JP7496523B2 - バリウム化合物構造体及びその製造方法 - Google Patents
バリウム化合物構造体及びその製造方法 Download PDFInfo
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- JP7496523B2 JP7496523B2 JP2022526904A JP2022526904A JP7496523B2 JP 7496523 B2 JP7496523 B2 JP 7496523B2 JP 2022526904 A JP2022526904 A JP 2022526904A JP 2022526904 A JP2022526904 A JP 2022526904A JP 7496523 B2 JP7496523 B2 JP 7496523B2
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- barium
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- 150000001553 barium compounds Chemical group 0.000 title claims description 130
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 150000001875 compounds Chemical class 0.000 claims description 174
- 239000002245 particle Substances 0.000 claims description 148
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 53
- 239000000843 powder Substances 0.000 claims description 47
- 239000000203 mixture Substances 0.000 claims description 28
- 239000007864 aqueous solution Substances 0.000 claims description 23
- 229910052710 silicon Inorganic materials 0.000 claims description 23
- DQBAOWPVHRWLJC-UHFFFAOYSA-N barium(2+);dioxido(oxo)zirconium Chemical compound [Ba+2].[O-][Zr]([O-])=O DQBAOWPVHRWLJC-UHFFFAOYSA-N 0.000 claims description 19
- 239000010703 silicon Substances 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 229910021523 barium zirconate Inorganic materials 0.000 claims description 18
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229910052788 barium Inorganic materials 0.000 claims description 9
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 8
- 229910002113 barium titanate Inorganic materials 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 6
- 229910021417 amorphous silicon Inorganic materials 0.000 claims description 2
- 238000012360 testing method Methods 0.000 description 25
- 239000011148 porous material Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 16
- 238000000034 method Methods 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000001878 scanning electron micrograph Methods 0.000 description 11
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 9
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 9
- 235000011130 ammonium sulphate Nutrition 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 7
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 6
- 239000000376 reactant Substances 0.000 description 6
- 229910052814 silicon oxide Inorganic materials 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 229910044991 metal oxide Inorganic materials 0.000 description 5
- 150000004706 metal oxides Chemical class 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 5
- 239000004566 building material Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000000921 elemental analysis Methods 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- QFFVPLLCYGOFPU-UHFFFAOYSA-N barium chromate Chemical compound [Ba+2].[O-][Cr]([O-])(=O)=O QFFVPLLCYGOFPU-UHFFFAOYSA-N 0.000 description 2
- 229940083898 barium chromate Drugs 0.000 description 2
- 229910001422 barium ion Inorganic materials 0.000 description 2
- RCMWGBKVFBTLCW-UHFFFAOYSA-N barium(2+);dioxido(dioxo)molybdenum Chemical compound [Ba+2].[O-][Mo]([O-])(=O)=O RCMWGBKVFBTLCW-UHFFFAOYSA-N 0.000 description 2
- SJPVUFMOBDBTHQ-UHFFFAOYSA-N barium(2+);dioxido(dioxo)tungsten Chemical compound [Ba+2].[O-][W]([O-])(=O)=O SJPVUFMOBDBTHQ-UHFFFAOYSA-N 0.000 description 2
- QKYBEKAEVQPNIN-UHFFFAOYSA-N barium(2+);oxido(oxo)alumane Chemical compound [Ba+2].[O-][Al]=O.[O-][Al]=O QKYBEKAEVQPNIN-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 229940071182 stannate Drugs 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 230000015654 memory Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Description
本実施形態のバリウム化合物構造体1は、図1に示すように、複数の第1化合物粒子2と、結合部3と、複数の第2化合物粒子4とを含んでいる。また、バリウム化合物構造体1には、第1化合物粒子2の各々の間であって、結合部3によって囲われる複数の気孔5が存在している。
次に、バリウム化合物構造体1の製造方法について説明する。バリウム化合物構造体1は、第1化合物粉末と、第2化合物粉末と、硫酸イオンを含む水溶液とを混合することにより混合物を得る工程と、当該混合物を加圧及び加熱する工程と、により製造することができる。
次に、バリウム化合物構造体1を備える部材について説明する。バリウム化合物構造体1は、誘電性に優れた部材として使用することができる。上記部材は、コンデンサ、圧電素子及びメモリのような電子部品に用いることができる。また、上記部材は、薄膜回路用基板、センサ部材用基板及び半導体プロセス用基板、半導体製造装置のセラミックス部材、並びにその他一般電子機器の筐体にも使用することができる。
(試験サンプルの作製)
まず、ジルコン酸バリウム粉末(シグマアルドリッチ社製)0.78g及びシリカ粉末(日本アエロジル株式会社製)0.0777gにアセトンを加え、メノウ乳鉢及びメノウ乳棒を用いて混合し、混合粉末を得た。得られた混合物を、内部空間を有する円筒状の成形用金型(Φ10)の内部に投入した。なお、本例において、ジルコン酸バリウム粉末は第1化合物粉末に相当し、シリカ粉末は第2化合物粉末に相当する。第2化合物粉末を構成する複数の粒子の平均粒子径は、12nmである。
[比較例1]
混合粉末に代えて上述したジルコン酸バリウム粉末0.78gのみを用いた以外は実施例1と同様の手順で、円柱状の試験サンプルを得た。
(結晶構造解析)
粉末X線回折(XRD)装置を用いて、実施例1及び比較例1の試験サンプルを粉砕した粉末のXRDパターンを測定した。図3は、実施例1、比較例1、並びにICSDに登録されたジルコン酸バリウム及び硫酸バリウムのXRDパターンを示すグラフである。また、図4は、図3のうち実施例1及び比較例1のXRDパターンを拡大したグラフである。
円柱状の試験サンプルを割断した断面を、走査型電子顕微鏡(SEM)を用いて観察した。また、実施例1の試験サンプルの異なる位置について、エネルギー分散型X線分光法(EDX)による元素分析を行った。なお、観察面には金のスパッタリングを施した。図5は実施例1の試験サンプルを1000倍で観察したSEM像である。図6は実施例1の試験サンプルを10000倍で観察したSEM像である。図7は実施例1の試験サンプルの図6とは異なる位置を10000倍で観察したSEM像である。図8は図5中の位置1におけるEDXスペクトルである。図9は図5中の位置2におけるEDXスペクトルである。図10は比較例1の試験サンプルを1000倍で観察したSEM像である。図11は比較例1の試験サンプルを10000倍で観察したSEM像である。
実施例1及び比較例1の試験サンプルのビッカース硬さを、JIS R1610に準拠して測定した。その結果、実施例1の試験サンプルのビッカース硬さは1.4GPa、比較例1の試験サンプルのビッカース硬さは0.45GPaであり、実施例1の試験サンプルの方が高い硬度を示した。
2 第1化合物粒子
3 結合部
4 第2化合物粒子
Claims (8)
- 硫酸バリウムとは異なり、結晶性を有するバリウム化合物を含む複数の第1化合物粒子と、
前記複数の第1化合物粒子の各々の表面を覆い、結晶性を有する硫酸バリウムを含む結合部と、
ケイ素を有する非晶質酸化物を含む複数の第2化合物粒子と、
を含み、
前記複数の第1化合物粒子の各々は前記結合部及び前記複数の第2化合物粒子の各々の少なくともいずれか一方を介して結合する、バリウム化合物構造体。 - 前記バリウム化合物はチタン酸バリウム及びジルコン酸バリウムの少なくともいずれか一方である、請求項1に記載のバリウム化合物構造体。
- 前記複数の第2化合物粒子に含まれる化合物は非晶質酸化ケイ素である、請求項1又は2に記載のバリウム化合物構造体。
- 前記複数の第1化合物粒子の前記結合部に対する体積比は1以上である、請求項1から3のいずれか一項に記載のバリウム化合物構造体。
- バリウムのケイ素に対するモル比は1以上である、請求項1から4のいずれか一項に記載のバリウム化合物構造体。
- 気孔率は30%以下である、請求項1から5のいずれか一項に記載のバリウム化合物構造体。
- 前記複数の第1化合物粒子の平均粒子径は50nm~100μmである、請求項1から6のいずれか一項に記載のバリウム化合物構造体。
- 硫酸バリウムとは異なり、結晶性を有するバリウム化合物を含む第1化合物粉末と、ケイ素を有する非晶質酸化物を含む第2化合物粉末と、硫酸イオンを含む水溶液とを混合することにより混合物を得る工程と、
前記混合物を、圧力が10~600MPaであり、かつ、温度が50~300℃である条件下で加圧及び加熱する工程と、
を有する、バリウム化合物構造体の製造方法。
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