Method for preparing nanostructured calcium-phosphate coating for medical implants

FIELD: medicine.

SUBSTANCE: what is described is a method for preparing a nanostructured calcium-phosphate coating for medical implants consisting in sputtering a target of stoichiometric hydroxyapatite Ca10(PO4)6(OH)2 in high-frequency magnetron discharge plasma in the argon environment under pressure of 0.1-1 Pa and target power density of 0.1-1 W/cm2 for 15-180 min at a distance from the target to a carrier within the range of 40 to 50 cm, wherein the nanostructure is formed after a coating procedure in the process of the controlled thermal annealing at a temperature of 700-750°C for 15-30 min.

EFFECT: higher post-coating effectiveness of the production process.

4 dwg

 

The invention relates to medical technology and concerns a method for obtaining nanostructured thin film of calcium phosphate coatings for medical implants that can be used in traumatology, orthopedics and dentistry.

Implants made of titanium and its alloys are widely used in dentistry and orthopedics [Dorozhkin S.V. Calcium orthophosphates // J.Mater. Sci. - 2007. - V.42. - P.1061-1095.]. Recently actively implemented implants of alumina ceramics [Gaydash A.A., O. Medvedko, Aronov, A.M., V.F. Pichugin, Berkin A.B., and other Structural and physico-chemical mechanisms of consolidation of bone tissue with Al2O3-ZrO2ceramic coated by magnetron sputtering mechanosensation hydroxyapatite. Proceedings of the III international scientific-practical conference "Modern ceramic materials. Properties. Technology. Application (Keremcem-2011)", September 14-16, 2011, Novosibirsk, Nonpareil, 2011, p.11-19.]. The problems associated with improving the biocompatibility introduced into the body material and the fixation of the prosthesis in the bone tissue, accelerating the healing process, increase the service life of the implant, are successfully solved by applying to the surface of a bioactive resorbable coatings of hydroxyapatite (HA) (ISO 13779-2:2008 [ISO 13779-2:2008 Implants for surgery. Hydroxyapatite. Part 2. Cover ishigakijima http://ww.iso.org/iso/ru/iso...file:///catalogue_tc_browse.htm?.]).

The presence of the coating of HA on the surface of the implant activates the processes of osteosynthesis and leads to rapid formation of bone tissue. Maximum biological activity have polycrystalline coating, the structure of which is as close to the biological HA [Yang Y., Kim, K.-N., Ong J.L. A review on calcium phosphate coatings produced using a sputtering process-an alternative to plasma spraying // Biomaterials. 2005. - V.26. - N.3. P.327-337.; Y. Chou, W.Huang, J.C.Y.Dunn, T.A.Miller and .M.Wu, "The effect of biomimetic apatite structure on osteoblast viability, proliferation, and gene expression", Biomaterials, vol. 26, pp.285-295, 2005/1].

A method of obtaining calcium-phosphate coating using RF magnetron sputtering on medical implants [K. van Dijk, H.G.Schaeken, J.C.G.Wolke, C.H.M.Maree, F.H.P.M.Habraken, J. Verhoeven, J.A.Jansen Influence of discharge power level on the properties of hydroxyapatite films deposited on Ti6A14V with RF magnetron sputtering, J. of Biomedical Materials MResearch, v.29, 269-276, 1995], which consists in spraying a ceramic target of HA in the plasma of RF discharge power 200-800 watts at an operating pressure of argon 0.1-1 PA at a temperature of samples 50-550°C.

The disadvantage of this method is the dependence of the composition and structure of the coatings on the locations of the samples relative to the target power in the discharge and temperature of samples.

A method of obtaining calcium phosphate coatings for medical implants [Xu, S., Long, J., Sim, L., Diong, C.H., Ostrikov, K., RF Plasma Sputtering Deposition of Hydroxyapatite Bioceramics: Synthesis, Performance, and Biocompatibility. Plasma Proc. Poly., 2005. 2 p.373-390], which is in the sputtering composite target containing hydroxyapatite - Ca10(PO4)6(OH)2(HA) with the ratio of calcium to phosphorus (Ca/P) 1,67 and titanium plasma-frequency (RF) discharge capacity of 700 watts at an operating pressure of argon in the vacuum chamber of 1.2-10 PA at a distance of 60 mm between the target and the samples at negative bias polictial 0-100 (0 corresponds to the case of grounded podarkticules) for 15-120 minutes.

The disadvantage of this method is the continued dependence of the composition and structure of the coatings on the locations of the samples relative to the target.

As a prototype the selected method of obtaining calcium phosphate micro/nanostructures on the sample [RF Patent №2421245, OH, MPK7: A61L 27/12 (2006.01), A61F 2/02 (2006.01) Application: 2010117527/15, 30.04.2010], which consists in sputtering of a target of hydroxyapatite Ca10(PO4)6(OH)2in the high-frequency plasma discharge in a vacuum chamber in an argon atmosphere at a pressure of argon from 0.1 to 1 PA during 15-180 min at a distance from the target to the substrate in the range from 40 to 50 mm Distinguishing feature is that the micro/nanostructured coating to form a negative offset on polictial samples at a density of high-frequency discharge from 0.1 to 0.5 W/cm2in the atmosphere or argon, or oxygen

The disadvantage of the proposed method is partial (5-27%) and uncontrolled degree of crystallization of the coating depends on the negative bias on polictial, but also on the location of the samples relative to the target power in the discharge and temperature of the sample. This disadvantage makes the process not technology for production, since such a process does not ensure reproducibility of results and the creation of a homogeneous coating with a given structure on the entire surface of the sample.

Object of the present invention is to improve the technological process of production of nanostructured calcium phosphate coatings for medical implants.

The problem is solved by a method for production of nanostructured calcium phosphate coatings for medical implants, in which the sputtering target of stoichiometric HA plasma RF magnetron discharge in argon atmosphere with a pressure of 0.1-1 PA and a power density on the target is 0.1-1 W/cm2unlike the prototype, the formation of nanostructures is performed after coating by thermal annealing at a temperature of 700-750 ° C for 15-30 minutes

Methods of control of thermal annealing process is well established. Therefore, the proposed method allows to obtain the entire area on which were acquired in controlled, do not depend on parameters of the deposition conditions of homogeneous nanostructured coating having a degree of crystallization of more than 90%.

Figure 1 shows diffraction spectra SI: 1 - target, 2 - HA (JCPDS - 09-0432).

Figure 2 shows the diffraction patterns of coatings on ceramics (a) and silicon (b) in the annealing process; * - peaks of the ceramic substrate.

Figure 3 shows the diffraction patterns of coatings on various substrates after annealing to 700°C: (a - si; b - ceramics; - pure titanium; g - oxidized titanium; d - HA (JCPDS 09-432).

Figure 4 shows photographs of the surface morphology of the coatings on ceramics (a) and silicon (b).

The inventive method is implemented using industrial installations high-frequency magnetron sputtering MRH 014. The process was carried out at a pressure of argon 0.1-0.3 PA. The frequency of the RF generator 13.56 MHz, the power in the discharge of up to 1 kW. The rate of deposition of the film (5-6) nm/min

Target served as a ceramic disc of compacted at a temperature of 1000°C powder stoichiometric hydroxyapatite (Ca10(PO4)6(OH)2).

As substrates for the study of the composition and structure of the coatings was used porous alumina-Zirconia ceramics, titanium brand Ti6Al14V and oxidized titanium brand Ti6Al14V. Development of research methodology and test analyses were performed on polished square is Stino monocrystalline silicon.

The peculiarity of the method, RF magnetron sputtering is a large dependence of the thickness, composition and structure of calcium-phosphate coating on the location of the substrate relative to the target [K. van Dijk, H.G.Schaeken, J.C.G.Wolke, C.H.M.Maree, F.H.P.M.Habraken, J. Verhoeven, J.AJansen Influence of discharge power level on the properties of hydroxyapatine films deposited on Ti6A14V with RF magnetron sputtering, J. of Biomedical Materials Research, v.29, 269-276, 1995Shuyan Xu, Jidong Long, Lina Sim Cheong Hoong Diong, Kostya (Ken) Ostrikov RF Plasma Sputtering Deposition of Hydroxyapatite Bioceramics: Synthesis, Performance, and Biocompatibility Plasma Process. Polym. 2005, 2, 373-390. Surmenev P.A., Armenia V.F., V.F. Pichugin, Epple M RF-magnetron calcium-phosphate coatings on materials for medical implants. Bulletin of the Tomsk Polytechnic University. 2009. t. No. 2, str-141]. So for spraying in the proposed method, the samples are placed during deposition on a rotating polictial. The speed of rotation of samples of 5-10 rpm Variation in thickness and composition of the films was less than 5%.

Structural studies of calcium-phosphate coatings made in the center for synchrotron radiation (SR) BINP. The radiation wavelength was 1.516 nm. Film thickness ~ 1 µm. To identify spectra were used JCPDS data [The International Centre for Diffraction Data (ICDD) Diffraction Data (ICDD), (Database of the Joint Committee on Powder Diffraction Standards (JCPDS)). http://rapidog.com/jcpds-database-rapidshare.html].

The surface morphology of the coatings was controlled by the method of scanning electron mi is roscopy on the high-resolution microscope Mira 3 (Tescan) and Hitachi S-3400N with energy dispersive x-ray analyzer (EDX-spectroscopy) - INCAx-Sight model 7940 (Oxford). To determine the elemental composition of the coatings selected energy analyzing electron beam of 10 Kev.

Properties of the formed coating are determined by the target material and mode of deposition. The structure and composition of the target material (figure 1) corresponded to the composition and structure of the powder stoichiometric hydroxyapatite Ca10(PO)6(OH)2used for pressing. Table 1 shows the results of EDX analysis of the composition of the target (in parentheses indicate the range of measurements).

Table 1
The original composition of the targetThe area of erosionThe center of the target
Ca/PCa/P
To start working1.65(1.6-1.7)
After 20 hours of operation1.73(1.61-1.85)1.71(1.7-1.73)

Table 2 shows the results of the study of the composition of the coatings obtained on different substrates and in different modes of deposition. When the coating on the substrate opposite the zone of erosion of the target, the calcium content is only slightly greater than stechiometric is s (Ca/P~1.7), if using a rotation ratio Ca/P is increased to ~ 1.9 - 2.1.

Crystal structure of the coatings is an important factor determining the behavior of cells on the implant surface, in particular the formation and fixation of cells on the surface of the film, proliferation and differentiation of cells on it. It is shown that amorphous HA proliferation and differentiation of cells is not observed. Good biological effect when tested in vitro and in vivo was observed for polycrystalline calcium phosphate coatings [Y. Yan, J.C.C. Wolke, A.De Ruijter, Li Yubao, J.A.jansen Growth behavior of rat bone marrow cells on RF magnetron sputtered hydroxyapatite and dicalcium pyrofosphate coatings J.of Biomedical Materials Research part A DOI 10,1002/jbm.a - . DOI: 10,1002/jbm.a.30665].

Table 2
No. p.pThe substrate materialCa/PThe condition of the substrate
No. 1Ceramics tight2,10rotation
No. 2Titanium oksidirovanii2,09rotation
No. 3Porous ceramics171 without rotation
No. 4Titanium onsiderably1,73without rotation
No. 5Porous ceramics2,01rotation

The formation of the crystal structure was investigated in sito during thermal annealing in air by the method of diffraction of synchrotron radiation.

The experimental results for implants made of ceramics is presented in figure 2. For comparison, there is shown the dynamics of crystallization coatings on silicon.

Directly after deposition, the coating thickness of 1 μm is practically amorphous, the degree of crystallization does not exceed 20-25%. There are only characteristic of the HA line spectrum corresponding to the reflection from the crystallographic planes 2Θ=25,8 (002), 31,7 (211), 32,2 (112). Changes in the spectra appear at temperatures of ~ 400°C, and the active crystallization coverage begins at 520...530°C. At 700°C the coating structure is formed and will not change later. The dwell time at a temperature of 700°C was 15-20 minutes are pretty much all peaks corresponding to the structure of the polycrystalline HA (JCPDS-09-432) [The International Centre for Diffraction Data (ICDD) Diffraction Data (ICDD), (Database Joint Comittee on Powder Diffraction Standards (JCPDS)). http://rapidog.com/jcpds-database-rapidshare.html]. The degree of crystallization of 90%. The in vivo experiments show that the best biological response observed in the coatings, the degree of crystallinity which is at least 70...80% [Shuxin Qu, Hong Song Fan, Jiyong chen, Jiamin Feng. Effect of the crystallinity of calcium phosphate ceramics on osteoblast proliferation in vitro. // Journal of Materials Science Letters, 2001. - Vol.20. - P.331-332].

At a temperature of about 400°C the diffraction pattern appears diffraction peak (29=36.5°), which corresponds to calcium oxide (CaO). The presence of calcium oxide, probably due to the excess of calcium in the films compared to stoichiometric. Peaks other calcium phosphate compounds, which are products of the decomposition of HA was not found.

The results of the study of the structure of the coatings after annealing at 700°C) on different substrates (ceramics, titanium, silicon) is shown in figure 3. In all cases, the coating corresponds to synthetic hydroxyapatite with hexagonal type crystal lattice. Small differences in the ratio of intensities of peaks HA for different substrates can be attributed to the capture spectra at different surface morphology.

Fine structure of the surface of the films were investigated by SEM, high resolution (figure 4):

is formed at the initial stage of crystallization of the amorphous phase HA microparticles have a size of 20 nm wide and 60 nm in D. the inu and consist of smaller particles with a size of 10-20 nm;

- during subsequent annealing, the growth and coalescence of particles with dense agglomerates with a size of 200×1000 nm, consisting of nanoparticles with a size of 10-100 nm.

The results prove the following General regularities of formation of structure of HA coating on various materials for medical implants:

- regardless of the material and surface morphology of the substrate (porous ceramics, titanium porous oxide coating, pure titanium) the main component patterns (over 85%) of calcium-phosphate coatings obtained by means of RF magnetron sputtering, after annealing at 700°C is hexagonal synthetic hydroxyapatite, the corresponding JCPDS-09-432;

- the dynamics of structural change in the coatings during annealing is practically the same for all investigated materials of the substrate;

the grain size of polycrystals is 10-100 nm, which corresponds to the size of the crystals of natural bioapatite bone tissue according to the microdiffraction C [Rindby, A., P. Voglis, Engstrom P. Microdiffraction studies of bone tissues using synchrotron radiation // Biomaterials. - 1998. - V. 19. - P.2083-2090];

- composition and structure of the resulting layer correspond to the ISO 13779-2:2008, defines the requirements for the coatings of hydroxyapatite for medical implants.

Thus, the proposed method provided achival the implementation of technological repeatable process for production of nanostructured calcium phosphate coating on the entire surface of the sample, which meets the requirements of international standard ISO 13779-2:2008, defines the requirements for coatings for medical implants. The coating structure is formed regardless of the coating during subsequent controlled thermal annealing at a temperature of 700-750°C for 15-30 minutes

The method of obtaining nanostructured calcium phosphate coatings for medical implants, in which the sputtering target of hydroxyapatite Ca10(PO4)6(OH)2in the high-frequency plasma discharge in a vacuum chamber in an argon atmosphere at a pressure of argon from 0.1 to 1 PA during 15-180 min at a distance from the target to the substrate in the range from 40 to 50 mm, wherein the nanostructure formation is performed after coating by thermal annealing at a temperature of 700-750aboutC for 15-30 minutes



 

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1 tbl, 1 ex, 2 dwg

FIELD: medicine.

SUBSTANCE: there is described method of obtaining of calcium phosphate nanoparticles, stabilised by salt matrix by interaction of components, first of which contains metal cation, and second contains anion. According to invention as the first component applied is water-soluble calcium salt, and as the second component, soluble orthophosphate, nanoparticles of water non-soluble calcium phosphate being formed, and salt matrix being formed from soluble by-product. Content of calcium phosphate nanoparticles in powder composite "oxide nanoparticles/salt matrix" constitutes 65-82 wt %.

EFFECT: method is aimed at creation of effective nanotechnologies, in order to prevent degradation, that is, aggregations of oxide nanoparticles of calcium phosphates.

5 tbl, 4 ex

FIELD: medicine.

SUBSTANCE: what is described is an umbrella device (occluder) with a modified coating layer for the left atrial appendage occlusion. The umbrella device (occluder) with the modified coating layer is made from a titanium nickelide alloy. It has the coating modified layer having a thickness of 80-95 nm which consists of at least two sub-layers: an external sub-layer having a thickness of 20-25 nm contains oxygen, carbon, silicone and titanium in the following ratio, at %: oxygen 25-65, carbon 1-5, silicone 1-10, titanium - the rest; an intermediate sub-layer having a thickness of 60-70 nm contains oxygen, carbon, silicone, titanium and nickel in the following ratio, at %: oxygen 5-30, carbon 1-5, silicone 10-30, nickel 1-50, titanium - the rest, with silicone reaching its maximum concentration at a depth of 30-35 nm from the surface. The modified coating layer of the umbrella device (occluder) has no evident interface of the sub-layers specific for a deposited layer.

EFFECT: umbrella device with the modified coating layer possesses biocompatibility, corrosive resistance and no toxicity.

9 cl, 2 dwg

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