CN103343375A - Method for improving biological activity of composite coating on surface of titanium through micro-arc oxidation and water vapour treatment - Google Patents
Method for improving biological activity of composite coating on surface of titanium through micro-arc oxidation and water vapour treatment Download PDFInfo
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- CN103343375A CN103343375A CN2013103029986A CN201310302998A CN103343375A CN 103343375 A CN103343375 A CN 103343375A CN 2013103029986 A CN2013103029986 A CN 2013103029986A CN 201310302998 A CN201310302998 A CN 201310302998A CN 103343375 A CN103343375 A CN 103343375A
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Abstract
The invention relates to a method for improving biological activity of a composite coating on a surface of titanium through micro-arc oxidation and water vapour treatment, aiming at solving the problems that the biological activity of the surface coating of the titanium and alloy thereof prepared by the existing method is weak, and conventional hydro-thermal treatment causes the biological active elements to be dissolved. The method comprises the following steps of polishing and washing the surface of titanium and an alloy sample; putting a titanium plate in a stainless steel tank body containing bioactive substance electrolyte for micro-arc oxidation, wherein the temperature of the electrolyzer liquid is controlled below 50 DEG C; and suspending the titanium sample with the micro-arc oxidized biological activity coating in a hydrothermal reactor, adding deionized water of 8-15% of total volume of the reactor, and keeping warm for 1-24hours at 60-250 DEG C for water vapour treatment. The method is used for preparing advanced medical implant substituted bone material.
Description
Technical field
The present invention relates to titanium surface by micro-arc oxidation/steam and handle the method for bioactivity composite coating, be specifically related to the method for a kind of differential arc oxidation/steam Processing of Preparation bioactivity composite coating.
Background technology
Titanium and alloy thereof are widely used in medical planting body material because of excellent anticorrosive and biocompatibility.But titanium and alloy thereof do not possess the osteogenesis of inducing ability, show as biologically inert, need carry out biological activity to its surface and handle, to adapt to the application in vivo of medical planting body.And differential arc oxidation method is a kind of common titanium surface bioactive method of modifying, can will be incorporated into life entity beneficial trace elements silicon, calcium, phosphorus, sodium in the middle of the coating that generates.But this method coatings prepared biological activity a little less than, this just need carry out secondary treatment to the generation coating, improving its biological activity, and common hydrothermal treatment consists can cause the stripping of biological activity element.
Summary of the invention
The objective of the invention is for the titanium that solves existing method preparation and alloy surface coating biological activity thereof a little less than, and conventional hydrothermal treatment consists can cause the problem of the stripping of biological activity element, and provides titanium surface by micro-arc oxidation/steam to handle the method for bioactivity composite coating.
Titanium surface by micro-arc oxidation of the present invention/steam is handled the method for bioactivity composite coating, carries out according to following steps:
One, adopt 200#, 400# and 1000# sand paper that the titanium sample is polished, polished successively after, use washed with de-ionized water, under 30～70 ℃ of temperature, dry 1～5h again;
Two, differential arc oxidation is handled: the titanium sample after the step 1 oven dry is placed the stainless steel trough body that contains electrolytic solution, is anode with the titanium sample, is negative electrode with the stainless steel trough body, carries out differential arc oxidation;
Three, steam is handled: add the deionized water that accounts for reactor cumulative volume 8～20% in reactor, be positioned in the hydrothermal reaction kettle and keep the titanium sample above the liquid level of deionized water the titanium sample behind the differential arc oxidation is unsettled, under 60～250 ℃ of temperature, be incubated 1～24h then.
The present invention comprises following beneficial effect:
The present invention has further significantly improved its biological activity and stability on the basis that keeps titanium surface by micro-arc oxidation coating biology activity, expanded differential arc oxidation and post-treatment coatings thereof the range of application in the planting body material.
Coating after the present invention handles is carried out diffractometer EDS spectroscopy detection, contains silicon, calcium, phosphorus, sodium trace active element in the coating, and X-ray diffractometer carries out the test of XRD diffraction and can detect in the coating pure at anatase octahedrite and phosphatic rock.The present invention adopts steam to handle at differential arc oxidation coating first, be an innovation at differential arc oxidation bioactive coating post-treating method, to obtain coatingsurface by the present invention and generate a large amount of phosphatic rock, putting into 3 days rear surface hydroxyapatites of simulated body fluid immersion reaches capacity, and common differential arc oxidation sample also generates without any phosphatic rock after identical soak time, illustrates that the titanium sample of handling through differential arc oxidation/steam among the present invention has than titanium and the more excellent biological activity of common biological activity differential arc oxidation coating thereof.
Steam post-treating method of the present invention can further improve the biological activity of siliceous, calcium, phosphorus, sodium biological activity element differential arc oxidation coating.Be applicable to the planting body of different shapes and size, contain the biological activity with excellence in the specimen surface coating that obtains, can successfully in simulated body fluid, induce hydroxyapatite, help to improve the binding ability of planting body and new bone tissue.
Description of drawings
Fig. 1 is the XRD power spectrum picture that differential arc oxidation/steam is handled bioactivity composite coating; Wherein, A is anatase octahedrite XRD curve, and B is titanium XRD curve, and C is phosphatic rock XRD curve;
Fig. 2 handles bioactivity composite coating scanning pattern SEM figure for test 1 differential arc oxidation/steam;
Fig. 3 handles the power spectrum spectrogram on bioactivity composite coating surface for test 1 differential arc oxidation/steam.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the titanium surface by micro-arc oxidation of present embodiment/steam is handled the method for bioactivity composite coating, carries out according to following steps:
One, adopt 200#, 400# and 1000# sand paper that the titanium sample is polished, polished successively after, use washed with de-ionized water, under 30～70 ℃ of temperature, dry 1～5h again;
Two, differential arc oxidation is handled: the titanium sample after the step 1 oven dry is placed the stainless steel trough body that contains electrolytic solution, is anode with the titanium sample, is negative electrode with the stainless steel trough body, carries out differential arc oxidation;
Three, steam is handled: add the deionized water that accounts for reactor cumulative volume 8～20% in reactor, be positioned in the hydrothermal reaction kettle and keep the titanium sample above the liquid level of deionized water the titanium sample behind the differential arc oxidation is unsettled, under 60～250 ℃ of temperature, be incubated 1～24h then.
Present embodiment has further significantly improved its biological activity and stability on the basis that keeps titanium surface by micro-arc oxidation coating biology activity, expanded differential arc oxidation and post-treatment coatings thereof the range of application in the planting body material.
Coating after present embodiment is handled is carried out diffractometer EDS spectroscopy detection, contains silicon, calcium, phosphorus, sodium trace active element in the coating, and X-ray diffractometer carries out the test of XRD diffraction and can detect in the coating pure at anatase octahedrite and phosphatic rock.Present embodiment adopts steam to handle at differential arc oxidation coating first, be an innovation at differential arc oxidation bioactive coating post-treating method, to obtain coatingsurface by present embodiment and generate a large amount of phosphatic rock, putting into 3 days rear surface hydroxyapatites of simulated body fluid immersion reaches capacity, and common differential arc oxidation sample also generates without any phosphatic rock after identical soak time, illustrates that the titanium sample of handling through differential arc oxidation/steam in the present embodiment has than titanium and the more excellent biological activity of common biological activity differential arc oxidation coating thereof.
The steam post-treating method of present embodiment can further improve the biological activity of siliceous, calcium, phosphorus, sodium biological activity element differential arc oxidation coating.Be applicable to the planting body of different shapes and size, contain the biological activity with excellence in the specimen surface coating that obtains, can successfully in simulated body fluid, induce hydroxyapatite, help to improve the binding ability of planting body and new bone tissue.
Embodiment two: what present embodiment and embodiment one were different is: the differential arc oxidation parameter described in the step 2 is as follows: differential arc oxidation adopts pulsed dc voltage, voltage is 200～600V, described differential arc oxidation pulse-repetition is 300～900Hz, the dutycycle 4～20% of described differential arc oxidation, described differential arc oxidation electrolyte temperature is 0～50 ℃, described differential arc oxidation time 3～15min.。Other is identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is: described pulsed dc voltage is 350～500V, the differential arc oxidation pulse-repetition is 400～800Hz, dutycycle 5～15%, electrolyte temperature are 20～50 ℃, differential arc oxidation time 5～12min.Other is identical with embodiment one or two.
Embodiment four: what present embodiment was different with one of embodiment one to three is: described pulsed dc voltage is 350～400V, the differential arc oxidation pulse-repetition is 500～700Hz, dutycycle 5～10%, electrolyte temperature are 20～40 ℃, differential arc oxidation time 5～10min.Other is identical with one of embodiment one to three.
Embodiment five: what present embodiment was different with one of embodiment one or four is: the electrolytic solution described in the step 2 is mixing of the calcium acetate solution solution that is 7～9g/L by the sodium silicate solution that concentration is the disodium ethylene diamine tetra-acetic acid solution of 10～15g/L, sodium hydroxide solution that concentration is 5～10g/L, concentration is 6～8g/L, biphosphate calcium solution that concentration is 5～8g/L and concentration, and each component of described electrolytic solution is that solvent is prepared with the deionized water.Other is identical with one of embodiment one or four.
Embodiment six: what present embodiment was different with one of embodiment one or five is: the electrolytic solution described in the step 2 is mixing of the calcium acetate solution solution that is 8.8g/L by the sodium silicate solution that concentration is the disodium ethylene diamine tetra-acetic acid solution of 15g/L, sodium hydroxide solution that concentration is 5g/L, concentration is 7.1g/L, biphosphate calcium solution that concentration is 6.3g/L and concentration, and each component of described electrolytic solution is that solvent is prepared with the deionized water.Other is identical with one of embodiment one or five.
Embodiment seven: what present embodiment was different with one of embodiment one to six is: add the deionized water that accounts for reactor cumulative volume 9～12% in the reactor described in the step 3.Other is identical with one of embodiment one to six.
Embodiment eight: what present embodiment was different with one of embodiment one to seven is: add the deionized water that accounts for reactor cumulative volume 10% in the reactor described in the step 3.Other is identical with one of embodiment one to seven.
Embodiment nine: what present embodiment was different with one of embodiment one to eight is: the steam treatment temp described in the step 3 is 60～100 ℃, and the steam treatment time is 1～12h.Other is identical with one of embodiment one to eight.
Embodiment ten: what present embodiment was different with one of embodiment one to nine is: the steam treatment temp described in the step 3 is 100～150 ℃, and the steam treatment time is 1～10h.Other is identical with one of embodiment one to nine.
Embodiment 11: what present embodiment was different with one of embodiment one to ten is: the steam treatment temp described in the step 3 is 150～200 ℃, and the steam treatment time is 12～24h.Other is identical with one of embodiment one to ten.
Embodiment 12: what present embodiment was different with one of embodiment one to 11 is: the steam treatment temp described in the step 3 is 150～200 ℃, and the steam treatment time is 12～24h.Other is identical with one of embodiment one to 11.
Embodiment 13: what present embodiment was different with one of embodiment one to 12 is: described titanium sample is TA2, TA3, TA4, TC4 or Ti2448 titanium alloy.Other is identical with one of embodiment one to 12.
By following verification experimental verification beneficial effect of the present invention:
Test 1
A kind of titanium surface by micro-arc oxidation of this test/steam is handled the method for composite biological coatings, carries out according to following steps:
Step 1, adopt 200#, 400# and 1000# sand paper that TA4 matrix sample is polished, polished successively, after washed with de-ionized water, oven dry is 2 hours under 40 ℃ of temperature;
The steam of step 3, TA4 matrix differential arc oxidation sample is handled: with unsettled being positioned in the hydrothermal reaction kettle of TA4 matrix differential arc oxidation sample, add the deionized water that accounts for reactor cumulative volume 8～20% to reactor, the TA4 matrix is kept unsettled being placed on the deionized water liquid level, under 60～250 ℃ of temperature, be incubated 1～24 hour.
This tests described differential arc oxidation pulsed dc voltage is 200～600V, described differential arc oxidation pulse-repetition is 400～1000Hz, the dutycycle of described differential arc oxidation is 4～20%, described differential arc oxidation electrolyte temperature is 0～50 ℃, described differential arc oxidation time 3～15min, by the control to the differential arc oxidation electrical parameter, make the differential arc oxidation coating of TA4 surface generation at 3～15 μ m.
Described biological activity electrolytic solution is to be that solvent makes each component of electrolytic solution with the deionized water, its concentration is respectively 15 grams per liter disodium ethylene diamine tetra-acetic acid solutions, 5 grams per liter sodium hydroxide solutions, 7.1 grams per liter sodium silicate solutions, 6.3 grams per liter biphosphate calcium solutions and 8.8 grams per liter calcium acetate solutions, makes differential arc oxidation prepare by above-mentioned electrolytic solution and contains silicon, calcium, phosphorus, sodium trace element in the coating.
Composite biological coatings after this test steam is handled carries out X-ray diffractometer XRD diffraction test (as shown in Figure 1) and can detect and have anatase octahedrite and phosphatic rock in the coating.Scanning electronic microscope SEM observes (as shown in Figure 2), as shown in Figure 2, finds that surface growth has column phosphatic rock, the phosphatic rock length-to-diameter ratio is between 50～500, diffractometer EDS spectroscopy detection (as shown in Figure 3) as shown in Figure 3, contains silicon, calcium, phosphorus, sodium trace active element in the coating.To test coating after steam is handled by this puts into simulated body fluid and soaks 3 days rear surface hydroxyapatites and reach capacity.
This test and test 1 are different to be: the voltage of differential arc oxidation described in the step 2 is 350～500V.Other step and parameter are identical with test 1.
There are anatase octahedrite and phosphatic rock in the coating after this test steam is handled.In the coatingsurface growth column phosphatic rock is arranged, the phosphatic rock length-to-diameter ratio contains silicon, calcium, phosphorus, sodium trace active element in the coating between 100～300.Titanium surface by micro-arc oxidation bioactive coating after will testing steam and handle by this is put into simulated body fluid and is soaked 3 days rear surface hydroxyapatites and reach capacity.
Test 3
This test and test 1 are different to be: the treatment temp of steam described in the step 3 is 100～200 ℃.Other step and parameter are identical with test 1.
There are anatase octahedrite and phosphatic rock in the coating after this test steam is handled.In the coatingsurface growth column phosphatic rock is arranged, the phosphatic rock length-to-diameter ratio contains silicon, calcium, phosphorus, sodium trace active element in the coating between 200～300.Titanium surface by micro-arc oxidation bioactive coating after will testing steam and handle by this is put into simulated body fluid and is soaked 3 days rear surface hydroxyapatites and reach capacity.
This test and test 1 are different to be: the treatment temp of steam described in the step 3 is 60～100 ℃, and used substrate titanium plate is TA4, and other step and parameter are identical with test 1.
There are anatase octahedrite and phosphatic rock in the coating after this test steam is handled.In the coatingsurface growth column phosphatic rock is arranged, the phosphatic rock length-to-diameter ratio contains silicon, calcium, phosphorus, sodium trace active element in the coating between 50～100.Titanium surface by micro-arc oxidation bioactive coating after will testing steam and handle by this is put into simulated body fluid and is soaked 5 days rear surface hydroxyapatites and reach capacity.
This test and test 1 are different to be: the treatment time of steam described in the step 3 is 12～24h, and used substrate titanium plate is TA4, and other step and parameter are identical with test 1.
There are anatase octahedrite and phosphatic rock in the coating after this test steam is handled.In the coatingsurface growth column phosphatic rock is arranged, the phosphatic rock length-to-diameter ratio contains silicon, calcium, phosphorus, sodium trace active element in the coating between 100～300.Titanium surface by micro-arc oxidation bioactive coating after will testing steam and handle by this is put into simulated body fluid and is soaked 3 days rear surface hydroxyapatites and reach capacity.
Above-mentioned test 1 is as shown in table 1 to test 5 described simulated body fluid component concentrations.
The chemical reagent content of 1 liter of simulated body fluid of table 1 preparation
Claims (10)
1. titanium surface by micro-arc oxidation/steam is handled the method for bioactivity composite coating, it is characterized in that it carries out according to following steps:
One, adopt 200#, 400# and 1000# sand paper that the titanium sample is polished, polished successively after, use washed with de-ionized water, under 30～70 ℃ of temperature, dry 1～5h again;
Two, differential arc oxidation is handled: the titanium sample after the step 1 oven dry is placed the stainless steel trough body that contains electrolytic solution, is anode with the titanium sample, is negative electrode with the stainless steel trough body, carries out differential arc oxidation;
Three, steam is handled: add the deionized water that accounts for reactor cumulative volume 8～20% in reactor, be positioned in the hydrothermal reaction kettle and keep the titanium sample above the liquid level of deionized water the titanium sample behind the differential arc oxidation is unsettled, under 60～250 ℃ of temperature, be incubated 1～24h then.
2. titanium surface by micro-arc oxidation according to claim 1/steam is handled the method for bioactivity composite coating, it is characterized in that the differential arc oxidation parameter described in the step 2 is as follows: differential arc oxidation adopts pulsed dc voltage, voltage is 200～600V, described differential arc oxidation pulse-repetition is 300～900Hz, the dutycycle 4～20% of described differential arc oxidation, described differential arc oxidation electrolyte temperature is 0～50 ℃, described differential arc oxidation time 3～15min.
3. titanium surface by micro-arc oxidation according to claim 2/steam is handled the method for bioactivity composite coating, it is characterized in that described voltage is 350～500V.
4. titanium surface by micro-arc oxidation according to claim 3/steam is handled the method for bioactivity composite coating, it is characterized in that the electrolytic solution described in the step 2 is mixing of the calcium acetate solution solution that is 5～10g/L by concentration is the disodium ethylene diamine tetra-acetic acid solution of 10～25g/L, sodium hydroxide solution that concentration is 5～20g/L, concentration is 5～10g/L sodium silicate solution, biphosphate calcium solution that concentration is 5～10g/L and concentration, each component of described electrolytic solution is that solvent is prepared with the deionized water.
5. titanium surface by micro-arc oxidation according to claim 4/steam is handled the method for bioactivity composite coating, it is characterized in that adding the deionized water that accounts for reactor cumulative volume 10% described in the step 3 in reactor.
6. titanium surface by micro-arc oxidation according to claim 5/steam is handled the method for bioactivity composite coating, it is characterized in that the steam treatment temp described in the step 3 is 60～100 ℃, and the steam treatment time is 1～12h.
7. titanium surface by micro-arc oxidation according to claim 6/steam is handled the method for bioactivity composite coating, it is characterized in that the steam treatment temp described in the step 3 is 100～150 ℃, and the steam treatment time is 1～10h.
8. titanium surface by micro-arc oxidation according to claim 7/steam is handled the method for bioactivity composite coating, it is characterized in that the steam treatment temp described in the step 3 is 150～200 ℃, and the steam treatment time is 12～24h.
9. titanium surface by micro-arc oxidation according to claim 8/steam is handled the method for bioactivity composite coating, it is characterized in that the steam treatment temp described in the step 3 is 180～250 ℃, and the steam treatment time is 16～24h.
10. titanium surface by micro-arc oxidation according to claim 8/steam is handled the method for bioactivity composite coating, it is characterized in that described titanium sample is TA2, TA3, TA4, TC4 or Ti2448 titanium alloy.
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| CN104645414A (en) * | 2015-02-15 | 2015-05-27 | 宝鸡文理学院 | Titanium-based surface antibacterial and bone tissue regeneration induced functional coating as well as preparation method and application thereof |
| CN105030353A (en) * | 2015-07-10 | 2015-11-11 | 中国人民解放军第四军医大学 | Preparation method of dental implant of multistage nano morphologic structure |
| CN105506709A (en) * | 2015-12-11 | 2016-04-20 | 广州医科大学 | Preparation method of bioactive coatings on surfaces of titanium metals |
| CN106400087A (en) * | 2016-09-08 | 2017-02-15 | 西安交通大学 | Method of preparing titanium implant having bioelectricity activity by carrying out water-vapor treatment on tin-bearing microarc oxidation coating |
| CN107012493A (en) * | 2017-04-12 | 2017-08-04 | 哈尔滨工业大学 | Using microwave steam the apatite nano wire of the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction preparation method |
| CN107034509A (en) * | 2017-04-12 | 2017-08-11 | 哈尔滨工业大学 | A kind of quick in situ has the preparation method for the apatite nanometer rods being necessarily orientated in titanium differential arc oxidation coating surface construction |
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| Publication number | Priority date | Publication date | Assignee | Title |
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Application publication date: 20131009 |