JP2021155235A - 誘電体磁器組成物および電子部品 - Google Patents
誘電体磁器組成物および電子部品 Download PDFInfo
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- JP2021155235A JP2021155235A JP2020054715A JP2020054715A JP2021155235A JP 2021155235 A JP2021155235 A JP 2021155235A JP 2020054715 A JP2020054715 A JP 2020054715A JP 2020054715 A JP2020054715 A JP 2020054715A JP 2021155235 A JP2021155235 A JP 2021155235A
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- 239000000203 mixture Substances 0.000 title claims abstract description 94
- 239000000919 ceramic Substances 0.000 title abstract description 10
- 239000011575 calcium Substances 0.000 claims abstract description 59
- 239000011521 glass Substances 0.000 claims abstract description 58
- 229910052839 forsterite Inorganic materials 0.000 claims abstract description 28
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052573 porcelain Inorganic materials 0.000 claims description 74
- 150000001875 compounds Chemical class 0.000 claims description 37
- 229910052791 calcium Inorganic materials 0.000 claims description 32
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 claims description 28
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 27
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 16
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 8
- VAWSWDPVUFTPQO-UHFFFAOYSA-N calcium strontium Chemical compound [Ca].[Sr] VAWSWDPVUFTPQO-UHFFFAOYSA-N 0.000 abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 37
- 238000010304 firing Methods 0.000 description 18
- 238000000034 method Methods 0.000 description 18
- 238000001354 calcination Methods 0.000 description 17
- 238000013001 point bending Methods 0.000 description 12
- 239000002994 raw material Substances 0.000 description 12
- 239000013078 crystal Substances 0.000 description 11
- 239000011777 magnesium Substances 0.000 description 10
- 238000002156 mixing Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 9
- 229910004283 SiO 4 Inorganic materials 0.000 description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 238000010298 pulverizing process Methods 0.000 description 7
- 229910018068 Li 2 O Inorganic materials 0.000 description 6
- 230000007423 decrease Effects 0.000 description 6
- 238000009766 low-temperature sintering Methods 0.000 description 6
- 239000007858 starting material Substances 0.000 description 6
- 239000000395 magnesium oxide Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000007580 dry-mixing Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- 238000010295 mobile communication Methods 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 150000003891 oxalate salts Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 150000003568 thioethers Chemical class 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- 230000002742 anti-folding effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920001483 poly(ethyl methacrylate) polymer Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/20—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in magnesium oxide, e.g. forsterite
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- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/22—Magnesium silicates
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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- C01G23/006—Alkaline earth titanates
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C10/0018—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents
- C03C10/0027—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents containing SiO2, Al2O3, Li2O as main constituents
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Abstract
Description
主成分としてフォルステライトおよびチタン酸ストロンチウムカルシウムを含み、
主成分におけるフォルステライトの含有割合が84.0モル部以上92.5モル部以下、チタン酸ストロンチウムカルシウムの含有割合が7.5モル部以上16.0モル部以下であり、
前記チタン酸ストロンチウムカルシウムにおける(Sr+Ca)/Tiがモル比で1.03〜1.20であり、
前記主成分と、Li含有ガラスを除く副成分と、の合計100質量部に対して、Li含有ガラスを2質量部以上10質量部以下、添加して得られる誘電体磁器組成物であって、
前記Li含有ガラスはAl2O3の含有量が1質量%以上10質量%以下のガラスである。
(a) 酸化マグネシウムの原料粉末と二酸化珪素の原料粉末とを混合して熱処理することでフォルステライト結晶粉末を作製するフォルステライト結晶粉末の作製工程
(b) チタン酸ストロンチウムカルシウム粉末を準備するチタン酸ストロンチウムカルシウム粉末の準備工程
(c) Li含有ガラスを準備するLi含有ガラスの準備工程
(d) フォルステライト結晶粉末およびチタン酸ストロンチウムカルシウム粉末に、副成分の原料粉末を添加し、仮焼する仮焼工程
(e) 仮焼後の粉末にLi含有ガラスを添加して粉砕することで誘電体磁器組成物を得る誘電体磁器組成物の作製工程
(f) 誘電体磁器組成物を焼成して、誘電体磁器組成物の焼結体を得る焼成工程
フォルステライト結晶粉末の準備方法には特に制限はない。例えば、まず、出発原料としてMgO、SiO2を準備し、Mg2SiO4が作製されるよう秤量する。次に、秤量した出発原料についてボールミルを用いて混合、粉砕した後、仮焼する。仮焼後の粉末がフォルステライト粉末となる。また、市販のフォルステライトを粉砕してフォルステライト粉末を得てもよい。このフォルステライト粉末が誘電体磁器組成物の主成分粉末として用いられる。
チタン酸ストロンチウムカルシウム粉末の準備方法には特に制限はない。例えば、出発原料としてSrCO3、CaCO3およびTiO2を準備し、(Sr+Ca)/TiおよびCa/(Sr+Ca)が所定の範囲内となるように組み合わせて秤量し、ボールミルを用いて混合、粉砕した後、仮焼することによってチタン酸ストロンチウムカルシウム粉末を合成してもよい。また、(Sr+Ca)/TiおよびCa/(Sr+Ca)が所定の範囲内である市販のチタン酸ストロンチウムカルシウムを粉砕してチタン酸ストロンチウムカルシウム粉末を得てもよい。このチタン酸ストロンチウムカルシウム粉末が誘電体磁器組成物の主成分粉末として用いられる。
Li含有ガラスの準備方法には特に制限はない。例えば、原料としてLi含有ガラスに含有させる各成分の出発原料を準備し、所望の割合となるように秤量し、混合する。混合の方法には特に制限はない。例えば10時間以上30時間以下、乾式混合を行ってもよい。次に、この混合物を、1500℃で溶融し、ロールアウトにより約0.5mm厚のリボン状成形体を得る。溶融に用いる炉には特に制限はない。例えば連続溶融炉であってもよい。このリボン状成形体をボールミルにて乾式粉砕した後、分級を行いながらボールミルにて平均粒径が0.5μm以上5μm以下になるように粉砕してもよい。また、所定の範囲内の組成を有する市販のLi含有ガラスを用いてもよい。
仮焼工程では、主成分の粉末および副成分の原料粉末を所定量秤量したのちに、これらを混合して熱処理する。副成分の原料として、後述する仮焼等の熱処理で焼成することによって酸化物となる化合物を用いることもできる。焼成により上記酸化物となる化合物としては、例えば、炭酸塩、硝酸塩、シュウ酸塩、水酸化物、硫化物、有機金属化合物等が例示される。なお、副成分に関しては、主成分の粉末の不純物として添加されてもよい。なお、副成分の各原料の秤量は、誘電体磁器組成物における各副成分の含有量(質量部)が所望の値となるように行う。仮焼条件には特に制限はない。
仮焼後の粉末に対してLi含有ガラスを添加し、粉砕して誘電体磁器組成物とする。具体的な方法には特に制限はない。例えば、仮焼後の粉末に対してLi含有ガラスを添加し、混合粉砕した後、乾燥してもよい。粉砕は乾式粉砕または湿式粉砕等の粉砕方式で行うことができる。粉砕時間は4時間以上24時間以下程度とすればよい。粉砕後の粉末の乾燥は、好ましくは80℃以上200℃以下、より好ましくは100℃以上140℃以下の処理温度で12時間以上36時間以下程度行ってもよい。
焼成工程では、得られた誘電体磁器組成物を焼成して、焼結体を得る。焼成は、例えば、空気中のような酸素雰囲気にて行うことが好ましい。焼成温度には特に制限はない。例えば、800℃以上1100℃以下であってもよく、800℃以上950℃以下であってもよい。
フォルステライト結晶粉末(Mg2SiO4粉末)に関しては、原料であるMgOおよびSiO2を、Mgのモル数がSiのモル数の2倍となるように、それぞれ秤量し、ボールミルを用いて混合、粉砕した後、仮焼することによって合成した。
焼成後の試験片が概ね4.5mm×3.2mm×0.8mmとなるように切断加工し、各方向の寸法をマイクロメーターで精密に測定した。また、電子天秤で切断加工後の試験片の質量を測定した、切断加工後の試験片の質量を切断加工後の試験片の体積で割ることにより、焼結密度を測定した。Mg2SiO4の密度を3.2g/cm3、CaTiO3の密度を4.1g/cm3、SrTiO3の密度を5.1g/cm3として各化合物の含有比率から算出される理論密度に対して、焼結密度が90%以下の場合に不可と判断した。焼結密度が不可である比較例6、7は焼結不足のため、以下に記載する評価を行わなかった。
焼結体の比誘電率εrおよびQ値は、日本工業規格「マイクロ波用ファインセラミックスの誘電特性の試験方法(JIS R1627 1996年度)」に従って測定した。具体的には、10mmφ×5mmの円柱(ペレット)を作製し、両端短絡形誘電体共振器法により比誘電率εrおよび誘電正接tanδを算出した。さらに、1/tanδ=Qとした。Q≧1500である場合にQ値が良好であるとした。Q≧1600である場合がさらに好ましいとした。
上記のペレットについて、日本工業規格「マイクロ波用ファインセラミックスの誘電特性の試験方法(JIS R1627 1996年度)」に従って25℃と85℃での共振周波数を測定し、基準温度を25℃とした場合における温度変化による共振周波数の変化率をτfとした。τfの絶対値が20ppm/℃以下、すなわちτfが−20ppm/℃以上20ppm/℃以下である場合に共振周波数温度特性が良好であるとした。
各誘電体磁器の試験片の厚みが0.4mm前後、幅が2.6mm前後になるように切断加工し、得られた試験片について3点曲げ強度を測定した。3点曲げ強度の測定には測定器(商品名:5543、Instron社製)を用いた。3点曲げ強度の測定時に試験片を支える2点間の距離(治具距離)は15mmとし、3点曲げ強度の測定速度は0.5mm/minとした。30個の試験片について3点曲げ強度を測定して得られた値の平均値(単位:MPa)を3点曲げ強度の測定値とした。なお、3点曲げ強度の測定値が250MPa以上である場合を良好とした。
Claims (6)
- 主成分としてフォルステライトおよびチタン酸ストロンチウムカルシウムを含み、
主成分におけるフォルステライトの含有割合が84.0モル部以上92.5モル部以下、チタン酸ストロンチウムカルシウムの含有割合が7.5モル部以上16.0モル部以下であり、
前記チタン酸ストロンチウムカルシウムにおける(Sr+Ca)/Tiがモル比で1.03〜1.20であり、
前記主成分と、Li含有ガラスを除く副成分と、の合計100質量部に対して、前記Li含有ガラスを2質量部以上10質量部以下、添加して得られる誘電体磁器組成物であって、
前記Li含有ガラスはAl2O3の含有量が1質量%以上10質量%以下のガラスである誘電体磁器組成物。 - 前記チタン酸ストロンチウムカルシウムにおけるCa/(Sr+Ca)がモル比で0.60以上1.00以下である請求項1に記載の誘電体磁器組成物。
- 前記Li含有ガラスはSiO2の含有量が25質量%以上45質量%以下、BaOの含有量が20質量%以上40質量%以下、CaOの含有量が10質量%以上30質量%以下、Li2Oの含有量が10質量%以上30質量%以下である請求項1または2に記載の誘電体磁器組成物。
- 前記Li含有ガラスがB2O3を実質的に含有しない請求項1〜3のいずれかに記載の誘電体磁器組成物。
- 前記主成分100質量部に対して、前記副成分としてCu含有化合物をCuO換算で0.5質量部以上3.0質量部以下、B含有化合物をB2O3換算で0.2質量部以上3.0質量部以下、Al含有化合物をAl2O3換算で0.3質量部以上3.0質量部以下、Mn含有化合物をMnO換算で0.05質量部以上1.5質量部以下、含む請求項1〜4のいずれかに記載の誘電体磁器組成物。
- 請求項1〜5のいずれかに記載の誘電体磁器組成物を有する電子部品。
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