300 ℃, the powder feeding rate is 20g/min, the gun swing speed is 500mm/s, the step is 4mm, the thickness of the obtained coating is 140 mu m, the porosity is 1.31%, and the crystallinity is 63.42%.
(2) Surface layer spraying: spraying hydroxyapatite powder on the preheated bottom layer (1) by adopting an atmosphere plasma spraying device, wherein the spraying process parameters are as follows: the working current is 400A, the working voltage is 40V, the argon flow is 40L/min, the spraying distance is 110mm, the temperature of the substrate before spraying is 300 ℃, the powder feeding rate is 20g/min, the gun swing speed is 500mm/s, the step is 4mm, the thickness of the obtained coating is 60 mu m, the porosity is 8.21%, and the content of the amorphous phase is 14.35%.
The bonding strength of the gradient structure coating reaches 32.86 MPa.
Claims (1)
1. A hydroxyapatite gradient structure coating comprises a bottom layer (1) connected with a substrate, and a surface layer (2) arranged on the bottom layer (1); wherein, the bottom layer (1) is a hydroxyapatite coating with the porosity of 0.98-1.31% and the crystallinity of 63.42-71.43%; the surface layer (2) is a hydroxyapatite coating with the porosity of 8.21-8.82% and the amorphous phase content of 10.12-14.35%; the thickness of the bottom layer (1) is 140-160 μm; the thickness of the surface layer (2) is 40-60 μm, and the bonding strength of the gradient structure coating is not lower than 30 MPa;
the preparation method is characterized by comprising the following steps:
1) selecting hydroxyapatite with the particle size range of 15-63 mu m and the purity of more than 99.5 percent as spraying powder, and drying the hydroxyapatite in an oven for 2 hours at 90 ℃ before spraying; the base material is TC4 alloy, the surface of the base material is cleaned by absolute ethyl alcohol before spraying, the surface of the base material is subjected to sand blasting roughening treatment by 16-22 meshes of brown corundum under the pressure of 0.5MPa, and then the surface is cleaned by the absolute ethyl alcohol;
2) spraying of the bottom layer (1): spraying the spraying powder in the step 1) onto the preheated substrate by adopting atmospheric plasma spraying equipment, wherein the spraying process parameters are as follows: the working current is 400A, the working voltage is 60V, the argon flow is 28-30L/min, the spraying distance is 110mm, the temperature of the substrate before spraying is 300-;
3) spraying of the surface layer (2): spraying the spraying powder in the step 1) onto the preheated bottom layer (1) by adopting atmospheric plasma spraying equipment, wherein the spraying process parameters are as follows: the working current is 400A, the working voltage is 40V, the argon flow is 40-42L/min, the spraying distance is 110mm, the temperature of the substrate before spraying is 300-.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101584881A (en) * | 2009-06-26 | 2009-11-25 | 北京工业大学 | Composite hydroxylapatite coating layer and preparing method thereof |
| CN102220551A (en) * | 2011-05-27 | 2011-10-19 | 华南理工大学 | Method for plasma spraying of Ca-P bioactive coating on surface of magnesium alloy |
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| DE3676741D1 (en) * | 1985-05-20 | 1991-02-14 | Sumitomo Chemical Co | METHOD FOR PRODUCING ENDOSSAL IMPLANTS. |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101584881A (en) * | 2009-06-26 | 2009-11-25 | 北京工业大学 | Composite hydroxylapatite coating layer and preparing method thereof |
| CN102220551A (en) * | 2011-05-27 | 2011-10-19 | 华南理工大学 | Method for plasma spraying of Ca-P bioactive coating on surface of magnesium alloy |
Non-Patent Citations (1)
| Title |
|---|
| The Influence of Spray Parameters on the Characteristics of Hydroxyapatite In-Flight Particles, Splats and Coatings by Micro-plasma Spraying;Xiao-mei Liu et al;《Journal of thermal spray technology》;20180202;全文 * |
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