JP2003073794A - 耐熱性被覆部材 - Google Patents
耐熱性被覆部材Info
- Publication number
- JP2003073794A JP2003073794A JP2001354673A JP2001354673A JP2003073794A JP 2003073794 A JP2003073794 A JP 2003073794A JP 2001354673 A JP2001354673 A JP 2001354673A JP 2001354673 A JP2001354673 A JP 2001354673A JP 2003073794 A JP2003073794 A JP 2003073794A
- Authority
- JP
- Japan
- Prior art keywords
- rare earth
- oxide
- earth element
- heat
- main component
- 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.)
- Pending
Links
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 50
- 239000012298 atmosphere Substances 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 35
- 239000000919 ceramic Substances 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 18
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 10
- 239000000956 alloy Substances 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 7
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 6
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 5
- 239000010410 layer Substances 0.000 claims description 29
- 239000011248 coating agent Substances 0.000 claims description 24
- 238000000576 coating method Methods 0.000 claims description 24
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 229910052772 Samarium Inorganic materials 0.000 claims description 5
- 229910052691 Erbium Inorganic materials 0.000 claims description 4
- 230000000737 periodic effect Effects 0.000 claims description 4
- 239000002356 single layer Substances 0.000 claims description 4
- 229910052775 Thulium Inorganic materials 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052771 Terbium Inorganic materials 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 9
- 230000007797 corrosion Effects 0.000 abstract description 7
- 238000005260 corrosion Methods 0.000 abstract description 7
- 239000011225 non-oxide ceramic Substances 0.000 abstract 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 abstract 1
- 239000011224 oxide ceramic Substances 0.000 abstract 1
- 229910052574 oxide ceramic Inorganic materials 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 12
- 230000004888 barrier function Effects 0.000 description 8
- 239000011247 coating layer Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 230000003746 surface roughness Effects 0.000 description 6
- 239000010936 titanium Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 2
- 229910052689 Holmium Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005422 blasting Methods 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 150000001247 metal acetylides Chemical class 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000007750 plasma spraying Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 1
- 102100033029 Carbonic anhydrase-related protein 11 Human genes 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910000599 Cr alloy Inorganic materials 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 101000867841 Homo sapiens Carbonic anhydrase-related protein 11 Proteins 0.000 description 1
- 101001075218 Homo sapiens Gastrokine-1 Proteins 0.000 description 1
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- 229910001199 N alloy Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000010285 flame spraying Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- -1 oxides Chemical class 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910003468 tantalcarbide Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
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- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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- C04B35/505—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds based on yttrium oxide
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
- C04B41/5045—Rare-earth oxides
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- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
ーボン及びそれらの合金並びにそれらの酸化物系セラミ
ックス、非酸化物系セラミックス及び炭化物系材料から
選ばれる材質を有する基材が、希土類元素含有酸化物を
主成分とする層で被覆されていることを特徴とする耐熱
性被覆部材。 【効果】 本発明の耐熱性被覆部材は、耐熱性、耐蝕
性、非反応性が良好で、真空、不活性雰囲気又は還元雰
囲気下での金属又はセラミックスを焼結又は熱処理する
のに有効に用いられるものである。
Description
性雰囲気又は還元雰囲気下において金属又はセラミック
スの焼結又は熱処理を行う際に使用する耐熱性被覆部材
に関するものである。
金製品は、一般に主合金にバインダー相を形成する粉末
を混ぜ合わせ、混合物の混練、加圧成形、及び焼結、後
加工により製造される。ここで、焼結工程においては、
真空雰囲気中や不活性ガス雰囲気中で、1000℃〜1
600℃の高温で焼結が行われる。
グステンとコバルト、炭化チタン、炭化タンタル等の固
溶体を粉砕、混合した後、乾燥、造粒工程を経て造粒粉
を作製し、次いでプレス成形を行う。その後、脱ワック
ス、予備焼結、焼結、加工等により超硬合金製品ができ
る。
o系の三元共晶温度は1298℃)以上で行われる。通
常は1350〜1550℃の温度範囲である。焼結で大
切なことは、目的とする炭素量を正確に含有した超硬合
金を安定して焼結しうるように雰囲気を制御することで
ある。
合、カーボン製のトレー上に載せられた成形体試料がト
レーと反応する問題がある。即ち、カーボンが試料に浸
透して試料強度の低下を招く、いわゆる浸炭現象が起こ
る問題である。このような問題を回避するためにトレー
材質を選定したり、トレー表面部に成形体試料と反応し
ない材料のバリアー層を設ける手段が採られている。例
えば、超硬合金材料の焼結の場合、ジルコニアやアルミ
ナ、酸化イットリウム等のセラミック粉が使われてい
る。これらのセラミック粉をトレー上に散布し、敷粉と
して使用したり、セラミック粉を溶剤に混ぜてトレー上
にスプレー塗布したり、粘度の高いスラリーを塗布した
り、或いは、溶射法などによりトレー上に緻密なセラミ
ック皮膜を付着させた被膜を形成させることが行われて
おり(特表2000−509102号公報参照)、トレ
ー表面部にこれらの酸化物層、いわゆるバリアー層を設
けることで、試料との反応も防止していた。
も、トレーと反応が起こり、1、2回の焼結によりバリ
アー層に割れ、剥がれが発生していた。
ントレーと試料との反応が起こりやすくなる。また、焼
結の際、皮膜が剥がれ、微細化して成形体試料に混入す
る恐れを生ずるため、新たなトレーを使用しなくてはな
らない。
用いる場合、試料とバリアー層が反応しないこと、そし
て、バリアー層とトレーとが反応せず、剥がれないこと
が求められ、粉末冶金製品を焼結する場合、何度使用し
ても試料とバリアー層が反応せず、バリアー層とトレー
基板が剥がれない高寿命のトレー材料が望まれている。
れたもので、特に真空、不活性雰囲気又は還元雰囲気下
で金属又はセラミックスを焼結又は熱処理を行う際に耐
熱性、耐蝕性、非反応性に優れ、しかも安価な被覆部材
を提供することを目的とする。
発明者は、上記目的を達成するため鋭意検討を行った結
果、Mo、Ta、W、Zr、Al、Ti、カーボン及び
それらの合金並びにそれらの酸化物系セラミックス、非
酸化物系セラミックス及び炭化物系材料から選ばれる材
質にて形成された基材に希土類元素含有酸化物を主成分
とする層を被覆することにより得られる耐熱性被覆部材
が、特に、真空、不活性雰囲気又は還元雰囲気下で金属
又はセラミックスの焼結又は熱処理を行う際に、優れた
耐熱性、耐蝕性、非反応性を与えることを知見し、本発
明をなすに至った。
W、Zr、Al、Ti、カーボン及びそれらの合金並び
にそれらの酸化物系セラミックス、非酸化物系セラミッ
クス及び炭化物系材料から選ばれる材質を有する基材
が、希土類元素含有酸化物を主成分とする層で被覆され
ていることを特徴とする耐熱性被覆部材、(2) 上記
希土類元素含有酸化物が、Dy、Ho、Er、Tb、G
d、Tm、Yb、Lu、Eu及びSmから選ばれる1種
類以上の元素を主成分とする希土類元素含有酸化物であ
ることを特徴とする(1)に記載の耐熱性被覆部材、
(3) 上記希土類元素含有酸化物が、Yb、Eu及び
Smから選ばれる1種類以上を主成分とする希土類元素
含有酸化物であることを特徴とする(2)に記載の耐熱
性被覆部材、(4) 上記希土類元素含有酸化物を主成
分とする層が、Ybを希土類元素を含む全金属元素の8
0原子%以上の割合で含む希土類元素含有酸化物層であ
ることを特徴とする(1)〜(3)のいずれか1項に記
載の耐熱性被覆部材、(5) 上記希土類元素含有酸化
物を主成分とする層の厚さが0.02mm以上0.4m
m以下であることを特徴とする(1)〜(4)のいずれ
か1項に記載の耐熱性被覆部材、(6) 上記希土類元
素含有酸化物を主成分とする層上に、短周期型周期律表
において3A族〜8族までの元素から選ばれる1種類以
上の元素の化合物の層を単層又は複数層積層させたこと
を特徴とする(1)〜(5)のいずれか1項に記載の耐
熱性被覆部材、(7) 上記基材が密度1.5g/cm
3以上のカーボンで形成されていることを特徴とする
(1)〜(6)のいずれか1項に記載の耐熱性被覆部
材、(8) 真空、不活性雰囲気又は還元雰囲気下での
金属又はセラミックスの焼結に用いる(1)〜(7)の
いずれか1項に記載の耐熱性被覆部材を提供する。
本発明の耐熱性被覆部材は、特に、真空、不活性雰囲気
又は還元雰囲気下で、製品となる金属又はセラミックス
の焼結又は熱処理を行う際に使用されるが、製品や使用
温度や使用ガスの種類によって、被覆酸化物と基材の種
類又は組み合わせを変えて、最適化する必要がある。
に、金属の溶解ルツボや各種複合酸化物を製造・焼結す
るための治具として有効であり、例えばセッター(敷
板)、サヤ、トレー、焼成こう鉢、金型といった部材及
び装置が挙げられる。
処理において使用される耐熱性及び耐蝕性のある部材を
形成するための基材として、本発明ではMo、Ta、
W、Zr、Al、Ti、カーボン及びそれらの合金並び
にそれらの酸化物系、非酸化物系セラミックス及び炭化
物系材料から選ばれる基材を用いるものである。
は、カーボン基材の密度を1.5g/cm3以上、特に
1.6〜1.9g/cm3とすることが好ましい。な
お、カーボンの真密度は2.26g/cm3である。基
材の密度が1.5g/cm3未満では、密度が小さいの
で熱衝撃には強いが、気孔率が高くなり、大気中の水分
・炭酸ガスを吸着しやすく、真空下では吸着した水分・
炭酸ガスを放出する場合がある。また、基材と皮膜の形
成状態を高めるために酸化物層の熱膨張係数を4〜7×
10-6以下にするとよい。
結する場合、1500〜1800℃で、真空、不活性雰
囲気又は弱い還元雰囲気下で処理するが、このように高
温のために、基材物質と皮膜酸化物との反応、及び皮膜
酸化物と製品との反応が起こりやすくなるので、基材物
質と皮膜酸化物との反応、及び皮膜酸化物と製品との反
応が共に起こりにくい組み合わせを選定することが重要
である。特に1500℃以上になると、Alや希土類元
素は、基材にカーボンを用いると、真空や還元雰囲気で
は炭化物になりやすい場合があるので、このような条件
下では、基材としてMo、Ta、Wを用いて、皮膜酸化
物に希土類元素含有酸化物を組み合わせた皮膜形成治具
を用いることが好ましい。
を皮膜酸化物として希土類元素含有酸化物を主成分とす
る層で被覆したものである。
化物は、原子番号57〜71までの希土類元素から選ば
れる希土類元素を含有する酸化物である。このうち、L
a、Ce、Pr、Ndの軽希土類は1500℃前後で結
晶構造の転移があるため、高温で使用する用途には、D
y、Ho、Er、Tm、Yb、Gd、Lu、Eu、Sm
から選ばれる少なくとも1種類以上の希土類元素を含有
する酸化物で被覆されることが好ましく、更にはYb、
Sm、Euから選ばれる1種類以上を含有する酸化物を
用いることが好ましい。また、特に基材との密着力の点
から、Ybを上記希土類元素を含む全金属元素の80原
子%以上の割合で含む酸化物がよい。
期律表において3A族〜8族までの元素から選ばれる金
属(但し、上記希土類元素を除く)の酸化物をこれら他
の金属の単独酸化物換算で0〜20重量%、特に10重
量%以下の割合で含有しても構わない。更に好ましく
は、Al、Si、Zn、Fe、Ti、Mn、V及びYか
ら選ばれる少なくとも1種類以上の金属の酸化物を含有
していてもよい。この場合、これら希土類元素以外の金
属は、希土類元素と複合酸化物を形成していても、これ
ら金属の単独酸化物を形成し、希土類元素含有酸化物や
上記複合酸化物と混合されていてもよい。
0μmの酸化物粒子がよく、上記の基材にアルゴン等の
不活性雰囲気下でプラズマ溶射又はフレーム溶射して本
発明の被覆部材を製造するものである。また必要によ
り、溶射する前に、基材表面にブラスト処理等の表面加
工を施してもよい。
とする層は1層単層でもよく、2層以上の複数層であっ
てもよい。その総厚さは、0.02mm以上0.4mm
以下がよい。より好ましくは0.1mm以上0.2mm
以下が望ましい。0.02mm未満では、繰り返し使用
した場合に、基材と焼結物質が反応する可能性がある。
0.4mmを超えると、被覆酸化物膜内で熱衝撃により
酸化物が剥離し、製品を汚染するおそれが生じる。
酸化物を主成分とする被膜上に短周期型周期律表の3A
族〜8族までの元素から選ばれる1種類以上の元素の化
合物からなる被膜層を単層又は複数層設けることができ
る。このような化合物としては、酸化物、窒化物等がよ
く、好ましくは、Yを含む希土類元素、Al、Ti、Z
r、Mn等の元素からなる化合物の層がよい。但し、Y
以外の希土類元素化合物としては、酸化物以外のもの、
特に窒化物とする。
0.01〜0.1mmの厚さになるように被覆すること
が望ましい。
含有酸化物を主成分とする層、この上に上記被覆層が形
成されている場合は該被覆層)の表面粗さ(Ra)が2
μm以上になるように形成し、必要により研磨等の表面
加工を施してもよい。製造される焼結体の焼結性の点か
ら、表面粗さ(Ra)は2μm以上30μm以下、更に
好ましくは3〜10μmが望ましい。表面粗さ(Ra)
が2μm未満では、被覆物層が平坦なため、被覆物層の
上にある被処理物が焼結収縮するのを邪魔する場合があ
る。
の金属、セラミックスを1800℃以下、更に好ましく
は900〜1700℃で1〜50時間加熱又は焼結する
ことがよく、雰囲気は真空又は酸素分圧0.01MPa
以下の不活性雰囲気又は還元雰囲気下であるのがよい。
理して得られるものであればよく、Cr合金、Mo合
金、炭化タングステン、炭化珪素、窒化珪素、ホウ化チ
タン、希土類−アルミニウム複合酸化物、希土類−遷移
金属合金、チタン合金、希土類元素含有酸化物、希土類
複合酸化物等が挙げられ、特に炭化タングステン、希土
類元素含有酸化物、希土類−アルミニウム複合酸化物、
希土類−遷移金属合金の製造において、本発明の治具等
の部材は有効である。具体的には、YAG等の透光性セ
ラミックスや炭化タングステン等の超硬材、焼結磁石に
用いるSm−Co系合金、Nd−Fe−B系合金、Sm
−Fe−N系合金の製造や焼結磁歪材に用いるTb−D
y−Fe合金や焼結蓄冷材に用いるEr−Ni合金の製
造において、本発明の治具等の部材は有効である。
又はN2ガス雰囲気であり、還元雰囲気としては、例え
ば不活性ガスとカーボンヒータを使用した雰囲気、不活
性ガス及び数パーセントの水素ガス混入雰囲気を示す酸
素分圧が0.01MPa以下であり、これらの雰囲気に
より、耐蝕性のある被覆部材が得られる。
蝕性、非反応性が良好で、真空、不活性雰囲気又は還元
雰囲気下での金属又はセラミックスを焼結又は熱処理す
るのに有効に用いられるものである。
発明を具体的に説明するが、本発明は下記の実施例に制
限されるものではない。
50×5mmの形状のMo、Ta、カーボン基材を準備
した。表面をプラズマ溶射する前に、ブラストで表面を
荒らし、次いで、表1に示す所定の組成、平均粒径の希
土類元素含有酸化物粒子を上記基材にアルゴン/水素で
プラズマ溶射することにより、上記基材を希土類元素含
有酸化物からなる層で被覆して、被覆部材を得た。
に示す。組成はICP(セイコーSPS−4000)
で、平均粒径はレーザ回折法(日機装FRA)で測定し
た。また、溶射皮膜の物性値を測定した結果を表2に示
す。溶射膜厚さは光学顕微鏡で断面を撮影した写真から
求めた。表面粗さ(Ra)は表面粗さ計(小阪研究所S
E3500K)で測定した。
00℃/hrの速度で昇温し、所定時間保持した後、4
00℃/hrの速度で冷却した。これを2回繰り返した
後の被覆部材の外観を観察した。結果を表2に示す。
ヒータ炉で熱処理後も処理前と変化はなかった。一方、
比較例1、2の治具は、カーボンヒータ炉での熱処理
後、表面にひびが入ったり、酸化物が剥がれたりしてお
り、腐食が起こっていた。
面積200m2/g)と0.01モルの表3に示す各原
料希土類元素含有酸化物の粉末(平均粒径1〜2μm)
とを、少量のエタノールとともに、乳鉢で十分粉砕混合
し、真空乾燥機中で乾燥して混合粉末を得た。各混合粉
末を、金型で加圧成形し、直径20mmのペレットとし
た。各ペレットを、アルゴン雰囲気中1420℃で2時
間焼成した。焼成後のペレットを手早く打砕して粗粉と
し、各試料について1.5gを密栓可能な試料瓶に採取
した。これに純水0.1cm3ずつ加えて密栓した。し
ばらく置いて平衡に達したのち、試料瓶中の気体をガス
クロマトグラフにかけ、アセチレンの定量を行った。結
果を表3に示す。
属酸化物に比べ、Er、Ybに代表される原子番号の比
較的大きい希土類元素の酸化物は、アセチレンの生成が
少ない。即ち、加水分解性の炭化物の生成が少ない。こ
のことは、炭素上に希土類元素含有酸化物層を被覆した
場合に加熱、冷却、大気開放のサイクルにより界面に炭
化物が生じ、それが加水分解することによって皮膜の密
着力が低下するという現象が起こりにくいことにつなが
る。希土類元素間の挙動の違いの原因の一つはイオン半
径であり、イオン半径が小さい方が炭化物の生成又は加
水分解のいずれか又は両方が起こりにくいのだと思料さ
れる。
が特に少ないのは、イオン半径の小ささに加えてこの元
素が一般の希土類元素と異なり酸化数2の状態を比較的
取り易いことも関係していると思量できる。このことを
検証するために、実施例6と同様にして作成した被覆部
材を高真空中で、光高温計によって1500℃以上と観
測されるまで高周波誘導加熱したところ、微量のYbO
が脱離ガス中に含まれていた。
基材を用意し、平均粒径40μmのYb2O3粒子をアル
ゴン/水素で溶射することにより、0.1mmの溶射被
膜を形成した。更に、平均粒径40μmのEr2O3粒子
を同雰囲気で供給しながら溶射し、0.2mmの被膜部
材を形成した。
60μmのY2O3を用いた以外は実施例13と同様にし
て0.2mmの被膜部材を得た。
Claims (8)
- 【請求項1】 Mo、Ta、W、Zr、Al、Ti、カ
ーボン及びそれらの合金並びにそれらの酸化物系セラミ
ックス、非酸化物系セラミックス及び炭化物系材料から
選ばれる材質を有する基材が、希土類元素含有酸化物を
主成分とする層で被覆されていることを特徴とする耐熱
性被覆部材。 - 【請求項2】 上記希土類元素含有酸化物が、Dy、H
o、Er、Tb、Gd、Tm、Yb、Lu、Eu及びS
mから選ばれる1種類以上の元素を主成分とする希土類
元素含有酸化物であることを特徴とする請求項1に記載
の耐熱性被覆部材。 - 【請求項3】 上記希土類元素含有酸化物が、Yb、E
u及びSmから選ばれる1種類以上を主成分とする希土
類元素含有酸化物であることを特徴とする請求項2に記
載の耐熱性被覆部材。 - 【請求項4】 上記希土類元素含有酸化物を主成分とす
る層が、Ybを希土類元素を含む全金属元素の80原子
%以上の割合で含む希土類元素含有酸化物層であること
を特徴とする請求項1〜3のいずれか1項に記載の耐熱
性被覆部材。 - 【請求項5】 上記希土類元素含有酸化物を主成分とす
る層の厚さが0.02mm以上0.4mm以下であるこ
とを特徴とする請求項1〜4のいずれか1項に記載の耐
熱性被覆部材。 - 【請求項6】 上記希土類元素含有酸化物を主成分とす
る層上に、短周期型周期律表において3A族〜8族まで
の元素から選ばれる1種類以上の元素の化合物の層を単
層又は複数層積層させたことを特徴とする請求項1〜5
のいずれか1項に記載の耐熱性被覆部材。 - 【請求項7】 上記基材が密度1.5g/cm3以上の
カーボンで形成されていることを特徴とする請求項1〜
6のいずれか1項に記載の耐熱性被覆部材。 - 【請求項8】 真空、不活性雰囲気又は還元雰囲気下で
の金属又はセラミックスの焼結に用いる請求項1〜7の
いずれか1項に記載の耐熱性被覆部材。
Priority Applications (3)
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JP2001354673A JP2003073794A (ja) | 2001-06-18 | 2001-11-20 | 耐熱性被覆部材 |
US10/173,030 US6753085B2 (en) | 2001-06-18 | 2002-06-18 | Heat-resistant coated member |
US10/825,303 US7157148B2 (en) | 2001-06-18 | 2004-04-16 | Heat-resistant coated member |
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JP2001-183510 | 2001-06-18 | ||
JP2001183510 | 2001-06-18 | ||
JP2001354673A JP2003073794A (ja) | 2001-06-18 | 2001-11-20 | 耐熱性被覆部材 |
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2001
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-
2002
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JP2003082402A (ja) * | 2001-09-11 | 2003-03-19 | Toshiba Tungaloy Co Ltd | 硬質焼結合金の焼結用セッター |
US7507481B2 (en) | 2002-11-20 | 2009-03-24 | Shin-Etsu Chemical Co., Ltd. | Heat resistant coated member, making method, and treatment using the same |
JP4716042B2 (ja) * | 2003-03-28 | 2011-07-06 | 信越化学工業株式会社 | 耐熱性被覆部材 |
JP2008019167A (ja) * | 2003-03-28 | 2008-01-31 | Shin Etsu Chem Co Ltd | 耐熱性被覆部材 |
JP2009001485A (ja) * | 2003-03-28 | 2009-01-08 | Shin Etsu Chem Co Ltd | 耐熱性被覆部材 |
JP2004315352A (ja) * | 2003-03-28 | 2004-11-11 | Shin Etsu Chem Co Ltd | 耐熱性被覆部材 |
JP2004332013A (ja) * | 2003-05-01 | 2004-11-25 | Hitachi Tool Engineering Ltd | 被覆グラファイトトレー |
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JP2005042145A (ja) * | 2003-07-24 | 2005-02-17 | Toshiba Ceramics Co Ltd | プラズマ耐食性溶射部材及びその製造方法 |
TWI404901B (zh) * | 2007-04-30 | 2013-08-11 | Gen Electric | 用以熔化鈦合金之坩堝 |
JP2009019280A (ja) * | 2008-09-26 | 2009-01-29 | Shin Etsu Chem Co Ltd | 超硬材料又はサーメット材料焼結用セッターの製造方法 |
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CN115028438A (zh) * | 2022-04-13 | 2022-09-09 | 江联国际工程有限公司 | 一种电力锅炉耐火涂层的制备方法 |
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US6753085B2 (en) | 2004-06-22 |
US20040191546A1 (en) | 2004-09-30 |
US20030017350A1 (en) | 2003-01-23 |
US7157148B2 (en) | 2007-01-02 |
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