CN112142454A - 一种具有自修复功能的烤瓷粉 - Google Patents

一种具有自修复功能的烤瓷粉 Download PDF

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CN112142454A
CN112142454A CN202011050429.3A CN202011050429A CN112142454A CN 112142454 A CN112142454 A CN 112142454A CN 202011050429 A CN202011050429 A CN 202011050429A CN 112142454 A CN112142454 A CN 112142454A
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porcelain powder
self
repairing function
powder
tcp material
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CN112142454B (zh
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李蛟
鄢新章
刘谋山
马勤
罗友明
刘帅
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Chengdu Besmile Biotechnology Co ltd
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Abstract

本发明涉及义齿加工技术领域，具体涉及一种具有自修复功能的烤瓷粉。具体技术方案为：一种具有自修复功能的烤瓷粉，包括基础瓷粉和经过表面处理后的纳米α‑TCP材料。本发明解决了现有技术中烤瓷层开裂后进行反复修补和脱落的问题。

Description

一种具有自修复功能的烤瓷粉
技术领域
本发明涉及义齿加工技术领域，具体涉及一种具有自修复功能的烤瓷粉。
背景技术
目前，市面上所有的牙科烤瓷粉都是将瓷粉调拌均匀后在底冠外面逐层堆叠然后烧结而成。但是，在患者口内长期使用过程中，可能出现裂纹甚至完全裂开的情况，而这种情况下一般很难被察觉，即使在肉眼观察下也不容易被发现，尤其是一些比较难以发现或隐秘的地方，就更不容易被发现了。而一旦发现烤瓷层开裂，患者就医修补裂缝，而修补裂缝的材料就存在与烤瓷层之间结合的问题，所以，也就会造成患者反复就医修补裂缝；如果烤瓷层开裂的位置比较难以发现，那么在使用时间久了之后，就会有烤瓷层脱落的风险；由于脱落的烤瓷层比较小，掉落在患者嘴里也不容易被发现，就会吞进消化系统，而烤瓷层的硬度较高，可能会对患者的身体造成严重的伤害。因此，急需一种烤瓷层在开裂后进行自动修复的烤瓷粉。
发明内容
针对现有技术的不足，本发明提供了一种具有自修复功能的烤瓷粉，解决了现有技术中烤瓷层开裂后进行反复修补和脱落的问题。
为实现以上目的，本发明通过以下技术方案予以实现：
本发明公开了一种具有自修复功能的烤瓷粉，包括基础瓷粉和经过表面处理后的纳米α-TCP材料。
优选的，按照质量百分比计，所述基础瓷粉为95～99.5％，表面处理后的纳米α-TCP材料为0.5～5％。
优选的，所述纳米α-TCP材料的表面处理过程为：将纳米α-TCP材料均匀分散到溶解有乙基纤维素的无水乙醇中，再进行喷雾干燥，即得到表面包覆有乙基纤维素薄膜的纳米α-TCP材料。
优选的，干燥温度为70～85℃，所述纳米α-TCP材料的粒径为90～110nm。
优选的，所述乙基纤维素和乙醇的质量比为1:90～100。
优选的，所述纳米α-TCP材料和溶解有乙基纤维素的无水乙醇的质量比为(5-10):(95-90)。
优选的，按照质量百分比计，所述基础瓷粉包括以下组分：SiO2 55～70％、Al2O3 6～11％、K2O 10～18％、Na2O 5～8％、CaO 1～2％、BaO 0～2％、ZrO2 0～1％、Li2O 0.5～1.5％、SnO2 0～0.5％、B2O3 0.5～0.9％、MgO 0～0.5％、ZnO 0.5～1.5％、Y2O3 0～0.2％、Tb2O3 0～0.5％。
优选的，所述基础瓷粉的制备过程为：
步骤1.按照上述原料组分配比进行称量并混合均匀，然后在高温条件下熔化后进行水淬，最后进行研磨，备用；
步骤2.按照上述原料配比称量K2O、SiO2、Al2O3和Na2O，混合均匀，在高温下保温，冷却后进行研磨，备用；
步骤3.将步骤1和步骤2制备好的物料混合均匀。
优选的，步骤1中，熔化温度为1600～1700℃，熔化时间为2.5～4h，研磨的粒径为50～75μm。
优选的，步骤2中，保温温度为1330～1370℃，保温时间为3～5h，研磨的粒径为2～4μm。
本发明具备以下有益效果：
1.本发明在基础瓷粉中加入一种纳米磷酸钙(α-TCP)骨水泥材料，具体为将经过表面处理后的纳米α-TCP材料与牙科的基础瓷粉均匀混合，通过调整基础瓷粉的配比以及与纳米α-TCP材料之间的比例，获得与传统瓷粉相同的烧结效果，同时还能有效防止烧结过程中开裂。而且，采用本发明所公开的烤瓷粉烧结的瓷层在患者口腔长期使用过程中，一旦出现细微的裂纹，唾液会渗透到裂纹内与经过表面处理后的纳米α-TCP材料接触，纳米α-TCP材料就会固化从而将裂纹进行修复，防止裂纹进一步扩大，从而防止烤瓷瓷层开裂。
2.本发明通过在纳米α-TCP材料的表面覆盖一层有机薄膜的方式，使其在与基础瓷粉进行调拌的过程中不会因与水接触而固定，同时在烧结的过程中还会完全挥发乙基纤维素，从而使纳米α-TCP材料从薄膜中脱离出来均匀分散在基础瓷粉中。
具体实施方式
下面将结合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。
若未特别指明，实施举例中所用的技术手段为本领域技术人员所熟知的常规手段。
本发明公开了一种具有自修复功能的烤瓷粉，包括基础瓷粉和经过表面处理后的纳米α-TCP材料。按照质量百分比计，基础瓷粉为95～99.5％，表面处理后的纳米α-TCP材料为0.5～5％。
具体的：纳米α-TCP材料的表面处理过程为：选用乙基纤维素作为薄膜包裹材料，将其加入到无水乙醇中，不断搅拌使乙基纤维素完全溶解在无水乙醇中形成透明均匀的液体。其中，乙基纤维素和乙醇的质量比为1:90～100，优选为1:99。
然后将市售的粒径为90～110nm的纳米α-TCP材料均匀分散到溶解有乙基纤维素的无水乙醇中，不断搅拌，形成乳浊液。最后，使用喷雾干燥机将搅拌好的乳浊液烘干，干燥温度为70～85℃，优选为79℃。最终即得到表面包覆有乙基纤维素薄膜的纳米α-TCP材料。
基础瓷粉的制备
按照质量百分比计，基础瓷粉包括以下组分：SiO2 55～70％、Al2O3 6～11％、K2O10～18％、Na2O 5～8％、CaO 1～2％、BaO 0～2％、ZrO2 0～1％、Li2O 0.5～1.5％、SnO2 0～0.5％、B2O3 0.5～0.9％、MgO 0～0.5％、ZnO 0.5～1.5％、Y2O3 0～0.2％、Tb2O3 0～0.5％。
基础瓷粉的制备过程为：
步骤1.基础玻璃粉的制备：
按照上述原料组分配比进行称量并混合均匀，然后将混合好的原料在1600～1700℃的高温条件下熔制2.5～4h，使其熔化均匀，得到玻璃液；然后将熔化好的玻璃也倒入冷水中水淬成玻璃渣；最后将玻璃渣进行球磨，粒度控制在50～75μm，备用；其中，熔化温度优选为1600℃，时间为3h；
步骤2.白石榴粉的制备：
按照上述原料配比称量K2O、SiO2、Al2O3和Na2O，混合均匀，然后将混合好的原料在1330～1370℃的高温下进行保温3～5h，冷却至室温后进行球磨至粒径为2～4μm，备用；其中，保温温度优选为1350℃，时间为4h；
步骤3.将步骤1和步骤2制备好的基础玻璃粉和白石榴粉混合均匀，备用。
本发明烤瓷粉的制备
将制备的基础瓷粉和表面包覆有乙基纤维素薄膜的纳米α-TCP材料按照比例混合均匀后即可。其中，纳米α-TCP材料和溶解有乙基纤维素的无水乙醇的质量比为(5-10):(95-90)。
实施例
采用上述的工艺步骤和配比对基础瓷粉进行制备，具体的组分配比见下表1所示。基础瓷粉由基础玻璃粉和白石榴粉混合而成。
表1基础瓷粉的配比
Figure BDA0002709366680000041
Figure BDA0002709366680000051
按照表1的组分配比制备的基础玻璃粉和白石榴粉混合后得到的基础瓷粉与制备的表面包覆有乙基纤维素薄膜的纳米α-TCP材料调制烤瓷粉，具体按照组1分别与组a1、a2、a3，组2分别与组a1、a2、a3，组3分别与组a1、a2、a3的方式将基础玻璃粉和白石榴粉进行混合。具体配比和相关参数见下表2所示。其中，透度是通过将瓷粉压成薄片，烧结后磨成1mm厚，然后比较透光效果；膨胀系数是通过把瓷粉烧结成方条，然后用热膨胀系数仪测试。结果显示，通过控制白石榴粉的含量可以调控基础瓷粉的热膨胀系数，白石榴粉的含量越多，基础瓷粉的热膨胀系数越大。表2，各分组，每个分组中，组别a1、a2、a3分别所对应的组1、组2和组3所制得瓷粉的膨胀系数之间的差值≤0.01，因此，表2中，所示的热膨胀系数为三组瓷粉的热膨胀系数的平均值。
表2基础瓷粉与处理后的纳米α-TCP材料的配比(％)
Figure BDA0002709366680000052
Figure BDA0002709366680000061
Figure BDA0002709366680000071
具体试验过程为：
使用氧化锆底冠，其热膨胀系数为10×10-6K-1。烤瓷粉的热膨胀系数与底冠热膨胀系数一致才能保证烧结过程中瓷与底冠结合紧密，从而不崩瓷。因此，基于底冠的热膨胀系数，选择与其热膨胀系数相近或相同的烤瓷粉。
1.准备普通烤瓷粉制作的义齿20颗，使用分组5中的组别3+a3号样品原料，将基础瓷粉和处理后的纳米α-TCP材料混合均匀后，烧结成义齿，共计20颗。
2.将所有义齿均经过高温烧结后直接降温至室温，利用急热急冷使义齿表面形成裂纹。
3.使用显微镜将形成裂纹的义齿筛选出来，放入自来水中浸泡，24小时后取出观察裂纹修复情况。
结果显示：用普通烤瓷粉制作的义齿经过自来水浸泡，裂纹全部没有修复；而加入了纳米α-TCP材料的烤瓷粉制作的义齿，裂纹经过自来水浸泡，形成了新的α-TCP固化后的结构，实现了裂纹的自我修复。
以上所述的实施例仅是对本发明的优选方式进行描述，并非对本发明的范围进行限定，在不脱离本发明设计精神的前提下，本领域普通技术人员对本发明的技术方案做出的各种变形和改进，均应落入本发明权利要求书确定的保护范围内。

Claims (10)

1.一种具有自修复功能的烤瓷粉，其特征在于：包括基础瓷粉和经过表面处理后的纳米α-TCP材料。
2.根据权利要求1所述的一种具有自修复功能的烤瓷粉，其特征在于：按照质量百分比计，所述基础瓷粉为95～99.5％，表面处理后的纳米α-TCP材料为0.5～5％。
3.根据权利要求1或2所述的一种具有自修复功能的烤瓷粉，其特征在于：所述纳米α-TCP材料的表面处理过程为：将纳米α-TCP材料均匀分散到溶解有乙基纤维素的无水乙醇中，再进行喷雾干燥，即得到表面包覆有乙基纤维素薄膜的纳米α-TCP材料。
4.根据权利要求3所述的一种具有自修复功能的烤瓷粉，其特征在于：干燥温度为70～85℃，所述纳米α-TCP材料的粒径为90～110nm。
5.根据权利要求3所述的一种具有自修复功能的烤瓷粉，其特征在于：所述乙基纤维素和乙醇的质量比为1:90～100。
6.根据权利要求3所述的一种具有自修复功能的烤瓷粉，其特征在于：所述纳米α-TCP材料和溶解有乙基纤维素的无水乙醇的质量比为(5-10):(95-90)。
7.根据权利要求1所述的一种具有自修复功能的烤瓷粉，其特征在于：按照质量百分比计，所述基础瓷粉包括以下组分：SiO2 55～70％、Al2O3 6～11％、K2O 10～18％、Na2O 5～8％、CaO 1～2％、BaO 0～2％、ZrO20～1％、Li2O 0.5～1.5％、SnO2 0～0.5％、B2O3 0.5～0.9％、MgO 0～0.5％、ZnO 0.5～1.5％、Y2O3 0～0.2％、Tb2O3 0～0.5％。
8.根据权利要求7所述的一种具有自修复功能的烤瓷粉，其特征在于：所述基础瓷粉的制备过程为：
步骤1.按照上述原料组分配比进行称量并混合均匀，然后在高温条件下熔化后进行水淬，最后进行研磨，备用；
步骤2.按照上述原料配比称量K2O、SiO2、Al2O3和Na2O，混合均匀，在高温下保温，冷却后进行研磨，备用；
步骤3.将步骤1和步骤2制备好的物料混合均匀。
9.根据权利要求8所述的一种具有自修复功能的烤瓷粉，其特征在于：步骤1中，熔化温度为1600～1700℃，熔化时间为2.5～4h，研磨的粒径为50～75μm。
10.根据权利要求8所述的一种具有自修复功能的烤瓷粉，其特征在于：步骤2中，保温温度为1330～1370℃，保温时间为3～5h，研磨的粒径为2～4μm。
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