CN112589954A - 一种二硅化钼陶瓷的注射成形方法 - Google Patents

一种二硅化钼陶瓷的注射成形方法 Download PDF

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CN112589954A
CN112589954A CN202011231961.5A CN202011231961A CN112589954A CN 112589954 A CN112589954 A CN 112589954A CN 202011231961 A CN202011231961 A CN 202011231961A CN 112589954 A CN112589954 A CN 112589954A
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molybdenum disilicide
injection molding
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王焱辉
刘奇
薄新维
韩校宇
王小宇
陈喜
何浩然
姚志远
刘成超
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Chongqing Materials Research Institute Co Ltd
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Abstract

本发明涉及粉末冶金技术领域，具体涉及一种二硅化钼陶瓷制品的注射成形方法，将粘结剂与二硅化钼粉末按照22g～30g:100g的比例在混炼机上混炼后制粒，将得到的颗粒注射成形得到生坯，再催化脱脂得到脱脂坯，最后将脱脂坯进行还原烧结得到二硅化钼陶瓷制品，本发明利用传统粉末冶金技术与塑料注射成形工艺相结合形成的一种近净成形技术，不但省去了传统粉末冶金工艺的中间机械加工环节，节省原材料的同时，实现了高效率、低成本的自动连续生产，降低了生产加工成本，还突破了传统金属粉末模压成形工艺在产品形状上的限制，可以一体成型制备形状复杂、体积小、尺寸精度高的二硅化钼陶瓷制品。

Description

一种二硅化钼陶瓷的注射成形方法
技术领域
本发明涉及粉末冶金技术领域，具体涉及一种二硅化钼陶瓷制品的注射成形方法。
背景技术
二硅化钼陶瓷具有高熔点、耐腐蚀、良好的导热性和导电性以及优良的高温抗氧化能力，被用作高温发热体材料和高温结构材料，在能源化工、航空航天、冶金环保等领域具有广阔的应用前景。
但是，由于二硅化钼陶瓷本身具有质脆和高硬度，在制造复杂结构件时，如果采用传统粉末冶金工艺，将二硅化钼粉末压制成形烧结后再进行机械加工，制品成形困难、加工成本高，难以制备形状复杂、体积小、尺寸精度高的构件。
发明内容
本发明的目的是针对现有技术对应的不足，提供一种二硅化钼陶瓷制品的注射成形方法，是利用传统粉末冶金技术与塑料注射成形工艺相结合形成的一种近净成形技术，不但省去了传统粉末冶金工艺的中间机械加工环节，节省原材料的同时，实现了高效率、低成本的自动连续生产，降低了生产加工成本，还突破了传统金属粉末模压成形工艺在产品形状上的限制，可以一体成型制备形状复杂、体积小、尺寸精度高的二硅化钼陶瓷制品。
本发明的目的是采用下述方案实现的：一种用于二硅化钼陶瓷制品注射成形的粘结剂，各组分的重量百分含量为：聚乙烯5％、微晶蜡0～3％、硬脂酸2～ 5％、乙烯-醋酸乙烯酯2～5％，余量为聚甲醛。
较好技术方案是，各组分的重量百分含量为：聚乙烯5％、微晶蜡3％、硬脂酸2％、乙烯-醋酸乙烯酯5％，余量为聚甲醛。
较好技术方案是，各组分的重量百分含量为：聚乙烯5％、微晶蜡3％、硬脂酸5％、乙烯-醋酸乙烯酯2％，余量为聚甲醛。
较好技术方案是，各组分的重量百分含量为：聚乙烯5％、硬脂酸5％、乙烯 -醋酸乙烯酯3％，余量为聚甲醛。
二硅化钼陶瓷制品的注射成形方法，包括以下步骤：
1)将粘结剂中的聚甲醛、聚乙烯、乙烯-醋酸乙烯酯与二硅化钼粉末加入混炼机，温度160℃～180℃下混炼40～60分钟，降温至130℃～150℃，再加入粘结剂中的微晶蜡和硬脂酸，混炼30～40分钟，制得混合物料；
其中，所述二硅化钼粉末与权利要求1所述粘结剂的重量比为22g～ 30g:100g；
2)将步骤1)得到的混合物料制粒，得到颗粒；
3)步骤2)得到的颗粒在温度160～180℃，压力为50～70MPa，模具温度为100～120℃注射成形得到生坯；
4)将步骤3)得到的生坯利用脱脂温度为110～125℃的催化脱脂炉进行催化脱脂，按0.01～0.05cc/min向催化脱脂炉中通入HNO3气体，脱脂5～8小时得到脱脂坯；
5)氢气气氛下，烧结步骤4)得到的脱脂坯，烧结温度从室温升至500℃，保温30min～60min，再升至1600℃，保温≥3小时，随炉冷却至室温，得到二硅化钼陶瓷制品。
步骤1)中混炼时采用氩气保护。
步骤1)中混炼转速为30～60r/min。
步骤2)中采用挤料机制粒。
步骤2)中制粒时挤料机的转速为600～800r/min。
步骤5)中氢气的通入速率为4～7L/min。
所述粘结剂采用上述含量的各组分的作用如下：
聚甲醛作为主要组分，是一种综合性能优良的工程塑料，具有高的力学性能，还具有优良的电绝缘性、耐溶剂性和可加工性；
聚乙烯在低温时仍能保持一定的韧性，在本发明中用作粘结剂的骨架组分，为生坯保持形状；
乙烯-醋酸乙烯酯具有良好的分散作用，促进各组分之间能够混合均匀；
微晶蜡作为填充剂改善混合物料的流动性；
硬脂酸作为表面活性剂可防止粉末与粘结剂的两相分离，使粘结剂与二硅化钼粉末具有良好的相容性。
因为聚甲醛、高密度聚乙烯、乙烯-醋酸乙烯酯为高熔点组分，微晶蜡和硬脂酸为低熔点组分，故，首先，将聚甲醛、高密度聚乙烯、乙烯-醋酸乙烯酯与二硅化钼粉末加入混炼机，混炼转速为30～60r/min，升温至160℃～180℃并混炼40～60分钟，再将温度降低至130℃～150℃，加入微晶蜡和硬脂酸，混炼 30～40分钟制得混合物料，使高熔点组分和低熔点组分更容易相互混匀。
由于采用了上述技术方案，利用注射成形机加工得到的生坯在注射成形的过程中不容易产生缺陷，并且具有足够的强度以抵抗脱模、重力引起的变形，以保证生坯成形后，在后面的工序中不会轻易产生形变。
使用HNO3气体作为脱脂催化剂进行催化脱脂得到的脱脂坯在脱脂过程中不会产生明显的缺陷，能够长时间维持原有的形状，而且催化脱脂速率可通过控制脱脂催化剂HNO3的流量、脱脂温度、脱脂时间来实现。
步骤1)中混炼时采用氩气保护，防止混合物料氧化。
通过本发明得到的二硅化钼陶瓷制品通过肉眼观察可知其表面光洁、无裂痕，且采用阿基米德排水法测得该二硅化钼陶瓷制品的密度为6.15～6.20g/cm3，为其理论密度的98.55％～99.30％，在CMT5305微机控制电子万能试验机上按照标准GB/T 4741-1999的三点弯曲法测得其抗弯强度为116～135MPa，采用标准 GB/T 7314-2005的气压和水压试验方法测得其耐压能力可以承受9.5～11MPa压力而不断裂，不但省去了传统粉末冶金工艺的中间机械加工环节，节省原材料的同时，实现了高效率、低成本的自动连续生产，降低了生产加工成本，还突破了传统金属粉末模压成形工艺在产品形状上的限制，可以一体成型制备形状复杂、体积小、尺寸精度高的二硅化钼陶瓷制品。
附图说明
图1为本发明的流程图。
具体实施方式
结合下列实施例1～3，按照图1所示的步骤分别制备二硅化钼陶瓷制品，对本发明的技术方案进行描述。
实施例1：
粘结剂各组分的重量百分含量为：聚乙烯5％、微晶蜡3％、硬脂酸2％、乙烯 -醋酸乙烯酯5％，余量为聚甲醛。
采用实施例1所述粘结剂制备U型二硅化钼陶瓷保护套管，包括以下步骤：
1)取粒度为20～40μm的二硅化钼粉末1000g，实施例1所述的粘结剂220g；
将粘结剂中的聚甲醛、聚乙烯、乙烯-醋酸乙烯酯与二硅化钼粉末加入混炼机，温度170℃下混炼40分钟，降温至130℃，再加入粘结剂中的微晶蜡和硬脂酸，混炼30分钟，制得混合物料；
步骤1)中混炼时采用氩气保护。
步骤1)中混炼转速为30r/min。
2)将步骤1)得到的混合物料制粒，得到颗粒；
步骤2)中采用挤料机制粒。
步骤2)中制粒时挤料机的转速为600r/min。
本实施例中，制粒时采用的挤料机为单螺杆挤料机。
3)步骤2)得到的颗粒在温度160℃，压力为70MPa，模具温度为100℃注射成形得到生坯；本实施例中，采用注射成形机进行此步骤；
4)将步骤3)得到的生坯利用脱脂温度为110℃的催化脱脂炉进行催化脱脂，按0.02cc/min向催化脱脂炉中通入HNO3气体，脱脂8小时得到脱脂坯；
5)按照7L/min的速率持续通入氢气，氢气气氛下，采用碳管炉烧结步骤4) 得到的脱脂坯，烧结温度以5℃/min从室温升至500℃，保温60min，再以10℃ /min将温度升至1600℃，保温3小时，随炉冷却至室温，得到U型二硅化钼陶瓷保护套管。
本实施例得到的U型二硅化钼陶瓷保护套管通过肉眼观察可知其表面光洁、无裂痕，且采用阿基米德排水法测得该U型二硅化钼陶瓷保护套管的密度为 6.17g/cm3，为其理论密度的98.87％，并将该U型二硅化钼陶瓷保护套管在 CMT5305微机控制电子万能试验机上按照标准GB/T 4741-1999的三点弯曲法测得其抗弯强度为118MPa，最后再采用标准GB/T7314-2005的气压和水压试验方法测得该U型二硅化钼陶瓷保护套管的耐压能力可以承受9.8MPa压力而不断裂。
实施例2：
粘结剂各组分的重量百分含量为：聚乙烯5％、微晶蜡3％、硬脂酸5％、乙烯 -醋酸乙烯酯2％，余量为聚甲醛。
采用实施例2所述粘结剂制备环型二硅化钼陶瓷发热体，包括以下步骤：
1)取粒度为20～40μm的二硅化钼粉末1000g，实施例2所述的粘结剂240g；
将粘结剂中的聚甲醛、聚乙烯、乙烯-醋酸乙烯酯与二硅化钼粉末加入混炼机，温度180℃下混炼45分钟，降温至150℃，再加入粘结剂中的微晶蜡和硬脂酸，混炼30分钟，制得混合物料；
步骤1)中混炼时采用氩气保护。
步骤1)中混炼转速为40r/min。
2)将步骤1)得到的混合物料制粒，得到颗粒；
步骤2)中采用挤料机制粒。
步骤2)中制粒时挤料机的转速为700r/min。
本实施例中，制粒时采用的挤料机为单螺杆挤料机。
3)步骤2)得到的颗粒在温度180℃，压力为65MPa，模具温度为120℃注射成形得到生坯；本实施例中，采用注射成形机进行此步骤；
4)将步骤3)得到的生坯利用脱脂温度为110℃的催化脱脂炉进行催化脱脂，按0.05cc/min向催化脱脂炉中通入HNO3气体，脱脂8小时得到脱脂坯；
5)按照6L/min的速率持续通入氢气，氢气气氛下，采用碳管炉烧结步骤4) 得到的脱脂坯，烧结温度以7℃/min从室温升至500℃，保温60min，再以8℃ /min将温度升至1600℃，保温3小时，随炉冷却至室温，得到环型二硅化钼陶瓷发热体。
本实施例得到的环型二硅化钼陶瓷发热体通过肉眼观察可知其表面光洁、无裂痕，且采用阿基米德排水法测得该环型二硅化钼陶瓷发热体的密度为 6.19g/cm3，为其理论密度的99.20％，并将该环型二硅化钼陶瓷发热体在CMT5305 微机控制电子万能试验机上按照标准GB/T 4741-1999的三点弯曲法测得其抗弯强度为127MPa，最后再采用标准GB/T7314-2005的气压和水压试验方法测得该环型二硅化钼陶瓷发热体的耐压能力可以承受10.2MPa压力而不断裂。
实施例3：
粘结剂各组分的重量百分含量为：聚乙烯5％、硬脂酸5％、乙烯-醋酸乙烯酯3％，余量为聚甲醛。
采用实施例3所述粘结剂制备螺旋型二硅化钼加热棒，包括以下步骤：
1)取粒度为20～40μm的二硅化钼粉末1000g，实施例2所述的粘结剂300g；
将粘结剂中的聚甲醛、聚乙烯、乙烯-醋酸乙烯酯与二硅化钼粉末加入混炼机，温度170℃下混炼40分钟，降温至140℃，再加入粘结剂中的硬脂酸，混炼30分钟，制得混合物料；
步骤1)中混炼时采用氩气保护。
步骤1)中混炼转速为45r/min。
2)将步骤1)得到的混合物料制粒，得到颗粒；
步骤2)中采用挤料机制粒。
步骤2)中制粒时挤料机的转速为650r/min。
本实施例中，制粒时采用的挤料机为单螺杆挤料机。
3)步骤2)得到的颗粒在温度170℃，压力为50MPa，模具温度为110℃注射成形得到生坯；本实施例中，采用注射成形机进行此步骤；
4)将步骤3)得到的生坯利用脱脂温度为120℃的催化脱脂炉进行催化脱脂，按0.04cc/min向催化脱脂炉中通入HNO3气体，脱脂8小时得到脱脂坯；
5)按照6L/min的速率持续通入氢气，氢气气氛下，采用碳管炉烧结步骤4) 得到的脱脂坯，烧结温度以8℃/min从室温升至500℃，保温60min，再以10℃ /min将温度升至1600℃，保温3小时，随炉冷却至室温，得到螺旋型二硅化钼加热棒。
本实施例得到的螺旋型二硅化钼加热棒通过肉眼观察可知其表面光洁、无裂痕，且采用阿基米德排水法测得该螺旋型二硅化钼加热棒的密度为6.16g/cm3，为其理论密度的98.72％，并将该螺旋型二硅化钼加热棒在CMT5305微机控制电子万能试验机上按照标准GB/T 4741-1999的三点弯曲法测得其抗弯强度为 132MPa，最后再采用标准GB/T 7314-2005的气压和水压试验方法测得该螺旋型二硅化钼加热棒的耐压能力可以承受9.6MPa压力而不断裂。
以上所述仅为本发明的优选实施例，并不用于限制本发明，本领域的技术人员在不脱离本发明的精神的前提提下，对本发明进行的改动均落入本发明的保护范围。

Claims (10)

1.一种用于二硅化钼陶瓷制品注射成形的粘结剂，其特征在于，各组分的重量百分含量为：聚乙烯5％、微晶蜡0～3％、硬脂酸2～5％、乙烯-醋酸乙烯酯2～5％，余量为聚甲醛。
2.根据权利要求1所述的粘结剂，其特征在于，各组分的重量百分含量为：聚乙烯5％、微晶蜡3％、硬脂酸2％、乙烯-醋酸乙烯酯5％，余量为聚甲醛。
3.根据权利要求1所述的粘结剂，其特征在于，各组分的重量百分含量为：聚乙烯5％、微晶蜡3％、硬脂酸5％、乙烯-醋酸乙烯酯2％，余量为聚甲醛。
4.根据权利要求1所述的粘结剂，其特征在于，各组分的重量百分含量为：聚乙烯5％、硬脂酸5％、乙烯-醋酸乙烯酯3％，余量为聚甲醛。
5.一种二硅化钼陶瓷制品的注射成形方法，其特征在于，包括以下步骤：
1)将粘结剂中的聚甲醛、聚乙烯、乙烯-醋酸乙烯酯与二硅化钼粉末加入混炼机，温度160℃～180℃下混炼40～60分钟，降温至130℃～150℃，再加入粘结剂中的微晶蜡和硬脂酸，混炼30～40分钟，制得混合物料；
其中，所述二硅化钼粉末与权利要求1所述粘结剂的重量比为22g～30g:100g；
2)将步骤1)得到的混合物料制粒，得到颗粒；
3)步骤2)得到的颗粒在温度160～180℃，压力为50～70MPa，模具温度为100～120℃注射成形得到生坯；
4)将步骤3)得到的生坯利用脱脂温度为110～125℃的催化脱脂炉进行催化脱脂，按0.01～0.05cc/min向催化脱脂炉中通入HNO3气体，脱脂5～8小时得到脱脂坯；
5)氢气气氛下，烧结步骤4)得到的脱脂坯，烧结温度从室温升至500℃，保温30min～60min，再升至1600℃，保温≥3小时，随炉冷却至室温，得到二硅化钼陶瓷制品。
6.根据权利要求5所述的注射成形方法，其特征在于：步骤1)中混炼时采用氩气保护。
7.根据权利要求5所述的注射成形方法，其特征在于：步骤1)中混炼转速为30～60r/min。
8.根据权利要求5所述的注射成形方法，其特征在于：步骤2)中采用挤料机制粒。
9.根据权利要求8所述的注射成形方法，其特征在于：步骤2)中制粒时挤料机的转速为600～800r/min。
10.根据权利要求5所述的注射成形方法，其特征在于：步骤5)中氢气的通入速率为4～7L/min。
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