CN115353371A - 一种用于大尺寸厚壁注射成型的zta陶瓷粉体催化脱脂型注射喂料及其制备方法 - Google Patents
一种用于大尺寸厚壁注射成型的zta陶瓷粉体催化脱脂型注射喂料及其制备方法 Download PDFInfo
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Abstract
本发明属于陶瓷粉体注射成型领域，具体公开了一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料及其制备方法,所述注射喂料按质量百分比计算，由以下成分组成：ZTA陶瓷粉体75‑78%，粘结剂22‑25%；其中粘结剂中各组分的占比为：POM 78‑85%；骨架组分4.5‑6%，抗氧化剂2.5‑5%；超分散剂3‑5%；润滑剂1‑4%。根据本发明所述的配方和制备方法，能够制备出流动性好，性能稳定的ZTA陶瓷喂料，用于成型大尺寸厚壁复杂形状产品如分血阀片，且催化脱脂效率高，脱脂无开裂等不良，烧结后产品的密度高，均一稳定，可应用高质量要求的精密零部件生产，如分血阀片等，具有很大的经济效益。
Description
技术领域
本发明属于陶瓷粉体注射成型领域，具体公开了一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料及其制备方法。
背景技术
粉末注射成型是行业内一直在研究的一种粉体成型方式，它可以补充目前粉末常规的干压成型，等静压成型方式，制作更为复杂，异形的产品，因此行业内普遍存在这种工艺，但这种工艺的重点是形成粘结性及流动性良好的喂料，通过注射成型后，能够顺利排出添加在喂料中占比20%左右的有机粘结剂，使陶瓷顺利烧结成瓷，不发生开裂，变形等不良缺陷，目前从粘结剂排出方式去划分，主要由溶剂脱脂型（蜡基）、催化脱脂型（POM基，直接热脱脂型（塑基）三种常规配方体系，蜡基由于配方中含有50-70%的石蜡成分，坯体强度较差，且需采用大量有机溶剂，环保要求高；而直接热脱脂型配方体系的脱脂效率慢，只适合做小型薄壁型产品，且热脱脂工艺与产品的形态，大小，脱脂炉等都有强关联，不适用于多品种产品的开发。
针对POM基催化脱脂配方体系，目前行业内并没有完全成熟的配方体系，可以广泛应用于多形态、高精密、高质量要求的产品上。主要是有多方面的问题存在：1、喂料的流动性差，注射时易冷出现流纹分层等缺陷，并针对不同的产品会有不同缺陷出现；2、喂料中粘结剂之间以及与纳米陶瓷粉的相容性差，导致注射后坯体强度低，易出现隐裂等显微缺陷；3、烧结后的制品密度低，普遍比干压成型、等静压成型的密度低、强度差，这个是主要的因素。因此陶瓷粉体注射成型的方式到目前为止并没有像干压成型、等静压成型那样有广泛的应用。
ZTA陶瓷，即氧化锆增韧氧化铝陶瓷，因为氧化锆在氧化铝中的增韧作用，使其具有比氧化铝陶瓷更好的强度和韧性，在表面质量要求高的医疗行业有广泛的应用，如分血阀片，这种形状复杂的陶瓷产品只能采用陶瓷注射成型的方式实现批量化生产，目前市面上采用溶剂脱脂型ZTA注射喂料开发此类产品，但由于此类产品的壁厚在7mm以上，采用溶剂脱脂在过程工艺及最终产品尺寸及性能上均存在众多问题：首先，大尺寸产品，蜡基喂料存在充模冷却后严重缩水问题，缩水凹坑深度可达1mm，在产品烧结后表面形成缩水凹坑；且7mm壁厚产品相较5mm以下注塑件需要经过更长时间的浸泡溶剂（30h，一般5mm左右厚度只需浸泡12h左右）才能排除石蜡，长时间的溶剂浸泡，其中的粘结剂高分子更容易发生较大溶胀，使坯体强度降低，在熔接线位置极易产生开裂，同时伴随变形缺陷产生，经过初步的小批量试验，基本在经过溶剂脱脂后，注射坯的良率就在20%以下。因此采用蜡基喂料基本很难实现量产。
发明内容
为了解决上述问题，本发明公开了一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料及其制备方法。
本发明的技术方案如下：
一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料，按质量百分比计算，由以下成分组成：ZTA陶瓷粉体75-78%，粘结剂22-25%；
其中粘结剂中各组分的占比为：POM 78-85%；骨架组分4.5-6%，抗氧化剂2.5-5%；超分散剂3-5%；润滑剂1-4%。
进一步的，上述一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料，所述ZTA陶瓷粉体的中位径粒度≥0.8μm。
进一步的，上述一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料，所述骨架组分为高强度的高分子树脂，拉伸屈服强度≥15MPa，熔融指数在10-15g/10min。
进一步的，上述一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料，所述骨架组分选自PP，PE，PET中的至少一种。
进一步的，上述一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料，所述润滑剂为酰胺类润滑物质。
进一步的，上述一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料，所述超分散剂为具有酯基的环状极性化合物。
进一步的，上述一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料的制备方法，包括以下步骤：首先预热粉体及密炼机混合腔，温度在120~150℃之间，加入陶瓷粉与超分散剂，混合使之充分混匀，后加入POM，骨架组分，抗氧化剂，润滑剂，在185~195℃下混炼后即可卸料冷却进行造粒，造粒后即成为喂料。
进一步的，上述一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料的制备方法，所述混合时间为10-30min，所述蜜炼时间为30-50min。
进一步的，上述一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料的注射方法，包括以下步骤：采用高压低速，高模温；催化脱脂采用草酸蒸汽作为催化剂，温度为120~140℃，脱脂后进入烧结工序，烧结成瓷。
进一步的，上述一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料的应用，应用于分血阀片的制备。
本发明具有如下有益效果:本发明公开了一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料及其制备方法。所述喂料的配方，是为了满足ZTA粉料，在壁厚＞7mm的大壁厚复杂结构件的批量生产需求，突破目前的配方应用瓶颈。现有技术方面有以下两点重大不同，一是应用粉料发生改变，ZTA粉区别于氧化铝粉，需采用更高效的分散剂；二是7mm以上壁厚产品的主要问题POM脱出率低可以通过增大POM比例得以改善，但POM比例增加意味着其他分散剂，粘结剂的减少，喂料的流动性以及催化脱脂后生坯的强度会降低，带来其他缺陷，基于此，改良配方优选了强度更好的粘结剂，来克服POM比例变化带来的其他影响。同时，POM为共聚甲醛，具有较好的温度稳定性，熔融指数为120g/10min，流动性高，润滑剂选择酰胺类润滑物质，对POM及HDPE均有极佳的内润滑剂外润滑效果；超分散剂为具有酯基的环状极性化合物，可以与粉体形成强吸附作用，增强粉体在有机物中的分散，同时保持分散后的稳定性，避免喂料注射时在强冲击或摩擦力作用下分层。
本发明涉及的配方体系，能够制备出流动性好，性能稳定的ZTA陶瓷喂料，用于成型大尺寸厚壁复杂形状产品，且催化脱脂效率高，无污染，脱脂无开裂等不良，烧结后产品的密度高，烧结后的瓷体各位置透光度高，均透度均一，密度能达到4.23g/cm3，抛光后表面光洁度高，无不良缺陷，可应用高质量要求的精密零部件生产，如分血阀片等，具有很大的经济效益。
具体实施方式
一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料，按质量百分比计算，由以下成分组成：ZTA陶瓷粉体75-78%，粘结剂22-25%；
其中粘结剂中各组分的占比为：POM 78-85%；骨架组分4.5-6%，抗氧化剂2.5-5%；超分散剂3-5%；润滑剂1-4%；
所述ZTA陶瓷粉体的中位径粒度≥0.8μm；
所述骨架组分为高强度的高分子树脂，拉伸屈服强度≥15MPa，熔融指数在10-15g/10min；
所述骨架组分选自PP，PE，PET中的至少一种；
所述润滑剂为酰胺类润滑物质；
所述超分散剂为具有酯基的环状极性化合物；
上述用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料的制备方法，包括以下步骤：首先预热粉体及密炼机混合腔，温度在120~150℃之间，加入陶瓷粉与超分散剂，混合使之充分混匀，后加入POM，骨架组分，抗氧化剂，润滑剂，在185~195℃下混炼后即可卸料冷却进行造粒，造粒后即成为喂料；
所述混合时间为10-30min，所述蜜炼时间为30-50min；
上述用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料的注射方法，包括以下步骤：采用高压低速，高模温；催化脱脂采用草酸蒸汽作为催化剂，温度为120~140℃，脱脂后进入烧结工序，烧结成瓷。
上述用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料应用于分血阀片的制备。
下面对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
本发明实施例中使用的试剂或仪器未注明生产厂商者，均为可以通过市购获得的常规试剂产品。
实施例1
中位径1.6μm的ZTA粉质量比为：75%，粘结剂占比为25%；粘结剂中，POM占比为85%，PET占比为5%，抗氧化剂为4.5%，润滑剂为4%，超分散剂为4.5%；在195℃进行密炼40min，催化脱脂温度为130℃，脱脂时间为20h，POM脱除率为95%以上；在1600℃下保温2h烧结得到的氧化铝陶瓷制品的密度为4.23g/cm3；抛光后表面光洁度≤0.05μm，满足客户对外观质感的要求。
实施例2
中位径1.6μm的ZTA粉质量比为：78%，粘结剂占比为22%；粘结剂中，POM占比为78%，HDPE占比为6%，抗氧化剂为6%，润滑剂为5%，超分散剂为5%；在195℃进行密炼40min，催化脱脂温度为130℃，脱脂时间为20h，POM脱除率为95%以上；在1600℃下保温2h烧结得到的氧化铝陶瓷制品的密度为4.23g/cm3；抛光后表面光洁度≤0.05μm，满足客户对外观质感的要求。
实施例3
中位径0.8μm的氧化铝粉质量比为：78%，粘结剂占比为23%；粘结剂中，POM占比为80%，HDPE占比为5%，抗氧化剂为5%，润滑剂为4%，超分散剂为6%；在185℃进行密炼40min，催化脱脂温度为130℃，脱脂时间为20h，POM脱除率为95%以上；在1600℃下保温2h烧结得到的氧化铝陶瓷制品的密度为4.23g/cm3；抛光后表面光洁度≤0.05μm，满足客户对外观质感的要求。
对比例1
中位径1.6μm的氧化铝粉质量比为：79%，粘结剂占比为21%；粘结剂中，POM占比为75%，HDPE占比为6%，抗氧化剂为8%，润滑剂为5%，超分散剂为6%；在185℃进行密炼40min，催化脱脂温度为130℃，脱脂时间为20h，POM脱除率只有85%，产品较厚区域仍有3mm厚度的未催化脱脂层，这在后续排胶过程中使坯体开裂。
对比例2
中位径1.6μm的氧化铝粉质量比为：74%，粘结剂占比为26%；粘结剂中，POM占比为85%，HDPE占比为4.5%，抗氧化剂为3%，润滑剂为3%，分散剂占比4.5%；在185℃进行密炼40min，催化脱脂温度为130℃，脱脂时间为20h，POM脱除率为95%以上；但催化脱脂后的坯体强度差，局部有裂纹，无法满足批量生产。
以上所述实施例仅表达了本发明的有限几种优选实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。
Claims (10)
1.一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料，其特征在于，按质量百分比计算，由以下成分组成：ZTA陶瓷粉体75-78%，粘结剂22-25%；
其中粘结剂中各组分的占比为：POM 78-85%；骨架组分4.5-6%，抗氧化剂2.5-5%；超分散剂3-5%；润滑剂1-4%。
2.根据权利要求1所述的一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料，其特征在于，所述ZTA陶瓷粉体的中位径粒度≥0.8μm。
3.根据权利要求1所述的一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料，其特征在于，所述骨架组分为高强度的高分子树脂，拉伸屈服强度≥15MPa，熔融指数在10-15g/10min。
4.根据权利要求3所述的一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料，其特征在于，所述骨架组分选自PP，PE，PET中的至少一种。
5.根据权利要求1所述的一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料，其特征在于，所述润滑剂为酰胺类润滑物质。
6.根据权利要求1所述的一种用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料，其特征在于，所述超分散剂为具有酯基的环状极性化合物。
7.如权利要求1-6任一项所述的用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料的制备方法，其特征在于，包括以下步骤：首先预热粉体及密炼机混合腔，温度在120~150℃之间，加入陶瓷粉与超分散剂，混合使之充分混匀，后加入POM，骨架组分，抗氧化剂，润滑剂，在185~195℃下混炼后即可卸料冷却进行造粒，造粒后即成为喂料。
8.根据权利要求7所述的制备方法，其特征在于，所述混合时间为10-30min，所述蜜炼时间为30-50min。
9.如权利要求1-6任一项所述的用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料的注射方法，其特征在于，包括以下步骤：采用高压低速，高模温；催化脱脂采用草酸蒸汽作为催化剂，温度为120~140℃，脱脂后进入烧结工序，烧结成瓷。
10.如权利要求1-6任一项所述的用于大尺寸厚壁注射成型的ZTA陶瓷粉体催化脱脂型注射喂料的应用，其特征在于，应用于分血阀片的制备。
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