Article(id=1319969652848046515, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1319969627665445134, articleNumber=null, orderNo=null, doi=10.14062/j.issn.0454-5648.20230395, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1686067200000, receivedDateStr=2023-06-07, revisedDate=1690646400000, revisedDateStr=2023-07-30, acceptedDate=null, acceptedDateStr=null, onlineDate=1792634889089, onlineDateStr=2026-10-22, pubDate=1705680000000, pubDateStr=2024-01-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1792634889089, onlineIssueDateStr=2026-10-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1792634889089, creator=13701087609, updateTime=1792634889089, updator=13701087609, issue=Issue{id=1319969627665445134, tenantId=1146029695717560320, journalId=1263187385517883426, year='2024', volume='52', issue='1', pageStart='1', pageEnd='370', issueExtLink='null', onlineDate='null', pubDate='1705680000000', pubDateStr='2024-01-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1792634883085, creator='13701087609', updateTime=1792641944622, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1319999245965443838, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1319969627665445134, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1319999245965443839, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1319969627665445134, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=154, endPage=160, ext={EN=ArticleExt(id=1319969653057761716, articleId=1319969652848046515, tenantId=1146029695717560320, journalId=1263187385517883426, language=EN, title=Fabrication and Characterization of Barium Titanate Based 1-3 Piezoelectric Composites by Stereolithography Technology, columnId=1319726165087077079, journalTitle=Journal of the Chinese Ceramic Society, columnName=Research Article, runingTitle=null, highlight=null, articleAbstract=
Introduction 1-3 type piezoelectric composites are widely used to fabricate high-sensitivity and broadband ultrasonic transducers due to the advantages like a low dielectric constant, a low acoustic impedance, and a high electromechanical coupling coefficient. However, some conventional manufacturing methods such as the cut-and-fill method, the arrangement-casting process, and the injection molding method have challenges to emanate from geometric complexity and structural integrity. Stereolithography technology based on the mask projection approach is an alternative method for manufacturing piezoelectric ceramics with a rapid prototyping and a high precision. Lead-free barium titanate BaTiO3 (BTO) ceramics are widely investigated for piezoelectric sensors and dielectric capacitors applications because of their high dielectric constant, good piezoelectric coefficient, and favorable electromechanical coupling coefficient. In this work, digital light processing (DLP) technology was used to manufacture barium titanate based 1-3 type piezoelectric composites. The influence of piezoelectric phase volume fraction (i.e., 20%-45%) on the micrograph, acoustic impedance and electrical properties of BTO 1-3 composites was investigated.
Methods The printed ceramic slurries with 84% (in mass fraction) BTO content, including BTO powders (d50=500 nm), dispersant, and liquid photopolymers, were mixed by a model ZYMC-180V homogenizer (ZYE) at 2 000 r/min for 90 s. The printed models were built by a software named Computer-Aided Design (CAD) and sliced to a thickness of 7 μm. The piezoelectric pillars (150 μm) with a support were printed layer by layer to form the physical models (i.e., Soon solid, TC-Ⅱ). The printed samples were washed in alcohol by aultrasonic cleaner to remove the residual slurry. Afterwards, the green bodies were treated by a two-step heating treatment, i.e., a debonding process and a sintering process, to obtain the piezoelectric phase structures. Two-time vacuum treatments below -100 kPa were introduced to remove air bubbles in epoxy resin (EPO-TEK301) that filled in the kerfs between piezoelectric pillars (width of 120 μm, height of 330 μm). The samples filled with epoxy resin were heat treated at 60 ℃ for 12 h and then coated with gold electrodes. The BTO 1-3 composites were polarized in an electric field of 4 kV/mm in silicone oil. The microstructures of samples were characterized by a model TM4 000 Plus scanning electron microscope (Hitachi Co., Lted., Japan). The dielectric constant εr, dielectric loss δ, and frequency impedance spectrum were measured by a model 6500B precision impedance analyzer (Wayne Kerr Co., Ltd., UK). Piezoelectric constant d33 was determined by a model ZJ-3A piezo-d33 meter (Institute of Acoustics, Chinese Academy of Sciences, China). The ferroelectric hysteresis loop was measured by a model 2000E ferroelectric analyzer (aixACCT Co., Germany).
Results and discussion The uniform piezoelectric pillars with a width of (150±10) μm are printed through optimizing the slurry formula, and the minimum distance between pillars is approximately 100 μm. The bending deformation of BTO pillars is negligible, and the lateral shrinkage rate is 20%. The forming mechanism of DLP technology results in a clear lamination of the piezoelectric pillar along the printing direction. The shrinkage of ceramics and the growth of grains fill the gap between interlayers, thus reducing the lamination after sintering. There are no residual bubbles in the epoxy resin after vacuum treatment. The density and acoustic impedance of the piezoelectric composites increase with the growth of the piezoelectric phase volume proportion. Compared with the acoustic impedance of BTO ceramics (i.e., Z=31.64 MRayl, 1Rayl=1 Pa·s/m=10-6 MRayl), the acoustic impedance of composites (45%, in volume fraction) is decreased by 67%.
The piezoelectric constant d33 and electromechanical coupling coefficient kt enhance with the piezoelectric phase volume proportion of the composites, meeting their maximum values of 74 pC/N and 0.48, respectively. Compared with the BTO ceramics (kt=0.37), the electromechanical coupling coefficient is improved by 30%. According to the frequency impedance spectra of piezoelectric composites, 1-3 type composites have a pure thickness vibration mode. The dielectric constant εr increases linearly with increasing the piezoelectric phase volume fraction, reaching its maximum of 1 167. The dielectric loss tanδ is lower than 3%, which can enhance the receiving sensitivity of ultrasound transducers. The residual polarization intensity increases with the increase of volume fraction of the piezoelectric phase. The residual polarization intensity of the piezoelectric composite with a volume fraction of 45% reaches a maximum of 1.77 μC/cm2 at 4 kV/mm.
Conclusions 1-3 type barium titanate/epoxy resin piezoelectric composites were fabricated by the DLP technology. The effect of volume fraction of piezoelectric phases on the electrical performances of composites was investigated. The electrical properties such as piezoelectric constant d33, electromechanical coupling coefficient kt, and dielectric constant εr were optimized as the volume fraction of the piezoelectric phase (≤45%) was increased. The polymer phase could effectively reduced the acoustic impedance of piezoelectric materials, thus obtaining an acoustic matching between the piezoelectric materials and tissues or water. Compared to pure barium titanate ceramics, 1-3 type composites as a material of ultrasound transducers could effectively suppress the lateral vibration of the material and enhance the thickness vibration mode, which could improve the pulse echo response. The DLP technology with a high resolution provides an effective and low-cost method for fabricating the piezoelectric composites.
, authors=Liuli CHEN, Yan CHEN, Xuanrong JI, authorsList=Liuli CHEN, Yan CHEN, Xuanrong JI, authorCompany=null, correspAuthors=Yan CHEN, authorNote=
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1-3型压电复合材料作为一种新型的功能材料，具有低介电常数，低声阻抗和高机电耦合系数的优点，常用于制备高灵敏度宽带超声换能器。采用光固化成型技术打印钛酸钡微柱状结构作为1-3型复合材料的压电相，通过优化浆料配方，坯体的平面尺寸精度可达到±10 μm，烧结后压电微柱的宽度和高度分别为120、330 μm，将环氧树脂填充于压电微柱的间隙制备1-3型压电复合材料，研究了不同压电相体积分数（20%~45%）对1-3型压电复合材料电学性能的影响。当压电相体积分数为45%时，压电复合材料的压电常数d33为74 pC/N，机电耦合系数kt为0.48，介电常数εr为1167，介电损耗tanδ为0.023，声阻抗Z为10.43 MRayl（1 Rayl=1 Pa·s/m=10-6 MRayl），与钛酸钡陶瓷相比（kt约为0.37，Z为31.64 MRayl），其机电耦合系数提高了30%，声阻抗降低67%。研究结果表明，光固化成型技术制备的压电复合材料兼具高机电耦合系数和低声阻抗的优势，为压电复合材料在高性能超声换能器的应用提供了一种高效、低成本的制备方法。
, authors=陈柳莉, 陈燕, 纪轩荣, authorsList=陈柳莉, 陈燕, 纪轩荣, authorCompany=null, correspAuthors=陈燕, authorNote=
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陈燕（1983—），女，博士，副教授。
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陈柳莉（1997—），女，硕士研究生。
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