CN114105633B - 提高氧化锆陶瓷抗老化性能的方法 - Google Patents
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Abstract
本发明涉及氧化锆陶瓷技术领域,具体涉及一种提高氧化锆陶瓷抗老化性能的方法。所述的提高氧化锆陶瓷抗老化性能的方法,在氧化锆陶瓷坯体烧结前,在氧化锆陶瓷坯体置于稳定剂溶液中浸渗,或者将稳定剂溶液雾化喷洒至氧化锆陶瓷坯体表面,然后再依次进行干燥、烧结;所述稳定剂溶液为含有Mg2+、Y3+、Al3+、Ce4+、La3+一种或多种的水溶液或乙醇溶液,稳定剂溶液中金属离子的总摩尔浓度为0.05‑3mol/L。本发明的方法工艺简单,操作方便,促进了生产效率的提高,大大提高了氧化锆陶瓷抗老化性能。
Description
技术领域
本发明涉及氧化锆陶瓷技术领域,具体涉及一种提高氧化锆陶瓷抗老化性能的方法。
背景技术
氧化锆陶瓷是一种重要的结构和功能材料,由于其熔点高、导热系数小、耐磨损和耐腐蚀等优点,使得氧化锆陶瓷备受关注,并广泛应用于各个领域。由于纯氧化锆陶瓷在一定温度范围内存在可逆相变,并且相变的过程伴随着体积的改变,极易造成产品的开裂,这限制了其在高温领域的应用,研究表明引入稳定剂可以控制氧化锆陶瓷的性能,目前已制备出在室温下性能优异的氧化锆陶瓷,例如部分稳定氧化锆陶瓷(PSZ)、四方多晶氧化锆陶瓷(TZP)及四方氧化锆弥散增韧陶瓷(ZTC)。
氧化钇稳定四方氧化锆陶瓷(Y-TZP)是得到最多研究的TZP材料,氧化钇的含量对氧化锆陶瓷的性能至关重要,例如当氧化钇的含量低于2mol%时,很难得到含量较高的四方相氧化锆,含量在2mol%时材料的韧性最好,而含量在2~3mol%之间时,材料的强度最高。然而,Y-TZP在低温潮湿的环境下使用,特别是在65-400℃这一温度区间下,极易发生低温老化现象,主要表现为表面产生微观或宏观的微裂纹,这使得材料的力学性能受到了一定的影响,并且限制其在特殊环境的应用。因此,防止Y-TZP低温老化至关重要。
研究表明Y-TZP低温老化现象产生的一种机制为水与氧化钇会相互作用生成Y(OH)3,这一反应可以消耗掉稳定剂,进而导致周围的氧化锆颗粒自由地变换到单斜相。主要表现为表面向内部发生t→m相变增韧,产生体积膨胀从而引发微裂纹。“Cattani-Lorente M,Scherrer S S,Ammann P,et al.Low temperature degradation of a Y-TZPdental ceramic[J].Acta Biomaterialia,2011,7:858-865.”
目前,防止Y-TZP低温老化的措施主要有以下几点:控制Y-TZP材料中氧化钇的含量;在Y-TZP材料中引入第二相粒子;控制Y-TZP材料的晶粒尺寸;对Y-TZP材料进行各种热处理以及对Y-TZP材料表面处理。
然而,这些传统的工艺工序繁琐,例如在引入氧化钇或第二相粒子需要其均匀分布在氧化锆中,这需要较长时间的预混合,而过高的浓度会对材料的性能产生不利影响;另一方面这些传统的工艺(例如打磨、抛光、上釉等)存在工序成本较高,工艺复杂等问题,不利于大规模应用。
发明内容
本发明要解决的技术问题是:提供一种提高氧化锆陶瓷抗老化性能的方法,工艺简单,操作方便,促进了生产效率的提高,大大提高了氧化锆陶瓷抗老化性能。
本发明所述的提高氧化锆陶瓷抗老化性能的方法,在氧化锆陶瓷坯体烧结前,在氧化锆陶瓷坯体置于稳定剂溶液中浸渗,或者将稳定剂溶液雾化喷洒至氧化锆陶瓷坯体表面,然后再依次进行干燥、烧结。
所述氧化锆陶瓷坯体为氧化锆粉体经干压、冷等静压成型后的陶瓷生坯,或者经密炼、注射成型、脱脂、预烧后的陶瓷素坯。
其中,氧化锆粉体的钇含量为2.1-3.5mol%。
在制备陶瓷生坯时,干压、冷等静压成型方法为常规方法。
在制备陶瓷素坯时,密炼、注射成型、脱脂、预烧均为常规方法,优选地,预烧温度为500-1000℃,保温时间为30min-5h。
所述稳定剂溶液为含有Mg2+、Y3+、Al3+、Ce4+、La3+一种或多种的水溶液或乙醇溶液,优选为含有Y3+、Al3+、Ce4+一种或多种的水溶液或乙醇溶液,金属离子的总摩尔浓度为0.05-3mol/L。
在进行浸渗操作时,陶瓷素坯浸渗时间为5s-180s,优选为5s-30s。
在进行雾化喷洒操作时,雾化喷洒时间为10s-30min,雾化喷洒温度为20-80℃。
将稳定剂溶液处理后氧化锆陶瓷坯体依次进行干燥、烧结,其中干燥方式为室温自然干燥或烘箱45-120℃干燥;烧结温度为1400-1500℃,烧结时间为2-10h。
本发明通过浸渍法或雾化法在氧化锆陶瓷表面引入稳定剂,一方面,引入多元稳定剂可以形成多元稳定晶相,降低氧化锆陶瓷由四方相向单斜相的转变;另一方面,可以提高氧化锆陶瓷表面稳定剂的浓度,减缓稳定剂损耗时间,从而提高其抗老化性。
具体地,所述提高氧化锆陶瓷抗老化性能的方法,包括以下步骤:
(1)将氧化锆粉体经成型得到氧化锆陶瓷坯体;
(2)将氧化锆陶瓷坯体置于稳定剂溶液中浸渗,或者将稳定剂溶液雾化喷洒至氧化锆陶瓷坯体表面;
(3)将稳定剂溶液处理后氧化锆陶瓷坯体在室温下自然干燥或烘箱45-120℃干燥;
(4)将干燥后的氧化锆陶瓷坯体置于高温烧结炉中烧结,烧结温度为1400-1500℃,烧结时间为2-10h,得到氧化锆陶瓷。
与现有技术相比,本发明具有以下有益效果:
(1)本方法采用含有Mg2+、Y3+、Al3+、Ce4+、La3+一种或多种的稳定剂对氧化锆陶瓷坯体进行处理,在氧化锆陶瓷材料中引入第二相粒子,避免了氧化锆颗粒自由地变换到单斜相,大大提高了氧化锆陶瓷抗老化性能;
(2)本方法将氧化锆陶瓷坯体置于稳定剂溶液中或者将稳定剂溶液雾化喷洒至其表面,仅仅对氧化锆材料表面进行处理,节省了预混合时间,降低了工业成本,提高了生产效率,通过控制表面稳定剂的组分、浓度、浸渗时间可以改变材料表面稳定剂含量变化,减少了过量稳定剂对材料的危害,满足大规模生产。
具体实施方式
为了使本发明的内容更容易被清楚的理解,对本发明作进一步详细的说明。
实施例1
将钇含量为2.5mol%的氧化锆造粒粉体干压预成型,然后利用冷等静压在200MPa条件下保压1min获得氧化锆生坯;将氧化锆生坯置于含有稳定剂离子的水溶液中,浸泡时间为5s,其中稳定剂溶液为硝酸钇溶液,浓度为1mol/L;然后将浸渗后的样品取出并置于60℃烘箱干燥24h;最后将干燥后的样品于1480℃高温炉烧结2h获得陶瓷样品。
实施例2
将钇含量为3.5mol%的氧化锆造粒粉体干压预成型,然后利用冷等静压在200MPa条件下保压1min获得氧化锆生坯;将氧化锆生坯置于含有稳定剂离子的水溶液中,浸泡时间为30s,其中稳定剂溶液为硝酸钇及硝酸铝混合溶液,硝酸钇溶液浓度为0.5mol/L,硝酸铝溶液浓度为0.5mol/L;然后将浸渗后的样品取出并置于120℃烘箱干燥10h;最后将干燥后的样品于1400℃高温炉烧结10h获得陶瓷样品。
实施例3
将钇含量为3mol%的氧化锆造粒粉体干压预成型,然后利用冷等静压在200MPa条件下保压1min获得氧化锆生坯;将氧化锆生坯置于含有稳定剂离子的乙醇溶液中,浸泡时间为10s,其中稳定剂溶液为硝酸钇、硝酸铝、硝酸铈混合溶液,硝酸钇溶液浓度为0.5mol/L,硝酸铝溶液浓度为0.3mol/L,硝酸铈溶液浓度为0.2mol/L;然后将浸渗后的样品取出并置于45℃烘箱干燥24h;最后将干燥后的样品于1500℃高温炉烧结2h获得陶瓷样品。
实施例4
将钇含量为2.1mol%的氧化锆造粒粉体干压预成型,然后利用冷等静压在200MPa条件下保压1min获得氧化锆生坯;将稳定剂溶液雾化喷洒至氧化锆生坯表面,雾化喷洒时间为20s,温度为60℃,其中稳定剂溶液为硝酸钇、硝酸铝、硝酸铈混合水溶液,硝酸钇溶液浓度为0.5mol/L,硝酸铝溶液浓度为0.3mol/L,硝酸铈溶液浓度为0.2mol/L;然后将雾化喷洒稳定剂溶液后的样品取出并室温自然干燥;最后将干燥后的样品于1450℃高温炉烧结6h获得陶瓷样品。
实施例5
将钇含量为3mol%的氧化锆造粒粉体经过密炼、注射成型及脱脂后,在800℃温度下预烧2h,获得氧化锆素坯;将氧化锆素坯置于含有稳定剂离子的水溶液中,浸泡时间为5s,其中稳定剂溶液为硝酸钇、硝酸铝、硝酸铈混合溶液,硝酸钇溶液浓度为0.5mol/L,硝酸铝溶液浓度为0.3mol/L,硝酸铈溶液浓度为0.2mol/L;然后将浸渗后的样品取出并置于60℃烘箱干燥24h;最后将干燥后的样品于1480℃高温炉烧结2h获得陶瓷样品。
对比例1
将钇含量为3mol%的氧化锆造粒粉体干压预成型,然后利用冷等静压在200MPa条件下保压1min获得氧化锆生坯;将氧化锆生坯置于纯水中,浸泡时间为5s;然后将浸渗后的样品取出并置于60℃烘箱干燥24h;最后将干燥后的样品于1480℃高温炉烧结2h获得陶瓷样品。
对比例2
将钇含量为3mol%的氧化锆造粒粉体与氧化钇、氧化铝、二氧化铈粉末装入三维运动混料机中,混料2h获得含有稳定剂的混合粉体,其中,氧化钇、氧化铝、二氧化铈与氧化锆造粒粉体的摩尔比值分别为0.5、0.3、0.2,然后将混合粉体干压预成型,然后利用冷等静压在200MPa条件下保压1min获得氧化锆生坯,最后将干燥后的样品于1480℃高温炉烧结2h获得陶瓷样品。
对比例3
将钇含量为3mol%的氧化锆造粒粉体干压预成型,然后利用冷等静压在200MPa条件下保压1min获得氧化锆生坯;将氧化锆生坯置于含有稳定剂离子的乙醇溶液中,浸泡时间为10s,其中稳定剂溶液为硝酸钇、硝酸铝、硝酸铈混合溶液,硝酸钇溶液浓度为2mol/L,硝酸铝溶液浓度为1.2mol/L,硝酸铈溶液浓度为0.8mol/L;然后将浸渗后的样品取出并置于60℃烘箱干燥24h;最后将干燥后的样品于1480℃高温炉烧结2h获得陶瓷样品。
将实施例和对比例制备的陶瓷样品进行性能测试,其中利用X射线衍射仪(XRD)对材料老化前后的物相进行分析并计算单斜相的相对含量,老化模拟环境为200℃高温水热反应24h,采用Instron 1195型万能材料试验机测试陶瓷样品的三点弯曲强度,利用阿基米德排水法测定陶瓷样品的烧密度。测试结果如表1所示。
表1陶瓷样品的性能指标
Claims (8)
1.一种提高氧化锆陶瓷抗老化性能的方法,其特征在于:包括以下步骤:在氧化锆陶瓷坯体烧结前,在氧化锆陶瓷坯体置于稳定剂溶液中浸渗,或者将稳定剂溶液雾化喷洒至氧化锆陶瓷坯体表面,然后再依次进行干燥、烧结;所述稳定剂溶液为含有Y3+、Al3+、Ce4+一种或多种的水溶液或乙醇溶液,稳定剂溶液中金属离子的总摩尔浓度为0.05-3mol/L;
所述提高氧化锆陶瓷抗老化性能的方法,包括以下步骤:
(1)将氧化锆粉体经成型得到氧化锆陶瓷坯体;
(2)将氧化锆陶瓷坯体置于稳定剂溶液中浸渗,或者将稳定剂溶液雾化喷洒至氧化锆陶瓷坯体表面;
(3)将稳定剂溶液处理后氧化锆陶瓷坯体在室温下自然干燥或烘箱45-120℃干燥;
(4)将干燥后的氧化锆陶瓷坯体置于高温烧结炉中烧结,烧结温度为1400-1500℃,烧结时间为2-10h,得到氧化锆陶瓷。
2.根据权利要求1所述的提高氧化锆陶瓷抗老化性能的方法,其特征在于:氧化锆陶瓷坯体为氧化锆粉体经干压、冷等静压成型后的陶瓷生坯,或者经密炼、注射成型、脱脂、预烧后的陶瓷素坯。
3.根据权利要求2所述的提高氧化锆陶瓷抗老化性能的方法,其特征在于:氧化锆粉体的钇含量为2.1-3.5mol%。
4.根据权利要求2所述的提高氧化锆陶瓷抗老化性能的方法,其特征在于:在制备陶瓷素坯时,预烧温度为500-1000℃,保温时间为30min-5h。
5.根据权利要求1所述的提高氧化锆陶瓷抗老化性能的方法,其特征在于:在进行浸渗操作时,陶瓷素坯浸渗时间为5s-180s。
6.根据权利要求1所述的提高氧化锆陶瓷抗老化性能的方法,其特征在于:在进行雾化喷洒操作时,雾化喷洒时间为10s-30min,雾化喷洒温度为20-80℃。
7.根据权利要求1所述的提高氧化锆陶瓷抗老化性能的方法,其特征在于:干燥方式为室温自然干燥或烘箱45-120℃干燥。
8.根据权利要求1所述的提高氧化锆陶瓷抗老化性能的方法,其特征在于:烧结温度为1400-1500℃,烧结时间为2-10h。
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