Article(id=1198667060881490280, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1198667059954545009, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2023.04.006, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1650211200000, receivedDateStr=2022-04-18, revisedDate=1652976000000, revisedDateStr=2022-05-20, acceptedDate=null, acceptedDateStr=null, onlineDate=1763714097470, onlineDateStr=2025-11-21, pubDate=1681920000000, pubDateStr=2023-04-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1763714097470, onlineIssueDateStr=2025-11-21, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1763714097470, creator=13701087609, updateTime=1763714097470, updator=13701087609, issue=Issue{id=1198667059954545009, tenantId=1146029695717560320, journalId=1149653034449285133, year='2023', volume='56', issue='4', pageStart='1', pageEnd='112', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1763714097249, creator=13701087609, updateTime=1766563529326, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210618444354023975, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1198667059954545009, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210618444354023976, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1198667059954545009, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=28, endPage=33, ext={EN=ArticleExt(id=1198667062513074539, articleId=1198667060881490280, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Hydrothermal preparation and dielectric research of Ba
1-xCa
xTiO
3 powders for MLCC insulating medium, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=
In order to improve the upper limit temperature and high temperature stability of BaTiO3 for MLCC insulating dielectric material, a Ba1-xCaxTiO3 nano-powder was prepared by using BaCl2·H2O, CaCl2, and H2TiO3 as raw materials and KOH as mineralizer under the condition of 210℃/22 h hydrothermal reaction. The phase structure, microstructure, and dielectric properties of the samples were characterized and analyzed by XRD, SEM, LCR detection methods. The results show that the obtained powders are uniformly dispersed and the particle size is (110±20) nm. The doping of Ca2+ increases the Curie temperature of BaTiO3, and a Ba0.91Ca0.09TiO3 ceramics with 136.2℃of Curie temperature, 1 882 of dielectric constant, and 0.02 of dielectric loss factor are obtained at 1 250℃/2 h. The preparation of MLCC insulating dielectric materials with small particle size, narrow distribution, low agglomeration, and high performance is realized.
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1-xCa
xTiO
3粉体的水热制备及介电研究, columnId=1190369066813591720, journalTitle=绝缘材料, columnName=材料研究, runingTitle=null, highlight=null, articleAbstract=
为提高MLCC绝缘介质材料BaTiO3的上限温度和高温稳定性,本文以BaCl2·H2O、CaCl2和H2TiO3为原料,KOH为矿化剂,在210℃/22 h水热反应条件下制备了Ba1-xCaxTiO3纳米粉体。利用XRD、SEM、LCR检测手段对样品物相结构、微观形貌和介电性能进行表征分析。结果表明:所得粉体样品均匀分散、粒径细小,粒径为(110±20)nm;Ca2+的掺杂提高了BaTiO3的居里温度,在1 250℃/2 h条件下获得了居里温度为136.2℃、常温介电常数为1 882、介质损耗因数为0.02的Ba0.91Ca0.09TiO3陶瓷,实现了小粒径、窄分布、低团聚、高性能MLCC绝缘介质材料的制备。
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朱归胜(1981-),男(汉族),湖南郴州人,教授,博士,主要从事电子信息材料与器件的研究。
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殷昊(1995-),男(汉族),山东潍坊人,硕士生,主要从事电子信息材料与器件的研究。
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1Electronical Information Materials and Devices Engineering Research Center of Ministry of Education, Guilin University of Electronic Technology, Guilin 541004, China
2Guangxi Key Laboratory of Information Materials, Guilin University of Electronic Technology, Guilin 541004, China
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1桂林电子科技大学,电子信息材料与器件教育部工程研究中心,广西 桂林 541004
2桂林电子科技大学,广西信息材料重点实验室,广西 桂林 541004
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殷昊(1995-),男(汉族),山东潍坊人,硕士生,主要从事电子信息材料与器件的研究。
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2Guangxi Key Laboratory of Information Materials, Guilin University of Electronic Technology, Guilin 541004, China
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1桂林电子科技大学,电子信息材料与器件教育部工程研究中心,广西 桂林 541004
2桂林电子科技大学,广西信息材料重点实验室,广西 桂林 541004
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1Electronical Information Materials and Devices Engineering Research Center of Ministry of Education, Guilin University of Electronic Technology, Guilin 541004, China
2Guangxi Key Laboratory of Information Materials, Guilin University of Electronic Technology, Guilin 541004, China
3School of Materials Science and Engineering, Guilin University of Electronic Technology, Guilin 541004, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1210986277109887024, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, authorId=1210986276795314206, language=CN, stringName=张秀云, firstName=秀云, middleName=null, lastName=张, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=
1桂林电子科技大学,电子信息材料与器件教育部工程研究中心,广西 桂林 541004
2桂林电子科技大学,广西信息材料重点实验室,广西 桂林 541004
3桂林电子科技大学,材料科学与工程学院,广西 桂林 541004, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1210986275830625244, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, xref=1, ext=[AuthorCompanyExt(id=1210986275839013854, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, companyId=1210986275830625244, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=
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1Electronical Information Materials and Devices Engineering Research Center of Ministry of Education, Guilin University of Electronic Technology, Guilin 541004, China
2Guangxi Key Laboratory of Information Materials, Guilin University of Electronic Technology, Guilin 541004, China
3School of Materials Science and Engineering, Guilin University of Electronic Technology, Guilin 541004, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1210986277445431365, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, authorId=1210986277193773110, language=CN, stringName=徐华蕊, firstName=华蕊, middleName=null, lastName=徐, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=
1桂林电子科技大学,电子信息材料与器件教育部工程研究中心,广西 桂林 541004
2桂林电子科技大学,广西信息材料重点实验室,广西 桂林 541004
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3桂林电子科技大学,材料科学与工程学院,广西 桂林 541004)])], figs=[ArticleFig(id=1210986280830234793, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=EN, label=Fig.1, caption=
Process flow chart of Ba1-xCaxTiO3 powder samples preparation, figureFileSmall=TwA0R+Wc7VRUCUJzqJp76g==, figureFileBig=UlRqacx+tLGGRVFJfTPiqQ==, tableContent=null), ArticleFig(id=1210986280901537965, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=CN, label=图1, caption=
Ba1-xCaxTiO3粉体样品制备工艺流程图, figureFileSmall=TwA0R+Wc7VRUCUJzqJp76g==, figureFileBig=UlRqacx+tLGGRVFJfTPiqQ==, tableContent=null), ArticleFig(id=1210986281002201267, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=EN, label=Fig.2, caption=
Process flow chart of Ba1-xCaxTiO3 ceramic samples preparation, figureFileSmall=MnwfnwA87rJNtgGXy1e+Mw==, figureFileBig=/yFA0UXmJ0nog3/qhZj4mQ==, tableContent=null), ArticleFig(id=1210986281086087349, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=CN, label=图2, caption=
Ba1-xCaxTiO3陶瓷样品制备工艺流程图, figureFileSmall=MnwfnwA87rJNtgGXy1e+Mw==, figureFileBig=/yFA0UXmJ0nog3/qhZj4mQ==, tableContent=null), ArticleFig(id=1210986281178362040, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=EN, label=Fig.3, caption=
XRD patterns of Ba1-xCaxTiO3 powder samples at room temperature, figureFileSmall=wjdSf4ODkVMD8yb5xyoYjw==, figureFileBig=wQaskrkapSdeCY05QOJ80g==, tableContent=null), ArticleFig(id=1210986281253859516, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=CN, label=图3, caption=
Ba1-xCaxTiO3粉体样品室温下的XRD图, figureFileSmall=wjdSf4ODkVMD8yb5xyoYjw==, figureFileBig=wQaskrkapSdeCY05QOJ80g==, tableContent=null), ArticleFig(id=1210986281333551297, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=EN, label=Fig.4, caption=
EDS diagram of Ba0.91Ca0.09TiO3 powder sample, figureFileSmall=4yw3jNtq7Q5oSUFxiFZkew==, figureFileBig=6w0PRhwVxB0ErfM0rMTw4w==, tableContent=null), ArticleFig(id=1210986281463574723, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=CN, label=图4, caption=
Ba0.91Ca0.09TiO3粉体样品的EDS图, figureFileSmall=4yw3jNtq7Q5oSUFxiFZkew==, figureFileBig=6w0PRhwVxB0ErfM0rMTw4w==, tableContent=null), ArticleFig(id=1210986281572626631, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=EN, label=Fig.5, caption=
SEM and particle size distribution of Ba1-xCaxTiO3 powder samples, figureFileSmall=ar8avvcYIvXrZLM1eRGFDw==, figureFileBig=0mG38rFtOVGeVs3GjOpQZQ==, tableContent=null), ArticleFig(id=1210986281673289930, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=CN, label=图5, caption=
Ba1-xCaxTiO3粉体样品的SEM和粒径分布图, figureFileSmall=ar8avvcYIvXrZLM1eRGFDw==, figureFileBig=0mG38rFtOVGeVs3GjOpQZQ==, tableContent=null), ArticleFig(id=1210986281786536141, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=EN, label=Fig.6, caption=
XRD patterns of Ba1-xCaxTiO3 ceramic samples at room temperature, figureFileSmall=5nHZbxkpGihicc1/nAOzaw==, figureFileBig=T0sk+mMc7Q0HCAbfydbgZQ==, tableContent=null), ArticleFig(id=1210986281883005135, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=CN, label=图6, caption=
Ba1-xCaxTiO3陶瓷样品室温下的XRD图, figureFileSmall=5nHZbxkpGihicc1/nAOzaw==, figureFileBig=T0sk+mMc7Q0HCAbfydbgZQ==, tableContent=null), ArticleFig(id=1210986281975279827, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=EN, label=Fig.7, caption=
Raman patterns of Ba1-xCaxTiO3 ceramic samples at room temperature, figureFileSmall=KLhywJ5vvwC7NkBOvXnwEA==, figureFileBig=zSr/fBNjVWYSiXnoCzIrhw==, tableContent=null), ArticleFig(id=1210986282159829206, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=CN, label=图7, caption=
Ba1-xCaxTiO3陶瓷样品室温下的Raman图, figureFileSmall=KLhywJ5vvwC7NkBOvXnwEA==, figureFileBig=zSr/fBNjVWYSiXnoCzIrhw==, tableContent=null), ArticleFig(id=1210986282226938071, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=EN, label=Fig.8, caption=
SEM images of Ba1-xCaxTiO3 ceramic samples, figureFileSmall=DoQCrInj5veUu/9u+T3+8Q==, figureFileBig=J1VlgdQLe/8Fyj4wKx0MVg==, tableContent=null), ArticleFig(id=1210986283422314713, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=CN, label=图8, caption=
Ba1-xCaxTiO3陶瓷样品的SEM图, figureFileSmall=DoQCrInj5veUu/9u+T3+8Q==, figureFileBig=J1VlgdQLe/8Fyj4wKx0MVg==, tableContent=null), ArticleFig(id=1210986283518783709, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=EN, label=Fig.9, caption=
Dielectric thermograms of Ba1-xCaxTiO3 ceramic samples at room temperature, figureFileSmall=3uUn2lEJ/OcHSRA9nRl63g==, figureFileBig=OB1J8thH0Ur2mV/529FOcA==, tableContent=null), ArticleFig(id=1210986283615252703, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=CN, label=图9, caption=
Ba1-xCaxTiO3陶瓷样品室温下的介电温谱图, figureFileSmall=3uUn2lEJ/OcHSRA9nRl63g==, figureFileBig=OB1J8thH0Ur2mV/529FOcA==, tableContent=null), ArticleFig(id=1210986283703333090, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=EN, label=Tab.1, caption=
Lattice constants and calculation results obtained by refining XRD at room temperature, figureFileSmall=null, figureFileBig=null, tableContent=
| Ba1-xCaxTiO3 | a/Å | b/Å | c/Å | c/a | V/Å3 |
|---|
| x=0 | 3.998 0 | 3.998 0 | 4.018 9 | 1.005 2 | 64.271 4 |
| x=0.03 | 3.994 6 | 3.994 6 | 4.014 1 | 1.004 9 | 64.050 9 |
| x=0.06 | 3.990 9 | 3.990 9 | 4.007 6 | 1.004 2 | 63.830 8 |
| x=0.09 | 3.986 9 | 3.986 9 | 4.001 4 | 1.003 6 | 63.602 6 |
| x=0.12 | 3.987 6 | 3.987 6 | 4.002 6 | 1.003 8 | 63.646 4 |
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对常温XRD精修获得的晶格常数和计算结果
, figureFileSmall=null, figureFileBig=null, tableContent=
| Ba1-xCaxTiO3 | a/Å | b/Å | c/Å | c/a | V/Å3 |
|---|
| x=0 | 3.998 0 | 3.998 0 | 4.018 9 | 1.005 2 | 64.271 4 |
| x=0.03 | 3.994 6 | 3.994 6 | 4.014 1 | 1.004 9 | 64.050 9 |
| x=0.06 | 3.990 9 | 3.990 9 | 4.007 6 | 1.004 2 | 63.830 8 |
| x=0.09 | 3.986 9 | 3.986 9 | 4.001 4 | 1.003 6 | 63.602 6 |
| x=0.12 | 3.987 6 | 3.987 6 | 4.002 6 | 1.003 8 | 63.646 4 |
), ArticleFig(id=1210986283904659685, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=EN, label=Tab.2, caption=
Average particle size and specific surface area of Ba1-xCaxTiO3 powder samples, figureFileSmall=null, figureFileBig=null, tableContent=
| Ba1-xCaxTiO3 | 平均粒径/nm | 比表面积/(m2/g) |
|---|
| x=0 | 115 | 10.92 |
| x=0.03 | 107 | 11.54 |
| x=0.06 | 101 | 13.76 |
| x=0.09 | 92 | 14.28 |
| x=0.12 | 127 | 8.96 |
), ArticleFig(id=1210986283984351464, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=CN, label=表2, caption=
Ba1-xCaxTiO3粉体样品的平均粒径和比表面积
, figureFileSmall=null, figureFileBig=null, tableContent=
| Ba1-xCaxTiO3 | 平均粒径/nm | 比表面积/(m2/g) |
|---|
| x=0 | 115 | 10.92 |
| x=0.03 | 107 | 11.54 |
| x=0.06 | 101 | 13.76 |
| x=0.09 | 92 | 14.28 |
| x=0.12 | 127 | 8.96 |
), ArticleFig(id=1210986284076626156, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=EN, label=Tab.3, caption=
Comparison of literature reports and this article, figureFileSmall=null, figureFileBig=null, tableContent=
| 制备方法 | 粉体平均粒径/nm | 陶瓷平均晶粒尺寸/µm | Tc/℃ | εr(10 kHz) | tanδ(10 kHz) | 参考文献 |
|---|
| 溶胶-凝胶 | — | 5 | 136.4 | 500 | — | [3] |
| 溶胶-凝胶水热 | <300 | 0.048 | 138.0 | 1 000 | 0.02 | [4] |
| 蛋白质溶胶-凝胶 | — | 4 | 130.0 | 250 (1 kHz) | — | [5] |
| 溶胶-凝胶 | 81 | 0.255 | 143.9 | 600 | — | [6] |
| 水热法 | 86 | 1 | 136.2 | 1 882 | 0.02 | 本文 |
), ArticleFig(id=1210986284168900843, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1198667060881490280, language=CN, label=表3, caption=
文献报道与本文对比
, figureFileSmall=null, figureFileBig=null, tableContent=
| 制备方法 | 粉体平均粒径/nm | 陶瓷平均晶粒尺寸/µm | Tc/℃ | εr(10 kHz) | tanδ(10 kHz) | 参考文献 |
|---|
| 溶胶-凝胶 | — | 5 | 136.4 | 500 | — | [3] |
| 溶胶-凝胶水热 | <300 | 0.048 | 138.0 | 1 000 | 0.02 | [4] |
| 蛋白质溶胶-凝胶 | — | 4 | 130.0 | 250 (1 kHz) | — | [5] |
| 溶胶-凝胶 | 81 | 0.255 | 143.9 | 600 | — | [6] |
| 水热法 | 86 | 1 | 136.2 | 1 882 | 0.02 | 本文 |
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