CN105777168A - 一种ZTA-SiCw陶瓷托槽材料及其制备方法 - Google Patents
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Abstract
本发明提供一种ZTA‑SiCw陶瓷托槽材料及其制备方法。该制备方法的生坯制备过程中利用拟薄水铝石作粘结剂,利用其脱水后得到与Al2O3基体组成相同这一性质,避免了传统热压铸成型中脱蜡工艺给最终样品带来的不利影响,生坯干燥后直接烧结成型,保证了陶瓷托槽的性能稳定性。同时利用拟薄水铝石胶凝特性,将Al2O3颗粒及增强相填充在拟薄水铝石双电层网络结构间隙中,提高堆砌密度,增加成分均匀性,可充分发挥增强相的增韧作用;此外,利用SiC晶须和ZrO2两增强相改善Al2O3基体本身的脆性缺陷,同时SiC晶须的存在能够减轻ZrO2在相变过程中局部大裂纹的贯穿,有效地与ZrO2的增韧起到协同作用。
Description
技术领域
本发明属于口腔正畸材料领域,特别是提供了一种低成本、高强度托槽用ZTA-SiCw陶瓷材料及其制备方法。
背景技术
ZTA陶瓷托槽材料具有优越的生物相容性、耐磨损性、质地致密、表面光洁、菌斑不易附着、使用安全,此外其独特的美学性能是高分子材料和金属材料无法比拟的,深受广大口腔医务人员及患者的青睐。但是现有的全瓷材料也仍然存在着强度不够以及韧性较低等缺陷,在临床使用过程中常常出现断裂问题,给患者带来很大烦恼,且影响矫正进度,还未完全达到临床广泛应用的要求,如何提高陶瓷托槽材料的强韧性是目前陶瓷托槽材料研究的重点。ZTA陶瓷托槽在使用过程中出现的断裂现象仍十分突出的主要原因是氧化锆对氧化铝托槽的增韧效果与制备过程中参数浮动之间的关系存在难以精确调控的问题,如氧化锆、氧化铝或其他分散剂或稳定剂种类、粒度相对关系、配比、混合方式、烧结工艺、相变机制等对最终陶瓷托槽性能的影响以及单一氧化锆增韧作用的有效率等,这些都是陶瓷托槽材料研究中有待探索的基础科学问题。
SiC晶须(SiCw)在陶瓷材料中的增韧作用相较于氧化锆增韧有更加突出的优点,不仅能够抑制氧化铝颗粒的增大,同时能够通过晶须的增韧机制改善氧化铝基体本身的脆性缺陷,与此同时,SiC晶须的存在能够减轻氧化锆在相变过程中局部大裂纹的贯穿,有效地与氧化锆的增韧起到协同作用。
热压铸成型在陶瓷托槽材料生产研究中是一种常用的成型方法。然而,热压铸成型中存在一个非常复杂且对性能影响很大的步骤——脱蜡,脱蜡后在生坯中遗留的缺陷将很大程度上增加制件的成本并降低成品性能。所以,对于生坯来讲,寻求一种生坯烧结尺寸稳定,制备工艺简单的成型方法迫在眉睫。
发明内容
本发明的内容在于提供一种低成本、高强韧的ZTA-SiCw陶瓷托槽材料的制备方法,该方法的特点是无毒性、无须排蜡、无挥发,因而不会对制品造成显微缺陷,具有广泛的应用领域。制备过程包括以下几个步骤:
1)按照设定的固含量,将9wt%的拟薄水铝石、0.3wt%的柠檬酸三铵和70ml蒸馏水加入球磨罐中充分搅拌均匀,然后按照比例加入α-Al2O3和增强相,再次球磨得到流动性较好的料浆。
2)按照的比例配酸,加入浆料中,搅拌测试pH至3~4左右形成稳定凝胶。
3)将浆料取出,制坯干燥(35℃干燥12h,之后60℃干燥24h),最后进行高温烧结,烧结温度为1560℃~1580℃。
如上所述的制备方法,其特征在于,生坯制备过程中利用拟薄水铝石作粘结剂,通过其脱水后得到与氧化铝基体组成相同这一性质,避免了传统热压铸成型中脱蜡工艺给最终样品带来的不利影响,生坯干燥后直接烧结成型,保证了陶瓷托槽的性能稳定性,且所有原料烧结后产物均为陶瓷体。同时利用拟薄水铝石胶凝特性,将Al2O3颗粒及增强相填充在拟薄水铝石双电层网络结构间隙中,提高堆砌密度,增加成分均匀性,可充分发挥增强相的增韧机理。
根据本发明的另一方式设计一种ZTA-SiCw陶瓷托槽材料,其特征在于,该复合材料是纯陶瓷体复合而成,其中ZrO2和SiC晶须两种增强相在复合材料中起到协同增韧的作用。所述的托槽材料抗弯强度可达到398MPa,吸水率低于0.0023%,满足牙科材料要求。
附图说明
图1为本发明的第一实施例所涉及的ZTA-SiCw陶瓷托槽材料的表面SEM。
图2为本发明的第一实施例所涉及的ZTA-SiCw陶瓷托槽材料的断面SEM。
图3为本发明的第一实施例所涉及的ZTA-SiCw陶瓷托槽材料的XRD图谱。
具体实施方式
以下将结合实施例对本发明技术方案做进一步的详述。
实施例1
按照固含量45%,将9%的拟薄水铝石、0.3%的柠檬酸三铵和70ml蒸馏水加入球磨罐中充分搅拌均匀,转数190rad/min,持续80min,然后按照比例加入α-Al2O3、30%的ZrO2、5%的SiCw,再次球磨,转数190rad/min,持续80min,得到流动性较好的料浆;按照的比例配酸,加入浆料中,搅拌测试pH至3~4左右;将浆料取出,制坯干燥(35℃干燥12h,之后60℃干燥24h);之后将生坯进行常压烧结。烧结工艺为:烧结温度为1570℃保温5h,随炉降温。所得陶瓷材料的抗弯强度为397.9032MPa,吸水率为0.0023%。
图1是实施例1的ZTA-SiCw陶瓷托槽材料的表面SEM,根据图1可知,各相分布均匀,体现了拟薄水铝石双电层作用;当烧结温度为1570℃时,由于ZrO2的钉扎作用,一定程度抑制基体Al2O3的过度长大,在此烧结温度下,试样已经达到致密化。图2是实施例1的ZTA-SiCw陶瓷托槽材料的断面SEM,根据图2可知,在断裂面上有SiC晶须拔出现象(图中黑色圆圈所示),它在断裂过程中能够起到增韧作用。图3是实施例1的ZTA-SiCw陶瓷托槽材料的XRD,它验证了托槽材料的相组成。
实施例2
按照固含量45%,将9%的拟薄水铝石、0.3%的柠檬酸三铵和70ml蒸馏水加入球磨罐中充分搅拌均匀,转数190rad/min,持续80min,然后按照比例加入α-Al2O3和25%的ZrO2、3%的SiCw,再次球磨,转数190rad/min,持续80min,得到流动性较好的料浆;按照的比例配酸,加入浆料中,搅拌测试pH至3~4左右;将浆料取出,制坯干燥(35℃干燥12h,之后60℃干燥24h);之后将生坯进行常压烧结。烧结工艺为:烧结温度为1570℃保温5h,随炉降温。所得陶瓷材料的抗弯强度为295.2974MPa,吸水率为0.049%。
实施例3
按照固含量45%,将9%的拟薄水铝石、0.3%的柠檬酸三铵和70ml蒸馏水加入球磨罐中充分搅拌均匀,转数190rad/min,持续80min,然后按照比例加入α-Al2O3、30%的ZrO2、5%的SiCw,再次球磨,转数190rad/min,持续80min,得到流动性较好的料浆;按照的比例配酸,加入浆料中,搅拌测试pH至3~4左右;将浆料取出,制坯干燥(35℃干燥12h,之后60℃干燥24h);之后将生坯进行常压烧结。烧结工艺为:烧结温度为1580℃保温5h,随炉降温。所得陶瓷材料的抗弯强度为347.8MPa。
实施例4
按照固含量45%,将9%的拟薄水铝石、0.3%的柠檬酸三铵和70ml蒸馏水加入球磨罐中充分搅拌均匀,转数190rad/min,持续80min,然后按照比例加入α-Al2O3和25%的ZrO2、5%的SiCw,再次球磨,转数190rad/min,持续80min,得到流动性较好的料浆;按照的比例配酸,加入浆料中,搅拌测试pH至3~4左右;将浆料取出,制坯干燥(35℃干燥12h,之后60℃干燥24h);之后将生坯进行常压烧结。烧结工艺为:烧结温度为1580℃保温5h,随炉降温。所得陶瓷材料的抗弯强度为301MPa,吸水率为0.042%。
根据本发明的ZTA-SiCw陶瓷托槽材料及其制备方法,能得到以下效果。
无毒性、无须排蜡、不易开裂而且还能促进烧结、无挥发,不会对制品造成显微缺陷。
所述的托槽用陶瓷材料无金属成分,生物相容性高,无毒,性能稳定,其抗弯强度及吸水率满足牙科材料使用要求。
所述的制备方法避免了热压铸成型的脱蜡损伤,利用拟薄水铝石烧结后产物与基体的一致性保证了托槽材料的纯陶瓷性能,同时利用其凝胶性能提高了原料的混合均匀性,保障各增强相的增强效果。
以上,说明了本发明的各种实施方式,但是通过其它实施方式也能够起到本发明所意图的作用效果,这对本领域技术人员来说是不言而喻的。特别是,能够不脱离本发明的技术范围地删除或置换前述的实施方式的结构要素,还能够进一步附加公知手段。另外,通过将本说明书中明示或暗示地公开的多个实施方式的特征任意地组合,也能够实施本发明,这对本领域技术人员来说是不言而喻的。
Claims (4)
1.一种ZTA-SiCw陶瓷托槽材料的制备方法,其特征在于,包括以下步骤:
步骤一:按照设定的固含量,将9wt%的拟薄水铝石、0.3wt%的柠檬酸三铵和70ml蒸馏水加入球磨罐中充分搅拌均匀,然后按照比例加入α-Al2O3和包含30wt%ZrO2和5wt%SiCw的增强相,再次球磨得到流动性好的料浆。
步骤二:向通过步骤一得到的料浆中滴加HNO3酒精溶液,调节pH至3~4形成稳定凝胶。
步骤三:将通过步骤二得到的凝胶在35℃下干燥12h、之后在60℃下干燥24h进行制坯干燥来形成生坯。
步骤四:将通过步骤三所得的生坯进行无压高温烧结,烧结温度为1560℃~1580℃。
2.一种ZTA-SiCw陶瓷托槽材料,其制备方法特征在于,
无毒性、无挥发,不会对制品造成显微缺陷。无须排蜡、工艺简单、不易开裂。所有原料烧结后产物均为陶瓷体。
3.根据权利要求1所述的ZTA-SiCw陶瓷托槽材料,其特征在于,
由纯陶瓷体复合而成,包含ZrO2和SiC晶须这两种增强相。
4.根据权利要求1所述的ZTA-SiCw陶瓷托槽材料,其特征在于,
所述托槽用陶瓷材料的抗弯强度高达398MPa,吸水率低于0.0023%。
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CN108158675A (zh) * | 2017-11-27 | 2018-06-15 | 桐庐宏远医疗器械有限公司 | 一种全陶瓷自锁托槽及其开启方法及锁定方法 |
CN111437201A (zh) * | 2020-03-18 | 2020-07-24 | 东华大学 | 一种齿科修复用可光固化牙本质粘结剂及其制备方法 |
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