Article(id=1320107635253301844, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320107605469544753, articleNumber=null, orderNo=null, doi=10.14062/j.issn.0454-5648.20250780, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1761494400000, receivedDateStr=2025-10-27, revisedDate=1768492800000, revisedDateStr=2026-01-16, acceptedDate=null, acceptedDateStr=null, onlineDate=1792667786657, onlineDateStr=2026-10-22, pubDate=1786982400000, pubDateStr=2026-08-18, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1792667786657, onlineIssueDateStr=2026-10-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1792667786657, creator=13701087609, updateTime=1792667786657, updator=13701087609, issue=Issue{id=1320107605469544753, tenantId=1146029695717560320, journalId=1263187385517883426, year='2026', volume='54', issue='9', pageStart='2949', pageEnd='3314', issueExtLink='null', onlineDate='null', pubDate='1789833600000', pubDateStr='2026-09-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1792667779556, creator='13701087609', updateTime=1792737576818, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1320400356446687492, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320107605469544753, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1320400356446687493, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320107605469544753, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=3047, endPage=3055, ext={EN=ArticleExt(id=1320107635463017045, articleId=1320107635253301844, tenantId=1146029695717560320, journalId=1263187385517883426, language=EN, title=Effect of B
4C Content on Densification and Microstructure of (Hf, Zr)B
2 Ceramics, columnId=1263922769897599102, journalTitle=Journal of the Chinese Ceramic Society, columnName=Research Articles, runingTitle=null, highlight=null, articleAbstract=
Introduction (Hf, Zr)B2 solid solutions are promising ultra-high temperature ceramics (UHTCs) for hypersonic applications based on the high-temperature stability of HfB2 and the low cost of ZrB2, exhibiting superior properties to single-component counterparts. However, a covalent bonding leads to a poor sinterability, making the pressureless densification of pure (Hf, Zr)B2 a challenge. While B4C is known as an effective sintering aid for monolithic borides, its role in the densification and microstructural evolution of (Hf, Zr)B2 solid solutions under pressureless sintering conditions remains unexplored. This study was to investigate the effects of B4C content (i.e., 0-5%) and sintering temperature (i.e., 1900-2200 ℃) on the densification behavior and microstructure of (Hf, Zr)B2, to provide theoretical guidance and process references for the pressureless sintering preparation and microstructural control of (Hf, Zr)B2-B4C composites.
Methods (Hf, Zr)B2 powders were synthesized via boro/carbothermal reduction at 1700 ℃ with HfO2, ZrO2, B4C, and graphite as raw materials. The obtained powders were then mixed with 0, 2% and 5% B4C by milling in ethanol for 12 h, followed by rotary evaporation and drying at 60 ℃. The mixed powders were uniaxially pressed into compacts and subsequently cold isostatically pressed at 200 MPa. The pressureless sintering was conducted in an ultra-high temperature furnace in argon atmosphere at a heating rate of 10 ℃/min. A holding step at 1600 ℃ for 30 min was employed before reaching target temperatures (i.e., 1900-2200 ℃) for 2 h.
The density was measured by the Archimedes method. The phase composition was analyzed by X-ray diffraction (XRD), and the microstructure was characterized by scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM/EDS). The grain size was determined based on the SEM images, and the electron backscatter diffraction was employed to evaluate the crystallographic orientation and geometrically necessary dislocation density.
Results and discussion (Hf, Zr)B2 without B4C addition exhibits a poor sinterability, achieving the relative density of only 57.2% at 1900 ℃. and gradually increasing to merely 88.6% even at 2200 ℃. The addition of B4C transforms a densification behavior. At 2000 ℃, the sample containing 2% and 5% B4C achieves the relative densities of 97.8% and 98.1%, respectively, representing an increase of >30% compared to the sample without B4C (i.e., 74.8% at 2000 ℃). This enhancement is attributed to the effective "deoxidizing" function of B4C, reacting with and removing surface oxide impurities, thereby activating mass transport mechanisms essential for pore elimination and grain boundary migration. At > 2000 ℃, the relative density decreases slightly for the samples with B4C. At 2100 ℃, accelerated grain boundary mobility begins to outpace pore migration, leading to the formation of some intragranular pores. At 2200 ℃, the B4C-(Hf, Zr)B2 system reaches its eutectic point, triggering liquid-phase sintering as evidenced by B4C exhibiting melt-like morphology along grain boundaries with good wetting characteristics. The samples with B4C addition exhibite a significant grain growth at elevated temperatures. For the sample with 2% B4C, the grain size increases from (4.81 ± 0.99) μm at 2000 ℃ to (45.07 ± 16.20) μm at 2200 ℃, while the sample with 5% B4C increases from (3.35 ± 0.84) μm to (26.21 ± 7.50) μm. The finer grain in the sample with the more addition of B4C is attributed to an enhanced pinning effect due to a higher content of secondary phase particles, which effectively inhibits a grain boundary migration. This grain coarsening, accompanied by pore coalescence, contributes to a slight decrease in relative density to 94.5% for the sample with 2% B4C and 94.6% for the sample with 5% B4C at 2200 ℃. The EBSD analysis reveals that the geometrically necessary dislocation density decreases at 2200 ℃, compared to the cases at lower sintering temperatures. The Kernel average misorientation mapping shows that the strain concentrations near grain boundaries and B4C particles are somewhat relieved in liquid-phase sintered samples. This phenomenon is related to the dissolution-reprecipitation mechanism and the presence of the liquid phase during sintering. Although B4C participates in liquid formation at 2200 ℃, it recrystallizes upon cooling and retains its 
structure in the final ceramic, indicating a chemical compatibility with the matrix throughout the thermal cycle.
Conclusions The introduction of B4C significantly promoted pressureless sintering densification of (Hf, Zr)B2 ceramics. The samples containing 2% and 5% B4C achieved the relative densities of 97.8% and 98.1% at 2000 ℃, respectively, which exceeded the sample without B4C. Sintering temperature critically controlled the microstructural evolution. The dense microstructures with fine grains were obtained at 2000 ℃. At 2100 ℃, accelerated mass transport led to intragranular pores and rapid grain growth during solid-state sintering. At 2200 ℃, liquid-phase formation caused a significant grain coarsening and a slight density decrease, while effectively relieving internal strain, with B4C recrystallizing upon cooling and retaining its 
structure. Considering both density and microstructure, the optimal pressureless sintering temperature for (Hf, Zr)B2 ceramics with B4C additions could be approximately 2000 ℃, providing a viable process window for (Hf, Zr)B2-based ultra-high temperature ceramic composites.
, authors=Liang XU, Kun WANG, Ji ZOU, Shuaihang QIU, Wei JI, Weimin WANG, Zhengyi FU, authorsList=Liang XU, Kun WANG, Ji ZOU, Shuaihang QIU, Wei JI, Weimin WANG, Zhengyi FU, authorCompany=null, correspAuthors=Ji ZOU, authorNote=
, correspAuthorsNote=
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4C含量对(Hf，Zr)B
2陶瓷的致密化及显微结构的影响, columnId=1263922770220560512, journalTitle=硅酸盐学报, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=
高超声速飞行器热端部件对超高温陶瓷的性能提出了日益严苛的要求。（Hf，Zr）B2固溶体因其兼具HfB2优异的高温稳定性和ZrB2的低成本优势，且表现出优于单一组元的综合性能，被视为极具潜力的下一代热防护材料。然而，其强共价键特性导致烧结活性差，纯相（Hf，Zr）B2难以实现无压烧结致密化。本工作聚焦于（Hf，Zr）B2体系，系统探究了B4C含量（0~5%）与烧结温度（1900~2200 ℃）对其无压烧结行为、致密化过程与显微结构演化的影响。结果表明，在无烧结助剂的情况下，即使烧结温度高达2200 ℃，（Hf，Zr）B2陶瓷的相对密度仅有88.6%；而B4C的添加可显著促进材料的致密化过程。在2000 ℃仅需添加2%（质量分数）的B4C即可实现样品相对密度超过97%。当烧结温度超过2000 ℃，由于晶粒的快速生长，导致晶内孔的形成，样品的相对密度有所下降。尤其当烧结温度为2200 ℃时，由于液相的生成，添加2%和5% B4C样品的晶粒尺寸分别为（45.07 ± 16.20） μm和（26.21 ± 7.50） μm，相对密度下降为94.5%和94.6%。B4C与基体在高温烧结过程中形成液相，在冷却过程中重新结晶析出，最终在样品中仍保持
结构。电子背散射衍射分析表明，和固相烧结的样品相比，液相烧结样品中B4C晶粒附近的硼化物晶格畸变明显下降。研究结果可为超高温硼化物陶瓷无压烧结助剂选择、致密化温度窗口和显微结构调控提供参考。
, authors=许亮, 王坤, 邹冀, 邱帅航, 季伟, 王为民, 傅正义, authorsList=许亮, 王坤, 邹冀, 邱帅航, 季伟, 王为民, 傅正义, authorCompany=null, correspAuthors=邹冀, authorNote=
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邹冀（1983—），男，博士，教授。
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XU Liang (1997-), male, Doctor candidate. E-mail: lx0035@whut.edu.cn
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XU Liang (1997-), male, Doctor candidate. E-mail: lx0035@whut.edu.cn
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许亮（1997—），男，博士研究生。
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许亮（1997—），男，博士研究生。
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