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CN106396676A - 透光性氧化锆烧结体及其制备方法与应用 - Google Patents

透光性氧化锆烧结体及其制备方法与应用 Download PDF

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Publication number
CN106396676A
CN106396676A CN201610793418.1A CN201610793418A CN106396676A CN 106396676 A CN106396676 A CN 106396676A CN 201610793418 A CN201610793418 A CN 201610793418A CN 106396676 A CN106396676 A CN 106396676A
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Prior art keywords
sintered body
zirconium oxide
powder
powder body
light transmittance
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CN201610793418.1A
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杨爱民
莫学魁
宋锡滨
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Shandong Sinocera Functional Material Co Ltd
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Shandong Sinocera Functional Material Co Ltd
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Priority to CN201610793418.1A priority Critical patent/CN106396676A/zh
Publication of CN106396676A publication Critical patent/CN106396676A/zh
Priority to US16/329,637 priority patent/US20190231650A1/en
Priority to PCT/CN2017/095746 priority patent/WO2018040834A1/zh
Pending legal-status Critical Current

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Abstract

本发明提供一种新型的透光性氧化锆烧结体，其是将透光性氧化锆烧结体用粉体经等静压成型制成生坯，生坯经脱脂素烧后，在常压大气中进行高温烧结制得的。所述透光性氧化锆烧结体是将氧化锆粉料分散于水中，添加适量分散剂和粘合剂，混匀形成浆料，再通过喷雾造粒的方式制得的；其中，氧化锆粉料中氧化钇的摩尔百分比为3‑5％。本发明的透光性氧化锆烧结体可用于制备牙科固定修复体。本发明提供的氧化锆烧结体具有高透光性、高强度的特点，所制备的义齿质感强、玉感好，与人类牙齿接近。

Description

透光性氧化锆烧结体及其制备方法与应用
技术领域
本发明涉及粉体工程领域，具体地说，涉及一种透光性氧化锆烧结体及其制备方法与应用。
背景技术
氧化锆陶瓷是一种新型的生物粉体，具有良好的生物相容性、优良的力学性能，已成为齿科陶瓷开发的重点。
CN 104016677A公开了一种透光性氧化锆烧结体及其制备方法，该方法制备出的齿科用氧化锆透性较低，整体质感及玉感较差，不够美观，应用具有一定的局限性。
发明内容
本发明的目的是提供一种新型的透光性氧化锆烧结体及其制备方法。
本发明的另一目的是提供所述透光性氧化锆烧结体在制备牙科固定修复体中的应用。
为了实现本发明目的，本发明首先提供一种透光性氧化锆烧结体用粉体，所述粉体是将氧化锆粉料分散于水(纯水)中，添加适量分散剂和粘合剂，混匀形成浆料，再通过喷雾造粒的方式制得的。造粒时粉体水分控制在0.1-0.5wt％，造粒颗粒的平均粒径为30-50μm。
其中，氧化锆粉料中氧化钇的摩尔百分比为3-5％；所述分散剂包括丙烯酸、聚丙烯酸、丙烯酰胺、聚氨酯等中的至少一种；所述粘合剂包括聚乙烯醇、聚乙二醇、丙烯酸树脂、羧甲基纤维素等中的至少一种。
本发明所用氧化锆粉料的比表面积BET为5-15m2/g，平均粒径为0.1-1.0μm。
可采用水热合成法制备所述氧化锆粉料，包括以下步骤：
S1、将可溶性锆盐和钇盐按照比例混合溶于水，搅拌条件下用氨水调浆料pH至8-10；
S2、将上述浆料于140-200℃水热合成10-72h；
S3、将上述所得反应溶液经水洗、干燥得粉体；
S4、上述粉体经800-1200℃热处理2-5h后进行研磨分散；
S5、将分散好的颗粒进行造粒，即得透光性氧化锆烧结体用粉末；
S1中，可溶性锆盐和钇盐的摩尔比为95-97：3-5，优选96：4。所述可溶性锆盐包括氧氯化锆、硝酸锆、硫酸锆等；所述可溶性钇盐包括氯化钇、硝酸钇、硫酸钇等。
用于制备本发明所述透光性氧化锆烧结体用粉体的各物料重量份如下：氧化锆粉料50-100份，分散剂0.1-0.5份，粘合剂0.1-8.0份和水50-100份。优选地，各物料重量份如下：氧化锆粉料100份，分散剂0.2份，粘合剂5份和水100份。
本发明还提供由所述粉体制备的透光性氧化锆烧结体。所述烧结体的三点抗弯强度≥900Mpa，四方相所占烧结体比例＞90％，透光率≥46％，烧结前后物料收缩率控制在18-25％。
本发明所述透光性氧化锆烧结体，可以按照以下方法制备得到：所述粉体经等静压(150-200MPa保压10-50s)成型制成生坯，生坯在900-1100℃脱脂素烧1-4h，然后在常压大气中于1400-1550℃进行高温烧结，时间为1-4h，即得。
前述的方法，经等静压后生坯的密度为2.5-3.3g/cm3。
本发明还提供所述透光性氧化锆烧结体在制备牙科固定修复体(包括义齿)中的应用。
本发明进一步提供由所述透光性氧化锆烧结体制备的牙科固定修复体。例如，氧化锆义齿。
本发明提供的氧化锆烧结体具有高透光性、高强度的特点，所制备的义齿质感强、玉感好，与人类牙齿接近。制备工艺所采用的烧结温度低，产品性状及品质可控。
具体实施方式
以下实施例用于说明本发明，但不用来限制本发明的范围。若未特别指明，实施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，所用原料均为市售商品。
本发明中涉及到的百分号“％”，若未特别说明，是指质量百分比；但溶液的百分比，除另有规定外。
实施例1-5透光性氧化锆烧结体用粉体
本发明的透光性氧化锆烧结体用粉体可按照以下方法制备得到：将氧化锆粉料分散于纯水中，添加适量分散剂和粘合剂，混匀形成浆料，再通过喷雾造粒的方式得到粉体，用于制备透光性氧化锆烧结体。(表1)
表1透光性氧化锆烧结体用粉体
采用水热合成法制备所述氧化锆粉料，包括以下步骤：
S1、将可溶性锆盐(硝酸锆)和钇盐(硝酸钇)按比例混合溶于水，搅拌条件下缓慢加入氨水，用氨水调浆料pH至8-10；
S2、将上述浆料转移至反应釜中，于140-200℃水热合成10-72h；
S3、将上述所得反应溶液经水洗、干燥得粉体；
S4、上述粉体经800-1200℃热处理2-5h后进行研磨分散；
S5、将分散好的颗粒进行造粒，即得透光性氧化锆烧结体用粉末。
实施例6-10透光性氧化锆烧结体及其制备方法
实施例1-5制备的粉体经等静压(150-200MPa保压10-50s)成型制成生坯，生坯在900-1100℃脱脂素烧1-4h，然后在常压大气中于1400-1550℃进行高温烧结，时间为1-4h，制得透光性氧化锆烧结体。
所得烧结体产品的各项指标见表2。
表2透光性氧化锆烧结体产品指标
本发明提供的透光性氧化锆烧结体可用于牙科固定修复体等齿科粉体，例如义齿。
虽然，上文中已经用一般性说明及具体实施方案对本发明作了详尽的描述，但在本发明基础上，可以对之作一些修改或改进，这对本领域技术人员而言是显而易见的。因此，在不偏离本发明精神的基础上所做的这些修改或改进，均属于本发明要求保护的范围。

Claims (10)

1.透光性氧化锆烧结体用粉体，其特征在于，所述粉体是将氧化锆粉料分散于水中，添加适量分散剂和粘合剂，混匀形成浆料，再通过喷雾造粒的方式制得的；
其中，氧化锆粉料中氧化钇的摩尔百分比为3-5％；所述分散剂所述分散剂包括丙烯酸、聚丙烯酸、丙烯酰胺、聚氨酯中的至少一种；所述粘合剂包括聚乙烯醇、聚乙二醇、丙烯酸树脂、羧甲基纤维素中的至少一种。
2.根据权利要求1所述的粉体，其特征在于，所述氧化锆粉料的比表面积BET为5-15m2/g，平均粒径为0.1-1.0μm。
3.根据权利要求1或2所述的粉体，其特征在于，所述氧化锆粉料经水热合成法制得，包括以下步骤：
S1、将可溶性锆盐和钇盐按照比例混合溶于水，搅拌条件下用氨水调浆料pH至8-10；
S2、将上述浆料于140-200℃水热合成10-72h；
S3、将上述所得反应溶液经水洗、干燥得粉体；
S4、上述粉体经800-1200℃热处理2-5h后进行研磨分散；
S5、将分散好的颗粒进行造粒，即得透光性氧化锆烧结体用粉末；
S1中，可溶性锆盐和钇盐的摩尔比为95-97：3-5，优选96：4。
4.权利要求1-3任一项所述的粉体，其特征在于，用于制备所述粉体的各物料重量份如下：氧化锆粉料50-100份，分散剂0.1-0.5份，粘合剂0.1-8.0份和水50-100份。
5.权利要求1-4任一项所述的粉体，其特征在于，造粒时粉体水分控制在0.1-0.5wt％，造粒颗粒的平均粒径为30-50μm。
6.由权利要求1-5任一项所述粉体制备的透光性氧化锆烧结体。
7.根据权利要求6所述的烧结体，其特征在于，所述烧结体的三点抗弯强度≥900Mpa，四方相所占烧结体比例＞90％，透光率≥46％，烧结前后物料收缩率控制在18-25％。
8.权利要求6或7所述烧结体的制备方法，其特征在于，所述粉体经等静压成型制成生坯，生坯在900-1100℃脱脂素烧1-4h，然后在常压大气中于1400-1550℃进行高温烧结，时间为1-4h，即得。
9.根据权利要求8所述的方法，其特征在于，所述等静压条件为：150-200MPa，保压10-50s；经等静压后生坯的密度为2.5-3.3g/cm3。
10.权利要求6或7所述烧结体在制备牙科固定修复体中的应用。
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