CN113105807B - Tantalum nitride reinforced polyether-ether-ketone composite coating and preparation method and application thereof - Google Patents

Tantalum nitride reinforced polyether-ether-ketone composite coating and preparation method and application thereof Download PDF

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CN113105807B
CN113105807B CN202110330636.2A CN202110330636A CN113105807B CN 113105807 B CN113105807 B CN 113105807B CN 202110330636 A CN202110330636 A CN 202110330636A CN 113105807 B CN113105807 B CN 113105807B
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tantalum nitride
ether
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composite coating
peek
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CN113105807A (en
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曹琳
林志丹
张鹏
黄素媛
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Jinan University
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
    • C09D161/04—Condensation polymers of aldehydes or ketones with phenols only
    • C09D161/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
    • 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
    • A61L27/28—Materials for coating prostheses
    • A61L27/34—Macromolecular materials
    • 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
    • A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
    • A61L27/44—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
    • A61L27/446—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix with other specific inorganic fillers other than those covered by A61L27/443 or A61L27/46
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
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    • C09D7/61—Additives non-macromolecular inorganic
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    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/02—Electrolytic coating other than with metals with organic materials
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

Abstract

The invention belongs to the technical field of biological materials, and particularly discloses a preparation method and application of a tantalum nitride reinforced polyether-ether-ketone composite coating. The method comprises the following steps: (1) uniformly mixing the chitosan solution and ethanol, sequentially adding PEEK powder and nano TaN to obtain a mixed solution, and performing ultrasonic dispersion to obtain a nano suspension; (2) putting cathode and anode electrode materials into the nano suspension solution obtained in the step (1); and introducing direct current, and depositing to obtain the tantalum nitride reinforced polyether-ether-ketone composite coating. The invention prepares PEEK coating on titanium and its alloy, stainless steel and other basal bodies by a cathodic electrodeposition method, and introduces tantalum nitride nano particles into PEEK material. The introduction of the tantalum nitride nano particles can enhance the osteogenic property of PEEK. The coating prepared by cathodic electrodeposition has short production time, simple equipment, low price and wide application prospect.

Description

Tantalum nitride reinforced polyether-ether-ketone composite coating and preparation method and application thereof
Technical Field
The invention belongs to the technical field of biological materials, and particularly relates to a tantalum nitride reinforced polyether-ether-ketone composite coating, and a preparation method and application thereof.
Background
Titanium and its alloys in artificial joint replacement materials have excellent properties such as low density, high specific strength, good electrochemical corrosion resistance, relatively low elastic modulus and good biocompatibility. Has wide application in biomedical engineering. The high suitability of titanium alloys is due to a good balance of mechanical properties and good castability, plastic workability, heat treatability and weldability. The main drawbacks of all titanium alloys are poor wear resistance, high coefficient of friction (COF) and relatively low hardness. When the method is applied to a joint abrasion structure, ion dissolution and stress shielding are easily caused, and the osteolysis implantation fails. The ideal artificial joint should meet the requirements of wear resistance and body fluid corrosion resistance on the basis of certain mechanical support.
The polyether-ether-ketone has excellent toughness and rigidity, good thermochemical stability and good tribological performance. However, pure PEEK is insufficient in mechanical strength when used as a weighing structure in a human body, and thus needs to be improved to improve mechanical strength.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a preparation method of a tantalum nitride reinforced polyether-ether-ketone composite coating.
The invention also aims to provide the tantalum nitride reinforced polyether-ether-ketone composite coating prepared by the method.
The invention further aims to provide application of the tantalum nitride reinforced polyether-ether-ketone composite coating in preparation of bone materials.
The purpose of the invention is realized by the following scheme:
a preparation method of a tantalum nitride reinforced polyether-ether-ketone composite coating comprises the following steps:
(1) uniformly mixing the chitosan solution and ethanol, sequentially adding PEEK powder and nano TaN to obtain a mixed solution, and performing ultrasonic dispersion to obtain a nano suspension;
(2) putting cathode and anode electrode materials into the nano suspension solution obtained in the step (1); and introducing direct current, and depositing to obtain the tantalum nitride reinforced polyether-ether-ketone composite coating.
Step (1), ethanol: the volume ratio of the chitosan solution is 1-2: 2-1;
the concentration of the chitosan solution in the step (1) is 0.5-0.1 wt%.
The PEEK content in the mixed solution in the step (1) is 1-4 wt%; the addition amount of the TaN is 0.01-3 wt%, and the preferable addition amount is 0.1 wt%. .
The particle size of the PEEK in the mixed solution in the step (1) is 20-30 μm; the particle size of the TaN is 250-270 nm, preferably 260 nm.
The cathode material in the step (2) is titanium alloy, pure titanium or stainless steel; preferably, before the cathode material is used, the cathode material is cleaned, specifically, the surface is subjected to sand blasting to form a rough surface, and the rough surface is cleaned by absolute ethyl alcohol and acetone. The anode material is a common inert electrode, and is preferably graphite or platinum sheet.
The voltage of the direct current in the step (2) is 10-30V, preferably 30V; the current density is 0.01-0.5A/cm2Preferably 0.01 to 0.05A/cm2. The distance between the electrodes is 1-3cm, preferably 1 cm; the deposition time is 1-5 min.
The tantalum nitride reinforced polyether-ether-ketone composite coating is prepared by the method.
The tantalum nitride reinforced polyether-ether-ketone composite coating is applied to the preparation of an osteogenic material.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the invention prepares PEEK coating on titanium and its alloy, stainless steel and other basal bodies by a cathodic electrodeposition method, and introduces tantalum nitride nano particles into PEEK material. The introduction of the tantalum nitride nano particles can improve the wear resistance and hardness of the titanium alloy and enhance the osteogenic property of PEEK. The coating prepared by cathodic electrodeposition has short production time, simple equipment, low price and wide application prospect.
Drawings
FIG. 1 is a TEM image of the coating obtained in example 5.
In FIG. 2, (a) and (b) are SEM images of the coating obtained in example 5, and (c) is an element distribution diagram.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
The reagents used in the examples are commercially available without specific reference.
The tantalum nitride reinforced polyetheretherketone composite coatings of examples 1-11 were prepared by the following method:
(1) chitosan solution: mixing 0.5g of chitosan, 5mL of glacial acetic acid and 500mL of deionized water;
(2) uniformly mixing the 50mL of chitosan solution with 50mL of ethanol, and then adding 1-5 g of PEEK powder (20-30 microns) and 0.01-0.2 g of nano tantalum nitride (260nm) to obtain a mixed solution;
(3) and (3) ultrasonically dispersing the mixed solution obtained in the step (2) for 20min, and stirring and dissolving for 7h to obtain a nano suspension solution.
(4) Cathode (pure titanium) and anode (Pt) electrode materials are put into the nano suspension solution obtained in the step (3), and the electrode distance is 1-2 cm; introducing direct current, applying voltage of 30V and current density of 0.01-0.5A/cm2And depositing for 1-5min to obtain the tantalum nitride reinforced polyether-ether-ketone composite coating.
TABLE 1 Condition parameters of examples 1-11 and properties of the coatings obtained
Figure BDA0002994362920000031
Figure BDA0002994362920000041
TaN is a nanoparticle with different sizes and irregular shapes, and has stronger hardness and extremely high stability. PEEK and TaN were each coated with chitosan in the deposition solution, adsorbed together, and the deposition process was assigned to each deposition (as shown in fig. 1). As shown in the table, the friction coefficient is obviously reduced (the contact force of materials is reduced due to the effect of rolling and sliding in the friction process) after the TaN is added, the wear rate is obviously reduced, and the wear depth is reduced. And because the nano particles are added into the PEEK matrix, the crystallization property of the PEEK can be improved when the composite material is formed by sintering, so that the overall properties of the material are changed, for example, the hardness is improved. As for scratch resistance, since the PEEK material is uniformly distributed (electrodeposition can be uniformly distributed, as shown in fig. 2), the hardness of the PEEK material is also improved, and stress can be dispersed during the scratch process to protect the PEEK material.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (7)

1. A preparation method of a tantalum nitride reinforced polyether-ether-ketone composite coating is characterized by comprising the following steps:
(1) uniformly mixing the chitosan solution and ethanol, sequentially adding PEEK powder and nano TaN to obtain a mixed solution, and performing ultrasonic dispersion to obtain a nano suspension;
(2) putting cathode and anode electrode materials into the nano suspension solution obtained in the step (1); introducing direct current, and depositing to obtain the tantalum nitride reinforced polyether-ether-ketone composite coating;
the dosage of the chitosan solution in the step (1) is 50mL, the dosage of ethanol is 50mL, the dosage of PEEK powder is 3g, and the dosage of nano TaN is 0.05 g;
the preparation method of the chitosan solution in the step (1) is to mix 0.5g of chitosan, 5mL of glacial acetic acid and 500mL of deionized water;
the concentration of the chitosan solution in the step (1) is 0.5-0.1 wt%.
2. The production method according to claim 1, characterized in that: the particle size of the PEEK powder in the mixed solution in the step (1) is 20-30 micrometers; the grain size of the nano TaN is 250-270 nm.
3. The method of claim 1, wherein: the voltage of the direct current in the step (2) is 30V; controlling the current to be 0.01-0.5A/cm2(ii) a The distance between the electrodes in the step (2) is 1-2 cm.
4. The production method according to claim 1, characterized in that: the deposition time is 1-5 min.
5. The method of claim 1, wherein: the cathode material in the step (2) is titanium alloy, pure titanium or stainless steel; the anode material is a commonly used inert electrode.
6. A tantalum nitride reinforced polyether-ether-ketone composite coating prepared by the method of any one of claims 1-5.
7. Use of the tantalum nitride reinforced polyetheretherketone composite coating of claim 6 in the preparation of an osteogenic material.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103614699A (en) * 2013-12-16 2014-03-05 中国科学院上海硅酸盐研究所 Method for modifying surface of polyetheretherketone by injecting tantalum ion and modified polyetheretherketone material

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103614699A (en) * 2013-12-16 2014-03-05 中国科学院上海硅酸盐研究所 Method for modifying surface of polyetheretherketone by injecting tantalum ion and modified polyetheretherketone material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Electrophoretic deposition and microstructure development of Si3N4/polyetheretherketone coatings on titanium alloy;Tomasz Moskalewicz,et al.;《Surface & Coatings Technology》;20180925;第634-647页 *

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