CN103334144B - The alkali liquor steam post-processing approach of titanium surface by micro-arc oxidation bioactivity coatings - Google Patents
The alkali liquor steam post-processing approach of titanium surface by micro-arc oxidation bioactivity coatings Download PDFInfo
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- CN103334144B CN103334144B CN201310302918.7A CN201310302918A CN103334144B CN 103334144 B CN103334144 B CN 103334144B CN 201310302918 A CN201310302918 A CN 201310302918A CN 103334144 B CN103334144 B CN 103334144B
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Abstract
The alkali liquor steam post-processing approach of titanium surface by micro-arc oxidation bioactivity coatings, it relates to the alkali liquor steam post-processing approach of titanium surface by micro-arc oxidation bioactivity coatings.The invention solves the problems that titanium prepared by existing method and alloy surface coating biological activity thereof are more weak, and the hydrothermal treatment consists of routine can cause the dissolution of biological active elements and the less problem of apatite generated.This method process is as follows: titanium and alloy sample surface finish, cleaning；Being placed in the stainless steel trough body containing bioactive ingredients electrolyte by titanium plate and carry out differential arc oxidation, cell liquid temperature controls below 50 DEG C；Being placed in hydrothermal reaction kettle by unsettled for the prepared titanium sample with differential arc oxidation bioactivity coatings, add the 0.001～5mol/L alkali liquor accounting for reactor cumulative volume 8～15%, at 80～220 DEG C, insulation 1-24h carries out alkali liquor Steam treatment.The present invention is used for preparing advanced medical implantation body for bone material.
Description
Technical field
The present invention relates to a kind of technical field of metal surface modification, be specifically related to the alkali liquor steam post-processing approach of a kind of titanium surface by micro-arc oxidation bioactivity coatings.
Background technology
Titanium and alloy thereof are the medical implantation body materials being widely used, but titanium and alloy thereof show as biologically inert in the application, do not possess self-bone grafting ability.Differential arc oxidization technique is a kind of common titanium surface bioactive method of modifying, relates to plasma chemistry, thermal chemical reaction.By regulating electrolyte, the trace element silicon that life entity is useful, calcium, phosphorus, sodium can be incorporated in the middle of the coating generated.But the coating biology activity prepared by the method is more weak, this is accomplished by generated coating is carried out after-treatment, to improve its biological activity.But common hydrothermal treatment consists can cause the dissolution of biological active elements, and the apatite generated is less.
Summary of the invention
The invention aims to solve titanium prepared by existing method and alloy surface coating biological activity is more weak, and the hydrothermal treatment consists of routine can cause the dissolution of biological active elements, and the less problem of apatite generated, and the alkali liquor steam post-processing approach of titanium surface by micro-arc oxidation bioactivity coatings is provided.
The alkali liquor steam post-processing approach of the titanium surface by micro-arc oxidation bioactivity coatings of the present invention, carries out according to following steps:
One, after adopting 200#, 400# and 1000# sand paper that titanium sample is polished, polished successively, clean with deionized water, then at 20～60 DEG C of temperature, dry 1～4h；
Two, differential arc oxidation processes: the titanium sample after step one being dried is placed in the stainless steel trough body containing electrolyte, with titanium sample for anode, with stainless steel trough body for negative electrode, carries out differential arc oxidation；
Three, Steam treatment: adding the concentration accounting for reactor cumulative volume 8～15% in reactor is 0.001～5mol/L alkali liquor, it is positioned in hydrothermal reaction kettle by unsettled for the titanium sample after differential arc oxidation and keep titanium sample at the ullage of alkali liquor, then, at 80～220 DEG C of temperature, it is incubated 1～24h.
The present invention comprises following beneficial effect:
The present invention, keeping on the basis of titanium surface by micro-arc oxidation coating biology activity, at a large amount of apatite of its Surface Creation, significantly improves its biological activity and stability further, extends differential arc oxidation and post-treatment coatings thereof the range of application in implantation body's material.
Coating after the present invention is processed carries out diffractometer EDS spectroscopy detection, and containing silicon, calcium, phosphorus, sodium Active trace element in coating, X-ray diffractometer carries out the test of XRD diffraction and can detect that in coating pure at anatase with apatite.The present invention adopts alkali liquor Steam treatment first on differential arc oxidation coating, it differential arc oxidation bioactivity coatings post-processing approach is an innovation, coating surface will be obtained by the present invention and generate a large amount of apatite, put into 3 days rear surface hydroxyapatite of immersion in simulated body fluid to reach capacity, and common differential arc oxidation sample generates but without any apatite after identical soak time, illustrate that the titanium sample through differential arc oxidation/Steam treatment in the present invention has the biological activity more excellent compared with titanium and common biological activity differential arc oxidation coating thereof.
The alkali liquor steam post-processing approach of the present invention, it is possible to improve biological activity siliceous, calcium, phosphorus, sodium biological active elements differential arc oxidation coating further.Suitable in the implantation body of difformity Yu size, the specimen surface coating surface obtained has a large amount of apatite, has the biological activity of excellence, it is possible to hydroxyapatite is induced in success in simulated body fluid, is favorably improved the binding ability of implantation body and new bone tissue.
Accompanying drawing explanation
Fig. 1 is differential arc oxidation coating surface topography SEM figure after test 1 alkali liquor Steam treatment；
Fig. 2 is the XRD power spectrum picture of differential arc oxidation coating after test 1 alkali liquor Steam treatment；Wherein, A is titanium XRD curve, and B is anatase XRD curve, and C is apatite XRD curve；
Fig. 3 is the power spectrum spectrogram on differential arc oxidation coating surface after test 1 alkali liquor Steam treatment.
Detailed description of the invention
Technical solution of the present invention is not limited to act detailed description of the invention set forth below, also includes the combination in any between each detailed description of the invention.
Detailed description of the invention one: the alkali liquor steam post-processing approach of the titanium surface by micro-arc oxidation bioactivity coatings of present embodiment, carries out according to following steps:
One, after adopting 200#, 400# and 1000# sand paper that titanium sample is polished, polished successively, clean with deionized water, then at 20～60 DEG C of temperature, dry 1～4h；
Two, differential arc oxidation processes: the titanium sample after step one being dried is placed in the stainless steel trough body containing electrolyte, with titanium sample for anode, with stainless steel trough body for negative electrode, carries out differential arc oxidation；
Three, Steam treatment: adding the concentration accounting for reactor cumulative volume 8～15% in reactor is 0.001～5mol/L alkali liquor, it is positioned in hydrothermal reaction kettle by unsettled for the titanium sample after differential arc oxidation and keep titanium sample at the ullage of alkali liquor, then, at 80～220 DEG C of temperature, it is incubated 1～24h.
Present embodiment is keeping on the basis of titanium surface by micro-arc oxidation coating biology activity, at a large amount of apatite of its Surface Creation, significantly improve its biological activity and stability further, extend differential arc oxidation and post-treatment coatings thereof the range of application in implantation body's material.
Coating after present embodiment is processed carries out diffractometer EDS spectroscopy detection, and containing silicon, calcium, phosphorus, sodium Active trace element in coating, X-ray diffractometer carries out the test of XRD diffraction and can detect that in coating pure at anatase with apatite.Present embodiment adopts alkali liquor Steam treatment first on differential arc oxidation coating, it differential arc oxidation bioactivity coatings post-processing approach is an innovation, coating surface will be obtained by present embodiment and generate a large amount of apatite, put into 3 days rear surface hydroxyapatite of immersion in simulated body fluid to reach capacity, and common differential arc oxidation sample generates but without any apatite after identical soak time, illustrate that the titanium sample through differential arc oxidation/Steam treatment in present embodiment has the biological activity more excellent compared with titanium and common biological activity differential arc oxidation coating thereof.
The alkali liquor steam post-processing approach of present embodiment, it is possible to improve biological activity siliceous, calcium, phosphorus, sodium biological active elements differential arc oxidation coating further.Suitable in the implantation body of difformity Yu size, the specimen surface coating surface obtained has a large amount of apatite, has the biological activity of excellence, it is possible to hydroxyapatite is induced in success in simulated body fluid, is favorably improved the binding ability of implantation body and new bone tissue.
Detailed description of the invention two: present embodiment and detailed description of the invention one the difference is that: the differential arc oxidation parameter described in step 2 is as follows: differential arc oxidation adopts pulsed dc voltage, voltage is 250～650V, described differential arc oxidation pulse frequency is 200～800Hz, the dutycycle 4～20% of described differential arc oxidation, described micro-arc oxidation electrolyte temperature is 0～50 DEG C, described differential arc oxidation time 5～20min.Other is identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment and detailed description of the invention one or two the difference is that: described pulsed dc voltage is 300～450V, differential arc oxidation pulse frequency is 400～800Hz, dutycycle 4～8%, electrolyte temperature is 20～40 DEG C, differential arc oxidation time 5～15min.Other is identical with detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three the difference is that: described pulsed dc voltage is 350～400V, differential arc oxidation pulse frequency is 500～600Hz, dutycycle 5～7%, electrolyte temperature is 30～40 DEG C, differential arc oxidation time 5～10min.Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one or four are mixing of the biphosphate calcium solution by concentration to be the disodium ethylene diamine tetra-acetic acid solution of 10～15g/L, concentration the be sodium hydroxide solution of 5～10g/L, concentration to be the sodium silicate solution of 6～8g/L, concentration be 6～8g/L and calcium acetate solution solution that concentration is 7～9g/L the difference is that: the electrolyte described in step 2, and each component of described electrolyte is prepared with deionized water for solvent.Other is identical with one of detailed description of the invention one or four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one or five are mixing of the biphosphate calcium solution by concentration to be the disodium ethylene diamine tetra-acetic acid solution of 15g/L, concentration the be sodium hydroxide solution of 5g/L, concentration to be the sodium silicate solution of 7.1g/L, concentration be 6.3g/L and calcium acetate solution solution that concentration is 8.8g/L the difference is that: the electrolyte described in step 2, and each component of described electrolyte is prepared with deionized water for solvent.Other is identical with one of detailed description of the invention one or five.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention one to six the difference is that: described in step 3 is 0.001～5mol/L alkali liquor to adding the concentration accounting for reactor cumulative volume 9～11% in reactor.Other is identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: one of present embodiment and detailed description of the invention one to seven the difference is that: described in step 3 is 0.001～5mol/L alkali liquor to adding the concentration accounting for reactor cumulative volume 10% in reactor.Other is identical with one of detailed description of the invention one to seven.
Detailed description of the invention nine: one of present embodiment and detailed description of the invention one to eight the difference is that: the alkali liquor described in step 3 is sodium hydroxide solution, ammonia or potassium hydroxide.Other is identical with one of detailed description of the invention one to eight.
Detailed description of the invention ten: one of present embodiment and detailed description of the invention one to nine the difference is that: the Steam treatment temperature described in step 3 is 100～200 DEG C, and the Steam treatment time is 1～20h.Other is identical with one of detailed description of the invention one to nine.
Detailed description of the invention 11: one of present embodiment and detailed description of the invention one to ten the difference is that: the Steam treatment temperature described in step 3 is 120～180 DEG C, and the Steam treatment time is 1～15h.Other is identical with one of detailed description of the invention one to ten.
Detailed description of the invention 11: one of present embodiment and detailed description of the invention one to ten the difference is that: the Steam treatment temperature described in step 3 is 150～200 DEG C, and the Steam treatment time is 12～24h.Other is identical with one of detailed description of the invention one to ten.
Detailed description of the invention 12: one of present embodiment and detailed description of the invention one to ten one the difference is that: the Steam treatment temperature described in step 3 is 140～160 DEG C, and the Steam treatment time is 1～15h.Other is identical with one of detailed description of the invention one to ten one.
Detailed description of the invention 13: one of present embodiment and detailed description of the invention one to ten two the difference is that: the concentration of lye described in step 3 is 0.001～0.01mol/L.Other is identical with one of detailed description of the invention one to ten two.
Detailed description of the invention 14: one of present embodiment and detailed description of the invention one to ten three the difference is that: the concentration of lye described in step 3 is 0.01～0.1mol/L.Other is identical with one of detailed description of the invention one to ten three.
Detailed description of the invention 15: one of present embodiment and detailed description of the invention one to ten four the difference is that: the concentration of lye described in step 3 is 0.1～1mol/L.Other is identical with one of detailed description of the invention one to ten four.
Detailed description of the invention 16: one of present embodiment and detailed description of the invention one to ten five the difference is that: the concentration of lye described in step 3 is 1～5mol/L.Other is identical with one of detailed description of the invention one to ten five.
Detailed description of the invention 17: one of present embodiment and detailed description of the invention one to ten six the difference is that: described titanium sample is TA2, TA3, TA4, TC4 or Ti2448 titanium alloy.Other is identical with one of detailed description of the invention one to ten six.
Beneficial effects of the present invention is verified by tests below:
Test 1
The alkali liquor steam post-processing approach of the titanium surface by micro-arc oxidation bioactivity coatings of this test, carries out according to following steps:
Step one: adopt 200#, 400# and 1000# sand paper that TA3 matrix titanium plate sample is polished, polished successively, after cleaning with deionized water, dries 2 hours at 40 DEG C of temperature；
Step 2: differential arc oxidation processes: being placed in the stainless steel trough body containing bioactive ingredients electrolyte by TA3 matrix titanium plate, with TA3 matrix titanium plate for anode, stainless steel trough body is negative electrode, carries out differential arc oxidation；
Step 3: the Steam treatment of TA3 differential arc oxidation sample: by unsettled for the TA3 differential arc oxidation sample hydrothermal reaction kettle being positioned over 50mL, the 0.01mol/L sodium hydroxide solution of 5mL is added to reactor, keep TA3 differential arc oxidation sample unsettled above sodium hydroxide solution liquid level, when temperature is 150 DEG C, it is incubated 3 hours.
Described differential arc oxidation pulsed dc voltage is 400V, and described differential arc oxidation pulse frequency is 700Hz, and the dutycycle of described differential arc oxidation is 6%, and described microarc oxidation solution temperature is 0～50 DEG C, and the described differential arc oxidation time is 10min.By the control to differential arc oxidation electrical quantity, make the differential arc oxidation coating of Surface Creation at 1～20 μm；
Described biological activity electrolyte is to make each component of electrolyte with deionized water for solvent, its concentration is 15 g/l of disodium ethylene diamine tetra-acetic acid solutions, 5 g/l of sodium hydroxide solutions, 7.1 g/l of sodium silicate solutions, 6.3 g/l of biphosphate calcium solutions and 8.8 g/l of calcium acetate solutions respectively, by above-mentioned electrolyte, differential arc oxidation are prepared in coating containing silicon, calcium, phosphorus, sodium trace element.
The coating that this test obtains carries out X-ray diffractometer and carries out XRD diffraction test (as shown in Figure 2), Fig. 2 can find out, it is possible to can detect that there is anatase and apatite in coating.Scanning electron microscope SEM observes (see figure 1), found that superficial growth has column apatite by Fig. 1, apatite draw ratio is between 100～500, diffractometer EDS spectroscopy detection (as shown in Figure 3), from the figure 3, it may be seen that containing silicon, calcium, phosphorus, sodium Active trace element in coating.3 days rear surface hydroxyapatite of immersion in simulated body fluid will be put into by this experiment acquisition titanium surface by micro-arc oxidation bioactivity coatings to reach capacity.
Test 2
This test with test 1 the difference is that: differential arc oxidation voltage described in step 2 is 300～450V.Other step and parameter and test 1 are identical.
The coating that this test obtains exists anatase and apatite.Having column apatite in coating surface growth, apatite draw ratio is between 300～500, containing silicon, calcium, phosphorus, sodium Active trace element in coating.3 days rear surface hydroxyapatite of immersion in simulated body fluid will be put into by this experiment acquisition titanium surface by micro-arc oxidation bioactivity coatings to reach capacity.
Test 3
This test with test 1 the difference is that: Steam treatment temperature described in step 3 is 150～220 DEG C.Other step and parameter and test 1 are identical.
The coating that this test obtains exists anatase and apatite.Having column apatite in coating surface growth, apatite draw ratio is between 150～200, containing silicon, calcium, phosphorus, sodium Active trace element in coating.3 days rear surface hydroxyapatite of immersion in simulated body fluid will be put into by this experiment acquisition titanium surface by micro-arc oxidation bioactivity coatings to reach capacity.
Test 4
This test with test 1 the difference is that: sodium hydroxide lye concentration described in step 3 is 0.001～0.01mol/L.Other step and parameter and test 1 are identical.
The coating that this test obtains exists anatase and apatite.Having column apatite in coating surface growth, apatite draw ratio is between 300～500, containing silicon, calcium, phosphorus, sodium Active trace element in coating.3 days rear surface hydroxyapatite of immersion in simulated body fluid will be put into by this experiment acquisition titanium surface by micro-arc oxidation bioactivity coatings to reach capacity.
Test 5
This test with test 1 the difference is that: sodium hydroxide lye concentration described in step 3 is 0.01～0.1mol/L.Other step and parameter and test 1 are identical.
The coating that this test obtains exists anatase and apatite.Having column apatite in coating surface growth, apatite draw ratio is between 200～300, containing silicon, calcium, phosphorus, sodium Active trace element in coating.3 days rear surface hydroxyapatite of immersion in simulated body fluid will be put into by this experiment acquisition titanium surface by micro-arc oxidation bioactivity coatings to reach capacity.
Test 6
This test with test 1 the difference is that: sodium hydroxide lye concentration described in step 3 is 0.1～1mol/L.Other step and parameter and test 1 are identical.
The coating that this test obtains exists anatase and apatite.Having column apatite in coating surface growth, apatite draw ratio is between 100～200, containing silicon, calcium, phosphorus, sodium Active trace element in coating.5 days rear surface hydroxyapatite of immersion in simulated body fluid will be put into by this experiment acquisition titanium surface by micro-arc oxidation bioactivity coatings to reach capacity.
Test 7
This test and test 1 the difference is that: sodium hydroxide lye concentration described in step 3 is 1～5mol/L, and substrate titanium plate used is TA3, and other step and parameter and test 1 are identical.
The coating that this test obtains exists anatase and apatite.Having column apatite in coating surface growth, apatite draw ratio is between 50～100, containing silicon, calcium, phosphorus, sodium Active trace element in coating.7 days rear surface hydroxyapatite of immersion in simulated body fluid will be put into by this experiment acquisition titanium surface by micro-arc oxidation bioactivity coatings to reach capacity.
Test 8
This test with test 1 the difference is that: the concentration of potassium hydroxide alkali liquor described in step 3 is 1～5mol/L.Other step and parameter and test 1 are identical.
The coating that this test obtains exists anatase and apatite.Having column apatite in coating surface growth, apatite draw ratio is between 80～150, containing silicon, calcium, phosphorus, sodium Active trace element in coating.7 days rear surface hydroxyapatite of immersion in simulated body fluid will be put into by this experiment acquisition titanium surface by micro-arc oxidation bioactivity coatings to reach capacity.
Test 9
This test with test 1 the difference is that: ammonia concentration of lye described in step 3 is 1～5mol/L.Other step and parameter and test 1 are identical.
The coating that this test obtains exists anatase and apatite.Having column apatite in coating surface growth, apatite draw ratio is between 200～300, containing silicon, calcium, phosphorus, sodium Active trace element in coating.7 days rear surface hydroxyapatite of immersion in simulated body fluid will be put into by this experiment acquisition titanium surface by micro-arc oxidation bioactivity coatings to reach capacity.
Above-mentioned test 1 is as shown in table 1 to the simulated body fluid constituent content described in test 9.
The chemical agent content of 1 liter of simulated body fluid prepared by table 1
Claims (4)
1. the alkali liquor steam post-processing approach of titanium surface by micro-arc oxidation bioactivity coatings, it is characterised in that it carries out according to following steps:
One, after adopting 200#, 400# and 1000# sand paper that titanium sample is polished, polished successively, clean with deionized water, then at 20～60 DEG C of temperature, dry 1～4h；
Two, differential arc oxidation processes: the titanium sample after step one being dried is placed in the stainless steel trough body containing electrolyte, with titanium sample for anode, with stainless steel trough body for negative electrode, carries out differential arc oxidation；
Three, Steam treatment: adding the concentration accounting for reactor cumulative volume 8～15% in reactor is 0.1～1mol/L alkali liquor, it is positioned in hydrothermal reaction kettle by unsettled for the titanium sample after differential arc oxidation and keep titanium sample at the ullage of alkali liquor, then, at 80～220 DEG C of temperature, it is incubated 1～24h；
Alkali liquor described in step 3 is sodium hydroxide solution, ammonia or potassium hydroxide；Described titanium sample is TA2, TA3, TA4, TC4 or Ti2448 titanium alloy；Electrolyte described in step 2 is mixing of the biphosphate calcium solution by concentration to be the disodium ethylene diamine tetra-acetic acid solution of 10～20g/L, concentration the be sodium hydroxide solution of 5～25g/L, concentration to be the sodium silicate solution of 5～9g/L, concentration be 4～8g/L and calcium acetate solution solution that concentration is 5～10g/L, and each component of described electrolyte is prepared with deionized water for solvent.
2. the alkali liquor steam post-processing approach of titanium surface by micro-arc oxidation bioactivity coatings according to claim 1, it is characterized in that the differential arc oxidation parameter described in step 2 is as follows: differential arc oxidation adopts pulsed dc voltage, voltage is 250～650V, described differential arc oxidation pulse frequency is 200～800Hz, the dutycycle 4～20% of described differential arc oxidation, described micro-arc oxidation electrolyte temperature is 0～50 DEG C, described differential arc oxidation time 5～20min.
3. the alkali liquor steam post-processing approach of titanium surface by micro-arc oxidation bioactivity coatings according to claim 1, it is characterised in that the Steam treatment temperature described in step 3 is 100～200 DEG C, and the Steam treatment time is 1～20h.
4. the alkali liquor steam post-processing approach of titanium surface by micro-arc oxidation bioactivity coatings according to claim 3, it is characterised in that the Steam treatment temperature described in described step 3 is 140～160 DEG C, and the Steam treatment time is 1～15h.
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| 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 |
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| CN107034509B (en) * | 2017-04-12 | 2019-04-16 | 哈尔滨工业大学 | A kind of quick in situ has the preparation method for the apatite nanometer rods being centainly orientated in the building of titanium differential arc oxidation coating surface |
| CN110219013A (en) * | 2019-06-24 | 2019-09-10 | 天津大学 | A kind of electrode material of self-supporting nitrogen modification nickel iron hydroxide |
| CN116535884B (en) * | 2023-05-26 | 2024-02-20 | 西安科技大学 | Compact corrosion-resistant wear-resistant SWF/LDHs composite coating on magnesium-lithium alloy surface and preparation method thereof |
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