JPH058142B2 - - Google Patents
Info
- Publication number
- JPH058142B2 JPH058142B2 JP61122682A JP12268286A JPH058142B2 JP H058142 B2 JPH058142 B2 JP H058142B2 JP 61122682 A JP61122682 A JP 61122682A JP 12268286 A JP12268286 A JP 12268286A JP H058142 B2 JPH058142 B2 JP H058142B2
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- aluminum nitride
- aln
- sintering
- alkali metal
- Prior art date
- Legal status (The legal status 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 status listed.)
- Expired - Lifetime
Links
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 31
- 238000005245 sintering Methods 0.000 claims description 17
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000012752 auxiliary agent Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- 241000286819 Malo Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001341 alkaline earth metal compounds Chemical class 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- FZFYOUJTOSBFPQ-UHFFFAOYSA-M dipotassium;hydroxide Chemical compound [OH-].[K+].[K+] FZFYOUJTOSBFPQ-UHFFFAOYSA-M 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary 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
- C01B21/072—Binary 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
- C01B21/0722—Preparation by direct nitridation of aluminium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Products (AREA)
Description
［産業上の利用分野］
本発明は新規な窒化アルミニウム焼結体の製造
方法に関するものである。
［従来の技術］
窒化アルミニウム（AlN）は高熱伝導性、高
電気絶縁性を有するため、近年IC、LSI等の放熱
基板材料として注目されている一方、室温から高
温までの強度が大きく、化学的安定性にも優れて
いるため種々の材料としても有望視されている。
とろこで、AlNをはじめ非酸化物は一般に難
焼結性物質で、AlN単独組成では1700〜2000℃
でホツトプレスするといつた高温高圧条件が緻密
化には必要である。しかし、ホツトプレス法では
形状の制御が難しい上、生産性が低くコスト高に
なるといつた問題がある。
そこで最近は焼結助剤を用いて常圧焼結法によ
り緻密な焼結体を得るための研究が盛んに行なわ
れている。今日では、焼結助剤としてアルカリ土
類金属化合物およびイツトリウムのような希土類
元素の化合物が主に用いられている。
［発明が解決しようとする問題点］
高熱伝導性を始めとする窒化アルミニウムの特
性は不純物の存在により著しく劣化する。特に原
料のAlN粉末表面はAl2O3で覆われており、これ
が焼結中に酸窒化物となり特性劣化の原因となつ
ている。今日、焼結性を向上させるためにAlN
の微粉末化が行なわれているが、微粉化すること
により逆にAl2O3の量が増すといつた結果にな
る。従つて、特性の良いAlN焼結体を得ようと
するためには焼結体中の酸素量を極力少なくして
やる必要がある。
前記の焼結助剤は焼結を促進させる効果ととも
に、焼結中にAlN粉末中の酸素を除去する効果
をもねらつたものである。例えば、酸化イツトリ
ウム（Y2O3）を助剤として加えた場合、焼結中
に酸化アルミニウム（Al2O3）と反応しAlNの粒
界にイツトリウムアルミニウムガーネツト
（YAG）相を形成することによつてAlN内への酸
素の混入を防いでいる。
しかし、前記のような焼結助剤を用いた場合、
特性が著しく向上するものは数少ない。具体的に
熱伝導率の値をとつてみると無添加の場合、40〜
50W／ｍ・Ｋに対し、助剤を添加しても50〜
50W／ｍ・Ｋ程度である。これは、添加した助剤
が何らかの形で焼結体中に残存し、熱伝導を阻害
していると考えられる。特に希土類等の原子量の
大きな元素が残存する場合に熱伝導率は低下する
ことは1973年発行のジヤーナル・オブ・ケミスト
リ・オブ・ソリツド誌、第34巻、第321ページ
（J.Phys.Chem.Solids、34、321（1973））に所載の
論文中に記述されている。
さらに、焼結助剤を添加する際、AlN粉末の
粒径より助剤の粒径が大きいと両者の混合、分散
状態が悪くなり、密度低下等による特性劣化が生
ずる。
本発明の目的は、このような従来の欠点を除去
せしめて高性能の窒化アルミニウム焼結体の製造
方法を提供することにある。
［問題点を解決するための手段］
本発明は窒化アルミニウム粉末にアルカリ金属
酸化物の１種もしくは２種以上を0.5〜10wt％添
加したセラミツク混合物を成形後、真空中若しく
は非酸化性雰囲気中、1600〜2000℃で焼結するこ
とを特徴とする窒化アルミニウム焼結体の製造方
法である。
本発明において焼結助剤として用いられるアル
カリ金属酸化物は焼結中にAlN粉末中に存在す
るAl2O3と反応し、MAlO2なる複酸化物を生じ
る。このためAlN内に酸素が残らず特性の良い
AlN焼結体が得られる。
また、たとえアルカリ金属酸化物が焼結体中に
残存しても原子量が小さいため、熱伝導性への影
響が少なく高性能の焼結体を得ることができる。
このようなアルカリ金属酸化物としてはたとえば
酸化ナトリウム（Na2O）、酸化カリウム（K2O）
が好ましく、これらの化合物の１種または２種以
上を混合したものを0.5〜10wt％用いる。
本発明では上記のアルカリ金属酸化物の粒径を
主成分であるAlN粉末の粒径と同じかあるいは
それよりも小さくすると、AlNの焼結が阻害さ
れず緻密で高性能の窒化アルミニウム焼結体を製
造することができる。ここでアルカリ金属酸化物
の粒径としては通常0.01〜3μｍのものが用いられ
る。
［実施例］
次に本発明の実施例について説明する。
実施例 １
平均粒径3μｍ、酸素量2wt％のAlN粉末に平均
粒径2μｍのK2O3wt％を加え、エタノール中でホ
ジナイザーにより混合、成形した後、窒素雰囲気
中1800℃で３時間常圧焼結を行なつた。得られた
窒化アルミニウム焼結体の密度は3.23ｇ／cm3、熱
伝導率は72W／ｍ・Ｋであつた。
実施例 ２〜９
実施例１と同じAlN粉末に平均粒径2μｍの
Na2Oを第１表に示した量だけ加えてエタノール
中ホモジナイザーで混合し、成形後第１表に示し
た焼結条件で焼結してAlN焼結体を製造した。
その結果を第１表に示す。
[Industrial Application Field] The present invention relates to a novel method for producing an aluminum nitride sintered body. [Conventional technology] Aluminum nitride (AlN) has high thermal conductivity and high electrical insulation properties, so it has recently been attracting attention as a heat dissipation substrate material for ICs, LSIs, etc.; Due to its excellent stability, it is considered promising as a variety of materials. In general, non-oxides such as AlN are difficult to sinter, and AlN alone has a temperature of 1700 to 2000℃.
High-temperature and high-pressure conditions, such as those used in hot pressing, are necessary for densification. However, the hot pressing method has problems such as difficulty in controlling the shape, low productivity, and high cost. Therefore, recently, research has been actively conducted to obtain dense sintered bodies by pressureless sintering using sintering aids. Today, alkaline earth metal compounds and compounds of rare earth elements such as yttrium are mainly used as sintering aids. [Problems to be Solved by the Invention] The properties of aluminum nitride, including high thermal conductivity, are significantly degraded by the presence of impurities. In particular, the surface of the raw material AlN powder is covered with Al 2 O 3 , which turns into oxynitride during sintering and causes property deterioration. Today, AlN is used to improve sinterability.
However, the result is that the amount of Al 2 O 3 increases due to pulverization. Therefore, in order to obtain an AlN sintered body with good properties, it is necessary to minimize the amount of oxygen in the sintered body. The above-mentioned sintering aid is intended not only to promote sintering but also to remove oxygen from the AlN powder during sintering. For example, when yttrium oxide (Y 2 O 3 ) is added as an auxiliary agent, it reacts with aluminum oxide (Al 2 O 3 ) during sintering to form a yttrium aluminum garnet (YAG) phase at the grain boundaries of AlN. This prevents oxygen from entering AlN. However, when using the above-mentioned sintering aid,
There are only a few cases where the characteristics are significantly improved. Looking specifically at the value of thermal conductivity, in the case of no additives, it is 40 ~
50W/m・K, even if an auxiliary agent is added, the power is 50~
It is about 50W/m・K. This is thought to be due to the added auxiliary agent remaining in the sintered body in some form and inhibiting heat conduction. In particular, the thermal conductivity decreases when elements with large atomic weights such as rare earths remain, as reported in the Journal of Chemistry of Solids, Volume 34, Page 321 (J.Phys.Chem. Solids, 34 , 321 (1973)). Furthermore, when adding a sintering aid, if the particle size of the aid is larger than the particle size of the AlN powder, the mixing and dispersion of the two will be poor, resulting in deterioration of properties due to a decrease in density and the like. An object of the present invention is to provide a method for producing a high-performance aluminum nitride sintered body by eliminating such conventional drawbacks. [Means for Solving the Problems] The present invention involves molding a ceramic mixture in which 0.5 to 10 wt% of one or more alkali metal oxides is added to aluminum nitride powder, and then molding the ceramic mixture in vacuum or in a non-oxidizing atmosphere. This is a method for producing an aluminum nitride sintered body, characterized by sintering at 1600 to 2000°C. The alkali metal oxide used as a sintering aid in the present invention reacts with Al 2 O 3 present in the AlN powder during sintering to produce a multiple oxide called MAlO 2 . Therefore, no oxygen remains in AlN, resulting in good characteristics.
An AlN sintered body is obtained. Moreover, even if the alkali metal oxide remains in the sintered body, since its atomic weight is small, it has little effect on thermal conductivity, and a high-performance sintered body can be obtained.
Examples of such alkali metal oxides include sodium oxide (Na 2 O) and potassium oxide (K 2 O).
are preferred, and one or a mixture of two or more of these compounds is used in an amount of 0.5 to 10 wt%. In the present invention, when the particle size of the alkali metal oxide is the same as or smaller than the particle size of the AlN powder, which is the main component, the sintering of AlN is not inhibited, resulting in a dense and high-performance aluminum nitride sintered compact. can be manufactured. The particle size of the alkali metal oxide used here is usually 0.01 to 3 μm. [Example] Next, an example of the present invention will be described. Example 1 K2O3wt % with an average particle size of 2μm was added to AlN powder with an average particle size of 3μm and an oxygen content of 2wt%, mixed in ethanol with a hogenizer, shaped, and then sintered under normal pressure at 1800°C for 3 hours in a nitrogen atmosphere. He concluded the ceremony. The obtained aluminum nitride sintered body had a density of 3.23 g/cm 3 and a thermal conductivity of 72 W/m·K. Examples 2 to 9 The same AlN powder as in Example 1 was coated with an average particle size of 2 μm.
Na 2 O was added in the amount shown in Table 1 and mixed in ethanol with a homogenizer, and after molding, sintering was performed under the sintering conditions shown in Table 1 to produce an AlN sintered body.
The results are shown in Table 1.
【表】
比較例
実施例１においてK2O3wt％のかわりに
Y2O33wt％を用いたほかは実施例１同様にして
AlN焼結体を製造した。得られた焼結体の密度
は3.24ｇ／cm3、熱伝導率は45W／ｍ・Ｋであつ
た。
［発明の効果］
以上説明したように、本発明の方法によれば焼
結助剤としてアルカリ金属酸化物を用いることに
より従来に比べて特性の優れた窒化アルミニウム
焼結体を製造することができる。[Table] Comparative example In place of K 2 O3wt% in Example 1
Same procedure as Example 1 except that 3wt% of Y 2 O 3 was used.
An AlN sintered body was manufactured. The density of the obtained sintered body was 3.24 g/cm 3 and the thermal conductivity was 45 W/m·K. [Effects of the Invention] As explained above, according to the method of the present invention, by using an alkali metal oxide as a sintering aid, it is possible to produce an aluminum nitride sintered body with superior properties compared to conventional methods. .
Claims (1)
の１種もしくは２種以上を0.5〜10wt％添加した
セラミツク混合物を成形後、真空中若しくは非酸
化性雰囲気中、1600〜2000℃で焼結することを特
徴とする窒化アルミニウム焼結体の製造方法。 ２ アルカリ金属酸化物はNa2Oまたは／および
K2Oである特許請求の範囲第１項記載の窒化アル
ミニウム焼結体の製造方法。 ３ アルカリ金属酸化物の粒径は窒化アルミニウ
ム粉末の粒径以下である特許請求の範囲第１項記
載の窒化アルミニウム焼結体の製造方法。[Claims] 1. After molding a ceramic mixture in which 0.5 to 10 wt% of one or more alkali metal oxides is added to aluminum nitride powder, it is sintered at 1600 to 2000°C in a vacuum or in a non-oxidizing atmosphere. 1. A method for producing an aluminum nitride sintered body, characterized by sintering. 2 Alkali metal oxide is Na 2 O or/and
The method for producing an aluminum nitride sintered body according to claim 1, wherein K 2 O is used. 3. The method for producing an aluminum nitride sintered body according to claim 1, wherein the particle size of the alkali metal oxide is equal to or less than the particle size of the aluminum nitride powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61122682A JPS62278171A (en) | 1986-05-27 | 1986-05-27 | Manufacture of aluminum nitride sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61122682A JPS62278171A (en) | 1986-05-27 | 1986-05-27 | Manufacture of aluminum nitride sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62278171A JPS62278171A (en) | 1987-12-03 |
| JPH058142B2 true JPH058142B2 (en) | 1993-02-01 |
Family
ID=14842016
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61122682A Granted JPS62278171A (en) | 1986-05-27 | 1986-05-27 | Manufacture of aluminum nitride sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62278171A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0747332B1 (en) * | 1994-12-01 | 2001-09-12 | Kabushiki Kaisha Toshiba | Aluminum nitride sinter and process for producing the same |
-
1986
- 1986-05-27 JP JP61122682A patent/JPS62278171A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62278171A (en) | 1987-12-03 |
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