CN113387704A - 一种碳化硼-硼化钛轻质高强复合陶瓷材料及其制备方法 - Google Patents
一种碳化硼-硼化钛轻质高强复合陶瓷材料及其制备方法 Download PDFInfo
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Abstract
本发明提供一种碳化硼‑硼化钛轻质高强复合陶瓷材料及其制备方法,由如下组分及其质量百分比:碳化硼(B4C)粉28.20‑82.05%、碳化钛(TiC)粉8.20‑32.75%、无定型硼(B)粉9.75‑39.05%,经如下步骤制备而成:称取碳化钛粉和无定型硼粉;碳化钛粉和无定型硼粉通过滚筒混料机进行混合、旋转蒸发、烘干,过筛后得到TiC‑B混合粉体;将TiC‑B混合粉体置于热压烧结炉中热处理后获得初级B4C‑TiB2复合粉体;称取初级B4C‑TiB2复合粉体、碳化硼粉体;将粉体通过行星球磨机进行球磨混合、旋转蒸发、烘干,过筛后得到B4C‑TiB2复合粉体;将B4C‑TiB2复合粉体置于石墨模具中在热压炉中进行热压烧结。本发明产品具有良好的烧结性、断裂韧性、导电性,能通过电火花进行加工,TiB2团聚体分散均匀,组分可控,弯曲强度高等优点。
Description
技术领域
本发明涉及陶瓷材料技术领域,具体涉及一种碳化硼-硼化钛轻质高强复合陶瓷材料及其制备方法。
背景技术
碳化硼(B4C)具有优异的综合性能,特别是其低密度(2.52g/cm3)、高硬度(37GPa)、高弹性模量(450GPa)和大中子吸收截面(600barns)的特性引起了广泛的关注。因此,B4C被广泛地应用于轻质防护材料、耐磨部件、刀具以及核工业等领域。B4C的共价键特性使其具有优异的性能,但也导致了较低的断裂韧性(2.2MPa·m1/2)和极差的烧结性能。
大量研究表明,引入第二相硬质颗粒是克服上述困难的有效方法。氧化铝(Al2O3)、碳化硅(SiC)、硼化钛(TiB2)以及硼化锆(ZrB2)等第二相能够有效地改善B4C基体的烧结性能和力学性能。其中,TiB2具有适中的密度、高硬度、高热膨胀系数以及良好的导电性,能够在保持B4C基体低密度、高硬度特点的同时提高材料的断裂韧性和导电性,使得B4C-TiB2复合陶瓷材料能够通过电火花(EDM)进行加工。然而,工业的TiB2粉体粒径粗大,会导致陶瓷复合材料的临界裂纹尺寸较大,将严重影响材料的力学性能。有研究者以B4C-TiO2-C为原料,通过反应烧结制备了B4C-TiB2陶瓷复合材料,该反应过程中会产生气体,并存在一定量的残余C,这将对材料的致密化和力学性能造成不利影响。有研究者以TiC-B为原料,通过反应烧结获得了抗弯强度高达891MPa的B4C-TiB2陶瓷复合材料。然而,该方法使得陶瓷复合材料的组成无法调整,材料的理论体积密度高达3.34g/cm3。
目前,还没有有效的途径能够获得成分可控、TiB2晶粒细小且综合性能优异的B4C-TiB2复合陶瓷材料。因此,有必要对现有技术进行改进,以克服现有技术的不足。
发明内容
本发明的目的是提供一种碳化硼-硼化钛轻质高强复合陶瓷材料及其制备方法,由碳化硼粉、碳化钛粉和无定型硼粉经两步热压烧结法制备,产品具有良好的烧结性、断裂韧性、导电性,能通过电火花进行加工,TiB2团聚体分散均匀,组分可控,弯曲强度高等优点。
为了实现上述目的,本发明采用的技术方案如下:
一种碳化硼-硼化钛轻质高强复合陶瓷材料,由如下组分及其质量百分比制备而成:碳化硼(B4C)粉28.20-82.05%、碳化钛(TiC)粉8.20-32.75%、无定型硼(B)粉9.75-39.05%。
一种碳化硼-硼化钛轻质高强复合陶瓷材料的制备方法,包括如下步骤:
1)按配比称取碳化钛粉和无定型硼粉;
2)将称取的碳化钛粉和无定型硼粉通过滚筒混料机进行混合成浆料,将混合好的浆料进行旋转蒸发,然后置于真空干燥箱中烘干,过筛后得到TiC-B混合粉体;
3)将TiC-B混合粉体置于热压烧结炉中,在热压炉中进行热处理后获得合成的初级B4C-TiB2复合粉体;
4)按配比称取初级B4C-TiB2复合粉体、碳化硼粉体;
5)将步骤4)的粉体通过行星球磨机进行球磨混合成浆料,将混合好的浆料进行旋转蒸发,然后置于真空干燥箱中烘干,过筛后得到B4C-TiB2复合粉体;
6)将B4C-TiB2复合粉体置于石墨模具中在热压炉中进行热压烧结。
根据以上方案,所述碳化硼粉体的平均粒径为2.5μm,纯度大于97wt%;碳化钛粉体的平均粒径6-10μm,纯度为99wt%;无定形硼粉的平均粒径为0.9μm,纯度大于95wt%。
根据以上方案,所述步骤3)热压烧结的工艺条件为:热压炉内真空度保持在40Pa以下,以10-20℃/min的升温速率升温至1400℃,保温60min。
根据以上方案,所述步骤5)行星球磨的工艺条件为:球磨罐为聚四氟乙烯材质,磨球为SiC球,SiC球与合成的B4C-TiB2复合粉体的球料比为5:1,球磨介质为无水乙醇,球磨机的转速为300rpm,球磨时间为120min。
根据以上方案,所述步骤6)热压烧结的工艺条件为:真空度保持在40Pa以下,初始压力为5.5MPa,升温至200℃,同时施加的压力匀速升至12MPa;然后以10-20℃/min的升温速率升温至1200℃,充入保护气氩气;再以10℃/min的速率升温至烧结温度,同时所施加的压力匀速升至30MPa,保温保压60min;自然冷却至室温后即可获得轻质高强的B4C-TiB2复合陶瓷材料。
根据以上方案,所述烧结温度为1850-1950℃。
本发明在两步热压烧结法制备B4C-TiB2复合陶瓷的过程中,TiC与无定形B通过原位反应生成了超细的B4C和TiB2。此时,B4C为分散的状态,而TiB2为以TiC为骨架的团聚状态。然后,合成的初级B4C-TiB2复合粉体与商业的B4C粉体通过球磨混合后,TiB2团聚体得到了有效的分散。TiB2具有适中的密度和较高的硬度,能够在保持B4C基体的低密度、高硬度特点的同时提高材料的烧结性能;另外,TiB2具有较高的热膨胀系数,当烧结温度冷却至室温的过程中,TiB2相与B4C基体相间的热膨胀系数失配导致晶界处产生较大的内应力,在材料断裂的过程中,当裂纹扩展至晶界处时,此内应力将会诱导裂纹偏转,从而消耗更多的裂纹扩展能而大幅度提高材料的断裂韧性;同时,TiB2具有优异的导电性能,使得B4C-TiB2复合陶瓷材料能够通过电火花(EDM)进行加工。采用两步热压烧结法的制备工艺能够通过短时间的球磨工艺处理使得具有疏松结构的TiB2团聚体被有效地分散、细化,并且能够获得组分可控的B4C-TiB2复合粉体。因此,通过热压烧结制备的B4C-TiB2复合陶瓷结构中TiB2的晶粒尺寸得到了有效地控制,临界裂纹尺寸大幅度降低,从而使得材料的弯曲强度大幅度提高。
本发明的有益效果在于:
本发明以B4C、TiC和B为原料,通过两步法制备了B4C-TiB2复合陶瓷,避免了现有技术中采用商业的B4C和TiB2为原料直接混合后进行烧结过程中的烧结致密化困难,B4C、TiB2晶粒粗大,样品的致密度、力学性能不理想等问题;同时,避免了现有技术中采用TiC和B为原料直接混合后进行烧结过程中的复合陶瓷的组分不可控,显微结构中TiB2晶粒尺寸偏大等问题。通过两步法制备的B4C-TiB2复合陶瓷能够在实现材料组分可控的同时极大程度地细化TiB2的晶粒尺寸,有利于材料综合性能的提高。
附图说明
图1为实施例1所制备的复合陶瓷材料的SEM图;
图2为实施例2所制备的复合陶瓷材料的SEM图;
图3为实施例3所制备的复合陶瓷材料的SEM图;
图4为实施例4所制备的复合陶瓷材料的SEM图;
图5为实施例5所制备的复合陶瓷材料的SEM图;
图6为对比例1所制备的复合陶瓷材料的SEM图。
具体实施方式
下面结合附图与实施例对本发明的技术方案进行说明。
以下实施例中,原料采用的碳化硼粉体的平均粒径为2.5μm,纯度大于97wt%;碳化钛粉体的平均粒径6-10μm,纯度为99wt%;无定形硼粉的平均粒径为0.9μm,纯度大于95wt%;混料机采用购自咸阳金宏通用机械有限公司的GMJ/B型滚筒混料机;旋转蒸发采用购自上海申科仪器有限公司的R型旋转蒸发仪;真空干燥箱采用购自上海精宏实验设备有限公司的DZF-6050型真空干燥箱;球磨机采用购自长沙天创粉末科技有限公司的QXQM-4L型行星球磨机;热压烧结炉采用购自美国热能技术有限公司的916G-GPress型热压烧结炉。
实施例1,见图1:
本发明提供一种碳化硼-硼化钛轻质高强复合陶瓷材料及其制备方法,由如下组分及其质量百分比制备而成:碳化硼粉82.05%、碳化钛粉8.20%、无定型硼粉9.75%,其制备方法,包括如下步骤:
1)按配比称取碳化钛粉和无定型硼粉;
2)将称取的碳化钛粉和无定型硼粉通过滚筒混料机进行混合成浆料;将混合好的浆料进行旋转蒸发,然后置于真空干燥箱中烘干,过筛后得到TiC-B混合粉体;
3)将TiC-B混合粉体置于热压烧结炉中,在热压炉中进行热处理后获得合成的初级B4C-TiB2复合粉体;
4)按配比称取初级B4C-TiB2复合粉体、碳化硼粉体;
5)将步骤4)的粉体通过行星球磨机进行球磨混合成浆料,将混合好的浆料进行旋转蒸发,然后置于真空干燥箱中烘干,过筛后得到B4C-TiB2复合粉体;
6)将B4C-TiB2复合粉体置于石墨模具中在热压炉中进行热压烧结。
进一步地,所述步骤3)热压烧结的工艺条件为:热压炉内真空度保持在40Pa以下,以10-20℃/min的升温速率升温至1400℃,保温60min;所述步骤5)行星球磨的工艺条件为:球磨罐为聚四氟乙烯材质,磨球为SiC球,SiC球与合成的B4C-TiB2复合粉体的球料比为5:1,球磨介质为无水乙醇,球磨机的转速为300rpm,球磨时间为120min;所述步骤6)热压烧结的工艺条件为:真空度保持在40Pa以下,初始压力为5.5MPa,非匀速升温至200℃,同时施加的压力匀速升至12MPa;然后以10-20℃/min的升温速率升温至1200℃,充入保护气氩气;再以10℃/min的速率升温至烧结温度1950℃,同时所施加的压力匀速升至30MPa,保温保压60min;自然冷却至室温后即可获得轻质高强的B4C-TiB2复合陶瓷材料(样品的SEM图见图1)。
实施例2,见图2:
本发明提供一种碳化硼-硼化钛轻质高强复合陶瓷材料及其制备方法,基本同实施例1,不同之处在于,由如下组分及其质量百分比制备而成:碳化硼粉64.10%、碳化钛粉16.40%、无定型硼粉19.50%(样品的SEM图见图2)。
实施例3,见图3:
本发明提供一种碳化硼-硼化钛轻质高强复合陶瓷材料及其制备方法,基本同实施例1,不同之处在于,由如下组分及其质量百分比制备而成:碳化硼粉46.15%、碳化钛粉24.55%、无定型硼粉29.30%(样品的SEM图见图3)。
实施例4,见图4:
本发明提供一种碳化硼-硼化钛轻质高强复合陶瓷材料及其制备方法,基本同实施例1,不同之处在于,由如下组分及其质量百分比制备而成:碳化硼粉28.20%、碳化钛粉32.75%、无定型硼粉39.05%(样品的SEM图见图4)。
实施例5,见图5:
本发明提供一种碳化硼-硼化钛轻质高强复合陶瓷材料及其制备方法,基本同实施例1,不同之处在于,由如下组分及其质量百分比制备而成:碳化硼粉64.10%、碳化钛粉16.40%、无定型硼粉19.50%,烧结温度为1850℃(样品的SEM图见图5)。
对比例1,见图6:
一种碳化硼-硼化钛基复合陶瓷材料,其制备原料包括以下组分:B4C粉84wt%、TiSi2粉16wt%;其制备方法包括以下步骤:1)按配比称取各原料粉体;2)将称取的原料粉体混合后在1800℃、40MPa的条件下,采用放电等离子烧结方式进行烧结,获得了相对密度超过99%的碳化硼-硼化钛复合陶瓷(Ceram Int.,47,10665–10671,2021)。
将本发明实施例1-5及对比例1制备的复合陶瓷材料分别进行如下检测:
(1)物相检测:使用X射线衍射仪(RigakuUltimaIII,日本)分析最终产品的物相组成。经检测,最终产品的物相组成为:碳化硼(B4C)、硼化钛钛(TiB2),无其它杂质相。
(2)微观结构表征:使用扫描电子显微镜(Hitachi3400,日本)表征最终产品的微观结构;实施例1-5及对比例1所述复合陶瓷材料的微观结构图分别见附图1-6,由附图1-6可见,实施例1-5制备复合陶瓷材料相较于例1的结构更为均匀。
(3)性能测试:产品的相对密度测定利用Archimedes排水法进行,硬度在维氏硬度仪(430SVD,美国)上进行测试,抗弯强度通过三点弯曲法测试,所使用的测试设备为微机控制电子万能试验机(CMT6503,济南美特斯测试技术有限公司),断裂韧性通过单边切口梁在相同的微机控制电子万能试验机上进行测试。性能检测结果见下表1:
表1.实施例1–5和对比例1的物理性能
从上表1可见,本发明的优势在于:获得了体积密度更小、维氏硬度和弯曲强度更高的碳化硼-硼化钛复合陶瓷样品(对比实施例1和对比例1);在体积密度和维氏硬度相当的情况下,获得了弯曲强度和断裂韧性更高的碳化硼-硼化钛复合陶瓷样品。
本发明以B4C-TiC-B为原料采用两步法(实施例4)与传统方法(Mater TodayCommun,26,102082,2021)以B4C-TiB2为原料在相同的烧结条件下制备样品的性能对比如表2所示:
表2.两步法与传统方法制备样品的物理性能
从上表2可见,本发明采用的两步法较传统的制备方法有着明显的优势。
以上实施例仅用以说明而非限制本发明的技术方案,尽管上述实施例对本发明进行了详细说明,本领域的相关技术人员应当理解:可以对本发明进行修改或者同等替换,但不脱离本发明精神和范围的任何修改和局部替换均应涵盖在本发明的权利要求范围内。
Claims (7)
1.一种碳化硼-硼化钛轻质高强复合陶瓷材料,其特征在于,由如下组分及其质量百分比制备而成:碳化硼粉28.20-82.05%、碳化钛粉8.20-32.75%、无定型硼粉9.75-39.05%。
2.根据权利要求1所述的碳化硼-硼化钛轻质高强复合陶瓷材料的制备方法,其特征在于,包括如下步骤:
1)按配比称取碳化钛粉和无定型硼粉;
2)将称取的碳化钛粉和无定型硼粉通过滚筒混料机进行混合成浆料,将混合好的浆料进行旋转蒸发,然后置于真空干燥箱中烘干,过筛后得到TiC-B混合粉体;
3)将TiC-B混合粉体置于热压烧结炉中,在热压炉中进行热处理后获得合成的初级B4C-TiB2复合粉体;
4)按配比称取初级B4C-TiB2复合粉体、碳化硼粉体;
5)将步骤4)的粉体通过行星球磨机进行球磨混合成浆料,将混合好的浆料进行旋转蒸发,然后置于真空干燥箱中烘干,过筛后得到B4C-TiB2复合粉体;
6)将B4C-TiB2复合粉体置于石墨模具中在热压炉中进行热压烧结。
3.根据权利要求1或2所述的碳化硼-硼化钛轻质高强复合陶瓷材料,其特征在于,所述碳化硼粉体的平均粒径为2.5μm,纯度大于97wt%;碳化钛粉体的平均粒径6-10μm,纯度为99wt%;无定形硼粉的平均粒径为0.9μm,纯度大于95wt%。
4.根据权利要求2所述的碳化硼-硼化钛轻质高强复合陶瓷材料的制备方法,其特征在于,所述步骤3)热压烧结的工艺条件为:热压炉内真空度保持在40Pa以下,以10-20℃/min的升温速率升温至1400℃,保温60min。
5.根据权利要求2所述的碳化硼-硼化钛轻质高强复合陶瓷材料的制备方法,其特征在于,所述步骤5)行星球磨的工艺条件为:球磨罐为聚四氟乙烯材质,磨球为SiC球,SiC球与合成的B4C-TiB2复合粉体的球料比为5:1,球磨介质为无水乙醇,球磨机的转速为300rpm,球磨时间为120min。
6.根据权利要求2所述的碳化硼-硼化钛轻质高强复合陶瓷材料的制备方法,其特征在于,所述步骤6)热压烧结的工艺条件为:真空度保持在40Pa以下,初始压力为5.5MPa,升温至200℃,同时施加的压力匀速升至12MPa;然后以10-20℃/min的升温速率升温至1200℃,充入保护气氩气;再以10℃/min的速率升温至烧结温度,同时所施加的压力匀速升至30MPa,保温保压60min;自然冷却至室温后即可获得轻质高强的B4C-TiB2复合陶瓷材料。
7.根据权利要求2或6所述的碳化硼-硼化钛轻质高强复合陶瓷材料的制备方法,其特征在于,所述烧结温度为1850-1950℃。
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