CN117285361A - 一种基于多相颗粒级配的光固化3d打印氮化硅陶瓷浆料及其打印方法 - Google Patents
一种基于多相颗粒级配的光固化3d打印氮化硅陶瓷浆料及其打印方法 Download PDFInfo
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Abstract
本发明公开了一种基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料及其打印方法,采用粗β相氮化硅粉末和细α相氮化硅粉末进行级配,能够显著降低光固化3D打印氮化硅陶瓷浆料的粘度,提高其固化深度,配置高固相含量的氮化硅陶瓷浆料。有利于打印高精度、无缺陷的氮化硅坯体。进一步的,本发明通过多相颗粒级配灵活调控粉末体系的烧结驱动力和相变机制,结合对烧结温度的合理选择,能够获得高致密、高强度的氮化硅陶瓷。实施例结果表明,本发明制备得到的氮化硅陶瓷致密度94.5%,抗弯强度为472MPa,具有优异的综合性能。
Description
技术领域
本发明属于陶瓷增材制造技术领域,具体涉及到一种基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料及其打印方法。
背景技术
氮化硅陶瓷具有优异的综合性能,包括高机械强度、低热膨胀系数和出色的热稳定性,是极端环境应用中最有前途的先进陶瓷材料之一。在航空航天、工业制造等领域,氮化硅陶瓷得到了广泛的应用。尽管氮化硅具有众多优点,但其高硬度和低韧性使得加工和生产复杂形状的零件具有挑战性。随着光固化成型技术的发展,制备复杂形状的陶瓷结构变得更加容易。
由于α相氮化硅粉末的相变增强机理,传统方法制备氮化硅陶瓷通常使用纳米级的α相氮化硅粉末。然而,使用纳米或亚微米级粉末配置的光固化3D打印浆料往往具有较高的粘度和较低的固化深度,这可能导致打印失败或样品缺陷,影响最终陶瓷制品的性能。此外由于强共价键的存在,较粗的微米级α相氮化硅粉末又难以转化烧结,也会对陶瓷性能产生不利影响。有研究学者通过添加其他陶瓷或表面涂层的方式来提高氮化硅浆料的固化深度,但制备的氮化硅陶瓷强度较差。专利CN202210179265使用高折射率的树脂来配置氮化硅浆料,但仅能小幅度提高浆料的固化深度。
因此,本专利提出了一种基于多相颗粒级配的光固化3D打印制备氮化硅陶瓷的方法。在改善氮化硅浆料性能的同时确保烧结过程中氮化硅粉体的相变机制,制备出高强度的光固化氮化硅陶瓷产品。
发明内容
本部分的目的在于概述本发明的实施例的一些方面以及简要介绍一些较佳实施例。在本部分以及本申请的说明书摘要和发明名称中可能会做些简化或省略以避免使本部分、说明书摘要和发明名称的目的模糊,而这种简化或省略不能用于限制本发明的范围。
鉴于上述和/或现有技术中存在的问题,提出了本发明。
因此,本发明的目的是,克服现有技术中的不足,提供一种基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料。
为解决上述技术问题,本发明提供了如下技术方案:包括,
陶瓷混合粉末、光敏树脂预混液、分散剂、触变剂;
其中,所述陶瓷混合粉末为多相颗粒级配氮化硅粉末与烧结助剂,所述光敏树脂预混液包括光敏树脂单体、预聚物、增塑剂以及光引发剂;
所述多相颗粒级配氮化硅粉末由粒径为3~50μm的粗β相氮化硅粉末和粒径为0.1~3μm的细α相氮化硅粉末级配得到,其中细α相氮化硅粉末的占比为20%~90%。
作为本发明所述基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料的一种优选方案,其中:以质量百分比计,所述陶瓷混合粉末中,多相颗粒级配氮化硅粉末的质量百分比为84~96%,烧结助剂的质量百分比为4%~16%,其中,所述烧结助剂为氧化铝与氧化钇的混合粉末,粒度为0.1~2μm。
作为本发明所述基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料的一种优选方案,其中:所述氧化铝质量为陶瓷混合粉末质量的2~8%,所述氧化钇质量为陶瓷混合粉末质量的2~8%。
作为本发明所述基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料的一种优选方案,其中:所述光敏树脂预混液包括,混合溶液,以及所述混合溶液质量2~5%的光引发剂;
其中,以质量百分比计,所述混合溶液包括,40~100%的光敏树脂单体,0~30%的预聚物、0~30%的增塑剂。
作为本发明所述基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料的一种优选方案,其中:所述光敏树脂单体包括丙烯酰吗啉、环三羟甲基丙烷甲缩醛丙烯酸酯、二乙氧化新二醇二丙烯酸酯、乙氧化三羟甲基丙烷三丙烯酸酯中的一种或多种;
所述预聚物包括环氧丙烯酸酯、聚氨酯丙烯酸酯中的一种或多种;
所述增塑剂包括聚乙二醇、2,2,4-三甲基-1,3-戊二醇二异酸酯和邻苯二甲酸二甲酯中的一种或多种;
所述光引发剂包括2,4,6-三甲基苯甲酰基-二苯基氧化膦。
作为本发明所述基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料的一种优选方案,其中:所述分散剂为SP710,添加量为陶瓷混合粉末的1~4%,所述触变剂为八甲基环四硅氧烷,添加量为陶瓷混合粉末的1~5%。
本发明的另一目的是,提供一种基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料的制备方法,包括,多相颗粒级配氮化硅粉末和烧结助剂混合球磨,得到陶瓷混合粉末;
光敏树脂单体、预聚物、增塑剂形成混合物,再往混合物中加入光引发剂形成预混液;
陶瓷混合粉末、预混液散剂和触变剂混合形成氮化硅陶瓷浆料。
本发明的另一目的是,提供一种光固化3D打印氮化硅陶瓷的方法。
为解决上述技术问题,本发明提供了如下技术方案:包括,
通过光固化打印机打印氮化硅陶瓷浆料,形成氮化硅打印坯体;
依次对打印坯体进行清洗、脱脂、高温烧结处理,得到氮化硅陶瓷。
作为本发明所述基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料的一种优选方案,其中:所述高温烧结为无压烧结或气压烧结,烧结温度为1700~1950℃。
本发明有益效果:
本发明采用粗β相氮化硅粉末和细α相氮化硅粉末进行级配,能够显著降低光固化3D打印氮化硅陶瓷浆料的粘度,提高其固化深度,配置高固相含量的氮化硅陶瓷浆料。有利于打印高精度、无缺陷的氮化硅坯体。进一步的,本发明通过多相颗粒级配灵活调控粉末体系的烧结驱动力和相变机制,结合对烧结温度的合理选择,能够获得高致密、高强度的氮化硅陶瓷。实施例结果表明,本发明制备得到的氮化硅陶瓷致密度94.5%,抗弯强度为472MPa,具有优异的综合性能。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对实施例描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其它的附图。其中:
图1为本发明基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料及其打印方法整体流程示意图。
图2为本发明实施例1中级配得到的陶瓷粉体的SEM图。
图3为本发明实施例1中级配得到的陶瓷粉体的XRD图。
图4为本发明实施例1烧结后的氮化硅陶瓷抛光表面的EBSD形貌图。
图5为实施例1~4以及对比例1~2陶瓷粉末混合后的粒径分布对比
图6为实施例1~4以及对比例1~2烧结得到氮化硅陶瓷的相组成对比图。
图7为实施例1~6不同烧结温度以及不同α-Si3N4粉末含量(Fn)制得氮化硅陶瓷的抗弯强度对比图。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合说明书实施例对本发明的具体实施方式做详细的说明。
在下面的描述中阐述了很多具体细节以便于充分理解本发明,但是本发明还可以采用其他不同于在此描述的其它方式来实施,本领域技术人员可以在不违背本发明内涵的情况下做类似推广,因此本发明不受下面公开的具体实施例的限制。
其次,此处所称的“一个实施例”或“实施例”是指可包含于本发明至少一个实现方式中的特定特征、结构或特性。在本说明书中不同地方出现的“在一个实施例中”并非均指同一个实施例,也不是单独的或选择性的与其他实施例互相排斥的实施例。
本发明中具体实施例中所用原料的英文缩写及全称对应关系如表1所示。
表1
本发明中所用原料无特殊说明均为本领域普通市售。
其中,Si3N4粉末购自中国山东瓷兴新材料有限公司,光敏树脂购自中山市千佑化学材料有限公司,SP710分散剂购自鑫博诚环保材料有限公司,引发剂Irgacure 819购自富斯曼科技(北京)有限公司。
本发明中所用3D打印机为QuickDemos智能制造高科技公司开发的CeraStation1.0陶瓷3D打印机,用于测试的陶瓷打印层厚度为25μm,曝光能量为22mW/cm2,曝光时间为10s。
本发明采用阿基米德排水法测定氮化硅陶瓷的实际密度;相对密度由实际密度与氮化硅陶瓷的理论密度的比值获得。
本发明在加载速度为5mm/min的情况下,进行三点弯曲试验,测定陶瓷的抗弯强度。
实施例1
本实施例提供了一种基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料及其打印方法,具体的:
1)按以下配方称取原料:
陶瓷混合粉末:88%的Si3N4粉末(3μm的β-Si3N4粉末与0.6μm的α-Si3N4粉末质量比为6:4),12%的烧结助剂(5%的Y2O3和7%的Al2O3);
光敏树脂预混液:
混合物:ACMO、DEGDA、TEGTA、EA、TBXI,质量比为2:3:3:2:1;
混合物质量3%的光引发剂Irgacure819;
陶瓷混合粉末与光敏树脂预混液的体积比1:1;
陶瓷混合粉末质量2%的分散剂SP710,陶瓷混合粉末质量3%的触变剂D4;
2)制备氮化硅陶瓷浆料:
陶瓷混合粉末原料混合置于球磨罐中,加入无水乙醇和研磨球,于行星式球磨机中球磨4h,干燥过筛备用;
ACMO、DEGDA、TEGTA、EA、TBXI混合后加入光引发剂Irgacure819,通过磁力搅拌机搅拌形成预混液;
预处理的陶瓷混合粉末和预混液混合,依次加入分散剂、触变剂D4,通过均质机搅拌均匀并真空脱泡后得到氮化硅陶瓷浆料。
图2、图3分别为氮化硅陶瓷粉体的SEM以及XRD图谱,可以看出,3μm的β-Si3N4粉末与0.6μm的α-Si3N4粉末均呈不规则形状,3μm的β-Si3N4物相均为β相,0.6μm的α-Si3N4粉末主要为α相含有少量的β相。
3)进行3D打印:
光固化3D打印氮化硅陶瓷浆料采用光固化3D打印成型得到氮化硅打印坯体,用异丙醇超声清洗3次,每次10min,清洗后采用两步脱脂法对打印坯体进行脱脂,首先在氮气气氛下以1℃/min的升温速率升温至418℃,并在此温度下保温2h,随后以同样升温速率升温至600℃并保温2h;随炉冷却后在氧气气氛下以5℃/min的升温速率升温至600℃并保温4h,以脱去坯体中残余的碳,脱脂完毕后进行高温烧结,烧结温度为1850℃,保温时间为4h,即得到α-Si3N4粉末掺杂量为40%的F40氮化硅陶瓷。
图4为本实施例烧结后的氮化硅陶瓷抛光表面的EBSD形貌,横截面显示出其许多长棒状β晶粒(深色),它们在裂纹偏转、晶粒拉出和桥接中起作用,大大提高了样品的强度。
实施例2
本实施例与实施例1不同之处在于调整Si3N4粉末中3μm的β-Si3N4粉末与0.6μm的α-Si3N4粉末质量比为4:6,其余配方以及工艺参数均与实施例1相同,制得本实施例的F60氮化硅陶瓷。
实施例3
本实施例与实施例1不同之处在于调整Si3N4粉末中3μm的β-Si3N4粉末与0.6μm的α-Si3N4粉末质量比为8:2,其余配方以及工艺参数均与实施例1相同,制得本实施例的F20氮化硅陶瓷。
实施例4
本实施例与实施例1不同之处在于调整Si3N4粉末中3μm的β-Si3N4粉末与0.6μm的α-Si3N4粉末质量比为2:8,其余配方以及工艺参数均与实施例1相同,制得本实施例的F80氮化硅陶瓷。
对比例1
本对比例与实施例1不同之处在于调整Si3N4粉末仅为0.6μm的α-Si3N4粉末,其余配方以及工艺参数均与实施例1相同,制得本对比例的F100氮化硅陶瓷。
对比例2
本对比例与实施例1不同之处在于调整Si3N4粉末仅为3μm的β-Si3N4粉末,其余配方以及工艺参数均与实施例1相同,制得本对比例的F0氮化硅陶瓷。图5为实施例1~4以及对比例1~2陶瓷粉末混合后的粒径分布对比,可以看到通过多项颗粒级配混合的粉末呈双峰分布,在此基础上才能制备出粘度低、稳定性好、固化深度高的浆料,有利于后续打印出层间结合良好、缺陷少的坯体。
图6为实施例1~4以及对比例1~2烧结得到氮化硅陶瓷的相组成对比,可以看出,烧结后试样的主要晶相为β-Si3N4相,表明发生了α-Si3N4相的相变,当0.6μm的α-Si3N4粉末含量小于40%时,α相完全转化为β相,而当0.6μm的α-Si3N4粉末含量大于40%时,仍有小部分α相未转化,测定各氮化硅陶瓷的x相对密度以及抗弯曲强度,结果如表2所示。
表2不同α-Si3N4粉末含量的陶瓷浆料及氮化硅陶瓷性能对比
从表2可以看出,Si3N4粉末中α-Si3N4粉末与β-Si3N4粉末的掺杂比例或含量对制备的Si3N4陶瓷的强度有重要影响,这是由于本发明精心设计的多相粒度级配策略,一方面优化了浆料性能,大大避免了坯体打印过程中可能引入的缺陷,另一方面,通过灵活调控粉末体系的烧结驱动力和相变机制,有利于通过光固化3D打印制备出高强度氮化硅陶瓷。
实施例5
本实施例用以探究当烧结温度为1750℃时,不同0.6μm的α-Si3N4粉末含量制得氮化硅陶瓷的性能,与实施例1不同之处在于,调整烧结温度为1750℃,调整0.6μm的α-Si3N4粉末含量分别为0%、20%、40%、60%、80%、100%,其余工艺步骤及参数均与实施例1相同,制得本实施例不同α-Si3N4粉末含量的氮化硅陶瓷。
实施例6
本实施例与实施例5不同之处在于,调整烧结温度为1950℃,其余工艺参数均与实施例5相同,制得本实施例不同0.6μm的α-Si3N4粉末含量的氮化硅陶瓷。
对比实施例1~6不同烧结温度以及不同0.6μm的α-Si3N4粉末含量制得氮化硅陶瓷的抗弯强度,结果如图7所示。
从图中可以看出,在1750℃时,由于小晶粒的细晶强化作用和α相的转变作用,随着0.6μm的α-Si3N4含量的增加,抗弯强度增加,有利于强度的提高,而当烧结温度达到1950℃时,随着0.6μm的α-Si3N4含量的增加,试样的抗弯强度反而降低,这主要是由于烧结颈搭接形成较大孔隙的试样相对密度降低,从而导致强度降低,而烧结温度为1850℃时,F40含量为40%的样品的最大抗弯强度为472.08MPa,显著高于其他样品。
综上,本发明采用粗β相氮化硅粉末和细α相氮化硅粉末进行级配,能够显著降低光固化3D打印氮化硅陶瓷浆料的粘度,提高其固化深度,配置高固相含量的氮化硅陶瓷浆料。有利于打印高精度、无缺陷的氮化硅坯体。进一步的,本发明通过多相颗粒级配灵活调控粉末体系的烧结驱动力和相变机制,结合对烧结温度的合理选择,能够获得高致密、高强度的氮化硅陶瓷。实施例结果表明,本发明制备得到的氮化硅陶瓷致密度94.5%,抗弯强度为472MPa,具有优异的综合性能。
应说明的是,以上实施例仅用以说明本发明的技术方案而非限制,尽管参照较佳实施例对本发明进行了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,其均应涵盖在本发明的权利要求范围当中。
Claims (10)
1.一种基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料,其特征在于:包括,陶瓷混合粉末、光敏树脂预混液、分散剂、触变剂;
其中,所述陶瓷混合粉末为多相颗粒级配氮化硅粉末与烧结助剂,所述光敏树脂预混液包括光敏树脂单体、预聚物、增塑剂以及光引发剂;
所述多相颗粒级配氮化硅粉末由粒径为3~50μm的粗β相氮化硅粉末和粒径为0.1~3μm的细α相氮化硅粉末级配得到,其中,细α相氮化硅粉末的占比为20%~90%。
2.如权利要求1所述的基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料,其特征在于:以质量百分比计,所述陶瓷混合粉末中,多相颗粒级配氮化硅粉末的质量百分比为84~96%,烧结助剂的质量百分比为4%~16%,其中,所述烧结助剂为氧化铝与氧化钇的混合粉末,粒度为0.1~2μm。
3.如权利要求2所述的基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料,其特征在于:所述氧化铝质量为陶瓷混合粉末质量的2~8%,所述氧化钇质量为陶瓷混合粉末质量的2~8%。
4.如权利要求1所述的基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料,其特征在于:所述光敏树脂预混液包括,混合溶液,以及所述混合溶液质量2~5%的光引发剂;
其中,以质量百分比计,所述混合溶液包括,40~100%的光敏树脂单体,0~30%的预聚物、0~30%的增塑剂。
5.如权利要求4所述的基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料,其特征在于:所述光敏树脂单体包括丙烯酰吗啉、环三羟甲基丙烷甲缩醛丙烯酸酯、二乙氧化新二醇二丙烯酸酯、乙氧化三羟甲基丙烷三丙烯酸酯中的一种或多种;
所述预聚物包括环氧丙烯酸酯、聚氨酯丙烯酸酯中的一种或多种;
所述增塑剂包括聚乙二醇、2,2,4-三甲基-1,3-戊二醇二异酸酯和邻苯二甲酸二甲酯中的一种或多种;
所述光引发剂包括2,4,6-三甲基苯甲酰基-二苯基氧化膦。
6.如权利要求1所述的基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料,其特征在于:所述分散剂为SP710,添加量为陶瓷混合粉末的1~4%,所述触变剂为八甲基环四硅氧烷,添加量为陶瓷混合粉末的1~5%。
7.如权利要求1所述的基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料,其特征在于:所述浆料的固含量为40~60vol%。
8.如权利要求1~7任一所述的基于多相颗粒级配的光固化3D打印氮化硅陶瓷浆料的制备方法,其特征在于:包括,
多相颗粒级配氮化硅粉末和烧结助剂混合球磨,得到陶瓷混合粉末;
光敏树脂单体、预聚物、增塑剂形成混合物,再往混合物中加入光引发剂形成预混液;
陶瓷混合粉末、预混液散剂和触变剂混合形成氮化硅陶瓷浆料。
9.一种应用如权利要求1~7任一所述浆料进行光固化3D打印氮化硅陶瓷的方法,其特征在于:包括,
通过光固化打印机打印氮化硅陶瓷浆料,形成氮化硅打印坯体;
依次对打印坯体进行清洗、脱脂、高温烧结处理,得到氮化硅陶瓷。
10.如权利要求9所述光固化3D打印氮化硅陶瓷的方法,其特征在于:所述高温烧结为无压烧结或气压烧结,烧结温度为1700~1950℃,保温时间为3~5h。
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5026671A (en) * | 1989-03-17 | 1991-06-25 | Ngk Insulators, Ltd. | Sintered silicon nitride and method for making the same |
CN107158474A (zh) * | 2017-05-26 | 2017-09-15 | 山东工业陶瓷研究设计院有限公司 | 光固化3d打印牙科种植体用浆料及其制备方法和应用 |
CN113511901A (zh) * | 2021-04-21 | 2021-10-19 | 广东工业大学 | 一种光固化成型的高固相含量氮化硅陶瓷及其制备方法和应用 |
CN113860880A (zh) * | 2021-09-03 | 2021-12-31 | 萍乡旭材科技有限公司 | 一种具有良好固化性能的氮化硅陶瓷浆料 |
CN115536401A (zh) * | 2022-10-31 | 2022-12-30 | 华中科技大学 | 一种基于放电等离子烧结的光固化成形陶瓷及其制备方法 |
CN116535220A (zh) * | 2023-05-29 | 2023-08-04 | 共享智能装备有限公司 | 一种氮化硅陶瓷粉末制品的脱脂烧结方法 |
-
2023
- 2023-08-07 CN CN202310982614.3A patent/CN117285361A/zh active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5026671A (en) * | 1989-03-17 | 1991-06-25 | Ngk Insulators, Ltd. | Sintered silicon nitride and method for making the same |
CN107158474A (zh) * | 2017-05-26 | 2017-09-15 | 山东工业陶瓷研究设计院有限公司 | 光固化3d打印牙科种植体用浆料及其制备方法和应用 |
CN113511901A (zh) * | 2021-04-21 | 2021-10-19 | 广东工业大学 | 一种光固化成型的高固相含量氮化硅陶瓷及其制备方法和应用 |
CN113860880A (zh) * | 2021-09-03 | 2021-12-31 | 萍乡旭材科技有限公司 | 一种具有良好固化性能的氮化硅陶瓷浆料 |
CN115536401A (zh) * | 2022-10-31 | 2022-12-30 | 华中科技大学 | 一种基于放电等离子烧结的光固化成形陶瓷及其制备方法 |
CN116535220A (zh) * | 2023-05-29 | 2023-08-04 | 共享智能装备有限公司 | 一种氮化硅陶瓷粉末制品的脱脂烧结方法 |
Non-Patent Citations (1)
Title |
---|
李荐等: "β-Si3 N4含量对Y2O3-MgO-α-Si3N4陶瓷性能的影响", 矿冶工程, pages 91 - 93 * |
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