KR100232057B1 - Sialon synthesis from natural silicon and aluminium powder using microwave heating - Google Patents

Sialon synthesis from natural silicon and aluminium powder using microwave heating Download PDF

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KR100232057B1
KR100232057B1 KR1019970014737A KR19970014737A KR100232057B1 KR 100232057 B1 KR100232057 B1 KR 100232057B1 KR 1019970014737 A KR1019970014737 A KR 1019970014737A KR 19970014737 A KR19970014737 A KR 19970014737A KR 100232057 B1 KR100232057 B1 KR 100232057B1
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powder
sialon
synthesis
microwave heating
aluminium powder
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KR1019970014737A
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KR19980077569A (en
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안주삼
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장기중
요업기술원
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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
    • C04B35/58—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
    • C04B35/597—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 silicon oxynitride, e.g. SIALONS
    • 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
    • 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
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium
    • 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
    • C04B2235/658—Atmosphere during thermal treatment
    • 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
    • C04B2235/74—Physical characteristics
    • C04B2235/76—Crystal structural characteristics, e.g. symmetry
    • C04B2235/767—Hexagonal symmetry, e.g. beta-Si3N4, beta-Sialon, alpha-SiC or hexa-ferrites

Abstract

본 발명은 천연규석 분말과 Al 분말 성형체로부터 새로운 싸이알론(sialon)합성공정 개발에 관한 것으로 종전의 매우 긴 사이알론 합성 시간을 줄일 수 있는 공정을 개발하고자 하였다. 이 제조공정은 마이크로파(2.54GHz)를 사용하여 천연규석 분말과 Al 분말 성형체를 자체전파고온합성법(Self-propagating High-temperature Combustion Synthesis) 반응을 시킨 후에 생긴 Si, Al2O3, AIN를 냉각과정 없이 곧바로 가열할 수가 있고 질소 분위기에서 질화 시켜서 3½시간안에 싸이알론상을 합성할 수 있음을 특징으로 한다.The present invention relates to the development of a new sialon synthesis process from natural silica powder and Al powder compacts, and to develop a process that can reduce the conventional very long sialon synthesis time. This manufacturing process uses microwave (2.54GHz) to cool Si, Al 2 O 3 , and AIN formed after self-propagating High-temperature Combustion Synthesis reaction of natural silica powder and Al powder compact. It can be heated directly without nitriding and nitrided in a nitrogen atmosphere to synthesize a thialone phase in 3½ hours.

Description

마이크로파(2.45GHz)를 사용한 천연규석 분말과 Al 분말성형체로부터 사이알론(sialon)합성법Synthesis of sialon from natural silica powder and Al powder compact using microwave (2.45 GHz)

본 발명은 천연규석 분말과 Al 분말로부터 새로운 sialon 합성 공정개발에 관한 것이다. sialon 합성법으로는 화산재에 Al을 환원제로 사용하거나 알루미나-규소계 광물에 탄소를 환원제로 사용하여 질화 분위기하에 고온에서 장시간 가열하는 방법이 있다. 그러나 이러한 합성법은 공정시간이 너무 긴 단점(10시간 이상)이 있다.The present invention relates to the development of a new sialon synthesis process from natural silica powder and Al powder. As the sialon synthesis method, Al is used as a reducing agent in volcanic ash or carbon is used as a reducing agent in alumina-silicon-based minerals, which is heated for a long time at high temperature in a nitriding atmosphere. However, this synthesis method has a disadvantage that the process time is too long (more than 10 hours).

본 발명은 긴 공정시간을 줄이기 위하여 발명된 것으로 SiO2분말과 Al 분말만을 혼합하여 (별도의 환원제 첨가없이 ) 마이크로파 에너지를 이용하여 자체전파고온합성법(Self-propagating High-temperature Combustion Synthesis)반응을 시키고 이 반응 생성물을 질화시켜서 사이알론을 짧은 시간(3½시간)내에 합성하는 방법을 제공하는데 그 목적이 있다.The present invention was invented in order to reduce the long process time, by mixing only SiO 2 powder and Al powder to perform a self-propagating High-temperature Combustion Synthesis reaction using microwave energy (without the addition of a separate reducing agent). The objective is to provide a method of nitriding this reaction product to synthesize sialon in a short time (3½ hours).

본 발명에서는 60중량부 천연규석분말과 40중량부 Al분말 성형체를 시편으로 사용했으며 이 시편을 마이크로파 반응기 안에 넣고 마이크로파를 조사하면 시편과 시편사이에서 점화가 일어나 연소파대가 시편 중앙 부분으로 전파되어 나가면서 자체전파고온합성법(SHS)반응이 완료된다. 반응후 XRD로 상분석을 해보면 미반응물은 없었으며 반응생성물인 Si, Al2O3AIN가 생성되어 있다. 이 때 마이크로파 출력이 연소파대의 속도에 영향을 미치는데, 출력이 너무 낮거나 너무 높으면 연소파대가 시편 중간에서 멈춰버리거나 너무 빨리 진행해 버려서 미반응물이 많이 남게 된다.In the present invention, 60 parts by weight of natural silica powder and 40 parts by weight of Al powder compacts were used as specimens. When the specimens were placed in a microwave reactor and irradiated with microwaves, ignition occurred between the specimens and the specimen, and the combustion band was propagated to the center portion of the specimen. The self propagation high temperature synthesis (SHS) reaction is completed. After the reaction, phase analysis by XRD showed no unreacted product and reaction product, Si, Al 2 O 3 AIN, was formed. At this time, the microwave output affects the speed of the combustion band. If the power is too low or too high, the combustion band will stop in the middle of the specimen or proceed too fast, leaving a lot of unreacted material.

적정 출력은 마이크로파 발진기와 가열하고자 하는 물질, 그리고 마이크로파 반응기의 구조에 따라서 다른 값을 가진다.The optimum power depends on the microwave oscillator, the material to be heated and the structure of the microwave reactor.

이렇게 생긴 SHS 반응생성물을 냉각과정없이 곧바로 마이크로파로 가열할 수 있는데 이것이 가능한 이유는 마이크로파 특성상 시편의 온도가 고온이면 고온일수록 마이크로파 흡수능력이 훨씬 좋아져서 가열이 용이하기 때문이다.This SHS reaction product can be directly heated by microwave without cooling process. This is possible because of the microwave characteristics, the higher the temperature of the specimen, the easier the microwave absorption capacity becomes.

SHS 반응생성물은 SHS 반응 바로 직후였을 때에는 온도가 고온이기 때문에 마이크로파 가열이 가능하게 되며 시편이 온도가 질화온도에 도달하면 사이알상이 형성되기 시작한다.Since the SHS reaction product is just after the SHS reaction, since the temperature is high, microwave heating is possible. As the specimen reaches the nitriding temperature, a sial phase starts to form.

미국 Cober 사 S6G 마이크로파 발진기를 사용한 경우 SHS합성시에는 출력이 1500W였으며, 실험시작후 질화온도(1500℃)까지 도달시간은 약 30분이 소요되었고 출력은 2000W이었다. 3시간의 질화공정후 X-ray 회절분석을 한 결과 β-sialon상만이 존재하였다.In the case of US Cober S6G microwave oscillator, the output was 1500W at the time of SHS synthesis. It took about 30 minutes to reach the nitriding temperature (1500 ℃) after the start of the experiment and the output was 2000W. After 3 hours of nitriding, X-ray diffraction analysis revealed only β-sialon phase.

상술한 바와 같이 본 발명은 별도의 카본등과 같은 환원제를 사용하지 않고 Al 분말자체가 환원제역할을 하므로 인해 종래의 긴 β-sialon 합성시간을 대폭 줄일 수 있었고 공정도 단순화 시킬 수 있었으며, 이에 따른 경비 절감효과도 기대할 수 있다.As described above, since the Al powder itself acts as a reducing agent without using a reducing agent such as carbon, the conventional long β-sialon synthesis time can be greatly reduced and the process can be simplified. Savings can also be expected.

Claims (1)

60 중량부 천연규석 분말과 40 중량부 Al 분말의 혼합성형체를 질소분위기를 사용한 마이크로파 반응기 안에서 SHS반응을 시키고 냉각과정없이 곧바로 가열시켜 질화온도에서 짧은 시간(3½시간)내에 β-sialon을 합성할 수 있는 제조방법.A mixture of 60 parts by weight of natural silica powder and 40 parts by weight of Al powder was subjected to SHS reaction in a microwave reactor using nitrogen atmosphere and heated immediately without cooling process to synthesize β-sialon within a short time (3½ hours) at nitriding temperature. Manufacturing method.
KR1019970014737A 1997-04-21 1997-04-21 Sialon synthesis from natural silicon and aluminium powder using microwave heating KR100232057B1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100395212C (en) * 2005-11-18 2008-06-18 清华大学 Process for sintering Sialong binding silicon carbide refractory by microwave tech.
CN106892666A (en) * 2017-03-17 2017-06-27 太原理工大学 A kind of coal gangue combustion synthesizes the method for β SIALON based composite powders

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101135515B1 (en) * 2009-11-23 2012-04-13 조선내화 주식회사 Method for manufacture of sialon
CN114956824B (en) * 2022-01-17 2023-04-25 昆明理工大学 Method for preparing MAX binder diamond composite material by using high-heat value alloy to induce microwave self-propagating sintering reaction

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100395212C (en) * 2005-11-18 2008-06-18 清华大学 Process for sintering Sialong binding silicon carbide refractory by microwave tech.
CN106892666A (en) * 2017-03-17 2017-06-27 太原理工大学 A kind of coal gangue combustion synthesizes the method for β SIALON based composite powders

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