Method of applying hydroxyapatite coat on implants

FIELD: process engineering.

SUBSTANCE: invention relates to method of applying hydroxyapatite coats and may be used in medicine for production of met implants with bioactive coat. Proposed method comprises mixing hydroxyapatite powder with biologically compatible binder representing a phosphate binder with binder-to-powder ratio of 1.0-1.5:1.5-2.0, applying obtained suspension on metal surface, drying and thermal treatment by argon plasma jet at arc current of 300-500 A for 0.5-2.0 min at distance of 40-100 mm.

EFFECT: higher mechanical strength of hydroxyapatite coat.

2 dwg, 1 tbl, 2 ex

 

The invention relates to medicine, namely to methods for applying a bioactive hydroxiapatite coatings on implants for dentistry, traumatology and orthopedics.

Hydroxyapatite coating of implants provides fast and efficient engraftment in the bone structures due to the high level of biological activity of the surface. The most common technology of powder coating hydroxiapatite coating is plasma spraying [1-3], which consists in passing the powder of hydroxyapatite through the plasma torch, melting of the powder particles in the plasma jet and their subsequent deposition on the surface of the implant. However, the application of hydroxiapatite powder coating-plasma method is a technologically complex process and is characterized by low economic efficiency of the flow rate of the sprayed material, as only 40-50% of the particles hydroxiapatite powder is deposited on the surface of the workpiece, and the rest of their number - on the walls of the sputtering chamber, not getting on the product. In this case, the mechanical strength of the coating in many cases is low, there is often a rebound of the powder particles from the substrate in the collision with her.

A known method of manufacturing implants with bio-ceramic coating (hydroxyapatite Biosite), applied by plasma spraying [4]. The disadvantage of this method is the high consumption of used powder material and inadequate for continuous functioning of the implant mechanical strength of the coating.

The closest prototype, according to the authors, is the method of applying hydroxiapatite coatings comprising mixing hydroxyapatite powder with a binder, which is used as the phosphate ligaments, taken in relation to the powder 1,0-1,5:1,5-2,0, drying and heat treatment annealing at a temperature varying between 250 and 600°C [5]. The method is characterized highly economical consumption hydroxiapatite powder, because all of its particles, which is mounted on the implant surface using a binder, participate in the process of creation of the coverage. However, the disadvantage of this method is the lack of mechanical strength of the coating.

The objective of the invention is to provide a cost-effective method of applying hydroxiapatite coating with high mechanical strength.

This object is achieved in that a mixed powder of hydroxyapatite and biocompatible binder, which is used as the phosphate ligaments, taken in relation to the powder 1,0-1,5:1,5-2,0, put the resulting suspension on a surface is the surface of the implant, produce drying the applied suspension for preliminary fixation to the implant and carry out heat treatment of argon plasma jet at arc current 300-500 And duration of 0.5-2.0 min at a distance of 40-100 mm

The difference of the proposed method from the prototype is that the heat treatment is carried out by exposure to argon plasma jet at arc current 300-500 And duration of 0.5-2.0 min at a distance of 40-100 mm

Given the limits of technological processing mode provide hydroxiapatite coatings with high adhesion and cohesion, which are the main indicators of the mechanical strength of the coatings.

Effective heat of argon plasma jet when the value of the mode I<300 a, τ<0.5 min is impossible, since the resulting coating does not possess high mechanical strength and are prone to fracture even at low functional load on the implant. This is because heat treatment of argon plasma jet at such values of the mode does not provide surface melting particles hydroxiapatite powder, resulting in not is their increased interaction with the implant and with each other.

Argon-plasma treatment at values of I>500 a, τ>2,0 min creates the danger of burning particles of hydroxyapatite in the volume forms the alignment coating, what is technologically unacceptable factor.

Distance (distance from the nozzle of the plasma torch to the surface of the product) is selected depending on the dispersion applied hydroxiapatite powder and the thickness of the created bioactive coatings and varies from 40 to 100 mm for surface melting of the particles of hydroxyapatite and their strong relationship with the implant surface and to each other.

When the distance processing less than 40 mm, the strength of the relationship of the coating with the surface of the implant is increased, but no pronounced roughness and porosity hydroxiapatite layer required for osseointegration of the implant and its secure attachment to the bone. At a distance of processing in excess of 100 mm, excludes the possibility of melting particles hydroxiapatite powder with no conditions of their enhanced relationship with the implant and with each other, which leads to a considerable reduction of the mechanical strength of the coating.

The invention consists in that the process of forming the coating is carried out by mixing the powder of hydroxyapatite phosphate-bonded, applying the resulting slurry to the surface of the implant, drying the applied suspension for preliminary fixing of the amount of coating of the mandate Elie and heat treatment of argon plasma jet at arc current 300-500 And, duration of 0.5-2.0 min, at a distance of 40-100 mm, While the hydroxyapatite powder is mixed with a binder to hold hydroxiapatite particles on the implant surface, and heat treatment of argon plasma jet is performed to ensure that surface melting of the powder particles and their enhanced physical and mechanical interconnection with a metal base and with each other due to the effect welding of the particles. The presence in the volume of coating does not pereplavlennyj solid core particles of hydroxyapatite creates a pronounced roughness and morphological heterogeneity of the surface with the presence of porous structure necessary for effective osseointegration of the implant.

The coating obtained by the claimed method, illustrated with photos, in which figure 1 shows surface osteointegration structure hydroxiapatite layer formed on the titanium (VT1-00) the dental implant as in figure 2 - steel (HT) orthopedic implant-osteofixation.

Example 1. Prepare a suspension of the powder of hydroxyapatite dispersion Δ=50 μm and a biocompatible binder to the resulting solution was saturated with hydroxyapatite particles and contained the minimum amount of binder sufficient to hold the suspension of poweredtemplates. As binders take calcium phosphate ligament and mix it with the powder of hydroxyapatite in a ratio of 1.0:1.5 to. Using a brush, the resulting suspension is applied to the implant and is subjected to drying in an oven at 50°C for 20 minutes Then the implant with a fixed suspension is placed in a plasma chamber installation type VRESSE and produce heat treatment of the coating argon-plasma jet when the value of the arc current I=350 A, the duration τ=1,0 min at a distance of L=70 mm In data technological terms is the melt surface hydroxiapatite particles, their welding to the base of the implant and to each other while maintaining solid nuclei in the volume of the particles.

Example 2. Prepare a suspension of the powder of hydroxyapatite dispersion Δ=70 μm and a biocompatible binder to the resulting solution was saturated with hydroxyapatite particles and contained the minimum amount of binder sufficient to hold the suspension on the surface of the implant. As binders take manifestou ligament and mix it with the powder of hydroxyapatite in a ratio of 1.2:1,9. Using a brush, the suspension is applied to the implant and is subjected to drying in an oven at 50°C for 20 minutes Then the implant with a fixed suspension is placed in a plasma chamber to set the key and produce heat treatment of the coating argon-plasma jet when the arc current I=450 A, duration τ=1.5 min at a distance of L=90 mm, the result is a bioactive mechanically durable coating of the surface-melted particles hydroxiapatite powder.

Obtained by this method hydroxyapatite coatings have been tested for mechanical strength, determined by the methods of normal tear and shear. The results of the tests are presented in table.

The positive effect of increased mechanical strength of the coating shear and highly economical consumption hydroxiapatite of the powder is achieved by the fact that, due to surface melting of the particles during the heat treatment is strengthening their relationship with the implant surface and to each other, greatly increasing the strength of the coating, and the amount of powder of hydroxyapatite, which is applied to the surface of the implant in the form of a mixture with the binder, is involved in the process of creating a cover with the exception of the rebound of the particles and their shedding with a metal base.

Dental intraosseous implants of titanium VT1-0, VT1-00, as well as orthopedic transosseous osteofixation of titanium alloy VT6, VT and stainless steel HT, 12H18N10T, covered with the proposed method can achieve the best treatment results due to the increased mechanical strength b is aktivnogo coverage, continuing throughout the term of functioning of the products.

Sources of information

1. Buttowski KG and other Electroplasma plating in the production of intraosseous implants. Saratov: Sarat. state technology. University, 2006. 200 S.

2. RF patent for the invention №2146535. A method of manufacturing intraosseous dental implant plasmolen multilayer bioactive coating. Publ. 20.03.2000.

3. RF patent for the invention №2134082. The method of manufacture of implants for transosseous osteosynthesis. Publ. 10.08.1999.

4. RF patent for the invention №2157245. A method of manufacturing implants. Publ. 10.10.2000.

5. RF patent for the invention №2158189. The method of applying hydroxiapatite coatings. Publ. 27.10.2000 (prototype).

The dispersion of powder of hydroxyapatite Δ, μmMode argon-plasma treatmentThe strength of the coating to peel σ, MPaThe strength of the coating when the shift σ, MPaThe strength of the coating when the shift σ, MPa (prototype)
I, Andτ minL, mm
50350 1,07021the 3.82,07-of 3.07
704501,59024the 4.7

The method of applying hydroxiapatite coating on the implant, comprising mixing a powder of hydroxyapatite and biocompatible binder, which is used as a phosphate binder in a ratio of ligaments and powder 1,0-1,5:1,5-2,0, applying the resulting slurry to the surface of the implant, drying and subsequent heat treatment, wherein the heat treatment is conducted argon plasma jet at arc current 300-500 And duration of 0.5-2.0 min at a distance of processing 40-100 mm



 

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