Method of obtaining super-hard composite material

FIELD: chemistry.

SUBSTANCE: initial composition, consisting of the following components, wt %, is prepared: C-60 or C-70 fullerenes - 30-50; heat-conducting component - 10-60; binding agent - the remaining part. The heat-conducting component is selected from the group: wurtzide boron nitride, cubic boron nitride, diamond or their mixtures. The binding agent is selected from elements of the group IVa of the Periodic system or their alloy with copper. The heat-conducting element can be preliminarily covered with the binding agent. The obtained composition is subjected to impact of static pressure from 8 to 13 GPa with heating to 900-2000°C for not less than 20 seconds. A superhard composite material with heat-conductivity to 330 W/m·K, a ratio of microhardness to an elasticity coefficient 0.12 is obtained.

EFFECT: high wear resistance of the material.

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The invention relates to the production of superhard composite material, namely, the method of production of superhard composite materials based on carbon for the manufacture of materials that can be used in tools for mining, stone processing and Metalworking industries.

Famous patent of the RF No. 2 127 225; IPC SW 31/06, priority from 11.10.1996,) /Superhard carbon material, its manufacturing method and a product made of carbon material"/.

As a source of carbon material using a new allotropic form of carbon, fullerene C-60. On the fullerene C-60 effect of quasi-hydrostatic pressure of 7.5 to 37 GPA and a temperature selected in the range 20-1830°C with a holding time of not less than one second, high pressure apparatus: type "toroid"type Bridgman anvils, etc. When exposed to the original fullerene pressure and temperature is the polymerization of the molecules or fragments of molecules of the fullerene. Depending on the devices receive the product in the form of films (in Bridgman anvils, pressure up to 37 GPA) or in the form of bulk samples, using other kinds of apparatus (pressure of 7.5-13 HPa). Compact samples of the material have high mechanical and electrical properties. For example, the indenter of the polymerized fullerene mo is but to cause scratches on the faces of the diamond single crystals. According to x-ray analysis and the structure of the obtained target product differs from the structure of diamond and depends on parameters when thermobaric treatment of the source material. The method allows from the original fullerene to produce items that have the specified form.

Following the highest characteristics of some structural types polymerized fullerenes: the hardness of superhard carbon material is 20% greater than the hardness of the diamond, the density of 2.1-3.5 g/cm3the hardness is 50-170 HPa and above, the electrical conductivity of 10-6-10-2Ω-1·cm-1, thermal stability up to 1000°C. the Material is not soluble in organic solvents and inorganic acids.

It is established that the speed of ultrasound (CL=26 km/s) in samples ultratorch modifications of fullerene C60and C70exceeds the speed of sound in diamond. The material has a high elastic moduli. When this modification of polymerized fullerene are different from the diamond crystalline or amorphous structure, the formation of which depends on pressure and temperature during the synthesis / Journal of experimental and theoretical physics, (1998) T, issue 4 (10), str-1374 /. Along with high mechanical properties of the polymerized fullerene has a very low thermal conductivity of ~ 3 W/m*K, which is significantly lower than th is provodnosti other superhard materials. The disadvantage of this method is the low thermal conductivity of polymerized fullerene, which complicates its use for the manufacture of tools for Metalworking, stone cutting, and drilling equipment. Method for obtaining a wear-resistant material containing superhard particles of fullerene C-60 in the matrix of the iron-based(RF Patent No. 2123473, with priority from 07.05.1998,, IPC SW 31/06, SS 26/00). "Method of production of superhard carbon particles and wear-resistant material, ObjectName these particles".

The invention relates to powder metallurgy, in particular the production of superhard carbon particles in the volume of iron-carbon alloys used for products operating in conditions of wear. The method allows to obtain superhard carbon particles up to 0.5 mm and is compressing the mixture of powders of iron and fullerites, the synthesis of superhard carbon particles at high pressures and temperatures and the subsequent removal of those particles. Isostatic pressing is carried out at a low pressure of 2.5 to 4.5 GPA and temperatures of 1000-1200°C. Wear-resistant material contains iron or carbon steel and superhard carbon particles up to 0.5 mm in an amount up to 20%. The technical result of the invention is to increase the size and number of superhard particles in the volume of the IU iron-carbon alloys and in the production of a material, the wear exceeds the wear resistance of the known alloys HM and satellite.

The disadvantage is the limited use of material tools designed for rock-work, since the concentration of carbon particles in a metal matrix is low and the hardness (~ 30 GPA) is significantly inferior to the diamond and other superhard materials.

The famous "Fullerene composite" (U.S. patent No. 5648056, SW 31/02, 15.07.1997,). Fullerene composite includes a matrix formed of ultrafine fullerene, such as fullerene C-60, having diameters of from 5 to 50 nm and a reinforcing element forming a mixture consisting of nanotubes, carbon nanocapsules and inevitable uncertain carbon impurities embedded in a matrix. The number of reinforcing element embedded in a matrix and are in the range from 15 to 45 wt.% relative to the matrix. Through the use of a reinforcing element, which contains carbon nanotubes and carbon nanocapsules made of fullerene composites provide an opportunity to achieve improved mechanical strength and resistance to deformation.

The material has a high tensile strength (15 MPa), however, other mechanical properties are insufficient to create effective tools to use when is the processing of stone and hard alloys.

The closest technical solution is Sintered carbon materials based on fullerene" (U.S. patent No. 6 783 745, SW 31/02, 31.08.2004,). Declared a new class of carbon materials based on fullerene and the method of their synthesis. Including a solid material having a density higher than 2.3 g/cm3and the hardness of from 1.0 to 50 HPa, formed in the process, including: 1) preparation of powder of carbon-based fullerene containing at least 99.9% of single-walled nanotubes; 2) the compacting of the specified powder to a density higher than 1.4 g/cm3; 3) the effect on the powder pressure of 1 to 10 GPA and temperature range from 300-1000°C for a period of time from 1 to 10000 seconds.

Stated also options that allow them to form a sintered conductive carbon material of high density (above 1.4 g/cm)and has a hardness of from 1 HPa to 50 HPa, including the preparation of carbon powder containing at least 99.9% of "buckyballs" or at least 99% of the fullerenes, and also include other processing steps to transform the carbon material in the polycrystalline or monocrystalline diamond.

The method also allows to produce ceramic composite materials. Materials can be obtained from the following operations: in the first phase of the porous composite sponge "sponges" of graphite, al the Aza, In In4C, SiC, TiC, WC/Co, Cu, Ti, Fe, Be, W, and other ceramic materials and/or metals were prepared by standard methods and is saturated with carbon black at a pressure of 1 GPA and a temperature of 300°C, then the sample is cooled, then the pressure is increased up to 2.5 GPA and temperatures of 400°C and maintained for 1000 seconds. After temperature treatment receive a composite material, superior hardness silicon carbide (30 HPa).

A method of obtaining a ceramic composite material in accordance with the prototype is multistage and complex in execution. Ceramic composite material with a hardness of about 30 GPA does not meet the requirements of materials for the manufacture of tools, suitable for operation in extreme conditions.

The objective of the proposed technical solution is to eliminate these disadvantages and to produce a material with high microTargeting, high elastic modules and at the same time a higher conductivity compared to the conductivity of the original fullerene (~2 W/m*K) or polymerized fullerene (~3 W/m*K).

The set task is solved as follows:

Form the original composition consisting of carbon content of the fullerene and supplements, and as carbon take fullerene C-60 and C-70, and Supplement take, with the present of thermally conductive components, selected from the range: wurtzitic boron nitride, cubic boron nitride, diamond, or mixtures thereof and a binder component selected from elements of group IVa of the Periodic system of the elements or their alloy with copper then the composition effect of static pressure from 8 to 13 GPA, heating is carried out in the range of 900-2000°C for at least 20 seconds, with components being taken in the ratio, wt.%:

fullerenes C-60 and C-7030-50
the heat-conducting component10-60
binderrest

When this heat-conducting component pre-cover binder additive, the result is a composite material with high thermal conductivity, hardness, high elastic moduli and high wear resistance.

The ranges of pressure and temperature selected experimentally. Going beyond the lower limits of these ranges does not allow to obtain high-quality samples of the material, going beyond the upper limit does not improve the material properties, but reduces the resource technological devices. Cooling mode for 20-120 seconds are optimal for obtaining the target product the KTA. The ratio of the components is established experimentally.

Way of the following examples.

Example 1. Prepared a mixture of powders containing fullerene C-60 (wt.% 40), wurtzite boron nitride (wt.% 15), diamond ASM/28 (wt.% 35), titanium (wt.% 10). Mixture by weight of 1 carat placed in the office of the high pressure type "anvil with a hole", has created a pressure of 12.5 GPA and heated to a temperature of 1500°C, held for 60 seconds, cooled to room temperature, reducing the pressure to atmospheric, and pulled a compact sample of the high-pressure apparatus.

The device Durascan 20 has determined the microhardness of the sample Vickers 70-120 HPa (mean 95 HPa). To determine the elastic moduli measured velocities of longitudinal and shear waves using laser ultrasonic flaw detector UDL-2M, the density of the sample was determined by hydrostatic method. Using experimental data, the calculated modulus of elasticity: E=815 HPa. To calculate thermal conductivity (K) has fulfilled the necessary experimental measurements of thermal diffusivity (α), specific heat (Cp) and density (ρ). Calculation of thermal conductivity was carried out according to the formula: λ=α·sp·ρ. λ=318 W/m·K. the ratio of the microhardness (Hv) modulus of elasticity (E) is equal to 0.117, indicating the high wear resistance of the composite material.

Example 2. When Otavio mixture of powders containing fullerene C-60 (wt.% 30), cubic boron nitride (wt.% 20), diamond AU 200/160 (wt.% 25), diamond detonation synthesis type DALAN (wt.% 15), Zr-Cu (mass%)). The mixture weight of 1.5 carats was placed in the office of the high pressure type "anvil with a hole", has created a pressure of 8.5 GPA and heated to a temperature of 1350°C, held for 90 seconds, cooled to room temperature, reducing the pressure to atmospheric, and pulled a compact sample of the high-pressure apparatus. Experimental measurements were performed as in example 1. Microhardness 63-125 GPA (the average value of Hv=94 HPa); the modulus of elasticity E=787 HPa, the relation of Hv/ E=0,119; λ=335 W/m·K.

Example 3. Prepared a mixture of powders containing fullerene-70 (wt.% 50), diamond AU 200/160 covered with a film of alloy Ti-Cu (wt.% 40), diamond ACM 10/7 (wt.% 10),. Mixture by weight of 1 carat placed in the office of the high pressure type "anvil with a hole", has created a pressure of 13 HPa, heated to a temperature of 1580°C, held for 35 seconds, cooled to room temperature, reducing the pressure to atmospheric, and pulled a compact sample of the high-pressure apparatus. Experimental measurements were performed as in example 1, 2. Microhardness 74-130 GPA (the average value of Hv=102 GPA); the modulus of elasticity E=842 HPa, the relation of Hv/ E=0,121; λ=296 W/m·K.

Thus, by selecting the original mother of the crystals, including fullerene C-60 and C-70, and subsequent exposure to high pressure and temperature obtained composite material with high thermal conductivity, microhardness, elastic moduli and high wear resistance. thermal conductivity of a composite material containing polymerized superhard fullerene increased from 3 W/m·K (polymerized superhard fullerene) to 336 W/m·K (composite material) while maintaining high mechanical characteristics. The presence of manufactured composite superhard material modifications of boron nitride can expand the scope of use of the composite, for example, tools for processing materials containing elements of group VIII of the Periodic system of elements.

1. A method of obtaining a superhard composite material comprising a high pressure and temperature on the initial composition consisting of carbon content of the fullerene and additives, characterized in that as the carbon take fullerene C-60 and C-70, and Supplement charge consisting of a thermally conductive component selected from the range: wurtzitic boron nitride, cubic boron nitride, diamond, or mixtures thereof and a binder component selected from elements of group IVa of the Periodic system of the elements or their alloy with copper then the composition effect statically the pressure from 8 to 13 GPA, heating is carried out in the range of 900-2000°C for at least 20 seconds, with components being taken in the ratio, wt.%:

fullerenes C-60 and C-7030-50
the heat-conducting component10-60
binderrest

2. The method according to p. 1, wherein thermally conductive component pre-cover binder additive.



 

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