CN101886264A - Surface treatment method for metal implant - Google Patents
Surface treatment method for metal implant Download PDFInfo
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- CN101886264A CN101886264A CN2009101412690A CN200910141269A CN101886264A CN 101886264 A CN101886264 A CN 101886264A CN 2009101412690 A CN2009101412690 A CN 2009101412690A CN 200910141269 A CN200910141269 A CN 200910141269A CN 101886264 A CN101886264 A CN 101886264A
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- metal implant
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Abstract
The invention relates to a surface treatment method for a metal implant. In the method, a high-temperature acid liquor is used for developing uniform micron-level holes on the surface of a titanium implant element, and then a composite acid liquor containing hydrogen peroxide is used for carrying out deoxidation/reoxidation treatment on the coarse surface of the titanium implant to generate a uniform oxidation layer, so as to increase the biocompatibility of the titanium implant.
Description
Technical field
The present invention relates to a kind of surface treatment method of metal implant, particularly can form the coarse hole of micron order, and generate the surface treatment method of the even zone of oxidation of one deck in the metal implant surface.
Background technology
At present, the method that forms vesicular structure on metal implant (implant) surface has multiple, as: sand-blast (sand blasting) or aciding (acid etching), by aforesaid method the surfaceness of metal implant is increased, generation has the surface of planting of even roughness degree, connects to promote and to implant zone osseous tissue on every side.
For instance, U.S. Patent number US 6,491,723 discloses a kind of surface treatment method of metal implant, and its surface treatment step utilizes hydrofluoric acid (HF) to carry out the acid etching first time earlier, in order to remove surperficial natural oxidizing layer; Again with pyritous sulfuric acid (H
2SO
4)/hydrochloric acid (HCl) mixed solution carries out the acid etching second time, forms irregular and uniform surface.
Yet hydrofluoric acid is the chemical of murther, can enter human body via approach such as mouth, nose, eye or skins, causes serious systemic toxicity symptoms such as low blood calcium, hypomagnesemia, pulmonary edema, metabolic acidosis, ventricle Arrhythmias even death.And sulfuric acid/hydrochloric acid mixed solution is the mixing of two kinds of strong acid, can produce the dehydration reaction of very exothermic when preparation, operator is caused burn.
Summary of the invention
In view of this, the invention provides a kind of surface treatment method of metal implant, in order to reducing in the surface treatment process chance, and increase the effect of biocompatibility the dangerous injury of human body.
The present invention proposes a kind of surface treatment method of metal implant in addition, and the surface of metal implant has one first zone of oxidation, and its step comprises: at first, metal implant is soaked in one first acid solution to remove first zone of oxidation.Afterwards, the metal implant that is soaked in first acid solution is taken out, metal implant is soaked in one second acid solution again, second acid solution comprises a hydrogen peroxide, in order to the surface of roughening metal implant and form one second zone of oxidation.At last, metal implant is taken out in second acid solution.
In an embodiment of the present invention, wherein second thickness of oxide layer greater than 10nm.
In an embodiment of the present invention, wherein the material of metal implant is the metal that a titanium metal, a titanium alloy or contain titanium elements.
In an embodiment of the present invention, wherein second acid solution more comprises sulfuric acid or a hydrochloric acid.
In an embodiment of the present invention, wherein when second acid solution was hydrogen peroxide and vitriolic mixing acid, hydrogen peroxide in its mixing acid and vitriolic volume ratio were 1: 1～6: 1, and wherein the concentration of hydrogen peroxide is 30%, and vitriolic concentration is 95%.
In an embodiment of the present invention, wherein when second acid solution was the mixing acid of hydrogen peroxide and hydrochloric acid, the hydrogen peroxide in its mixing acid and the volume ratio of hydrochloric acid were 1: 1～6: 1, and wherein the concentration of hydrogen peroxide is 30%, and the concentration of hydrochloric acid is 37%.
In an embodiment of the present invention, the time that wherein is soaked in first acid solution is several minutes to 60 minutes.
In an embodiment of the present invention, the time that wherein is soaked in second acid solution is several minutes to 24 hours.
Treatment temp when in an embodiment of the present invention, wherein being soaked in first acid solution is 60 ℃ to 80 ℃.
Treatment temp when in an embodiment of the present invention, wherein being soaked in second acid solution is 20 ℃ to 80 ℃.
In an embodiment of the present invention, wherein first acid solution is selected from the group that is made up of nitric acid, hydrochloric acid and sulfuric acid.
In an embodiment of the present invention, when wherein metal implant was soaked in this first acid solution, its surface formed the micron-sized coarse hole of plural number.
In an embodiment of the present invention, the surfaceness (Ra value) that wherein is formed at second zone of oxidation on this metal implant surface is about 0.3～0.7 μ m.
In sum, the present invention at first carries out titanium metal implant surface roughened with pyritous hydrochloric acid or sulfuric acid, makes it have micron-sized hole.This stage mainly is that the hydrofluoric acid that utilizes hydrochloric acid or sulfuric acid to replace to have high risk carries out the acid etching first time, and makes uneven surface simultaneously.And with the gentle hydrogen peroxide (H that reacts under the room temperature
2O
2)/sulfuric acid (H
2SO
4) mixed solution, the hydrochloric acid/sulfuric acid mixture liquid that replaces high-temperature operation generation vigorous reaction carries out the acid etching second time, so, can reduce the chance to the dangerous injury of human body.
For above-mentioned feature and advantage of the present invention can be become apparent, embodiment cited below particularly, and conjunction with figs. are described in detail below.
Description of drawings
Fig. 1 is the schema of metal implant surface treatment method of the present invention; And
Fig. 2 A and Fig. 2 B are the surperficial SEM figure of metal implant.
[main element nomenclature]
S100, S200 steps flow chart
Embodiment
Fig. 1 is the schema of the metal implant surface treatment method of one embodiment of the invention.Wherein, the material of metal implant can be the metal that a titanium metal, a titanium alloy or contain titanium elements, and these metal implants are with after air contacts, and its surface all has a zone of oxidation usually, and this zone of oxidation can be titanium monoxide layer (TiO
2).
See also Fig. 1, metal implant surface-treated method may further comprise the steps: at first, carry out an acid etching (step S100) for the first time, it is in 37% hydrochloric acid (HCl) solution that metal implant is soaked in weight percent, wherein metal implant can be soak fully or local soaking in above-mentioned hydrochloric acid (HCl) solution, to remove the metal implant surface oxide layer, and form the micron-sized coarse hole of plural number in the surface, and the relevant operating parameters of acid etching for the first time, can be to allow the metal implant be effect several minutes to 60 minutes in 60～80 ℃ the hydrochloric acid soln in temperature, in present embodiment, the action time of metal implant in hydrochloric acid soln is 10～30 minutes.Then, metal implant is carried out rinse and neutral program in regular turn, wherein rinse program can adopt ultrapure water to clean and be moistening.
For the first time acid etching (step S100) is carried out an acid etching (step S200) for the second time afterwards, is about to the metal implant crossed through persalt acid etching and neutralizing treatment, is soaked in the middle of the mixing acid.Wherein, mixing acid can be the mixing acid of hydrogen peroxide (30%)/sulfuric acid (95%) or the mixing acid of hydrogen peroxide (30%)/hydrochloric acid (37%).
What should be specified is, the mixing acid of hydrogen peroxide (30%)/sulfuric acid (95%) is equal-volume mixed or different volumes mixed, and wherein preferably hydrogen peroxide and vitriolic volume ratio are 1: 1～6: 1.In like manner, the mixing acid of hydrogen peroxide (30%)/hydrochloric acid (37%) is equal-volume mixed or different volumes mixed, and wherein preferably the volume ratio of hydrogen peroxide and hydrochloric acid is 1: 1～6: 1.
The relevant operating parameters of acid etching for the second time, can be to allow metal implant in the mixed acid solution of room temperature, act on several minutes to 24 hours, in present embodiment, the action time of metal implant in mixed acid solution is-10 minutes, carry out rinse, neutralization and action such as air-dry at last again, wherein rinse program can adopt ultrapure water to clean and be moistening.
Through acid etching second time metal implant later, its surface can form one second zone of oxidation, and this second zone of oxidation can be titanium monoxide layer (TiO
2).Wherein, the oxidated layer thickness that is after acid etching to be produced that should be specified, its size is greater than 10nm, the natural oxidation layer thickness that is produced before acid etching with metal implant has significant difference.
Please consult Fig. 2 A and Fig. 2 B respectively, it is respectively the surperficial SEM figure of the metal implant after above-mentioned flow processing, and its SEM figure multiplying power is respectively 2500 times and 5K times.Shown in Fig. 2 A and 2B, find that the metal implant surface is by a plurality of irregular and uniform uneven surface that slightly sharp taper monomer forms, rough 1～3 μ m apart between each taper monomer of presenting.Surfaceness (Ra value) is about 0.3～0.7 μ m.
In simple terms, fs acid etching step of the present invention is mainly with pyritous first acid solution, example hydrochloric acid, replace the removal that hydrofluoric acid carries out surperficial natural oxidizing layer, and make micron-sized coarse hole, and subordinate phase acid etching step mainly is with second acid solution in the surface, as hydrogen peroxide/sulfuric acid mixed solution at room temperature, carry out the acid etching second time, carry out deoxidation/reoxidize processing, make the metal implant surface generate the even purified zone of oxidation of one deck.So, not only can avoid the vigorous reaction that produces when using acid solution or preparation acid solution, reduce dangerously, and the metal implant surface generates the even purified zone of oxidation of one deck, can be in order to increase the biocompatibility of implant.Though the present invention is with previous embodiment openly as above, so it is not in order to limiting the present invention, any those skilled in the art, and without departing from the spirit and scope of the present invention, institute does to change and the equivalence replacement of retouching, and still is in the scope of patent protection of the present invention.
Claims (13)
1. the surface treatment method of a metal implant, the surface of this metal implant has first zone of oxidation, and its step comprises:
This metal implant is soaked in first acid solution to remove this first zone of oxidation;
This metal implant that is soaked in this first acid solution is taken out, this metal implant is soaked in second acid solution again, this second acid solution comprises hydrogen peroxide, in order to the surface of this metal implant of roughening and form second zone of oxidation; And
This metal implant is taken out in this second acid solution.
2. surface treatment method as claimed in claim 1, wherein this second thickness of oxide layer is greater than 10nm.
3. surface treatment method as claimed in claim 1, wherein the material of this metal implant is titanium metal, titanium alloy or the metal that contains titanium elements.
4. surface treatment method as claimed in claim 1, wherein this second acid solution also comprises sulfuric acid or hydrochloric acid.
5. surface treatment method as claimed in claim 4, wherein when this second acid solution is hydrogen peroxide and vitriolic mixing acid, hydrogen peroxide in its mixing acid and vitriolic volume ratio are 1: 1～6: 1, and wherein the concentration of hydrogen peroxide is 30%, and vitriolic concentration is 95%.
6. surface treatment method as claimed in claim 4, wherein when this second acid solution is the mixing acid of hydrogen peroxide and hydrochloric acid, the hydrogen peroxide in its mixing acid and the volume ratio of hydrochloric acid are 1: 1～6: 1, and wherein the concentration of hydrogen peroxide is 30%, and the concentration of hydrochloric acid is 37%.
7. surface treatment method as claimed in claim 1, the time that wherein is soaked in this first acid solution is several minutes to 60 minutes.
8. surface treatment method as claimed in claim 1, the time that wherein is soaked in this second acid solution is several minutes to 24 hours.
9. surface treatment method as claimed in claim 1, the treatment temp when wherein being soaked in this first acid solution are 60 ℃ to 80 ℃.
10. surface treatment method as claimed in claim 1, the treatment temp when wherein being soaked in this second acid solution are 20 ℃ to 80 ℃.
11. surface treatment method as claimed in claim 1, wherein this first acid solution is selected from the group that is made up of nitric acid, hydrochloric acid and sulfuric acid.
12. surface treatment method as claimed in claim 1, when wherein this metal implant was soaked in this first acid solution, its surface formed the micron-sized coarse hole of plural number.
13. surface treatment method as claimed in claim 1, the surface roughness Ra value that wherein is formed at second zone of oxidation on this metal implant surface is about 0.3～0.7 μ m.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101412690A CN101886264A (en) | 2009-05-14 | 2009-05-14 | Surface treatment method for metal implant |
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| CN2009101412690A CN101886264A (en) | 2009-05-14 | 2009-05-14 | Surface treatment method for metal implant |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106880870A (en) * | 2017-03-07 | 2017-06-23 | 珠海乔丹科技股份有限公司 | A kind of processing method of titanium-based implant surface activation |
-
2009
- 2009-05-14 CN CN2009101412690A patent/CN101886264A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106880870A (en) * | 2017-03-07 | 2017-06-23 | 珠海乔丹科技股份有限公司 | A kind of processing method of titanium-based implant surface activation |
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Application publication date: 20101117 |