CN106676608A - Preparation method of medical pure magnesium surface electrophoretic deposition carried bone growth inducing traditional Chinese medicine coating - Google Patents
Preparation method of medical pure magnesium surface electrophoretic deposition carried bone growth inducing traditional Chinese medicine coating Download PDFInfo
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- CN106676608A CN106676608A CN201611034629.3A CN201611034629A CN106676608A CN 106676608 A CN106676608 A CN 106676608A CN 201611034629 A CN201611034629 A CN 201611034629A CN 106676608 A CN106676608 A CN 106676608A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/448—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications characterised by the additives used
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Abstract
The invention discloses a preparation method of a medical pure magnesium surface electrophoretic deposition carried bone growth inducing traditional Chinese medicine coating, and relates to a preparation method of a medical pure magnesium surface coating, in order to solve the technical problems that the existing medical magnesium and magnesium alloy materials are too high in degradation rates and cause inflammatory reaction. The preparation method comprises the following steps: one, pure magnesium specimen surface pretreatment is carried out; two, a micro-arc oxidation electrolytic solution is prepared; three, ultrasound micro-arc oxidation treatment is carried out; and four, post treatment is carried out. According to the preparation method, after magnesium and magnesium alloy ultrasound micro-arc oxidation is carried out, electrophoretic deposition is carried out on a hydrophilic and hydrophobic carried purified traditional Chinese medicine coating, after assembly, the matching between a degradation rate and an osseous tissue regenerating or fracture healing rate in vivo is achieved, the surface carried purified traditional Chinese medicine coating has antibacterial and antiphlogistic properties and bone tissue regeneration inducing property; the influencing mechanism of hydrophilic and hydrophobic medicine carrying surfaces on the antibacterial property, the corrosion resistance and the degradation property of the traditional Chinese medicine coating is provided; and a magnesium bone internal fixation material has good mechanical properties of a metallic material, and has corrosion resistance, antibacterial property and excellent bioactivity.
Description
Technical field
The present invention relates to a kind of preparation method of medical pure magnesium surface coating.
Background technology
Magnesium and magnesium alloy have become the focus of people's research, and many scholars are for magnesium alloy in multi-porous tissue engineering
The medical science such as frame, intravascular stent, bone implant material aspect has extensive research, for medical magnesium-base metal vivo degradation speed with
Freshman bone tissue or the unmatched problem of speed of fracture union.How effectively to improve magnesium-base metal degradation rate it is too fast and
The problem of corrosion resistance difference, only studies medical magnesium alloy mechanism of degradation in vivo, can just find out solve problem effective way.
Chinese medicine is with a long history, abundance, draws materials conveniently, and usage is simple, evident in efficacy, and toxic and side effects are slightly enjoyed
Concern.The Cortex Eucommiae is recorded in earliest《Sheng Nong's herbal classic》, the effects such as with invigorating the liver and kidney, bone and muscle strengthening, strong waist and knee, antiabortive gas, blood pressure lowering.
The scholar's research such as Xu Xianghe find that the Cortex Eucommiae can be by promoting MC3T3-E1 osteoblastic proliferations and differentiation and maturation, indirectly to suppress
The differentiation of osteoclast and maturation, so as to suppress bone resorption.The scholar's research such as Lin Jun find Folium Eucommiae extract/calcium skeleton cement
Complex carrier has the effect for promoting osteoblastic propagation and growing and adhere to.Herba Epimedii is in traditional kidney invigorating and YANG supporting
Medicine, has functions that invigorating kidney-YANG, hard muscles and bones, wind-damp dispelling, is the conventional medicine of clinical treatment osteoporosises.Herba Epimedii it is main effectively
Composition is flavone compound, and icariin is the Main Flavonoids monomer component of Herba Epimedii.Herba Epimedii total flavones (TFE) can lead to
Impact osteoblastic proliferation, differentiation, mineralising promoting bone growing etc. are crossed, icariin has the work for promoting Oesteoblast growth propagation
With.
The research of magnesium alloy vivo degradation speed is controlled around Magnesiumalloy surface modifying, gratifying progress is had been achieved with.But
Have been found that after we carry out finishing analysis to result of study：(1) magnesium alloy is restricted as bone internal fixation material clinical practice one
Individual key issue is how to make matching between vivo degradation speed and osseous tissue new life or speed of fracture union, especially
Premature degradation is controlled；(2) medical magnesium alloy surface modified coating vivo degradation Study on product is little, to cytoactive, antibiotic property
How affect, degradation in vivo product deposition, absorb and be a non-negligible problem with organism interactively；(3) cure
With monotechnics is adopted Magnesiumalloy surface modifying method more, respectively with advantage and deficiency, such as Mg alloy surface prepares coating or film
Low with substrate combinating strength, coating is easy to fall off, and protective effect is lost too early；(4) medical magnesium alloy surface is modified, drug-carried coat
The pharmacological mechanism few people research of induction of bone growth.
Magnesium and magnesium alloy have that degradation speed is too fast, inflammatory reaction deadly defect, seriously hinder magnesium and magnesium alloy material
Expect the development in clinical practice field.
The content of the invention
The present invention be in order to solve current medical magnesium and magnesium alloy materials to there is degradation speed too fast, inflammatory reaction fatal
Weakness, seriously hinders the technical problem of magnesium and magnesium alloy materials in the development in clinical practice field, and provides a kind of medical pure
Magnesium surface electrophoretic deposition carries the preparation method of medicine coating in induction of bone growth.
The present invention a kind of medical pure magnesium surface electrophoretic deposition carry induction of bone growth in medicine coating preparation method be by with
What lower step was carried out：
First, pure magnesium specimen surface pretreatment：Pending pure magnesium specimen surface is roughly ground with sand paper, is then used successively
Acetone and each ultrasonic 25min of distilled water, are put in hermetic bag after drying up and seal standby；
2nd, micro-arc oxidation electrolyte is configured：Distilled water is fitted in beaker, then sequentially add sodium silicate, potassium hydroxide,
Potassium fluoride and disodiumedetate, a kind of reagent under adding again after being required to stir when often adding a kind of reagent, all
Sonic oscillation is carried out after adding, being completely dissolved to all reagents, micro-arc oxidation electrolyte is obtained；Described differential arc oxidation electricity
The concentration of sodium silicate is 15g/L~20g/L in solution liquid, and the concentration of potassium hydroxide is 10g/L~20g/L, and the concentration of potassium fluoride is
8g/L~20g/L, the concentration of disodiumedetate is 1g/L~10g/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 connects surface in step one
The complete pure magnesium sample of pretreatment, it is 40mm~60mm to arrange microarc oxidation equipment provided anode cathode separation, starts differential arc oxidation and sets
Standby and supersonic oscillations instrument, ultrasonic frequency be 40KHz~60KHz, differential arc oxidation voltage be 200V~400V, pulsewidth be 40
μ s~60 μ s, pulse frequency be 400Hz~700Hz and dutycycle be ultrasonic microarc oxidation 5min under conditions of 2.5%~
20min, closes microarc oxidation equipment provided and supersonic oscillations instrument, and sample taking-up is clean with distilled water flushing, dries naturally；
4th, post processing：
1. the magnesium sample for step 3 ultrasonic microarc oxidation having been processed is put in the NaOH aqueous solutions of 1mol/L~3mol/L,
Insulation 1h~2h in the water-bath that temperature is 60 DEG C~80 DEG C is subsequently placed in, is dried naturally after being cleaned with water, obtain the magnesium of alkali process
Sample；
2. configuration concentration is the chitosan solution of 1g/L~3g/L, is subsequently adding the Chinese Medicines that concentration is 2mg/mL, surpasses
Sound 10min~30min, obtains electrophoresis liquid；The concentration of Chinese medicine is 0.4mg/mL~1.9mg/mL in described electrophoresis liquid；Described
It is 1 that solvent in chitosan solution is the volume ratio of the mixed liquor of water and glacial acetic acid, glacial acetic acid and water:100；3. electrophoresis liquid is put
In stainless steel tank, the magnesium sample of alkali process is placed in electrophoresis liquid, then the magnesium sample with alkali process is as negative pole, rustless steel
Groove is positive pole, and voltage is electrophoretic deposition 3min~6min under conditions of 10V~20V, is dried naturally after taking-up, obtains pure magnesium surface
Electrophoretic deposition carries medicine coating in induction of bone growth.
The present invention is proposed after magnesium and magnesium alloy ultrasound differential arc oxidation, then is carried out in the hydrophilic, hydrophobic load purification of electrophoretic deposition
Medicine coating, it is assembled after reach degradation in vivo speed with matching between freshman bone tissue or speed of fracture union, surface
Carry purification Chinese traditional medicine layer has antibacterial anti-inflammatory and induction osteanagenesiss performance, and propose it is hydrophilic, hydrophobic load medicine surface to its antibacterial,
The influencing mechanism of corrosion degradation performance, the good mechanical property of this existing metal material of magnesium bone internal fixation material also has concurrently anti-corrosion
Property, antibiotic property and excellent biological activity.
The present invention provide the good mechanical property of existing metal material of a kind of magnesium and Mg alloy surface also have concurrently corrosion resistance,
Antibiotic property and excellent biological activity sclerous tissueses replacement and the material repaired, the biological active coating for being substantially shorter bone healing time
The preparation method of the composite of layer.
It is of the invention to pass through this technological means of surface treatment, build the immersion of controllable body fluid, resist in magnesium and Mg alloy surface
Medicine coating in bacterium, the hydrophilic, hydrophobic load purification of the Complicated primary of promotion bone so as to vivo degradation speed and freshman bone tissue can be reached
Matching, antibacterial anti-inflammatory, and promote implantation initial stage Bone Defect Repari with excellent biological activated energy, can be used as bone internal fixation material.
The present invention is proposed after magnesium and magnesium alloy ultrasound differential arc oxidation, then is carried out in the hydrophilic, hydrophobic load purification of electrophoretic deposition
Medicine coating, it is assembled after reach degradation in vivo speed with matching between freshman bone tissue or speed of fracture union, surface
The performance that purification Chinese traditional medicine layer has antibacterial anti-inflammatory and induction osteanagenesiss is carried, this existing metal material of magnesium bone internal fixation material is good
Good mechanical property also has corrosion resistance, antibiotic property and excellent biological activity concurrently.
The present invention solves the scheme that adopted of technical problem：Based on biomedical magnesium and magnesium alloy, propose to adopt
Ultrasound-differential arc oxidization technique composite electrophoresis deposition post-processing technology, to pure magnesium surface modification treatment is carried out, and makes magnesium and magnesium alloy table
Face is differential arc oxidation load Chinese medicine extraction nitride layer, and regulates and controls the various parameters of differential arc oxidation, electrophoretic deposition, and finally prepared magnesium and magnesium are closed
Gold surface is hydrophilic, hydrophobic to carry Chinese medicine extract coating material.
The invention has the advantages that：
(1) present invention proposes a kind of ultrasound-differential arc oxidation composite electrophoresis deposition technique, prepares bottom dense skin many
Hole outermost layer is the hydrophilic, hydrophobic load Chinese medicine extract coating material of chitosan-loaded Chinese medicine extraction nitride layer, magnesium alloy coating and matrix
Bond strength be 6MPa~18MPa；
(2) coating material of the invention is to carry Chinese traditional medicine purification thing coating by the biological activity shitosan on magnesium alloy and its surface
It is composited, the hydrophilic, hydrophobic good mechanical property of the existing metal material of Chinese medicine extract coating material that carries also has corrosion resistance concurrently, resists
Bacterium property and excellent biological activity, can be used for Bone Defect Repari and replacement, with controlled degradation and absorbability as load bone；
(3) coating of the bioactivity coatings composite is in magnesium alloy table by ultrasound-differential arc oxidation complex technique
Face in-situ high temperature is generated, and coating and matrix are metallurgical binding, and bond strength is higher than single differential arc oxidation treatment technology；
(4) coating material thickness of the invention is adjustable between 5 μm~40 μm；
(5) the hydrophilic, hydrophobic load Chinese medicine extract coating material is loaded into Chinese medicine in Mg alloy surface by carrier of shitosan, can
Shorten bone healing time, with anti-microbial property and can improve the speed and Bone Defect Repari quality of Bone Defect Repari.
Electrolyte used is salt that is safe and nontoxic and will not producing the three wastes in the present invention, be analysis it is pure, its into
This is low.
Chinese medicine extract used such as Cortex Eucommiae chlorogenic acid and icariin in the present invention.The Cortex Eucommiae is recorded in earliest《Legendary god of farming's sheet
Careless Jing》, the effects such as with invigorating the liver and kidney, bone and muscle strengthening, strong waist and knee, antiabortive gas, blood pressure lowering, the Cortex Eucommiae can be by promoting MC3T3-E1 skeletonization
Cell is bred and differentiation and maturation, indirectly to suppress differentiation and the maturation of osteoclast, so as to suppress bone resorption.Herba Epimedii is biography
The kidney invigorating and YANG supporting Chinese medicine of system, has functions that invigorating kidney-YANG, hard muscles and bones, wind-damp dispelling, is the conventional medicine of clinical treatment osteoporosises.It is excessive
The principle active component of the sheep leaves of pulse plants is flavone compound, and icariin is the Main Flavonoids monomer component of Herba Epimedii.Herba Epimedii is total
Flavone (TFE) can have promotion skeletonization thin by affecting osteoblastic proliferation, differentiation, mineralising promoting bone growing etc., icariin
The effect of intracellular growth propagation.
Description of the drawings
Fig. 1 is to test the contact angle pattern that a pure magnesium surface electrophoretic deposition for preparing carries medicine coating in induction of bone growth；
Fig. 2 is to test the contact angle pattern that the two pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Fig. 3 is to test the contact angle pattern that the three pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Fig. 4 is to test the contact angle pattern that the four pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Fig. 5 is to test the contact angle pattern that the five pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Fig. 6 is to test the contact angle pattern that the six pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Fig. 7 is to test the contact angle pattern that the seven pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Fig. 8 is to test the contact angle pattern that the eight pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Fig. 9 is to test the contact angle pattern that the nine pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Figure 10 is to test the contact angle pattern that the ten pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Figure 11 is to test the SEM figures that the five pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Figure 12 is to test the SEM figures that the six pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Figure 13 is to test the SEM figures that the seven pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Figure 14 is to test the SEM figures that the eight pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Figure 15 is to test the SEM figures that the nine pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Figure 16 is to test the SEM figures that the ten pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth；
Figure 17 is to test the 11 pure magnesium surface electrophoretic deposition coatings for preparing to colibacillary fungistatic effect figure；
Figure 18 be test five prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to colibacillary suppression
Bacterium design sketch；
Figure 19 be test six prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to colibacillary suppression
Bacterium design sketch；
Figure 20 be test seven prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to colibacillary suppression
Bacterium design sketch；
Figure 21 be test eight prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to colibacillary suppression
Bacterium design sketch；
Figure 22 be test nine prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to colibacillary suppression
Bacterium design sketch；
Figure 23 be test ten prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to colibacillary suppression
Bacterium design sketch；
Figure 24 is the fungistatic effect figure for testing the 11 pure magnesium surface electrophoretic deposition coatings for preparing to staphylococcus aureuses；
Figure 25 be test five prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to Staphylococcus aureus
The fungistatic effect figure of bacterium；
Figure 26 be test six prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to Staphylococcus aureus
The fungistatic effect figure of bacterium；
Figure 27 be test seven prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to Staphylococcus aureus
The fungistatic effect figure of bacterium；
Figure 28 be test eight prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to Staphylococcus aureus
The fungistatic effect figure of bacterium；
Figure 29 be test nine prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to Staphylococcus aureus
The fungistatic effect figure of bacterium；
Figure 30 be test ten prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to Staphylococcus aureus
The fungistatic effect figure of bacterium.
Specific embodiment
Specific embodiment one：Present embodiment carries induction of bone growth Chinese medicine and applies for a kind of medical pure magnesium surface electrophoretic deposition
The preparation method of layer, is specifically carried out according to the following steps：
First, pure magnesium specimen surface pretreatment：Pending pure magnesium specimen surface is roughly ground with sand paper, is then used successively
Acetone and each ultrasonic 25min of distilled water, are put in hermetic bag after drying up and seal standby；
2nd, micro-arc oxidation electrolyte is configured：Distilled water is fitted in beaker, then sequentially add sodium silicate, potassium hydroxide,
Potassium fluoride and disodiumedetate, a kind of reagent under adding again after being required to stir when often adding a kind of reagent, all
Sonic oscillation is carried out after adding, being completely dissolved to all reagents, micro-arc oxidation electrolyte is obtained；Described differential arc oxidation electricity
The concentration of sodium silicate is 15g/L~20g/L in solution liquid, and the concentration of potassium hydroxide is 10g/L~20g/L, and the concentration of potassium fluoride is
8g/L~20g/L, the concentration of disodiumedetate is 1g/L~10g/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 connects surface in step one
The complete pure magnesium sample of pretreatment, it is 40mm~60mm to arrange microarc oxidation equipment provided anode cathode separation, starts differential arc oxidation and sets
Standby and supersonic oscillations instrument, ultrasonic frequency be 40KHz~60KHz, differential arc oxidation voltage be 200V~400V, pulsewidth be 40
μ s~60 μ s, pulse frequency be 400Hz~700Hz and dutycycle be ultrasonic microarc oxidation 5min under conditions of 2.5%~
20min, closes microarc oxidation equipment provided and supersonic oscillations instrument, and sample taking-up is clean with distilled water flushing, dries naturally；
4th, post processing：
1. the magnesium sample for step 3 ultrasonic microarc oxidation having been processed is put in the NaOH aqueous solutions of 1mol/L~3mol/L,
Insulation 1h~2h in the water-bath that temperature is 60 DEG C~80 DEG C is subsequently placed in, is dried naturally after being cleaned with water, obtain the magnesium of alkali process
Sample；
2. configuration concentration is the chitosan solution of 1g/L~3g/L, is subsequently adding the Chinese Medicines that concentration is 2mg/mL, surpasses
Sound 10min~30min, obtains electrophoresis liquid；The concentration of Chinese medicine is 0.4mg/mL~1.9mg/mL in described electrophoresis liquid；Described
It is 1 that solvent in chitosan solution is the volume ratio of the mixed liquor of water and glacial acetic acid, glacial acetic acid and water:100；
3. electrophoresis liquid is placed in stainless steel tank, the magnesium sample of alkali process is placed in electrophoresis liquid, then with alkali process
Magnesium sample be negative pole, stainless steel tank be positive pole, voltage be 10V~20V under conditions of electrophoretic deposition 3min~6min, after taking-up
Naturally dry, obtain pure magnesium surface electrophoretic deposition and carry medicine coating in induction of bone growth.
Specific embodiment two：Present embodiment is with the difference of specific embodiment one：It is micro- described in step 2
The concentration of sodium silicate is 15g/L in arc oxidation electrolyte, and the concentration of potassium hydroxide is 10g/L, and the concentration of potassium fluoride is 8g/L, second
The concentration of edetate disodium is 1g/L.Other are identical with specific embodiment one.
Specific embodiment three：Present embodiment is with the difference of specific embodiment one：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：Present embodiment is with the difference of specific embodiment one：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：Present embodiment is with the difference of specific embodiment one：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：Present embodiment is with the difference of specific embodiment one：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 carries the preparation side of medicine coating in induction of bone growth for a kind of medical pure magnesium surface electrophoretic deposition
Method, is specifically carried out according to the following steps：
First, pure magnesium specimen surface pretreatment：Pending pure magnesium specimen surface is roughly ground with sand paper, is then used successively
Acetone and each ultrasonic 25min of distilled water, are put in hermetic bag after drying up and seal standby；
2nd, micro-arc oxidation electrolyte is configured：Distilled water is fitted in beaker, then sequentially add sodium silicate, potassium hydroxide,
Potassium fluoride and disodiumedetate, a kind of reagent under adding again after being required to stir when often adding a kind of reagent, all
Sonic oscillation is carried out after adding, being completely dissolved to all reagents, micro-arc oxidation electrolyte is obtained；Described differential arc oxidation electricity
The concentration of sodium silicate is 15g/L in solution liquid, and the concentration of potassium hydroxide is 10g/L, and the concentration of potassium fluoride is 8g/L, ethylenediamine tetrem
The concentration of acid disodium is 1g/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 connects surface in step one
The complete pure magnesium sample of pretreatment, it is 50mm to arrange microarc oxidation equipment provided anode cathode separation, is started microarc oxidation equipment provided and super
Sonication instrument, ultrasonic frequency be 400H, differential arc oxidation voltage be 300V, pulsewidth be 50 μ s, pulse frequency be 500Hz and
Dutycycle is ultrasonic microarc oxidation 2min~25min under conditions of 2.5%, closes microarc oxidation equipment provided and supersonic oscillations instrument,
Sample taking-up is clean with distilled water flushing, dry naturally；
4th, post processing：
1. the magnesium sample for step 3 ultrasonic microarc oxidation having been processed is put in the NaOH aqueous solutions of 2mol/L, is subsequently placed in
Temperature is to be incubated 2h in 60 DEG C of water-bath, is dried naturally after being cleaned with water, obtains the magnesium sample of alkali process；
2. configuration concentration is the chitosan solution of 2g/L, is subsequently adding the Chinese Medicines that concentration is 2mg/mL, ultrasound
20min, obtains electrophoresis liquid；The concentration of Chinese medicine is 1mg/mL in described electrophoresis liquid；Step 4 2. described in Chinese Medicines in
Chinese medicine be Cortex Eucommiae chlorogenic acid, solvent is water；Solvent in described chitosan solution is the mixed liquor of water and glacial acetic acid, ice second
The volume ratio of acid and water is 1:100；
3. electrophoresis liquid is placed in stainless steel tank, the magnesium sample of alkali process is placed in electrophoresis liquid, then with alkali process
Magnesium sample be negative pole, stainless steel tank be positive pole, voltage be 20V under conditions of electrophoretic deposition 3min, dry naturally after taking-up, obtain
Medicine coating in induction of bone growth is carried to pure magnesium surface electrophoretic deposition.
Test two：This test carries the preparation side of medicine coating in induction of bone growth for a kind of medical pure magnesium surface electrophoretic deposition
Method：
This test from test one unlike step 4 3. middle voltage be 20V under conditions of electrophoretic deposition 5min, other with
Test one identical.
Test three：This test carries the preparation side of medicine coating in induction of bone growth for a kind of medical pure magnesium surface electrophoretic deposition
Method：
This test and step 4 unlike test one 2. described in Chinese Medicines in Chinese medicine be icariin, solvent
It is dehydrated alcohol, other are identical with test one.
Test four：This test carries the preparation side of medicine coating in induction of bone growth for a kind of medical pure magnesium surface electrophoretic deposition
Method：
This test from test three unlike step 4 3. middle voltage be 20V under conditions of electrophoretic deposition 5min, other with
Test three identical.
Fig. 1 is to test the contact angle pattern that a pure magnesium surface electrophoretic deposition for preparing carries medicine coating in induction of bone growth, Fig. 2
It is to test the contact angle pattern that the two pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth, Fig. 3 is three systems of test
Standby pure magnesium surface electrophoretic deposition carries the contact angle pattern of medicine coating in induction of bone growth, and Fig. 4 is to test the four pure magnesium tables for preparing
Face electrophoretic deposition carries the contact angle pattern of medicine coating in induction of bone growth, and as can be seen from the figure various aftertreatment technologys make material
The angle of wetting on material surface becomes big, i.e., hydrophobicity becomes strong.The drug-carried coat that electrophoretic deposition method is obtained when middle concentration is 1mg/mL
Surface is more uniformly distributed, densification；Middle concentration has a significant impact to the wettability of material.
Test five：This test carries the preparation side of medicine coating in induction of bone growth for a kind of medical pure magnesium surface electrophoretic deposition
Method：
The concentration of Chinese medicine is 0.4mg/mL in this test electrophoresis liquid 2. described from step 4 unlike test one, other
It is identical with test one.
Test six：This test carries the preparation side of medicine coating in induction of bone growth for a kind of medical pure magnesium surface electrophoretic deposition
Method：
This test from test five unlike step 4 3. middle voltage be 10V under conditions of electrophoretic deposition 6min, other with
Test five identical.
Test seven：This test carries the preparation side of medicine coating in induction of bone growth for a kind of medical pure magnesium surface electrophoretic deposition
Method：
This test from test six unlike step 4 3. middle voltage be 10V under conditions of electrophoretic deposition 3min, other with
Test three identical.
Test eight：This test carries the preparation side of medicine coating in induction of bone growth for a kind of medical pure magnesium surface electrophoretic deposition
Method：
This test and step 4 unlike test five 2. described in Chinese Medicines in Chinese medicine be icariin, solvent
It is dehydrated alcohol, other are identical with test seven.
Test nine：This test carries the preparation side of medicine coating in induction of bone growth for a kind of medical pure magnesium surface electrophoretic deposition
Method：
This test from test eight unlike step 4 3. middle voltage be 10V under conditions of electrophoretic deposition 6min, other with
Test three identical.
Test ten：This test carries the preparation side of medicine coating in induction of bone growth for a kind of medical pure magnesium surface electrophoretic deposition
Method：
This test from test nine unlike step 4 3. middle voltage be 10V under conditions of electrophoretic deposition 3min, other with
Test one identical.
Fig. 5 is to test the contact angle pattern that the five pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth, Fig. 6
It is to test the contact angle pattern that the six pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth, Fig. 7 is seven systems of test
Standby pure magnesium surface electrophoretic deposition carries the contact angle pattern of medicine coating in induction of bone growth, and Fig. 8 is to test the eight pure magnesium tables for preparing
Face electrophoretic deposition carries the contact angle pattern of medicine coating in induction of bone growth, and Fig. 9 is to test the nine pure magnesium surface electrophoretic depositions for preparing
The contact angle pattern of medicine coating in induction of bone growth is carried, Figure 10 is to test the ten pure magnesium surface electrophoretic depositions for preparing to carry induction bone life
The contact angle pattern of medicine coating in length, as can be seen from the figure pure magnesium surface electrophoretic deposition carry Cortex Eucommiae chlorogenic acid coating hydrophobicity
It is better, hydrophobic material surface is obtained under the technique of electrophoretic deposition 20V, 3min, angle of wetting is 106.08 degree.
Figure 11 is to test the SEM figures that the five pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth, Tu12Shi
The SEM figures that the six pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth are tested, Figure 13 is the pure of the preparation of test seven
Magnesium surface electrophoretic deposition carries the SEM figures of medicine coating in induction of bone growth, and Figure 14 is to test the eight pure magnesium surface electrophoretic depositions for preparing
The SEM figures of medicine coating in induction of bone growth are carried, Figure 15 is to test the nine pure magnesium surface electrophoretic depositions for preparing to carry in induction of bone growth
The SEM figures of medicine coating, Figure 16 is to test the SEM figures that the ten pure magnesium surface electrophoretic depositions for preparing carry medicine coating in induction of bone growth,
It can be seen that when electrophoretic deposition voltage is 20V, 3min coating sealing of hole preferably, sees once in a while tiny hole；In
The species of medicine also has a significant impact to the effect of sealing of hole, and the green untouched hole effect of the Cortex Eucommiae is better than excessive sheep under same preparation process condition
The sealing of hole effect of icariin.
Test 11：This test be contrast test, a kind of preparation method of medical pure magnesium surface electrophoretic deposition coating, specifically
For：
First, pure magnesium specimen surface pretreatment：Pending pure magnesium specimen surface is roughly ground with sand paper, is then used successively
Acetone and each ultrasonic 25min of distilled water, are put in hermetic bag after drying up and seal standby；
2nd, micro-arc oxidation electrolyte is configured：Distilled water is fitted in beaker, then sequentially add sodium silicate, potassium hydroxide,
Potassium fluoride and disodiumedetate, a kind of reagent under adding again after being required to stir when often adding a kind of reagent, all
Sonic oscillation is carried out after adding, being completely dissolved to all reagents, micro-arc oxidation electrolyte is obtained；Described differential arc oxidation electricity
The concentration of sodium silicate is 15g/L in solution liquid, and the concentration of potassium hydroxide is 10g/L, and the concentration of potassium fluoride is 8g/L, ethylenediamine tetrem
The concentration of acid disodium is 1g/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 connects surface in step one
The complete pure magnesium sample of pretreatment, it is 50mm to arrange microarc oxidation equipment provided anode cathode separation, is started microarc oxidation equipment provided and super
Sonication instrument, ultrasonic frequency be 400H, differential arc oxidation voltage be 300V, pulsewidth be 50 μ s, pulse frequency be 500Hz and
Dutycycle is ultrasonic microarc oxidation 2min~25min under conditions of 2.5%, closes microarc oxidation equipment provided and supersonic oscillations instrument,
Sample taking-up is clean with distilled water flushing, dry naturally；
4th, post processing：
1. the magnesium sample for step 3 ultrasonic microarc oxidation having been processed is put in the NaOH aqueous solutions of 2mol/L, is subsequently placed in
Temperature is to be incubated 2h in 60 DEG C of water-bath, is dried naturally after being cleaned with water, obtains the magnesium sample of alkali process；
2. configuration concentration is the chitosan aqueous solution of 2g/L as electrophoresis liquid；Solvent in described chitosan solution is water
It is 1 with the volume ratio of the mixed liquor of glacial acetic acid, glacial acetic acid and water:100；
3. electrophoresis liquid is placed in stainless steel tank, the magnesium sample of alkali process is placed in electrophoresis liquid, then with alkali process
Magnesium sample be negative pole, stainless steel tank be positive pole, voltage be 20V under conditions of electrophoretic deposition 3min, dry naturally after taking-up, obtain
To pure magnesium surface electrophoretic deposition coating.
Figure 17 is to test the 11 pure magnesium surface electrophoretic deposition coatings for preparing to colibacillary fungistatic effect figure, Tu18Shi
Medicine coating is to colibacillary fungistatic effect figure, Tu19Shi in pure magnesium surface electrophoretic deposition load induction of bone growth prepared by test five
Medicine coating is to colibacillary fungistatic effect figure, Tu20Shi in pure magnesium surface electrophoretic deposition load induction of bone growth prepared by test six
Medicine coating is to colibacillary fungistatic effect figure, Tu21Shi in pure magnesium surface electrophoretic deposition load induction of bone growth prepared by test seven
Medicine coating is to colibacillary fungistatic effect figure, Tu22Shi in pure magnesium surface electrophoretic deposition load induction of bone growth prepared by test eight
Medicine coating is to colibacillary fungistatic effect figure, Tu23Shi in pure magnesium surface electrophoretic deposition load induction of bone growth prepared by test nine
Test ten prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to colibacillary fungistatic effect figure, from figure
As can be seen that medicine coating improves material to colibacillary fungistatic effect in carrying, bacteriostasis rate is reached from 84%~92%, is embodied
Introduce the fungistatic effect after Chinese medicine.
Figure 24 is the fungistatic effect figure for testing the 11 pure magnesium surface electrophoretic deposition coatings for preparing to staphylococcus aureuses,
Figure 25 be test five prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to the antibacterial of staphylococcus aureuses
Design sketch, Figure 26 be test six prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to staphylococcus aureuses
Fungistatic effect figure, Figure 27 be test seven prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to golden yellow Portugal
The fungistatic effect figure of grape coccus, Figure 28 be test eight prepare pure magnesium surface electrophoretic depositions carry induction of bone growth in medicine coating to gold
The fungistatic effect figure of Staphylococcus aureus, Figure 29 is to test the nine pure magnesium surface electrophoretic depositions for preparing to carry the painting of induction of bone growth Chinese medicine
Fungistatic effect figure of the layer to staphylococcus aureuses, Figure 30 is to test the ten pure magnesium surface electrophoretic depositions for preparing to carry induction of bone growth
Fungistatic effect figure of the middle medicine coating to staphylococcus aureuses, it can be seen that carrying Chinese medicine extract coating improves material
Fungistatic effect of the material to staphylococcus aureuses, bacteriostasis rate is reached from 97%~98%, after embodying introducing Chinese medicine extract
Fungistatic effect.
Claims (6)
1. a kind of medical pure magnesium surface electrophoretic deposition carries the preparation method of medicine coating in induction of bone growth, it is characterised in that medical pure
Magnesium surface electrophoretic deposition carries the preparation method of medicine coating in induction of bone growth and carries out according to the following steps：
First, pure magnesium specimen surface pretreatment：Pending pure magnesium specimen surface is roughly ground with sand paper, acetone is then used successively
Ultrasonic 25min each with distilled water, is put in hermetic bag after drying up and seals standby；
2nd, micro-arc oxidation electrolyte is configured：Distilled water is fitted in beaker, sodium silicate, potassium hydroxide, fluorination is then sequentially added
Potassium and disodiumedetate, a kind of reagent under adding again after being required to stir when often adding a kind of reagent, all add
After carry out sonic oscillation, being completely dissolved to all reagents, obtain micro-arc oxidation electrolyte；Described micro-arc oxidation electrolyte
The concentration of middle sodium silicate is 15g/L~20g/L, and the concentration of potassium hydroxide is 10g/L~20g/L, and the concentration of potassium fluoride is 8g/L
~20g/L, the concentration of disodiumedetate is 1g/L~10g/L；
3rd, ultrasonic microarc oxidation is processed：Micro-arc oxidation electrolyte prepared by step 2 is put in electrolysis bath, then by electrolysis bath
In transferring supersonic oscillations instrument, microarc oxidation equipment provided negative electrode connects stainless steel electrolytic groove, and anode connects surface in step one and locates in advance
The pure magnesium sample managed, 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 40KHz~60KHz, differential arc oxidation voltage be 200V~400V, pulsewidth be 40 μ s~
60 μ s, pulse frequency are 400Hz~700Hz and dutycycle is ultrasonic microarc oxidation 5min~20min 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. in the NaOH aqueous solutions of 1mol/L~3mol/L, then the magnesium sample for step 3 ultrasonic microarc oxidation having been processed is put into
Insulation 1h~2h in the water-bath that temperature is 60 DEG C~80 DEG C is placed in, is dried naturally after being cleaned with water, obtain the magnesium sample of alkali process；
2. configuration concentration is the chitosan solution of 1g/L~3g/L, is subsequently adding the Chinese Medicines that concentration is 2mg/mL, ultrasound
10min~30min, obtains electrophoresis liquid；The concentration of Chinese medicine is 0.4mg/mL~1.9mg/mL in described electrophoresis liquid；Described shell
It is 1 that solvent in polysaccharide solution is the volume ratio of the mixed liquor of water and glacial acetic acid, glacial acetic acid and water:100；
3. electrophoresis liquid is placed in stainless steel tank, the magnesium sample of alkali process is placed in electrophoresis liquid, then with the magnesium of alkali process
Sample is negative pole, and stainless steel tank is positive pole, and voltage is electrophoretic deposition 3min~6min under conditions of 10V~20V, natural after taking-up
Dry, obtain pure magnesium surface electrophoretic deposition and carry medicine coating in induction of bone growth.
2. a kind of medical pure magnesium surface electrophoretic deposition according to claim 1 carries the preparation side of medicine coating in induction of bone growth
Method, it is characterised in that the concentration of sodium silicate is 15g/L in the micro-arc oxidation electrolyte described in step 2, the concentration of potassium hydroxide
It is 10g/L, the concentration of potassium fluoride is 8g/L, and the concentration of disodiumedetate is 1g/L.
3. a kind of medical pure magnesium surface electrophoretic deposition according to claim 1 carries the preparation side of medicine coating in induction of bone growth
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. a kind of medical pure magnesium surface electrophoretic deposition according to claim 1 carries the preparation side of medicine coating in induction of bone growth
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. a kind of medical pure magnesium surface electrophoretic deposition according to claim 1 carries the preparation side of medicine coating in induction of bone growth
Method, it is characterised in that step 4 2. described in Chinese Medicines in Chinese medicine be icariin, solvent is dehydrated alcohol.
6. a kind of medical pure magnesium surface electrophoretic deposition according to claim 1 carries the preparation side of medicine coating in induction of bone growth
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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