CN116639982B - 一种碳化硼陶瓷的制备方法及其在防弹头盔中的应用 - Google Patents
一种碳化硼陶瓷的制备方法及其在防弹头盔中的应用 Download PDFInfo
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- Y02E30/30—Nuclear fission reactors
Abstract
本发明提供了一种碳化硼陶瓷的制备方法及其在防弹头盔中的应用,所述碳化硼陶瓷的制备方法,包括制备混合料、制备改性混合料、制备浆料、造粒、密闭处理、制备坯体、烧结步骤;所述制备浆料步骤为,将改性混合料与胡麻胶、酚醛树脂、海藻酸钠、氧化锌、轻钙粉混合,加入去离子水,进行球磨处理,球磨结束后以0.8‑1.2℃/min速率降温至1.0‑1.5℃,在1.0‑1.5℃下静置1.2‑1.4h,恢复至室温制得浆料。本发明制得的碳化硼陶瓷,在降低陶瓷密度的同时,提高防弹性能和抗氧化性能,应用至防弹头盔中,经实弹测试,凹陷17.3‑18.4mm,裂痕只在弹着点附近陶瓷块内,没有明显扩展。
Description
技术领域
本发明属于陶瓷制备技术领域,具体涉及一种碳化硼陶瓷的制备方法及其在防弹头盔中的应用。
背景技术
碳化硼陶瓷具有质轻、硬度高、耐高温等优良的性能,是防弹头盔的绝佳用材;
但是,碳化硼陶瓷属于无机材料,分子之间只有共价键,所以性脆,导致其受到子弹高速撞击时容易崩解和碎裂;因此,提高碳化硼陶瓷的抗弯强度和断裂热性,从而增强防弹性能是非常必要的。
现有技术通常是通过加入二硼化钛等硼化物、碳化钛等碳化物等助剂的方法以解决上述问题,但是助剂与在碳化硼基体内很难形成完美的均匀分布,在助剂加入量较少时,抗弯强度和断裂韧性的提升性能有限,其防弹性能仍然较差;助剂加入量较多时,会明显提高防弹性能,但是会因为加入了较多的密度较大的助剂,使得产物的密度明显大于单相碳化硼的理论密度,不能满足防弹头盔质轻的需求;
并且,现有技术制备的碳化硼陶瓷抗氧化性能较差,在高温氧化之后,陶瓷的抗弯强度和断裂韧性明显下降,不能满足使用要求。
因此,提供一种碳化硼陶瓷的制备方法及其在防弹头盔中的应用,在降低陶瓷密度的同时,提高防弹性能以及抗氧化性能是现有技术亟待解决的技术问题。
发明内容
针对现有技术存在的不足,本发明提供了一种碳化硼陶瓷的制备方法及其在防弹头盔中的应用,在降低陶瓷密度的同时,提高防弹性能和抗氧化性能。
为解决上述技术问题,本发明采取的技术方案如下:
1.制备混合料
将碳化硼粉、氧化铝、金属铝、单质硅、二氧化钛、石墨粉混合,进行第一次球磨处理,控制第一次球磨处理的球料比为6-10:1,转速为660-680rpm,球磨时间为2.3-2.5h,球磨温度为65-67℃,第一次球磨处理结束后得到初混料,然后向初混料中加入木鱼石粉、海藻酸钠进行第二次球磨处理,控制第二次球磨处理的球料比为10-14:1,转速为730-750rpm,球磨时间为2.0-2.2h,球磨温度为50-54℃,第二次球磨结束后得到混合料;
所述碳化硼粉、氧化铝、金属铝、单质硅、二氧化钛与石墨粉的质量比为80-85:4.8-5.2:3.8-4.2:2.6-3.3:1.7-2.4:3.9-4.2;
所述初混料与木鱼石粉、海藻酸钠的质量比为100-120:1-2.5:4-6;
所述金属铝的粒径为70-80μm,所述单质硅的粒径为60-65μm;
所述碳化硼粉中B4C>99wt%,碳化硼粉的粒径为12-14μm;
所述石墨粉的粒径为78-82μm。
2.制备改性混合料
(1)初步改性
将混合料进行超声-低温等离子体处理,超声波的频率为56-58kHz,声能密度为0.6-0.8W/mL,超声时间为13-18min,低温等离子体处理气氛为氮气和氧气的混合气体,氮气和氧气的体积比为1.5-1.8:1,处理压力为58-62Pa,放电功率为115-125W,处理时间为7-9min,超声-低温等离子体处理结束后制得初步改性混合料;
(2)深度改性
将初步改性混合料与改性剂混合,然后置于均质机中进行两次均质处理,控制第一次均质时间为10-14min,均质温度为38-42℃,均质压力为28-33MPa,第一次均质处理结束后第二次均质处理,控制第二次均质时间为7-9min,均质温度为43-47℃,均质压力为24-26MPa,第二次均质结束后,干燥,完成深度改性步骤,制得改性混合料;
所述改性剂的制备步骤为,将乙醇、棕榈酸、β-二酮、季戊四醇、羧甲基纤维素钠、硬脂酸钙混合,控制搅拌速度为440-460rpm,搅拌时间为9-12min,搅拌结束后置于1.8-2.3℃下静置1.3-1.7h,静置结束,自然恢复至室温后制得改性剂;
所述初步改性混合料与改性剂的质量比为1:4.5-5.6;
所述乙醇、棕榈酸、β-二酮、季戊四醇、羧甲基纤维素钠、硬脂酸钙的质量比为38-46:1.2-1.5:1.5-1.7:3.5-4.6:2.7-3.2:2.6-3.4。
3.制备浆料
将改性混合料与胡麻胶、酚醛树脂、海藻酸钠、氧化锌、轻钙粉混合,然后加入去离子水,进行球磨处理,控制球料比为5-7:1,球磨转速为565-600rpm,球磨温度为43-47℃,球磨时间为1.2-1.6h,球磨结束后以0.8-1.2℃/min速率将温度降低至1.0-1.5℃,置于1.0-1.5℃下静置1.2-1.4h,静置结束后自然恢复至室温,制得浆料;
所述轻钙粉的粒径为12-15μm;
所述改性混合料、去离子水、胡麻胶、酚醛树脂、海藻酸钠、氧化锌与轻钙粉的质量比为36-40:100-120:1.2-1.4:2.4-2.6:2.7-3.2:1.8-2.1:1.0-1.4。
4.造粒
将浆料喷雾干燥进行造粒,控制喷雾干燥的进口温度为200-220℃,出口温度为95-105℃,控制造粒机的温度为135-140℃,制得造粒粉。
5.密闭处理
将造粒粉置于真空手套箱中,控制温度为78-82℃,通入氩气,保持压力为0.08-0.12MPa,处理时间为2.7-3.2h,完成密闭处理。
6.制备坯体
将密闭处理后的造粒料在128-132℃、48-52MPa条件下进行注射成型,注射完毕后,冷却得到素坯, 将素坯置于真空炉中进行脱脂,控制真空度为96-105Pa,脱脂时间为2.1-2.5h,脱脂温度为345-354℃,制得坯体。
7.烧结
(1)预烧结
将坯体置于真空炉中通入氮气进行预烧结,控制预烧结的真空度为0.03-0.05MPa,烧结温度为1080-1150℃,烧结时间为1.5-2.0h,然后以1.0-1.2℃/min速率将温度降低至7.5-8.4℃,完成预烧结步骤,制得预烧结坯体;
(2)二次烧结
将预烧结坯体置于真空炉中进行二次烧结,控制真空度为为0.03-0.05MPa,先是在770-790℃下烧结1.4-2.3h,然后以1.3-1.7℃/min速率升温至1650-1680℃,在1650-1680℃下烧结1.1-1.3h,再以2.8-3.3℃/min速率降温至810-830℃,在810-830℃下烧结1.5-1.8h,自然冷却至室温后制得碳化硼陶瓷。
与现有技术相比,本发明的有益效果如下:
1.本发明碳化硼陶瓷的制备方法,在制备混合料的过程中,采用氧化铝、石墨作为原料,降低了陶瓷的密度;
本发明采用特定的改性混合料,提高了粉料之间的相容性,与特定的制备浆料步骤、密闭处理步骤相结合,提高了陶瓷内部的致密度和均匀度,从而提高了陶瓷的硬度、弯曲强度、断裂韧性以及高温抗氧化性能;
本发明碳化硼陶瓷的制备方法,使得粉料在碳化硼基体中呈现均匀的分布,不会出现团聚现象,密度均匀,致密度好,从而增强了陶瓷的防弹能力;
2.本发明制得的碳化硼陶瓷,密度为2.18-2.21g/cm3,致密度为98.4-98.7%(GB/T25995-2010);
3.本发明制得的碳化硼陶瓷,硬度为34-37Gpa,抗弯强度为476-479MPa,断裂韧性为6.2-6.4 MPa·m0.5;
在温度为1350℃中氧化7d后,硬度为31-36Gpa(GB/T 16534-2009),抗弯强度为470-477MPa(GB/T 6569-2006),断裂韧性为5.9-6.3 MPa·m0.5(GB/T 23806-2009);
4.本发明制得的碳化硼陶瓷应用至防弹头盔中,经实弹测试,凹陷17.3-18.4mm,裂痕只在弹着点附近陶瓷块内,没有明显扩展。
具体实施方式
为了对本发明的技术特征、目的和效果有更加清楚的理解,现说明本发明的具体实施方式。
实施例1
1.制备混合料
将碳化硼粉、氧化铝、金属铝、单质硅、二氧化钛、石墨粉混合,进行第一次球磨处理,控制第一次球磨处理的球料比为8:1,转速为670rpm,球磨时间为2.4h,球磨温度为66℃,第一次球磨处理结束后得到初混料,然后向初混料中加入木鱼石粉、海藻酸钠进行第二次球磨处理,控制第二次球磨处理的球料比为12:1,转速为740rpm,球磨时间为2.1h,球磨温度为52℃,第二次球磨结束后得到混合料;
所述碳化硼粉、氧化铝、金属铝、单质硅、二氧化钛与石墨粉的质量比为82:5:4:3:2:4;
所述初混料与木鱼石粉、海藻酸钠的质量比为110:2:5;
所述金属铝的粒径为75μm,所述单质硅的粒径为 62μm;
所述碳化硼粉中B4C>99wt%,碳化硼粉的粒径为13μm;
所述石墨粉的粒径为80μm。
2.制备改性混合料
(1)初步改性
将混合料进行超声-低温等离子体处理,超声波的频率为57kHz,声能密度为0.7W/mL,超声时间为15min,低温等离子体处理气氛为氮气和氧气的混合气体,氮气和氧气的体积比为1.6:1,处理压力为60Pa,放电功率为120W,处理时间为8min,超声-低温等离子体处理结束后制得初步改性混合料;
(2)深度改性
将初步改性混合料与改性剂混合,然后置于均质机中进行两次均质处理,控制第一次均质时间为12min,均质温度为40℃,均质压力为30MPa,第一次均质处理结束后第二次均质处理,控制第二次均质时间为8min,均质温度为45℃,均质压力为25MPa,第二次均质结束后,干燥,完成深度改性步骤,制得改性混合料;
所述改性剂的制备步骤为,将乙醇、棕榈酸、β-二酮、季戊四醇、羧甲基纤维素钠、硬脂酸钙混合,控制搅拌速度为450rpm,搅拌时间为10min,搅拌结束后置于2℃下静置1.5h,静置结束,自然恢复至室温后制得改性剂;
所述初步改性混合料与改性剂的质量比为1:5;
所述乙醇、棕榈酸、β-二酮、季戊四醇、羧甲基纤维素钠、硬脂酸钙的质量比为40:1.4:1.6:4:3:3。
3.制备浆料
将改性混合料与胡麻胶、酚醛树脂、海藻酸钠、氧化锌、轻钙粉混合,然后加入去离子水,进行球磨处理,控制球料比为6:1,球磨转速为580rpm,球磨温度为45℃,球磨时间为1.4h,球磨结束后以1℃/min速率将温度降低至1.2℃,置于1.2℃下静置1.3h,静置结束后自然恢复至室温,制得浆料;
所述轻钙粉的粒径为13μm;
所述改性混合料、去离子水、胡麻胶、酚醛树脂、海藻酸钠、氧化锌与轻钙粉的质量比为38:100:1.3:2.5:3:2:1.2。
4.造粒
将浆料喷雾干燥进行造粒,控制喷雾干燥的进口温度为210℃,出口温度为100℃,控制造粒机的温度为138℃,制得造粒粉。
5.密闭处理
将造粒粉置于真空手套箱中,控制温度为80℃,通入氩气,保持压力为0.1MPa,处理时间为3h,完成密闭处理。
6.制备坯体
将密闭处理后的造粒料在130℃、50MPa条件下进行注射成型,注射完毕后,冷却得到素坯, 将素坯置于真空炉中进行脱脂,控制真空度为100Pa,脱脂时间为2.3h,脱脂温度为350℃,制得坯体。
7.烧结
(1)预烧结
将坯体置于真空炉中通入氮气进行预烧结,控制预烧结的真空度为0.04MPa,烧结温度为1100℃,烧结时间为1.7h,然后以1.1℃/min速率将温度降低至8℃,完成预烧结步骤,制得预烧结坯体;
(2)二次烧结
将预烧结坯体置于真空炉中进行二次烧结,控制真空度为为0.04MPa,先是在780℃下烧结2h,然后以1.5℃/min速率升温至1670℃,在1670℃下烧结1.2h,再以3℃/min速率降温至820℃,在820℃下烧结1.6h,自然冷却至室温后制得碳化硼陶瓷。
实施例2
1.制备混合料
将碳化硼粉、氧化铝、金属铝、单质硅、二氧化钛、石墨粉混合,进行第一次球磨处理,控制第一次球磨处理的球料比为6:1,转速为660rpm,球磨时间为2.3h,球磨温度为65℃,第一次球磨处理结束后得到初混料,然后向初混料中加入木鱼石粉、海藻酸钠进行第二次球磨处理,控制第二次球磨处理的球料比为10:1,转速为730rpm,球磨时间为2.2h,球磨温度为50℃,第二次球磨结束后得到混合料;
所述碳化硼粉、氧化铝、金属铝、单质硅、二氧化钛与石墨粉的质量比为80:4.8:3.8:2.6:1.7:3.9;
所述初混料与木鱼石粉、海藻酸钠的质量比为100:1:4;
所述金属铝的粒径为70μm,所述单质硅的粒径为 60μm;
所述碳化硼粉中B4C>99wt%,碳化硼粉的粒径为12μm;
所述石墨粉的粒径为78μm。
2.制备改性混合料
(1)初步改性
将混合料进行超声-低温等离子体处理,超声波的频率为56kHz,声能密度为0.6W/mL,超声时间为13min,低温等离子体处理气氛为氮气和氧气的混合气体,氮气和氧气的体积比为1.5:1,处理压力为58Pa,放电功率为115W,处理时间为7min,超声-低温等离子体处理结束后制得初步改性混合料;
(2)深度改性
将初步改性混合料与改性剂混合,然后置于均质机中进行两次均质处理,控制第一次均质时间为10min,均质温度为38℃,均质压力为28MPa,第一次均质处理结束后第二次均质处理,控制第二次均质时间为7min,均质温度为43℃,均质压力为24MPa,第二次均质结束后,干燥,完成深度改性步骤,制得改性混合料;
所述改性剂的制备步骤为,将乙醇、棕榈酸、β-二酮、季戊四醇、羧甲基纤维素钠、硬脂酸钙混合,控制搅拌速度为440rpm,搅拌时间为9min,搅拌结束后置于1.8℃下静置1.3h,静置结束,自然恢复至室温后制得改性剂;
所述初步改性混合料与改性剂的质量比为1:4.5;
所述乙醇、棕榈酸、β-二酮、季戊四醇、羧甲基纤维素钠、硬脂酸钙的质量比为38:1.2:1.5:3.5:2.7:2.6。
3.制备浆料
将改性混合料与胡麻胶、酚醛树脂、海藻酸钠、氧化锌、轻钙粉混合,然后加入去离子水,进行球磨处理,控制球料比为5:1,球磨转速为565rpm,球磨温度为43℃,球磨时间为1.6h,球磨结束后以0.8℃/min速率将温度降低至1.0℃,置于1.0℃下静置1.2h,静置结束后自然恢复至室温,制得浆料;
所述轻钙粉的粒径为12μm;
所述改性混合料、去离子水、胡麻胶、酚醛树脂、海藻酸钠、氧化锌与轻钙粉的质量比为36:100:1.2:2.4:2.7:1.8:1.0。
4.造粒
将浆料喷雾干燥进行造粒,控制喷雾干燥的进口温度为200℃,出口温度为95℃,控制造粒机的温度为135℃,制得造粒粉。
5.密闭处理
将造粒粉置于真空手套箱中,控制温度为78℃,通入氩气,保持压力为0.08MPa,处理时间为3.2h,完成密闭处理。
6.制备坯体
将密闭处理后的造粒料在128℃、48MPa条件下进行注射成型,注射完毕后,冷却得到素坯, 将素坯置于真空炉中进行脱脂,控制真空度为96Pa,脱脂时间为2.1h,脱脂温度为345℃,制得坯体。
7.烧结
(1)预烧结
将坯体置于真空炉中通入氮气进行预烧结,控制预烧结的真空度为0.03MPa,烧结温度为1080℃,烧结时间为1.5h,然后以1.0℃/min速率将温度降低至7.5℃,完成预烧结步骤,制得预烧结坯体;
(2)二次烧结
将预烧结坯体置于真空炉中进行二次烧结,控制真空度为为0.03MPa,先是在770℃下烧结1.4h,然后以1.3℃/min速率升温至1650℃,在1650℃下烧结1.3h,再以2.8℃/min速率降温至810℃,在810℃下烧结1.8h,自然冷却至室温后制得碳化硼陶瓷。
实施例3
1.制备混合料
将碳化硼粉、氧化铝、金属铝、单质硅、二氧化钛、石墨粉混合,进行第一次球磨处理,控制第一次球磨处理的球料比为10:1,转速为680rpm,球磨时间为2.5h,球磨温度为67℃,第一次球磨处理结束后得到初混料,然后向初混料中加入木鱼石粉、海藻酸钠进行第二次球磨处理,控制第二次球磨处理的球料比为14:1,转速为750rpm,球磨时间为2.0h,球磨温度为54℃,第二次球磨结束后得到混合料;
所述碳化硼粉、氧化铝、金属铝、单质硅、二氧化钛与石墨粉的质量比为85:5.2:4.2:3.3:2.4:4.2;
所述初混料与木鱼石粉、海藻酸钠的质量比为120:2.5:6;
所述金属铝的粒径为80μm,所述单质硅的粒径为65μm;
所述碳化硼粉中B4C>99wt%,碳化硼粉的粒径为14μm;
所述石墨粉的粒径为82μm。
2.制备改性混合料
(1)初步改性
将混合料进行超声-低温等离子体处理,超声波的频率为58kHz,声能密度为0.8W/mL,超声时间为18min,低温等离子体处理气氛为氮气和氧气的混合气体,氮气和氧气的体积比为1.8:1,处理压力为62Pa,放电功率为125W,处理时间为9min,超声-低温等离子体处理结束后制得初步改性混合料;
(2)深度改性
将初步改性混合料与改性剂混合,然后置于均质机中进行两次均质处理,控制第一次均质时间为14min,均质温度为42℃,均质压力为33MPa,第一次均质处理结束后第二次均质处理,控制第二次均质时间为9min,均质温度为47℃,均质压力为26MPa,第二次均质结束后,干燥,完成深度改性步骤,制得改性混合料;
所述改性剂的制备步骤为,将乙醇、棕榈酸、β-二酮、季戊四醇、羧甲基纤维素钠、硬脂酸钙混合,控制搅拌速度为460rpm,搅拌时间为12min,搅拌结束后置于2.3℃下静置1.7h,静置结束,自然恢复至室温后制得改性剂;
所述初步改性混合料与改性剂的质量比为1:5.6;
所述乙醇、棕榈酸、β-二酮、季戊四醇、羧甲基纤维素钠、硬脂酸钙的质量比为46:1.5:1.7:4.6:3.2:3.4。
3.制备浆料
将改性混合料与胡麻胶、酚醛树脂、海藻酸钠、氧化锌、轻钙粉混合,然后加入去离子水,进行球磨处理,控制球料比为7:1,球磨转速为600rpm,球磨温度为47℃,球磨时间为1.2h,球磨结束后以1.2℃/min速率将温度降低至1.5℃,置于1.5℃下静置1.4h,静置结束后自然恢复至室温,制得浆料;
所述轻钙粉的粒径为15μm;
所述改性混合料、去离子水、胡麻胶、酚醛树脂、海藻酸钠、氧化锌与轻钙粉的质量比为40:120:1.4:2.6:3.2:2.1:1.4。
4.造粒
将浆料喷雾干燥进行造粒,控制喷雾干燥的进口温度为220℃,出口温度为105℃,控制造粒机的温度为140℃,制得造粒粉。
5.密闭处理
将造粒粉置于真空手套箱中,控制温度为82℃,通入氩气,保持压力为0.12MPa,处理时间为2.7h,完成密闭处理。
6.制备坯体
将密闭处理后的造粒料在132℃、52MPa条件下进行注射成型,注射完毕后,冷却得到素坯, 将素坯置于真空炉中进行脱脂,控制真空度为105Pa,脱脂时间为2.5h,脱脂温度为354℃,制得坯体。
7.烧结
(1)预烧结
将坯体置于真空炉中通入氮气进行预烧结,控制预烧结的真空度为0.05MPa,烧结温度为1150℃,烧结时间为2.0h,然后以1.2℃/min速率将温度降低至8.4℃,完成预烧结步骤,制得预烧结坯体;
(2)二次烧结
将预烧结坯体置于真空炉中进行二次烧结,控制真空度为为0.05MPa,先是在790℃下烧结2.3h,然后以1.7℃/min速率升温至1680℃,在1680℃下烧结1.1h,再以3.3℃/min速率降温至830℃,在830℃下烧结1.5h,自然冷却至室温后制得碳化硼陶瓷。
对比例1
在实施例1的基础上,改变之处为,在制备混合料步骤中,省略球磨处理步骤,直接将碳化硼粉、氧化铝、金属铝、二氧化钛、石墨粉混合均匀得到混合料,其余操作均相同。
对比例2
在实施例1的基础上,改变之处为,省略对混合料的改性步骤,其余操作均相同。
对比例3
在实施例1的基础上,改变之处为,在制备浆料步骤中,省略“球磨结束后以1℃/min速率将温度降低至1.2℃,置于1.2℃下静置1.3h,静置结束后自然恢复至室温”步骤,并且省略密闭处理步骤,其余操作均相同。
性能检测实验
1.按照GB/T 25995-2010测试标准检测实施例1-3与对比例1-3的密度、致密度,结果如下:
2.分别按照GB/T 16534-2009、GB/T 6569-2006、GB/T 23806-2009测试标准检测实施例1-3与对比例1-3的硬度、抗弯强度与断裂韧性,结果如下:
3.将实施例1-3与对比例1-3的产品分别置于温度为1350℃中氧化7d,再次分别按照GB/T 16534-2009、GB/T 6569-2006、GB/T23806-2009测试标准检测产品的硬度、抗弯强度与断裂韧性,结果如下:
4.防弹测试
测试方法:将实施例1-3与对比例1-3制得的产品应用在防弹头盔上,防弹头盔一般是用迎弹面即防弹陶瓷与超高分子量的聚乙烯材料组成,防弹陶瓷为实施例1-3与对比例1-3制得的碳化硼陶瓷;
分别在实施例1-3与对比例1-3的防弹头盔上取三点进行实弹打靶测试,打靶距离均为15米,弹速为弹头出枪口时速度,测试防弹效果,具体结果如下:
除非另有说明,本发明中所采用的百分数均为质量百分数。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种碳化硼陶瓷的制备方法,其特征在于,所述碳化硼陶瓷的制备方法,包括制备混合料、制备改性混合料、制备浆料、造粒、密闭处理、制备坯体、烧结步骤;
所述制备混合料的步骤为,将碳化硼粉、氧化铝、金属铝、单质硅、二氧化钛、石墨粉混合,进行第一次球磨处理,控制球料比为6-10:1,转速为660-680rpm,球磨时间为2.3-2.5h,球磨温度为65-67℃,第一次球磨结束后得到初混料,然后向初混料中加入木鱼石粉、海藻酸钠进行第二次球磨处理,控制球料比为10-14:1,转速为730-750rpm,球磨时间为2.0-2.2h,球磨温度为50-54℃,第二次球磨结束后得到混合料;
所述碳化硼粉、氧化铝、金属铝、单质硅、二氧化钛与石墨粉的质量比为80-85:4.8-5.2:3.8-4.2:2.6-3.3:1.7-2.4:3.9-4.2;
所述初混料与木鱼石粉、海藻酸钠的质量比为100-120:1-2.5:4-6;
所述制备改性混合料,包括初步改性和深度改性;
所述初步改性步骤为,将混合料进行超声-低温等离子体处理,结束后制得初步改性混合料;
所述深度改性步骤为,将初步改性混合料与改性剂混合,然后置于均质机中进行两次均质处理,控制第一次均质时间为10-14min,均质温度为38-42℃,均质压力为28-33MPa,第一次均质处理结束后第二次均质处理,控制第二次均质时间为7-9min,均质温度为43-47℃,均质压力为24-26MPa,第二次均质结束后,干燥,完成深度改性步骤,制得改性混合料;
所述初步改性混合料与改性剂的质量比为1:4.5-5.6;
所述改性剂的制备步骤为,将乙醇、棕榈酸、β-二酮、季戊四醇、羧甲基纤维素钠、硬脂酸钙混合,搅拌均匀后,置于1.8-2.3℃下静置1.3-1.7h,静置结束,自然恢复至室温后制得改性剂;
所述乙醇、棕榈酸、β-二酮、季戊四醇、羧甲基纤维素钠、硬脂酸钙的质量比为38-46:1.2-1.5:1.5-1.7:3.5-4.6:2.7-3.2:2.6-3.4;
所述制备浆料步骤为,将改性混合料与胡麻胶、酚醛树脂、海藻酸钠、氧化锌、轻钙粉混合,然后加入去离子水,进行球磨处理,球磨结束后以0.8-1.2℃/min速率将温度降低至1.0-1.5℃,置于1.0-1.5℃下静置1.2-1.4h,静置结束后自然恢复至室温,制得浆料;
所述改性混合料、去离子水、胡麻胶、酚醛树脂、海藻酸钠、氧化锌与轻钙粉的质量比为36-40:100-120:1.2-1.4:2.4-2.6:2.7-3.2:1.8-2.1:1.0-1.4;
所述密闭处理步骤为,将造粒粉置于真空手套箱中,控制温度为78-82℃,通入氩气,保持压力为0.08-0.12MPa,处理时间为2.7-3.2h,完成密闭处理。
2.根据权利要求1所述的一种碳化硼陶瓷的制备方法,其特征在于,
所述金属铝的粒径为70-80μm,所述单质硅的粒径为60-65μm;
所述碳化硼粉中B4C>99wt%,碳化硼粉的粒径为12-14μm;
所述石墨粉的粒径为78-82μm。
3.根据权利要求1所述的一种碳化硼陶瓷的制备方法,其特征在于,
所述初步改性步骤中,所述超声-低温等离子体处理, 超声波的频率为56-58kHz,声能密度为0.6-0.8W/mL,超声时间为13-18min;处理气氛为氮气和氧气的混合气体,氮气和氧气的体积比为1.5-1.8:1,处理压力为58-62Pa,放电功率为115-125W,处理时间为7-9min。
4.根据权利要求1所述的一种碳化硼陶瓷的制备方法,其特征在于,
所述制备浆料步骤中,所述球磨处理,球料比为5-7:1,球磨转速为565-600rpm,球磨温度为43-47℃,球磨时间为1.2-1.6h;
所述轻钙粉的粒径为12-15μm。
5.根据权利要求1所述的一种碳化硼陶瓷的制备方法,其特征在于,
所述造粒步骤为,将浆料喷雾干燥进行造粒,控制喷雾干燥的进口温度为200-220℃,出口温度为95-105℃,控制造粒机的温度为135-140℃,制得造粒粉。
6.根据权利要求1所述的一种碳化硼陶瓷的制备方法,其特征在于,
所述制备坯体步骤为,将密闭处理后的造粒料在128-132℃、48-52MPa条件下进行注射成型,注射完毕后,冷却得到素坯,将素坯置于真空炉中进行脱脂,控制真空度为96-105Pa,脱脂时间为2.1-2.5h,脱脂温度为345-354℃,制得坯体。
7.根据权利要求1所述的一种碳化硼陶瓷的制备方法,其特征在于,
所述烧结步骤包括预烧结、二次烧结;
所述预烧结步骤为,将坯体置于真空炉中通入氮气进行预烧结,控制预烧结的真空度为0.03-0.05MPa,烧结温度为1080-1150℃,烧结时间为1.5-2.0h,然后以1.0-1.2℃/min速率将温度降低至7.5-8.4℃,完成预烧结步骤,制得预烧结坯体。
8.根据权利要求7所述的一种碳化硼陶瓷的制备方法,其特征在于,
所述二次烧结步骤为,将预烧结坯体置于真空炉中进行二次烧结,控制真空度为为0.03-0.05MPa,先是在770-790℃下烧结1.4-2.3h,然后以1.3-1.7℃/min速率升温至1650-1680℃,在1650-1680℃下烧结1.1-1.3h,再以2.8-3.3℃/min速率降温至810-830℃,在810-830℃下烧结1.5-1.8h,自然冷却至室温后制得碳化硼陶瓷。
9.碳化硼陶瓷在防弹头盔中的应用,其特征在于,使用权利要求1-8任一项制备方法制得的碳化硼陶瓷。
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CN113912399A (zh) * | 2021-12-15 | 2022-01-11 | 山东金鸿新材料股份有限公司 | 一种高密度无压烧结碳化硅陶瓷的制备方法 |
CN114538929A (zh) * | 2022-03-17 | 2022-05-27 | 南通三责精密陶瓷有限公司 | 一种高致密度碳化硼陶瓷的制备方法 |
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