CN106521601B - The preparation method of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling carries - Google Patents
The preparation method of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling carries Download PDFInfo
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Abstract
The preparation method of medicine coating, is related to a kind of preparation method of pure titanium mouth cavity planting body coating during a kind of pure titanium mouth cavity planting body differential arc oxidation DOPA amine coupling carries.The present invention be in order to solve current titanium mouth cavity planting body plant immediate union slowly, bacterium intrusion causes early infection to occur, plantation is made to fail after Implant after plantation the technical issues of.The present invention：One, pure titanium specimen surface pretreatment；Two, micro-arc oxidation electrolyte is configured；Three, ultrasonic microarc oxidation is handled；Four, it post-processes.The present invention is by after to pure titanium planting material surface by micro-arc oxidation, Chinese medicine is carried using dopamine as articulation agent to be modified, promote bone growth and development using it, reinforce human body cell metabolism, muscle skeleton aging is prevented, broad-spectrum antibacterial action raising acquisition biocompatibility is more preferable, heal novel bone planting body faster.
Description
Technical field
The present invention relates to a kind of preparation methods of pure titanium mouth cavity planting body coating.
Background technology
With the increase of the wounds such as bone injury and bone defect and the raising of human living standard, to the mouth cavity planting body of Bone Defect Repari
The problems such as bacterium infection caused by implantation, also gradually attracts much attention.Compared with natural teeth, implant denture has its particularity,
Planting body cuff wraps planting body and wears the oral soft tissue at gum, junctional epithelium herein mainly plays barrier action, to plantation
Form good biology closing body week.But compared with natural teeth, the junctional epithelium attachment at planting body cuff is relatively thin, therefore its
Barrier action is also just relatively weak.In addition, the blood vessel in bone regeneration around implant connective tissue is less relative to natural teeth, planting body with
The combination interface of bone lacks parodontium, and when there is bacterial invasion, the inflammatory reaction in the region will be relatively low, immune defense ability
Corresponding weaker, bacterium will assemble at this position to be bred, and then bone regeneration around implant infection occurs.Planting body and peri-implant
These features of structure determine that surrounding soft tissue is easier to be influenced by bacterial plaque, and its impaired rear surrounding tissue
There are larger gaps compared with natural teeth for repair ability.
Early stage after Implant, due to the destruction to local system of defense in the wound and art of operation, at this time
Bacterium is easiest to the mucous membrane of invasion bone regeneration around implant.Once the mucous membrane closing of bone regeneration around implant is destroyed, pathogenic bacteria can
It is directly entered planting body-synosteosis interface.And this interface feels more blunt to the adverse factor of pathogenic bacteria etc., it is long this with
It is past that bone regeneration around implant infection and its complication can not only occur, but also may finally by the loosening for leading to planting body and fall off.
Chinese medicine and Chinese medical extract have the function of anti-inflammatory, antibacterial and promote bone uptake.By taking pueraria lobata as an example, pueraria lobata is pulse family
The drying of the root of plant elegant jessamine or sweet kudzu is made.Pueraria lobata has anti-inflammatory, antipyretic, the effect of antibacterial.Puerarin is to osteoclast
Bone information function have direct repression, and osteoclastic bone resorption function be actively osteoporosis occur pathologic, physiologic it
One, it can promote the increasing of osteoblast, differentiation, improve alkaline phosphatase activities, the expression of enhancing correlation mRNA, this illustrates Pueraria lobota
Root can promote the growth and development of bone.And the Puerarin active ingredient one of more as content in pueraria lobata, in nature
In be widely present., with multiple pharmacological effect, drug effect is clear for it, and safety and low toxicity, clinical application is extensive, and pueraria lobata is resourceful,
It is cheap.Therefore pueraria lobata be can yet be regarded as a kind of suitably used in a herb of mouth cavity planting body.
Coupling agent dopamine largely exist in organism, since dopamine and its derivative not only have waterproof adhesive energy
Power and the substrate of its modified have good biocompatibility, will not encroach on human body cell and cause immune response, dopamine
Have the adherency feature similar to marine organisms Mussels, to be formed in the reaction of adherency in addition to that can participate in, and can be with
It reacts to form stronger covalent bond and non-covalent bond with base material, chelate can be formed and makes the fixation of its stabilization
On the surface of titanium ion, therefore the most suitable function served as bridge for acting as connection titanium and Chinese medicine to human body without having damage.
Invention content
The present invention is that in plantation immediate union, slowly, after plantation bacterium invades and causes in order to solve current titanium mouth cavity planting body
The technical issues of early infection occurs after Implant, plantation is made to fail, and it is more to provide a kind of pure titanium mouth cavity planting body differential arc oxidation-
The preparation method of medicine coating during bar amine coupling carries.
The present invention a kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling carry in medicine coating preparation method be by
What following steps carried out：
One, pure titanium specimen surface pretreatment：Pending pure titanium specimen surface is roughly ground with sand paper, is then used successively
Acetone and each ultrasound 25min of distilled water, be put into after drying in hermetic bag seal it is spare；
By HF acid, dense HNO3It is uniformly mixed with deionized water, obtains mixed acid, the pure titanium sample after drying is put into mixing
20s~40s is impregnated in acid, obtains acid treated pure titanium sample；The mass concentration of the HF acid is 40%~44%；It is described
Dense HNO3Mass concentration be 65%；The HF acid and dense HNO3Volume ratio be 1:2, the HF acid and deionized water
Volume ratio be 1:3；
Two, micro-arc oxidation electrolyte is configured：Sequentially added in beaker sodium metasilicate, potassium hydroxide, potassium fluoride, sodium phosphate and
Distilled water, sonic oscillation stand for 24 hours~36h, obtain micro-arc oxidation electrolyte until all reagents are completely dissolved；Described
The concentration of sodium metasilicate is 3g/L~6g/L in micro-arc oxidation electrolyte, and the concentration of potassium hydroxide is 3g/L~6g/L, potassium fluoride
Concentration is 4g/L~8g/L, and the concentration of sodium phosphate is 12g/L~18g/L；
Three, ultrasonic microarc oxidation is handled：Micro-arc oxidation electrolyte prepared by step 2 is put into electrolytic cell, it then will be electric
Solution slot is transferred in supersonic oscillations instrument, and microarc oxidation equipment provided cathode connects stainless steel electrolytic slot, and anode connects in step 1 at acid
Pure titanium sample after reason, be arranged microarc oxidation equipment provided anode cathode separation be 40mm~60mm, start it is microarc oxidation equipment provided and
Supersonic oscillations instrument, ultrasonic frequency is 30KHz~60KHz, differential arc oxidation voltage is 350V~450V, pulsewidth be 30 μ s~
80 μ s, pulse frequency be 300Hz~800Hz and duty ratio be 2.5% under conditions of ultrasonic microarc oxidation 3min~12min, close
Microarc oxidation equipment provided and supersonic oscillations instrument is closed, sample taking-up distilled water flushing is clean, naturally dry；
Four, it post-processes：
1. the titanium sample that step 3 ultrasonic microarc oxidation has been handled is put into the NaOH aqueous solutions of 3mol/L~5mol/L,
It is subsequently placed in the water-bath that temperature is 60 DEG C~80 DEG C and keeps the temperature 20min~40min, wash with water rear naturally dry, obtain at alkali
The titanium sample of reason；
2. configuring the mixed aqueous solution of dopamine and trishydroxymethylaminomethane, it is with the hydrochloric acid tune pH of a concentration of 3mol/L
7~8, Chinese Medicines are then added, ultrasonic 10min~30min obtains the mixed solution of dopamine-Chinese medicine；By step 4 1. in
The titanium sample of alkali process is put into the mixed solution of dopamine-Chinese medicine, then ultrasonic 10min is placed on room temperature and not light-exposed item
It stands under part for 24 hours, dries in the shade naturally after taking-up, obtain medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling carries；
The concentration of Chinese medicine is 2g/L~8g/L in the mixed solution of the dopamine-Chinese medicine；The dopamine and three
In the mixed aqueous solution of hydroxymethyl aminomethane the concentration of dopamine be 1.5g/L~2.5g/L, trishydroxymethylaminomethane it is dense
Degree is 1.0g/L~1.5g/L；The volume of the mixed aqueous solution and Chinese Medicines of the dopamine and trishydroxymethylaminomethane
It is equal.
The present invention is by the way that after to pure titanium planting material surface by micro-arc oxidation, Chinese medicine (such as pueraria lobata is carried by articulation agent of dopamine
Element) it is modified, promote bone growth and development using it, reinforces human body cell metabolism, prevent muscle skeleton aging, wide spectrum
Antibacterial action raising acquisition biocompatibility is more preferable, heal novel bone planting body faster.This not only solves titanium this inertia
The compatibility of matrix and bone, and solve and invaded all the time due to damaged caused by operation in plantation due to microorganism
Mucous membrane, and tooth-planting is made to fail.
In view of bacterium infection frequent occurrence after tooth-planting, tooth-planting is made to fail, and many Chinese medicines such as pueraria lobata has it
It strengthens muscles and bones, reinforces human body cell metabolism, prevent muscle skeleton aging, and have very good antibiotic property, add differential of the arc oxygen
Change technology has high-efficiency environment friendly, easy to operate, coating and substrate combinating strength height, by high temperature sintering and can be put in coating surface
Electrical breakdown acts on the advantages that porous ceramics coating material to be formed containing required function element, therefore the present invention mainly uses the differential of the arc
Oxidation technology carries medicine on pure titanium surface, will combine with the advantages of Chinese medicine the advantages of differential arc oxidation, has efficiently to obtain
The new composite material of Biofunctional mouth cavity planting body of the load Chinese medicine of bioactivity.
The present invention provides a kind of differential arc oxidation titanium surface and carries Chinese medicine by coupling agent (dopamine), and obtaining has biology living
Property, resistance to human body environment's corrosivity and low production cost, high efficiency, be substantially shorter bone healing time, and there is antibacterial work(
The preparation method of the novel titanium implant composite material of energy.
The present invention is used in pure titanium surface by micro-arc oxidation, is carried Chinese medicine by DOPA amine coupling, is obtained functional living being coating,
The Biocomposite material can make up the shortcomings that clinical application successful titanium or titanium alloy, effective to improve the biological of titanium alloy
Energy.The biological property for carrying Chinese medicine film layer is ion exchange can occur with body fluid, in surface one layer of HA (hydroxy-apatite of deposition
Stone) film layer, there is good biocompatibility, along with Chinese medicine (such as pueraria lobata) has antibacterial, promote the growth and development of bone.System
Standby planting body material combines Chinese medicine and the excellent feature of differential arc oxidation, has antibiotic property and accelerates the growth and reparation of bone
New features.Therefore the composite material can be used for mouth cavity planting body, and can be additionally used in bone tissue defect, and damage etc. is repaired and replaced
It changes, the clinical requirement to biological hard tissue alternate material can be met.
Method is used by the present invention solves technical problem：Using biomedical pure titanium as matrix, using differential arc oxidation skill
Functional living being composite coating material green wood is finally made in art, alkali process technology, DOPA amine coupling Chinese medicine (such as pueraria lobata) method
Material.
The present invention has following feature：
(1) proposition is a kind of using differential arc oxidation complex technique, prepares the porous bioactivity coatings of bottom dense skin,
Alkali process is used to activate afterwards, dopamine carries Chinese medicine as coupling agent, to obtain the biological coating for having and carrying Chinese medicine；Titanium alloy is micro-
Arc oxidation carries medicine coating in medicine and meets mouth cavity planting body antibacterial, prevents the infection of early implantation body；
(2) the functional living being coating composite material is to prepare the compound bio containing Chinese medicine in pure titanium differential arc oxidization surface
Ceramic coating material, such composite biological coating material have suitable binding force, corrosion-resistant and good good biocompatibility
Feature；
(3) medicine coating is reacted with human body fluid in the load, can pass through the negative ions of ion in titanium Chinese medicine coating surface
It attracts each other, deposits one layer of hydroxyapatite (HA) coating on surface, there is good biocompatibility, and Chinese medicine can promote
The synthesis of certain ribose of bone uptake promotes skeleton development, accelerates bone early growth；
(4) medicine coating has fabulous antibiotic property during the bioactivity carries, and up to 99%, this is largely solved antibiotic rate
The case where having determined mouth cavity planting body easy inflammation on oral cavity, having grown bacterium, leads to secondary plantation because of infection to prevent oral cavity；
(5) differential arc oxidization technique that medicine coating uses in the load, DOPA amine coupling carry Chinese medicine.Differential arc oxidization technique, which has, to be set
Standby to be simple and convenient to operate, the characteristics of economical and efficient, three-waste free discharge, the synthesis of dopamine coupling agent is simple, is largely present in biology
In vivo, therefore both methods has the characteristics that simple, pollution-free, easy to operate and is environmentally protective treatment technology；
(6) the bioactivity coatings composite material has good corrosion resistance, plants rub resistance abrasion, life in human body environment
Object compatibility does not generate man body pollution as implantation material；Intensity height, good toughness, can be applied to the bone at the big position of human body stress
Repair of tissue defect and replacement are also used as degradable, absorbable bone renovating material for short at defect of human body bone
Phase repairs；
(7) the bioactive ceramic coating composite material can form HA coatings, with human body after the immersion of SBF simulated body fluids
Bone has good compatibility, and pueraria lobata, which is added, in surface can shorten bone healing time, improves early stage Bone Defect Repari speed and Bone Defect Repari
Quality.
Bioactivity coatings composite material prepared by the present invention is by the bioactive ceramic coating and load on pure titanium surface
Medicine coating is combined, the characteristics of having metal material and ceramic material concurrently, and introduces Chinese medicine, has good antibacterial property and rush
Into the development of early stage bone, preparation method ultrasound-differential arc oxidation complex technique is that can ensure to give birth to well for environmentally protective technique
Produce the better bone tissue impairment renovation material of at low cost and Bone Defect Repari performance and bone tissue engineer cell scaffold material.
Pure titanium used in the present invention is biomedical special pure titanium, has the characteristics that nontoxic, safety, mechanical property are good.
Electrolyte used in the present invention is salt that is safe and nontoxic and not will produce the three wastes, is that analysis is pure, at
This is low.
The HA that prepared bioactivity coatings composite material is deposited in application in the present invention be skeleton at
Point, any toxic side effect will not be generated to human body.
The present invention is ultrasonic microarc oxidation treatment technology to be respectively adopted and differential arc oxidation post-processing is compound handles biological doctor
With pure titanium, surface modification treatment is carried out to it, to improve its surface bioactive and corrosion resistance.
The bioactivity coatings composite material of the present invention has good antibiotic property, while it can also promote osteoblast
Adherency, increment, differentiation and alkaline phosphatase expression of enzymes, be conducive to implantation planting body primary stability and early stage mineralising,
It is a kind of ideal planting body coating material.
Description of the drawings
Fig. 1 is the SEM surface topography maps for testing pure titanium surface by micro-arc oxidation -2000 times of dopamine coating in four；
Fig. 2 is the SEM surface topographies for testing 2000 times of medicine coating in pure titanium surface by micro-arc oxidation in one-DOPA amine coupling load
Figure；
Fig. 3 is the SEM surface topographies for testing 2000 times of medicine coating in pure titanium surface by micro-arc oxidation in two-DOPA amine coupling load
Figure；
Fig. 4 is the SEM surface topographies for testing 2000 times of medicine coating in pure titanium surface by micro-arc oxidation in three-DOPA amine coupling load
Figure；
Fig. 5 is XRD diagram,It is TiO2, figure a is pure titanium surface by micro-arc oxidation-dopamine coating in experiment four, and figure b is experiment
Medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling carries in one, figure c are pure titanium surface by micro-arc oxidation-DOPA in experiment two
Medicine coating during amine coupling carries, figure d are medicine coatings in pure titanium surface by micro-arc oxidation in experiment three-DOPA amine coupling load；
Fig. 6 is electrochemistry Tafel curve figure, and Fig. 1 is pure titanium surface by micro-arc oxidation-dopamine coating in experiment four, Fig. 2
It is medicine coating in pure titanium surface by micro-arc oxidation in experiment one-DOPA amine coupling load, Fig. 3 is pure titanium surface by micro-arc oxygen in experiment two
Medicine coating during change-DOPA amine coupling carries, Fig. 4 are medicine coatings in pure titanium surface by micro-arc oxidation in experiment three-DOPA amine coupling load.
Specific implementation mode
Specific implementation mode one：Present embodiment is during a kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling carries
The preparation method of medicine coating specifically carries out according to the following steps：
One, pure titanium specimen surface pretreatment：Pending pure titanium specimen surface is roughly ground with sand paper, is then used successively
Acetone and each ultrasound 25min of distilled water, be put into after drying in hermetic bag seal it is spare；
By HF acid, dense HNO3It is uniformly mixed with deionized water, obtains mixed acid, the pure titanium sample after drying is put into mixing
20s~40s is impregnated in acid, obtains acid treated pure titanium sample；The mass concentration of the HF acid is 40%~44%；It is described
Dense HNO3Mass concentration be 65%；The HF acid and dense HNO3Volume ratio be 1:2, the HF acid and deionized water
Volume ratio be 1:3；
Two, micro-arc oxidation electrolyte is configured：Sequentially added in beaker sodium metasilicate, potassium hydroxide, potassium fluoride, sodium phosphate and
Distilled water, sonic oscillation stand for 24 hours~36h, obtain micro-arc oxidation electrolyte until all reagents are completely dissolved；Described
The concentration of sodium metasilicate is 3g/L~6g/L in micro-arc oxidation electrolyte, and the concentration of potassium hydroxide is 3g/L~6g/L, potassium fluoride
Concentration is 4g/L~8g/L, and the concentration of sodium phosphate is 12g/L~18g/L；
Three, ultrasonic microarc oxidation is handled：Micro-arc oxidation electrolyte prepared by step 2 is put into electrolytic cell, it then will be electric
Solution slot is transferred in supersonic oscillations instrument, and microarc oxidation equipment provided cathode connects stainless steel electrolytic slot, and anode connects in step 1 at acid
Pure titanium sample after reason, be arranged microarc oxidation equipment provided anode cathode separation be 40mm~60mm, start it is microarc oxidation equipment provided and
Supersonic oscillations instrument, ultrasonic frequency is 30KHz~60KHz, differential arc oxidation voltage is 350V~450V, pulsewidth be 30 μ s~
80 μ s, pulse frequency be 300Hz~800Hz and duty ratio be 2.5% under conditions of ultrasonic microarc oxidation 3min~12min, close
Microarc oxidation equipment provided and supersonic oscillations instrument is closed, sample taking-up distilled water flushing is clean, naturally dry；
Four, it post-processes：
1. the titanium sample that step 3 ultrasonic microarc oxidation has been handled is put into the NaOH aqueous solutions of 3mol/L~5mol/L,
It is subsequently placed in the water-bath that temperature is 60 DEG C~80 DEG C and keeps the temperature 20min~40min, wash with water rear naturally dry, obtain at alkali
The titanium sample of reason；
2. configuring the mixed aqueous solution of dopamine and trishydroxymethylaminomethane, it is with the hydrochloric acid tune pH of a concentration of 3mol/L
7~8, Chinese Medicines are then added, ultrasonic 10min~30min obtains the mixed solution of dopamine-Chinese medicine；By step 4 1. in
The titanium sample of alkali process is put into the mixed solution of dopamine-Chinese medicine, then ultrasonic 10min is placed on room temperature and not light-exposed item
It stands under part for 24 hours, dries in the shade naturally after taking-up, obtain medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling carries；Described is more
The concentration of Chinese medicine is 2g/L~8g/L in the mixed solution of bar amine-Chinese medicine；The dopamine and trishydroxymethylaminomethane
In mixed aqueous solution the concentration of dopamine be 1.5g/L~2.5g/L, trishydroxymethylaminomethane concentration be 1.0g/L~
1.5g/L；The mixed aqueous solution of the dopamine and trishydroxymethylaminomethane is equal with the volume of Chinese Medicines.
Specific implementation mode two：The difference of present embodiment and specific implementation mode one is：It is micro- described in step 2
The concentration of sodium metasilicate is 5g/L in arc oxidation electrolyte, and the concentration of potassium hydroxide is 5g/L, and the concentration of potassium fluoride is 6g/L, phosphoric acid
The concentration of sodium is 14g/L.Other are same as the specific embodiment one.
Specific implementation mode three：The difference of present embodiment and specific implementation mode one is：Step 4 2. described in
Chinese medicine in Chinese Medicines is Cortex Eucommiae chlorogenic acid, and solvent is water.Other are same as the specific embodiment one.
Specific implementation mode four：The difference of present embodiment and specific implementation mode one is：Step 4 2. described in
Chinese medicine in Chinese Medicines is kudzu-vine root powder, and solvent is water.Other are same as the specific embodiment one.
Specific implementation mode five：The difference of present embodiment and specific implementation mode one is：Step 4 2. described in
Chinese medicine in Chinese Medicines is icariin, and solvent is absolute ethyl alcohol.Other are same as the specific embodiment one.
Specific implementation mode six：The difference of present embodiment and specific implementation mode one is：Step 4 2. described in
Chinese medicine in Chinese Medicines is Drynaria rhizome powder, and solvent is water.Other are same as the specific embodiment one.
Effect of the present invention is verified by following tests：
Experiment one：This experiment is the preparation of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling carries
Method specifically carries out according to the following steps：
One, pure titanium specimen surface pretreatment：Pending pure titanium specimen surface is roughly ground with sand paper, is then used successively
Acetone and each ultrasound 25min of distilled water, be put into after drying in hermetic bag seal it is spare；
By HF acid, dense HNO3It is uniformly mixed with deionized water, obtains mixed acid, the pure titanium sample after drying is put into mixing
40s is impregnated in acid, obtains acid treated pure titanium sample；The mass concentration of the HF acid is 40%；The dense HNO3's
Mass concentration is 65%；The HF acid and dense HNO3Volume ratio be 1:2, the volume ratio of the HF acid and deionized water is
1:3；
Two, micro-arc oxidation electrolyte is configured：Sequentially added in beaker sodium metasilicate, potassium hydroxide, potassium fluoride, sodium phosphate and
Distilled water, sonic oscillation stand 36h, obtain micro-arc oxidation electrolyte until all reagents are completely dissolved；The differential of the arc oxygen
The concentration for changing sodium metasilicate in electrolyte is 6g/L, and the concentration of potassium hydroxide is 6g/L, and the concentration of potassium fluoride is 8g/L, sodium phosphate
Concentration is 18g/L；
Three, ultrasonic microarc oxidation is handled：Micro-arc oxidation electrolyte prepared by step 2 is put into electrolytic cell, it then will be electric
Solution slot is transferred in supersonic oscillations instrument, and microarc oxidation equipment provided cathode connects stainless steel electrolytic slot, and anode connects in step 1 at acid
Pure titanium sample after reason, it is 50mm that microarc oxidation equipment provided anode cathode separation, which is arranged, starts microarc oxidation equipment provided and ultrasonic wave
Shaker, ultrasonic frequency is 50KHz, differential arc oxidation voltage is 400V, pulsewidth is 60 μ s, pulse frequency is 600Hz and is accounted for
Sky ratio is ultrasonic microarc oxidation 9min under conditions of 2.5%, closes microarc oxidation equipment provided and supersonic oscillations instrument, sample is taken out
It is clean with distilled water flushing, naturally dry；
Four, it post-processes：
1. the titanium sample that step 3 ultrasonic microarc oxidation has been handled is put into the NaOH aqueous solutions of 4mol/L, it is subsequently placed in
30min is kept the temperature in the water-bath that temperature is 70 DEG C, rear naturally dry is washed with water, obtains the titanium sample of alkali process；
2. configuring the mixed aqueous solution of dopamine and trishydroxymethylaminomethane, it is with the hydrochloric acid tune pH of a concentration of 3mol/L
7, Chinese Medicines are then added, ultrasonic 20min obtains the mixed solution of dopamine-Chinese medicine；By step 4 1. in alkali process titanium
Sample is put into the mixed solution of dopamine-Chinese medicine, ultrasonic 10min, be then placed on room temperature and it is not light-exposed under conditions of stand
For 24 hours, it dries in the shade naturally after taking-up, obtains medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling carries；In the dopamine-
The concentration of Chinese medicine is 2.5g/L in the mixed solution of medicine；In the mixed aqueous solution of the dopamine and trishydroxymethylaminomethane
The concentration of dopamine be 2g/L, trishydroxymethylaminomethane concentration be 1.0g/L；The dopamine and trihydroxy methyl amino
The mixed aqueous solution of methane is equal with the volume of Chinese Medicines；Step 4 2. described in Chinese Medicines in Chinese medicine be pueraria lobata
Powder, solvent are water.
Experiment two：This experiment is the preparation of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling carries
Method：
This experiment from experiment one unlike step 4 2. described in dopamine-Chinese medicine mixed solution in Chinese medicine it is dense
Degree is 3.75g/L, other identical as experiment one.
Experiment three：This experiment is the preparation of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling carries
Method：
This experiment from experiment one unlike step 4 2. described in dopamine-Chinese medicine mixed solution in Chinese medicine it is dense
Degree is 5g/L, other identical as experiment one.
Experiment four：This experiment is contrast test, a kind of preparation side of pure titanium mouth cavity planting body differential arc oxidation-dopamine coating
Method, specifically：
One, pure titanium specimen surface pretreatment：Pending pure titanium specimen surface is roughly ground with sand paper, is then used successively
Acetone and each ultrasound 25min of distilled water, be put into after drying in hermetic bag seal it is spare；
By HF acid, dense HNO3It is uniformly mixed with deionized water, obtains mixed acid, the pure titanium sample after drying is put into mixing
40s is impregnated in acid, obtains acid treated pure titanium sample；The mass concentration of the HF acid is 40%；The dense HNO3's
Mass concentration is 65%；
Two, micro-arc oxidation electrolyte is configured：Sequentially added in beaker sodium metasilicate, potassium hydroxide, potassium fluoride, sodium phosphate and
Distilled water, sonic oscillation stand 36h, obtain micro-arc oxidation electrolyte until all reagents are completely dissolved；The differential of the arc oxygen
The concentration for changing sodium metasilicate in electrolyte is 6g/L, and the concentration of potassium hydroxide is 6g/L, and the concentration of potassium fluoride is 8g/L, sodium phosphate
Concentration is 18g/L；
Three, ultrasonic microarc oxidation is handled：Micro-arc oxidation electrolyte prepared by step 2 is put into electrolytic cell, it then will be electric
Solution slot is transferred in supersonic oscillations instrument, and microarc oxidation equipment provided cathode connects stainless steel electrolytic slot, and anode connects in step 1 at acid
Pure titanium sample after reason, it is 50mm that microarc oxidation equipment provided anode cathode separation, which is arranged, starts microarc oxidation equipment provided and ultrasonic wave
Shaker, ultrasonic frequency is 50KHz, differential arc oxidation voltage is 400V, pulsewidth is 60 μ s, pulse frequency is 600Hz and is accounted for
Sky ratio is ultrasonic microarc oxidation 9min under conditions of 2.5%, closes microarc oxidation equipment provided and supersonic oscillations instrument, sample is taken out
It is clean with distilled water flushing, naturally dry；
Four, it post-processes：
1. the titanium sample that step 3 ultrasonic microarc oxidation has been handled is put into the NaOH aqueous solutions of 4mol/L, it is subsequently placed in
30min is kept the temperature in the water-bath that temperature is 70 DEG C, rear naturally dry is washed with water, obtains the titanium sample of alkali process；
2. configuring the mixed aqueous solution of dopamine and trishydroxymethylaminomethane, it is with the hydrochloric acid tune pH of a concentration of 3mol/L
7；By step 4 1. in the titanium sample of alkali process be put into the mixed aqueous solution of dopamine and trishydroxymethylaminomethane, ultrasound
10min, be then placed on room temperature and it is not light-exposed under conditions of stand for 24 hours, dry in the shade naturally after taking-up, obtain pure titanium surface by micro-arc oxygen
Change-dopamine coating；In the mixed aqueous solution of the dopamine and trishydroxymethylaminomethane the concentration of dopamine be 2g/L,
The concentration of trishydroxymethylaminomethane is 1.0g/L.
Fig. 1 is the SEM surface topography maps for testing pure titanium surface by micro-arc oxidation -2000 times of dopamine coating in four, and Fig. 2 is examination
The SEM surface topography maps of 2000 times of medicine coating during pure titanium surface by micro-arc oxidation in one-DOPA amine coupling carries are tested, Fig. 3 is experiment two
In pure titanium surface by micro-arc oxidation-DOPA amine coupling carry in 2000 times of medicine coating SEM surface topography maps, Fig. 4 is pure in experiment three
The SEM surface topography maps of 2000 times of medicine coating during titanium surface by micro-arc oxidation-DOPA amine coupling carries, as can be seen from the figure pure titanium is micro-
Arc oxidized surface carries pueraria lobata surface compact, the micropore that aperture is not much different, and most hole is sealed by Chinese medicine, and some holes are in
Chinese medicine has just enter into state, and the coarse hole of differential arc oxidation is conducive to the loading of the pueraria lobata under action of coupling agents.
Fig. 5 is XRD diagram,It is TiO2, figure a is pure titanium surface by micro-arc oxidation-dopamine coating in experiment four, and figure b is experiment
Medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling carries in one, figure c are pure titanium surface by micro-arc oxidation-DOPA in experiment two
Medicine coating during amine coupling carries, figure d are medicine coatings in pure titanium surface by micro-arc oxidation in experiment three-DOPA amine coupling load, can from figure
To find out that pure titanium differential arc oxidization surface carries the mutually predominantly TiO on pueraria lobata surface2。
Fig. 6 is electrochemistry Tafel curve figure, and Fig. 1 is pure titanium surface by micro-arc oxidation-dopamine coating in experiment four, Fig. 2
It is medicine coating in pure titanium surface by micro-arc oxidation in experiment one-DOPA amine coupling load, Fig. 3 is pure titanium surface by micro-arc oxygen in experiment two
Medicine coating during change-DOPA amine coupling carries, Fig. 4 are medicine coatings in pure titanium surface by micro-arc oxidation in experiment three-DOPA amine coupling load, from
The pure titanium differential arc oxidization surface of it can be seen from the figure that carries the plan voltage of pueraria lobata face coat higher than the differential arc oxidation for only adding coupling agent
Coating, current potential is high, corrosion resistance excellent.
Claims (6)
- The preparation method of medicine coating during 1. a kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling carries, it is characterised in that pure The preparation method of medicine coating carries out according to the following steps during titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling carries：One, pure titanium specimen surface pretreatment：Pending pure titanium specimen surface is roughly ground with sand paper, then uses acetone successively With each ultrasound 25min of distilled water, be put into after drying in hermetic bag seal it is spare；By HF acid, dense HNO3It is uniformly mixed with deionized water, obtains mixed acid, the pure titanium sample after drying is put into mixed acid 20s~40s is impregnated, acid treated pure titanium sample is obtained；The mass concentration of the HF acid is 40%~44%；Described is dense HNO3Mass concentration be 65%；The HF acid and dense HNO3Volume ratio be 1:2, the body of the HF acid and deionized water Product is than being 1:3；Two, micro-arc oxidation electrolyte is configured：Sodium metasilicate, potassium hydroxide, potassium fluoride, sodium phosphate and distillation are sequentially added in beaker Water, sonic oscillation stand for 24 hours~36h, obtain micro-arc oxidation electrolyte until all reagents are completely dissolved；The differential of the arc The concentration of sodium metasilicate is 3g/L~6g/L in oxidation electrolyte, and the concentration of potassium hydroxide is 3g/L~6g/L, the concentration of potassium fluoride It is 4g/L~8g/L, the concentration of sodium phosphate is 12g/L~18g/L；Three, ultrasonic microarc oxidation is handled：Micro-arc oxidation electrolyte prepared by step 2 is put into electrolytic cell, then by electrolytic cell It transfers in supersonic oscillations instrument, microarc oxidation equipment provided cathode connects stainless steel electrolytic slot, and anode connects in step 1 after acid processing Pure titanium sample, be arranged microarc oxidation equipment provided anode cathode separation be 40mm~60mm, start it is microarc oxidation equipment provided and ultrasonic Wave shaker, ultrasonic frequency is 30KHz~60KHz, differential arc oxidation voltage is 350V~450V, pulsewidth is 30 μ of μ s~80 S, pulse frequency be 300Hz~800Hz and duty ratio be 2.5% under conditions of ultrasonic microarc oxidation 3min~12min, close it is micro- Arc oxidation furnaces and supersonic oscillations instrument, sample taking-up distilled water flushing is clean, naturally dry；Four, it post-processes：1. the titanium sample that step 3 ultrasonic microarc oxidation has been handled is put into the NaOH aqueous solutions of 3mol/L~5mol/L, then It is placed in the water-bath that temperature is 60 DEG C~80 DEG C and keeps the temperature 20min~40min, wash with water rear naturally dry, obtain alkali process Titanium sample；2. configure the mixed aqueous solution of dopamine and trishydroxymethylaminomethane, with the hydrochloric acid tune pH of a concentration of 3mol/L be 7~ 8, Chinese Medicines are then added, ultrasonic 10min~30min obtains the mixed solution of dopamine-Chinese medicine；By step 4 1. in alkali The titanium sample of processing is put into the mixed solution of dopamine-Chinese medicine, then ultrasonic 10min is placed on room temperature and not light-exposed condition Lower standing for 24 hours, is dried in the shade naturally after taking-up, obtains medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling carries；The DOPA The concentration of Chinese medicine is 2g/L~8g/L in the mixed solution of amine-Chinese medicine；The dopamine and trishydroxymethylaminomethane mixes In Heshui solution the concentration of dopamine be 1.5g/L~2.5g/L, trishydroxymethylaminomethane concentration be 1.0g/L~1.5g/ L；The mixed aqueous solution of the dopamine and trishydroxymethylaminomethane is equal with the volume of Chinese Medicines.
- The system of medicine coating during 2. a kind of pure titanium mouth cavity planting body differential arc oxidation according to claim 1-DOPA amine coupling carries Preparation Method, it is characterised in that the concentration of sodium metasilicate is 5g/L in the micro-arc oxidation electrolyte described in step 2, potassium hydroxide Concentration is 5g/L, and the concentration of potassium fluoride is 6g/L, and the concentration of sodium phosphate is 14g/L.
- The system of medicine coating during 3. a kind of pure titanium mouth cavity planting body differential arc oxidation according to claim 1-DOPA amine coupling carries Preparation Method, it is characterised in that step 4 2. described in Chinese Medicines in Chinese medicine be Cortex Eucommiae chlorogenic acid, solvent is water.
- The system of medicine coating during 4. a kind of pure titanium mouth cavity planting body differential arc oxidation according to claim 1-DOPA amine coupling carries Preparation Method, it is characterised in that step 4 2. described in Chinese Medicines in Chinese medicine be kudzu-vine root powder, solvent is water.
- The system of medicine coating during 5. a kind of pure titanium mouth cavity planting body differential arc oxidation according to claim 1-DOPA amine coupling carries Preparation Method, it is characterised in that step 4 2. described in Chinese Medicines in Chinese medicine be icariin, solvent is absolute ethyl alcohol.
- The system of medicine coating during 6. a kind of pure titanium mouth cavity planting body differential arc oxidation according to claim 1-DOPA amine coupling carries Preparation Method, it is characterised in that step 4 2. described in Chinese Medicines in Chinese medicine be Drynaria rhizome powder, solvent is water.
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| CN111467572B (en) * | 2020-04-09 | 2022-07-29 | 上海交通大学医学院附属第九人民医院 | Implant material and preparation method and application thereof |
| CN112402693A (en) * | 2020-11-17 | 2021-02-26 | 上海市嘉定区中心医院(上海健康医学院附属嘉定区中心医院、上海交通大学医学院附属仁济医院嘉定分院) | Orthopedic implant instrument with surface provided with bone promoting coating and preparation method |
| CN113304316A (en) * | 2021-05-27 | 2021-08-27 | 南京医科大学附属口腔医院 | Treatment method for promoting bone formation activation on surface of zirconia implant |
| CN114129773B (en) * | 2021-12-06 | 2022-12-20 | 泰州市捷创生物科技研发有限公司 | Titanium implant with surface having bone-promoting performance and preparation method thereof |
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