CN106913905A - A kind of anti-degraded and the good ceria doping calcium silicates coating of anti-microbial property and its preparation method and application - Google Patents
A kind of anti-degraded and the good ceria doping calcium silicates coating of anti-microbial property and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to good ceria doping calcium silicates coating of a kind of anti-degraded and anti-microbial property and its preparation method and application, the ceria doping calcium silicates coating is sprayed on substrate surface and is formed by the calcium silicates original washing powder body that ceria adulterates by plasma spray technology.The present invention can assign material preferable antibacterial activity by the appropriate ceria that adulterates.The biological coating that the present invention is provided, not only with excellent bioactivity and biocompatibility, and with anti-degradability and antibiotic property, solves the defect problem in the presence of prior art, promotes the reparation of sclerous tissues and the development in alternate material field.
Description
Technical field
The present invention relates to the good ceria doping calcium silicates coating and preparation method thereof of a kind of anti-degraded and anti-microbial property and
Using being to be related to a kind of using plasma spraying technology to be sprayed at the two of the metallic substrate surfaces such as pure titanium, titanium alloy specifically
Calcium silicates base coating of cerium oxide-doped and its preparation method and application, belongs to medical bio coating technology field.
Background technology
Causing the main cause of operative failure in the operation of orthopaedics implant includes synosteosis energy between implant and adjacent bone tissue
The performances such as power is poor, implant and bone tissue mechanics mismatch and operation in the implant infection that triggers etc..Wherein it is implanted into body-sensing
Dye for one of problem most severe in orthopaedics implant surgery.According to the literature, fracture fixation, joint replacement, femur and knee
Implant infection rate in joint repair operation respectively reaches 2%, 5%, 14%, and the related infection of implant is postoperative more to patient
Conjunction brings great inconvenience.For the infection for preventing implant related, comparatively ideal method is implant is possessed anti-sense in itself
Dye ability.Therefore, the coating for preparing antibacterial on implant material surface gets the attention.
Titanium and titanium alloy etc. are clinically conventional bone implant materials, are prepared on its surface using plasma spray process
Calcium silicates coating can assign its good biocompatibility, strengthen itself combination and between bone tissue.Calcium silicates coating material is in body
Good bioactivity, biocompatibility are shown in outer experiment, and it is higher with metal base bond strength；Animal in vivo
The coating has the ability of induction ostosis in experiment, has stronger binding ability with bone tissue.But, coating is in life
Degradation speed under reason body fluid corrodes is too fast, and its long-term stability can have much room for improvement；And coating does not have antibiotic property, postoperative anti-sense
Dye ability is poor.
In sum, study it is a kind of not only there is excellent bioactivity and biocompatibility, and with anti-degradability and
The biological coating of antibiotic property, to promoting the reparation of sclerous tissues and the development in alternate material field, will have far-reaching significance.
The content of the invention
The present invention is in order to solve the defect problem in the presence of prior art, there is provided a kind of not only to have excellent bioactivity
And biocompatibility, and the biological coating with anti-degradability and antibiotic property and preparation method thereof.
It is described it is an object of the invention to provide the good ceria doping calcium silicates coating of a kind of anti-degraded and anti-microbial property
Ceria doping calcium silicates coating is sprayed on base material by the calcium silicates original washing powder body that ceria adulterates by plasma spray technology
Surface is formed.
Biological coating of the invention has obvious antibacterial effect to staphylococcus aureus, Escherichia coli, and antibiotic rate reaches
More than 99%；And the mass area ratio after being soaked 21 days in the solution equivalent to human physiological environment is lost less than 5
mg/cm2, with good anti-degradability, can be used as reparation and the alternate material of sclerous tissues.Rare-Earth Ce ion has preferable
Antibacterial activity, have stronger killing effect to gram-positive bacteria and negative bacterium, the present invention is by appropriate titanium dioxide of adulterating
Cerium, can assign material preferable antibacterial activity.The biological coating that the present invention is provided, not only with excellent bioactivity and life
Thing compatibility, and with anti-degradability and antibiotic property, the defect problem in the presence of prior art is solved, promote hard group
The reparation and the development in alternate material field knitted.
Used as a kind of preferred scheme, the mass fraction of ceria is in the calcium silicates original washing powder body of the ceria doping
10~50%, excessive ceria doping can cause more cerium ion to discharge, and easily cause cytotoxicity, and doping is very few
Antibacterial effect and chemical stability can be caused to improve unobvious.Described powder is by particle group that particle diameter is 10~200 microns
Into the particle in the size range has enough mobility, is conducive to being deposited on matrix surface, improves the bond strength of coating.
The mass fraction of ceria is 15~30% in the calcium silicates original washing powder body of more preferably described ceria doping.
Used as a kind of preferred scheme, the base material is pure titanium, titanium alloy, stainless steel or cobalt chrome molybdenum (CoCrMo) alloy.
Such material can provide preferable intensity, toughness and excellent processing characteristics.
It is a further object to provide a kind of preparation method of the ceria doping calcium silicates coating, the system
Preparation Method includes：As raw material, using plasma spraying technology sprays the raw material to calcium silicates original washing powder body with ceria doping
The substrate surface after surface treated is coated in, the ceria doping calcium silicates coating is obtained.
Preparation method using plasma spraying coating process of the invention, the calcium silicates original washing powder body spraying that the ceria is adulterated
Substrate surface after to treatment is obtained described coating, with simple to operate, efficiency high, favorable repeatability, is adapted to scale metaplasia
The advantages of product.
Used as a kind of preferred scheme, the calcium silicates original washing powder body of the ceria doping is obtained by solid sintering technology, specific bag
Include：According to 10~50：25~45：42~75 mass ratio mixes ceria powder, silicon-dioxide powdery, calcium carbonate powder
Ball milling, mixed powder is obtained after being incubated 1~3 hour in 1100~1450 DEG C, will obtain described after mixed powder sieving, drying
The calcium silicates original washing powder body of ceria doping.
Used as a kind of preferred scheme, the condition of plasma spray coating process is as follows：Plasma gas Ar flows are 30~50
slpm；Plasma gas H2Flow is 6~18slpm；Powder carrier gas Ar flows are 1.5~5slpm；Spray distance is
80~330 millimeters；Spray power is 30~55 kilowatts；Powder feeding rate is 8.0~30 gram/minutes.Described slpm is index
Accurate liter/min.Suitable process conditions are selected, can be carried while the bioactivity and biocompatibility of biological coating is ensured
Bond strength between matrix high and coating.
Used as a kind of preferred scheme, the base material is pure titanium, titanium alloy, stainless steel or vitallium.The surface of base material
Treatment, refers to after substrate surface is processed through sandblasting or sand papering, to be obtained, the pressure of blasting treatment through being cleaned by ultrasonic, drying
Preferably 0.1~0.8MPa.So, the bond strength of coating and matrix can be improved.
Repairing for sclerous tissues is being prepared the present invention also aims to provide a kind of ceria doping calcium silicates coating
Application in multiple and alternate material.Biological coating of the invention not only has excellent bioactivity and biocompatibility, and tool
There are anti-degradability and antibiotic property, solve the defect problem in the presence of prior art, promote the reparation of sclerous tissues and replace material
The development in material field.
Brief description of the drawings
Fig. 1 is XRD spectrum of the calcium silicates original washing powder body of the ceria of embodiment 1 doping before and after coating is formed, in figure：
A collection of illustrative plates is the XRD spectrum to form the powder before coating；B collection of illustrative plates is the XRD spectrum to form the coating after coating；
Fig. 2 is the stereoscan photograph of the coating of embodiment 1；
Fig. 3 is the calcium silicates base coating and CaSiO of the ceria of embodiment 1 doping3Immersion of the coating in Tris-HCl cushioning liquid
The relation curve compares figure that time loses with coating unit area quality, in figure：A curves are CaSiO3Coating is in Tris-HCl
The relation curve that soak time in cushioning liquid is lost with coating unit area quality；B curves are that ceria of the invention is mixed
The relation curve that soak time of the miscellaneous calcium silicates base coating in Tris-HCl cushioning liquid is lost with coating unit area quality；
Fig. 4 is the antibacterial effect figure of the calcium silicates base coating to staphylococcus aureus of the ceria of embodiment 1 doping, in figure：A shines
It is in piece and the visible bacterium after Ti-6Al-4V effects 24h；B photos are that the calcium silicates base coating adulterated with ceria is acted on
Visible bacterium after 24h；
Fig. 5 is the antibacterial effect figure of the calcium silicates base coating to Escherichia coli of the ceria of embodiment 1 doping.In figure：It is in a photos
With the visible bacterium after Ti-6Al-4V effects 24h；B photos are after the calcium silicates base coating adulterated with ceria acts on 24h
Visible bacterium.
Specific embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and following implementation methods, it should be appreciated that following implementation methods are only used for
The bright present invention, is not intended to limit the present invention.
Refer to pure the invention provides the good ceria doping calcium silicates coating of a kind of anti-degraded and anti-microbial property
The substrate surfaces such as titanium, titanium alloy, stainless steel or CoCrMo alloys are sprayed by the calcium silicates original washing powder body that ceria adulterates
Coating.The present invention is using plasma spraying coating process, the powder is sprayed to the substrate surface after treatment described painting is obtained
Layer.The mass fraction of ceria is 10~50% in powder, and described powder is by particle group that particle diameter is 10~200 microns
Into preferable particle size is 60~150 microns.The thickness of the ceria doping calcium silicates coating is micro- for tens microns~hundreds of
Rice.If coating layer thickness is too thin, then undercoating can be degradable in the period of shorter, so as to coating and bone tissue cannot be realized
Be completely combined；If coating layer thickness is too thick, then coating can be reduced substantially with the bond strength of base material, it may occur that coating is from base
The risk that material surface is peeled off.
The biological coating that the present invention is provided, not only with excellent bioactivity and biocompatibility, and with anti-degraded
Property and antibiotic property, solve the defect problem in the presence of prior art, promote the reparation of sclerous tissues with alternate material field
Development.
Present invention also offers a kind of preparation side of the good ceria doping calcium silicates coating of anti-degraded and anti-microbial property
Method, is using plasma spraying coating process, and the calcium silicates original washing powder body that ceria adulterates is sprayed into the alloy base material table after treatment
Face forms.
In the preparation method, the condition of plasma spray process is as follows：Plasma gas Ar flows be 30~
50slpm；Plasma gas H2Flow is 6~18slpm；Powder carrier gas Ar flows are 1.5~5slpm；Spray distance
It is 80~330mm；Spray power is 30~55kW；Powder feeding rate is 8.0~30gmin-1.Described slpm refers to standard
Liter/min.Using plasma spraying coating process has that coating deposition efficiency is high, coating layer thickness is controllable, can prepare different shape applies
Layer and the advantage for being easy to industrialization.
In the present invention, the calcium silicates original washing powder body of described ceria doping can be prepared by solid sintering technology.As one
Individual example, such as according to 10~50：25~45：42~75 mass ratio is by ceria powder, silicon-dioxide powdery, calcium carbonate
Powder mixes, and ball milling is carried out in planetary ball mill, and rotational speed of ball-mill is 70~170r/min, and Ball-milling Time is 60~180
min.1100~1450 DEG C insulation 1~3 hour after obtain mixed powder, powder crosses 80~200 (such as 80) mesh sieves,
Dried at 100~120 DEG C, obtain the calcium silicates original washing powder body of the ceria doping.
Base material of the invention can select pure titanium, titanium alloy, stainless steel or CoCrMo alloys.The surface treatment of base material, be
Refer to after substrate surface is processed through sandblasting or sand papering, obtained through being cleaned by ultrasonic, drying.The pressure of blasting treatment is preferably
0.1~0.8MPa.
Because experiment is proved：There is biological coating of the invention obvious antibacterial to imitate to staphylococcus aureus, Escherichia coli
Really, antibiotic rate reaches more than 99%；And the unit area matter after being soaked 21 days in the solution equivalent to human physiological environment
Amount loss is less than 5mg/cm2, with good anti-degradability, can be used as reparation and the alternate material of sclerous tissues.In addition, research
It was found that compatibility of the cerium oxide particle in various kinds of cell type is good, and in the case of reasonable Control granularity and concentration, cerium oxide
Biology toxicity effect extremely limit to.
Compared with prior art, the present invention has the advantages that：
1) biological coating that the present invention is provided, not only with excellent bioactivity and biocompatibility, and with anti-degradability and
Antibiotic property；
2) preparation method of the invention has the advantages that simple to operate, efficiency high, favorable repeatability, is adapted to large-scale production.
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this hair
Bright to be further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is of the invention
Some nonessential modifications and adaptations that the above is made belong to protection scope of the present invention.Following specific technique ginsengs of example
Number etc. is also only an example in OK range, i.e. those skilled in the art can be done in suitable scope by the explanation of this paper
Selection, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment
A, the calcium silicates original washing powder body that ceria doping is prepared with solid reaction process
Ceria powder, silicon-dioxide powdery, calcium carbonate powder and zirconium oxide abrasive ball are pressed 10:45:75:260 mass ratio mixing,
It is put into the grinding pot of polytetrafluoroethylene (PTFE), ball milling is carried out in planetary ball mill, rotational speed of ball-mill is 400r/min, Ball-milling Time
It is 300min.1300 DEG C insulation 1 hour after obtain mixed powder, powder crosses 80 mesh sieves, at 100~120 DEG C dry, it is standby
With；
B, using plasma spraying technology prepares coating
After pure titanium or Ti-6Al-4V alloy surfaces are processed through sandblasting or sand papering, ultrasound 1~2 time in ethanol solution, often
It is secondary 3~5 minutes, standby then in 100~120 DEG C of dryings 1~2 hour；The pressure of blasting treatment is 0.1~0.5MPa.Using
Plasma spray process, the pure titanium or Ti-6Al-4V alloy surfaces after treatment, plasma spray process are sprayed to by powder
Condition it is as follows：Plasma gas Ar flows are 40slpm, plasma gas H2Flow is 10slpm, powder carrier gas
Ar flows are 3slpm, and spray distance is 100mm, and spray power is 40kW, and powder feeding rate is 24gmin-1.Described
Slpm refers to standard liter/min.
The calcium silicates original washing powder body of ceria doping as shown in Figure 1 is visible with the XRD spectrum of coating：Coating and powder
Not there is significant change in composition structure, but occur in that partial amorphization phenomenon in coating after spraying, and this is due to quick cooled
Cheng Zhong, mutually crystallization is not caused in time for partial melting.
Coating has a coarse surface topography as seen from Figure 2, shaggy coating material, in human body, favorably
Combined in bone tissue.
The anti-degradability experiment of C, the calcium silicates base coating of ceria doping
The calcium silicates base coating and the CaSiO of pure phase that ceria is adulterated3Coating is separately immersed in Tris-HCl cushioning liquid, than
Situation is changed over time compared with the loss of coating unit area quality.
Result is as shown in figure 3, as seen from Figure 3：Soak the 1st day, CaSiO3Coating unit area quality is lost up to 4
mg/cm2, and the coating after ceria doping is only 0.5mg/cm2, hence it is evident that less than the former；After immersion 21 days, after doping
Coating unit area quality lose less than 5mg/cm2, and CaSiO3Coating has exceeded 10mg/cm2.By comparing：
Ceria is doped in calcium silicates base ceramics can improve the degradability of calcium silicates base coating.
The antibiotic property experiment of D, the calcium silicates base coating of ceria doping
Using the anti-microbial property of colony counting method quantitative determination material：Using staphylococcus aureus, Escherichia coli as experiment strain；
Take strain and be inoculated in nutrient agar surface, 18h is cultivated in insulating box；With reference to bacterium standard opacity tube, 2 × 10 are diluted to8It is individual
Bacterium/ml, carry out 10 times to be serially diluted is 10-2Concentration bacterium solution；Through the pure Ti of the 30mm × 10mm × 2mm of high-temperature sterilization
The calcium silicates base coating surface of (control piece), ceria doping is added dropwise 50 μ l bacterium solutions of each dropwise addition, sticks through the guarantor of alcohol disinfecting
Fresh film, 37 DEG C of insulation 24h.Sample is put into respectively in the test tube equipped with 5ml PBS, vortex concussion 30s takes test tube successively
Middle 0.5ml liquid, carries out 10-1With 10-2Dilution, respectively takes 0.2ml and is inoculated into nutrient agar, cultivates 48h.
Fig. 4,5 be ceria doping calcium silicates base coating to staphylococcus aureus, the antibacterial effect of Escherichia coli
Figure, compared with control piece, being coated with coating has obvious antibacterial effect, and antibiotic rate reaches more than 99%.
Claims (8)
1. a kind of anti-degraded and the good ceria doping calcium silicates coating of anti-microbial property, it is characterised in that ceria doping calcium silicates coating is sprayed on substrate surface and is formed by the calcium silicates original washing powder body that ceria adulterates by plasma spray technology.
2. ceria according to claim 1 doping calcium silicates coating, it is characterised in that the mass fraction of ceria is 10~50% in the calcium silicates original washing powder body of the ceria doping, and described powder is made up of the particle that particle diameter is 10~200 microns.
3. ceria according to claim 1 and 2 doping calcium silicates coating, it is characterised in that the base material is pure titanium, titanium alloy, stainless steel or vitallium.
4. a kind of ceria any one of claims 1 to 3 adulterates the preparation method of calcium silicates coating, it is characterised in that the preparation method includes：As raw material, the raw material is sprayed on substrate surface to calcium silicates original washing powder body with ceria doping by using plasma spraying technology, obtains the ceria doping calcium silicates coating.
5. preparation method according to claim 4, it is characterised in that the calcium silicates original washing powder body of the ceria doping is obtained by solid sintering technology, is specifically included：According to 10~50：25~45：Ceria powder, silicon-dioxide powdery, calcium carbonate powder mixing and ball milling are obtained mixed powder by 42~75 mass ratio after being incubated 1~3 hour in 1100~1450 DEG C, will obtain the calcium silicates original washing powder body that the ceria adulterates after mixed powder sieving, drying.
6. the preparation method according to claim 4 or 5, it is characterised in that the condition of plasma spray coating process is as follows：Plasma gas Ar flows are 30~50 slpm；Plasma gas H2Flow is 6~18 slpm；Powder carrier gas Ar flows are 1.5~5 slpm；Spray distance is 80~330 millimeters；Spray power is 30~55 kilowatts；Powder feeding rate is 8.0~30 gram/minutes.
7. the preparation method according to any one of claim 4 to 6, it is characterised in that the base material is pure titanium, titanium alloy, stainless steel or vitallium.
8. the ceria doping calcium silicates coating any one of a kind of claims 1 to 3 is being prepared for the application in the reparation of sclerous tissues and alternate material.
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| CN112805243A (en) * | 2019-03-06 | 2021-05-14 | Toto株式会社 | Coated body and coating composition |
| CN115029752A (en) * | 2022-06-28 | 2022-09-09 | 郑州大学 | Preparation method of composite coating suitable for bone implantation magnesium or magnesium alloy |
| CN115558426A (en) * | 2022-09-23 | 2023-01-03 | 无锡兴华衡辉科技有限公司 | Method for grinding chip surface, suspension grinding and polishing liquid for grinding chip surface and preparation method thereof |
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