CN112121227A - Preparation method of medical composite coating of strontium titanate/strontium hydroxyapatite on titanium metal surface - Google Patents
Preparation method of medical composite coating of strontium titanate/strontium hydroxyapatite on titanium metal surface Download PDFInfo
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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
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/32—Phosphorus-containing materials, e.g. apatite
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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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- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/54—Biologically active materials, e.g. therapeutic substances
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/412—Tissue-regenerating or healing or proliferative agents
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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
- A61L2300/606—Coatings
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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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
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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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
The invention relates to a preparation method of a medical composite coating of strontium titanate/strontium hydroxyapatite on the surface of titanium metal, which comprises the following steps: polishing the titanium sheet by using SiC sand paper step by step, ultrasonically washing, soaking in a mixed acid solution for 10-15 seconds, ultrasonically washing and drying; taking the pretreated titanium sheet as an anode and a platinum sheet electrode as a cathode, carrying out anodic oxidation at room temperature, cleaning and drying the titanium sheet, and carrying out annealing treatment in a tubular furnace; putting the obtained titanium sheet into 16ml of Sr (OH)2 solution, carrying out hydrothermal reaction for 1.5-2h at 200 ℃, taking out, cleaning and drying; placing the obtained titanium sheet in a mixed electrolyte of calcium salt and strontium salt for constant-current deposition, wherein the electrolyte comprises the following components: 0.034M-0.04M Ca (NO)3, 0.02M-0.06M Sr (NO)3, 0.025M NH4H2PO3, 0.1M Na (NO) 3. The invention relates to a preparation method of a medical composite coating of strontium titanate/strontium hydroxyapatite on the surface of titanium metal, which prepares a composite coating containing strontium element on the surface of a titanium matrix for the first time, wherein the composite coating is divided into a strontium-containing nanotube coating and a strontium-containing hydroxyapatite coating, and the performance of a titanium matrix implant is greatly improved.
Description
Technical Field
The invention belongs to the technical field of crossing of materials and biomedicine, and particularly relates to a preparation method of a strontium titanate/strontium hydroxyapatite composite medical coating on the surface of titanium metal.
Background
Titanium and titanium alloys are the most excellent implant materials at present because of their high mechanical strength, low elastic modulus and chemical inertness. Because the difference of the properties of titanium and titanium-based alloy and human bone tissues is still large, the titanium and titanium-based alloy still have the following two problems after being used as an implant material to enter human environment: 1. because titanium metal has biological inertia and unsatisfactory surface biological activity, the osteogenesis promoting capability of the titanium metal is poor, so that the combination of an implant body and surrounding tissues is poor, and the implant body is loosened after a long time; 2. since titanium metal implants alone do not have bactericidal anti-inflammatory properties, the implants enter the body and may cause an inflammatory reaction around the implant due to bacterial infection. At present, functional modification of titanium surfaces to improve their osseointegration with surrounding tissues is still a hot spot of research. The micro-nano structure effect on the surface of the titanium implant plays a leading role in inducing osteoblast proliferation and differentiation, and people mainly aim to change the surface appearance, structure and component characteristics of the titanium material of the implant through physical and chemical means, so that the aim of improving the biological performance of the implant is fulfilled.
Hydroxyapatite, abbreviated as HA, is widely used as a bone tissue repair substitute material at present because the hydroxyapatite HAs very similar composition with human skeleton component calcium phosphate salt, good biocompatibility and bone-promoting capability. However, hydroxyapatite also has disadvantages such as poor tensile strength and low toughness, which also largely limits the application of hydroxyapatite in implant materials.
In recent years, strontium ranelate has wide application in treating female osteoporosis, and the effect of strontium in bone repair is verified by people. After the strontium-containing medicine is introduced into patients with osteoporosis, the fracture risk is obviously reduced. Strontium is a natural trace element in human bone and has the effect of stimulating osteoblast differentiation.
However, a method for improving the performance of a titanium matrix implant by combining strontium, hydroxyapatite and titanium metal is not available so far, and if the method can be effectively combined, the method is a new attempt and must have wide application value.
Disclosure of Invention
The invention aims to provide a preparation method of a strontium titanate/strontium hydroxyapatite composite medical coating on the surface of titanium metal, which aims to overcome the defects of poor antibacterial property and biocompatibility of the existing medical titanium material. The method is characterized in that a uniform titanium dioxide nanotube array is generated by surface anodic oxidation, the titanium dioxide nanotube array is hydrothermally modified into a strontium titanate nanotube, a strontium-doped hydroxyapatite biological composite coating is electrochemically deposited on the surface of the strontium titanate nanotube array, strontium ions in the composite coating are gradually released into the environment around an implant along with time, the bone-promoting performance of the implant can be improved, the strontium hydroxyapatite coating on the surface of the strontium hydroxyapatite array is compact in structure and rough in surface, and compared with a pure titanium implant, the strontium hydroxyapatite array is beneficial to successful implantation of the implant in a human body; the electrochemical method and the hydrothermal method are combined, the condition is mild, and the biological performance of the conventional implant can be effectively improved.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a medical composite coating of strontium titanate/strontium hydroxyapatite on the surface of titanium metal comprises the following steps:
A. titanium pretreatment
Polishing the titanium sheet with the purity of more than or equal to 99.7% step by using SiC abrasive paper until the surface of the titanium sheet has no obvious scratch, ultrasonically washing the titanium sheet by using an organic reagent and deionized water, soaking the titanium sheet in a mixed acid solution for 10-15 seconds, and ultrasonically washing and drying the titanium sheet by using the deionized water;
B. anodic oxidation
B, taking the titanium sheet pretreated in the step A as an anode, taking a platinum sheet electrode as a cathode, carrying out anodic oxidation at room temperature, keeping the distance between the two electrodes at 5cm, and cleaning and drying the titanium sheet after anodic oxidation, and carrying out annealing treatment in a tubular furnace;
C. hydrothermal reaction
Adding the titanium sheet obtained in the step B into 16ml of Sr (OH)2Carrying out hydrothermal reaction in the solution at 200 ℃ for 1.5-2h, taking out, cleaning and drying;
D. electrochemical deposition
And D, placing the titanium sheet obtained in the step C in a mixed electrolyte of calcium salt and strontium salt for constant-current deposition, wherein the electrolyte comprises the following components: 0.034M-0.04M Ca (NO)30.02M-0.06M Sr (NO)30.025M NH4H2PO30.1M of Na (NO)3。
Further, in step A, the organic reagent is ethanol and acetone.
Further, in the step A, the mixed acid solution is HF and HNO3:H2O＝1:5:10vt％。
Further, in the step B, the anodic oxidation voltage is 30V-50V, and the anodic oxidation time is 1-2 h.
Further, step B, the annealing treatment specifically comprises the steps of: placing the titanium sheet in a tube furnace for temperature programming, firstly setting the temperature-raising rate to be 10 ℃/min, raising the temperature to 500 ℃, keeping the temperature for 2h, and then cooling the titanium sheet to the room temperature along with the furnace.
Further, step C, the Sr (OH)2The concentration of the solution is 0.018M-0.025M.
Step D, a three-electrode system is adopted in the constant-current deposition process, the titanium sheet obtained in the step C is used as a working electrode, a platinum electrode is used as a counter electrode, and a Saturated Calomel Electrode (SCE) is used as a reference electrode, wherein the constant-current deposition current density is 0.8-2mA/cm2The deposition time is 40-60 min.
Further, the electrolyte pH was maintained at 4.5, the deposition temperature was maintained at 65 ℃ and magnetic stirring was used.
Compared with the prior art, the invention has the beneficial effects that: the invention prepares a strontium-containing composite coating on the surface of a titanium substrate for the first time, wherein the coating is divided into a strontium-containing nanotube coating and a strontium-containing hydroxyapatite coating; strontium in the composite coating is gradually released into the human environment, and the effect of strontium ions on bone repair can be exerted; secondly, the rough surface appearance of the hydroxyapatite is also beneficial to the colonization of osteoblasts; wherein, the tubular titanium dioxide coating is selected to strengthen the mechanical embedding of the composite coating and the substrate, and the practical problem that the existing coating is easy to fall off can be solved.
Drawings
FIG. 1 is an electron micrograph of the titanium dioxide nanotube coating of example 1;
FIG. 2 Electron micrograph of strontium titanate coating in example 1;
FIG. 3 SEM image of example 1.
Detailed Description
Example 1
Cutting a titanium plate with the thickness of 1mm into titanium sheets with the size of 10x10mm, and gradually polishing the surfaces of the titanium sheets by 400, 800 and 1200 abrasive paper until the surfaces of the titanium sheets are smooth and have no obvious scratches. Then, the titanium sheet is respectively immersed in 10ml of ethanol, acetone and deionized water and ultrasonically cleaned for 10min, and cleaned and dried to remove impurities on the surface of the titanium sheet. Then, HF and HNO with the volume ratio of 1:5:10 are prepared3、H2And O, immersing the titanium sheet into mixed acid for 10-15s to remove the surface metal oxide film, cleaning and drying.
The pretreated titanium sheet is used as an anode, a platinum sheet electrode is used as a cathode, and anodic oxidation is carried out in 0.5 wt% of HF solution. The voltage was 50v and the oxidation time was 1 h. After cleaning and drying, annealing the titanium sheet, heating at a rate of 10 ℃/min, keeping the temperature at 500 ℃ for 90min, and then cooling with a furnace to obtain more stable anatase titanium dioxide.
The heat-treated titanium plate was immersed in 16ml of 0.02M Sr (OH)2In the solution, a 25ml high-pressure reaction kettle is selected as the reaction kettle. Carrying out hydrothermal reaction for 2h at 200 ℃, cooling, washing redundant solution on the surface by deionized water, and drying at 60 ℃ for later use.
And performing one-step constant-current deposition by taking the titanium sheet after the hydrothermal reaction as a substrate. The electrolyte composition is 0.034M Ca (NO)3，0.06MSr(NO)3，0.025M NH4H2PO3，0.1M Na(NO)3. The pH of the electrolyte was adjusted to 4.5, and the temperature was maintained at 65 ℃ during the electrochemical deposition with magnetic stirring. The deposition current was selected to be 1mA/cm2Deposition time 40 mm.
Example 2
Cutting a titanium plate with the thickness of 1mm into titanium sheets with the size of 10x10mm, and adopting 400, 800 and 120And (4) polishing the surface of the titanium sheet step by 0 abrasive paper until the surface of the titanium sheet is smooth and has no obvious scratch. Then, the titanium sheet is respectively immersed in 10ml of ethanol, acetone and deionized water and ultrasonically cleaned for 10min, and cleaned and dried to remove impurities on the surface of the titanium sheet. Then preparing HF and HNO with the volume ratio of 1:5:103、H2And O, immersing the titanium sheet into mixed acid for 10-15s to remove the surface metal oxide film, cleaning and drying.
The pretreated titanium sheet is used as an anode, a platinum sheet electrode is used as a cathode, and anodic oxidation is carried out in 0.5 wt% of HF solution. The voltage is 60v, and the oxidation time is 2 h. After cleaning and drying, annealing the titanium sheet, heating at a rate of 10 ℃/min, keeping at 500 ℃ for 90min, and then cooling with a furnace to obtain more stable anatase titanium dioxide.
The heat-treated titanium sheet was immersed in 16ml of 0.025M Sr (OH)2In the solution, a 25ml high-pressure reaction kettle is selected as the reaction kettle. Carrying out hydrothermal reaction for 2h at 200 ℃, cooling, washing redundant solution on the surface by deionized water, and drying at 60 ℃ for later use.
And performing one-step constant-current deposition by taking the titanium sheet after the hydrothermal reaction as a substrate. Electrolyte composition 0.04M Ca (NO)30.02M of Sr (NO)3，0.025M NH4H2PO3，0.1M Na(NO)3. The pH of the electrolyte was adjusted to 4.5, and the temperature was maintained at 65 ℃ during the electrochemical deposition with magnetic stirring. The deposition current is 2mA/cm2And the deposition time is 60 mm.
Claims (8)
1. A preparation method of a medical composite coating of strontium titanate/strontium hydroxyapatite on the surface of titanium metal is characterized by comprising the following steps:
A. titanium pretreatment
Gradually polishing titanium sheets with the purity of more than or equal to 99.7% by using SiC sand paper until no obvious scratch is formed on the surfaces, ultrasonically washing by using an organic reagent and deionized water, soaking in a mixed acid solution for 10-15 seconds, and ultrasonically washing and drying by using the deionized water;
B. anodic oxidation
B, taking the titanium sheet pretreated in the step A as an anode, taking a platinum sheet electrode as a cathode, carrying out anodic oxidation at room temperature, keeping the distance between the two electrodes at 5cm, and cleaning and drying the titanium sheet after anodic oxidation, and carrying out annealing treatment in a tubular furnace;
C. hydrothermal reaction
Adding the titanium sheet obtained in the step B into 16ml of Sr (OH)2Carrying out hydrothermal reaction in the solution at 200 ℃ for 1.5-2h, taking out, cleaning and drying;
D. electrochemical deposition
And D, placing the titanium sheet obtained in the step C in a mixed electrolyte of calcium salt and strontium salt for constant-current deposition, wherein the electrolyte comprises the following components: 0.034M-0.04M Ca (NO)30.02M-0.06M Sr (NO)30.025M NH4H2PO30.1M of Na (NO)3。
2. The preparation method of the medical composite coating of strontium titanate/strontium hydroxyapatite on titanium metal surface according to claim 1, characterized in that: step A, the organic reagent is ethanol and acetone.
3. The preparation method of the medical composite coating of strontium titanate/strontium hydroxyapatite on titanium metal surface according to claim 1, characterized in that: step A, the mixed acid solution is HF HNO3:H2O＝1:5:10vt％。
4. The preparation method of the medical composite coating of strontium titanate/strontium hydroxyapatite on titanium metal surface according to claim 1, characterized in that: and step B, the anodic oxidation voltage is 30V-50V, and the anodic oxidation time is 1-2 h.
5. The preparation method of the medical composite coating of strontium titanate/strontium hydroxyapatite on titanium metal surface according to claim 1, characterized in that: and step B, the annealing treatment comprises the following specific steps: placing the titanium sheet in a tube furnace for temperature programming, firstly setting the temperature-raising rate to be 10 ℃/min, raising the temperature to 500 ℃, keeping the temperature for 2h, and then cooling the titanium sheet to the room temperature along with the furnace.
6. The preparation method of the medical composite coating of strontium titanate/strontium hydroxyapatite on titanium metal surface according to claim 1, characterized in that: step C, the Sr (OH)2The concentration of the solution is 0.018M-0.025M.
7. The preparation method of the medical composite coating of strontium titanate/strontium hydroxyapatite on titanium metal surface according to claim 1, characterized in that: and D, adopting a three-electrode system in the constant-current deposition process, taking the titanium sheet obtained in the step C as a working electrode, a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, wherein the constant-current deposition current density is 0.8-2mA/cm2The deposition time is 40-60 min.
8. The preparation method of the medical composite coating of strontium titanate/strontium hydroxyapatite on titanium metal surface according to claim 7, characterized in that: the electrolyte pH was maintained at 4.5, the deposition temperature was maintained at 65 ℃ and magnetic stirring was used.
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| CN112875665A (en) * | 2021-02-07 | 2021-06-01 | 吉林大学 | Hydroxyapatite microspheres for injection filling preparation and preparation method thereof |
| CN113151828A (en) * | 2021-03-05 | 2021-07-23 | 中山大学 | Biological coating with osteogenic and antibacterial functions on titanium alloy surface and preparation method and application thereof |
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| CN113151828A (en) * | 2021-03-05 | 2021-07-23 | 中山大学 | Biological coating with osteogenic and antibacterial functions on titanium alloy surface and preparation method and application thereof |
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Application publication date: 20201225 |