CN113461421A - 一种叠层氧化锆牙科陶瓷材料及其制备方法 - Google Patents
一种叠层氧化锆牙科陶瓷材料及其制备方法 Download PDFInfo
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Abstract
本发明属于牙科陶瓷材料技术领域，本发明公开了一种叠层氧化锆牙科陶瓷材料及其制备方法，该制备方法主要内容为粉体成型之前对不同层粉体界面进行处理，通过造粒和过筛，制备出第一、第二混合物筛选粉体，将第一混合物筛选粉体平铺在下层粉体上，第二混合物筛选粉体平铺在第一混合物筛选粉体上，然后叠加上层粉体。本发明解决了叠层氧化锆牙科陶瓷界面容易开裂的问题。所得产品不仅可以用于成形盘状坯料，还可以在预备体上成形个性化形状修复体的坯料。
Description
技术领域
本发明涉及牙科陶瓷材料技术领域，更具体的说是一种叠层牙科陶瓷材料及其制备方法。
背景技术
全瓷修复技术作为牙体缺损缺失固定修复、前牙区美容修复等口腔修复学领域的治疗方式，已在临床上得到广泛应用，越来越受到医师和患者的欢迎。氧化锆陶瓷作为全瓷修复体材料，凭借其优良的理化性能、稳定的生物相容性和良好的美观修复效果，在全球迅速普及。然而，完美的修复体除了形态、大小满足要求外，还需要有与天然牙齿接近的颜色和力学性能。未着色的氧化锆陶瓷多呈现白色或象牙白，难以满足临床对修复体色彩性的要求。为了增加氧化锆陶瓷修复体的美观效果和仿生力学性能，人们发明了颜色和强度呈梯度变化的氧化锆牙科陶瓷。
中国专利申请公布号为CN 105622096A，名称为“彩色渐变氧化锆材料及其制备方法”的专利，公开的氧化锆材料包括底层、中间层和外层三层结构。制备方法为将三种不同的氧化锆粉体依次置于模腔的不同位置，经干压成型、冷等静压成型、预烧结、切削和二次烧结，最终得到氧化锆牙科陶瓷材料。
中国专利申请公布号为CN 10527228A的专利公开了一种强度、颜色均匀过渡的牙科氧化锆修复材料的制备方法。该方法按照每层强度由高到低，颜色由深到浅的顺序将着色氧化锆粉体倒进干压模具中干压成型，再进行冷等静压成型，随后预烧结，得到素胚，再然后对素胚进行切削加工与终烧结，得到牙科氧化锆修复材料。
目前，彩色渐变氧化锆陶瓷材料一般都涉及到叠层氧化锆陶瓷制备技术，现有的技术中基本都是对氧化锆粉体进行分层放置于磨具中再干压成型，然后进行冷等静压。由于不同层的组分存在差异，导致烧结后容易出现分层和开裂等问题，从而增大了陶瓷块体产品的废品率，造成资源浪费和经济损失。同时，又由于界面处氧化锆陶瓷的力学性能发生突变，会降低陶瓷块体整体力学特性。
因此，如何提供一种不产生分层缺陷的氧化锆牙科陶瓷材料的制备方法成为了本领域技术人员亟需解决的问题。
发明内容
有鉴于此，本发明提供了一种叠层氧化锆牙科陶瓷材料及其制备方法，此制备方法主要解决了叠层氧化锆牙科陶瓷界面容易开裂的问题。其制备出的氧化锆陶瓷材料不仅可以用于成形盘状坯料，还可以在预备体上成形个性化形状修复体的坯料。
为了达到上述目的，本发明采用如下技术方案：
本发明提供了一种叠层氧化锆牙科陶瓷材料的制备方法，该叠层材料由多层氧化锆粉体分层压制成型，包括以下步骤：
S1、分层压制时，将10份~40份上层粉体与90份~60份下层粉体混合，得到第一混合物；
S2、分层压制时，将10份~40份下层粉体与90份~60份上层粉体混合，得到第二混合物；
S3、在第一混合物中加入酒精，使粉体潮湿，然后过两层不同目数的筛子，得到通过第一层筛子而未通过第二层筛子的第一混合物筛选粉体，其中第一层筛子目数≤50目，第二层筛子目数＞50目；
S4、在第二混合物中加入酒精，使粉体潮湿，然后过两层不同目数的筛子，得到通过第一层筛子而未通过第二层筛子的第二混合物筛选粉体，其中第一层筛子目数≤50目，第二层筛子目数＞50目；
S5、将第一混合物筛选粉体平铺在下层粉体上；
S6、将第二混合物筛选粉体平铺在第一混合物筛选粉体上；
S7、待第二混合物筛选粉体干燥后，再在第二层筛选粉体层上叠加上层粉体；
S8、干压成型后，再进行冷等静压成型，预烧结后得到素坯，对素坯进行终烧结后得到氧化锆陶瓷块体。
作为优选，所述步骤S1中将20份上层粉体与80份下层粉体混合，得到第一混合物；
作为优选，所述步骤S2中将20份下层粉体与80份上层粉体混合，得到第二混合物；
作为优选，所述步骤S3中采用喷雾法在第一混合物中加入酒精，酒精的加入量为混合物粉体质量的2%~4%；进一步优选，酒精的加入量为混合物粉体质量的3%；
作为优选，所述步骤S3中的第一层筛子的目数为30目，第二层筛的目数为200目；
作为优选，所述步骤S4中采用喷雾法在第二混合物中加入酒精，酒精的加入量为混合物粉体质量的2%~4%；进一步优选，酒精的加入量为混合物粉体质量的3%；
作为优选，所述步骤S4中的第一层筛子的目数为30目，第二层筛的目数为200目；
作为优选，所述步骤S5中的第一混合物筛选粉体的质量为下层粉体质量的2%~9%；
作为优选，所述步骤S6中的第二混合物筛选粉体的质量为上层粉体质量的2%~9%。
本发明还提供了一种按照上述叠层氧化锆牙科陶瓷材料的制备方法制备得到的叠层氧化锆牙科陶瓷材料。
本发明所应用的原理为：采用酒精加入粉体的目的是为了造粒。潮湿的粉体，经过两次过筛，得到粒径均匀的大颗粒粉体，通常情况下，其粒径均大于上下两层氧化锆粉体的粒径。经过筛选后，颗粒较大的第一混合物粉体和第二混合物粉体在后续的干压成型和冷等静压过程中，由于颗粒之间存在间隙，粉体能够彼此嵌合，且有少量的上下层粉体渗入，从而达到生成连续梯度界面的效果。
经由上述的技术方案可知，与现有技术相比，本发明的有益效果如下：
本发明通过改善界面处粉体成分分布，制备出连续梯度界面层，实现叠层氧化锆牙科陶瓷内部颜色和力学性能连续渐变，解决了叠层氧化锆牙科陶瓷界面容易开裂的问题。本发明不仅可以用于成形盘状坯料，还可以在预备体上成形个性化形状修复体的坯料，能够提高产品质量，增加经济效益。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术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的前提下，还可以根据提供的附图获得其他的附图。
图1 附图为实施例1中得到的叠层氧化锆牙科陶瓷块切削后图片；
图2 附图为实施例2中得到的叠层氧化锆牙科陶瓷试样切削后图片；
图3 附图为实施例2中得到的叠层氧化锆牙科陶瓷试样切削后图片。
具体实施方式
下面将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他实施例，都属于本发明保护的范围。
实施例1
2021年6月上旬，在秦皇岛某厂的三层氧化锆牙科陶瓷制备过程中，按照物理空间分为下、中、上三层，先将下层粉体放置在模型中，将10份中层粉体与90份下层粉体混合，得到混合物A1，将10下层粉体与90份中层粉体混合，得到混合物A2，采用喷雾法分别在A1和A2混合物中加入酒精，酒精质量分别为相应粉体质量的2%，混合均匀后，分别过筛30目和100目筛子，取两筛之间的粉体，得到A1筛选粉体和A2筛选粉体。称取A1筛选粉体的质量为模型组下层粉体总质量的2%，A2筛选粉体为中层粉体总质量的2%。将A1和A2筛选粉体依次平铺在下层粉体之上。静置一段时间，待粉体干燥后，再将中层粉体放在A2粉体层上。随后将10份上层粉体与90份中层粉体混合，得到混合物B1，将10中层粉体与90份上层粉体混合，得到混合物B2，采用喷雾法分别在B1和B2混合物中加入酒精，混合均匀后，分别过筛30目和100目筛子，取两筛之间的粉体，得到B1筛选粉体和B2筛选粉体。称取B1筛选粉体的质量为模型组下层粉体总质量的2%，B2筛选粉体为中层粉体总质量的2%。将B1和B2筛选粉体依次平铺在中层粉体之上。静置一段时间，待粉体干燥后，再将上层粉体放在B2粉体层上。干压成型后，再进行冷等静压成型，预烧结后得到素坯，对素坯进行终烧结后得到氧化锆陶瓷块体。随后，对陶瓷块体进行切削加工后，切削后照片如图1所示，从图中可以看出瓷块内未发现分层和开裂。
实施例2
2021年6月中旬，在秦皇岛某企业的六四层氧化锆牙科陶瓷制备过程中，按照物理空间分为一、二、三、四、五、六层，每两层之间，按照物理空间将20份上层粉体与80份下层粉体混合，得到混合物A1，将20下层粉体与80份上层粉体混合，得到混合物A2，采用喷雾法分别在A1和A2混合物中加入酒精，酒精添加量为相应粉体质量的3%，混合均匀后，分别过筛40目和120目筛子，取两筛之间的粉体，得到A1筛选粉体和A2筛选粉体。称取A1筛选粉体的质量为模型组下层粉体总质量的5%，A2筛选粉体为中层粉体总质量的5%。将A1和A2筛选粉体依次平铺在第一层粉体之上。静置一段时间，待粉体干燥后，再将第二层粉体放在A2粉体层上。六层粉体叠加完成后，干压成型，再进行冷等静压成型，预烧结后得到素坯，对素坯进行终烧结后得到氧化锆陶瓷块体。然后对陶瓷块体进行切削加工，切削后的试样如图2、图3所示，由图中可以看出该样品内部没有出现分层和开裂，表明该发明具有实用性。
Claims (7)
1.一种叠层氧化锆牙科陶瓷材料的制备方法，该叠层材料由多层氧化锆粉体分层压制成型，其特征在于，包括以下步骤：
S1、分层压制时，将10份~40份上层粉体与90份~60份下层粉体混合，得到第一混合物；
S2、分层压制时，将10份~40份下层粉体与90份~60份上层粉体混合，得到第二混合物；
S3、在第一混合物中加入酒精，然后过两层不同目数的筛子，得到通过第一层筛子而未通过第二层筛子的第一混合物筛选粉体，其中第一层筛子目数≤50目，第二层筛子目数＞50目；
S4、在第二混合物中加入酒精，然后过两层不同目数的筛子，得到通过第一层筛子而未通过第二层筛子的第二混合物筛选粉体，其中第一层筛子目数≤50目，第二层筛子目数＞50目；
S5、将第一混合物筛选粉体平铺在下层粉体上；
S6、将第二混合物筛选粉体平铺在第一混合物筛选粉体上；
S7、待第二混合物筛选粉体干燥后，再在第二层筛选粉体层上叠加上层粉体；
S8、干压成型后，再进行冷等静压成型，预烧结后得到素坯，对素坯进行终烧结后得到氧化锆陶瓷块体。
2.根据权利要求1所述的一种叠层氧化锆牙科陶瓷材料的制备方法，其特征在于，所述第一混合物和第二混合物中的上层粉体与下层粉体以总质量100份计算。
3.根据权利要求1所述的一种叠层氧化锆牙科陶瓷材料的制备方法，其特征在于，所述步骤S3中在第一混合物中加入酒精的量为混合物粉体质量的1%~5%。
4.根据权利要求1所述的一种叠层氧化锆牙科陶瓷材料的制备方法，其特征在于，所述步骤S4中在第二混合物中加入酒精的量为混合物粉体质量的1%~5%。
5.根据权利要求1所述的一种叠层氧化锆牙科陶瓷材料的制备方法，其特征在于，所述步骤S5中的第一混合物筛选粉体的质量为下层粉体质量的1%~10%。
6.根据权利要求1所述的一种叠层氧化锆牙科陶瓷材料的制备方法，其特征在于，所述步骤S6中的第二混合物筛选粉体的质量为上层粉体质量的1%~10%。
7.如权利要求1~6任一项所述的叠层氧化锆牙科陶瓷材料的制备方法制备得到的叠层氧化锆牙科陶瓷材料。
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