JP4667520B2 - 窒化ケイ素基複合セラミックス及びその製造方法 - Google Patents
窒化ケイ素基複合セラミックス及びその製造方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims description 111
- 239000002131 composite material Substances 0.000 title claims description 98
- 229910052581 Si3N4 Inorganic materials 0.000 title claims description 34
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims description 34
- 238000004519 manufacturing process Methods 0.000 title claims description 17
- 229910052582 BN Inorganic materials 0.000 claims description 46
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 46
- 239000000843 powder Substances 0.000 claims description 42
- 239000002994 raw material Substances 0.000 claims description 40
- 230000003647 oxidation Effects 0.000 claims description 31
- 238000007254 oxidation reaction Methods 0.000 claims description 31
- 230000035939 shock Effects 0.000 claims description 25
- 238000013001 point bending Methods 0.000 claims description 24
- 239000013078 crystal Substances 0.000 claims description 20
- 239000011148 porous material Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 17
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 14
- 238000002441 X-ray diffraction Methods 0.000 claims description 10
- 238000010304 firing Methods 0.000 claims description 10
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 9
- 229910052727 yttrium Inorganic materials 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 229910052765 Lutetium Inorganic materials 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052785 arsenic Inorganic materials 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 229910010293 ceramic material Inorganic materials 0.000 claims description 2
- 239000012071 phase Substances 0.000 description 60
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910003443 lutetium oxide Inorganic materials 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- MPARYNQUYZOBJM-UHFFFAOYSA-N oxo(oxolutetiooxy)lutetium Chemical compound O=[Lu]O[Lu]=O MPARYNQUYZOBJM-UHFFFAOYSA-N 0.000 description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 3
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910003454 ytterbium oxide Inorganic materials 0.000 description 3
- 229940075624 ytterbium oxide Drugs 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 239000000075 oxide glass Substances 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C04B35/584—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 based on silicon nitride
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Description
JIS R1601に準拠した25℃での四点曲げ強度をσi、JIS R1615に準拠した水中投下法によって800℃以上から25℃の水中に投下による急冷で熱衝撃を与えた後の四点曲げ強度をσfとしたとき、σiの値が400MPa以上で、かつσf/σiの比の値が0.85以上であることを特徴とする複合セラミックスを提供するものである。
また本発明は、窒化ケイ素基セラミックスを母相とし、窒化ホウ素が2.5vol.%以上、10vol.%以下の割合で分散相として複合されており、
JIS R1601に準拠した25℃での四点曲げ強度をσ i 、JIS R1615に
準拠した水中投下法によって800℃以上から25℃の水中に投下による急冷で熱衝撃を与えた後の四点曲げ強度をσ f としたとき、σ i の値が400MPa以上で、かつσ f /σ i の比の値が0.85以上であり、
JIS R1601に準拠した1200℃での四点曲げ強度をσ h としたとき、σ h と前記のσ i との比率σ h /σ i が0.85以上であり、
大気中で1300℃又は1400℃・100時間酸化処理した後の複合セラミックスの重量から酸化処理前の重量を差し引き、それを酸化処理前の重量で除して100を乗じた値が0.01〜0.10%であることを特徴とする複合セラミックスを提供するものである。
母相を形成する窒化ケイ素基セラミックス原料粉末と分散相を形成する窒化ホウ素原料粉末を混合して成形し、焼成する工程を含み、
窒化ホウ素原料粉末として、t=0.9λ/(BcosθB)(式中、λはX線管球の波長(nm)を表し、Bは半値幅(rad)を表し、θBは回折角(rad)を表す。)で定義される結晶子サイズが40nm以上、48nm未満のものを用いることを特徴とする複合セラミックスの製造方法を提供するものである。
相対積分強度=シリケート相又はオキシナイトライド相の積分強度/窒化ケイ素母相の積分強度
表1に示す原料粉末を混合し、混合粉末に対して150重量%のエタノールを配合してスラリーとなした。各原料粉末の平均粒径は0.1〜3μmの範囲であった。得られたスラリーをボールミルに充填して混合した。混合完了後、エバポレーターによってエタノールを除去して混合粉末を乾燥した。一軸成形機を用い混合粉末に2MPaの圧力を加えて成形した後、200MPaのCIP成形によって45×45×7tmmのプレートを作製した。このプレートを焼成炉に入れて、9気圧の窒素雰囲気(100%窒素ガス)中、最高1850℃まで昇温し、8時間保持して焼成した。このようにして、目的とする窒化ケイ素基複合セラミックスを得た。
実施例1において用いたYb2O3原料粉末の使用量を25部に増量し、かつSi3N4原料粉末の使用量を70部に減量した。これ以外は実施例1と同様にして複合セラミックスを得た。
実施例1において用いたYb2O3原料粉末の使用量を15部に増量し、かつSi3N4原料粉末の使用量を80部に減量した。これ以外は実施例1と同様にして複合セラミックスを得た。
実施例1において用いたt−BN原料粉末の使用量を5部に増量した。これ以外は実施例1と同様にして複合セラミックスを得た。
実施例1において用いたt−BN原料粉末の使用量を10部に増量した。これ以外は実施例1と同様にして複合セラミックスを得た。
実施例3において用いたt−BN原料粉末として、結晶子サイズが47.3nmのものを用いた。これ以外は実施例3と同様にして複合セラミックスを得た。
実施例3において用いたt−BN原料粉末の使用量を1部に減量した。これ以外は実施例3と同様にして複合セラミックスを得た。
表1に示す原料粉末を用いた以外は実施例1と同様にして複合セラミックスを得た。
表1に示す原料粉末を用いた以外は実施例1と同様にして複合セラミックスを得た。
比較例3において用いたh−BN原料粉末の使用量を5部に増量した。これ以外は比較例3と同様にして複合セラミックスを得た。
実施例及び比較例で得られた複合セラミックスについて、窒化ホウ素の割合、25℃での四点曲げ強度σi、1200℃での四点曲げ強度σh、熱衝撃を与えた後の四点曲げ強度σf、重量基準重量増加率及び表面積基準重量増加率を、上述の方法で測定した。また、Alに起因する結晶相の有無、シリケート又はオキシライド相の有無、X線回折の相対積分強度及び該結晶相の存在位置を、上述の方法で求めた。更に、気孔含有率及び熱伝導率を、上述の方法で測定した。これらの結果を以下の表2に示す。
Claims (8)
- 窒化ケイ素基セラミックスを母相とし、窒化ホウ素が2.5vol.%以上、10vol.%以下の割合で分散相として複合されており、かつAl元素を含まず、
JIS R1601に準拠した25℃での四点曲げ強度をσi、JIS R1615に
準拠した水中投下法によって800℃以上から25℃の水中に投下による急冷で熱衝撃を与えた後の四点曲げ強度をσfとしたとき、σiの値が400MPa以上で、かつσf/σiの比の値が0.85以上であることを特徴とする複合セラミックス。 - 窒化ケイ素基セラミックスを母相とし、窒化ホウ素が2.5vol.%以上、10vol.%以下の割合で分散相として複合されており、
JIS R1601に準拠した25℃での四点曲げ強度をσi、JIS R1615に
準拠した水中投下法によって800℃以上から25℃の水中に投下による急冷で熱衝撃を与えた後の四点曲げ強度をσfとしたとき、σiの値が400MPa以上で、かつσf/σiの比の値が0.85以上であり、
JIS R1601に準拠した1200℃での四点曲げ強度をσhとしたとき、σhと前記のσiとの比率σh/σiが0.85以上であり、
大気中で1300℃又は1400℃・100時間酸化処理した後の複合セラミックスの重量から酸化処理前の重量を差し引き、それを酸化処理前の重量で除して100を乗じた値が0.01〜0.10%であることを特徴とする複合セラミックス。 - Y、Yb又はLu元素を含むシリケート又はオキシナイトライド相の結晶相がX線回折によって確認され、その回折ピークが主要結晶相に対して相対積分強度0.01〜0.6である請求項1又は2に記載の複合セラミックス。
- Y、Yb又はLu元素を含むシリケート又はオキシナイトライド相の結晶相が窒化ケイ素基セラミックス母相の粒界相として存在する請求項1ないし3のいずれかに記載の複合セラミックス。
- 気孔径1〜10μmの気孔を1.5vol.%以下で含む請求項1ないし4のいずれかに記載の複合セラミックス。
- レーザーフラッシュ法によって測定した熱伝導率が50W/mK以上である請求項1ないし5のいずれかに記載の複合セラミックス。
- 請求項2に記載の複合セラミックスの製造方法であって、
母相を形成する窒化ケイ素基セラミックス原料粉末と分散相を形成する窒化ホウ素原料粉末を、90:10〜98:2の重量比で混合して成形し、焼成する工程を含み、
窒化ホウ素原料粉末として、t=0.9λ/(BcosθB)(式中、λはX線管球の
波長(nm)を表し、Bは半値幅(rad)を表し、θBは回折角(rad)を表す。)
で定義される結晶子サイズが40nm以上、48nm未満のものを用いることを特徴とする複合セラミックスの製造方法。 - 窒化ホウ素原料粉末として、X線回折法によって確認できる乱層構造を有するt−BNを用いる請求項7に記載の製造方法。
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