CN102145192A - Metal implant and surface treatment method thereof - Google Patents
Metal implant and surface treatment method thereof Download PDFInfo
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- CN102145192A CN102145192A CN2010101139808A CN201010113980A CN102145192A CN 102145192 A CN102145192 A CN 102145192A CN 2010101139808 A CN2010101139808 A CN 2010101139808A CN 201010113980 A CN201010113980 A CN 201010113980A CN 102145192 A CN102145192 A CN 102145192A
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- fiber network
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Abstract
The invention discloses a metal implant and a surface treatment method thereof. A plurality of micron-sized pits are arranged on the surface of the metal implant, the micron-sized pits comprise a nano-sized fiber network, the aperture of the micron-sized pits is 1 micron to 100 microns, the nano-sized fiber network contains a plurality of nano-sized holes, and the aperture of the nano-sized holes is 10 nanometers to 1000 nanometers. The method comprises the following steps: providing the metal implant; performing primary surface treatment on the surface of the metal implant so as to form the plurality of micron-sized pits on the surface of the metal implant; and performing secondary surface treatment on the surface of the metal implant so as to form the nano-sized fiber network in the micron-sized pits, wherein the nano-sized fiber network contains the plurality of nano-sized holes, and the aperture of the nano-sized holes is 10 nanometers to 1000 nanometers. The external micro-sized pits can protect the structure of the nano-sized fiber network and reduce the risk of damaging the structure of the nano-sized fiber network during an implantation operation.
Description
Technical field
The present invention relates to a kind of metal implant and surface-treated method thereof, and relate in particular to a kind of surface morphology has a nano-scale fiber network for the micron order pothole metal implant and surface-treated method thereof.
Background technology
At present, the method that forms loose structure on metal implant (implant) surface has multiple, for example: sand-blast (sand blasting) or aciding (acid etching), by said method the surface roughness of metal implant is increased, so can be beneficial to metal implant implantable bioartificial body inner posterior quadrant and seek connections with and impel wound healing time to shorten.
For instance, United States Patent (USP) font size US5609633 discloses a kind of surface treatment method of metal implant, the method is utilized alkaline etching collocation heat treatment (Alkali-heat treatment, AH) condition, can on the surface of metal implant, produce nanofiber layer, this nanofiber layer can promote the calcium phosphate deposition, has the osteocyte inductivity, and the osteocyte inductivity then can be quickened implant surrounding tissue rate of reconstitution.
But the surface treatment method of this metal implant is very fragile in the nanofiber layer that the metal implant surface is produced, and is just destroyed in the implant surgery process easily.
Summary of the invention
The invention provides a kind of metal implant, its surface morphology has a nano-scale fiber network for the micron order pothole.
In addition, the present invention provides a kind of surface-treated method of metal implant in addition, can produce a kind of surface morphology has a nano-scale fiber network for the micron order pothole metal implant.
The present invention proposes a kind of metal implant, the surface of metal implant has a plurality of micron order potholes, and the micron order pothole has a nano-scale fiber network, the aperture of its micron order pothole is between 1 micron to 100 microns, the nano-scale fiber network comprises a plurality of nanoscale holes, and the aperture of nanoscale hole is between 10 nanometer to 1000 nanometers.
In an embodiment of the present invention, wherein said micron order pothole also comprises a plurality of sub-micron grade potholes, and the aperture of those sub-micron grade potholes is between 100 nanometer to 1000 nanometers.
In an embodiment of the present invention, wherein said metal implant is the alloy that a titanium or contains titanium elements.
In an embodiment of the present invention, wherein said micron order pothole is to produce by acid etching technology after a blasting treatment or the sandblast.
In an embodiment of the present invention, wherein said nano-scale fiber network is handled by an alkaline etching or alkaline etching is handled collocation one pickling processes and a heat treatment produces.
In an embodiment of the present invention, the composition of wherein said nano-scale fiber network is a rutile phase oxidation titanium or an anatase phase oxidation titanium.
In addition, the present invention proposes a kind of surface treatment method of metal implant, comprising: a metal implant is provided; Carry out a first surface on the surface of this metal implant and handle, form a plurality of micron order potholes with surface at this metal implant; And carry out a second surface on the surface of this metal implant and handle, to generate a nano-scale fiber network at those micron order potholes, wherein this second surface treatment step is that an alkaline etching is handled.
In an embodiment of the present invention, wherein said alkaline etching more comprises a pickling processes and a heat treatment after handling.
In an embodiment of the present invention, wherein said metal implant is the alloy that a titanium or contains titanium elements.
In an embodiment of the present invention, the aperture of wherein said micron order pothole is between 1 micron to 100 microns.
In an embodiment of the present invention, wherein said nano-scale fiber network comprises a plurality of nanoscale holes, and the aperture of those nanoscale holes is between 10 nanometer to 1000 nanometers.
In an embodiment of the present invention, wherein said first surface is treated to a blasting treatment.
In an embodiment of the present invention, wherein said first surface is treated to acid etching after the sandblast, and in order to generating a plurality of sub-micron grade potholes in those micron order potholes, and the aperture of those sub-micron grade potholes is between 100 nanometer to 1000 nanometers.
In an embodiment of the present invention, wherein said alkaline etching is handled the alkaline etching chemical compound of use for containing a sodium ion (Na
+), a potassium ion (K
+) or a calcium ion (Ca
2+) hydroxide.
In an embodiment of the present invention, the acid solution used of wherein said pickling processes is hydrochloric acid (HCl) or sulphuric acid (H
2SO
4).
In sum; metal implant of the present invention; surface after sandblast or sandblast-pickling processes can produce the micron order pothole; carry out alkaline etching-pickling-heat treatment (Alkali-Acid-heat treatment; AAH) after; the surface of metal implant can present the nano-scale fiber network; because its composition of nano-scale fiber network is a titanium oxide; have bone bioactivity and can promote the calcium phosphate deposition; be applicable in the implantable bioartificial body; the micron order pothole can be protected the nano-scale fiber network structure in addition, reduces its ruined probability in implant surgery.
For above-mentioned feature and advantage of the present invention can be become apparent, embodiment cited below particularly, and cooperate appended graphicly, be described in detail below.
Description of drawings
Fig. 1 is the sketch map of one embodiment of the invention metal implant;
Fig. 2 is the flow chart of metal implant surface treatment method of the present invention;
Fig. 3 A is that multiplying power is the surperficial SEM figure of 500 times of metal implants;
Fig. 3 B is that multiplying power is the surperficial SEM figure of 2500 times of metal implants;
Fig. 4 be metal implant surperficial SEM figure;
Fig. 5 A is the surface of metal titanium photo that carries out blasting treatment;
Fig. 5 B is the surface of metal titanium photo that does not carry out blasting treatment;
Fig. 6 be metal implant surperficial SEM figure;
Fig. 7 be metal implant surperficial SEM figure;
Fig. 8 A be metal implant surperficial SEM figure;
Fig. 8 B is a place enlarged drawing of Fig. 8 A;
Fig. 8 C is the b place enlarged drawing of Fig. 8 B;
Wherein, Reference numeral:
S100～S300 process step
10: the micron order pothole
20: the sub-micron grade pothole
30: the nano-scale fiber network
The specific embodiment
Fig. 1 is the sketch map of one embodiment of the invention metal implant, see also Fig. 1, the surface of metal implant has a plurality of micron order potholes 10, and micron order pothole 10 has micron hole 20 a plurality of times, inferior micron hole 20 has a nano-scale fiber network 39, the aperture of micron order pothole 10 is between 1 micron to 100 microns, the aperture of sub-micron grade pothole 20 is between 100 nanometer to 1000 nanometers, nano-scale fiber network 30 comprises a plurality of nanoscale holes, and the aperture of nanoscale hole is between 10 nanometer to 1000 nanometers.
In other words, the surface of metal implant has a plurality of micron order potholes 10, and all contain sub-micron grade pothole 20 in each micron order pothole 10, each sub-micron grade pothole 20 contains a nano-scale fiber network 30, and these nano-scale fiber networks 30 are the structure of a similar sponge, so nano-scale fiber network 30 comprises a plurality of nanoscale holes.
Fig. 2 is the flow chart of metal implant surface treatment method of the present invention.See also Fig. 2, metal implant surface-treated method comprises: at first, provide a metal implant (step S100).Metal implant is the alloy that a titanium or contains titanium elements.
Afterwards, carry out a first surface on the surface of this metal implant and handle (step S200), form a plurality of micron order potholes with the surface at this metal implant, what should be specified is that the aperture of a plurality of micron order potholes described here is between 1 micron to 100 microns.
In detail, first surface processing (step S200) can be an acid etching after a blasting treatment or the sandblast.The mode of operation of blasting treatment is: with a sand body one metal implant is carried out sand and be coated with, wherein the granular size of sand body described here is a particle diameter less than 400 microns ceramic sand body (as: aluminum oxide sand or titanium dioxide sand), and so blasting treatment metal implant surface later can have a plurality of micron order potholes.
The mode of operation of acid etching is after the sandblast: carry out above-mentioned blasting treatment earlier, carry out an acid etching afterwards again.In detail, acid etching is for to be soaked in metal implant in one acid solution, and acid solution can be sulphuric acid, hydrogen peroxide, hydrochloric acid or mixed acid, and the mixed acid of indication can be the above-mentioned acid solution acid solution that other acid solution or above-mentioned acid solution form of arranging in pairs or groups here.Because the blasting treatment meeting can produce the micron order pothole on metal implant surface, and acid etching can form a plurality of sub-micron grade potholes again in these micron order potholes, wherein here the aperture of the sub-micron grade pothole of indication between 100 nanometer to 1000 nanometers.
First surface is handled (step S200) afterwards, carries out a second surface on the surface of this metal implant and handles (step S300), to generate a nano-scale fiber network in micron order pothole or sub-micron grade pothole.In detail, the nano-scale fiber network of indication comprises a plurality of nanoscale holes here, and the aperture of those nanoscale holes is between 10 nanometer to 1000 nanometers.The composition of this nano-scale fiber network is a rutile phase oxidation titanium or an anatase phase oxidation titanium, therefore has bone bioactivity and can promote the calcium phosphate deposition.
Second surface processing (step S300) step can be alkaline etching processing or alkaline etching is handled collocation one pickling processes and a heat treatment carries out.The mode of operation that alkaline etching is handled is for to be soaked in an alkaline solution with metal implant, and wherein alkaline solution comprises a plurality of alkaline etching chemical compounds, and the alkaline etching chemical compound is sodium ion (Na
+), potassium ion (K
+) or calcium ion (Ca
2+) hydroxide.
The mode of operation of pickling processes is for to be soaked in an acid solution with metal implant, and acid solution wherein described here is hydrochloric acid (HCl) or sulphuric acid (H
2SO
4).
Heat treated mode of operation is with the space of metal implant as for a thermally equivalent, and its proper temperature is provided.Wherein heat treated range of reaction temperature can be between 400 to 800 ℃, and reaction time range can be between 30 minutes to 8 hours.
After metal implant carried out the first surface processing, the metal implant after the blasting treatment can present different color and lusters (for example Lycoperdon polymorphum Vitt), so the tangible identification of medical device product tool; In addition, first surface is handled the micron order pothole of back generation and can be protected second surface to handle the nano-scale fiber network that produces, and reduces nano-scale fiber network ruined probability in implant surgery.
Below enumerate specific embodiment 1 the present invention is described, but the present invention is not limited in following embodiment.
The metal implant of embodiment 1 is an example with a titanium, surface of metal titanium is after 100 microns aluminum oxide sand is carried out blasting treatment (first surface processing), the surface of titanium can produce the about 10 microns micron order pothole of hole diameter, place titanium the 5M sodium hydrate aqueous solution after 4 hours afterwards, place the aqueous hydrochloric acid solution HCl (aq) 3 hours of 50mM again, last under 600 ℃ environment heat treatment 1 hour (second surface processing), after the processing of first surface processing collocation second surface, the surface texture result of titanium as shown in Figure 3.
See also Fig. 3, the surperficial SEM figure of Fig. 3 A and Fig. 3 B are respectively multiplying power when being 500 times and the 2500 times metal implant of embodiment 1, by Fig. 3 A and Fig. 3 B as can be known, the surface of metal implant comprises a plurality of micron order potholes, and these micron order potholes comprise the nano-scale fiber network.
After in the titanium of the embodiment 1 immersion simulated body fluid (SBF) one day, the result is shown in Figure 4, as shown in Figure 4, metal implant soaked in the simulated body fluid after one day, its surface has the calcium phosphate granules of ball-shaped to generate, therefore, the surface texture of metal implant of the present invention has bone bioactivity, and can promote the calcium phosphate deposition.
In addition, the titanium of embodiment 1 (A group) is locked in the imitative bone (saw-bone) with normal implantation flow process, withdraw from the observation surface morphology again, and more only carry out the titanium (B group) that above-mentioned second surface is handled (nothing is carried out first surface and handled), lock in the same manner in the imitative bone, withdraw from the surface morphology of observing surface morphology again.By Fig. 5 A as can be known, do not carry out the titanium (B group) of blasting treatment, its surface of metal titanium has obvious scratch, and by Fig. 5 B as can be known, the titanium (A group) that carries out blasting treatment is arranged, and the hole of its surface of metal titanium is still kept its roughness.
In addition, with the surface of metal titanium structure of electron microscope observation B group, before locking experiment, though the surface of metal titanium of B group has the nano-scale fiber of presenting network (Fig. 6), after locking experiment, its nano-scale fiber network is all polished (Fig. 7).
Similarly; surface of metal titanium structure with electron microscope observation A group; please refer to Fig. 8 A, 8B and 8C; though the rough surface higher position of titanium after locking experiment of A group polished; but the nano-scale fiber network in the micron order pothole is still very complete; therefore, the micron order pothole can protect first surface to handle the nano-scale fiber network that produces, and reduces nano-scale fiber network ruined probability in implant surgery.
In sum; metal implant of the present invention; surface after sandblast or sandblast-pickling processes can produce the micron order pothole; carry out alkaline etching-pickling-heat treatment (Alkali-Acid-heat treatment; AAH) after; the surface of metal implant can present the nano-scale fiber network; because its composition of nano-scale fiber network is a titanium oxide; have bone bioactivity and can promote the calcium phosphate deposition; be applicable in the implantable bioartificial body; the micron order pothole can be protected the nano-scale fiber network structure in addition, reduces its ruined probability in implant surgery.
Certainly; the present invention also can have other various embodiments; under the situation that does not deviate from spirit of the present invention and essence thereof; those of ordinary skill in the art work as can make various corresponding changes and distortion according to the present invention, but these corresponding changes and distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (10)
1. a metal implant has a surface, it is characterized in that, comprising:
A plurality of micron order potholes, and this micron order pothole comprises a nano-scale fiber network, wherein the aperture of this micron order pothole is between 1 micron to 100 microns, and this nano-scale fiber network comprises a plurality of nanoscale holes, and the aperture of this nanoscale hole is between 10 nanometer to 1000 nanometers.
2. metal implant according to claim 1 is characterized in that, this micron order pothole comprises a plurality of sub-micron grade potholes, and this nanoscale hole is positioned at this sub-micron grade pothole, and the aperture of this sub-micron grade pothole is between 100 nanometer to 1000 nanometers.
3. metal implant according to claim 1 is characterized in that, this metal implant is the alloy that a titanium or contains titanium elements.
4. metal implant according to claim 1 is characterized in that, the composition of this nano-scale fiber network is a rutile phase oxidation titanium or an anatase phase oxidation titanium.
5. the surface treatment method of a metal implant is characterized in that, comprising:
One metal implant is provided;
Carry out a first surface on the surface of this metal implant and handle, form a plurality of micron order potholes with the surface at this metal implant, the aperture of this micron order pothole is between 1 micron to 100 microns; And
Carry out a second surface on the surface of this metal implant and handle, to form a nano-scale fiber network in this micron order pothole, this nano-scale fiber network comprises a plurality of nanoscale holes, and the aperture of this nanoscale hole is between 10 nanometer to 1000 nanometers.
6. surface treatment method according to claim 5 is characterized in that, this second surface treatment step is that an alkaline etching is handled.
7. surface treatment method according to claim 6 is characterized in that, this alkaline etching also comprises a pickling processes and a heat treatment after handling.
8. surface treatment method according to claim 6 is characterized in that, this first surface is handled and comprised:
One blasting treatment forms this micron order pothole in order to the surface at this metal implant; And
Acid etching after one sandblast, in order to form a plurality of sub-micron grade potholes in this micron order pothole, this nanoscale hole is positioned at this sub-micron grade pothole, and the aperture of this sub-micron grade pothole is between 100 nanometer to 1000 nanometers.
9. surface treatment method according to claim 6 is characterized in that, it is the hydroxide that contains a sodium ion, a potassium ion or a calcium ion that this alkaline etching is handled the alkaline etching chemical compound that uses.
10. surface treatment method according to claim 7 is characterized in that, the acid solution that pickling processes is used is hydrochloric acid or sulphuric acid.
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|---|---|---|---|
| CN2010101139808A CN102145192A (en) | 2010-02-05 | 2010-02-05 | Metal implant and surface treatment method thereof |
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|---|---|---|---|
| CN2010101139808A CN102145192A (en) | 2010-02-05 | 2010-02-05 | Metal implant and surface treatment method thereof |
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| CN102626345A (en) * | 2012-04-12 | 2012-08-08 | 王玉元 | Method for fusing bioactive material on surface of artificial tooth pure titanium spiral-shafted implant |
| CN104147636A (en) * | 2014-07-14 | 2014-11-19 | 大连大学 | Method for treating surface of Ti6Al7Nb by promoting osteoblast proliferation, adhesion and differentiation |
| CN104451685A (en) * | 2014-12-30 | 2015-03-25 | 哈尔滨工业大学 | Preparation method for forming second-level porous active surface structure on titanium material surface through mixed alkali |
| CN105441960A (en) * | 2014-08-22 | 2016-03-30 | 广州中国科学院先进技术研究所 | Method for constructing micrometer/nanometer hierarchical structure with super hydrophilicity on surface of titanium dental implant |
| CN105537589A (en) * | 2016-01-28 | 2016-05-04 | 佛山市安齿生物科技有限公司 | Surface treatment method for SLM molded titanium implant |
| CN105696054A (en) * | 2016-01-18 | 2016-06-22 | 南京医科大学附属口腔医院 | Preparation method for forming calcium-containing nanosheet film layer on surface of sandblasted and acid-etched titanium |
| CN106377495A (en) * | 2016-09-23 | 2017-02-08 | 中南大学 | Composite surface drug-carrying slow-release system and preparation method thereof |
| CN104451684B (en) * | 2014-09-27 | 2017-02-15 | 浙江大学 | Method for constructing surface of bionic multifunctional titanium-based implant |
| CN106388957A (en) * | 2016-10-19 | 2017-02-15 | 中国科学院上海硅酸盐研究所慈溪生物材料表面工程中心 | Method for manufacturing implant dental pin and implant dental pin manufactured by method |
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| CN102626345A (en) * | 2012-04-12 | 2012-08-08 | 王玉元 | Method for fusing bioactive material on surface of artificial tooth pure titanium spiral-shafted implant |
| CN104147636A (en) * | 2014-07-14 | 2014-11-19 | 大连大学 | Method for treating surface of Ti6Al7Nb by promoting osteoblast proliferation, adhesion and differentiation |
| CN104147636B (en) * | 2014-07-14 | 2016-01-20 | 大连大学 | A kind of Ti6Al7Nb surface treatment method promoting osteoblastic proliferation, stick and break up |
| CN105441960A (en) * | 2014-08-22 | 2016-03-30 | 广州中国科学院先进技术研究所 | Method for constructing micrometer/nanometer hierarchical structure with super hydrophilicity on surface of titanium dental implant |
| CN104451684B (en) * | 2014-09-27 | 2017-02-15 | 浙江大学 | Method for constructing surface of bionic multifunctional titanium-based implant |
| CN104451685A (en) * | 2014-12-30 | 2015-03-25 | 哈尔滨工业大学 | Preparation method for forming second-level porous active surface structure on titanium material surface through mixed alkali |
| CN105696054A (en) * | 2016-01-18 | 2016-06-22 | 南京医科大学附属口腔医院 | Preparation method for forming calcium-containing nanosheet film layer on surface of sandblasted and acid-etched titanium |
| CN105537589A (en) * | 2016-01-28 | 2016-05-04 | 佛山市安齿生物科技有限公司 | Surface treatment method for SLM molded titanium implant |
| CN106377495A (en) * | 2016-09-23 | 2017-02-08 | 中南大学 | Composite surface drug-carrying slow-release system and preparation method thereof |
| CN106377495B (en) * | 2016-09-23 | 2019-06-21 | 中南大学 | A kind of composite surface drug loading slow-released system and preparation method thereof |
| CN106388957A (en) * | 2016-10-19 | 2017-02-15 | 中国科学院上海硅酸盐研究所慈溪生物材料表面工程中心 | Method for manufacturing implant dental pin and implant dental pin manufactured by method |
| CN106725930A (en) * | 2016-12-23 | 2017-05-31 | 大连三生科技发展有限公司 | Planting body with BMP/PLA controlled-release coatings |
| CN106725935A (en) * | 2016-12-23 | 2017-05-31 | 大连三生科技发展有限公司 | Planting body with high content, high stability BMP coatings |
| CN111020685A (en) * | 2019-11-01 | 2020-04-17 | 浙江大学 | Preparation method of fiber metal laminated plate for improving interlayer strength |
| CN111020685B (en) * | 2019-11-01 | 2021-01-08 | 浙江大学 | Preparation method of fiber metal laminated plate for improving interlayer strength |
| CN111041490A (en) * | 2019-12-28 | 2020-04-21 | 高岩 | Pure titanium surface treatment method capable of promoting contact osteogenesis |
| CN113652735A (en) * | 2021-08-26 | 2021-11-16 | 安徽工业大学 | Zr-based metal glass and preparation method and application thereof |
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Application publication date: 20110810 |