JP5094259B2 - Circuit board - Google Patents
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- JP5094259B2 JP5094259B2 JP2007195912A JP2007195912A JP5094259B2 JP 5094259 B2 JP5094259 B2 JP 5094259B2 JP 2007195912 A JP2007195912 A JP 2007195912A JP 2007195912 A JP2007195912 A JP 2007195912A JP 5094259 B2 JP5094259 B2 JP 5094259B2
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本発明は、回路基板に関し、特に、窒化珪素質焼結体からなる母基板に導体層を形成してなる回路基板に関する。 The present invention relates to a circuit board, in particular, it relates to a circuit board obtained by forming a conductor layer on the base substrate made of a silicon nitride sintered body.
従来、電気絶縁性に優れたアルミナ（Ａｌ２Ｏ３）焼結体の表面に導体層を形成し、半導体素子を実装した絶縁回路基板が普及している。特に大電力で動作する半導体を実装する、いわゆるパワー半導体モジュールに使用する絶縁回路基板には、パワー半導体から発する熱を拡散して放熱する必要がある。 Conventionally, an insulating circuit board in which a conductor layer is formed on a surface of an alumina (Al 2 O 3 ) sintered body excellent in electrical insulation and a semiconductor element is mounted has been widespread. In particular, it is necessary to diffuse and dissipate heat generated from a power semiconductor in an insulating circuit board used for a so-called power semiconductor module on which a semiconductor operating with high power is mounted.
このような放熱が要求される回路基板にはアルミナ焼結体のほかに、窒化アルミニウム（ＡｌＮ）焼結体が用いられている。 In addition to alumina sintered bodies, aluminum nitride (AlN) sintered bodies are used for circuit boards that require such heat dissipation.
ところが、近年、このようなパワー半導体モジュールにおいて、パワー半導体の発熱量
増加や実装密度向上への対策として基板の放熱性を向上する要求や、小型・薄型化への要求が高まっている。このような要求に対して、アルミナ焼結体では、その熱伝導率が２０〜３０Ｗ／ｍ・Ｋ程度と低いことから上記要求を満足できない。また、窒化アルミニウム焼結体はその強度が低い（三点曲げ強度で約３００ＭＰａ程度）ことから、実装信頼性に問題があり、小型・薄型化を満足できない。そこで、高放熱性かつ高強度である窒化珪素（Ｓｉ３Ｎ４）焼結体が注目されている。
However, in recent years, in such power semiconductor modules, there are increasing demands for improving the heat dissipation of the substrate and for reducing the size and thickness of the power semiconductor as a measure for increasing the heat generation amount of the power semiconductor and improving the mounting density. In response to such a demand, the alumina sintered body cannot satisfy the above demand because its thermal conductivity is as low as about 20 to 30 W / m · K. Moreover, since the strength of the aluminum nitride sintered body is low (three-point bending strength is about 300 MPa), there is a problem in mounting reliability, and the size and thickness cannot be satisfied. Therefore, a silicon nitride (Si 3 N 4 ) sintered body having high heat dissipation and high strength has attracted attention.
窒化珪素質焼結体は、エンジニアリングセラミックスとして知られており、高強度、高温高強度、高靭性である上、耐熱性、耐熱衝撃性、耐摩耗性および耐酸化性に優れることから、特にガスタービンやターボロータ等の熱機関用部品や切削工具として応用されている（特許文献１参照）。 Silicon nitride-based sintered bodies are known as engineering ceramics. They are particularly strong because they have high strength, high temperature, high strength, and high toughness, as well as excellent heat resistance, thermal shock resistance, wear resistance, and oxidation resistance. It is applied as a heat engine component such as a turbine or a turbo rotor or a cutting tool (see Patent Document 1).
この特許文献１の表には、炭酸リチウムを全量中０．２〜１２モル％添加することが記載されており、１７５０℃以下で４時間窒素ガス中で焼成し、冷却工程で１４００℃、１０５０℃の温度で熱処理し、窒化珪素結晶粒子の粒界にリチウムと希土類元素を含む複合酸化物からなる結晶相を存在せしめ、自動車部品やガスタービンエンジン用部品等で使用される温度域における強度を向上させた窒化珪素質焼結体が記載されている。 In the table of Patent Document 1, it is described that 0.2 to 12 mol% of lithium carbonate is added in the total amount. Heat treatment is performed at a temperature of ℃, and a crystal phase composed of a complex oxide containing lithium and rare earth elements is present at the grain boundaries of silicon nitride crystal particles, so that the strength in the temperature range used for automobile parts, gas turbine engine parts, etc. An improved silicon nitride sintered body is described.
一方、１９８０年代後半から１９９０年代には、窒化珪素質焼結体は、パワー半導体モジュール用放熱性基板としての応用が活発に検討されたが、熱伝導率に勝る窒化アルミニウム焼結体に実用面では先を越されていた。ところが、上記したように、窒化珪素質焼結体は高強度であるために薄型化できることから、厚い窒化アルミニウム焼結体からなる基板に肉薄する放熱性が期待でき、さらなる高熱伝導率化が検討されている（特許文献２、３等参照）。 On the other hand, in the late 1980s to 1990s, silicon nitride sintered bodies were actively studied for application as heat dissipation substrates for power semiconductor modules. Then it was past. However, as described above, since the silicon nitride sintered body has high strength and can be thinned, heat dissipation can be expected to be thinned on a substrate made of a thick aluminum nitride sintered body, and further higher thermal conductivity is studied. (See Patent Documents 2 and 3, etc.).
これらの特許文献２、３には、Ｌｉ、Ａｌ、Ｎａ、Ｋ等の不可避不純物は、熱伝導率を低下させるので、含有量を合計で０．５質量％以下とすることが記載されている。
しかしながら、特許文献１〜３では未だ熱伝導率が低いという問題があった。即ち、特許文献１に記載された窒化珪素質焼結体は、自動車部品やガスタービンエンジン用部品用であり、実施例からＬｉ２Ｏ換算で１．２モル％以上添加し、これらは熱処理によりリチウムと希土類元素の複合酸化物として存在せしめているが、Ｌｉは焼成中に蒸発し易い物質であり、焼結後にどの程度Ｌｉを含有しているか全く記載されておらず、どの程度の熱伝導率を有するか全く記載されていない。 However, Patent Documents 1 to 3 still have a problem that the thermal conductivity is low. That is, the silicon nitride-based sintered body described in Patent Document 1 is for automobile parts and gas turbine engine parts, and is added in an amount of 1.2 mol% or more in terms of Li 2 O from the examples. Although it is present as a complex oxide of lithium and rare earth elements, Li is a substance that easily evaporates during firing, it does not describe how much Li is contained after sintering, and how much heat conduction It is not described at all.
また、窒化珪素Ｓｉ３Ｎ４は難焼結体であることから、焼結助剤としてＹ２Ｏ３などの希土類酸化物やアルミナなどを添加する必要があるが、特許文献２、３では、このような焼結助剤としての様々な添加物や、この添加物中に含まれるＬｉ、Ａｌ、Ｎａ、Ｋ等の不純物が原因となって窒化珪素質焼結体の熱伝導率を低下させてしまうことが記載され、具体的には、添加物や不純物は窒化珪素質焼結体中に高熱抵抗の粒界相を形成したり、窒化珪素結晶相の中に固溶してしまい、窒化珪素結晶の熱拡散率を低下させ、熱伝導率を低下させてしまうと考えられていた。従って、特許文献２、３では、Ｌｉについても含有しないように制御していた。 Further, since silicon nitride Si 3 N 4 is a hardly sintered body, it is necessary to add a rare earth oxide such as Y 2 O 3 or alumina as a sintering aid. Due to various additives such as a sintering aid and impurities such as Li, Al, Na and K contained in the additive, the thermal conductivity of the silicon nitride sintered body is lowered. Specifically, the additives and impurities form a grain boundary phase with high thermal resistance in the silicon nitride sintered body or are dissolved in the silicon nitride crystal phase, resulting in nitridation. It was thought that the thermal diffusivity of the silicon crystal was lowered and the thermal conductivity was lowered. Therefore, in patent document 2, 3, it controlled so that it may not contain Li.
本発明は、母基板の熱伝導率を向上できる回路基板を提供することを目的とする。 The present invention aims to provide a circuit board capable of improving the thermal conductivity of the mother board.
本発明者等は、従来、熱伝導率向上を阻害すると考えられていたＬｉについては、母基板中に一定量含有させることにより、熱伝導率を低下させる要因とならず、却って熱拡散率を高め、熱伝導率を向上させることができることを見出し、本発明に至った。 The present inventors have conventionally considered that Li, which has been considered to hinder improvement in thermal conductivity, does not cause a decrease in thermal conductivity by containing a certain amount in the mother substrate, but instead increases thermal diffusivity. It has been found that the thermal conductivity can be increased and the present invention has been achieved.
即ち、本発明の回路基板は、窒化珪素質焼結体からなる母基板に導体層を形成してなる回路基板であって、前記母基板が、希土類元素を酸化物換算で全量中１．３〜２．０質量％含有するとともに、Ｌｉを全量中０．０２〜０．０３質量％含有することを特徴とする。このような回路基板では、母基板が、希土類元素を酸化物換算で全量中１．３〜２．０質量％含有するため、母基板の焼結性を向上でき、母基板の緻密化を促進し、強度を向上することができるとともに、全量中Ｌｉを０．０２〜０．０３質量％含有するため、母基板の熱拡散率を向上でき、これにより、母基板の熱伝導率を向上できる。 That is, the circuit board of the present invention is a circuit board obtained by forming a conductor layer on the base substrate made of a silicon nitride sintered body, the mother substrate, in a total volume in terms of oxide of rare earth element 1.3 While containing -2.0 mass%, Li is contained 0.02-0.03 mass% in the whole quantity, It is characterized by the above-mentioned. In such a circuit board, the mother board contains rare earth elements in an amount of 1.3 to 2.0% by mass in terms of oxide, so that the sinterability of the mother board can be improved and the mother board is made denser. In addition, the strength can be improved, and since 0.02 to 0.03 mass% of Li is contained in the total amount, the thermal diffusivity of the mother substrate can be improved, and thereby the thermal conductivity of the mother substrate can be improved. .
即ち、母基板中にＬｉを全量中０．０２〜０．０３質量％含有するということは、焼結時までＬｉが０．０２〜０．０３質量％存在していたということであり、これにより、後述するように、窒化珪素結晶中への添加元素やＬｉ以外の不純物の固溶を抑制でき、これにより、窒化珪素結晶が本来有する熱拡散率の低下を抑制し、その結果、母基板の熱伝導率を従来よりも大幅に向上できると考えている。 That is, containing 0.02-0.03% by mass of Li in the total amount in the mother substrate means that 0.02-0.03% by mass of Li was present until sintering. Thus, as described later, it is possible to suppress solid solution of impurities other than additive elements and Li in the silicon nitride crystal, thereby suppressing a decrease in the thermal diffusivity inherent in the silicon nitride crystal, and as a result, the mother substrate It is thought that the thermal conductivity of can be greatly improved than before.
また、本発明の回路基板は、前記Ｌｉの少なくとも一部は、窒化珪素結晶中に固溶していることを特徴とする。このような回路基板では、Ｌｉの少なくとも一部が窒化珪素結晶中に固溶することにより、理由は明確ではないが、窒化珪素結晶中への添加元素やＬｉ以外の不純物の固溶をさらに抑制でき、これにより、母基板の熱伝導率をさらに向上できると考えている。 The circuit board of the present invention is characterized in that at least a part of the Li is dissolved in a silicon nitride crystal. In such a circuit board, at least part of Li is dissolved in the silicon nitride crystal, but the reason is not clear, but further suppresses the solid solution of impurities other than additive elements and Li in the silicon nitride crystal. This is considered to further improve the thermal conductivity of the mother substrate.
さらに、本発明の回路基板は、前記母基板中に、Ａｌ、Ｎａ、Ｋ、Ｆｅ、Ｂａ、ＭｎおよびＢを、合量で０．０１質量％以下含有することを特徴とする。このような回路基板では、Ｌｉ以外の不純物量が、合量で０．０１質量％以下であるため、さらに母基板の熱伝導率を高めることができる。 Furthermore, the circuit board of the present invention is characterized in that the mother board contains Al, Na, K, Fe, Ba, Mn and B in a total amount of 0.01% by mass or less. In such a circuit board, since the total amount of impurities other than Li is 0.01% by mass or less, the thermal conductivity of the mother board can be further increased.
本発明の回路基板では、母基板が、希土類元素を酸化物換算で全量中１．３〜２．０質量％含有するとともに、全量中Ｌｉを０．０２〜０．０３質量％含有するため、母基板の緻密化を促進し、強度を向上することができるとともに、母基板の熱拡散率を向上でき、これにより、母基板の熱伝導率を向上できる。 In the circuit board of the present invention, the mother board contains 1.3 to 2.0% by mass of the rare earth element in terms of oxide and 0.02 to 0.03% by mass of Li in the total quantity. The densification of the mother substrate can be promoted, the strength can be improved, and the thermal diffusivity of the mother substrate can be improved, whereby the thermal conductivity of the mother substrate can be improved.
本発明の回路基板は、窒化珪素質焼結体からなる母基板に導体層（金属回路を含む）を形成してなるもので、母基板の上面、または下面、さらには上下両面に導体層を設けたもので、この導体層には、半導体素子が搭載される。 The circuit board of the present invention is formed by forming a conductor layer (including a metal circuit) on a mother board made of a silicon nitride sintered body, and has a conductor layer on the upper surface or lower surface of the mother board, and further on both upper and lower surfaces. A semiconductor element is mounted on the conductor layer.
そして、窒化珪素質焼結体からなる母基板は、窒化珪素を主成分とし、希土類元素を酸化物換算で全量中１．３〜２．０質量％含有するとともに、ＬｉをＬｉ金属換算で母基板全量中０．０２〜０．０３質量％含有することを特徴とする。このような回路基板では、母基板の熱拡散率を向上でき、これにより、母基板の熱伝導率を向上できる。このようなＬｉの少なくとも一部は、窒化珪素結晶中に固溶しているものと考えられる。 The mother substrate made of a silicon nitride-based sintered body contains silicon nitride as a main component and contains rare earth elements in an amount of 1.3 to 2.0% by mass in terms of oxide, and Li in terms of Li metal. It is characterized by containing 0.02 to 0.03% by mass in the total amount of the substrate. In such a circuit board, the thermal diffusivity of the mother board can be improved, thereby improving the thermal conductivity of the mother board. At least a part of such Li is considered to be dissolved in the silicon nitride crystal.
また、原料中にはＡｌ、Ｎａ、Ｋ、Ｆｅ、Ｂａ、ＭｎおよびＢ等の不可避不純物を混入しており、これらの不可避不純物は、母基板全量中に合量で０．０１質量％以下であるこ
とが望ましい。これにより母基板の熱拡散率の低下を抑制でき、結果として母基板の熱伝導率を向上できる。
In addition, inevitable impurities such as Al, Na, K, Fe, Ba, Mn, and B are mixed in the raw material, and these inevitable impurities are in a total amount of 0.01% by mass or less in the total amount of the mother substrate. It is desirable to be. Thereby, the fall of the thermal diffusivity of a mother board | substrate can be suppressed, and the thermal conductivity of a mother board | substrate can be improved as a result.
さらに、母基板中に、希土類元素を酸化物換算で全量中１．３〜２．０質量％含有することにより、焼結性が向上する。窒化珪素は前述したように、難焼結性であるので、焼結助剤を添加することが望ましく、一般的に知られている希土類元素酸化物、例えば特にＹ２Ｏ３、Ｅｒ２Ｏ３、Ｄｙ２Ｏ３などを焼結助剤として１．３〜２．０質量％添加含有することができる。 Further, in the base substrate, by containing 1.3 to 2.0 mass% in total amount in terms of oxide of the rare earth elements, sintering property is improved. As described above, since silicon nitride is difficult to sinter, it is desirable to add a sintering aid, and generally known rare earth element oxides such as Y 2 O 3 and Er 2 O 3 in particular. , Dy 2 O 3 and the like as a sintering aid may be added in an amount of 1.3 to 2.0 % by mass.
本発明の回路基板は、窒化珪素質焼結体からなる母基板に導体層を形成して作製される。母基板は、窒化珪素粉末にＹ ２ Ｏ ３ 、Ｅｒ ２ Ｏ ３ 、Ｄｙ ２ Ｏ ３ などを焼結助剤として１．３〜２．０質量％、Ｌｉ化合物をＬｉ２Ｏ換算で全量中０．７〜１．０質量％添加した混合粉末を成形して焼成し、Ｌｉを全量中０．０２〜０．０３質量％含有せしめて作製することができる。 Circuit board of the present invention is produced by forming a conductor layer on the base substrate made of a silicon nitride sintered body. The mother substrate is 1.3 to 2.0% by mass of silicon nitride powder with Y 2 O 3 , Er 2 O 3 , Dy 2 O 3 or the like as a sintering aid, and the Li compound is 0 % in total in terms of Li 2 O. The mixed powder added with 0.7 to 1.0% by mass is molded and fired, and Li can be produced by containing 0.02 to 0.03% by mass in the total amount.
窒化珪素粉末は、酸素を１．７質量％以下、不純物イオンとしてのＡｌ、Ｎａ、Ｋ、Ｆｅ、Ｂａ、ＭｎおよびＢを合計で０．０１質量％以下、α相型窒化珪素を９０質量％以上含有し、平均粒径１μｍ以下の粉末を用いることが望ましい。 The silicon nitride powder has oxygen of 1.7% by mass or less, Al, Na, K, Fe, Ba, Mn and B as impurity ions in total of 0.01% by mass or less, and α-phase silicon nitride of 90% by mass. It is desirable to use a powder containing the above and having an average particle size of 1 μm or less.
Ｌｉ化合物としては、例えばＬｉ２ＣＯ３粉末を用いることができる。このようなＬｉ２ＣＯ３粉末はＬｉ２Ｏ換算で全量中０．７〜１．０質量％添加する。 As the Li compound, for example, Li 2 CO 3 powder can be used. Such Li 2 CO 3 powder is added in an amount of 0.7 to 1.0% by mass in terms of Li 2 O.
そして、本発明では、Ｌｉ化合物をＬｉ２Ｏ換算で全量中０．７〜１．０質量％添加した混合粉末を成形して焼成し、Ｌｉを母基板全量中０．０２〜０．０３質量％含有せしめることが重要である。 In the present invention, and firing the molded mixed powder was added 0.7 to 1.0 wt% in the total amount of Li compound Li 2 O in terms, 0.02-0.03 mass in the mother board the total amount of Li % Is important.
本発明では、Ｌｉ化合物を添加し、一定量母基板中に含有せしめることを特徴とするが、その効果は、Ｌｉが焼結過程において窒化珪素結晶に固溶することによって、焼結助剤（希土類等）の添加元素や不純物元素が固溶することを抑えることができ、これによって窒化珪素焼結体の熱拡散率が向上すると考えている。 The present invention is characterized in that a Li compound is added and contained in a predetermined amount in the mother substrate. The effect is that the Li is dissolved in the silicon nitride crystal during the sintering process, so that the sintering aid ( It is believed that the rare earth and other additive elements and impurity elements can be prevented from forming a solid solution, thereby improving the thermal diffusivity of the silicon nitride sintered body.
ところが、焼結過程でＬｉが蒸発してしまうと、その効果が無くなるため、Ｌｉ化合物をＬｉ２Ｏ換算で全量中０．７〜１．０質量％添加し、母基板全量中０．０２〜０．０３質量％残存させるべく、焼成に際してＬｉの蒸発を抑制するため、窒化珪素粉末とＬｉ化合物を含有する混合粉末の成形体を、窒化珪素焼結体製の鉢の中に、Ｌｉ化合物を含有していない、窒化珪素粉末のとも材を充填し、成形体をこのとも材の中に埋め込んで焼成する。 However, when Li evaporates during the sintering process, the effect is lost. Therefore, the Li compound is added in an amount of 0.7 to 1.0 % by mass in terms of Li 2 O, and 0.02 to 0.02 in the total amount of the mother substrate. In order to suppress the evaporation of Li during firing so that 0.03 % by mass remains, a molded body of a mixed powder containing silicon nitride powder and Li compound is placed in a pot made of a silicon nitride sintered body, A silicon nitride powder that is not contained is filled with a material, and the compact is embedded in the material and fired.
成形体を窒化珪素粉末のとも材中に埋設して焼成しているため、Ｌｉの蒸発がある程度抑制されるものの、とも材がＬｉ化合物を含有していないため、Ｌｉがある程度蒸発することになり、Ｌｉ化合物をＬｉ２Ｏ換算で全量中０．７〜１．０質量％添加し、母基板全量中０．０２〜０．０３質量％残存することになる。 Since the molded body is embedded and fired in silicon nitride powder, the evaporation of Li is suppressed to some extent, but since the material does not contain a Li compound, Li will evaporate to some extent. The Li compound is added in an amount of 0.7 to 1.0 % by mass in terms of Li 2 O, and 0.02 to 0.03 % by mass remains in the total amount of the mother substrate.
本発明の範囲において熱拡散率は０．５２８［ｍ２／秒］以上と高い値が得られる。 The thermal diffusivity in the onset bright range 0.528 [m 2 / sec] or higher and a high value is obtained.
本発明の回路基板の母基板は、熱拡散率は０．５２８［ｍ２／秒］以上、特には０．６［ｍ２／秒］以上であり、熱伝導率は１１７［Ｗ・ｍ／Ｋ］以上、特には、１３０［Ｗ・ｍ／Ｋ］以上のものが得られる。 The mother board of the circuit board of the present invention has a thermal diffusivity of 0.528 [m 2 / sec] or more, particularly 0.6 [m 2 / sec] or more, and a thermal conductivity of 117 [W · m / sec]. K] or more, in particular, 130 [W · m / K] or more is obtained.
さらに、本発明の母基板では、熱伝導率が高いため、厚さを薄くすることにより、窒化
珪素からなるものとしては窒化アルミニウムに比べてもそん色のない高放熱性の母基板が得られ、一方、より強度を高くするため、０．５ｍｍ以上の厚みとした場合でも、熱伝導率が高いため、回路基板として用いることができる。
Furthermore, since the mother substrate of the present invention has a high thermal conductivity, a thin substrate having a high heat dissipation property that is comparable to aluminum nitride when compared with aluminum nitride can be obtained by reducing the thickness. On the other hand, in order to increase the strength, even when the thickness is 0.5 mm or more, the thermal conductivity is high, so that it can be used as a circuit board.
出発原料として、窒化珪素α相を９５％含み、酸素を１質量％含み、平均粒径０．５μｍの窒化珪素粉末と、平均粒径１．５μｍのＬｉ２ＣＯ３粉末と、平均粒径１．０μｍのＹ２Ｏ３粉末、平均粒径１．０μｍのＥｒ２Ｏ３粉末、平均粒径１．０μｍのＤｙ２Ｏ３粉末を用意した。 As starting materials, silicon nitride α-phase containing 95%, oxygen containing 1% by mass, silicon nitride powder having an average particle size of 0.5 μm, Li 2 CO 3 powder having an average particle size of 1.5 μm, and an average particle size of 1 0.02 μm Y 2 O 3 powder, an average particle diameter of 1.0 μm Er 2 O 3 powder, and an average particle diameter of 1.0 μm Dy 2 O 3 powder were prepared.
これらの原料粉末を用いて、表１に示す組成比率になるように秤量し、溶媒としてイソプロピルアルコールを、メディアとして窒化珪素焼結体製のボールを加えて振動ミルにて７２時間混合した。その後スラリーはイソプロピルアルコールを乾燥させて混合粉体とし、この混合粉末を０．５ｔｏｎ／ｃｍ３の圧力で金型プレスした後、３ｔｏｎ／ｃｍ３の圧力にて静水圧プレスを施して成形体を得た。尚、表１の試料Ｎｏ．１で説明すると、Ｙ２Ｏ３粉末を１質量％、Ｌｉ２ＣＯ３粉末を０．３質量％、窒化珪素粉末を９８．７質量％添加したことになる。 These raw material powders were weighed so as to have the composition ratios shown in Table 1, and isopropyl alcohol as a solvent and balls made of a silicon nitride sintered body as a medium were added and mixed in a vibration mill for 72 hours. Thereafter, the slurry is dried with isopropyl alcohol to form a mixed powder, and this mixed powder is die-pressed at a pressure of 0.5 ton / cm 3 , and then subjected to an isostatic pressing at a pressure of 3 ton / cm 3 to obtain a molded body. Obtained. In addition, sample No. in Table 1 In other words, 1% by mass of Y 2 O 3 powder, 0.3% by mass of Li 2 CO 3 powder, and 98.7% by mass of silicon nitride powder are added.
次いで、窒化珪素焼結体製の鉢の中に、Ｌｉ２ＣＯ３粉末を含有していない、窒化珪素粉末のとも材を充填し、上記成形体をこのとも材の中に埋め込んだ後、０．９ＭＰａの圧力の窒素ガス雰囲気下で１９５０℃の温度にて焼成して焼結体を得た。 Next, a silicon nitride sintered body containing a silicon nitride powder that does not contain Li 2 CO 3 powder is filled in a pot made of a silicon nitride sintered body, and the molded body is embedded in this material. A sintered body was obtained by firing at a temperature of 1950 ° C. in a nitrogen gas atmosphere at a pressure of 9 MPa.
なお、本発明の実施例については、とも材として１質量％の酸化珪素を添加含有した窒化珪素粉末を用い、表１の試料Ｎｏ．２３については、とも材として１．５質量％のＬｉ２ＣＯ３を添加含有した窒化珪素粉末を用い、試料Ｎｏ．２２についてはとも材を使用しなかった。 For the examples of the present invention, silicon nitride powder containing 1% by mass of silicon oxide as an additive material was used. For No. 23, silicon nitride powder containing 1.5% by mass of Li 2 CO 3 as an additive material was used. No material was used for No. 22.
こうして得られた試料Ｎｏ．１〜２５に係る各窒化珪素焼結体について、熱拡散率をレーザーフラッシュ法（試料の両面にＡｕ蒸着し、両面を黒化処理して２５℃でルビーレーザーパルス光を均一に照射）にて測定し、測定した熱拡散率と比熱、密度を掛け合わせて熱伝導率を算出した。その結果を表１に示す。 Sample No. obtained in this way. For each of the silicon nitride sintered bodies according to 1 to 25, the thermal diffusivity is measured by a laser flash method (Au is vapor-deposited on both sides of the sample, both sides are blackened, and the ruby laser pulse light is uniformly irradiated at 25 ° C.) The thermal conductivity was calculated by multiplying the measured thermal diffusivity, specific heat, and density. The results are shown in Table 1.
また、不純物イオンとしてのＡｌ、Ｎａ、Ｋ、Ｆｅ、Ｂａ、ＭｎおよびＢを、ＩＣＰ
発光分光分析で測定し、表１に記載した。さらに、Ｌｉ量をＩＣＰ発光分光分析で測定し、Ｌｉ金属換算して表１に記載した。
Measured by emission spectroscopic analysis and listed in Table 1. Furthermore, the amount of Li was measured by ICP emission spectroscopic analysis and listed in Table 1 in terms of Li metal.
この表１によれば、本発明の範囲内にある試料Ｎｏ．３、５〜１０は熱拡散率が０．５２８×１０−４［ｍ２／秒］以上の優れた特性を有していることがわかる。一方、焼成時にとも材を用いなかった試料Ｎｏ．２２では、Ｌｉの蒸発量が多くなり、熱拡散率が低く、とも材として１．５質量％のＬｉ２ＣＯ３を添加含有した試料Ｎｏ．２３では、焼結体中のＬｉ量が多くなり、熱拡散率が低かった。 According to this Table 1, sample Nos. Within the scope of the present invention. 3 and 5 to 10 have excellent thermal diffusivity of 0.528 × 10 −4 [m 2 / sec] or more. On the other hand, Sample No. which did not use any material during firing. In 22, the number evaporation amount of Li, low thermal diffusivity, the sample was added containing 1.5 mass% of Li 2 CO 3 as a common material No. In No. 23, the amount of Li in the sintered body increased and the thermal diffusivity was low.
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