CN107012493A - Using microwave steam the apatite nano wire of the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction preparation method - Google Patents
Using microwave steam the apatite nano wire of the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction preparation method Download PDFInfo
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Abstract
Using microwave steam in the preparation method of the apatite nano wire of the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction, the preparation method of the nano wire of periodontal membrane fiber beam is similar to the present invention relates to a kind of titanium differential arc oxidation coating surface construction.The invention solves the problems that root of the tooth planting body lacks the structure similar to periodontal membrane fiber beam, the problem of being easily caused the failure of operation in existing tooth-implanting technology.Method：First, the pretreatment of titanium material；2nd, differential arc oxidation is handled；3rd, microwave Steam treatment.The present invention is used for the preparation in the apatite nano wire of the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction using microwave steam.
Description
Technical field
The preparation of the nano wire of periodontal membrane fiber beam is similar to the present invention relates to a kind of titanium differential arc oxidation coating surface construction
Method.
Background technology
Current tooth-implanting technology is the important means that tooth defect or missing are repaired, but tooth root planting body lacks and is similar to
The structure of periodontal membrane fiber beam, is easily caused the failure of operation, and current clinic there is no basic solution.Normal periodontium
Structure is cementum, parodontium, alveolar bone and gum composition successively outwards by root of the tooth.Cementum surrounds root surface
A thin layer osteoid tissue, parodontium is made up of dense connective tissue, most fiber alignment bunchys, and one end of fiber is embedded in dentale
In matter, the other end is then embedded in tooth socket bone wall, tooth is seated in tooth socket.Between cementum, parodontium and alveolar bone
The ligament anchor chain structure of foundation is the key of Periodontal Supporting Tissue, and parodontium serves vital work in periodontium
With.
The content of the invention
The invention solves the problems that root of the tooth planting body lacks the structure similar to periodontal membrane fiber beam in existing tooth-implanting technology, hold
The problem of being easily caused the failure of operation, and provide fine in the similar parodontium of titanium differential arc oxidation coating surface construction using microwave steam
Tie up the preparation method of the apatite nano wire of beam.
Using microwave steam titanium differential arc oxidation coating surface construction similar periodontal membrane fiber beam apatite nano wire
Preparation method, is specifically followed the steps below：
First, the pretreatment of titanium material：Titanium material surface is beaten using 200#, 400# and 1000# abrasive paper for metallograph successively
After mill and polishing, cleaned successively with acetone, absolute ethyl alcohol and deionized water, 3h is dried under conditions of temperature is 40 DEG C~80 DEG C
~5h, obtains pretreated titanium material；
2nd, differential arc oxidation is handled：Pretreated titanium material is placed in the stainless steel containing bioactive ingredients electrolyte
In electrolytic cell, using pretreated titanium material as anode, stainless-steel sheet is negative electrode, differential arc oxidation is carried out, using pulse direct current
Voltage, is that 350V~450V, pulse frequency are that 500Hz~800Hz, dutycycle are 4%~10% and electrolyte temperature in voltage
Under conditions of 0 DEG C~35 DEG C, differential arc oxidation 5min~40min obtains the titanium material after differential arc oxidation processing；
Described contains bioactive ingredients electrolyte by deionized water, disodium ethylene diamine tetraacetate, sodium hydroxide, silicic acid
Sodium, calcium dihydrogen phosphate and calcium acetate are mixed；Described contains disodium ethylene diamine tetraacetate in bioactive ingredients electrolyte
Concentration be 8g/L~25g/L；The described concentration containing sodium hydroxide in bioactive ingredients electrolyte is 3g/L~25g/
L；The described concentration containing sodium metasilicate in bioactive ingredients electrolyte is 5g/L~25g/L；Described contains bioactivity
The concentration of calcium dihydrogen phosphate is 5g/L~10g/L in composition electrolyte；Described contains acetic acid in bioactive ingredients electrolyte
The concentration of calcium is 5g/L~20g/L；
3rd, microwave Steam treatment：Into the special hydrothermal reaction kettle of the microwave hydrothermal of polytetrafluoroethylene (PTFE) material add pure water or
Concentration is 0.01mol/L~5.0mol/L alkali lye, and the titanium material after differential arc oxidation is handled is suspended from is apart from pure water or concentration
0.01mol/L~5.0mol/L more than alkali lye water surface 30mm, is then placed in microwave attenuation materials parallelometer by hydrothermal reaction kettle
In, under conditions of temperature is 180 DEG C~250 DEG C, 60min~300min is incubated, that is, is completed using microwave steam in the titanium differential of the arc
The preparation method of the apatite nano wire of the similar periodontal membrane fiber beam of oxide covering surface construction；
It is hydro-thermal that the alkali lye volume that pure water or concentration are 0.01mol/L~5.0mol/L is added in described hydrothermal reaction kettle
The 10%~30% of reactor cumulative volume；
Described alkali lye is sodium hydroxide solution, ammoniacal liquor or potassium hydroxide solution.
The beneficial effects of the invention are as follows：The present invention prepares base on the basis of pure titanium using differential arc oxidation and microwave steam method
The apatite nano wire that layer building imitates periodontal membrane fiber beam is applied in titanium dioxide ceramic, differential arc oxidation coating imitates the tooth of periodontium
Essence, apatite nano wire imitates the fibre bundle of parodontium, and apatite nano-thread in-situ is formed at differential arc oxidation coating surface.The differential of the arc
The substantial amounts of apatite nano wire in oxide covering surface has certain orientation, but Growth In Space exist on direction be it is different, this
Sample meets the different directions of periodontal membrane fiber beam and plays different effect and function in diverse location.Apatite nano wire is by applying
Layer inner element is diffused into surface, and formed by then forming core is grown up, therefore, nano-thread in-situ, which is grown on coating surface, to be had well
Binding ability, can also carry the scattered of different directions power in tooth engagement process, it is ensured that tooth root planting body is present in tooth socket
It is interior, keep stable.Sample after present invention processing is carried out micro containing calcium phosphorus silicon sodium in diffractometer EDS spectroscopy detections, coating
Element.X-ray diffractometer carries out the detection of XRD diffraction and specimen surface after the sample after present invention processing and immersion simulated body fluid is deposited
In anatase and apatite phase.The sign of the structure of sample after processing of the present invention is carried out by SEM.The present invention
Microwave and hydro-thermal are combined first, applied to periodontal membrane fiber beam function and the structure of effect, differential arc oxidation coating imitates tooth
The function of essence and effect, surface apatite nano wire imitate function and the effect of fibre bundle.The present invention is obtained into coating to have generated
It is a large amount of that there is the apatite being necessarily orientated, it is put into simulated body fluid and soaks surface hydroxyl apatite after 20h and reach saturation, and it is conventional
The sample that hydro-thermal process (mutually synthermal, time) is obtained passes through identical soak time, and surface does not have any apatite to give birth to substantially
Into.Illustrate in the present invention differential arc oxidation titanium of the more conventional Steam treatment of titanium of the differential arc oxidation coating after microwave Steam treatment and its
Common differential arc oxidation coating has higher bioactivity and apatite inducibility.
The present invention is used for the phosphorus ash in the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction using microwave steam
The preparation method of stone nano wire.
Brief description of the drawings
The XRD spectrum of differential arc oxidation coating after the microwave Steam treatment that Fig. 1 is prepared for embodiment one；A is anatase peak,
B is titanium peak, and C is apatite peak；
The scanned photograph of differential arc oxidation coating after the microwave Steam treatment that Fig. 2 is prepared for embodiment one；
The EDS power spectrum spectrograms of differential arc oxidation coating after the microwave Steam treatment that Fig. 3 is prepared for embodiment one；
Fig. 4 is that the differential arc oxidation coating after microwave Steam treatment prepared by embodiment one soaks sweeping after simulated body fluid 20h
Retouch photo.
Embodiment
Technical solution of the present invention is not limited to the embodiment of act set forth below, in addition to each embodiment it
Between any combination.
Embodiment one：Use microwave steam described in present embodiment is in titanium differential arc oxidation coating surface construction class
Followed the steps below like the preparation method of the apatite nano wire of periodontal membrane fiber beam：
First, the pretreatment of titanium material：Titanium material surface is beaten using 200#, 400# and 1000# abrasive paper for metallograph successively
After mill and polishing, cleaned successively with acetone, absolute ethyl alcohol and deionized water, 3h is dried under conditions of temperature is 40 DEG C~80 DEG C
~5h, obtains pretreated titanium material；
2nd, differential arc oxidation is handled：Pretreated titanium material is placed in the stainless steel containing bioactive ingredients electrolyte
In electrolytic cell, using pretreated titanium material as anode, stainless-steel sheet is negative electrode, differential arc oxidation is carried out, using pulse direct current
Voltage, is that 350V~450V, pulse frequency are that 500Hz~800Hz, dutycycle are 4%~10% and electrolyte temperature in voltage
Under conditions of 0 DEG C~35 DEG C, differential arc oxidation 5min~40min obtains the titanium material after differential arc oxidation processing；
Described contains bioactive ingredients electrolyte by deionized water, disodium ethylene diamine tetraacetate, sodium hydroxide, silicic acid
Sodium, calcium dihydrogen phosphate and calcium acetate are mixed；Described contains disodium ethylene diamine tetraacetate in bioactive ingredients electrolyte
Concentration be 8g/L~25g/L；The described concentration containing sodium hydroxide in bioactive ingredients electrolyte is 3g/L~25g/
L；The described concentration containing sodium metasilicate in bioactive ingredients electrolyte is 5g/L~25g/L；Described contains bioactivity
The concentration of calcium dihydrogen phosphate is 5g/L~10g/L in composition electrolyte；Described contains acetic acid in bioactive ingredients electrolyte
The concentration of calcium is 5g/L~20g/L；
3rd, microwave Steam treatment：Into the special hydrothermal reaction kettle of the microwave hydrothermal of polytetrafluoroethylene (PTFE) material add pure water or
Concentration is 0.01mol/L~5.0mol/L alkali lye, and the titanium material after differential arc oxidation is handled is suspended from is apart from pure water or concentration
0.01mol/L~5.0mol/L more than alkali lye water surface 30mm, is then placed in microwave attenuation materials parallelometer by hydrothermal reaction kettle
In, under conditions of temperature is 180 DEG C~250 DEG C, 60min~300min is incubated, that is, is completed using microwave steam in the titanium differential of the arc
The preparation method of the apatite nano wire of the similar periodontal membrane fiber beam of oxide covering surface construction；
It is hydro-thermal that the alkali lye volume that pure water or concentration are 0.01mol/L~5.0mol/L is added in described hydrothermal reaction kettle
The 10%~30% of reactor cumulative volume；
Described alkali lye is sodium hydroxide solution, ammoniacal liquor or potassium hydroxide solution.
The beneficial effect of present embodiment is：Present embodiment uses differential arc oxidation and microwave steam side on the basis of pure titanium
Prepared by method applies the apatite nano wire that layer building imitates periodontal membrane fiber beam based on titanium dioxide ceramic, and differential arc oxidation coating imitates periodontal
The dentine of tissue, apatite nano wire imitates the fibre bundle of parodontium, and apatite nano-thread in-situ is formed at differential arc oxidation coating
Surface.The substantial amounts of apatite nano wire in differential arc oxidation coating surface has certain orientation, but exists in Growth In Space on direction and be
It is different, so meet the different directions of periodontal membrane fiber beam and play different effect and function in diverse location.Apatite is received
Rice noodles are that formed by then forming core is grown up, therefore, nano-thread in-situ is grown on coating by coat inside elements diffusion to surface
There is good binding ability on surface, can also carry the scattered of different directions power in tooth engagement process, it is ensured that tooth root planting body is deposited
It is in tooth socket, keeps stable.Sample after present embodiment processing contain in diffractometer EDS spectroscopy detections, coating
There is calcium phosphorus silicon sodium trace element.X-ray diffractometer carries out the detection of XRD diffraction to the sample after present embodiment processing and immersion mould
Intend specimen surface after body fluid and there is anatase and apatite phase.Carry out trying after present embodiment processing by SEM
The sign of the structure of sample.Present embodiment first combines microwave and hydro-thermal, applied to periodontal membrane fiber beam function and work
Structure, differential arc oxidation coating imitates function and the effect of dentine, and surface apatite nano wire imitates the function and work of fibre bundle
With.Present embodiment is obtained into coating and has generated a large amount of apatite for having and being necessarily orientated, is put into simulated body fluid and soaks after 20h
Surface hydroxyl apatite reaches saturation, and the sample that conventional hydrothermal processing (mutually synthermal, time) is obtained soaks by identical
Time, surface does not have any apatite to generate substantially.Illustrate that differential arc oxidation coating is after microwave Steam treatment in present embodiment
The more conventional Steam treatment of titanium differential arc oxidation titanium and its common differential arc oxidation coating have higher bioactivity and apatite
Inducibility.
Embodiment two：Present embodiment from unlike embodiment one：Titanium described in step one
Expect for titanium or titanium alloy.It is other identical with embodiment one.
Embodiment three：Unlike one of present embodiment and embodiment one or two：Described titanium
Expect for TA2, TA3, TA4, TC4 or Ti2448.It is other identical with embodiment one or two.
Embodiment four：Unlike one of present embodiment and embodiment one to three：In step 2
Voltage be 350V~450V, pulse frequency be 600Hz~800Hz, dutycycle be 4%~10% and electrolyte temperature be 0 DEG C~
Under conditions of 35 DEG C, differential arc oxidation 5min~40min.It is other identical with embodiment one to three.
Embodiment five：Unlike one of present embodiment and embodiment one to four：In step 2
Voltage be 400V~450V, pulse frequency be 600Hz~700Hz, dutycycle be 4%~7% and electrolyte temperature be 10 DEG C~
Under conditions of 20 DEG C, differential arc oxidation 5min~30min.It is other identical with embodiment one to four.
Embodiment six：Unlike one of present embodiment and embodiment one to five：Institute in step 3
It is that hydrothermal reaction kettle is overall that the alkali lye volume that pure water or concentration are 0.01mol/L~5.0mol/L is added in the hydrothermal reaction kettle stated
Long-pending 20%.It is other identical with embodiment one to five.
Embodiment seven：Unlike one of present embodiment and embodiment one to six：In step 3 to
It is 3.0mol/L~5.0mol/L's that pure water or concentration are added in the special hydrothermal reaction kettle of microwave hydrothermal of polytetrafluoroethylene (PTFE) material
Alkali lye, the titanium material after differential arc oxidation is handled is suspended from apart from the alkali lye water surface that pure water or concentration are 3.0mol/L~5.0mol/L
Hydrothermal reaction kettle, is then placed in microwave attenuation materials parallelometer by more than 30mm, in the condition that temperature is 180 DEG C~200 DEG C
Under, it is incubated 240min~300min.It is other identical with embodiment one to six.
Embodiment eight：Unlike one of present embodiment and embodiment one to seven：In step 3 to
It is 1.0mol/L~2.5mol/L's that pure water or concentration are added in the special hydrothermal reaction kettle of microwave hydrothermal of polytetrafluoroethylene (PTFE) material
Alkali lye, the titanium material after differential arc oxidation is handled is suspended from apart from the alkali lye water surface that pure water or concentration are 1.0mol/L~2.5mol/L
Hydrothermal reaction kettle, is then placed in microwave attenuation materials parallelometer by more than 30mm, in the condition that temperature is 200 DEG C~220 DEG C
Under, it is incubated 120min~240min.It is other identical with embodiment one to seven.
Embodiment nine：Unlike one of present embodiment and embodiment one to eight：In step 3 to
It is 0.1mol/L~1.0mol/L's that pure water or concentration are added in the special hydrothermal reaction kettle of microwave hydrothermal of polytetrafluoroethylene (PTFE) material
Alkali lye, the titanium material after differential arc oxidation is handled is suspended from apart from the alkali lye water surface that pure water or concentration are 0.1mol/L~1.0mol/L
Hydrothermal reaction kettle, is then placed in microwave attenuation materials parallelometer by more than 30mm, in the condition that temperature is 220 DEG C~240 DEG C
Under, it is incubated 60min~90min.It is other identical with embodiment one to eight.
Embodiment ten：Unlike one of present embodiment and embodiment one to nine：In step 3 to
It is 0.01mol/L~0.1mol/L's that pure water or concentration are added in the special hydrothermal reaction kettle of microwave hydrothermal of polytetrafluoroethylene (PTFE) material
Alkali lye, the titanium material after differential arc oxidation is handled is suspended from the alkali lye water surface apart from pure water or concentration 0.01mol/L~0.1mol/L
Hydrothermal reaction kettle, is then placed in microwave attenuation materials parallelometer by more than 30mm, in the condition that temperature is 240 DEG C~250 DEG C
Under, it is incubated 90min~120min.It is other identical with embodiment one to nine.
Embodiment 11：Unlike one of present embodiment and embodiment one to ten：In step 2
Voltage be 400V~450V, pulse frequency be 500Hz~700Hz, dutycycle is 5%~7% and electrolyte temperature is 15 DEG C
Under conditions of~20 DEG C, differential arc oxidation 5min~20min.It is other identical with embodiment one to ten.
Embodiment 12：Present embodiment from unlike embodiment one to one of 11：Step 2
Described in the concentration containing disodium ethylene diamine tetraacetate in bioactive ingredients electrolyte be 15g/L；Described contains biology
The concentration of sodium hydroxide is 5g/L in active component electrolyte；It is described containing in bioactive ingredients electrolyte sodium metasilicate it is dense
Spend for 7.1g/L；The described concentration containing calcium dihydrogen phosphate in bioactive ingredients electrolyte is 6.3g/L；Described contains
The concentration of calcium acetate is 8.8g/L in bioactive ingredients electrolyte.It is other identical with embodiment one to 11.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：
Use microwave steam described in the present embodiment is in the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction
The preparation method of apatite nano wire, is specifically followed the steps below：
First, the pretreatment of titanium material：Titanium material surface is beaten using 200#, 400# and 1000# abrasive paper for metallograph successively
After mill and polishing, cleaned successively with acetone, absolute ethyl alcohol and deionized water, dry 4h under conditions of temperature is 60 DEG C, obtain
Pretreated titanium material；
Described titanium material is 10mm × 10mm × 1mm TA2 matrix titanium plate samples；
2nd, differential arc oxidation is handled：Pretreated titanium material is placed in the stainless steel containing bioactive ingredients electrolyte
In electrolytic cell, using pretreated titanium material as anode, stainless-steel sheet is negative electrode, differential arc oxidation is carried out, using pulse direct current
Voltage, is that 400V, pulse frequency are that 600Hz, dutycycle are 8% and electrolyte temperature is the differential of the arc under conditions of 10 DEG C in voltage
5min is aoxidized, the titanium material after differential arc oxidation processing is obtained；
Described contains bioactive ingredients electrolyte by deionized water, disodium ethylene diamine tetraacetate, sodium hydroxide, silicic acid
Sodium, calcium dihydrogen phosphate and calcium acetate are mixed；Described contains disodium ethylene diamine tetraacetate in bioactive ingredients electrolyte
Concentration be 15g/L；The described concentration containing sodium hydroxide in bioactive ingredients electrolyte is 5g/L；Described contains life
The concentration of sodium metasilicate is 7.1g/L in thing active component electrolyte；Described contains biphosphate in bioactive ingredients electrolyte
The concentration of calcium is 6.3g/L；The described concentration containing calcium acetate in bioactive ingredients electrolyte is 8.8g/L；
3rd, microwave Steam treatment：Concentration is added into the special hydrothermal reaction kettle of the microwave hydrothermal of polytetrafluoroethylene (PTFE) material is
0.5mol/L alkali lye, the titanium material after differential arc oxidation is handled is suspended from the alkali lye water surface 35mm that distance concentration is 0.5mol/L
Hydrothermal reaction kettle, is then placed in microwave attenuation materials parallelometer by place, under conditions of temperature is 200 DEG C, is incubated 60min,
The differential arc oxidation coating after microwave Steam treatment is obtained, that is, is completed using microwave steam in titanium differential arc oxidation coating surface construction class
Like the preparation method of the apatite nano wire of periodontal membrane fiber beam；
It is hydrothermal reaction kettle cumulative volume that the alkali lye volume that concentration is 0.5mol/L is added in described hydrothermal reaction kettle
20%；
Described alkali lye is sodium hydroxide solution.
The XRD spectrum of differential arc oxidation coating after the microwave Steam treatment that Fig. 1 is prepared for embodiment one；A is anatase peak,
B is titanium peak, and C is apatite peak；As seen from the figure, it is capable of detecting when in coating there is anatase, apatite.
The scanned photograph of differential arc oxidation coating after the microwave Steam treatment that Fig. 2 is prepared for embodiment one；As seen from the figure, apply
Layer surface forms a large amount of apatite nanometer rods for having and being necessarily orientated.
The EDS power spectrum spectrograms of differential arc oxidation coating after the microwave Steam treatment that Fig. 3 is prepared for embodiment one；Can by figure
Know, calcium, phosphorus, silicon, sodium isoreactivity element are contained in coating.
Fig. 4 is that the differential arc oxidation coating after microwave Steam treatment prepared by embodiment one soaks sweeping after simulated body fluid 20h
Retouch photo；As seen from the figure, the sample after microwave Steam treatment soaks the hydroxyapatite on surface after 20h in simulated body fluid and reached
Saturation, can not see the original structure of coating.
Differential arc oxidation coating sample immersion simulated body fluid 20h surfaces hydroxyl after microwave Steam treatment prepared by embodiment one
Base apatite reaches saturation.
Embodiment two：The present embodiment from unlike embodiment one：In voltage it is that 350V, pulse frequency are in step 2
600Hz, dutycycle are 8% and electrolyte temperature is differential arc oxidation 5min under conditions of 10 DEG C.It is other identical with embodiment one.
There is anatase, apatite in the coating that the present embodiment is obtained.Coating surface, which is formed, largely has what is be necessarily orientated
Apatite nanometer rods.Contain calcium, phosphorus, silicon, sodium isoreactivity element in coating.Embodiment is obtained into the immersion of differential arc oxidation coating sample
1 day surface hydroxyl apatite of simulated body fluid reaches saturation.
Embodiment three：The present embodiment from unlike embodiment one：In step 3 under conditions of temperature is 220 DEG C, protect
Warm 60min.It is other identical with embodiment one.
There is anatase and apatite in the coating that the present embodiment is obtained.Coating surface, which is formed, largely has what is be necessarily orientated
Apatite nanometer rods.Contain calcium, phosphorus, silicon, sodium isoreactivity element in coating.Embodiment is obtained into differential arc oxidation active coating sample
Immersion 1 day surface hydroxyl apatite of simulated body fluid reaches saturation.
Example IV：The present embodiment from unlike embodiment one：Titanium material after differential arc oxidation is handled in step 3
It is suspended from the alkali lye water surface 35mm that distance concentration is 0.01mol/L.It is other identical with embodiment one.
There is anatase and apatite in the coating that the present embodiment is obtained.Coating surface, which is formed, largely has what is be necessarily orientated
Apatite nanometer rods.Contain calcium, phosphorus, silicon, sodium isoreactivity element in coating.Embodiment is obtained into differential arc oxidation active coating sample
Immersion 1 day surface hydroxyl apatite of simulated body fluid reaches saturation.
Embodiment five：The present embodiment from unlike embodiment one：Titanium material after differential arc oxidation is handled in step 3
It is suspended from the alkali lye water surface 35mm that distance concentration is 1.0mol/L.It is other identical with embodiment one.
There is anatase, apatite and sodium titanate in the coating that the present embodiment is obtained.Coating surface forms a large amount of with one
Surely the apatite nanometer rods being orientated.Contain calcium, phosphorus, silicon, sodium isoreactivity element in coating.Embodiment is obtained into differential arc oxidation activity
Coating sample immersion 5 days surface hydroxyl apatite of simulated body fluid reaches saturation.
Embodiment six：The present embodiment from unlike embodiment one：Titanium material after differential arc oxidation is handled in step 3
It is suspended from the alkali lye water surface 35mm that distance concentration is 3.0mol/L.It is other identical with embodiment one.
There is anatase, apatite and sodium titanate in the coating that the present embodiment is obtained.Coating surface forms a large amount of with one
Surely the apatite nanometer rods being orientated.Contain calcium, phosphorus, silicon, sodium isoreactivity element in coating.The present embodiment is obtained into differential arc oxidation to live
Property coating sample immersion 7 days surface hydroxyl apatite of simulated body fluid reach saturation.
Embodiment seven：The present embodiment from unlike embodiment one：Titanium material after differential arc oxidation is handled in step 3
It is suspended from the alkali lye water surface 35mm that distance concentration is 5.0mol/L.It is other identical with embodiment one.
There is anatase, apatite and sodium titanate in the coating that the present embodiment is obtained.Coating surface forms a large amount of with one
Surely the apatite nanometer rods being orientated.Contain calcium, phosphorus, silicon, sodium isoreactivity element in coating.The present embodiment is obtained into differential arc oxidation to live
Property coating sample immersion 9 days surface hydroxyl apatite of simulated body fluid reach saturation.
Embodiment eight：The present embodiment from unlike embodiment one：Titanium material after differential arc oxidation is handled in step 3
It is suspended from pure water water surface 35mm.It is other identical with embodiment one.
There is anatase and apatite in the coating that the present embodiment is obtained.Coating surface, which is formed, largely has what is be necessarily orientated
Apatite nanometer rods.Contain calcium, phosphorus, silicon, sodium isoreactivity element in coating.The present embodiment is obtained into the examination of differential arc oxidation active coating
Sample immersion 14 days surface hydroxyl apatite of simulated body fluid reaches saturation.
Simulated body fluid constituent content described in embodiment one to eight is as shown in table 1
Table 1 configures 1L simulated body fluid chemical agent contents
Claims (10)
1. microwave steam is used in the system of the apatite nano wire of the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction
Preparation Method, it is characterised in that use microwave steam in the apatite of the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction
The preparation method of nano wire is followed the steps below：
First, the pretreatment of titanium material：Titanium material surface is polished using 200#, 400# and 1000# abrasive paper for metallograph successively and
After polishing, cleaned successively with acetone, absolute ethyl alcohol and deionized water, temperature be 40 DEG C~80 DEG C under conditions of drying 3h~
5h, obtains pretreated titanium material；
2nd, differential arc oxidation is handled：Pretreated titanium material is placed in the stainless steel electrolytic containing bioactive ingredients electrolyte
In groove, using pretreated titanium material as anode, stainless-steel sheet is negative electrode, carries out differential arc oxidation, using pulsed dc voltage,
Voltage be 350V~450V, pulse frequency be 500Hz~800Hz, dutycycle is 4%~10% and electrolyte temperature is 0 DEG C
Under conditions of~35 DEG C, differential arc oxidation 5min~40min obtains the titanium material after differential arc oxidation processing；
It is described containing bioactive ingredients electrolyte by deionized water, disodium ethylene diamine tetraacetate, sodium hydroxide, sodium metasilicate,
Calcium dihydrogen phosphate and calcium acetate are mixed；It is described containing in bioactive ingredients electrolyte disodium ethylene diamine tetraacetate it is dense
Spend for 8g/L~25g/L；The described concentration containing sodium hydroxide in bioactive ingredients electrolyte is 3g/L~25g/L；Institute
The concentration containing sodium metasilicate in bioactive ingredients electrolyte stated is 5g/L~25g/L；Described contains bioactive ingredients
The concentration of calcium dihydrogen phosphate is 5g/L~10g/L in electrolyte；Described contains calcium acetate in bioactive ingredients electrolyte
Concentration is 5g/L~20g/L；
3rd, microwave Steam treatment：Pure water or concentration are added into the special hydrothermal reaction kettle of the microwave hydrothermal of polytetrafluoroethylene (PTFE) material
For 0.01mol/L~5.0mol/L alkali lye, the titanium material after differential arc oxidation is handled is suspended from is apart from pure water or concentration
0.01mol/L~5.0mol/L more than alkali lye water surface 30mm, is then placed in microwave attenuation materials parallelometer by hydrothermal reaction kettle
In, under conditions of temperature is 180 DEG C~250 DEG C, 60min~300min is incubated, that is, is completed using microwave steam in the titanium differential of the arc
The preparation method of the apatite nano wire of the similar periodontal membrane fiber beam of oxide covering surface construction；
It is hydro-thermal reaction that the alkali lye volume that pure water or concentration are 0.01mol/L~5.0mol/L is added in described hydrothermal reaction kettle
The 10%~30% of kettle cumulative volume；
Described alkali lye is sodium hydroxide solution, ammoniacal liquor or potassium hydroxide solution.
2. use microwave steam according to claim 1 is in the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction
Apatite nano wire preparation method, it is characterised in that titanium material described in step one is titanium or titanium alloy.
3. use microwave steam according to claim 2 is in the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction
Apatite nano wire preparation method, it is characterised in that described titanium material be TA2, TA3, TA4, TC4 or Ti2448.
4. use microwave steam according to claim 1 is in the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction
Apatite nano wire preparation method, it is characterised in that in voltage be that 350V~450V, pulse frequency are 600Hz in step 2
~800Hz, dutycycle are 4%~10% and electrolyte temperature is differential arc oxidation 5min~40min under conditions of 0 DEG C~35 DEG C.
5. use microwave steam according to claim 1 is in the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction
Apatite nano wire preparation method, it is characterised in that in voltage be that 400V~450V, pulse frequency are 600Hz in step 2
~700Hz, dutycycle are 4%~7% and electrolyte temperature is differential arc oxidation 5min~30min under conditions of 10 DEG C~20 DEG C.
6. use microwave steam according to claim 1 is in the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction
Apatite nano wire preparation method, it is characterised in that pure water or concentration are added in the hydrothermal reaction kettle described in step 3 is
0.01mol/L~5.0mol/L alkali lye volume is the 20% of hydrothermal reaction kettle cumulative volume.
7. use microwave steam according to claim 1 is in the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction
Apatite nano wire preparation method, it is characterised in that to the special hydro-thermal of microwave hydrothermal of polytetrafluoroethylene (PTFE) material in step 3
The alkali lye of pure water or concentration for 3.0mol/L~5.0mol/L is added in reactor, the titanium material after differential arc oxidation is handled is suspended from
It is 3.0mol/L~5.0mol/L more than alkali lye water surface 30mm apart from pure water or concentration, hydrothermal reaction kettle is then placed in microwave
In Hydrothermal Synthesiss parallelometer, under conditions of temperature is 180 DEG C~200 DEG C, 240min~300min is incubated.
8. use microwave steam according to claim 1 is in the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction
Apatite nano wire preparation method, it is characterised in that to the special hydro-thermal of microwave hydrothermal of polytetrafluoroethylene (PTFE) material in step 3
The alkali lye of pure water or concentration for 1.0mol/L~2.5mol/L is added in reactor, the titanium material after differential arc oxidation is handled is suspended from
It is 1.0mol/L~2.5mol/L more than alkali lye water surface 30mm apart from pure water or concentration, hydrothermal reaction kettle is then placed in microwave
In Hydrothermal Synthesiss parallelometer, under conditions of temperature is 200 DEG C~220 DEG C, 120min~240min is incubated.
9. use microwave steam according to claim 1 is in the similar periodontal membrane fiber beam of titanium differential arc oxidation coating surface construction
Apatite nano wire preparation method, it is characterised in that to the special hydro-thermal of microwave hydrothermal of polytetrafluoroethylene (PTFE) material in step 3
The alkali lye of pure water or concentration for 0.1mol/L~1.0mol/L is added in reactor, the titanium material after differential arc oxidation is handled is suspended from
It is 0.1mol/L~1.0mol/L more than alkali lye water surface 30mm apart from pure water or concentration, hydrothermal reaction kettle is then placed in microwave
In Hydrothermal Synthesiss parallelometer, under conditions of temperature is 220 DEG C~240 DEG C, 60min~90min is incubated.
10. use microwave steam according to claim 1 is in the similar periodontal membrane fiber of titanium differential arc oxidation coating surface construction
The preparation method of the apatite nano wire of beam, it is characterised in that to the microwave hydrothermal dedicated water of polytetrafluoroethylene (PTFE) material in step 3
The alkali lye of pure water or concentration for 0.01mol/L~0.1mol/L, the titanium material after differential arc oxidation is handled are added in thermal response kettle
More than the alkali lye water surface 30mm apart from pure water or concentration 0.01mol/L~0.1mol/L is suspended from, then hydrothermal reaction kettle is placed in
In microwave attenuation materials parallelometer, under conditions of temperature is 240 DEG C~250 DEG C, 90min~120min is incubated.
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| JPH0747268A (en) * | 1993-08-05 | 1995-02-21 | Nikon Corp | Adsorbent for filler and its manufacture |
| CN103334144A (en) * | 2013-07-18 | 2013-10-02 | 哈尔滨工业大学 | Alkaline liquid water vapor post-treatment method of micro-arc oxidation biological active coating on surface of titanium |
| CN103343375A (en) * | 2013-07-18 | 2013-10-09 | 哈尔滨工业大学 | Method for improving biological activity of composite coating on surface of titanium through micro-arc oxidation and water vapour treatment |
| CN103498183A (en) * | 2013-10-17 | 2014-01-08 | 赵全明 | Preparation technology of hydroxyapatite-containing composite biological film on titanium-base surface |
| CN105943150A (en) * | 2016-06-06 | 2016-09-21 | 广州雄俊智能科技有限公司 | Personalized bone fracture plate and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0747268A (en) * | 1993-08-05 | 1995-02-21 | Nikon Corp | Adsorbent for filler and its manufacture |
| CN103334144A (en) * | 2013-07-18 | 2013-10-02 | 哈尔滨工业大学 | Alkaline liquid water vapor post-treatment method of micro-arc oxidation biological active coating on surface of titanium |
| CN103343375A (en) * | 2013-07-18 | 2013-10-09 | 哈尔滨工业大学 | Method for improving biological activity of composite coating on surface of titanium through micro-arc oxidation and water vapour treatment |
| CN103498183A (en) * | 2013-10-17 | 2014-01-08 | 赵全明 | Preparation technology of hydroxyapatite-containing composite biological film on titanium-base surface |
| CN105943150A (en) * | 2016-06-06 | 2016-09-21 | 广州雄俊智能科技有限公司 | Personalized bone fracture plate and manufacturing method thereof |
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