Method for making intraosseous carbon-nanocoated dental implant

FIELD: medicine.

SUBSTANCE: invention refers to medicine, namely to orthopaedic dentistry. A method for making an intraosseous dental implant involves sand-blast finish of an implant surface by alimunium oxide particles, plasma-based layer-by-layer deposition of a system of biocompatible coatings containing mixed titanium or titanium hydride or calcium hydroxyapatite powders onto an implant carrier. The first layer consists of titanium or titanium hydride of dispersity 3-5 mcm at spraying distance 70-80 mm and thickness 5-10 mcm. The second layer is titanium or titanium hydride of dispersity 50-100 mcm at spraying distance 100 mm and thickness 50-115 mcm. The third layer represents mixed titanium or titanium hydride of dispersity 40-70 mcm and calcium hydroxyapatite of dispersity 5-10 mcm in ratio 60-80 and 20-40 wt % respectively, at spraying distance 80 mm and layer thickness 15 -20 mcm. The forth layer consists of calcium hydroxyapatite of dispersity 40-70 mcm at spraying distance 70 mm and layer thickness 20-30 mcm. Thereafter, the multilayered system of the biocompatible coatings is covered by a metal film consisting of a ferric triad (iron, cobalt or nickel) of thickness 20-35 nm by magnetron sputtering. A carbon nanocoating of thickness up to 1 mcm is prepared thereon. The carbon nanocoating represents carbon nanotubes and carbon nanofibres of diameter 50-200 nm.

EFFECT: method provides making the implant coated so that to promote the active growth of bone tissue.

3 cl, 1 tbl, 4 dwg

 

The invention relates to the field of medical equipment, namely to prosthetic dentistry and can be used in the manufacture of intraosseous implants.

A known method of manufacturing an implant for replacement of bone tissue [RF Patent №2025132, IPC: A61F 2/28], according to which the implant is made of a metal or metal-ceramic alloy in the form of a pin, put a three-layer coating, the first layer contains biostable on the basis of calcium phosphate with the addition of the metal oxide, the second layer is a mixture of calcium phosphate and hydroxyapatite, and the intermediate layer contains calcium phosphate.

However, multi-component coating system (CaP-glass, hydroxyapatite, tricalcium phosphate and the addition of oxides of metals with different coefficients of thermal expansion does not contribute to the strong anchoring of the coating layers (especially the first layer) with a metal implant, the coating also does not have a high bioactivity.

A known method of manufacturing intraosseous dental implant plasmolen multilayer bioactive coating [RF Patent №2146535 IPC: A61L 27/00, A61C 8/00], consisting of plasma spraying method on titanium implant system of coatings of various particle size and thickness, consisting of five layers: the first two from titanium or titanium hydride is, the next two layers of a mixture of titanium or titanium hydride with hydroxyapatite, different content components in layers, and the outer, the fifth layer of hydroxyapatite. The coating layers are in different modes, providing a smooth transition from the compact structure of the titanium bases of the implant through a multi-layer system of the transition of the coating to thin the biologically active surface of the porous layer.

However, when plasma spraying bioactive hydroxiapatite powder lost many of the original chemical properties, which reduces the bioactivity of the coating. In addition, the coating is fragile, so you cannot use it in the manufacture of high-loaded implants.

Closest to the proposed invention is a method of manufacturing intraosseous dental implants [RF Patent №2074674, IPC: A61F 2/28], including the manufacture of metal or alloy in a generic way (lathe, milling and other processing methods or by using special electro-physical methods) basics of implant cylindrical, plate or tubular form, applied to the implant by the method of plasma spray coating system consists of four layers - two layers of titanium or titanium hydride different dispersion and the thickness of the third layer from the milling is eskay mixture of titanium or titanium hydride or hydroxyapatite ratio respectively 60-80 wt.% and 20-40 wt.% and the outer layer is hydroxyapatite.

The disadvantage of this invention is the low bioactivity of the coatings, as after plasma spraying, lost many chemical properties of sputtered bioactive hydroxyapatite powders.

The objective of the invention is to improve the bioactivity of the implant, namely to increase the speed osteointegration processes.

The technical result of the invention is the formation on the surface of the multilayer coating system of the implant carbon coating, contributing to more rapid bone growth, since the carbon nano-coating is the most similar to the crystalline structure of hydroxyapatite natural bone [Kaplan FS, Hayes WC, Keaveny TM, Boskey A, Einhorn TA, Iannoti JP. From and function of bone. In: Simon SR, editor. French Brasserie basic science. Rosemont, IL: American Academy of French Brasserie Surgeons, 1994. p.127-85].

This object is achieved in that in the method of manufacturing intraosseous dental implant with carbon nanocoating, including sandblasting the surface of the implant particles of aluminum oxide, layer-by-layer deposition plasma method on the basis of the implant system of biocompatible coatings of a mixture of powders of titanium or titanium hydride and calcium hydroxylapatite, while the first layer is sprayed titanium or titanium hydride dispersion of 3-5 microns with a spraying distance of 70-80 mm and thickness is th 5-10 μm, the second layer is titanium or titanium hydride dispersion 50 to 100 microns with a spraying distance of 100 mm, a thickness of 50-115 μm, the third layer is sprayed with a mixture of titanium or titanium hydride dispersion of 40-70 μm and calcium hydroxyapatite particle size of 5-10 μm, with a ratio of 60-80 and 20-40 wt.% accordingly, the spraying distance of 80 mm and a thickness of 15-20 μm, the fourth layer sprayed hydroxyapatite calcium dispersion of 40-70 microns with a spraying distance of 70 mm and a thickness of 20-30 μm, according to the proposed technical solution, multi-layered system of biocompatible coatings by magnetron sputtering is applied a film of a metal of the iron triad thickness of 20-35 nm, which receive carbon nanocoating thickness up to 1 mm.

When this carbon nano-coating is a carbon nanotubes and carbon nanofibers with a diameter of 50-200 nm.

The film of metal of the iron triad represents the metals iron, cobalt or Nickel.

The invention is illustrated by drawings, where figure 1 presents the scheme of the layer of coating formation, figure 2 - diagram of the magnetron sputtering figure 3 - installation of the pyrolysis of hydrocarbons, figure 4 - image of a carbon coating, where the positions are marked: 1 - the surface of the metal titanium implant; 2 - the first layer of titanium powder or titanium hydride; 3 - W is Roy the layer of titanium; 4 - the third intermediate layer of a mixture of titanium powder or titanium hydride with hydroxyapatite; 5 - the fourth layer of hydroxyapatite; 6 - implant; 7 - polictial; 8 - clip; 9 - working camera; 10 - magnetron; 11 - catalyst; 12 - valve; 13 - channel pumping atmospheric environment; 14 - gauge; 15 - tube inlet working gas; 16 - plasma glow discharge; 17 - quartz tube; 18 - reactor; 19 - gauge; 20 - cylinder inert gas; 21 - gas reducer; 22 - the device finish drying gas; 23 - device finish cleaning gas; 24 - rotameter; 25 - line power reactor; 26 - cylinder ammonia; 27 - heating element; 28 - thermocouple; 29 - a balloon with carbon-containing gas; 30 - a branch pipe of system of cooling of the reactor.

The proposed method for the manufacture of intraosseous dental implant with carbon nanocoating is as follows (figure 1). The surface of the metal titanium implant 1 before coating is subjected to a blasting treatment with particles of aluminum oxide. Then put two layers of titanium powder or titanium hydride thickness in the range of 60-125 μm at a current plasma arc 540-560 A. the First layer 2 of the titanium powder or titanium hydride dispersion of 3-5 μm sprayed directly on the metal compact implant from a distance of 70-80 mm, a thickness of 5-10 μm. The second layer 3 sprayed titanium or hidri the titanium particle size of 50-100 μm from a distance of 100 mm, the thickness of 50-115 mm. Application of two-layer titanium coating provides a smooth transition from the surface of the metal titanium implant 1 to the second layer 3 and a porosity of 45 to 50%. The third transition layer 4 sprayed a mechanical mixture of titanium powder or titanium hydride dispersion of 40-70 μm and hydroxyapatite particle size of 5-10 μm, with a ratio of respectively 60-80 wt.% and 20-40 wt.%, the thickness of this layer is equal to 15-20 microns. The range of coating composition from a mixture of titanium and hydroxyapatite is selected so as to provide maximum adhesion to plasmolen titanium layer. The deposition of the third transition layer 4 is carried out at the current plasma arc 540-560 and A spraying distance of 80 mm Past the fourth layer 5 sprayed hydroxyapatite dispersion of 40-70 μm and a thickness of 20-30 μm. Current plasma arc 450-540 A spraying distance of 70 mm

Layer-by-layer plasma spray coatings is carried out in a stream of protective inert gas, such as argon, the plasma gas flow is 4-16 l/min moving Speed of the plasma torch during the deposition 80-700 mm/min, the arc voltage 30 B, the rotation speed of the details about 110-160/min

Then a multilayer system of biocompatible coatings by magnetron sputtering is applied a film of a metal of the iron triad, for example, iron, which is the catalyst tol is another 20-35 nm. For this purpose, the implant 6 with a multilayer system of biocompatible coatings fix on polictial 7 clamp 8 (see figure 2) in the working chamber 9 magnetron sputtering system, for example, "VUP-5M" (VLADIMIR Petukhov, Gumarov, "Ion-beam techniques for thin films" 2010 Kazan: Kazan state University). The magnetron 10 installing the catalyst 11, made of iron triad, for example of iron, cobalt or Nickel, tested the operation of the valve 12 and pumped atmospheric environment from the working chamber 9 by using, for example, the booster pump through the channel pumping atmospheric environment 13 to a pressure of 10-4-10-5PA, which is determined using the gauge 14. Then in the working chamber 9 sleuth inert gas, such as argon, through the pipe inlet working gas 15 to the pressure (0.5 to 5)·10-5PA in the working chamber 9 defined using 14 gauge. On the catalyst 11 serves a negative DC voltage, and the implant 6, fixed to polictial 7 clamp 8-positive DC voltage 395-400 B, in the area between the implant 6 and the catalyst 11 occurs inhomogeneous electric field which excites the plasma glow discharge 16 in an inert gas environment. The resulting ions from the plasma glow discharge 16 in an inhomogeneous electric field bombard the catalyst 1, when this happens two main effects: electron emission and sputtering the surface of the catalyst 11.

Issued with catalyst 11 under the action of ion bombardment electrons are accelerated by the electric field and begin to move towards the implant 6 is fixed on polictial 7. When moving electrons make ionizing collision, moving in a constant magnetic field, the atoms of the inert gas until, until you annihilate with plasma glow discharge 16. This cycloidal motion of electrons increases the efficiency of the ionization process, the maximum plasma density in the glow discharge 16 is concentrated near the surface of the catalyst 11. This causes an increase in the intensity of the ion bombardment of the surface of the catalyst 11 and a significant increase in the rate of sputtering and, in the end, and the deposition rate of the atoms of the catalyst 11 on the surface of the implant 6 is fixed on polictial 7 clamp 8.

Sprayed film, the iron triad, for example, of iron, when the discharge voltage 395-400 B, the discharge current of 1-2 A, the pressure of the discharge from 0.6 to 0.66 PA, the inert gas pressure is 0.5-0.6 PA, the time dispersion of the catalyst 11 25-45 sec, the distance between the catalyst 11 and the implant 6 is fixed on polictial 7 clamp 8 costal is no 58-60 mm In the spraying of the catalyst 11, receive a film thickness of 20 to 35 nm and a diameter of catalyst particles of 5-150 nm.

Further, the implant 6 with a multilayer system of biocompatible coatings and sprayed layer of the catalyst 11, which is a metal of the iron triad set in a quartz tube reactor 18 17 installation of chemical deposition from the gas phase (see figure 3) in a vertical position so that the contact surface of the multilayer coating system intrabone 6 with the space of the quartz tube 17 was the greatest. Before you begin, that is, the operation of the synthesis of carbon coating, hollow quartz tube 17 of the reactor 18 is blown with an inert gas, such as argon, to remove atmospheric air, as in a mixture with hydrocarbon gases in the cavity of the tube 17 of the reactor 18 can form an explosive mixture, which is inadmissible under the rules of safety. To do this, using, for example, booster pump, pump the pressure in the cavity of the quartz tube 17 of the reactor 18 to the value of 10-12 kPa by controlling the value using, for example, gauge 19, and then served in the cavity of a quartz tube reactor 18 17 inert gas, such as argon, is fed to the container with the inert gas 20 gas through the gear 21, the device finish drying gas 22, the device of the finish on isdi gas 23, rotameters 24 and the supply line of the reactor 25 with a gas flow rate of 100-150 ml/min, controlled by, for example, flow meters 24, for 10-15 minutes. Then in a quartz tube 17 via the supply line of the reactor 25 of the tank with ammonia 26 serves ammonia, which is required for activation of the catalyst particles 11, sprayed on a multilayer system of biocompatible coatings, the feed rate of the inert gas in a mixture of ammonia is 50-100 ml/min by adjusting the gas flow rate, for example, using a flowmeter 24. Next, increase the temperature of the hollow quartz tube 17 of the reactor 18 to a temperature 650-655°C using heating elements 27, which represents a nichrome wire wound on a quartz pipe 17 controlled by mounted in the cavity of a quartz tube reactor 18 17 thermocouple 28, the rate of increase of temperature of 5-10°C/min

After activation of the catalyst particles 11, switch off the supply of inert gas from the container with the inert gas 20, using, for example, gas reducer 21 or float flowmeter 24. Next, the temperature of the hollow quartz tube 17 is increased to temperature synthesis of carbon nanocoatings 800-810°C, with a rate of 5-10°C/min, then served from a container with a carbon-containing gas 29 through rotameters 24 to the supply line of the reactor 25 carbon-containing gas which enters the cavity of the quartz tube 17 in a mixture with and what MIAK. As a carbon-containing gas using carbon monoxide, various hydrocarbons, including those containing oxygen, such as formaldehyde, acetaldehyde, acetone, methanol, ethanol or their mixture, as well as aromatic hydrocarbons: benzene, toluene, xylene, cumene, ethylbenzene, naphthalene, phenanthrene, anthracene or mixtures thereof, can also be used non-aromatic hydrocarbons, such as methane, ethane, propane, ethylene, propylene or acetylene, or a mixture thereof. As a carbon-containing gas is used, for example, hexane. Synthesis of carbon coating is carried out at a temperature of cavity quartz tube 17 800°C for 5-30 minutes with a ratio of 2:1 mixture of hexane - ammonia, respectively. In the process, the reactor 18 is cooled by water supplied through a branch pipe of system of cooling of the reactor 30 from a public water system.

After synthesis of the carbon coating is cooled cavity quartz tube 17, in an atmosphere of inert gas to room temperature. To do this, shut off the supply of carbon gas and ammonia, using a flowmeter 22 and sleuth from the container with the inert gas 20 inert gas into the cavity of the quartz tube 17 with a gas flow rate of 100-150 ml/min and shut off the heating element 27, which leads to cooling of the reactor 18 and the cavity of the quartz tube 17, which is controlled by means of thermocouples is 28. After cooling cavity quartz tube 17, the reactor 18 to disconnect the supply of inert gas from the container with the inert gas 20 with a gas reducer 21. As a result of receiving the implant 6 with a multilayer system of biocompatible coatings and with a layer of carbon coating thickness up to 1 μm, for example, in the form of carbon nanotubes and carbon nanofibers with a diameter of 50-200 nm.

The table presents the results of studies of the biological activity of the obtained carbon nano-coatings consisting of carbon nanofibers and nanotubes with a diameter of 5 to 250 nm.

Table
The thickness and diameter of carbon nanotubes and nanofibersThe number of cells
With the carbon-
dnim of nanopore-
the Tille
5-20 nm30%
20-40 nm35%
40-50 nm60%
50-100 nm67%
100-200 nm66%
200-220 nm50%
220-250 nm 28%
Without carbon coating25%

The table shows that the highest bioactive effect have carbon coating with a diameter of carbon nanotubes and nanofibers in the range of 50-200 nm, since in this range of diameters manifested the highest percentage entered in the biological relationship living bone cells (number of cells) with carbon nanocoating.

Kinetics of the formation of carbon nanotubes and carbon nanofibers on floured catalyst of the iron triad is as follows: hydrocarbon molecules decompose on the surface of the catalyst particles emitted carbon diffuses into the volume of the catalyst particles until full saturation, resulting in carbon molecules form a structure in the form of carbon nanotubes and carbon nanofibers. The diameter of carbon nanotubes and carbon nanofibers depends on the size of the catalyst particles and the speed of the individual stages of the process.

Choice as a diluent gas of ammonia is due to the properties of the catalyst. For example, the catalyst in the form of iron tends to ageing and partial loss of activity during storage. Thus, the catalyst of iron requires activation (annealing in an inert or in stravitelne environment) immediately before use. Pre-treatment of the catalyst particles of iron ammonia causes a sharp increase in the rate of pyrolysis at 700°C. the Acceleration due to the formation of iron nitride, repair or decomposition which accelerates the process of saturation of the carbon on the catalyst particles.

The surface of the obtained carbon nanocoatings presented at the electron-microscopic image of Fig.4, which shows that the diameter of the resulting carbon nanofibers and tubes is in the range of 50-200 nm. Thus, the proposed solution allows to increase the bioactivity of the coating of implants, namely to accelerate osteointegration processes due to active growth of bone tissue.

1. A method of manufacturing intraosseous dental implant with carbon nanocoating, including sandblasting the surface of the implant particles of aluminum oxide, layer-by-layer deposition plasma method on the basis of the implant system of biocompatible coatings of a mixture of powders of titanium or titanium hydride and calcium hydroxylapatite, while the first layer is sprayed titanium or titanium hydride dispersion of 3-5 microns with a spraying distance of 70-80 mm and a thickness of 5-10 μm, the second layer is titanium or titanium hydride dispersion 50 to 100 microns with a spraying distance of 100 mm, a thickness of 50-115 μm, the third layer is sprayed with a mixture of titanium or is idrica titanium dispersion of 40-70 μm and calcium hydroxyapatite particle size of 5-10 microns with ratio and 60-80 20-40 wt.% accordingly, with the spraying distance of 80 mm and a thickness of 15-20 μm, the fourth layer sprayed hydroxyapatite calcium dispersion of 40-70 microns with a spraying distance of 70 mm and a thickness of 20-30 μm, characterized in that a multilayer system of biocompatible coatings by magnetron sputtering is applied a film of a metal of the iron triad thickness of 20-35 nm, which receive carbon nanocoating thickness up to 1 mm.

2. A method of manufacturing intraosseous dental implant with carbon nano-coating according to claim 1, characterized in that the carbon nano-coating is a carbon nanotubes and carbon nanofibers with a diameter of 50-200 nm.

3. A method of manufacturing intraosseous dental implant with carbon nano-coating according to claim 1, wherein the film of metal of the iron triad represents the metals iron, cobalt or Nickel.



 

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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: invention refers to the method for making bioactive calcium-phosphate coatings and can be used in manufacturing of orthopaedic and tooth prostheses. The method for making supported calcium-phosphate coating involves radio-frequency magnetron sputtering of hydroxyapatite target Ca10(PO4)6(OH)2 during 15-150 min with using argon as a working gas at pressure in a working chamber 0.1 Pa. The coating is settled over a support over a ring of magnetron cathode region, where field lines of magnetron magnetic field localise high-frequency plasma with maximal effect of charged particle on the support at specific power of high-frequency discharge 50 W cm-2 that provides formation of coating composition close to that of stoichiometric hydroxyapatite Ca10(PO4)6(OH)2.

EFFECT: application of the method ensures activation of coating crystallisation during growth with final phase formation that corresponds to composition of the target.

6 dwg, 3 ex

FIELD: medicinal materials, chemical technology.

SUBSTANCE: method for preparing calcium phosphate-base ceramic materials involves interaction of calcium soluble salts and soluble phosphates, separation of deposit, molding articles and their roasting at temperature 1000-1300°C. A deposit of the specific surface value 30-60 m2 is subjected for treatment at temperature 50-60°C with aqueous or alcoholic solution containing ions chosen from the following order: Na1+4, NO1-3, Ca2+, Cl1-, Na1+, OH1-, HCO1-3, K1+, Mg2+, Al3+, Zn2+, F1-, CH3COO1-, CO2-3, SO2-4, PO3-4, HPO2-4 and SiO4-4 in the total concentration of ions in solution 1.6-4.6 M and in the volume ratio "solid phase/liquid" = (1-100):(1-25). Method involves stirring for 30-40 min, or a deposit is subjected for treatment with a solution containing ions taken from the following group: Ca2+, NH1+4, NO1-3, Cl1-, HPO2-4, Na1+, OH1-. Method provides controlling the material thickening process and ceramics microstructure that allows approaching its chemical composition and crystalline structure to natural bone. Invention can be used in medicine in making osseous implants.

EFFECT: improved preparing method, improved and valuable properties of materials.

2 tbl, 4 dwg, 2 ex

FIELD: medicine.

SUBSTANCE: invention refers to a method for preparing a biocompatible nanostructured conducting composite. The method involves preparing an ultra-disperse suspension of carboxymethyl cellulose and carbon nanotubes with the mechanical system of carbon nanotube structuring wherein nanostructuring is enabled by exposing the suspension to laser light in a continuous mode at generation wave lengths 0.81÷0.97 mcm and light intensity 0.5÷5 Wt/cm2.

EFFECT: invention provides preparing the high-conductivity bio-composite.

1 tbl, 1 ex

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