CN113304314A - Porous polyether-ether-ketone-based coating material and preparation method thereof - Google Patents
Porous polyether-ether-ketone-based coating material and preparation method thereof Download PDFInfo
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- CN113304314A CN113304314A CN202110580943.6A CN202110580943A CN113304314A CN 113304314 A CN113304314 A CN 113304314A CN 202110580943 A CN202110580943 A CN 202110580943A CN 113304314 A CN113304314 A CN 113304314A
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- 239000004696 Poly ether ether ketone Substances 0.000 title claims abstract description 144
- 229920002530 polyetherether ketone Polymers 0.000 title claims abstract description 144
- 238000000576 coating method Methods 0.000 title claims abstract description 113
- 239000011248 coating agent Substances 0.000 title claims abstract description 112
- 239000000463 material Substances 0.000 title claims abstract description 112
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 46
- 238000010288 cold spraying Methods 0.000 claims abstract description 29
- 239000000378 calcium silicate Substances 0.000 claims abstract description 25
- 229910052918 calcium silicate Inorganic materials 0.000 claims abstract description 25
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims abstract description 25
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims abstract description 22
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 19
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 19
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 claims abstract 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 40
- 238000005406 washing Methods 0.000 claims description 40
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 34
- 239000007789 gas Substances 0.000 claims description 26
- 238000005507 spraying Methods 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 24
- 238000000151 deposition Methods 0.000 claims description 22
- 239000012153 distilled water Substances 0.000 claims description 20
- 238000005516 engineering process Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 15
- 239000001307 helium Substances 0.000 claims description 10
- 229910052734 helium Inorganic materials 0.000 claims description 10
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 10
- 230000010355 oscillation Effects 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims 2
- 239000000758 substrate Substances 0.000 abstract description 16
- 210000000988 bone and bone Anatomy 0.000 abstract description 13
- 239000002131 composite material Substances 0.000 abstract description 7
- 238000010883 osseointegration Methods 0.000 abstract description 6
- 238000002513 implantation Methods 0.000 abstract description 2
- 239000011812 mixed powder Substances 0.000 description 15
- 239000011159 matrix material Substances 0.000 description 10
- 239000007943 implant Substances 0.000 description 9
- 230000008021 deposition Effects 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- 238000003760 magnetic stirring Methods 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 238000000498 ball milling Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000004071 biological effect Effects 0.000 description 3
- 230000000975 bioactive effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000004372 laser cladding Methods 0.000 description 1
- 210000003041 ligament Anatomy 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000000399 orthopedic effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/14—Macromolecular materials
- A61L27/18—Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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- A61L27/56—Porous materials, e.g. foams or sponges
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Abstract
本发明公开了一种多孔聚醚醚酮基涂层材料及其制备方法，对聚醚醚酮表面进行处理，在聚醚醚酮表面形成多孔结构，采用冷喷涂技术或真空冷喷涂技术，将可降解材料粉末沉积在聚醚醚酮的多孔结构表面上，得到所述的多孔聚醚醚酮基复合材料；其中，可降解材料粉末采用羟基磷灰石、硅酸钙和β‑磷酸三钙中的一种或多种；本发明通过将聚醚醚酮的表面处理为多孔结构，有效提高了涂层与聚醚醚酮基材的接触面积，采用冷喷涂或真空冷喷涂，能够确保可降解材料进入多孔结构的内部，有效增加涂层和聚醚醚酮基材的结合强度；涂层采用可降解材料，可引导或诱导新生骨组织长入多孔结构内部，能够大大增强骨/植入物界面的骨整合性和稳定性。
The invention discloses a porous polyetheretherketone-based coating material and a preparation method thereof. The surface of the polyetheretherketone is treated to form a porous structure on the surface of the polyetheretherketone. The degradable material powder is deposited on the surface of the porous structure of polyether ether ketone to obtain the porous polyether ether ketone-based composite material; wherein, the degradable material powder adopts hydroxyapatite, calcium silicate and β-tricalcium phosphate One or more of the following; the present invention effectively improves the contact area between the coating and the polyetheretherketone substrate by treating the surface of the polyetheretherketone into a porous structure, and cold spraying or vacuum cold spraying can ensure the The degradable material enters the interior of the porous structure, which effectively increases the bonding strength of the coating and the PEEK substrate; the coating adopts degradable material, which can guide or induce the new bone tissue to grow into the porous structure, which can greatly enhance the bone/implantation Osseointegration and stability of the physical interface.
Description
Technical Field
The invention belongs to the technical field of coating materials, and particularly relates to a porous polyether-ether-ketone-based coating material and a preparation method thereof.
Background
The common orthopedic clinical internal implant recovers the integrity of joints and bones, the common internal implant material is a metal material, the elastic modulus of the metal material is far higher than that of normal bone tissues, and the stress shielding effect is easy to generate to cause the failure of the internal implant; polyetheretherketone (PEEK) is a thermoplastic with an elastic modulus close to that of human bone tissue, is chemically stable, biocompatible, and highly machinable, and has been used to prepare spinal interbody fusion cages and anchor anchors for ligament reconstruction; however, PEEK lacks biological activity and osseointegration is inefficient after implantation in vivo; thus, there is a need for modification of PEEK to improve its bioactivity and osteointegration.
In the prior art, methods commonly used for PEEK modification include: surface treatment, preparation of composites and surface coatings; among them, the surface treatment has problems: the surface of the activated material is not stable enough in the operation process and the physiological environment and is greatly influenced by the experimental conditions; problems with the preparation of the complexes: the mechanical properties of the PEEK material are influenced to a certain extent by the excessively high doping proportion of the bioactive material; the surface coating does not substantially affect the mechanical properties of PEEK, and the surface coating is coated with a large amount of bioactive materials to greatly improve the bioactivity of the PEEK, but the bonding strength of the coating and a substrate needs to be concerned.
The method adopted when preparing the biological coating usually comprises the processes of thermal spraying, plasma deposition, laser cladding and the like, but the processes often have high temperature processes, so that not only can the coating generate cracks and holes, but also the decomposition and phase change of the biological coating material can be caused, and the uniformity and the stability of the coating are poor; therefore, how to prepare a coating with degradable function and good bioactivity on the surface of the PEEK implant still belongs to a great technical problem.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a porous polyether-ether-ketone-based coating material and a preparation method thereof, aiming at solving the technical problems that when a surface coating is used for modifying polyether-ether-ketone in the prior art, the bonding strength of the coating and a base material is low, the stability is poor and the difficulty in the preparation process is high.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a preparation method of a porous polyether-ether-ketone-based coating material, which comprises the following steps:
step 2, depositing degradable material powder on the surface of the porous structure of the polyetheretherketone by adopting a cold spraying technology or a vacuum cold spraying technology to obtain the porous polyetheretherketone-based coating material;
wherein, the degradable material powder adopts one or more of hydroxyapatite, calcium silicate and beta-tricalcium phosphate.
Further, in step 1, the surface of the polyetheretherketone is treated, specifically:
and (3) soaking the polyether-ether-ketone in concentrated sulfuric acid for 4-6min, then taking out the soaked polyether-ether-ketone, washing to remove residual sulfuric acid, and airing to obtain the polyether-ether-ketone with the porous structure surface.
Further, when the soaked polyether-ether-ketone is washed, firstly, distilled water is adopted for repeatedly washing for 3-5 times; then, under the ultrasonic oscillation environment, acetone is adopted for washing to remove residual sulfuric acid; and repeatedly washing by using distilled water to remove residual acetone.
Further, in the step 2, the process parameters for depositing the degradable material powder by adopting the vacuum cold spraying technology are as follows:
spraying under vacuum environment and room temperature, wherein the working gas is one of helium, nitrogen and compressed air, the pressure of the working gas is 0.1-1.0MPa, and the spraying distance is 4-10 mm.
Further, in step 2, the process parameters for performing the degradable material powder deposition by using the cold spraying technology are as follows:
spraying under the conditions of atmospheric environment and room temperature, wherein the working gas is one of helium, nitrogen and compressed air, the pressure of the working gas is 0.1-1.0MPa, and the spraying distance is 4-10 mm.
Further, in step 2, the particle size of the degradable material powder is 0.1-10 μm.
Further, in step 2, the deposition thickness of the degradable material powder is 2-10 μm.
The invention also provides a porous polyether-ether-ketone-based coating material which is prepared by the preparation method of the porous polyether-ether-ketone-based coating material.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a preparation method of a porous polyether-ether-ketone-based coating material, which is characterized in that the surface of polyether-ether-ketone is processed into a porous structure, and the surface of the porous structure is coated, so that the contact area between the coating and a polyether-ether-ketone substrate is effectively increased, the binding force between the coating and the polyether-ether-ketone substrate is increased, and the stability of a composite coating is ensured; by adopting cold spraying or vacuum cold spraying, the degradable material can be ensured to enter the porous structure, the bonding strength of the coating and the polyether-ether-ketone base material is effectively increased, and the thermal degradation of the polyether-ether-ketone base material and coating particles is avoided; the coating is made of degradable materials, and can guide or induce new bone tissues to grow into the porous structure along with the gradual degradation of the coating materials, so that the osseointegration and stability of a bone-implant interface can be greatly enhanced, the preparation process is simple and practical, the cost is low, and the industrial production is convenient to put into.
Furthermore, the degradable material is one or more of hydroxyapatite, calcium silicate and beta-tricalcium phosphate, and the hydroxyapatite, the calcium silicate and the beta-tricalcium phosphate all have good biological activity.
Furthermore, a porous structure can be formed on the surface of the polyetheretherketone by treating the surface of the polyetheretherketone by concentrated sulfuric acid, the formation of the porous structure is favorable for the coating material to enter the inside of the pores, the combination of the coating material and the matrix is firmer by utilizing the increase of the contact area, the treatment process by the concentrated sulfuric acid is simple, and the operation is convenient.
Furthermore, the vacuum cold spraying technology or the cold spraying technology has the advantages of large coating area in a short time, strong coating binding force, uniform coating, capability of avoiding thermal degradation of matrix and coating particles by low-temperature environment operation and the like.
Furthermore, the particle size of the degradable material powder is 0.1-10 μm, which is beneficial to accelerating the powder particles to the surface of the substrate by airflow, ensures the uniformity of powder deposition and ensures the stability of the material surface in the using process.
Furthermore, the deposition thickness of the degradable material powder is 2-10 μm, which ensures that the coating on the surface of the implant polyetheretherketone can be effectively degraded in a living body, is convenient for guiding or inducing the growth of new bone tissues into a porous structure, and greatly enhances the osseointegration and stability of the bone/implant interface.
The invention also provides a porous polyether-ether-ketone-based coating material, which is characterized in that a surface coating is subjected to cold spraying or vacuum cold spraying on the porous surface of polyether-ether-ketone, so that the aim of improving the biological activity of the polyether-ether-ketone without influencing the biomechanical property of the polyether-ether-ketone is fulfilled on the premise of ensuring strong binding force of the coating; the porous structure on the surface of the polyetheretherketone is beneficial for the coating material to enter the porous structure, on one hand, the combination of the coating material and the matrix is firmer due to the increase of the contact area, on the other hand, the new bone tissue can be guided or induced to grow into the porous structure along with the gradual degradation of the coating material, and the osseointegration and stability of the bone/implant interface can be greatly enhanced.
Drawings
FIG. 1 is a flow chart of a preparation method of a porous polyetheretherketone-based coating material according to the present invention
FIG. 2 is a microscopic morphology of the calcium silicate powder of example 1;
FIG. 3 is a microscopic view of a porous PEEK-based coating material prepared in example 1;
FIG. 4 is a microscopic morphology of a mixed powder of calcium silicate and β -tricalcium phosphate of example 2;
fig. 5 is a microstructure diagram of the porous peek-based coating material prepared in example 2.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects of the present invention more apparent, the following embodiments further describe the present invention in detail. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in the attached figure 1, the invention provides a preparation method of a porous polyether-ether-ketone-based coating material, which comprises the following steps:
The method specifically comprises the following steps of treating the surface of the polyetheretherketone:
soaking the polyether-ether-ketone in concentrated sulfuric acid for 4-6min, taking out the soaked polyether-ether-ketone, washing to remove residual sulfuric acid, and airing to obtain the polyether-ether-ketone with the porous structure surface; when the soaked polyether-ether-ketone is washed, firstly, distilled water is adopted to repeatedly wash for 3-5 times; then, under the ultrasonic oscillation environment, acetone is adopted for washing to remove residual sulfuric acid; and repeatedly washing by using distilled water to remove residual acetone.
And 2, depositing degradable material powder on the surface of the porous structure of the polyetheretherketone by adopting a cold spraying technology or a vacuum cold spraying technology to obtain the porous polyetheretherketone-based coating material.
Wherein, the degradable material powder adopts one or more of hydroxyapatite, calcium silicate and beta-tricalcium phosphate.
In the invention, the technological parameters for depositing the degradable material powder by adopting the vacuum cold spraying technology are as follows:
spraying under the conditions of vacuum environment and room temperature, wherein the pressure of a vacuum chamber is 180-220 Pa; the working gas is one of helium, nitrogen and compressed air, the pressure of the working gas is 0.1-1.0MPa, the spraying distance is 4-10mm, the particle size of the degradable material powder is 0.1-10 mu m, and the deposition thickness is 2-10 mu m.
The technological parameters for the degradable material powder deposition by adopting the cold spraying technology are as follows:
spraying under the conditions of atmospheric environment and room temperature, wherein one or more of helium, nitrogen and compressed air are adopted as working gas, the pressure of the working gas is 0.1-1.0MPa, the spraying distance is 4-10mm, the particle size of the degradable material powder is 0.1-10 mu m, and the deposition thickness is 2-10 mu m.
The invention provides a porous polyether-ether-ketone-based coating material and a preparation method thereof, wherein the surface of polyether-ether-ketone is processed into a porous structure, and the surface of the porous structure is coated, so that the contact area between the coating and a polyether-ether-ketone substrate is effectively increased, the binding force between the coating and the polyether-ether-ketone substrate is increased, and the stability of a composite coating is ensured; by adopting cold spraying or vacuum cold spraying, the degradable material can be ensured to enter the porous structure, the bonding strength of the coating and the polyether-ether-ketone base material is effectively increased, and the thermal degradation of the polyether-ether-ketone base material and coating particles is avoided; when the porous polyether ether ketone-based composite material is applied to bone repair, the coating is made of degradable materials, so that new bone tissues can be guided or induced to grow into the porous structure along with gradual degradation of the coating materials, the osseointegration and stability of a bone/implant interface can be greatly enhanced, the preparation process is simple and practical, the cost is low, and the porous polyether ether ketone-based composite material is convenient to put into industrial production.
Example 1
Step 2, depositing degradable material powder on the surface of the porous structure of the polyetheretherketone by adopting a vacuum cold spraying technology to obtain the porous polyetheretherketone-based coating material; wherein the degradable material powder is calcium silicate powder, the morphology of the calcium silicate powder is shown in figure 2, and the particle size of the calcium silicate powder is 0.1-10 μm.
In this example 1, spraying is performed under vacuum environment and room temperature, helium is used as working gas, and the pressure of the working gas is 0.1 MPa; the vacuum environment is adopted in a vacuum chamber, and the pressure of the vacuum chamber is 200 Pa; the spraying distance was 5mm and the deposit thickness was 6 μm.
As shown in the attached figure 3, the microscopic structure of the porous PEEK-based coating material prepared in the example 1 is shown in the attached figure 3, and it can be seen from the attached figure 3 that the coating is uniformly distributed on the surface of the matrix, the dispersibility of the coating particles is good, and the bonding between the coating and the matrix is good.
Example 2
Embodiment 2 provides a porous polyetheretherketone-based coating material and a method for preparing the same, comprising the steps of:
Step 2, depositing degradable material powder on the surface of the porous structure of the polyetheretherketone by adopting a vacuum cold spraying technology to obtain the porous polyetheretherketone-based coating material; wherein, the degradable material powder adopts mixed powder of calcium silicate and beta-tricalcium phosphate; wherein, in the mixed powder of calcium silicate and beta-tricalcium phosphate, the mass ratio of the calcium silicate to the beta-tricalcium phosphate is 1:1, and the calcium silicate and the beta-tricalcium phosphate are mixed by adopting a ball milling process; FIG. 4 is a graph showing the morphology of the mixed powder of calcium silicate and β -tricalcium phosphate in example 2, wherein the particle size of the mixed powder of calcium silicate and β -tricalcium phosphate is 0.1-10 μm.
In the embodiment 2, spraying is performed under the conditions of vacuum environment and room temperature, nitrogen is used as working gas, and the pressure of the working gas is 0.5 MPa; the vacuum environment is adopted in a vacuum chamber, and the pressure of the vacuum chamber is 200 Pa; the spraying distance was 4mm and the deposit thickness was 4 μm.
As shown in figure 5, the microstructure of the porous polyether ether ketone based composite material prepared in example 2 is shown in figure 5, and it can be seen from figure 5 that the coating is uniformly distributed on the surface of the matrix, the dispersibility of the coating particles is good, and the bonding between the coating and the matrix is good.
Example 3
Embodiment 3 provides a porous polyetheretherketone-based coating material and a method for preparing the same, comprising the steps of:
Step 2, depositing degradable material powder on the surface of the porous structure of the polyetheretherketone by adopting a cold spraying technology to obtain the porous polyetheretherketone-based coating material; wherein, the degradable material powder adopts mixed powder of calcium silicate and hydroxyapatite; wherein, in the mixed powder of calcium silicate and hydroxyapatite, the mass ratio of calcium silicate to hydroxyapatite is 1:1, and the calcium silicate and hydroxyapatite are mixed by adopting a ball milling process; the mixed powder has a particle size of 0.1-10 μm.
In the embodiment 3, spraying is performed at room temperature, helium is used as working gas, and the pressure of the working gas is 0.8 MPa; the spraying distance was 10mm and the deposit thickness was 4 μm.
The coating of the porous polyether-ether-ketone-based coating material prepared in the embodiment 3 is uniformly distributed on the surface of the matrix, the dispersibility of coating particles is good, and the combination between the coating and the matrix is good.
Example 4
Embodiment 4 provides a porous polyetheretherketone-based coating material and a method for preparing the same, comprising the steps of:
Step 2, depositing degradable material powder on the surface of the porous structure of the polyetheretherketone by adopting a cold spraying technology to obtain the porous polyetheretherketone-based coating material; the degradable material powder is mixed powder of hydroxyapatite and beta-tricalcium phosphate, wherein the mass ratio of the hydroxyapatite to the beta-tricalcium phosphate in the mixed powder of the hydroxyapatite and the beta-tricalcium phosphate is 1:1, and the degradable material powder is obtained by mixing through a ball milling process; the mixed powder has a particle size of 0.1-10 μm.
In the embodiment 4, spraying is performed at room temperature, helium is used as working gas, and the pressure of the working gas is 1.0 MPa; the spraying distance was 4mm and the deposit thickness was 10 μm.
The coating of the porous polyetheretherketone-based coating material prepared in example 4 was uniformly distributed on the surface of the substrate, the particles of the coating were well dispersed, and the coating and the substrate were well bonded.
Example 5
Embodiment 5 provides a porous polyetheretherketone-based coating material and a method for preparing the same, comprising the steps of:
Step 2, depositing degradable material powder on the surface of the porous structure of the polyetheretherketone by adopting a vacuum cold spraying technology to obtain the porous polyetheretherketone-based coating material; wherein, the degradable material powder is hydroxyapatite mixed powder; wherein the particle size of the hydroxyapatite is 0.1-10 μm; spraying is carried out under the conditions of vacuum environment and room temperature, nitrogen is adopted as working gas, and the pressure of the working gas is 0.1 MPa; the vacuum environment is adopted in a vacuum chamber, and the pressure of the vacuum chamber is 180 Pa; the spraying distance was 7mm and the deposit thickness was 2 μm.
The coating of the porous polyetheretherketone-based coating material prepared in example 5 was uniformly distributed on the surface of the substrate, the particles of the coating were well dispersed, and the bonding between the coating and the substrate was good.
Example 6
Embodiment 5 provides a porous polyetheretherketone-based coating material and a method for preparing the same, comprising the steps of:
Step 2, depositing degradable material powder on the surface of the porous structure of the polyetheretherketone by adopting a vacuum cold spraying technology to obtain the porous polyetheretherketone-based coating material; wherein the degradable material powder adopts beta-tricalcium phosphate powder; wherein the grain diameter of the beta-tricalcium phosphate is 0.1-10 mu m; spraying is carried out under the conditions of vacuum environment and room temperature, helium is used as working gas, and the pressure of the working gas is 0.8 MPa; the vacuum environment is adopted in a vacuum chamber, and the pressure of the vacuum chamber is 220 Pa; the spraying distance was 10mm and the deposit thickness was 6 μm.
The coating of the porous polyetheretherketone-based coating material prepared in example 6 was uniformly distributed on the surface of the substrate, the particles of the coating were well dispersed, and the coating and the substrate were well bonded.
Example 7
Embodiment 7 provides a porous polyetheretherketone-based coating material and a method for preparing the same, comprising the steps of:
Step 2, depositing degradable material powder on the surface of the porous structure of the polyetheretherketone by adopting a cold spraying technology to obtain the porous polyetheretherketone-based coating material; wherein, the degradable material powder is mixed powder of calcium silicate, hydroxyapatite and beta-tricalcium phosphate; wherein, in the mixed powder of calcium silicate, hydroxyapatite and beta-tricalcium phosphate, the mass ratio of the calcium silicate to the hydroxyapatite to the beta-tricalcium phosphate is 1:1:1, and the calcium silicate to the hydroxyapatite and the beta-tricalcium phosphate are mixed by adopting a ball milling process to obtain the calcium silicate-beta-tricalcium phosphate powder; the mixed powder has a particle size of 0.1-10 μm.
In this example 7, spraying is performed at room temperature, and compressed air is used as working gas, wherein the pressure of the working gas is 0.1 MPa; the spraying distance was 6mm and the deposit thickness was 8 μm.
The coating of the porous polyetheretherketone-based coating material prepared in example 7 was uniformly distributed on the surface of the substrate, the particles of the coating were well dispersed, and the bonding between the coating and the substrate was good.
The porous polyether-ether-ketone-based coating material disclosed by the invention is a coating technology for coating accelerated powder particles onto the surface of a matrix through air flow in cold spraying or vacuum cold spraying, and the coating is established through the shaping deformation of the particles during impact.
The above-described embodiment is only one of the embodiments that can implement the technical solution of the present invention, and the scope of the present invention is not limited by the embodiment, but includes any variations, substitutions and other embodiments that can be easily conceived by those skilled in the art within the technical scope of the present invention disclosed.
Claims (8)
1. The preparation method of the porous polyether-ether-ketone-based coating material is characterized by comprising the following steps of:
step 1, processing the surface of polyether-ether-ketone to form a porous structure on the surface of the polyether-ether-ketone to obtain the polyether-ether-ketone with the porous structure surface;
step 2, depositing degradable material powder on the surface of the porous structure of the polyetheretherketone by adopting a cold spraying technology or a vacuum cold spraying technology to obtain the porous polyetheretherketone-based coating material; wherein, the degradable material powder adopts one or more of hydroxyapatite, calcium silicate and beta-tricalcium phosphate.
2. The method for preparing a porous PEEK-based coating material according to claim 1, wherein the treatment process of the surface of the PEEK in step 1 specifically comprises:
and (3) soaking the polyether-ether-ketone in concentrated sulfuric acid for 4-6min, then taking out the soaked polyether-ether-ketone, washing to remove residual sulfuric acid, and airing to obtain the polyether-ether-ketone with the porous structure surface.
3. The method for preparing a porous PEEK-based coating material according to claim 2, wherein the soaked PEEK is washed by repeatedly washing with distilled water for 3-5 times; then, under the ultrasonic oscillation environment, acetone is adopted for washing to remove residual sulfuric acid; and repeatedly washing by using distilled water to remove residual acetone.
4. The method for preparing a porous polyetheretherketone-based coating material according to claim 1, wherein in step 2, the process parameters for depositing the degradable material powder by using the vacuum cold spray technique are as follows:
spraying under vacuum environment and room temperature, wherein the working gas is one of helium, nitrogen and compressed air, the pressure of the working gas is 0.1-1.0MPa, and the spraying distance is 4-10 mm.
5. The method for preparing a porous polyetheretherketone-based coating material according to claim 1, wherein in step 2, the process parameters for depositing the degradable material powder by using the cold spray technique are as follows:
spraying under the conditions of atmospheric environment and room temperature, wherein the working gas is one of helium, nitrogen and compressed air, the pressure of the working gas is 0.1-1.0MPa, and the spraying distance is 4-10 mm.
6. The method for preparing a porous PEEK-based coating material according to claim 1, wherein in step 2, the degradable material powder has a particle size of 0.1-10 μm.
7. The method for preparing a porous PEEK-based coating material according to claim 1, wherein the degradable material powder is deposited to a thickness of 2-10 μm in step 2.
8. A porous peek-based coating material, characterized in that it is prepared by the method of preparing a porous peek-based coating material according to any one of claims 1 to 7.
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