Multicomponent bioactive nanocomposite coating with antibacterial effect

FIELD: chemistry.

SUBSTANCE: coating is based on titanium carbonitride with addition of additional elements which provide the required set of mechanical and tribological properties, as well as biologically active and antibacterial properties. Overall concentrations of basic and additional elements are in the following ratio: 1,2 < X i Y j < 20, where Xi is the overall concentration of basic elements Ti, C, N in the coating, Yj is the overall concentration of additional elements Ag, Ca, Zr, Si, O, P, K, Mn in the coating.

EFFECT: coating has high hardness, low modulus of elasticity, high value of elastic recovery, low coefficient of friction and rate of wear in different physiological media.

1 tbl, 2 ex

 

The invention relates to medical equipment, namely to biocompatible wear resistant nanocomposite thin-film materials used as coatings in the fabrication of implants designed to replace damaged areas of bone tissue: orthopedic and dental implants, the implants used in maxillofacial surgery and spine surgery, artificial joints, clamps, etc. These materials should possess high strength, wear and corrosion resistance, bio and antibacterial activity.

Known biocompatible coating based on titanium nitride and carbide sodium (SU 1803096, publ. 23.03.93) in the following ratio, wt.%:

the titanium nitride - 20-50

the titanium silicide - 2-5

hydrogenated carbide sodium 25-30

oxides of silicon - rest.

This coating has high adhesion strength plastic with a metal base in prosthetic dentistry, however, has a sufficiently high wear resistance required for a long service life and the required osteoinductive properties.

Known biocompatible coating with an amorphous layer of gidroksiapatita and titanium (US No. 6344276, publ. 05.02.02).

This coating has an increased strength of its connection with the substrate and a low dissolution rate of the material pok is itia, however, it does not possess the whole complex of physical, mechanical, chemical and biological properties required for the material of the implant, working under load.

The prototype of the claimed invention are biocompatible multicomponent nanostructured coatings for medicine (RU 2281122, publ. 10.08.06) - based carbonitride with the introduction of additional elements which improve the mechanical and tribological properties of the coatings, as well as providing its bioactivity and biocompatibility, at a certain ratio of the total concentrations of major and minor elements. The concentration of elements in the coating is selected when the following ratio of components, at.%: Ti 30-50, C 15-40, N 0.5-30, O 5-25, Sa 0-7, Zr 0-20, Si 0-30, P 0-1 .5, Mn 0-1 .0, 0-1 K .0.

The disadvantages of this coating is that it has no antibacterial properties.

The invention achieves the technical result consists in making the coatings of a new quality - antibacterial activity - while maintaining good biocompatibility and high bioactivity, as well as provide a set of good mechanical and tribological characteristics: high hardness, low modulus, high elastic recovery, low friction coefficient and wear rate at different physiologist is economic environments.

This technical result is achieved as follows.

Multicomponent nanocomposite coating for metal, polymer and natural bone implants designed to replace damaged areas of bone tissue. The coating is made on the basis of titanium carbonitride with the introduction of additional elements that provide the desired set of mechanical and tribological properties as well as bioactive and antibacterial properties.

Total concentrations of major and minor elements have the following relationship:

1,2<XiYj<20,

where Xi- the total concentration of major elements of Ti, C, N in the floor,

Yj- total concentration of the additional elements Ag, Ca, Zr, Si, O, P, K, Mn in the coating.

The concentration of elements in the coating is selected when the following ratio of components, at.%:

Ti - 25-50

C - 15-40

N - 0.5-35

O - 5-25

Ca - 0.5-7

Zr - 0-20

Si - 0-30

P - 0.1-1.5

Mn - 0-1 .0

K - 0-1 .0

Ag - 0.3-8.0.

The necessary combination of physical, mechanical, tribological and biological properties of the coating is achieved by inclusion in the composition of the thin film materials of the components if the natural enemy ratios, above. This leads to the formation of a nanocomposite structure in which each structural component plays a specific role: the titanium carbonitride, including doped Zr, provides high hardness, wear and corrosion resistance; Si, Ca, P, O, K and Mn form an amorphous phase, which provides a bioactive surface characteristics, the excess carbon in the form of diamond-like structures leads to a decrease of the coefficient of friction, and the presence of silver in the form of metal or oxide phases gives the material an antibacterial effect, which is due to release from the surface of silver ions, resulting in the suppression of bacterial growth and death.

Coating deposition in argon leads to the formation of coarse columnar structure with high porosity. Introduction in the coating composition of nitrogen leads to grinding and compaction patterns, and in some cases to a complete suppression of the growth column structure. The roughness of the coatings decreases with the introduction of nitrogen in the coating composition.

The optimal upper limit of the nitrogen content in the coating equal to 35 at.%, leads to the substitution of the nitrogen atoms of carbon atoms in the metallic sublattice of a face-centered cubic phase, and the excess carbon is emitted in the form of diamond or graphite-like carbon, which leads to additional the decrease of the coefficient of friction.

A further reduction in friction is achieved as a result of the choice of the lower limit of the concentration of titanium equal to 25 at.%.

The optimum ratio of the metal (Me) and non-metallic elements (NMe) Me/NMe=1.0-1.7, in which the main phase of the coating has a cubic NaCl-type structure.

Any infection in the area of operation is one of the main problems associated with implants. It is known that silver is bactericidal component, however, under certain, often high concentrations may lead to negative impact is the destruction of living cells. The introduction of silver in the indicated ranges of 0.3-8 at.% gives the coating a new quality - they acquire an antibacterial effect, preserving bioactive properties. While silver can be dissolved in solid solution, and to stand out as individual metal particles in the coverage volume.

Supplements of silver do not change the high mechanical and tribological behavior of the coatings, in particular hardness is 16-28 GPA, the modulus of elasticity is in the range 185-230 GPA, a coefficient of friction not greater than 0.27, and the wear rate of less than 3×10-6mm3N-1m-1. When this coating retains its bioactive characteristics.

Bioactive properties of the surface contacted by the formation of hydroxyl functional groups on the negatively charged surface of bioactive ceramics in the internal environment of the organism. For this coating are introduced elements such as CA, P and O in the claimed amount. The presence of calcium ions stimulates the growth of cells on the implant surface. The increase in the content of CA, P and O more than the claimed amount leads to reduction of mechanical and tribological properties of coatings, as well as to the destruction of the actin cytoskeleton of cells.

In the whole investigated range of pH values (4,5<pH<9) surface coating has a negative charge. This means that the surface coatings can attract positively charged ions of CA2+that are in the internal environment of the body that promotes formation of the first intermediate calcium-bearing phases, and then a layer of hydroxyapatite, which is a stable phase in the physiological environment.

Introduction in the coating composition of elements (CA, Zr and leads to a significant reduction of the friction coefficient to 0.17-0.25 compared to coatings on the basis of carbide (CTD.=0.85) or nitride (CTD.=0.55) titanium.

Attachment of cells to the implant surface is determined by the formation of integrin-mediated focal contacts in cells from the subject surface. Silicon increases the activity of osteoblasts and the formation of a layer of Apatite. When its content is less than 30 at.% coatings have a single-phase face-centered cubic structure type NCl, which has a positive effect on the mechanical and tribological properties.

The claimed technical result can be achieved by introducing into the composition of the coatings of additional elements Ag, Ca, Zr, Si, O, P, K, Mn in different ratios according to the formula1.2<XiYj<20where Xi=Ti, C, N and Yj=Ag, Ca, Zr, Si, O, P, K, Mn.

These elements in the coating composition may be introduced through the precursor, for example, by doping the composite cathode target, using by ion-plasma and/or ion-beam sputtering, and/or electrodes, through which the spark deposition. As alloying apply the following inorganic additives: CA10(PO4)6(OH)2Ca3(PO4)2, CaO, Si3N4, ZrO2, KMnO4and TiO2entered in shytobuy mixture at the stage of production of composite cathodes target and electrodes.

Composite target and the electrodes can be obtained by the method of self-propagating high temperature synthesis (SHS). Unlike other known methods of producing composite cathodes and electrodes of refractory compounds (press the ENT-sintering, gas-static pressing, thermal spraying and other) technology SVS has the following advantages: self-cleaning of combustion products from harmful soluble and adsorbed impurities as a result of the high temperatures (2500-3000°C) and the rate of burning (2-10 cm/s)developed in the combustion wave SHS-systems, achieving high values of relative density (97-99%) of ceramic materials and refractory compounds at relatively low pressing pressures; obtaining metastable States is supersaturated solid solutions; obtaining functional gradient materials (Levashov E.A., Rogachev A.S., Kubatkin CENTURIES, Maksimov, Y.M., Yukhvid V.I. Perspective materials and technologies of self-propagating high temperature synthesis. The tutorial. ISBN 978-5-87623-463-6, 2011, the Publishing house Misa, 377 S.).

The main technological advantage of the coating is the presence of a complex of properties required for materials of implants operating under load:

- high hardness N=16-28 HPa,

- low modulus of elasticity E=185-230 HPa,

- low coefficient of friction µ=0.18-0.27,

low speed wear Vw- less than 2.7×10-6mm3/Nm,

- hydrophilic surface characteristics

- no destruction of the actin cytoskeleton of cells cytocompatibility,

- cash is having bioactive surfaces higher alkaline phosphatase activity compared to the control during the cultivation of osteoblasts,

the presence of antibacterial effect, at least 30% compared to control.

Low modulus of elasticity of the coating is favorable from the viewpoint of reducing stresses between the coating and the implant, which is often used stainless steel E=190-200 HPa or titanium E=116 GPA. The low young's modulus also leads to better transfer of bone functional loads and stimulates the growth of bone tissue. The combination of high hardness and elastic recovery characterizes the coating as a unique firm, and at the same time, the elastic material that is the most important factor for medical supplies, working under load.

The deviation of at least one of the above properties of coatings entails the loss of the performance characteristics of all the products of the implant as a whole.

Examples of specific embodiment of the invention.

Example 1

Technological cycle of obtaining multicomponent bioactive nanocomposite coatings with antibacterial effect TiCaP-CON-Ag consists of two main stages: the production of composite target TiC0.5+Ca3(PO4)2the method of self-propagating high temperature synthesis (SHS) and its subsequent magnet is as a spray in one technological cycle with a sputtering target made of pure silver on the substrate. The sputtering target of Ag was carried out at an ion current of 50 mA, a voltage of 1 kV and the aperture diameter 6 mm

The deposition of the coating TiCaPCON-Ag was carried out in a gaseous environment Ar+N2at a partial pressure of nitrogen is 14%. The resulting coating of the following composition, at. %:

C - 31.8

O - 5.1

N - 31.9

Ti - 28.1

Sa - 1.3

P - 0.6

Ag - 1.2

For measuring physico-mechanical and tribological properties of coatings deposited on a substrate of titanium alloy grades W, 1-0.

Physico-mechanical and tribological properties of MNP was determined using the following high-precision devices: Anotherdomain (Nano-Hardness Tester, CSM Instruments, Switzerland); Scratch-tester (Revetest, CSM Instruments, Switzerland); friction Machine (Tribometer, CSM Instruments, Switzerland); Optical AXIOVERT microscope equipped with digital camera and image analysis (Karl Zeiss, Germany). The hardness and elastic modulus were determined according to the method of Oliver and Headlight [G.M. Pharr, W.C. Oliver, F.R. Brotzen. J. Mater. Res. 3, 613 (1992)] using the indenter of the named Berkovich.

The amount of elastic recovery (Wecoating was calculated by curve loading - unloading by the formula: We=(hmax-hr)/hmaxwhere hmax- the maximum depth of penetration of the indenter, a hrresidual depth after removal of the load. The friction coefficient and wear rate of the coatings was measured using machines the friction on the ball - disk at a load of 1 N and a linear velocity of 10 cm/s Tests were carried out in saline solution (100 ml H2O + 0.9 g NaCl). As counterbody was used stationary ball of sintered Al2O3with a diameter of 3 mm.

The resulting coating had a hardness of 16 GPA, the modulus of 190 GPA, elastic recovery of 51%, the friction coefficient is 0.21 and the wear rate of 2.5×10-6mm3/Nm. Wetting angle was 53°.

As model systems in biological research were used osteoblasts line MC3T3-E1 cultured on the surface of the tested materials. Adhesion of cells with subsequent rasplachivayas on the surface of the substrate is the first phase of interaction between cells and the implant and therefore the quality of this first phase is crucial for the biocompatibility of the material. Morphometric analysis area rasplastyvanija cells on the surface of the coatings showed that osteoblasts well was sprawled on the surface of the tested samples. Immunomorphological study of the actin cytoskeleton showed that the destruction of the actin cytoskeleton of the cells does not occur.

Using a quantitative colorimetric method using as a marker of early differentiation marker, alkaline phosphatase also assessed the ability of p. the floor to influence the differentiation of osteoblastic MC3T3-E1 when their growth in differentiating medium. Studies have shown that osteoblasts growing on the surface TiCaPCON-Ag are able to differentiate. After two weeks of culturing MC3T3-E1 osteoblasts quantitative colorimetric analysis showed a higher level of alkaline phosphatase activity in the cells growing on the surface compared to control.

As test cultures of microorganisms for research bacteriostatic and bactericidal activity of the coatings used were single-celled yeast Saccharomyces cerevisiae (S.cerevisiae) and gram-positive lactic acid bacterium Lactobacillus acidophilus (L.acidophilus). Bacteriostatic activity was estimated by the method of diffusion in agar and method coincubation samples in suspension of microorganisms. Estimated change in absolute concentration of yeast fungi and bacteria over time. After 2 days, the concentration of yeast fungi decreased by 55% compared with control and concentration of bacteria L.Acidophilus in 1 ml of the solution decreased 2.5 times.

Example 2

Changed modes sputtering of silver. The sputtering target of Ag was carried out at an ion current of 50 mA, a voltage of 2.5 kV and the aperture diameter 16 mm

The resulting coating of the following composition, at. %:

C - 30.4

O - 7.0

N - 25.8

Ti - 32.3

Ca - 1.5

Ag - 3.0

The resulting coating had a hardness of 28 GPA, moulopoulos 230 GPA, elastic recovery of 68%, the coefficient of friction of 0.18 and wear rate of 2.7×10-6mm3N-1m-1.

The destruction of the actin cytoskeleton of the cells was not detected. Studies in vitro showed that the coating TiCaPCON-Ag is biocompatible and shows the level of alkaline phosphatase activity by 30% more than in the control, indicating its bioactive characteristics. The coating possessed antibacterial effect: after 2 days, the concentration of S.cerevisiae yeast fungi decreased by 35% compared with control and concentration of bacteria L.Acidophilus 21%.

Examples 3-18

To optimize the composition of the coatings were carried out numerous experiments on the deposition of coatings using different cathodes target.

Table 1 summarizes the research results and properties of the coatings, confirming the validity of the claimed coating compositions.

Coatings have one or more competitive advantages necessary for implant materials, working under load: high hardness; low modulus; low friction coefficient and wear rate; high resistance to elastic and plastic deformation; biocompatibility, bio and antibacterial activity.

Multicomponent of Nanak positionne coating for metal, polymer and natural bone implants designed to replace damaged areas of bone tissue, based on titanium carbonitride with the introduction of additional elements that provide the desired set of mechanical and tribological properties as well as bioactive and antibacterial properties, in the following ratio of the total concentrations of major and minor elements:
1,2<XiYj<20,
where Xi- the total concentration of major elements of Ti, C, N in the floor,
Yj- total concentration of the additional elements Ag, Ca, Zr, Si, O, P, K, Mn in the floor,
the concentration of elements in the coating is selected when the following ratio of components, at.%:
Ti - 25-50
- 15-40
N - 0.5-35
On - 5-25
Ca - 0.5-7
Zr - 0-20
Si - 0-30
R - 0.1-1.5
Mn - 0-1 .0
K - 0-1 .0
Ag - 0.3-8.0.



 

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SUBSTANCE: membrane is made of a tetrafluoroethylene copolymer with functional perfluorinated comonomers of the general structural formula: where R: (D), (E), (K), M-H, Li, K, Na; a=24.75-18.38 mol.%; b=78.62-81.12 mol.%; c=5.0-0.5 mol.%; and is from 10 mcm and higher thick, density is 1.93-2.10 g/cm3, mechanical strength is 16-22 MPa and a coefficient of gas permeability by hydrogen (K) is 1-3.7×10-16 m3m m-2Pa-1s-1 at 20-90°C. A method of obtaining consists in combination of a porous polytetrafluoroethylene film with a perfluorosulphocationite polymer in a medium of an organic or a water-organic solvent in the presence of a modifier. The modifier is represented by hydrocarbon polymers, fluoropolymers, perfluoropolymers or their mixtures, inorganic compounds or their mixtures.

EFFECT: high drops of pressure, high current density and efficiency of an electrolysis cell exploitation.

13 cl, 3 tbl, 28 ex

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

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