Composite filler in the form of powder and a process for preparation thereof

FIELD: composite materials.

SUBSTANCE: invention relates to powdered composite filler for elastomer materials suitable for fabrication of articles operated under dry friction or increased wear conditions used in engine, compressor, and pump manufacturing industries. Particles of filler comprise at least one nucleus of inorganic material, in particular quasi-crystalline alloy Al-Cu-Fe or quasi-crystalline alloy Al-Cu-Cr and shell made from thermoplastic polymer with elasticity modulus 0.5 to 5.0 GPa and volume fraction of nuclei in a filler particle 1 to 10%. Process of preparing such composite filler resides in that inorganic material particles are activated in a mechanochemical activator with mechanical energy supply intensity 1 to 5 kW/kg and dose 30 to 1000 kJ/kg in a medium selected from a series: air, nitrogen, argon, and vacuum at pressure from 10-2 to 1 atm until particles with average size not larger than 15 μm are obtained, after which shell polymer is added to activator and inorganic material particles are modified at mechanical energy supply intensity 0,05 to 0.5 kW/kg and dose 3 to 100 kJ/kg in a medium selected from a series: air, nitrogen, argon, and vacuum at pressure from 10-2 to 1 atm.

EFFECT: lowered coefficient of friction under dry friction conditions and substantionally reduced summary rate of wear of friction pair under hydroabrasive wear conditions.

3 cl, 2 dwg, 3 tbl

 

The present invention relates to fillers for elastomeric materials, working in conditions of dry friction or increased wear and used in the engine, compressor, naaso-building and other industries.

Know the use of powders of metals and alloys as filler in polymer compositions to obtain a wear-resistant products. (Gscas, Dvilansky. Fillers for polymer composites. M.: Chemistry, 1981, S. 234, 245). However, metal powders have low adhesion to the elastomeric matrix, which makes it impossible to obtain high-quality products made of elastomeric materials.

Know the use of quasicrystal Al-Cu-Fe composite Al-Cu-Fe occurring quasicrystal/high-pressure polyethylene for the manufacture of biomaterials for prosthetic hip joint. (Anderson, B., Bloom, P.D., Al-Cu-Fe Quasicrystal/Ultra High Molecular Weight Polyethylene Composites as Biomaterials for Acetabular Cup Prosthetics, Biomateriaals 2002, 23, 1761).

Know the use of quasicrystal Al-Cu-Fe composite Al-Cu-Fe occurring quasicrystal/epoxy material (Bloom, P.D., Baikeraker, K.G., Fabrication and weer resistance of Al-Cu-Fe Quasicrystal-epoxy composite materials, Materials Science and Engineering A, 2003, 360 (1-2), 46.

Know the use of quasi-crystals in the polymer/quasicrystal composites. (Bloom, P.D., Baikeraker, K.G.,Development of Novel Polymer/Quasicrystal Composite Materials, Materials Science and Engineering A, 2000 294-296,156). Use fill the lei of the quasi-crystals in a polymer matrix attached to the products antiwear properties, but due to poor adhesion of the particles of the quasi-crystal elastomer matrix, it is impossible to obtain high-quality products with their use of elastomeric materials.

As a prototype for the composite filler in powder form and method thereof selected composite filler in powder form and method thereof disclosed in the description of the patent US 5182173, WV 25/20, 1993, the Filler contains a single particle, at least one core of inorganic material, for example of metal, and a shell made of silicone elastomer which is the reaction product of monofunctional siloxane and secondary multifunctional silane. The connection of the core with the shell chemical.

The method of obtaining the specified filler includes bringing in the interaction liquid polysiloxane and Milanovich components, application received reactionepisode liquid on the surface of inorganic particles by stirring in a stirrer - mixer drum with the addition of solvent.

The specified filler is well distributed in the polymer matrix, allows to obtain high-quality products, but as the shell includes a shell made of a polymer derived from silicon rubber, and does not involve the manufacture of the shell of the other polymer materiality the method involves obtaining a composite filler in the form of powder in the shell from the liquid phase and does not allow you to get the filler in the shell of the solid phase.

The objectives of the present invention are expanding the range of fillers having high adhesion to the elastomeric matrix, with the shell not only from polymers derived from silicone rubber, and a method of obtaining a composite filler in powder form, the particles of which contain quasi-crystalline alloy in the shell in which the shell is made of solid phase.

These problems are solved by creating a composite filler in powder form, the particles of which contain at least one core of inorganic material and a shell of polymer, in which the inorganic material it contains quasicrystalline alloy Al-Cu-Fe or quasicrystalline alloy Al-Cu-Cr, and as the polymer shell contains a thermoplastic with a modulus of elasticity of from 1.5 to 5.0 GPA, and volume fraction of nuclei in the particle composite filler is from 0.1 to 10.0%. The particle size of the composite filler is not more than 50 μm.

The method of obtaining the specified composite filler in powder form lies in the interaction of particles of inorganic material and a polymer in which particles of inorganic material in the form of quasi-crystalline alloy Al-Cu-Fe or quasicrystalline alloy Al-Cu-Cr activate in mechanochemical activator with the intensity of the supply of fur is practical energy from 1 to 5 kW/kg and a dose of from 30 to 1000 kJ/kg in the environment, chosen from a number of: air, nitrogen, argon, vacuum pressure of 10-2to 1 ATM, to obtain particles with an average size of not more than 15 μm, after which the activator is injected polymer in the form of a thermoplastic polypropylene polymer with a modulus of elasticity of from 1.5 to 5.0 GPA and modify particles quasicrystalline alloy Al-Cu-Fe or quasicrystalline alloy Al-Cu-Cr intensity of the supply of mechanical energy from 0.05 to 0.5 kW/kg and a dose of from 3 to 100 kJ/kg in an environment selected from a number of: air, nitrogen, argon, vacuum pressure of 10-2to 1 ATM.

The invention is illustrated by drawings, where figure 1 presents a composite filler in powder form with a single core-shell, figure 2 - composite filler in powder form with multiple nuclei in the shell.

Composite filler comprises at least one core 1 and sheath 2. The core 1 is made of quasicrystalline alloy Al-Cu-Fe or quasicrystalline alloy Al-Cu-Cr, the shell 2 of the polymer. As the polymer contains a thermoplastic with a modulus of elasticity of from 1.5 to 5 GPA, for example high density polyethylene (modulus of 1.9 to 2.2 GPA), polytetrafluoroethylene (elastic modulus of 1.5 to 1.6 GPA), polyster (modulus of 4.9-5.0 GPA). The elastic modulus measured at room temperature. (For reference: the modulus of elasticity of the polymer on the basis of silicone rubber - prototype - is 0,0-1,0 HPa). The volume fraction of nuclei in the particle composite powder filler is from 0.1 to 10.0%.

The method of obtaining the proposed filler implemented as follows.

Particles quasicrystalline alloy Al-Cu-Fe or quasicrystalline alloy Al-Cu-Cr is placed in the working chamber of mechanochemical activator together with grinding bodies. Volume chamber, the volume of the grinding bodies, the dynamic characteristics of mechanochemical activator selected so as to ensure that the intensity of the supply of mechanical energy to obrabativaem material. The activation process was performed at room temperature with the intensity of the supply of mechanical energy from 1 to 5 kW/kg in an environment selected from a number of: air, nitrogen, argon, vacuum pressure of 10-2to 1 ATM. The required dose summed mechanical energy in the range from 30 to 1000 kJ/kg is achieved by processing at a given intensity. The activated receive particles quasicrystalline alloy Al-Cu-Fe or quasicrystalline alloy Al-Cu-Cr with an average particle size of not more than 15 μm.

Through a boot device in the working chamber of mechanochemical activator impose additional powder of a thermoplastic polypropylene polymer with a modulus of elasticity of from 1.5 to 5.0 GPA with an average particle size up to 100 microns. The amount of injected thermoplastic must meet the AMB volume fraction of thermoplastic in the final product. Dynamic parameters of mechanochemical activator (frequency and amplitude) change in such a way as to ensure the intensity of the supply of mechanical energy to the processed material in the range of 0.05 to 0.5 kW/kg Required dose summed mechanical energy in the range from 3 to 100 kJ/kg is achieved by a sufficient duration of processing at a given intensity. The environment in which the processing is selected from a range of: air, nitrogen, argon, vacuum pressure of 10-2to 1 ATM.

As a result of processing particles quasicrystalline alloy Al-Cu-Fe or quasicrystalline alloy Al-Cu-Cr receive composite filler in powder form, the particles of which contain quasi-crystalline alloy in the shell of polymer.

As a matrix, use composition based on butadiene-nitrile, ethylene-propylene rubbers, butyl rubber, fluorinated rubber.

The invention is illustrated by the following examples.

Particles quasicrystalline alloy Al-Cu-Fe or quasicrystalline alloy Al-Cu-Cr with a particle size of from 10 to 80 μm and an average particle size of 50 microns is placed in the working chamber of mechanochemical activator together with grinding bodies - a set of metal and/or agate balls ranging in size from 3 to 15 mm in diameter and activate the modes (the intensity of the supply of mechanical energy, with the Tav processing environment), listed in table 1. The activated receive particles of quasi-crystalline alloy with an average particle size shown in table 1. Through a boot device in the working chamber of mechanochemical activator impose additional granules of high-pressure polyethylene (LDPE), having a modulus of 1.9 to 2.2 GPA, or granules of polytetrafluoroethylene (PTFE)having an elastic modulus of 1.5 to 1.6 GPA, or granules polyster (SFC), having a modulus of 4.9 to 5.0 GPA, with an average particle size up to 100 microns. Characteristics of the activation process quasicrystalline alloys (intensity, dose supply mechanical energy to the processed material, as well as the composition of the medium processing) shown in table 1. The size obtained after processing of particles and volume fraction of nuclei in the particle of the filler shown in table 1. Particle size was determined using semimetrics analysis.

The obtained composite material was inserted in the rubber mixture based on butadiene-nitrile rubber SKN-26, full of technical carbon (120 parts by weight), it was molded workpiece and vulcanizable products. Samples obtained from the specified rubber mixtures containing composite filler and without it (control sample), were investigated on the machine end friction MTT-2 at sliding velocity of 4.4 m/s under normal loads the ke 16 and 19.2 N without lubrication (dry friction) and on the installation, simulating friction axial bearing stage submersible pump ESP. Testing of the lower washer impeller (NSRC) was performed at the stand for accelerated tribological testing of elastomeric bearings degrees with the vertical location of the pump Assembly. Experimental pump consisted of a 5-speed manual ESP 5-50, made by powder metallurgy. The material response NSRC details - clamp guide vanes (BSEARCH)-powder steel Ggrd. The concentration of the abrasive material in the fluid was 0.2% (2 g/l). Comparative values of velocities of the wear test samples NSRC obtained in pumping mode 50 m3/day. Test duration for each group of samples NSRC was 6 hours. The coefficients of friction under conditions of dry friction are given in table 2. Frictional properties of samples in terms of hydroabrasive wear are shown in table 3.

From the data presented in table. 1, it is seen that the present invention allows to obtain a composite filler in powder form, the particles of which contain at least one core of the quasicrystal in the shell, which has adhesion to the polymer matrix, thus expanding the range of fillers in powder form by increasing classes of polymers used as the shell having adhesion to the polymer matrix, the proposed method of manufacturing a composite filler in powder form by processing the quasicrystalline alloy Al-Cu-Fe or quasicrystalline alloy Al-Cu-Cr solid thermoplastic.

From the data presented in table 2 and 3, it is seen that the introduction of a composite filler in powder form in the rubber mixture leads to a decrease of the coefficient of friction under conditions of dry friction and a significant reduction in the total wear rate of the friction pair in terms of hydroabrasive wear.

Proposed by the present invention a composite filler expands the range of fillers having adhesion to the polymer matrix, which enable the production of their use of wear-resistant under conditions of dry friction and abrasive wear of elastomeric materials, and the proposed method for the specified filler allows to obtain a composite filler in powder form, the particles of which contain at least one core of the quasicrystal and a shell of a polymer made from a solid phase.

Table 1
Characteristics of the method of obtaining a composite filler in powder form
# exampleOccurring quasicrystalPolymerThe intensity of the supply of mechanical power, kW/kgDose of mechanical energy, kJ/kg Pressure, ATM.The average particle size, micronsThe volume fraction of nuclei in the particle filler, %The resulting structure filler
When activatedWhen modificationsWhen activatedWhen modificationsWednesdayWhen activatedWhen modificationsAfter activationAfter modification
12456789101112131415
1Al-Cu-FeHDPE20,151000100The vacuum10-210-215402,0Composite filler in the sheath of HDPE
2Al-Cu-FePTFE40,2510030Nitrogen115406,0Composite filler in the PTFE membrane
3Al-Cu-CrHDPE1 0,05303The air1110509,6Composite filler in the sheath of HDPE
4Al-Cu-CrPTFE50,550050Argon115401,2Composite filler in the PTFE membrane
5Al-Cu-FeSFC30,2500100The air1110409,6Composite filler in the shell of the SFC

Table 2
The coefficient of friction under conditions of dry friction
# exampleLoadThe coefficient of friction
Without fillerContent filler
10 parts by weight20 parts by weight
Control160,25
19,20,28
1160,090,11
19,20,130,145
2160,070,08
19,20,120,125
3160,080,09
19,20,120,125
4160,0650,085
19.20,110,10
Table 3
Frictional properties in terms of hydroabrasive wear
IndicatorsTest caseExample 4 according to the invention
Content filler
10 parts by weight20 parts by weight30 parts by weight
The average wear rate NSRC, µm/h3,140,370,280,27
The standard deviation of the wear rate NSRC, µm/h3,260,140,070,12
The average wear rate BSEARCH, µm/h17,115,314,718,3
The standard deviation of the wear rate BSEARCH, µm/h32,45,64,17,4
The total wear rate pairs NSRC-BSEARCH, µm/h20,2415,6714,98a 18.57

1. Composite filler in powder form, the particles of which contain at least one core of inorganic material and a shell of polymer, characterized in that the inorganic material it contains quasicrystalline alloy Al-Cu-Fe or quasicrystalline alloy Al-Cu-r, and as the polymer shell contains a thermoplastic with a modulus of 1, 5 to 5.0 GPA, and volume fraction of nuclei in the particle filler is from 1 to 10%.

2. Composite filler in powder form according to claim 1, characterized in that the particle size of the filler is not more than 50 μm.

3. A method of obtaining a composite filler in powder form, the particles of which contain at least one core of inorganic material and a shell of polymer, which consists in the interaction of particles of inorganic material and a polymer, wherein the particles of inorganic material in the form of quasi-crystalline alloy Al-Cu-Fe or quasicrystalline alloy Al-Cu-Cr activate in mechanochemical activator with the intensity of the supply of mechanical energy from 1 to 5 kW/kg and a dose of from 30 to 1000 kJ/kg in an environment selected from a number of: air, nitrogen, argon, vacuum pressure from 10-2to 1 ATM, to obtain particles with an average size of not more than 15 μm, after which the activator is injected polymer in the form of a thermoplastic polypropylene polymer with a modulus of elasticity of from 1.5 to 5.0 GPA and modify particles quasicrystalline alloy Al-Cu-Fe or quasicrystalline alloy Al-Cu-Cr intensity of the supply of mechanical energy from 0.05 to 0.5 kW/kg and a dose of from 3 to 100 kJ/kg in an environment selected from a number of: air, nitrogen, argon, vacuum pressure of 10-2to 1 ATM.

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