WO2020027688A1 - Méthode de production d'un matériau extra-dur et matériau extra-dur à base de pentaborure de tungstène - Google Patents

Méthode de production d'un matériau extra-dur et matériau extra-dur à base de pentaborure de tungstène Download PDF

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WO2020027688A1
WO2020027688A1 PCT/RU2018/000777 RU2018000777W WO2020027688A1 WO 2020027688 A1 WO2020027688 A1 WO 2020027688A1 RU 2018000777 W RU2018000777 W RU 2018000777W WO 2020027688 A1 WO2020027688 A1 WO 2020027688A1
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tungsten
carborane
boron
superhard material
sintering
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PCT/RU2018/000777
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Vadim Veniaminovich BRAZHKIN
Vasily Ivanovich BUGAKOV
Igor Petrovich ZIBROV
Vladimir Pavlovich FILONENKO
Artem Romaevich OGANOV
Alexandr Gennadievich KVASHNIN
Artem Yaudatovich ZAKIROV
Andrey Alexandrovich OSIPTSOV
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Obschestvo S Ogranichennoi Otvetstvennostyu "Gaspromneft Nauchno-Tehnichesky Tsentr" (Ooo "Gaspromneft Ntc")
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Publication of WO2020027688A1 publication Critical patent/WO2020027688A1/fr

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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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    • C01B35/04—Metal borides
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    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/5805—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
    • C04B35/58064—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C22C1/053—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/14—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on borides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F2005/001—Cutting tools, earth boring or grinding tool other than table ware
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/404—Refractory metals
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/421—Boron
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Definitions

  • the invention relates to synthesis of new materials and can be used for the following purposes:
  • cutting tools scaling, scissors, chisels
  • the developed material with improved properties and cheaper production technology makes it possible to replace conventional materials (including superhard materials and hard alloys) used for cutting, crushing, chipping, abrasion, application/formation of wear- resistant and superhard surfaces by various methods.
  • bits for rock cutting and crushing tools are mainly made of two types of superhard materials: synthetic polycrystalline diamond (PCD) and polycrystalline cubic boron nitride (PCBN), or their combination (patent RU2484888).
  • PCD polycrystalline diamond
  • PCBN polycrystalline cubic boron nitride
  • Diamond is the most durable material (Vickers hardness up to 100 GPa).
  • the pressure range of 5-6 GPa i.e., tens of thousands of atmospheres
  • Diamond composites with silicon carbide are known to have much higher thermal stability. These composites are produced by infiltrating liquid silicon into the diamond layer or by sintering a homogeneous powder mixture (patents US81681 15, RU2036779). Later ideas of using intermetallic compounds to ensure heat resistance coupled with high strength are reviewed in patent US7473287B2. In the proposed method, once the diamond coalescence is finished cobalt forms an intermetallic compound which makes it inert to the reverse transition of diamond into graphite.
  • patent RU2622276 describes a method for production of a boride ceramic consisting of 90% wt. of (Ti 0 .9Cr 0 .i)B 2 and 10% wt. of CrB.
  • the Vickers hardness of this ceramic does not exceed 26 GPa which is significantly lower than the conventional superhardness threshold which is normally considered to be 40 GPa.
  • the closest analog to the proposed method is a method for production of tungsten tetraboride with WB 4 stoichiometry (patent CN1061 16593), comprising the following stages:
  • tungsten powder and boron powder are mixed together; 2) the mixed powder is placed in a graphite mold, heated in a vacuum oven to 1200-1600°C and kept at these temperatures and pressures of 10-100 MPa for 30-180 minutes.
  • the synthesis process results in the formation of a soft compact substance which is ground to produce WB 4 in the form of a powder. That is, the proposed method is intended to production of tungsten tetraboride powder only, which requires further development of methods for its consolidation, i.e. additional high-temperature processing at high pressures (1-2 GPa) to produce a superhard material.
  • the proposed invention is intended to solve the task of replacing conventional superhard materials for cutting inserts of rockcutting tools (drill bits) with new materials having improved properties.
  • the technical result of the invention is the production of a new superhard material based on synthesized tungsten boride WB 5 with predicted properties which combines high hardness and thermal stability with high fracture toughness.
  • This material can be competitive as compared to composites based on diamond or diamond-like boron nitride, and can also be a better and more affordable replacement for hard alloys based on tungsten carbide (WC).
  • WC tungsten carbide
  • the method for production of a superhard material was implemented by sintering the source mixtures at pressures of 1.5- 8 GPa and temperatures of 1000-1500°C with a holding time of 1 to 10 minutes.
  • the toroid chamber consists of two coaxial hard-alloy shaped anvils fastened with steel rings. Between the anvils, a cell of lithographic stone is placed and compressed. Heating of the chamber is provided by passing electric current through the graphite heater inside the cell.
  • a mixture of submicron and micron powders of tungsten and submicron powder of boron was also sintered in the toroid and piston- cylinder chambers.
  • the source mixtures for a superhard material based on tungsten pentaboride include tungsten powder with a particle size of 1-10 pm, and M-carborane or submicron (0.1 -0.5 pm) boron at the following ingredients ratio, % wt.:
  • High-strength WB 5 compacts were produced at moderate reactive sintering temperatures and without the application of high pressures (which are necessary for synthesis of diamonds and cubic boron nitride). Thanks to this factor, the cost of the material is significantly reduced, the production process scaling becomes much easier, and service life of working elements of drill bits used in some applications becomes much longer compared to PCD.
  • the materials produced on the basis of WB 5 tungsten boride are characterized by high structural dispersion.
  • the tungsten pentaboride crystals have the size of less than 1 micron and an equiaxed shape (Fig. 1 shows the microstructure of the WB 5 cleavage surface).
  • Fig. 2 shows a diffractogram of the sintered materials where 1 is sintering of submicron tungsten and boron powders (1.5 GPa, 1200°C, 10 minutes), and 2 is sintering of micron tungsten powder with M-carborane (4.0 GPa, 1300°C, 1.5 minutes).
  • the VKe hard alloy has a Rockwell hardness of 86-88 HRA which corresponds to standard samples.
  • Rockwell hardness of the material (compact) produced from tungsten pentaboride reached 93-95 HRA. If we compare the average area of the imprints made by a diamond cone, in the test sample it was 0.91 mm 2 , and in the hard alloy it was 1.52 mm 2 . This means that the area of the imprint in the tungsten pentaboride compact is almost 1.7 times smaller than that in the standard sample which evidences a very high hardness of the tungsten pentaboride compact.
  • Tungsten with particle sizes of 1-10 pm and M-carborane are used as a source material for the synthesis process.
  • the tungsten share in the mixture is 50% wt.
  • the M-carbon share is also 50% wt.
  • Tungsten is sintered with M-carborane in a toroid chamber at 7 GPa, 1500°C and a holding time of 1.0 minute.
  • the WB 5 tungsten boride crystallites have a size of about 1 pm and an equiaxed shape.
  • the samples contain about 20% of the WB 2 boride.
  • Rockwell hardness of the tested sample was 88-90 HRA, and the wear spot area was 1.45 mm 2 .
  • Thermal stability of the material is guaranteed by the fact that the material is synthesized at a temperature of 1500°C, i.e. in an inert environment the material will work at least up to this temperature.
  • the synthesized WB 5 -based composition showed a lower wear rate compared to the industrial sample based on a hard alloy.
  • Submicron tungsten and boron powders are used as source materials for the synthesis process.
  • the 1-10 pm tungsten share in the mixture is 70% wt., and the submicron (0.1 -0.5 pm) boron share is 30% wt.
  • Tungsten is sintered with boron in a piston-cylinder chamber at 1.5 GPa, 1200°C and a holding time of 10 minutes.
  • the sample hardness was determined by the Rockwell method, the wear resistance was determined by the area of the wear spot caused by abrasion.
  • the hardness of the sample is 93-95 HRA
  • the wear spot area is 0.91 mm 2 .
  • a high thermal stability is guaranteed by the absence of components with a low melting point.
  • Submicron tungsten and boron powders are used as source materials for the synthesis process.
  • the 1-10 pm tungsten share of in the mixture is 90% wt., and the submicron (0.1 -0.5 pm) boron share is 10% wt.
  • Tungsten is sintered with boron in a toroid chamber at 4.5 GPa
  • the phase composition of the sample after sintering is 90% of WB 5 and 10% of WB 2 .
  • Table 1 shows the properties of the tungsten pentaboride samples. Table 1.
  • tungsten pentaboride The materials produced on the basis of tungsten pentaboride can be used for the manufacture of:
  • end-face seals of shafts in mechanisms operating in highly abrasive or highly viscous media.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Ceramic Products (AREA)

Abstract

L'invention concerne la synthèse de nouveaux matériaux extra-durs. La méthode de production d'un matériau extra-dur à base de pentaborure de tungstène comprend le frittage des poudres de tungstène et de bore à des températures et des pressions élevées. Les matériaux sources pour cette méthode sont du tungstène (taille des particules de 1 à 10 µm) et du bore submicronique (taille des particules de 0,1 à 0,5 µm) ou du carborane de composé de bore. Le frittage est effectué à des pressions de 1 à 8 GPa, des températures de 1 000 à 1 500 °C, un temps de maintien de 1 à 10 minutes, la part de tungstène dans le mélange étant de 50 à 90 % en poids. Le proccédé de frittage est réalisé dans des chambres toroïdales ou piston-cylindre. Le matériau extra-dur à base de pentaborure de tungstène est constitué de poudre de tungstène et de composé de bore. La poudre de tungstène a des tailles de particules de 1 à 10 µm, et le composé de bore est représenté par 1,7-di(oxyméthyl)-M-carborane (M-carborane). Le matériau a la proportion suivante d'ingrédients en poids : poudre de tungstène ayant des tailles de particules de 1 à 10 µm - 90 à 50 % en poids, et M-carborane - 10 à 50 % en poids.
PCT/RU2018/000777 2018-08-01 2018-12-03 Méthode de production d'un matériau extra-dur et matériau extra-dur à base de pentaborure de tungstène WO2020027688A1 (fr)

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RU2018128234 2018-08-01
RU2018128234A RU2698827C1 (ru) 2018-08-01 2018-08-01 Способ получения сверхтвердого материала и сверхтвердый материал на основе пентаборида вольфрама

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11351609B2 (en) 2020-07-15 2022-06-07 Millennitek Llc Synthesis of tungsten tetraboride

Citations (4)

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SU206350A1 (ru) * Г. В. Самсонов, А. Я. Артамонов, А. Л. Бурыкина, А. И. Безыкорнов, О. В. Евтушенко , В. В. Стасовска Абразивный материал
CN105692641A (zh) * 2015-12-25 2016-06-22 洛阳金鹭硬质合金工具有限公司 一种硼化钨的制备方法及应用
CN106116593A (zh) * 2016-06-28 2016-11-16 东北大学 一种四硼化钨陶瓷粉体的制备方法
CN107473237A (zh) * 2017-08-24 2017-12-15 广东工业大学 一种二元钨硼化物超硬材料的制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU206350A1 (ru) * Г. В. Самсонов, А. Я. Артамонов, А. Л. Бурыкина, А. И. Безыкорнов, О. В. Евтушенко , В. В. Стасовска Абразивный материал
CN105692641A (zh) * 2015-12-25 2016-06-22 洛阳金鹭硬质合金工具有限公司 一种硼化钨的制备方法及应用
CN106116593A (zh) * 2016-06-28 2016-11-16 东北大学 一种四硼化钨陶瓷粉体的制备方法
CN107473237A (zh) * 2017-08-24 2017-12-15 广东工业大学 一种二元钨硼化物超硬材料的制备方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11351609B2 (en) 2020-07-15 2022-06-07 Millennitek Llc Synthesis of tungsten tetraboride

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