CN112851308B - 一种用于超高温环境下陶瓷钉及制备方法 - Google Patents
一种用于超高温环境下陶瓷钉及制备方法 Download PDFInfo
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- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
本发明涉及陶瓷钉生产技术领域，尤其涉及一种用于超高温环境下陶瓷钉及制备方法，该陶瓷钉按质量份计包括以下原料：氧化铝粉80～90份、二氧化钛粉2～6份、氧化镁粉2～8份、纳米陶瓷粉体0.5～1.5份、纳米二氧化硅1.5～3.5份、甲基丙烯酸甲酯12～18份和抗腐蚀添加剂25～45份，且其制备方法包括以下步骤：S1、按量称取原料，备用；S2、将原料中的固体研磨成粉并与其余粉体相混合，得到生料粉末，再将生料粉末倒入抗腐蚀添加剂中搅拌混匀，得生料；S3、将生料装入模具，经脉冲电流烧结后得到氧化铝陶瓷。本发明不仅能够改善陶瓷钉的可降解能力，而且还能改善其抗腐蚀能力。
Description
技术领域
本发明涉及陶瓷钉生产技术领域，尤其涉及一种用于超高温环境下陶瓷钉及制备方法。
背景技术
随着高温领域技术的发展，人们对用于制备高温器件的材料提出了更高的性能要求。陶瓷基复合材料具有耐高温、高比强等优良性能，在高温领域已经得到了广泛应用。传统的金属螺钉虽然易加工成型，但其相较于强度低且不耐高温，由石墨、C/C复合材料制备的螺钉而言，在高温下易氧化且强度不够，均不适用于高温器件的连接，而陶瓷钉由于其优良的性能更适用于高温领域。
现有的陶瓷钉在腐蚀性偏强的环境下使用时，容易造成大面积的腐蚀，影响该陶瓷钉的连接作用，而且废弃的陶瓷钉也并不具备可降解能力。因此，我们提出了一种用于超高温环境下陶瓷钉及制备方法用于解决上述问题。
发明内容
本发明的目的是为了解决现有技术中存在的缺点，而提出的一种用于超高温环境下陶瓷钉及制备方法。
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉80～90份、二氧化钛粉2～6份、氧化镁粉2～8份、纳米陶瓷粉体0.5～1.5份、纳米二氧化硅1.5～3.5份、甲基丙烯酸甲酯12～18份和抗腐蚀添加剂25～45份；
其中，所述纳米陶瓷粉体为氮化硅粉与氧化锆粉的混合粉体。
优选的，所述氧化铝粉和抗腐蚀添加剂的质量比为(2～3)：1。
优选的，所述抗腐蚀添加剂由镍基合金、无机硅酸锌和无机抗菌粉制成，其中，镍基合金为Ni-Mo合金，无机抗菌粉的型号为JDGKP-010E，且抗腐蚀添加剂的制备方法如下：将镍基合金、无机硅酸锌粉碎后与无机抗菌粉混合，混匀后于造粒机内造粒，得颗粒状的抗腐蚀添加剂。
优选的，所述提取液浓缩的工艺采用的是反透析浓缩法。
优选的，所述提取液浓缩后的溶液密度为1.12～1.15。
一种用于超高温环境下陶瓷钉的制备方法，包括以下步骤：
S1、按量称取原料，备用；
S2、将原料中的固体研磨成粉并与其余粉体相混合，得到生料粉末，再将生料粉末倒入抗腐蚀添加剂中搅拌混匀，得生料；
S3、将生料装入模具，经脉冲电流烧结后得到氧化铝陶瓷；
S4、以聚氧硅烷为先驱体，对氧化铝陶瓷进行真空浸渍和惰性气氛裂解，得到初坯；
S5、将初坯按螺钉要求加工成半成品；
S6、将半成品再经过8～12次真空浸渍和惰性气氛裂解处理，最终得到成品的陶瓷钉。
优选的，所述S2中粉体的粒度≤1μm。
优选的，所述S6中真空浸渍的时间为2～8h，惰性气氛裂解的温度为800℃～1000℃。
优选的，所述真空浸渍是以聚氧硅烷溶液为浸渍液，聚氧硅烷质量分数为50％，以乙醇为溶剂。
本发明的有益效果是：
1、在原料组成中加入甲基丙烯酸甲酯，经过磨粉、混合、浸渍及裂解等工序制成陶瓷钉，令加入的甲基丙烯酸甲酯在高温下分解，从而使得陶瓷钉内部形成多个空隙，进而提高该陶瓷钉的可降解能力。
2、在原料组成中加入由抗腐蚀添加剂，能够提高该陶瓷钉的抗腐蚀能力，有利于在恶劣环境下进行使用。
具体实施方式
下面结合具体实施例对本发明作进一步解说。
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉80～90份、二氧化钛粉2～6份、氧化镁粉2～8份、纳米陶瓷粉体0.5～1.5份、纳米二氧化硅1.5～3.5份、甲基丙烯酸甲酯12～18份和抗腐蚀添加剂25～45份；
其中，所述纳米陶瓷粉体为氮化硅粉与氧化锆粉的混合粉体，氧化铝粉和抗腐蚀添加剂的质量比为(2～3)：1。
抗腐蚀添加剂由镍基合金、无机硅酸锌和无机抗菌粉制成，其中，镍基合金为Ni-Mo合金，无机抗菌粉的型号为JDGKP-010E，且抗腐蚀添加剂的制备方法如下：将镍基合金、无机硅酸锌粉碎后与无机抗菌粉混合，混匀后于造粒机内造粒，得颗粒状的抗腐蚀添加剂。
一种用于超高温环境下陶瓷钉的制备方法，包括以下步骤：
S1、按量称取原料，备用；
S2、将原料中的固体研磨成粒度≤1μm的粉并与其余粉体相混合，得到生料粉末，再将生料粉末倒入抗腐蚀添加剂中搅拌混匀，得生料；
S3、将生料装入模具，经脉冲电流烧结后得到氧化铝陶瓷；
S4、以聚氧硅烷为先驱体，对氧化铝陶瓷进行真空浸渍和惰性气氛裂解，得到初坯；
S5、将初坯按螺钉要求加工成半成品；
S6、将半成品再经过8次真空浸渍和惰性气氛裂解处理，最终得到成品的陶瓷钉。
其中，S6中真空浸渍的时间为3h，惰性气氛裂解的温度为800℃，真空浸渍是以聚氧硅烷溶液为浸渍液，聚氧硅烷质量分数为50％，以乙醇为溶剂。
实施例一：
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉80份、二氧化钛粉2份、氧化镁粉2份、纳米陶瓷粉体0.5份、纳米二氧化硅1.5份、甲基丙烯酸甲酯12份和抗腐蚀添加剂40份。
实施例二：
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉85份、二氧化钛粉4份、氧化镁粉5份、纳米陶瓷粉体1份、纳米二氧化硅2.5份、甲基丙烯酸甲酯15份和抗腐蚀添加剂42.5份。
实施例三：
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉90份、二氧化钛粉6份、氧化镁粉8份、纳米陶瓷粉体1.5份、纳米二氧化硅3.5份、甲基丙烯酸甲酯18份和抗腐蚀添加剂45份。
在实施例一～实施例三中，氧化铝粉和抗腐蚀添加剂的质量比为2:1，且由上述各个实施例中的原料来制备陶瓷钉的方法，包括以下步骤：
S1、按量称取原料，备用；
S2、将原料中的固体研磨成粒度≤1μm的粉并与其余粉体相混合，得到生料粉末，再将生料粉末倒入抗腐蚀添加剂中搅拌混匀，得生料；
S3、将生料装入模具，经脉冲电流烧结后得到氧化铝陶瓷；
S4、以聚氧硅烷为先驱体，对氧化铝陶瓷进行真空浸渍和惰性气氛裂解，得到初坯；
S5、将初坯按螺钉要求加工成半成品；
S6、将半成品再经过8次真空浸渍和惰性气氛裂解处理，最终得到成品的陶瓷钉。
试验一：对该陶瓷钉可降解能力的测定
对比例一：
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉80份、二氧化钛粉2份、氧化镁粉2份、纳米陶瓷粉体0.5份、纳米二氧化硅1.5份和抗腐蚀添加剂40份。
对比例二：
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉85份、二氧化钛粉4份、氧化镁粉5份、纳米陶瓷粉体1份、纳米二氧化硅2.5份和抗腐蚀添加剂42.5份。
对比例三：
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉90份、二氧化钛粉6份、氧化镁粉8份、纳米陶瓷粉体1.5份、纳米二氧化硅3.5份和抗腐蚀添加剂45份。
上述对比例均可采用下述步骤来制备陶瓷钉的方法：
S1、按量称取原料，备用；
S2、将原料中的固体研磨成粉并与其余粉体相混合，得到生料粉末，再将生料粉末倒入抗腐蚀添加剂中搅拌混匀，得生料；
S3、将生料装入模具，经脉冲电流烧结后得到氧化铝陶瓷；
S4、以聚氧硅烷为先驱体，对氧化铝陶瓷进行真空浸渍和惰性气氛裂解，得到初坯；
S5、将初坯按螺钉要求加工成半成品；
S6、将半成品再经过8次真空浸渍和惰性气氛裂解处理，最终得到成品的陶瓷钉。
有机染料溶液的配置：分别称取0.0050g的有机染料(曙红、甲基橙、酸性品红和甲基红)于小烧杯中，用移液管移取10ml蒸馏水溶解，再用移液管移取5ml溶液至250ml的容量瓶中，接着定容，摇匀，配置成有机染料溶液；
光催化降解：向上述有机染料溶液中分别加入一枚上述实施例和对比例中的陶瓷钉，在黑暗条件下搅拌2h，然后置于自然光下进行降解反应，每隔5min取一次上清液，然后用离心机离心，取清液，通过紫外-可见分光光度计检测有机染料溶液的降解率，具体结果见下表。
| 降解率/％ | 曙红 | 甲基橙 | 酸性品红 | 甲基红 |
| 实施例一 | 97.3 | 99.2 | 89.5 | 94.6 |
| 实施例二 | 97.2 | 98.7 | 89.1 | 93.9 |
| 实施例三 | 97.0 | 98.8 | 90.2 | 95.3 |
| 对比例一 | 37.8 | 38.5 | 40.3 | 45.6 |
| 对比例二 | 38.1 | 38.5 | 41.6 | 45.0 |
| 对比例三 | 36.8 | 37.2 | 46.1 | 44.3 |
由上表数据可知，实施例中的降解率相对于对比例中的降解率而言要更高，也就是说，由实施例的配方及其方法步骤制得的陶瓷钉的可降解能力更优。
试验二：对该陶瓷钉抗腐蚀能力的测定
对比例四：
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉80份、二氧化钛粉2份、氧化镁粉2份、纳米陶瓷粉体0.5份、纳米二氧化硅1.5份和甲基丙烯酸甲酯12份。
对比例五：
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉85份、二氧化钛粉4份、氧化镁粉5份、纳米陶瓷粉体1份、纳米二氧化硅2.5份和甲基丙烯酸甲酯15份。
对比例六：
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉90份、二氧化钛粉6份、氧化镁粉8份、纳米陶瓷粉体1.5份、纳米二氧化硅3.5份和甲基丙烯酸甲酯18份。
上述对比例均可采用下述步骤来制备陶瓷钉的方法：
S1、按量称取原料，备用；
S2、将原料中的固体研磨成粉并与其余粉体相混合，得到生料粉末；
S3、将生料粉末装入模具，经脉冲电流烧结后得到氧化铝陶瓷；
S4、以聚氧硅烷为先驱体，对氧化铝陶瓷进行真空浸渍和惰性气氛裂解，得到初坯；
S5、将初坯按螺钉要求加工成半成品；
S6、将半成品再经过8次真空浸渍和惰性气氛裂解处理，最终得到成品的陶瓷钉。
采用中性盐雾试验(NSS试验)来进行耐腐蚀测试，将实施例一～实施例三以及对比例四～对比例中的陶瓷钉置于盐雾箱内进行实验，观察并记录下五天(120h)内陶瓷钉表面开始出现被腐蚀的时间，具体见下表：
由上表数据可知，实施例中制得的陶瓷钉相对于对比例中制得的陶瓷钉而言，其开始被腐蚀的时间要更延后一些，也就是说，由实施例的配方及其方法步骤制得的陶瓷钉的抗腐蚀能力更优。
试验三：对氧化铝粉和抗腐蚀添加剂的质量比的测定
对比例七：
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉120份、二氧化钛粉2份、氧化镁粉2份、纳米陶瓷粉体0.5份、纳米二氧化硅1.5份、甲基丙烯酸甲酯12份和抗腐蚀添加剂40份。
对比例八：
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉40份、二氧化钛粉2份、氧化镁粉2份、纳米陶瓷粉体0.5份、纳米二氧化硅1.5份、甲基丙烯酸甲酯12份和抗腐蚀添加剂40份。
对比例九：
一种用于超高温环境下陶瓷钉，按质量份计包括以下原料：氧化铝粉160份、二氧化钛粉2份、氧化镁粉2份、纳米陶瓷粉体0.5份、纳米二氧化硅1.5份、甲基丙烯酸甲酯12份和抗腐蚀添加剂40份。
上述各个实施例中的原料来制备陶瓷钉的方法，包括以下步骤：
S1、按量称取原料，备用；
S2、将原料中的固体研磨成粒度≤1μm的粉并与其余粉体相混合，得到生料粉末，再将生料粉末倒入抗腐蚀添加剂中搅拌混匀，得生料；
S3、将生料装入模具，经脉冲电流烧结后得到氧化铝陶瓷；
S4、以聚氧硅烷为先驱体，对氧化铝陶瓷进行真空浸渍和惰性气氛裂解，得到初坯；
S5、将初坯按螺钉要求加工成半成品；
S6、将半成品再经过8次真空浸渍和惰性气氛裂解处理，最终得到成品的陶瓷钉。
根据试验一中的测试方法对上述对比例和实施例一中的陶瓷钉进行实验，此试验中仅设计曙红和甲基橙两组有机染料溶液，然后再以与试验一相同的步骤检测其降解率，具体结果见下表。
| 降解率/％ | 质量比 | 曙红 | 甲基橙 |
| 实施例一 | 2:1 | 97.3 | 99.2 |
| 对比例七 | 3:1 | 96.9 | 98.8 |
| 对比例八 | 1:1 | 88.1 | 89.3 |
| 对比例九 | 4:1 | 87.9 | 88.1 |
由上表数据可知，当氧化铝粉和抗腐蚀添加剂的质量比在2:1～3:1的范围内时，其降解率相对于其他比例下的降解率要更高。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。
Claims (6)
1.一种用于超高温环境下陶瓷钉，其特征在于，按质量份计包括以下原料：氧化铝粉80～90份、二氧化钛粉2～6份、氧化镁粉2～8份、纳米陶瓷粉体0.5～1.5份、纳米二氧化硅1.5～3.5份、甲基丙烯酸甲酯12～18份和抗腐蚀添加剂25～45份，所述抗腐蚀添加剂由镍基合金、无机硅酸锌和无机抗菌粉制成，其中，镍基合金为Ni-Mo合金，无机抗菌粉的型号为JDGKP-010E，且抗腐蚀添加剂的制备方法如下：将镍基合金、无机硅酸锌粉碎后与无机抗菌粉混合，混匀后于造粒机内造粒，得颗粒状的抗腐蚀添加剂；
其中，所述纳米陶瓷粉体为氮化硅粉与氧化锆粉的混合粉体。
2.根据权利要求1所述的一种用于超高温环境下陶瓷钉，其特征在于，所述氧化铝粉和抗腐蚀添加剂的质量比为（2～3）：1。
3.一种根据权利要求1～2中的任意一种用于 超高温环境下陶瓷钉的制备方法，其特征在于，包括以下步骤：
S1、按量称取原料，备用；
S2、将原料中的固体研磨成粉并与其余粉体相混合，得到生料粉末，再将生料粉末倒入抗腐蚀添加剂中搅拌混匀，得生料；
S3、将生料装入模具，经脉冲电流烧结后得到氧化铝陶瓷；
S4、以聚氧硅烷为先驱体，对氧化铝陶瓷进行真空浸渍和惰性气氛裂解，得到初坯；
S5、将初坯按螺钉要求加工成半成品；
S6、将半成品再经过8～12次真空浸渍和惰性气氛裂解处理，最终得到所述陶瓷钉。
4.根据权利要求3所述的一种用于超高温环境下陶瓷钉的制备方法，其特征在于，所述S2中粉体的粒度≤1μm。
5.根据权利要求3所述的一种用于超高温环境下陶瓷钉的制备方法，其特征在于，所述S6中真空浸渍的时间为2～8h，惰性气氛裂解的温度为800℃～1000℃。
6.根据权利要求3所述的一种用于超高温环境下陶瓷钉的制备方法，其特征在于，所述真空浸渍是以聚氧硅烷溶液为浸渍液，聚氧硅烷质量分数为50%，以乙醇为溶剂。
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