CN106521601A - Preparation method for micro-arc oxidation-dopamine coupling carried traditional Chinese medicine coating of pure titanium oral implant - Google Patents
Preparation method for micro-arc oxidation-dopamine coupling carried traditional Chinese medicine coating of pure titanium oral implant Download PDFInfo
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Abstract
The invention discloses a preparation method for a micro-arc oxidation-dopamine coupling carried traditional Chinese medicine coating of a pure titanium oral implant and relates to a preparation method for a pure titanium oral implant. The preparation method disclosed by the invention aims to solve the technical problem of implantation failure as an existing titanium oral implant is slowly healed in the early implanting period and bacteria invade after implantation to lead to early infection after an implant surgery. The preparation method provided by the invention comprises the steps of: I, pre-treatment of the surface of a pure titanium test sample; II, preparation of a micro-arc oxidation electrolyte; III, ultrasonic micro-arc oxidation treatment; and IV, post-treatment. After micro-arc oxidation on the surface of a pure titanium implanting material, the material is modified by taking dopamine as a coupling agent carrying traditional Chinese medicines, so that growth and development of skeleton are promoted, material metabolism of human cells is enhanced, aging of muscles and skeleton is prevented, and the broad-spectrum antibacterial action is improved, and therefore, a novel bone implant which is better in biocompatibility and faster to heal is obtained.
Description
Technical field
The present invention relates to a kind of preparation method of pure titanium mouth cavity planting body coating.
Background technology
With the increase and the raising of human living standard of the wounds such as bone injury and Cranial defect, the mouth cavity planting body to Bone Defect Repari
The problems such as bacterium infection that implantation causes, also gradually attracts much attention.Compared with natural teeth, implant denture has its particularity,
Implantation body's cuff, i.e. wrapping implantation body wear the oral soft tissue at gum, and junctional epithelium herein acts primarily as barrier action, to plantation
Define good biological closing body week.But compared with natural teeth, the junctional epithelium attachment at implantation body's 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, implantation body with
The combination interface of bone lacks periodontal membrane, and when there is bacterial invasion, the inflammatory reaction in the region will be relatively low, immune defence ability
Corresponding weaker, antibacterial in this position aggregation breeding, and then will occur bone regeneration around implant infection.Implantation body and peri-implant
These features of structure determine that the soft tissue around which is easier to be affected by bacterial plaque, and impaired rear its surrounding tissue
There is larger gap compared with natural teeth in repair ability.
Early stage after Implant, due to destruction to local system of defense in the wound performed the operation and art, now
Antibacterial is easiest to the mucosa for invading bone regeneration around implant.Once the mucosa closing of bone regeneration around implant is destroyed, pathogenic bacterium just can be with
It is directly entered implantation body-synosteosis interface.And this interface feels more blunt to the harmful factor of pathogenic bacterium etc., it is long this with
Infect and its complication toward bone regeneration around implant can not only occur, and most may cause the loosening of implantation body at last and come off.
Chinese medicine and Chinese medicine extract have antiinflammatory, antibacterial and promote the function of osteogenesis.By taking Radix Puerariae as an example, Radix Puerariae is pulse family
The root of plant Herba Gelsemii Elegantis or Radix Puerariae rattan is dried and makes.Radix Puerariae has antiinflammatory, antipyretic, the effect of antibacterial.Puerarin is to osteoclast
Bone resorption function has a direct repression, and osteoclastic bone resorption function enliven be the Pathophysiology that occurs of osteoporosises it
One, it can promote osteoblastic increasing, differentiation, improve alkaline phosphatase activitieses, strengthen the expression of correlation mRNA, this explanation Pueraria lobota
Root can promote the g and D of bone.And puerarin is used as one of more effective ingredient of content in Radix Puerariae, in nature
In be widely present.Which has multiple pharmacological effect, and clearly, safety and low toxicity, clinical practice are extensive, and Radix Puerariae aboundresources for drug effect,
It is cheap.Therefore Radix Puerariae be can yet be regarded as a kind of suitable a herb for being used in mouth cavity planting body.
Coupling agent dopamine is present in a large number with biology in vivo, as dopamine and its derivant not only have waterproof adhesive energy
The substrate of power and its modified has good biocompatibility, will not encroach on human body cell and cause immunoreation, dopamine
Possess the adhesion feature similar to marine organisms Mussels, to be formed in the middle of the reaction of adhesion except participating in, and can be with
React to form stronger covalent bond and non-covalent bond with base material, the fixation that chelate can be formed and stabilized it
On the surface of titanium ion therefore most suitable act as connecting the function served as bridge of titanium and Chinese medicine without having infringement to human body.
The content of the invention
The present invention is that plantation immediate union is slow, after plantation, antibacterial invades and causes in order to solve current titanium mouth cavity planting body
There is early infection after Implant, make the technical problem of plantation failure, and a kind of pure titanium mouth cavity planting body differential arc oxidation-is provided more
The preparation method of medicine coating in bar amine coupling load.
A kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling of the present invention carry in medicine coating preparation method be by
What following steps were carried out：
First, pure titanium specimen surface pretreatment：Pending pure titanium specimen surface is roughly ground with sand paper, then use successively
Acetone and each ultrasonic 25min of distilled water, seal standby in being put into hermetic bag after drying up；
By HF sour, dense HNO3Uniformly mix with deionized water, obtain mixed acid, the pure titanium sample after drying up is put into mixing
20s～40s is soaked in acid, the pure titanium sample after acid treatment is obtained；The mass concentration of described HF acid is 40%～44%；It is described
Dense HNO3Mass concentration be 65%；Described HF is sour with dense HNO3Volume ratio be 1:2, described HF acid and deionized water
Volume ratio be 1:3；
2nd, configure micro-arc oxidation electrolyte：Sequentially add in beaker sodium silicate, potassium hydroxide, potassium fluoride, sodium phosphate and
Distilled water, sonic oscillation is completely dissolved to all reagents, stands 24h～36h, obtains micro-arc oxidation electrolyte；Described
In micro-arc oxidation electrolyte, the concentration of sodium silicate is 3g/L～6g/L, 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；
3rd, ultrasonic microarc oxidation is processed：Micro-arc oxidation electrolyte prepared by step 2 is put in electrolysis bath, then by electricity
Solution groove is transferred in supersonic oscillations instrument, and microarc oxidation equipment provided negative electrode connects stainless steel electrolytic groove, and anode is connect in step one at acid
Pure titanium sample after reason, it is 40mm～60mm to arrange microarc oxidation equipment provided anode cathode separation, start it is microarc oxidation equipment provided and
Supersonic oscillations instrument, ultrasonic frequency be 30KHz～60KHz, differential arc oxidation voltage be 350V～450V, pulsewidth be 30 μ s～
80 μ s, pulse frequency are 300Hz～800Hz and dutycycle is ultrasonic microarc oxidation 3min～12min under conditions of 2.5%, are closed
Microarc oxidation equipment provided and supersonic oscillations instrument is closed, sample taking-up is clean with distilled water flushing, dry naturally；
4th, post processing：
1. the titanium sample for step 3 ultrasonic microarc oxidation having been processed is put in the NaOH aqueous solutions of 3mol/L～5mol/L,
20min～40min is incubated in being subsequently placed in the water-bath that temperature is 60 DEG C～80 DEG C, is dried after being cleaned with water naturally, is obtained at alkali
The titanium sample of reason；
2. the mixed aqueous solution of dopamine and trishydroxymethylaminomethane is configured, with the hydrochloric acid tune pH that concentration is 3mol/L is
7～8, Chinese Medicines are subsequently adding, ultrasonic 10min～30min obtains the mixed solution of dopamine-Chinese medicine；By step 4 1. in
The titanium sample of alkali process is put in the mixed solution of dopamine-Chinese medicine, ultrasonic 10min, is then placed on room temperature and is loseed the bar of light
24h is stood under part, is dried in the shade after taking-up naturally, obtain medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling is carried；
In the mixed solution of described dopamine-Chinese medicine, the concentration of Chinese medicine is 2g/L～8g/L；Described 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 mixed aqueous solution of described dopamine and trishydroxymethylaminomethane and the volume of Chinese Medicines
It is equal.
The present invention carries Chinese medicine (such as Radix Puerariae by articulation agent of dopamine after to pure titanium planting material surface by micro-arc oxidation
Element) it is modified, promote bone growth and development using which, strengthen human body cell metabolism, prevent muscle skeleton aging, wide spectrum
Antibacterial action raising acquisition biocompatibility is more preferably, heal new bone planting body faster.This not only solves titanium this inertia
The compatibility of matrix and bone, and solve all the time as microorganism invades the breakage caused due to performing the operation in plantation
Mucosa, and make tooth-planting fail.
In view of Jing often occurs bacterium infection after tooth-planting, make tooth-planting fail, and many Chinese medicines such as Radix Puerariae has which
Bone and muscle strengthening, strengthens human body cell metabolism, prevents muscle skeleton aging, and have very good antibiotic property, along with differential of the arc oxygen
Change technology has high-efficiency environment friendly, easy to operate, coating and substrate combinating strength height, can pass through high temperature sintering in coating surface and put
The advantages of electrical breakdown acts on the porous ceramicss coating material to be formed containing required function element, therefore the present invention mainly adopts the differential of the arc
Oxidation technology carries medicine on pure titanium surface, and the advantage of differential arc oxidation is combined with the advantage of Chinese medicine, has efficiently so as to obtain
The new composite of Biofunctional mouth cavity planting body of the load Chinese medicine of biological activity.
The present invention provides a kind of differential arc oxidation titanium surface and carries Chinese medicine by coupling agent (dopamine), obtains with biological 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 new titanium implant composite of energy.
The present invention carries Chinese medicine by DOPA amine coupling using in pure titanium surface by micro-arc oxidation, obtains functional living being coating,
The Biocomposite material can make up the shortcoming of the successful titanium or titanium alloy of clinical practice, effectively improve the biological of titanium alloy
Energy.The biological property for carrying Chinese medicine film layer is ion exchange can occur with body fluid, deposits one layer of HA (hydroxy-apatite on surface
Stone) film layer, with good biocompatibility, along with Chinese medicine (such as Radix Puerariae) is with antibacterial, promote the growth and development of bone.System
The characteristics of standby planting body material combines Chinese medicine and excellent differential arc oxidation, possesses antibiotic property and accelerates the growth of bone and repair
New features.Therefore the composite can be used for mouth cavity planting body, and can be additionally used in osseous tissue defect, and damage etc. is repaired and replaced
Change, the clinical requirement to biological hard tissue alternate material can be met.
The present invention solves the method that adopted of technical problem：Based on biomedical pure titanium, using differential arc oxidation skill
Art, alkali process technology, DOPA amine coupling Chinese medicine (such as Radix Puerariae) method, are finally obtained functional living being composite coating material green wood
Material.
The present invention has following feature：
(1) propose that one kind adopts differential arc oxidation complex technique, prepare the bioactivity coatings of bottom dense skin porous,
Activated using alkali process afterwards, dopamine carries Chinese medicine as coupling agent, so as to obtain with the biological coating for carrying Chinese medicine；Titanium alloy is micro-
During arc oxidation carries medicine, medicine coating 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 adhesion, corrosion-resistant and good good biocompatibility
Feature；
(3) in the load, medicine coating and human body fluid react, negative ions that can be in titanium Chinese medicine coating surface by ion
Attract each other, one layer of hydroxyapatite (HA) coating is deposited on surface, can be promoted with good biocompatibility, and Chinese medicine
The synthesis of osteogenesis certain ribose, promotes skeleton development, accelerates bone early growth；
(4) during the biological activity is carried, medicine coating has fabulous antibiotic property, and up to 99%, this largely solves antibiotic rate
Determine mouth cavity planting body easy inflammation on oral cavity, the situation of breed bacteria, in case oral cavity causes secondary plantation because of infection；
(5) differential arc oxidization technique that medicine coating is adopted in the load, DOPA amine coupling carry Chinese medicine.Differential arc oxidization technique have set
It is standby to be simple and convenient to operate, economical and efficient, the characteristics of three-waste free discharge, the synthesis of dopamine coupling agent is simple, is present in biology in a large number
In vivo, therefore the features such as both approaches have simple, pollution-free, easy to operate and it is environmental protection treatment technology；
(6) the bioactivity coatings composite has good corrosion resistance, plants rub resistance abrasion, life in human body environment
The thing compatibility, does not produce man body pollution as implant；Intensity is high, good toughness, can be applicable 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 can form HA coatings, with human body after the immersion of SBF simulated body fluids
Skeleton has the good compatibility, and surface adds Radix Puerariae shorten bone healing time, improves early stage Bone Defect Repari speed and Bone Defect Repari
Quality.
Bioactivity coatings composite prepared by the present invention is by the bioactive ceramic coating and load on pure titanium surface
Medicine coating is composited, and the characteristics of have metal material and ceramic material concurrently, and introduces Chinese medicine, with good antibiotic property and rush
Enter the development of early stage bone, preparation method ultrasound-differential arc oxidation complex technique is as environmental protection technique, can ensure life well
Produce low cost and the more preferable osseous tissue impairment renovation material of Bone Defect Repari performance and bone tissue engineer cell scaffold material.
In the present invention, pure titanium used is biomedical special pure titanium, with nontoxic, safety, mechanical property is good the features such as.
In the present invention, electrolyte used is salt that is safe and nontoxic and will not producing the three wastes, and it is pure to be analysis, its into
This is low.
In the present invention prepared bioactivity coatings composite using when the HA that deposited be skeleton into
Point, any toxic and side effects will not be produced to human body.
The present invention is ultrasonic microarc oxidation treatment technology to be respectively adopted and differential arc oxidation post processing is combined to process biological doctor
Pure titanium is used, surface modification treatment is carried out to which, to improve its surface bioactive and corrosion resistance.
The bioactivity coatings composite of the present invention has good antibiotic property, while it can also promote osteoblast
Adhesion, increment, differentiation and alkaline phosphatase expression of enzymes, be conducive to be implanted into implantation body primary stability and early stage mineralising,
It is a kind of preferable implantation body's 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-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 figure,It is TiO2, figure a is pure titanium surface by micro-arc oxidation-dopamine coating in test four, and figure b is test
Medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling is carried in one, figure c are pure titanium surface by micro-arc oxidation-DOPA in test two
Amine coupling carry in medicine coating, figure d is medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling is carried in test three；
Fig. 6 is electrochemistry Tafel curve figure, and Fig. 1 is pure titanium surface by micro-arc oxidation-dopamine coating in test four, Fig. 2
It is medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling is carried in test one, Fig. 3 is pure titanium surface by micro-arc oxygen in test two
Change-DOPA amine coupling carry in medicine coating, Fig. 4 is medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling is carried in test three.
Specific embodiment
Specific embodiment one：Present embodiment is during a kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling is carried
The preparation method of medicine coating, is specifically carried out according to the following steps：
First, pure titanium specimen surface pretreatment：Pending pure titanium specimen surface is roughly ground with sand paper, then use successively
Acetone and each ultrasonic 25min of distilled water, seal standby in being put into hermetic bag after drying up；
By HF sour, dense HNO3Uniformly mix with deionized water, obtain mixed acid, the pure titanium sample after drying up is put into mixing
20s～40s is soaked in acid, the pure titanium sample after acid treatment is obtained；The mass concentration of described HF acid is 40%～44%；It is described
Dense HNO3Mass concentration be 65%；Described HF is sour with dense HNO3Volume ratio be 1:2, described HF acid and deionized water
Volume ratio be 1:3；
2nd, configure micro-arc oxidation electrolyte：Sequentially add in beaker sodium silicate, potassium hydroxide, potassium fluoride, sodium phosphate and
Distilled water, sonic oscillation is completely dissolved to all reagents, stands 24h～36h, obtains micro-arc oxidation electrolyte；Described
In micro-arc oxidation electrolyte, the concentration of sodium silicate is 3g/L～6g/L, 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；
3rd, ultrasonic microarc oxidation is processed：Micro-arc oxidation electrolyte prepared by step 2 is put in electrolysis bath, then by electricity
Solution groove is transferred in supersonic oscillations instrument, and microarc oxidation equipment provided negative electrode connects stainless steel electrolytic groove, and anode is connect in step one at acid
Pure titanium sample after reason, it is 40mm～60mm to arrange microarc oxidation equipment provided anode cathode separation, start it is microarc oxidation equipment provided and
Supersonic oscillations instrument, ultrasonic frequency be 30KHz～60KHz, differential arc oxidation voltage be 350V～450V, pulsewidth be 30 μ s～
80 μ s, pulse frequency are 300Hz～800Hz and dutycycle is ultrasonic microarc oxidation 3min～12min under conditions of 2.5%, are closed
Microarc oxidation equipment provided and supersonic oscillations instrument is closed, sample taking-up is clean with distilled water flushing, dry naturally；
4th, post processing：
1. the titanium sample for step 3 ultrasonic microarc oxidation having been processed is put in the NaOH aqueous solutions of 3mol/L～5mol/L,
20min～40min is incubated in being subsequently placed in the water-bath that temperature is 60 DEG C～80 DEG C, is dried after being cleaned with water naturally, is obtained at alkali
The titanium sample of reason；
2. the mixed aqueous solution of dopamine and trishydroxymethylaminomethane is configured, with the hydrochloric acid tune pH that concentration is 3mol/L is
7～8, Chinese Medicines are subsequently adding, ultrasonic 10min～30min obtains the mixed solution of dopamine-Chinese medicine；By step 4 1. in
The titanium sample of alkali process is put in the mixed solution of dopamine-Chinese medicine, ultrasonic 10min, is then placed on room temperature and is loseed the bar of light
24h is stood under part, is dried in the shade after taking-up naturally, obtain medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling is carried；Described is more
In the mixed solution of bar amine-Chinese medicine, the concentration of Chinese medicine is 2g/L～8g/L；Described dopamine and trishydroxymethylaminomethane
In mixed aqueous solution the concentration of dopamine be 1.5g/L～2.5g/L, the concentration of trishydroxymethylaminomethane be 1.0g/L～
1.5g/L；The mixed aqueous solution of described dopamine and trishydroxymethylaminomethane is equal with the volume of Chinese Medicines.
Specific embodiment two：Difference of the present embodiment from specific embodiment one is：It is micro- described in step 2
In arc oxidation electrolyte, the concentration of sodium silicate is 5g/L, 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 identical with specific embodiment one.
Specific embodiment three：Difference of the present embodiment from specific embodiment one is：Step 4 2. described in
Chinese medicine in Chinese Medicines is Cortex Eucommiae chlorogenic acid, and solvent is water.Other are identical with specific embodiment one.
Specific embodiment four：Difference of the present embodiment from specific embodiment one is：Step 4 2. described in
Chinese medicine in Chinese Medicines is powder of Radix Puerariae, and solvent is water.Other are identical with specific embodiment one.
Specific embodiment five：Difference of the present embodiment from specific embodiment one is：Step 4 2. described in
Chinese medicine in Chinese Medicines is icariin, and solvent is dehydrated alcohol.Other are identical with specific embodiment one.
Specific embodiment six：Difference of the present embodiment from specific embodiment one is：Step 4 2. described in
Chinese medicine in Chinese Medicines is Drynaria rhizome powder, and solvent is water.Other are identical with specific embodiment one.
Effect of the present invention is verified by tests below：
Test one：This test is the preparation of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling is carried
Method, is specifically carried out according to the following steps：
First, pure titanium specimen surface pretreatment：Pending pure titanium specimen surface is roughly ground with sand paper, then use successively
Acetone and each ultrasonic 25min of distilled water, seal standby in being put into hermetic bag after drying up；
By HF sour, dense HNO3Uniformly mix with deionized water, obtain mixed acid, the pure titanium sample after drying up is put into mixing
40s is soaked in acid, the pure titanium sample after acid treatment is obtained；The mass concentration of described HF acid is 40%；Described dense HNO3's
Mass concentration is 65%；Described HF is sour with dense HNO3Volume ratio be 1:2, described HF acid with the volume ratio of deionized water is
1:3；
2nd, configure micro-arc oxidation electrolyte：Sequentially add in beaker sodium silicate, potassium hydroxide, potassium fluoride, sodium phosphate and
Distilled water, sonic oscillation is completely dissolved to all reagents, stands 36h, obtains micro-arc oxidation electrolyte；Described differential of the arc oxygen
The concentration for changing sodium silicate 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；
3rd, ultrasonic microarc oxidation is processed：Micro-arc oxidation electrolyte prepared by step 2 is put in electrolysis bath, then by electricity
Solution groove is transferred in supersonic oscillations instrument, and microarc oxidation equipment provided negative electrode connects stainless steel electrolytic groove, and anode is connect in step one at acid
Pure titanium sample after reason, it is 50mm to arrange microarc oxidation equipment provided anode cathode separation, starts microarc oxidation equipment provided and ultrasound wave
Shaker, ultrasonic frequency be 50KHz, differential arc oxidation voltage be 400V, pulsewidth be 60 μ s, pulse frequency be 600Hz and to account for
Empty 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, dry naturally；
4th, post processing：
1. the titanium sample for step 3 ultrasonic microarc oxidation having been processed is put in the NaOH aqueous solutions of 4mol/L, is subsequently placed in
Temperature is to be incubated 30min in 70 DEG C of water-bath, dries naturally, obtain the titanium sample of alkali process after being cleaned with water；
2. the mixed aqueous solution of dopamine and trishydroxymethylaminomethane is configured, with the hydrochloric acid tune pH that concentration is 3mol/L is
7, Chinese Medicines are subsequently adding, ultrasonic 20min obtains the mixed solution of dopamine-Chinese medicine；By the titanium of step 4 1. middle alkali process
Sample is put in the mixed solution of dopamine-Chinese medicine, ultrasonic 10min, is then placed on room temperature and is stood under conditions of loseing light
24h, dries in the shade after taking-up naturally, obtains medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling is carried；Described dopamine-in
In the mixed solution of medicine, the concentration of Chinese medicine is 2.5g/L；In the mixed aqueous solution of described dopamine and trishydroxymethylaminomethane
It is 1.0g/L that the concentration of dopamine is 2g/L, the concentration of trishydroxymethylaminomethane；Described 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 Radix Puerariae
Powder, solvent are water.
Test two：This test is the preparation of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling is carried
Method：
This test from test one unlike step 4 2. described in dopamine-Chinese medicine mixed solution in Chinese medicine it is dense
Degree is 3.75g/L, and other are identical with test one.
Test three：This test is the preparation of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling is carried
Method：
This test from test one unlike step 4 2. described in dopamine-Chinese medicine mixed solution in Chinese medicine it is dense
Degree is 5g/L, and other are identical with test one.
Test four：This test be contrast test, a kind of preparation side of pure titanium mouth cavity planting body differential arc oxidation-dopamine coating
Method, specifically：
First, pure titanium specimen surface pretreatment：Pending pure titanium specimen surface is roughly ground with sand paper, then use successively
Acetone and each ultrasonic 25min of distilled water, seal standby in being put into hermetic bag after drying up；
By HF sour, dense HNO3Uniformly mix with deionized water, obtain mixed acid, the pure titanium sample after drying up is put into mixing
40s is soaked in acid, the pure titanium sample after acid treatment is obtained；The mass concentration of described HF acid is 40%；Described dense HNO3's
Mass concentration is 65%；
2nd, configure micro-arc oxidation electrolyte：Sequentially add in beaker sodium silicate, potassium hydroxide, potassium fluoride, sodium phosphate and
Distilled water, sonic oscillation is completely dissolved to all reagents, stands 36h, obtains micro-arc oxidation electrolyte；Described differential of the arc oxygen
The concentration for changing sodium silicate 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；
3rd, ultrasonic microarc oxidation is processed：Micro-arc oxidation electrolyte prepared by step 2 is put in electrolysis bath, then by electricity
Solution groove is transferred in supersonic oscillations instrument, and microarc oxidation equipment provided negative electrode connects stainless steel electrolytic groove, and anode is connect in step one at acid
Pure titanium sample after reason, it is 50mm to arrange microarc oxidation equipment provided anode cathode separation, starts microarc oxidation equipment provided and ultrasound wave
Shaker, ultrasonic frequency be 50KHz, differential arc oxidation voltage be 400V, pulsewidth be 60 μ s, pulse frequency be 600Hz and to account for
Empty 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, dry naturally；
4th, post processing：
1. the titanium sample for step 3 ultrasonic microarc oxidation having been processed is put in the NaOH aqueous solutions of 4mol/L, is subsequently placed in
Temperature is to be incubated 30min in 70 DEG C of water-bath, dries naturally, obtain the titanium sample of alkali process after being cleaned with water；
2. the mixed aqueous solution of dopamine and trishydroxymethylaminomethane is configured, with the hydrochloric acid tune pH that concentration is 3mol/L is
7；The titanium sample of step 4 1. middle alkali process is put in the mixed aqueous solution of dopamine and trishydroxymethylaminomethane, ultrasound
10min, is then placed on room temperature and stands 24h under conditions of loseing light, dry in the shade naturally, obtain pure titanium surface by micro-arc oxygen after taking-up
Change-dopamine coating；In the mixed aqueous solution of described 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-DOPA amine coupling is carried are tested, Fig. 3 is test 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 test three
The SEM surface topography maps of 2000 times of medicine coating in titanium surface by micro-arc oxidation-DOPA amine coupling load, as can be seen from the figure pure titanium is micro-
Arc oxidized surface carries Radix Puerariae surface compact, and the micropore that aperture is more or less the same, most hole are 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 Radix Puerariae under action of coupling agents.
Fig. 5 is XRD figure,It is TiO2, figure a is pure titanium surface by micro-arc oxidation-dopamine coating in test four, and figure b is test
Medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling is carried in one, figure c are pure titanium surface by micro-arc oxidation-DOPA in test two
Amine coupling carry in medicine coating, figure d is medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling is carried in test three, can from figure
To find out that pure titanium differential arc oxidization surface carries the mutually predominantly TiO on Radix Puerariae surface2。
Fig. 6 is electrochemistry Tafel curve figure, and Fig. 1 is pure titanium surface by micro-arc oxidation-dopamine coating in test four, Fig. 2
It is medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling is carried in test one, Fig. 3 is pure titanium surface by micro-arc oxygen in test two
Change-DOPA amine coupling carry in medicine coating, Fig. 4 is medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling is carried in test three, from
Can be seen that in figure that pure titanium differential arc oxidization surface carries the plan voltage of Radix Puerariae face coat higher than the differential arc oxidation for only adding coupling agent
Coating, current potential are high, corrosion resistance excellent.
Claims (6)
1. the preparation method of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling is carried, it is characterised in that pure
In titanium mouth cavity planting body differential arc oxidation-DOPA amine coupling load, the preparation method of medicine coating is carried out according to the following steps：
First, pure titanium specimen surface pretreatment：Pending pure titanium specimen surface is roughly ground with sand paper, then use acetone successively
Ultrasonic 25min each with distilled water, seals standby in being put into hermetic bag after drying up；
By HF sour, dense HNO3Uniformly mix with deionized water, obtain mixed acid, the pure titanium sample after drying up is put in mixed acid
Immersion 20s～40s, obtains the pure titanium sample after acid treatment；The mass concentration of described HF acid is 40%～44%；Described is dense
HNO3Mass concentration be 65%；Described HF is sour with dense HNO3Volume ratio be 1:The sour body with deionized water of 2, described HF
Product is than being 1:3；
2nd, configure micro-arc oxidation electrolyte：Sodium silicate, potassium hydroxide, potassium fluoride, sodium phosphate and distillation are sequentially added in beaker
Water, sonic oscillation is completely dissolved to all reagents, stands 24h～36h, obtains micro-arc oxidation electrolyte；The described differential of the arc
In oxidation electrolyte, the concentration of sodium silicate is 3g/L～6g/L, 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；
3rd, ultrasonic microarc oxidation is processed：Micro-arc oxidation electrolyte prepared by step 2 is put in electrolysis bath, then by electrolysis bath
Transfer in supersonic oscillations instrument, microarc oxidation equipment provided negative electrode connects stainless steel electrolytic groove, anode is connect in step one after acid treatment
Pure titanium sample, it is 40mm～60mm to arrange microarc oxidation equipment provided anode cathode separation, is started microarc oxidation equipment provided and ultrasonic
Ripple shaker, ultrasonic frequency be 30KHz～60KHz, differential arc oxidation voltage be 350V～450V, pulsewidth be 30 μ s～80 μ
S, pulse frequency are 300Hz～800Hz and dutycycle is ultrasonic microarc oxidation 3min～12min under conditions of 2.5%, are closed micro-
Arc oxidation furnaces and supersonic oscillations instrument, sample taking-up is clean with distilled water flushing, dry naturally；
4th, post processing：
1. in the NaOH aqueous solutions of 3mol/L～5mol/L, then the titanium sample for step 3 ultrasonic microarc oxidation having been processed is put into
Insulation 20min～40min in the water-bath that temperature is 60 DEG C～80 DEG C is placed in, is dried after being cleaned with water naturally, is obtained alkali process
Titanium sample；
2. configure the mixed aqueous solution of dopamine and trishydroxymethylaminomethane, with the hydrochloric acid that concentration is 3mol/L adjust pH be 7～
8, Chinese Medicines are subsequently adding, ultrasonic 10min～30min obtains the mixed solution of dopamine-Chinese medicine；By step 4 1. middle alkali
The titanium sample of process is put in the mixed solution of dopamine-Chinese medicine, ultrasonic 10min, is then placed on room temperature and is loseed the condition of light
Lower standing 24h, dries in the shade after taking-up naturally, obtains medicine coating during pure titanium surface by micro-arc oxidation-DOPA amine coupling is carried；Described DOPA
In the mixed solution of amine-Chinese medicine, the concentration of Chinese medicine is 2g/L～8g/L；Described dopamine and trishydroxymethylaminomethane it is mixed
In Heshui solution the concentration of dopamine be 1.5g/L～2.5g/L, the concentration of trishydroxymethylaminomethane be 1.0g/L～1.5g/
L；The mixed aqueous solution of described dopamine and trishydroxymethylaminomethane is equal with the volume of Chinese Medicines.
2. the system of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation according to claim 1-DOPA amine coupling is carried
Preparation Method, it is characterised in that the concentration of sodium silicate 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.
3. the system of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation according to claim 1-DOPA amine coupling is carried
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.
4. the system of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation according to claim 1-DOPA amine coupling is carried
Preparation Method, it is characterised in that step 4 2. described in Chinese Medicines in Chinese medicine be powder of Radix Puerariae, solvent is water.
5. the system of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation according to claim 1-DOPA amine coupling is carried
Preparation Method, it is characterised in that step 4 2. described in Chinese Medicines in Chinese medicine be icariin, solvent is dehydrated alcohol.
6. the system of medicine coating during a kind of pure titanium mouth cavity planting body differential arc oxidation according to claim 1-DOPA amine coupling is carried
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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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108187135A (en) * | 2018-02-07 | 2018-06-22 | 四川大学 | Multifunctional titanium planting body based on poly-dopamine modification and preparation method thereof |
| CN111467572A (en) * | 2020-04-09 | 2020-07-31 | 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 |
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Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07305178A (en) * | 1994-05-02 | 1995-11-21 | Noboru Naruo | Aluminum utensil and its production |
| US20080086195A1 (en) * | 2006-10-05 | 2008-04-10 | Boston Scientific Scimed, Inc. | Polymer-Free Coatings For Medical Devices Formed By Plasma Electrolytic Deposition |
| CN101632842A (en) * | 2009-08-20 | 2010-01-27 | 华南理工大学 | Modification method used for surface of magnesium alloy stent |
| CN101721753A (en) * | 2009-12-23 | 2010-06-09 | 天津大学 | Absorbable magnesium alloy bracket of inorganic and organic antiseptic biocompatible composite coating and preparation method thereof |
| CN101797191A (en) * | 2009-12-31 | 2010-08-11 | 哈尔滨工业大学 | Corrosion-resistant magnesium alloy bracket and preparation method thereof |
| CN101899700A (en) * | 2009-05-25 | 2010-12-01 | 佳木斯大学 | Preparation method of ultrasonic microarc oxidation silver-carrying antibiotic bioactive coating on magnesium and titanium surface |
| CN102058904A (en) * | 2010-12-31 | 2011-05-18 | 重庆大学 | Biological functionalized nano titanium material and preparation method thereof |
| CN103556204A (en) * | 2013-11-04 | 2014-02-05 | 佳木斯大学 | Preparation method of magnesium surface ultrasonic micro-arc oxidation-HF-silane coupling agent multistage compound bioactive coating |
| CN103556203A (en) * | 2013-11-04 | 2014-02-05 | 佳木斯大学 | Preparation method of magnesium surface ultrasonic micro-arc oxidation-HF-silica sol multistage compound bioactive coating composite material |
| CN103882497A (en) * | 2014-04-16 | 2014-06-25 | 长安大学 | Method for preparing composite ceramic membrane on surface of magnesium alloy intravascular stent by micro-arc oxidation |
| CN104233431A (en) * | 2014-09-26 | 2014-12-24 | 佳木斯大学 | Preparation method of composite material of pure magnesium surface ultrasonic microarc oxidation-phytic acid-silk fibroin multistage composite biologically-active coating |
| CN105442022A (en) * | 2015-11-24 | 2016-03-30 | 哈尔滨医科大学 | Method for preparing gentamicin-loaded magnesium-based calcium phosphate/chitosan/nanotube medicine carrying film layer through electrophoresis method |
-
2016
- 2016-11-22 CN CN201611034630.6A patent/CN106521601B/en not_active Expired - Fee Related
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07305178A (en) * | 1994-05-02 | 1995-11-21 | Noboru Naruo | Aluminum utensil and its production |
| US20080086195A1 (en) * | 2006-10-05 | 2008-04-10 | Boston Scientific Scimed, Inc. | Polymer-Free Coatings For Medical Devices Formed By Plasma Electrolytic Deposition |
| CN101899700A (en) * | 2009-05-25 | 2010-12-01 | 佳木斯大学 | Preparation method of ultrasonic microarc oxidation silver-carrying antibiotic bioactive coating on magnesium and titanium surface |
| CN101632842A (en) * | 2009-08-20 | 2010-01-27 | 华南理工大学 | Modification method used for surface of magnesium alloy stent |
| CN101721753A (en) * | 2009-12-23 | 2010-06-09 | 天津大学 | Absorbable magnesium alloy bracket of inorganic and organic antiseptic biocompatible composite coating and preparation method thereof |
| CN101797191A (en) * | 2009-12-31 | 2010-08-11 | 哈尔滨工业大学 | Corrosion-resistant magnesium alloy bracket and preparation method thereof |
| CN102058904A (en) * | 2010-12-31 | 2011-05-18 | 重庆大学 | Biological functionalized nano titanium material and preparation method thereof |
| CN103556204A (en) * | 2013-11-04 | 2014-02-05 | 佳木斯大学 | Preparation method of magnesium surface ultrasonic micro-arc oxidation-HF-silane coupling agent multistage compound bioactive coating |
| CN103556203A (en) * | 2013-11-04 | 2014-02-05 | 佳木斯大学 | Preparation method of magnesium surface ultrasonic micro-arc oxidation-HF-silica sol multistage compound bioactive coating composite material |
| CN103882497A (en) * | 2014-04-16 | 2014-06-25 | 长安大学 | Method for preparing composite ceramic membrane on surface of magnesium alloy intravascular stent by micro-arc oxidation |
| CN104233431A (en) * | 2014-09-26 | 2014-12-24 | 佳木斯大学 | Preparation method of composite material of pure magnesium surface ultrasonic microarc oxidation-phytic acid-silk fibroin multistage composite biologically-active coating |
| CN105442022A (en) * | 2015-11-24 | 2016-03-30 | 哈尔滨医科大学 | Method for preparing gentamicin-loaded magnesium-based calcium phosphate/chitosan/nanotube medicine carrying film layer through electrophoresis method |
Non-Patent Citations (4)
| Title |
|---|
| DAI YAO等: "Preparation and characterization of icariin/PHBV drug delivery coatings on anodic oxidized titanium", 《TRANS. NONFERROUS MET. SOC. CHINA》 * |
| 戴瑶: "增强生物相容性的医用钛生物材料的研究", 《湖南大学硕士学位论文》 * |
| 李慕勤 等: "褪黑素对纯钛超声微弧氧化膜层体内植入骨结合的影响", 《口腔颌面外科杂志》 * |
| 王静 等: "超声微弧氧化在医用钛合金表面制备生物活性涂层", 《材料热处理学报》 * |
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| CN108187135A (en) * | 2018-02-07 | 2018-06-22 | 四川大学 | Multifunctional titanium planting body based on poly-dopamine modification and preparation method thereof |
| CN111467572A (en) * | 2020-04-09 | 2020-07-31 | 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 |
| CN114129773A (en) * | 2021-12-06 | 2022-03-04 | 泰州市捷创生物科技研发有限公司 | Titanium implant with osteogenesis promoting and antibacterial properties on surface and preparation method thereof |
| 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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