KR20020004129A - Preparation Method of High Toughened Silicon Carbide with Sialon Grain Boundary - Google Patents

Preparation Method of High Toughened Silicon Carbide with Sialon Grain Boundary Download PDF

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KR20020004129A
KR20020004129A KR1020000037641A KR20000037641A KR20020004129A KR 20020004129 A KR20020004129 A KR 20020004129A KR 1020000037641 A KR1020000037641 A KR 1020000037641A KR 20000037641 A KR20000037641 A KR 20000037641A KR 20020004129 A KR20020004129 A KR 20020004129A
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silicon carbide
sialon
grain boundary
phase
preparation
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이종국
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이종국
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/56Shaped 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
    • C04B35/565Shaped 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 silicon carbide
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38Non-oxide ceramic constituents or additives
    • C04B2235/3852Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
    • C04B2235/3865Aluminium nitrides
    • C04B2235/3869Aluminium oxynitrides, e.g. AlON, sialon
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/76Crystal structural characteristics, e.g. symmetry

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
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Abstract

PURPOSE: Provided is a preparation method of toughened silicon carbide forming sialon in the grain boundary phase by hot pressing sialon-added raw materials and thermal treating. Therefore, the resultant silicon carbide has improved creep-resistance and high temperature strength compared with conventional silicon carbide. CONSTITUTION: The preparation method is as follows: preparing granulated silicon carbide powder by adding 2mol% of sialon composition powder(9wt.% of y2O3 + 16wt.% of AlN + 75wt.% of Si3N4) to SiC powder(alpha-phase + beta-phase) with 0.45 micrometer of size, and mixing for 5hrs.; hot-pressing at 1850deg.C for 30min. under 50MPa of pressure; thermal treating at 1950deg.C for 5hrs.

Description

시알론 입계상을 갖는 강인화 탄화규소 제조법{Preparation Method of High Toughened Silicon Carbide with Sialon Grain Boundary}Preparation Method of High Toughened Silicon Carbide with Sialon Grain Boundary

▲ 발명이 속하는 기술분야▲ Field of invention

- 본 기술은 벌크상 탄화규소 제조시 소결조제로 시알론 조성(질화규소, 질화알루미늄, 이트리아)을 출발 분말상에 혼합하여 가압소결시킨 다음 열처리하여입계상을 시알론으로 전이시킨 강인성 탄화규소 소결체임.-This technology is a tough silicon carbide sintered body in which the sintering aid in the manufacture of bulk silicon carbide is mixed with sintering composition (silicon nitride, aluminum nitride, yttria) in the starting powder, pressurized and sintered, and then transferred the grain boundary phase to sialon. .

▲ 그 분야의 종래기술▲ Prior art in the field

① 종래의 일예① Conventional example

탄화규소에 보론, 알루미늄, 탄소등을 첨가시켜 소결한 연구사례가 보고됨.A case study of sintering by adding boron, aluminum, and carbon to silicon carbide has been reported.

② 종래의 다른예② Other conventional example

탄화규소에 이트리아, 알루미나 등 산화물을 첨가시켜 소결밀도와 인성을 향상시키는 연구사례가 보고됨.Case studies have been reported to improve the sintered density and toughness by adding oxides such as yttria and alumina to silicon carbide.

▲ 기존에 나와있는 기술의 문제점 설명▲ Describe the problem of existing technology

① 탄화규소에 보론, 탄소, 알루미늄등을 첨가하여 소결한 탄화규소는 소결온도가 높아 입자 크기가 크고 이로 인하여 인성이 떨어지는 문제가 있슴.① Silicon carbide sintered by adding boron, carbon, aluminum, etc. to silicon carbide has a high sintering temperature, resulting in a large particle size, which causes inferior toughness.

② 탄화규소에 이트리아, 알루미나 등 산화물을 첨가시켜 소결한 탄화규소는 입계에 산화물 유리상을 형성하기 때문에 인성 및 강도가 떨어짐.(2) Silicon carbide sintered by adding oxides such as yttria and alumina to silicon carbide forms an oxide glass phase at grain boundaries, resulting in poor toughness and strength.

① 본 기술은 탄화규소의 입계에 강도가 큰 시알론 상을 형성시켜 인성이 증가된 탄화규소를 제조하기 위한 기술임.① This technique is for producing silicon carbide with increased toughness by forming sialon phase with high strength at grain boundary of silicon carbide.

② 종래의 탄화규소에 비하여 입계에 내크립성이 우수한 시알론 상을 입계에 형성시켜 고온강도가 우수한 소결체를 제공하기 위한 기술임.② It is a technology to provide a sintered body with excellent high temperature strength by forming sialon phase at the grain boundary, which has excellent creep resistance at the grain boundary, compared to conventional silicon carbide.

도1은 6H, 4H 상이 각각 주상인 시알론 입계 탄화규소 소결체의 x-ray 회절도로 (a)는 α상 탄화규소를 출발원료로 한 경우이고 (b)는 β상 탄화규소를 출발원료로 한 경우이다.1 is an x-ray diffraction diagram of a sialon grained silicon carbide sintered body having 6H and 4H phases as the main phase, respectively, (a) using α-phase silicon carbide as the starting material, and (b) using β-phase silicon carbide as the starting material. If it is.

도2는 시알론 입계상을 보여주는 전자현미경 사진 및 EDS 분석도Figure 2 is an electron micrograph and EDS analysis showing the sialon grain boundary image

도3은 α-SiC 및 β-SiC 를 출발원료로 한 시알론 입계 강화 탄화규소 소결체의 전자현미경 사진3 is an electron micrograph of a sialon grain boundary reinforced silicon carbide sintered body using α-SiC and β-SiC as starting materials.

도4는 시알론 입계 강화 탄화규소 소결체의 미세구조 인자와 파괴인성Figure 4 shows the microstructural factors and fracture toughness of sialon grain boundary silicon carbide sintered body

도5는 강인성 탄화규소에서 균열 진전시 균열편향, 균열굴절, grain bridging이 일어나는 탄화규소 소결체 사진Fig. 5 is a photograph of silicon carbide sintered body in which crack deflection, crack refraction, and grain bridging occur during crack propagation in tough silicon carbide;

① 조성① Composition

- Sialon 조성 ; 9 wt% Y2O3+ 16 wt% AIN + 75 wt% Si3N4 -Sialon composition; 9 wt% Y 2 O 3 + 16 wt% AIN + 75 wt% Si 3 N 4

- 탄화규소 조성 : 0.45 ㎛의 α상 + 2 mol% Sialon 조성-Silicon carbide composition: 0.45 ㎛ α phase + 2 mol% Sialon composition

0.45 ㎛의 β상 + 2 mol% Sialon 조성Β phase + 2 mol% Sialon composition of 0.45 μm

② 제조방법② Manufacturing Method

- α상과 β상 SiC 분말에 시알론 조성 분말 2mol%를 첨가한 다음, 5시간 혼합한 후 과립분말을 제조함.-2 mol% of sialon composition powder is added to α- and β-phase SiC powders, and then mixed for 5 hours to prepare granule powder.

- Hot Press를 이용하여 50MPa의 압력으로 1850℃의 온도에서 아르곤 분위기로 30분 동안 소결.Sintering for 30 minutes in an argon atmosphere at a temperature of 1850 ° C. at a pressure of 50 MPa using a Hot Press.

- 1950℃로 승온하여 5시간 동안 열처리하여 최종 소결체로 제조함.-Heated at 1950 ° C. for 5 hours to prepare final sintered body.

③ 시험결과③ Test result

- 99%이상인 소결밀도와 6H, 4H 상이 각각 주상인 시알론 입계 탄화규소 소결체가 제조됨 (도1 및 도2)-A sintered density of more than 99% and a sialon grain-based silicon carbide sintered body having 6H and 4H phases as main phases, respectively (FIGS. 1 and 2)

- α- SiC를 출발원료로 한 경우 등면체상 입자를 갖는 치밀한 소결체가 제조됨.-When α-SiC is used as a starting material, a dense sintered body having isotropic particles is produced.

- β- SiC를 출발원료로 한 경우 막대상과 판상입자를 갖는 치밀한 소결체가 제조됨(도3)-When β-SiC is used as a starting material, a dense sintered body having rod-shaped and plate-shaped particles is produced (Fig. 3)

- 장단축비가 3.1, 4.2 파괴인성이 5,0, 6.0 인 강인성 탄화규소 소결체가 제조됨(도4)-A tough silicon carbide sintered body having a short-to-short ratio of 3.1, 4.2 and fracture toughness of 5,0, 6.0 was produced (Fig. 4).

- 균열 진전시 균열편향이나 균열굴절, grain bridging이 일어나는 강인성 탄화규소 소결체가 제조됨(도5).-A tough silicon carbide sintered body is produced in which crack deflection, crack refraction, and grain bridging occur (FIG. 5).

- 탄화규소의 파괴인성과 강도를 향상시킴.-Improves fracture toughness and strength of silicon carbide.

- 탄화규소의 내크립성 및 고온강도를 향상시킴.-Improves creep resistance and high temperature strength of silicon carbide.

- 탄화규소 분쇄용 볼, 노즐, 베어링에 적용 가능함.-Applicable to silicon carbide grinding balls, nozzles and bearings.

- 열교환기, 반응관, 열처리용 치구 등에 적용 가능함.-Applicable to heat exchanger, reaction tube, heat treatment jig, etc.

Claims (1)

시알론 조성을 입계로 하여 탄화규소 소결체를 제조함에 있어서In producing silicon carbide sintered body with sialon composition as grain boundary 소결조제로 시알론 조성(질화규소, 질화알루미늄, 이트리아)을 첨가하는 방법Method of adding sialon composition (silicon nitride, aluminum nitride, yttria) as sintering aid 소결 및 열처리시 계면에 시알론상을 형성시키면서 고밀도 소결체를 얻는 방법Method of obtaining high density sintered body by forming sialon phase at interface during sintering and heat treatment 시알론 입계상 및 고밀도 형성에 의한 고인성 탄화규소를 제조하는 방법Method for producing highly tough silicon carbide by sialon grain boundary and high density formation 소결조건 및 열처리 조건 제어에 의하여 탄화규소의 미세구조를 제어하는 방법Method of controlling microstructure of silicon carbide by controlling sintering condition and heat treatment condition
KR1020000037641A 2000-07-03 2000-07-03 Preparation Method of High Toughened Silicon Carbide with Sialon Grain Boundary KR20020004129A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115894058A (en) * 2022-11-25 2023-04-04 南京航空航天大学 Method for flash-burning rapid densification of SiC/SiC composite material

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0193472A (en) * 1987-09-30 1989-04-12 Toshiba Corp Heat-exchanger
KR900007722A (en) * 1988-11-24 1990-06-01 니혼 도꾸쇼 도오교오 가부시끼가이샤 Silicon Nitride Base Sintered Body
JPH06298568A (en) * 1993-04-09 1994-10-25 Toshiba Tungaloy Co Ltd Whisker-reinforced sialon-based sintered compact and sintered and coated material
JPH07277835A (en) * 1994-04-01 1995-10-24 Toyota Central Res & Dev Lab Inc Production of combined sintered compact
JPH1029869A (en) * 1996-07-15 1998-02-03 Honda Motor Co Ltd Silicon nitride-silicon carbide composite sintered compact and its production
KR0168303B1 (en) * 1995-07-11 1999-01-15 니시므로 타이조우 Aluminum nitride sinter and process for the production thereof
JPH1179849A (en) * 1997-09-09 1999-03-23 Sumitomo Electric Ind Ltd Silicon carbide sintered compact and its production

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0193472A (en) * 1987-09-30 1989-04-12 Toshiba Corp Heat-exchanger
KR900007722A (en) * 1988-11-24 1990-06-01 니혼 도꾸쇼 도오교오 가부시끼가이샤 Silicon Nitride Base Sintered Body
JPH06298568A (en) * 1993-04-09 1994-10-25 Toshiba Tungaloy Co Ltd Whisker-reinforced sialon-based sintered compact and sintered and coated material
JPH07277835A (en) * 1994-04-01 1995-10-24 Toyota Central Res & Dev Lab Inc Production of combined sintered compact
KR0168303B1 (en) * 1995-07-11 1999-01-15 니시므로 타이조우 Aluminum nitride sinter and process for the production thereof
JPH1029869A (en) * 1996-07-15 1998-02-03 Honda Motor Co Ltd Silicon nitride-silicon carbide composite sintered compact and its production
JPH1179849A (en) * 1997-09-09 1999-03-23 Sumitomo Electric Ind Ltd Silicon carbide sintered compact and its production

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115894058A (en) * 2022-11-25 2023-04-04 南京航空航天大学 Method for flash-burning rapid densification of SiC/SiC composite material

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