RU2530573C1 - Method for making bioactive coated endosseous implant - Google Patents

Abstract

FIELD: medicine.

SUBSTANCE: what is described is a method for making a bioactive coated endosseous implant involving a layer-by-layer deposition of four layers on a titanium base of the implant; the first layer represents a titanium powder having a dispersion of 3-5 mcm, a deposition distance of 70-80 mm and a thickness of 5-10 mcm; the second layer consists of the titanium powder having a dispersion of 50-100 mcm, a deposition distance of 100 mm, and a thickness of 50-115 mcm; as a third layer, a mechanical mixture of the titanium powder having a dispersion of 40-70 mcm and hydroxyapatite having a dispersion of 5-10 mcm related as 60-80 and 20-40 wt % respectively, with a deposition distance of 80 mm and a layer thickness 15-20 mcm is applied; the fourth layer is a mechanical mixture of bioactive powders of hydroxyapatite of a distance of 70 mm and a thickness of 20-30 mcm; according to the declared technical decision, when forming the fourth layer, the hydroxyapatite powder having a dispersion of 70-90 mcm in an amount of 60% of the total amount of the mixture is mixed with the fluorohydroxyapatite powder having a dispersion of 40-70 mcm in an amount of 40% of the total amount of the mixture.

EFFECT: endosseous implants possess high osteointegration properties and are characterised by the developed surface microrelief and homogeneity.

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Description

The invention relates to medicine, namely to maxillofacial surgery and traumatology, and can be used for the manufacture of interstitial endoprostheses on a titanium basis.

A known method of applying a hydroxyapatite coating to an implant of bioinert materials and their alloys (RF patent for the invention No. 2417107, IPC A61L 27/30, B05D 7/24, A61L 27/32 C1, publ. 04/27/2011), which is carried out by mixing powder hydroxyapatite with a biologically compatible binder in the form of a phosphate binder with a binder to powder ratio of 1.0-1.5: 1.5-2.0, applying the resulting suspension to a metal surface, drying and subsequent heat treatment with an argon-plasma jet at an arc current 30-500 A, duration 0.5-2.0 min per d station 40-100 mm.

However, the obtained bioactive coatings do not have sufficient strength and developed surface morphology.

A known method of manufacturing an intraosseous dental implant with a plasma-sprayed multilayer bioactive coating (RF patent for the invention No. 2146535, IPC A61L 27/00, F61C 8/00, publ. March 20, 2000), in which the increase in the adhesion of the coating and the achievement of the necessary porous structure is solved by plasma spraying on the titanium base of the implant under various modes of the coating system of five layers consisting of five layers: the first two of titanium or titanium hydride, the next two layers of a mixture of titanium or titanium hydride with hydroxyapati ohm calcium content differing components in layers, and outer, fifth layer of calcium hydroxyapatite

However, this method is expensive and time-consuming, while it does not provide coverage with developed microrelief and uniformity.

Closest to the proposed solution is a method of manufacturing intraosseous implants (RF patent for the invention No. 2443434, IPC A61L 27/02, A61L 27/06, A61L 27/12, A61F 2/28, B82B 3/00, publ. 02.27.2012 g .), which consists in layer-by-layer spraying, with the first layer spraying titanium with a dispersion of 3 ÷ 5 μm, a spraying distance of 70 ÷ 80 mm and a thickness of 5 ÷ 10 μm, the second layer spraying titanium with a dispersion of 50 ÷ 100 μm, a spraying distance of 100 ÷ 100 μm, a spraying distance of 100 mm, thickness 50 ÷ 115 μm, the third layer is applied a mechanical mixture of titanium with a fineness of 40 ÷ 70 microns and hydroxyapatite with a fineness of 5 ÷ 10 microns with a ratio 60–80 and 20–40 wt.%, respectively, with a spraying distance of 80 mm and a layer thickness of 15–20 μm, the fourth layer is applied with a spraying distance of 70 mm, a thickness of 20–30 μm, and in the preparation of the fourth layer, alumina or hydroxyapatite powders are mixed fineness of 40 ÷ 90 microns with a hydroxyapatite powder of fineness of less than 40 microns or alumina powder of fineness of 1 ÷ 3 microns in the amount of 70 ÷ 95 wt.% and 5 ÷ 30 wt.%, respectively, the mixture is stirred, annealed for 1.5 ÷ 3 hours and grind.

However, this method does not allow to obtain a biocompatible coating with developed surface morphology.

The objective of the invention is the creation of intraosseous implants with a biocompatible coating, with high osseointegration properties and characterized by developed microrelief and surface uniformity.

The technical result consists in obtaining a coating with a developed microrelief and surface uniformity using a mechanical mixture of hydroxyapatite and fluorohydroxyapatite, used as a component that is part of the plasma spray coating.

This object is achieved by the fact that in the method of manufacturing intraosseous implants with a bioactive coating, which consists in layer-by-layer plasma spraying on a titanium base of an implant of five layers, the first layer is sprayed with titanium powder with a dispersion of 3-5 microns, a spraying distance of 70-80 mm and a thickness of 5 -10 microns, a second layer is sprayed with titanium powder with a dispersion of 50-100 microns, a spraying distance of 100 mm, a thickness of 50-115 microns, the third layer is applied with a mechanical mixture of titanium powders with a dispersion of 40-70 microns and hydroxyapatite dispersion with a ratio of 5–10 μm with a ratio of 60–80 and 20–40 wt.%, respectively, with a spraying distance of 80 mm and a layer thickness of 15–20 μm, the fourth layer is formed on the basis of a mechanical mixture of bioactive powders based on hydroxyapatite with a distance of 70 mm and a thickness of 20– 30 microns, according to the claimed technical solution, when forming the fourth layer, hydroxyapatite powder with a dispersion of 70-90 microns in an amount of 60% of the total mixture is mixed with fluorohydroxyapatite powder with a dispersion of 40-70 microns in an amount of 40% of the total amount of the mixture.

The invention is illustrated in the drawing: Figure 1 - Structure of the coating.

Where the positions in the drawing indicate:

1 - titanium base

2 - the first layer,

3 - the second layer,

4 - the third layer,

5 - the fourth layer.

A method of manufacturing intraosseous implants with a bioactive coating is as follows.

The first layer 2 (FIG. 1) sputter titanium with a dispersion of 3 ÷ 5 μm, a spraying distance of 70 ÷ 80 mm and a thickness of 5 ÷ 10 μm on a titanium base 1, the second layer 3 (FIG. 1) - titanium with a dispersion of 50 ÷ 100 μm, a distance sputtering 100 mm, a thickness of 50 ÷ 115 μm, the third layer 4 (figure 1) apply a mechanical mixture of titanium with a dispersion of 40 ÷ 70 μm and a hydroxyapatite dispersion of 5 ÷ 10 μm with a ratio of 60 ÷ 80 and 20 ÷ 40 wt.%, respectively, the spraying distance 80 mm and a layer thickness of 15 ÷ 20 μm, the fourth layer 5 (Fig. 1) is coated with a spraying distance of 70 mm, a thickness of 20 ÷ 30 μm. To prepare the fourth layer 5, a mechanical mixture is prepared, for example, using a glass rod, hydroxyapatite (HA) powder with a dispersion of 70-90 microns in an amount of 60% of the total mixture with a fluorohydroxyapatite powder (PHA) with a dispersion of 40-70 microns in an amount of 40% of total amount of the mixture.

During plasma spraying of the hydroxyapatite powder, it disperses, therefore, when using a hydroxyapatite powder with a dispersion of 70-90 μm in an amount of 60% of the total amount of the mixture, an optimal coating with the desired morphology and uniformity is obtained (Table 1).

The use of fluorohydroxyapatite with a dispersion of 40-70 microns in the stated percentage is justified by the fact that the use of fluorohydroxyapatite powder in an amount of less than 40% of the total amount of the mixture will not lead to the desired increase in morphology, i.e. values of roughness parameters, and uniformity of the bioactive coating, and the use of more than 40% of the total amount of the mixture will contribute to a change in the porous structure of the bioactive coating (Table 1), which allows bone tissue to grow into the coating structure without the formation of a connective tissue capsule, i.e. osseointegration.

Table 1 Roughness parameters of plasma-sprayed mechanical sweep of PHA and HA powders depending on the dispersion of the initial powders Experience Number Roughness parameters Dispersed
HA powder, μm Dispersed
PHA powder, μm Containing
HA powder in the mixture,% Containing
PHA powder in the mixture,% R _z , μm R _max , MKM S _m , MKM one 39.19 58.37 47.53 60 thirty 60 40 2 43.61 59.24 65.72 70 40 3 44,2 60,2 66.3 80 fifty four 44.9 60.9 67.1 85 60 5 45.6 61.5 68,2 90 70 6 38.53 96.1 46.14 one hundred 80 7 55.11 41.18 77.31 110 90

When using fluorohydroxyapatite powder as a component of a bioactive coating, a greater number of hematopoietic cells and a smaller number of stromal cells are formed, which, based on literature data, can be considered a positive factor contributing to the construction of bone tissue and stimulation of osseointegration (Kurdyumov S.G. Fluorohydroxyapatite for dental implantation / С. G. Kurdyumov, A.I. Volozhin, V.P. Orlovsky // Modern problems of implantology: proceedings of the VI International scientific and technical conference. - Saratov, 2002. - P.69-71).

Preliminary preparation of the surface of a medical implant is carried out, for example, by spraying with electrocorundum powder with a particle size of 150-250 μm under a pressure of 6.5 atm (Lyasnikova A.V. Dental implants. Research, development, production, clinical application / A.V. Lyasnikova et al. - Saratov: Sarat. State Technical University, 2006. - 254 pp .; Lyasnikova A.V. Biocompatible materials and coatings of a new generation: production features, nanostructuring, study of properties, prospects for clinical use / A. B. Las Nikova et al. - Saratov: Scientific Book, 2011. - 220 p.).

Then ultrasonic degreasing is performed, for example, by loading implants that have undergone air-abrasive treatment into an ultrasonic bath UZUMI-2 with a special solution (3 ... 6 g / l Na ₃ PO ₄ and 3 ... 6 g / l surfactant OP- 10), the frequency of ultrasonic vibrations is 35 kHz, the processing time is 5 minutes Due to this degreasing, the contamination of the implant surface with residual organic matter is reduced to a level of 10 ^-9 g / cm ² .

Then produce layer-by-layer plasma spraying of coatings on samples of titanium VT1-00 brand in accordance with RF patent No. 2443434.

Layer-by-layer plasma spraying of coatings was carried out in the atmosphere in an argon shielding gas jet, while the plasma-forming gas flow rate was 20–40 l / min, the plasma torch displacement velocity during spraying was 80–700 mm / min, the arc voltage was 30–40 V, and the workpiece rotation speed was 110–10 160 rpm The last layers were not sprayed at a plasma arc current of 450–500 A, with a spraying distance of 100 mm.

Thus, a method has been developed for the manufacture of intraosseous implants with a bioactive coating, which allows one to obtain a coating that will facilitate fast and reliable osseointegration of the implant with biological tissues, and at the same time have developed morphology and surface uniformity.

Claims (1)

A method of manufacturing intraosseous implants with a bioactive coating, which consists in layer-by-layer plasma spraying on a titanium base of an implant of four layers, with the first layer spraying titanium powder with a dispersion of 3-5 microns, a spraying distance of 70-80 mm and a thickness of 5-10 microns, the second layer is sprayed titanium powder with a dispersion of 50-100 microns, a spraying distance of 100 mm, a thickness of 50-115 microns, the third layer is applied a mechanical mixture of titanium powders with a dispersion of 40-70 microns and hydroxyapatite with a dispersion of 5-10 microns with a ratio of 60-80 and 20-40 wt. %, respectively, with a spraying distance of 80 mm and a layer thickness of 15-20 μm, the fourth layer is formed on the basis of a mechanical mixture of bioactive powders based on hydroxyapatite with a distance of 70 mm and a thickness of 20-30 μm, characterized in that when the fourth layer is formed, hydroxyapatite powder is dispersed with a dispersion of 70 -90 microns in an amount of 60% of the total mixture with fluorohydroxyapatite powder with a dispersion of 40-70 microns in an amount of 40% of the total mixture.

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