JP4825081B2 - Method for producing sintered boron nitride - Google Patents
Method for producing sintered boron nitride Download PDFInfo
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本発明は、窒化ホウ素焼結体、その製造方法及び用途に関する。 The present invention relates to a boron nitride sintered body, a manufacturing method thereof, and an application.
近年、例えば窒化ガリウム（ＧａＮ）を用いたＬＥＤの普及が急速に進んでおり、信号機、照明、携帯カメラのライトなどに使用されている。ＧａＮの製造には高温のアンモニアガスの使用が不可欠であるので、そのガスに対して耐食性のある例えば窒化ホウ素焼結体を治具として用いることが提案されている。しかし、窒化ホウ素焼結体の熱伝導率が大きいので、例えば炉の内壁のように、断熱を必要とする用途には適用することができなかった。窒化ホウ素を断熱材用途として用いる場合は、窒化ホウ素製繊維とするか（特許文献１）、窒化ホウ素粉体間に空気を含ませること（特許文献２）が提案されている。しかしながら、窒化ホウ素製繊維を製造することは極めて高度な技術であり、また粉体間に空気を含ませる技術には、粉末の飛散や不純物が混入しＧａＮに悪影響を及ぼす恐れがあった。
本発明の目的は、高温アンモニアガスに対する耐食性に優れ、しかも耐熱性があり、低熱伝導性である窒化ホウ素焼結体と、それを用いた半導体製造装置用の断熱部材を提供するものである。 An object of the present invention is to provide a boron nitride sintered body that is excellent in corrosion resistance against high-temperature ammonia gas, has heat resistance, and has low thermal conductivity, and a heat insulating member for a semiconductor manufacturing apparatus using the boron nitride sintered body.
本発明は、窒化ホウ素粉末１００質量部に対しアクリル系樹脂１０〜４０質量部を含む混合物を成型後、アクリル系樹脂を除去して嵩密度が０．９〜１．２ｇ／ｃｍIn the present invention, after molding a mixture containing 10 to 40 parts by mass of acrylic resin with respect to 100 parts by mass of boron nitride powder, the acrylic resin is removed and the bulk density is 0.9 to 1.2 g / cm. ３3 の多孔質成形体とした後、常圧焼結することを特徴とする質量と外寸より算出された嵩密度が０．７〜０．９ｇ／ｃｍThe bulk density calculated from the mass and the outer dimension is 0.7 to 0.9 g / cm. ３3 、ＪＩＳ Ｒ １６１１のレーザーフラッシュ法により測定された熱伝導率が２０Ｗ／ｍ・Ｋ以下である窒化ホウ素焼結体の製造方法である。, A method for producing a boron nitride sintered body having a thermal conductivity of 20 W / m · K or less measured by a laser flash method of JIS R 1611.
本発明によれば、高温アンモニアガスに対する耐食性に優れ、しかも耐熱性があり、低熱伝導性である窒化ホウ素焼結体と、それを用いた半導体製造装置用の断熱部材が提供される。 ADVANTAGE OF THE INVENTION According to this invention, the boron nitride sintered compact which is excellent in the corrosion resistance with respect to high temperature ammonia gas, is heat resistant, and is low thermal conductivity, and the heat insulation member for semiconductor manufacturing apparatuses using the same are provided.
窒化ホウ素焼結体の嵩密度が０．７ｇ／ｃｍ３未満では、窒化ホウ素焼結体の強度が小さいため、例えば半導体製造装置用断熱部材として、反応炉内壁に窒化ホウ素焼結体を貼り付ける際に、割れや欠け等が生じる恐れがあり、また保持性（断熱材の施工時から断熱材が炉壁から剥離するまでの期間）も低下する。嵩密度が０．９ｇ／ｃｍ３をこえると、閉気孔量が多くなるため、加熱と冷却の繰り返しにより、閉気孔部にクラックが入り、封入したガスが噴出する恐れがある。閉気孔部が多くなると、封入されているガス量も多くなるため、ＧａＮの発光特性に悪影響を及ぼす恐れがある。一方、熱伝導率が２０Ｗ／ｍ・Ｋをこえると、半導体製造装置用断熱部材としての断熱効果が不十分となる。その結果、反応炉内の温度が低下し、発光特性に優れたＧａＮを得ることが困難となる。 When the bulk density of the boron nitride sintered body is less than 0.7 g / cm 3 , the boron nitride sintered body has low strength. For example, the boron nitride sintered body is attached to the inner wall of the reaction furnace as a heat insulating member for a semiconductor manufacturing apparatus. At this time, there is a risk that cracks, chips, etc. may occur, and retention (a period from when the heat insulating material is applied until the heat insulating material is peeled off from the furnace wall) also decreases. When the bulk density exceeds 0.9 g / cm 3 , the amount of closed pores increases, so that the closed pores may crack due to repeated heating and cooling, and the enclosed gas may be ejected. If the number of closed pores increases, the amount of gas enclosed increases, which may adversely affect the light emission characteristics of GaN. On the other hand, when the thermal conductivity exceeds 20 W / m · K, the heat insulating effect as a heat insulating member for a semiconductor manufacturing apparatus becomes insufficient. As a result, the temperature in the reaction furnace decreases, making it difficult to obtain GaN with excellent light emission characteristics.
嵩密度は、アクリル系樹脂の使用量を変えて焼結前の多孔質成形体の密度を制御すること、窒化ホウ素粉末中の揮発性物質量を制御すること、成型圧力を制御すること、などによって調製することができる。 The bulk density is to control the density of the porous molded body before sintering by changing the amount of acrylic resin used, to control the amount of volatile substances in the boron nitride powder, to control the molding pressure, etc. Can be prepared.
本発明に用いるアクリル系樹脂とは、アクリル酸、メタアクリル酸、アクリル酸エステル、メタアクリル酸エステルの共重合体などのことであり、これには大日本インキ社製商品名「ＮＣＢ−１２１」、「ＮＣＢ−１５６」、ライオン社製商品名「ＡＱ−３３００」、「ＡＱ−２５５９」、日本触媒社製商品名「アクリセット」、中央理化工業社製商品名「リカボンド」、ユケン工業社製商品名「セランダー」、共栄社化学社製商品名「オリコックス」などの市販品がある。本発明において、種々ある有機結合材の中から、アクリル系樹脂を選んだ理由は、４００〜５００℃でほぼ完全に分解する良好な熱分解性を示すこと、樹脂そのものに分散剤としての機能があるため分散剤などを特に使用しなくても窒化ホウ素粉末との混合性が良好になること、吸湿性が少ないため乾燥後の原料粉末の取り扱いが容易であるため、などである。 The acrylic resin used in the present invention is acrylic acid, methacrylic acid, acrylic acid ester, a copolymer of methacrylic acid ester, and the like, and for this, trade name “NCB-121” manufactured by Dainippon Ink Co., Ltd. , “NCB-156”, product names “AQ-3300”, “AQ-2559” manufactured by Lion Corporation, product names “Akreset” manufactured by Nippon Shokubai Co., Ltd., product names “Rikabond” manufactured by Chuo Rika Kogyo Co., Ltd., manufactured by Yuken Industry Co., Ltd. There are commercial products such as “Serander” under the trade name and “Oricox” under the name of Kyoeisha Chemical Co. In the present invention, the reason why acrylic resin is selected from various organic binders is that it exhibits good thermal decomposability that almost completely decomposes at 400 to 500 ° C., and the resin itself has a function as a dispersant. Therefore, the mixing with the boron nitride powder is good without using a dispersant or the like, and the raw material powder after drying is easy to handle because of its low hygroscopicity.
アクリル系樹脂はそのまま用いても良いが、エマルジョン又は溶液の形態で用いることが好ましく、その場合には成型する前に溶剤を乾燥除去しておくことが望ましい。溶剤としては、水や、例えばエタノール、メタノール等のアルコールなどが使用される。アクリル系樹脂の使用量は、窒化ホウ素粉末１００質量部に対し固形分として１０〜４０質量部、特に１５〜３０質量部の割合であることが好ましい。４０質量部よりも多いと、窒化ホウ素焼結体の嵩密度が０．７ｇ／ｃｍ３よりも小さくなり、１０質量部よりも少ないと、嵩密度が０．９ｇ／ｃｍ３よりも大きくなる。 The acrylic resin may be used as it is, but is preferably used in the form of an emulsion or a solution. In that case, it is desirable to dry and remove the solvent before molding. As the solvent, water or alcohol such as ethanol or methanol is used. The amount of the acrylic resin used is preferably 10 to 40 parts by mass, particularly 15 to 30 parts by mass as a solid content with respect to 100 parts by mass of the boron nitride powder. When the amount is more than 40 parts by mass, the bulk density of the boron nitride sintered body is smaller than 0.7 g / cm 3 , and when the amount is less than 10 parts by mass, the bulk density is larger than 0.9 g / cm 3 .
窒化ホウ素粉末は、市販品で十分であり特に制約はない。窒化ホウ素粉末中の揮発性物質の含有量が０．０１〜０．３質量％であるものが好ましい。ここで、揮発性物質とは、ホウ酸、及びホウ酸化合物のことである。揮発性物質の含有量が０．０１質量％未満であると、多孔質成形体の低密度化が不十分となる恐れがあり、０．３質量％をこえると窒化ホウ素焼結体にクラックやワレ等が発生する恐れがある。揮発性物質の含有量の調整は、高めたいときにはホウ酸及び/又はホウ酸化合物を添加すればよく、低めたいときには、窒素、アルゴン等の不活性雰囲気気中、８００〜１５００℃で加熱すればよい。 As the boron nitride powder, a commercially available product is sufficient and there is no particular limitation. The volatile substance content in the boron nitride powder is preferably 0.01 to 0.3% by mass. Here, volatile substances are boric acid and boric acid compounds. If the content of the volatile substance is less than 0.01% by mass, the density of the porous molded body may be insufficiently reduced. If the content exceeds 0.3% by mass, the boron nitride sintered body may be cracked or cracked. There is a risk of cracking. To adjust the content of volatile substances, boric acid and / or a boric acid compound may be added when it is desired to be increased, and when it is desired to be lowered, heating is performed at 800 to 1500 ° C. in an inert atmosphere such as nitrogen or argon. Good.
本発明の窒化ホウ素焼結体は、窒化ホウ素粉末とアクリル系樹脂を含む混合物を成型した後、アクリル系樹脂を除去して多孔質成形体となし、それを焼結することによって製造することができる。 The boron nitride sintered body of the present invention can be manufactured by molding a mixture containing boron nitride powder and an acrylic resin, removing the acrylic resin to form a porous molded body, and sintering the mixture. it can.
窒化ホウ素粉末とアクリル系樹脂の混合には、例えばジューサーミキサー、ヘンシェルミキサー、Ｖブレンダー、ボールミル等の混合装置が使用される。混合にあたっては、例えばポリエチレングリコール、グリセリン等の可塑剤、例えばポリオキシエチレンアルキルエーテル、ポリオキシエチレン脂肪酸エステル等の離型剤を、窒化ホウ素粉末１００質量部に対し最大５質量部まで添加することができる。 For mixing the boron nitride powder and the acrylic resin, for example, a mixing device such as a juicer mixer, a Henschel mixer, a V blender, or a ball mill is used. In mixing, for example, a plasticizer such as polyethylene glycol or glycerin, for example, a release agent such as polyoxyethylene alkyl ether or polyoxyethylene fatty acid ester may be added up to 5 parts by mass with respect to 100 parts by mass of boron nitride powder. it can.
混合物の成型は、乾式プレス成形、冷間等方圧プレス成形法（ＣＩＰ法）等が用いられる。成形圧力は、アクリル系樹脂除去後の多孔質成形体の密度を０．９〜１．２ｇ／ｃｍ３とするため、２０〜５０ＭＰａ、特に２５〜４０ＭＰａの範囲で選択することが望ましい。成型圧力が２０ＭＰａ未満では、後でアクリル系樹脂を除去した多孔質成形体の密度が０．９ｇ／ｃｍ３未満になりやすく、また５０ＭＰａをこえると、アクリル系樹脂の染みだしによって多孔質成形体の密度が１．２ｇ／ｃｍ３よりも大きくなる恐れがある。 For the molding of the mixture, a dry press molding, a cold isostatic press molding method (CIP method) or the like is used. The molding pressure is preferably selected in the range of 20 to 50 MPa, particularly 25 to 40 MPa in order to adjust the density of the porous molded body after removing the acrylic resin to 0.9 to 1.2 g / cm 3 . When the molding pressure is less than 20 MPa, the density of the porous molded body from which the acrylic resin is removed later tends to be less than 0.9 g / cm 3 , and when the molding pressure exceeds 50 MPa, the porous molded body is caused by the oozing of the acrylic resin. There is a possibility that the density of the above becomes larger than 1.2 g / cm 3 .
アクリル系樹脂の除去は、例えば窒素ガス、空気等の気流中、３５０〜７００℃で３〜１２時間加熱することによって行うことができる。アクリル系樹脂として、エマルジョン又は溶液を用いたときは、溶剤の除去と同時にアクリル系樹脂の除去を行うこともできる。この段階で密度が０．９〜１．２ｇ／ｃｍ３との多孔質成形体となる。 The acrylic resin can be removed by heating at 350 to 700 ° C. for 3 to 12 hours in an air flow such as nitrogen gas or air. When an emulsion or a solution is used as the acrylic resin, the acrylic resin can be removed simultaneously with the removal of the solvent. At this stage, a porous molded body having a density of 0.9 to 1.2 g / cm 3 is obtained.
ついで、多孔質成形体は窒素、アルゴンなどの非酸化性雰囲気下、温度１８００〜２３００℃、特に１９００〜２２００℃で常圧焼結されて、嵩密度が０．７〜０．９ｇ／ｃｍ３、熱伝導率が２０Ｗ／ｍ・Ｋ以下の窒化ホウ素焼結体が製造される。焼結温度が１８００℃未満であると、多孔質成形体中の揮発性物質を十分に除去することができなり、窒化ホウ素焼結体の嵩密度が０．９ｇ／ｃｍ３をこえる恐れがある。また、焼結温度が２３００℃をこえると、窒化ホウ素が分解する恐れがある。 Next, the porous molded body is sintered under normal pressure at a temperature of 1800 to 2300 ° C., particularly 1900 to 2200 ° C. in a non-oxidizing atmosphere such as nitrogen and argon, and a bulk density of 0.7 to 0.9 g / cm 3. A boron nitride sintered body having a thermal conductivity of 20 W / m · K or less is manufactured. When the sintering temperature is less than 1800 ° C., volatile substances in the porous molded body cannot be sufficiently removed, and the bulk density of the boron nitride sintered body may exceed 0.9 g / cm 3. . Further, when the sintering temperature exceeds 2300 ° C., boron nitride may be decomposed.
熱伝導率は、窒化ホウ素粉末の粒子径、常圧焼結の保持時間などによって調整することができる。窒化ホウ素粉末の粒子径が大きくなると熱伝導率が高くなりすぎるので、例えばボールミルなどにより原料粉末をあらかじめ粉砕しておき、平均粒径を１５μｍ以下、特に１０μｍ以下に調整しておくことが好ましい。また、焼結温度１８００〜２３００℃における保持時間が長くなると、窒化ホウ素粒子の成長が過大となって熱伝導率が高くなりすぎ、一方、保持時間が短すぎると、焼結が不足し強度が低下する恐れがあるので、保持時間は１〜５時間とすることが好ましい。 The thermal conductivity can be adjusted by the particle size of the boron nitride powder, the holding time of atmospheric pressure sintering, and the like. Since the thermal conductivity becomes too high when the particle size of the boron nitride powder becomes large, it is preferable to pulverize the raw material powder in advance by, for example, a ball mill and adjust the average particle size to 15 μm or less, particularly 10 μm or less. Further, if the holding time at a sintering temperature of 1800 to 2300 ° C. becomes long, the growth of boron nitride particles becomes excessive and the thermal conductivity becomes too high. On the other hand, if the holding time is too short, the sintering becomes insufficient and the strength becomes high. Since there exists a possibility that it may fall, it is preferable that holding time shall be 1 to 5 hours.
実施例１
市販の六方晶窒化ホウ素粉末（電気化学工業社製商品名「デンカボロンナイトライド」グレード名「ＳＧＰＳ」、比表面積：３ｍ２／ｇ、平均粒径：１３μｍ、Ｂ２Ｏ３含有量：０．０１質量％）１００ｇと、市販のアクリル樹脂エマルジョン（大日本インキ社製商品名「ＮＣＢ−１５６」）を固形分として２０ｇとをジューサーミキサーで混合し、１２０℃で１０時間乾燥した00。得られた混合粉末をプレス成型機にて４０ＭＰａで成型し、空気気流中、温度４５０℃で６時間保持してアクリル樹脂を除去し、多孔質成形体（密度が１．１ｇ／ｃｍ３）とした。これを窒素雰囲気下、温度２０００℃で３時間の常圧焼結を行った。その結果、嵩密度が０．７８ｇ／ｃｍ３、熱伝導率が１０．５Ｗ／ｍ・Ｋの窒化ホウ素焼結体が得られた。
Example 1
Commercially available hexagonal boron nitride powder (trade name “DENCABORON NITRIDE” manufactured by Denki Kagaku Kogyo Co., Ltd., grade name “SGPS”, specific surface area: 3 m 2 / g, average particle size: 13 μm, B 2 O 3 content: 0.00 (01% by mass) 100 g and a commercially available acrylic resin emulsion (trade name “NCB-156” manufactured by Dainippon Ink Co., Ltd.) as a solid content and 20 g were mixed with a juicer mixer and dried at 120 ° C. for 10 hours 00. The obtained mixed powder was molded at 40 MPa with a press molding machine, held in an air stream at a temperature of 450 ° C. for 6 hours to remove the acrylic resin, and a porous molded body (density: 1.1 g / cm 3 ). did. This was sintered under normal pressure at a temperature of 2000 ° C. for 3 hours in a nitrogen atmosphere. As a result, a boron nitride sintered body having a bulk density of 0.78 g / cm 3 and a thermal conductivity of 10.5 W / m · K was obtained.
実施例２
アクリル樹脂エマルジョンを固形分として４０ｇとしたこと以外は、実施例１と同様にして窒化ホウ素焼結体を製造した。その結果、嵩密度が０．７1ｇ／ｃｍ３、熱伝導率が９．２Ｗ／ｍ・Ｋの窒化ホウ素焼結体が得られた。
Example 2
A boron nitride sintered body was produced in the same manner as in Example 1 except that the acrylic resin emulsion was 40 g in solid content. As a result, a boron nitride sintered body having a bulk density of 0.71 g / cm 3 and a thermal conductivity of 9.2 W / m · K was obtained.
実施例３
窒化ホウ素粉末として、電気化学工業社製六方晶窒化ホウ素 商品名「デンカボロンナイトライド」グレード名「ＡＰ６５０」 比表面積：３３ｍ２／ｇ、平均粒径：７μｍ、Ｂ２Ｏ３含有量：０．２８質量％）としたこと以外は、実施例１と同様にして窒化ホウ素焼結体を製造した。その結果、嵩密度が０．８５ｇ／ｃｍ３、熱伝導率が７Ｗ／ｍ・Ｋであった。
Example 3
As boron nitride powder, hexagonal boron nitride manufactured by Denki Kagaku Kogyo Co., Ltd. Trade name “DENCABORON NITRIDE” Grade name “AP650” Specific surface area: 33 m 2 / g, average particle size: 7 μm, B 2 O 3 content: 0. A boron nitride sintered body was produced in the same manner as in Example 1 except that the content was 28% by mass). As a result, the bulk density was 0.85 g / cm 3 and the thermal conductivity was 7 W / m · K.
実施例４
アクリル樹脂エマルジョンの変わりに市販のアクリル樹脂の水溶液（ライオン社製商品名「ＡＱ−３３００」）を固形分として１０ｇ用いたこと以外は、実施例１と同様にして窒化ホウ素焼結体を製造した。その結果、嵩密度が０．８４ｇ／ｃｍ３、熱伝導率が１３．０Ｗ／ｍ・Ｋであった。
Example 4
A boron nitride sintered body was produced in the same manner as in Example 1 except that 10 g of a commercially available aqueous solution of acrylic resin (trade name “AQ-3300” manufactured by Lion Corporation) was used as the solid content instead of the acrylic resin emulsion. . As a result, the bulk density was 0.84 g / cm 3 and the thermal conductivity was 13.0 W / m · K.
比較例１
アクリル樹脂エマルジョンの使用量を固形分として８ｇ（窒化ホウ素粉末１００質量部に対し８質量部）に変更したこと以外は、実施例１と同様にして窒化ホウ素焼結体を製造した。その結果、嵩密度が０．９２ｇ／ｃｍ３、熱伝導率は２５Ｗ／ｍ・Ｋであった。
Comparative Example 1
A boron nitride sintered body was produced in the same manner as in Example 1, except that the amount of the acrylic resin emulsion used was changed to 8 g (8 parts by mass with respect to 100 parts by mass of boron nitride powder) as the solid content. As a result, the bulk density was 0.92 g / cm 3 and the thermal conductivity was 25 W / m · K.
比較例２
有機結合材の量を固形分として４５ｇとしたこと以外は、実施例１と同様にして窒化ホウ素焼結体を製造した。その結果、窒化ホウ素焼結体は破損しており、密度は０．６８ｇ／ｃｍ３。焼結体は非常に脆く、熱伝導率は測定できなかった。
Comparative Example 2
A boron nitride sintered body was produced in the same manner as in Example 1 except that the amount of the organic binder was 45 g as a solid content. As a result, the boron nitride sintered body is broken and the density is 0.68 g / cm 3 . The sintered body was very brittle and the thermal conductivity could not be measured.
比較例３
アクリル樹脂エマルジョンの変わりに一般的な有機結合材として粉末状メチルセルロース（信越化学工業社製商品名「メトローズＳＨ」）の１０ｇを窒化ホウ素粉末に混合し、さらに水４０ｇに混合して用いたこと以外は、実施例１と同様にして窒化ホウ素焼結体を製造した。その結果、窒化ホウ素焼結体には直径５ｍｍ程度の空孔が多数認められ、密度は０．８０ｇ／ｃｍ３であった。貫通孔が多数存在したため、熱伝導率は測定できなかった。
Comparative Example 3
Aside from using 10 g of powdered methylcellulose (trade name “Metroze SH” manufactured by Shin-Etsu Chemical Co., Ltd.) as a general organic binder instead of acrylic resin emulsion, mixed with boron nitride powder and further mixed with 40 g of water. Produced a boron nitride sintered body in the same manner as in Example 1. As a result, a large number of pores having a diameter of about 5 mm were observed in the boron nitride sintered body, and the density was 0.80 g / cm 3 . Since there were many through holes, the thermal conductivity could not be measured.
熱伝導率は、市販の測定機（真空理工社製商品名「ＴＣ−７０００」）を用い、試料厚みを２ｍｍに機械加工し、ＪＩＳ Ｒ １６１１に準じレーザーフラッシュ法により測定した。また、嵩密度は、窒化ホウ素焼結体の外寸をノギスにより測定して体積を求め、電子天秤で求めた質量を体積で除すことで算出した。 The thermal conductivity was measured by a laser flash method according to JIS R 1611 using a commercially available measuring machine (trade name “TC-7000” manufactured by Vacuum Riko Co., Ltd.), machining the sample thickness to 2 mm. The bulk density was calculated by measuring the outer dimension of the boron nitride sintered body with calipers to determine the volume, and dividing the mass determined by the electronic balance by the volume.
つぎに、実施例、比較例で製造された窒化ホウ素焼結体が半導体製造装置用断熱部材としての適用可能性を評価するため、環状炉内に焼結体（４０ｍｍφ×１０ｍｍ）を配置し、アンモニア気流中、１４００℃で１時間加熱後、室温への冷却操作を５回繰り返した。実施例１〜４の窒化ホウ素焼結体には破損は認められなかったが、比較例１の窒化ホウ素焼結体では２回目に、比較例２、３の窒化ホウ素焼結体では１回目の操作によりクラックが発生し破損した。 Next, in order to evaluate the applicability of the boron nitride sintered bodies manufactured in Examples and Comparative Examples as a heat insulating member for a semiconductor manufacturing apparatus, a sintered body (40 mmφ × 10 mm) is arranged in an annular furnace, After heating at 1400 ° C. for 1 hour in an ammonia stream, the cooling operation to room temperature was repeated 5 times. No damage was observed in the boron nitride sintered bodies of Examples 1 to 4, but the second time for the boron nitride sintered body of Comparative Example 1 and the first time for the boron nitride sintered bodies of Comparative Examples 2 and 3. The operation caused a crack and was damaged.
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