CN111620685B - 一种利用镁铝尖晶石透明陶瓷的防弹聚氨酯复合镜片 - Google Patents
一种利用镁铝尖晶石透明陶瓷的防弹聚氨酯复合镜片 Download PDFInfo
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Abstract
本发明涉及一种利用镁铝尖晶石透明陶瓷的防弹聚氨酯复合镜片的制造方法,(1)将氧化镁粉体和α‑氧化铝粉体三种原料混合均匀得到原料粉体;(2)将步骤(1)制备的原料粉体放到特定模具中,得到素坯;(3)将步骤(2)制备的素坯先经素烧、无压预烧和热等静压烧结后,得到镁铝尖晶石透明陶瓷件A和B;(4)将步骤(3)制备的镁铝尖晶石透明陶瓷件A和B和胶带加工成中空的模具件;(5)在步骤(4)制备的中空的模具件间注入聚氨酯树脂,然后进行固化和镀膜;(6)镀膜后,得到最终产品镜片。本申请通过重量为16G+0.1G,直径为16mm的钢珠在氮气20KG时发射速度为220米/秒的强力冲击下,镜片不破裂,镜片具有防弹功能的要求。
Description
技术领域
本发明涉及镜片技术领域,具体的说,是一种利用镁铝尖晶石透明陶瓷的防弹聚氨酯复合镜片。
背景技术
防弹玻璃一般是由坚韧的塑料内层(pc/PVB)将两片玻璃在一定温度和压力下粘贴而成,夹层pc厚度一般为0.5mm-5mm.也称为夹层玻璃或胶合玻璃,其塑料内层可以吸收冲击和爆炸过程中所产生的部分能量和冲击波压力,即使被震碎也不会四散飞溅。夹层玻璃根据不同的需要可用普通玻璃、钢化玻璃、热增强玻璃来制成,也可制成中空玻璃。安全玻璃具有良好的安全性,抗冲击性和抗穿透性,具有防盗、防弹、防爆功能。为了达到防弹的效果,防弹玻璃的厚度一般需要达到10mm以上的厚度。
研究发现镁铝尖晶石透明陶瓷具有良好的光学性能、高的力学强度以及稳定的物理化学性能广泛应用于透明装甲、智能显示设备视窗、红外光学窗口/导引头整流罩头罩、紫外光刻机透镜、高温窗口等军、民用领域。1961年,美国通用电气公司首次发现镁铝尖晶石陶瓷的透明性,采用固相反应法合成镁铝尖晶石粉体,以Li2O和SiO2为烧结助剂,用真空烧结或氢气气氛烧结首次制备出半透明的镁铝尖晶石陶瓷,随后世界多国的研究人员对镁铝尖晶石透明陶瓷的制备、及其致密化机理方面进行了大量研究。Krell等人使用粒径53nm的特殊MgAl2O4粉体,采用350MPa冷等静压成型,在无压条件下1240-1260℃烧结,在低于1300℃下热等静压制得平均晶粒尺寸0.2-0.3μm的镁铝尖晶石透明陶瓷(Krell A,HutzlerT,Klimke J,et al.,Fine-Grained Transparent Spinel Windows by the Processingof Different Nanopowders[J].Journal of the American Ceramic Society,2010,93(9):2656-2666.),样品厚度4-10mm的情况下可见光区域透过率达到80%,该方法对原料粉体粒径要求高,成本高昂。
中国专利申请号CN200610022318.5,镁铝尖晶石纳米透明陶瓷的制备方法,以纯度>99%的镁铝尖晶石纳米粉体为原料,工艺步骤包括粉体成型和高压烧结。粉体成型是将纯度大于99%的镁铝尖晶石纳米粉体装入模具中,在常温、5~20MPa压力下成型为素坯;高压烧结是将素坯放入两面顶压机中,在2~5GPa压力下烧结,烧结温度为500~700℃,烧结时间至少为20分钟,即制得镁铝尖晶石纳米透明陶瓷。
中国专利申请号CN200610022482.6,一种增韧镁铝尖晶石透明陶瓷的制备方法,以化学纯MgSO4、NH4Al(SO4)2为原料,工艺步骤:(1)粉体制备与造粒,采用熔盐焙烧法制备镁铝尖晶石纳米粉体,将所制得的纳米粉体加粘结剂球磨24~48小时,然后造粒,形成40~100μm的微粒;(2)成型,将镁铝尖晶石微粒装入模具中初压成型,然后再冷等静压得到致密化素坯;(3)烧结,将素坯进行真空烧结后再放入热等静压炉中烧结。其制备的镁铝尖晶石透明陶瓷通式为MgO·nAl2O3,其中1.3≤n≤1.6,在可见波段透过率达到80%以上,n=1.3时,断裂韧性为2.7MPa·m1/2,n=1.5时,断裂韧性为3.2MPa·m1/2。
但是,镁铝尖晶石透明陶瓷的脆性已经严重地限制了它在更多领域的应用。如果采用镁铝尖晶石透明陶瓷直接加工成防弹眼镜的话,如果将镜片中心厚度加工在3mm以内,镜片会出现太脆和抗冲击力不达标问题。本发明提供一种具有防弹功能的镁铝尖晶石透明陶瓷复合聚氨酯镜片的制造方法,其特征在于:镁铝尖晶石透明陶瓷件是桶MgO粉体纯度≥99.95%、粒径为10~50nm;α-Al2O3粉体的纯度≥99.95%、粒径为10~50nm;烧结助剂氧化镧的纯度≥99.95%、粒径为50~100nm。将氧化镁粉体和α-氧化铝粉体按摩尔比1:3配比,氧化镧质量浓度为10~50ppm,三种原料混合均匀得到原料粉体;将所得原料粉体放到特定模具中,得到素坯;将所得素坯先经素烧、无压预烧和热等静压烧结后,得到特定弯度镁铝尖晶石透明陶瓷件。将A和B两片特定弯度镁铝尖晶石透明陶瓷件和胶带加工成中空的模具件,其中A片镁铝尖晶石透明陶瓷件作为镜片的前表面弯度;B片镁铝尖晶石透明陶瓷件作为镜片的后表面弯度。在中空的模具件间注入聚氨酯树脂,聚氨酯树脂由降冰片烷二异氰酸酯和四(3-巯基丙酸)季戊四醇酯以及含质量比为1.5%的二丁基二氯化锡;随后将注入聚氨酯树脂的模具件放入烘箱,按照特定的固化程序进行固化。固化后的模具组件既是防弹镜片的毛坯,将该镜片清洗烘干后,进行真空镀膜,使得防弹镜片的反射率达到1%,就可以得到具有防弹功能的镁铝尖晶石透明陶瓷和聚氨酯复合镜片。通过本发明提供一种具有防弹功能的镁铝尖晶石透明陶瓷和聚氨酯复合镜片中心厚度达到3.00mm可以通过重量为16G+0.1G,直径为16mm的钢珠在氮气20KG时发射速度为220米/秒的强力冲击下,镜片不破裂,镜片具有防弹功能的要求。
发明内容
本发明的目的在于克服现有技术的不足,提供一种利用镁铝尖晶石透明陶瓷的防弹聚氨酯复合镜片。
本发明的目的是通过以下技术方案来实现的:
一种利用镁铝尖晶石透明陶瓷的防弹聚氨酯复合镜片的制造方法,其具体步骤为:
(1)将氧化镁粉体和α-氧化铝粉体按摩尔比1:3配比,氧化镧相对于氧化镁粉体和α-氧化铝粉体的混合物的质量浓度为10~50ppm,三种原料混合均匀得到原料粉体;
镁铝尖晶石透明陶瓷件是通过MgO粉体纯度≥99.95%、粒径为10~50nm;α-Al2O3粉体的纯度≥99.95%、粒径为10~50nm;烧结助剂氧化镧的纯度≥99.95%、粒径为10~50nm。
(2)将步骤(1)制备的原料粉体放到特定模具中,得到素坯;
(3)将步骤(2)制备的素坯先经素烧、无压预烧和热等静压烧结后,得到镁铝尖晶石透明陶瓷件A和镁铝尖晶石透明陶瓷件B;
镁铝尖晶石透明陶瓷件A和镁铝尖晶石透明陶瓷件B的弯度的曲率半径范围是50~2000mm,其直径大小范围是300~900mm。
镁铝尖晶石透明陶瓷件A和镁铝尖晶石透明陶瓷件B的弯度的曲率半径范围是500~1000mm,其直径大小范围是500~800mm。
(4)将步骤(3)制备的镁铝尖晶石透明陶瓷件A和镁铝尖晶石透明陶瓷件B和胶带加工成中空的模具件,其中镁铝尖晶石透明陶瓷件A作为镜片的前表面弯度;镁铝尖晶石透明陶瓷件B作为镜片的后表面弯度;
镜片的中心厚度范围在0.1~6.0毫米,镜片面弯的曲率半径范围是50~2000mm。
优选的,镜片的中心厚度范围在0.1~3.0毫米,镜片面弯的曲率半径范围是500~1000mm。
(5)在步骤(4)制备的中空的模具件间注入聚氨酯树脂,聚氨酯树脂由降冰片烷二异氰酸酯和四(3-巯基丙酸)季戊四醇酯以及二丁基二氯化锡;降冰片烷二异氰酸酯和四(3-巯基丙酸)季戊四醇酯的摩尔比1:1~1.1:1,二丁基二氯化锡在降冰片烷二异氰酸酯和四(3-巯基丙酸)季戊四醇酯二者混合物中的质量分数为1.5%,随后将注入聚氨酯树脂的模具件放入烘箱,按照特定的固化程序进行固化;固化程序为:
室温-20℃ 0.5h~3h
20℃~40℃ 8h~12h
40℃~50℃ 2h~5h
50℃~70℃ 3h~4h
70℃~95℃ 3h~5h
95℃~120℃ 1h~3h
120℃~120℃ 2h~3h
120℃~80℃ 1h~2h
80℃~80℃ 保温
优选的固化程序为:
室温-20℃ 2h
20℃~40℃ 9h
40℃~50℃ 3h
50℃~70℃ 3h
70℃~95℃ 4h
95℃~120℃ 2h
120℃~120℃ 2h
120℃~80℃ 2h
80℃~80℃ 保温
在80℃时,拆除胶带,进行边缘美化和清洗;随后将清洗后镜片进行二次固化,二次固化的温度为100℃,2~4小时;二次固化后镜片在降低到室温以后,进行镜片的表面镀膜处理;
镀膜采用的材料是为氧化硅、氧化锆、三氧化二铝、氧化铟锡和氟化物;氟化物在膜层的最外面一层,采用电子枪和主蒸两种方式中一种进行镀膜;优选的,化物在膜层的最外面一层,采用主蒸方式进行镀膜;
(6)镀膜后,防弹镜片的反射率小于等于的1%,得到具有防弹功能的镁铝尖晶石透明陶瓷和聚氨酯复合镜片。
与现有技术相比,本发明的积极效果是:
相对于现有技术,本申请通过镁铝尖晶石透明陶瓷和聚氨酯复合镜片在中心厚度达到3.00mm的情况下可以通过重量为16G+0.1G,直径为16mm的钢珠在氮气20KG时发射速度为220米/秒的强力冲击下,镜片不破裂,镜片具有防弹功能的要求。
本申请通过镁铝尖晶石透明陶瓷和聚氨酯复合技术解决了现有技术中的镁铝尖晶石透明陶瓷的脆性问题。
具体实施方式
以下提供本发明一种利用镁铝尖晶石透明陶瓷的防弹聚氨酯复合镜片的具体实施方式。
实施例1
镁铝尖晶石透明陶瓷件是通过40千克MgO粉体,其中纯度=99.98%、粒径为30~50nm;306千克α-Al2O3粉体,其中纯度=99.96%、粒径为30~50nm;3克氧化镧,其中纯度=99.95%、粒径为30~50nm。三种原料混合均匀得到原料粉体。将所得原料粉体放到特定模具中,得到素坯。将所得素坯先经素烧、无压预烧和热等静压烧结后,得到特定弯度镁铝尖晶石透明陶瓷件A和B。将A和B两片特定弯度镁铝尖晶石透明陶瓷件和胶带加工成中空的模具件,其中A片镁铝尖晶石透明陶瓷件作为镜片的前表面弯度;B片镁铝尖晶石透明陶瓷件作为镜片的后表面弯度。镁铝尖晶石透明陶瓷件A和B弯度的曲率半径范围是1000mm,其直径大小范围是700mm。镜片的中心厚度范围在3.0毫米,镜片面弯的曲率半径范围是1000mm。在中空的模具件间注入聚氨酯树脂,聚氨酯树脂由降冰片烷二异氰酸酯和四(3-巯基丙酸)季戊四醇酯以及含质量比为1.5%的二丁基二氯化锡;随后将注入聚氨酯树脂的模具件放入烘箱,按照特定的固化程序进行固化。固化程序为
室温-20℃ 2h
20℃~40℃ 9h
40℃~50℃ 3h
50℃~70℃ 3h
70℃~95℃ 4h
95℃~120℃ 2h
120℃~120℃2h
120℃~80℃ 2h
80℃~80℃ 保温
在80℃时,拆除胶带,进行边缘美化和清洗;随后将清洗后镜片进行二次固化,二次固化的温度为100℃,2小时;二次固化后镜片在降低到室温以后,进行镜片的表面镀膜处理。镀膜采用的材料是为氧化硅、氧化锆、三氧化二铝、氧化铟锡和氟化物。氟化物在膜层的最外面一层,采用主蒸方式进行镀膜。镀膜后,防弹镜片的反射率等于的0.6%,就可以得到利用镁铝尖晶石透明陶瓷的防弹聚氨酯复合镜片。本申请的镜片通过镁铝尖晶石透明陶瓷和聚氨酯复合镜片在中心厚度达到3.00mm的情况下可以通过重量为16G+0.1G,直径为16mm的钢珠在氮气20KG时发射速度为220米/秒的强力冲击下,镜片不破裂,镜片具有防弹功能的要求。
实施例2
镁铝尖晶石透明陶瓷件是通过40千克MgO粉体,其中纯度=99.98%、粒径为10~30nm;306千克α-Al2O3粉体,其中纯度=99.96%、粒径为10~30;3克氧化镧,其中纯度=99.95%、粒径为10~30nm。三种原料混合均匀得到原料粉体。将所得原料粉体放到特定模具中,得到素坯。将所得素坯先经素烧、无压预烧和热等静压烧结后,得到特定弯度镁铝尖晶石透明陶瓷件A和B。将A和B两片特定弯度镁铝尖晶石透明陶瓷件和胶带加工成中空的模具件,其中A片镁铝尖晶石透明陶瓷件作为镜片的前表面弯度;B片镁铝尖晶石透明陶瓷件作为镜片的后表面弯度。镁铝尖晶石透明陶瓷件A和B弯度的曲率半径范围是500mm,其直径大小范围是700mm。镜片的中心厚度范围在3.0毫米,镜片面弯的曲率半径范围是500mm。在中空的模具件间注入聚氨酯树脂,聚氨酯树脂由降冰片烷二异氰酸酯和四(3-巯基丙酸)季戊四醇酯以及含质量比为1.5%的二丁基二氯化锡;随后将注入聚氨酯树脂的模具件放入烘箱,按照特定的固化程序进行固化。固化程序为
室温-20℃ 2h
20℃~40℃ 12h
40℃~50℃ 3h
50℃~70℃ 3h
70℃~95℃ 4h
95℃~120℃ 2h
120℃~120℃2h
120℃~80℃ 3h
80℃~80℃ 保温
在80℃时,拆除胶带,进行边缘美化和清洗;随后将清洗后镜片进行二次固化,二次固化的温度为100℃,2小时;二次固化后镜片在降低到室温以后,进行镜片的表面镀膜处理。镀膜采用的材料是为氧化硅、氧化锆、三氧化二铝、氧化铟锡和氟化物。氟化物在膜层的最外面一层,采用主蒸方式进行镀膜。镀膜后,防弹镜片的反射率等于的0.6%,就可以得到利用镁铝尖晶石透明陶瓷的防弹聚氨酯复合镜片。本申请的镜片通过镁铝尖晶石透明陶瓷和聚氨酯复合镜片在中心厚度达到3.00mm的情况下可以通过重量为16G+0.1G,直径为16mm的钢珠在氮气20KG时发射速度为220米/秒的强力冲击下,镜片不破裂,镜片具有防弹功能的要求。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员,在不脱离本发明构思的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围内。
Claims (4)
1.一种利用镁铝尖晶石透明陶瓷的防弹聚氨酯复合镜片的制造方法,其特征在于,其具体步骤为:
(1)将氧化镁粉体和α-氧化铝粉体按摩尔比1:3配比,氧化镧相对于氧化镁粉体和α-氧化铝粉体的混合物的质量浓度为10~50ppm,三种原料混合均匀得到原料粉体;
(2)将步骤(1)制备的原料粉体放到特定模具中,得到素坯;
(3)将步骤(2)制备的素坯先经素烧、无压预烧和热等静压烧结后,得到镁铝尖晶石透明陶瓷件A和镁铝尖晶石透明陶瓷件B;
(4)将步骤(3)制备的镁铝尖晶石透明陶瓷件A和镁铝尖晶石透明陶瓷件B和胶带加工成中空的模具件,其中镁铝尖晶石透明陶瓷件A作为镜片的前表面弯度;镁铝尖晶石透明陶瓷件B作为镜片的后表面弯度;
(5)在步骤(4)制备的中空的模具件间注入聚氨酯树脂,聚氨酯树脂由降冰片烷二异氰酸酯和四(3-巯基丙酸)季戊四醇酯以及二丁基二氯化锡;降冰片烷二异氰酸酯和四(3-巯基丙酸)季戊四醇酯的摩尔比1:1~1.1:1,二丁基二氯化锡在降冰片烷二异氰酸酯和四(3-巯基丙酸)季戊四醇酯二者混合物中的质量分数为1.5%,随后将注入聚氨酯树脂的模具件放入烘箱,然后进行固化;
在80℃时,拆除胶带,进行边缘美化和清洗;随后将清洗后镜片进行二次固化,二次固化的温度为100℃,2~4小时;二次固化后镜片在降低到室温以后,进行镜片的表面镀膜处理;
(6)镀膜后,防弹镜片的反射率小于等于的1%,得到具有防弹功能的镁铝尖晶石透明陶瓷和聚氨酯复合镜片;
镁铝尖晶石透明陶瓷件是通过 MgO 粉体纯度≥99.95%、粒径为10~50nm;α-Al2O3粉体的纯度≥99.95%、粒径为10~50nm;烧结助剂氧化镧的纯度≥99.95%、粒径为10~50nm;
镁铝尖晶石透明陶瓷件A和镁铝尖晶石透明陶瓷件B的弯度的曲率半径范围是50~2000mm,其直径大小范围是300~900mm;
固化程序为:
室温-20℃ 0.5h~3h
20℃~40℃ 8h~12h
40℃~50℃ 2h~5h
50℃~70℃ 3h~4h
70℃~95℃ 3h~5h
95℃~120℃ 1h~3h
120℃~120℃ 2h~3h
120℃~80℃ 1h~2h
80℃~80℃ 保温
镜片的中心厚度范围在0.1~3.0毫米,镜片面弯的曲率半径范围是500~1000mm;
镀膜采用的材料是为氧化硅、氧化锆、三氧化二铝、氧化铟锡和氟化物;氟化物在膜层的最外面一层,采用电子枪和主蒸两种方式中一种进行镀膜。
2.如权利要求1所述的一种利用镁铝尖晶石透明陶瓷的防弹聚氨酯复合镜片的制造方法,其特征在于,镁铝尖晶石透明陶瓷件A和镁铝尖晶石透明陶瓷件B的弯度的曲率半径范围是500~1000mm,其直径大小范围是500~800mm。
3.如权利要求1所述的一种利用镁铝尖晶石透明陶瓷的防弹聚氨酯复合镜片的制造方法,其特征在于,镜片的中心厚度范围在0.1~6.0毫米,镜片面弯的曲率半径范围是50~2000mm。
4.如权利要求1所述的一种利用镁铝尖晶石透明陶瓷的防弹聚氨酯复合镜片的制造方法,其特征在于,氟化物在膜层的最外面一层,采用主蒸方式进行镀膜。
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