JP2006265036A - Conductive aluminum nitride material and production method therefor - Google Patents
Conductive aluminum nitride material and production method therefor Download PDFInfo
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この発明は、カーボンナノチューブ（以下「ＣＮＴ」という。）を含む窒化アルミニウム焼結体及びその製造方法に関する。この窒化アルミニウム焼結体は導電体や抵抗体等に応用できる。 The present invention relates to an aluminum nitride sintered body containing carbon nanotubes (hereinafter referred to as “CNT”) and a method for producing the same. This aluminum nitride sintered body can be applied to a conductor or a resistor.
窒化アルミニウムは、耐熱性、高熱伝導性、電気絶縁性、耐食性、耐熱衝撃性などの優れた特徴を有するため、機能性セラミックスとして注目され、これまで放熱材としてのＩＣ／ＬＳＩの基板パッケージ、半導体製造用の耐食部材、圧電体、樹脂基板用フィラーなどとして注目され利用されている。
しかし、この材料は本質的に電気的に絶縁体であるため、これが逆に使用中に静電気を生じて微粉体を付着させる結果を招き、導電性を期待する用途への応用を阻んできた。そのため導電性の窒化アルミニウムセラミックスの開発が強く求められていた。
Aluminum nitride has attracted attention as a functional ceramic because it has excellent characteristics such as heat resistance, high thermal conductivity, electrical insulation, corrosion resistance, and thermal shock resistance, and so far, IC / LSI substrate packages and semiconductors as heat dissipation materials It is attracting attention and used as a corrosion-resistant member for manufacturing, a piezoelectric body, a filler for resin substrates, and the like.
However, since this material is essentially an electrically insulating material, it causes static electricity during use and causes fine powders to adhere to it, which has hindered its application in applications where electrical conductivity is expected. Therefore, there has been a strong demand for the development of conductive aluminum nitride ceramics.
このような目的の下に、窒化アルミニウム−希土類化合物、窒化アルミニウム−アルカリ土類化合物、窒化アルミニウム−希土類化合物−アルカリ土類化合物系に他の導電性物を添加すること検討されてきたが、この場合はかなり多量の導電体が必要であり、本来の窒化アルミニウムの性質を失ってしまう。
また、導電性炭素物質を添加することも考えられるが、炭素粉末を加えた場合かなり多くの炭素を加えることが必要であり、一方で炭素の添加が窒化アルミニウム−焼結助剤系の緻密化を大幅に阻害するため、緻密体を得ることが極めて難しい。
そこで，窒化アルミニウム−焼結助剤系に通常の炭素繊維を添加することも考えられたが、炭素粉体を用いる以上に緻密化は困難であった。
これまで窒化ケイ素にＣＮＴを配して導電性を向上させた例はあるが、窒化アルミニウム焼結体の粒界にＣＮＴを導入した導電性の窒化アルミニウム焼結体の例は存在しない（特許文献１、２、非特許文献１、２）。
For such purposes, it has been studied to add other conductive materials to the aluminum nitride-rare earth compound, aluminum nitride-alkaline earth compound, and aluminum nitride-rare earth compound-alkaline earth compound system. In this case, a considerably large amount of conductor is required, and the original properties of aluminum nitride are lost.
In addition, it is conceivable to add a conductive carbon material. However, when carbon powder is added, it is necessary to add a large amount of carbon. On the other hand, the addition of carbon densifies the aluminum nitride-sintering aid system. Therefore, it is extremely difficult to obtain a dense body.
Therefore, it has been considered to add ordinary carbon fibers to the aluminum nitride-sintering aid system, but densification is more difficult than using carbon powder.
There has been an example of improving conductivity by arranging CNT in silicon nitride, but there is no example of a conductive aluminum nitride sintered body in which CNT is introduced into the grain boundary of the aluminum nitride sintered body (Patent Literature). 1, 2, Non-Patent Documents 1, 2).
本発明は、導電性及び緻密性を有する窒化アルミニウム焼結体を提供することを目的とする。 An object of this invention is to provide the aluminum nitride sintered compact which has electroconductivity and denseness.
窒化アルミニウム焼結体にカーボンナノチューブ（ＣＮＴ）を含有させると焼結性を低下させるが、この度合いは、使用する原料粉末の粒径、希土類化合物、アルカリ土類酸化物の選択と割合、総量の選定によって変化するので、これらを種々の最適に組み合わせることにより、導電性及び緻密性を有する窒化アルミニウム焼結体を得ることができる。 When carbon nanotubes (CNT) are included in the aluminum nitride sintered body, the sinterability is reduced. This degree depends on the particle size of the raw material powder to be used, the selection and ratio of the rare earth compound and alkaline earth oxide, and the total amount. Since it varies depending on the selection, an aluminum nitride sintered body having conductivity and denseness can be obtained by variously combining them.
即ち、本発明は、相対密度９５％以上の窒化アルミニウム焼結体の粒界部にカーボンナノチューブ（ＣＮＴ）を含む窒化アルミニウム燒結体であって、該窒化アルミニウムに対してＣＮＴを外掛けで０．３〜１２重量％含む導電性窒化アルミニウム焼結体である。
また本発明は、窒化アルミニウム−希土類化合物、窒化アルミニウム−アルカリ土類化合物、又は窒化アルミニウム−希土類化合物−アルカリ土類化合物系にＣＮＴを外掛けで０．３〜１２重量％含む混合物を成形し、焼結してなる導電性窒化アルミニウム焼結体である。
更に本発明は、上記窒化アルミニウム焼結体から成る導電体又は抵抗体である。
That is, the present invention is an aluminum nitride sintered body containing carbon nanotubes (CNTs) at the grain boundary part of an aluminum nitride sintered body having a relative density of 95% or more, and the CNT is clad to the aluminum nitride to give an O.D. A conductive aluminum nitride sintered body containing 3 to 12% by weight.
Further, the present invention forms an aluminum nitride-rare earth compound, aluminum nitride-alkaline earth compound, or aluminum nitride-rare earth compound-alkaline earth compound based mixture containing 0.3 to 12% by weight of CNT, It is a conductive aluminum nitride sintered body obtained by sintering.
Furthermore, the present invention is a conductor or resistor comprising the aluminum nitride sintered body.
本発明の窒化アルミニウム焼結体は、ＣＮＴを含むため導電性であり、かつ、ＣＮＴを含むにもかかわらず緻密性が確保されている。従って、このような窒化アルミニウム焼結体は、高熱伝導性と導電性同時に有するもので、その他の性質も従来の特性を低下させるものではない。そのため高熱伝導性を有する導電体として抵抗体や窒化アルミニウム焼結体と接合させて使用することができるなど新たの用途展開が期待され、工業的な価値は極めて高い。また、熱伝導率が必ずしも高くない場合も目的によっては許容される。 Since the aluminum nitride sintered body of the present invention contains CNTs, it is conductive, and denseness is ensured despite containing CNTs. Therefore, such an aluminum nitride sintered body has high thermal conductivity and electrical conductivity at the same time, and other properties do not deteriorate conventional characteristics. Therefore, new applications such as being able to be used as a conductor having high thermal conductivity by being joined to a resistor or an aluminum nitride sintered body are expected, and the industrial value is extremely high. Also, the case where the thermal conductivity is not necessarily high is allowed depending on the purpose.
窒化アルミニウムは難焼結性物質であることから、焼結体の作製にあたっては焼結助剤を中心に、種々の添加剤が用いられている。その主流の組成系としては、イットリアに代表される希土類化合物、或いは酸化カルシウム（カルシア）に代表されるアルカリ土類金属化合物、及びこれらを併用したものが用いられている。
希土類化合物やアルカリ土類化合物などの焼結助剤は焼成過程でおおむね酸化物に変化し、窒化アルミニウムの表面に存在するアルミナと反応してＲ−Ａｌ−Ｏ−Ｎ化合物、Ｒ−Ｍ−Ａｌ−Ｏ−Ｎ化合物、Ｒ−Ｍ−Ｏ−Ｎ化合物（Ｒは希土類元素を、Ｍはアルカリ土類元素を表す）などからなる粒界相を生成し、焼結体を緻密化する。
この窒化アルミニウム焼結体においては、焼結助剤の添加によって、粒界相は、窒化アルミニウム結晶粒に存在する不純物固溶酸素をトラップして窒化アルミニウム結晶粒を高純度化し、高熱伝導化や耐食性の向上をもたらすことができる。
またこの窒化アルミニウム燒結体は、窒化アルミニウムから成る結晶粒を母相とし、希土類元素やアルカリ土類元素を含むアルミネート化合物を主とする粒界相を含む。
Since aluminum nitride is a hard-to-sinter material, various additives, mainly sintering aids, are used in the production of sintered bodies. As the mainstream composition system, a rare earth compound typified by yttria, an alkaline earth metal compound typified by calcium oxide (calcia), and a combination thereof are used.
Sintering aids such as rare earth compounds and alkaline earth compounds generally change to oxides during the firing process and react with alumina present on the surface of the aluminum nitride to react with R-Al-O-N compounds and R-M-Al. A grain boundary phase composed of —O—N compound, R—M—O—N compound (R represents a rare earth element, and M represents an alkaline earth element) or the like is generated, and the sintered body is densified.
In this aluminum nitride sintered body, by adding a sintering aid, the grain boundary phase traps impurity solid solution oxygen present in the aluminum nitride crystal grains, thereby purifying the aluminum nitride crystal grains and increasing the thermal conductivity. Corrosion resistance can be improved.
The aluminum nitride sintered body includes a grain boundary phase mainly composed of an aluminate compound containing a rare earth element or an alkaline earth element.
この窒化アルミニウム燒結体は、焼結助剤である希土類化合物を酸化物換算で１０重量％以下、及びアルカリ土類化合物を酸化物換算で５重量％以下含み、残部が酸素含有量が２重量％以下の窒化アルミニウムであることが好ましい。窒化アルミニウムは９０重量％以上であることが好ましい。この窒化アルミニウム燒結体は、平均粒子径が１．０μｍ以下の窒化アルミニウム粉末から成る混合物であって、更にＣＮＴを外掛けで０．３〜１２重量％含む混合物を焼結させることにより形成される。 This aluminum nitride sintered body contains 10% by weight or less of a rare earth compound as a sintering aid in terms of oxide and 5% by weight or less of an alkaline earth compound in terms of oxide, with the remainder having an oxygen content of 2% by weight. The following aluminum nitride is preferable. Aluminum nitride is preferably 90% by weight or more. This aluminum nitride sintered body is formed by sintering a mixture made of aluminum nitride powder having an average particle diameter of 1.0 μm or less and further containing 0.3 to 12% by weight of CNT as an outer shell. .
この窒化アルミニウム燒結体の原料（前駆体）としては、具体的には、窒化アルミニウム−希土類化合物、窒化アルミニウム−アルカリ土類化合物、又は窒化アルミニウム−希土類化合物−アルカリ土類化合物系が用いられ、例えば、以下のような組み合わせが用いられる。
（１）ＡｌＮ（８５〜９７重量％）−Ｙ２Ｏ３（０．５〜１０重量％）−ＣＮＴ（０．３〜１２重量％、焼結助剤を単独で添加する場合は下限は０．５重量％）を基本系とする。
（２）ＡｌＮ（８５〜９７重量％）−ＣａＣＯ３（０．５〜５重量％（ＣａＯ換算））−ＣＮＴ（０．３〜１２重量％、焼結助剤を単独で添加する場合は下限は０．５重量％）を基本系とする。
（３）ＡｌＮ（８５〜９７重量％）−Ｙ２Ｏ３（０〜１０重量％）−ＣａＣＯ３（０〜５重量％（ＣａＯ換算））−ＣＮＴ（０．３〜１２重量％、焼結助剤を単独で添加する場合は下限は０．５重量％）を基本系とする。
Specifically, as the raw material (precursor) of the aluminum nitride sintered body, an aluminum nitride-rare earth compound, an aluminum nitride-alkaline earth compound, or an aluminum nitride-rare earth compound-alkaline earth compound system is used, for example. The following combinations are used.
(1) AlN (85 to 97% by weight) -Y 2 O 3 (0.5 to 10% by weight) -CNT (0.3 to 12% by weight, when adding a sintering aid alone, the lower limit is 0 .5 wt%) is the basic system.
(2) AlN (85 to 97% by weight) -CaCO 3 (0.5 to 5% by weight (calculated as CaO))-CNT (0.3 to 12% by weight, lower limit when adding sintering aid alone Is 0.5% by weight).
(3) AlN (85~97 wt%) - Y 2 O 3 ( 0~10 wt%) - CaCO 3 (0~5 wt% (CaO terms)) - CNT (0.3~12 wt%, sintering When an auxiliary agent is added alone, the lower limit is 0.5% by weight).
窒化アルミニウム原料粉末は平均粒子径が１．５μｍ以下で、かつ酸素含有量が２重量％以下であることが好ましい。このような微細でかつ不純物の少ない窒化アルミニウム粉末を用いることによって、気孔率及び最大気孔径が小さい高密度の窒化アルミニウム焼結体が得易くなる。窒化アルミニウム原料粉末の平均粒子径は０．４〜０．８μｍの範囲であることがより好ましい。 The aluminum nitride raw material powder preferably has an average particle size of 1.5 μm or less and an oxygen content of 2% by weight or less. By using such fine aluminum nitride powder with few impurities, a high-density aluminum nitride sintered body having a small porosity and a maximum pore diameter can be easily obtained. The average particle diameter of the aluminum nitride raw material powder is more preferably in the range of 0.4 to 0.8 μm.
希土類化合物は、特に限定されるものではないが、イットリウム（Ｙ）、ランタン（Ｌａ）、セリウム（Ｃｅ）、サマリウム（Ｓｍ）、ネオジウム（Ｎｄ）、ジスプロシウム（Ｄｙ）、エルビウム（Ｅｒ）などの酸化物、窒化物、硼化物、炭化物、珪化物の少なくとも１種が好ましい。 The rare earth compound is not particularly limited, but oxidation of yttrium (Y), lanthanum (La), cerium (Ce), samarium (Sm), neodymium (Nd), dysprosium (Dy), erbium (Er), etc. At least one of an oxide, a nitride, a boride, a carbide, and a silicide is preferable.
本発明の窒化アルミニウム焼結体は、上記以外の他の成分を含有していてもよい。例えば、窒化アルミニウム焼結体のさらなる緻密化のために、特性を損なわない範囲で他の酸化物、窒化物、硼化物、珪化物やシリカなどを含有していてもよい。これらの化合物の含有量は総量で０．１〜２重量％の程度に抑えることが好ましい。 The aluminum nitride sintered body of the present invention may contain components other than those described above. For example, for further densification of the aluminum nitride sintered body, other oxides, nitrides, borides, silicides, silicas, and the like may be contained within a range that does not impair the characteristics. The total content of these compounds is preferably suppressed to about 0.1 to 2% by weight.
カーボンナノチューブ（ＣＮＴ）としては、米国特許４６６３２３０号、米国特許４６６３２３０号、米国特許５１６５９０９号、米国特許５１７１５６０号、米国特許５５７８５４３号、米国特許５５８９１５２号、米国特許５６５０３７０号、米国特許６２３５６７４号等に記載の中空構造で分岐の少ない炭素系繊維をいう。このＣＮＴのサイズは、通常平均直径０．４〜２００ｎｍ、好ましくは２０ｎｍ、平均長径１〜１０００μｍ、好ましくは１００〜５００μｍである。その添加量は外掛け（即ち、ＣＮＴを含まない窒化アルミニウム焼結体の重量を基準として）で０．３〜１２重量％、好ましくは１．２〜４．２重量％であればよく、その量に応じて導電率を制御することができ、本発明の窒化アルミニウム焼結体の導電率は約１０−３〜１０３Ｓｍ−１である。ＣＮＴが少ないと焼結性は良好であるが、導電率が低くなり、一方、ＣＮＴが多いと焼結性が低下するため好ましくない。 The carbon nanotube (CNT) is described in US Pat. No. 4,663,230, US Pat. No. 4,663,230, US Pat. No. 5,165,909, US Pat. No. 5,171,560, US Pat. No. 5,578,543, US Pat. This is a carbon-based fiber having a hollow structure with few branches. The size of the CNT is usually an average diameter of 0.4 to 200 nm, preferably 20 nm, and an average major axis of 1 to 1000 μm, preferably 100 to 500 μm. The addition amount may be 0.3 to 12% by weight, preferably 1.2 to 4.2% by weight (ie, based on the weight of the aluminum nitride sintered body not containing CNT), The conductivity can be controlled according to the amount, and the conductivity of the aluminum nitride sintered body of the present invention is about 10 −3 to 10 3 Sm −1 . If the amount of CNTs is small, the sinterability is good, but the electrical conductivity is low.
次に、本発明の製造方法について説明する。その製造法は特に限定されないが、通常は次のようなプロセスを基本とする。
各添加物粉末を窒化アルミニウム原料粉末に対して所定量添加し、更に有機バインダや分散媒などを加えてよく混合した後、一軸プレスやラバープレスなどの公知の成形法を適用して原料混合体を所望の形状に成形する。各原料粉末の混合にあたっては、各微細粒子の凝集を防ぎ均一に分散させることが必要であり、それによって焼結促進効果が大きくなることが期待される。
Next, the manufacturing method of this invention is demonstrated. The manufacturing method is not particularly limited, but is usually based on the following process.
A predetermined amount of each additive powder is added to the aluminum nitride raw material powder, an organic binder and a dispersion medium are added and mixed well, and then a raw material mixture is applied by applying a known molding method such as uniaxial press or rubber press. Is formed into a desired shape. In mixing the raw material powders, it is necessary to prevent the fine particles from agglomerating and uniformly disperse, which is expected to increase the sintering promoting effect.
次に、上記のように作製した成形体に脱脂処理を施して脱脂成形体を作製する。この脱脂成形体を１６００〜２０００℃、好ましくは１７５０〜１９００℃で焼結して窒化アルミニウム焼結体が得られる。この温度が低いと緻密化が進みにくく、高いと窒化アルミニウムの分解するため好ましくない。
焼結法としては常圧焼結、雰囲気加圧焼結、ホットプレス焼結、放電プラズマ焼結、マイクロ波焼結、熱間静水圧加圧によるが、とくに、緻密化が困難な場合は、ホットプレス、放電プラズマ焼結、マイクロ波焼結、熱間静水圧加圧を優先的に使用する。
Next, a degreasing process is performed on the molded body produced as described above to produce a degreased molded body. The degreased molded body is sintered at 1600 to 2000 ° C., preferably 1750 to 1900 ° C., to obtain an aluminum nitride sintered body. If this temperature is low, densification is difficult to proceed, and if it is high, aluminum nitride is decomposed, which is not preferable.
Sintering methods are atmospheric pressure sintering, atmospheric pressure sintering, hot press sintering, discharge plasma sintering, microwave sintering, hot isostatic pressing, especially when densification is difficult, Hot press, spark plasma sintering, microwave sintering and hot isostatic pressing are preferentially used.
より高密度の焼結体の作製と焼結体の強度を支配する欠陥を除去するために、無加圧焼結後にＨＩＰ処理を行うなど、複数の方法を組合せてもよい。目的に応じて使い分ければよいが、コストの面からは常圧焼結或いは雰囲気加圧焼結が好ましい。 In order to remove a defect governing the strength of the sintered body and manufacture a higher density sintered body, a plurality of methods may be combined, such as HIP treatment after pressureless sintering. Although it may be properly used depending on the purpose, atmospheric pressure sintering or atmospheric pressure sintering is preferable from the viewpoint of cost.
このようにして得られた窒化アルミニウム焼結体は好ましくは以下の性質を持つ。
窒化アルミニウム焼結体の相対密度は９５％以上である。ＣＮＴは主として粒界相近傍（即ち、粒界部）に存在し、そのアスペクト比は５００〜１００００であり、その含有量は０．３〜１２質量％の範囲にある。この窒化アルミニウム焼結体の３点曲げ強度は３００〜４００ＭＰａ程度である。
以下、実施例にて本発明を例証するが本発明を限定することを意図するものではない。
The aluminum nitride sintered body thus obtained preferably has the following properties.
The relative density of the aluminum nitride sintered body is 95% or more. CNT exists mainly in the vicinity of the grain boundary phase (that is, the grain boundary part), its aspect ratio is 500 to 10,000, and its content is in the range of 0.3 to 12% by mass. The three-point bending strength of this aluminum nitride sintered body is about 300 to 400 MPa.
The following examples illustrate the invention but are not intended to limit the invention.
酸素含有量が１．３重量％、平均粒子径が０．５５μｍのＡｌＮ（窒化アルミニウム）原料粉末（トクヤマーＦ粉末）９５重量％に、焼結助剤として平均粒子径が０．９μｍのＹ２Ｏ３（酸化イットリウム）粉末（信越化学工業製）を３．７５重量％、平均粒子径が０．７μｍのＣａＣＯ３（炭酸カルシウム）粉末（純正化学製）を１．２５重量％（ＣａＯ換算）を秤量した。更に、これらの外掛けでＣＮＴを１．８重量％秤量した．これらをエチルアルコール中で９６時間湿式混合した後に乾燥して原料混合物を調製した。 Y 2 having an average particle size of 0.9 μm as a sintering aid was added to 95% by weight of AlN (aluminum nitride) raw material powder (Tokuyama F powder) having an oxygen content of 1.3% by weight and an average particle size of 0.55 μm. 3.75% by weight of O 3 (yttrium oxide) powder (manufactured by Shin-Etsu Chemical Co., Ltd.), 1.25% by weight of CaCO 3 (calcium carbonate) powder (manufactured by Junsei Kagaku) having an average particle size of 0.7 μm (CaO equivalent) Was weighed. Furthermore, 1.8 wt% of CNT was weighed with these outer covers. These were wet mixed in ethyl alcohol for 96 hours and then dried to prepare a raw material mixture.
得られた原料混合物に有機バインダを所定量添加して調合造粒粉とした後、５０ＭＰａの成形圧力でプレス成形し、曲げ強度測定用サンプルとして直径１５ｍｍ×厚み５ｍｍ及び直径２５ｍｍ×厚み５ｍｍの円板状成形体を多数作製した。
各成形体を４５０℃の空気気流中にて４時間脱脂した後、０．１ＭＰａの窒素ガス雰囲気中にて１３５０℃×１時間の条件で保持した後、０．６ＭＰａの窒素ガス雰囲気中にて１８００℃×２時間の条件で焼結して、窒化アルミニウム焼結体を作製した。
この窒化アルミニウム焼結体中の粒界相をＸ線マイクロアナライザー（日本電子（株）製）で観察したところ、Ａｌ−Ｙ−Ｃａ―Ｏ−Ｎ化合物が主成分であった。
得られた窒化アルミニウム焼結体の導電率は１５Ｓｍ−１であり、他の特性は概ねＣＮＴ無添加と同等であった。
A predetermined amount of an organic binder is added to the obtained raw material mixture to prepare a blended granulated powder, which is then press-molded at a molding pressure of 50 MPa, and a 15 mm diameter x 25 mm x 25 mm x 5 mm thick circle is used as a sample for bending strength measurement. A large number of plate-like molded bodies were produced.
Each molded body was degreased in an air stream at 450 ° C. for 4 hours, then held in a nitrogen gas atmosphere of 0.1 MPa at 1350 ° C. for 1 hour, and then in a nitrogen gas atmosphere of 0.6 MPa. Sintering was performed at 1800 ° C. for 2 hours to produce an aluminum nitride sintered body.
When the grain boundary phase in the aluminum nitride sintered body was observed with an X-ray microanalyzer (manufactured by JEOL Ltd.), the Al—Y—Ca—O—N compound was the main component.
The conductivity of the obtained aluminum nitride sintered body was 15 Sm −1 , and other characteristics were almost the same as those without CNT addition.
実施例２〜１２
実施例１で使用した窒化アルミニウム原料粉末、希土類酸化物粉末、導電性を持つＣＮＴ等を、それぞれ表１に示す組成比となるように調合して原料混合物を調製し、実施例１と同様に窒化アルミニウム焼結体を作製した。焼成の詳細な条件は表１の注に記す。
Examples 2-12
The aluminum nitride raw material powder, rare earth oxide powder, conductive CNT, and the like used in Example 1 were prepared so as to have the composition ratios shown in Table 1 to prepare a raw material mixture. An aluminum nitride sintered body was produced. Detailed conditions for firing are described in the notes in Table 1.
比較例１〜２
比較例１としてＣＮＴを用いない以外は実施例１と同一条件で窒化ケイ素焼結体を作製
し、同様に窒化アルミニウム製ボールを作製した。
比較例２としてＣＮＴを１３重量％添加した以外は実施例１と同一条件で窒化ケイ素焼
結体を作製した。
Comparative Examples 1-2
As Comparative Example 1, a silicon nitride sintered body was produced under the same conditions as in Example 1 except that CNT was not used, and an aluminum nitride ball was similarly produced.
As Comparative Example 2, a silicon nitride sintered body was produced under the same conditions as in Example 1 except that 13% by weight of CNT was added.
このようにして得た実施例及び比較例による各窒化アルミニウム焼結体の組成及び特性を表１に示す。
２）ＣＮＴの重量はSi3N4, R2O3, CaOの合計重量100に対する重量を表す。
Table 1 shows the compositions and characteristics of the aluminum nitride sintered bodies according to the examples and comparative examples thus obtained.
2) The weight of CNT represents the weight with respect to the total weight of Si 3 N 4 , R 2 O 3 and CaO of 100.
表１から明らかなように、本発明の窒化アルミニウム焼結体は、いずれも緻密で優れた導電性が確保されることが認められる。実施例１で得られた窒化アルミニウム焼結体の走査型電子顕微鏡写真（日本電子（株）TSM-5200、二次電子像）を用いて観察した結果、ＣＮＴが粒界部に囲まれて存在していることが確認された。
比較例２は導電性は示したが、緻密化が不十分であった。
As is apparent from Table 1, it is recognized that the aluminum nitride sintered body of the present invention is dense and has excellent conductivity. As a result of observation using the scanning electron micrograph (JEOL Co., Ltd. TSM-5200, secondary electron image) of the aluminum nitride sintered body obtained in Example 1, CNT is surrounded by the grain boundary part. It was confirmed that
Comparative Example 2 showed electrical conductivity, but the densification was insufficient.
Claims (8)
The electrical conductivity which consists of the aluminum nitride sintered compact as described in any one of Claims 1-4 or the aluminum nitride sintered compact manufactured by the manufacturing method as described in any one of Claims 5-7 is 10 <-3>. A conductor or resistor of 10 < 3 > Sm < -1 >.
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| JP2013010676A (en) * | 2011-06-30 | 2013-01-17 | Sumitomo Electric Ind Ltd | Aluminum nitride sintered compact and wafer holder for semiconductor manufacturing device or inspection device using the same |
| CN115819092A (en) * | 2022-10-25 | 2023-03-21 | 杭州大和江东新材料科技有限公司 | Aluminum nitride ceramic with high volume resistivity and high thermal conductivity and preparation method thereof |
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| JP2004119739A (en) * | 2002-09-26 | 2004-04-15 | Kyocera Corp | Electrostatic chuck |
| JP2005041765A (en) * | 2003-07-07 | 2005-02-17 | Ngk Insulators Ltd | Aluminum nitride sintered body, electrostatic chuck, electrically conductive component, component for apparatus for manufacturing semiconductor, and method for manufacturing aluminum nitride sintered body |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2004119739A (en) * | 2002-09-26 | 2004-04-15 | Kyocera Corp | Electrostatic chuck |
| JP2005041765A (en) * | 2003-07-07 | 2005-02-17 | Ngk Insulators Ltd | Aluminum nitride sintered body, electrostatic chuck, electrically conductive component, component for apparatus for manufacturing semiconductor, and method for manufacturing aluminum nitride sintered body |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013010676A (en) * | 2011-06-30 | 2013-01-17 | Sumitomo Electric Ind Ltd | Aluminum nitride sintered compact and wafer holder for semiconductor manufacturing device or inspection device using the same |
| CN115819092A (en) * | 2022-10-25 | 2023-03-21 | 杭州大和江东新材料科技有限公司 | Aluminum nitride ceramic with high volume resistivity and high thermal conductivity and preparation method thereof |
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