CN105536068A - Method for improving surface bioactivity of polyether ether ketone - Google Patents
Method for improving surface bioactivity of polyether ether ketone Download PDFInfo
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- CN105536068A CN105536068A CN201610029559.6A CN201610029559A CN105536068A CN 105536068 A CN105536068 A CN 105536068A CN 201610029559 A CN201610029559 A CN 201610029559A CN 105536068 A CN105536068 A CN 105536068A
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- A—HUMAN NECESSITIES
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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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- 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
- A61L27/56—Porous materials, e.g. foams or sponges
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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Abstract
The invention provides a method for improving surface bioactivity of polyether ether ketone (PEEK). The method is characterized in that in a PEEK preparation process or a PEEK re-formation process, a porous metal layer with excellent biocompatibility is embedded in the surface of PEEK, thereby obtaining a porous fiber/PEEK composite material; the structure of the composite material is that the surface is a bioactivity coating, and the base is a composite material of the metal porous layer and the PEEK. The method provided by the invention integrates PEEK surface modification and PEEK preparation; the method is simple and has low requirements on instruments. The prepared novel composite material has excellent performances, the bioactivity of the PEEK is improved, bone conduction and body fluid transmission are facilitated, the mechanical property and osteogenesis efficiency are improved, and the prepared composite material has stronger binding force between the porous metal layer and the PEEK so as to meet most application requirements, such as bone filling, bone repair, bone transplantation and bone fixation, and in particular the composite material can be applied to bone transplantation under loading conditions, such as interbody fusion cage, vertebral replacement, femoral head diseases, acetabular cup, fixing bolt and fixing plate.
Description
Technical field
The present invention relates to a kind of medical bio composite, be specifically related to one and improve the bioactive method of polyether-ether-ketone (PEEK) material surface, belong to biology medical material technical field.
Background technology
Polyethers ether copper (PEEK) is a kind of novel organic high molecular compound, has the semi-transmissive and advantage of elastic modelling quantity between spongy bone and compact bone of lonizing radiation, is all widely used in the fields such as damage, vertebra, joint and shaping.But PEEK is as bio-inert material, be but difficult to and skeleton shape bone osteogenic fusion, limit its application as bone renovating material.Not enough for this, many scholars apply diverse ways process PEEK, to improve its skeletonization usefulness; Comprise: PEEK-hydroxyapatite (HA) composite, PEEK-HA-carbon fibre composite, nanometer fluor-apatite-PEEK composite, nano titanium oxide-PEEK composite etc.But complicated for the apparatus for preparation of these coatings, preparation technology is loaded down with trivial details, and prepared biological coating cannot form stronger combination with PEEK, and during clinical practice, coating often easily comes off.
Winding-type porous layer is successfully applied to hip cotyle cup, and large quantity research shows, it has good biocompatibility and bone formation performance.For PEEK Problems existing, we are on the basis of a large amount of research work, in PEEK preparation process and PEEK reshaping process, imbed winding-type porous metals, form a kind of novel fibercoating/PEEK composite, the filling of most of bone can be met, Bone Defect Repari, bone collection, bone are fixed etc. application, such as: Invasive lumbar fusion device, vertebral body prosthesis, femur disease, acetabular cup, hold-down screw and fixing head etc.
Summary of the invention
The object of the invention is, overcome the deficiencies in the prior art, a kind of method improving polyether-ether-ketone surface bioactive is provided, one deck porous metallic layers is embedded on polyether-ether-ketone (PEEK) surface, form a kind of novel porousfiber/PEEK composite, to improve the biological activity on PEEK surface, mechanical property and skeletonization usefulness, the multiporous biological coating simultaneously prepared and PEEK have stronger adhesion, thus meet the application requirement that the filling of most of bone, Bone Defect Repari, bone collection and bone such as to fix at the aspect.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of method improving polyether-ether-ketone surface bioactive, it is characterized in that: in polyether-ether-ketone preparation process or polyether-ether-ketone reshaping process, embed the porous metallic layers with good biocompatibility on the surface of polyether-ether-ketone, obtain porousfiber/PEEK composite; The structure of this composite is: top layer is bioactivity coatings, and matrix is the composite of described metal porous layer and polyether-ether-ketone.
As further improvement, described porous metallic layers adopts medical metallic fiber to be entwined, and the string diameter size of the pore size of this porous metallic layers and porosity and described metallic fiber can require to adjust according to the bio-medical under different occasion.
As further improvement, described metallic fiber is titanium or titanium alloy fiber, tantalum or tantalum alloy fiber or stainless steel fibre.
As further improvement, described polyether-ether-ketone is the polyether-ether-ketone of medical any composition, or through the polyether-ether-ketone of modification, or through the polyether-ether-ketone of overdoping, or the polyether-ether-ketone through strengthening.
As further improvement, described bioactivity coatings carries out follow-up surface bioactive process and is formed on the surface of porous metallic layers, described surface bioactive is treated to the combination of one or more in differential arc oxidation, anodic oxidation, coating hydroxyapatite coating layer, the hydroxyapatite coating layer applying doping strontium and coating bioactive ceramic coating.
As further improvement, described metal porous layer and the compound of polyether-ether-ketone can realize in the polymerization process of polyether-ether-ketone, also can realize in the reshaping process of polyether-ether-ketone.
As further improvement, described porous metallic layers and the complex method of polyether-ether-ketone can be twin-screw extruder and molding, also can be infiltrations.
Compared with prior art, the present invention has the following advantages:
1, by the advanced composite material (ACM) that the present invention obtains, its surface is bioactivity coatings, greatly improves the biological activity of PEEK, is conducive to bone conduction and body fluid transmission, improves the skeletonization usefulness on PEEK surface; Modified matrix is the composite of porous metallic layers and PEEK, improves mechanical property more greatly, and the porous metallic layers of preparation and PEEK have stronger adhesion.The contrast of the hot strength of described advanced composite material (ACM) and adhesion strength and existing bone renovating material can consult Fig. 6 and Fig. 7.
2, described method technique is simple, not high to instrument requirements, is a kind of method that the PEEK of collection surface modification and PEEK are prepared in one.
3, advanced composite material (ACM) excellent performance, rational in infrastructure, the application requirements such as the filling of most of bone, Bone Defect Repari, bone collection, bone be fixing can be met, especially can be used in the bone collection under load condition, such as: Invasive lumbar fusion device, vertebral body prosthesis, femur disease, acetabular cup, hold-down screw and fixing head etc.
Accompanying drawing explanation
Fig. 1 is unmodified PEEK surface topography schematic diagram.
Fig. 2 is the surface topography schematic diagram after PEEK surface modification.
Fig. 3 is the primary morphology schematic diagram of porous metals.
Fig. 4 is the schematic appearance of the composite of metallic fiber and PEEK.
Fig. 5 is the schematic diagram of metallic fiber and PEEK combination interface.
Fig. 6 is the hot strength comparison diagram of the composite that formed of the porous metallic layers of 60% porosity and PEEK and PEEK.
Fig. 7 is adhesion strength contrast schematic diagram (embeding layer thickness 2 millimeters, embeding layer porosity 50%, metallic fiber string diameter 200 microns) of different PEEK composites.
Detailed description of the invention
The present invention relates to a kind of PEEK of improvement surface activity, improve the new method of its skeletonization usefulness, namely a kind of new composite construction is formed by twin-screw extrusion technology or other technologies, one deck porous metallic layers is embedded on polyether-ether-ketone (PEEK) surface, matrix is the composite of PEEK/ metallic fiber, to improve the mechanical property of PEEK.
The method of described improvement polyether-ether-ketone surface bioactive comprises, the porous metallic layers (see Fig. 2) that one deck has good biocompatibility is embedded on the surface of polyether-ether-ketone (PEEK) (see Fig. 1), this porous metallic layers is the porous fibre (see Fig. 3) of winding-type, its material can be any metallic fiber or tinsel with good biocompatibility, by twin-screw extruder and forming technique or other technology, as infiltration, in the monomer polymerization or reshaping process of polyether-ether-ketone, porous metallic layers is imbedded, form a kind of novel porousfiber/PEEK composite (see Fig. 4), the structure of this composite is: top layer is bioactivity coatings, and matrix is the composite (see Fig. 5) of described metal porous layer and polyether-ether-ketone.
Described porous metallic layers adopts medical metallic fiber to be entwined by conventional winding machine tool, the structural parameters such as the string diameter size of the pore size of this porous metallic layers and porosity and described metallic fiber can adjust, flexibly with the bio-medical requirement under satisfied different occasion.
Described metallic fiber is titanium or titanium alloy fiber, or tantalum or tantalum alloy fiber, or stainless steel fibre.
Described polyether-ether-ketone (PEEK) is the PEEK of medical any composition, or through the PEEK of modification, or through the PEEK of overdoping, or through PEEK of strengthening etc.
Described bioactivity coatings carries out follow-up surface bioactive process and is formed on the surface of porous metallic layers, to improve biological activity and the bone formation performance of described composite further.Described surface bioactive is treated to the combination of one or more in differential arc oxidation, anodic oxidation, coating hydroxyapatite coating layer, the hydroxyapatite coating layer applying doping strontium and coating bioactive ceramic coating.
Below in conjunction with the drawings and specific embodiments the method improving polyether-ether-ketone surface bioactive of the present invention done and further elaborate, but should not limit the scope of the invention with this.
Embodiment 1
Adopt the titanium silk of the diameter 0.005mm of medical grade, be prepared into the POROUS TITANIUM of setting shape and setting porosity with coiling machinery, its porosity is 45%; Adopt nucleophilic displacement of fluorine legal system for PEEK, by impregnation technology in preparation process, form the porous titanium layer of one deck 2mm on PEEK surface, modified PEEK intensity is 180MPa, and the adhesion strength of coating is 80MPa, is applicable to the occasions such as Invasive lumbar fusion device.
Embodiment 2
Adopt the titanium tantalum alloy silk of the diameter 3mm of medical grade, the porous metals of setting shape and setting porosity are prepared into coiling machinery, its porosity is 10%, utilize twin-screw extruder and forming technique, these porous metals are imbedded PEEK, and form the porous metallic layers of top layer 3mm, modified PEEK intensity is 150MPa, coating adhesion strength is 210MPa, is applicable to the occasions such as femoral stem.
Embodiment 3
The diameter of employing medical grade is the 316L stainless steel silk of 0.27mm, the porous metals of setting shape and setting porosity are prepared into coiling machinery, its porosity is 71%, in the process of PEEK polycondensation, imbedded by porous stainless steel in PEEK, form the porous stainless steel layer of top layer 1mm, modified PEEK intensity is 120MPa, coating adhesion strength is 160MPa, is applicable to the occasions such as acetabular cup.
Embodiment 4
The diameter adopting medical grade is the tantalum wire of 1mm, the porous tantalum of setting shape and setting porosity is prepared into coiling machinery, its porosity is 30%, in the process of PEEK polycondensation, imbed in PEEK by this porous tantalum, form the porous tantalum layer of top layer 1.5mm, modified PEEK intensity is 136MPa, coating adhesion strength is 192MPa, is applicable to the occasions such as acetabular cup.
Above are only the preferred embodiments of the present invention, it must be noted that, the various equivalent modifications that those skilled in the art is all to be done according to the present patent application content, change and correction, all should become the protection domain of patent of the present invention.
The medical composite material prepared by the present invention greatly improves the biological activity of PEEK, and be conducive to bone conduction, body fluid transmission, the mechanical property of matrix material and skeletonization usefulness have had larger improvement.The application such as the filling of most of bone, Bone Defect Repari, bone collection, bone be fixing can be met, can be used for the bone collection under load condition, such as: Invasive lumbar fusion device, vertebral body prosthesis, femur disease, acetabular cup, hold-down screw and fixing head etc.
Claims (7)
1. one kind is improved the method for polyether-ether-ketone surface bioactive, it is characterized in that: in polyether-ether-ketone preparation process or polyether-ether-ketone reshaping process, embed the porous metallic layers with good biocompatibility on the surface of polyether-ether-ketone, obtain porousfiber/PEEK composite; The structure of this composite is: top layer is bioactivity coatings, and matrix is the composite of described metal porous layer and polyether-ether-ketone.
2. the method improving polyether-ether-ketone surface bioactive according to claim 1, it is characterized in that: described porous metallic layers adopts medical metallic fiber to be entwined, the string diameter size of the pore size of this porous metallic layers and porosity and described metallic fiber can require to adjust according to the bio-medical under different occasion.
3. the method improving polyether-ether-ketone surface bioactive according to claim 2, is characterized in that: described metallic fiber is titanium or titanium alloy fiber, tantalum or tantalum alloy fiber or stainless steel fibre.
4. the method improving polyether-ether-ketone surface bioactive according to claim 1, it is characterized in that: described polyether-ether-ketone is the polyether-ether-ketone of medical any composition, or through the polyether-ether-ketone of modification, or through the polyether-ether-ketone of overdoping, or the polyether-ether-ketone through strengthening.
5. the method improving polyether-ether-ketone surface bioactive according to claim 1, it is characterized in that: described bioactivity coatings carries out follow-up surface bioactive process and formed on the surface of porous metallic layers, described surface bioactive is treated to the combination of one or more in differential arc oxidation, anodic oxidation, coating hydroxyapatite coating layer, the hydroxyapatite coating layer applying doping strontium and coating bioactive ceramic coating.
6. the method improving polyether-ether-ketone surface bioactive according to claim 1, it is characterized in that: described metal porous layer and the compound of polyether-ether-ketone can realize in the polymerization process of polyether-ether-ketone, also can realize in the reshaping process of polyether-ether-ketone.
7. the method improving polyether-ether-ketone surface bioactive according to claim 1, is characterized in that: described porous metallic layers and the complex method of polyether-ether-ketone can be twin-screw extruder and molding, also can be infiltration.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106178104A (en) * | 2016-08-29 | 2016-12-07 | 上海交通大学 | A kind of medical medicine-carried porous polyether-ether-ketone and manufacture method thereof and application |
| CN106178105A (en) * | 2016-08-29 | 2016-12-07 | 上海交通大学 | A kind of medical polyether-ether-ketone of porous surface and its preparation method and application |
| CN106267361A (en) * | 2016-08-29 | 2017-01-04 | 上海交通大学 | A kind of medical gradient porous composite of medicine-carried metal-polymer |
| CN112169017A (en) * | 2020-09-29 | 2021-01-05 | 西安交通大学 | Hydroxyapatite nano coating and preparation method thereof |
| CN113527748A (en) * | 2021-07-12 | 2021-10-22 | 南方科技大学 | Polyether-ether-ketone surface modification method, polyether-ether-ketone obtained through modification and application of polyether-ether-ketone |
| CN114176811A (en) * | 2021-11-15 | 2022-03-15 | 浙江大学 | PEEK base station of nano-needle interface and preparation method thereof |
| CN114642770A (en) * | 2022-03-22 | 2022-06-21 | 中国人民解放军总医院第一医学中心 | Implant composite material and preparation method and application thereof |
| CN114805888A (en) * | 2022-03-29 | 2022-07-29 | 陕西师范大学 | Method for improving surface bioactivity and osseointegration performance of polyether-ether-ketone substrate |
| CN116672508A (en) * | 2023-08-03 | 2023-09-01 | 北京德益达美医疗科技有限公司 | Medical polyether-ether-ketone composite material and preparation method and application thereof |
-
2016
- 2016-01-18 CN CN201610029559.6A patent/CN105536068A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106178104A (en) * | 2016-08-29 | 2016-12-07 | 上海交通大学 | A kind of medical medicine-carried porous polyether-ether-ketone and manufacture method thereof and application |
| CN106178105A (en) * | 2016-08-29 | 2016-12-07 | 上海交通大学 | A kind of medical polyether-ether-ketone of porous surface and its preparation method and application |
| CN106267361A (en) * | 2016-08-29 | 2017-01-04 | 上海交通大学 | A kind of medical gradient porous composite of medicine-carried metal-polymer |
| CN106178105B (en) * | 2016-08-29 | 2019-12-10 | 上海交通大学 | medical polyether-ether-ketone with porous surface and preparation method and application thereof |
| CN112169017A (en) * | 2020-09-29 | 2021-01-05 | 西安交通大学 | Hydroxyapatite nano coating and preparation method thereof |
| CN113527748A (en) * | 2021-07-12 | 2021-10-22 | 南方科技大学 | Polyether-ether-ketone surface modification method, polyether-ether-ketone obtained through modification and application of polyether-ether-ketone |
| CN113527748B (en) * | 2021-07-12 | 2023-01-03 | 南方科技大学 | Polyether-ether-ketone surface modification method, polyether-ether-ketone obtained through modification and application of polyether-ether-ketone |
| CN114176811A (en) * | 2021-11-15 | 2022-03-15 | 浙江大学 | PEEK base station of nano-needle interface and preparation method thereof |
| CN114642770A (en) * | 2022-03-22 | 2022-06-21 | 中国人民解放军总医院第一医学中心 | Implant composite material and preparation method and application thereof |
| CN114805888A (en) * | 2022-03-29 | 2022-07-29 | 陕西师范大学 | Method for improving surface bioactivity and osseointegration performance of polyether-ether-ketone substrate |
| CN114805888B (en) * | 2022-03-29 | 2023-08-08 | 陕西师范大学 | Method for improving surface bioactivity and osseointegration performance of polyether-ether-ketone base material |
| CN116672508A (en) * | 2023-08-03 | 2023-09-01 | 北京德益达美医疗科技有限公司 | Medical polyether-ether-ketone composite material and preparation method and application thereof |
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