Method of producing galvanic composite coating containing nanodiamond powder

FIELD: chemistry.

SUBSTANCE: method involves preparation of a suspension of nanodiamond powder and a liquid phase, adding the suspension to an electrolyte and conducting electrolysis to deposit a composite coating. The liquid phase used to prepare the suspension is ethyl alcohol or acetone, wherein the nanodiamond powder is added to the liquid phase in amount of 60-80 vol. %, and the powder in the suspension is dispersed by crushing and attrition grinding with a lap, after which the suspension is added to the electrolyte.

EFFECT: dispersing nanodiamond powder and endowing the powder with resistance to sedimentation and coagulation in the electrolyte.

 

The invention relates to the production of galvanic composite coatings, in particular on the basis of Nickel dispersed phase in the form of nano-diamond powders.

The method can be used for the manufacture of diamond tools in which the cutting of the diamond grains are held on the tool body by means of the galvanic composite coatings based on Nickel containing nanodiamond powders. Also the method can be used for deposition of composite coatings to improve hardness, wear resistance of machine parts, instruments, cutting tools, etc.

Galvanic composite coatings are metallic matrix containing a dispersed phase, in particular nano-diamond powders deposited on the surface of an electrolyte containing a salt of the deposited metal and nano-diamond powders. The coating quality is largely determined by the state of the dispersed phase, its concentration and distribution in surface and coating thickness. The concentration and distribution of the particles in the coating to a greater extent depends on sedimentation and coagulation stability of the dispersed phase in the electrolyte, the concentration of particles in the electroplating bath.

A method of obtaining composite coatings comprising introducing into the electrolyte diamond particles RA is the mayor of 1-1000 nm, suspending electrolyte gas, containing oxygen (JP No. 2006225730, CL C25D 15/02, 2006). The result is an electrolyte with evenly distributed over the volume of the diamond particles. The disadvantage of this method is that the suspending of the diamond particles in the electrolyte gas is not attached to the particle sedimentation and coagulation of sustainability, as it does not guarantees the complete destruction of the conglomerates of particles, which does not allow to obtain high-quality coverage.

A method of obtaining composite coatings of electrolytes, including the introduction of electrolyte dispersed phase of nanodiamonds and dispersion effects on the electrolyte cavitation, passing it through cavitation disperser, or the use of hydrodynamic or acoustic dispersant (RU # 2368709, CL C25D 15/00, 2007). The disadvantage of this method lies in the use of complex devices for dispersion of the particles in the electrolyte.

A method of obtaining composite coatings of electrolytes, including effects on electrolyte containing solid submicroscale ultrasonic vibrations. Under the action of ULTRASONIC vibrations is diperkirakan conglomerates submicroscale to the level of initial formations or crystallites, thus increasing the viscosity of the electrolyte and increased sedimentation stability (EN No. 2088689, CL C25C 18/00, 1996).

<> A method of obtaining composite coatings, offering to use colloidal cluster diamond particles with a size of 0.001-0,120 μm, the shape close to spherical or oval without sharp edges, in an amount of 0.1 to 35 g/l, which form a sedimentation and coagulation sustainable system in the electrolyte (RU # 2191227, CL C25D 15/00, 2000).

The drawback of these methods is that the sedimentation stability of the particles is provided defined by the shape and size of the particles, which significantly narrows the scope of the use of such an electrolyte.

A method of obtaining composite coatings of electrolytes, which is injected surfactant containing one amino group and one carboxypropyl or their mixture. Surfactant forms on the surface of the shell particles, preventing their agglomeration (RU # 1097718, CL C25D 15/00, 1982). A method of obtaining composite coatings comprising introducing into the electrolyte diamond particles treated with anionic wetting agent of the type that increases agglomeration resistant particles (GB No. 1391001, CL C25D 15/00, 1975). The disadvantage of the methods is that the surfactants and wetting agent adsorbed on the surface of dispersed particles, enters the coating material, affecting its physical and mechanical properties. In addition, surfactants and wetting, reducing the degree of agglomeration of the particles, do not provide endostatin dispersion in the electrolyte.

A method of obtaining composite coatings comprising preparing a suspension of ultradispersed diamond size up to 300 nm water-based with the addition of stearates and silicon dioxide. After mixing the ingredients, the suspension is injected into the electrolyte and carry out the electrolysis. The introduction of electrolyte additives allows to obtain a stable suspension of certain sizes of units (RU # 2094371, CL C25D 15/00, 1991). The disadvantage of this method is that introduced into the electrolyte additives during electrolysis, getting into the coating material, negative impact on the physico-mechanical characteristics of the coating.

A method of obtaining composite coatings comprising preparing a suspension of water-based, which after the introduction into it of the dispersed phase in the form of detonation diamond process for desegregation high sedimentation and coagulation stability on rotor-pulse or ultrasonic installation heated for 2 hours in hydrochloric acid, washed sediment from excess acid, then treated for 2 hours with a solution of caustic soda (RU # 2357017, CL C25D 15/00, 2007). The disadvantage of this method lies in the complexity and duration of the slurry preparation, significant loss of diamond powders in the preparation of the suspension.

A method of obtaining composite n the floor, comprising preparing a suspension of water-based, which is injected into the electrolyte. The suspension contains particles of synthetic diamond carbon material containing carbon in the form nuclei of ultradispersed diamond, surrounded by a shell containing x-ray amorphous carbon, and having on the surface of the particle surface functional groups containing oxygen, nitrogen and hydrogen (RU # 2404294, CL C25D 15/00, 2009). Diamond-containing material obtained by processing pre-dried powder of diamond-containing mixture which is a mixture of diamond and non-diamond forms of carbon with nitric acid at boiling within 2-5 hours, the Suspension is introduced into the electrolyte, provides a high dispersive capacity of the electrolyte. The disadvantage of this method lies in the complexity of the process of obtaining particles of synthetic diamond carbon material.

The closest way is to obtain a composite metalloorganic coatings from an electrolyte containing ultra-fine diamond powders with a specific surface area of 400-500 m2/g high degree of purification in the amount of 2-20 g/l (RU # 2156838, CL C25D 15/00, 1999). To obtain a homogeneous system of ultradispersed diamond powder is introduced into the electrolyte in the form of a suspension. A suspension is prepared from ultrafine diamond and electrolyte with concentration is the situation ultrafine particles 28-30%, then concentrate in a few tricks dilute electrolyte with thorough stirring to obtain a suspension with a concentration of ultradispersed diamonds 8-10%. The obtained suspension is injected into the electrolyte. The method allows easy enough to mix the ultra-dispersed diamond powders with electrolyte. The disadvantage of this method is that when mixing the suspension with a concentration of ultrafine particles 28-30% is disaggregation, i.e. ultrafine diamond particles constituting the aggregates of different sizes and different shapes, suspensions retain their original condition. In addition, the processing of ultrafine particles in the same electrolyte, in which electrolysis is carried out, not attached to the particles of the required sedimentation and coagulation stability.

The technical challenge is to create a method of producing composite coatings, allowing you to simply and efficiently perform the disaggregation of nanodiamond powders and give them high sedimentation and coagulation stability in the electrolyte, which allows to obtain coatings with a uniform distribution of the nanoparticles on the surface and the volume of coverage.

The technical solution of the problem is that in the process for electroplating composite coatings containing nasoalmo the nye powders, comprising preparing a suspension of nanodiamond powders and liquid phase, the introduction of the suspension into the electrolyte and electrolysis for the deposition of composite coatings, as a liquid phase to obtain a suspension take ethyl alcohol or acetone, with nanodiamond powders injected into the liquid phase in an amount of 60-80% vol. and perform disaggregation in suspension of nanodiamond powders by crushing and abrasion, after which the suspension is introduced into the electrolyte.

As the liquid phase is also possible to take an aqueous solution of ethyl alcohol or acetone.

The method consists in the following. Crushing and abrasion of nanodiamond powders produce, for example, in a vessel with curved bottom by priter. When high concentrations of nano-diamond powder in suspension, aggregative state which approaches pasty, disaggregation will occur not only due to the crushing and abrasive effects of priter powders on the sides and bottom of the vessel, but also the influence of aggregated nano-diamond powders on each other. It is not only a disaggregation of powders, but the simultaneous handling of ethyl alcohol or acetone to form on the surface of nanodiamond powders shell, caking of the particles in the electrolyte, which increases sedimentati is nnow stability of particles in a long time.

The method is as follows.

From nanodiamonds preparing a suspension containing ethyl alcohol or acetone. The number of nanodiamonds in the liquid medium should be 60-80%. At a concentration of nanodiamond suspension has a state of near pasty. The suspension is prepared mainly in a porcelain vessel, the bottom of which has a curved shape. For the disaggregation of nanodiamond particles their crushed and grated, for example, preterm, the shape of the working surface of which is similar to the shape of the bottom porcelain vessel. Crushing and abrasion produced manually or mechanized.

The electrolyte is prepared by dissolving metal salts in distilled water and work it under shock for 1 h Then an electrolyte is injected part. After mixing the components in a bath of the Nickel plating enter suspension with nanodiamonds. After that make electrolysis, in which the surface is deposited composite coating containing nano-diamond powders.

The concentration of 60-80% of nanodiamond powders in suspension provides effective disaggregation. At a lower content of nanopowders in suspensions in the past will be present a large amount of liquid phase, which will substantially increase the complexity of disaggregation of nanopowders and possible partial dezagregare the interview. Increasing the concentration of nano-powders in suspension will greatly reduce the amount of liquid phase is ethyl alcohol or acetone, with a small number of these components will not be sufficient for effective wetting of nanodiamond powders and education sheath that prevents them from sticking together in the electrolyte and provide sedimentation stability.

Ethyl alcohol and acetone, in contrast to the electrolyte, well moisten diamond powders and spreading on the surface of nanodiamond particles penetrate inside the unit. Simultaneously, ethyl alcohol and acetone interact with polar functional groups adsorbed on the particles of the diamond, forming on their surfaces positively charged membrane, which provides a wedging action on the particles prevents their aggregation in the electrolyte and on the electrophoretic mechanism contributes to the movement of particles to the cathode. Crushing and abrasion of nanodiamond powders in an aqueous solution of ethyl alcohol or acetone allows you to more effectively and efficiently to produce the dispersion of powders in a short time.

In addition, introduced into the electrolyte ethyl alcohol or acetone, which is the liquid phase in suspension work in the electrolyte as a leveling additive, allowing for smooth high-quality coverage. If neo is needed, ethyl alcohol and acetone can be introduced into the electrolyte additionally in the required amount.

Ethyl alcohol and acetone in a suspension can be used in the form of 70-80% water solution. The use of aqueous solutions of these components is more economical.

Under the proposed method produced diamond tools - diamond tube drills.

In the diamond tool of the composite coating is a material retaining workers of diamond grains on the body of the tool.

In a vessel with a curved bottom was preparing two suspensions containing nanodiamond powders and liquid phase. In the same suspension as the liquid phase used an aqueous solution of ethyl alcohol, another aqueous solution of acetone. The concentration of nanodiamond powders were 60-80 vol.%. Preterm manually crushed and rubbed aggregates of nano-diamond powders for 15 minutes. The result has been close to the pasty state of a homogeneous mass of nanodiamond powders without conglomerates, clots, etc.

Prepared two baths of the following composition:

Nickel sulfate 7-water and 300 g/l

Nickel duplissy 6-water - 50 g/l

Boric acid 40 g/l

The first bath was carried out by attaching and partial silting on the housing of the working tool diamond powder grain 125/100 layer of Nickel values is 20 microns.

The tool body part is overgrown with partially into the first tub working diamond powders were draped in the second tub. The electrolyte was introduced to one of the suspensions were thoroughly mixed and produced by electrolysis before the deposition of the layer composite coating to silting working diamond powders on the value of 70-80% of their size. The number of nanodispersed powder in the coating is regulated by the amount introduced into the electrolyte suspension.

Received the tool, in which the matrix finally sarasaviya working diamond powders on the tool body, was a composite coating containing nano-diamond powders. The coating had a uniform thickness of sediment. To determine the quality of galvanic coatings containing nano-diamond powders, the coating was applied on a specially prepared foil and the surface was examined with an electron microscope (photos, pictures in dark field and their Fourier images). The surface had a low uniform roughness for the given current density, nano-diamonds were found in the structure of the Nickel coating in the form of agglomerates. Use ethyl alcohol or acetone led to a decrease in the number of agglomerates and to a more uniform distribution of the particles in the structure of the Nickel cover the Oia.

Thus, the introduction into the electrolyte nanodiamond powders by means of preliminary preparation of suspensions with a high content of nano-diamond powders in the liquid phase of ethanol or acetone allowed to provide effective disaggregation of nanodiamond powders and to obtain a coating with high physical-mechanical properties due to high sedimentation and coagulation stability of the particles in the electrolyte.

A method of obtaining a composite electroplating coatings containing nano-diamond powders, comprising preparing a suspension of nanodiamond powders and liquid phase, the introduction of the suspension into the electrolyte and electrolysis for the deposition of composite coatings, characterized in that the liquid phase to obtain a suspension take ethyl alcohol or acetone, with nanodiamond powders injected into the liquid phase in an amount of 60-80% vol. and perform disaggregation of powders in suspension by crushing and abrasion by Pitirim, after which the suspension is introduced into the electrolyte.



 

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