Article(id=1320090228883309512, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320090155155829136, articleNumber=null, orderNo=null, doi=10.14062/j.issn.0454-5648.20240575, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1725120000000, receivedDateStr=2024-09-01, revisedDate=1726761600000, revisedDateStr=2024-09-20, acceptedDate=null, acceptedDateStr=null, onlineDate=1792663636655, onlineDateStr=2026-10-22, pubDate=1742400000000, pubDateStr=2025-03-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1792663636655, onlineIssueDateStr=2026-10-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1792663636655, creator=13701087609, updateTime=1792663636655, updator=13701087609, issue=Issue{id=1320090155155829136, tenantId=1146029695717560320, journalId=1263187385517883426, year='2025', volume='53', issue='3', pageStart='495', pageEnd='732', issueExtLink='null', onlineDate='null', pubDate='1742400000000', pubDateStr='2025-03-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1792663619078, creator='13701087609', updateTime=1792663815055, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1320090977214255163, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320090155155829136, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1320090977214255164, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320090155155829136, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=658, endPage=665, ext={EN=ArticleExt(id=1320090229176910793, articleId=1320090228883309512, tenantId=1146029695717560320, journalId=1263187385517883426, language=EN, title=Preparation of Al2O3-ZrO2 Nanostructured Amorphous Composites by Phase Transformation Assisted Flash Sintering, columnId=1319726165087077079, journalTitle=Journal of the Chinese Ceramic Society, columnName=Research Article, runingTitle=null, highlight=null, articleAbstract=
Introduction

Nanostructured amorphous composites are novel materials composed of nanostructured amorphous matrix and precipitated nanocrystalline phases. However, their preparation requires large and expensive equipment. Flash sintering (FS) ensures a rapid densification at low temperatures and offers an effective approach for the preparation of nanostructured amorphous composites with simple and economical equipment. The amorphous powders by FS show denser microstructures, compared to the crystalline powders by FS. The phase transition from a metastable phase to a stable phase during the sintering process can expedite atomic diffusion and particle rearrangement, thereby promoting structural densification. In this paper, nanostructured amorphous powders in three systems, i.e., Al2O3-La2O3(AL), Al2O3-La2O3-ZrO2(ALZ) and Al2O3-ZrO2(AZ), were prepared by a sol-gel method and densified into dense bulks via flash sintering. The flash sintering behaviors of these different systems were compared, and the promotion of phase transformation on the densification was discussed.

Methods

The three systems of amorphous powders, i.e., AL, ALZ, and AZ, were synthesized via a sol-gel method and subsequently calcined at 600 ℃ for 1 h. Before flash sintering, the powders were consolidated into cylindrical green bodies (φ8 mm×2.3 mm) through uniaxial compression molding at 500 MPa. A platinum wire and electrodes were used to establish electrical connections between a DC power supply and the sample in electric fields of 1000 V/cm and 1600 V/cm, and a heating rate of 10 ℃/min. At a predetermined maximum current of 0.26 A/cm2, the control mode of the power supply was swiftly switched from voltage control to current control. The voltage and current both were measured by a digital electrical multimeter. After continuous energizing for 60 s, the furnace and power supply both were powered off and naturally cooled to ambient temperature.

Results and discussion

The powders of AL, AZ and ALZ all exhibit weak and broad scattering peaks without any detectable crystallization peaks, indicating their amorphous nature. The average particle sizes of the AL, AZ and ALZ powders are 13.7, 6.7 nm and 11.6 nm, respectively. Flash sintering occurs in each system at an electric field intensity of 1000 V/cm with increasing current density. Among the flash-sintered ceramics samples, the sample AZ shows the maximum crystallinity of 69.82% and the relative density of 89%. The crystallinity and relative density of the sample AZ further increase when the electric field intensity increases to 1 600 V/cm. The densification during flash sintering is enhanced by crystallization as crystallization promotes the atomic diffusion and particle rearrangement. Based on the high-resolution transmission electron microscopy images, the uniform precipitation of nanocrystalline phases within an amorphous matrix in the flash-sintered sample AZ with the average particle sizes of 8.74 nm for nanocrystalline regions and 3.15 nm for amorphous regions.

Conclusions

This study conducted an investigation on the flash sintering behavior of three amorphous nanopowders (i.e., AL, AZ and ALZ), and examined the relationship between densification and phase transition. Flash sintering occurred in each nanopowder at an electric field intensity of 1000 V/cm, and the sample AZ exhibited the maximum crystallinity of 69.82% and relative density of 89%. The crystallinity and relative density of the AZ sample further increased to 74.11% and 96%, respectively, when the electric field intensity increased to 1600 V/cm. This study confirmed a positive correlation between crystallization and densification during flash sintering as crystallization and phase transition accelerated atomic diffusion and particle rearrangement, thereby enhancing ceramic densification. The HRTEM images of the sample AZ after flash sintering at 1600 V/cm revealed the uniform precipitation of nanocrystalline phases within an amorphous matrix, indicating that low-temperature rapid preparation of nanostructured amorphous composites was achieved via phase transformation-assisted flash sintering.

, authors=Shuhuai WANG, Jianglin WANG, Yongkang YANG, Ziqi JIA, Xinghua SU, Xiqing XU, authorsList=Shuhuai WANG, Jianglin WANG, Yongkang YANG, Ziqi JIA, Xinghua SU, Xiqing XU, authorCompany=null, correspAuthors=Xiqing XU, authorNote=

WANG Shuhuai (2001-), male, Master candidate. E-mail:

, correspAuthorsNote=
XU Xiqing (1990-), male, Ph.D., Associate Professor. E-mail:
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纳米非晶复合材料是以纳米非晶材料为基体并析出一定纳米晶相的新型材料,具有很多特殊性能,但其制备需要庞大且昂贵的烧结设备,相比之下闪烧设备简单经济,可在较低温度实现快速致密化,为纳米非晶复合材料的制备提供新的途径。采用溶胶凝胶法制备了Al2O3-La2O3(AL)、Al2O3La2O3-ZrO2(ALZ)、Al2O3-ZrO2(AZ)3种纳米非晶粉体,通过闪烧技术制备了纳米非晶复合材料。3种体系在1000 V/cm下发生闪烧后,AZ纳米非晶复合材料具有最大结晶度(69.82%)和最高相对密度(89%)的均匀显微组织。将电场强度提升至1600 V/cm,AZ的结晶度和相对密度进一步提高至74.11%和96%。研究表明,闪烧可以加速非晶样品粉体向晶态的转变,同时相变过程促进了原子扩散和颗粒重排,对闪烧过程中的致密化起到了改善作用。AZ闪烧样品的HRTEM证实了纳米非晶结构的存在,t-ZrO2、α-Al2O3和m-ZrO2纳米晶相在非晶基质中均匀析出,纳米晶和非晶区域的平均粒径分别为8.74 nm和3.15 nm,表明相变辅助闪烧致密化可实现纳米非晶复合陶瓷材料的低温快速制备。

, authors=王竖淮, 王江林, 杨永康, 贾子祺, 苏兴华, 许西庆, authorsList=王竖淮, 王江林, 杨永康, 贾子祺, 苏兴华, 许西庆, authorCompany=null, correspAuthors=许西庆, authorNote=

王竖淮(2001—),男,硕士研究生。

, correspAuthorsNote=
许西庆(1990—),男,博士,副教授。
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相变辅助闪烧制备Al2O3-ZrO2纳米非晶复合材料
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王竖淮 , 王江林 , 杨永康 , 贾子祺 , 苏兴华 , 许西庆
硅酸盐学报 | 研究论文 2025,53(3): 658-665
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硅酸盐学报 |研究论文 2025 , 53 (3) : 658 -665
相变辅助闪烧制备Al2O3-ZrO2纳米非晶复合材料
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王竖淮 , 王江林, 杨永康, 贾子祺, 苏兴华, 许西庆
作者信息
  • 长安大学材料科学与工程学院,西安 710061
通讯作者:
许西庆(1990—),男,博士,副教授。
作者简介:

王竖淮(2001—),男,硕士研究生。

Preparation of Al2O3-ZrO2 Nanostructured Amorphous Composites by Phase Transformation Assisted Flash Sintering
Shuhuai WANG , Jianglin WANG, Yongkang YANG, Ziqi JIA, Xinghua SU, Xiqing XU
Affiliations
  • School of Materials Science and Engineering, Chang'an University, Xi'an 710061, China
  • Corresponding Author:
    XU Xiqing (1990-), male, Ph.D., Associate Professor. E-mail:

    WANG Shuhuai (2001-), male, Master candidate. E-mail:

出版时间: 2025-03-20 doi: 10.14062/j.issn.0454-5648.20240575
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纳米非晶复合材料是以纳米非晶材料为基体并析出一定纳米晶相的新型材料,具有很多特殊性能,但其制备需要庞大且昂贵的烧结设备,相比之下闪烧设备简单经济,可在较低温度实现快速致密化,为纳米非晶复合材料的制备提供新的途径。采用溶胶凝胶法制备了Al2O3-La2O3(AL)、Al2O3La2O3-ZrO2(ALZ)、Al2O3-ZrO2(AZ)3种纳米非晶粉体,通过闪烧技术制备了纳米非晶复合材料。3种体系在1000 V/cm下发生闪烧后,AZ纳米非晶复合材料具有最大结晶度(69.82%)和最高相对密度(89%)的均匀显微组织。将电场强度提升至1600 V/cm,AZ的结晶度和相对密度进一步提高至74.11%和96%。研究表明,闪烧可以加速非晶样品粉体向晶态的转变,同时相变过程促进了原子扩散和颗粒重排,对闪烧过程中的致密化起到了改善作用。AZ闪烧样品的HRTEM证实了纳米非晶结构的存在,t-ZrO2、α-Al2O3和m-ZrO2纳米晶相在非晶基质中均匀析出,纳米晶和非晶区域的平均粒径分别为8.74 nm和3.15 nm,表明相变辅助闪烧致密化可实现纳米非晶复合陶瓷材料的低温快速制备。

纳米非晶材料  /  闪烧  /  低温烧结  /  氧化铝-氧化锆  /  相变
Introduction

Nanostructured amorphous composites are novel materials composed of nanostructured amorphous matrix and precipitated nanocrystalline phases. However, their preparation requires large and expensive equipment. Flash sintering (FS) ensures a rapid densification at low temperatures and offers an effective approach for the preparation of nanostructured amorphous composites with simple and economical equipment. The amorphous powders by FS show denser microstructures, compared to the crystalline powders by FS. The phase transition from a metastable phase to a stable phase during the sintering process can expedite atomic diffusion and particle rearrangement, thereby promoting structural densification. In this paper, nanostructured amorphous powders in three systems, i.e., Al2O3-La2O3(AL), Al2O3-La2O3-ZrO2(ALZ) and Al2O3-ZrO2(AZ), were prepared by a sol-gel method and densified into dense bulks via flash sintering. The flash sintering behaviors of these different systems were compared, and the promotion of phase transformation on the densification was discussed.

Methods

The three systems of amorphous powders, i.e., AL, ALZ, and AZ, were synthesized via a sol-gel method and subsequently calcined at 600 ℃ for 1 h. Before flash sintering, the powders were consolidated into cylindrical green bodies (φ8 mm×2.3 mm) through uniaxial compression molding at 500 MPa. A platinum wire and electrodes were used to establish electrical connections between a DC power supply and the sample in electric fields of 1000 V/cm and 1600 V/cm, and a heating rate of 10 ℃/min. At a predetermined maximum current of 0.26 A/cm2, the control mode of the power supply was swiftly switched from voltage control to current control. The voltage and current both were measured by a digital electrical multimeter. After continuous energizing for 60 s, the furnace and power supply both were powered off and naturally cooled to ambient temperature.

Results and discussion

The powders of AL, AZ and ALZ all exhibit weak and broad scattering peaks without any detectable crystallization peaks, indicating their amorphous nature. The average particle sizes of the AL, AZ and ALZ powders are 13.7, 6.7 nm and 11.6 nm, respectively. Flash sintering occurs in each system at an electric field intensity of 1000 V/cm with increasing current density. Among the flash-sintered ceramics samples, the sample AZ shows the maximum crystallinity of 69.82% and the relative density of 89%. The crystallinity and relative density of the sample AZ further increase when the electric field intensity increases to 1 600 V/cm. The densification during flash sintering is enhanced by crystallization as crystallization promotes the atomic diffusion and particle rearrangement. Based on the high-resolution transmission electron microscopy images, the uniform precipitation of nanocrystalline phases within an amorphous matrix in the flash-sintered sample AZ with the average particle sizes of 8.74 nm for nanocrystalline regions and 3.15 nm for amorphous regions.

Conclusions

This study conducted an investigation on the flash sintering behavior of three amorphous nanopowders (i.e., AL, AZ and ALZ), and examined the relationship between densification and phase transition. Flash sintering occurred in each nanopowder at an electric field intensity of 1000 V/cm, and the sample AZ exhibited the maximum crystallinity of 69.82% and relative density of 89%. The crystallinity and relative density of the AZ sample further increased to 74.11% and 96%, respectively, when the electric field intensity increased to 1600 V/cm. This study confirmed a positive correlation between crystallization and densification during flash sintering as crystallization and phase transition accelerated atomic diffusion and particle rearrangement, thereby enhancing ceramic densification. The HRTEM images of the sample AZ after flash sintering at 1600 V/cm revealed the uniform precipitation of nanocrystalline phases within an amorphous matrix, indicating that low-temperature rapid preparation of nanostructured amorphous composites was achieved via phase transformation-assisted flash sintering.

nanostructured amorphous materials  /  flash sintering  /  low temperature sintering  /  alumina-zirconia  /  phase transition
王竖淮, 王江林, 杨永康, 贾子祺, 苏兴华, 许西庆. 相变辅助闪烧制备Al2O3-ZrO2纳米非晶复合材料. 硅酸盐学报, 2025 , 53 (3) : 658 -665 . DOI: 10.14062/j.issn.0454-5648.20240575
Shuhuai WANG, Jianglin WANG, Yongkang YANG, Ziqi JIA, Xinghua SU, Xiqing XU. Preparation of Al2O3-ZrO2 Nanostructured Amorphous Composites by Phase Transformation Assisted Flash Sintering[J]. Journal of the Chinese Ceramic Society, 2025 , 53 (3) : 658 -665 . DOI: 10.14062/j.issn.0454-5648.20240575
  • 国家自然科学基金(52102062)
  • 中央高校基础研究基金(CHD300102313204)
  • 西安市科技计划项目(23LLRH0004)
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doi: 10.14062/j.issn.0454-5648.20240575
  • 接收时间:2024-09-01
  • 首发时间:2026-10-22
  • 出版时间:2025-03-20
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  • 收稿日期:2024-09-01
  • 修回日期:2024-09-20
基金
国家自然科学基金(52102062)
中央高校基础研究基金(CHD300102313204)
西安市科技计划项目(23LLRH0004)
作者信息
    长安大学材料科学与工程学院,西安 710061

通讯作者:

许西庆(1990—),男,博士,副教授。
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2种不同金属材料的力学参数
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属数
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genus
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Number of
species
占总种数比例
Percentage of
total species (%)
属
Genus
种数
Number of
species
占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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