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Article(id=1321927417929773569, tenantId=1146029695717560320, journalId=1220038251117760515, issueId=1321927171292123557, articleNumber=null, orderNo=null, doi=10.11868/j.issn.1001-4381.2024.000143, pmid=null, cstr=32421.14.j.issn.1001-4381.2024.000143, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1709049600000, receivedDateStr=2024-02-28, revisedDate=null, revisedDateStr=null, acceptedDate=1715702400000, acceptedDateStr=2024-05-15, onlineDate=1793101656657, onlineDateStr=2026-10-27, pubDate=1773936000000, pubDateStr=2026-03-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1793101656657, onlineIssueDateStr=2026-10-27, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1793101656657, creator=13701087609, updateTime=1793101656657, updator=13701087609, issue=Issue{id=1321927171292123557, tenantId=1146029695717560320, journalId=1220038251117760515, year='2026', volume='54', issue='3', pageStart='1', pageEnd='272', issueExtLink='null', onlineDate='null', pubDate='1773936000000', pubDateStr='2026-03-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1793101597855, creator='13701087609', updateTime=1793101597855, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext=null, issueFiles=null, downloadFileDto=null}, startPage=236, endPage=243, ext={EN=ArticleExt(id=1321927420408607235, articleId=1321927417929773569, tenantId=1146029695717560320, journalId=1220038251117760515, language=EN, title=Effect of carbon fiber content on compositional structure and properties of reaction-sintered B4C composites, columnId=1220689384450478826, journalTitle=Journal of Materials Engineering, columnName=RESEARCH ARTICLE, runingTitle=null, highlight=null, articleAbstract=

In this study，B4C-C green containing carbon fibers are prepared by hot pressure molding process used carbon fiber，boron carbide powder，and graphite powder as raw materials，phenolic resin as molding agent，wherein，carbon fiber and powder are dispersed through shear mixing. Then B4C composites （RBBC） are prepared by reaction sintering of B4C-C green at 1550 ℃. The influence of carbon fiber content on the density，composition，structure，and mechanical properties of composites is studied.The results show that the RBBC has the best synthetic property when the volume fraction of carbon fiber reaches 5% in the green.The bending strength，fracture toughness，elastic modulus，and hardness reach 453 MPa，6.7 MPa·m1/2，349 GPa，and 23.5 GPa，respectively. Carbon fiber partially reacts with silicon as a "slow-release" carbon source during the reaction sintering process，slowing down the reaction rate，avoiding material cracking and deformation during the reaction sintering process. It is also helpful for reducing the size of Si islands and content of residual Si in composites，refining the SiC grains generated by the reaction.

, authors=Wei HE, Xiaodong HE, Yanju GU, Xiaoyan HU, Yudi ZHANG, authorsList=Wei HE, Xiaodong HE, Yanju GU, Xiaoyan HU, Yudi ZHANG, authorCompany=null, correspAuthors=Yudi ZHANG, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1321927426750394899, articleId=1321927417929773569, tenantId=1146029695717560320, journalId=1220038251117760515, language=CN, title=碳纤维含量对反应烧结B4C复合材料组成结构及性能的影响, columnId=1220689384622445292, journalTitle=材料工程, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=

以碳纤维、碳化硼粉体、石墨粉体为原料，酚醛树脂为成型剂，采用剪切混合方式分散碳纤维和粉体，采用热模压工艺制备含碳纤维的B4C-C素坯，在1550 ℃下反应烧结制备了B4C复合材料（RBBC）。研究了碳纤维含量对复合材料的致密度、组成结构和力学性能的影响。结果表明，当碳纤维在素坯中的体积分数为5%时，制备的复合材料的综合性能达到最佳，弯曲强度、断裂韧度、弹性模量和硬度分别达到453 MPa、6.7 MPa·m1/2、349 GPa和23.5 GPa。碳纤维在反应烧结过程中部分作为“缓释”碳源参与了反应，减缓了硅碳反应速率，避免了材料在烧结过程中的开裂变形；同时有助于降低复合材料中Si岛尺寸与残Si量，细化反应生成的SiC晶粒。

, authors=何维, 何晓东, 顾艳菊, 胡小燕, 张玉娣, authorsList=何维, 何晓东, 顾艳菊, 胡小燕, 张玉娣, authorCompany=null, correspAuthors=张玉娣, authorNote=null, correspAuthorsNote=
张玉娣（1976—），女，副研究员，研究方向为陶瓷基复合材料，联系地址：湖南省长沙市岳麓区麓山南路1号湖南大学南校区材料科学与工程学院（410082），E-mail：
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Boca Raton： CRC Press， 2002., articleTitle=null, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1321927428772049428, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, xref=null, ext=[AuthorCompanyExt(id=1321927428801409557, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, companyId=1321927428772049428, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=College of Materials Science and Engineering，Hunan University，Changsha 410082，China), AuthorCompanyExt(id=1321927428809798166, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, companyId=1321927428772049428, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=湖南大学 材料科学与工程学院，长沙 410082)])], figs=[ArticleFig(id=1321927433012490814, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=EN, label=Fig.1, caption=X-ray diffractograms and local enlarged view of RBBC composites with addition of non-content fibers, figureFileSmall=JpjLGlXuhn+aovLaSkP3/w==, figureFileBig=KnzhAwGBWxxhG74QJCVhkg==, tableContent=null), ArticleFig(id=1321927433083793983, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=CN, label=图1, caption=添加不同含量纤维的RBBC复合材料的X射线衍射图及局部放大图, figureFileSmall=JpjLGlXuhn+aovLaSkP3/w==, figureFileBig=KnzhAwGBWxxhG74QJCVhkg==, tableContent=null), ArticleFig(id=1321927433545167424, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=EN, label=Fig.2, caption=Surface morphology of ceramic green body with 5% short carbon fiber addition, figureFileSmall=wqoATZKzj7UwslUjDilUoA==, figureFileBig=Lz5CSOY0odXWkEz4bauJPg==, tableContent=null), ArticleFig(id=1321927433851351617, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=CN, label=图2, caption=添加5%短切碳纤维的陶瓷素坯表面形貌, figureFileSmall=wqoATZKzj7UwslUjDilUoA==, figureFileBig=Lz5CSOY0odXWkEz4bauJPg==, tableContent=null), ArticleFig(id=1321927433918460482, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=EN, label=Fig.3, caption=Sectional morphology of RBBC materials with fiber additions ranging from 0% to 15%, figureFileSmall=7g/HjMBJ+9wgrsS4ySO+hQ==, figureFileBig=pemDzzZF42qWdf9omilnaQ==, tableContent=null), ArticleFig(id=1321927434237227587, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=CN, label=图3, caption=纤维添加量为0%~15%的RBBC材料切面形貌

（a）CF0；（b）CF5；（c）CF10；（d）CF15

（a）CF0；（b）CF5；（c）CF10；（d）CF15

, figureFileSmall=7g/HjMBJ+9wgrsS4ySO+hQ==, figureFileBig=pemDzzZF42qWdf9omilnaQ==, tableContent=null), ArticleFig(id=1321927434660852292, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=EN, label=Fig.4, caption=Microscopic morphology of CF5 samples at the original fiber before and after Si removal by acid etching, figureFileSmall=Hk/+Tbc5BTvbAyzFGXgEFw==, figureFileBig=dUsyaPGsDLyUoam2MKTxYA==, tableContent=null), ArticleFig(id=1321927435076088390, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=CN, label=图4, caption=CF5样品酸刻蚀除硅前后原纤维处微观形貌（a）除硅前；（b）除硅后

（a）before silicon etching；（b）after silicon etching

, figureFileSmall=Hk/+Tbc5BTvbAyzFGXgEFw==, figureFileBig=dUsyaPGsDLyUoam2MKTxYA==, tableContent=null), ArticleFig(id=1321927435193528903, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=EN, label=Fig.5, caption="Core-shell" structure formed by fibers in RBBC materials

（a）sample fracture；（b）fiber state；（c）EDS analysis

, figureFileSmall=HLCKWPyw2zGQnnV4N8CL6A==, figureFileBig=RxSzqqo+6BWzzX958f9B5g==, tableContent=null), ArticleFig(id=1321927435533267528, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=CN, label=图5, caption=RBBC材料中纤维形成的“芯-壳”结构

（a）样品断口；（b）纤维状态；（c）EDS分析

, figureFileSmall=HLCKWPyw2zGQnnV4N8CL6A==, figureFileBig=RxSzqqo+6BWzzX958f9B5g==, tableContent=null), ArticleFig(id=1321927435889783369, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=EN, label=Fig.6, caption=Mechanical properties of RBBC materials with different fiber contents（a）flexural strength and modulus；（b）fracture toughness；（c）hardness, figureFileSmall=2zW+z59lnSLXNiJeYOzpcg==, figureFileBig=vsHE/KzdWZUvFP5e7dbZPA==, tableContent=null), ArticleFig(id=1321927437353595466, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=CN, label=图6, caption=不同纤维含量的RBBC材料力学性能（a）弯曲强度及模量；（b）断裂韧度；（c）硬度, figureFileSmall=2zW+z59lnSLXNiJeYOzpcg==, figureFileBig=vsHE/KzdWZUvFP5e7dbZPA==, tableContent=null), ArticleFig(id=1321927437596865099, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=EN, label=Fig.7, caption=Fiber morphology at the fracture of RBBC material

（a）fiber break；（b）fiber pull-out；（c）debonding

, figureFileSmall=KNmIG1YsN+P42sCK7pQLIQ==, figureFileBig=OYKH+tHdImzadjLJqT6tNw==, tableContent=null), ArticleFig(id=1321927437693334092, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=CN, label=图7, caption=RBBC材料断口处纤维形态

（a）纤维断裂；（b）纤维拔出；（c）纤维脱粘

, figureFileSmall=KNmIG1YsN+P42sCK7pQLIQ==, figureFileBig=OYKH+tHdImzadjLJqT6tNw==, tableContent=null), ArticleFig(id=1321927437756248653, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=EN, label=Table 1, caption=

Composition and density of B4C-C porous blanks

, figureFileSmall=null, figureFileBig=null, tableContent=
SampleVolume fraction/%

Density/

（g·cm-3）

Porosity/

%

CfGraphiteB4CResin carbon
CF0016.04461.54134.0
CF5511.84461.54133.2
CF10107.64461.54032.4
CF15153.44461.54031.6
), ArticleFig(id=1321927437848523342, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=CN, label=表1, caption=

B4C-C多孔素坯组成及密度

, figureFileSmall=null, figureFileBig=null, tableContent=
SampleVolume fraction/%

Density/

（g·cm-3）

Porosity/

%

CfGraphiteB4CResin carbon
CF0016.04461.54134.0
CF5511.84461.54133.2
CF10107.64461.54032.4
CF15153.44461.54031.6
), ArticleFig(id=1321927437986935375, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=EN, label=Table 2, caption=

Density and residual silica of RBBC composites with different contents of fibers added

, figureFileSmall=null, figureFileBig=null, tableContent=
Sample

Density/

（g·cm-3）

Volume fraction of

residual Si/%

Open porosity/%
CF02.7214.62.10
CF52.8011.00-0.10
CF102.7911.70.15
CF152.7513.20.80
), ArticleFig(id=1321927438054044240, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321927417929773569, language=CN, label=表2, caption=

添加不同含量纤维的RBBC复合材料的密度及残硅量

, figureFileSmall=null, figureFileBig=null, tableContent=
Sample

Density/

（g·cm-3）

Volume fraction of

residual Si/%

Open porosity/%
CF02.7214.62.10
CF52.8011.00-0.10
CF102.7911.70.15
CF152.7513.20.80
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碳纤维含量对反应烧结B4C复合材料组成结构及性能的影响
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何维 , 何晓东 , 顾艳菊 , 胡小燕 , 张玉娣
材料工程 | 研究论文 2026,54(3): 236-243
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材料工程 |研究论文 2026 , 54 (3) : 236 -243
碳纤维含量对反应烧结B4C复合材料组成结构及性能的影响
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何维, 何晓东, 顾艳菊, 胡小燕, 张玉娣
作者信息
  • 湖南大学 材料科学与工程学院，长沙 410082
通讯作者:
张玉娣（1976—），女，副研究员，研究方向为陶瓷基复合材料，联系地址：湖南省长沙市岳麓区麓山南路1号湖南大学南校区材料科学与工程学院（410082），E-mail：
Effect of carbon fiber content on compositional structure and properties of reaction-sintered B4C composites
Wei HE, Xiaodong HE, Yanju GU, Xiaoyan HU, Yudi ZHANG
Affiliations
  • College of Materials Science and Engineering，Hunan University，Changsha 410082，China
出版时间: 2026-03-20 doi: 10.11868/j.issn.1001-4381.2024.000143
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摘要
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以碳纤维、碳化硼粉体、石墨粉体为原料，酚醛树脂为成型剂，采用剪切混合方式分散碳纤维和粉体，采用热模压工艺制备含碳纤维的B4C-C素坯，在1550 ℃下反应烧结制备了B4C复合材料（RBBC）。研究了碳纤维含量对复合材料的致密度、组成结构和力学性能的影响。结果表明，当碳纤维在素坯中的体积分数为5%时，制备的复合材料的综合性能达到最佳，弯曲强度、断裂韧度、弹性模量和硬度分别达到453 MPa、6.7 MPa·m1/2、349 GPa和23.5 GPa。碳纤维在反应烧结过程中部分作为“缓释”碳源参与了反应，减缓了硅碳反应速率，避免了材料在烧结过程中的开裂变形；同时有助于降低复合材料中Si岛尺寸与残Si量，细化反应生成的SiC晶粒。

碳纤维  /  碳化硼  /  碳源  /  反应烧结  /  增强机制

In this study，B4C-C green containing carbon fibers are prepared by hot pressure molding process used carbon fiber，boron carbide powder，and graphite powder as raw materials，phenolic resin as molding agent，wherein，carbon fiber and powder are dispersed through shear mixing. Then B4C composites （RBBC） are prepared by reaction sintering of B4C-C green at 1550 ℃. The influence of carbon fiber content on the density，composition，structure，and mechanical properties of composites is studied.The results show that the RBBC has the best synthetic property when the volume fraction of carbon fiber reaches 5% in the green.The bending strength，fracture toughness，elastic modulus，and hardness reach 453 MPa，6.7 MPa·m1/2，349 GPa，and 23.5 GPa，respectively. Carbon fiber partially reacts with silicon as a "slow-release" carbon source during the reaction sintering process，slowing down the reaction rate，avoiding material cracking and deformation during the reaction sintering process. It is also helpful for reducing the size of Si islands and content of residual Si in composites，refining the SiC grains generated by the reaction.

carbon fiber  /  boron carbide  /  carbon source  /  reaction sintering  /  enhancement mechanism
何维, 何晓东, 顾艳菊, 胡小燕, 张玉娣. 碳纤维含量对反应烧结B4C复合材料组成结构及性能的影响. 材料工程, 2026 , 54 (3) : 236 -243 . DOI: 10.11868/j.issn.1001-4381.2024.000143
Wei HE, Xiaodong HE, Yanju GU, Xiaoyan HU, Yudi ZHANG. Effect of carbon fiber content on compositional structure and properties of reaction-sintered B4C composites[J]. Journal of Materials Engineering, 2026 , 54 (3) : 236 -243 . DOI: 10.11868/j.issn.1001-4381.2024.000143
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装甲防护材料具备出色的抵御能力，能够有效地遏制高速破片或弹丸等冲击，从而为作战装备和人员提供可靠的保护措施［1-2］。当前，新一代的装甲大多采用轻质的陶瓷/纤维复合装甲，用于抗弹的陶瓷材料主要为Al2O3、SiC、TiB2和B4C等［3-5］。碳化硼因其低比密度（2.52 g/cm3）、超高硬度（>2300HV）、高弹性模量（≈450 GPa）等优点，在受到子弹冲击时能形成更大体积的破碎锥，从而分散更多的冲击能量，更适宜用于防护性能要求高的装甲领域［6-7］。
碳化硼由于晶体结构中的硼-碳强共价键导致其自扩散系数极低、烧结过程中晶界迁移困难，因而产生韧性低（KIC≈2 MPa·m1/2）和致密化成本高等问题［8］。工业生产中通常需要添加助烧剂或借助特殊的烧结工艺提高碳化硼陶瓷的制备效率，如热压烧结、放电等离子烧结和微波辅助无压烧结等［9-12］。相比较于上述烧结工艺，反应烧结碳化硼（reaction bonded boron carbide，RBBC）复相陶瓷具有低成本、高致密度且近净尺寸的优点，极适用于大尺寸或异形结构件的制备［13］。RBBC陶瓷制备流程类似于反应烧结碳化硅（reaction bonded silicon carbide，RBSC）陶瓷，其步骤包括：（1）B4C-C多孔素坯的制备；（2）真空烧结将熔融Si通过毛细管渗入坯体；（3）硅碳反应生成β-SiC实现坯体致密化。
然而反应熔渗工艺不可避免地会存在烧结体残硅问题，硅在烧结体中属于脆性相不利于综合力学性能。RBBC陶瓷的力学性能可以通过B4C-C多孔素坯优化降低硅相含量与掺入增强体提高，其中硅相可以通过调整素坯游离碳含量、碳源类型、原料粉体级配及烧结制度等参数控制［14-16］。近年来，Sha等［17］选用炭黑作为B4C-C生坯的碳源反应烧结制备了RBBC复合材料。通过调整B4C/C比，烧结体渗透完全且相结构均匀，最高弯曲强度达到444 MPa。但炭黑作为碳源时，较高碳含量可能出现C粉团聚、过量C生成β-SiC堵塞渗硅通道或反应剧烈放热使坯体变形，导致烧结体残C或残Si含量偏高，因而力学性能提高有限。
针对碳含量受限的问题，Song等［18］在制备RBSC材料时提出，坯体中可使用缓释碳源降低硅化反应速率，从而达到降低硅碳反应放热破坏坯体的风险以及延后渗Si通道的堵塞。短切碳纤维（Cf）中碳的质量分数超过90%，并且在高温热处理后碳的质量分数可达99%以上，掺入到RBBC材料中能充当碳源的作用［19］。此外，碳纤维本身具有高强度、高模量等优良性能，反应后可能为烧结体提供新的增强机制。Solodkyi等［20］在碳化硼中掺入短碳纤维作为碳源，碳纤维与Si反应后产生的特殊SiC形态一定程度上降低了Si相含量。但使用纤维作为单一碳源时，纤维含量提高容易导致团聚和缺陷，不利于样品的微观均匀性［21］。相比较于传统反应烧结的单一碳源方案，使用片状石墨与短碳纤维搭配作为混合碳源有望在提高素坯碳密度的同时保证渗硅通道的顺畅。
在本研究中，采用一种快速低成本工艺制备B4C-C素坯，并在1550 ℃下烧结制备RBSC陶瓷。研究了高碳含量素坯反应烧结的RBBC复合材料相组成及微观形貌随纤维掺入量变化产生的演变，同时结合力学性能分析Cf在RBBC材料中的增强机理。
1 实验材料与方法
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1.1 实验材料
本实验中，主要原料为商用碳化硼粉（7~10 μm，中硼科技威海有限公司），石墨粉（5000目），高温热处理后的短切碳纤维（密度≈1.76 g/cm3，T300，直径7 μm，长度3 mm，碳的质量分数98.7%）和金属硅颗粒（质量分数约99%，200目），采用高碳产量酚醛树脂（残碳的质量分数55%，裂解碳密度1.61 g/cm3）作为热模压成型中的黏合剂及附加碳源。首先，以无水乙醇为混合介质将碳化硼粉、石墨粉及酚醛树脂按一定比例采用“机械搅拌+超声震荡”共混3 h，混合过程滴入硅烷偶联剂KH550改善粉体分散性。随后将浆料中的无水乙醇挥发，混合粉体过200目筛后与短切碳纤维置于剪切混合器中混合均匀。在保持碳含量不变（质量比B4C∶C＝72∶28）的情况下，根据表1设计改变石墨碳与短切碳纤维配比制备了混合粉料，通过热模压成型过程调节压力将四组样品精确控制为同一体积，在四组样品素坯中Cf分别为0%（体积分数，下同）、5%、10%、15%，命名为CF0、CF5、CF10、CF15。模压成型后的样品经高温碳化成为C-B4C多孔素坯，最后将素坯包埋于Si颗粒中高温真空熔渗制得 RBBC复合材料。本工艺中热模压温度为180~200 ℃，碳化温度为800~1000 ℃，熔渗温度为1550 ℃，真空压强30~50 Pa，保温时间为1.5 h。
1.2 性能检测与分析
使用金刚石膏研磨抛光后的样品进行性能分析测试。根据 Archimedes 原理，采用排水法测定B4C-SiC 复合材料的体积密度及开口孔隙率；利用混合酸溶液腐蚀（混合液摩尔浓度比HNO3∶HF=1∶3）除硅的方法测定材料中的残硅率；利用FALCON 500 维氏硬度计测定材料的硬度（载荷9.8 N，保压时间5 s）；使用CSC-1101型万能试验机采用三点弯曲法和SENB法测量抗弯强度和断裂韧度。其中抗弯测试样品尺寸为35 mm×4 mm×3 mm，断裂韧度试样尺寸为35 mm×3 mm×6 mm，跨距为30 mm，缺口为0.2 mm×3 mm，加载速度为0.05 mm/min。通过 X’Pert Pro MRD 衍射仪（XRD）测定材料的物相组成及晶粒尺寸；采用 JSM-7610 FPlus 型扫描电子显微镜（SEM）结合能谱仪（EDS）观察分析材料微观组织及断口形貌。
2 结果与分析
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2.1 RBBC复合材料相组成与致密度
图1为原料中掺入不同含量碳纤维的RBBC陶瓷熔渗后的XRD图谱，四组样品中主要的相组成包括B4C、β-SiC和Si，在CF15样品中还出现了B12（C，Si，B）3 峰（图1局部放大图）。B12（C，Si，B）3 三元相通常出现在B4C颗粒边缘位置，其生成机理为扩散在液态Si中的C、B原子不同步析出，即过饱和的C优先与Si原子结合析出β-SiC，导致液Si局部区域内的B和C比例发生变化，冷却过程中进一步析出三元相［22］。CF15样品中B、C原子与Si形成的产物B12（C，Si，B）3较为微量，且该相有利于延缓其在冲击载荷下发生的非晶化，不会降低材料的机械动态性能［20］。在生坯石墨含量较高的样品（CF0、CF5、CF10）XRD图谱并未发现该三元相衍射峰，说明坯体中高含量石墨C会降低B4C中的B、C原子向Si中扩散速率，进而抑制B12（C，Si，B）3的产生。
RBBC复合材料中的主相B4C、β-SiC和Si体积分数共同决定了烧结体密度。由于B4C在渗硅过程基本不参与反应，因此烧结体的体积密度的变化意味着β-SiC和残Si含量的变化。通过对比图1中的CF0与CF5样品XRD图谱能观察到，随着碳纤维的掺入，RBBC复合材料中β-SiC的主衍射峰（2θ=35.6°和60.1°）相对强度出现明显的增强趋势，同时Si的主衍射峰呈先降低后增加的趋势。
结合表2密度与残硅含量分析，短碳纤维作为碳源部分取代石墨掺入，当纤维含量为5%时，素坯中纤维四周的孔隙提供了更好的渗硅通道，保证了硅的渗入与碳源反应完全，烧结体密度达到最大的2.80 g/cm3；当纤维含量继续提高时，纤维作为碳源在坯体中分布不均匀导致部分区域碳源富集，反应不充分的现象出现，烧结体残硅含量增加，致密度下降严重。
2.2 RBBC复合材料的微观形貌
短切碳纤维由于具有较高的长径比，在复合材料分散成型工艺中极易因范德瓦耳斯力发生团聚纠缠等现象，严重破坏材料微观结构的均匀性。目前高体积分数短切碳纤维在陶瓷基体中的均质化分散仍需依靠干法混合工艺，但干法混合不可避免地会降低纤维整体长度，不利于纤维对复合材料韧性的提高［23］。相比于传统的球磨分散，剪切分散工艺能更合理控制剪切速度与时间，在一定范围内保留纤维的长度。
本课题采用低速剪切分散的方案，实现了纤维与基体在局部空间内均匀分散。图2为纤维体积分数为5%的RBBC陶瓷素坯SEM图像，经过前期预分散，纤维在基体中整体呈现随机且自由的取向分布，并且纤维周围相对较大的孔隙也为素坯提供了适宜的渗硅通道。如图2所示，经过剪切分散后短碳纤维在B4C-C素坯中长度集中在几百微米的区间范围。
RBBC复合材料烧结后的切面SEM图像如图3所示，SEM背散射模式下黑色相主要为B4C，灰色相为反应过程中形成的β-SiC，白色相则为残余硅，部分棒状细长的黑色相为未反应的碳纤维。图3（a）是未添加碳纤维的RBBC陶瓷切面微观形貌，熔渗过程中薄片状石墨的高比表面积和多反应位点使其可以接触更多的液态Si，并在溶解-沉淀机制的促进作用下使石墨颗粒表面C原子可以迅速在液Si发生溶解扩散［24］。当高含量的石墨C在短时间内同时发生溶解放热行为，陶瓷坯体整体热量很难达到平衡，局部高温使得材料热膨胀失配而出现裂纹或孔洞。如图3（a）所示，熔渗初期形成的裂纹会被液态硅进一步填充，最终材料中出现硅线、微气孔等缺陷导致力学性能下降严重。
图3（b）为含碳纤维5%制备的复合材料的微观形貌，纤维状呈现碳化硅的灰色相，对其进行EDS能谱分析，纤维状物质主要组分为SiC和Si。对其进行酸刻蚀除硅后的微观形貌如图4所示，原纤维边缘位置出现大量纳米及微米尺寸SiC晶粒，而芯部位置则是被酸刻蚀去除的Si与纳米尺寸SiC。在反应烧结过程中，熔融硅首先与反应活性较高的石墨进行反应，同时迅速在碳纤维表面形成致密的SiC壳，减缓了纤维内部碳与Si的反应。纤维的芯部区域由于硅短缺形成Si-C基团，Si-C基团由多重组分的C-Si混合物构成［25］。随着反应进一步进行，Si-C基团中高浓度的C逐渐穿过SiC壳层扩散到浓度较低位置，并在B4C颗粒或反应初始形成的β-SiC表面析出。
当Cf掺入量继续提高到10%时（图3（c）），烧结体中纤维位置除形成上述的SiC-Si形态外，还出现了一种由SiC壳包裹C纤维芯的“核芯-边缘”结构［20］。如图5所示，在Cf密集区域，液Si与纤维芯部C浓度梯度相对较小，减缓了纤维芯部C扩散速率，纤维芯部碳得以保留。纤维掺入量达到15%时，过高纤维体积分数导致纤维分散不均匀，素坯局部区域出现纤维团聚成束，烧结过程中液态Si难以浸渗到纤维聚集束内部，导致RBBC材料内部出现气孔缺陷，如图3（d）所示。孔隙缺陷附近的纤维与基体接触界面不充分，材料在受力过程中在气孔位置易出现灾难性断裂（图5（a））。
2.3 力学性能及断口分析
RBBC复合材料强度、韧性等力学性能主要取决于相的组成分布、界面结合以及缺陷等结构特征。图6为碳纤维掺入量对RBBC复合材料的弯曲强度、断裂韧度、硬度及弹性模量等力学性能的影响。
当纤维体积分数从0%增加到5%，复合材料弯曲强度从251 MPa增加到453 MPa，断裂韧度也从3.2 MPa·m1/2提升到了6.7 MPa·m1/2。CF5样品相对CF0样品弯曲强度和断裂韧度的提高可以归因于碳纤维的“缓释”碳源作用。一方面，纤维的缓慢硅化控制了C在Si液中的扩散-析出速率，避免了坯体因碳源急剧Si-C反应造成的毛细管变窄、堵塞和局部自发高温造成缺陷［26］；另一方面，C扩散-析出速率的降低有利于限制β-SiC长大，使得结构薄弱位置B4C-Si界面、SiC-Si界面尺寸降低。
烧结降温阶段，RBBC材料中会因B4C、SiC、Si热膨胀系数不同而发生非均匀性的收缩，冷却到室温时相界面处会残留积聚性的热应力，微裂纹一般萌生于高残余应力界面，RBBC材料中以B4C-Si界面应力最大。与CF0样品相比，CF5中Si尺寸使得B4C-Si界面分布更均匀分散，有效降低了界面应力集中程度；其次，小尺寸的游离Si在受压缩载荷时，其晶体内部受力状态更均匀，力学性能相对大尺寸Si更高［27］。理想状态下，残余应力在弱界面引发的裂纹与晶粒直径相当［28］，而裂纹缺陷与材料弯曲强度关系如式（1）所示：
σ=KICYa
式中：KIC为断裂韧度，MPa·m1/2；σ为弯曲强度，MPa；α为微裂纹缺陷尺寸，m；Y为校准常数。
材料薄弱位置B4C-Si、SiC-Si界面尺寸降低意味着微裂纹缺陷尺寸的下降和强度性能的提高。此外，在RBBC材料受力变形初始阶段，更低含量、更小尺寸的硅意味着材料的形变量可以更均匀分布到各相晶粒中，避免了局部应力的过度集中，延迟了裂纹产生与延伸。
当纤维含量进一步提高到10%，CF10样品强度开始出现下降趋势。较多的碳纤维已经使材料整体开始出现组分分布不均匀现象，部分区域因硅相对含量低形成纤维“芯-壳”结构，部分区域则因局部碳相对含量低出现大尺寸硅岛缺陷。此过程中在Cf含量较低的区域产生的“芯-壳”结构中，致密SiC壳层与芯部C纤维属于强结合界面。当裂纹延展过程经过该Cf-SiC界面时，发生剪切作用所需能量远低于拉伸作用，造成芯部C纤维直接断裂（图7（a）），不利于材料强度的提高。
值得注意的是，通过观察CF10样品的断裂面（图7（b），（c））发现，并非所有“芯-壳”结构位置在裂纹扩展时都发生断裂。在一些C含量较饱和的区域中，纤维反应程度更轻，“芯-壳”结构外侧SiC壳层较薄，物理形态保留完好，这些纤维提供的类似拔出、纤维脱粘等内在增韧机制延后了RBBC材料灾难性断裂，使得CF10样品断裂韧度高于CF5。
对于复合材料体系而言，材料硬度及弹性模量主要取决于材料组分、颗粒粒径和不同组分间的界面。硅的维氏硬度约为7 GPa，远低于碳化硅（约24 GPa）和碳化硼（28~35 GPa）。基体中高含量的B4C保证了复合材料的较高硬度和模量，而随着纤维的加入，复合材料中的Si体积比降低，而β-SiC结晶性与体积含量都得到提升，因此在硬度测试过程中，硬度得到大幅度提高。当纤维体积分数为5%时，维氏硬度达到最高的23.5 GPa；当纤维含量进一步提高，由于复合材料出现残硅含量增加、纤维“芯部”的残碳以及局部出现疏松孔隙的缺陷等，硬度性能呈现下降趋势。
3 结论
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（1）短切碳纤维作为“缓释”碳源部分取代石墨，在烧结过程中降缓了硅碳反应速率，避免了材料在烧结过程中的开裂变形；合理掺入碳纤维取代石墨有助于降低Si岛尺寸与残Si量，同时起到了细化β-SiC晶粒，提高复合材料强度的作用。
（2）碳纤维与液态Si反应可能形成两种结构，即纤维状SiC-Si与“SiC壳-C芯”结构，纤维状SiC-Si结构主要为烧结体提供晶粒细化的强韧化机制，纤维物理形态保存良好的“壳-芯”结构处则提供类似纤维脱粘、拔出等内在增韧机制。
（3）当应用RBBC复合材料作为抗弹陶瓷时，碳纤维掺入量为5%的样品综合力学性能表现最佳，弯曲强度、弹性模量、断裂韧度和硬度分别达到453 MPa、349 GPa、6.7 MPa·m1/2和23.5 GPa。

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doi: 10.11868/j.issn.1001-4381.2024.000143
  • 接收时间：2024-02-28
  • 首发时间：2026-10-27
  • 出版时间：2026-03-20
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  • 收稿日期：2024-02-28
  • 录用日期：2024-05-15
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    湖南大学 材料科学与工程学院，长沙 410082

通讯作者:

张玉娣（1976—），女，副研究员，研究方向为陶瓷基复合材料，联系地址：湖南省长沙市岳麓区麓山南路1号湖南大学南校区材料科学与工程学院（410082），E-mail：
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
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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