CN119818720A - Surface dual drug release system of titanium-based implant, preparation method and application thereof - Google Patents
Surface dual drug release system of titanium-based implant, preparation method and application thereof Download PDFInfo
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Abstract
本发明属于医用材料技术领域，涉及一种钛基植入体表面双重药物释放系统及其制备方法与应用。包括钛基植入体和贴合在其表面的水凝胶层，钛基植入体表面为纳米管阵列结构，钛基植入体与水凝胶层之间设有氧化锌纳米颗粒和上转换发光材料颗粒，水凝胶层内装载MgO2纳米颗粒；其中，所述上转换发光材料颗粒的材质为NaYF4:Yb3+,Er3+，水凝胶层由明胶‑海藻酸钠水凝胶构成。本发明提供的钛基植入体表面双重药物释放系统不仅能够实现不同药物的装载，可以用于治疗多种疾病，而且具有较好的时序控制效果，作用时间长，成本低，具有广阔的应用前景。
The present invention belongs to the technical field of medical materials, and relates to a dual drug release system on the surface of a titanium-based implant, and a preparation method and application thereof. It includes a titanium-based implant and a hydrogel layer attached to its surface, the surface of the titanium-based implant is a nanotube array structure, zinc oxide nanoparticles and upconversion luminescent material particles are arranged between the titanium-based implant and the hydrogel layer, and MgO2 nanoparticles are loaded in the hydrogel layer; wherein the material of the upconversion luminescent material particles is NaYF4 : Yb3 + , Er3 + , and the hydrogel layer is composed of gelatin-sodium alginate hydrogel. The dual drug release system on the surface of the titanium-based implant provided by the present invention can not only realize the loading of different drugs, but also can be used to treat a variety of diseases, and has a good timing control effect, a long action time, low cost, and broad application prospects.
Description
Technical Field
The invention belongs to the technical field of medical materials, and relates to a titanium-based implant surface dual drug release system, and a preparation method and application thereof.
Background
The disclosure of this background section is only intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art.
Osteosarcoma is a primary malignancy common in children and adolescents. The existing treatment means mainly remove peripheral residual tumor cells and tissues by means of chemotherapy, radiotherapy and the like after surgical excision. However, this treatment has significant drawbacks. Chemotherapy and radiotherapy can damage surrounding normal tissues and cells, and tumor tissues and cells which are not removed from the surrounding are even at risk of recurrence. Meanwhile, the filling part is extremely easy to be infected by bacteria. Meanwhile, differences exist among different patients, and mass production of titanium implants is difficult. Among the numerous implant materials, 3D printed titanium and its alloys have been widely used for the treatment of bone tissue defects due to their good combination of properties. However, 3D printed titanium implants have limited surface binding to surrounding bone tissue and limited anti-tumor and anti-infection capabilities.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a titanium-based implant surface dual drug release system, a preparation method and application thereof, the titanium-based implant surface dual drug release system provided by the invention not only can realize loading of different drugs, can be used for treating various diseases, but also has a good time sequence control effect, long action time, low cost and wide application prospect.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the surface dual drug release system of the titanium-based implant comprises a titanium-based implant body and a hydrogel layer attached to the surface of the titanium-based implant body, wherein the surface of the titanium-based implant body is of a nanotube array structure, zinc oxide nano particles and up-conversion luminescent material particles are arranged between the titanium-based implant body and the hydrogel layer, mgO 2 nano particles are loaded in the hydrogel layer, the up-conversion luminescent material particles are made of NaYF 4: Yb3+, Er3+, and the hydrogel layer is made of gelatin-sodium alginate hydrogel.
Firstly, micro-nano structure and zinc ions have proved to have bone and antibacterial effects, so the invention firstly adopts a nanotube array structure on the surface of the titanium-based implant and loads zinc oxide nano particles, so that the titanium-based implant has the bone and antibacterial effects. Secondly, magnesium peroxide has multiple effects of promoting bones, resisting bacteria and resisting tumors, so the invention adds the magnesium peroxide into a system. However, magnesium peroxide is chemically active and difficult to directly attach to the surface of a titanium-based implant compared to metal oxide, and thus the present invention adopts a hydrogel loading method, and is disposed on the titanium-based implant through a hydrogel layer. Meanwhile, up-conversion luminescent material particles are arranged, and degradation of a hydrogel system is accelerated through the photo-thermal conversion capability of the up-conversion luminescent material particles, so that release of magnesium peroxide and delayed release of zinc oxide nanoparticles are realized. The NaYF 4: Yb3+, Er3+ is selected to have good biocompatibility, so that the normal function of the titanium-based implant is maintained, and meanwhile, the NaYF 4: Yb3+, Er3+ is matched with gelatin-sodium alginate hydrogel, so that the release of double medicaments is facilitated.
In a second aspect, a method for preparing the surface dual drug delivery system of a titanium-based implant comprises the following steps:
preparing MgO 2 nano-particles, and loading MgO 2 nano-particles into the hydrogel;
Removing residual particles on the surface of the titanium-based implant by adopting an acid etching method and an anodic oxidation method, and constructing a nanotube array on the surface of the titanium-based implant to obtain a pretreated titanium-based implant;
firstly depositing zinc oxide nano particles on the surface of a pretreated titanium-based implant, and then depositing up-conversion luminescent material particles on the surface of the pretreated titanium-based implant by a hydrothermal method to obtain a surface double-modified titanium-based implant;
And coating the hydrogel loaded with MgO 2 nano particles on the surface of the titanium-based implant to obtain the nano-sized MgO-nanoparticle.
The method deposits zinc oxide nano particles on the surface of the pretreated titanium-based implant, which is beneficial to the subsequent deposition of NaYF 4: Yb3 +, Er3+ on the surface of the pretreated titanium-based implant, and meanwhile, the method avoids the inactivation of NaYF 4: Yb3+, Er3+ caused by the deposition of NaYF 4: Yb3+, Er3+ and then the deposition of zinc oxide nano particles because the preparation process of the zinc oxide nano particles needs pyrolysis.
In the anodic oxidation, titanium is used as an anode in electrolyte based on fluoride, constant voltage is applied, titanium dioxide nano tubes are generated on the surface, in the anodic oxidation process, titanium reacts with the electrolyte under the action of an electric field to generate a titanium dioxide layer, but the titanium dioxide layer can prevent electrochemical reaction, at the moment, the titanium dioxide reacts with F - in the solution to generate water-soluble [ TiF 6]2-, a titanium substrate is exposed, a closely arranged nano tube array is formed in dynamic circulation of dissolution and generation, and the nano tubes gradually extend towards a substrate along with the extension of time, so that the length gradually increases, and the reaction equation is as follows:
in a third aspect, the use of a titanium-based implant surface dual drug delivery system as described above for the preparation of an implant material for the treatment of osteosarcoma.
The beneficial effects of the invention are as follows:
According to the titanium-based implant surface dual-drug release system provided by the invention, under the cooperation of the up-conversion luminescent material and the hydrogel, the dual-drug release can be realized under the excitation of near infrared light (with the wavelength of 808 nm), so that the system has a good time sequence control effect and a long action time.
The preparation method comprises the steps of firstly constructing a nanotube array on the surface of a titanium-based implant, attaching zinc oxide nano particles to the nanotube array to construct a first heavy zinc ion release system, then further depositing up-conversion luminescent material particles on the surface of the titanium-based implant through hydrothermal treatment to construct a photo-thermal switch, loading MgO 2 nano particles through a gelatin-sodium alginate system, and coating the MgO 2 nano particles on the titanium-based implant to construct a second heavy drug release system. Under the irradiation of near infrared light, the surface temperature is increased, the degradation of the hydrogel system is accelerated, and then the release of the medicine is realized, so that the preparation of the dual medicine release system is completed. The method has strong operability, better time sequence control effect, long acting time and lower cost, can realize loading of different medicines, is used for treating various diseases, and has wide application prospect.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a Scanning Electron Microscope (SEM) picture of magnesium peroxide particles prepared according to example 1 of the present invention;
FIG. 2 is a Transmission Electron Microscope (TEM) image of the magnesium peroxide particles prepared in example 1 of the present invention;
FIG. 3 is an SEM image of a surface-once-modified implant prepared according to example 1 of the present invention;
FIG. 4 is an SEM image of a surface dual modified titanium-based implant prepared according to example 1 of the present invention;
FIG. 5 is an SEM image of a partially immersed hydrogel crosslinked titanium-based implant prepared in example 1 of the present invention, with the left side being the non-immersed hydrogel and the right side being the immersed hydrogel;
FIG. 6 is an enlarged surface SEM image of a dual drug delivery system for a titanium-based implant surface prepared according to example 1 of the present invention;
FIG. 7 is a graph showing the result of photo-thermal conversion of the surface dual modified titanium-based implant prepared in example 1 of the present invention;
FIG. 8 is a graph showing the Mg ion release profile of a surface dual modified titanium-based implant prepared in example 1 of the present invention;
FIG. 9 is a Zn ion release curve of a surface double modified titanium-based implant prepared in example 1 of the present invention;
FIG. 10 is a curcumin release profile of a surface double modified titanium-based implant prepared in example 2 of the present invention;
FIG. 11 is a paclitaxel release profile of a surface dual modified titanium-based implant prepared in example 3 of the present invention;
FIG. 12 is a graph showing the results of the expression of an osteogenic related gene in mesenchymal stem cells according to an embodiment of the present invention, wherein A is the ALP gene, B is BMP-2, C is Runx-2, D is OPN, E is OCN, and F is Col-I;
FIG. 13 is a graph showing the results of the activity detection of osteosarcoma cells with or without near infrared illumination according to the present invention, wherein A is no near infrared illumination and B is near infrared illumination;
FIG. 14 is a graph showing the results of bacterial plate coating in examples of the present invention.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present invention. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
In order to solve the problems of limited binding capacity of the surface of the titanium implant and surrounding bone tissues, limited anti-tumor and anti-infection capacity and the like, the invention provides a dual drug release system for the surface of the titanium implant and a preparation method and application thereof.
The invention provides a surface dual drug release system of a titanium-based implant, which comprises a titanium-based implant and a hydrogel layer attached to the surface of the titanium-based implant, wherein the surface of the titanium-based implant is of a nanotube array structure, zinc oxide nano particles and up-conversion luminescent material particles are arranged between the titanium-based implant and the hydrogel layer, mgO 2 nano particles are loaded in the hydrogel layer, the up-conversion luminescent material particles are made of NaYF 4: Yb3+, Er3+, and the hydrogel layer is made of gelatin-sodium alginate hydrogel.
In some embodiments, the titanium-based implant is a porous titanium-based implant. Specifically, the porous titanium-based implant has a three-period extremely small curved surface structure. Specifically, the pore diameter of the porous titanium-based implant is 600-800 mu m. Specifically, the porosity of the porous titanium-based implant is 65-75%.
In some embodiments, the titanium-based implant is a Ti-6Al-4V implant.
In some embodiments, the hydrogel layer also has an active drug loaded therein. In particular, the active drug comprises curcumin and/or paclitaxel.
In another embodiment of the present invention, a method for preparing the surface dual drug delivery system of a titanium-based implant is provided, comprising the steps of:
preparing MgO 2 nano-particles, and loading MgO 2 nano-particles into the hydrogel;
Removing residual particles on the surface of the titanium-based implant by adopting an acid etching method and an anodic oxidation method, and constructing a nanotube array on the surface of the titanium-based implant to obtain a pretreated titanium-based implant;
firstly depositing zinc oxide nano particles on the surface of a pretreated titanium-based implant, and then depositing up-conversion luminescent material particles on the surface of the pretreated titanium-based implant by a hydrothermal method to obtain a surface double-modified titanium-based implant;
And coating the hydrogel loaded with MgO 2 nano particles on the surface of the titanium-based implant to obtain the nano-sized MgO-nanoparticle.
In some embodiments, mgO nanoparticles are produced with hydrogen peroxide by a metathesis reaction to produce MgO 2 nanoparticles. Specifically, the process of preparing MgO 2 nano-particles is performed in an alcohol solvent. The alcohol solvent of the present invention may be methanol, ethanol, isopropanol, etc., more specifically, the alcohol solvent is ethanol.
In some embodiments, the titanium-based implant is prepared using a selective laser melting (SELECTIVE LASER MELTING, SLM) technique.
In some embodiments, the acid solution used in the acid etch process is a mixed solution of hydrofluoric acid and nitric acid.
In some embodiments, the anodic oxidation is performed using a 24-26V DC power supply.
In some embodiments, the anodic oxidation process is performed in an aqueous NH 4 F-glycerol solution.
In some embodiments, depositing zinc oxide nanoparticles on the surface of the pretreated titanium-based implant is performed by immersing the pretreated titanium-based implant in a zinc salt solution and then pyrolysing to convert the zinc salt to zinc oxide. Specifically, the pyrolysis condition is that the vacuum heating is carried out to 400-500 ℃. The zinc salt is a compound with cations of zinc ions, such as zinc nitrate, zinc sulfate, zinc acetate and the like. Specifically, the zinc salt adopted by the invention is zinc acetate.
In some embodiments, the process of depositing up-conversion luminescent material particles comprises adding the pretreated titanium-based implant into a solution containing urea, yttrium salt, ytterbium salt and erbium salt, heating to 85-95 ℃ for soaking, then adding into a mixed solution containing NaF and HF for hydrothermal treatment, and then washing and drying. The hydrothermal treatment of the present invention is a method of treating a reaction system under a high pressure state by heating the reaction system under a closed condition with water as a solvent. Specifically, the temperature of the hydrothermal treatment is 100-110 ℃. Specifically, the time of the hydrothermal treatment is 20-40 min. The yttrium salt refers to a compound of which the cation is yttrium ion, such as yttrium nitrate and the like. The ytterbium salt in the invention refers to a compound of which the cation is ytterbium ion, such as ytterbium nitrate and the like. The erbium salt refers to a compound of which the cations are erbium ions, such as erbium nitrate and the like.
Specifically, the molar ratio of yttrium salt to ytterbium salt to erbium salt is 200-300:60-70:5-10, preferably 240-260:60-65:5-7.
In a third embodiment of the present invention, there is provided an application of the above-mentioned dual drug delivery system for titanium-based implant surfaces in preparing implant materials for treating osteosarcoma.
In order to enable those skilled in the art to more clearly understand the technical scheme of the present invention, the technical scheme of the present invention will be described in detail with reference to specific embodiments.
Examples
The preparation method of the titanium-based implant surface dual drug release system comprises the following steps:
MgO 2 preparation method:
MgO nanoparticles were ultrasonically dispersed in absolute ethanol, followed by adding hydrogen peroxide and stirring for 4 hours, and the resulting solution was transferred into a centrifuge tube, centrifuged at high speed for 5min, and then in a vacuum oven overnight. The obtained product is MgO 2 nano-particles.
The preparation method of the sample comprises the following steps:
a porous Ti-6Al-4V implant (denoted Ti) based on a three-period minimum curved surface, having a pore size of 700 μm and a porosity of 70% was prepared using a selective laser melting technique.
Preparing a mixed acid solution from 65% nitric acid, 40% hydrofluoric acid and water according to a volume ratio of 31:5:64, carrying out mobile acid etching treatment on the implant by using the mixed acid solution of 90 s, and carrying out anodic oxidation treatment on the implant in an aqueous solution of NH 4 F-glycerol (NH 4 F with a concentration of 0.27 mol.L -1 and a volume ratio of glycerol to water of 1:1) under a direct-current voltage of 25V for 1h, and drying to obtain the pretreated implant.
The pretreated implant (10×10× mm 3) was immersed in 50 mL of a 0.3mmol·l -1 zinc acetate solution, taken out, and then vacuum-heated at 450 ℃ for 2h to obtain a surface-once modified implant (denoted as ti—zn).
0.25 G urea was dissolved in 25 mL deionized water, and then 250 μ L Y (NO 3)3, 0.63M of 100 μl Yb (NO 3)3 and 0.4M of 15 μl Er (NO 3)3) were sequentially added at a concentration of 1.0M to obtain a rare earth mixed solution.
The implant with the surface modified at one time is placed in rare earth mixed solution and soaked in water bath at 90 ℃ for 3 h. Taking out, adding into 20mL of mixed solution of NaF (0.01 g.mL -1) and HF (0.03 mol.L -1), placing into a 30 mL hydrothermal reaction kettle, performing hydrothermal treatment at 100 ℃ for 30min, taking out, performing ultrasonic cleaning in deionized water, and drying in air to obtain the titanium-based implant with double modified surfaces.
Preparing gelatin-sodium alginate hydrogel, namely weighing 0.5g gelatin and 0.125g sodium alginate, weighing 100 mug MgO 2 nano particles, heating, stirring and dissolving the nano particles in 5mL deionized water, cooling the hydrogel, immersing the titanium-based implant with double modified surfaces in the hydrogel for 5 minutes, using 2% CaCl 2 solution, and crosslinking for 5 minutes at room temperature to complete filling of the surface and the interior of the implant (marked as Ti-Zn-Mg).
The magnesium peroxide particles synthesized in this example are shown in fig. 1 to 2, which shows that the particle size of the magnesium peroxide particles synthesized in this example is about 80 nm.
As shown in fig. 3, the implant of this example forms nanotubes in an ordered arrangement after the acid etching anodic oxidation treatment, and ZnO nanoparticles are formed around the nanotubes.
As shown in fig. 4, in the surface double-modified titanium-based implant prepared in this example, square rare earth element particles were deposited on the surface of the nanotube.
To demonstrate the difference between before and after coating the hydrogel, this example additionally takes a titanium-based implant with a surface double modified partially immersed in the hydrogel for 5 minutes, crosslinked at room temperature for 5 minutes using 2% CaCl 2 solution, and as a result, as shown in fig. 5, no gel was added to the left side, the gel was added to the right side, and it was observed that residual particles during 3D printing were completely removed and micro-scale pits were formed on the surface, and in addition, a loose porous structure was formed after the gel was added, confirming that the gel was filled into the porous implant. Meanwhile, the hydrogel has larger specific surface area and forms larger holes, as shown in fig. 6.
Example 2
The same as in example 1, except that 75. Mu.g of curcumin was also added to the hydrogel.
Example 3
The same as in example 1, except that 17. Mu.g of paclitaxel was also added to the hydrogel.
Performance test:
surface temperature monitoring:
The surface double modified titanium-based implant prepared in example 1 was irradiated with near infrared light (wavelength 808 nm), and the photo-thermal conversion effect was examined, and the result is shown in fig. 7, which shows that the surface temperature was increased under irradiation of near infrared light to achieve photo-thermal conversion, and the temperature was finally stabilized at about 53 ℃.
Drug release detection:
Experimental method to evaluate the ion and drug release behavior of the samples, the samples were placed in 1ml of 37 ℃ PBS solution for 60 days while one group of samples was irradiated with 808nm near infrared light for 10 minutes per day. Samples were evaluated for ion and drug release behavior every 3 days. Determination of Zn 2+ and Mg 2+ release concentrations was performed using inductively coupled plasma mass spectrometry. And the loading of the drug on the surface can be determined through calculation of curcumin and paclitaxel. For curcumin, absorbance was measured at 428nm using an ultraviolet-visible spectrophotometer. For paclitaxel, the measurement was performed at 230 nm. The release concentration was characterized by the standard curve obtained.
As shown in the results of figures 8-11, after photo-thermal addition, the release rate of Mg is obviously improved, the first re-release effect is finished in advance, and the release effects of curcumin and paclitaxel are the same as the release effects of Mg. In addition, under the action of photo-heat, release of the second drug (i.e., zinc) is advanced, and the release result is reached in advance, as shown in fig. 9.
RT-qPCR detection of mesenchymal stem cell osteoblast related genes:
Experimental methods cells were seeded onto the sample surface at a density of 1X 10 5 cells/mL. After 7 days and 14 days of incubation, the cells on the sample surface were washed with PBS. mu.L of Trizol-lysed cells were added to each sample well. RNA concentration was measured using a spectrophotometer at 260/280 nm. The RNA was then converted to cDNA using a reverse transcription kit. ALP, OCN, col-I, BMP-2, OPN and Runx-2 were selected as target genes for detection, and GAPDH was selected as an internal gene to normalize the expression level of the target gene. Detection was performed using a real-time fluorescent quantitative PCR instrument and calculation and analysis of sample results were performed using a relative quantitative comparison method (2 -ΔΔCT method).
As a result, as shown in FIG. 12, the expression of the osteogenic related gene in the mesenchymal stem cells was significantly enhanced under the action of the dual release system, contributing to the next new bone formation.
CCK-8 assay for cell viability of osteosarcoma cells:
Experimental methods cells were seeded at a density of 2X 10 4 cells/mL on the surface of a porous sample of size 10X 2mm 3 placed in a 24 well plate. After 1,4,7 days of incubation, the sample was transferred to a new sample well, and 1mL of medium and 100. Mu. LCCK-8 stain were added to the well. After incubation for 1h in a 37 ℃ incubator, 200 μl of liquid was pipetted into a 96-well plate. Absorbance of each set of samples was measured at 450nm using an enzyme-labeled instrument.
As a result, as shown in FIG. 13, in the absence of near infrared irradiation, mgO 2 was slowly released to decrease the cell viability, while in the presence of near infrared irradiation, the surface temperature was increased, the degradation and release of hydrogel were accelerated, and at the same time, the tumor cell viability was significantly decreased under the therapeutic effect of photothermal and photodynamic.
Bacterial plate coating
The experimental method is that a 24-well plate inoculated with bacterial liquid is placed in a 37 ℃ constant temperature incubator for culture for 24 hours, the concentration of the bacterial liquid is 1 multiplied by 10 5CFU·mL-1, then a sample is transferred into a new sample hole, 1mL of PBS is added into each hole, and living bacteria are blown off from the surface. The resulting solution was then diluted 10-fold with PBS. Thereafter, the liquid was dropped into a petri dish containing LB solid medium, and the liquid was spread evenly using a sterilized glass bent rod. The dishes were placed in a 37℃incubator for 12 hours, and after removal, the colonies were photographed for size.
As a result, as shown in FIG. 14, the MgO 2 particles significantly inhibited the bacterial growth, and the colony forming area was further significantly reduced under the effects of photothermal treatment and gel-accelerated release.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
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| CN120420497A (en) * | 2025-07-08 | 2025-08-05 | 山东大学 | Near infrared light response titanium-based implant, and preparation method and application thereof |
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| WO2008000888A2 (en) * | 2006-06-28 | 2008-01-03 | Vivoxid Oy | Implant containing a source of oxygen |
| DE102009016554A1 (en) * | 2009-02-19 | 2010-09-09 | Heraeus Kulzer Gmbh | Medical implant i.e. dental implant, for implanting in human body, has metallic body comprising surface layer which contains calcium and/or phosphorus, where zirconium and/or zirconium dioxide are stored in surface layer |
| US20160325112A1 (en) * | 2009-08-30 | 2016-11-10 | Stephen Eliot Zweig | Photon upconverting implantable medical devices |
| EP3666932A1 (en) * | 2018-12-14 | 2020-06-17 | Nano-implant Sp. z o.o. | Production method of a personalised, biocompatible and bioactive orthopaedic implant |
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| WO2008000888A2 (en) * | 2006-06-28 | 2008-01-03 | Vivoxid Oy | Implant containing a source of oxygen |
| DE102009016554A1 (en) * | 2009-02-19 | 2010-09-09 | Heraeus Kulzer Gmbh | Medical implant i.e. dental implant, for implanting in human body, has metallic body comprising surface layer which contains calcium and/or phosphorus, where zirconium and/or zirconium dioxide are stored in surface layer |
| US20160325112A1 (en) * | 2009-08-30 | 2016-11-10 | Stephen Eliot Zweig | Photon upconverting implantable medical devices |
| EP3666932A1 (en) * | 2018-12-14 | 2020-06-17 | Nano-implant Sp. z o.o. | Production method of a personalised, biocompatible and bioactive orthopaedic implant |
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| CN120420497A (en) * | 2025-07-08 | 2025-08-05 | 山东大学 | Near infrared light response titanium-based implant, and preparation method and application thereof |
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