WO2018040834A1 - 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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WO2018040834A1
WO2018040834A1 PCT/CN2017/095746 CN2017095746W WO2018040834A1 WO 2018040834 A1 WO2018040834 A1 WO 2018040834A1 CN 2017095746 W CN2017095746 W CN 2017095746W WO 2018040834 A1 WO2018040834 A1 WO 2018040834A1
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Prior art keywords
powder
sintered body
zirconia
zirconia sintered
light
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PCT/CN2017/095746
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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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Priority to US16/329,637 priority Critical patent/US20190231650A1/en
Publication of WO2018040834A1 publication Critical patent/WO2018040834A1/zh

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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00—Dental prostheses; Making same
    • A61C13/0003—Making bridge-work, inlays, implants or the like
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61C13/00—Dental prostheses; Making same
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    • A61C13/0022—Blanks or green, unfinished dental restoration parts
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Definitions

  • the present invention relates to the field of powder engineering, and in particular to a translucent zirconia sintered body and a preparation method and application thereof.
  • Zirconia ceramic is a new type of biological powder with good biocompatibility and excellent mechanical properties, which has become the focus of dental ceramic development.
  • CN 104016677A discloses a translucent zirconia sintered body and a preparation method thereof.
  • the zirconia for dental preparation prepared by the method has low permeability, poor overall texture and jade feeling, is not aesthetically pleasing, and has certain limitations in application. .
  • An object of the present invention is to provide a novel light-transmitting zirconia sintered body and a method of producing the same.
  • Another object of the present invention is to provide an application of the light-transmitting zirconia sintered body in the preparation of a dental fixed restoration.
  • the present invention first provides a powder for a light-transmitting zirconia sintered body, which is obtained by dispersing a zirconia powder in water (pure water), adding an appropriate amount of a dispersant and a binder. It is mixed to form a slurry and then obtained by spray granulation.
  • the powder moisture is controlled to be 0.1 to 0.5% by weight at the time of granulation, and the granulated particles have an average particle diameter of 30 to 50 ⁇ m.
  • the molar percentage of cerium oxide in the zirconia powder is 3-5%;
  • the dispersing agent comprises at least one of acrylic acid, polyacrylic acid, acrylamide, polyurethane, etc.;
  • the binder comprises polyvinyl alcohol, poly In ethylene glycol, acrylic resin, carboxymethyl cellulose, etc. One less.
  • the zirconia powder used in the present invention has a specific surface area BET of 5 to 15 m 2 /g and an average particle diameter of 0.1 to 1.0 ⁇ m.
  • the zirconia powder can be prepared by hydrothermal synthesis, and includes the following steps:
  • the soluble zirconium salt and the cerium salt are mixed and dissolved in water according to the ratio, and the pH of the slurry is adjusted to 8-10 with ammonia water under stirring;
  • the above slurry is hydrothermally synthesized at 140-200 ° C for 10-72h;
  • the powder is heat-treated at 800-1200 ° C for 2-5 hours, and then ground and dispersed;
  • the molar ratio of the soluble zirconium salt to the onium salt is from 95 to 97:3-5, preferably 96:4.
  • the soluble zirconium salt includes zirconium oxychloride, zirconium nitrate, zirconium sulfate, and the like; and the soluble cerium salt includes cerium chloride, cerium nitrate, cerium sulfate, and the like.
  • each material used for preparing the powder for a transparent zirconia sintered body of the present invention are as follows: 50-100 parts of zirconia powder, 0.1-0.5 parts of dispersant, 0.1-8.0 parts of binder and water 50. -100 copies.
  • the parts by weight of each material are as follows: 100 parts of zirconia powder, 0.2 parts of dispersant, 5 parts of binder and 100 parts of water.
  • the present invention also provides a light-transmitting zirconia sintered body prepared from the powder.
  • the three-point bending strength of the sintered body is ⁇ 900Mpa
  • the ratio of the square body to the sintered body is >90%
  • the light transmittance is ⁇ 46%
  • the material shrinkage rate before and after sintering is controlled at 18-25%.
  • the translucent zirconia sintered body of the invention can be prepared according to the following method: the powder is formed into a green body by isostatic pressing (150-200 MPa holding pressure 10-50 s), and the green body is at 900-1100 ° C. The defattin is burned for 1-4 hours, and then sintered at a high temperature at 1400-1550 ° C in a normal pressure atmosphere for 1-4 h.
  • the density of the green body after isostatic pressing is 2.5-3.3 g/cm 3 .
  • the present invention also provides the use of the translucent zirconia sintered body in the preparation of a dental fixed prosthesis (including dentures).
  • the present invention further provides a dental fixed prosthesis prepared from the translucent zirconia sintered body.
  • a dental fixed prosthesis prepared from the translucent zirconia sintered body.
  • zirconia dentures for example, zirconia dentures.
  • the zirconia sintered body provided by the invention has the characteristics of high light transmittance and high strength, and the prepared denture has strong texture and good jade feeling, and is close to human teeth.
  • the sintering temperature used in the preparation process is low, and the product properties and quality are controllable.
  • the percent "%" referred to in the present invention means a percentage by mass unless otherwise specified; however, the percentage of the solution, unless otherwise specified.
  • Example 1-5 Powder for a transparent zirconia sintered body
  • the powder for a translucent zirconia sintered body of the present invention can be obtained by dispersing a zirconia powder in pure water, adding an appropriate amount of a dispersant and a binder, mixing to form a slurry, and then forming by spraying.
  • a powder was obtained in the form of a granule for preparing a translucent zirconia sintered body. (Table 1)
  • the preparation of the zirconia powder by hydrothermal synthesis comprises the following steps:
  • the soluble zirconium salt (zirconium nitrate) and the cerium salt (cerium nitrate) are mixed and dissolved in water in proportion, slowly adding ammonia water under stirring, and adjusting the pH of the slurry to 8-10 with ammonia water;
  • the slurry is transferred to a reaction kettle, hydrothermal synthesis at 140-200 ° C for 10-72h;
  • the powder is heat-treated at 800-1200 ° C for 2-5 hours, and then ground and dispersed;
  • Embodiment 6-10 Translucent zirconia sintered body and preparation method thereof
  • the powder prepared in Examples 1-5 was shaped into a green body by isostatic pressing (150-200 MPa holding pressure 10-50 s), and the green body was burned at 900-1100 ° C for 1-4 h, then in a normal pressure atmosphere.
  • the high-temperature sintering was carried out at 1400-1550 ° C for 1-4 h to obtain a light-transmitting zirconia sintered body.
  • the indexes of the obtained sintered body products are shown in Table 2.
  • the translucent zirconia sintered body provided by the present invention can be used for a dental fixed body such as a dental fixed prosthesis, such as a denture.
  • the translucent zirconia sintered body provided by the present invention can be used for preparing a dental fixed prosthesis.
  • the zirconia sintered body provided by the invention has the characteristics of high light transmittance and high strength, and the prepared denture has strong texture and good jade feeling, and is close to human teeth.

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Abstract

一种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。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%。该透光性氧化锆烧结体可用于制备牙科固定修复体。

Description

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201610793418.1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；
步骤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
Figure PCTCN2017095746-appb-000001
Figure PCTCN2017095746-appb-000002
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
Figure PCTCN2017095746-appb-000003
Figure PCTCN2017095746-appb-000004
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。
工业实用性
本发明提供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。

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；
    步骤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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