JP3141505B2 - Aluminum nitride sintered body and method for producing the same - Google Patents

Aluminum nitride sintered body and method for producing the same

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Publication number
JP3141505B2
JP3141505B2 JP04081628A JP8162892A JP3141505B2 JP 3141505 B2 JP3141505 B2 JP 3141505B2 JP 04081628 A JP04081628 A JP 04081628A JP 8162892 A JP8162892 A JP 8162892A JP 3141505 B2 JP3141505 B2 JP 3141505B2
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Prior art keywords
sintered body
sintering
aluminum nitride
thermal conductivity
carbon
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JP04081628A
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Japanese (ja)
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JPH0912370A (en
Inventor
英子 福島
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Hitachi Metals Ltd
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Hitachi Metals Ltd
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Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【産業上の利用分野】本発明は窒化アルミニウム焼結体の製造
方法および窒化アルミニウム焼結体に関するものであり、特に
半導体の放熱性基板等に用いられるほぼ窒化アルミニウム単相
からなり均一な高熱伝導率を有する窒化アルミニウム焼結体の
製造方法および窒化アルミニウム焼結体に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing an aluminum nitride sintered body and an aluminum nitride sintered body. TECHNICAL FIELD The present invention relates to a method for producing an aluminum nitride sintered body having a high modulus and an aluminum nitride sintered body.

【0002】[0002]

【従来の技術】窒化アルミニウム(AlN)は、その材料がもつ高
い電気絶縁性、Siに近い熱膨張係数、高熱伝導性等の特
性により放熱性基板としての利用が検討されている。特
に、AlN原料粉末や焼結方法を検討することにより、AlN
の特性として非常に重要である熱伝導率を向上させる研
究が各方面で盛んに行われている。
2. Description of the Related Art Aluminum nitride (AlN) has been studied for use as a heat dissipating substrate because of its properties such as high electrical insulation, thermal expansion coefficient close to that of Si, and high thermal conductivity. In particular, by examining the AlN raw material powder and sintering method,
Research on improving the thermal conductivity, which is very important as a characteristic of, is being actively conducted in various fields.

【0003】一般に、AlN焼結体はAlN粉末とアルカリ土類や
希土類元素の化合物等の焼結助剤とを配合、混合、造
粒、成形し、常圧焼結により焼結体を得るという方法に
よって製作されている。これらのアルカリ土類や希土類元素
の化合物等の焼結助剤は、焼結時にAlN粉末中に不可避
的に混入されている酸素と反応し、アルミナと焼結助剤との
複合酸化物からなる液相を生成することにより焼結過程
における緻密化を可能にしている。また、この複合酸化
物の生成は、結果的に不純物酸素を粒界に固定し、粒内
への酸素の固溶を抑制しているため、熱伝導率を向上さ
せることにも寄与している。しかし、最終的に、その複
合酸化物が焼結体中に残存した場合、得られるAlN焼結
体の熱伝導率には限界があり、その熱伝導率は170W/m・K
以下であった。
In general, an AlN sintered body is obtained by mixing, mixing, granulating and molding AlN powder and a sintering aid such as a compound of an alkaline earth element or a rare earth element, and obtaining a sintered body by normal pressure sintering. Made by the method. These sintering aids such as alkaline earth and rare earth compounds react with oxygen unavoidably mixed into the AlN powder during sintering and consist of a composite oxide of alumina and the sintering aid. The formation of a liquid phase enables densification in the sintering process. In addition, the formation of the composite oxide also contributes to improving the thermal conductivity because, as a result, the impurity oxygen is fixed at the grain boundaries and the solid solution of oxygen in the grains is suppressed. . However, when the composite oxide finally remains in the sintered body, the thermal conductivity of the obtained AlN sintered body is limited, and its thermal conductivity is 170 W / mK
It was below.

【0004】現在、半導体の高容量化が進められる中
で、半導体搭載用の回路基板、放熱基板等にはより高い
熱伝導率を有する材料が必要とされており、かかるニース゛
に応えるために窒化アルミニウムを適用するにあたっては、酸
素その他の不純物の存在、焼結助剤添加の結果として粒
界に生成する粒界相の存在等の問題を解消する必要があ
る。
At present, as the capacity of semiconductors is increased, materials having higher thermal conductivity are required for circuit boards for mounting semiconductors, heat radiation boards, and the like. In applying aluminum, it is necessary to eliminate problems such as the presence of oxygen and other impurities and the presence of a grain boundary phase generated at the grain boundary as a result of the addition of a sintering aid.

【0005】この様な観点から特開昭63-277573には熱
伝導性により優れた窒化アルミニウム焼結体を提供することを
目的として焼結助剤としてイットリウムおよび/またはカルシウム
化合物をAlN粉末に添加し、これを窒素カ゛スを含む還元
性雰囲気中で焼成することによって、YーAlーO系化合物お
よび/またはCa-Al-O系化合物相等の粒界相の存在量を
従来の窒化アルミニウム焼結体に比べて減少させると共に、
低温と高温の2段階で焼結する多段階のフ゜ロク゛ラムからなる
焼結を行うことによって、高い熱伝導率を有する窒化アル
ミニウム焼結体を得るための最適条件を種々検討し、かかる
検討に基づく窒化アルミニウムの製造方法が提案されている。
この特開昭63-277573に記載された窒化アルミニウムの製造方
法における焼結過程の反応のメカニス゛ムは、最表面の複合酸
化物が還元窒化反応により除去されると複合酸化物の濃
度勾配が生じ、それが駆動力となり、内部の複合酸化物
が表面へ移動する、という繰り返しにより高熱伝導性Al
N焼結体が作製されるというものである。
[0005] From this viewpoint, Japanese Patent Application Laid-Open No. 63-277573 discloses the addition of a yttrium and / or calcium compound to AlN powder as a sintering aid in order to provide an aluminum nitride sintered body having excellent thermal conductivity. By firing this in a reducing atmosphere containing nitrogen gas, the amount of grain boundary phase such as Y-Al-O-based compound and / or Ca-Al-O-based compound phase can be reduced by conventional aluminum nitride sintering. While reducing it compared to the body,
By performing sintering consisting of multi-stage sintering in two stages of low temperature and high temperature, we examined various optimum conditions to obtain aluminum nitride sintered body with high thermal conductivity, A method for producing aluminum has been proposed.
The mechanism of the reaction during the sintering process in the method for producing aluminum nitride described in Japanese Patent Application Laid-Open No. 63-277573 is such that when the composite oxide on the outermost surface is removed by the reductive nitridation reaction, a concentration gradient of the composite oxide occurs. It becomes the driving force and the internal composite oxide moves to the surface.
An N sintered body is produced.

【0006】[0006]

【発明が解決しようとする課題】しかし、以上の特開昭
63-277573に記載された窒化アルミニウムの製造方法について
もさらに次のような問題がある。すなわち特開昭63-277
573に記載された窒化アルミニウムの製造方法によって得られ
る焼結体は、最表面と中心部では複合酸化物を形成する
焼結助剤の組成が異なり、均一な特性、特に均一な熱伝
導率を有する焼結体を得るためには還元窒素雰囲気中で
高温長時間の焼結が必要であり、それは工業的な生産過
程においては生産性の上からは非現実的な方法である。
特にこの特開昭63-277573に記載された窒化アルミニウムの製
造方法によっては、厚さのある大型AlN焼結体を工業的
な生産過程で厚さ方向に均一な高熱伝導率をもたせて生
産することはできない。
SUMMARY OF THE INVENTION
The method for producing aluminum nitride described in 63-277573 also has the following problem. That is, JP-A-63-277
The sintered body obtained by the method for producing aluminum nitride described in 573 has a different composition of the sintering aid forming the composite oxide at the outermost surface and the central portion, and has uniform characteristics, particularly uniform thermal conductivity. In order to obtain a sintered body, sintering at a high temperature for a long time in a reduced nitrogen atmosphere is necessary, which is an impractical method in terms of productivity in an industrial production process.
In particular, depending on the method of manufacturing aluminum nitride described in Japanese Patent Application Laid-Open No. 63-277573, a large-sized thick AlN sintered body is produced with uniform high thermal conductivity in the thickness direction in an industrial production process. It is not possible.

【0007】本発明は、以上の従来技術における問題に
鑑みてなされたものであり、熱伝導率に優れ、均一な特
性を持つ窒化アルミニウム焼結体を提供することを目的とす
る。
[0007] The present invention has been made in view of the above-mentioned problems in the prior art, and has as its object to provide an aluminum nitride sintered body having excellent thermal conductivity and uniform characteristics.

【0008】[0008]

【課題を解決するための手段】本発明者は本発明の目的
を達成するために窒化アルミニウム粉末に添加する焼結助剤、
焼結条件、焼結体組成、焼結体微細構造等と熱伝導率の
関係につき種々実験・検討を重ね、新たに発見された新
規事項に基づき本発明を創出するに至った。
In order to achieve the object of the present invention, the present inventor has added a sintering aid to aluminum nitride powder,
Various experiments and studies were conducted on the relationship between the sintering conditions, the sintered body composition, the sintered body microstructure, and the like, and the thermal conductivity, and the present invention was created based on newly discovered new matters.

【0009】すなわち、AlN粉末にアルカリ土類元素および/
または希土類元素を所定量添加し、有機系ハ゛インタ゛を加
え、更に、焼結過程で粒界の複合酸化物を還元する物質
としての炭素源、例えば炭素そのもの、あるいは非酸化
性雰囲気中、加熱処理により炭素を発生する有機系ハ゛イン
タ゛等を加え、それらをホ゛ールミル等を用いて粉砕、混合し、
スフ゜レート゛ライヤーなどにより造粒する。次いでその造粒粉を
所定の形状に成形した後、加熱してハ゛インタ゛中に含まれる
水素分や酸素分を除去する。つづいて、その成形体を焼
結炉内にセットし、窒素カ゛ス雰囲気中で焼結温度を1200〜19
00℃として第1段焼結を行いさらに、1800〜2200℃で1〜
5時間保持する第2段焼結を行う。この様にして作製され
たAlN焼結体の熱伝導率は均一で、かつその焼結体の熱
伝導率は170W/m・K以上となる。
That is, an alkaline earth element and / or
Alternatively, a predetermined amount of a rare earth element is added, an organic binder is added, and further, a carbon source as a substance for reducing a complex oxide at a grain boundary in a sintering process, for example, carbon itself, or a heat treatment in a non-oxidizing atmosphere, Add organic binders and the like that generate carbon, pulverize and mix them using a ball mill, etc.
Granulate with a flat layerer. Next, the granulated powder is formed into a predetermined shape, and then heated to remove hydrogen and oxygen contained in the binder. Subsequently, the compact is set in a sintering furnace, and the sintering temperature is set to 1200 to 19 in a nitrogen gas atmosphere.
Perform the first stage sintering at 00 ° C, and at 1800-2200 ° C,
Perform second-stage sintering for 5 hours. The thermal conductivity of the AlN sintered body thus manufactured is uniform, and the thermal conductivity of the sintered body is 170 W / m · K or more.

【0010】本発明はかかる新たな知見に基づきなされ
たものである。すなわち本発明の窒化アルミニウム焼結体の製
造方法は、窒化アルミニウムと炭素(C)および/または炭素含
有物と希土類および/またはアルカリ土類化合物とを混合
し、その混合粉を直径10mmの球体を少なくとも一部に包
含し得る幾何形状を外形として有する成形体に成形し、
液相生成温度以下の温度で第1段階の焼結を行い、さら
に液相生成温度以上の温度で第2段階の焼結を行うこと
を特徴とするものである。また本発明の窒化アルミニウム焼結
体の製造方法は、窒化アルミニウムと炭素(C)と希土類および
/またはアルカリ土類化合物とを成分とし、直径10mmの球体
を少なくとも一部に包含し得る幾何形状を外形として有
する被焼結体に液相生成温度以下の温度で第1段階の焼
結を行い、さらに液相生成温度以上の温度で第2段階の
焼結を行うことを特徴とするものである。
The present invention has been made based on such new findings. That is, the method for producing an aluminum nitride sintered body of the present invention comprises mixing aluminum nitride with carbon (C) and / or a carbon-containing material and a rare earth and / or alkaline earth compound, and forming a mixed powder into a sphere having a diameter of 10 mm. Molded into a molded article having a geometric shape that can be included at least in part as an outer shape,
The first stage sintering is performed at a temperature equal to or lower than the liquid phase generation temperature, and the second stage sintering is performed at a temperature equal to or higher than the liquid phase generation temperature. In addition, the method for producing an aluminum nitride sintered body of the present invention includes a geometrical shape containing aluminum nitride, carbon (C), a rare earth and / or an alkaline earth compound as components, and at least partially including a sphere having a diameter of 10 mm. The first stage sintering is performed on the object to be sintered having an outer shape at a temperature equal to or lower than the liquid phase generation temperature, and the second stage sintering is performed at a temperature equal to or higher than the liquid phase generation temperature. .

【0011】さらに本発明の窒化アルミニウム焼結体は、直径
10mmの球体を少なくとも一部に包含し得る3次元形状を
外形として有する窒化アルミニウム焼結体において、前記球体
の中心点に相当する位置の熱伝導率と前記球体の外部の
任意の点に相当する位置の熱伝導率との比が0.85以上で
あることを特徴とするものである。本発明において用い
られる窒化アルミニウム原料粉末は酸素を1.5重量%以下、実用
上は0.01〜1.0重量%含有するものとするのが好ましい。
またその平均粒径は焼結性、熱伝導性を考慮した場合、
0.5〜5μm程度であるのが好ましい。
Further, the aluminum nitride sintered body of the present invention has a diameter
In an aluminum nitride sintered body having a three-dimensional shape having an outer shape that can at least partially include a sphere of 10 mm, the thermal conductivity at a position corresponding to the center point of the sphere and an arbitrary point outside the sphere correspond to The ratio of the position to the thermal conductivity is 0.85 or more. The aluminum nitride raw material powder used in the present invention preferably contains 1.5% by weight or less of oxygen, and practically 0.01 to 1.0% by weight.
In addition, the average particle size, when considering the sinterability and thermal conductivity,
It is preferably about 0.5 to 5 μm.

【0012】本発明において焼結助剤として添加される
添加物は、希土類元素化合物および/またはアルカリ土類元
素化合物である。希土類元素およびアルカリ土類元素の化合
物としては、希土類元素およびアルカリ土類元素の酸化物、
窒化物、フッ化物、酸フッ化物、酸窒化物、焼成によりこれ
らの化合物となる物質が挙げられる。例えば、焼成によ
ってこれらの酸化物となる物質には希土類元素およびアル
カリ土類元素の炭酸塩、硝酸塩、シュウ酸塩、水酸化物等が
ある。また希土類および/またはアルカリ土類元素化合物の
添加量は、0.5〜15重量%とするのが良い。0.5重量%未満
では添加物の効果が充分に発揮されず、焼結体の緻密化
が不十分となり、AlN結晶中に酸素が固溶して高熱伝導
焼結体が得られない。一方、15重量%を超える場合は粒
界相が焼結体中に残存して、熱処理過程で除去される粒
界相の体積が大きくなるという問題が生じる。この希土
類および/またはアルカリ土類元素化合物の添加量は、好ま
しくは4.0〜12重量%とするのが良く、より好ましくは5
〜10重量%とするのが良い。
In the present invention, the additive added as a sintering aid is a rare earth element compound and / or an alkaline earth element compound. Compounds of rare earth elements and alkaline earth elements include oxides of rare earth elements and alkaline earth elements,
Examples include nitrides, fluorides, oxyfluorides, oxynitrides, and substances that become these compounds by firing. For example, substances that become these oxides by firing include carbonates, nitrates, oxalates, and hydroxides of rare earth elements and alkaline earth elements. The amount of the rare earth and / or alkaline earth element compound is preferably 0.5 to 15% by weight. If the content is less than 0.5% by weight, the effect of the additive is not sufficiently exerted, the densification of the sintered body becomes insufficient, and oxygen is dissolved in the AlN crystal to form a high heat conductive sintered body. On the other hand, when the content exceeds 15% by weight, a problem occurs that the grain boundary phase remains in the sintered body and the volume of the grain boundary phase removed in the heat treatment process increases. The amount of the rare earth and / or alkaline earth compound added is preferably 4.0 to 12% by weight, more preferably 5 to 12% by weight.
It is good to be ~ 10% by weight.

【0013】本発明においては混合粉中に、あるいは焼
結過程において複合酸化物の還元に炭素が寄与すること
ができるように、炭素を含有する物質を例えばハ゛インタ゛ー
として被焼結体に添加し焼結を行う。この炭素を添加す
る量はAlN原料粉中に存在する酸素量と最終的に目標と
する焼結体の熱伝導率により適宜調製することができ
る。例えば、原料粉末中に存在する酸素量が0.5〜1.5wt
%、目標とする熱伝導率が170〜200W/m・Kの場合、炭素含
有物質の添加量は炭素量に換算して0.5〜1.5wt%が適当
である。
In the present invention, a carbon-containing substance is added to the sintered body as a binder, for example, so that carbon can contribute to the reduction of the composite oxide in the mixed powder or in the sintering process. Perform a knot. The amount of carbon to be added can be appropriately adjusted depending on the amount of oxygen present in the AlN raw material powder and the ultimately desired thermal conductivity of the sintered body. For example, the amount of oxygen present in the raw material powder is 0.5 to 1.5 wt.
%, And when the target thermal conductivity is 170 to 200 W / m · K, the amount of the carbon-containing substance is suitably 0.5 to 1.5 wt% in terms of the amount of carbon.

【0014】本発明では焼結過程における焼成雰囲気
は、窒素カ゛スを含む非酸化性雰囲気とする。非酸化性雰
囲気は、CO2、H2カ゛スおよびC(カ゛スそして固相)などを、
一種または二種以上存在させることによって作ることが
できる。非酸化性雰囲気、特には還元性雰囲気としてCO
雰囲気とする場合には分圧として0.01×105〜1.5×105P
a程度生成するカ゛スを1200〜1900℃の焼結温度範囲におい
て用いるのがよい。かかるカーホ゛ンカ゛スは焼成中のAlNを還
元し、粒界相を焼結体中より除去することにより窒化アル
ミニウム焼結体をAlN単相化し、その結果として高熱伝導性
のAlN焼結体が得られる。このカーホ゛ンカ゛スにより除去され
る粒界相は(希土類元素)-Al-Oまたは/および(アルカリ土
類元素)-Al-O三元系化合物である。
In the present invention, the firing atmosphere in the sintering process is a non-oxidizing atmosphere containing nitrogen gas. Non-oxidizing atmosphere, such as CO 2 , H 2 gas and C (gas and solid phase),
It can be made by the presence of one or more. CO as a non-oxidizing atmosphere, especially a reducing atmosphere
In case of atmosphere, partial pressure 0.01 × 10 5 to 1.5 × 10 5 P
It is preferable to use a gas generated to a degree in the sintering temperature range of 1200 to 1900 ° C. Such a carbon case reduces the AlN during firing and removes the grain boundary phase from the sintered body to convert the aluminum nitride sintered body into an AlN single phase, thereby obtaining an AlN sintered body having high thermal conductivity. . The grain boundary phase removed by the carbon gas is a ternary compound of (rare earth element) -Al-O and / or (alkaline earth element) -Al-O.

【0015】本発明において焼結に用いる焼成容器はカー
ホ゛ン製容器とするのが最も簡便である。すなわち焼成用
容器としてはh-BN窒化アルミニウム、アルミナ、Mo製容器を用いる
こともできるが、本発明においては焼成中にカーホ゛ンカ゛ス雰
囲気を作り出す容器を用いることもでき、そのようにす
ることが本発明の目的からは好ましい。このカーホ゛ンカ゛ス雰
囲気を作り出す容器としては、容器全体がカーホ゛ン製の
物、容器全体がカーホ゛ン製で試料を設置する箇所にAlN板、
BN板、W板等を敷いた物、窒化アルミニウム製の容器で上部蓋
がカーホ゛ン製の物等を適用することができる。
In the present invention, the firing container used for sintering is most simply a container made of carbon. That is, a container made of h-BN aluminum nitride, alumina, or Mo can be used as the firing container, but in the present invention, a container that creates a carbon gas atmosphere during firing can also be used. Preferred for the purpose of the invention. As a container for creating the atmosphere of the carcass, an entire container is made of a car- phone, an entire container is made of a car- phone, and an AlN plate is provided at a place where a sample is placed.
An object in which a BN plate, a W plate, or the like is laid, an aluminum nitride container having an upper lid made of carbon, or the like can be used.

【0016】次に本発明における焼結時間および焼結温
度につき説明する。焼結時間および焼結温度は使用する
AlN原料粉末の粒径、酸素量および焼結助剤種により異
なる。
Next, the sintering time and the sintering temperature in the present invention will be described. Sintering time and sintering temperature use
It varies depending on the particle size of the AlN raw material powder, the amount of oxygen and the type of sintering aid.

【0017】本発明の窒化アルミニウムの製造方法の焼結過程
においては第1段焼結では1200〜1900℃で昇温速度を0.5
〜10.0℃/minとするのが良い。0.5℃/min未満では焼結
時間が長くなりすぎ、また10.0℃/minを越えると還元が
充分に行われないからである。この第1段階の焼結では
原料粉末表面の酸素が粒界相にトラッフ゜された後還元され
る作用が進行する。特に希土類元素化合物を焼結助剤と
して用いた場合には、最初から高温で焼結する場合には
(希土類元素)-N化合物が生成して焼結体中に残存し、
熱伝導率低下の原因となる。また、アルカリ土類元素化合物
を焼結助剤として用いた場合には、最初から高温で焼結
するとアルカリ土類元素が揮散する結果としてAlN成形体は
緻密化しない。
In the sintering process of the method for producing aluminum nitride according to the present invention, in the first stage sintering, the temperature is raised at a temperature of 1200 to 1900 ° C. and 0.5
It is good to be ~ 10.0 ° C / min. If it is less than 0.5 ° C./min, the sintering time becomes too long, and if it exceeds 10.0 ° C./min, the reduction is not performed sufficiently. In the first stage of sintering, oxygen on the surface of the raw material powder is trapped in the grain boundary phase and then reduced. In particular, when a rare earth element compound is used as a sintering aid, when sintering at a high temperature from the beginning, a (rare earth element) -N compound is generated and remains in the sintered body,
This causes a decrease in thermal conductivity. Further, when an alkaline earth element compound is used as a sintering aid, if the sintering is carried out at a high temperature from the beginning, the alkaline earth element is volatilized, so that the AlN compact is not densified.

【0018】次に第2段階焼結では第1段階より高温の18
00〜2100℃で0.5時間以上、好ましくは2時間以上焼結す
るのが良い。焼結時間が0.5時間未満では緻密化、粒界
相除去および粒成長による高熱伝導率化が充分進行せ
ず、高熱伝導率のAlN焼結体を得ることはできない。
Next, in the second stage sintering, 18
Sintering at 00 to 2100 ° C for 0.5 hour or more, preferably 2 hours or more is good. If the sintering time is less than 0.5 hours, densification, removal of the grain boundary phase, and high thermal conductivity due to grain growth do not sufficiently proceed, and an AlN sintered body with high thermal conductivity cannot be obtained.

【0019】以上の本発明の窒化アルミニウム焼結体の製造方
法により得られたAlN焼結体の特性及び組織について測
定・分析した結果、多結晶体としては非常に高い170w
/mK以上の熱伝導率構成相はAlN結晶粒のみあるいはAl
N結晶粒と希土類およびアルカリ土類酸化物であり、他の相
は観察されない。ことが判明した。本発明の製造方法に
より得られる窒化アルミニウム焼結体の最終的な不純物酸素は
2.0wt%以下とするのが好ましい。それを超えて不純物酸
素が含有される場合には、均一な熱伝導率向上という本
発明の目的に対する悪影響が生じる。
As a result of measuring and analyzing the characteristics and the structure of the AlN sintered body obtained by the above-described method for manufacturing an aluminum nitride sintered body of the present invention, it was found that the AlN sintered body had a very high 170 watts as a polycrystal.
/ mK or higher thermal conductivity component phase is only AlN grains or Al
N grains and rare earth and alkaline earth oxides, no other phases are observed. It has been found. The final impurity oxygen of the aluminum nitride sintered body obtained by the production method of the present invention is
Preferably, the content is 2.0 wt% or less. If the impurity oxygen is contained in excess of that, the adverse effect on the object of the present invention, that is, the uniform improvement of the thermal conductivity occurs.

【0020】[0020]

【作用】次に本発明の窒化アルミニウムの製造方法により得ら
れる窒化アルミニウム焼結体につき均一な高熱伝導率の達成さ
れる要因につき説明する。本発明によれば希土類および
/またはアルカリ土類元素化合物を焼結助剤として添加する
ことによって、不純物酸素が(希土類元素)-Al-Oおよ
び/または(アルカリ土類元素)-Al-O系化合物等の形でAlN
結晶粒界に固定され、AlN格子中への酸素の固溶が防止
される結果として、Alの酸窒化物(AlON)、AlNのホ゜リタイフ
゜(27R型)の生成を防止される。この様に低熱伝導率化の
原因が抑制されることが高熱伝導率化の一因となる。
Next, a description will be given of factors that achieve a uniform high thermal conductivity in the aluminum nitride sintered body obtained by the method for producing aluminum nitride of the present invention. According to the present invention, by adding a rare earth and / or alkaline earth element compound as a sintering aid, impurity oxygen can be reduced to (rare earth element) -Al-O and / or (alkaline earth element) -Al-O system. AlN in the form of compounds, etc.
As a result of being fixed at the grain boundaries and preventing solid solution of oxygen in the AlN lattice, formation of Al oxynitride (AlON) and AlN polytype (27R type) is prevented. Suppressing the cause of the low thermal conductivity in this way contributes to the high thermal conductivity.

【0021】また、第1段階目の焼結過程の初期に、例
えば希土類元素としてYを選んだ場合3Y2O3、Al2O3、Y2O
3・Al2O3、2Y2O3・Al2O3、Y2O5等の化合物が、アルカリ土類元
素としてCaを選んだ場合、1CaO・6Al2O3、1CaO・2Al2O3
1CaO・1Al2O3、CaOなどの化合物が生成する。次いでそれ
以降の焼結過程で、被焼結体に均一に分散する炭素(C)
が被焼結体全域に渡り粒界相を均一に還元し、粒界相が
徐々に除去される。その結果、粒界相は焼結体の系外へ
と移動し、焼結体はAlN単相となると共に均一に熱伝導
率が上昇する。すなわち、被焼結体の外側の雰囲気がカー
ホ゛ン雰囲気として寄与して最表面の複合酸化物が還元窒
化反応により除去され複合酸化物の濃度勾配が生じ、そ
れが駆動力となり、内部の複合酸化物が表面へ移動する
という従来の窒化アルミニウムの製造方法のメカニス゛ムとは異な
り、本発明では特に焼結前に被焼結体に炭素(C)が均一
に分散・混合され、被焼結体の内部も含め、被焼結体全
体として複合酸化物の還元窒化反応がほぼ均一に進行す
るので、焼結体全体として均一に高い熱伝導率が達成さ
れる。またそのため長時間の焼成は必要なく、比較的短
時間でも焼結体のAlN粒子が成長し、熱抵抗となる粒界
数が減少し、工業的に適用可能な短時間の処理で窒化アル
ミニウムの熱伝導率を均一に向上させることができる。
In the early stage of the first sintering process, for example, when Y is selected as a rare earth element, 3Y 2 O 3 , Al 2 O 3 , Y 2 O
3 · Al 2 O 3, 2Y 2 O 3 · Al 2 O 3, Y 2 O compounds such as 5, when you choose Ca as an alkaline earth element, 1CaO · 6Al 2 O 3, 1CaO · 2Al 2 O 3 ,
1CaO · 1Al 2 O 3, compounds such as CaO is produced. Next, in the subsequent sintering process, carbon (C) that is uniformly dispersed in the sintered body
Reduces the grain boundary phase uniformly throughout the sintered body, and the grain boundary phase is gradually removed. As a result, the grain boundary phase moves out of the system of the sintered body, and the sintered body becomes an AlN single phase and the thermal conductivity uniformly increases. That is, the atmosphere outside the sintered body contributes as a carbon dioxide atmosphere, and the outermost composite oxide is removed by the reductive nitridation reaction, and a concentration gradient of the composite oxide is generated. Unlike the conventional mechanical method of manufacturing aluminum nitride, which moves to the surface, in the present invention, carbon (C) is uniformly dispersed and mixed in the sintered body, particularly before sintering, and the inside of the sintered body is Since the reductive nitridation reaction of the composite oxide proceeds substantially uniformly in the entire sintered body including the sintered body, a uniform high thermal conductivity is achieved in the entire sintered body. Also, calcination for a long time is not necessary, and AlN particles of the sintered body grow even in a relatively short time, the number of grain boundaries that become a thermal resistance decreases, and aluminum nitride can be treated in a short time that is industrially applicable. Thermal conductivity can be improved uniformly.

【0022】[0022]

【実施例】次に実施例並びに比較例によって本発明を具
体的に説明する。
Next, the present invention will be described specifically with reference to examples and comparative examples.

【0023】実施例1 不純物としての酸素を1.2重量%含有し、平均粒径が0.5
μmの窒化アルミニウム粉末に焼結助剤として、 酸化イットリウム(Y
2O3)5.7重量%添加し、さらにカーホ゛ン粉末0.6重量%を添加
した。この混合粉末をホ゛ールミルで混合、造粒した後、フ゜レス
成形(1000kg/cm2)することによって100×100×15mmの直
方形状の圧粉体に成形した。この成形体は図1に示すよ
うに直径10mmの球体1を少なくとも一部に包含し得る幾
何形状を外形として有する成形体2である。さらにこの
成形体2からハ゛インタ゛ーを除去して得た被焼結体をBN製容器
に収容し、次の条件で常圧焼結した。 (1)焼結温度・昇温速度・焼結時間 (2)焼結雰囲気 窒素カ゛ス−1気圧中 以上の焼結により最終的な炭素量を0.02wt%、酸素量を
1.5wt%まで減少した焼結体を得た。得られた焼結体を分
析し、炭素含有量、酸素含有量、熱伝導率を測定した。
熱伝導率測定にあったっては前記球体1の中心点に相当
する位置Aの熱伝導率と前記球体1の外部の任意の点に相
当する位置Bの熱伝導率とを測定し、その比を求めた。
以上の結果を表1に示す。また、球体1の焼結体における
中心からの距離と熱伝導率との関係を図4に示す。
Example 1 Oxygen as an impurity was contained in an amount of 1.2% by weight, and the average particle diameter was 0.5%.
Yttrium oxide (Y
2 O 3 ) 5.7% by weight, and further 0.6% by weight of carbon powder were added. This mixed powder was mixed and granulated by a ball mill, and then formed into a rectangular compact of 100 × 100 × 15 mm by press molding (1000 kg / cm 2). As shown in FIG. 1, this molded body is a molded body 2 having, as an outer shape, a geometrical shape capable of at least partially including a sphere 1 having a diameter of 10 mm. Further, the sintered body obtained by removing the binder from the molded body 2 was accommodated in a BN container, and sintered under normal pressure under the following conditions. (1) Sintering temperature, heating rate, sintering time (2) Sintering atmosphere Nitrogen gas-1 atm By sintering above, the final carbon content is reduced to 0.02 wt% and oxygen content is reduced to
A sintered body reduced to 1.5 wt% was obtained. The obtained sintered body was analyzed, and the carbon content, the oxygen content, and the thermal conductivity were measured.
In the thermal conductivity measurement, the thermal conductivity at a position A corresponding to the center point of the sphere 1 and the thermal conductivity at a position B corresponding to an arbitrary point outside the sphere 1 are measured, and the ratio is determined. I asked.
Table 1 shows the above results. FIG. 4 shows the relationship between the distance from the center of the sintered body of the sphere 1 and the thermal conductivity.

【0024】実施例2 焼結助剤として 酸化シ゛スフ゜ロシウム(Dy2O3)7.0重量%(シ゛スフ゜
ロシウム元素の重量換算)を添加した他は実施例1と同様に
して焼結体を得、実施例1と同様にして焼結体の特性を
評価した。その結果を表1に示す。また、球体1の中心か
らの距離と熱伝導率との関係を図5に示す。
Example 2 A sintered body was obtained in the same manner as in Example 1 except that 7.0% by weight of calcium sprosium oxide (Dy 2 O 3 ) (in terms of the weight of calcium spherurosium) was added as a sintering aid. The characteristics of the sintered body were evaluated in the same manner as described above. The results are shown in Table 1. FIG. 5 shows the relationship between the distance from the center of the sphere 1 and the thermal conductivity.

【0025】実施例3 第1段階焼結における昇温速度を3℃/minとした他は実施
例1と同様にして焼結体を得、実施例1と同様にして焼結
体の特性を評価した。その結果を表1に示す。
Example 3 A sintered body was obtained in the same manner as in Example 1 except that the heating rate in the first stage sintering was set at 3 ° C./min. evaluated. The results are shown in Table 1.

【0026】実施例4 第1段階焼結の昇温速度を5℃/minとし、最終の炭素量を
0.03wt%、酸素量を1.7wt%とした他は実施例1と同様にし
て焼結体を製造した。その焼結体につき実施例1と同様
にして特性を評価した。その結果を表1に示す。
Example 4 The temperature rise rate of the first stage sintering was 5 ° C./min, and the final carbon amount was
A sintered body was manufactured in the same manner as in Example 1 except that 0.03 wt% and the amount of oxygen were 1.7 wt%. The characteristics of the sintered body were evaluated in the same manner as in Example 1. The results are shown in Table 1.

【0027】実施例5 第1段階焼結の焼結温度範囲を1200〜1500℃、昇温速度
を0.5℃/minとした他は実施例1と同様にして焼結体を製
造した。その焼結体につき実施例1と同様にして特性を
評価した。その結果を表1に示す。
Example 5 A sintered body was manufactured in the same manner as in Example 1 except that the sintering temperature range of the first stage sintering was 1200 to 1500 ° C., and the heating rate was 0.5 ° C./min. The characteristics of the sintered body were evaluated in the same manner as in Example 1. The results are shown in Table 1.

【0028】実施例6 焼結助剤としてScを添加し、他は実施例1と同様にして
焼結体を製造した。その焼結体につき実施例1と同様に
して特性を評価した。その結果を表1に示す。
Example 6 A sintered body was produced in the same manner as in Example 1 except that Sc was added as a sintering aid. The characteristics of the sintered body were evaluated in the same manner as in Example 1. The results are shown in Table 1.

【0029】実施例7 焼結助剤としてSrを添加し、他は実施例1と同様にして
焼結体を製造した。その焼結体につき実施例1と同様に
して特性を評価した。その結果を表1に示す。
Example 7 A sintered body was produced in the same manner as in Example 1 except that Sr was added as a sintering aid. The characteristics of the sintered body were evaluated in the same manner as in Example 1. The results are shown in Table 1.

【0030】実施例 8 焼結助剤としてCaを添加し、他は実施例1と同様にして
焼結体を製造した。その焼結体につき実施例1と同様に
して特性を評価した。その結果を表1に示す。
Example 8 A sintered body was produced in the same manner as in Example 1 except that Ca was added as a sintering aid. The characteristics of the sintered body were evaluated in the same manner as in Example 1. The results are shown in Table 1.

【0031】実施例 9 焼結助剤としてCeを添加し、他は実施例1と同様にして
焼結体を製造した。その焼結体につき実施例1と同様に
して特性を評価した。その結果を表1に示す。
Example 9 A sintered body was produced in the same manner as in Example 1 except that Ce was added as a sintering aid. The characteristics of the sintered body were evaluated in the same manner as in Example 1. The results are shown in Table 1.

【0032】実施例 10 焼結助剤としてBaを添加し、他は実施例1と同様にして
焼結体を製造した。その焼結体につき実施例1と同様に
して特性を評価した。その結果を表1に示す。
Example 10 A sintered body was produced in the same manner as in Example 1 except that Ba was added as a sintering aid. The characteristics of the sintered body were evaluated in the same manner as in Example 1. The results are shown in Table 1.

【0033】実施例 11 焼結助剤としてErを添加し、他は実施例1と同様にして
焼結体を製造した。その焼結体につき実施例1と同様に
して特性を評価した。その結果を表1に示す。
Example 11 A sintered body was manufactured in the same manner as in Example 1 except that Er was added as a sintering aid. The characteristics of the sintered body were evaluated in the same manner as in Example 1. The results are shown in Table 1.

【0034】実施例 12 図2に示されるように、直径10mmの球体1を少なくとも一
部に包含し得る幾何形状を外形として有する成形体とし
て20×20×20mmの成形体3を形成して焼結した他は実施
例1と同様にして焼結体を製造した。その焼結体につき
実施例1と同様にして特性を評価した。その結果を表1に
示す。
Example 12 As shown in FIG. 2, a molded body 3 of 20 × 20 × 20 mm was formed as a molded body having a geometrical shape capable of at least partially including a sphere 1 having a diameter of 10 mm. A sintered body was manufactured in the same manner as in Example 1 except for tying. The characteristics of the sintered body were evaluated in the same manner as in Example 1. The results are shown in Table 1.

【0035】実施例 13 不純物としての酸素を1.2重量%含有し、平均粒径が0.5
μmの窒化アルミニウム粉末に焼結助剤として、 酸化シ゛スフ゜ロシウ
ム(Dy2O3)5.7重量%添加(シ゛スフ゜ロシウム元素の重量換算)し
た。この混合粉末をホ゛ールミルで混合、造粒した後、成形し
た。成形にあたっては炭素含有有機樹脂系ハ゛インタ゛ーを炭
素分量に換算して0.8重量%添加して造粒し、さらにフ゜レス
成形(1000kg/cm2)することによって図1に示される100×
100×15mmの直方形状の圧粉体2に成形した。さらにこの
成形体から炭素以外のハ゛インタ゛ーをN2中にて除去して得た
被焼結体をカーホ゛ン製容器に収容し、次の条件で常圧焼結
した。 (1)焼結温度・昇温速度・焼結時間 第1段階焼結−1200から1800℃(液相生成温度以下) 昇温速度1℃/min 第2段階焼結−1950℃(液相生成温度以上)の温度1h (2)焼結雰囲気 COカ゛ス 分圧−0.2×105Pa中 窒素カ゛ス 分圧−1.8×105Pa中 以上の焼結により最終的な炭素量を0.03wt%、酸素量を
1.6wt%まで減少した焼結体を得た。得られた焼結体を分
析し、酸素含有量、密度、粒径、熱伝導率を測定した。
Example 13 Oxygen as an impurity was contained in an amount of 1.2% by weight, and the average particle size was 0.5%.
As a sintering aid, 5.7% by weight of disulfide (Dy 2 O 3 ) was added to the aluminum nitride powder of μm (in terms of the weight of disulfide). This mixed powder was mixed and granulated by a ball mill, and then molded. In molding, the carbon-containing organic resin-based binder was converted to a carbon content of 0.8% by weight, granulated, and further subjected to pressure molding (1000 kg / cm2) to obtain 100 × as shown in FIG.
It was formed into a green compact 2 having a rectangular shape of 100 × 15 mm. Further, the sintered body obtained by removing the binder other than carbon from the molded body in N 2 was accommodated in a container made of carbon dioxide and sintered under normal pressure under the following conditions. (1) Sintering temperature, heating rate, sintering time First stage sintering -1200 to 1800 ° C (less than liquid phase forming temperature) Heating rate 1 ° C / min Second stage sintering-1950 ° C (liquid phase forming (More than temperature) 1h (2) Sintering atmosphere CO gas Partial pressure -0.2 × 10 5 Pa Nitrogen gas Partial pressure -1.8 × 10 5 Pa Sintering above results in a final carbon content of 0.03 wt%, oxygen The amount
A sintered body reduced to 1.6 wt% was obtained. The obtained sintered body was analyzed, and the oxygen content, density, particle size, and thermal conductivity were measured.

【0036】比較例1 他は実施例1と同様にして、カーホ゛ン無添加の造粒粉により
作製した成形体をカーホ゛ン製容器からなる還元雰囲気中で
焼結した。得られた焼結体につき実施例1と同様にして
特性を調査した結果を表1に示す。また、球体1の焼結体
の中心からの距離と熱伝導率との関係を図4に示す。
COMPARATIVE EXAMPLE 1 In the same manner as in Example 1 except for the above, a green body produced from granulated powder without carbon was sintered in a reducing atmosphere consisting of a container made of carbon. Table 1 shows the results of investigating the characteristics of the obtained sintered body in the same manner as in Example 1. FIG. 4 shows the relationship between the distance from the center of the sintered body of the sphere 1 and the thermal conductivity.

【0037】比較例2 他は実施例2と同様にして、カーホ゛ン無添加の造粒粉により
作製した成形体を還元雰囲気中で焼結した。得られた焼
結体につき実施例2と同様にして特性を調査した結果を
表1に示す。また、球体1の中心からの距離と熱伝導率と
の関係を図5に示す。
COMPARATIVE EXAMPLE 2 In the same manner as in Example 2 except for the above, a compact produced from granulated powder without carbon was sintered in a reducing atmosphere. Table 1 shows the results obtained by examining the characteristics of the obtained sintered body in the same manner as in Example 2. FIG. 5 shows the relationship between the distance from the center of the sphere 1 and the thermal conductivity.

【0038】比較例3 特に第1段階焼結過程と第2段焼結過程として段階分けす
ることなく焼結温度範囲を0〜2000℃とすると共に、昇
温速度を5℃/minとして1段階で焼結した他は実施例1と
同様にして窒化アルミニウム焼結体を製造した。得られた焼結
体につき実施例1と同様にして特性を調査した結果を表1
に示す。
Comparative Example 3 In particular, the sintering temperature range was set to 0 to 2000 ° C. and the temperature was raised at a rate of 5 ° C./min. An aluminum nitride sintered body was manufactured in the same manner as in Example 1 except that the sintering was carried out. Table 1 shows the results of investigating the characteristics of the obtained sintered body in the same manner as in Example 1.
Shown in

【0039】[0039]

【表1】[Table 1]

【0040】 以上の各実施例および比較例により得られ
た焼結体の特性を示す表1からわかるように、実施例の
焼結体はいずれも熱伝導率が170以上であり、特に図1、
図2に示される前記球体の中心点に相当する位置Aの熱
伝導率と前記球体の外部の任意の点に相当する位置Bの
熱伝導率との比が0.85以上であることが確認される。一
方、比較例1、2、3の焼結体は図1、図2に示される前記
球体の中心点に相当する位置Aの熱伝導率と前記球体の
外部の任意の点に相当する位置Bの熱伝導率との比が0.
85未満であり、焼結体各部における熱伝導率が不均一で
あることが確認される。この点については特に図4、5に
示されるように実施例1および実施例2の焼結体では前記
球体1の中心部からの距離が大きくなっても熱伝導率は
ほぼ均一に高い数値を示すのに対し、比較例1、2の焼結
体では球体1の中心部における熱伝導率が低く、中心部
からの距離が大きくなるに従い、熱伝導率が増加する傾
向を示し、焼結体の中心部と外側部とでは熱伝導率が不
均一であり、特に中心部の熱伝導率が低いことがわか
る。また、カーホ゛ン無添加であっても、直径10mmの球体を
内部に包含し得ない幾何形状を外形として有する焼結体
は、その内部の熱伝導率と外部の熱伝導率との比が0.85
以上であり、本発明の窒化アルミニウム焼結体の製造方法は特
に直径10mmの球体を内部に包含し得る幾何形状を外形と
して有する大型焼結体を得る方法として有効であること
がわかる。
As can be seen from Table 1 showing the characteristics of the sintered bodies obtained in each of the above Examples and Comparative Examples, the sintered bodies of the Examples all had a thermal conductivity of 170 or more, and in particular, FIG. ,
It is confirmed that the ratio between the thermal conductivity at the position A corresponding to the center point of the sphere shown in FIG. 2 and the thermal conductivity at the position B corresponding to an arbitrary point outside the sphere is 0.85 or more. . On the other hand, the sintered bodies of Comparative Examples 1, 2, and 3 have the thermal conductivity at the position A corresponding to the center point of the sphere and the position B corresponding to an arbitrary point outside the sphere shown in FIGS. The ratio with the thermal conductivity of 0.
It is less than 85, and it is confirmed that the thermal conductivity in each part of the sintered body is not uniform. Regarding this point, particularly in the sintered bodies of Examples 1 and 2 as shown in FIGS. 4 and 5, even when the distance from the center of the sphere 1 increases, the thermal conductivity shows a substantially uniform high value. On the other hand, in the sintered bodies of Comparative Examples 1 and 2, the thermal conductivity at the center of the sphere 1 was low, and as the distance from the center increased, the thermal conductivity tended to increase. It can be seen that the thermal conductivity is not uniform between the central portion and the outer portion, and the thermal conductivity is particularly low at the central portion. Further, even without the addition of carbon, a sintered body having a geometrical shape in which a sphere having a diameter of 10 mm cannot be contained inside has a ratio of the internal thermal conductivity to the external thermal conductivity of 0.85.
From the above, it can be seen that the method for producing an aluminum nitride sintered body of the present invention is particularly effective as a method for obtaining a large-sized sintered body having a geometric shape capable of containing a sphere having a diameter of 10 mm inside.

【0041】[0041]

【発明の効果】以上説明したように、本発明の窒化アルミニ
ウム焼結体の製造方法によれば、特性が均一で、かつ高熱
伝導性のAlNが得られる。また本発明の窒化アルミニウム焼結
体によれば、直径10mmの球体を少なくとも一部に包含し
得る3次元形状を外形として有する大型窒化アルミニウム焼結
体の前記球体の中心点に相当する位置の熱伝導率と前記
球体の外部の任意の点に相当する位置の熱伝導率との比
が0.85以上であることから、強い放熱機能を発揮すると
共に、かかる大型焼結体を切断して使用に供した場合
も、個々の切断片につき熱伝導率等の特性の不均一とい
う問題が生じないという極めて優れた効果が奏される。
As described above, according to the method for producing an aluminum nitride sintered body of the present invention, AlN having uniform properties and high thermal conductivity can be obtained. Further, according to the aluminum nitride sintered body of the present invention, the heat of a large aluminum nitride sintered body having a three-dimensional shape having an outer shape that can at least partially include a sphere having a diameter of 10 mm corresponds to the central point of the sphere. Since the ratio between the conductivity and the thermal conductivity at a position corresponding to an arbitrary point outside the sphere is 0.85 or more, a strong heat dissipation function is exhibited, and the large sintered body is cut for use. Also in this case, an extremely excellent effect that the problem of non-uniformity in characteristics such as thermal conductivity of individual cut pieces does not occur is exhibited.

【図面の簡単な説明】[Brief description of the drawings]

【図1】 本発明の一実施例の焼結体の形態を示す斜視
図である。
FIG. 1 is a perspective view showing a form of a sintered body according to one embodiment of the present invention.

【図2】 本発明の他の実施例の焼結体の形態を示す斜
視図である。
FIG. 2 is a perspective view showing a form of a sintered body according to another embodiment of the present invention.

【図3】 本発明の実施例1の焼結体と比較例1の焼結体
とで熱伝導率の均一性を対比して示す図である。
FIG. 3 is a view showing the thermal conductivity uniformity of the sintered body of Example 1 of the present invention and the sintered body of Comparative Example 1 in comparison.

【図4】 本発明の実施例2の焼結体と比較例2の焼結
体とで熱伝導率の均一性を対比して示す図である。
FIG. 4 is a diagram showing the uniformity of thermal conductivity of the sintered body of Example 2 of the present invention and the sintered body of Comparative Example 2 in comparison.

【符号の説明】 A 球体中心点 B 球体の外部の任意の点に相当する位置 1 球体 2,3 成形体 [Explanation of symbols] A spherical center point B position corresponding to an arbitrary point outside the spherical body 1 spherical body 2, 3 molded body

───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7,DB名) C04B 35/581 - 35/5835 C04B 35/64 ──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int.Cl. 7 , DB name) C04B 35/581-35/5835 C04B 35/64

Claims (5)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 窒化アルミニウムと炭素(C)および/
または炭素含有物と希土類および/またはアルカリ土類
化合物とを混合し、その混合粉を成形体として直径10
mmの球体を内包する外形に成形し、液相生成温度以下
の温度で第1段階の焼結を行い、さらに液相生成温度以
上の温度で第2段階の焼結を行うことを特徴とする窒化
アルミニウム焼結体の製造方法。
An aluminum nitride and carbon (C) and / or
Alternatively, a carbon-containing material is mixed with a rare earth and / or alkaline earth compound, and the mixed powder is formed into a molded product having a diameter of 10%.
It is characterized in that it is formed into an outer shape containing a sphere of mm, and the first stage of sintering is performed at a temperature equal to or lower than the liquid phase generation temperature, and the second stage is sintered at a temperature equal to or higher than the liquid phase generation temperature. A method for producing an aluminum nitride sintered body.
【請求項2】 直径10mmの球体を内包する外形であ
窒化アルミニウム焼結体において、任意焼結体断面の
任意位置の熱伝導率比が任意二点間において0.85以
上であることを特徴とする窒化アルミニウム焼結体。
2. An outer shape containing a sphere having a diameter of 10 mm.
That the aluminum nitride sintered body, any sintered body section
An aluminum nitride sintered body characterized in that a thermal conductivity ratio at an arbitrary position is 0.85 or more between two arbitrary points .
【請求項3】 熱伝導率が170w/m・k以上である
請求項に記載した窒化アルミニウム焼結体。
3. The aluminum nitride sintered body according to claim 2 , having a thermal conductivity of 170 w / m · k or more.
【請求項4】 焼結を非酸化性雰囲気中で行う請求項1
に記載した窒化アルミニウム焼結体の製造方法。
4. The method according to claim 1, wherein the sintering is performed in a non-oxidizing atmosphere.
3. The method for producing an aluminum nitride sintered body described in 1. above.
【請求項5】 第1段階の焼結温度を1200〜190
0℃とすると共に、第2段階の焼結温度を1800〜2
100℃とする請求項1に記載した窒化アルミニウム焼
結体の製造方法。
5. The sintering temperature in the first stage is set at 1200 to 190.
0 ° C. and the sintering temperature of the second stage is 1800-2
The method for producing an aluminum nitride sintered body according to claim 1, wherein the temperature is set to 100 ° C.
JP04081628A 1992-03-03 1992-03-03 Aluminum nitride sintered body and method for producing the same Expired - Lifetime JP3141505B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP04081628A JP3141505B2 (en) 1992-03-03 1992-03-03 Aluminum nitride sintered body and method for producing the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP04081628A JP3141505B2 (en) 1992-03-03 1992-03-03 Aluminum nitride sintered body and method for producing the same

Publications (2)

Publication Number Publication Date
JPH0912370A JPH0912370A (en) 1997-01-14
JP3141505B2 true JP3141505B2 (en) 2001-03-05

Family

ID=13751602

Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

Country Link
JP (1) JP3141505B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2703564C1 (en) * 2018-09-18 2019-10-21 Общество с ограниченной ответственностью "Научно-производственное предприятие "НАНОЭЛЕКТРО" Composite contact wire

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4812144B2 (en) 1998-07-22 2011-11-09 住友電気工業株式会社 Aluminum nitride sintered body and manufacturing method thereof
JP5031147B2 (en) * 2001-03-29 2012-09-19 電気化学工業株式会社 Method for producing aluminum nitride sintered body

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2703564C1 (en) * 2018-09-18 2019-10-21 Общество с ограниченной ответственностью "Научно-производственное предприятие "НАНОЭЛЕКТРО" Composite contact wire

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