CN114042187A - Preparation method of micro-area titanium oxide nanotube structure bone dental implant material - Google Patents
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Abstract
The invention provides a preparation method of a micro-area titanium oxide nanotube structure bone dental implant material, which comprises S1), carrying out anodic oxidation surface treatment on titanium or titanium alloy to obtain a surface nanotube structure; s2), carrying out ablation treatment on partial area of the titanium or titanium alloy surface nanotube structure to obtain micro-area bone dental implant material, wherein the bone dental implant material consists of the original nanotube structure area and an ablation structure area. The invention is realized by a mode of changing the structure of a micro-area nanotube of titanium and titanium alloy materials by focused laser beam selective induced ablation; the constructed micro-region nanotube structure bone dental implant material can simulate an intraosseous micro-nano multilevel structure to apply biomechanical signals to cells, and regulate osteogenic differentiation and osseointegration processes of bone marrow mesenchymal stem cells; the bone dental implant material can simulate a bone matrix micro-nano multilevel structure formed by assembling collagen fibers and hydroxyapatite in bones in space, and has the effects of regulating cell behaviors and remarkably promoting bones.
Description
Technical Field
The invention relates to the technical field of biomedical materials, in particular to a preparation method of a micro-area titanium oxide nanotube structure bone dental implant material.
Background
Titanium-based metal is one of the largest biological materials in clinical application, and is widely applied to bone and dental implantation instruments. However, the lack of bioactive structure on the titanium-based metal surface causes the problem of slow osteogenesis at the interface of the titanium-based implant instrument. Constructing a bionic functional structure on the surface of the titanium-based metal is an important way for improving the osteogenesis performance of the titanium-based metal. At present, a nanometer topological structure can be constructed on the surface of titanium-based metal through chemical and electrochemical treatment, and the osteogenesis speed can be accelerated to a certain extent, wherein the construction of the titanium dioxide nanotube through the electrochemical anodic oxidation technology is a method for improving the osteogenesis performance of the surface of a common titanium-based metal material, and a certain effect is achieved at present. The natural bone has a micro-nano multilevel structure, and the micro-nano structure of the bone tissue can exert a mechanical transduction effect on cells, regulate and control osteogenic differentiation of bone marrow mesenchymal stem cells on the surface of the titanium-based implant material, and accelerate interface osteogenesis.
Therefore, the construction of the titanium dioxide nanotube array structure with spatial distribution is expected to improve the osteogenesis performance of the material interface. At present, a periodic titanium dioxide nanotube array micro-area structure can be prepared by combining photoetching with electrochemical anodic oxidation, but the photoetching technology is high in cost, difficult to construct on the surface of a complex metal implant, and has the problems of photoresist pollution and the like.
In conclusion, no convenient and efficient method for constructing the surface of the titanium-based implant material with the periodic controllable micro-nano multilevel structure exists at present.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a micro-area titanium oxide nanotube structure bone dental implant material and a preparation method thereof.
The technical scheme of the invention is as follows: a preparation method of a micro-area titanium oxide nanotube structure bone dental implant material comprises the following steps:
s1), carrying out anodic oxidation surface treatment on the titanium or the titanium alloy to obtain a surface nanotube structure;
s2), performing ablation treatment on partial area of the titanium or titanium alloy surface nanotube structure to obtain a micro-area bone dental implant material, wherein the bone dental implant material consists of an original nanotube structure area and an ablation structure area;
the original nanotube structure area and the ablation structure area are adjacent, at least one of the original nanotube structure area and the ablation structure area is a plurality of independent areas, each independent area in the plurality of independent areas is a micro-area, and the micro-area refers to the micron-sized width, diameter and/or area of the independent area.
Preferably, in step S1), the surface nanotube structure is prepared in an acidic or alkaline electrolyte.
Preferably, in step S1), the surface nanotube structured material is a hollow nanotube-shaped structure with a high aspect ratio.
Preferably, in step S1), the titanium or titanium alloy surface nanotube structure is a nanotube structure with lateral dimension, longitudinal dimension and height dimension all in the range of 10-500 nm.
Preferably, in step S2), when the original nanotube structure region and the ablated structure region are both a plurality of independent regions, the original nanotube structure region and the ablated structure region are alternately arranged or periodically arranged.
Preferably, in step S2), when the original nanotube structure region is an entire region and the ablated structure region is a plurality of independent regions, the ablated structure regions are periodically arranged, and the original nanotube structure region is located around each ablated structure region.
Preferably, in step S2), the width of the independent area refers to a distance between two opposite straight lines or curved lines, and the distance between the two opposite straight lines or curved lines is smaller than the distance between the two opposite straight lines or curved lines forming the area. Wherein, the area is rectangular, and the width is micron-sized; the area is circular, and the diameter is micron-sized; the area is elliptical, and the minor axis is in the order of microns.
Preferably, in step S2), the ablation treatment is to perform laser treatment on a partial region of the nanotube structure on the surface of the titanium alloy by using a laser to ablate the partial region;
the laser treatment conditions are that the laser power is 0.1-100W and the scanning speed is 1-10000 mm/s.
Preferably, in step S2), the laser is a fiber laser, a gas laser, a solid laser, or a semiconductor laser.
Preferably, in step S2), the difference between the lengths of the surface nanotube structures in the original nanotube structure region and the laser ablation region is 1-500nm, and the difference between the diameters is 1-500 nm.
Preferably, in step S2), the width and diameter are in the range of 1-800 μm when they are in the micrometer range.
The invention has the beneficial effects that:
1. the invention is realized by a mode of changing the structure of a micro-area nanotube of titanium and titanium alloy materials by focused laser beam selective induced ablation; the micro-area nanotube structure bone dental implant material constructed by the invention can simulate an intraosseous micro-nano multilevel structure to apply biomechanical signals to cells, and regulate and control osteogenic differentiation and osseointegration processes of bone marrow mesenchymal stem cells;
2. the osteodental implant material can simulate a bone matrix micro-nano multilevel structure formed by assembling collagen fibers and hydroxyapatite in bone space, and has the effects of regulating cell behaviors and remarkably promoting bone;
3. the method is simple and efficient, and realizes the construction of the bone-imitating micro-nano multilevel structure implant material quickly, efficiently and accurately.
Drawings
FIG. 1 is a schematic diagram of the structural characteristics of the implant material of the micro-nano-tube structure according to the present invention;
FIG. 2 is a scanning electron microscope image of the structure of a micro-domain ablated titanium dioxide nanotube in example 1 of the present invention, wherein (a) is a low-power image showing periodically distributed micro domains of titanium dioxide nanotubes and micro domains of nanotube removal, (b) is a micro domain of titanium dioxide nanotubes, and (c) is a micro domain of nanotube removal;
fig. 3 is a spreading fluorescence staining pattern of the present invention in example 1, wherein (a) is a cell adhesion spreading fluorescence staining pattern of the micro-domain nanotube structure bone dental implant material in example 1, and (b) is a cell spreading fluorescence staining pattern of the medical pure titanium surface.
Detailed Description
The following further describes embodiments of the present invention with reference to the accompanying drawings:
the topological structure characteristic diagram of the micro-area nanotube structure bone dental implant material is shown in fig. 1, wherein the nanotube structure of the laser-unaffected micro-area is a nanotube structure (an example is a nanowire structure) constructed on the surface of the original titanium alloy; the laser-affected micro-areas (ablated areas) then cause the nanotube structure to be removed or converted to have new nanostructures due to the laser thermal effect.
Example 1
The embodiment provides a preparation method of a micro-area titanium oxide nanotube structure bone dental implant material, which comprises the following steps:
1) carrying out gradient polishing on the medical titanium material by using sand paper, then carrying out ultrasonic cleaning by using acetone, ethanol and deionized water, and carrying out vacuum drying;
2) carrying out anodic oxidation on the cleaned and dried medical titanium material in ammonium fluoride and oxalic acid solution to prepare a titanium dioxide nanotube coating;
the reaction conditions are as follows: ammonium fluoride concentration, oxalic acid concentration, voltage, electrochemical anodization time.
3) Focusing the fiber laser, and performing micro-area laser treatment on the titanium surface nanotube by using the fiber laser to initiate micro-area ablation so as to construct the osteo-dental implant material with different micro-area nanotube structure appearances; the conditions for laser ablation are: the laser power is 2.4W, the scanning speed is 80mm/s, and the scanning path is stripes which are periodically distributed at intervals of 100 mu m;
the bone dental implant material consists of an original nanotube structure area and an ablated nanotube structure area which are distributed at intervals in a stripe shape, and the width of the original nanotube structure area and the width of the ablated nanotube structure area are 100 mu m.
The morphology of the orthopaedics and dentistry implantation material prepared by the embodiment is shown in fig. 2 by a scanning electron microscope, and as can be seen from fig. 2(a), fig. 2(b) and fig. 2(c), the surface morphology of the material is changed due to laser ablation. The structure of the laser ablation micro-area tends to be flat, and the structure of the laser ablation micro-area is different from that of the original nanotube structure area.
In the osteodental implant material of the embodiment, the original nanotube structure area is adjacent to the ablated nanotube structure area, and the surface nanostructures of the adjacent micro-areas have differences.
The micro-area titanium dioxide nanotube implant material prepared by the embodiment can simulate a bone tissue micro-nano multilevel structure, applies biomechanical signals to stem cells to regulate osteogenic differentiation, and has a remarkable bone promoting effect. FIG. 3 is an alkaline phosphatase staining chart of the osteodental implant material of the micro-domain titanium dioxide nanotube according to the present embodiment; as can be seen from fig. 3(a) and (b), the micro-region titanium dioxide nanotube orthopedics implant material can significantly promote the expression of the bone mesenchymal stem cell alkaline phosphatase, thereby promoting osteogenic differentiation (cell seeding density 10000/mL, cell culture time 7 days).
Example 2
The embodiment provides a preparation method of a micro-area titanium oxide nanotube structure bone dental implant material, which comprises the following steps:
4) gradient polishing is carried out on the medical titanium material by using sand paper, and the medical titanium material is ultrasonically cleaned by acetone, ethanol and deionized water and is dried in vacuum;
5) and carrying out anodic oxidation on the cleaned and dried medical titanium material in ammonium fluoride and oxalic acid solution to prepare the titanium dioxide nanotube coating, wherein the reaction conditions are as follows: ammonium fluoride concentration, oxalic acid concentration, voltage, electrochemical anodization time;
6) focusing the fiber laser, and performing micro-area laser treatment on the titanium surface nanotube material by using the fiber laser to initiate micro-area ablation so as to construct the osteo-dental implant material with different micro-area nanotube structure morphologies;
the conditions for laser ablation are: the laser power is 2.4W, the scanning speed is 80mm/s, and the scanning path is a periodic 200-micrometer interval distribution stripe;
the bone dental implant material consists of an original nanotube structure area and an ablated nanotube structure area which are distributed at intervals in a stripe shape, and the width of the original nanotube structure area and the width of the ablated nanotube structure area are 200 mu m.
In the embodiment, the surface topography of the material is changed due to laser ablation, the structure of the laser ablation micro-area tends to be flat, and the difference of the structure of the nanotube with the original nanotube structure area is formed.
In the osteodental implant material of the embodiment, the original nanotube structure area is adjacent to the ablated nanotube structure area, and the nanotube structures on the surfaces of the adjacent micro areas are different.
Example 3
The embodiment provides a preparation method of a micro-area titanium oxide nanotube structure bone dental implant material, which comprises the following steps:
7) gradient polishing is carried out on the medical titanium material by using sand paper, and the medical titanium material is ultrasonically cleaned by acetone, ethanol and deionized water and is dried in vacuum;
8) and carrying out anodic oxidation on the cleaned and dried medical titanium material in ammonium fluoride and oxalic acid solution to prepare the titanium dioxide nanotube coating, wherein the reaction conditions are as follows: ammonium fluoride concentration, oxalic acid concentration, voltage, electrochemical anodization time.
9) Focusing the fiber laser, and performing micro-area laser treatment on the titanium surface nanotube material by using the fiber laser to initiate micro-area ablation so as to construct the osteo-dental implant material with different micro-area nanotube structure morphologies;
the conditions for laser ablation are: the laser power is 2.4W, the scanning speed is 80mm/s, the scanning path is a circular micro-area which is periodically arranged, the distance between the circle centers is 200 mu m, and the diameter of the circle is 100 mu m;
the bone dental implant material consists of an original nanotube structure and periodically distributed laser ablation structure areas, wherein the diameter of each laser ablation area is 100 mu m, and the circle center distance of the laser ablation areas is 200 mu m.
In this example, laser ablation causes changes in the surface topography of the material. The structure of the laser ablation micro-area tends to be flat, and the structure of the laser ablation micro-area is different from that of the original nanotube structure area.
In the osteodental implant material of the embodiment, the original nanotube structure area is adjacent to the ablated nanotube structure area, and the nanotube structures on the surfaces of the adjacent micro areas are different.
Example 4
The embodiment provides a preparation method of a micro-area titanium oxide nanotube structure bone dental implant material, which comprises the following steps:
10) gradient polishing is carried out on the medical titanium material by using sand paper, and the medical titanium material is ultrasonically cleaned by acetone, ethanol and deionized water and is dried in vacuum;
11) and carrying out micro-arc oxidation on the cleaned and dried medical titanium material in ammonium fluoride and oxalic acid solution to prepare the titanium dioxide nanotube coating, wherein the reaction conditions are as follows: ammonium fluoride concentration, oxalic acid concentration, voltage, electrochemical anodization time.
12) Focusing the fiber laser, and performing micro-area laser treatment on the titanium surface nanotube material by using the fiber laser to initiate micro-area ablation so as to construct the osteo-dental implant material with different micro-area nanotube structure morphologies;
the conditions for laser ablation are: the laser power is 2.4W, the scanning speed is 80mm/s, and the scanning path is a periodic 200-micrometer interval distribution stripe;
the bone dental implant material consists of an original nanotube structure area and an ablated nanotube structure area which are distributed at intervals in a stripe shape, and the width of the original nanotube structure area and the width of the ablated nanotube structure area are 200 mu m.
In this example, laser ablation causes changes in the surface topography of the material. The structure of the laser ablation micro-area tends to be flat, and the structure of the laser ablation micro-area is different from that of the original nanotube structure area.
In the osteodental implant material of the embodiment, the original nanotube structure area is adjacent to the ablated nanotube structure area, and the surface nanostructures of the adjacent micro-areas have differences.
The foregoing embodiments and description have been presented only to illustrate the principles and preferred embodiments of the invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention as hereinafter claimed.
Claims (10)
1. A preparation method of a micro-area titanium oxide nanotube structure bone dental implant material is characterized by comprising the following steps:
s1), carrying out anodic oxidation surface treatment on the titanium or the titanium alloy to obtain a surface nanotube structure;
s2), performing ablation treatment on partial area of the titanium or titanium alloy surface nanotube structure to obtain a micro-area bone dental implant material, wherein the bone dental implant material consists of an original nanotube structure area and an ablation structure area;
the original nanotube structure area and the ablation structure area are adjacent, at least one of the original nanotube structure area and the ablation structure area is a plurality of independent areas, each independent area in the plurality of independent areas is a micro-area, and the micro-area refers to the micron-sized width, diameter and/or area of the independent area.
2. The method for preparing the micro-area titanium oxide nanotube structure bone dental implant material according to claim 1, wherein the method comprises the following steps: in step S1), the surface nanotube structure is prepared in an acidic or alkaline electrolyte.
3. The method for preparing the micro-area titanium oxide nanotube structure bone dental implant material according to claim 2, wherein the method comprises the following steps: in step S1), the surface nanotube structure material is a hollow nanotube-like structure with a high aspect ratio;
and the titanium or titanium alloy surface nanotube structure is a nanotube structure with the transverse dimension, the longitudinal dimension and the height dimension of 10-500 nm.
4. The method for preparing the micro-area titanium oxide nanotube structure bone dental implant material according to claim 1, wherein the method comprises the following steps: step S2), when the original nanotube structure region and the ablation structure region are both multiple independent regions, the original nanotube structure region and the ablation structure region are arranged alternately or periodically.
5. The method for preparing the micro-area titanium oxide nanotube structure bone dental implant material according to claim 1, wherein the method comprises the following steps: step S2), when the original nanotube structure region is an integral region and the ablation structure region is a plurality of independent regions, the ablation structure regions are periodically arranged, and the periphery of each ablation structure region is the original nanotube structure region.
6. The method for preparing the micro-area titanium oxide nanotube structure bone dental implant material according to claim 1, wherein the method comprises the following steps: in step S2), the width of the independent area refers to a distance between two opposite straight lines or curves, and the distance between the two opposite straight lines or curves is smaller than the distance between other opposite straight lines or curves forming the area.
7. The method for preparing the micro-area titanium oxide nanotube structure bone dental implant material according to claim 1, wherein the method comprises the following steps: in the step S2), the ablation treatment is to perform laser treatment on a partial region of the titanium alloy surface nanotube structure by using a laser to ablate the partial region;
the laser treatment conditions are that the laser power is 0.1-100W and the scanning speed is 1-10000 mm/s.
8. The method for preparing the micro-area titanium oxide nanotube structure bone dental implant material according to claim 7, wherein the method comprises the following steps: in step S2), the laser is a fiber laser, a gas laser, a solid laser, or a semiconductor laser.
9. The method for preparing the micro-area titanium oxide nanotube structure bone dental implant material according to claim 1, wherein the method comprises the following steps: in step S2), the difference between the lengths of the surface nanotube structures in the original nanotube structure region and the laser ablation region is 1-500nm, and the difference between the diameters is 1-500 nm.
10. The method for preparing the micro-area titanium oxide nanotube structure bone dental implant material according to claim 1, wherein the method comprises the following steps: in step S2), when the width and the diameter are in micron order, the width and the diameter are 1-800 μm.
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