CN109608233A - 一种改善牙科用二氧化锆陶瓷通透性的技术 - Google Patents

一种改善牙科用二氧化锆陶瓷通透性的技术 Download PDF

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Publication number
CN109608233A
CN109608233A CN201910092490.5A CN201910092490A CN109608233A CN 109608233 A CN109608233 A CN 109608233A CN 201910092490 A CN201910092490 A CN 201910092490A CN 109608233 A CN109608233 A CN 109608233A
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China
Prior art keywords
color liquid
zirconia ceramic
permeability
group
screening
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CN201910092490.5A
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Inventor
马勤
李蛟
潘许松
吴丹
刘帅
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Chengdu Baesch Beauty Medical Polytron Technologies Inc
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Chengdu Baesch Beauty Medical Polytron Technologies Inc
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Priority to CN201910092490.5A priority Critical patent/CN109608233A/zh
Publication of CN109608233A publication Critical patent/CN109608233A/zh
Priority to PCT/CN2019/084893 priority patent/WO2020155446A1/zh
Priority to US17/388,007 priority patent/US11858867B2/en
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Abstract

本发明属于口腔材料领域，具体涉及一种改善牙科用二氧化锆陶瓷通透性的技术。具体包括一种遮色液，配方包括硝酸钾、氯化钇、硝酸镨、醇类、柠檬酸、葡萄糖酸和水。在二氧化锆陶瓷完成最后一次烧结前，将所述遮色液涂刷在二氧化锆表面，再进行最后一次烧结即可。使用本发明提供的遮色液和方法，遮色液不仅与陶瓷结合紧密，且不会增加陶瓷的厚度，同时在通透性和遮盖效果间取得了很好的平衡。

Description

一种改善牙科用二氧化锆陶瓷通透性的技术
技术领域
本发明属于口腔材料领域，具体涉及一种改善牙科用二氧化锆陶瓷通透性的技术。
背景技术
二氧化锆是目前牙科修复界广泛使用的复合材料，随着多年来不断发展，其通透性越来越接近天然牙修复的要求。但使用二氧化锆制作种植义齿上部修复体时，不仅要求其通透性好、接近天然牙，还要求其具有一定的遮盖效果，以避免种植体基台的金属颜色外透、影响美观。而通透性和遮盖效果间存在一定的矛盾性，该矛盾是困扰业界人士已久。
目前，针对这一矛盾，国内外普遍采用的方法是选用通透度低的氧化锆做基底，再在氧化锆表面做饰面瓷处理，利用瓷面遮盖金属；但这样做不仅工序繁琐、成本增加，而且还需考虑氧化锆和瓷面的结合问题，还需另外对瓷面的颜色进行调整，非常麻烦。业内也有选用通透度高的氧化锆做基底，基底完成后，再涂刷遮色材料以达到遮色效果；但遮色材料刷得过厚影响美观，刷得过薄则无法实现遮挡效果，难以把握涂刷技术，另外还需考虑遮色材料与氧化锆结合的问题。更重要的是，无论是贴瓷还是涂刷的方法，都需在氧化锆基底外部增加一层材料、占用一定的空间，对于义齿这样对尺寸精确度要求较高的产品而言，如果要考虑增加的空间，会大大增加制作的难度和成本；如果不考虑增加的空间，又会影响义齿的安装和使用效果。
因此，市场急需一种不会成本低廉、使用简单、不会改变氧化锆基底尺寸、有效解决通透性和遮盖效果间的矛盾的遮色技术。
发明内容
本发明的目的是提供一种改善牙科用二氧化锆陶瓷通透性的技术。
为实现上述发明目的，本发明所采用的技术方案是：一种遮色液，配方包括：硝酸钾、氯化钇、硝酸镨、醇类、柠檬酸、葡萄糖酸和水。
优选的，按质量分数，所述配方为：95～98％的母液、1.3～1.6％的醇、0.03～0.40％的硝酸钾、0.1～0.3％的氯化钇、0.3～0.4％的柠檬酸；
按质量分数，所述母液为：18～23％的乙二醇、1～5％的葡萄糖酸、1～3％的柠檬酸、1～3％的硝酸镨和余量的水。
相应的，所述的遮色液在改变二氧化锆陶瓷通透性上的应用。
优选的，在二氧化锆陶瓷完成最后一次烧结前，将所述遮色液涂刷在二氧化锆表面。
优选的，所述应用包括如下步骤：
(1)在二氧化锆陶瓷完成最后一次烧结前，将所述遮色液涂刷在二氧化锆表面；
(2)将带遮色液的二氧化锆陶瓷烘干；
(3)对烘干后的二氧化锆陶瓷进行烧结。
优选的，步骤(2)所述烘干的温度为90℃。
优选的，步骤(3)所述烧结的条件为：1530℃、2h。
相应的，一种改善二氧化锆陶瓷通透性的方法，在进行二氧化锆陶瓷的最后一次烧结工艺前，在所述二氧化锆陶瓷表面涂刷遮色液，干燥后，再进行最后一次烧结工艺；所述遮色液中至少包括含K的化合物。
本发明具有以下有益效果：本发明提供了一种改善二氧化锆陶瓷通透性的全新思路：不对已制备完成的二氧化锆进行贴片/涂刷等处理，而是对尚未完成最后一次烧结的二氧化锆陶瓷进行遮色液处理，随后再对带有遮色液的二氧化锆陶瓷进行最后一次烧结工艺，使遮色液的成分与二氧化锆陶瓷一起反应结晶，成为二氧化锆陶瓷的一部分。遮色液不仅与陶瓷结合紧密，且不会增加陶瓷的厚度，同时在通透性和遮盖效果间取得了很好的平衡。
具体实施方式
本发明提供了一种改善/平衡牙科用二氧化锆陶瓷通透性和遮盖性的产品(以下简称遮色液)，其配方为：按质量分数，95～98％的母液、1.3～1.6％的醇、0.03～0.40％的硝酸钾、0.1～0.3％的氯化钇、0.3～0.4％的柠檬酸。
所述母液的配方为：按质量分数，18～23％的乙二醇、1～5％的葡萄糖酸、1～3％的柠檬酸、1～3％的硝酸镨和余量的水。
其中，所述硝酸钾可以使氧化锆基底在烧结后形成乳白色的遮色层，从而达到遮色的效果；硝酸钾浓度增加，一般而言，遮色效果也会增强。所述醇类因其良好的相容性，从而具有分散剂的作用。所述氯化钇起到催化剂的作用。
将所述遮色液除母液外的各组分准确称量后，常温下进行初混，再加入母液，充分搅拌溶解混匀，即得所需遮色液。
所述遮色液的使用方法为：取遮色液涂刷于牙齿表面需要遮色处(单颗义齿表面的遮色液用量≤0.001g，实际操作时蘸取少许遮色液进行无重复路径涂刷即可)，重复涂刷两遍，然后放入烘箱90℃烘干。半小时后取出，放入有锆珠的坩埚内，放进烧结炉中，设置烧结炉的温度曲线，1530℃下保温2h，完成烧结即可。
在氧化锆基底初步制作成型、未进行最后的烧结前，将所述遮色液涂刷在基底上，再将氧化锆基底进行最后的烧结工序，使遮色液与氧化锆基底一起反应结晶，利用遮色液直接对氧化锆基底进行染色，使遮色层成为氧化锆基底内部的一部分，成为基底自带的颜色，遮色层与基底反应后结合紧密，不会额外增加基底的体积。
下面结合具体实施例，对本发明进行进一步的阐述。
实施例一：遮色液配方对效果的影响
1、使用上述方法制备9组遮色液，其中，各组遮色液的配方为：96.83％的母液、1.52％的乙醇、1.1％的硝酸钾、0.2％的氯化钇、0.35％的柠檬酸。所述母液的配方如表1所示，表中数字表示该组分在遮色液中占的质量分数，余量为去离子水，各组分总和为100％。所述遮色液的具体使用方法为：取等量各组遮色液涂刷于牙齿表面需要遮色处，重复涂刷两遍，然后放入烘箱90℃烘干。半小时后取出，放入有锆珠的坩埚内，放进烧结炉中完成烧结即可。
表1 各组所用母液的配方表
组别 乙二醇 葡萄糖酸 柠檬酸 硝酸镨
组1 18％ 3％ 2％ 2％
组2 20％ 3％ 2％ 2％
组3 23％ 3％ 2％ 2％
组4 20％ 1％ 2％ 2％
组5 20％ 5％ 2％ 2％
组6 20％ 3％ 1％ 2％
组7 20％ 3％ 3％ 2％
组8 20％ 3％ 2％ 1％
组9 20％ 3％ 2％ 3％
2、单独制备一组氧化锆基底，未进行遮色液涂刷，其余制备和烧结条件完全相同，作为空白对照组。
对各组氧化锆基底进行透光率检测、三点抗弯强度检测、厚度检测和遮色情况检测。其中，所述厚度检测为：分别检测各组氧化锆基底三点的厚度(各基底选择的三点位置相同)，并分别与空白对照组的三点厚度进行对比，获得三组差异率，取平均值，厚度差异低于万分之一，视为无差异。所述遮色情况检测方法为：将各组制备的氧化锆基底分别套于相同的金属基台上，在日常光照情况下肉眼观察是否透色，并观察通透性和美观程度。各组结果如表2所示。
表2 各组二氧化锆基底结果展示
3、使用步骤1的组2中母液的配方制备母液，再以该母液制备14组遮色液(组10～组23)，其中，各组遮色液的配方如表3所示，表中数字表示该组分在遮色液中占的质量分数。所述遮色液的具体使用方法为：取等量各组遮色液涂刷于牙齿表面需要遮色处，重复涂刷两遍，然后放入烘箱90℃烘干。半小时后取出，放入有锆珠的坩埚内，放进烧结炉中完成烧结即可。
表3 各组所用遮色液的配方表
组别 母液 醇的种类 醇 硝酸钾 氯化钇 柠檬酸
组10 95.00％ 乙醇 4.15％ 0.30％ 0.20％ 0.35％
组11 96.63％ 乙醇 2.52％ 0.30％ 0.20％ 0.35％
组12 96.83％ 乙醇 1.52％ 0.30％ 0.20％ 0.35％
组13 97.88％ 乙醇 1.27％ 0.30％ 0.20％ 0.35％
组14 95.00％ 乙醇 1.52％ 2.93％ 0.20％ 0.35％
组15 96.63％ 乙醇 1.52％ 1.30％ 0.20％ 0.35％
组16 96.83％ 乙醇 1.52％ 1.10％ 0.20％ 0.35％
组17 97.88％ 乙醇 1.52％ 0.05％ 0.20％ 0.35％
组18 96.93％ 乙醇 1.52％ 1.10％ 0.10％ 0.35％
组19 96.93％ 乙醇 1.52％ 1.10％ 0.30％ 0.35％
组20 96.93％ 乙醇 1.52％ 1.10％ 0.20％ 0.20％
组21 96.93％ 乙醇 1.52％ 1.10％ 0.20％ 0.40％
组22 96.83％ 乙二醇 1.52％ 1.10％ 0.20％ 0.35％
组23 96.83％ 甲醇 1.52％ 1.10％ 0.20％ 0.35％
4、对各组氧化锆基底进行透光率检测、三点抗弯强度检测、厚度检测和遮色情况检测。其中，所述厚度检测为：分别检测各组氧化锆基底三点的厚度(各基底选择的三点位置相同)，并分别与空白对照组的三点厚度进行对比，获得三组差异率，取平均值。所述遮色情况检测方法为：将各组制备的氧化锆基底分别套于相同的金属基台上，在日常光照情况下肉眼观察是否透色。各组结果如表4所示。
表4 各组二氧化锆基底结果展示
实施例二：遮色液使用方法对效果的影响
1、使用实施例一组16的配方制备8组遮色液，再分别对本实施例各组采用不同的使用方法。其中，各组处理方法如表5所示。
表5 各组遮色液使用方法对照表
组别 遮色液涂刷时机 遮色液涂刷次数 是否烘干 烘干温度
组1 氧化锆基底最后一次烧结前 两遍 是 90℃
组2 氧化锆基底完成烧结后 两遍 是 90℃
组3 氧化锆基底最后一次烧结前 一遍 是 90℃
组4 氧化锆基底最后一次烧结前 四遍 是 90℃
组5 氧化锆基底最后一次烧结前 两遍 否 /
组6 氧化锆基底最后一次烧结前 两遍 是 30℃
组7 氧化锆基底最后一次烧结前 两遍 是 60℃
组8 氧化锆基底最后一次烧结前 两遍 是 120℃
2、单独制备一组氧化锆基底，未进行遮色液涂刷，其余制备和烧结条件完全相同，作为空白对照组。各组结果如表6所示。其中，未烘干是指未进行烘干，直接进行烧结工艺。
表6 各组二氧化锆基底结果展示

Claims (8)

1.一种遮色液，其特征在于：配方包括：硝酸钾、氯化钇、硝酸镨、醇、柠檬酸、葡萄糖酸和必要的溶剂。
2.根据权利要求1所述的遮色液，其特征在于：按质量分数，所述配方为：95～98％的母液、1.3～1.6％的醇、0.03～0.40％的硝酸钾、0.1～0.3％的氯化钇、0.3～0.4％的柠檬酸；
按质量分数，所述母液为：18～23％的乙二醇、1～5％的葡萄糖酸、1～3％的柠檬酸、1～3％的硝酸镨和余量的水。
3.权利要求1或2所述的遮色液在改变二氧化锆陶瓷通透性上的应用。
4.根据权利要求3所述的遮色液在改变二氧化锆陶瓷通透性上的应用，其特征在于：在二氧化锆陶瓷进行最后一次烧结前，将所述遮色液涂刷在陶瓷表面，再对处理后的陶瓷进行最后一次烧结。
5.根据权利要求4所述的遮色液在改变二氧化锆陶瓷通透性上的应用，其特征在于：所述应用包括如下步骤：
(1)在二氧化锆陶瓷完成最后一次烧结前，将所述遮色液涂刷在二氧化锆表面；
(2)将带遮色液的二氧化锆陶瓷烘干；
(3)对烘干后的二氧化锆陶瓷进行烧结。
6.根据权利要求5所述的遮色液在改变二氧化锆陶瓷通透性上的应用，其特征在于：步骤(2)所述烘干的温度为90℃。
7.根据权利要求5所述的遮色液在改变二氧化锆陶瓷通透性上的应用，其特征在于：步骤(3)所述烧结的条件为：1530℃、2h。
8.一种改善二氧化锆陶瓷通透性的方法，其特征在于：在进行二氧化锆陶瓷的最后一次烧结工艺前，先在所述二氧化锆陶瓷表面涂刷遮色液，再进行最后一次烧结工艺；所述遮色液中至少包括含K的化合物。
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