CN102674888A - 用于牙科氧化锆陶瓷制品的着色溶液及使用方法 - Google Patents

用于牙科氧化锆陶瓷制品的着色溶液及使用方法 Download PDF

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Publication number
CN102674888A
CN102674888A CN2012101495214A CN201210149521A CN102674888A CN 102674888 A CN102674888 A CN 102674888A CN 2012101495214 A CN2012101495214 A CN 2012101495214A CN 201210149521 A CN201210149521 A CN 201210149521A CN 102674888 A CN102674888 A CN 102674888A
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China
Prior art keywords
coloring solution
ion
solution
solvent
dental
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN2012101495214A
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English (en)
Inventor
王鸿娟
严庆云
黄东斌
何玲玲
郑艳春
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Liaoning Upcera Biomaterial Co Ltd
SHENZHEN ULTRA TECHNOLOGY Co Ltd
Original Assignee
Liaoning Upcera Biomaterial Co Ltd
SHENZHEN ULTRA TECHNOLOGY Co Ltd
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Publication date
Application filed by Liaoning Upcera Biomaterial Co Ltd, SHENZHEN ULTRA TECHNOLOGY Co Ltd filed Critical Liaoning Upcera Biomaterial Co Ltd
Priority to CN2012101495214A priority Critical patent/CN102674888A/zh
Publication of CN102674888A publication Critical patent/CN102674888A/zh
Priority to CN201210558349.8A priority patent/CN103113132B/zh
Priority to PT13791600T priority patent/PT2850043T/pt
Priority to KR1020147031997A priority patent/KR101691575B1/ko
Priority to EP13791600.3A priority patent/EP2850043B1/en
Priority to PCT/CN2013/074962 priority patent/WO2013170705A1/en
Priority to US14/397,449 priority patent/US9554881B2/en
Priority to DK13791600.3T priority patent/DK2850043T3/da
Priority to ES13791600T priority patent/ES2744715T3/es
Pending legal-status Critical Current

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    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00—Dental prostheses; Making same
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Abstract

本发明涉及用于牙科氧化锆陶瓷制品的着色溶液。着色溶液由着色剂、溶剂和添加剂组成，着色剂为稀土金属离子，在溶液中的含量为0.05~3摩尔/升溶剂，添加剂含量为0~50wt%。本发明还涉及使用着色溶液处理经过预烧结的氧化锆坯体制备仿牙色的牙科陶瓷制品的方法。本发明使牙科氧化锆制品着色更均匀；无需添加保持稳定作用的络合剂或增大着色溶液中酸的含量；提高了牙科氧化锆制品的透光性。

Description

用于牙科氧化锆陶瓷制品的着色溶液及使用方法
技术领域
本发明涉及一种牙科用着色溶液，尤其涉及一种着色剂均为稀土金属离子的用于牙科氧化锆陶瓷制品的着色溶液以及该着色溶液在牙科领域中的使用方法。
背景技术
口腔修复学中，颜色的再现问题是影响修复体和牙齿客观性的一个重要指标，未着色的氧化锆陶瓷颜色多呈白色到象牙色，制备出的修复体颜色单一，难以满足临床对材料色彩复杂性的要求，所以必须要依靠饰面瓷来完成。口腔修复的一项原则是在尽可能保留牙体组织的前提下获得机械性能与美学性能的统一。通过染色，使氧化锆基底冠本身具有与天然牙牙本质色泽相近，在修复体制作过程中减少饰面瓷厚度或完全不使用饰面瓷仍可达到理想的美学效果，同时还可以降低备牙量，更有利于保留更多的牙体组织。
目前，氧化锆修复体的着色方法主要有两种：一种方法则是在氧化锆粉体中引入着色剂，制备出已着色的陶瓷坯体，在经过切削加工、烧结，从而得到与天然牙颜色相近的修复体。另一种是配置特定的着色溶液，将经过切削加工的未作色的氧化锆基底冠在着色溶液中浸泡几分钟，或将染色液涂刷在氧化锆修复体上。
现在，已有一些关于用于陶瓷制品的着色溶液方面的专利。
WO2009/014903（对应于CN 101778807 A），涉及用于使牙科陶瓷制品着色的着色溶液，所述溶液包含：溶剂和着色剂，所述的着色剂包含稀土元素金属和过渡金属或离子，所述稀土元素金属或离子在所述溶液中的存在量为约0.05至约1摩尔/升溶剂，所述过渡金属或离子在所述溶液中的含量为约0.00001至约0.05摩尔/升溶剂。
WO2004/110959（对应于CN 1805913 A），涉及用于陶瓷框架的着色溶液、用所述溶液着色的陶瓷框架以及获得均匀着色陶瓷框架的方法。所述溶液包括溶剂、金属盐和Mn范围为1000至200000的聚乙二醇。
目前的牙科氧化锆陶瓷制品着色溶液主要存在以下问题：着色溶液一般均含第一过渡系金属元素，如Fe、Mn等，易导致着色不均匀；第一过渡系金属元素一般只能存在于晶界内；着色离子存在于晶界，会降低牙科氧化锆制品的透光性，若存在于晶界的着色离子的含量高，还可能会降低牙科氧化锆制品的强度。另外，为防止着色离子从溶液中沉淀出来，提高着色溶液的稳定性，需添加络合剂或增大着色溶液中酸的浓度。
发明内容
本发明针对上述现有技术中存在的问题，提供了一种用于牙科氧化锆陶瓷制品的着色溶液，解决了现有技术中着色不均匀，透光性差的问题，而且本发明强度高，无需添加络合剂或增大着色溶液中酸的浓度。
本发明的另一目的在于提供一种用于牙科氧化锆陶瓷制品的着色溶液的使用方法。
本发明的技术方案如下：
着色溶液由着色剂、溶剂和添加剂组成；
着色剂为稀土金属离子，所述稀土金属离子在溶液中的含量为 0.05~3摩尔/升溶剂；
添加剂含量为0~50wt%。
所述着色剂是包括金属阳离子和阴离子的可溶性盐，其中所述的阳离子包括镨离子、铒离子、钕离子、铈离子、钐离子、铕离子、钆离子、铽离子、镝离子、钬离子、铥离子；所述的阴离子包括氯离子、醋酸根、硝酸根、硫氰根、硫酸根。
所述的溶剂以能溶解所选着色剂为最低标准，可单独或混合使用水、醇类溶剂；所述的醇类选用在水中溶解度较大的小分子醇，小分子醇包括甲醇、乙醇、异丙醇、正丙醇、丙三醇、乙二醇。
所述添加剂为在烧结后无任何有害残留物的纯有机物质，所述的添加剂包括触变剂；所述的触变剂包括多糖、聚乙烯醇、聚乙二醇。
所述添加剂包括表面活性剂，表面活性剂包括辛基酚聚氧乙烯醚、壬基酚聚氧乙烯醚、高碳脂肪醇聚氧乙烯醚、 脂肪酸聚氧乙烯酯、聚氧乙烯胺。
本发明还涉及使用着色溶液处理经过预烧结的氧化锆坯体制备仿牙色的牙科陶瓷制品的方法，该方法主要包括以下步骤：
步骤1：准备本发明中所述的着色溶液和经过预烧结的氧化锆坯体；
步骤2：用着色溶液处理氧化锆坯体；
步骤3：对经过处理的氧化锆坯体进行干燥；
步骤4：将经过干燥的氧化锆坯体高温烧结。
所述的步骤2中处理氧化锆坯体的方法是将氧化锆坯体浸泡到着色溶液中或将着色溶液涂刷、喷涂、漆涂到氧化锆坯体，或通过使用海绵将溶液施加到制品，上述不同处理方式单独使用或结合使用。
所述的步骤3中干燥方式为常温干燥、红外干燥、冷冻干燥或微波干燥的方式。
所述的步骤4中烧结温度一般为1300～1700℃，优选于1480～1600℃，保温时间为0.5～3h，优选于2h。
本发明的优点效果如下：
1.现市售的牙科氧化锆陶瓷制品的着色溶液一般均含第一过渡系金属元素，如Fe、Mn等，与第一过渡系金属元素相比，稀土元素离子半径大，可以具有的配位基相对较多，有可能导致着色离子在牙科氧化锆制品中，使牙科氧化锆制品着色更均匀；
2.与第一过渡系金属元素相比，稀土元素离子与锆离子半径接近，可具有的配位数接近，而且稀土元素相应的氧化物结构与氧化锆相似，导致着色离子经过高温烧结后固溶于氧化锆晶格内，而第一过渡系金属元素一般只能存在于晶界内；着色离子存在于晶界，会降低牙科氧化锆制品的透光性，若存在于晶界的着色离子的含量高，还可能会降低牙科氧化锆制品的强度。
3.与第一过渡系金属元素相比（主要指现市售的牙科氧化锆陶瓷制品的着色溶液中所含的Fe元素），稀土元素离子水解所需溶液的PH值相对较高，无需添加具有防止着色剂从溶液中沉淀出来，使溶液在储存期间保持稳定作用的络合剂或者增大着色溶液中酸的浓度。
4.着色离子均为稀土元素离子的着色溶液，着色离子固溶于氧化锆晶格内，有可能导致氧化锆由四方相转变为立方相，立方相的存在，可以提高牙科氧化锆制品的透光性。
具体实施方式
实施例1
着色溶液由着色剂、溶剂和添加剂组成；所述的着色剂为Pr(NO3)3 0.005摩尔/升溶剂和Er(NO3)3 0.060摩尔/升溶剂；所述溶剂为水；所述的添加剂为PEG ，PEG含量为10 wt%。
本发明还涉及使用着色溶液处理经过预烧结的氧化锆坯体制备仿牙色的牙科陶瓷制品的方法，该方法主要包括以下步骤：
步骤1：准备本发明中所述的着色溶液和经过预烧结的氧化锆坯体；
步骤2：用着色溶液涂刷氧化锆坯体；
步骤3：对经过处理的氧化锆坯体进行红外干燥；
步骤4：将经过干燥的氧化锆坯体高温烧结1600℃，保温时间为1.5h。
实施例2
着色溶液由着色剂、溶剂和添加剂组成；所述的着色剂为PrCl3 0.009摩尔/升溶剂、ErCl3 0.153摩尔/升溶剂和NdCl3 0.027摩尔/升溶剂；所述溶剂为水；所述的添加剂为蔗糖，蔗糖含量为30 wt%。
本发明还涉及使用着色溶液处理经过预烧结的氧化锆坯体制备仿牙色的牙科陶瓷制品的方法，该方法主要包括以下步骤：
步骤1：准备本发明中所述的着色溶液和经过预烧结的氧化锆坯体；
步骤2：使用海绵将着色溶液施加到氧化锆坯体；
步骤3：对经过处理的氧化锆坯体进行冷冻干燥；
步骤4：将经过干燥的氧化锆坯体高温烧结，烧结温度1300℃，保温时间为3h。
实施例3
着色溶液由着色剂、溶剂和添加剂组成；所述的着色剂为PrAc3 0.015摩尔/升溶剂、ErAc3 0.252摩尔/升溶剂和NdAc3 0.107摩尔/升溶剂；所述溶剂为水；所述的添加剂为PEG ，PEG含量为25 wt%。
本发明还涉及使用着色溶液处理经过预烧结的氧化锆坯体制备仿牙色的牙科陶瓷制品的方法，该方法主要包括以下步骤：
步骤1：准备本发明中所述的着色溶液和经过预烧结的氧化锆坯体；
步骤2：用着色溶液处理氧化锆坯体；处理氧化锆坯体的方法是将氧化锆坯体浸泡到着色溶液中；
步骤3：对经过处理的氧化锆坯体进行常温干燥；
步骤4：将经过干燥的氧化锆坯体高温烧结，烧结温度1480℃，保温时间为2h。
实施例4
着色溶液由着色剂、溶剂和添加剂组成；所述的着色剂为Pr(NO3)3 0.018摩尔/升溶剂、Er(NO3)3 0.262摩尔/升溶剂和Nd(NO3)3 0.092摩尔/升溶剂；所述溶剂为水；所述的添加剂为PEG ，PEG含量为20 wt%。
本发明还涉及使用着色溶液处理经过预烧结的氧化锆坯体制备仿牙色的牙科陶瓷制品的方法，该方法主要包括以下步骤：
步骤1：准备本发明中所述的着色溶液和经过预烧结的氧化锆坯体；
步骤2：用着色溶液涂刷氧化锆坯体，再用着色溶液喷涂氧化锆坯体；
步骤3：对经过处理的氧化锆坯体进行微波干燥；
步骤4：将经过干燥的氧化锆坯体高温烧结，烧结温度1700℃，保温时间为0.5 h。
实施例5
着色溶液由着色剂、溶剂和添加剂组成；所述的着色剂为PrCl3 0.035摩尔/升溶剂、ErCl3 0.438摩尔/升溶剂和NdCl3 0.211摩尔/升溶剂；所述溶剂为水；所述的添加剂为PEG ，PEG含量为15 wt%。
实施例6
着色溶液由着色剂和溶剂组成；所述的着色剂为醋酸镝 0.542摩尔/升溶剂、醋酸钬 1.339摩尔/升溶剂和醋酸铥 0.228摩尔/升溶剂；所述溶剂为丙三醇。
实施例7
着色溶液由着色剂、溶剂和添加剂组成；所述的着色剂为硫酸铈 1.230摩尔/升溶剂、硫酸钆 0.635摩尔/升溶剂和硫酸铽 1.135摩尔/升溶剂；所述溶剂为乙二醇；所述的添加剂为聚乙烯醇和辛基酚聚氧乙烯醚，聚乙烯醇含量为30 wt%，辛基酚聚氧乙烯醚含量为0.2wt%。
实施例8
着色溶液由着色剂、溶剂和添加剂组成；所述的着色剂为硫氰化铈 1.031摩尔/升溶剂、硫氰化铕 0.125摩尔/升溶剂和硫氰化钕 1.335摩尔/升溶剂；所述溶剂为甲醇和水；所述的添加剂为PEG和聚氧乙烯胺，PEG含量为15 wt%，聚氧乙烯胺含量为0.1wt%。
所述着色剂是包括金属阳离子和阴离子的可溶性盐，其中所述的阳离子包括镨离子、铒离子、钕离子、铈离子、钐离子、铕离子、钆离子、铽离子、镝离子、钬离子、铥离子；所述的阴离子包括氯离子、醋酸根、硝酸根、硫氰根、硫酸根。
所述的溶剂以能溶解所选着色剂为最低标准，可单独或混合使用水、醇类溶剂；所述的醇类选用在水中溶解度较大的小分子醇，小分子醇包括甲醇、乙醇、异丙醇、正丙醇、丙三醇、乙二醇。
所述添加剂为在烧结后无任何有害残留物的纯有机物质，所述的添加剂包括触变剂，所述的触变剂包括多糖、聚乙烯醇、聚乙二醇；所述的添加剂包括表面活性剂，所述的表面活性剂包括辛基酚聚氧乙烯醚、壬基酚聚氧乙烯醚、高碳脂肪醇聚氧乙烯醚、脂肪酸聚氧乙烯酯、聚氧乙烯胺等。
表1
注：通过比较反射率对比度可以间接比较透光性，反射率对比度数值越大，透光性越差。

Claims (9)

1.用于牙科氧化锆陶瓷制品的着色溶液，其特征在于着色溶液由着色剂、溶剂和添加剂组成；着色剂为稀土金属离子，所述稀土金属离子在溶液中的含量为 0.05~3摩尔/升溶剂；
添加剂含量为0~50wt%。
2.根据权利要求1所述的用于牙科氧化锆陶瓷制品的着色溶液，其特征在于所述着色剂是包括金属阳离子和阴离子的可溶性盐，其中所述的阳离子包括镨离子、铒离子、钕离子、铈离子、钐离子、铕离子、钆离子、铽离子、镝离子、钬离子、铥离子；所述的阴离子包括氯离子、醋酸根、硝酸根、硫氰根、硫酸根。
3.根据权利要求1所述的用于牙科氧化锆陶瓷制品的着色溶液，其特征在于所述的溶剂以能溶解所选着色剂为最低标准，可单独或混合使用水、醇类溶剂；所述的醇类选用在水中溶解度较大的小分子醇，小分子醇包括甲醇、乙醇、异丙醇、正丙醇、丙三醇、乙二醇。
4.根据权利要求1所述的用于牙科氧化锆陶瓷制品的着色溶液，其特征在于所述添加剂为在烧结后无任何有害残留物的纯有机物质，所述的添加剂包括触变剂，所述的触变剂包括多糖、聚乙烯醇、聚乙二醇。
5.根据权利要求1所述的用于牙科氧化锆陶瓷制品的着色溶液，其特征在于所述添加剂包括表面活性剂，所述的表面活性剂包括辛基酚聚氧乙烯醚、壬基酚聚氧乙烯醚、高碳脂肪醇聚氧乙烯醚、脂肪酸聚氧乙烯酯、聚氧乙烯胺。
6.根据权利要求1所述的用于牙科氧化锆陶瓷制品的着色溶液的使用方法，其特征在于包括以下步骤：
步骤1：准备本发明中所述的着色溶液和经过预烧结的氧化锆坯体；
步骤2：用着色溶液处理氧化锆坯体；
步骤3：对经过处理的氧化锆坯体进行干燥；
步骤4：将经过干燥的氧化锆坯体高温烧结。
7.根据权利要求6所述的用于牙科氧化锆陶瓷制品的着色溶液的使用方法，其特征在于所述的步骤2中处理氧化锆坯体的方法是将氧化锆坯体浸泡到着色溶液中或将着色溶液涂刷、喷涂、漆涂到氧化锆坯体，或通过使用海绵将溶液施加到制品，上述不同处理方式单独使用或结合使用。
8.根据权利要求6所述的用于牙科氧化锆陶瓷制品的着色溶液的使用方法，其特征在于所述的步骤3中干燥方式为常温干燥、红外干燥、冷冻干燥或微波干燥的方式。
9.根据权利要求6所述的用于牙科氧化锆陶瓷制品的着色溶液的使用方法，其特征在于所述的步骤4中烧结温度一般为1300～1700℃，优选于1480～1600℃，保温时间为0.5～3h，优选于2h。
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PT13791600T PT2850043T (pt) 2012-05-15 2013-04-28 Solução colorante para cerâmica de zircónia dentária e método para utilizar a mesma
KR1020147031997A KR101691575B1 (ko) 2012-05-15 2013-04-28 치아 지르코니아 세라믹용 착색 용액 및 이를 사용하는 방법
EP13791600.3A EP2850043B1 (en) 2012-05-15 2013-04-28 Coloring solution for dental zirconia ceramics and method for using the same
PCT/CN2013/074962 WO2013170705A1 (en) 2012-05-15 2013-04-28 Coloring solution for dental zirconia ceramics and method for using the same
US14/397,449 US9554881B2 (en) 2012-05-15 2013-04-28 Coloring solution for dental zirconia ceramics and method for using the same
DK13791600.3T DK2850043T3 (da) 2012-05-15 2013-04-28 Farveopløsning til dental zirconiumkeramik og fremgangsmåde til anvendelse heraf
ES13791600T ES2744715T3 (es) 2012-05-15 2013-04-28 Solución de coloración para materiales cerámicos dentales de circonia y método de uso de los mismos

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CN111732449A (zh) * 2020-06-22 2020-10-02 嘉兴饶稷科技有限公司 一种氧化锆陶瓷牙冠三维染色用染色剂和染色方法
CN113105754A (zh) * 2020-10-10 2021-07-13 深圳爱尔创口腔技术有限公司 氧化锆牙科制品染色液、氧化锆牙科制品的制备方法和氧化锆牙科制品
CN115124338A (zh) * 2022-06-27 2022-09-30 潮州三环（集团）股份有限公司 一种彩色涂层浆料、彩色氧化锆陶瓷及其制备方法
CN115124338B (zh) * 2022-06-27 2023-02-28 潮州三环（集团）股份有限公司 一种彩色涂层浆料、彩色氧化锆陶瓷及其制备方法
CN115820042A (zh) * 2023-02-24 2023-03-21 山东新华医疗器械股份有限公司 氧化锆义齿的染色液及其染色工艺

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CN103113132A (zh) 2013-05-22
DK2850043T3 (da) 2019-09-23
WO2013170705A1 (en) 2013-11-21
EP2850043A4 (en) 2016-01-27
ES2744715T3 (es) 2020-02-26
US9554881B2 (en) 2017-01-31
EP2850043A1 (en) 2015-03-25
US20150122147A1 (en) 2015-05-07
KR20150008876A (ko) 2015-01-23

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