JPWO2008093871A1 - 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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- JPWO2008093871A1 JPWO2008093871A1 JP2008556214A JP2008556214A JPWO2008093871A1 JP WO2008093871 A1 JPWO2008093871 A1 JP WO2008093871A1 JP 2008556214 A JP2008556214 A JP 2008556214A JP 2008556214 A JP2008556214 A JP 2008556214A JP WO2008093871 A1 JPWO2008093871 A1 JP WO2008093871A1
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- Prior art keywords
- sintered body
- aluminum nitride
- oxygen
- nitride sintered
- concentration
- 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.)
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 96
- 238000004519 manufacturing process Methods 0.000 title claims description 38
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 106
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 106
- 239000001301 oxygen Substances 0.000 claims abstract description 106
- 239000000843 powder Substances 0.000 claims abstract description 68
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 27
- 150000004645 aluminates Chemical class 0.000 claims description 27
- 229910052799 carbon Inorganic materials 0.000 claims description 23
- 239000002184 metal Substances 0.000 claims description 23
- 239000012535 impurity Substances 0.000 claims description 12
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 9
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 7
- 150000002910 rare earth metals Chemical class 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 5
- 150000001342 alkaline earth metals Chemical group 0.000 claims description 3
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 3
- 238000005245 sintering Methods 0.000 abstract description 50
- 239000002994 raw material Substances 0.000 abstract description 34
- 239000002131 composite material Substances 0.000 abstract description 23
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 description 50
- 238000000034 method Methods 0.000 description 32
- 239000012298 atmosphere Substances 0.000 description 15
- 238000010304 firing Methods 0.000 description 13
- 238000000465 moulding Methods 0.000 description 13
- 238000005092 sublimation method Methods 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 150000004767 nitrides Chemical class 0.000 description 12
- 239000010408 film Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 6
- 229910002091 carbon monoxide Inorganic materials 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000005121 nitriding Methods 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 230000002829 reductive effect Effects 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 238000005238 degreasing Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 2
- -1 aluminate salt Chemical class 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- HIGRAKVNKLCVCA-UHFFFAOYSA-N alumine Chemical compound C1=CC=[Al]C=C1 HIGRAKVNKLCVCA-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000002109 crystal growth method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 150000002314 glycerols Chemical class 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical class OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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Abstract
Description
また、スプレードライ法によりスラリーを噴霧し、顆粒を作製した後、プレス成形法により成形体を得ることもできる。
1)残留酸素の濃度(付着酸素を含む)
(株)堀場製作所製 酸素・窒素同時分析装置(EMGA−550A)を用いて、不活性ガス中でインパルス加熱融解法によりAlNを融解して抽出された酸素を一酸化炭素の形態として、この一酸化炭素を非分散赤外線検出器にて測定した。キャリアガスとしてHeガス(純度:99.995%以上)を用いた。
2)残留酸素の濃度(付着酸素を除く)
(株)堀場製作所製 酸素・窒素同時分析装置(EMGA−620W/C)を用いて室温〜3000℃の温度範囲における酸素および窒素の昇温脱離スペクトルを得て、付着酸素と結晶粒界及び結晶中に固溶した酸素とを分離した。1100℃以下で検出される酸素を付着酸素とした。
3)金属濃度
AlNセラミックスの粉砕粉末に硝酸及びリン酸を加え加熱分解し、島津製作所製ICPS−1000−IIを用いてICP発光分光分析法によりAlNセラミックス中の不純物金属(Al以外の金属)濃度を測定した。
4)残留炭素の濃度
(株)堀場製作所製 金属中炭素分析装置(EMIA−110)を用いて、AlNセラミックスの粉砕粉末を酸素気流中で燃焼させた。生成したガス中の二酸化炭素を非分散型赤外線検出器で検出し炭素濃度を測定した。
内容積が2.4Lのナイロン製ポットに、鉄心をナイロンで被覆した、直径15mmのナイロンボール(表面硬度100kgf/mm2以下、密度3.5g/cm3)を入れ、次いで、還元窒化法により製造された、平均粒径が1.3μm、比表面積が3.39m2/g、酸素濃度(付着酸素を含む。)0.8wt%、金属元素濃度35ppmのAlN粉末100重量部に対して、焼結助剤粉末として平均粒径が1.8μm、比表面積が3.75m2/gのカルシウムアルミネート化合物(Ca3Al2O6)をAlN粉末中の酸素1molに対してカルシウム原子のモル数が0.6molになるように添加し、次いで、エタノールを溶媒として40重量部加えて湿式混合した。この時、前記ナイロンボールはポットの内容積の40%(見かけの体積)充填した。混合はポットの回転数70rpmで3時間行った。更に、得られたスラリーを乾燥して窒化アルミニウム粉末を得た。
焼結助剤中のカルシウム原子モル数をAlN粉末中の酸素1molに対して0.9molとしたこと以外は、実施例1と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼結助剤中のカルシウム原子モル数をAlN粉末中の酸素1molに対して1.2molとしたこと以外は、実施例1と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼結助剤中のカルシウム原子モル数をAlN粉末中の酸素1molに対して1.5molとしたこと以外は、実施例1と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼結助剤中のカルシウム原子モル数をAlN粉末中の酸素1molに対して2.1molとしたこと以外は、実施例1と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼成時間を30時間としたこと以外は、実施例3と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼成時間を100時間としたこと以外は、実施例3と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼成温度を1800℃としたこと以外は、実施例3と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼結助剤をCaO・Al2O3としたこと以外は、実施例3と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼成温度を2000℃としたこと以外は、実施例3と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
AlN粉末として、気相法により製造された、平均粒径が1.7μm、比表面積が2.0m2/g、酸素濃度(付着酸素を含む。)0.6wt%、金属元素濃度34ppmのAlN粉末を用いたこと以外は、実施例3と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼結助剤を添加しないこと以外は、実施例1と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼結助剤中のカルシウム原子モル数をAlN粉末中の酸素1molに対して0.15molとしたこと以外は、実施例1と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼結助剤中のカルシウム原子モル数をAlN粉末中の酸素1molに対して3molとしたこと以外は、実施例1と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼成温度を1680℃としたこと以外は、実施例3と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼結助剤をY2O3としたこと以外は、実施例3と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼結助剤をY2O3とし、焼成雰囲気を中性雰囲気にて焼成したこと以外は、実施例3と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
焼成雰囲気を中性雰囲気にて焼成したこと以外は、実施例3と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
AlN粉末として、直接窒化法により製造された、平均粒径が1.6μm、比表面積が3.7m2/g、酸素濃度(付着酸素を含む。)1.2wt%、金属元素濃度130ppmのAlN粉末を用いたこと以外は、実施例3と同様の操作を行った。窒化アルミニウム焼結体の製造条件及び得られた窒化アルミニウム焼結体の特性を表1に示す。
Claims (7)
- 付着酸素を除く残留酸素の濃度が350ppm以下である窒化アルミニウム焼結体。
- 残留酸素(付着酸素を含む。)の濃度が700ppm以下であり、アルミニウム以外の金属元素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。
- アルミニウム以外の金属元素の濃度が合計で100ppm以下である請求項2に記載の窒化アルミニウム焼結体。
- 希土類金属元素の濃度が1ppm以下である請求項2または3に記載の窒化アルミニウム焼結体。
- 残留酸素の濃度が0.9%以下である窒化アルミニウム粉末と、該粉末中に含まれる酸素原子1モル当り0.6〜2.1モルのアルカリ土類金属原子を含むアルカリ土類アルミン酸塩とを含有する混合粉末を所定の形状に成形後、この成形体をカーボン製容器中に収納し、直接カーボンに触れることなく載置して、温度1700〜2100℃にて10〜100時間焼結することを特徴とする請求項1〜4のいずれかに記載の窒化アルミニウム焼結体の製造方法。
- 窒化アルミニウム粉末の、アルミニウム以外の不純物金属元素の濃度が50ppm以下である請求項5に記載の窒化アルミニウム焼結体の製造方法。
- 前記アルカリ土類アルミン酸塩が3CaO・Al2O3である請求項5または6に記載の窒化アルミニウム焼結体の製造方法。
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JP2010076995A (ja) * | 2008-09-29 | 2010-04-08 | Denki Kagaku Kogyo Kk | 3−5族化合物半導体の製造装置用サセプタ部材およびその製造方法 |
JP5258650B2 (ja) * | 2009-03-25 | 2013-08-07 | 株式会社トクヤマ | 窒化アルミニウム焼結体の製造方法 |
DE102009016133B4 (de) * | 2009-04-03 | 2012-12-20 | Sicrystal Ag | Herstellungsverfahren für einen sauerstoffarmen AlN-Volumeneinkristall |
JP5495748B2 (ja) * | 2009-12-10 | 2014-05-21 | 株式会社トクヤマ | 窒化アルミニウム粉末 |
WO2012056807A1 (ja) * | 2010-10-25 | 2012-05-03 | 日本碍子株式会社 | セラミックス材料、積層体、半導体製造装置用部材及びスパッタリングターゲット部材 |
TWI450855B (zh) * | 2011-08-04 | 2014-09-01 | 高純度氮化鋁製造方法 | |
KR102431063B1 (ko) * | 2017-05-22 | 2022-08-09 | 도요 알루미늄 가부시키가이샤 | 질화알루미늄계 분말 및 그 제조방법 |
JP6932995B2 (ja) * | 2017-05-23 | 2021-09-08 | Tdk株式会社 | 窒化物の単結晶 |
JP6725115B2 (ja) * | 2017-12-25 | 2020-07-15 | 昭和電工株式会社 | アルミナ焼結体、砥粒、及び砥石 |
KR20200081969A (ko) | 2018-12-28 | 2020-07-08 | 한국세라믹기술원 | 질화알루미늄 소결용 조성물 및 질화알루미늄 소결체 |
KR102205085B1 (ko) | 2018-12-31 | 2021-01-19 | 한국세라믹기술원 | 고강도 질화알루미늄 소결용 조성물 및 고강도 질화알루미늄 소결체 |
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KR102299212B1 (ko) | 2019-10-22 | 2021-09-09 | 한국세라믹기술원 | 고강도 질화알루미늄 소결체 |
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JP2856734B2 (ja) | 1987-01-13 | 1999-02-10 | 株式会社東芝 | 高熱伝導性窒化アルミニウム焼結体 |
US4847221A (en) | 1987-01-13 | 1989-07-11 | Kabushiki Kaisha Toshiba | AlN sintered body having high thermal conductivity and a method of fabricating the same |
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