CN110467475A - 一种梯度功能陶瓷的制备方法 - Google Patents
一种梯度功能陶瓷的制备方法 Download PDFInfo
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Abstract
本发明涉及陶瓷制备技术领域,尤其涉及一种梯度功能陶瓷的制备方法。本发明通过优化浆料及3D打印的工艺参数,尤其是优化浆料中陶瓷复合粉体中的烧结添加剂及3D打印的曝光能量,根据不同的浆料采用相应的曝光能量打印坯体,由3D打印所得坯体均匀且成型率高,由所述坯体在一定条件下脱脂烧结形成的陶瓷其变形性小,结构及尺寸精度高,层间粘结性好,密度和抗弯强度高。通过本发明方法制备的梯度功能陶瓷不仅成型效率高,成型尺寸精度高,而且结构可精确调控,实现功能化,并且可降低材料成本,提高生产效率。
Description
技术领域
本发明涉及陶瓷制备技术领域,尤其涉及一种梯度功能陶瓷的制备方法。
背景技术
梯度功能陶瓷是由两种或两种以上材料复合且成分和结构呈梯度变化的一种复合材料。与传统复合材料相比,其具有减小界面残余应力和热应力,提高粘结强度,实现不同空间上的功能化的特点。目前制造这种梯度陶瓷部件的成型方法包括冷自蔓延高温合成法、干压成型、颗粒共沉降和激光加热合成等方法。干压成型的方法效率较高,但存在显微结构不均匀的问题,同时不易成型复杂形状和异形产品;自蔓延高温合成法制备金属-陶瓷复合材料存在合成产物孔隙率大,反应过程速度快、温度高、内应力大,致使陶瓷相的大小和形貌难以控制等不足的问题。颗粒共沉降法制备FGM具有设备简单、操作简便、得到的梯度材料成分渐变性更好等许多特点,但其难以应用化。
光固化成型技术(3D打印技术),其原理是通过计算机控制特定波长与强度的光束在x-y面进行扫描,使陶瓷浆料选择性固化,完成一个层面的绘图作业,然后升降台在垂直方向移动一个层片的高度,再固化另一个层面,如此循环构成一个陶瓷坯体。由以上可知,光固化成型技术打印的坯体是通过层层累加而成,这对制备梯度功能材料层内层间结构设计提供了巨大优势,有望拓展梯度功能陶瓷的应用领域。
发明内容
本发明针对现有技术制备梯度功能陶瓷存在坯体不均匀,成型效率低及加工成本高的问题,提供一种高效制备梯度功能陶瓷的方法,坯体均匀,层间结合性好,可制备高精度形状复杂的梯度功能陶瓷。
为实现上述目的,本发明采用以下技术方案。
一种梯度功能陶瓷的制备方法,浆料通过3D打印形成坯体,3D打印使用的模型为具有不同陶瓷层结构的梯度结构模型;所述的制备方法包括以下步骤:
S1制备陶瓷复合粉体:根据梯度结构模型分别配制用于3D打印对应陶瓷层的陶瓷复合粉体,与各陶瓷层对应的陶瓷复合粉体按以下重量份将各组分混合均匀制得:10-30份的陶瓷粉体、0-15份的烧结添加剂、0-15份的造孔剂。
优选的,所述陶瓷粉体选自氧化铝、氧化锆、氧化镁、氧化钇、氮化硅、碳化硅、氮化硼中的至少一种。
优选的,所述烧结添加剂选自碳纳米管、石墨烯、Re2O3中的至少一种,其中Re为Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。
优选的,所述造孔剂选自淀粉、酚醛树脂、尼龙纤维中的至少一种。
优选的,所述溶剂选自去离子水、无水乙醇、丙酮中的至少一种。
S2制备浆料:根据梯度结构模型分别配制用于3D打印对应陶瓷层的浆料,与各陶瓷层对应的浆料按以下重量份将各组分混合均匀制得:100-120份的陶瓷复合粉体,90-110份的光敏树脂,0.1-5份的光引发剂,0.1-5份的分散剂。
优选的,所述光敏树脂选自1,6-乙二醇二丙烯酸酯、三羟甲基丙烷三丙烯酸酯和聚氨酯丙烯酸酯中的至少一种。
优选的,所述光引发剂选自2-羟基-2-甲基-1-苯基-1-丙酮、苯基双(2,4,6-三甲基苯甲酰基)氧化膦、1-羟基环已基苯基酮中的至少一种。
优选的,所述分散剂为硅烷偶联剂KH560、油酸、铝酸酯中的至少一种。
S3成型:按照梯度结构模型,将与陶瓷层对应的浆料置于3D打印设备的打印料槽中,进行逐层打印,制得坯体。
S4脱脂烧结:先以0.1-5℃/min的速率升温至300-800℃并保温2-4h,对坯体进行脱脂处理;然后坯体在空气、氮气气氛或者真空下,以5-20℃/min的速率升温至1300-1850℃并保温1-4h,制得梯度功能陶瓷。
进一步地,经步骤S4烧结制备的梯度功能陶瓷中各陶瓷层的孔隙率小于或等于50vol%。
优选的,以上所述的梯度功能陶瓷的制备方法,步骤S1中所述陶瓷粉体中的氮化硅含量小于10%,所述烧结添加剂选自Re2O3中的至少一种,其中Re为Y、Sc、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu时,步骤S3中进行3D打印的曝光能量设置如下:所述陶瓷复合粉体中烧结添加剂的含量为陶瓷粉体的10wt%以内时,曝光能量E为40mJ/cm2≤E<80mJ/cm2。
优选的,以上所述的梯度功能陶瓷的制备方法,步骤S1中所述陶瓷粉体中的氮化硅含量大于或等于90%,所述烧结添加剂选自Re2O3中的至少一种,其中Re为Y、Sc、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu,所述陶瓷复合粉体中烧结添加剂的含量为陶瓷粉体的5wt%以内时,步骤S3中进行3D打印的曝光能量E为100mJ/cm2≤E≤120mJ/cm2;更优选的,步骤S1中所述陶瓷粉体由氮化硅和氧化铝组成。
优选的,以上所述的梯度功能陶瓷的制备方法,步骤S1中所述陶瓷粉体中的氮化硅含量大于或等于90%,所述烧结添加剂由石墨烯或碳纳米管与Y2O3组成,所述陶瓷复合粉体中烧结添加剂的含量为陶瓷粉体的1-5wt%时,步骤S3中进行3D打印的曝光能量E为140mJ/cm2≤E≤200mJ/cm2;更优选的,步骤S1中所述陶瓷粉体由氮化硅和氧化铝组成。
与现有技术相比,本发明的有益效果是:
本发明通过优化浆料及3D打印的工艺参数,尤其是优化浆料中陶瓷复合粉体中的烧结添加剂及3D打印的曝光能量,根据不同的浆料采用相应的曝光能量打印坯体,由3D打印所得坯体均匀且成型率高,由所述坯体在一定条件下脱脂烧结形成的陶瓷其变形性小,结构及尺寸精度高,层间粘结性好,密度和抗弯强度高。通过本发明方法制备的梯度功能陶瓷不仅成型效率高,成型尺寸精度高,而且结构可精确调控,实现功能化,并且可降低材料成本,提高生产效率。
附图说明
图1为实施例1制备的梯度功能陶瓷的第1-5层的SEM图。
具体实施方式
为了更充分的理解本发明的技术内容,下面结合具体实施例对本发明的技术方案作进一步介绍和说明。
实施例1
本实施例提供一种由八层结构为一层叠结构单元的梯度功能陶瓷及其制备方法。具体制备步骤如下:
(1)制备陶瓷复合粉体:根据梯度结构模型分别制备用于3D打印对应陶瓷层的浆料中的陶瓷复合粉体。以无水乙醇为溶剂,将组成陶瓷复合粉体的各组分按照比例加入无水乙醇中,超声分散10min,然后球磨12h,球磨转速为250r/min,使得各组分充分混合。将超声后的混合物倒入旋转蒸发仪中,并在60℃下蒸发溶剂,再经过100目筛,得到陶瓷复合粉体。
用于制备层叠结构单元中各层陶瓷的陶瓷复合粉体的组成如下:
第一层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3;
第二层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,1gLa2O3;
第三层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,3gLa2O3;
第四层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,5gLa2O3;
第五层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,10gLa2O3;
第六层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,10gLa2O3,1g尼龙纤维;
第七层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,10gLa2O3,5g尼龙纤维;
第八层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,10gLa2O3,10g尼龙纤维。
(2)制备浆料:将步骤(1)制备的用于各陶瓷层的陶瓷复合粉体按配比与光敏树脂、光引发剂和分散剂混合均匀,分别制得用于制备各陶瓷层的浆料。具体为是将50g 1,6-乙二醇二丙烯酸酯和50g三羟甲基丙烷三丙烯酸酯均匀混合形成树脂预混液,然后将各陶瓷层的陶瓷复合粉体分别与树脂预混液混合,控制混合物的固含量均为50vol%。接着再加入5g油酸,球磨2h使各组分分散均匀,转速350r/min,再接着继续添加1g 2-羟基-2-甲基-1-苯基-1-丙酮,继续球磨30min,制得八种浆料。
(3)成型
按照梯度结构模型,将与陶瓷层对应的浆料置于3D打印设备的打印料槽中,进行逐层打印,制得坯体。
坯体的层叠结构单元中各浆料层的曝光能量分别如下:用第一至第五层的浆料打印对应的层时的曝光能量是40mJ/cm2,用第六至第八层的浆料打印对应的层时的曝光能量是60mJ/cm2,并将1-8层的打印层厚度均设置为20μm,每层的每种浆料只打印一次。重复上述层叠结构单元的打印,打印由10个层叠结构单元叠加构成的坯体。
(4)脱脂:将坯体置于空气气氛脱脂炉内,以2℃/min的速率升温至650℃并保温4h。
(5)烧结:将坯体置于空气气氛下烧结,以10℃/min的速率升温至1500℃并保温2h,制得具有八层结构的梯度功能陶瓷。
本实施例制备的梯度功能陶瓷,每一层叠结构单元的表层致密,内层多孔,层叠结构单元的整体孔隙率为25%;通过扫描电子显微镜观察陶瓷的截面,各陶瓷层间结合良好,层与层间无裂纹;如图1所示为梯度功能陶瓷的层叠结构单元中第1-5层的SEM图,相邻的上下两层陶瓷结合良好;陶瓷性能良好,其抗弯强度为150MPa。
实施例2
本实施例提供一种六层结构的梯度功能陶瓷及其制备方法。具体制备步骤如下:
(1)制备陶瓷复合粉体:根据梯度结构模型分别制备用于3D打印对应陶瓷层的浆料中的陶瓷复合粉体。以无水乙醇为溶剂,将组成陶瓷复合粉体的各组分按照比例加入无水乙醇中,超声分散10min,然后球磨12h,球磨转速为250r/min,使得各组分充分混合。将超声后的混合物倒入旋转蒸发仪中,并在60℃下蒸发溶剂,再经过100目筛,得到陶瓷复合粉体。
用于制备各层陶瓷的陶瓷复合粉体的组成如下:
第一层陶瓷的陶瓷复合粉体:90g Si3N4,5g Al2O3,5g Y2O3;
第二层陶瓷的陶瓷复合粉体:90g Si3N4,5g Al2O3,5g β-Si3N4,5g Y2O3;
第三层陶瓷的陶瓷复合粉体:90g Si3N4,5g Al2O3,5g β-Si3N4,5g Y2O3;1g石墨烯;
第四层陶瓷的陶瓷复合粉体:90g Si3N4,5gAl2O3,5g β-Si3N4,5gY2O3;2g石墨烯;
第五层陶瓷的陶瓷复合粉体:90g Si3N4,5g Al2O3,5g β-Si3N4,5g Y2O3;3g石墨烯;
第六层陶瓷的陶瓷复合粉体:90g Si3N4,5g Al2O3,5g β-Si3N4,5g Y2O3;5g石墨烯。
(2)制备浆料:将步骤(1)制备的用于各陶瓷层的陶瓷复合粉体按配比与光敏树脂、光引发剂和分散剂混合均匀,分别制得用于制备各陶瓷层的浆料。具体为是将50g1,6-乙二醇二丙烯酸酯和50g三羟甲基丙烷三丙烯酸酯均匀混合形成树脂预混液,然后将各陶瓷层的陶瓷复合粉体分别与树脂预混液混合,控制混合物的固含量均为40vol%。接着再加入5g铝酸酯,球磨2h使各组分分散均匀,转速350r/min,再接着继续添加1g苯基双(2,4,6-三甲基苯甲酰基)氧化膦,继续球磨30min,制得六种浆料。
(3)成型
按照梯度结构模型,将与陶瓷层对应的浆料置于3D打印设备的打印料槽中,进行逐层打印,制得坯体。
坯体的中各浆料层的曝光能量分别如下:用第一至第六层的浆料打印对应的层时的曝光能量分别是100mJ/cm2,120mJ/cm2,140mJ/cm2,160mJ/cm2,180mJ/cm2,200mJ/cm2,将1-2层的打印层厚度均设置为50μm,将3-6层的打印层厚度均设置为20μm,坯体中每层浆料的总厚度均为500μm。
(4)脱脂:将坯体置于真空气氛脱脂炉内,以3℃/min的速率升温至750℃并保温3h。
(5)烧结:将坯体置于氮气气氛下烧结,以20℃/min的速率升温至1200℃,然后以10℃/min升温至1800℃并保温2h,制得具有六层结构的梯度功能陶瓷。
本实施例制备的梯度功能陶瓷表层致密,内层多孔,层叠结构单元的整体孔隙率为20%;通过扫描电子显微镜观察陶瓷的截面,各陶瓷层间结合良好,层与层间无裂纹;陶瓷性能良好,其抗弯强度为300MPa。
实施例3
本实施例提供一种十层结构的梯度功能陶瓷及其制备方法。具体制备步骤如下:
(1)制备陶瓷复合粉体:根据梯度结构模型分别制备用于3D打印对应陶瓷层的浆料中的陶瓷复合粉体。以丙酮为溶剂,将组成陶瓷复合粉体的各组分按照比例加入丙酮中,超声分散10min,然后球磨12h,球磨转速为250r/min,使得各组分充分混合。将超声后的混合物倒入旋转蒸发仪中,并在60℃下蒸发溶剂,再经过100目筛,得到陶瓷复合粉体。
用于制备各层陶瓷的陶瓷复合粉体的组成如下:
第一层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3;
第二层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,1gCeO2;
第三层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,3g CeO2;
第四层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,5g CeO2;
第五层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,10g CeO2;
第六层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,10g CeO2,1gCNT;
第七层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,10g CeO2,3gCNT;
第八层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,10g CeO2,5gCNT;
第九层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,10g CeO2,7gCNT;
第十层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,10g CeO2,10gCNT。
(2)制备浆料:将步骤(1)制备的用于各陶瓷层的陶瓷复合粉体按配比与光敏树脂、光引发剂和分散剂混合均匀,分别制得用于制备各陶瓷层的浆料。具体为是将50g 1,6-乙二醇二丙烯酸酯和50g三羟甲基丙烷三丙烯酸酯均匀混合形成树脂预混液,然后将各陶瓷层的陶瓷复合粉体分别与树脂预混液混合,按以下要求控制各混合物的固含量:一至五层对应的混合物的固含量为50vol%,六至八层对应的混合物的固含量为40vol%,九至十层对应的混合物的固含量为30vol%。接着再加入5g硅烷偶联剂KH560,球磨2h使各组分分散均匀,转速350r/min,再接着继续添加1g 2-羟基-2-甲基-1-苯基-1-丙酮,继续球磨30min,制得十种浆料。
(3)成型
按照梯度结构模型,将与陶瓷层对应的浆料置于3D打印设备的打印料槽中,进行逐层打印,制得坯体。
坯体中各浆料层的曝光能量分别如下:用第1层至第5层的浆料打印对应的层时的曝光能量是60mJ/cm2,用第6层至第8层的浆料打印对应的层时的曝光能量是100mJ/cm2,用第9层、第10层的浆料打印对应的层时的曝光能量是200mJ/cm2,将1-5层的打印层厚度均设置为50μm,将5-10层的打印层厚度均设置为20μm,坯体中每层浆料的总厚度为200μm。
(4)脱脂:将坯体置于空气气氛脱脂炉内,以2℃/min的速率升温至650℃并保温4h。
(5)烧结:将坯体置于真空下烧结,以10℃/min的速率升温至1750℃并保温2h,制得具有十层结构的梯度功能陶瓷。
本实施例制备的梯度功能陶瓷表层致密,内层多孔,层叠结构单元的整体孔隙率为15%;通过扫描电子显微镜观察陶瓷的截面,各陶瓷层间结合良好,层与层间无裂纹;陶瓷性能良好,其抗弯强度为200MPa。
对比例1
本对比例提供一种由八层结构为一层叠结构单元的梯度功能陶瓷及其制备方法,包括以下制备步骤:(1)制备陶瓷复合粉体,(2)制备浆料,(3)成型,(4)脱脂,(5)烧结。与实施例1相比,本对比例仅成型步骤中3D打印设置的曝光能量不同,其它步骤与实施例1的一致。本对比例中,用第1层至第8层的浆料打印对应的层时的曝光能量均是40mJ/cm2。
通过扫描电子显微镜观察陶瓷的截面,梯度功能陶瓷的层叠结构单元中,第1层至第5层间的结合良好,但第5层与第6层间出现裂纹,第6层与第7层间也出现裂纹。
对比例2
本对比例提供一种由八层结构为一层叠结构单元的梯度功能陶瓷及其制备方法,包括以下制备步骤:(1)制备陶瓷复合粉体,(2)制备浆料,(3)成型,(4)脱脂,(5)烧结。与实施例1相比,本对比例的制备陶瓷复合粉体步骤中制备陶瓷复合粉体的组分不同,以及成型步骤中3D打印设置的曝光能量不同,其它步骤与实施例1的一致。
本对比例的步骤(1)中,用于制备各层陶瓷的陶瓷复合粉体的组成如下:
第一层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3;
第二层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,1g石墨烯;
第三层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,2g石墨烯;
第四层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,3g石墨烯;
第五层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,4g石墨烯;
第六层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,5g石墨烯,1gNa2SO4;
第七层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,6g石墨烯,3gNa2SO4;
第八层陶瓷的陶瓷复合粉体:20gZrO2,80gAl2O3,7g石墨烯,5gNa2SO4。
本对比例中,用第1层至第8层的浆料打印对应的层时的曝光能量均是160mJ/cm2。
通过扫描电子显微镜观察陶瓷的截面,梯度功能陶瓷的层叠结构单元中,第1层至第8层间出现裂纹。
以上所述仅以实施例来进一步说明本发明的技术内容,以便于读者更容易理解,但不代表本发明的实施方式仅限于此,任何依本发明所做的技术延伸或再创造,均受本发明的保护。
Claims (10)
1.一种梯度功能陶瓷的制备方法,其特征在于,浆料通过3D打印形成坯体,3D打印使用的模型为具有不同陶瓷层结构的梯度结构模型;所述制备方法包括以下步骤,
S1 制备陶瓷复合粉体:根据梯度结构模型分别配制用于3D打印对应陶瓷层的陶瓷复合粉体,与各陶瓷层对应的陶瓷复合粉体按以下重量份将各组分混合均匀制得:10-30份的陶瓷粉体、0-15wt份的烧结添加剂、0-15份的造孔剂;
S2 制备浆料:与各陶瓷层对应的浆料按以下重量份将各组分混合均匀制得:100-120份的陶瓷复合粉体,90-110份的光敏树脂,0.1-5份的光引发剂,0.1-5份的分散剂;
S3 成型:按照梯度结构模型,将与陶瓷层对应的浆料置于3D打印设备的打印料槽中,进行逐层打印,制得坯体;
S4 脱脂烧结:先以0.1-5℃/min的速率升温至300-800℃并保温2-4h,对坯体进行脱脂处理;然后坯体在空气气氛下,以5-10℃/min的速率升温至1300-1850℃并保温1-4h,制得梯度功能陶瓷。
2.根据权利要求1所述的一种梯度功能陶瓷的制备方法,其特征在于,步骤S1中,所述陶瓷粉体选自氧化铝、氧化锆、氧化镁、氧化钇、氮化硅、碳化硅、氮化硼中的至少一种。
3.根据权利要求2所述的一种梯度功能陶瓷的制备方法,其特征在于,步骤S1中,所述烧结添加剂选自碳纳米管、石墨烯、Re2O3中的至少一种,其中Re为Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。
4.根据权利要求1所述的一种梯度功能陶瓷的制备方法,其特征在于,步骤S1中,所述造孔剂选自淀粉、酚醛树脂、尼龙纤维中的至少一种。
5.根据权利要求1所述的一种梯度功能陶瓷的制备方法,其特征在于,步骤S2中,所述光敏树脂选自1,6-乙二醇二丙烯酸酯、三羟甲基丙烷三丙烯酸酯、聚氨酯丙烯酸酯中的至少一种。
6.根据权利要求1所述的一种梯度功能陶瓷的制备方法,其特征在于,步骤S2中,所述光引发剂选自2-羟基-2-甲基-1-苯基-1-丙酮、苯基双(2,4,6-三甲基苯甲酰基)氧化膦、1-羟基环已基苯基酮中的至少一种。
7.根据权利要求1所述的一种梯度功能陶瓷的制备方法,其特征在于,经步骤S4烧结制备的梯度功能陶瓷中各陶瓷层的孔隙率小于或等于50vol%。
8.根据权利要求1-7任一项所述的一种梯度功能陶瓷的制备方法,其特征在于,步骤S1中所述陶瓷粉体中的氮化硅含量小于10%,所述烧结添加剂选自Re2O3中的至少一种,其中Re为Y、Sc、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu时,步骤S3中进行3D打印的曝光能量设置如下:所述陶瓷复合粉体中烧结添加剂的含量为陶瓷粉体的10wt%以内时,曝光能量E为40mJ/cm2≤E<80mJ/cm2。
9.根据权利要求1-7任一项所述的一种梯度功能陶瓷的制备方法,其特征在于,步骤S1中所述陶瓷粉体中的氮化硅含量大于或等于90%,所述烧结添加剂选自Re2O3中的至少一种,其中Re为Y、Sc、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu时,所述陶瓷复合粉体中烧结添加剂的含量为陶瓷粉体的5wt%以内时,步骤S3中进行3D打印的曝光能量E为100mJ/cm2≤E≤120mJ/cm2。
10.根据权利要求1-7任一项所述的一种梯度功能陶瓷的制备方法,其特征在于,步骤S1中所述陶瓷粉体中的氮化硅含量大于或等于90%,所述烧结添加剂由石墨烯或碳纳米管与Y2O3组成,所述陶瓷复合粉体中烧结添加剂的含量为陶瓷粉体的1-5wt%时,步骤S3中进行3D打印的曝光能量E为140mJ/cm2≤E≤200mJ/cm2。
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