WO2016118038A1

WO2016118038A1 - Titanium implant having porous surface, and method for producing same

Info

Publication number: WO2016118038A1
Application number: PCT/RU2015/000031
Authority: WO
Inventors: Илья Юльевич ФРИДМАН; Сергей Александрович КИСЕЛЕВ; Павел Александрович ЗАБУРСКИЙ; Андрей Викторович ОЛЕНИН
Original assignee: Общество с ограниченной ответственностью "Альфа Биотех"
Priority date: 2015-01-21
Filing date: 2015-01-21
Publication date: 2016-07-28

Abstract

The invention relates to the field of medicine, and specifically to dentistry, and may be used for forming the surface of titanium dental implants, with the aim of subsequently allowing for the successful integration of the implant into bone tissue. To achieve said aim, a method is proposed for forming a surface of a dental implant which includes shot-peening a titanium implant using aluminum oxide, and subsequent chemical etching, characterized in that the chemical etching is carried out using an acid composition containing sulfuric acid and hydrochloric acid, which are diluted in a 50% concentration, over the course of 20 minutes at a solution temperature of 22-25°C and an illuminance of 0.25-0.4 lx and with the simultaneous application of ultrasound having a power of 457-507 ergs/sec. The surface of an implant formed using the proposed method allows for creating optimum conditions for protein adhesion by means of forming a maximum possible area of the implant surface and by means of a three-tier structure of formed microcavities.

Description

POROUS SURFACE TITANIUM IMPLANT

AND METHOD FOR ITS PRODUCTION

The invention relates to medicine, namely to dentistry, and can be used to form the surface of dental titanium implants in order to ensure further successful integration of the implant into bone tissue.

State of the art

One of the main directions of improving the biological qualities of products by manufacturers of advanced implantation systems is the development of new types of surfaces.

Currently, the most popular types of biocompatible dental implant surfaces are: TiUnite from Nobel Biocare, NanoTechTM developed by Alpha-Bio Tes, and SLActive from Straumann. All of them are more osteoconductive than osteinductive. TiUnite technology implies a process when, under the action of electrolysis, the released gas in the titanium oxide layer creates pores and thereby increases the thickness of the oxide layer itself and, as a result, the total surface area of the implant. Alpha-Bio Tes, in turn, has developed an NanoTecTM surface that is exceptional in micromechanical and biological properties. The NanoTecTM surface is the result of a multi-stage process, which essentially consists in sandblasting the implant body with a titanium oxide powder consisting of particles from 20 to 40 microns in size followed by double thermal acid etching to achieve microporosity from 1 to 5 microns in size. Straumann developed the SLActive implant surface, during the formation of which the titanium implant body is sandblasted, acid-etched and then washed with water using a nitrogen atmosphere, which leads to the formation of a hydroxylated, chemically active layer on the surface of the implant body with hydrophilic properties. This hydrophilic surface is designed to optimize the formation of a new bone structure around the implant due to its potentiated ability to retain a blood clot in the peri-implant region during its retraction.

However, the known techniques for processing implants for controlled surface formation with the desired three-dimensional organization at the nanoscale are imperfect. Disclosure of invention

The present invention is the formation of the surface of the dental implant, ensuring the successful integration of the implant into the bone tissue.

The problem is solved by achieving a technical result - creating such an outer surface of the implant, which provides optimal conditions for protein adhesion due to the technologically formed maximum possible surface area of the implant and the three-level structure of the formed microcavities: less than 1 micron (nanoscale), 1-5 micron (microscale) and 20-40 microns (macro level).

The achievement of the specified technical result is achieved as a result of the implementation of the method of forming the surface of the dental implant, including bead blasting of the titanium implant with aluminum oxide and subsequent chemical etching, in which the chemical etching is carried out using an acid composition containing sulfuric and hydrochloric acids diluted in a 50% concentration, within 20 minutes at a temperature of the solution from 22 to 25 ° C and illumination from 0.25 to 0.4 lux and simultaneous exposure to ultrasound with a power of 45 ⁷ to 50 ⁷ erg / s.

DETAILED DESCRIPTION OF THE INVENTION

For the implementation of the invention, titanium implants are used, made of technically pure titanium, for example, titanium of grades VT 1-0 and BT 1-00 (GOST 19807-91) or of “commercially pure” titanium of four grades (Grade 1-4 ASTM, ISO) or titanium alloy Ti-6AI-4V (ASTM, ISO), subjected to preliminary bead-blasting with aluminum oxide (Al ₂ 0 ₃ ). For example, in one embodiment of the invention, titanium implants of Alpha BIO company (Israel) can be used. Preliminary shot blasting is necessary for texturing the titanium surface in preparation for etching to achieve the desired etching result. In this case, the roughness size, etching carried out after bead-blasting, and the subsequent ultrasonic washing do not affect the result of subsequent modification by the proposed method.

For acid modification of the titanium surface, the titanium implant is placed in an ultrasonic bath, where it is etched in a mixture of hydrochloric (hydrochloric acid OSCH 20-4 GOST 14261-77, and 26-4 GOST 14261-77) and sulfuric acid (sulfuric acid OSCH 11-5 (very pure) GOST 14262-78 (mass fraction of the main substance 95.6%)) in equal proportions diluted with distilled water in a 50% concentration. Etching is carried out within 20 minutes. at a temperature solution from 22 to 25 ° C and illumination from 0.25 to 0.4 lux (lux) and the simultaneous exposure to ultrasound with a power of 45 ⁷ to 50 ⁷ erg / s.

As a result of this effect, a modified implant surface is formed having a three-level structure of microcavities:

• less than 1 micron - the nanoscale required to optimize the absorption of bone morphogenetic proteins; formed pores with a size range from 1-5 nm to 200 nm and a maximum in the region of 50 nm provide the ability to sorb proteins in larger quantities than known analogues, providing the induction of bone morphogenetic proteins necessary for osseointegration;

• 1-5 microns - the micro level necessary for reliable fixation of the fibrin filaments that make up the basis of the blood clot, which is guaranteed to prevent their separation from the implant surface during retraction of the blood clot;

• 20-40 microns - macro level, corresponding to the average size of osteogenic cells - active osteoblasts and necessary for their optimal placement on the implant surface.

Thus, in comparison with known analogues, the implant surface formed by the proposed method provides the creation of optimal conditions for protein adhesion by forming the maximum possible surface area of the implant having a three-level structure of microcavities.

It is known that the preservation of the maximum possible amount of a blood clot during and after its retraction on the implant surface is the main resolution point in the development of contact osteogenesis, which is considered to be the success of osseointegration. This process is normally considered to be the initial stage of osteoconductive reactions that occur in each first case during the installation of a dental implant.

The set of characteristics inherent in the implant surface obtained by the proposed method provides its osteinductive and osteoconductive properties, which, in turn, ensures successful osseointegration of bone tissue during implantation. Since the retraction of a blood clot on a titanium implant occurs more slowly in the region of pores having a size of less than 1 micron, the retraction of the entire clot does not occur simultaneously, since the farther the clot is located from the wound surface, the weaker its retraction. This prevents the development of such complications as epithelial ingrowth and the formation of a bone pocket around the cervical part of the implant.

s The invention is illustrated by the following figures:

Fig. 1 - micrographs of the implant surface formed by the method according to the invention, photo of the Microanalysis Laboratory of the Skolkovo Technopark:

a) an increase of 150 times, b) an increase of 500 times, c) an increase of 1000 times, d) an increase of 2500 times, e) an increase of 10 ⁴ , f) an increase of 4x10 ⁴ ,

g) - an increase of 4x10 ⁴ , h) - an increase of 2x10 ⁴ , and) an increase of 16x10 ⁴ ,

k) - an increase of 8x10 ⁴ , l) - an increase of 30x10 ⁴ , m) an increase of 30x10 ⁴ ,

m) - increase 2x10 ⁴ , b) - increase 60x10 ⁴ ;

Fig. 2 - microphotographs of the surface of the implant obtained by Antozhir (Anthogyr), France: a) a 150-fold increase, b) a 500-fold increase, c) a 1000-fold increase, d) a 2,500-fold increase, e) - increase 10 ⁴ , e) increase 4x10 ⁴ , g) - increase 8x10 ⁴ , h) - increase 5,000 times;

Fig. 3 - micrographs of the surface of the implant obtained by the Tornado company (Makhachkala): a) an increase of 150 times, b) an increase of 500 times, c) an increase of 1000 times, d) an increase of 10 ⁴ , e) an increase of 8x10 ^4, e) increase in 1000, g) - an increase of 5,000 times, s) - an increase of 5,000 times;

Fig. 4 - micrographs of the surface of the Atid implant company AlphaBioTec (Israel): a) an increase of 2x10 ⁴ , b) an increase of 4x10 ⁴ , c) an increase of 8x10 ⁴ ,

Fig. 5 is a micrograph of the NanoTec surface of the Alpha Bio Tes ATID implant (magnification 4x10 ⁴ );

Fig. 6 is a photomicrograph of a Nobel Wüsage TiUnite surface (enlarged

U ⁴ );

Fig. 7 is a micrograph of the surface of the SLA of Straumann Wüsage (magnification 2x10 ⁴ );

Fig. 8 shows the results of spectral analysis of the surface of an ATID implant;

Fig. 9 shows the results of spectral analysis of the ICE implant surface;

Fig. 10 shows the results of spectral analysis of the surface of an SPI implant;

Fig. 11 shows the results of spectral analysis of the surface of a DFI implant;

Fig. 12 shows the results of spectral analysis of the surface of a Mirell implant;

Fig. 13 - results of spectral analysis of the surface of the Noris implant;

Fig. 14 shows the results of spectral analysis of the surface of the SIN implant.

In the micrographs it is seen that the implant surface obtained by the method according to the invention is more structured than the implant surfaces of known analogues.

The invention is further illustrated by the following non-limiting example. Example

For surface modification, Atid implants of AlphaBioTec company (Israel) made of Grade 2 ASTM grade titanium were used (see Fig. 4).

Titanium implants were subjected to acid etching in a mixture of hydrochloric and sulfuric acids, mixed in equal proportions and diluted with distilled water in a 50% concentration. Etching was carried out for 20 minutes. at a solution temperature of 24 ° С and illumination of 0.4 lux with simultaneous exposure to ultrasound with a power of 50 ⁷ erg / s.

As a result of this effect, a modified implant surface was formed having a three-level structure of microcavities (see Fig. 1).

Claims

Claim

A method of forming the surface of a dental implant, including bead blasting a titanium implant with aluminum oxide and subsequent chemical etching, characterized in that the chemical etching is carried out using an acid composition containing sulfuric and hydrochloric acids diluted in 50% concentration for 20 minutes. at a temperature of the solution from 22 to 25 ° C and illumination from 0.25 to 0.4 lux and simultaneous exposure to ultrasound with a power of 45 ⁷ to 50 ⁷ erg / s.