JP5159625B2 - 窒化アルミニウム焼結体およびその製造方法 - Google Patents
窒化アルミニウム焼結体およびその製造方法 Download PDFInfo
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- JP5159625B2 JP5159625B2 JP2008528774A JP2008528774A JP5159625B2 JP 5159625 B2 JP5159625 B2 JP 5159625B2 JP 2008528774 A JP2008528774 A JP 2008528774A JP 2008528774 A JP2008528774 A JP 2008528774A JP 5159625 B2 JP5159625 B2 JP 5159625B2
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- aluminum nitride
- sintered body
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- powder
- volume resistivity
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims description 92
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 239000002245 particle Substances 0.000 claims description 41
- 239000000843 powder Substances 0.000 claims description 39
- 229910052782 aluminium Inorganic materials 0.000 claims description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 27
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 25
- 238000010304 firing Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 14
- 239000011230 binding agent Substances 0.000 claims description 7
- 238000002441 X-ray diffraction Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000004435 EPR spectroscopy Methods 0.000 claims description 3
- 239000011812 mixed powder Substances 0.000 claims 2
- 238000001272 pressureless sintering Methods 0.000 claims 1
- 238000005259 measurement Methods 0.000 description 15
- 239000002184 metal Substances 0.000 description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 230000007547 defect Effects 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- 229910052760 oxygen Inorganic materials 0.000 description 13
- 239000004065 semiconductor Substances 0.000 description 13
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 230000007423 decrease Effects 0.000 description 7
- 238000011156 evaluation Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000008187 granular material Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000006104 solid solution Substances 0.000 description 5
- 238000005238 degreasing Methods 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 4
- 150000002367 halogens Chemical class 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- -1 aluminate compound Chemical class 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000012778 molding material Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 229940048086 sodium pyrophosphate Drugs 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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Description
本発明における窒化アルミニウム焼結体のESRによる測定で磁場336mT以上342mT以下におけるスピン濃度が1×1015spins/cm3以上1×1020spins/cm3以下、好ましくは1×1016spins/cm3以上1×1019spins/cm3以下である。本発明者らは、室温レベルではスピン濃度の増加に伴い体積抵抗率は低下するという知見を得た。即ち、スピン濃度が1015spins/cm3より小さい場合、体積抵抗率は大きくなり1013Ω・mを超え、1×1020spins/cm3より大きい場合は、体積抵抗率は小さくなり108Ω・mを下回る。一方、500℃程度の高温域ではスピン濃度によらず、体積低効率が108Ω・m以上1012Ω・m以下となる。従って、静電チャック等に用いた場合でも、使用温度域である室温から数百度の温度まで安定した物性を示す。
本発明において、窒化アルミニウム焼結体は、後述するようないくつかの条件を満たすことにより、個別の要件自体は公知の方法によって作製することができる。具体的には、窒化アルミニウム(AlN)粉末と所定量のα−アルミナ粉末からなる焼成用粉末を有機バインダーと混合して造粒粉末或いはペーストなどの成形用材料を調製し、この成形材料を既知の成形方法にて成形し、得られた成形体を脱脂し、焼成することにより作製することができる。
得られる窒化アルミニウム焼結体中のアルミニウム以外の金属総含有量を少なくするために、当該α−アルミナとしても高純度のものを使用することが好ましい。好ましくは純度99%以上であり、より好ましくは99.5%以上である。
なお、上記原料として用いる窒化アルミニウムおよびα−アルミナの平均粒径は、レーザー回折法により測定される個数平均粒子径である。
(1)XRD測定
φ15mm×t1mmの試料片を作製し、(株)リガク製X線回折分析装置RINT1200を用いて測定した。その後、窒化アルミニウム[100]回折ピーク(2θ=33.2°)のピーク面積S1と2θ=34°以上35°以下の回折ピークのピーク面積S2(積分強度)よりS2/S1を算出した。
2mm×2mm×20mmの試料片を焼結体より切り出し、日本電子(株)製電子スピン共鳴装置JES−FE1XGにて測定した。得られたスペクトルを解析ソフト(Thermo Galactic社GRAMS)を用いて積分曲線を求めた後、前述のソフトにてガウス曲線に従うようにピーク分離処理をした後、磁場336mT以上342mT以下のピーク面積を求め、スピン量既知サンプルのピーク面積との比より、スピン量を求め、測定サンプルの体積で除した値をスピン濃度とした。
35mm×35mm×1mmの試料片を焼結体より切り出し、JIS C2141に準拠した方法で、体積抵抗率測定装置(株)アドバンテスト製R8340にて測定を行った。
窒化アルミニウム焼結体の任意の場所より5mm×5mm×1mmの試料片を切出し、走査型電子顕微鏡FEI製Quanta200により1000倍以上10000倍以下の倍率で観察した。
(5)原料の平均粒子径測定
原料粉末を超音波ホモジナイザー(株)日本精機製作所製US−300Tにて、5wt%ピロリン酸ソーダ溶液中に分散させて希薄分散液を調製し、これをレーザー回折粒度分布測定器(MICROTRAC HRA、日機装(株)製)にて測定して個数平均粒子径を求めた。
窒化アルミニウム粉末((株)トクヤマ製、平均粒径1.0μm、金属総濃度240ppm)100質量部に対してα−アルミナ粉末(住友化学(株)製、平均粒径0.6μm、窒化アルミニウム粉末平均粒径に対する比0.6)2質量部、有機バインダー4質量部を加えトルエン/エタノール中で混合した後、スプレードライヤーにて造粒し、70μmの顆粒を得た。
α−アルミナの添加量を変えた以外は、実施例1と同様の方法にて、窒化アルミニウム焼結体を得た。焼結体製造条件を表1に、焼結体評価結果を表2に示す。
α−アルミナの粒子径を変えた以外は、実施例1と同様の方法にて、窒化アルミニウム焼結体を得た。焼結体製造条件を表1に、焼結体評価結果を表2に示す。
焼成温度を変えた以外は、実施例1と同様の方法にて、窒化アルミニウム焼結体を得た。焼結体製造条件を表1に、焼結体評価結果を表2に示す。
焼成時間を変えた以外は、実施例1と同様の方法にて、窒化アルミニウム焼結体を得た。焼結体製造条件を表1に、焼結体評価結果を表2に示す。
窒化アルミニウム粉末およびα−アルミナ粉末の平均粒径を変えた以外は、実施例1と同様の方法にて、窒化アルミニウム焼結体を得た。焼結体製造条件を表1に、焼結体評価結果を表2に示す。
窒化アルミニウム粉末((株)トクヤマ製、平均粒径1.0μm)100質量部に対してα−アルミナ粉末(住友化学(株)製、平均粒径0.6μm、窒化アルミニウム粉末平均粒径に対する比0.6)0.1質量部、有機バインダー4質量部を加えトルエン/エタノール中で混合した後、スプレードライヤーにて造粒し、70μmの顆粒を得た。
窒化アルミニウム粉末((株)トクヤマ製、平均粒径1.0μm)100質量部に対してα−アルミナ粉末(住友化学(株)製、平均粒径0.6μm、窒化アルミニウム粉末平均粒径に対する比0.6)20質量部、有機バインダー4質量部を加えトルエン/エタノール中で混合した後、スプレードライヤーにて造粒し、70μmの顆粒を得た。
窒化アルミニウム粉末またはα−アルミナ粉末の平均粒径を変えることによりα−アルミナ粉末平均粒径の窒化アルミニウム粉末平均粒径に対する比を変えた以外は、実施例1と同様の方法にて、窒化アルミニウム焼結体を得た。焼結体製造条件を表1に、焼結体評価結果を表2に示す。
α−アルミナの添加量を変えた以外は、実施例1と同様の方法にて、窒化アルミニウム焼結体を得た。焼結体製造条件を表1に、焼結体評価結果を表2に示す。
Claims (4)
- X線回折における、窒化アルミニウム結晶面[100]の回折ピークのピーク面積S1に対する、酸窒化アルミニウム相に相当する2θ=34°以上35°以下の回折ピークのピーク面積S2の比S2/S1が0.01以上0.3以下であり、且つ、電子スピン共鳴法による測定で磁場336mT以上342mT以下におけるスピン濃度が1×1015spins/cm3以上1×1020spins/cm3以下であり、且つ、アルミニウム以外の金属元素の総含有量が400ppm以下であることを特徴とする窒化アルミニウム焼結体。
- 焼結助剤を実質的に含有しない、請求項1に記載の窒化アルミニウム焼結体。
- 温度25℃以上500℃以下における体積抵抗率が1×108Ω・cm以上1×1012Ω・cm以下である請求項1に記載の窒化アルミニウム焼結体。
- 窒化アルミニウム粉末と、平均粒子径が0.3μm以上2μm以下であり、且つ、該窒化アルミニウム粉末に対する平均粒子径比が0.3以上0.8以下の範囲にある、α−アルミナ粉末とを焼結成分とする混合粉末を常圧焼結する方法であって、
窒化アルミニウム粉末100質量部に対して、α−アルミナ粉末を0.5質量部以上5質量部以下添加することで混合粉末を形成し、
窒素雰囲気下、1800℃以上1950℃以下で、30時間以上100時間以下、常圧焼成する、窒化アルミニウム焼結体の製造方法。
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JP5225043B2 (ja) * | 2008-11-26 | 2013-07-03 | 京セラ株式会社 | 静電チャック |
JP5527821B2 (ja) * | 2010-12-03 | 2014-06-25 | 信越化学工業株式会社 | 耐蝕性部材 |
TWI583622B (zh) * | 2012-09-07 | 2017-05-21 | 德山股份有限公司 | 耐水性氮化鋁粉末之製造方法 |
WO2014123247A1 (ja) * | 2013-02-08 | 2014-08-14 | 株式会社トクヤマ | 窒化アルミニウム粉末 |
EP3858803A4 (en) * | 2018-09-27 | 2022-05-11 | Sumitomo Electric Hardmetal Corp. | POLYCRYSTALLINE BODY OF CUBIC BORON NITRIDE AND METHOD FOR PRODUCTION |
KR102270157B1 (ko) * | 2020-12-24 | 2021-06-29 | 한국씰마스타주식회사 | 산질화알루미늄 세라믹 히터 및 그 제조 방법 |
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KR101101214B1 (ko) | 2012-01-04 |
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JPWO2008018302A1 (ja) | 2009-12-24 |
US20090311162A1 (en) | 2009-12-17 |
KR20090040430A (ko) | 2009-04-24 |
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