CN113321505A - 一种氧化锆基陶瓷材料及其制备方法 - Google Patents
一种氧化锆基陶瓷材料及其制备方法 Download PDFInfo
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 15
- 239000003381 stabilizer Substances 0.000 claims abstract description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 11
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 8
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims abstract description 8
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 87
- 239000002994 raw material Substances 0.000 claims description 55
- 239000000919 ceramic Substances 0.000 claims description 31
- 238000005245 sintering Methods 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 14
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- 238000003826 uniaxial pressing Methods 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 14
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 2
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- 239000003462 bioceramic Substances 0.000 abstract description 9
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- 230000000694 effects Effects 0.000 abstract description 3
- 230000009466 transformation Effects 0.000 abstract description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 2
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- 238000011160 research Methods 0.000 abstract description 2
- 239000003826 tablet Substances 0.000 description 13
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Abstract
本发明涉及一种氧化锆基陶瓷材料及其制备方法,为了抑制氧化锆在环境中发生四方相向单斜相的转变,提高其低温老化性能,本发明以3Y‑TZP(氧化钇稳定的四方多晶氧化锆,其中氧化钇的摩尔含量为3%),以氧化铝和/或二氧化铈作为稳定剂,制备出了Y2O3‑ZrO2‑Al2O3/CeO2复合陶瓷材料。研究表明,稳定剂的加入可以大大优化其性能,进而延长氧化锆基生物陶瓷作为口腔种植体的使用时间,并且,同时添加两种稳定剂所取得的效果比单种稳定剂更佳。
Description
技术领域
本发明涉及陶瓷材料领域,具体涉及一种氧化锆基陶瓷材料及其制备方法。
背景技术
陶瓷是指用天然或人工合成的粉末化合物经过成形和高温烧结制成的一类无机非金属材料,因其具有高硬度、高熔点、高耐腐蚀性能等优点而广泛应用于各个领域。
另外,口腔种植是指通过在牙槽骨内植入牙种植体,借以支撑、固定义齿完成缺牙修复的方法。伴随口腔种植技术的进步,口腔种植的目的从早期的缺牙功能修复发展到如今对修复美观与健康的更高追求;适应症也从无牙颌或游离端缺失扩展至各类牙缺失。另外,种植体还可以用于口腔颅颌面缺损修复,以解决赝复体的固位问题。
由于牙种植体出于口腔的特殊环境,种植体材料必须具备以下条件:①口腔组织对材料有较好的耐受性,材料对组织没有或仅有极弱的化学刺激,不产生支持骨的吸收;②对体液有抗腐蚀性,能长期保持所需的机械性能;③必须具有良好的生物相容性;④材料对骨组织应有良好的生物力学适应性。由于具有优异的耐腐蚀性能,良好的生物相容性,惰性生物陶瓷氧化锆已成为广泛应用的口腔种植体材料。然而,在口腔的低温潮湿环境中,氧化锆生物陶瓷会发生T-M相变,从而降低其力学性能,这个过程称之为低温老化过程。有鉴于此,如何使生物陶瓷氧化锆保持良好的低温老化性能,将直接决定其在口腔中的使用时长。
发明内容
针对现有技术存在的问题,本发明旨在提供一种氧化锆基陶瓷材料及其制备方法,以解决传统的氧化锆陶瓷低温老化性能不佳的问题。
一种氧化锆基陶瓷材料的制备方法,包括以下步骤:
A.按化学计量准确称量氧化钇稳定氧化锆粉末和稳定剂粉末作为原料,将原料粉末在880-950℃下煅烧2.5-3.0h;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20-24h;
C.在25-28MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250-260MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5-3.0h得到氧化锆生物陶瓷材料,烧结温度为1200-1400℃。
进一步地,所述氧化钇稳定氧化锆粉末中氧化钇的摩尔含量为3%。
进一步地,所述氧化锆为四方多晶相。
进一步地,所述稳定剂为氧化铝或二氧化铈中的一种或两种。
进一步地,所述稳定剂的含量为0.5wt-2.4wt%。
进一步地,所述稳定剂为氧化铝和二氧化铈。
进一步地,所述氧化铝的含量为1.0wt%,所述二氧化铈的含量为1.4wt%。
另外,本发明还提供了一种氧化锆基陶瓷材料,所述陶瓷材料由上述方法制备而得。
为了抑制氧化锆在环境中发生四方相向单斜相的转变,提高其低温老化性能,本发明以3Y-TZP(氧化钇稳定的四方多晶氧化锆,其中氧化钇的摩尔含量为3%),以氧化铝和/或二氧化铈作为稳定剂,制备出了Y2O3-ZrO2-Al2O3/CeO2复合生物陶瓷材料。研究表明,稳定剂的加入可以大大优化其性能,进而延长氧化锆基生物陶瓷作为口腔种植体的使用时间,并且,同时添加两种稳定剂所取得的效果比单种稳定剂更佳。
具体实施方式
下面通过具体实施例来验证本发明的技术效果,但是本发明的实施方式不局限于此。
实施例1
A.按化学计量准确称量3Y-TZP粉末和Al2O3粉末作为原料,将原料粉末在880℃下煅烧2.5h,其中Al2O3粉末的质量含量为原料粉末总质量的0.5%;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20h;
C.在25MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5h得到氧化锆生物陶瓷材料,烧结温度为1400℃。
实施例2
A.按化学计量准确称量3Y-TZP粉末和Al2O3粉末作为原料,将原料粉末在880℃下煅烧2.5h,其中Al2O3粉末的质量含量为原料粉末总质量的1.0%;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20h;
C.在25MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5h得到氧化锆生物陶瓷材料,烧结温度为1400℃。
实施例3
A.按化学计量准确称量3Y-TZP粉末和Al2O3粉末作为原料,将原料粉末在880℃下煅烧2.5h,其中Al2O3粉末的质量含量为原料粉末总质量的1.4%;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20h;
C.在25MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5h得到氧化锆生物陶瓷材料,烧结温度为1400℃。
实施例4
A.按化学计量准确称量3Y-TZP粉末和Al2O3粉末作为原料,将原料粉末在880℃下煅烧2.5h,其中Al2O3粉末的质量含量为原料粉末总质量的2.0%;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20h;
C.在25MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5h得到氧化锆生物陶瓷材料,烧结温度为1400℃。
实施例5
A.按化学计量准确称量3Y-TZP粉末和CeO2粉末作为原料,将原料粉末在880℃下煅烧2.5h,其中CeO2粉末的质量含量为原料粉末总质量的0.5%;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20h;
C.在25MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5h得到氧化锆生物陶瓷材料,烧结温度为1400℃。
实施例6
A.按化学计量准确称量3Y-TZP粉末和CeO2粉末作为原料,将原料粉末在880℃下煅烧2.5h,其中CeO2粉末的质量含量为原料粉末总质量的1.0%;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20h;
C.在25MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5h得到氧化锆生物陶瓷材料,烧结温度为1400℃。
实施例7
A.按化学计量准确称量3Y-TZP粉末和CeO2粉末作为原料,将原料粉末在880℃下煅烧2.5h,其中CeO2粉末的质量含量为原料粉末总质量的1.4%;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20h;
C.在25MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5h得到氧化锆生物陶瓷材料,烧结温度为1400℃。
实施例8
A.按化学计量准确称量3Y-TZP粉末和CeO2粉末作为原料,将原料粉末在880℃下煅烧2.5h,其中CeO2粉末的质量含量为原料粉末总质量的2.0%;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20h;
C.在25MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5h得到氧化锆生物陶瓷材料,烧结温度为1400℃。
实施例9
A.按化学计量准确称量3Y-TZP粉末、Al2O3粉末和CeO2粉末作为原料,将原料粉末在880℃下煅烧2.5h,其中Al2O3的质量含量为原料粉末总质量的1.0%粉末,CeO2粉末的质量含量为原料粉末总质量的1.4%;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20h;
C.在25MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5h得到氧化锆生物陶瓷材料,烧结温度为1400℃。
实施例10
A.按化学计量准确称量3Y-TZP粉末和Al2O3粉末作为原料,将原料粉末在880℃下煅烧2.5h,其中Al2O3的质量含量为原料粉末总质量的2.4%粉末;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20h;
C.在25MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5h得到氧化锆生物陶瓷材料,烧结温度为1400℃。
实施例11
A.按化学计量准确称量3Y-TZP粉末和CeO2粉末作为原料,将原料粉末在880℃下煅烧2.5h,其中CeO2粉末的质量含量为原料粉末总质量的2.4%;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20h;
C.在25MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5h得到氧化锆生物陶瓷材料,烧结温度为1400℃。
实施例12
A.按化学计量准确称量3Y-TZP粉末、Al2O3粉末和CeO2粉末作为原料,将原料粉末在880℃下煅烧2.5h,其中Al2O3的质量含量为原料粉末总质量的1.0%粉末,CeO2粉末的质量含量为原料粉末总质量的1.0%;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20h;
C.在25MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5h得到氧化锆生物陶瓷材料,烧结温度为1400℃。
接下来,采用高压反应釜对不同样品在130℃的水蒸气中进行72h的低温老化实验,并以3Y-TZP粉末制备而得的生物陶瓷材料作为对照组。使用X射线衍射仪,衍射靶Cu-Kα在40kV工作电压和40mA工作电流下以0.02°/s扫描速度和27-33°(2θ)扫描范围测量所有实验样品的相变含量。
表1 各样品相变含量
编号 | 各样品相变含量/% |
实施例1 | 25.37 |
实施例2 | 22.89 |
实施例3 | 15.54 |
实施例4 | 14.31 |
实施例5 | 28.96 |
实施例6 | 23.76 |
实施例7 | 17.21 |
实施例8 | 15.20 |
实施例9 | 7.52 |
实施例10 | 12.28 |
实施例11 | 13.01 |
实施例12 | 12.99 |
对照组 | 47.69 |
在向Y-TZP(氧化钇稳定的四方多晶氧化锆)材料中加入Al2O3或CeO2后,可以有效阻碍生物陶瓷发生t(四方相)→m(单斜相)转变,进而提高了陶瓷材料的低温老化性能。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明技术原理的前提下,还可以做出若干改进和变型,这些改进和变型也应视为本发明的保护范围。
Claims (8)
1.一种氧化锆基陶瓷材料的制备方法,其特征在于:包括以下步骤:
A.按化学计量准确称量氧化钇稳定氧化锆粉末和稳定剂粉末作为原料,将原料粉末在880-950℃下煅烧2.5-3.0h;
B.将原料粉末放入行星式球磨机中,在乙醇环境下球磨20-24h;
C.在25-28MPa下使用压片机单轴压下得到生物陶瓷胚体;
D.采用冷等静压工艺,在250-260MPa的压力下进一步致密化生物陶瓷胚体;
E.在空气中烧结2.5-3.0h得到氧化锆生物陶瓷材料,烧结温度为1200-1400℃。
2.一种如权利要求1所述的制备方法,其特征在于:所述氧化钇稳定氧化锆粉末中氧化钇的摩尔含量为3%。
3.一种如权利要求1所述的制备方法,其特征在于:所述氧化锆为四方多晶相。
4.一种如权利要求1所述的制备方法,其特征在于:所述稳定剂为氧化铝或二氧化铈中的一种或两种。
5.一种如权利要求1所述的制备方法,其特征在于:所述稳定剂的含量为0.5wt-2.4wt%。
6.一种如权利要求4所述的制备方法,其特征在于:所述稳定剂为氧化铝和二氧化铈。
7.一种如权利要求4所述的制备方法,其特征在于:所述氧化铝的含量为1.0wt%,所述二氧化铈的含量为1.4wt%。
8.一种氧化锆基陶瓷材料,其特征在于,所述陶瓷材料由权利要求1-7中任一方法制备而得。
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