Device for synthesis of coatings

FIELD: chemistry.

SUBSTANCE: device for synthesis of composite coatings contains a working vacuum chamber 1, an emission net 2 from a precipitated metal, a hollow cathode 3, limited by the emission net 2, an anode 4 inside the hollow cathode 3, a source 5 of an electric discharge supply, with a positive pole connected to the anode 4, and with a negative pole connected to the hollow cathode 4, a target 6, installed on the bottom of the hollow cathode 3 opposite to the emission net 2, a source 7 of high voltage, with a positive pole connected to the hollow cathode 3, and with a negative pole connected to the target 6, a source 8 of net voltage, with a positive pole connected to the anode 4 and with a negative pole connected via a high voltage diode 9 to the emission net 2, and a generator 10 of high voltage impulses, with a positive pole connected to the anode 4 and with a negative pole connected to the emission net 2.

EFFECT: creation of a device for synthesis of both conductive and dielectric coatings on products from conductive and dielectric materials, which would ensure the reduction to zero of current of accelerated ions on the surface of the product and impulse-periodical bombing of a synthesised on it coating by molecules of gas with energy of tens of keV.

1 dwg

 

The invention relates to a vacuum-plasma technique, namely the sources of metal atoms, mainly for the synthesis of wear-resistant nanocomposite coating in a vacuum chamber, and to the sources of the fast gas molecules, mainly for cleaning and heating products before synthesis of coatings to improve their adhesion to the product, as well as for bombarding the surface of the coating in the process of synthesis of fast molecules in order to give coverage required properties and further improve the adhesion by increasing the width of the interface (transition layer between the coating and the product) to several micromeres.

Known planar magnetron, in which the flat target of the necessary sprayed metal ions from a plasma glow discharge in the arched magnetic field near the surface of the target, which is the cathode discharge (U.S. patent No. 3878085, 1975). At the bombardment of the target ions, it emits electrons that are accelerated in the layer of positive space charge between the plasma and the cathode to energy eUtowhere Uto- the potential drop between the plasma and the cathode. Every electron that flew into the plasma, moving it along the segment of a circle, the perpendicular magnetic field is returned to the layer and reflected it back into the plasma. As a result, he passes through a closed polyline of kivalina the second path near the surface of the target path, exceeding the size of the target in hundreds and thousands of times. This allows you to maintain the discharge at a gas pressure of 0.1-1 PA transport of sputtered atoms to products.

Properties of the coating synthesized using a planar magnetron, strongly depend on the density allocated to its surface energy and the method of its supply. If, for example, when using a mixture of argon with nitrogen on a conductive substrate that is installed near a titanium target, serves the pulse voltage up to 50 kV negative polarity with a duration of 20 μs, following each other with a frequency of 25 Hz, instead of the standard coating of titanium nitride with a hardness of 2500 HV synthesized more viscous nanocomposite coating thickness up to 50 microns with a microhardness 5000 HV and the width of the interface is greater than 5 microns (C. Ruset, E. Grigore The influence of ion implantation on the properties of titanium nitride layer deposited by magnetron sputtering // Surface and Coating Technology. 2002. V.156. P.159-161).

The main disadvantage of the planar magnetron is the low utilization of the target material, spray only in a small area of its surface in the area of the arched magnetic field. In addition, the degree of ionization of the sputtered metal atoms does not exceed 10%, and the concentration of the discharge plasma is reduced outside the arched magnetic field at the surface of the substrate by several orders of magnitude. When the distance IU the control target and the product of 0.2 m and above it is impossible to provide the necessary current density bombarding floor ions, accelerated from the plasma acts on the substrate to a negative voltage. Therefore, to make the coating of the required properties are sources of ions or fast atoms and molecules.

Known sources of broad beams of fast molecules, in which the emitter of ions is plasma, glow discharge at a gas pressure of about 0.1 PA with electrostatic confinement of electrons in the trap formed by a hollow cathode and a negative attitude emission mesh (U.S. patent No. 6285025, 2001). Ions are accelerated between the plasma emitter and a secondary plasma in the vacuum chamber, separated from each other emission grid source with an opacity of 80%. Mesh absorbs 20% of the accelerated ions, but the rest come through its hole in the camera and as a result of collisions with the gas molecules become fast molecules. The number of fast molecules bombarding the surface of the product that is installed at a distance of 0.2 m from the grid source, exceeds the number of accelerated ions.

The main disadvantages of these sources are limited energy of fast atoms and molecules and the inability to reduce to zero the contents of the beam of charged ions that charge the surface of the dielectric products, which leads to uneven current density distribution of ions on the surface of the product and reduction and the energy consequently, unevenness of the surface treatment.

The closest solution to the technical nature of the invention is a device for the synthesis of coatings containing the working vacuum chamber, the emission grid, hollow cathode covered by the emission grid, the anode inside the hollow cathode, the power source of the discharge, a positive pole connected to the anode and the negative pole - hollow cathode, a target mounted on the bottom of the hollow cathode opposite the emission grid, high voltage source, the positive pole is connected to the hollow cathode, and the negative pole with the target and the source of grid voltage, a positive pole connected to the anode and the negative pole - emission net (Grigoriev S., Miller Y.A., Blizzard A.S. Discharge source of metal vapor and fast gas atoms // Instruments and experimental techniques. 2013. Issue 3. S-135. Fig.16). The device generates a mixed flux of metal atoms and bombarding synthesized floor fast molecules of the gas generated in the working vacuum chamber in the charge-exchange ions accelerated by the voltage between the plasma emitter inside the hollow cathode source and the secondary plasma inside the vacuum chamber, which are separated from each other emission grid. The metal atoms are formed as a result is asplenia target by argon ions from the plasma emitter, accelerated voltage of up to several kilovolts between the anode gas discharge chamber and a target. These atoms pass through the plasma emitter, and then together with accelerated ions fly through the emission grid with an opacity of 80% at the camera. From metal atoms and added to the argon reactive gas on the surface installed in the camera dielectric or conductive products synthesized wear-resistant coating, and the resulting recharge fast ions molecules bombard the coating in the process of its synthesis. The device allows to synthesize as conductive and dielectric coatings.

The disadvantage of this device is the inability to increase the energy of the bombarding synthesized floor fast gas molecules to 0.5 Kev and above due to the fact that during the continuous bombardment by argon atoms with such energy, all deposited on the product atoms are sprayed, as well as to reduce to zero the content in the mixed flow of metal atoms and fast gas molecules, ions that charge the surface of the dielectric products, which leads to uneven current density distribution of ions on the surface of the product and reduce their energy, and hence the unevenness of the surface treatment.

The technical task proposed solution is the creation of devices is to synthesize as conductive, and dielectric coating of conductive and dielectric materials, which would provide a pulse-periodic bombardment synthesized on her coverage of gas molecules with energies of tens of Kev and the reduction to zero of the current of accelerated ions on the surface of the product.

The problem is solved in that the device for the synthesis of coatings containing the working vacuum chamber, the emission grid, hollow cathode covered by the emission grid, the anode inside the hollow cathode, the power source of the discharge, a positive pole connected to the anode and the negative pole - hollow cathode, a target mounted on the bottom of the hollow cathode opposite the emission grid, a source of high voltage, positive terminal connected to the hollow cathode, and the negative pole with the target and the source of grid voltage, a positive pole connected to the anode, characterized in that it further comprises a generator of high voltage pulses, positive pole connected to the anode and the negative pole with the emission grid, and a high voltage diode, the positive output of the diode is connected to the emission grid, the negative output of the diode is connected to the negative pole of the source of grid voltage and the anode of the device connected to the working vacuum chamber.

The invention explains what I'm drawing in figure 1, which shows the diagram of a device for the synthesis of coatings.

A device for the synthesis of coatings contains a working vacuum chamber 1, the emission grid 2 of the deposited metal, the hollow cathode 3, a limited emission grid 2, the anode 4 inside the hollow cathode 3, the power source 5 of the discharge, a positive pole connected to the anode 4, and a negative pole connected to the hollow cathode 3, target 6, installed on the bottom of the hollow cathode 3 opposite the emission grid 2, 7 high-voltage source, the positive pole is connected to the hollow cathode 3, and a negative pole connected to the target 6, the source 8 of the grid voltage, a positive pole connected to the anode 4 and a negative pole connected through a high voltage diode 9 with the emission grid 2, and the generator 10 pulses of high voltage, a positive pole connected to the anode 4 and the negative pole is connected with the emission grid 2.

A device for the synthesis of coatings is as follows.

The working vacuum chamber 1 with the processed dielectric product 11 inside her pumped up to a pressure of 1 MPa, and then served in the camera 1 working gas, for example a mixture of argon with nitrogen (15%), and increase the pressure in the chamber 1 to 0.5 PA. Switching on the power source 5 is applied between the anode 4 and the hollow cathode 3 voltage UK of about 300 C. switching on the power source 8 is relativit between the anode 4 and the emission grid 2 voltage U cseveral times the voltage Utothat is necessary to prevent leaving a hollow cathode 3 issued them fast electrons through the holes of the grid 2. Using a control device (not shown) to ignite the gas discharge between the anode 4 and the hollow cathode 3. In the hollow cathode 3 is filled with a homogeneous plasma emitter 12 is separated from the surface of the hollow cathode 3 with a layer of positive space charge 13, from target 6 - layer 14, and from grid 2 - layer 15.

When Uwithfor ≥1 kV and 50 a/m2current density of argon ions from the plasma emitter on the cathode 3, the target 6 and the grid 2, the width d of the layer 15 between the grid 2 and the plasma emitter 12 exceeds the radius of 2.3 mm hole grid 2, drilled at a distance of 5 mm between their centers, which eliminates the leakage of plasma 12 of the hollow cathode 3 in the chamber 1. At an energy of 1 Kev accelerated in the layer 15 of the ions and the density of molecules no=1020m-3(suitable at room temperature, the gas pressure of 0.4 PA) length of the charge exchange ions of argon λp=1/σpnowhere σp=2,7×10 m2- cross recharge argon ions with an energy of 1 Kev, equivalent to 37 mm, which is 16 times greater than the width d of the layer 13. Ions 16, accelerated in the layer 15 and passed through the holes of the grid 2, decelerated in the layer 17 between the grid 2 and the secondary plasma 18 in the chamber 1 and go back to CE is ke 2. The boundaries between the layers 15 and 17 when the voltage on the grid of 1 kV is shown in figure 1 by the dashed lines. Plasma 18 is formed by the low-voltage discharge between the grid 2, a cathode, and the camera 1, which is its anode. Therefore, the concentration of plasma 18 is significantly less than the plasma concentration is 12, its potential is almost equal to the potential of the grounded chamber 1, and the width of the layer 17 is several times greater than the width d of the layer 15. After a few oscillations through the grid 2 all ions fall on its surface, whereas the average it does not exceed 1 see This is substantially less than the length of the recharge λp=37 mm, which almost completely eliminates the formation of the layers 15 and 17 fast neutral atoms and molecules.

When applying to the target 6 voltage 2 kV from source 7 ions 19 are accelerated in the layer 14 and with energies > 2 Kev and bombard spray the target 6. Resulting from its sputtering atoms 20 metal through the holes of the emission grid 2 is flown into the chamber 1 and are deposited on the article 11.

When applying for grid 2 voltage pulse amplitude 40 kV width d of the layer 15 between the plasma emitter 12 and the grid 2 at the same current density of ions 50 a/m2increases to d=0,037 m At an energy of argon ions ε=40 Kev, the cross section of their recharge is reduced to λp=10 m, and the length of the recharge increases to λp=1/σpno=0,1 m Is greater than the width d=0,37 m the Loya 15, but less than the sum of the widths of the layers 15 and 17. Therefore, when the migration of ions between 16 shown in figure 1 by solid lines the boundaries of the plasma emitter 12 and the secondary plasma 18 almost all of them become as a result of collisions with the gas molecules in the fast atoms and molecules 21 bombarding synthesized on the product 11 floor. Only a small number of ions, which has landed to the border of the secondary plasma 18, is reflected from it and returns to the grid 2. Since the energy of fast atom or molecule corresponds to the potential difference between the emission grid point in the layer 15 or layer 17 where there was a recharge, this energy is distributed continuously from zero to 40 Kev, and at a length of recharge λpgreater than the width d of the layer 15 in a few times, the maximum of the distribution is shifted towards the maximum ion energy ε=40 Kev.

The use of the generator high-voltage pulses connected to the positive terminal to the anode and the negative - emissions grid, allows to increase the total width of the layers between the plasma emitter and emission grid, and between the emission grid and a secondary plasma in the chamber to a value greater than the length of the charge exchange ions, which enables the generation of a neutral gas molecules with energies of tens of Kev and pulse-periodic bombing them as the wire is common, and dielectric coating of conductive and dielectric materials.

The use of high-voltage diode, the positive terminal of which is connected to the emission grid and the negative output is connected to the negative pole of the source of grid voltage, protects the source of grid voltage from the negative effects of pulses with amplitude up to 40 kV, which ensures trouble-free operation.

The connection of the anode of the device with the working vacuum chamber ensures the equality of the potentials of the plasma emitter ions and secondary plasma in the working vacuum chamber and reflected by the boundary of the secondary plasma accelerated ions, not turned into a fast neutral atoms and molecules, back in the direction of emission of the grid, which reduces the current of accelerated ions on the surface of the product to zero.

Compared with the prototype of the proposed device for the synthesis of coatings allows to synthesize viscous nanocomposite coatings with increased microhardness and interface width of up to 5 microns, and more. It provides superior adhesion and wear resistance of the coatings.

Analysis of the claimed technical solution for compliance with the conditions of patentability showed that specified in the independent claim, the symptoms are significant and inter is vasani between the formation of stable aggregates, unknown at the date of priority from the prior art, the required characteristics, sufficient to obtain the desired synergistic (sverhsummarny) technical result.

Thus, the above data confirm that the implementation of the use of the claimed technical solution the following cumulative conditions:

object embodying the claimed technical solution, it is suitable for synthesis of both conductive and dielectric coating of conductive and dielectric materials;

for the declared object as it is described in the following formula, confirmed the possibility of its implementation using the above described in the application or known from the prior art on the priority date tools and methods;

object embodying the claimed technical solution, its implementation is able to achieve perceived by the applicant of the technical result.

Therefore, the claimed object meets the requirements of patentability "novelty", "inventive step" and "industrial applicability" under the current law.

A device for the synthesis of coatings containing the working vacuum chamber, the emission grid, hollow cathode covered by the emission grid, the anode inside the hollow Kato is a, the power source of the discharge, a positive pole connected to the anode and the negative pole - hollow cathode, a target mounted on the bottom of the hollow cathode opposite the emission grid, a source of high voltage, positive terminal connected to the hollow cathode, and the negative pole with the target and the source of grid voltage, a positive pole connected to the anode, characterized in that it further comprises a generator of high voltage pulses, a positive pole connected to the anode and the negative pole with the emission grid, high voltage diode, the positive output of the diode is connected to the emission grid, the negative output of the diode is connected to the negative pole of the source of grid voltage and the anode of the device connected to the working vacuum chamber.



 

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