CN103334144A - Alkaline liquid water vapor post-treatment method of micro-arc oxidation biological active coating on surface of titanium - Google Patents
Alkaline liquid water vapor post-treatment method of micro-arc oxidation biological active coating on surface of titanium Download PDFInfo
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Abstract
The invention relates to an alkaline liquid water vapor post-treatment method of a micro-arc oxidation biological active coating on the surface of titanium, and aims to solve the problems that biological activity of coatings on surfaces of titanium and alloys of the titanium is weaker, conventional hydro-thermal treatment can cause dissolving-out of biological active elements, and less apatite is generated. The method comprises the processes as follows; surfaces of the titanium and the alloy samples are polished and washed; a titanium plate is placed into a stainless steel cell containing a bioactive constituent electrolyte for micro-arc oxidation, and the temperature of the liquid inside the electrolytic cell is controlled to be 50 DEG C below; and a prepared titanium sample provided with the micro-arc oxidation biological active coating is suspended and placed into a hydrothermal reaction kettle, 0.001mol/L-5mol/L of an alkali liquid accounting for 8%-15% of the total volume of the reaction kettle is added, heat preservation is performed at the temperature of 80 DEG C-220 DEG C for 1-24 hours, and then alkaline liquid water vapor treatment is performed. The method is used for preparing an advanced medical implant materials used as a bone substitute.
Description
Technical field
The present invention relates to a kind of Metal Surface Modification Technique field, be specifically related to a kind of alkali lye steam post-treating method of titanium surface by micro-arc oxidation bioactive coating.
Background technology
Titanium and alloy thereof are the medical planting body materials that has been widely used, but titanium and alloy thereof show as biologically inert in application, do not possess the bone inducibility.Differential arc oxidization technique is a kind of common titanium surface bioactive method of modifying, relates to plasma chemistry, thermal chemical reaction.By regulating electrolytic solution, 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, to improve its biological activity.But common hydrothermal treatment consists can cause the stripping of biological activity element, and the phosphatic rock that generates is less.
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 stripping of biological activity element, and the problem that the phosphatic rock that generates is less, and provide the alkali lye steam post-treating method of titanium surface by micro-arc oxidation bioactive coating.
The alkali lye steam post-treating method of titanium surface by micro-arc oxidation bioactive coating of the present invention, carry 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 20～60 ℃ of temperature, dry 1～4h 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: adding the concentration that accounts for reactor cumulative volume 8～15% in the reactor is 0.001～5mol/L alkali lye, be positioned in the hydrothermal reaction kettle and keep the titanium sample above the liquid level of alkali lye the titanium sample behind the differential arc oxidation is unsettled, under 80～220 ℃ of temperature, be incubated 1～24h then.
The present invention comprises following beneficial effect:
The present invention generates a large amount of phosphatic rock on its surface on the basis that keeps titanium surface by micro-arc oxidation coating biology activity, further significantly improved its biological activity and stability, has expanded differential arc oxidation and post-treatment coatings thereof the range of application in the planting body material.
Coating after the present invention's processing is carried out diffractometer EDS spectroscopy detection, contain silicon, calcium, phosphorus, sodium trace active element in the coating, 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 alkali lye 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.
Alkali lye 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, the specimen surface coatingsurface that obtains has a large amount of phosphatic rock, have excellent biological activity, 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 handles the XRD power spectrum picture of back differential arc oxidation coating for test 1 alkali lye steam; Wherein, A is titanium XRD curve, and B is anatase octahedrite XRD curve, and C is phosphatic rock XRD curve;
Fig. 2 handles back differential arc oxidation coating surface topography SEM figure for test 1 alkali lye steam;
Fig. 3 handles the power spectrum spectrogram on differential arc oxidation coating surface, back for test 1 alkali lye 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 alkali lye steam post-treating method of the titanium surface by micro-arc oxidation bioactive coating of present embodiment, carry 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 20～60 ℃ of temperature, dry 1～4h 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: adding the concentration that accounts for reactor cumulative volume 8～15% in the reactor is 0.001～5mol/L alkali lye, be positioned in the hydrothermal reaction kettle and keep the titanium sample above the liquid level of alkali lye the titanium sample behind the differential arc oxidation is unsettled, under 80～220 ℃ of temperature, be incubated 1～24h then.
Present embodiment is on the basis that keeps titanium surface by micro-arc oxidation coating biology activity, generate a large amount of phosphatic rock on its surface, further significantly improve its biological activity and stability, expanded differential arc oxidation and post-treatment coatings thereof the range of application in the planting body material.
Coating after the present embodiment processing is carried out diffractometer EDS spectroscopy detection, contain silicon, calcium, phosphorus, sodium trace active element in the coating, 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 alkali lye 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 alkali lye 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, the specimen surface coatingsurface that obtains has a large amount of phosphatic rock, have excellent biological activity, 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 250～650V, described differential arc oxidation pulse-repetition is 200～800Hz, the dutycycle 4～20% of described differential arc oxidation, described differential arc oxidation electrolyte temperature is 0～50 ℃, described differential arc oxidation time 5～20min.Other is identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is: described pulsed dc voltage is 300～450V, the differential arc oxidation pulse-repetition is 400～800Hz, dutycycle 4～8%, electrolyte temperature are 20～40 ℃, differential arc oxidation time 5～15min.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 500～600Hz, dutycycle 5～7%, electrolyte temperature are 30～40 ℃, 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 6～8g/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: described in the step 3 to add the concentration that accounts for reactor cumulative volume 9～11% in the reactor be 0.001～5mol/L alkali lye.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: described in the step 3 to add the concentration that accounts for reactor cumulative volume 10% in the reactor be 0.001～5mol/L alkali lye.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 alkali lye described in the step 3 is sodium hydroxide solution, ammoniacal liquor or potassium hydroxide.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 100～200 ℃, and the steam treatment time is 1～20h.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 120～180 ℃, and the steam treatment time is 1～15h.Other is identical with one of embodiment one to ten.
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 140～160 ℃, and the steam treatment time is 1～15h.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: the concentration of lye described in the step 3 is 0.001～0.01mol/L.Other is identical with one of embodiment one to 12.
Embodiment 14: what present embodiment was different with one of embodiment one to 13 is: the concentration of lye described in the step 3 is 0.01～0.1mol/L.Other is identical with one of embodiment one to 13.
Embodiment 15: what present embodiment was different with one of embodiment one to 14 is: the concentration of lye described in the step 3 is 0.1～1mol/L.Other is identical with one of embodiment one to 14.
Embodiment 16: what present embodiment was different with one of embodiment one to 15 is: the concentration of lye described in the step 3 is 1～5mol/L.Other is identical with one of embodiment one to 15.
Embodiment 17: what present embodiment was different with one of embodiment one to 16 is: described titanium sample is TA2, TA3, TA4, TC4 or Ti2448 titanium alloy.Other is identical with one of embodiment one to 16.
By following verification experimental verification beneficial effect of the present invention:
Test 1
The alkali lye steam post-treating method of the titanium surface by micro-arc oxidation bioactive coating of this test, carry out according to following steps:
Step 1: adopt 200#, 400# and 1000# sand paper that TA3 matrix titanium plate sample is polished, polished successively, after washed with de-ionized water, oven dry is 2 hours under 40 ℃ of temperature;
Step 2: differential arc oxidation is handled: TA3 matrix titanium plate is placed the stainless steel trough body that contains bioactive ingredients electrolytic solution, is anode with TA3 matrix titanium plate, and stainless steel trough body is negative electrode, carries out differential arc oxidation;
Step 3: the steam of TA3 differential arc oxidation sample is handled: in the unsettled hydrothermal reaction kettle that is positioned over 50mL of TA3 differential arc oxidation sample, the 0.01mol/L sodium hydroxide solution that adds 5mL to reactor, keep TA3 differential arc oxidation sample unsettled above the sodium hydroxide solution liquid level, be under 150 ℃ the condition, to be incubated 3 hours in temperature.
Described differential arc oxidation pulsed dc voltage is 400V, and described differential arc oxidation pulse-repetition is 700Hz, and the dutycycle of described differential arc oxidation is 6%, and described differential arc oxidation solution temperature is 0～50 ℃, and the described differential arc oxidation time is 10min.By the control to the differential arc oxidation electrical parameter, make the differential arc oxidation coating of surface generation at 1～20 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.
The coating that this test obtains is carried out X-ray diffractometer and is carried out XRD diffraction test (as shown in Figure 1), can be found out by Fig. 1, can detect to have anatase octahedrite and phosphatic rock in the coating.Scanning electronic microscope SEM observes (seeing shown in Figure 2), find that by Fig. 2 surface growth has column phosphatic rock, the phosphatic rock length-to-diameter ratio between 100～500, diffractometer EDS spectroscopy detection (as shown in Figure 3), as shown in Figure 3, contain silicon, calcium, phosphorus, sodium trace active element in the coating.To put into 3 days rear surface hydroxyapatites of simulated body fluid immersion by this experiment acquisition titanium surface by micro-arc oxidation bioactive coating reaches capacity.
Test 2
This test and test 1 are different to be: the voltage of differential arc oxidation described in the step 2 is 300～450V.Other step and parameter are identical with test 1.
There are anatase octahedrite and phosphatic rock in the coating that this test obtains.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 300～500.To put into 3 days rear surface hydroxyapatites of simulated body fluid immersion by this experiment acquisition titanium surface by micro-arc oxidation bioactive coating reaches capacity.
Test 3
This test and test 1 are different to be: the treatment temp of steam described in the step 3 is 150～220 ℃.Other step and parameter are identical with test 1.
There are anatase octahedrite and phosphatic rock in the coating that this test obtains.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 150～200.To put into 3 days rear surface hydroxyapatites of simulated body fluid immersion by this experiment acquisition titanium surface by micro-arc oxidation bioactive coating reaches capacity.
This test and test 1 are different to be: the concentration of sodium hydroxide lye described in the step 3 is 0.001～0.01mol/L.Other step and parameter are identical with test 1.
There are anatase octahedrite and phosphatic rock in the coating that this test obtains.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 300～500.To put into 3 days rear surface hydroxyapatites of simulated body fluid immersion by this experiment acquisition titanium surface by micro-arc oxidation bioactive coating reaches capacity.
This test and test 1 are different to be: the concentration of sodium hydroxide lye described in the step 3 is 0.01～0.1mol/L.Other step and parameter are identical with test 1.
There are anatase octahedrite and phosphatic rock in the coating that this test obtains.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.To put into 3 days rear surface hydroxyapatites of simulated body fluid immersion by this experiment acquisition titanium surface by micro-arc oxidation bioactive coating reaches capacity.
This test and test 1 are different to be: the concentration of sodium hydroxide lye described in the step 3 is 0.1～1mol/L.Other step and parameter are identical with test 1.
There are anatase octahedrite and phosphatic rock in the coating that this test obtains.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 100～200.To put into 5 days rear surface hydroxyapatites of simulated body fluid immersion by this experiment acquisition titanium surface by micro-arc oxidation bioactive coating reaches capacity.
Test 7
This test and test 1 are different to be: the concentration of sodium hydroxide lye described in the step 3 is 1～5mol/L, and used substrate titanium plate is TA3, and other step and parameter are identical with test 1.
There are anatase octahedrite and phosphatic rock in the coating that this test obtains.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.To put into 7 days rear surface hydroxyapatites of simulated body fluid immersion by this experiment acquisition titanium surface by micro-arc oxidation bioactive coating reaches capacity.
Test 8
This test and test 1 are different to be: the alkali lye of potassium hydroxide described in step 3 concentration is 1～5mol/L.Other step and parameter are identical with test 1.
There are anatase octahedrite and phosphatic rock in the coating that this test obtains.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 80～150.To put into 7 days rear surface hydroxyapatites of simulated body fluid immersion by this experiment acquisition titanium surface by micro-arc oxidation bioactive coating reaches capacity.
Test 9
This test and test 1 are different to be: the concentration of lye of ammoniacal liquor described in the step 3 is 1～5mol/L.Other step and parameter are identical with test 1.
There are anatase octahedrite and phosphatic rock in the coating that this test obtains.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.To put into 7 days rear surface hydroxyapatites of simulated body fluid immersion by this experiment acquisition titanium surface by micro-arc oxidation bioactive coating reaches capacity.
Above-mentioned test 1 is as shown in table 1 to test 9 described simulated body fluid component concentrations.
The chemical reagent content of 1 liter of simulated body fluid of table 1 preparation
Claims (10)
1. the alkali lye steam post-treating method of titanium surface by micro-arc oxidation bioactive coating 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 20～60 ℃ of temperature, dry 1～4h 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: adding the concentration that accounts for reactor cumulative volume 8～15% in the reactor is 0.001～5mol/L alkali lye, be positioned in the hydrothermal reaction kettle and keep the titanium sample above the liquid level of alkali lye the titanium sample behind the differential arc oxidation is unsettled, under 80～220 ℃ of temperature, be incubated 1～24h then.
2. the alkali lye steam post-treating method of titanium surface by micro-arc oxidation bioactive coating according to claim 1, 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 250～650V, described differential arc oxidation pulse-repetition is 200～800Hz, the dutycycle 4～20% of described differential arc oxidation, described differential arc oxidation electrolyte temperature is 0～50 ℃, described differential arc oxidation time 5～20min.
3. the alkali lye steam post-treating method of titanium surface by micro-arc oxidation bioactive coating according to claim 2, 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 10～20g/L, sodium hydroxide solution that concentration is 5～25g/L, concentration is 5～9g/L sodium silicate solution, biphosphate calcium solution that concentration is 4～8g/L and concentration, each component of described electrolytic solution is that solvent is prepared with the deionized water.
4. the alkali lye steam post-treating method of titanium surface by micro-arc oxidation bioactive coating according to claim 3, it is characterized in that described in the step 3 to add the concentration that accounts for reactor cumulative volume 10% in the reactor be 0.001～5mol/L alkali lye.
5. the alkali lye steam post-treating method of titanium surface by micro-arc oxidation bioactive coating according to claim 4 is characterized in that the alkali lye described in the step 3 is sodium hydroxide solution, ammoniacal liquor or potassium hydroxide.
6. the alkali lye steam post-treating method of titanium surface by micro-arc oxidation bioactive coating according to claim 5 is characterized in that the steam treatment temp described in the step 3 is 100～200 ℃, and the steam treatment time is 1～20h.
7. the alkali lye steam post-treating method of titanium surface by micro-arc oxidation bioactive coating according to claim 6 is characterized in that the steam treatment temp described in the described step 3 is 140～160 ℃, and the steam treatment time is 1～15h.
8. the alkali lye steam post-treating method of titanium surface by micro-arc oxidation bioactive coating according to claim 7 is characterized in that described alkali lye 0.1～1mol/L.
9. the alkali lye steam post-treating method of titanium surface by micro-arc oxidation bioactive coating according to claim 8 is characterized in that described alkali lye 1～5mol/L.
10. the alkali lye steam post-treating method of titanium surface by micro-arc oxidation bioactive coating according to claim 9 is characterized in that described titanium sample is TA2, TA3, TA4, TC4 or Ti2448 titanium alloy.
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| 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 |
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| CN116535884A (en) * | 2023-05-26 | 2023-08-04 | 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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