JP2021532568A - 酸化亜鉛バリスタの最適化方法 - Google Patents
酸化亜鉛バリスタの最適化方法 Download PDFInfo
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- JP2021532568A JP2021532568A JP2020572643A JP2020572643A JP2021532568A JP 2021532568 A JP2021532568 A JP 2021532568A JP 2020572643 A JP2020572643 A JP 2020572643A JP 2020572643 A JP2020572643 A JP 2020572643A JP 2021532568 A JP2021532568 A JP 2021532568A
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 278
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 139
- 239000013078 crystal Substances 0.000 claims abstract description 51
- 238000010586 diagram Methods 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 34
- 230000000694 effects Effects 0.000 claims abstract description 21
- 238000013329 compounding Methods 0.000 claims abstract description 18
- 238000005457 optimization Methods 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims description 57
- 235000013339 cereals Nutrition 0.000 claims description 36
- 150000002500 ions Chemical class 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 16
- 230000007423 decrease Effects 0.000 claims description 14
- 238000004832 voltammetry Methods 0.000 claims description 13
- 238000012360 testing method Methods 0.000 claims description 11
- 230000008859 change Effects 0.000 claims description 9
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 8
- 238000002441 X-ray diffraction Methods 0.000 claims description 8
- 238000009472 formulation Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000000556 factor analysis Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- 230000009977 dual effect Effects 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 5
- 238000004088 simulation Methods 0.000 claims description 5
- 238000010183 spectrum analysis Methods 0.000 claims description 5
- 229910052787 antimony Inorganic materials 0.000 claims description 4
- 239000003574 free electron Substances 0.000 claims description 4
- 238000001453 impedance spectrum Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 230000001629 suppression Effects 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000001566 impedance spectroscopy Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 230000007246 mechanism Effects 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
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- 235000009566 rice Nutrition 0.000 claims description 2
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- 229910052596 spinel Inorganic materials 0.000 description 11
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- 230000003247 decreasing effect Effects 0.000 description 10
- 239000011651 chromium Substances 0.000 description 9
- 230000003287 optical effect Effects 0.000 description 9
- 239000000843 powder Substances 0.000 description 5
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
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- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 3
- 238000002050 diffraction method Methods 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 230000020169 heat generation Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910007541 Zn O Inorganic materials 0.000 description 1
- PRTIWZOVTNONNN-UHFFFAOYSA-N [Bi].[Cr] Chemical compound [Bi].[Cr] PRTIWZOVTNONNN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005094 computer simulation Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
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- 239000011521 glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
Abstract
Description
+:ZnO
S:スピネル
w:ZnSiO4 ウレイマイト
#:Bi2O3
&:BiO2-X
x:Bi16CrO27
(1) Ni2O3含有量 0mol%; (2)Ni2O3含有量 0.5mol%; (3)Ni2O3含有量 1mol% (4)Ni2O3含有量 2mol%; (5)Ni2O3含有量 3mol%
Claims (8)
- ZnO結晶粒インピーダンスに対するドープ元素の最適化、Al元素ドープによるZnO結晶粒インピーダンスの最適化、リーク電流増大要因分析を含むことを特徴とする酸化亜鉛バリスタの最適化方法。
前記ドープ元素によるZnO結晶粒インピーダンスの最適化手順に、以下を含む。
固定成分の配合法を用いて、異なる温度を用いてタブレット成形原料を高温焼結した。
異なる温度で、Bi元素、Mn元素、Co元素、Cr元素、Sb元素、Si元素によるZnO結晶粒インピーダンスの最適化。
前記Al元素ドープによるZnO結晶粒インピーダンスの最適化手順に、以下を含む。
ZnO−Al抵抗率に及ぼす保温時間の影響;
ZnO−Al二元試料の微細構造特性;
ZnO−Al二元試料のX線回折スペクトル分析;
AlドープZnOバリスタ試料の調製と試験;
前記リーク電流増大の要因分析は、以下を含む。
Al元素によるリーク電流増大の要因分析;
リーク電流抑制の最適化。 - 前記ドープ元素によるZnO結晶粒インピーダンスの最適化工程には以下を含むことを特徴とする請求項1に記載の酸化亜鉛バリスタの最適化方法。
1100℃、1200℃、1300℃で固定成分配合法によるタブレット成形原料を焼結し、前記固定組成物配合量はモル質量パーセントが94.8mol%のZnO、モル質量パーセントがそれぞれ0.7mol%、0.5mol%、1.0mol%、0.5mol%、1.0mol%、1.25mol%、0.25mol%のBi2O3、MnO2、Co2O3、Cr2O3、Sb2O3、SiO2、Al(NO)3を含む。
焼結手順は、Alドープ量0.25 mol%の従来のZnOバリスタ配合物を用いた上で、被測定元素を含む7成分のうちの1種類のxmol%含有量を調整し、ZnOの含有量を(94−x)mol%−(96−x)mol%としてタブレット成形後、それぞれ1100℃、1200℃、1300℃の温度で高温焼結し、
得られた平均結晶粒サイズおよび不均一度を統計し、SEM画像を分析して結晶の物性を得、また結晶試料の電気的および微細構造特性パラメータを解析し、
前記焼結手順を繰り返し、Bi元素、Mn元素、Co元素、Cr元素、Sb元素、Si元素の最適化実験データ収集を完了させる。 - Al元素ドープによるZnO結晶粒インピーダンスの最適化工程には、以下を含むことを特徴とする請求項1に記載の酸化亜鉛バリスタの最適化方法。
Alイオンを加えた後、Alイオンは結晶格子中のZnイオンを置換して以下のような反応が起こる。
AlZnはZnO結晶格子中のZnイオンを置換したAlイオンであり、e'は放出された電子であり、放出された電子はZnO結晶粒中の自由電子を増加させ、それによって導電率を高めた。
Al添加量を増加させた後、次のような反応が起こる。
Ali'はZnO結晶粒界の隙間内に位置するAlイオンを表し、電子を吸着し、近傍に正孔hが形成され、正孔の出現により一部の自由電子が中和され、それによってZnO結晶粒の導電率が低下し、Alイオン含有量の増加に伴いZnO結晶粒の抵抗がU字状の曲線となり、
それぞれ2ロットのZnO-Al(NO3)3二元配合法の試料を調製し、試料調製と対応する性能テストと最適化を通じて、ZnOバリスタ中の結晶粒インピーダンスを最小にすることができる適切なAlイオン添加量を決定する。 - ZnO−Al二元試料のX線回折スペクトル分析では、ZnOバリスタの従来の配合法に基づき、Al(NO)3のドープ量xをそれぞれ0、0.01、0.05、0.1、0.175、0.25、0.5および1mol%とし、ZnOの含有量は(95.05−x)mol%とし、Bi2O3、MnO2、Co2O3、Cr2O3、Sb2O3、SiO2はそれぞれ0.7、0.5、1.0、0.5、1.0、1.25mol%であり、最高焼結温度は1200℃で、焼結時間は4.5 hであることを特徴とする請求項1に記載の酸化亜鉛バリスタの最適化方法。
上記の一部の試料のX線回折スペクトルをX線回折分析装置XRD、Rigaku H/max 2500を用いて分析した。 - Al元素によるリーク電流増大の要因分析では、ZnOバリスタのシミュレーションモデルをベースに、Al元素ドープによるZnOバリスタリーク電流増大のメカニズムを深く分析し、
ZnOバリスタの小電流領域ボルタンメトリー特性曲線に及ぼす結晶粒ドナー密度の影響効果も、結晶粒ドナー密度が大きくなるに伴い曲線が右下へ著しくずれていることを示したことを特徴とする請求項1に記載の酸化亜鉛バリスタの最適化方法。 - リーク電流抑制の最適化では、Al含有量が低い場合には、結晶粒ドナー密度増加の影響がリーク電流の増加の主な原因となり、結晶粒界表面状態密度を高めることでAlや他の元素ドープによるドナー密度増加がもたらすリーク電流の増加を抑制することができ、結晶粒界の機能材料のドープ量を変化させることで結晶粒界表面状態密度を向上させることができることを特徴とする請求項1に記載の酸化亜鉛バリスタの最適化方法。
- 保温時間がZnO-Al の抵抗率に及ぼす影響について、
1300℃の焼結温度で、焼結保温時間がそれぞれ2h、4h、8hで、異なる含有量のAl(NO3)3のZnOバリスタを加え、直流抵抗の変化傾向を観測し、
1300℃で2h、4hと8h保温したZnO−Al試料の電圧電流特性をソースメーター2410を用いて測定し、試料間のサイズと体積の影響を除去するために、電圧電流特性を電流密度Jと電圧勾配Eに換算し、
1300℃で4h保温したZnO−Al二元試料インピーダンススペクトルを広帯域誘電体分光Concept 80を用いて測定し、室温で測定した周波数範囲を1 Hzから20 MHzとし、試料インピーダンスの実部と虚部、実部インピーダンスと虚部インピーダンスからなるコル−コル(Cole−Cole)図を得、各試料曲線は座標軸と交点のない半円弧を示しており、円弧右側の点は低周波で測定したインピーダンス値であり、左側の点は高周波測定値であり、円弧右側フィッティング延長線とインピーダンス実部軸の交点は試料の結晶粒インピーダンスと結晶粒界インピーダンスの和であって、円弧左側フィッティング延長線とインピーダンス実部軸の交点は試料結晶粒インピーダンスであり、コル−コル図を円弧に適合すると試料の結晶粒抵抗と結晶粒界インピーダンス値が得られることを特徴とする請求項3に記載の酸化亜鉛バリスタの最適化方法。 - ZnO−Alの二元試料の微細構造特性において、
関連する実験現象を合理的に解釈し、ZnO−Al二元配合試料に対してより多くの特性テストと分析を行い、
焼結温度1300℃、焼結時間4hのとき、異なるAlイオン含有量でドープした系列試料を選び、試料片の表面に拡大倍率が10で、ZnO−Al二元試料の微細構造特性を0倍の光学顕微鏡Microscope Mitutoyo FS 70 Z−Sを用いて観測し、
上記試料の断面を走査型電子顕微鏡SEM、JSM−6700Fを用いて観測したことを特徴とする請求項3に記載の酸化亜鉛バリスタの最適化方法。
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