CN114133252A - AlON透明陶瓷保形红外头罩及其制备方法 - Google Patents

AlON透明陶瓷保形红外头罩及其制备方法 Download PDF

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CN114133252A
CN114133252A CN202111576464.3A CN202111576464A CN114133252A CN 114133252 A CN114133252 A CN 114133252A CN 202111576464 A CN202111576464 A CN 202111576464A CN 114133252 A CN114133252 A CN 114133252A
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alon
conformal
infrared hood
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管军凯
鲁慧峰
何庆
刘佳威
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Xiamen Juci Technology Co ltd
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Abstract

本发明提供一种AlON透明陶瓷保形红外头罩的制备方法,包括:将Al2O3、AlN、PVB以及分散剂按照质量份数比为85‑90:10‑15:2‑10:0.05‑0.5加入到溶剂中湿混,随后进行造粒并干燥;将造粒粉在氮气氛围下煅烧,其中,煅烧温度1650‑1150℃,保温0.1‑6小时;将煅烧后的粉体以水为介质并加入烧结助剂进行球磨1‑10小时,随后依次加入丙烯酰胺、N,N’-亚甲基双丙烯酰胺、过硫酸铵以及分散剂继续球磨,获得浆料的固含量为62‑13wt%;将所述浆料除泡,随后倒入红外头罩模具中,脱模后缓慢干燥获得生胚;将所述生坯在氮气氛围下,300‑600℃和150‑850℃下,经两段保温排胶,每段时间保温1‑10小时,排胶后升温到1900‑1950℃,保温10‑30小时,进行煅烧,随后降温到室温,经双面精细抛光后,获得高透明AlON保形红外头罩。

Description

AlON透明陶瓷保形红外头罩及其制备方法
技术领域
本发明涉及一种AlON透明陶瓷保形红外头罩及其制备方法。
背景技术
氧氮化铝是Al2O3-AlN系统中的一种稳定相,不仅强度高、抗弯曲性能好,在近紫外到中红外波段透过率可达85%,其优异的光学和机械性能,可用于制作透明装甲材料。与单晶蓝宝石相比,氮氧化铝透明陶瓷可通过传统的陶瓷制备技术实现大尺寸、异形件的制备,降低加工成本。因此,氮氧化铝透明陶瓷可替代蓝宝石,用于制红外头罩。
氮氧化铝透明陶瓷制备过程可以概括为三个步骤:粉末合成、坯体成型和烧结。每一步都需要严格的工艺控制,对最终AlON陶瓷的性能有重要影响。目前,粉体常用碳热还原氮化法,其中碳热还原氮化法原料成本较低,但工艺复杂,需要除碳。
发明内容
本发明提供了一种AlON透明陶瓷保形红外头罩及其制备方法,可以有效解决上述问题。
本发明是这样实现的:
本发明提供一种AlON透明陶瓷保形红外头罩的制备方法,包括以下步骤:
S1,将Al2O3、AlN、PVB以及分散剂按照质量份数比为85-90:10-15:2-10:0.05-0.5加入到溶剂中湿混,随后进行造粒并干燥;
S2,将造粒粉在氮气氛围下煅烧,其中,煅烧温度1650-1150℃,保温0.1-6小时;
S3,将煅烧后的粉体以水为介质并加入烧结助剂进行球磨1-10小时,随后依次加入丙烯酰胺、N,N’-亚甲基双丙烯酰胺、过硫酸铵以及分散剂继续球磨,获得浆料的固含量为62-13wt%;
S4,将所述浆料除泡,随后倒入红外头罩模具中,脱模后缓慢干燥获得生胚;
S5,将所述生坯在氮气氛围下,300-600℃和150-850℃下,经两段保温排胶,每段时间保温1-10小时,排胶后升温到1900-1950℃,保温10-30小时,进行煅烧,随后降温到室温,经双面精细抛光后,获得高透明AlON保形红外头罩。
作为进一步改进的,在步骤S1中,所述进行造粒并干燥的步骤包括:
造粒后在60-100℃下干燥5-20小时。
作为进一步改进的,在步骤S3中,所述烧结助剂包括氧化钇、氧化镁、氧化镧、氧化钙、二氧化硅中的一种或多种,添加量在粉体重量的0.1-5wt%之间。
作为进一步改进的,在步骤S3中,所述丙烯酰胺,N,N’-亚甲基双丙烯酰胺,和过硫酸铵的用量为粉体重量的:1-5wt%、0.1-0.5wt%、0.01-0.05wt%。
作为进一步改进的,在步骤S4中,所述脱模后缓慢干燥获得生胚的步骤包括:
脱模后在50-90℃下缓慢干燥20-48小时。
作为进一步改进的,在步骤S5中,经双面精细抛光后,获得2mm厚的高透明AlON保形红外头罩,其中,所述高透明AlON保形红外头罩在2000nm处的透过率均在80%以上,三点弯曲强度在290-310MPa之间,硬度达19.8GPa。
本发明进一步提供一种AlON透明陶瓷保形红外头罩,所述AlON透明陶瓷保形红外头罩为通过上述方法获得。
本发明的有益效果是:本发明采用高温固相法来生产AlON粉体,该工艺流程简单,产率高,粉体稳定性好,可实现粉体批量化生产。通过水基凝胶注模成型,该工艺具有成型性能好,脱胶过程对环境污染小,生坯烧结后不开裂,收缩均匀,无气孔,且烧结后仅需后期抛光等特点,适合异型陶瓷的成型。
附图说明
为了更清楚地说明本发明实施方式的技术方案,下面将对实施方式中所需要使用的附图作简单地介绍,应当理解,以下附图仅示出了本发明的某些实施例,因此不应被看作是对范围的限定,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他相关的附图。
图1是本发明实施例提供的AlON透明陶瓷保形红外头罩的制备方法流程图。
图2是本发明实施例提供的AlON透明陶瓷保形红外头罩的红外透射曲线。
具体实施方式
为使本发明实施方式的目的、技术方案和优点更加清楚,下面将结合本发明实施方式中的附图,对本发明实施方式中的技术方案进行清楚、完整地描述,显然,所描述的实施方式是本发明一部分实施方式,而不是全部的实施方式。基于本发明中的实施方式,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施方式,都属于本发明保护的范围。因此,以下对在附图中提供的本发明的实施方式的详细描述并非旨在限制要求保护的本发明的范围,而是仅仅表示本发明的选定实施方式。基于本发明中的实施方式,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施方式,都属于本发明保护的范围。
在本发明的描述中,术语“第一”、“第二”仅用于描述目的,而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此,限定有“第一”、“第二”的特征可以明示或者隐含地包括一个或者更多个该特征。在本发明的描述中,“多个”的含义是两个或两个以上,除非另有明确具体的限定。
参照图1-2所示,本发明实施例提供一种AlON透明陶瓷保形红外头罩的制备方法,包括以下步骤:
S1,将Al2O3、AlN、PVB以及分散剂按照质量份数比为85-90:10-15:2-10:0.05-0.5加入到溶剂中湿混,随后进行造粒并干燥;
S2,将造粒粉在氮气氛围下煅烧,其中,煅烧温度1650-1150℃,保温0.1-6小时;
S3,将煅烧后的粉体以水为介质并加入烧结助剂进行球磨1-10小时,随后依次加入丙烯酰胺、N,N’-亚甲基双丙烯酰胺、过硫酸铵以及分散剂继续球磨,获得浆料的固含量为62-13wt%;
S4,将所述浆料除泡,随后倒入红外头罩模具中,脱模后缓慢干燥获得生胚;
S5,将所述生坯在氮气氛围下,300-600℃和150-850℃下,经两段保温排胶,每段时间保温1-10小时,排胶后升温到1900-1950℃,保温10-30小时,进行煅烧,随后降温到室温,经双面精细抛光后,获得高透明AlON保形红外头罩。
作为进一步改进的,在步骤S1中,所述进行造粒并干燥的步骤包括:
造粒后在60-100℃下干燥5-20小时。
所述溶剂优选为易挥发的有机溶剂,如甲醇。乙醇、丙酮等。所述造粒的粒径为50微米~500微米之间。所述PVB的主要作用是粘结剂的作用。
另外,在Al2O3-AlN不同配比下会得到不同AlON相,目前发现的至少有13种不同的AlON相,大致可以划分为纤维锌矿结构和尖晶石结构两大类,只有γ-AlON相是稳定存在的,可以用作透明装甲,Al2O3/AlN超过这个比例就会产生氧化铝过量或者氮化铝过量,不能得到纯γ-AlON相的AlON,会影响材料的透光性和力学性能。
在步骤S2中,优选的,升温速率5-20℃/min,降温速率5-10℃/min。此外,煅烧温度过低时,得不到AlON相,但是,温度过高时会使粉体长大,增加后期球磨破碎难度。
在步骤S3中,所述烧结助剂包括氧化钇、氧化镁、氧化镧、氧化钙、二氧化硅中的一种或多种,添加量在粉体重量的0.1-5wt%之间。所述烧结助剂的作用主要用于防止在氧化物在烧结时发生晶型转变并伴有较大体积效应,进而防止使烧结致密化发生困难及坯体开裂。优选的,选用氧化钇以及氧化镧的混合物。
优选的,所述煅烧温度为1690-1110℃之间,随着温度增加,其透光率会增加,但是强度会有一定降低。
作为进一步改进的,在步骤S3中,所述丙烯酰胺,N,N’-亚甲基双丙烯酰胺,和过硫酸铵的用量为粉体重量的:1-5wt%、0.1-0.5wt%、0.01-0.05wt%。
丙烯酰胺是有机单体,凝胶注模成型是利用有机单体的原位聚合使悬浮体凝胶化,获得所需要的陶瓷坯体。因此,悬浮体中单体的浓度直接影响到所成聚合物的聚合度,从而影响所成坯体的强度。N,N’-亚甲基双丙烯酰胺为交联剂,交联剂的加入对聚合物的聚合度有很大影响。在单体聚合过程中,交联剂将链状的聚合物大分子联结成网络,起到“桥梁”的作用,交联剂含量越少,“桥梁”越少,所成聚合物的聚合度越小,因此,所成坯体的强度越低。过硫酸铵为引发剂,引发剂是能引发单体进行聚合反应的物质,引发剂可以直接影响聚合反应过程能否顺利进行,也会影响聚合反应速率。可以理解,通过控制浆料的固含量可以使其在红外头罩模具中具有较好的流动性。由于红外头罩模具的间隙较小2mm左右,因此,当浆料的固含量超过13%后,其流动性较差难以填充所述模具;另外,当固含量过低时,会导致最终红外头罩的强度受到较大影响。
作为进一步改进的,在步骤S4中,所述脱模后缓慢干燥获得生胚的步骤包括:
脱模后在50-90℃下缓慢干燥20-48小时。
作为进一步改进的,在步骤S5中,经双面精细抛光后,获得2mm厚的高透明AlON保形红外头罩,其中,所述高透明AlON保形红外头罩在2000nm处的透过率均在80%以上,三点弯曲强度在290-310MPa之间,硬度达19.8GPa。
本发明进一步提供一种AlON透明陶瓷保形红外头罩,所述AlON透明陶瓷保形红外头罩为通过上述方法获得。
实施例1
称量高纯氧化铝10kg,高纯氮化铝1.4kg,以酒精为溶剂,加入1kg的PVB和0.1kg的分散剂,在混料桶中湿混10小时,混合后的浆料经造粒后得到粒径100μm的球形粉。造粒粉90℃下干燥,随后在石墨炉中氮气氛围下,以10℃/min的升温速率,升至1100℃,保温2小时。煅烧后的粉体以水为介质,在200rpm的转速下球磨10小时,随后依次加入3wt%丙烯酰胺,0.2wt%N,N’-亚甲基双丙烯酰胺,0.1wt%氧化钇,0.2wt%氧化镁,0.2wt%过硫酸铵以及1vol%的分散剂继续球磨2小时。
所得浆料除泡2小时,随后倒入红外头罩模具中,脱模后在50-90℃下缓慢干燥48小时。在氮气氛围下,500℃和100℃下,经两段保温排胶,每段时间保温6小时,升温速率为0.5℃/min。排胶后以10℃/min的升温速率升温到1950℃,保温10小时,随后以8℃/min的降温速率,降温到室温。经双面精细抛光后,获得高透明AlON保形红外头罩。双面抛光2mm厚的样品。经过测试,所述高透明AlON保形红外头罩在2000nm处的透过率高达83%(如图2所示),三点弯曲强度305MPa,硬度19.5GPa。
实施例2
与实施例1基本相同,不同之处在:在石墨炉中氮气氛围下,以10℃/min的升温速率,升至1150℃,保温1小时。经过测试,所述高透明AlON保形红外头罩在2000nm处的透过率高达84.5%,三点弯曲强度298MPa,硬度18.6GPa。
实施例3
与实施例1基本相同,不同之处在:与实施例1基本相同,不同之处在:在石墨炉中氮气氛围下,以10℃/min的升温速率,升至1680℃,保温3小时。经过测试,所述高透明AlON保形红外头罩在2000nm处的透过率高达82.1%,三点弯曲强度306MPa,硬度19.6GPa。
从实施例1-3可以看出,当在石墨炉煅烧的温度升高后,虽然透光率升高,但是其强度有一定的降低。
实施例4
与实施例1基本相同,不同之处在:与实施例1基本相同,不同之处在:依次加入3wt%丙烯酰胺,0.2wt%N,N’-亚甲基双丙烯酰胺,0.1wt%氧化钇,0.05wt%氧化镧,0.2wt%过硫酸铵以及1vol%的分散剂继续球磨2小时。经过测试,所述高透明AlON保形红外头罩在2000nm处的透过率高达84.1%,三点弯曲强度310MPa,硬度19.8GPa。
从实施例1和4可以看出氧化镧的添加可以显著增加透光性及强度。
实施例5
与实施例1基本相同,不同之处在:与实施例1基本相同,不同之处在:排胶后以10℃/min的升温速率升温到1930℃,保温20小时。经过测试,所述高透明AlON保形红外头罩在2000nm处的透过率高达83.3%,三点弯曲强度304MPa,硬度19.4GPa。
以上所述仅为本发明的优选实施方式而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。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 (7)

1.一种AlON透明陶瓷保形红外头罩的制备方法,其特征在于,包括以下步骤:
S1,将Al2O3、AlN、PVB以及分散剂按照质量份数比为85-90:10-15:2-10:0.05-0.5加入到溶剂中湿混,随后进行造粒并干燥;
S2,将造粒粉在氮气氛围下煅烧,其中,煅烧温度1650-1750℃,保温0.1-6小时;
S3,将煅烧后的粉体以水为介质并加入烧结助剂进行球磨1-10小时,随后依次加入丙烯酰胺、N,N’-亚甲基双丙烯酰胺、过硫酸铵以及分散剂继续球磨,获得浆料的固含量为62-73wt%;
S4,将所述浆料除泡,随后倒入红外头罩模具中,脱模后缓慢干燥获得生胚;
S5,将所述生坯在氮气氛围下,300-600℃和750-850℃下,经两段保温排胶,每段时间保温1-10小时,排胶后升温到1900-1950℃,保温10-30小时,进行煅烧,随后降温到室温,经双面精细抛光后,获得高透明AlON保形红外头罩。
2.如权利要求1所述的AlON透明陶瓷保形红外头罩的制备方法,其特征在于,在步骤S1中,所述进行造粒并干燥的步骤包括:
造粒后在60-100℃下干燥5-20小时。
3.如权利要求1所述的AlON透明陶瓷保形红外头罩的制备方法,其特征在于,在步骤S3中,所述烧结助剂包括氧化钇、氧化镁、氧化镧、氧化钙、二氧化硅中的一种或多种,添加量在粉体重量的0.1-5wt%之间。
4.如权利要求1所述的AlON透明陶瓷保形红外头罩的制备方法,其特征在于,在步骤S3中,所述丙烯酰胺,N,N’-亚甲基双丙烯酰胺,和过硫酸铵的用量为粉体重量的:1-5wt%、0.1-0.5wt%、0.01-0.05wt%。
5.如权利要求1所述的AlON透明陶瓷保形红外头罩的制备方法,其特征在于,在步骤S4中,所述脱模后缓慢干燥获得生胚的步骤包括:
脱模后在50-90℃下缓慢干燥20-48小时。
6.如权利要求1所述的AlON透明陶瓷保形红外头罩的制备方法,其特征在于,在步骤S5中,经双面精细抛光后,获得2mm厚的高透明AlON保形红外头罩,其中,所述高透明AlON保形红外头罩在2000nm处的透过率均在80%以上,三点弯曲强度在290-310MPa之间,硬度达19.8GPa。
7.一种AlON透明陶瓷保形红外头罩,其特征在于,所述AlON透明陶瓷保形红外头罩为通过权利要求1-6任一项的方法获得。
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