JPWO2020032067A1 - 結晶性炭化ケイ素繊維、及びその製造方法、並びにセラミックス複合基材 - Google Patents
結晶性炭化ケイ素繊維、及びその製造方法、並びにセラミックス複合基材 Download PDFInfo
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- JPWO2020032067A1 JPWO2020032067A1 JP2020535812A JP2020535812A JPWO2020032067A1 JP WO2020032067 A1 JPWO2020032067 A1 JP WO2020032067A1 JP 2020535812 A JP2020535812 A JP 2020535812A JP 2020535812 A JP2020535812 A JP 2020535812A JP WO2020032067 A1 JPWO2020032067 A1 JP WO2020032067A1
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- silicon carbide
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- crystalline silicon
- carbide fiber
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 185
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- 229910052582 BN Inorganic materials 0.000 claims abstract description 32
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—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
- C04B35/56—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 carbides or oxycarbides
- C04B35/565—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 carbides or oxycarbides based on silicon carbide
- C04B35/571—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 carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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Abstract
Description
AVE4 =(d1+d2+d3+d4)/4
・・・
AVEn−1=(dn−4+dn−3+dn−2+dn−1)/4
AVEn =(dn−3+dn−2+dn−1+dn)/4
AVEn+1=(dn−2+dn−1+dn+dn+1)/4
Δ3=AVE4−AVE3
Δ4=AVE5−AVE4
・・・
Δn−1=AVEn−AVEn−1
Δn =AVEn+1−AVEn
結晶性炭化ケイ素繊維100の製造方法の一例を以下に説明する。本例では、有機ケイ素重合体と有機ホウ素化合物とを含む熱可塑性ポリマー組成物を溶融紡糸して繊維を得る紡糸工程と、当該繊維を、酸素を含む雰囲気中で加熱してポリマー同士を架橋させる不融化工程と、不融化した繊維を、不活性ガス中、800〜1500℃の温度範囲で加熱して、ホウ素を含有する非晶質炭化ケイ素繊維を得る加熱工程と、非晶質炭化ケイ素繊維を、窒素を含む不活性雰囲気中、1550〜2200℃に加熱して、表面部に、深さ方向に向かって炭化ケイ素の含有量が増加し且つ窒化ホウ素の含有量が減少する組成傾斜層を形成する焼成工程と、を有する。
<結晶性炭化ケイ素繊維の調製>
無水キシレン1000重量部にナトリウム400重量部を配合してキシレン溶液を調製した。このキシレン溶液を窒素ガス気流下で加熱還流させながら、キシレン溶液中にジメチルジクロロシラン1034重量部を滴下した。滴下後、10時間加熱還流を継続して沈澱物を生成させた。この沈澱物をろ取した後、メタノ−ル及び水で順次洗浄した。このようにして、白色のポリジメチルシラン420重量部を得た。
得られた結晶性炭化ケイ素繊維を粉砕し、元素分析装置(LECO)及びICP−AESを用いて化学組成を分析した。その結果、Si:68.8重量%、C:30.2重量%、O:0.04重量%、Al:0.23重量%、B:0.23重量%、N:0.51重量%であった。Tiは、検出下限未満であった。結晶性炭化ケイ素繊維の密度は3.09g/cm3であった。この密度から、非晶質炭化ケイ素繊維は、緻密な焼結構造を有することが確認された。また、結晶性炭化ケイ素繊維の表面には、窒化ホウ素が生成していた。
式(2)中、R0は加熱前の結晶性炭化ケイ素繊維の曲率(=ロッドの曲率)であり、Raは加熱後にロッドから取り外した後の結晶性炭化ケイ素繊維の曲率である。結果は、表4に示すとおりであった。
ポリジメチルシラン100重量部に対する有機ホウ素化合物及び有機金属化合物(有機アルミニウム化合物)の一方又は双方の配合量を表2に示すとおりに変更したこと以外は、実施例1と同様にして結晶性炭化ケイ素繊維を調製した。そして、実施例1と同様にして結晶性炭化ケイ素繊維の評価及び分析を行った。結果は表2及び表3に示すとおりであった。なお、表2には、有機金属化合物を構成する金属元素の種類を「有機金属化合物」の右側に記載した。また、表3の「M」は、表2における金属元素である。
焼成工程の加熱温度を2200℃にした以外は、実施例1と同様にして結晶性炭化ケイ素繊維を調製した。そして、実施例1と同様にして結晶性炭化ケイ素繊維の評価及び分析を行った。結果は表2,表3及び表4に示すとおりであった。
有機アルミニウム化合物の代わりに有機イットリウム化合物を用いたこと、及び、ポリジメチルシラン100重量部に対する有機ホウ素化合物及び有機イットリウム化合物の配合量を、それぞれ30重量部及び12重量部としたこと以外は、実施例1と同様にして結晶性炭化ケイ素繊維を調製した。有機イットリウム化合物としては、イットリウムアセチルアセトナートを用いた。そして、実施例1と同様にして結晶性炭化ケイ素繊維の評価及び分析を行った。結果は表2,表3及び表4に示すとおりであった。
ポリジメチルシラン100重量部に対する有機ホウ素化合物及び有機金属化合物(有機イットリウム化合物)の一方又は双方の配合量を表2に示すとおりに変更したこと以外は、実施例8と同様にして結晶性炭化ケイ素繊維を調製した。そして、実施例1と同様にして結晶性炭化ケイ素繊維の評価及び分析を行った。結果は表2,表3及び表4に示すとおりであった。
有機アルミニウム化合物の代わりに有機マグネシウム化合物を用いたこと、及び、ポリジメチルシラン100重量部に対する有機ホウ素化合物及び有機マグネシウム化合物の配合量を、それぞれ30重量部及び12重量部としたこと以外は、実施例1と同様にして結晶性炭化ケイ素繊維を調製した。有機マグネシウム化合物としては、マグネシウムアセチルアセトナートを用いた。そして、実施例1と同様にして結晶性炭化ケイ素繊維の評価及び分析を行った。結果は表2,表3及び表4に示すとおりであった。
ポリジメチルシラン100重量部に対する有機ホウ素化合物及び有機金属化合物(有機マグネシウム化合物)の一方又は双方の配合量を表2に示すとおりに変更したこと以外は、実施例13と同様にして結晶性炭化ケイ素繊維を調製した。そして、実施例1と同様にして結晶性炭化ケイ素繊維の評価及び分析を行った。結果は表2,表3及び表4に示すとおりであった。
有機アルミニウム化合物の代わりに有機ジルコニウム化合物を用いたこと、及び、ポリジメチルシラン100重量部に対する有機ホウ素化合物及び有機ジルコニウム化合物の配合量を、それぞれ30重量部及び12重量部としたこと以外は、実施例1と同様にして結晶性炭化ケイ素繊維を調製した。有機ジルコニウム化合物としては、ジルコニウムアセチルアセトナートを用いた。そして、実施例1と同様にして結晶性炭化ケイ素繊維の評価及び分析を行った。結果は表2,表3及び表4に示すとおりであった。
ポリジメチルシラン100重量部に対する有機ホウ素化合物及び有機金属化合物(有機ジルコニウム化合物)の一方又は双方の配合量を表2に示すとおりに変更したこと以外は、実施例18と同様にして結晶性炭化ケイ素繊維を調製した。そして、実施例1と同様にして結晶性炭化ケイ素繊維の評価及び分析を行った。結果は表2,表3及び表4に示すとおりであった。
焼成工程の加熱温度を2200℃にした以外は、実施例20と同様にして結晶性炭化ケイ素繊維を調製した。そして、実施例1と同様にして結晶性炭化ケイ素繊維の評価及び分析を行った。結果は表2,表3及び表4に示すとおりであった。
有機アルミニウム化合物を配合しなかったこと、及び、ポリジメチルシラン100重量部に対する有機ホウ素化合物の配合量を30重量部としたこと以外は、実施例1と同様にして結晶性炭化ケイ素繊維を調製した。そして、実施例1と同様にして結晶性炭化ケイ素繊維の評価及び分析を行った。結果は表2,表3及び表4に示すとおりであった。
ポリジメチルシラン100重量部に対する有機ホウ素化合物の配合量を表2に示すとおりに変更したこと以外は、実施例1と同様にして結晶性炭化ケイ素繊維を調製した。そして、実施例1と同様にして結晶性炭化ケイ素繊維の評価及び分析を行った。結果は表2,表3及び表4に示すとおりであった。
焼成工程の加熱温度を2200℃にしたこと以外は、実施例27と同様にして結晶性炭化ケイ素繊維を調製した。そして、実施例1と同様にして結晶性炭化ケイ素繊維の評価及び分析を行った。結果は表2,表3及び表4に示すとおりであった。
有機ホウ素化合物を用いなかったこと、及び、焼成工程をアルゴンガス雰囲気中で行ったこと以外は、実施例1と同様にして結晶性炭化ケイ素繊維を調製した。そして、実施例1と同様にして結晶性炭化ケイ素繊維の評価を行った。得られた結晶性炭化ケイ素繊維の化学組成は、Si:69.8重量%、C:29.8重量%、O:0.11重量%、Al:0.19重量%、B:0.14重量%であった。なお、Nは含まれていなかった。結晶性炭化ケイ素繊維の密度は3.00g/cm3であった。
Claims (11)
- 炭化ケイ素と窒化ホウ素とを含有し、
Siの含有量が64〜72重量%、Cの含有量が28〜35重量%、及びBの含有量が0.1〜3.0重量%であり、
表面部に、深さ方向に向かって炭化ケイ素の含有量が増加し且つ窒化ホウ素の含有量が減少する組成傾斜層を備える、結晶性炭化ケイ素繊維。 - 前記組成傾斜層よりも中心側に主成分として炭化ケイ素を含有する本体部を備え、
前記組成傾斜層は、表面側にSiよりもBの原子比率が高いBリッチ部と、前記Bリッチ部よりも前記本体部側にBよりもSiの原子比率が高いSiリッチ部と、を備える、請求項1に記載の結晶性炭化ケイ素繊維。 - 前記Bリッチ部の厚みが30nm以上である、請求項2に記載の結晶性炭化ケイ素繊維。
- 前記Bリッチ部におけるBの原子比率が5原子%以上である、請求項2又は3に記載の結晶性炭化ケイ素繊維。
- 前記組成傾斜層の厚みが30nm以上である、請求項1〜4のいずれか一項に記載の結晶性炭化ケイ素繊維。
- Al、Y、Zr、及びMgからなる群より選ばれる少なくとも一種の元素を含み、
Alを含む場合、その含有量が3.8重量%以下であり、
Yを含む場合、その含有量が3.8重量%以下であり、
Zrを含む場合、その含有量が3.8重量%であり、
Mgを含む場合、その含有量が3.8重量%以下である、請求項1〜5のいずれか一項に記載の結晶性炭化ケイ素繊維。 - ホウ素を含有する非晶質炭化ケイ素繊維を、窒素を含む不活性雰囲気中、1550〜2200℃に加熱して、表面部に、深さ方向に向かって炭化ケイ素の含有量が増加し且つ窒化ホウ素の含有量が減少する組成傾斜層を形成する焼成工程を有し、
Siの含有量が64〜72重量%、Cの含有量が28〜35重量%、及びBの含有量が0.1〜3.0重量%である、結晶性炭化ケイ素繊維の製造方法。 - 前記焼成工程の前に、ホウ素を含有する前記非晶質炭化ケイ素繊維を、窒素とは異なる不活性雰囲気中で1550〜1850℃で加熱して加熱処理物を得る前処理工程を有し、
前記焼成工程では、窒素を含む不活性雰囲気中、前記前処理工程よりも高い温度で前記加熱処理物を加熱する、請求項7に記載の結晶性炭化ケイ素繊維の製造方法。 - 前記焼成工程では、前記加熱処理物を1900〜2200℃に加熱する、請求項8に記載の結晶性炭化ケイ素繊維の製造方法。
- 有機ケイ素重合体と有機ホウ素化合物とを含む熱可塑性ポリマー組成物を溶融紡糸して繊維を得る紡糸工程と、
前記繊維を、酸素を含む雰囲気中で加熱する不融化工程と、
不融化した前記繊維を、不活性ガス中、800〜1500℃の温度範囲で加熱して、前記非晶質炭化ケイ素繊維を得る加熱工程と、を有する、請求項7〜9のいずれか一項に記載の結晶性炭化ケイ素繊維の製造方法。 - セラミックスと、請求項1〜6のいずれか一項に記載の結晶性炭化ケイ素繊維と、を含むセラミックス複合基材。
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