WO2020202878A1 - ホウ化ジルコニウム／炭化ホウ素コンポジット及びその製造方法 - Google Patents

ホウ化ジルコニウム／炭化ホウ素コンポジット及びその製造方法 Download PDF

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WO2020202878A1
WO2020202878A1 PCT/JP2020/006751 JP2020006751W WO2020202878A1 WO 2020202878 A1 WO2020202878 A1 WO 2020202878A1 JP 2020006751 W JP2020006751 W JP 2020006751W WO 2020202878 A1 WO2020202878 A1 WO 2020202878A1
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zrb
boron carbide
zirconium
powder
vol
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PCT/JP2020/006751
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English (en)
French (fr)
Japanese (ja)
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健 廣田
将樹 加藤
博之 宮本
ヅウィ レ トゥン
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学校法人同志社
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Priority to JP2021511212A priority Critical patent/JP7414300B2/ja
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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
    • C04B35/515—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
    • C04B35/56—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 carbides or oxycarbides
    • C04B35/563—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 carbides or oxycarbides based on boron carbide
    • 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
    • C04B35/515—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
    • 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
    • C04B35/64—Burning or sintering processes
    • C04B35/645—Pressure sintering

Definitions

  • zirconium boride / carbide boron (ZrB 2 / B 4 C) composites particularly Vickers hardness H v is at least 23 GPa
  • fracture toughness value K IC is 9.0 MPa ⁇ m 1/2 or more dense ZrB 2 / B 4 relates C composite and a manufacturing method thereof.
  • UHTC ultra-high temperature heat-resistant ceramic
  • Patent Document 1 a predetermined amount of Zr powder, a predetermined amount of tungsten (W) powder, and a predetermined amount of B powder are wet-mixed and then pressure-molded to obtain a molded product, and the molded product is discharged.
  • a method for producing tungsten-added ZrB 2 by plasma sintering [also known as pulse energization pressure sintering method] is disclosed.
  • Vickers hardness (H v) of the sintered body obtained using this manufacturing method is 20.7GPa at maximum, the mechanical properties further improve, to be particularly improve the strength properties at high temperatures It is desired.
  • Vickers hardness H v is at least 23 GPa
  • fracture toughness value K IC is an object of the present invention to provide a 9.0 MPa ⁇ m 1/2 or more dense ZrB 2 / B 4 C composite. Further, an object of the present invention is also to provide a manufacturing method of ZrB 2 / B 4 C composite having excellent physical properties mentioned above.
  • the present inventors have, as a result of various investigations, the carbon C of amorphous particles, boron B amorphous powder were homogeneously mixed in a predetermined molar ratio, and this mixture and ZrB 2 powder
  • a green compact is prepared by mixing at a predetermined volume ratio and molding, and the green compact is pulsed and pressure-sintered (PECPS), a self-propagating high-temperature synthesis is performed during the PECPS heat treatment. : SHS) is induced, the temperature inside the sample rises above the external heating temperature, thereby, it has found that a composite of dense sintered is sintered ZrB 2 / B 4 C can be produced, and completed the present invention .
  • the present inventors have obtained a ZrB 2 / B 4 C composite having a volume ratio of 10/90 to 60/40 of ZrB 2 / B 4 C obtained by using the above production method, and the ZrB 2 / B 4 C composite has a Vickers hardness. It was also found that it is a high-density ceramic having excellent mechanical properties of H v 23 GPa or more and a fracture toughness value of 9.0 MPa ⁇ m 1/2 or more.
  • the Vickers hardness H v is at least 23 GPa
  • fracture toughness value K IC is at 9.0 MPa ⁇ m 1/2 or more
  • zirconium boride / The theoretical volume ratio of boron carbide is 10/90 to 60/40 vol%.
  • the present invention provides a ZrB 2 / B 4 C composite having the above physical properties, the volume ratio of the theoretical zirconium boride / boron carbide is 40/60 ⁇ 60 / 40vol% , bending at 1000 ⁇ 1600 ° C. It is characterized in that the intensity ⁇ b is 500 MPa or more.
  • ZrB 2 / B 4 C composite of the present invention the Vickers hardness H v is at least 29 GPa, fracture toughness value K IC is at 9.3 MPa ⁇ m 1/2 or more, theoretical zirconium boride / boron carbide The volume ratio of the above is 20/80 to 50/50 vol%.
  • a step of performing mold molding using the mixed powder to obtain a molded product having a desired shape, sintering the obtained molded product, and synthesizing and simultaneously sintering a zirconium boride / boron carbide composite is included. It is characterized by.
  • the present invention provides a ZrB 2 / B 4 production method of C composite having the above characteristics, the sintering, in a vacuum of 10 Pa, a sintering temperature of 1800 ⁇ 2000 ° C., pressure of 10 ⁇ 100 MPa It is characterized by pulse energization pressure sintering under the condition of holding time of 5 to 30 minutes.
  • the present invention provides a ZrB 2 / B 4 production method of C composite having the above characteristics, the volume ratio of the theoretical of the ZrB 2 and B 4 C is in the range of 20/80 ⁇ 50 / 50vol% It is also characterized by that.
  • ZrB 2 / B 4 is a flowchart showing a procedure in an example of the manufacturing method of the present invention for the production of C composite, manufacturing conditions used in Examples are also shown together. It is an SEM image of the ZrB 2 powder used as a starting material, and is an image taken at a magnification of 1000 times in the upper photograph and 2000 times in the lower photograph. It is a graph which shows the relative density of the green compact after uniaxial pressing, cold isostatic pressing (CIP), and the sintered body after PECPS.
  • CIP cold isostatic pressing
  • FIG. 1 is a flowchart showing a procedure in an example of the manufacturing method of the present invention.
  • the amorphous boron powder and the amorphous carbon powder have a molar ratio of (3.6 to 6.5): 1 (13.4 to 21.6 atomic% C), preferably (3). Weighed so that it was 9.9 to 5.2): 1 (16.4 to 20.4 atomic% C), more preferably 4.4: 1, and mixed (preferably wet mixing) to carry out amorphous.
  • a starting material in which quality boron and amorphous carbon are uniformly mixed is prepared.
  • amorphous boron and amorphous carbon and as boron powder
  • boron powder It is preferable to use one having an average particle size of about 1.5 ⁇ m, and it is preferable to use a carbon powder having an average particle size of about 30 nm.
  • alcohol for example, ethanol
  • the solvent is limited to this. It's not something.
  • ZrB 2 is based on the theoretical volume of boron carbide (B 4 C, theoretical density 2.515 Mg ⁇ m -3 ) synthesized from the above mixture of amorphous boron and amorphous carbon.
  • / B 4 C 10/90 to 60/40 vol% of zirconium borohydride (ZrB 2 ) powder (average particle size: about 3 ⁇ m) is prepared, and this ZrB 2 is added to the starting material and mixed. And obtain a mixed powder.
  • ZrB 2 zirconium borohydride
  • Uniaxial mold molding is generally used as a means for forming the molded body in this step, but the present invention is not limited to this, and the molded body is subjected to cold hydrostatic press (CIP) treatment or the like. After increasing the density, it is preferable to perform pulse energization pressure sintering.
  • synthetic simultaneous sintering refers to a dense sintered body (ZrB 2 / B 4 C composite) from a homogeneous mixture of starting materials (a mixture of B and C containing a specific amount of ZrB 2 ). It shall indicate that it is produced.
  • pulse energization pressure sintering When performing pulse energization pressure sintering by the production method of the present invention, it can be carried out using a commercially available pulse energization pressure sintering apparatus.
  • pulsed energization pressurization sintering under uniaxial pressurization (10 to 100 MPa), a large pulsed DC current (several tens to several hundreds of 100A to 1500A: this current value changes depending on the size of the sample) at a low voltage (several V).
  • Diffusion and self-burning synthesis (SHS) occur.
  • a dense sintered body (high density, fine crystal grain size) with suppressed grain growth is obtained by high-speed temperature rise (50 to 100 ° C./min) and short-time sintering (5 to 30 minutes) under high pressure. be able to.
  • boron B and microparticle powders of carbon C of amorphous by pulse current pressure sintering a mixed powder obtained by mixing with zirconium boride ZrB 2 powder, when Atsushi Nobori utilizing energy produced at the time of generating is B 4 C from B and C, and a relatively mild heat treatment conditions of 1900 °C / 50MPa / 10 min, it is possible to generate a B 4 C by the self-combustion synthesis.
  • (4 ⁇ B + C) fine particles are arranged in the gap between the ZrB 2 particles during molding, and at the time of PECPS, they also play a role as a binder that holds the ZrB 2 particles together with the synthetic simultaneous sintering of B 4 C. As a result, a dense sintered body can be obtained.
  • the pulse energization pressure sintering in the production method of the present invention is performed in a vacuum of 10 Pa or less under the conditions of a sintering temperature of 1800 to 2000 ° C., a pressing force of 10 to 100 MPa, and a holding time of 5 to 30 minutes. It is preferable, and more preferable conditions for pulse energization pressure sintering are a sintering temperature of 1850 to 1950 ° C., a holding time of 7 to 15 minutes, a pressing force of 30 to 70 MPa under a vacuum of 10 Pa or less, and 1900 ° C./50 MPa / The condition of 10 minutes is particularly preferable.
  • the pressing force is less than 10 MPa
  • the sintering density becomes low, and conversely, if it exceeds 100 MPa, the strength of the mold used for pulse energization pressure sintering has an upper limit and cannot be used.
  • the sintering temperature is less than 1800 ° C.
  • the density becomes low, and conversely, when the sintering temperature exceeds 2000 ° C., grain growth tends to occur, which is not preferable.
  • the holding time is 5 to 30 minutes for sufficient compaction.
  • Vickers hardness to produce a more ceramic 20GPa It is not possible.
  • the present invention will be specifically described based on Examples, but the present invention is not limited to Examples.
  • uniaxial mold molding (20 mm ⁇ , 75 MPa, addition of 3% acrylic / PVA) was performed, and then cold hydrostatic pressure (245 MPa, 3 minutes) was pressed. ..
  • the obtained molded body is heat-treated (950 ° C./2 h / vacuum), and further, using a commercially available pulse energization pressure sintering apparatus (using SPS Syntex Co., Ltd./SPS-510A), 10 Pa or less. under vacuum, the sintering temperature 1900 ° C., holding time 10 min, subjected to pulse current pressure sintering under a pressure 50 MPa, the 100 ° C.
  • the sintered body (ZrB 2 / B 4 C composite) Got Regarding the evaluation of the manufactured sintered body, the phase characteristics were evaluated by the XRD pattern, the morphology was observed by the SEM image, and the Vickers hardness (JIS R 1610: 2003 Fine Ceramics Hardness Test Method, Load: The mechanical properties were evaluated by the fracture toughness value (measured at 2 kgf) and the fracture toughness value (using the IF method of the room temperature fracture toughness (toughness) test method for fine ceramics).
  • a bending tester Autograph-AG-X Plus, manufactured by Shimadzu Corporation
  • the bending strength at three points in the temperature range from room temperature to 1800 ° C in argon gas. Evaluated by test.
  • FIG. 2 is a scanning electron microscope (SEM) image (measured by FE-SEM, JEOL Ltd., JSM 7000) of ZrB 2 powder (manufactured by JEOL Ltd.) used as a starting material. Is an image taken at a magnification of 1000 times, and the lower photograph is an image taken at a magnification of 2000 times. From the photograph of FIG. 2, the particle size of ZrB 2 powder used in Example approximately 2 ⁇ 4 [mu] m: an (average of about 3 [mu] m), it small variation was confirmed.
  • SEM scanning electron microscope
  • the relative density is higher in the case of ZrB 2 / (4B + C) composite than in the case of ZrB 2 (100 vol%) because the B in the gap between the particles of ZrB 2 having a large particle size has a small particle size. It is probable that C was added and the relative density increased.
  • the relative density of the sintered body after PECPS showed a high value of 96.7% or more in the range of 0 to 70 vol% of ZrB 2 .
  • the bright part is ZrB 2 from the analysis (EDS analysis) result using the energy dispersive X-ray Spectrometer for the bright part and the dark part. It was confirmed that the dark part was B 4 C, and it was confirmed that a very dense composite was obtained when the PECPS temperature was 1900 ° C.
  • Figure 6 is a graph showing the sintered sample (50vol% ZrB 2 / 50vol% B 4 C), and sintering temperature, bulk density, a relationship between the relative density of the ZrB 2, bulk density and relative density Is also shown. From the experimental results of FIG. 6, when performing PECPS at a temperature of 1900 ° C., the ZrB 2 / B 4 C composite, the relative density of 99.8% or more dense ceramic is prepared, with a composition consisting of ZrB 2 is It was confirmed that the density was only 70.3%.
  • FIG. 9 is a graph showing the relationship between the ZrB 2 content, the relative density, and the ZrB 2 crystal grain size of the sintered body sintered at 1900 ° C.
  • Graph of Figure 9 if PECPS temperature is 1900 ° C., in ZrB 2 / B 4 C composite content ZrB 2 is 40 ⁇ 70 vol% composition, relative density of 99% or more of the dense sintered body is obtained, It is shown that as the content of ZrB 2 increases (40 ⁇ 70 vol%), the crystal grain size of ZrB 2 increases.
  • Figure 10 is a graph showing the mechanical properties of the sintered body sintered at 1900 ° C. (Vickers hardness H v and fracture toughness value K IC). From the graph of FIG. 10, ZrB 2 / B 4 C composite content ZrB 2 is 10/90 ⁇ 60 / 40vol% composition, Vickers hardness H v is at least 23 GPa, the fracture toughness value K IC 9.0 MPa -It can be seen that it is a dense sintered body of m 1/2 or more. Further, in the graph of FIG.
  • the fracture toughness value of ZrB 2 is 3.5 to 4.2 MPa ⁇ m 1/2
  • the fracture toughness value of B 4 C is 5.0 MPa ⁇ m 1/2 or less. It was confirmed that the ZrB 2 / B 4 C composite obtained by using the above manufacturing method has a larger fracture toughness value than the ZrB 2 and B 4 C single-phase ceramics, and has excellent mechanical properties. It was.

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PCT/JP2020/006751 2019-04-02 2020-02-20 ホウ化ジルコニウム／炭化ホウ素コンポジット及びその製造方法 WO2020202878A1 (ja)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112522546A (zh) * 2020-10-26 2021-03-19 中北大学 一种利用slm技术制备b4c增强铝基复合材料的方法
RU2812539C1 (ru) * 2023-06-02 2024-01-30 Федеральное Государственное Бюджетное Образовательное Учреждение Высшего Образования "Новосибирский Государственный Технический Университет" Способ изготовления композиционной керамики карбид бора - диборид циркония

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112522546A (zh) * 2020-10-26 2021-03-19 中北大学 一种利用slm技术制备b4c增强铝基复合材料的方法
CN112522546B (zh) * 2020-10-26 2022-02-08 中北大学 一种利用slm技术制备b4c增强铝基复合材料的方法
RU2812539C1 (ru) * 2023-06-02 2024-01-30 Федеральное Государственное Бюджетное Образовательное Учреждение Высшего Образования "Новосибирский Государственный Технический Университет" Способ изготовления композиционной керамики карбид бора - диборид циркония

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