CN116409998A - 一种碳化硅石墨烯复合防弹陶瓷及制备方法 - Google Patents
一种碳化硅石墨烯复合防弹陶瓷及制备方法 Download PDFInfo
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Abstract
一种碳化硅石墨烯复合防弹陶瓷,按重量百分数计,包含以下组分:碳化硅96%‑99%、三氧化二铝0.5%‑1%及石墨烯0.5%‑3%;所述碳化硅石墨烯复合防弹陶瓷的抗弯强度为490‑560Mpa,维氏硬度为2400‑2500HV,断裂韧性为5‑6.5Mpa•m1/2,密度为2.6‑3.1g/cm3;一种碳化硅石墨烯复合防弹陶瓷制备方法,包括以下步骤:S1、备料;S2、石墨烯的溶解;S3、石墨烯溶液的分散;S4、混料;S5、均料;S6、造粒;S7、压制成型;S8、无压烧结。
Description
技术领域
本发明涉及防弹陶瓷技术领域,特别涉及一种碳化硅石墨烯复合防弹陶瓷及制备方法。
背景技术
防弹插板材料作为防弹衣的防护核心,对于保障战士的生命安全、提高作战效能都具有极其重要的作用。现有防弹材料中,陶瓷材料因具有高强度、高硬度及高耐磨性的性能特点而作为首选材料。在陶瓷材料中,碳化硅因其较低的密度、适中的硬度及高性价比被选为第三代防弹插板材料而被广泛应用;碳化硼因其仅次于金刚石和立方氮化硼的超高硬度、及低密度、高弹性模量而作为性能优良的***防弹插板材料。与碳化硅相比,碳化硼虽然性能优良,但其成本较高,因此,如何进一步增加具有高性价比的碳化硅材料的强度、韧性,以及降低其密度,成为热门的研究方向。
发明内容
有鉴于此,有必要提供一种碳化硅石墨烯复合防弹陶瓷及其制备方法。
根据本发明的一个方面,提供了一种碳化硅石墨烯复合防弹陶瓷,按重量百分数计,包含以下组分:碳化硅96%-99%、三氧化二铝0.5%-1%及石墨烯0.5%-3%;所述碳化硅石墨烯复合防弹陶瓷的抗弯强度为490-560Mpa,维氏硬度为2400-2500HV,断裂韧性为5-6.5Mpa·m1/2、密度为2.6-3.1g/cm3。
根据本发明的另一方面,还提供了一种碳化硅石墨烯复合防弹陶瓷的制备方法,包括以下步骤:
S1、备料:
按重量份数计,准备以下原料:碳化硅粉100份、PVA 4-6份、树脂8-11份、正辛醇0.5-1.5份、丙三醇1-1.5份、三氧化二铝0.5-1份、石墨烯0.5-3份及聚乙烯吡咯烷酮0.5-1份;
S2、石墨烯的溶解:
将石墨烯充分溶解于去离子水中,获得石墨烯溶液;
S3、石墨烯溶液的分散:
先将石墨烯溶液利用微波辐射1h;然后向石墨烯溶液中加入聚乙烯吡咯烷酮,搅拌1h,获得石墨烯分散液;
S4、混料:
首先将PVA、树脂、正辛醇、丙三醇、三氧化二铝及碳化硅粉加入高速球磨罐中,均匀混料1h,获得碳化硅浆料;
然后将石墨烯分散液加入高速球磨罐中,和碳化硅浆料一起混合12h,获得碳化硅石墨烯浆料;
S5、均料:
将上述碳化硅石墨烯浆料在均质机中均匀混合,获得均匀化的碳化硅石墨烯浆料;
S6、造粒:
采用喷雾造粒塔将碳化硅石墨烯浆料进行喷雾造粒,获得100-200μm的造粒粉小球;
S7、压制成型:采用液压机将造粒粉小球压制成预定规格的陶瓷素坯;
S8、无压烧结:将陶瓷素坯进行温度为2100-2200℃,保温时间3-4h的无压烧结,获得碳化硅石墨烯复合防弹陶瓷。
优选的,步骤S1中,按重量份数计,准备以下原料:碳化硅粉100份、PVA4.5-5.5、树脂9-11、正辛醇0.4-0.6份、丙三醇1-1.5份、三氧化二铝0.5-1份、石墨烯1-2份及聚乙烯吡咯烷酮0.5-1份。
优选的,所述步骤S1中,按重量份数计,准备以下原料:碳化硅粉100份、PVA5份、树脂10份、正辛醇1份、丙三醇1.25份、三氧化二铝0.75份、石墨烯2份及聚乙烯吡咯烷酮0.75份。
优选的,所述树脂为酚醛树脂。
优选的,所述碳化硅粉颗粒粒度D50不大于0.5μm,纯度不低于99%;所述石墨烯的颗粒粒度D50不大于12μm。
优选的,所述碳化硅粉颗粒粒度D50为0.5μm,纯度为99.5%;所述石墨烯的颗粒粒度D50为12μm。
优选的,所述碳化硅粉由颗粒粒度D50不大于12μm的碳化硅原料经过研磨和提纯获得。
优选的,所述研磨和提纯步骤如下:
将碳化硅原料通过砂磨机研磨成D50不大于0.5μm的碳化硅微粉,然后投入盐酸和氢氟酸中,加热搅拌1h,接着用去离子水清洗6-8遍,再依次进行压滤、烘干和破碎,获得颗粒粒度D50不大于0.5μm、纯度不低于99%的碳化硅粉。所述盐酸和氢氟酸的质量百分比均为15%-20%;所述盐酸和氢氟酸的质量百分比以碳化硅原料的质量为基准。
上述碳化硅石墨烯复合防弹陶瓷,通过在碳化硅中引入具有低密度、高强度等优异性能,且与碳化硅的相容性良好、热膨胀系数相近的石墨烯作为第二相材料,并通过调控石墨烯在碳化硅中的含量,以及通过本发明提供的制备方法,使石墨烯在碳化硅中分散更加稳定及均匀,以复合增强、增韧及降低密度的机制来提高碳化硅作为防弹陶瓷材料的整体性能;与现有技术中的碳化硅陶瓷相比,本发明提供的碳化硅石墨烯复合防弹陶瓷,在抗弯强度、维氏硬度、断裂韧性上具有显著的提高,而密度均有显著的减小;因此,本发明提供的碳化硅石墨烯复合防弹陶瓷,具有更优良的抗弯性能、更高的强度及韧性,以及更轻的重量,质量及防护性能得到了进一步提高。
附图说明
图1为本发明为本发明中碳化硅石墨烯复合防弹陶瓷的制备方法流程。
具体实施方式
以下结合本发明的附图,对本发明实施例的技术方案以及技术效果做进一步的详细阐述。
在本发明一种典型的实施方式中,提供了一种碳化硅石墨烯复合防弹陶瓷,按重量百分数计,包含以下组分:碳化硅96%-99%、三氧化二铝0.5%-1%及石墨烯0.5%-3%;所述碳化硅石墨烯复合防弹陶瓷的抗弯强度为490-560Mpa,维氏硬度为2400-2500HV,断裂韧性为5-6.5Mpa·m1/2,密度为2.6-3.1g/cm3。
在本发明实施例中,由于石墨烯具有低密度、高强度等优异性能,且与碳化硅的相容性良好,热膨胀系数相近,在碳化硅中引入石墨烯作为第二相材料,并通过调控石墨烯在碳化硅中的含量,通过复合增强、增韧及降低密度的机制来提高碳化硅作为陶瓷材料时的整体性能。
参见图1所示,在本发明又一种典型的实施方式中,还提供了一种上述碳化硅石墨烯复合防弹陶瓷的制备方法,包括以下步骤:
S1、备料:
按重量份数计,准备以下原料:碳化硅粉100份、PVA 4-6份、树脂8-11份、正辛醇0.5-1.5份、丙三醇1-1.5份、三氧化二铝0.5-1份、石墨烯0.5-3份及聚乙烯吡咯烷酮0.5-1份;
S2、石墨烯的溶解:
将石墨烯充分溶解于去离子水中,获得石墨烯溶液;
S3、石墨烯溶液的分散:
先将石墨烯溶液利用微波辐射1h;然后向石墨烯溶液中加入聚乙烯吡咯烷酮,搅拌1h,获得石墨烯分散液;所述石墨烯溶液置于微波热解炉中进行微波加热辐射,所述石墨烯溶液被微波热解炉所产生的微波包围,以便石墨烯溶液能够被微波辐射所发出的热量更加均匀地包围。
由于石墨烯溶液的稳定性差,不易分散,且分散不好容易产生聚沉的问题,对最终制备的碳化硅石墨烯复合防弹陶瓷的性能产生负面影响,因此,本发明实施例中,通过物理和化学改性方法相结合的方式,对石墨烯溶液进行分散;先通过微波进行辐射加热1h,通过将石墨烯溶液置于微波热解炉中,按照每分钟5摄氏度的升温速率进行升温,升至80摄氏度后,恒温保温10min;,由于微波辐射时,微波直接与受热物质的粒子相作用,因此通过微波加热的方法能够更直接地破坏石墨烯片层间的范德华力,促进石墨烯的分散,且微波辐射加热时,石墨烯受热更加均匀,且在几分钟到十几分钟的短时间内即可完成,效率更高;之后再向石墨烯溶液中加入聚乙烯吡咯烷酮,由于聚乙烯吡咯烷酮具有优良的分散性能,在片层间的范德华力已被破坏的石墨烯的表面进行枝接,以进一步扩大石墨烯的层间距,阻碍石墨烯片层的团聚,加上搅拌,最终得到均匀、稳定且具有高分散性的石墨烯分散液;
S4、混料:
首先将PVA、树脂、正辛醇、丙三醇、三氧化二铝及碳化硅粉加入高速球磨罐中,均匀混料1h,获得碳化硅浆料;
然后将石墨烯分散液加入高速球磨罐中,和碳化硅浆料一起混合12h,获得碳化硅石墨烯浆料;
S5、均料:
将上述碳化硅石墨烯浆料在均质机中均匀混合,获得均匀化的碳化硅石墨烯浆料;例如,所述均质机可以采用MXR-D450型实验室均质机,均料转速为3000rpm;
S6、造粒:
采用喷雾造粒塔将均匀化的碳化硅石墨烯浆料进行喷雾造粒,获得100-200μm的造粒粉小球;
S7、压制成型:采用液压机将造粒粉小球压制成预定规格的陶瓷素坯;
S8、无压烧结:将陶瓷素坯进行温度为2100-2200℃,保温时间3-4h的无压烧结,获得碳化硅石墨烯复合防弹陶瓷。
进一步地,步骤S1中,按重量份数计,准备以下原料:碳化硅粉100份、PVA4.5-5.5份、树脂9-11份、正辛醇0.4-0.6份、丙三醇1-1.5份、三氧化二铝0.5-1份、石墨烯1-2份及聚乙烯吡咯烷酮0.5-1份。
进一步地,步骤S1中,按重量份数计,准备以下原料:碳化硅粉100份、PVA5份、树脂10份、正辛醇1份、丙三醇1.25份、三氧化二铝0.75份、石墨烯2份及聚乙烯吡咯烷酮0.75份。
进一步地,所述树脂为酚醛树脂。
进一步地,所述碳化硅粉颗粒粒度D50不大于0.5μm,纯度不低于99%;所述石墨烯的颗粒粒度D50不大于12μm。
进一步地,所述碳化硅粉颗粒粒度D50为0.5μm,纯度为99.5%;所述石墨烯的颗粒粒度D50为12μm。
进一步地,所述碳化硅粉由颗粒粒度D50不大于12μm的碳化硅原料经过研磨和提纯获得。
进一步地,所述研磨和提纯步骤如下:
将碳化硅原料通过砂磨机研磨成D50不大于0.5μm的碳化硅微粉,然后投入盐酸和氢氟酸中加热搅拌1h,接着用去离子水清洗6-8遍,再依次进行压滤、烘干和破碎,获得颗粒粒度D50不大于0.5μm、纯度不低于99%的碳化硅粉;所述盐酸和氢氟酸的质量百分比均为15%-20%;所述盐酸和氢氟酸的质量百分比以碳化硅原料的质量为基准。例如,碳化硅原料为1000g,则盐酸和氢氟酸均为15~20g。
由于碳化硅原料中的O、N及C等杂质在高温烧结过程中往往通过气相发挥,会增加陶瓷的气孔率,其它杂质在高温下也会在一定程度上参与物化反应,生成的物相易在晶界处聚集,最终影响产品的性能;碳化硅原料通过上述提纯和研磨的过程,杂质被清除干净,纯度提高,使得最终制得的产品性能更加优良。
下面将结合具体实施例对本发明的有益效果进一步详细说明。
实施例1~实施例12
本发明实施例提供的碳化硅石墨烯复合防弹陶瓷,由本发明提供的上述制备方法制备而得。
其中,在本发明实施例中,石墨烯的颗粒粒度D50为12μm;
碳化硅粉的颗粒粒度D50为0.5μm,纯度为99.5%,由颗粒粒度D50为12μm的碳化硅原料,首先经过砂磨机研磨,然后投入盐酸和氢氟酸溶液中,加热搅拌1h,接着用去离子水清洗,再依次进行压滤、烘干和破碎而得;
所述树脂采用酚醛树脂;
所述石墨烯溶液的分散:先将石墨烯溶液利用微波辐射1h;然后向石墨烯溶液中加入聚乙烯吡咯烷酮,搅拌1h,获得石墨烯分散液;
所述配料中,首先将PVA、树脂、正辛醇、丙三醇、三氧化二铝及碳化硅粉加入高速球磨罐中,均匀混料1h,获得碳化硅浆料;
然后将石墨烯分散液加入高速球磨罐中,和碳化硅浆料一起混合12h,获得碳化硅石墨烯浆料;
所述无压烧结工艺中,将陶瓷素坯进行温度为2100-2200℃,保温时间3-4的无压烧结,获得碳化硅石墨烯复合防弹陶瓷。
其它参数详见表1。
通过上述方法制备的碳化硅石墨烯复合防弹陶瓷的性能详见表2。
表1
现有技术中碳化硅防弹陶瓷的性能为,抗弯强度400MPa,维氏硬度2400HV,断裂韧性5MPa·m1/2,密度3.15g/cm3,本发明具体实施例中制备的碳化硅石墨烯复合防弹陶瓷的性能如表2中所列,相较之下,可知,本发明提供的碳化硅石墨烯复合防弹陶瓷,在抗弯强度、维氏硬度、断裂韧性上具有显著的提高,而密度均有显著的减小;因此,与现有技术相比,本发明提供的碳化硅石墨烯复合防弹陶瓷,具有更优良的抗弯性能、更高的强度及韧性,以及更轻的重量,质量及防护性能得到了进一步提高。
表2
以上所揭露的仅为本发明较佳实施例而已,当然不能以此来限定本发明之权利范围,本领域普通技术人员可以理解实现上述实施例的全部或部分流程,并依本发明权利要求所作的等同变化,仍属于发明所涵盖的范围。
Claims (9)
1.一种碳化硅石墨烯复合防弹陶瓷,其特征在于,按重量百分数计,包含以下组分:碳化硅96%-99%、三氧化二铝0.5%-1%及石墨烯0.5%-3%;所述碳化硅石墨烯复合防弹陶瓷的抗弯强度为490-560Mpa,维氏硬度为2400-2500HV,断裂韧性为5-6.5Mpa•m1/2,密度为2.6-3.1g/cm3。
2.如权利要求1所述的碳化硅石墨烯复合防弹陶瓷的制备方法,其特征在于:包括以下步骤:
S1、备料:
按重量份数计,准备以下原料:碳化硅粉100份、PVA 4-6份、树脂8-11份、正辛醇0.5-1.5份、丙三醇1-1.5份、三氧化二铝0.5-1份、石墨烯0.5-3份及聚乙烯吡咯烷酮0.5-1份;
S2、石墨烯的溶解:
将石墨烯充分溶解于去离子水中,获得石墨烯溶液;
S3、石墨烯溶液的分散:
先将石墨烯溶液利用微波辐射1h;然后向石墨烯溶液中加入聚乙烯吡咯烷酮,搅拌1h,获得石墨烯分散液;
S4、混料:
首先将PVA、树脂、正辛醇、丙三醇、三氧化二铝及碳化硅粉加入高速球磨罐中,均匀混料1h,获得碳化硅浆料;
然后将石墨烯分散液加入高速球磨罐中,和碳化硅浆料一起混合12h,获得碳化硅石墨烯浆料;
S5、均料:
将上述碳化硅石墨烯浆料在均质机中均匀混合,获得均匀化的碳化硅石墨烯浆料;
S6、造粒:
采用喷雾造粒塔将均匀化的碳化硅石墨烯浆料进行喷雾造粒,获得100-200μm的造粒粉小球;
S7、压制成型:采用液压机将造粒粉小球压制成预定规格的陶瓷素坯;
S8、无压烧结:将陶瓷素坯进行温度为2100-2200℃,保温时间3-4h的无压烧结,获得碳化硅石墨烯复合防弹陶瓷。
3.如权利要求2所述的碳化硅石墨烯复合防弹陶瓷的制备方法,其特征在于:所述步骤S1中,按重量份数计,准备以下原料:碳化硅粉100份、PVA4.5-5.5份、树脂9-11份、正辛醇0.4-0.6份、丙三醇1-1.5份、三氧化二铝0.5-1份、石墨烯1-2份及聚乙烯吡咯烷酮0.5-1份。
4.如权利要求2所述的碳化硅石墨烯复合防弹陶瓷的制备方法,其特征在于:所述步骤S1中,按重量份数计,准备以下原料:碳化硅粉100份、PVA5份、树脂10份、正辛醇1份、丙三醇1.25份、三氧化二铝0.75份、石墨烯2份及聚乙烯吡咯烷酮0.75份。
5.如权利要求2~4所述的碳化硅石墨烯复合防弹陶瓷的制备方法,其特征在于:所述树脂为酚醛树脂。
6.如权利要求2~4所述的碳化硅石墨烯复合防弹陶瓷的制备方法,其特征在于:所述碳化硅粉颗粒粒度D50不大于0.5μm,纯度不低于99%;所述石墨烯的颗粒粒度D50不大于12μm。
7.如权利要求2~4所述的碳化硅石墨烯复合防弹陶瓷的制备方法,其特征在于:所述碳化硅粉颗粒粒度D50为0.5μm,纯度为99.5%;所述石墨烯的颗粒粒度D50为12μm。
8.如权利要求2~4所述的碳化硅石墨烯复合防弹陶瓷制备方法,其特征在于:所述碳化硅粉由颗粒粒度D50不大于12μm的碳化硅原料经过研磨和提纯获得。
9.如权利要求8所述的碳化硅石墨烯复合防弹陶瓷制备方法,其特征在于:所述研磨和提纯步骤如下:
将碳化硅原料通过砂磨机研磨成D50不大于0.5μm的碳化硅微粉,然后投入盐酸和氢氟酸中,加热搅拌1h,接着用去离子水清洗6-8遍,再依次进行压滤、烘干和破碎,获得颗粒粒度D50不大于0.5μm、纯度不低于99%的碳化硅粉。
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