CN110241453A - A kind of release fluoride and the degradable kirsite bone nail of cerium and preparation method thereof - Google Patents
A kind of release fluoride and the degradable kirsite bone nail of cerium and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B17/00—Surgical instruments, devices or methods, e.g. tourniquets
- A61B17/56—Surgical instruments or methods for treatment of bones or joints; Devices specially adapted therefor
- A61B17/58—Surgical instruments or methods for treatment of bones or joints; Devices specially adapted therefor for osteosynthesis, e.g. bone plates, screws, setting implements or the like
- A61B17/68—Internal fixation devices, including fasteners and spinal fixators, even if a part thereof projects from the skin
- A61B17/84—Fasteners therefor or fasteners being internal fixation devices
- A61B17/86—Pins or screws or threaded wires; nuts therefor
- A61B17/866—Material or manufacture
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- C—CHEMISTRY; METALLURGY
- 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
- C25D11/02—Anodisation
- C25D11/024—Anodisation under pulsed or modulated current or potential
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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- 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
- C25D11/02—Anodisation
- C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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Abstract
The present invention is a kind of release fluoride and degradable kirsite bone nail of cerium and preparation method thereof, and this bone nail is that matrix and load are made of the Zinc oxide coating of Trace Fluoride and cerium by kirsite.The Zinc oxide coating with Trace Fluoride and cerium constructs in conjunction with metal base surface, by differential arc oxidization technique in kirsite matrix surface, and degradation rate is controllable in human body, has the function of antibacterial anti-inflammatory and promotes damaged bony tissues restoration and reconstruction.The ion motion and electrochemical action that Trace Element Fluorine and cerium are generated by differential arc oxidation electric field are doped.The method of preparation are as follows: selection kirsite is processed into the effigurate bone nail of tool first；Then it is used to matrix degradation rate in its surface building Zinc oxide coating using differential arc oxidization technique；It adds the soluble-salt containing fluorine element and Ce elements in the electrolytic solution simultaneously and carries out microelement doping using electric field caused by differential arc oxidation.
Description
Technical field
The present invention relates to it is a kind of with antibacterial anti-inflammatory and promote the release fluoride of bone tissue restoration and reconstruction effect, cerium it is degradable
The controllable building of kirsite bone nail and preparation method thereof, especially Zinc oxide coating and tool antibacterial anti-inflammatory ability and rush bone are again
The microelement doping of raw ability belongs to human body hard tissue implantation Material Field.
Background technique
Bone nail be Orthopedic Clinical commonly a kind of bone tissue reparation, correction orthopaedics implant.Common bone nail prepares material
Material includes cochrome, titanium alloy, stainless steel and magnesium alloy.Wherein, the non-degradable material that cochrome, titanium alloy etc. one arranges
Expect the influence acted on due to rejection, is unable in long-term existence human body.Patient need to carry out second operation, increase pain and infection wind
Danger.Degradable magnesium alloy materials can effectively avoid the above problem.However, causing such since its own corrosion potential is excessively high
Material life cycle in human body is too short, often rebuilds prior to tissue and completes to crumble with regard to degradation.In addition, magnesium alloy was degraded
Cheng Zhongchang is discharged with hydrogen, to induce inflammation and inhibit sticking and growing for implant surfaces osteoblast.
Zinc has the corrosion potential lower than magnesium, and degradation rate can more match body bone tissue restoration and reconstruction.In addition, Chinese
Zinc is mentioned in patent CN201810243999 to be largely present in human body, human tolerance is good, can promote bone cell differentiation and
Mineralising enhances the absorption of osteoblast in bone and osteoblast is promoted to express.But the mechanical property of pure zinc is not good enough, is unable to satisfy
The requirement of damaged bony tissues restoration and reconstruction, this problem can be solved perfectly by carrying out alloying to it.For example, Zn-(2 ~ 4at%) Li conjunction
Gold is keeping about 14% elongation percentage to can provide the tensile strength close to 400MPa simultaneously, can effectively meet the mechanical property of bone nail
It is required that.In addition, the corrosion of zinc-containing alloy is homogeneous corrosion, material caused by avoidable local corrosion is excessive crumbles.Therefore, zinc closes
Gold is a kind of bone nail having a high potential.
Biocompatibility can be improved in zinc alloy surface building coating and control matrix corrosion rate.Differential arc oxidization technique can
Oxide ceramic coating is constructed on valve metal surface, has been widely used in the building of the medical metals surface covering such as titanium, magnesium at present.Cause
This, this technology also has broad prospects in the related fields of medical zinc alloy surface building high bioactivity coating.
In micro-arc oxidation process, material surface will form the electric field of similar anodic oxidation, facilitate ion transport and chemistry
Reaction.It therefore, can be while constructing coating by adding the soluble-salt containing microelement in micro-arc oxidation electrolyte
Microelement doping is carried out, to further increase its surface bioactive.
Zinc oxide has good biocompatibility, and human absorptivity is high, participates in the formation of nucleic acid and nucleoprotein, participates in
The energetic supersession of cell enhances sticking and expressing for osteoblast.In addition, zinc oxide participates in generating oxidation activity also in body
Substance can decompose microorganism constituent, have antibacterial action, help organized renewing, improve matrix oxidation resistance.
Fluorine and cerium are the necessary microelement of human body, have important physiological function and and extensive pharmacological action.China
Fluorine element is mentioned in patent CN201610127249 to promote apatite raw by carrying out ion exchange with bone salts crystal surface
It is long, to improve bone tissue reparation ability.Mentioned in Chinese patent CN201010017104 Ce elements have inhibit bacterial growth,
The effects of mitigating inflammatory reaction, will mitigate the inflammatory reaction at implant implantation initial stage, be implanted to power to improve.
Huge life is shown doped with the Zinc oxide coating of fluorine, cerium in zinc alloy surface preparation using differential arc oxidization technique
Object medicine potentiality.Coating feature can be changed by adjusting micro-arc oxidation process parameter, be finally reached regulation kirsite implant and exist
The controllable purpose of degradation rate in human body environment；Meanwhile fluorine, the Ce elements being sustained in degradation process antibacterial anti-inflammatory and can promote to plant
Enter body bone tissue restoration and reconstruction nearby.In consideration of it, drawing the invention.
Summary of the invention
The purpose of the present invention is being directed to the above-mentioned deficiency of human body bone nail, propose that a kind of surface has controllable matrix degradation speed
Rate, energy slowly releasing trace element fluorine and cerium are with antibacterial anti-inflammatory and promote bone cell differentiation and mineralising, the suction for enhancing osteoblast in bone
It is attached and promote osteoblast to express and help the bone nail and its differential arc oxidation preparation method of damaged bony tissues restoration and reconstruction.
Release fluoride, cerium degradable kirsite bone nail metal base surface have one layer using differential of the arc technology obtain having
Antibacterial anti-inflammatory and promote bone tissue restoration and reconstruction and can be to the Zinc oxide coating that matrix degradation rate is regulated and controled, surface utilizes
Micro-arc oxidation process mixes micro functional elements fluorine and cerium.Zinc oxide coating is generated in micro-arc oxidation process, it is micro- by adjusting
Arc oxidation technology parameter change coating feature regulates and controls degradation rate of the implant in human body environment.Matrix can be improved in Zn-ef ficiency
The metabolic function of surface peripheral cell promotes bone cell differentiation and mineralising, enhances the absorption and promotion of osteoblast in bone
Osteoblast expression.Fluorine element can promote apatite to grow, and improve matrix biocompatibility.Cerium has the work of antibacterial growth anti-inflammatory
With, can mitigate implant implantation initial stage inflammatory reaction, thus improve be implanted to power.
The present invention is realized by the following technical programs:
The degradable kirsite bone nail of the release fluoride and cerium is by kirsite matrix and using differential arc oxidization technique in its table
What face obtained forms doped with the Zinc oxide coating of Trace Fluoride and cerium.In the bone nail of this Trace Element Fluorine and cerium slow-release function
Metal base surface has one layer of antibacterial anti-inflammatory and promotes the Zinc oxide coating of damaged bony tissues restoration and reconstruction.The zinc oxide applies
Layer carries out differential arc oxidation generation by kirsite matrix surface in conjunction with metal base surface in specific electrolyte system；Institute
The fluorine element and Ce elements stated by add soluble villiaumite in electrolyte system and cerium salt using differential of the arc process generate from
Son movement and electrochemical reaction are doped in surface.
Preparation method includes the following steps:
(1) kirsite is selected to be processed into bone nail；
(2) provide it is a kind of include fluorine ion and cerium ion special electrolytic solutions；
(3) bone nail surface polishing, using bone nail as anode in above-mentioned specific electrolyte, stainless steel is cathode, using double
Pole pulse is microarc oxidation equipment provided to carry out differential arc oxidation to bone nail, constructs Zinc oxide coating in bone nail matrix surface；It is sharp at the same time
Fluorine element in electrolyte system and Ce elements are doped in zinc oxide by the ion motion and electrochemical reaction generated with differential of the arc process
In coating, its surface is made to form microelement doping；
(4) after eluting above-mentioned bone nail taking-up with deionized water, vacuum drying, Preservation in sterile condition after disinfection is spare, and can be obtained can delay
Release the degradable kirsite bone nail of fluorine and cerium.
Further, the step (2) include fluorine ion and cerium ion specific electrolyte solution, comprising as follows at
Point: the Na of 2 ~ 50g/L2CO3/Na3PO4/Na2SiO3Electrolyte system, 0.1 ~ 10mmol/L of soluble fluoride salinity, soluble cerium
Salinity is 0.1 ~ 10mmol/L, and additive is the KOH of 0.5 ~ 5g/L；The working method of the differential arc oxidation of the step (3) is
Constant voltage mode.
Further, the step (3) is microarc oxidation equipment provided to bone nail progress differential arc oxidation using bipolar pulse, can be into one
Step reaches final adjustment bone by control micro-arc oxidation process parameter to regulate and control the features such as coating layer thickness, microscopic appearance, phase composition
Follow closely matrix degradation rate purpose, the micro-arc oxidation process parameter are as follows: operating voltage regulation range be forward voltage 200 ~
0 ~ 300V of 1000V and negative voltage, pulse frequency adjustable range are direct impulse 50Hz ~ 1000Hz and negative-going pulse frequency 50Hz
~ 1000Hz, duty ratio are forward direction 4% ~ 50% and negative sense 4% ~ 50%, 0.5 ~ 10min of reaction time.
The utility model has the advantages that
(1) bone nail that the present invention addresses meets the mechanical property requirements of orthopaedics implantation, constructs Zinc oxide coating on its surface, passes through
Micro-arc oxidation process parameter change coating feature is adjusted, degradation rate of the kirsite implant in human body environment, matching are regulated and controled
The restoration and reconstruction of different degrees of damaged bony tissues.With the restoration and reconstruction of body bone tissue, bone nail is gradually degraded in vivo.
(2) the bone nail surface that the present invention addresses, which is negative, is loaded with the Zinc oxide coating of Trace Element Fluorine and cerium.Coating has good
Good biocompatibility, surrounding osteoblast sticking and express in implant surfaces can be enhanced by being implanted into after human body.Two kinds of fluorine, cerium
Element is sustained with matrix in the intracorporal degradation of people, is had implantation antibacterial anti-inflammatory early period and is promoted bone cell differentiation, mine for a long time
The benefit of change is used.
Detailed description of the invention
Fig. 1 is that the scanning electron microscope of the surface covering of the zinc oxide bone nail of energy release fluoride and cerium prepared in embodiment 1 is shone
Piece.
Fig. 2 is the power spectrum of the surface covering of the zinc oxide bone nail of energy release fluoride and cerium prepared in embodiment 1.
Fig. 3 is that the thickness measure of the surface covering of the zinc oxide bone nail of energy release fluoride and cerium prepared in embodiment 1 is shone
Piece.
Specific example mode
Embodiment 1
(1) pure zinc is selected to be processed into bone nail first；
(2) bone nail pre-processes: by bone nail using label be followed successively by the abrasive paper for metallograph of 600#, 800#, 1000# by coarse sand to fine sand by
Grade sanding and polishing, then with acetone, dehydrated alcohol, deionized water ultrasonic cleaning, dried for standby；
(3) addition of the configuration of electrolyte and fluorine, Ce elements: sodium carbonate liquor system is used, it is 20g/L that configuration 4L, which contains concentration,
Sodium carbonate liquor and 1g/L potassium hydroxide solution；Then the sodium fluoride of 1mmol/L and the cerous nitrate of 0.5mmol/L is added,
Stirring at normal temperature dissolution, for use；
(4) differential arc oxidation of bone nail: bone nail is placed in the microarc oxidation equipment provided electrolytic cell of bipolar pulse and is added configured
Electrolyte, using bone nail as anode, stainless steel electrolytic cell is cathode, adjusts technological parameter and carries out differential arc oxidation to it.Technological parameter
Are as follows: constant voltage mode, operating voltage regulation range forward voltage 500V, negative voltage 0V, pulse frequency adjustable range direct impulse
600Hz, negative-going pulse frequency 0Hz, duty ratio forward direction 12%, negative sense 0%, reaction time 5min；
(5) after eluting above-mentioned bone nail taking-up with deionized water, dry, Preservation in sterile condition after disinfection is spare, can obtain of the invention anti-
Bacterium anti-inflammatory and the bone nail for promoting bone tissue restoration and reconstruction.
Fig. 1 is the stereoscan photograph of the surface covering of the zinc oxide bone nail of energy release fluoride prepared by this example and cerium.
On its surface, the Zinc oxide coating of building adjusts micro-arc oxidation process parameter change coating surface for regulating and controlling matrix degradation rate
Feature realizes implant controlled degradation in human body environment.
Fig. 2 is the power spectrum of the surface covering of the zinc oxide bone nail of energy release fluoride prepared by this example and cerium.Microelement
Fluorine and cerium have successfully been adulterated on the Zinc oxide coating of building by differential arc oxidation, are delayed with matrix in the intracorporal degradation of people
It releases, there is implantation antibacterial anti-inflammatory early period and the benefit of bone cell differentiation, mineralising is promoted to use for a long time.
Fig. 3 is the thickness measure photo of the surface covering of the zinc oxide bone nail of energy release fluoride prepared by this example and cerium.
Micro-arc oxidation process parameter change coating layer thickness is adjusted, realizes implant controlled degradation in human body environment.
Embodiment 2
(1) pure zinc is selected to be processed into bone nail first；
(2) bone nail pre-processes: by bone nail using label be followed successively by the abrasive paper for metallograph of 600#, 800#, 1000# by coarse sand to fine sand by
Grade sanding and polishing, then with acetone, dehydrated alcohol, deionized water ultrasonic cleaning, dried for standby；
(3) addition of the configuration of electrolyte and fluorine, Ce elements: sodium carbonate liquor system is used, it is 20g/ that configuration 10L, which contains concentration,
The sodium carbonate liquor of L and the potassium hydroxide solution of 1g/L；Then the sodium fluoride of 1mmol/L and the cerous nitrate of 1mmol/L is added, often
Warm stirring and dissolving, for use；
(4) differential arc oxidation of bone nail: bone nail is placed in the microarc oxidation equipment provided electrolytic cell of bipolar pulse and is added configured
Electrolyte, using bone nail as anode, stainless steel electrolytic cell is cathode, adjusts technological parameter and carries out differential arc oxidation to it.Technological parameter
Are as follows: constant voltage mode, operating voltage regulation range forward voltage 500V, negative voltage 0V, pulse frequency adjustable range direct impulse
600Hz, negative-going pulse frequency 0Hz, duty ratio forward direction 12%, negative sense 0%, reaction time 3min；
(5) after eluting above-mentioned bone nail taking-up with deionized water, dry, Preservation in sterile condition after disinfection is spare, can obtain of the invention anti-
Bacterium anti-inflammatory and the bone nail for promoting bone tissue restoration and reconstruction.
Embodiment 3
(1) pure zinc is selected to be processed into bone nail first；
(2) bone nail pre-processes: by bone nail using label be followed successively by the abrasive paper for metallograph of 600#, 800#, 1000# by coarse sand to fine sand by
Grade sanding and polishing, then with acetone, dehydrated alcohol, deionized water ultrasonic cleaning, dried for standby；
(3) addition of the configuration of electrolyte and fluorine, Ce elements: sodium carbonate liquor system is used, it is 20g/ that configuration 10L, which contains concentration,
The sodium carbonate liquor of L and the potassium hydroxide solution of 1g/L；Then the sodium fluoride of 2mmol/L and the cerous nitrate of 2mmol/L is added, often
Warm stirring and dissolving, for use；
(4) differential arc oxidation of bone nail: bone nail is placed in the microarc oxidation equipment provided electrolytic cell of bipolar pulse and is added configured
Electrolyte, using bone nail as anode, stainless steel electrolytic cell is cathode, adjusts technological parameter and carries out differential arc oxidation to it.Technological parameter
Are as follows: constant voltage mode, operating voltage regulation range forward voltage 600V, negative voltage 0V, pulse frequency adjustable range direct impulse
60Hz, negative-going pulse frequency 0Hz, duty ratio forward direction 20%, negative sense 0%, reaction time 5min；
(5) after eluting above-mentioned bone nail taking-up with deionized water, dry, Preservation in sterile condition after disinfection is spare, can obtain of the invention anti-
Bacterium anti-inflammatory and the bone nail for promoting bone tissue restoration and reconstruction.
Obviously, the above embodiment of the present invention is just for the sake of clearly illustrating examples made by the present invention, and being not is pair
The restriction of embodiments of the present invention.It for those of ordinary skill in the art, can also be on the basis of the above description
It makes other variations or changes in different ways, there is no need and unable to be exhaustive to all embodiments, and these belong to
Spiritual changes and variations that derived from of the invention are still in protection scope of the present invention.
Claims (3)
1. a kind of release fluoride and the degradable kirsite bone nail of cerium and preparation method thereof, which is characterized in that the release fluoride and
The degradable kirsite bone nail of cerium by kirsite matrix and using differential arc oxidization technique its surface obtain doped with micro
The Zinc oxide coating of fluorine and cerium composition；The preparation method of the degradable kirsite bone nail of the release fluoride and cerium, including it is as follows
Step:
(1) kirsite is selected to be processed into bone nail；
(2) provide it is a kind of include fluorine ion and cerium ion special electrolytic solutions；
(3) bone nail surface polishing, using bone nail as anode in above-mentioned specific electrolyte, stainless steel is cathode, using double
Pole pulse is microarc oxidation equipment provided to carry out differential arc oxidation to bone nail, constructs Zinc oxide coating in bone nail matrix surface；It is sharp at the same time
Fluorine element in electrolyte system and Ce elements are doped in zinc oxide by the ion motion and electrochemical reaction generated with differential of the arc process
In coating, its surface is made to form microelement doping；
(4) after eluting above-mentioned bone nail taking-up with deionized water, vacuum drying, Preservation in sterile condition after disinfection is spare, and can be obtained can delay
Release the degradable kirsite bone nail of fluorine and cerium.
2. release fluoride according to claim 1 and the degradable kirsite bone nail of cerium and preparation method thereof, which is characterized in that
The step (2) include fluorine ion and cerium ion specific electrolyte solution, include following ingredient: 2 ~ 50g/L's
Na2CO3/Na3PO4/Na2SiO3Electrolyte system, 0.1 ~ 10mmol/L of soluble fluoride salinity, soluble cerium salt concentration be 0.1 ~
10mmol/L, additive are the KOH of 0.5 ~ 5g/L；The working method of the differential arc oxidation of the step (3) is constant voltage mode.
3. release fluoride according to claim 1 and the degradable kirsite bone nail of cerium and preparation method thereof, which is characterized in that
The step (3) carries out differential arc oxidation to bone nail using bipolar pulse is microarc oxidation equipment provided, can further pass through the control differential of the arc
Oxidation technology parameter reaches final adjustment bone nail matrix degradation rate to regulate and control the features such as coating layer thickness, microscopic appearance, phase composition
Purpose, the micro-arc oxidation process parameter are as follows: operating voltage regulation range be 200 ~ 1000V of forward voltage and negative voltage
0 ~ 300V, pulse frequency adjustable range are direct impulse 50Hz ~ 1000Hz and negative-going pulse frequency 50Hz ~ 1000Hz, duty ratio
For forward direction 4% ~ 50% and negative sense 4% ~ 50%, 0.5 ~ 10min of reaction time.
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| CN114921833A (en) * | 2022-06-13 | 2022-08-19 | 苏州大学 | Medical pure zinc material and preparation method and application thereof |
| CN116850342A (en) * | 2023-06-09 | 2023-10-10 | 北京尚宁科智医疗器械有限公司 | Zinc plate with belt loop |
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