WO2014120044A1 - Procede d'alliage de céramique en oxyde d'alumine - Google Patents

Procede d'alliage de céramique en oxyde d'alumine Download PDF

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Publication number
WO2014120044A1
WO2014120044A1 PCT/RU2014/000016 RU2014000016W WO2014120044A1 WO 2014120044 A1 WO2014120044 A1 WO 2014120044A1 RU 2014000016 W RU2014000016 W RU 2014000016W WO 2014120044 A1 WO2014120044 A1 WO 2014120044A1
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Prior art keywords
ceramic
temperature
strength
slip
doping
Prior art date
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PCT/RU2014/000016
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English (en)
Russian (ru)
Inventor
Пётр Яковлевич ДЕТКОВ
Валентин Кириллович МЯКИН
Игорь Леонидович ПЕТРОВ
Original Assignee
Detkov Pyotr Yakovlevich
Myakin Valentin Kirillovich
Petrov Igor Leonidovich
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Application filed by Detkov Pyotr Yakovlevich, Myakin Valentin Kirillovich, Petrov Igor Leonidovich filed Critical Detkov Pyotr Yakovlevich
Priority to CN201480004611.1A priority Critical patent/CN105189407B/zh
Publication of WO2014120044A1 publication Critical patent/WO2014120044A1/fr
Priority to HK16106888.4A priority patent/HK1219942A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C04B35/111—Fine ceramics
    • C04B35/117—Composites
    • C04B35/119—Composites with zirconium oxide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C—CHEMISTRY; METALLURGY
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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
    • 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
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/638—Removal thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/443—Nitrates or nitrites
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • C04B2235/6027—Slip casting
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B2235/65—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
    • C04B2235/6562—Heating rate
    • C—CHEMISTRY; METALLURGY
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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
    • C04B2235/6565—Cooling rate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/661—Multi-step sintering
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Definitions

  • the invention relates to technologies for producing ceramic materials, in particular to methods of doping ceramics, and can be used in the field of electrical engineering and mechanical engineering for the manufacture of high-strength ceramic products.
  • a known method of manufacturing ceramic products based on zirconium and aluminum oxides including the preparation of a workpiece from ultrafine powders of the aforementioned oxides, its preliminary sintering and subsequent high-temperature deformation at a temperature of 1400-1600 ° C, according to the invention, high-temperature deformation of the workpiece is carried out at a pressure 3-10 MPa and then subjected to recrystallization calcined under vacuum at a residual a pressure of not lower than 5 to 10 "5 torr and a temperature of 1500-1700 ° C, the content of aluminum hydroxy yes a mixture of ultrafine powders is 10 to 80 wt.% (the invention according to the patent RU 2304566).
  • a known method of producing alumina ceramics by mixing alumina and an organotitanium additive, drying, molding and firing, according to the invention, in the process of mixing an additional zirconium-organic compound and water are introduced in the following ratio of components, wt.%: Alumina - 96.0-97 , 8, organo-titanium compound - 0.6-1.5, organo zirconium compound - 0.6-1.5, water - the rest (invention according to the copyright certificate SU 1747424).
  • the high strength properties provided by the introduction of a zirconium-containing additive in the form of an organ zirconium compound can be achieved at a temperature of 1400-1500 ° C.
  • the powder of corundum ceramics containing magnesium oxide, sodium oxide, silicon oxide, micro impurities and alumina is mixed with partially stabilized zirconia and calcium fluoride in the following ratio of components, May: stabilized zirconia - 5.0-15, 0, calcium fluoride - 0.5-6.0, magnesium oxide - 0.2-0.4, sodium oxide - 0.1-0.2, silicon oxide - 0.1-0.2, trace elements - 0, 02-0.04, alumina 78.16-94.08.
  • Ceramics are prepared as follows: a casting slurry is prepared from a fine powder, the composition of the slurry, May: a mixture of powders - 85.5, a binder - 14.5 (paraffin - 14, wax - 0.5), the products are molded by hot casting under a pressure of 1-4 atm. at a slurry temperature of 60-65 ° C, preliminary burning of the binder in a bed of aluminum oxide to 90 ° C with a temperature rise of 50 ° C per hour, final firing in air.
  • the process of high-temperature firing mainly shows, but does not determine, as is commonly believed, the level of homogeneity and homogeneity of the material incorporated in the manufacture of slip and workpieces.
  • the technical task of the alleged invention is the creation of a simpler and more economical way to obtain durable ceramics, providing products of any shape.
  • the technical result of the invention is to increase the strength and reduce the dispersion of the strength of alumina ceramics.
  • the preparation is impregnated with an aqueous solution of zirconyl nitrate ⁇ ( ⁇ 0 3 ) 2 * 2 ⁇ 2 0, then it is heated with increasing temperature to 400 ° ⁇ .
  • Impregnation of zirconyl nitrate with an aqueous solution ensures saturation of the internal capillary-porous structure of the preform with the solution, which contributes to the uniform coating of each A1 2 0 3 particle with the micro-layer of the solution.
  • the water content in the ZrO (N0 3 ) 2 x 2 ⁇ 2 0 salt ensures the maximum possible density of the solution, which allows to achieve a high concentration of zirconium dioxide in the product and to provide the required strength.
  • zirconium dioxide was introduced in the form of aqueous solutions of salts into a ceramic semi-finished product, which represents a ceramic preform after forming and removing a technological binder from it.
  • the ceramic semi-finished product having a capillary-porous structure was saturated with an aqueous solution of zirconyl nitrate ZrO (N0 3 ) 2 ⁇ 2 H 2 0.
  • Subsequent stepwise heating of the ceramic billet removes moisture, decomposes zirconyl nitrate to zirconium dioxide, and removes volatile products.
  • zirconyl nitrate is in a state of molecular dis-
  • the arrangement of zirconia introduced in the aqueous solution mirrors the porous structure of the preform.
  • Capillaries and pores represent is the free volume previously occupied by the technological bundle covering the surface of aluminum oxide particles at the stage of preparing the slip.
  • capillary potential is much greater than gravity ( ⁇ ⁇ > fpt.) -
  • Zirconia nanoparticles formed as a result of thermal decomposition of zirconyl nitrate are tetragonal crystals with a size of tens of nanometers, which provide an increase in the strength of ceramics.
  • the proposed method can be implemented on an industrial scale and will find application in the field of electrical engineering and mechanical engineering for the manufacture of high-strength ceramic products, i.e. characterized by the criterion of “industrial applicability”.
  • the essence of the claimed technical solution is illustrated on the graph of the dependence of the temperature of the furnace on time when removing a temporary binder from ceramic billets.
  • the method is as follows.
  • a preform is obtained.
  • a ceramic billet having a capillary-porous internal structure is obtained.
  • the shape, volume, spatial structure of the pores repeat the remote temporal ligament and consists mainly of pores and capillaries, the radius of which is ⁇ 10 "7 m.
  • the preform After removal of the temporary ligament, the preform is saturated with an aqueous solution of zirconyl nitrate ZrO (N0 3 ) 2 ⁇ 2 H 2 0.
  • an aqueous solution of zirconyl nitrate fills the capillary-porous interior of the ceramic billet, covering the surface of each particle A1 2 0 3 with a micro layer.
  • Subsequent removal of water, decomposition of zirconyl nitrate to zirconium dioxide and removal of volatile products is carried out in the process of heating the workpiece with increasing temperature to 400 ° C.
  • ultrafine particles of Zr0 2 are formed in the monoclinic phase.
  • the particles of zirconium dioxide transfer to the tetragonal phase, which is maintained upon cooling to room temperature.
  • the firing of the ceramic sample is carried out at a temperature of ⁇ 1600 - 1650 ° C.
  • a feature of the present method of doping alumina ceramics is that doping occurs with zirconia released during the thermal dissociation of aqueous solutions of salts. Zirconium dioxide is formed in a highly dispersed state and is evenly distributed in the volume of the ceramic.
  • a sample was prepared from a slip of the following composition:
  • the studies were carried out on cylindrical samples with a diameter of 7 ⁇ 1 mm and a length of 60 ⁇ 5 mm.
  • the samples were made from a slip industrial production brand VK94-1.
  • the strength of the samples was evaluated according to the results of tests for three-point bending according to the Russian standard.
  • Billets of cylindrical samples were made from a slip of the VK94-1 grade, consisting of 87.5% (May.) Ceramic powder and 12.5% paraffin.
  • the slip slip injection method was used, subject to the following process conditions:
  • the obtained ceramic preforms were placed in a ceramic cell and filled with alumina so that the alumina layer between the preforms was not less than 5 mm, between the blanks and the walls of the cell - at least 10 mm.
  • alumina with a mass fraction of a - A1 2 0 3 - not less than 35%, specific surface area - 10 m 2 / g, mass fraction of moisture - not more than 2.5%.
  • the cuvette with the blanks was placed in a high-temperature laboratory chamber electric resistance furnace.
  • the used electric furnace allows heat treatment at temperatures up to 1,100 ° C.
  • the cuvette with blanks was removed from the furnace, the blanks were removed from alumina.
  • the preforms were impregnated with an aqueous solution of ZrO (N0 3 ) 2 ⁇ 2 ⁇ 2 0. salt. Samples were placed horizontally in the aqueous solution of salt and kept for some time, periodically turning them around its axis.
  • the samples were removed from the solution and dried to remove moisture, thermal destruction of the zirconium salt and removal of the products of thermal destruction.
  • the blanks After drying the blanks, they were fired in air at high temperatures in a furnace with fibrous insulation, a stainless steel casing, designed for universal use at temperatures up to 1800 ° C.
  • the preforms were placed on corundum substrates.
  • the temperature regime of firing consisted of several stages:
  • the tests were carried out using the three-point bending method for cylindrical specimens with a diameter of 7 ⁇ 1 mm and a length of 60 ⁇ 5 mm with a distance between supports of 50 mm according to the scheme.
  • the table shows the strength test results of ceramic samples at three-point bending.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Composite Materials (AREA)

Abstract

Le procédé d'alliage de céramique en oxyde d'alumine comprenant la fabrication d'une ébauche à partir de barbotine, l'élimination du liant technique et le recuit après l'invention ; après l'élimination du liant technique l'ébauche est imprégnée avec une solution aqueuse de nitrate de zirconyle ZrO(NO3)2×2H2O puis chauffée à une température allant jusqu'à 400°C.
PCT/RU2014/000016 2013-01-30 2014-01-15 Procede d'alliage de céramique en oxyde d'alumine WO2014120044A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201480004611.1A CN105189407B (zh) 2013-01-30 2014-01-15 一种氧化铝陶瓷掺杂方法
HK16106888.4A HK1219942A1 (zh) 2013-01-30 2016-06-15 種氧化鋁陶瓷摻雜方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RU2013106318/03A RU2525889C1 (ru) 2013-01-30 2013-01-30 Способ легирования алюмооксидной керамики
RU2013106318 2013-01-30

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WO2014120044A1 true WO2014120044A1 (fr) 2014-08-07

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CN (1) CN105189407B (fr)
HK (1) HK1219942A1 (fr)
RU (1) RU2525889C1 (fr)
WO (1) WO2014120044A1 (fr)

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RU2728911C1 (ru) * 2019-08-06 2020-08-03 Российская Федерация, От Имени Которой Выступает Министерство Промышленности И Торговли Российской Федерации Способ изготовления корундовой керамики

Citations (4)

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SU1747424A1 (ru) * 1990-07-19 1992-07-15 Институт Химии Силикатов Им.И.В.Гребенщикова Способ получени алюмооксидной керамики
US5164348A (en) * 1987-05-27 1992-11-17 Minnesota Mining And Manufacturing Company Abrasive grits formed by ceramic impregnation method of making the same, and products made therewith
RU2148567C1 (ru) * 1995-04-05 2000-05-10 Сент-Гобэн Индастриал Керамикс, Инк. Способ получения альфа-оксида алюминия (варианты), абразивные частицы и абразивный материал (варианты)
US6206942B1 (en) * 1997-01-09 2001-03-27 Minnesota Mining & Manufacturing Company Method for making abrasive grain using impregnation, and abrasive articles

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US5164348A (en) * 1987-05-27 1992-11-17 Minnesota Mining And Manufacturing Company Abrasive grits formed by ceramic impregnation method of making the same, and products made therewith
SU1747424A1 (ru) * 1990-07-19 1992-07-15 Институт Химии Силикатов Им.И.В.Гребенщикова Способ получени алюмооксидной керамики
RU2148567C1 (ru) * 1995-04-05 2000-05-10 Сент-Гобэн Индастриал Керамикс, Инк. Способ получения альфа-оксида алюминия (варианты), абразивные частицы и абразивный материал (варианты)
US6206942B1 (en) * 1997-01-09 2001-03-27 Minnesota Mining & Manufacturing Company Method for making abrasive grain using impregnation, and abrasive articles

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Title
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Publication number Publication date
CN105189407B (zh) 2017-04-19
CN105189407A (zh) 2015-12-23
RU2525889C1 (ru) 2014-08-20
RU2013106318A (ru) 2014-08-10
HK1219942A1 (zh) 2017-04-21

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