WO2018040835A1 - 高透光性氧化锆烧结体及其制备方法与应用 - Google Patents

高透光性氧化锆烧结体及其制备方法与应用 Download PDF

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WO2018040835A1
WO2018040835A1 PCT/CN2017/095747 CN2017095747W WO2018040835A1 WO 2018040835 A1 WO2018040835 A1 WO 2018040835A1 CN 2017095747 W CN2017095747 W CN 2017095747W WO 2018040835 A1 WO2018040835 A1 WO 2018040835A1
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sintered body
powder
zirconia
zirconia sintered
parts
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PCT/CN2017/095747
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English (en)
French (fr)
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杨爱民
莫雪魁
宋锡滨
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山东国瓷功能材料股份有限公司
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Publication of WO2018040835A1 publication Critical patent/WO2018040835A1/zh
Priority to US16/289,369 priority Critical patent/US10759708B2/en

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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9646—Optical properties
    • C04B2235/9653—Translucent or transparent ceramics other than alumina
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts

Definitions

  • the present invention first provides a material for a highly transparent zirconia sintered body which is prepared by adding an appropriate amount of water to a zirconia powder for grinding, and adding ⁇ -oxidation during the grinding process.
  • the aluminum powder is then subjected to spray granulation to obtain a powder material having an average particle diameter of 0.1 to 0.4 ⁇ m.
  • Example 1-5 The powder prepared in Example 1-5 was subjected to dry pressing molding (molding pressure: 150 to 250 MPa), and then sintered at 1400 to 1550 ° C in a normal pressure atmosphere for a period of 1-4 h to obtain a highly transparent zirconia sintered body.
  • the indexes of the obtained sintered body products are shown in Table 2.

Abstract

一种高透光性氧化锆烧结体，其是将高透光性氧化锆烧结体用材料加工成型，然后在常压大气中进行高温烧结制得的。高透光性氧化锆烧结体用材料是由氧化锆粉料和α-氧化铝为原料制成；其中，氧化锆粉料中氧化钇的摩尔百分比为4-6%。高透光性氧化锆烧结体可用于制备牙科固定修复体。氧化锆烧结体，其晶粒大小为0.1-0.7μm，且通过氧化铝的弥散增韧，氧化锆烧结体具有较高的强度和韧性；添加氧化铝可排除氧化锆粉料内的气孔，氧化锆烧结体具有较高的光学透性，所制备的义齿质感强、玉感好，与人类牙齿更接近。

Description

高透光性氧化锆烧结体及其制备方法与应用
相关申请的交叉引用
本发明要求2016年8月31日提交、申请号为201610793366.8的中国专利申请的优先权，其所公开的内容作为参考全文并入本申请。
技术领域
本发明涉及材料工程领域，具体地说，涉及一种高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材料，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。ZL201010604330.3公开了牙科用高透氧化锆材料及制备工艺，其采用干混工艺制备氧化锆，易导致氧化锆强度分布不均匀且强度偏低，陶瓷烧结体应用时容易出现开裂现象。
发明内容
本发明的目的是提供一种新型的高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高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高透光性氧化锆烧结体用材料，所述材料按如下方法制备：向氧化锆粉料中加入适量水进行研磨，研磨过程中添加α-氧化铝粉体，然后通过喷雾造粒的方式得到平均粒径为0.1-0.4μm的粉体材料。
其中，氧化锆粉料中氧化钇的摩尔百分比为4-6％。
所述α-氧化铝粉体的比表面积BET为5-16m2/g。
所述氧化锆粉料的比表面积BET为8-16m2/g，平均粒径为0.1-0.4μm。
所述氧化锆粉料的制备方法如下：
S1、将可溶性锆盐和钇盐按照比例混合溶于水，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，即得高透光性氧化锆烧结体用粉末；
步骤S1中，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。可溶性锆盐和钇盐的摩尔比为94-96：4-6，优选95：5。
在制备所述材料时，还包括向所述氧化锆和α-氧化铝的混合料中添加分散剂和粘合剂的步骤。
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。
用于制备本发明所述高透光性氧化锆烧结体用材料的各物料重量份如下：氧化锆粉料50-100份，α-氧化铝粉体0.01-0.1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，α-氧化铝粉体0.1份，分散剂0.2份，粘合剂5份和水100份。
本发明所述高透光性氧化锆烧结体用材料，可以按照以下方法制备得到：向氧化锆粉料中加入适量水进行研磨，研磨过程中添加α-氧化铝粉体，水和氧化铝浆料搅拌分数5-30min，然后通过喷雾造粒 的方式得到平均粒径为0.1-0.4μm的粉体材料，用于制备高透光性氧化锆烧结体。
本发明还提供由所述材料制备的高透光性氧化锆烧结体。所述烧结体1mm厚度瓷片的直线透过率>47％，三点抗弯强度>600Mpa，所得烧结体晶粒大小为0.1-0.7μm，且由于氧化铝的弥散增韧作用，韧性较好，所述烧结体在140℃20h老化条件下，老化后烧结体的单斜相＜10％，抗老化性能优异。
本发明所述高透光性氧化锆烧结体，可以按照以下方法制备得到：将所述高透光性氧化锆烧结体用材料加工成型，然后在常压大气中进行高温烧结，即得。例如，将高温烧结时的温度保持在1400-1550℃，时间为1-4h。
本发明还提供所述高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高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，其晶粒大小为0.1-0.7μm，且通过氧化铝的弥散增韧作用，氧化锆烧结体具有较高的强度和韧性；添加氧化铝可排除氧化锆粉料内的气孔，氧化锆烧结体具有较高的光学透性，所制备的义齿质感强、玉感好，与人类牙齿更接近。
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。
以下实施例中所用α-氧化铝粉体比表面积BET为5-16m2/g。
实施例1-5 高透光性氧化锆烧结体用材料
本发明的高透光性氧化锆烧结体用材料可以按照以下方法制备得到：向氧化锆粉料中加入适量水进行研磨，研磨过程中添加α-氧化铝粉体，然后通过喷雾造粒的方式得到平均粒径为0.1-0.4μm的粉体材料，用于制备高透光性氧化锆烧结体。(表1)
表1高透光性氧化锆烧结体用粉末
Figure PCTCN2017095747-appb-000001
所述氧化锆粉料的制备方法如下：
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，即得高透光性氧化锆烧结体用粉末。
实施例6-10 高透光性氧化锆烧结体及其制备方法
实施例1-5制备的粉末经干压成型(成型压力150-250MPa)后，在常压大气中，于1400-1550℃进行烧结，时间1-4h制得高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高透光性氧化锆烧结体产品指标
Figure PCTCN2017095747-appb-000002
本发明提供的高透光性氧化锆烧结体可用于牙科固定修复体等齿科材料，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。
工业实用性
本发明提供的氧化锆烧结体，其晶粒大小为0.1-0.7μm，且通过氧化铝的弥散增韧作用，氧化锆烧结体具有较高的强度和韧性；添加氧化铝可排除氧化锆粉料内的气孔，氧化锆烧结体具有较高的光学透性，所制备的义齿质感强、玉感好，与人类牙齿更接近。

Claims (10)

  1. 高透光性氧化锆烧结体用材料，其特征在于，所述材料按如下方法制备：向氧化锆粉料中加入适量水进行研磨，研磨过程中添加α-氧化铝粉体，然后通过喷雾造粒的方式得到平均粒径为0.1-0.4μm的粉体材料；
    其中，氧化锆粉料中氧化钇的摩尔百分比为4-6％。
  2. 根据权利要求1所述的材料，其特征在于，所述氧化锆粉料的比表面积BET为8-16m2/g，平均粒径为0.1-0.4μm；
    所述氧化锆粉料的制备方法如下：
    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，即得高透光性氧化锆烧结体用粉末；
    步骤S1中，可溶性锆盐和钇盐的摩尔比为94-96：4-6，优选95：5。
  3. 根据权利要求1或2所述的材料，其特征在于，所述α-氧化铝粉体比表面积BET为5-16m2/g。
  4. 根据权利要求1-3任一项所述的材料，其特征在于，制备所述材料时，还包括向所述氧化锆和α-氧化铝的混合料中添加分散剂和粘合剂的步骤；
    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。
  5. 根据权利要求4所述的材料，其特征在于，用于制备所述材 料的各物料重量份如下：氧化锆粉料50-100份，α-氧化铝粉体0.01-0.1份，分散剂0.1-0.5份，粘合剂0.1-8.0份和水50-100份。
  6. 由权利要求1-5任一项所述材料制备的高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1mm厚度瓷片的直线透过率>47％，三点抗弯强度>600Mpa，所述烧结体在140℃ 20h老化条件下，老化后烧结体的单斜相＜10％。
  8. 权利要求6或7所述烧结体的制备方法，其特征在于，将所述材料加工成型，然后在常压大气中进行高温烧结，即得。
  9. 根据权利要求8所述的方法，其特征在于，高温烧结时的温度保持在1400-1550℃，时间为1-4h。
  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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