CN107362390B - Preparation method of zirconium oxide/polylactic acid-glycolic acid copolymer anti-corrosion hybrid coating based on atomic layer deposition - Google Patents
Preparation method of zirconium oxide/polylactic acid-glycolic acid copolymer anti-corrosion hybrid coating based on atomic layer deposition Download PDFInfo
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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
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- A61L27/28—Materials for coating 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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- A—HUMAN NECESSITIES
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/602—Type of release, e.g. controlled, sustained, slow
- A61L2300/604—Biodegradation
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- A—HUMAN NECESSITIES
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- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/02—Methods for coating medical devices
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- A—HUMAN NECESSITIES
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- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
Abstract
A preparation method of an anti-corrosion hybrid coating of a zirconia/polylactic acid-glycolic acid copolymer based on atomic layer deposition comprises the following steps: s1, taking a magnesium metal wafer as a substrate, performing ultrasonic treatment, and naturally airing for later use; s2, carrying out atomic layer deposition on the substrate dried in the step S1 to obtain a substrate with a zirconia coating on the surface; s3, preparing a PLGA solution, dripping the PLGA solution on the substance obtained in the step S2, and spin-coating, namely obtaining the corrosion-resistant hybrid coating with the zirconium oxide/polylactic acid-glycolic acid copolymer on the surface of the substrate. The advantages are that: the anti-corrosion hybrid coating is prepared on the surface of a substrate by an atomic deposition method and a spin coating method in sequence by combining the biocompatibility, wear resistance, corrosion resistance, pressure resistance, osteogenesis property, mechanical property and low toxicity of zirconium oxide and the good biocompatibility, biodegradability and non-toxicity of PLGA, so that the anti-corrosion hybrid coating is obtained on the surface of the substrate, and the anti-corrosion performance is high through the synergistic effect of the anti-corrosion hybrid coating and the anti-corrosion hybrid coating.
Description
Technical Field
The invention relates to the technical field of application of a hybrid film of a nano ceramic film and a polymer, in particular to a preparation method of an anti-corrosion hybrid coating of a zirconia/polylactic acid-glycolic acid copolymer based on atomic layer deposition.
Background
Biomedical materials such as stainless steel and titanium alloy have good mechanical properties and fracture toughness, so that they can better maintain mechanical integrity and biocompatibility when bone tissues are healed, and thus, the biomedical materials are widely applied. However, certain metal biomaterials, such as nitinol, release toxic ions during corrosion, causing allergic reactions. More importantly, these conventional bio-metallic materials are not degradable in physiological environments, which may require a subsequent procedure to remove the implant material after bone healing. This not only increases the pain of the patient but also increases the economic burden of the patient. A suitable biomaterial that is degradable is therefore imperative. The magnesium alloy has good mechanical property and biodegradability and has a Young modulus which is closer to that of natural bones, so that the stress shielding effect and the osteolysis phenomenon can be relieved, and the magnesium alloy is more and more concerned by people.
In addition, magnesium is an essential element of the human body, and is involved in the synthesis of proteins, the activation of various enzymes, and the regulation of activities in the neuromuscular and central nervous systems to ensure normal myocardial contraction and thermoregulation. The magnesium-based implant has excellent osteoconductivity, promotes the growth of new bone tissue, and promotes osseointegration to enhance the stability of the implant. Finally, the magnesium alloy can be biodegraded due to the small electrode potential, thereby avoiding the secondary operation. However, the metal is more active and degrades too fast in vivo, so that the injured bone tissue is not repaired, the magnesium metal loses the inherent mechanical property and cannot play a role in fixation and protection, and the generated hydrogen and-OH can influence the growth of surrounding tissue cells in the degradation process and cannot achieve a certain clinical effect, so that the surface of the metal is modified to have larger early corrosion resistance, and the metal has greater practical significance.
Disclosure of Invention
One of the objects of the present invention is to provide a method for preparing a zirconium oxide/polylactic acid-glycolic acid copolymer anti-corrosion hybrid coating based on atomic layer deposition, so as to prepare an anti-corrosion coating with good anti-corrosion nano/polymer hybrid. The other purpose of the invention is to prepare the zirconium oxide nano ceramic coating with corrosion resistance by utilizing the atomic layer deposition technology. The third purpose of the invention is to obtain a polylactic acid-glycolic acid copolymer film by spin coating to obtain a zirconium oxide/polylactic acid-glycolic acid copolymer hybrid coating, so that the nano zirconium oxide and the polylactic acid-glycolic acid copolymer have a synergistic corrosion resistance effect.
The invention provides a preparation method of a zirconium oxide/polylactic acid-glycolic acid copolymer anti-corrosion hybrid coating based on atomic layer deposition, which comprises the following steps:
s1, polishing the surface of a magnesium metal wafer step by using abrasive paper to serve as a substrate, then sequentially performing ultrasonic treatment on the substrate in ethanol and acetone for 25-45 min, and naturally airing for later use;
s2, carrying out atomic layer deposition on the substrate dried in the step S1: heating a zirconium source to 130-160 ℃, then using deionized water at 30-40 ℃ as an O source, depositing at 150-300 ℃, and performing circulation for 25-200 times to obtain a substrate with a zirconium oxide coating on the surface;
preferably, in step S2, one cycle consists of pulse of tetrakis (dimethylamino) zirconium for 20-30ms, high purity nitrogen purge for 15-20S, pulse of deionized water for 100-150ms, and high purity nitrogen purge for 15-20S;
s3, preparing a 4% (w/v) PLGA (polylactic-co-glycolic acid) solution, dripping the PLGA solution on the substance obtained in the step S2, and performing spin coating to obtain the zirconium oxide/polylactic-co-glycolic acid anti-corrosion hybrid coating on the surface of the substrate.
In step S3, the molecular weight of PLGA is 120000, the ratio of polylactic acid to glycolic acid is 85:15, and the viscosity is 0.61;
in step S3, the spin coating parameters are that the spin coating is performed for 10-20S under the condition that the rotating speed is 500-600rmp, then the spin coating is performed for 30-40S under the condition that the rotating speed is 4000-5000rmp, and the spin coating is repeated for 2-6 times.
The second aspect of the invention protects the corrosion resistant hybrid coating produced by the method of the first aspect.
The preparation method of the zirconium oxide/polylactic acid-glycolic acid copolymer anti-corrosion hybrid coating based on the atomic layer deposition has the advantages that:
the anti-corrosion hybrid coating is prepared on the surface of a substrate by an atomic deposition method and a spin coating method in sequence by combining the biocompatibility, wear resistance, corrosion resistance, pressure resistance, osteogenesis property, mechanical property and low toxicity of zirconium oxide and the good biocompatibility, biodegradability and non-toxicity of PLGA, so that the anti-corrosion hybrid coating is obtained on the surface of the substrate, and the anti-corrosion hybrid coating is placed in a human body to have high anti-corrosion performance through the synergistic effect of the anti-corrosion hybrid coating and the PLGA;
the thickness of the zirconia deposit on the surface of the substrate is controllable, compact and uniform, and the method is simple and has high safety.
Drawings
FIG. 1 is a graph of the surface topography of pure magnesium metal, as measured by scanning electron microscopy
The surface appearance of the sample is obtained by characterization;
FIG. 2 is a graph showing the morphology of the magnesium metal of example 1 after zirconium oxide deposition;
FIG. 3 is a graph of the morphology of the magnesium metal of example 1 after depositing zirconia on the surface and spin-coating PLGA;
fig. 4 is an electrochemical impedance plot of a pure magnesium metal sample.
FIG. 5 is a graph of the electrochemical impedance of the sample of example 2.
FIG. 6 is a graph of the electrochemical impedance of the sample of example 1.
Detailed Description
For a better understanding of the present invention, reference is made to the following detailed description taken in conjunction with the accompanying drawings and examples, but the scope of the invention as claimed is not limited to the scope of the examples shown.
Example one
S1, polishing the surface of a magnesium metal wafer (16mm by 5mm) by using sand paper step by step to serve as a substrate (the surface structure appearance figure of the substrate is shown in figure 1), then sequentially carrying out ultrasonic treatment on the substrate in ethanol and acetone for 30min, and naturally airing for later use;
s2, carrying out atomic layer deposition on the substrate dried in the step S1: heating a zirconium source to 150 ℃, then using deionized water with the temperature of 35 ℃ as an O source, setting the deposition temperature to be 250 ℃, and performing 100 times of circulation, wherein one circulation consists of pulse of tetra (dimethylamino) zirconium for 30ms, pulse of high-purity nitrogen for 20s, pulse of deionized water for 150ms and pulse of high-purity nitrogen for 20 s; obtaining a substrate with a zirconia coating on the surface (the surface structure topography is shown in figure 2);
s3, preparing a 4% (w/v) PLGA (polylactic-co-glycolic acid) solution, dripping 0.4ml of the PLGA solution onto the substance obtained in the step S2, and carrying out spin coating, wherein the spin coating parameters are that the substance is rotated for 10S under the condition that the rotating speed is 600rmp, and then is rotated for 30S under the condition that the rotating speed is 5000rmp, and the steps are repeated for 3 times; namely, a zirconium oxide/polylactic acid-glycolic acid copolymer anti-corrosion hybrid coating (the surface structure topography of which is shown in figure 3) is obtained on the surface of a substrate;
wherein the molecular weight of PLGA is 120000, the ratio of polylactic acid to glycolic acid is 85:15, and the viscosity is 0.61.
Example two
The difference from the first embodiment is that:
in step S2: the atomic layer deposition parameters were: the zirconium source is heated to 150 ℃, deionized water with the temperature of 35 ℃ is used as an O source, the deposition temperature is 250 ℃, 25 times of circulation are carried out, and one circulation consists of pulse of tetra (dimethylamino) zirconium for 30ms, pulse of high-purity nitrogen for 20s, pulse of deionized water for 150ms and pulse of high-purity nitrogen for 20 s.
EXAMPLE III
The difference from the first embodiment is that:
in step S2: the atomic layer deposition parameters were: the zirconium source is heated to 150 ℃, deionized water with the temperature of 35 ℃ is used as an O source, the deposition temperature is 200 ℃, 100 times of circulation is carried out, and one circulation consists of pulse of tetra (dimethylamino) zirconium for 30ms, pulse of high-purity nitrogen for 20s, pulse of deionized water for 150ms and pulse of high-purity nitrogen for 20 s.
Example four
The difference from the first embodiment is that:
the spin coating parameters were 10s at 600rmp and 30s at 5000rmp, repeated 6 times.
The surface topography of pure magnesium metal and magnesium metal in the first embodiment is characterized by a scanning electron microscope after zirconia is deposited on the surface of the pure magnesium metal and the magnesium metal, and after the zirconia is deposited on the surface of the magnesium metal and PLGA is spin-coated, and the topography shown in FIGS. 1, 2 and 3 is obtained.
Performing impedance detection on the obtained products of the first and second embodiments, wherein a pure magnesium sheet is used as a reference;
detection of electrochemical impedance: the impedance of the sample is tested by adopting an electrochemical workstation under the test conditions that the interference voltage is 5mV and the scanning frequency range is 10 mV-2Hz-105Hz, the obtained result is fitted by Zsimpwin 3.21 software;
as can be seen from fig. 4, 5 and 6, the electrochemical impedance of the samples obtained in examples 2 and 1 is obviously increased compared with that of pure magnesium metal, which indicates that the modified samples have obvious corrosion resistance; meanwhile, under the same condition, the corrosion resistance of the coating can be enhanced by increasing the cycle number of ALD.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A preparation method of a zirconium oxide/polylactic acid-glycolic acid copolymer anti-corrosion hybrid coating based on atomic layer deposition is characterized by comprising the following steps: the method comprises the following steps:
s1, polishing the surface of a magnesium metal wafer step by using abrasive paper to serve as a substrate, then sequentially performing ultrasonic treatment on the substrate in ethanol and acetone for 25-45 min, and naturally airing for later use;
s2, carrying out atomic layer deposition on the substrate dried in the step S1: heating a zirconium source to 130-160 ℃, then using deionized water at 30-40 ℃ as an O source, depositing at 150-300 ℃, and performing circulation for 25-200 times to obtain a substrate with a zirconium oxide coating on the surface;
s3, preparing a 4% (w/v) PLGA solution, dripping the PLGA solution on the substance obtained in the step S2, and performing spin coating to obtain the zirconium oxide/polylactic acid-glycolic acid copolymer anti-corrosion hybrid coating on the surface of the substrate;
the molecular weight of PLGA in step S3 was 120000, the ratio of polylactic acid to glycolic acid was 85:15, and the viscosity was 0.61.
2. The method of claim 1, further comprising: in step S2, a cycle consists of pulsing tetrakis (dimethylamino) zirconium for 20-30ms, purging with high purity nitrogen for 15-20S, pulsing deionized water for 100-150ms, and purging with high purity nitrogen for 15-20S.
3. The method of claim 1, further comprising: in step S3, the spin coating parameters are that the spin coating is performed for 10-20S under the condition that the rotating speed is 500-600rmp, then the spin coating is performed for 30-40S under the condition that the rotating speed is 4000-5000rmp, and the spin coating is repeated for 2-6 times.
4. Protecting an anti-corrosion hybrid coating prepared by the method of any one of claims 1 to 3.
5. Protecting the application of the anti-corrosion hybrid coating of claim 4 to biomedical materials for bone tissue repair.
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CN105963773A (en) * | 2016-04-28 | 2016-09-28 | 南京凤源新材料科技有限公司 | Preparation method of polylactide acid glycolic acid copolymer-hydroxylapatite composite microspheres |
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FR2988300B1 (en) * | 2012-03-26 | 2014-04-11 | Bjr France | IMPLANTABLE BONE REPAIR AND RECONSTRUCTION DEVICE CAPABLE OF ADSORBING BIOACTIVE AGENTS AND METHODS OF MAKING SUCH A DEVICE |
WO2016083456A1 (en) * | 2014-11-26 | 2016-06-02 | Swiss Medical Coatings Sarl | Process for forming a thermally and chemically inert multilayer film |
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CN102245220A (en) * | 2008-12-01 | 2011-11-16 | Ucl商业有限公司 | Article and method of surface treatment of an article |
CN103132045A (en) * | 2011-11-28 | 2013-06-05 | 英作纳米科技(北京)有限公司 | Preparation method for coatings of medical supplies and products thereof |
CN103007356A (en) * | 2012-12-19 | 2013-04-03 | 南京理工大学 | UHMWPE (Ultra High Molecular Weight Polyethylene) artificial joint with surface wear-resistant layer and preparation method of same |
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