Method of obtaining two-phase nanocomposite coating, consisting of titanium carbide nanoclusters, distributed in amorphous matrix, on products from hard alloys

FIELD: chemistry.

SUBSTANCE: invention relates to field of obtaining nanocomposite coatings and can be used in creation of optic microelectronic devices and materials with increased corrosion resistance and wear resistance. Method of obtaining two-phase nanocomposite coating, consisting of titanium carbide nanoclusters, distributed in amorphous hydrocarbon matrix, on products from hard alloys, includes application of adhesive titanium or chromium sublayer, magnetron sputtering of titanium target in gas mixture of acetylene and argon under pressure 0.01-1 Pa and precipitation of dispersed particles of target and carbon-containing radicals on product surface in combination with bombardment of surface with ions, accelerated by bias voltage, with product surface being subjected to purification with argon ions from plasma, generated by electronic beam, before application of adhesive sublayer, and gas mixture being activated in the process of coating application by impact with beam of electrons with energy 100 eV.

EFFECT: invention is aimed at increase of coating adhesion and micro-hardness of obtained products, as well as at provision of high efficiency of application of acetylene in the process of coating application.

1 ex, 2 dwg

 

The invention relates to methods for two-phase nanocomposite coatings consisting of nanocrystals of titanium carbide dispersed in an amorphous hydrocarbon matrix. Such coatings have a high hardness, thermal conductivity, chemically inert, have a low coefficient of friction and good resistance against mechanical wear, therefore they find application in areas such as microelectronics and optical devices, biomedical products, corrosion-resistant materials, as well as in micromechanical systems.

Known method of applying TiC/a-C:H coatings based on magnetron sputtering of titanium target in C2H2+Ar gas mixture at pressures of 0.01 to 1 PA, and the deposition of the sputtered target particles and carbon-containing radicals on the surface of the products in combination with the bombardment of the surface by ions accelerated by the bias voltage. The microhardness of these coatings are nonmonotonically depends on the relative content of titanium in the coating. The maximum microhardness (30-40 GPA) is achieved when the content of Ti~40 at.%. The size of the cluster TiC is usually a few nm, and a thickness separating the TiC crystallites amorphous phase, a fraction of a nm.

Because magnetron sputtering particles of the target are scattered predominantly in the neutral state, the main mechanism of decomposition �of catilina serve mainly, the reaction of the charge exchange ions of argon atoms of acetylene with subsequent dissociative recombination ion C2H2+with the participation of the slow electron and the formation of active radicals having a high coefficient of adhesion to surfaces. Most likely the formation of radical C2H2[1].

Closest to the proposed is a method of producing nanocomposite TiC/a-C:H-coatings magnetron sputtering at a pressure of a gas mixture of 0.3-0.4 PA, the argon flow 45 ml/min, the flow of acetylene to 24 ml/min, power magnetron discharge 1.5 kW diameter sputtering target 100 mm. To reduce the likelihood of arc-magnetron operates in a pulsed mode with a frequency of 1 kHz, the pulse modulation frequency of 100 kHz. The speed of coating was up to 7 μm/h, the maximum microhardness of the coatings was 42 HPa at a flow of acetylene 8 ml/min To improve adhesion of the coating to the substrate before applying the coating on the surface of the substrate was applied a thin underlayer of chromium (0.3 µm) [2].

An object of the invention is to provide a method of obtaining a two-phase nanocomposite coatings consisting of nanoclusters of titanium carbide dispersed in an amorphous hydrocarbon matrix, providing a high efficiency of utilization of azeti�ena in the coating process, improved adhesion of the coating and high microhardness of the coatings obtained.

To solve this problem is proposed in the coating process, magnetron sputtering of titanium target in C2H2+Ar gas mixture to affect the gas mixture a broad electron beam with a current density of ~10-100 mA/cm2and the electron energy corresponding to the maximum ionization cross sections of electron impact (~100 eV) and to ion cleaning of the surface from contamination in the plasma generated under the action of the electron beam before applying the metal coating to improve adhesion.

The technical result of the proposed method is a multiple decrease in the value of the stream of acetylene required for the formation of the coating with maximum hardness and high adhesion of the coating due to ion cleaning of the surface of products in the plasma generated under the action of the electron beam.

The reason for the decrease in the consumption of acetylene is its rapid decomposition into active radicals under the action of the electron beam as a result of intensive ionization and dissociation of molecules of acetylene. The resulting radicals have a high coefficient of adhesion to the surface, resulting in increased deposition rate of carbon on the surface and allows multiple�about to reduce the flow rate of acetylene, necessary to achieve the maximum microhardness of the coating.

To generate the electron beam is proposed to use stable in the pressure range of 0.01-1 PA plasma electron source based on low-voltage glow discharge with cold cathode [3] or arc discharge samankaltainen cathode [4], in which a part of the anode discharge is made in the form of a fine-grained grid, and for acceleration of electrons and forming an electron beam with large cross section is used, the space charge layer between the plasma gas discharge, the position of the emitting surfaces of which stable fine-grained grid, and a movable anode, which is the plasma created by ionization of the gas mixture low-energy electron beam.

The problem is solved as follows: to the bit interval of an electron source (Fig.1) put argon, apply the voltage between the cathode 1 and the hollow anode 2 arc or glow discharge, ignite the discharge, which creates a plasma emitting surface in the area of fine-grained grid 3, which is part of a hollow anode discharge, served between fine-grained grid and anode 4 disposed inside the chamber coater 5, or a grounded chamber walls coating a voltage of 100 V, providing�I development in the chamber coating processes gas ionization by fast electrons and the creation of a plasma beam. Served on placed in the plasma products 6 offset voltage (300 To 500) and carry out the cleaning of surfaces by ion sputtering for 20 min, then applied the voltage between the cathode of the magnetron 7 and the walls of the chamber coating and produce on the product chromium or titanium sublayer to improve adhesion of the coating. Then into the chamber coating serves acetylene and conduct the deposition of TiC/a-C:H coating at a constant power of the magnetron, the flow of argon, the bias voltage and the beam current and the flow of acetylene, which assures the maximum microhardness.

An example implementation of the proposed method. In the experiments, the chamber coating with a diameter of 260 mm and a length of 300 mm, on the side surface which is planar magnetron with a diameter titanium target 70 mm, operating in a pulsed mode (50 kHz, 10 mA, 2 A) with an average power of 1 kW. On the lid of the chamber coating was located plasma electron source based on glow discharge of low pressure with a mesh size of 80 cm2similar to that described in [5]. To the bit interval of the electron source was snarled a stream of argon, 40 ml/min, which flowed through fine-grained grid in the camera coating, in which is installed a pressure of 0.15-0.2 PA. Source �of elektronov was ignited discharge constant current (1 A). Then a voltage is applied (100-500) between fine-grained grid and anode with a diameter of 6 mm and a length of 250 mm, installed in the chamber coater, and within 20 min was carried out ion surface cleaning products at a bias voltage of-500V relative to the chamber walls coating at a current density of ions 1-2 mA/cm2. After ion cleaning, the bias voltage was reduced to 100, were lit magnetron discharge and were produced applying the adhesive sublayer of titanium with a thickness of 0.1 μm. Then into the chamber of the coating was assailed acetylene, the flow of which was set within the range 1 to 16 ml/min, the energy of the electron beam was reduced to 100 eV, set the beam current in the range of 0-1 A and produced a drawing of TiC/a-C:H coating thickness of 1-2 μm for 1-2 h at the temperature of the products is not more than 200°C.

An example implementation of the treatment by the proposed method are shown in Fig.2 in the form of dependences of microhardness of the surface of products made of hard alloy TC with coatings of TiC/a-C:H with a thickness of 1.5-2 μm, deposited at different electron beam currents (1-0; 2-0,5; 3-1 (A), obtained using microthermometry PMT-3. With increasing beam current from 0 to 1 And the flow rate of acetylene at which the maximum microhardness of the coatings decreases from 10 to 2 ml/min an increase in the beam current leads to an increase�Oia titanium content in the maximum of the curves from 26 to 38 at.%, what contributes to the growth of microhardness from 21.5 to 26 GPA GPA.

The experiment was conducted on the basis of his estimates show that implementation of the proposed method using the electron source with samankaltainen cathode allows to increase the beam current by more than an order of magnitude (up to 20 A), and treating the product with a large surface. Avoid heating the coating above 300°C and graphitization of the amorphous phase, resulting in decrease of microhardness, such a source should be used for the coating of large surfaces in combination with a more powerful magnetron (~10 kW). This setup will allow to process products with a total area of several thousand square centimeter

Sources of information taken into account

1. A. Baby, C. M. O. Mahony, P. D. Maguire. Acetylene-argon plasmas measured at a biased substrate electrode for diamond-like carbon deposition: I. Mass spectrometry. Plasma Sources Sci. Technol. 20 (2011) 015003.

2. A. Czy zniewski, W. Precht. Deposition and some properties of nanocrystalline, panel and amorphous carbon-based coatings for tribological applications. Journal of Materials Processing Technology 157-158 (2004) 274-283.

3. N. In. Gavrilov, D. R. Emlin, A. S. Kamenetsky. Highly efficient emission of the plasma cathode with grid stabilization. Technical physics, 2008, V. 78, no.10, pp. 59-64.

4. N. In. Gavrilov, A. I. Marshakov. A source of wide electron beams with samankaltainen hollow cathode for plasma nitriding of stainless steel. PTE, 2011, No. 5, pp. 140-148.

5. N. In. Gavrilov, A.�. Kaigorodov, A. S. Mamaev. Deposition of diamond-likeand-C:H coatings in a nonself-sustained discharge with a plasma cathode. Technical physics letters. 2009. Vol. 35. V. 1. P. 69-75.

The method of obtaining the products of hard alloys of two-phase nanocomposite coatings consisting of nanoclusters of titanium carbide dispersed in an amorphous hydrocarbon matrix, comprising applying the adhesive sublayer of titanium or chromium, magnetron sputtering of titanium target in a gas mixture of acetylene and argon at a pressure of 0.01 to 1 PA, and the deposition of the sputtered target particles and carbon-containing radicals on the surface of the products in combination with the bombardment of the surface by ions accelerated by the bias voltage, characterized in that before applying the adhesive sublayer product is subjected to surface cleaning by argon ions from the plasma generated by an electron beam, in the coating process, the gas mixture activated by impact of a beam of electrons with energy of 100 eV.



 

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1 ex, 1 tbl

FIELD: technological processes.

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3 cl, 1 tbl, 1 ex

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4 cl, 1 tbl

FIELD: metallurgy.

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1 tbl

FIELD: chemistry.

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2 cl, 2 ex

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9 cl, 6 dwg

FIELD: metallurgy.

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EFFECT: improving operability of a cutting tool.

1 tbl

FIELD: metallurgy.

SUBSTANCE: vacuum plasma application of multi-layered coating is performed. First, lower layer of nitride of titanium, aluminium and chrome is applied at the following component ratio, wt %: titanium 70.5-79.5, aluminium 14.0-20.0, chrome 6.5-9.5. Then, an upper layer of niobium nitride is applied. Application of coating layers is performed with three cathodes located horizontally in one plane, the first one of which consists of titanium and aluminium alloy, and the second one consists of niobium and is located opposite to the first one, and the third one consists of titanium and chrome and is located between them. The lower layer is applied using the first and the third cathodes, and the upper layer is applied using the second cathode.

EFFECT: obtaining of multi-layer coating, which improves operability of cutting tool.

1 tbl

FIELD: metallurgy.

SUBSTANCE: vacuum plasma application of multi-layered coating is performed. First, lower layer of nitride of titanium, aluminium and chrome is applied at the following component ratio, wt %: titanium 70.5-79.5, aluminium 14.0-20.0, chrome 6.5-9.5. Then, an upper layer of chrome nitride is applied. Coating layers are applied by cathodes arranged in the same horizontal plane, where first cathode is composed of titanium and aluminium, second cathode is made of chromium and opposed to the first cathode, and third cathode is made of titanium and chromium and positioned between first and second cathodes. The lower layer is applied using first and third cathodes, the upper layer - by the second cathode.

EFFECT: obtaining of multi-layer coating, which improves operability of the cutting tool.

1 tbl

FIELD: metallurgy.

SUBSTANCE: vacuum plasma application of multi-layered coating is performed. First, a lower layer of niobium nitride is applied. Further, top layer of titanium, zirconium and chrome composition nitride is applied at the following component ratio, wt %: titanium 78.0-84.0, zirconium 6.0-10.0, chromium 8.0-12.0. Coating layers are applied by cathodes arranged in the same horizontal plane, where first cathode is composed of titanium and zirconium, second cathode is made of niobium and opposed to the first cathode, and third cathode is made of titanium and niobium and positioned between first and second cathodes. The lower layer is applied using the second cathode, and upper layer - by first and third cathodes.

EFFECT: improving operability of a cutting tool.

1 tbl

FIELD: chemistry.

SUBSTANCE: catalyst contains carrier from porous zeolite KL and binding agent and catalytically active substance - platinum. Carrier additionally contains tin tetrachloride pentahydrate nanopowder, and as binding agent - mixture of gibbsite and rutile powders in equal proportions, with particle size of each not exceeding 40 mcm. Ratio of ingredients is in the following range, wt %: platinum - 0.3-0.8, mixture of gibbsite and rutile powders - 25-70, zeolite KL - 29.12-74.69, tin tetrachloride pentahydrate - 0.01-0.08. Claimed catalyst is characterised by high activity in reactions of aromatisation of synthetic hydrocarbons.

EFFECT: invention also relates to method of obtaining such catalyst.

2 cl, 1 tbl, 4 ex

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