CN107012493B - The preparation method of the apatite nano wire of similar periodontal membrane fiber beam is constructed on titanium differential arc oxidation coating surface using microwave steam - Google Patents
The preparation method of the apatite nano wire of similar periodontal membrane fiber beam is constructed on titanium differential arc oxidation coating surface using microwave steam Download PDFInfo
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Abstract
The preparation method of the apatite nano wire of similar periodontal membrane fiber beam is constructed on titanium differential arc oxidation coating surface using microwave steam, the present invention relates to the preparation methods that a kind of titanium differential arc oxidation coating surface is configured similarly to the nano wire of periodontal membrane fiber beam.The problem of lacking the structure similar to periodontal membrane fiber beam the invention solves root of the tooth planting body in existing tooth-implanting technology, be easy to cause the failure of operation.Method: the one, pretreatment of titanium material；Two, micro-arc oxidation treatment；Three, microwave Steam treatment.The present invention is used to construct the preparation of the apatite nano wire of similar periodontal membrane fiber beam on titanium differential arc oxidation coating surface using microwave steam.
Description
Technical field
The present invention relates to the preparations that a kind of titanium differential arc oxidation coating surface is configured similarly to the nano wire of periodontal membrane fiber beam
Method.
Background technique
Tooth-implanting technology is tooth defect or the important means that missing is repaired at present, but tooth root planting body lacks and is similar to
The structure of periodontal membrane fiber beam, is easy to cause the failure of operation, and current clinic there is no basic solution.Normal periodontium
Structure is outside by root of the tooth, is successively cementum, parodontium, alveolar bone and gum composition.Cementum surrounds root surface
A thin layer osteoid tissue, parodontium are made of dense connective tissue, and most fiber alignment bunchys, one end of fiber is embedded in dentale
In matter, the other end is then embedded in tooth socket bone wall, is seated in tooth in tooth socket.Between cementum, parodontium and alveolar bone
The ligament anchor chain structure of foundation is the key that Periodontal Supporting Tissue, and parodontium plays vital work in periodontium
With.
Summary of the invention
The invention solves root of the tooth planting bodies in existing tooth-implanting technology to lack the structure similar to periodontal membrane fiber beam, holds
The problem of easily leading to the failure of operation, and provide and similar parodontium fibre is constructed on titanium differential arc oxidation coating surface using microwave steam
Tie up the preparation method of the apatite nano wire of beam.
The apatite nano wire of similar periodontal membrane fiber beam is constructed on titanium differential arc oxidation coating surface using microwave steam
Preparation method specifically follows the steps below:
One, the pretreatment of titanium material: successively titanium material surface is beaten using 200#, 400# and 1000# abrasive paper for metallograph
It after mill and polishing, is successively cleaned with acetone, dehydrated alcohol and deionized water, dries 3h under conditions of temperature is 40 DEG C~80 DEG C
~5h obtains pretreated titanium material；
Two, pretreated titanium material micro-arc oxidation treatment: is placed in the stainless steel containing bioactive ingredients electrolyte
In electrolytic cell, using pretreated titanium material as anode, stainless-steel sheet is cathode, differential arc oxidation is carried out, using pulse direct current
Voltage, voltage is 350V~450V, pulse frequency is 500Hz~800Hz, duty ratio is 4%~10% and electrolyte temperature
Under conditions of 0 DEG C~35 DEG C, differential arc oxidation 5min~40min, the titanium material after obtaining micro-arc oxidation treatment；
Described contains bioactive ingredients electrolyte by deionized water, disodium ethylene diamine tetraacetate, sodium hydroxide, silicic acid
Sodium, calcium dihydrogen phosphate and calcium acetate mix；Described contains disodium ethylene diamine tetraacetate in bioactive ingredients electrolyte
Concentration be 8g/L~25g/L；The concentration containing sodium hydroxide in bioactive ingredients electrolyte is 3g/L~25g/
L；The 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 ingredient electrolyte；Described contains acetic acid in bioactive ingredients electrolyte
The concentration of calcium is 5g/L~20g/L；
Three, microwave Steam treatment: into the dedicated hydrothermal reaction kettle of microwave hydrothermal of polytetrafluoroethylene (PTFE) material be added pure water or
Concentration is the lye of 0.01mol/L~5.0mol/L, the titanium material after micro-arc oxidation treatment is suspended from is apart from pure water or concentration
The lye water surface 30mm or more of 0.01mol/L~5.0mol/L, is then placed in microwave attenuation materials parallelometer for hydrothermal reaction kettle
In, under conditions of temperature is 180 DEG C~250 DEG C, 60min~300min is kept the temperature, that is, is completed using microwave steam in the titanium differential of the arc
Oxide covering surface constructs the preparation method of the apatite nano wire of similar periodontal membrane fiber beam；
The lye volume that addition pure water or concentration are 0.01mol/L~5.0mol/L in the hydrothermal reaction kettle is hydro-thermal
The 10%~30% of reaction kettle total volume；
The lye is sodium hydroxide solution, ammonium hydroxide or potassium hydroxide solution.
The beneficial effects of the present invention are: the present invention prepares base using differential arc oxidation and microwave steam method on the basis of pure titanium
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 imitate the fibre bundle of parodontium, and apatite nano-thread in-situ is formed in differential arc oxidation coating surface.The differential of the arc
The a large amount of apatite nano wire in oxide covering surface has certain orientation, but in Growth In Space there are being different on direction, this
The different directions that sample meets periodontal membrane fiber beam play different effect and function in different location.Apatite nano wire is by applying
Layer inner element is diffused into surface, and then forming core is grown up and formed, and therefore, nano-thread in-situ, which is grown on coating surface, to be had well
Binding performance, can also carry the dispersion of different directions power in tooth engagement process, guarantee that tooth root planting body is present in tooth socket
It is interior, it keeps stablizing.Diffractometer EDS spectroscopy detection carried out to the present invention treated sample, it is micro containing calcium phosphorus silicon sodium in coating
Element.X-ray diffractometer carries out the detection of XRD diffraction, and to the present invention treated sample and after impregnating simulated body fluid, specimen surface is deposited
In anatase and apatite phase.Pass through the characterization of the structure of sample after scanning electron microscope progress processing of the present invention.The present invention
Microwave and hydro-thermal are combined for the first time, applied to the building of periodontal membrane fiber Shu Gongneng and effect, differential arc oxidation coating imitates tooth
The function and effect of essence, surface apatite nano wire imitate the function and effect of fibre bundle.The present invention is obtained coating to have generated
It is a large amount of that there is the apatite being centainly orientated, it is put into immersion 20h rear surface hydroxyapatite in simulated body fluid and reaches saturation, and it is conventional
The sample that hydro-thermal process (mutually synthermal, time) obtains passes through identical soaking time, and surface is substantially raw without any apatite
At.Illustrate differential arc oxidation titanium through microwave steam treated the more conventional Steam treatment of titanium of differential arc oxidation coating in the present invention and its
Common differential arc oxidation coating has higher bioactivity and apatite inducibility.
The present invention is used to construct the phosphorus ash of similar periodontal membrane fiber beam on titanium differential arc oxidation coating surface using microwave steam
The preparation method of stone nano wire.
Detailed description of the invention
Fig. 1 is the XRD spectrum of microwave steam treated differential arc oxidation coating prepared by embodiment one；A is anatase peak,
B is titanium peak, and C is apatite peak；
Fig. 2 is the scanned photograph of microwave steam treated differential arc oxidation coating prepared by embodiment one；
Fig. 3 is the EDS power spectrum spectrogram of microwave steam treated differential arc oxidation coating prepared by embodiment one；
Fig. 4 is that microwave steam treated differential arc oxidation coating prepared by embodiment one impregnates sweeping after simulated body fluid 20h
Retouch photo.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, further include each specific embodiment it
Between any combination.
Specific embodiment 1: constructing class on titanium differential arc oxidation coating surface using microwave steam described in present embodiment
It is followed the steps below like the preparation method of the apatite nano wire of periodontal membrane fiber beam:
One, the pretreatment of titanium material: successively titanium material surface is beaten using 200#, 400# and 1000# abrasive paper for metallograph
It after mill and polishing, is successively cleaned with acetone, dehydrated alcohol and deionized water, dries 3h under conditions of temperature is 40 DEG C~80 DEG C
~5h obtains pretreated titanium material；
Two, pretreated titanium material micro-arc oxidation treatment: is placed in the stainless steel containing bioactive ingredients electrolyte
In electrolytic cell, using pretreated titanium material as anode, stainless-steel sheet is cathode, differential arc oxidation is carried out, using pulse direct current
Voltage, voltage is 350V~450V, pulse frequency is 500Hz~800Hz, duty ratio is 4%~10% and electrolyte temperature
Under conditions of 0 DEG C~35 DEG C, differential arc oxidation 5min~40min, the titanium material after obtaining micro-arc oxidation treatment；
Described contains bioactive ingredients electrolyte by deionized water, disodium ethylene diamine tetraacetate, sodium hydroxide, silicic acid
Sodium, calcium dihydrogen phosphate and calcium acetate mix；Described contains disodium ethylene diamine tetraacetate in bioactive ingredients electrolyte
Concentration be 8g/L~25g/L；The concentration containing sodium hydroxide in bioactive ingredients electrolyte is 3g/L~25g/
L；The 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 ingredient electrolyte；Described contains acetic acid in bioactive ingredients electrolyte
The concentration of calcium is 5g/L~20g/L；
Three, microwave Steam treatment: into the dedicated hydrothermal reaction kettle of microwave hydrothermal of polytetrafluoroethylene (PTFE) material be added pure water or
Concentration is the lye of 0.01mol/L~5.0mol/L, the titanium material after micro-arc oxidation treatment is suspended from is apart from pure water or concentration
The lye water surface 30mm or more of 0.01mol/L~5.0mol/L, is then placed in microwave attenuation materials parallelometer for hydrothermal reaction kettle
In, under conditions of temperature is 180 DEG C~250 DEG C, 60min~300min is kept the temperature, that is, is completed using microwave steam in the titanium differential of the arc
Oxide covering surface constructs the preparation method of the apatite nano wire of similar periodontal membrane fiber beam；
The lye volume that addition pure water or concentration are 0.01mol/L~5.0mol/L in the hydrothermal reaction kettle is hydro-thermal
The 10%~30% of reaction kettle total volume；
The lye is sodium hydroxide solution, ammonium hydroxide 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
Method preparation 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 imitate the fibre bundle of parodontium, and apatite nano-thread in-situ is formed in differential arc oxidation coating
Surface.The a large amount of apatite nano wire in differential arc oxidation coating surface has certain orientation, but there are be on direction in Growth In Space
Different, the different directions for meeting periodontal membrane fiber beam in this way play different effect and function in different location.Apatite is received
Rice noodles are by coat inside elements diffusion to surface, and then forming core is grown up and formed, and therefore, nano-thread in-situ is grown on coating
There is good binding performance on surface, can also carry the dispersion of different directions power in tooth engagement process, guarantees that tooth root planting body is deposited
It is in tooth socket, keeps stablizing.Diffractometer EDS spectroscopy detection is carried out to present embodiment treated sample, is contained in coating
There is calcium phosphorus silicon sodium microelement.X-ray diffractometer carries out the detection of XRD diffraction to present embodiment treated sample and impregnates mould
There are anatases and apatite phase for specimen surface after quasi- body fluid.It is tried after carrying out present embodiment processing by scanning electron microscope
The characterization of the structure of sample.Present embodiment for the first time combines microwave and hydro-thermal, is applied to periodontal membrane fiber Shu Gongneng and work
Building, differential arc oxidation coating imitate the function and effect of dentine, and surface apatite nano wire imitates the function and work of fibre bundle
With.Present embodiment acquisition coating has been generated into a large amount of apatite for having and being centainly orientated, has been put into after impregnating 20h in simulated body fluid
Surface hydroxyl apatite reaches saturation, and the sample that conventional hydrothermal processing (mutually synthermal, time) obtains is by identical immersion
Time, surface are generated without any apatite 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.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: titanium described in step 1
Material is titanium or titanium alloy.It is other same as the specific embodiment one.
Specific embodiment 3: unlike one of present embodiment and specific embodiment one or two: the titanium
Material is TA2, TA3, TA4, TC4 or Ti2448.It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: in step 2
Voltage is 350V~450V, pulse frequency is 600Hz~800Hz, duty ratio is 4%~10% and electrolyte temperature be 0 DEG C~
Under conditions of 35 DEG C, differential arc oxidation 5min~40min.It is other identical as specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: in step 2
Voltage is 400V~450V, pulse frequency is 600Hz~700Hz, duty ratio is 4%~7% and electrolyte temperature be 10 DEG C~
Under conditions of 20 DEG C, differential arc oxidation 5min~30min.It is other identical as specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: institute in step 3
The lye volume that addition pure water or concentration are 0.01mol/L~5.0mol/L in the hydrothermal reaction kettle stated is hydrothermal reaction kettle totality
Long-pending 20%.It is other identical as specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: in step 3 to
Pure water is added in the dedicated hydrothermal reaction kettle of the microwave hydrothermal of polytetrafluoroethylene (PTFE) material or concentration is 3.0mol/L~5.0mol/L's
Titanium material after micro-arc oxidation treatment is suspended from the lye water surface for being 3.0mol/L~5.0mol/L apart from pure water or concentration by lye
Then hydrothermal reaction kettle is placed in microwave attenuation materials parallelometer by 30mm or more, the condition for being 180 DEG C~200 DEG C in temperature
Under, keep the temperature 240min~300min.It is other identical as specific embodiment one to six.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: in step 3 to
Pure water is added in the dedicated hydrothermal reaction kettle of the microwave hydrothermal of polytetrafluoroethylene (PTFE) material or concentration is 1.0mol/L~2.5mol/L's
Titanium material after micro-arc oxidation treatment is suspended from the lye water surface for being 1.0mol/L~2.5mol/L apart from pure water or concentration by lye
Then hydrothermal reaction kettle is placed in microwave attenuation materials parallelometer by 30mm or more, the condition for being 200 DEG C~220 DEG C in temperature
Under, keep the temperature 120min~240min.It is other identical as specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: in step 3 to
Pure water is added in the dedicated hydrothermal reaction kettle of the microwave hydrothermal of polytetrafluoroethylene (PTFE) material or concentration is 0.1mol/L~1.0mol/L's
Titanium material after micro-arc oxidation treatment is suspended from the lye water surface for being 0.1mol/L~1.0mol/L apart from pure water or concentration by lye
Then hydrothermal reaction kettle is placed in microwave attenuation materials parallelometer by 30mm or more, the condition for being 220 DEG C~240 DEG C in temperature
Under, keep the temperature 60min~90min.It is other identical as specific embodiment one to eight.
Specific embodiment 10: unlike one of present embodiment and specific embodiment one to nine: in step 3 to
Pure water is added in the dedicated hydrothermal reaction kettle of the microwave hydrothermal of polytetrafluoroethylene (PTFE) material or concentration is 0.01mol/L~0.1mol/L's
Titanium material after micro-arc oxidation treatment is suspended from the lye water surface apart from pure water or concentration 0.01mol/L~0.1mol/L by lye
Then hydrothermal reaction kettle is placed in microwave attenuation materials parallelometer by 30mm or more, the condition for being 240 DEG C~250 DEG C in temperature
Under, keep the temperature 90min~120min.It is other identical as specific embodiment one to nine.
Specific embodiment 11: unlike one of present embodiment and specific embodiment one to ten: in step 2
Voltage is 400V~450V, pulse frequency is 500Hz~700Hz, duty ratio 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 as specific embodiment one to ten.
Specific embodiment 12: present embodiment is unlike specific 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 constituent electrolyte；It is described containing in bioactive ingredients electrolyte sodium metasilicate it is dense
Degree is 7.1g/L；The 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 as specific embodiment one to 11.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one:
Similar periodontal membrane fiber beam is constructed on titanium differential arc oxidation coating surface using microwave steam described in the present embodiment
The preparation method of apatite nano wire, specifically follows the steps below:
One, the pretreatment of titanium material: successively titanium material surface is beaten using 200#, 400# and 1000# abrasive paper for metallograph
It after mill and polishing, is successively cleaned with acetone, dehydrated alcohol and deionized water, dries 4h under conditions of temperature is 60 DEG C, obtain
Pretreated titanium material；
The titanium material is 10mm × 10mm × 1mm TA2 matrix titanium plate sample；
Two, pretreated titanium material micro-arc oxidation treatment: is placed in the stainless steel containing bioactive ingredients electrolyte
In electrolytic cell, using pretreated titanium material as anode, stainless-steel sheet is cathode, differential arc oxidation is carried out, using pulse direct current
Voltage, under conditions of voltage is 400V, pulse frequency 600Hz, duty ratio are 8% and electrolyte temperature is 10 DEG C, the differential of the arc
Aoxidize 5min, the titanium material after obtaining micro-arc oxidation treatment；
Described contains bioactive ingredients electrolyte by deionized water, disodium ethylene diamine tetraacetate, sodium hydroxide, silicic acid
Sodium, calcium dihydrogen phosphate and calcium acetate mix；Described contains disodium ethylene diamine tetraacetate in bioactive ingredients electrolyte
Concentration be 15g/L；The concentration containing sodium hydroxide in bioactive ingredients electrolyte is 5g/L；Described contains life
The concentration of sodium metasilicate is 7.1g/L in object active constituent electrolyte；Described contains biphosphate in bioactive ingredients electrolyte
The concentration of calcium is 6.3g/L；The concentration containing calcium acetate in bioactive ingredients electrolyte is 8.8g/L；
Three, microwave Steam treatment: concentration, which is added, into the dedicated hydrothermal reaction kettle of microwave hydrothermal of polytetrafluoroethylene (PTFE) material is
Titanium material after micro-arc oxidation treatment is suspended from the lye water surface 35mm that distance concentration is 0.5mol/L by the lye of 0.5mol/L
Hydrothermal reaction kettle, is then placed in microwave attenuation materials parallelometer by place, under conditions of temperature is 200 DEG C, keeps the temperature 60min,
Microwave steam is obtained treated differential arc oxidation coating, that is, completes to construct class on titanium differential arc oxidation coating surface using microwave steam
Like the preparation method of the apatite nano wire of periodontal membrane fiber beam；
It is hydrothermal reaction kettle total volume that the lye volume that concentration is 0.5mol/L is added in the hydrothermal reaction kettle
20%；
The lye is sodium hydroxide solution.
Fig. 1 is the XRD spectrum of microwave steam treated differential arc oxidation coating prepared by 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 that there are anatases, apatite.
Fig. 2 is the scanned photograph of microwave steam treated differential arc oxidation coating prepared by embodiment one；As seen from the figure, it applies
Layer surface forms a large amount of apatite nanometer rods for having and being centainly orientated.
Fig. 3 is the EDS power spectrum spectrogram of microwave steam treated differential arc oxidation coating prepared by embodiment one；It can by figure
Know, calcium, phosphorus, silicon, sodium isoreactivity element are contained in coating.
Fig. 4 is that microwave steam treated differential arc oxidation coating prepared by embodiment one impregnates sweeping after simulated body fluid 20h
Retouch photo；As seen from the figure, the hydroxyapatite of microwave steam treated sample impregnates in simulated body fluid 20h rear surface reaches
Saturation, can not see the original structure of coating.
Microwave steam prepared by embodiment one treated differential arc oxidation coating sample impregnates the surface simulated body fluid 20h hydroxyl
Base apatite reaches saturation.
Embodiment two: the present embodiment is unlike embodiment one: voltage is 350V, pulse frequency is in step 2
Under conditions of 600Hz, duty ratio are 8% and electrolyte temperature is 10 DEG C, differential arc oxidation 5min.It is other to be the same as example 1.
There are anatases, apatite in the coating that the present embodiment obtains.Coating surface formed it is a large amount of have centainly be orientated
Apatite nanometer rods.Contain calcium, phosphorus, silicon, sodium isoreactivity element in coating.Embodiment is obtained differential arc oxidation coating sample to impregnate
1 day surface hydroxyl apatite of simulated body fluid reaches saturation.
Embodiment three: the present embodiment is unlike embodiment one: in step 3 under conditions of temperature is 220 DEG C, protecting
Warm 60min.It is other to be the same as example 1.
There are anatases and apatite in the coating that the present embodiment obtains.Coating surface formed it is a large amount of have centainly be orientated
Apatite nanometer rods.Contain calcium, phosphorus, silicon, sodium isoreactivity element in coating.Embodiment is obtained into differential arc oxidation active coating sample
It impregnates 1 day surface hydroxyl apatite of simulated body fluid and reaches saturation.
Example IV: the present embodiment is unlike embodiment one: by the titanium material after micro-arc oxidation treatment in step 3
It is suspended from the lye water surface 35mm that distance concentration is 0.01mol/L.It is other to be the same as example 1.
There are anatases and apatite in the coating that the present embodiment obtains.Coating surface formed it is a large amount of have centainly be orientated
Apatite nanometer rods.Contain calcium, phosphorus, silicon, sodium isoreactivity element in coating.Embodiment is obtained into differential arc oxidation active coating sample
It impregnates 1 day surface hydroxyl apatite of simulated body fluid and reaches saturation.
Embodiment five: the present embodiment is unlike embodiment one: by the titanium material after micro-arc oxidation treatment in step 3
It is suspended from the lye water surface 35mm that distance concentration is 1.0mol/L.It is other to be the same as example 1.
There are anatase, apatite and sodium titanates in the coating that the present embodiment obtains.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 impregnates 5 days surface hydroxyl apatite of simulated body fluid and reaches saturation.
Embodiment six: the present embodiment is unlike embodiment one: by the titanium material after micro-arc oxidation treatment in step 3
It is suspended from the lye water surface 35mm that distance concentration is 3.0mol/L.It is other to be the same as example 1.
There are anatase, apatite and sodium titanates in the coating that the present embodiment obtains.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.It is living that the present embodiment is obtained into differential arc oxidation
Property coating sample impregnate 7 days surface hydroxyl apatite of simulated body fluid reach saturation.
Embodiment seven: the present embodiment is unlike embodiment one: by the titanium material after micro-arc oxidation treatment in step 3
It is suspended from the lye water surface 35mm that distance concentration is 5.0mol/L.It is other to be the same as example 1.
There are anatase, apatite and sodium titanates in the coating that the present embodiment obtains.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.It is living that the present embodiment is obtained into differential arc oxidation
Property coating sample impregnate 9 days surface hydroxyl apatite of simulated body fluid reach saturation.
Embodiment eight: the present embodiment is unlike embodiment one: by the titanium material after micro-arc oxidation treatment in step 3
It is suspended from pure water water surface 35mm.It is other to be the same as example 1.
There are anatases and apatite in the coating that the present embodiment obtains.Coating surface formed it is a large amount of have centainly be 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 impregnates 14 days surface hydroxyl apatite of simulated body fluid and 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 content
Claims (3)
1. constructing the system of the apatite nano wire of similar periodontal membrane fiber beam on titanium differential arc oxidation coating surface using microwave steam
Preparation Method, it is characterised in that the apatite of similar periodontal membrane fiber beam is constructed on titanium differential arc oxidation coating surface using microwave steam
The preparation method of nano wire follows the steps below:
One, the pretreatment of titanium material: successively using 200#, 400# and 1000# abrasive paper for metallograph to titanium material surface carry out polishing and
After polishing, successively cleaned with acetone, dehydrated alcohol and deionized water, temperature be 40 DEG C~80 DEG C under conditions of drying 3h~
5h obtains pretreated titanium material；
Two, pretreated titanium material micro-arc oxidation treatment: is placed in the stainless steel electrolytic containing bioactive ingredients electrolyte
In slot, using pretreated titanium material as anode, stainless-steel sheet is cathode, carries out differential arc oxidation, using pulsed dc voltage,
Under conditions of voltage is 400V, pulse frequency 600Hz, duty ratio are 8% and electrolyte temperature is 10 DEG C, differential arc oxidation
5min, the titanium material after obtaining micro-arc oxidation treatment；
It is described containing bioactive ingredients electrolyte by deionized water, disodium ethylene diamine tetraacetate, sodium hydroxide, sodium metasilicate,
Calcium dihydrogen phosphate and calcium acetate mix；It is described containing in bioactive ingredients electrolyte disodium ethylene diamine tetraacetate it is dense
Degree is 15g/L；The concentration containing sodium hydroxide in bioactive ingredients electrolyte is 5g/L；Described is living containing biology
Property ingredient electrolyte in sodium metasilicate concentration be 7.1g/L；Described contains calcium dihydrogen phosphate in bioactive ingredients electrolyte
Concentration is 6.3g/L；The concentration containing calcium acetate in bioactive ingredients electrolyte is 8.8g/L；
Three, pure water or concentration microwave Steam treatment: are added into the dedicated hydrothermal reaction kettle of microwave hydrothermal of polytetrafluoroethylene (PTFE) material
For the lye of 0.01mol/L~5.0mol/L, the titanium material after micro-arc oxidation treatment is suspended from it is apart from pure water or concentration
The lye water surface 30mm or more of 0.01mol/L~5.0mol/L, is then placed in microwave attenuation materials parallelometer for hydrothermal reaction kettle
In, under conditions of temperature is 200 DEG C~220 DEG C, 60min is kept the temperature, that is, is completed using microwave steam in titanium differential arc oxidation coating
Surface constructs the preparation method of the apatite nano wire of similar periodontal membrane fiber beam；
The lye volume that addition pure water or concentration are 0.01mol/L~5.0mol/L in the hydrothermal reaction kettle is hydro-thermal reaction
The 10%~30% of kettle total volume；
The lye is sodium hydroxide solution, ammonium hydroxide or potassium hydroxide solution.
2. according to claim 1 construct similar periodontal membrane fiber beam on titanium differential arc oxidation coating surface using microwave steam
Apatite nano wire preparation method, it is characterised in that titanium material described in step 1 be titanium or titanium alloy.
3. according to claim 2 construct similar periodontal membrane fiber beam on titanium differential arc oxidation coating surface using microwave steam
Apatite nano wire preparation method, it is characterised in that the titanium material be TA2, TA3, TA4, TC4 or Ti2448.
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| JPH0747268A (en) * | 1993-08-05 | 1995-02-21 | Nikon Corp | Adsorbent for filler and its manufacture |
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| 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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| 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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