CN102190958B - Biocompatibility coating composition and application thereof - Google Patents
Biocompatibility coating composition and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 claims abstract description 139
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- 230000000975 bioactive effect Effects 0.000 claims abstract description 58
- 239000000560 biocompatible material Substances 0.000 claims abstract description 43
- 239000002105 nanoparticle Substances 0.000 claims abstract description 26
- 238000000576 coating method Methods 0.000 claims description 96
- 239000011248 coating agent Substances 0.000 claims description 76
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 71
- 238000000034 method Methods 0.000 claims description 61
- 239000004408 titanium dioxide Substances 0.000 claims description 34
- 239000010936 titanium Substances 0.000 claims description 27
- 229910052719 titanium Inorganic materials 0.000 claims description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 25
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 25
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Abstract
Disclose formation high degree of biocompatibility coating composition, and this coating composition is applied to implant to improve its biocompatibility.In one embodiment, coating composition includes macromolecular material, account for the nano-scale particle of described composition total weight 0.1 10%, or/and account for the biocompatible material of described composition total weight 1 50% or account for bioactive materials or both combinations of described composition total weight 0.1 20%, wherein, when described compositions includes described macromolecular material and described biocompatible material or/and during described bioactive materials, described macromolecular material and described biocompatible material are or/and described bioactive materials exists with micron order form of mixtures in the composition.
Description
Technical Field
The present application relates to forming a biocompatible coating composition, and the use of the coating composition to improve the biocompatibility of an implant.
Background
With the increase of incidence of diseases such as trauma, degenerative tumor and the like, more and more orthopedic operations need to use implants, for example, internal fixation instruments are needed for fracture, artificial joint prostheses are needed for joint replacement, fusion devices are needed for spinal operations, dental implants are needed for dental implant transplantation, and the like. Various orthopedic implants play an important role in promoting bone healing after trauma, recovering the anatomical structures of bones and joints and improving the stability of joints. However, due to the differences in physical and biological properties of various implant Materials, mechanical degeneration (J.B.Brunski, "biological Factors influencing the Bone-fractional Implantation interface," Clinical Materials, Vol.10, pp.153-201, 1992), biological rejection problems (K.das, S.Bose, A.Bandypapdhayy, B.Karandikar, and B.L.Gibbins, "Surface Coatings for improvement of Bone Materials and Antimicrobial Activities of migration, journal.455-460, 2008) often occur when implants are implanted into humans or animals.
Taking titanium as an example, titanium and titanium alloys have been widely used in the field of transplantation of hard tissues such as bones and teeth in clinical practice, based on their excellent model properties, corrosion resistance, high biocompatibility, light weight, and wide sources. However, due to the biological inertness of the titanium metal and titanium alloy surfaces, when the titanium metal or titanium alloy implant is implanted into a human or animal, the bond between the implant and the bone is only a mechanical interlocking, and often no chemical bond is formed, so that a fibrous barrier is formed between the cells in the body and the implant, and the bonding between the titanium and titanium alloy implant and the bone cells is reduced, thereby reducing the service life of the titanium and titanium alloy bone implant (S.Szmukler-Moncler, H.Salama, Y.Reindewittz, and J.H.Dubruille, "Timing of attachment and impact of a microbial bone-representative interface of experimental tissue," journal of biological Materials Research, Vol.43, pp.192-203, 1998).
Therefore, the study of modifying the surface of an implant to improve the mechanical and biological properties of the implant has been receiving increasing attention. At present, a plurality of techniques for modifying the surface of an implant are available, including (1) modification of the surface morphology and roughness of the implant, which can be accomplished by mechanical and micro-mechanical processing methods, plasma spraying methods, sand blasting and acid etching methods, coating roughening techniques, and the like; (2) forming a coating for improving the corrosion resistance and corrosion resistance of the surface of the implant, wherein the coating can be formed by a diamond coating method, a nitride coating method and the like; (3) the surface bioactivity modification method of the implant can be carried out by using a surface spraying method (including a plasma spraying method and an electrochemical deposition method), a surface oxidation method (including an alkali heat treatment method and a sol-gel method), a composite coating method and the like.
The above-described methods for modifying the bioactivity of implant surfaces still have several problems. The plasma spraying method is a method which is mature in process and common in application at present. The method comprises ionizing gas phase between two direct current electrodes by electric arc generated between the two direct current electrodes to form high temperature plasma, introducing bioactive material powder into ultrahigh temperature plasma flame, heating and melting, spraying onto the surface of the implant with high speed airflow, and rapidly solidifying to form coating. The method has the advantages of high speed, mature condition and process, uniform coating, good repeatability and suitability for industrial production. However, this method has problems of expensive equipment, unsuitability for spraying porous metal surfaces, low adhesion strength of the coating to the implant body, and poor long-term stability of the coating (K. James, H. Leven, J.R. Parsons, and J.Kohn, "Evaluation of a series of discrete type-derived polycarbonates in-wafer defects," Biomaterials, Vol.20, pp.2203-2212, 1999).
Surface oxidation may be applied to titanium implants. Titanium for bone implantation is often found in natural conditionsCan be oxidized to form a titanium metal oxide film with the thickness of a few nanometers, and the film is a biological inert layer and has poor biological activity. The active titanium metal oxide coating can be prepared by activating and modifying the inert surface through proper treatment. The coating has good wear resistance and corrosion resistance, and can promote the formation of chemical combination between the coating and bone tissues. Common titanium surface oxide activation methods are alkaline heat treatment (H.B.Wen, J.R.De Wijn, F.Z.Cui, and K.De Groot, "Preparation of calcium phosphate on titanium oxide chemical chemistry," Journal of biological Materials Research, Vol.41, pp.227-236, 1998), sol-gel methods (A.F. Maximian Haenne, Carmen Zitz, Ranier Bader, Fraidenau, Wolfram Mittelmei and Hans gold window, "extended particulate metal oxides (TiO)2) coating for metallic implants: in vitro efficiency learning MRSAand mechanical properties, "Journal of Materials Science: materials in Medicine2010), and the like. The basic treatment method is a common chemical treatment method, and the mechanism of the method is mainly that a layer of bioactive porous reticular sodium titanate gel can be formed on the surface of a titanium implant in a sodium hydroxide solution, and then the titanium implant is converted into an anatase titanium dioxide layer after being treated by hot water. The oxide film of the layer is compact, can enhance the wear resistance and corrosion resistance of metal, and enhances the chemical stability and service life of the metal after being implanted into a body. In-vitro simulated body fluid experiments also prove that the anatase titanium dioxide oxide layer has bioactivity and can induce the formation of apatite deposition. However, the titanium dioxide oxidation coating obtained by the method is thin, and has the defect of low bonding strength.
Composite coating methods (J.Repending, G.Venkataraman, J.Chen, and N.Stafford, "Electrochemical preparation of chemical/hydrolytic coatings on substrates," Journal of biomedical materials Research, Vol.66A, pp.411-416, 2003) are also currently widely used and promising technologies. Specifically, the method combines the metal surface coating with the metal surface oxidation, which comprises the steps of firstly carrying out oxidation treatment on the surface of a metal implant to obtain activityAnd (3) coating and depositing a bioactive coating on the surface of the metal oxide layer to prepare the bioactive coating-metal oxide layer composite coating. The coating can be combined with the bone tissue in an early stage, so that the combination force between the implant and the bone tissue is improved. Meanwhile, the functions of abrasion resistance and corrosion resistance of the compact metal oxide layer and the function of inhibiting ion release ensure the stability of the implant in the body and effectively improve the performance of the implant (Z.B. Zhang C, ZhaoZJ, Deng CF, Effect of HA/TiO)2coating titanium surface on the growing of MG63, "Shanghai Kou Qiang Yixue, Vol.18, pp.411-4, 2009). However, the composite method adopts two technologies simultaneously, so that the product performance influence factors are more, and the interface between the two coatings is easy to fall off.
In summary, although there are many methods for modifying the bioactivity of the surface of the implant, each method still has different disadvantages, and therefore, further research and improvement are still needed, and a new method for improving the bioactivity of the surface of the implant is sought.
SUMMARY
One aspect of the present application provides a coating composition comprising
A polymeric material (generally from 30 to 90%, preferably from 40 to 75%, more preferably from 50 to 65% by weight of the total composition), and
0.1-10% by weight of nanoscale particles, based on the total weight of the composition, or/and
1-50% by total weight of the composition of a biocompatible material, or 0.1-20% by total weight of the composition of a bioactive material, or a combination thereof,
wherein, when the composition comprises the polymer material and the biocompatible material or/and the bioactive material, the polymer material and the biocompatible material or/and the bioactive material exist in a micron-scale mixture form.
In some embodiments of the coating composition, the polymeric material may be selected from the group consisting of coatings, resins, and adhesives, including but not limited to epoxy resins, polyacrylates, polyurethanes, polyesters, and mixtures thereof.
In some embodiments of the coating composition, the nanoscale particles can be titanium dioxide, silica, or alumina. The nanoscale particles may be present in the coating composition in an amount ranging from 0.3 to 5% by weight, in some embodiments, and from 0.5 to 2% by weight, in other embodiments, based on the total weight of the composition.
In some embodiments of the coating composition, the biocompatible material can be selected from the group consisting of bioinert ceramics such as oxide ceramics, Si3N4 ceramics, glass ceramics, medical carbon materials, and medical metallic materials and metal oxides such as metallic titanium, titanium alloys, titanium dioxide, cobalt oxide, calcium oxide, zirconium oxide, and the like.
In some embodiments of the coating composition, the biocompatible material can comprise 10 to 30% of the total weight of the composition, in other embodiments the biocompatible material can comprise 10 to 25% of the total weight of the composition, and in certain particular embodiments the biocompatible material can comprise 25% of the total weight of the composition.
In certain embodiments of the coating composition, the bioactive material may be selected from bioactive ceramic-like materials, such as calcium phosphate-based bioceramics, tricalcium silicate, dicalcium silicate, calcium hydroxide, and the like; mineral materials, such as MTA (mineral oxides aggregates), hydroxyapatite.
In some embodiments of the coating composition, the bioactive material can comprise 1 to 10% by weight of the total composition, and in some embodiments, can comprise 5 to 10% by weight of the total composition. In certain particular embodiments, it may comprise 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, or 10% of the total weight of the composition.
Another aspect of the present application relates to the use of the coating composition provided herein for improving the biocompatibility of an implant, comprising applying said coating composition to the surface of said implant.
In some embodiments of this application, the application comprises applying the coating composition to a surface of an implant.
In yet another aspect, the present application provides a method of improving the biocompatibility of an implant comprising applying the coating composition provided herein to the surface of the implant.
In yet another aspect, the present application provides an implant comprising an implant body and a coating adhered to a surface of the body, wherein the coating comprises the coating composition provided herein.
Another aspect of the present application provides a method of making an implant, the implant comprising a body, the method comprising: the coating composition provided herein is applied to the surface of the body to form a coating.
In various aspects of the application of the coating composition described above herein, the coating composition can be applied to the surface of the implant by a spray coating process, such as by a powder spray coating process.
Drawings
FIG. 1 is a schematic diagram of the process of forming a composite material of the present application of a polymeric material and a biocompatible or/and bioactive material.
Fig. 2 illustrates the spray application of the coating composition of the present application to an implant and the curing process.
FIG. 3 shows the results of a cell count experiment performed after application of some of the coating compositions of the present application.
FIG. 4 shows the results of a cell count experiment performed after application of further coating compositions of the present application.
Detailed Description
Various aspects of the present application are illustrated and described in detail below with reference to specific embodiments or examples. It should be understood that these embodiments/examples are merely illustrative and should not be construed as limiting the scope of the claimed invention.
Definition of
As used herein, the term "about"/"about," when used in conjunction with a size range or other physical property of a particle, such as temperature or chemical characteristics, is intended to encompass slight variations that may exist in the upper and lower limits of the size range of the particle, thus avoiding embodiments in which most average sizes are met but statistical sizes may fall outside the range. The present invention is not intended to exclude such embodiments.
The term "implant" as used herein refers to various medical implants useful in living organisms (primarily humans and animals) for the replacement and repair of tissue and organs, including but not limited to: orthopedic implants, dental implants, and the like include natural or artificial materials such as metallic materials, inorganic materials (e.g., ceramic materials), organic materials (e.g., synthetic polymeric materials), natural biomaterials, and the like.
The term "biocompatible material" as used in this application means that the material does not have a significant deleterious effect on an organism after implantation in the organism.
The term "bioactive material" as used herein means that the material, when implanted in a living organism, can react with the surrounding environment in a benign physiological manner to stimulate the regeneration of cells in the organism.
The term "polymeric material" as used herein refers to those polymeric materials known to those skilled in the art and useful in the art, including coatings, resins, rubbers, plastics, fibers, adhesives, polymer-based composites, and the like, and generally refers to polymeric materials of the coatings, resins, adhesives, and the like.
The term "nanoscale particles" as used herein refers to particles having an average particle diameter in the range of about 1 nanometer to about 100 nanometers.
The term "submicron particle" as used herein refers to a particle having an average particle diameter in the range of about 100 nanometers to about 1 micrometer.
The term "micron-sized particles" as used herein refers to particles having an average particle diameter in the range of about 1.0 micron to about 100 microns.
In view of the shortcomings of current methods of modifying the surface of an implant, the inventors have discovered that the application of the coating compositions disclosed herein to an implant can improve the biocompatibility properties of the surface of the implant.
One aspect of the present application provides a coating composition comprising:
a polymeric material (generally from 30 to 90%, preferably from 40 to 75%, more preferably from 50 to 65% by weight of the total composition), and
0.1-10% by weight of nanoscale particles, based on the total weight of the composition, or/and
1-50% by total weight of the composition of a biocompatible material, or 0.1-20% by total weight of the composition of a bioactive material, or a combination thereof,
wherein, when the composition comprises the polymer material and the biocompatible material or/and the bioactive material, the polymer material and the biocompatible material or/and the bioactive material are present in the composition in the form of a micron-sized mixture.
In the coating composition of the present application, the polymer material is a base material of the coating composition, and may be generally selected from polymer materials of resin, adhesive, and the like. Those skilled in the art will readily determine the particular materials that may be selected for use in a particular embodiment. For example, resinous materials having relatively strong adhesion may be selected, such as suitable molecular weight epoxies, polyacrylates, polyurethanes, polyesters, or mixtures thereof. The content of the polymeric material in the coating composition is not particularly limited, mainly considering the amount of other components added in the composition. Typically the polymeric material may comprise from 30 to 90% by weight of the total composition. In some preferred embodiments, it may comprise from 40 to 75% by weight of the total composition, and in other preferred embodiments, it may comprise from 50 to 65% by weight of the total composition.
The nanoscale particulate material in the coating composition of the present application serves to modify the surface structure of the implant. Without being bound by theory, it is understood that the addition of nanoscale particulate materials allows the implant surface coating to form nanoscale morphologies, thereby increasing the biocompatibility of the coating. The nanoscale particles may be present in the coating composition in an amount generally ranging from 0.1 to 10% by weight, in some embodiments from 0.5 to 2% by weight, and in other embodiments, from 2 to 5% by weight, based on the total weight of the composition. The nanoscale particulate material is typically chosen to be biocompatible, but may also be non-biocompatible due to its low loading, provided that the nanoscale particulate material is chosen to favor the formation of a coating nanostructure morphology. The nano-scale particle material can be inorganic nano-materials such as inorganic minerals or metal oxides, and comprises titanium dioxide, silicon dioxide and aluminum oxide, wherein the titanium dioxide is preferred.
In the coating composition, a biocompatible material may be further included. In this case, the micro-scale composite powder is formed by uniformly fusing the high molecular material and the material having high biocompatibility, so that the biocompatibility of the formed coating can be increased. The biocompatible material may comprise 1-50% of the total weight of the composition. In some embodiments, the biocompatible material may comprise 10 to 30% by weight of the total composition, and in other embodiments, the biocompatible material may comprise 10 to 20% by weight of the total composition. The biocompatible material may be selected from the group consisting of bioinert ceramics such as oxide ceramics, Si3N4 ceramics, glass ceramics, medical carbon materials, and medical metallic materials and metal oxides such as metallic titanium, titanium alloys, titanium dioxide, cobalt oxide, calcium oxide, zirconium oxide, and the like. In some embodiments, the biocompatible material is selected from titanium dioxide or metallic titanium.
In coating composition embodiments of the present application, bioactive materials may be included. In this case, the micro-scale composite powder is formed by uniformly fusing the polymer material and the material having the biological activity, so that the biocompatibility of the formed coating can be increased. The inclusion of bioactive materials in the coating itself may further increase the biocompatibility of the coating. The bioactive material may be present in an amount of from 0.1 to 20% by weight of the total composition, in certain embodiments from 1 to 10% by weight of the total composition, and in certain other embodiments from 5 to 10% by weight of the total composition. In certain particular embodiments, it may comprise 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, or 10% of the total weight of the composition.
Bioactive materials that may be selected include ceramic-like materials such as calcium phosphate-based bioceramics, tricalcium silicate, dicalcium silicate, calcium hydroxide, and the like; mineral materials such as MTA (mineral polyoxeagregates).
In the coating composition of the present application, other additive materials, for example, pigments such as organic red, organic yellow, fillers such as barium sulfate, etc., and other auxiliaries such as leveling agents, degassing agents, etc., may be added. It should be understood that the addition of these additional materials is not essential to the present invention and can be easily determined as needed by those skilled in the art, but the addition thereof should not affect the solution of the technical problems of the various aspects of the present application. The specific additive material and amount may be determined according to the specific use of the implant.
The formation of a biocompatible coating on an implant with the coating composition of the present application can be carried out by various methods. For example, the coating composition is powdered, and the spraying can be carried out using conventional powder spraying methods, such as corona or tribostatic spraying. For example, if the coating composition is prepared as a liquid, or dissolved or suspended in a liquid, the coating composition can be sprayed by a conventional liquid spraying method.
Some particular embodiments of coating compositions that may be exemplified include:
1, a.55% of high molecular material (epoxy resin or polyester),
b.25% of a biocompatible material (titanium dioxide or metallic titanium)
c.0.5-2% of a nanoscale particulate material (titanium dioxide or silicon dioxide)
d. The rest of filler and other additive materials.
A.55% of high molecular material (epoxy resin or polyester),
b.25% of a biocompatible material (titanium dioxide or metallic titanium)
c.0.5-2% of a nanoscale particulate material (titanium dioxide or silicon dioxide)
d.1-10% bioactive material (MTA or hydroxyapatite)
e. The rest of filler and other additive materials.
A.55% of high molecular material (epoxy resin or polyester),
0.5-2% of a nanoscale particulate material (titanium dioxide or silicon dioxide)
c. The rest of filler and other additive materials.
The preparation of the coating composition of the present application and the method of forming the coating composition on the surface of the implant to form a coating layer will be described below by taking a coating composition in the form of powder as an example.
When the coating composition includes a polymeric material and a biocompatible or/and bioactive material, see fig. 1: firstly, the polymer material is fully and uniformly mixed with the biocompatibility or/and the biological active material in a physical way according to a certain proportion. The mixture is then introduced into an extruder, mixed with other additives, if desired, and the like, and then melted at high temperature in the extruder, extruded from the extruder in the form of a paste, shaped and cooled to form a sheet. The extruded sheet material is homogeneous mixture of polymer material and additive material with biocompatibility and/or bioactivity, and is crushed into micron level size particle of 10-50 micron size. Screening is then performed using a mesh screen of appropriate pore size. Thus, the composite powder of the high molecular material and the biocompatible or/and bioactive material is prepared. If no biocompatible or/and bioactive material is added during this process, the material produced is a polymeric spray material as is commonly used in the powder spray art.
If the nano-scale particle material is required to be added into the micron-scale composite powder material obtained in the above step, the two kinds of powder are fully mixed.
If the coating composition only contains the high molecular material and the nano-scale particle material, the high molecular material and the necessary additive material are fused, extruded, crushed and sieved to prepare micron-scale powder, and then the micron-scale powder and the nano-scale particle material are fully mixed.
FIG. 2 shows one embodiment of applying the coating composition to the surface of the implant body. The nano-scale particle material and the micron-scale polymer powder are fully and uniformly mixed and then sprayed to the surface of the implant through an electrostatic spray gun. Then the coating components are melted, leveled and cured by heat treatment (sometimes by other means such as ultraviolet light) at a certain temperature, and after cooling, a coating which is tightly combined with the implant is formed.
Examples
The test method comprises the following steps:
the following method was applied to the testing of the coatings prepared in examples 1 and 2.
A. Physical Property testing of coating materials
a) Observation of the coating surface with a scanning electron microscope
b) Observing the three-dimensional morphological structure of the coating by using an atomic force microscope
c) Testing the surface roughness of a coating with a step profiler
d) Elemental composition of the coating was observed using an X-ray energy analysis spectrometer
e) Testing the adhesive force of the coating and the biological material by using a universal lattice scriber and a special adhesive tape in the spraying industry
B. And (3) testing the biocompatibility:
f) after 24 hours and 72 hours of culture, the growth and proliferation of cells cultured on the coated surface were observed by scanning electron microscope
g) After 72 hours and 7 days of culture, the morphological structure of cytoskeleton of the cells cultured on the coating surface was observed by fluorescence microscopy, so as to understand the growth and propagation conditions of the cells on the coating surface
h) After 24 hours and 72 hours of culture, the number and metabolic activity of cells growing on the surface of the coating are tested by using a cell counting test and an MTT (methyl thiazolyl tetrazolium) analysis method, so that the growth and reproduction conditions of the cells on the surface of the coating are known
i) After 4 weeks of culture, useAlizarin Red StainingThe test is to perform calcium element staining on the cells growing on the surface of the coating, thereby knowing the differentiation condition of the cells on the surface of the coating
j) After 4 weeks of culture, the expression of genes promoting cell differentiation, such as osteogenic differentiation promoting genes GAPDH, Collagen I and Runx 2, was tested using RNA extraction technology, reverse transcriptase-polymerase chain reaction technology, and thus the differentiation of cells on the surface of the coating was known.
Example 1
In this experiment, we designed 8 materials to prepare the coating composition. The composition of the 8 materials is shown in table 1 below (the components are referred to in weight percent, based on the total weight of the coating material as 100%):
TABLE 1
The filler in the table is barium sulfate, and the auxiliary agent is selected from a degassing agent, a leveling agent and a curing agent.
In the test, polymer powder (epoxy resin, DER 663, Dow chemical, USA; polyester, CrylCoat2440-2, UCB Surface Specialities, USA) and titanium dioxide biocompatible material are fully and physically mixed (the PPC-1 does not contain titanium dioxide), and are mixed with filler and other additive materials, and then the mixture is put into an extruder (SLJ30 twin-screw extruder, Nicotine powder equipment, Inc.) to be fused in the extruder at 95 ℃ for months, and after molding and cooling, the sheet composite powder is crushed into micron-sized particles with the average particle diameter of 15-30 microns by a high-speed crusher. Then sieving with 45 μm sieve, adding certain amount of submicron Polytetrafluoroethylene (PTFE) to the sieved micron-sized particlesMP1000, dupont, usa) and further nanoscale titanium dioxide (P25, Evonik, usa) or silica particles (R972, Evonik, usa). The nanometer-level addition material and the micron-level particles are fully and uniformly mixed by a pulverizer, sprayed on the surface of the metal titanium implant substrate by an electrostatic spray gun to form a coating, and cured for 10 ten minutes at 200 ℃.
For the cured powder coating, we performed a series of tests for physical properties as well as biocompatibility. The results show that, in terms of the physical properties of the implant surface coating:
(1) compared with coating materials with different components in PPC-1 to PPC-8, the addition of submicron Polytetrafluoroethylene (PTFE) obviously increases the micron-scale morphological structure of the coating surface, and the addition of nano-scale titanium dioxide or silicon dioxide particles obviously increases the nano-scale morphological structure of the coating surface.
(2) The various constituents of the materials of all the coating compositions PPC-1 to PPC-8 can be well combined and form a coating with uniform composition.
(3) All coatings from PPC-1 to PPC-8 have strong adhesion to the substrate.
Figure 3 shows the results of the 24 hour and 72 hour cell counting experiments.
1) After 24 hours of culture on the surface of each of PPC-1 to PPC-8 coatings, the number of mesenchymal cells of embryonic palatal Process grown on the surface of PPC-6 coating was the greatest.
2) After 72 hours of culture on the surface of each of PPC-1 to PPC-8 coatings, the number of mesenchymal cells of embryonic palatine growing on the surface of PPC-6 coating was the greatest, and the increase was most significant compared to 24 hours.
The result shows that the PPC-6 coating has the most obvious promotion effect on the growth and the reproduction of mesenchymal cells of the embryonic palatine.
Tests in terms of biocompatibility showed that:
(1) PPC-1 to PPC-8 are all biocompatible, and cells can grow again.
(2) PPC-1 is the least biocompatible, mainly due to the absence of significant amounts of titanium dioxide in PPC-1.
(3) The biocompatibility of PPC-2 is greater than that of PPC-1 and less than that of PPC-3, indicating that the biocompatibility is increased with the increase of the amount of titanium dioxide.
(4) Compared with the nano-scale silicon dioxide, the nano-scale titanium dioxide has stronger biocompatibility besides increasing the surface nano-structure, so that the biocompatibility of the PPC-4 is greater than that of the PPC-3.
(5) Although the submicron Polytetrafluoroethylene (PTFE) can obviously increase the micron-sized morphological structure of the coating surface, the micron-sized structure has no obvious effect on increasing the biocompatibility of the coating. In contrast, the nano-scale titanium dioxide particles can obviously increase the nano-scale structure of the surface of the coating, and the large amount of nano-structures can greatly improve the biocompatibility of the coating.
(6) PPC-6 shows the best biocompatibility and can well promote mesenchymal cells of embryonic palatal processhuman embryonic palatal mesenchymalcells) to adhere to, grow, multiply, and differentiate on the substrate surface. This is mainly due to the addition of large amounts of titanium dioxide with biocompatible properties and the reinforcement of the nano-scale titanium dioxide to the coating surface nanostructure in the coating composition, while at the same time avoiding the presence of large amounts of micro-morphology structures caused by sub-micron Polytetrafluoroethylene (PTFE).
Example 2
The effect of adding the bioactive material MTA (mineral TrioxidieAggregates) on coating performance was studied for the purpose of this study.
In this experiment, we designed 6 coating materials and compared them with the PPC-6 of example 1. The composition of the 6 coating materials is shown in table 2 below:
TABLE 2
The filler in the table is barium sulfate, and the auxiliary agent is selected from a degassing agent, a leveling agent and a curing agent.
In the test, polyester (CrylCoat 2440-2, UCB surface specialities, USA) powder is fully and physically mixed with 1%, 5%, 10% MTA (ProRoot MTA, Dentsply, USA) and titanium dioxide, then mixed with required fillers, pigments and the like, and then high-temperature fusion is carried out in an extruding machine, then the uniform mixture of the block material and the bioactive additive material extruded from the extruding machine is crushed into micron-sized particles with the particle diameter of 15-30 microns by a high-speed crusher, and then the micron-sized particles are screened by a 45-micron mesh screen. 0.5 percent of nano-scale titanium dioxide additive material is added into the screened micron-scale composite powder, the nano-scale particle additive and the micron-scale composite powder are fully and uniformly mixed by a pulverizer, a powder coating is formed on the surface of the metal titanium substrate by a corona electrostatic spray gun, and the curing is carried out for 10 ten minutes at the temperature of 200 ℃.
For the cured coating, we performed a series of physical properties and biocompatibility tests.
The results show that, in terms of the physical properties of the coating:
(1) the surfaces of PPC-6, GMPPC-6 and WMPPC-6 have similar nano-scale structures.
(2) The PPC-6, GMPPC-6 and WMPPC-6 coating materials can be well fused with each other to form a coating with uniform composition.
(3) PPC-6, GMPPC-6 and WMPPC-6 have strong adhesion with the base material.
Figure 4 shows the results of the 24 hour and 72 hour cell counting experiments.
1) After 24 hours of culture on the coating surfaces of PPC-6, GMPPC-6a, GMPPC-6b, GMPPC-6c, WMPPC-6a, WMPPC-6b and WMPPC-6c, the amount of the mesenchymal cells of the embryonic palatal Process growing on the coating surfaces of the GMPPC-6 and WMPPC-6 is more than that of the PPC-6.
2) After 72 hours of culture on the surfaces of PPC-6, GMPPC-6 and WMPPC-6 coatings, the quantity of the embryonic palatal mesenchymal cells growing on the surfaces of the GMPPC-6 and WMPPC-6 coatings is more than that of the PPC-6, and the quantity of the embryonic palatal mesenchymal cells growing on the surfaces of the GMPPC-6 coatings is increased most obviously compared with the quantity of the cells in 24 hours.
The result shows that the GMPPC-6 and WMPPC-6 coatings have more remarkable promoting effect on the growth and the reproduction of mesenchymal cells of the embryo palatine compared with the PPC-6 coatings.
Tests on biocompatibility show that:
(1) compared with a PPC-6 coating with high biocompatibility, the addition of the gray MTA and the white MTA with high bioactivity can further greatly improve the biocompatibility of the coating and greatly promote the adhesion, growth, reproduction and differentiation of mesenchymal cells of the embryonic palatine process on the surface of pure titanium.
(2) As the content of the grey and white MTAs in the coating composition increases, the biocompatibility of the GMPPC, WMPPC coatings also increases. This additional increase in biocompatibility may result primarily from the addition of MTA, a highly bioactive agent.
It is to be understood that the specific features and elements (compounds, compositions, components, steps) described herein with respect to a particular aspect, embodiment, or embodiment of the invention are not to be limited to those specific aspects, embodiments, or embodiments. It is to be understood that each specific feature, each component element (compound, composition, component, step), and each specific feature, each component element (compound, composition, component, step), and each like described herein can also be used in other aspects, embodiments, and examples herein, unless the specific features, each component element (compound, composition, component, step), and each like conflict with each other, as will be apparent to one of ordinary skill in the art.
Also, unless expressly conflicting, all features disclosed in this application (including all steps in a method) may be combined in any form to form different embodiments of the invention.
Claims (37)
1. Use of a coating composition for improving the biocompatibility of an implant, said composition comprising:
a polymeric material in an amount of 30-90% by weight of the total composition, and
0.1-10% by weight of the total composition of nanoscale particles intended to form nanoscale morphological structures, and:
1-50% by total weight of the composition of a biocompatible material, or 0.1-20% by total weight of the composition of a bioactive material, or a combination thereof,
wherein,
the polymeric material and the biocompatible material or/and the bioactive material are present in the composition as a micron-sized mixture;
the composition is in powder form;
the high polymer material is a high polymer material of paint, resin and adhesive; the biocompatible material is selected from bioinert ceramics, medical metal materials or medical metal oxides; the bioactive material is selected from bioactive ceramic materials or mineral materials;
the nano-scale particles are titanium dioxide, silicon dioxide or aluminum oxide.
2. The use according to claim 1, wherein the polymeric material comprises 40-75% by weight of the total composition.
3. The use according to claim 2, wherein the polymeric material comprises 50-65% by weight of the total composition.
4. The use according to claim 1, said nanoscale particles comprising from 0.3 to 5% by weight of the total composition.
5. The use according to claim 4, said nanoscale particles comprising from 0.5 to 2% by weight of the total composition.
6. The use according to claim 1, wherein said biocompatible material comprises 10-25% by weight of the total composition.
7. The use according to claim 6, wherein the bioactive material comprises 0.1-10% by weight of the total composition.
8. Use according to claim 1, the bioactive ceramic-based material being selected from calcium phosphate-based bioceramics, tricalcium silicate, dicalcium silicate, calcium hydroxide, the mineral material being selected from MTA, hydroxyapatite.
9. Use according to claim 1, the bioinert ceramic being selected from oxide ceramics, Si3N4 ceramics, glass ceramics, medical carbon materials, the medical metallic materials or medical metal oxides being selected from metallic titanium, titanium alloys, titanium dioxide, calcium oxide, zirconium oxide.
10. Use according to any one of claims 1 to 9, which comprises applying the composition to the surface of an implant.
11. The use of claim 10, the coating comprising applying the composition to the surface of the implant using a spray coating process.
12. Use according to claim 11, the spray coating process being a powder spray coating process.
13. Use according to any one of claims 1 to 9, the polymeric material being selected from the group consisting of epoxy resins, polyacrylates, polyurethanes, polyesters, and mixtures thereof.
14. The use according to any one of claims 1 to 9, wherein the biologically active material is MTA.
15. A method of improving the biocompatibility of an implant, said method comprising applying to the surface of the implant a coating composition comprising:
a polymeric material in an amount of 30-90% by weight of the total composition, and
0.1-10% by weight of the total composition of nanoscale particles intended to form nanoscale morphological structures, and:
1-50% by total weight of the composition of a biocompatible material, or 0.1-20% by total weight of the composition of a bioactive material, or a combination thereof,
wherein the polymeric material and the biocompatible material or/and the bioactive material are present in the composition as a micron-sized mixture,
and the coating composition is in powder form;
the high polymer material is a high polymer material of paint, resin and adhesive; the biocompatible material is selected from bioinert ceramics, medical metal materials or medical metal oxides; the bioactive material is selected from bioactive ceramic materials or mineral materials;
the nano-scale particles are titanium dioxide, silicon dioxide or aluminum oxide.
16. The method of claim 15, wherein the bioactive material is selected from the group consisting of calcium phosphate-based bioceramics, tricalcium silicate, dicalcium silicate, calcium hydroxide, MTA, and hydroxyapatite.
17. The method of claim 15, wherein the biocompatible material is selected from the group consisting of oxide ceramics, Si3N4 ceramics, glass ceramics, medical grade carbon materials, metallic titanium, titanium alloys, titanium dioxide, calcium oxide, or zirconium oxide.
18. A method according to any one of claims 15 to 17, comprising applying the composition to the surface of the implant using a powder spray process.
19. The method of any one of claims 15-17, wherein the polymeric material is selected from the group consisting of epoxy, polyacrylate, polyurethane, polyester, and mixtures thereof.
20. The method of any one of claims 15-17, wherein the bioactive material is MTA.
21. An implant comprising an implant body and a coating composition adhered to a surface of the body, wherein the coating composition comprises:
30-90% by weight of the total composition of a polymeric material, and
0.1-10% by weight of the total composition of nanoscale particles intended to form nanoscale morphological structures, and:
1-50% by total weight of the composition of a biocompatible material, or 0.1-20% by total weight of the composition of a bioactive material, or a combination thereof,
wherein the polymeric material and the biocompatible material or/and the bioactive material are present in the composition as a micron-sized mixture;
the composition is in powder form;
the high polymer material is a high polymer material of paint, resin and adhesive; the biocompatible material is selected from bioinert ceramics, medical metal materials or medical metal oxides; the bioactive material is selected from bioactive ceramic materials or mineral materials;
the nano-scale particles are titanium dioxide, silicon dioxide or aluminum oxide.
22. The implant of claim 21, wherein the bioactive material is selected from the group consisting of calcium phosphate-based bioceramics, tricalcium silicate, dicalcium silicate, calcium hydroxide, MTA, and hydroxyapatite.
23. The implant of claim 21, wherein the biocompatible material is selected from the group consisting of oxide ceramics, Si3N4 ceramics, glass ceramics, medical grade carbon materials, metallic titanium, titanium alloys, titanium dioxide, calcium oxide, or zirconium oxide.
24. The implant of claim 21, comprising applying the coating composition to the surface of the implant using a powder spray process to form the coating.
25. The implant of any one of claims 21-24, wherein the polymeric material is selected from the group consisting of epoxy, polyacrylate, polyurethane, polyester, and mixtures thereof.
26. The implant of any one of claims 21-24, wherein the bioactive material is MTA.
27. A method of making an implant, the implant comprising a body, the method comprising applying a composition to a surface of the body to form a coating, the composition comprising:
30-90% of a polymeric material, and 0.1-10% of nanoscale particles, said nanoscale particles being configured to form nanoscale morphologies, based on the total weight of the composition, and:
1-50% by total weight of the composition of a biocompatible material, or 0.1-20% by total weight of the composition of a bioactive material, or a combination thereof,
wherein the polymeric material and the biocompatible material or/and the bioactive material are present in the composition as a micron-sized mixture;
the composition is in powder form;
the high polymer material is a high polymer material of paint, resin and adhesive; the biocompatible material is selected from bioinert ceramics, medical metal materials or medical metal oxides; the bioactive material is selected from bioactive ceramic materials or mineral materials;
the nano-scale particles are titanium dioxide, silicon dioxide or aluminum oxide.
28. The method of claim 27, wherein the bioactive material is selected from the group consisting of calcium phosphate-based bioceramics, tricalcium silicate, dicalcium silicate, calcium hydroxide, MTA, and hydroxyapatite.
29. The method of claim 27, wherein the biocompatible material is selected from the group consisting of oxide ceramics, Si3N4 ceramics, glass ceramics, medical grade carbon materials, metallic titanium, titanium alloys, titanium dioxide, calcium oxide, or zirconium oxide.
30. The method of any one of claims 27-29, wherein the coating is formed by a powder spray process of the composition on the surface of the implant.
31. The method of any one of claims 27-29, wherein the polymeric material is selected from the group consisting of epoxy, polyacrylate, polyurethane, polyester, and mixtures thereof.
32. The method of any one of claims 27-29, wherein the bioactive material is MTA.
33. A coating composition for improving biocompatibility of an implant, comprising:
a polymeric material in an amount of 30-90% by weight of the total composition, and
0.1-10% by weight of the total composition of nanoscale particles intended to form nanoscale morphological structures, and:
1-50% by total weight of the composition of a biocompatible material, or 0.1-20% by total weight of the composition of a bioactive material, or a combination thereof,
wherein the polymeric material and the biocompatible material or/and the bioactive material are present in the composition as a micron-sized mixture;
the composition is in powder form;
the high polymer material is a high polymer material of paint, resin and adhesive; the biocompatible material is selected from bioinert ceramics, medical metal materials or medical metal oxides; the bioactive material is selected from bioactive ceramic materials or mineral materials;
the nano-scale particles are titanium dioxide, silicon dioxide or aluminum oxide.
34. The composition of claim 33, wherein the bioactive material is selected from the group consisting of calcium phosphate-based bioceramics, tricalcium silicate, dicalcium silicate, calcium hydroxide, MTA, or hydroxyapatite.
35. The composition of claim 33, wherein the polymeric material is selected from the group consisting of epoxy, polyacrylate, polyurethane, polyester, and mixtures thereof.
36. The composition of claim 33, wherein the biocompatible material is selected from the group consisting of oxide ceramics, Si3N4 ceramics, glass ceramics, medical grade carbon materials, metallic titanium, titanium alloys, titanium dioxide, cobalt oxide, calcium oxide, or zirconium oxide.
37. The composition of any one of claims 33-36, wherein the bioactive material is MTA.
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| CN101491693A (en) * | 2008-09-23 | 2009-07-29 | 西北有色金属研究院 | Preparation method of hydroxylapatite/titanic oxide composite biological coatings |
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| CN101491693A (en) * | 2008-09-23 | 2009-07-29 | 西北有色金属研究院 | Preparation method of hydroxylapatite/titanic oxide composite biological coatings |
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