CN113582698A - 一种ZrB2-SiC增韧B4C防弹片的制备方法 - Google Patents
一种ZrB2-SiC增韧B4C防弹片的制备方法 Download PDFInfo
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
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Abstract
本发明涉及一种ZrB2‑SiC增韧B4C防弹片的制备方法,属于新型防弹装甲制造领域。该防弹片由以下方法获得:首先选取ZrSi2、B4C和C作为原料,按照摩尔比2:1:3取料混合,然后将上述混合粉体与B4C粉按照体积比1:9、1.5:8.5、2:8、2.5:7.5、3:7混合,随后将混合粉体依次经湿法球磨,旋转蒸发仪干燥,筛网过筛,最后在热压炉中对粉体进行烧结,通过调控原料配比以及烧结工艺,制备获得B4C‑ZrB2‑SiC防弹片复合材料。采用该方法制备的B4C‑ZrB2‑SiC防弹片复合材料各相分布均匀,具有断裂韧性强,强度高等优点。
Description
技术领域
本发明属于防弹装甲制造领域技术领域,具体而言,涉及一种ZrB2-SiC增韧B4C防弹片的制备方法。
背景技术
防弹陶瓷材料(Al2O3、SiC、B4C等)相对于传统金属材料具有低密度、高硬度、高强度、高弹性模量等性能,且在生产方面绿色、节能,因此近年来备受追捧。与Al2O3、SiC防弹陶瓷相比,碳化硼陶瓷具有硬度更高、密度更小、抗冲击力更强等优点,因而在高温结构材料、轻质人员和车辆防弹装甲材料等领域应用前景更为广阔。然而B4C共价键含量高导致烧结困难且韧性较差从而限制其广泛应用。
目前,制备高性能B4C复合材料的常用方法是直接添加SiC、ZrB2、TiB2、TiC等第二相或添加能够降低B4C烧结温度并诱导产生烧结助剂用于提高B4C致密度、强度以及韧性,然而会不可避免地引入低强度相。如Sung Min So等人研究采用热压烧结制备B4C-SiC复合材料,当B4C和SiC均匀分散在复合材料中时,抑制晶粒生长,获得晶粒细小均匀、高强度的烧结体,但增韧效果不足。现有的B4C基复合材料直接以第二相为添加剂,不能显著降低烧结温度,明显提升材料的机械性能。
因此,如何提供一种烧结方法使得生成的ZrB2和SiC增韧相均匀分布在B4C基体中,与B4C具有良好的结合性,能够提升B4C防弹陶瓷材料韧性,且能降低烧结温度是本领域技术人员亟需解决的问题。
发明内容
本发明正是基于上述技术问题,本发明旨在提供一种原位反应烧结生成ZrB2和SiC增强增韧B4C防弹片复合陶瓷的方法,该复合材料物相纯度高,组元分布均匀,在确保B4C陶瓷低密度的同时,提高B4C复合材料的抗弯强度、断裂韧性,降低烧结温度。
有鉴于此,本发明提出了一种包含ZrB2-SiC的B4C防弹片包含体积分数为B4C 60-90%和体积分数为ZrB2-SiC 10-40%。
根据本发明的第二方面,提出了制备包含ZrB2-SiC的B4C防弹片的方法,包括以下步骤:
(1)将摩尔比为2:1:3的ZrSi2粉、B4C粉和C粉的粉体与按体积配比的B4C粉混合,球磨后得到悬浊液;
(2)将悬浊液40-55℃,干燥0.5-1h后研磨,过筛,得到待烧粉体;
(3)将待烧粉体置于石墨模具内,烧结气氛内1700-2000 ℃,20-60 MPa,进行热压烧结;并保温1-3 h;
(4)随炉冷却,将陶瓷样品与模具取出分离即可。
本发明反应方程式 2ZrSi2 +B4C+3C=2ZrB2+4SiC。
优选的,步骤(2)中热压烧结温度1900 oC,保温时间60 min。
根据本发明的一个实施例,B4C粉纯度99.9%,粒径为0.5 μm;ZrB2粉纯度99.5%,粒径为1-2 μm;C粉纯度99.5%,粒径为30 nm。
优选的B4C粒度选用0.5 μm级,B4C粉含量70%、ZrB2-SiC含量为30%。
根据本发明的一个实施例,步骤(1)中球磨过程为:步骤(1)中球磨过程为:将混合粉料放进聚四氟乙烯罐中,加入无水乙醇,用球磨氧化锆球,采用滚筒球磨机球磨混合成悬浊液;球料质量比为1:1。
根据本发明的一个实施例,球磨转速为60-120 r/min,时间为12-24h。
优选的,步骤(1)中球磨混料时间为24 h,球磨机转速为100 r/min。
根据本发明的一个实施例,步骤(2)中悬浊液干燥后过200目筛。
本发明球磨结束后将浆料与ZrO2球磨球分离,随后采用旋转蒸发仪对浆料进行干燥,干燥后的混合粉体经200目筛网过筛后备用。
根据本发明的一个实施例,步骤(3)中热压烧结工艺参数如下:烧结气氛为氩气;升温速率:室温-1000 ℃为10 ℃/min;1000 ℃-1600 ℃,为8 ℃/min;1600 ℃-2000 ℃为5 ℃/min。
通过以上技术方案,本发明提出了一种原位反应生成ZrB2-SiC增韧B4C防弹片的制备方法,具有如下技术效果:
(1)本发明采用ZrSi2粉、B4C粉和C粉为添加剂原料,原位反应烧结生成B4C-ZrB2-SiC 复合材料,与直接采用第二相陶瓷添加剂与B4C粉体混合的方法相比,原位反应生成的ZrB2和SiC晶粒更加细小,分布更加均匀,与B4C晶界结合更加紧密,生成的ZrB2和SiC晶粒形貌多为棒状或者板条状,能够有效提升B4C韧性。本发明制备的B4C-ZrB2-SiC复合陶瓷,弯曲强度350-500 MPa,维氏硬度17-25 GPa,断裂韧性3.5-5.5 MPa·m1/2;
(2)本发明提供的一种原位反应生成ZrB2-SiC增韧B4C防弹片的制备方法,重复性好,步骤简单,易于实现。
附图说明
图1是本发明实施例1-5所制备的B4C-ZrB2-SiC复合材料XRD;
图2是实施例5中采用体积分数为70% B4C、30%(2ZrSi2 +B4C+3C)配方制备的B4C-ZrB2-SiC烧结体断口SEM。
具体实施方式
为了能够更清楚地理解本发明的上述目的、特征和优点,下面结合附图和具体实施方式对本发明进行进一步的详细描述。需要说明的是,在不冲突的情况下,本发明的实施例及实施例中的特征可以相互组合。
在下面的描述中阐述了很多具体细节以便于充分理解本发明,但是,本发明还可以采用其他不同于在此描述的其他方式来实施,因此,本发明的保护范围并不受下面公开的具体实施例的限制。
本发明实施例所用的B4C粉购于郑州嵩山硼业科技有限公司,其平均粒径0.5 μm,纯度99.9%。所用的ZrSi2粉购于北京华威锐科化工有限公司,粒径1-2 μm,纯度99.5%。所用的C粉购于北京华威锐科化工有限公司,平均粒径30 nm,纯度99.5%。
实施例1
B4C-ZrB2-SiC防弹片材料由如下体积分数的原料组成:B4C粉90%、添加剂10%。
B4C-ZrB2-SiC防弹片复合材料的制备方法如下:
1)添加剂与原料混合粉体配制:选择ZrSi2粉、B4C粉和C粉为原料,按照摩尔比2:1:3称量配料,再按体积配比称量B4C粉后混合;
2)球磨:将B4C与配制好的添加剂置于聚四氟乙烯罐,并添加等质量的ZrO2球磨球,无水乙醇作为球磨介质,采用滚筒球磨机进行球磨,球磨时间24 h,转速100 r/min;
3)干燥:球磨结束后将浆料与ZrO2球磨球分离,紧接着采用旋转蒸发仪对浆料进行干燥,干燥后的混合粉体经200目筛网过筛后备用;
4)烧结:按照配方称量B4C粉与添加剂,将混合后的粉体置于石墨模具,随后经热压烧结,烧结温度1900 oC,压强30 MPa,保温保压时间60 min,烧结完成后随炉冷却,取出模具后将烧结体与模具分离,即得到B4C-ZrB2-SiC防弹片复合材料。
本实施例所制得的B4C-ZrB2-SiC防弹片复合材料的维氏硬度为 19 GPa、弯曲强度为 370 MPa、断裂韧性为 3.6 MPa·m1/2。
实施例2
B4C-ZrB2-SiC防弹片复合材料由如下体积分数的原料组成:B4C粉85%、添加剂15%。
B4C-ZrB2-SiC防弹片复合材料的制备方法如下:
1)添加剂与原料混合粉体配制:选择ZrSi2粉、B4C粉和C粉为原料,按照摩尔比2:1:3称量配料,再按体积配比称量B4C粉后混合;
2)球磨:将B4C与配制好的添加剂置于聚四氟乙烯罐,并添加等质量的ZrO2球磨球,无水乙醇作为球磨介质,采用滚筒球磨机进行球磨,球磨时间24 h,转速120 r/min;
3)干燥:球磨结束后将浆料与ZrO2球磨球分离,紧接着采用旋转蒸发仪对浆料进行干燥,干燥后的混合粉体经200目筛网过筛后备用;
4)烧结:按照配方称量B4C粉与添加剂,将混合后的粉体置于石墨模具;随后经热压烧结,烧结温度1900 oC,压强30 MPa,保温保压时间60 min,烧结完成后随炉冷却,取出模具后将烧结体与模具分离,即得到B4C-ZrB2-SiC防弹片复合材料。
本实施例制备的B4C-ZrB2-SiC防弹片复合材料维氏硬度为19 GPa、弯曲强度为380 MPa、断裂韧性为 3.7 MPa·m1/2。
实施例3
B4C-ZrB2-SiC防弹片复合材料由如下体积分数的原料组成:B4C粉80%、添加剂20%。
B4C-ZrB2-SiC防弹片复合材料的制备方法如下:
1)添加剂与原料混合粉体配制:选择ZrSi2粉、B4C粉和C粉为原料,按照摩尔比2:1:3称量配料,再按体积配比称量B4C粉后混合;
2)球磨:将B4C与配制好的添加剂置于聚四氟乙烯罐,并添加等质量的ZrO2球磨球,无水乙醇作为球磨介质,采用滚筒球磨机进行球磨,球磨时间24 h,转速100 r/min;
3)干燥:球磨结束后将浆料与ZrO2球磨球分离,紧接着采用旋转蒸发仪对浆料进行干燥,干燥后的混合粉体经200目筛网过筛后备用;
4)烧结:按照配方称量B4C粉与添加剂,将混合后的粉体置于石墨模具;随后经热压烧结,烧结温度1950oC,压力30 MPa,保温保压时间60 min,烧结完成后随炉冷却,取出模具后将烧结体与模具分离,即得到B4C-ZrB2-SiC防弹片复合材料。
本实施例所制备的B4C-ZrB2-SiC防弹片复合材料维氏硬度为20 GPa、弯曲强度为390 MPa、断裂韧性为 3.8 MPa·m1/2。
实施例4
B4C-ZrB2-SiC防弹片复合材料由如下体积分数原料组成:B4C粉75%、添加剂25%。
B4C-ZrB2-SiC防弹片复合材料的制备方法如下:
1)添加剂与原料混合粉体配制:选择ZrSi2粉、B4C粉和C粉为原料,按照摩尔比2:1:3称量配料,再按体积配比称量B4C粉后混合;
2)球磨:将B4C与配制好的添加剂放入聚四氟乙烯罐,并添加等质量的ZrO2球磨球,无水乙醇作为球磨介质,采用滚筒球磨机进行球磨,球磨时间24 h,转速100 r/min;
3)干燥:球磨结束后将浆料与ZrO2球磨球分离,紧接着采用旋转蒸发仪对浆料进行干燥,干燥后的混合粉体经200目筛网过筛后备用;
4)烧结:按照配方称量B4C粉与添加剂,将混合后的粉体置于石墨模具;随后经热压烧结,烧结温度1900 oC,压强30 MPa,保温保压时间120 min,烧结完成后随炉冷却,取出模具后将烧结体与模具分离,即得到致密的B4C-ZrB2-SiC防弹片复合材料。
本实施例所制备的B4C-ZrB2-SiC防弹片复合材料维氏硬度为22 GPa、弯曲强度为430 MPa、断裂韧性为 4.5 MPa·m1/2。
实施例5
B4C-ZrB2-SiC防弹片复合材料由如下体积分数的原料组成:B4C粉70%、添加剂30%。
B4C-ZrB2-SiC防弹片复合材料的制备方法如下:
1)添加剂与原料混合粉体配制:选择ZrSi2粉、B4C粉和C粉为原料,按照摩尔比2:1:3称量配料,再按体积配比称量B4C粉后混合;
2)球磨:将B4C与配制好的添加剂置于聚四氟乙烯罐,并添加等质量的ZrO2球磨球,无水乙醇作为球磨介质,采用滚筒球磨机进行球磨,球磨时间24 h,转速120 r/min;
3)干燥:球磨结束后将浆料与ZrO2球磨球分离,紧接着采用旋转蒸发仪对浆料进行干燥,干燥后的混合粉体经200目筛网过筛后备用;
4)烧结:按照配方称量B4C粉与添加剂,将混合后的粉体置于石墨模具;随后经热压烧结,烧结温度1900 oC,压强30 MPa,保温保压时间60 min,烧结完成后随炉冷却,取出模具后将烧结体与模具分离,即得到B4C-ZrB2-SiC防弹片复合材料。
本实施例制备的B4C-ZrB2-SiC防弹片复合材料维氏硬度为22 GPa、弯曲强度为460 MPa、断裂韧性为 5.6 MPa·m1/2。
实施例6
将实施例1-5中得到的B4C-ZrB2-SiC防弹片复合材料进行XRD测试,结果相同如图1,如图1结果表明,该方法所制备的复合材料均为纯相,组元分别为B4C、ZrB2、SiC,反应物无残留。
将实施例5制备的B4C-ZrB2-SiC防弹片复合材料断口进行SEM扫描,结果表明,生成的ZrB2和SiC晶粒形貌多为棒状或者板条状,在陶瓷断裂时的作用机理有拔出与桥接,能够有效提升B4C韧性。
以上仅为本发明的优选实施例而已,并不用于限制本发明。应当理解的是,对于本领域的技术人员来说,无需创造性劳动就可以根据本发明的构思作出诸多修改和变化,根据本发明构思加以改进和变换,所作的任何修改、等同替换、改进等,所有的这些改进和变换都应属于本发明所附权利的要求的保护范围。因此,凡依本发明的构思在现有技术的基础上通过逻辑分析、推理或者有限的实验可以得到的技术方案,皆应在由权利要求书所确定的保护范围内。
Claims (7)
1.一种包含ZrB2-SiC的B4C防弹片,其特征在于,包含体积分数为B4C 60-90%和体积分数为ZrB2-SiC 10-40%。
2.制备权利要求1所述B4C防弹片的方法,其特征在于,包括以下步骤:
(1)将摩尔比为2:1:3的ZrSi2粉、B4C粉和C粉的粉体与按体积配比的B4C粉混合,球磨后得到悬浊液;
(2)将所述悬浊液40-55℃,干燥0.5-1h后研磨,过筛,得到待烧粉体;
(3)将所述待烧粉体置于石墨模具内,烧结气氛内1700-2000 ℃,20-60 MPa,进行热压烧结;并保温1-3 h;
(4)随炉冷却,将陶瓷样品与模具取出分离即可。
3.根据权利要求2所述的方法,其特征在于,所述B4C粉纯度99.9%,粒径为0.5 μm;所述ZrB2粉纯度99.5%,粒径为1-2 μm;所述C粉纯度99.5%,粒径为30 nm。
4.根据权利要求2所述的方法,其特征在于,步骤(1)中所述球磨过程为:将混合粉料放进聚四氟乙烯罐中,加入无水乙醇,用球磨氧化锆球球磨混合成悬浊液;球料质量比为1:1。
5.根据权利要求2所述的方法,其特征在于,所述球磨转速为60-120 r/min,时间为12-24h。
6.根据权利要求2所述的方法,其特征在于,步骤(2)中所述悬浊液干燥后过200目筛。
7.根据权利要求2所述的方法,其特征在于,步骤(3)中热压烧结工艺参数如下:所述烧结气氛为氩气或真空;升温速率:室温-1000 ℃为10 ℃/min;1000 ℃-1600 ℃,为8 ℃/min;1600 ℃-2000 ℃为5 ℃/min。
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