[go: up one dir, main page]
More Web Proxy on the site http://driver.im/

KR840008789A - High purity aluminum nitride fine powder, compositions thereof and sintered bodies thereof, and methods for producing them - Google Patents

High purity aluminum nitride fine powder, compositions thereof and sintered bodies thereof, and methods for producing them Download PDF

Info

Publication number
KR840008789A
KR840008789A KR1019840001357A KR840001357A KR840008789A KR 840008789 A KR840008789 A KR 840008789A KR 1019840001357 A KR1019840001357 A KR 1019840001357A KR 840001357 A KR840001357 A KR 840001357A KR 840008789 A KR840008789 A KR 840008789A
Authority
KR
South Korea
Prior art keywords
weight
metal
aluminum nitride
less
fine
Prior art date
Application number
KR1019840001357A
Other languages
Korean (ko)
Other versions
KR880002226B1 (en
Inventor
노부유끼 구라모또 (외 1)
Original Assignee
오노우에 야스하루
도꾸야마 소다 가부시기 가이샤
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 오노우에 야스하루, 도꾸야마 소다 가부시기 가이샤 filed Critical 오노우에 야스하루
Publication of KR840008789A publication Critical patent/KR840008789A/en
Application granted granted Critical
Publication of KR880002226B1 publication Critical patent/KR880002226B1/en

Links

Classifications

    • 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
    • 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
    • C04B35/58Shaped 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
    • 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
    • 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
    • C04B35/58Shaped 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
    • C04B35/581Shaped 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 aluminium nitride
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/06Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/072Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
    • C01B21/0726Preparation by carboreductive nitridation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/10Solid density
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/32Thermal properties
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Landscapes

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

Abstract

내용 없음No content

Description

고순도의 질화알루미늄 미분말, 그의 조성물 및 그의 소결체, 및 그들의 제조방법High purity aluminum nitride fine powder, compositions thereof and sintered bodies thereof, and methods for producing them

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음Since this is an open matter, no full text was included.

제1도 광선의 파장에 따른 본 발명 소결체의 광선 투과율 관계를 나타낸다. 제2도 본 발명 소결체의 견본사진. 제3도는 본 발명열압소결체의 견본의 기계적으로 분열된 표면을 찍은 주사 전자 현미경 사진.1 shows the light transmittance relationship of the sintered body of the present invention according to the wavelength of light. 2 is a sample photograph of the sintered body of the present invention. 3 is a scanning electron micrograph of a mechanically cleaved surface of a sample of the inventive thermocompression compact.

Claims (54)

2마이크론 이하의 평균 입자 직경을 갖고 94중량% 이상의 질화 알루미늄, 3중량%이하의 결합산소 및 0.5중량%이하(금속으로 계산된)의 불순물로서의 금속 화합물을 함유하는 질화 알루미늄 미분말.An aluminum nitride fine powder having an average particle diameter of 2 microns or less and containing 94% by weight or more of aluminum nitride, 3% by weight or less of bound oxygen, and a metal compound as impurities of 0.5% or less (calculated by metal). 제1항에 있어서, 결합산소의 함량이 1.5중량%이하인 질화 알루미늄 미분말.The fine aluminum nitride powder according to claim 1, wherein the content of bound oxygen is 1.5% by weight or less. 제1항에 있어서, 불순물로서의 금속 화합물의 함량이 0.3중량%이하(금속으로 계산된)인 질화 알루미늄 미분말.The fine aluminum nitride powder according to claim 1, wherein the content of the metal compound as an impurity is 0.3 wt% or less (calculated as a metal). 제1항에 있어서, 금속 화합물의 금속이 탄소, 실리콘, 망간, 철, 크롬, 니켈, 코발트, 구리, 아연 또는 티타늄인 질화 알루미늄 미분말.The fine aluminum nitride powder according to claim 1, wherein the metal of the metal compound is carbon, silicon, manganese, iron, chromium, nickel, cobalt, copper, zinc or titanium. 제1항에 있어서, 금속화합물의 금속이 철,크롬, 니켈, 코발트, 구리, 아연 또는 티타늄이고 이들 금속화합물의 총함량이 0.3중량%이하(금속으로 계산된)인 질화 알루미늄 미분말.The fine aluminum nitride powder according to claim 1, wherein the metal of the metal compound is iron, chromium, nickel, cobalt, copper, zinc or titanium, and the total content of these metal compounds is 0.3 wt% or less (calculated as metal). 제1항에 있어서, 질화알루미늄의 함량이 97중량%이상인 질화 알루미늄 미분말.The fine powder of aluminum nitride of Claim 1 whose content of aluminum nitride is 97 weight% or more. 제1항에 있어서, 3마이크론 이하의 입자 직경을 갖는 입자를 70부피%이상 함유하는 질화 알루미늄 미분말.The fine aluminum nitride powder according to claim 1, which contains 70% by volume or more of particles having a particle diameter of 3 microns or less. 제1항에 있어서, 2마이크론 이하의 평균 입자직경을 갖는 5구형입자 또는 그의 2차 단괴로 이루어진 질화 알루미늄 미분말.The fine powder of aluminum nitride according to claim 1, which is composed of five spherical particles having a mean particle diameter of 2 microns or less, or secondary nodules thereof. (1) 2마이크론 이하의 평균입자 직경을 갖는 알루미나 미분말 0.2%이하의 제함량 및 1마이크론이하의 평균 입자 직경을 갖는 탄소 미분말과 액체 분산매질내에서 알루미나 미분말 대 탄소 미분말의 중량비를 1 : 0.36내지 1 : 1로하여 고르게 혼합하고, (2) 제조된 고른 혼합물을 임의로 건조시킨후 질소 또는 암모니아 분위기하에, 1,400내지 1,700℃의 온도에서 연소시키고, (3) 그 다음 제조된 미분말을 600내지 900℃의 온도에서 가열해서 비반응 탄소를 제거함으로써 2마이크론 이하의 평균입자 직경을 갖고 94중량%이상의 질화 알루미늄, 3중량%이하의 결합 산소 및 0.5중량%이하(금속으로 계산된)의 불순물로서의 금속 화합물을 함유하는 질화 알루미늄 미분말을 제조함을 특징으로하는 질화 알루미늄 미분말의 제조방법.(1) The weight ratio of fine alumina powder to fine carbon powder in a liquid dispersion medium of carbon fine powder having an average particle diameter of 0.2% or less and an average particle diameter of 1 micron or less with an average particle diameter of 2 microns or less is 1: 0.36-1. : Uniformly mixed with (1), (2) optionally drying the prepared mixture, and then burning it under a nitrogen or ammonia atmosphere at a temperature of 1,400 to 1,700 ° C, and (3) preparing the fine powder at 600 to 900 ° C. By heating at temperature to remove unreacted carbon, a metal compound having an average particle diameter of 2 microns or less, 94% by weight or more of aluminum nitride, 3% by weight or less of bound oxygen, and 0.5% or less by weight (calculated as metal) as an impurity A process for producing an aluminum nitride fine powder, which comprises producing an aluminum nitride fine powder containing it. 제9항에 있어서, 알루미늄 미분말이 99.0중량%이상의 순도를 갖는 방법.10. The method of claim 9, wherein the fine aluminum powder has a purity of at least 99.0% by weight. 제9항에 있어서, 알루미나 미분말 대 탄소 미분말의 중량비가 1 : 0.4내지 1 : 1인 방법.The method of claim 9 wherein the weight ratio of fine alumina powder to fine carbon powder is from 1: 0.4 to 1: 1. 제9항에 있어서, 액체 분산 매질이 물, 탄화수소, 지방족 알콜 또는 이들의 혼합물인 방법.10. The method of claim 9, wherein the liquid dispersion medium is water, hydrocarbons, aliphatic alcohols or mixtures thereof. 90중량%이상의 질화 알루미늄, 4.5중량%이하의 결합산소 및 알칼리토금속, 란탄족 금속 및 이트륨 또는 그의 화합물중에서 선택된 하나 이상의 금속 원소의최고 원자가를 갖는 산화물 0.02내지 5.0중량%, 및 상술한 금속의 화합물과는 다른 불순물로서의 금속 화합물의 금속 5.0중량%이하를 함유하는 질화 알루미늄 미분말의 고른 조성물.At least 90% by weight of aluminum nitride, at most 4.5% by weight of bonded oxygen and alkaline earth metals, lanthanide metals and yttrium or at least 0.02 to 5.0% by weight of oxides having the highest valence of at least one metal element, and compounds of the metals described above The even composition of the aluminum nitride fine powder containing 5.0 weight% or less of the metal of a metal compound as an impurity different from that. 제13항에 있어서, 결합산소의 함량이 3중량%이하인 조성물.The composition of claim 13, wherein the content of bound oxygen is 3% by weight or less. 제13항에 있어서, 불순물로서의 금속 화합물의 함량이 0.3중량%이하인 조성물.The composition according to claim 13, wherein the content of the metal compound as an impurity is 0.3 wt% or less. 제13항에 있어서, 불순물로서의 금속 화합물의 금속이 탄소, 실리콕, 망간, 철, 크롬, 니켈, 코발트, 구리, 아연, 또는 티타늄인 조성물.The composition of claim 13, wherein the metal of the metal compound as an impurity is carbon, silicon, manganese, iron, chromium, nickel, cobalt, copper, zinc, or titanium. 제13항에 있어서, 불순물로서의 상술한 금속화합물의 금속이 철, 크롬, 니켈, 코발트, 구리, 아연 또는 티타늄이고 금속으로 계산된 이들 불순물의 총함량이 0.1중량%이하인 조성물.The composition according to claim 13, wherein the metal of the above-described metal compound as an impurity is iron, chromium, nickel, cobalt, copper, zinc or titanium and the total content of these impurities calculated as metal is 0.1% by weight or less. 제13항에 있어서, 알칼리 토금속이 칼슘, 스트론튬 및 바륨인 조성물.The composition of claim 13 wherein the alkaline earth metal is calcium, strontium and barium. 제13항에 있어서, 란탄족 금속이 란탄, 네오디뮴 및 세륨인 조성물.The composition of claim 13 wherein the lanthanide metal is lanthanum, neodymium and cerium. 제13항에 있어서, 질화 알루미늄의 함량이 93중량% 이상인 조성물.The composition of claim 13, wherein the content of aluminum nitride is at least 93% by weight. (1) 2마이크론 이하의 평균입자 직경을 갖는 알루미나 미분말, 0.2중량%이하의 재함량 및 1마이크론 이하의 평균 입자 직경을 갖는 탄소 미분말 및 알칼리 토금속, 란탄족 금속 및 이트륨중에서 선택된 금속의 화합물을 액체매질내에서 알루미나 미분말대 탄소미분말의 중량비를 1 : 0.36내지 1 : 1로 하고 최고 원자가를 갖는 금속 산화물로 계산된 금속화합물의 양을 최종 생성물에 대해 0.02내지 5.0중량%로 하여 고르게 혼합하고, (2) 제조된 고른 혼합물을 임의로 건조시킨후, 질소 또는 암모니아 분위기하에 1,400내지 900℃의 온도에서 연소시키고, (3) 그런후 제조된 미분말을 산소를 함유하는 분위기하에 600내지 00℃의 온도에서 가열해서 비반응 탄소를 제거함으로써 90중량% 이상의 질화 알루미늄, 4.5중량%이하의 결합 탄소, 및 알칼리 토금속, 란탄족 금속 및 이트륨 또는 그의 화합물중에서 선택된 하나 이상의 금속 원소의 최고 원자가를 갖는 산화물 0.02내지 5.0중량 및 상술한 금속의 화합물과는 다른 불순물로서의 금속화합물 0.5중량%이하(금속으로 계산된)를 함유하는 고른 조성물을 제조함을 특징으로 하는 질화 알루미늄 미분말의 고른 조성물의 제조방법.(1) A fine powder of alumina having an average particle diameter of 2 microns or less, a carbon fine powder having a recontent of 0.2 wt% or less and an average particle diameter of 1 micron or less, and a compound of a metal selected from alkaline earth metals, lanthanide metals and yttrium The weight ratio of the fine alumina powder to the fine carbon powder in the medium is 1: 0.36 to 1: 1, and the amount of the metal compound calculated as the metal oxide having the highest valence is 0.02 to 5.0% by weight based on the final product, and mixed evenly ( 2) optionally drying the prepared mixture, and then burning it at a temperature of 1,400 to 900 ° C. under a nitrogen or ammonia atmosphere, and (3) heating the prepared fine powder at a temperature of 600 to 00 ° C. under an atmosphere containing oxygen. 90% by weight or more of aluminum nitride, 4.5% by weight or less of bonded carbon, and alkaline earth metals and lanthanides by removing unreacted carbon An even composition containing from 0.02 to 5.0 weights of an oxide having the highest valence of at least one metal element selected from the genus and yttrium or compounds thereof and less than or equal to 0.5% by weight (calculated as metal) of the metal compound as an impurity other than the above-described metal compound Method for producing an even composition of the aluminum nitride fine powder, characterized in that to prepare. 2마이크론 이하의 평균 입자 직경을 갖고 94중량% 이상의 질화 알루미늄, 3중량%이하의 결합 산소 및 불순물로서의 금속화합물 0.5중량%이하 (금속으로 계산된)를 함유하는 질화 알루미늄 미분말을 알칼리 토금속, 라탄족 금속 및 이트륨중에서 선택된 하나 이상의 금속의 화합물과 혼합하되 최고 원자가를 갖는 금속 산화물로서 계산된 상술한 금속의 화합물의 함량이 최종 조성물에 대해 0.02내지 5.0중량%가 되는 비율로 고르게 혼합함으로써 90중량%이상의 질화 알루미늄, 4.5중량%이하의 결합 산소 및 알칼리 토금속, 라탄족, 금속 및 이트륨 또는 그의 화합물중에서 선택된 하나 이상의 금속 원소의 최고원자가를 갖는 산화물 0.02내지 5.0중량% 및 상술한 금속의 화합물과는 다른 불순물로서의 금속화합물 0.5중량%이하(금속으로 계산된)를 함유하는 고른 조성물을 제조함을 특징으로 하는 질화 알루미늄 미분말의 고른 조성물의 제조방법.Finely divided aluminum nitride powders having an average particle diameter of 2 microns or less and containing 94% by weight or more of aluminum nitride, 3% by weight or less of bound oxygen, and a metal compound of 0.5% or less (calculated by metal) as impurities are alkaline earth metals and rattans. 90% by weight or more by mixing with a compound of one or more metals selected from metals and yttrium, but evenly mixing at a rate such that the content of the compound of the metals described above as the metal oxide having the highest valence is 0.02 to 5.0% by weight relative to the final composition. Aluminum nitride, up to 4.5% by weight of bonded oxygen and oxides having the highest valence of at least one metal element selected from alkaline earth metals, ratans, metals and yttrium or compounds thereof and impurities other than the compounds of the metals described above It contains less than 0.5% by weight of metal compound (calculated as metal) The method for producing an even composition of fine aluminum nitride powder, characterized in that to produce an even composition. 고순도 및 2.9g/㎤이상의 밀도를 갖고 94중량%이상의 질화 알루미늄, 1.5중량%이하의 결합 산소 및 불순물로서의 금속화합물 0.5중량%이하(금속으로 계산된)를 함유하는 질화 알루미늄 소결체.An aluminum nitride sintered body having high purity and a density of at least 2.9 g / cm 3 and containing not less than 94% by weight of aluminum nitride, not more than 1.5% by weight of bound oxygen, and not more than 0.5% by weight of a metal compound (calculated as a metal) as impurities. 제23항에 있어서, 결합 산소의 함량이 0.75중량%이하인 소결체.The sintered compact according to claim 23, wherein the content of bound oxygen is 0.75% by weight or less. 제23항에 있어서, 불순물로서의 금속 화합물의 함량이 금속으로 계산하여 0.3중량%이하인 소결체.The sintered compact according to claim 23, wherein the content of the metal compound as an impurity is 0.3 wt% or less, calculated as a metal. 제23항에 있어서, 불순물로서의 금속 화합물의 금속이 탄소, 실리콘, 망간, 철, 크롬, 니켈, 코발트, 구리, 아연 또는 티타늄인 소결체.The sintered compact according to claim 23, wherein the metal of the metal compound as an impurity is carbon, silicon, manganese, iron, chromium, nickel, cobalt, copper, zinc or titanium. 제23항에 있어서, 불순물로서의 금속 화합물의 금속이 철, 크롬, 니켈, 코발트, 구리, 아연 또는 티타늄이고, 이들 불순물의 총량이 0.1중량%이하(금속으로 계산된)인 소결체.The sintered compact according to claim 23, wherein the metal of the metal compound as an impurity is iron, chromium, nickel, cobalt, copper, zinc or titanium, and the total amount of these impurities is 0.1 wt% or less (calculated as a metal). 제23항에 있어서, 질화 알루미늄의 함량이 97중량%이상인 소결체The sintered compact according to claim 23, wherein the content of aluminum nitride is 97% by weight or more. 제23항에 있어서, 3.16g/㎤이상의 밀도를 갖는 소결체.The sintered compact according to claim 23, having a density of at least 3.16 g / cm 3. 2마이크론 이하의 평균 입자 직경을 갖고 94중량%이상의 질화 알루미늄, 3.0중량%이하의 결합산소 및 불순물로서 금속 화합물 0.5중량%이하(금속으로 계산된)를 함유하는 질화 알루미늄 미분말을 모올딩시키고, 모울딩된 물질을 불활성 분위기하에 1,700내지 2,100℃의 온도에서 소결시킴으로써 2.9g/㎤이상의 밀도를 갖고 94중량% 이상의 질화 알루미늄, 1.5중량%이하의 결합산소 및 불순물로서의 금속화합물 0.5중량%이하(금속으로 계산된)를 함유하는 질화 알루미늄 소결체를 제조함을 특징으로 하는 고순도 및 고밀도를 갖는 질화 알루미늄 소결체의 제조방법.A fine aluminum nitride powder having an average particle diameter of 2 microns or less and containing not less than 94% by weight of aluminum nitride, not more than 3.0% by weight of bound oxygen and a metal compound of 0.5% by weight or less (calculated as a metal) as impurities, The sintered material is sintered at an inert atmosphere at a temperature of 1,700 to 2,100 ° C., having a density of at least 2.9 g / cm 3, at least 94% by weight of aluminum nitride, at most 1.5% by weight of bound oxygen, and at most 0.5% by weight of a metal compound as impurities A method for producing an aluminum nitride sintered body having high purity and high density, characterized by producing an aluminum nitride sintered body containing the calculated). 제30항에 있어서, 소결을 20㎏/㎠이상의 압력하에서 수행하는 방법.31. The method of claim 30, wherein sintering is carried out at a pressure of at least 20 kg / cm 2. 제30항에 있어서, 소결을 질소 분위기하에서 수행하는 방법.31. The method of claim 30, wherein sintering is carried out in a nitrogen atmosphere. 제30항에 있어서, 소결을 실제 압력부재하에 수행하는 방법.31. The method of claim 30, wherein sintering is carried out under actual pressure. 제33항에 있어서, 소결을 질소 분위기하에서 수행하는 방법.The method of claim 33, wherein the sintering is carried out in a nitrogen atmosphere. 제30항에 있어서, 소결을 진공에서 수행하는 방법.31. The method of claim 30, wherein sintering is performed in vacuo. 3.0g/㎡이상의 밀도를 갖고 90중량%이상의 질화 알루미늄, 3.5중량%이하의 결합 산소 및 알칼리 토금속, 란탄족 금속 및 이트륨 또는 그의 화합물중에서 선택된 하나 이상의 금속 원소의 최고원자가를 갖는 산화물 0.02내지 5.0중량% 및 상술한 금속의 화합물과는 다른 불순물로서의 금속화합물의 금속 0.5중량% 이하를 함유하는 고밀도 및 순도의 질화 알루미늄 소결체.Oxides having a density of at least 3.0 g / m 2 and at least 90% by weight of aluminum nitride, at most 3.5% by weight of bonded oxygen and oxides having a highest atom of at least one metal element selected from alkaline earth metals, lanthanide metals and yttrium or compounds thereof A high-density and purity aluminum nitride sintered body containing 0.5% by weight or less of a metal compound as an impurity different from the compound of the metal and the aforementioned metal. 제36항에 있어서, 결합 산소의 함량이 2.0중량%이하인 소결체.The sintered compact according to claim 36, wherein the content of bound oxygen is 2.0 wt% or less. 제36항에 있어서, 불순물로서의 금속 화합물의 함량이 금속으로 계산하여 0.3중량이하인 소결체.The sintered compact according to claim 36, wherein the content of the metal compound as an impurity is 0.3 wt% or less, calculated as a metal. 제36항에 있어서, 불순물로서의 금속 화합물의 금속이 탄소, 실리콘, 망간, 철, 크롬, 니켈, 코발트, 구리, 아연 또는 티타늄인 소결체.The sintered compact according to claim 36, wherein the metal of the metal compound as an impurity is carbon, silicon, manganese, iron, chromium, nickel, cobalt, copper, zinc or titanium. 제36항에 있어서, 불순물로서의 금속화합물의 금속이 철, 크롬, 니켈, 코발트, 구리, 아연 또는 티타늄이고 이들불순물의 총함량이 금속으로 계산하여 0.1중량%이하인 소결체.The sintered compact according to claim 36, wherein the metal of the metal compound as an impurity is iron, chromium, nickel, cobalt, copper, zinc, or titanium, and the total content of these impurities is 0.1% by weight or less, calculated as metal. 제36항에 있어서, 질화알루미늄의 함량이 93중량%이상인 소결체.The sintered compact according to claim 36, wherein the content of aluminum nitride is 93% by weight or more. 제36항에 있어서, 3.16g/㎤이상의 밀도를 갖는 소결체.The sintered compact according to claim 36, having a density of at least 3.16 g / cm 3. 90중량%이상의 질화 알루미늄, 4.5중량%이하의 결합 산소 및 알칼리 토금속, 란탄족 금속 및 이트륨 또는 그의 화합물중에서 선택된 하나 이상의 금속원소의 최고 원자를 갖는 산화물 0.02내지 5.0중량% 및 상술한 금속의 화합물과는 다른 불순불로서의 금속화합물 0.5중량%이하(금속으로 계산된)를 함유하는 질화 알루미늄 미분말을 모울딩 시키고, 모올딩된 물질을 불활성분위기 하에 1,600내지 2,100℃의 온도에서 소결시킴으로써 3.0g/㎤ 이상의 밀도를 갖고 90중량% 이상의 질화 알루미늄, 3.5중량%이하의 결합산소 및 알칼리 토금속, 란탄족 금속 및 이트륨 또는 그의 화합물중에서 선택된 하나 이상의 금속원소의 최고 원자가를 갖는 산화물 0.02내지 5.0중량% 및 상술한 금속의 화합물과는 다른 불순물로서의 금속화합물 0.5중량%이하(금속으로 계산)를 함유하는 소결체를 제조함을 특징으로 하는 고순도 및 밀도를 갖는 질화 알루미늄 소결체의 제조방법.At least 90% by weight of aluminum nitride, at most 4.5% by weight of bonded oxygen and at least 0.02 to 5.0% by weight of oxides having the highest atoms of at least one metal element selected from alkaline earth metals, lanthanide metals and yttrium or compounds thereof; Is 3.0 g / cm 3 or more by molding a fine aluminum nitride powder containing not more than 0.5% by weight (calculated as metal) as another impurity, and sintering the molded material at a temperature of 1,600 to 2,100 ° C. under an inert atmosphere. Oxides having a density of at least 90% by weight aluminum nitride, at most 3.5% by weight of bonded oxygen and alkaline earth metals, lanthanide metals and yttrium or at least one metal element selected from yttrium or compounds thereof 0.5 wt% or less of metal compound as impurity A method for producing an aluminum nitride sintered body having high purity and density, characterized by producing a sintered body containing a). 제43항에 있어서, 소결을 20㎏/㎠이상의 압력하에서 수행하는 방법.44. The method of claim 43, wherein the sintering is carried out at a pressure of at least 20 kg / cm 2. 제43항에 있어서, 소결을 질소 분위기하에서 수행하는 방법.The method of claim 43 wherein the sintering is carried out in a nitrogen atmosphere. 제43항에 있어서, 소결을 실제 압력 부재하에서 수행하는 방법.44. The method of claim 43, wherein sintering is carried out in the absence of actual pressure. 제46항에 있어서, 소결을 질소 분위기하에서 수행하는 방법.47. The process of claim 46, wherein sintering is carried out in a nitrogen atmosphere. 제43항에 있어서, 소결을 전공에서 수행하는 방법.44. The method of claim 43, wherein sintering is performed in the major. 고밀도를 가지며, 그의 기계적으로 분열된 표면이 뚜렷한 형태에 의해 서로 구분되는 촘촘히 페킹된 미립자로 구성되고, 분열된 표면에서 상술한 결정 미립자의 뚜렷한 형태가 다각형이며, 뚜렷한 형태에 의해 구분되는 상술한 분열표면에서 결정 입자의 70%이상이 0.5내지 1.5(여기서 마이크론 단위의는 결정 미립자의 평균 입자 직경이다.)범위의 입자 직경을 갖는 질화 알루미늄 소결체.The above-mentioned cleavage, which has a high density, is composed of closely pegged fine particles whose mechanically divided surfaces are distinguished from each other by distinct shapes, and in which the distinct shapes of the above-mentioned crystal grains are polygonal and are distinguished by distinct shapes. At least 70% of the crystal grains on the surface are 0.5 To 1.5 (Where the micron unit Is an average particle diameter of crystal fine particles.) An aluminum nitride sintered compact having a particle diameter in the range. 제49항에 있어서, 분열된 표면이 62.5±2.5℃에서 20분간 35% 인산 수용액으로 처리된 후에, 처리된 표면상에 각의 형태를 갖는 결정입자가 존재하는 소결체.50. The sintered compact according to claim 49, wherein after the cleaved surface has been treated with an aqueous 35% phosphoric acid solution at 62.5 ± 2.5 ° C. for 20 minutes, crystal particles having a angular form are present on the treated surface. 제49항에 있어서, 그의 X-선 회절방식에 있어서, 육각형 질화 알루미늄 결정에 기인한 6개의 선명한 회절선을 30°와 70°사이의 회절각(2θ)에서 보여주는 그러나 실제로 기타 다른 회설선은 전혀 보여주지 않는 소결체.50. The method of claim 49, wherein in its X-ray diffraction scheme, six clear diffraction lines resulting from hexagonal aluminum nitride crystals are shown at a diffraction angle (2θ) between 30 ° and 70 °, but in fact no other skew line is found at all. Sintered body not shown. 제49내지 51항중 어느 하나에 있어서, 압력 소결에 의해 제조되는 소결체.The sintered compact according to any one of claims 49 to 51, which is produced by pressure sintering. 제49내지 51항중 어느 하나에 있어서, 무압소결에 의해 제조되는 소결체.The sintered compact according to any one of claims 49 to 51, which is produced by pressureless sintering. ※ 참고사항 : 최초출원내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019840001357A 1983-05-13 1984-03-16 Method for preparing fine aluminum nitride powder KR880002226B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP82536 1983-05-13
JP58-82536 1983-05-13
JP58082536A JPS59207814A (en) 1983-05-13 1983-05-13 Aluminum nitride powder

Publications (2)

Publication Number Publication Date
KR840008789A true KR840008789A (en) 1984-12-19
KR880002226B1 KR880002226B1 (en) 1988-10-20

Family

ID=13777224

Family Applications (3)

Application Number Title Priority Date Filing Date
KR1019840001357A KR880002226B1 (en) 1983-05-13 1984-03-16 Method for preparing fine aluminum nitride powder
KR1019870004864A KR890002053B1 (en) 1983-05-13 1987-05-16 A method and composition for aluminium nitride
KR1019870004865A KR890002054B1 (en) 1983-05-13 1987-05-16 A method and composition for aluminium nitride

Family Applications After (2)

Application Number Title Priority Date Filing Date
KR1019870004864A KR890002053B1 (en) 1983-05-13 1987-05-16 A method and composition for aluminium nitride
KR1019870004865A KR890002054B1 (en) 1983-05-13 1987-05-16 A method and composition for aluminium nitride

Country Status (5)

Country Link
JP (1) JPS59207814A (en)
KR (3) KR880002226B1 (en)
CA (1) CA1223114A (en)
FR (2) FR2545810B1 (en)
NL (1) NL188280C (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61178470A (en) * 1985-02-04 1986-08-11 イビデン株式会社 Manufacture of high size-precision nitride sintered body andsame sintered body for heat-resistant tools
US4992253A (en) * 1989-12-29 1991-02-12 National Science Council Process for producing an ultrafine powder of aluminum nitride
KR101409182B1 (en) * 2012-04-02 2014-06-19 한국세라믹기술원 Manufacturing method of high purity aluminium nitride
KR101884979B1 (en) 2016-03-10 2018-08-02 이건배 A manufacturing method of aluminum nitride and an aluminum nitride prepared by the same

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE284531C (en) *
JPS5849510B2 (en) * 1973-06-30 1983-11-04 株式会社東芝 Chitsuka Aluminum Shouketsutaino
JPS5839764B2 (en) * 1978-03-10 1983-09-01 株式会社東芝 Method for producing aluminum nitride powder
JPS5855377A (en) * 1981-09-28 1983-04-01 株式会社東芝 Manufacture of aluminum nitride sintered body

Also Published As

Publication number Publication date
KR880002226B1 (en) 1988-10-20
FR2545810A1 (en) 1984-11-16
KR880014859A (en) 1988-12-24
JPS59207814A (en) 1984-11-26
FR2549822B1 (en) 1991-02-08
KR870011832A (en) 1987-12-26
KR890002053B1 (en) 1989-06-15
NL188280B (en) 1991-12-16
NL188280C (en) 1992-05-18
FR2549822A1 (en) 1985-02-01
NL8400796A (en) 1984-12-03
FR2545810B1 (en) 1990-07-13
KR890002054B1 (en) 1989-06-15
CA1223114A (en) 1987-06-23

Similar Documents

Publication Publication Date Title
EP0176737B1 (en) Process for production of readily sinterable aluminum nitride powder
US4778778A (en) Process for the production of sintered aluminum nitrides
JP2001080964A (en) POLYCRYSTAL SiC SINTERED COMPACT PRODUCTION OF THE SAME AND PRODUCT OBTAINED BY APPLYING THE SAME
EP0232094B1 (en) Chemical preparation of zirconium-aluminum-magnesium oxide composites
EP0186144B1 (en) Process for preparing aluminum nitride powder
JPH02503790A (en) sinterable nitride
US5004710A (en) Method for the chemical preparation of zirconia alloy powders and article
CA2083614A1 (en) Method for the preparation of .alpha.-aluminium oxide powder
KR900007723A (en) Aluminium Nitride And Method Of Manufacturing The Same
JP3280688B2 (en) Production method of rare earth oxide
KR840008789A (en) High purity aluminum nitride fine powder, compositions thereof and sintered bodies thereof, and methods for producing them
JPH0647447B2 (en) Method for producing aluminum nitride powder
JPS60210508A (en) Manufacture of sinterable ceramic fine powder
US5362691A (en) Sintered material based on Si3 N4 and processes for its production
US4774068A (en) Method for production of mullite of high purity
US3274008A (en) Refractory compositions and methods of preparation
US20060087063A1 (en) Process for preparing improved silicon carbide powder
US2733134A (en) Method for making titanium carbide
JPS5891065A (en) Manufacture of silicon carbide ceramic sintered body
JPH02160610A (en) Production of aluminum nitride powder
US5169810A (en) Process for forming tin-zirconia ceramics
EP0481563B1 (en) Process for preparing fine aluminium nitride powder.
JPS63159259A (en) High toughness silicon nitride base sintered body
JPH0519486B2 (en)
JPS61227908A (en) Preparation of raw material powder for sintered silicon nitride

Legal Events

Date Code Title Description
A201 Request for examination
E902 Notification of reason for refusal
E601 Decision to refuse application
J2X1 Appeal (before the patent court)

Free format text: APPEAL AGAINST DECISION TO DECLINE REFUSAL

G160 Decision to publish patent application
E701 Decision to grant or registration of patent right
GRNT Written decision to grant
FPAY Annual fee payment

Payment date: 20031013

Year of fee payment: 16

EXPY Expiration of term