CN113582677A - 一种低温烧结瓷化粉及其制备方法 - Google Patents
一种低温烧结瓷化粉及其制备方法 Download PDFInfo
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Abstract
本发明提供了一种低温烧结瓷化粉及其制备方法,所述低温烧结瓷化粉由重量份如下的原料制成:无机填料Ⅰ5‑50份、无机填料Ⅱ10‑60份、助熔剂30‑60份、矿化剂2‑10份、增效剂1‑8份,低温烧结瓷化粉的制备方法简单,包括如下步骤:将无机填料Ⅰ、无机填料Ⅱ、助熔剂和增效剂干燥,再与矿化剂搅拌混合。本发明的低温烧结瓷化粉生产成本较低,可以实现中温段快速瓷化,能大幅度降烧结后陶瓷的开裂现象,瓷化形成完整致密的壳体。
Description
技术领域
本发明属于无机材料的加工与应用领域,尤其涉及一种低温烧结瓷化粉及其制备方法。
背景技术
传统电线电缆材料在发生火灾时会熔滴滴落,且伴随着聚合物降解会排放出有毒或有害气体,具有一定的局限性。近年来,一种新型的耐火材料——陶瓷化聚合物材料成为研究热点。陶瓷化聚合物材料是在聚合物基体中添加一定比例的成瓷填料和助熔剂制得的复合材料,其在常温下能够保持良好的弹性和力学性能,热稳定性好、耐老化、加工性能强、绝缘性能好,当遇到明火或处于高温环境时,这种复合材料能转变为具有自支撑性的陶瓷体,即可在火灾发生时形成陶瓷保护层覆盖在缆芯上,阻止火焰向材料内部蔓延,为人员撤离与抢险救灾赢得宝贵时间。
在聚合物基体中添加瓷化粉制备的陶瓷化聚合物耐火电缆材料,对电缆输电电压的提升和耐火性能的提高具有重要意义,瓷化粉作为一种能在500~1000℃实现快速成瓷的无机复合粉体,是制备陶瓷化聚合物耐火电缆材料的技术关键。瓷化粉的成瓷温度、成瓷性能以及在聚合物中的分散性等对陶瓷化聚合物耐火电缆材料的性能具有重大影响。
公开号为CN112174639A的中国专利文献中公开了一种陶瓷化高分子材料用低温烧结瓷化粉及其应用,该发明中,所述的陶瓷化高分子材料用低温烧结瓷化粉按以下质量配比混合得到:硅灰细粉10~50份、白云母细粉20~50份、硬脂酸0.8~1.6份、铝酸酯2~5份、叶蜡石细粉5~20份、低熔点玻璃细粉10~60份。
公开号为CN107424667A的中国专利文献中公开了一种无卤阻燃耐火电缆及其制备方法,该电缆具有不燃陶瓷化填充层,不燃陶瓷化填充层包括瓷化粉100份,胶黏剂60~150份和纳米增强助剂1~50份,其中,瓷化粉包括高岭土、滑石粉、云母粉、碳酸锶、硅酸镁、硅酸铝、硅酸钙、硅酸锆、硅酸钡、硫酸钡、氧化铝、氧化钙、氧化锆、氧化镁和氧化锌中的一种或多种;胶黏剂包括氯氧镁水泥基胶黏剂、复合磷硅酸盐无机胶黏剂、锂水玻璃、钠水玻璃和钾水玻璃中的一种或多种;纳米增强助剂包括纳米镁基蒙脱土、纳米二氧化硅、碳纳米管、纳米层状双氢氧化物、纳米磷酸锆、聚倍半硅氧烷和氧化石墨烯中的一种或多种。
公开号为CN108841072A的中国专利文献中公开了一种陶瓷化聚烯烃耐火电缆材料的制备方法,该电缆材料包括以重量计的以下组分:聚烯烃,40-100份;相容剂,1-30份;瓷化粉,350-500份;助熔剂,20-200份;阻燃剂,20-100份;润滑剂,2-20份;及抗氧剂,1-10份;所述的瓷化粉选自陶土、滑石粉、云母粉、叶腊石、硼镁石、硅钙硼石、方解石、石灰石、硅灰石、锂辉石和黏土中的一种或几种。
现有技术方案中的大多数耐火电缆材料所用的瓷化粉存在以下两个问题:
(1)烧结所需温度高,在中温段(600-900℃)的成瓷强度较低,往往高于1000℃才能够形成坚硬的陶瓷状的壳体;
(2)无法在低温下短时间内快速瓷化形成完整致密的陶瓷状的壳体。
发明内容
本发明提供了一种低温烧结瓷化粉及其制备方法,制备工艺简单,生产成本较低,可以实现中温段快速陶瓷化,该瓷化粉瓷化后可形成完整且致密不开裂的壳体。
具体采用的技术方案如下:
本发明提供了一种低温烧结瓷化粉,所述的低温烧结瓷化粉由重量份如下的原料制成:
所述的无机填料Ⅰ为石英粉、白炭黑、高岭土或叶蜡石中的至少一种;所述的无机填料Ⅱ为硅灰石、透辉石、碳酸钙、钙长石或白云石中的至少一种;所述的助熔剂为低熔点磷酸盐玻璃粉或低熔点硼酸盐玻璃粉,始熔温度为350-600℃;所述的矿化剂为氟化镁(MgF2)、氟化钡(BaF2)、氟化钙(CaF2)、氟化锂(LiF)、氟化钠(NaF)或氟化铝(AlF3)中的至少一种;所述的增效剂为镁基蒙脱土或水镁石。
本发明以硅酸盐矿物、矿化剂和助熔剂等为主要原料,无机填料Ⅰ与无机填料Ⅱ在瓷化粉中相互补充,主要起骨架作用;增效剂起补强作用,可以提高瓷化粉的成瓷强度,多种不同的无机填料混合使用来达到最佳的烧结效果。助熔剂的加入可以降低瓷化温度。此外,在瓷化粉烧结成瓷过程中,矿化剂可以和其他原料发生化学反应促进新的物相形成,有利于提高瓷化粉的成瓷性能,能大幅度降烧结后陶瓷的开裂现象,瓷化形成完整致密的壳体。
原料的颗粒尺寸与瓷化粉的烧结性能息息相关。优选的,所述的无机填料Ⅰ的粒径为500-1500目;无机填料Ⅱ的粒径为500-1500目;助熔剂的粒径为600-1500目;增效剂的粒径为500-1500目。
考虑到低温烧结瓷化粉的成瓷性能,优选的,所述的低温烧结瓷化粉由重量份如下的原料制成:
进一步优选的,所述的无机填料Ⅰ的粒径为600-1500目;所述的无机填料Ⅱ的粒径为800-1500目;所述的助熔剂为低熔点磷酸盐玻璃粉,始熔温度为440℃,粒径为700-1500目;所述的增效剂粒径为600-1500目。
原料的分散性、均匀性对瓷化粉的烧结性能有很大影响,所以不能将所述的低温烧结瓷化粉的原料简单混合。
所述的低温烧结瓷化粉的制备方法包括以下步骤:
(1)称取无机填料Ⅰ、无机填料Ⅱ、助熔剂、矿化剂和增效剂,并将无机填料Ⅰ、无机填料Ⅱ、助熔剂和增效剂干燥;
(2)将干燥好的无机填料Ⅰ、无机填料Ⅱ、助熔剂和增效剂与矿化剂混合,搅拌混合均匀,即得到所述的低温烧结瓷化粉。
步骤(1)中,所述的干燥条件为:80-250℃,6-24h。
优选的,步骤(1)中,所述的干燥条件为80-110℃,6h,此条件下可以有效去除物料的物理吸附水,不破坏其结构,能耗低。
步骤(2)中,所述的搅拌的条件为400-800rpm,15-60min。
优选的,步骤(2)中,所述的搅拌的条件为600rpm,20min,此条件下可以更好地实现物料的充分混匀,制备效率高。
所述的低温烧结瓷化粉在600-900℃下烧结20-60min可形成完整致密且不开裂的壳体。
优选的,所述的低温烧结瓷化粉在700-900℃下烧结30min可形成完整致密且不开裂的壳体。
所述的低温烧结瓷化粉可以加入到聚合物基体中,如橡胶或聚烯烃等,制成陶瓷化聚合物耐火电缆材料置于外层用以保护内层材料。
与现有技术相比,本发明的有益效果在于:
本发明公开的低温烧结瓷化粉制备方法简单,生产成本较低,可以实现中温段快速陶瓷化,该瓷化粉瓷化后可形成完整且致密的壳体,且壳体不开裂。
本发明公开的低温烧结瓷化粉配方中添加有矿化剂,矿化剂在烧结成瓷过程中,矿化剂可以和其他原料发生化学反应形成新的物相,有利于提高瓷化粉的成瓷性能。
附图说明
图1为实施例1制备得到的低温烧结瓷化粉在900℃烧结30min成瓷情况图片,A为俯视图,B为截面图。
图2为实施例1制备得到的低温烧结瓷化粉在900℃烧结30min后的XRD图。
图3为实施例2制备得到的低温烧结瓷化粉在900℃烧结30min成瓷情况图片,A为俯视图,B为截面图。
图4为实施例3制备得到的低温烧结瓷化粉在900℃烧结30min成瓷情况图片,A为俯视图,B为截面图。
图5为实施例4制备得到的低温烧结瓷化粉在700℃烧结30min成瓷情况图片,A为俯视图,B为截面图。
图6为对比例1制备得到的瓷化粉在900℃烧结30min成瓷情况图片。
图7为对比例1制备得到的瓷化粉在900℃烧结30min后的XRD图。
图8为对比例2制备得到的瓷化粉在900℃烧结30min成瓷情况图片。
具体实施方式
实施例1
(1)分别称取60g石英粉(粒径600-1500目),120g硅灰石(粒径800-1500目),120g低熔点磷酸盐玻璃粉(始熔温度为440℃,粒径700-1500目),3g镁基蒙脱土(粒径600-1500目)在80℃烘箱中干燥6h;
(2)将干燥好的石英粉、硅灰石、低熔点磷酸盐玻璃粉、镁基蒙脱土放入高速搅拌机里,再加入15g分析纯的MgF2,搅拌混合均匀,搅拌转速为600rpm,搅拌时间为20min,即得到所述的低温烧结瓷化粉。
取上述得到的低温烧结瓷化粉15g,置于陶瓷坩埚中压实,放入马弗炉中900℃烧结30min,升温速率为10℃/min,再随炉冷却至室温。低温烧结瓷化粉的成瓷情况如图1所示,图1A为俯视图,1B为截面图,即该低温烧结瓷化粉在900℃下烧结30min可形成完整致密的壳体。将壳体从15cm高处自由跌落发出清脆响声,未开裂,具有较高成瓷强度,低温烧结瓷化粉在900℃烧结30min后的XRD图如图2所示,烧结后的产物中主要存在石英、AlPO4以及氟磷灰石物相,即烧结过程中矿化剂与原料中的其他组分发生反应生成了氟磷灰石物相,这可以显著提高瓷化粉的成瓷性能。
实施例2
(1)分别称取80g石英粉(粒径600-1500目),10g白炭黑(粒径600-1500目),50g硅灰石(粒径800-1500目),40g碳酸钙(粒径800-1500目),120g低熔点磷酸盐玻璃粉(始熔温度为440℃,粒径700-1500目),6g水镁石(粒径600-1500目)在80℃烘箱中进行干燥6h;
(2)将干燥好的石英粉、白炭黑、硅灰石、碳酸钙、低熔点磷酸盐玻璃粉、水镁石放入高速搅拌机里,再加入12g CaF2,搅拌混合均匀,搅拌转速为600rpm,搅拌时间为20min,即得到所述的低温烧结瓷化粉。
取上述得到的低温烧结瓷化粉15g,置于陶瓷坩埚中压实,放入马弗炉中900℃烧结30min,升温速率为10℃/min,再随炉冷却至室温。低温烧结瓷化粉的成瓷情况如图3所示,图3A为俯视图,3B为截面图,即该低温烧结瓷化粉在900℃下烧结30min可形成完整且致密的壳体,将壳体从15cm高处自由跌落发出清脆响声,未开裂,具有较高成瓷强度。
实施例3
分别称取70g石英粉(粒径600-1500目),20g高岭土(粒径600-1500目),80g硅灰石(粒径800-1500目),20g钙长石(粒径800-1500目),140g低熔点磷酸盐玻璃粉(始熔温度为440℃,粒径700-1500目),3g镁基蒙脱土(粒径600-1500目)在80℃烘箱中进行干燥6h;
(2)将干燥好的石英粉、高岭土、硅灰石、钙长石、低熔点磷酸盐玻璃粉、镁基蒙脱土放入高速搅拌机里,再加入6g MgF2和3g BaF2,搅拌混合均匀,搅拌转速为600rpm,搅拌时间为20min,即得到所述的低温烧结瓷化粉。
取上述得到的低温烧结瓷化粉15g,置于陶瓷坩埚中压实,放入马弗炉中900℃烧结30min,升温速率为10℃/min,再随炉冷却至室温。低温烧结瓷化粉的成瓷情况如图4所示,图4A为俯视图,4B为截面图,即该低温烧结瓷化粉在900℃下烧结30min可形成完整且致密的壳体,将壳体从15cm高处自由跌落发出清脆响声,未开裂,具有较高成瓷强度。
实施例4
(1)分别称取100g石英粉(粒径600-1500目),20g白炭黑(粒径600-1500目),50g硅灰石(粒径800-1500目),10g碳酸钙(粒径800-1500目),120g低熔点磷酸盐玻璃粉(始熔温度为440℃,粒径700-1500目),6g水镁石(粒径600-1500目)在80℃烘箱中进行干燥6h;
(2)将干燥好的石英粉、白炭黑、硅灰石、碳酸钙、低熔点磷酸盐玻璃粉、水镁石放入高速搅拌机里,再加入12g MgF2,搅拌混合均匀,搅拌转速为600rpm,搅拌时间为20min,即得到所述的低温烧结瓷化粉。
取上述得到的低温烧结瓷化粉15g,置于陶瓷坩埚中压实,放入马弗炉中700℃烧结30min,升温速率为10℃/min,再随炉冷却至室温。低温烧结瓷化粉的成瓷情况如图5所示,图5A为俯视图,5B为截面图,即该低温烧结瓷化粉在700℃下烧结30min可形成完整且致密的壳体,将壳体从15cm高处自由跌落发出清脆响声,未开裂,具有较高成瓷强度。
实施例5
(1)分别称取80g石英粉(粒径600-1500目),10g叶蜡石(粒径600-1500目),90g硅灰石(粒径800-1500目),20g透辉石(粒径800-1500目),10g白云石(粒径800-1500目),120g低熔点硼酸盐玻璃粉(始熔温度为400℃,粒径700-1500目),3g镁基蒙脱土(粒径600-1500目)在100℃烘箱中进行干燥6h;
(2)将干燥好的石英粉、叶蜡石、硅灰石、透辉石、白云石、低熔点硼酸盐玻璃粉、镁基蒙脱土放入高速搅拌机里,再加入4g LiF、4g NaF和4g AlF3,搅拌混合均匀,搅拌转速为500rpm,搅拌时间为30min,即得到所述的低温烧结瓷化粉。
对比例1
(1)分别称取60g石英粉(粒径600-1500目),120g硅灰石(粒径800-1500目),120g磷酸盐玻璃粉(始熔温度为440℃,粒径700-1500目),3g镁基蒙脱土(粒径600-1500目)在80℃烘箱中进行干燥6h;
(2)将干燥好的石英粉、硅灰石、低熔点磷酸盐玻璃粉、镁基蒙脱土放入高速搅拌机里搅拌混合均匀,搅拌转速为600rpm,搅拌时间为20min,得到瓷化粉。
取上述得到的瓷化粉15g,置于陶瓷坩埚中压实,放入马弗炉中900℃烧结30min,升温速率为10℃/min,再随炉冷却至室温。该瓷化粉的成瓷情况如图6所示,该瓷化粉烧结后形成的壳体存在明显的开裂,将样品从15cm高处自由跌落发出清脆响声。瓷化粉在900℃烧结30min后的XRD图如图7所示,烧结后的产物中主要存在石英、AlPO4和硅酸钙水合物。
对比例2
(1)分别称取150g石英粉(粒径600-1500目),30g硅灰石(粒径800-1500目),120g磷酸盐玻璃粉(始熔温度为440℃,粒径700-1500目),4g镁基蒙脱土(粒径600-1500目)在80℃烘箱中进行干燥6h;
(2)再将上述石英粉、硅灰石、低熔点磷酸盐玻璃粉、镁基蒙脱土放入高速搅拌机里混合均匀,搅拌转速为600rpm,搅拌时间为20min,得到瓷化粉。
取上述得到的瓷化粉称15g,置于陶瓷坩埚中压实,放入马弗炉中进行900℃烧结30min,升温速率为10℃/min,再随炉冷却至室温。瓷化粉成瓷情况如图8所示,可以发现瓷化形成的壳体存在明显的开裂,将样品从15cm高处自由跌落发出清脆响声。
样品分析
实施例1-4与对比例1-2制备的样品成瓷性能如表1所示:
表1实施例1-4的低温烧结瓷化粉与对比例1-2的瓷化粉成瓷性能
注:(1)是否成瓷判断方法:将壳体样品从15cm高处自由跌落,跌落时是否发出清脆响声。
(2)是否具有一定成瓷强度判断方法:将壳体样品从15cm高处自由跌落,跌落是否开裂。
(3)严重开裂的壳体样品无法判断其成瓷强度,用“/”表示。
根据表1中实施例与对比例烧结后的成瓷情况可知,加入矿化剂的体系能大幅度降烧结后的开裂现象,瓷化形成完整不开裂的壳体,并具有一定力学性能。
Claims (9)
2.根据权利要求1所述的低温烧结瓷化粉,其特征在于,所述的无机填料Ⅰ的粒径为500-1500目;无机填料Ⅱ的粒径为500-1500目;助熔剂的粒径为600-1500目;增效剂的粒径为500-1500目。
4.根据权利要求3所述的低温烧结瓷化粉,其特征在于,所述的无机填料Ⅰ的粒径为600-1500目;所述的无机填料Ⅱ的粒径为800-1500目;所述的助熔剂为低熔点磷酸盐玻璃粉,始熔温度为440℃,粒径为700-1500目;所述的增效剂粒径为600-1500目。
5.根据权利要求1所述的低温烧结瓷化粉,其特征在于,所述的低温烧结瓷化粉的制备方法包括以下步骤:
(1)称取无机填料Ⅰ、无机填料Ⅱ、助熔剂、矿化剂和增效剂,并将无机填料Ⅰ、无机填料Ⅱ、助熔剂和增效剂干燥;
(2)将干燥好的无机填料Ⅰ、无机填料Ⅱ、助熔剂和增效剂与矿化剂混合,搅拌混合均匀,即得到所述的低温烧结瓷化粉。
6.根据权利要求5所述的低温烧结瓷化粉,其特征在于,步骤(1)中,所述的干燥条件为:80-250℃,6-24h。
7.根据权利要求5所述的低温烧结瓷化粉,其特征在于,步骤(2)中,所述的搅拌的条件为400-800rpm,15-60min。
8.根据权利要求1-7任一项所述的低温烧结瓷化粉,其特征在于,所述的低温烧结瓷化粉在600-900℃下烧结20-60min形成完整不开裂的壳体。
9.根据权利要求1-7任一项所述的低温烧结瓷化粉在耐火电缆材料中的应用。
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