Method of production of multi-layer gradient coating by method of magnetron deposition

FIELD: metallurgy.

SUBSTANCE: invention relates to method of application of the gradient coatings by the magnetron deposition, in particular to application of coatings based on high-melting metals, and can be used to produce coatings with high adhesive and cohesive properties, as well as with optimal combination of strength and plasticity. On pre-cleaned surface of the metal backing the adhesive alloy of high-melting metals is applied in inert gas, and layer of nitrides of high-melting metals in gas mixture of inert and reacting gases. Content of nitrides of high-melting metals varies from 0% to 100%, holding is performed until achievement of the required thickness of the nitride layer, then it is reduced in reverse order, held until achievement of the required layer thickness of high-melting metals, and re-increased in direction to thickness of the deposited layer. For content increasing and decreasing of the nitrides of high-melting metals the reacting gas pressure is varied as per linear law from 0 to 8×10-2 Pa, and then in reverse order.

EFFECT: method produces materials with high strength characteristics and optimal combination of hardness (H>40 GPa) and plasticity (We > 70%).

2 cl, 1 dwg, 2 ex

 

The invention relates to the field of application of gradient coatings, in particular to the application of coatings based on titanium or zirconium with special protective properties, and can be used for the production of coatings with high adhesive and cohesive characteristics and optimal combination of strength and plasticity.

Known method of applying a multilayer wear-resistant coating (RU # 2346078, CL C23C 14/24, publ. 10.02.2009), in which first cause the microlayer TiZr, then carry out thermo-mechanical activation of the surface layers by ion bombardment, and then put a layer based on titanium nitride and zirconium (Ti, Zr)N. Deposition of layers TiZr, (Ti, Zr)N and ion bombardment is repeated at least three times, the latter put a layer of (Ti, Zr)N. the Application of the coating layers is carried out by evaporation of two titanium and one of zirconium cathode. The disadvantage of this known method of coating is a significant difference between the coefficients of expansion between the metal substrate and the applied coating, which leads to stress coefficient and, as a rule, and possible delamination of the coating.

The closest in technical essence and the achieved effect is a method for coating according to the patent No. 2433209 (CL C23C 14/06, publ. 10.11.2011), taken as a prototype. The essence with�person obtaining a multilayer coating is on the precleaned surface of the substrate is first applied to the adhesion layer of titanium magnetron sputtering of titanium target in an inert gas, then put a layer of titanium nitride by sputtering a titanium target in a gas mixture of inert and reactive gases, then put alternate layers of two-component zirconium nitride ZrN zirconium sputtering target in a gas mixture of inert and reactive gases and zirconium sputtering of zirconium target in an inert gas, and then put alternating layers of three-component titanium nitride and zirconium TiZrN simultaneous sputtering of titanium and zirconium targets in a gas mixture of inert and reactive gases and zirconium sputtering of zirconium target in an inert gas.

The disadvantages of the prototype lies in the fact that the coating has a sharp interfacial boundary between the metallic and non-metallic layers, with a significant difference in the coefficients of thermal expansion. This creates significant mechanical stresses during cyclic thermal loads, which often leads to the destruction of the coating and the decommissioning of the finished product. The presence of such boundaries also affects the integral cohesive strength and reduces the life of the product.

In addition, according to the scheme of the prototype of the availability coefficient of the stress lets not get�th coating with thickness, in excess of 12-15 µm, which is clearly insufficient for products operated at the hard impact of secondary factors.

To eliminate these negative factors it is necessary to create a structure with one-dimensional boundaries between phases (powder reinforced components), i.e. nanostructured component coating, which will provide a high volume fraction of the phase boundary along the entire cross section of the coating.

The presence of a large area of the phase separation (volume fraction which can be up to <50%) in nanostructured coatings and films can significantly change their properties by modifying the structure and electronic structure, and various alloying elements. The strength of the boundary increases the resistance of nanostructured coatings to deformation. The absence of dislocations inside the crystallites increases the elasticity of the coatings. These properties allow to obtain materials with improved physico-chemical and physico-mechanical properties such as high hardness (H > 40 GPA), elastic recovery (We>70%), strength, heat resistance and abrasion resistance.

Thus, the technical result of the present invention is to provide a method of obtaining gradient multilayer coatings with high adhesion strength with �oblojkoi, increased durability of the coating by substantially less influence of the difference of coefficients of thermal expansion, and thus less mechanical stress in the coating during thermal Cycling loads, and a higher viscosity of the coating due to the absence of two-dimensional boundary layers with different hardness, which provides cushioning for the relaxation of the stress and stop the growth of cracks.

The technical result is achieved due to the fact that when using the magnetron sputtering gradient multilayer coating spraying is done when the regulated flow of the reaction gas of nitrogen in the vacuum chamber is linear from 0 to a pressure of 8×10-2PA, then the pressure is held until the receipt of the nitride layer of the desired thickness, then decreases by the same linear law of 8×10-2PA to 0, and the zero pressure value is maintained until the required thickness of the layer of refractory metal, and then the sputtering process at controlled increase and decrease the pressure of the reaction gas of nitrogen at the specified linear repeat until the desired number of layers. In this surface layer must be mentioned nitride layer.

The specified maximum value of the pressure of nitrogen is optimal, as it provides the deposition of nitrides with �primulinum stoichiometric composition of TiN. With further increase of nitrogen pressure in the chamber leads to the formation of brittle phases of TiN2. At lower pressures in addition to the nitrides of metal phase is present in excess of the optimum, which significantly reduces the coating properties.

Implementation of a multilayer structure of the coating with gradient transitions between layers enables a higher viscosity of the coating compared to monoclonal coating and thus the ability of a material to absorb energy during deformation without fracture. Improving the wear resistance of the coating is due to the fact that layers with high hardness gradient transform into softer layers, which provides cushioning for the relaxation of the stress and stop the growth of cracks that may emerge in a more solid layer under the influence of elastic and thermoelastic stresses.

The essence of the method lies in the fact that the prepared substrate is placed in a vacuum chamber of magnetron sputtering, pre-heated in vacuum to a temperature of 400-450°C, and then carry out the deposition of the first layer of titanium or zirconium in the environment of the plasma gas argon, then at the camera unleashes the reaction gas is nitrogen, and the pressure to maintain a constant argon, and nitrogen pressure change is linear from 0 to 8×10-2PA. According to�to meet maximum value withstand the specified pressure to obtain the desired thickness of the nitride layer, then reduce by the same linear law (Fig. 1). As a result, the content of nitride in the coating varies from 0 to 100% and then drops again to 0% of the adhesive layer to the surface. This constant increase and decrease of pressure of nitrogen provides the alternation in the metal coating layer plastic and solid nitride, which significantly increases the wear resistance of the coating due to the high adhesive and cohesive properties.

Examples of the method:

The proposed method is tested on nanotechnology research complex of the FSUE "CRISM "Prometey".

Example 1.

At install magnetron sputtering using a metal target of Ti (grade VT 1-0) was produced by applying a gradient multilayer coating on a metal plate made of titanium grade W 1-0 100×150×2.

Surface preparation of parts before loading into the vacuum chamber was to remove different kinds of dirt and was conducted according to the scheme: chemical cleaning, drying.

For chemical cleaning detail was placed in a container of solvent so that she was fully immersed in it. Capacity to detail was placed in an ultrasonic bath the TGS-0.25 and has been cleaned ultrasonically for at least 10 minutes. After which the plates were removed from the tank with solvent and wiped with a soft cloth.

Drying the item� is performed in a drying Cabinet at a temperature of 100°C at least 15 minutes.

After putting the plates in the gateway download the magnetron vacuum chamber was pumped to a residual pressure of not higher than 3×10-3PA. Further included quartz heaters located in the gateway download. While holding the plates at a temperature of 400C°±30°C was 5 min. Further, plates of gateway download using a special rotating mechanism "carousel" type was transferred to the position of the ion source. Thereafter, the vacuum chamber filed a plasma gas argon to a pressure of 5×10-1PA and maintained at a predetermined level throughout the ion cleaning process. Using the same rotary movement plates were placed in a position magnetron sputtering. Re-evacuate the chamber until reaching a residual pressure of not higher than 2×10-3PA and gave plasma gas argon to a pressure of 3×10-1PA. On a metal titanium target applied voltage and the excited plasma discharge with a current density of 0.3 A/cm2when the diameter of the target is 100 mm. for 5 minutes produced a coating of pure titanium on the surface of the plates. Then the vacuum chamber included the supply of the reaction gas of nitrogen, increasing the partial pressure of nitrogen is linear from 0 to 8×10-2PA for 5 minutes, then made a deposition at the specified pressure for 5 minutes. Further along on�inverse linear relationship for 5 minutes reduced the partial pressure of nitrogen of 8×10 -2PA to 0. The above cycle of spraying was repeated until the desired number of layers with the formation on the coating surface nitride layer.

Example 2.

At install magnetron sputtering using a metal target Zr (zirconium iodide) was produced by applying a gradient multilayer coating on the metal plates of steel grade St35 size 100×150×2.

Surface preparation of parts before loading into the vacuum chamber was to remove different kinds of dirt and was conducted according to the scheme: chemical treatment, then drying.

For chemical cleaning detail was placed in a container of solvent so that she was fully immersed in it. Capacity to detail was placed in an ultrasonic bath the TGS-0.25 and has been cleaned ultrasonically for at least 10 minutes. After which the plates were removed from the tank with solvent and wiped with a soft cloth.

Drying of parts produced in a drying Cabinet at a temperature of 100°C at least 15 minutes.

After putting the plates in the gateway download the magnetron vacuum chamber was pumped to a residual pressure of not higher than 3×10-3PA. Further included quartz heaters located in the gateway download. While holding the plates at a temperature of 400C°±30°C was 5 min. Further, plates of gateway download via a special p�gate mechanism "carousel" type was transferred to the position of the ion source. Thereafter, the vacuum chamber filed a plasma gas argon to a pressure of 5×10-1PA and maintained at a predetermined level throughout the ion cleaning process. Using the same rotary movement plates were placed in a position magnetron sputtering. Re-evacuate the chamber until reaching a residual pressure of not higher than 2×10-3PA and gave plasma gas argon to a pressure of 5×10-1PA. On a metallic zirconium target applied voltage and the excited plasma discharge with a current density of 0.25 A/cm2when the diameter of the target is 100 mm. for 5 minutes was carried out spraying of pure zirconium on the surface of the plates. Then the vacuum chamber included the supply of the reaction gas is nitrogen, increasing the partial pressure of nitrogen is linear from 0 to 8×10-2PA for 5 minutes, then made a deposition at the specified pressure for 5 minutes. Next on the inverse linear relationship for 5 minutes reduced the partial pressure of nitrogen of 8×10-2PA to 0. The above cycle of spraying was repeated until the desired number of layers with the formation on the coating surface nitride layer.

1. A method of obtaining a multilayer coating comprising a magnetron spraying of the adhesive layer of refractory metal in an inert gas on the pre-filter�nnow the surface of the metal substrate, and then a layer of nitride of refractory metal in a gas mixture of inert and reactive gases, characterized in that the nitride layer of refractory metal is performed with a gradient content of nitrides of refractory metal in the direction of increasing the thickness of the deposited layer, the content of nitrides of refractory metals change from 0% to 100%, withstand to obtain the desired thickness of the nitride layer, then reduce the content of nitrides of refractory metals, in reverse order, withstand to obtain the desired thickness of the layer of refractory metal and again increase the content of nitrides of refractory metals in the direction of increasing the thickness of the deposited layer with obtaining on the surface of the coating mentioned nitride layer, wherein the increase and decrease of the content of nitrides of refractory metals, the pressure of the reaction gas change for a linear relationship respectively from 0 to 8·10-2PA, and then in reverse order.

2. A method according to claim 1, characterized in that the process is repeated until the desired thickness of the coating.



 

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1 tbl

FIELD: metallurgy.

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1 tbl

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1 tbl

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1 tbl

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EFFECT: higher cutting efficiency.

1 tbl

FIELD: process engineering.

SUBSTANCE: invention relates to application of wearproof coating on cutting tool and can be used in machining. Vacuum-plasma application of wearproof coating is performed, coating being composed of titanium, aluminium, silicon, molybdenum and zirconium nitride or carbonitride at the following ratio, wt %: titanium - 39.9, molybdenum - 14.2, aluminium - 12.1.1, silicon - 1.3, zirconium - 32.4. Application is executed by three cathodes arranged horizontally in one plane. First cathode is made of molybdenum and aluminium alloy, second cathode is made of zirconium is arranged opposite the first one while third cathode is made of titanium and is arranged there between.

EFFECT: higher cutting efficiency.

1 tbl

FIELD: process engineering.

SUBSTANCE: invention relates to application of wearproof coating on cutting tool and can be used in machining. Vacuum plasma sandwiched coating is applied. First, bottom ply of niobium nitride is applied. Then, applied is top ply of titanium, aluminium and chromium nitrides at the following ratio of components in wt %: titanium - 70.5-79.5, aluminium - 14.0-20.0, niobium - 6.5-9.5.Coating plies are applied by three cathodes arranged horizontally in one plane. First cathode are made of titanium and aluminium alloy, second cathode is made of niobium and arranged opposite the first one while third cathode is made of titanium and chromium and arranged there between. Bottom ply is applied with the help of second cathode while top ply is applied by first and third cathodes.

EFFECT: higher cutting efficiency.

1 tbl

FIELD: machine building.

SUBSTANCE: vacuum-plasma application of multilayer coating is performed. First, the lower titanium nitride layer is applied. Then the upper layer of titanium compound nitride is applied, silicon and niobium at the mass ratio, wt %: titanium 88.6-93.0, silicon 1.0-1.4, niobium 6.0-10.0. Coating layers are applied by three cathodes located horizontally in the same plane, the first of which is made from titanium and silicon alloy, the second one - from titanium and is placed opposite to the first, and the third is made compound from titanium and niobium and placed between them, and the lower layer is applied using the second cathode, and the upper layer - using the first and third cathodes.

EFFECT: improved serviceability of a cutting tool.

1 tbl

FIELD: metal coats, in particular for gas turbine engines operating at high temperature.

SUBSTANCE: claimed metal coat contains (mass %) cobalt up to 18; chromium 3.0-18; aluminum 5.0-15; yttrium 0.1-1.0; hafnium up to 0.6; silicium up to 0.3; tantalum 3/0-10; tungsten up to 9.0; rhenium 1.0-6.0, molybdenum up to 10, and balance - nickel. Method of invention includes providing of support from at least one metal materials based on nickel, cobalt or iron followed by application of coating layer.

EFFECT: coats of high oxidation resistance and endurance strength.

33 cl, 1 tbl

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