CN113929468A - 一种粉色氮化硅陶瓷及其制备方法和应用 - Google Patents
一种粉色氮化硅陶瓷及其制备方法和应用 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 48
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000003086 colorant Substances 0.000 claims abstract description 14
- 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 7
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 7
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Abstract
本发明涉及一种粉色氮化硅陶瓷及其制备方法和应用。本发明以Al2O3和Er2O3作为烧结助剂,且Er2O3同时作为着色剂,经气压烧结后,得到粉色氮化硅陶瓷。
Description
技术领域
本发明涉及一种粉色氮化硅陶瓷及其制备方法和应用,具体说,是以Al2O3和Er2O3作为烧结助剂,且Er2O3同时作为着色剂,经气压烧结所得的具有高强度、高硬度和高韧性特性的粉色氮化硅陶瓷,属于氮化硅陶瓷的制备领域。
背景技术
氮化硅陶瓷具有密度低、力学性能好、耐磨损、耐腐蚀及生物相容性好等优点,是一种理想的股骨球头材料。由于禁带宽度较大(3.5-5.5eV),氮化硅本身是无色的。但是由于受到添加剂的影响,氮化硅的颜色通常会有所变化。例如,当采用使用作为广泛Al2O3-Y2O3体系作为烧结助剂时,氮化硅陶瓷的颜色通常为灰色。作为一种人体植入物材料,其颜色若能与人体骨骼或组织相近,则更能为患者所接纳。赛琅泰克公司开发的ZTA陶瓷球头材料即为粉色。
因此,若能将氮化硅陶瓷股骨球头的颜色调节为粉色,其接受程度会更高。要想改变氮化硅陶瓷的颜色,通常需要加入着色剂。但多数着色剂的熔点较低,易在氮化硅陶瓷的烧结过程中分解,无法其他改变氮化硅陶瓷颜色的目的,且会阻碍氮化硅陶瓷的致密化。另一方面,作为一种生物材料,氮化硅陶瓷中的元素应较为稳定,且具有生物安全性。
发明内容
针对上述问题,本发明的目的在于提供一种粉色氮化硅陶瓷及其制备方法和应用。
一方面,本发明提供了一种粉色氮化硅陶瓷,以Al2O3和Er2O3作为烧结助剂,且Er2O3同时作为着色剂,经气压烧结后,得到粉色氮化硅陶瓷。
本发明中,采用Al2O3和Er2O3作为烧结助剂,且Er2O3同时作为着色剂,制备粉色氮化硅陶瓷。这样一方面可以减少氮化硅陶瓷中引入的元素种类,减少第二相对氮化硅陶瓷致密化的抑制作用。另一方面,Er2O3的离子半径较小,可以制备出强度和韧性更高的氮化硅陶瓷。本发明通过合理设计Al2O3和Er2O3的比例,并进行烧结工艺调控,可获得同时满足高强度、高韧性和高硬度的粉色氮化硅陶瓷。
较佳的,所述粉色氮化硅陶瓷中Al2O3的含量为0.71~2.78wt%,Er2O3的含量为3.91~8.82wt%。
较佳的,所述粉色氮化硅陶瓷的相对密度为97.6%~99.6%,抗弯强度为1088.9~1357.3MPa,维氏硬度为14.31~15.42GPa,断裂韧性为10.4~13.5MPa·m1/2。
另一方面,本发明提供了一种粉色氮化硅陶瓷的制备方法,包括:
以α-Si3N4粉体为初始原料,Al2O3和Er2O3作为烧结助剂,且Er2O3同时作为着色剂,经球磨混合,得到混合粉体;
将混合粉体进行干压预成型和冷等静压成型,得到素坯;
将素坯装入BN坩埚,置于烧结炉中,在氮气气氛下进行气压烧结,得到所述粉色氮化硅陶瓷。
较佳的,所述球磨混合的参数包括:球磨转速为200~400rpm,球磨时间为2~4小时。
较佳的,经过球磨混合之后,再经干燥和过筛,得到混合粉条;所述过筛的目数为100~400目。
较佳的,所述干压成型的压力为10~30MPa,所述冷等静压成型的压力为150~250MPa。
较佳的,所述气压烧结的参数包括:烧结温度为1750~1850℃,保温时间为1~4小时,氮气气压为1MPa~3MPa。
再一方面,本发明提供了一种粉色氮化硅陶瓷在制备陶瓷股骨球头中的应用。
有益效果:
本发明中,添加Er2O3,既作为烧结助剂又作为着色剂,可以消除额外添加着色剂对生物安全性和烧结致密化的影响。同时,与常用的Y2O3烧结助剂相比,Er2O3阳离子半径更小,可以促进氮化硅陶瓷中的晶粒发育为更为细长的枝晶,形成晶粒互锁的微结构,获得高强度、高韧性和高硬度的粉色氮化硅陶瓷。
该方法制备的Si3N4陶瓷具有高强度、高硬度和高韧性等突出优点,且呈粉色,可用作人工股骨球头。
附图说明
图1为实施例1制得的氮化硅陶瓷断口形貌图;
图2为实施例4制得的氮化硅陶瓷抛光面光学图像;
图3为实施例6制得的氮化硅陶瓷抛光面光学图像。
具体实施方式
以下通过下述实施方式进一步说明本发明,应理解,下述实施方式仅用于说明本发明,而非限制本发明。
本发明中,以Al2O3和Er2O3作为烧结助剂,且Er2O3同时作为着色剂,气压烧结制备具有高强度、高韧性和高硬度特性的粉色氮化硅陶瓷,其综合性能优良。
以下示例性地说明粉色氮化硅陶瓷的制备方法。
以α-Si3N4粉体为初始原料,Al2O3和Er2O3作为烧结助剂,且Er2O3同时作为着色剂,作为原料粉末。其中控制Al2O3的含量可为原料粉末总质量0.71~2.78wt%。Er2O3的含量可为原料粉末总质量的3.91~8.82wt%。
将原料粉末以Si3N4球为研磨介质,球磨,烘干,研磨,过筛,制备出混合粉体。作为一个示例,以酒精为溶剂,将上述原料配成一定固含量的浆料,以Si3N4球为研磨介质,球磨,烘干,研磨,过筛,制备出混合粉体。所述球磨转速为200-400rpm,球磨时间为2-4h。过筛目数为100~400目。
将混合粉体进行干压预成型和冷等静压成型,得到成型后的素坯。其中,干压预成型压力可为10~30MPa;冷等静压压力可为150~250MPa。
将素坯装入BN坩埚,置于烧结炉中,在氮气气氛下进行气压烧结,可得到高强度、高韧性和高硬度的粉色氮化硅陶瓷。所述气压烧结温度可为1750~1850℃,保温时间可为1~4h(例如,1-3小时),氮气气压可为1~3MPa。
在本公开中,采用阿基米德排水法测试粉色氮化硅陶瓷的相对密度为97.6%~99.6%。
在本公开中,用万能材料试验机测试粉色氮化硅陶瓷的抗弯强度为1088.9~1357.3MPa。
在本公开中,采用维氏硬度计测试粉色氮化硅陶瓷的维氏硬度为14.31~15.42GPa。
在本公开中,采用单边开口梁法测试粉色氮化硅陶瓷的断裂韧性为10.4~13.5MPa·m1/2。
下面进一步例举实施例以详细说明本发明。同样应理解,以下实施例只用于对本发明进行进一步说明,不能理解为对本发明保护范围的限制,本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。下述示例具体的工艺参数等也仅是合适范围中的一个示例,即本领域技术人员可以通过本文的说明做合适的范围内选择,而并非要限定于下文示例的具体数值。
实施例1
一种粉色氮化硅陶瓷及其制备方法,包括以下步骤:
S1:称取94g Si3N4,2.09gAl2O3和3.91g Er2O3一共100g;
S2:将步骤S1混合粉体配置成一定固含量的浆料,行星球磨2h,转速为400rpm;
S3:将步骤S2所得浆料烘干后研磨,过400目筛后在10MPa压力下干压预成型,再经250MPa冷等静压成型;
S4:将步骤S3所得陶瓷素坯放入BN模具中,并置于气压烧结炉中,充入N2作为保护气,在1750℃,3MPa压力下烧结4h,得到粉色氮化硅陶瓷。所得粉色氮化硅陶瓷的相对密度为98.3%,抗弯强度为1186.7±18.6MPa,断裂韧性为10.8±0.1MPa·m1/2,维氏硬度为14.99±0.17GPa。采用爱色丽X-Rite Ci62分光测色仪测试,所得粉色氮化硅陶瓷的色度值为L=69.72±0.21,a=3.55±0.15,b=8.61±0.23。对本实施例1得到的氮化硅陶瓷的断口进行观察,结果如图1所示,样品致密度较高,晶粒尺寸较小,约为1-2μm。
实施例2
一种粉色氮化硅陶瓷及其制备方法,包括以下步骤:
S1:称取94g Si3N4,0.71gAl2O3和5.29g Er2O3一共100g;
S2:将步骤S1混合粉体配置成一定固含量的浆料,行星球磨2h,转速为400rpm;
S3:将步骤S2所得浆料烘干后研磨,过200目筛后在20MPa压力下干压预成型,再经200MPa冷等静压成型;
S4:将步骤S3所得陶瓷素坯放入BN模具中,并置于气压烧结炉中,充入N2作为保护气,在1750℃,2MPa压力下烧结3h,即得所述相对密度为97.6%,抗弯强度为1136.7±47.8MPa,断裂韧性为10.6±0.2MPa·m1/2,维氏硬度为15.28±0.14GPa。采用爱色丽X-Rite Ci62分光测色仪测试,所得粉色氮化硅陶瓷的色度值为L=88.44±0.28,a=4.55±0.42,b=5.61±0.33。
实施例3
一种粉色氮化硅陶瓷及其制备方法,包括以下步骤:
S1:称取92g Si3N4,2.78gAl2O3和5.22g Er2O3一共100g;
S2:将步骤S1混合粉体配置成一定固含量的浆料,行星球磨3h,转速为300rpm;
S3:将步骤S2所得浆料烘干后研磨,过100目筛后在30MPa压力下干压预成型,再经150MPa冷等静压成型;
S4:将步骤S3所得陶瓷素坯放入BN模具中,并置于气压烧结炉中,充入N2作为保护气,在1800℃,2MPa压力下烧结3h,得到粉色氮化硅陶瓷。所得粉色氮化硅陶瓷的相对密度为98.9%,抗弯强度为1265.6±33.2MPa,断裂韧性为12.4±0.3MPa·m1/2,维氏硬度为14.82±0.11GPa。采用爱色丽X-Rite Ci62分光测色仪测试,所得粉色氮化硅陶瓷的色度值为L=69.34±0.36,a=2.68±0.46,b=5.28±0.21。
实施例4
一种粉色氮化硅陶瓷及其制备方法,包括以下步骤:
S1:称取92g Si3N4,0.94gAl2O3和7.06g Er2O3一共100g;
S2:将步骤S1混合粉体配置成一定固含量的浆料,行星球磨3h,转速为300rpm;
S3:将步骤S2所得浆料烘干后研磨,过200目筛后在20MPa压力下干压预成型,再经250MPa冷等静压成型;
S4:将步骤S3所得陶瓷素坯放入BN模具中,并置于气压烧结炉中,充入N2作为保护气,在1800℃,3MPa压力下烧结2h,得到粉色氮化硅陶瓷。所述粉色氮化硅陶瓷的相对密度为98.6%,抗弯强度为1215±23.3MPa,断裂韧性为11.7±0.2MPa·m1/2,维氏硬度为14.77±0.08GPa。采用爱色丽X-Rite Ci62分光测色仪测试,所得粉色氮化硅陶瓷的色度值为L=87.08±0.48,a=4.73±0.35,b=5.64±0.19。对本实施例4得到的氮化硅陶瓷的抛光面光学图像进行观察,结果如图2所示,样品表面具有镜面光泽,呈粉色。
实施例5
一种粉色氮化硅陶瓷及其制备方法,包括以下步骤:
S1:称取90g Si3N4,3.48gAl2O3和6.52g Er2O3一共100g;
S2:将步骤S1混合粉体配置成一定固含量的浆料,行星球磨4h,转速为200rpm;
S3:将步骤S2所得浆料烘干后研磨,过100目筛后在30MPa压力下干压预成型,再经200MPa冷等静压成型;
S4:将步骤S3所得陶瓷素坯放入BN模具中,并置于气压烧结炉中,充入N2作为保护气,在1850℃,2MPa压力下烧结1h,得到粉色氮化硅陶瓷。所得粉色氮化硅陶瓷的相对密度为99.6%,抗弯强度为1322.6±34.7MPa,断裂韧性为13.4±0.1MPa·m1/2,维氏硬度为14.54±0.13GPa。采用爱色丽X-Rite Ci62分光测色仪测试,所得粉色氮化硅陶瓷的色度值为:L=54.98±0.18,a=1.36±0.27,b=1.41±0.08。
实施例6
一种粉色氮化硅陶瓷及其制备方法,包括以下步骤:
S1:称取90g Si3N4,1.18gAl2O3和8.82g Er2O3一共100g;
S2:将步骤S1混合粉体配置成一定固含量的浆料,行星球磨4h,转速为200rpm;
S3:将步骤S2所得浆料烘干后研磨,过400目筛后在30MPa压力下干压预成型,再经150MPa冷等静压成型;
S4:将步骤S3所得陶瓷素坯放入BN模具中,并置于气压烧结炉中,充入N2作为保护气,在1850℃,1MPa压力下烧结3h,得到粉色氮化硅陶瓷。所得粉色氮化硅陶瓷的相对密度为99.2%,抗弯强度为1288.5±22.4MPa,断裂韧性为13.1±0.1MPa·m1/2,维氏硬度为14.42±0.11GPa。采用爱色丽X-Rite Ci62分光测色仪测试,所得粉色氮化硅陶瓷的色度值为:L=83.99±0.65,a=5.66±0.45,b=2.46±0.31。
对本实施例6得到的氮化硅陶瓷的抛光面光学图像进行观察,结果如图2所示,样品表面具有镜面光泽,呈粉色。
从上述6个案例可以看出,本发明通过在Si3N4基体中添加Al2O3和Er2O3作为烧结助剂,且Er2O3同时作为着色剂,采用气压烧结工艺,可以获得高强度、高韧性和高硬度特性的粉色氮化硅陶瓷。
最后有必要说明的是:以上实施例只用于对本发明的技术方案作进一步详细说明,不能理解为对本发明保护范围的限制,本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。
Claims (9)
1.一种粉色氮化硅陶瓷,其特征在于,以Al2O3和Er2O3作为烧结助剂,且Er2O3同时作为着色剂,经气压烧结后,得到粉色氮化硅陶瓷。
2.根据权利要求1所述粉色氮化硅陶瓷,其特征在于,所述粉色氮化硅陶瓷中Al2O3的含量为0.71~2.78 wt%,Er2O3的含量为3.91~8.82 wt%。
3.根据权利要求1或2所述粉色氮化硅陶瓷,其特征在于,所述粉色氮化硅陶瓷的相对密度为97.6%~99.6%,抗弯强度为1088.9~1357.3 MPa,维氏硬度为14.31~15.42 GPa,断裂韧性为10.4~13.5 MPa·m1/2。
4.一种权利要求1-3中任一项所述的粉色氮化硅陶瓷的制备方法,其特征在于,包括:
以α-Si3N4粉体为初始原料,Al2O3和Er2O3作为烧结助剂,且Er2O3同时作为着色剂,经球磨混合,得到混合粉体;
将混合粉体进行干压预成型和冷等静压成型,得到素坯;
将素坯装入BN坩埚,置于烧结炉中,在氮气气氛下进行气压烧结,得到所述粉色氮化硅陶瓷。
5.根据权利要求4所述的制备方法,其特征在于,所述球磨混合的参数包括:球磨转速为200~400 rpm,球磨时间为2~4小时。
6.根据权利要求4或5所述的制备方法,其特征在于,经过球磨混合之后,再经干燥和过筛,得到混合粉条;所述过筛的目数为100~400目。
7.根据权利要求4-6中任一项所述的制备方法,其特征在于,所述干压成型的压力为10~30 MPa,所述冷等静压成型的压力为150~250 MPa。
8.根据权利要求4-7中任一项所述的制备方法,其特征在于,所述气压烧结的参数包括:烧结温度为1750~1850℃,保温时间为1~4小时,氮气气压为1MPa~3 MPa。
9.一种权利要求1-3中任一项所述的粉色氮化硅陶瓷在制备陶瓷股骨球头中的应用。
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