CN114644513B - 一种莫来石红外透明陶瓷的制备方法 - Google Patents
一种莫来石红外透明陶瓷的制备方法 Download PDFInfo
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Abstract
本发明公开了一种莫来石红外透明陶瓷的制备方法。所述方法包括:按摩尔比1.70~1.94:1称取氧化铝和二氧化硅,球磨得到混合粉体;将所得混合粉体于700~900℃煅烧2~4小时;将经煅烧处理的混合粉体成型得到素坯;以及对所得素坯于700~900℃进行预烧结处理2~3小时,然后于真空条件下在1700~1800℃烧结4~8小时得到莫来石红外透明陶瓷。所述方法步骤简单,制备周期短,制备过程中没有引入外来污染,为制备大尺寸和复杂形状的莫来石红外透明陶瓷提供一种新方法。
Description
本发明涉及一种莫来石红外透明陶瓷的制备方法,具体涉及一种固相反应烧结法制备的莫来石红外透明陶瓷及其制备方法,属于透明陶瓷制备领域。
背景技术
飞行器在高速飞行时,前端的红外光学窗口和整流罩温度会急剧升高;传统的红外透明材料如蓝宝石单晶、氧化钇、氧化镁、镁铝尖晶石和氮氧化铝透明陶瓷等在高温下力学性能会有大幅度下降,不能满足未来超高速飞行器的发展需求;莫来石陶瓷的抗弯强度在1400℃开始只有少量的降低,而且部分力学性能还会有所增强,此外莫来石具有优异的抗热震性、高的热稳定性、良好的耐腐蚀能力,有潜力作为红外窗口和整流罩;想要制备出具有实际应用价值的莫来石透明陶瓷,就必须选择合适的原料和烧结方法。
1983年,F.J.Klug等用溶胶凝胶法合成粉体制备莫来石透明陶瓷,并对其透红外性能进行研究,获得了透红外的莫来石陶瓷(Infrared-transparent mullite ceramic[J].Journal of the American Ceramic Society,1983,66(12):874-880);Ohashi等制备出半透明的莫来石陶瓷(Preparation of translucent mullite.Journal of materialsscience letters[J],1987(6):528-530);国内张桂敏等人在2009年用溶胶凝胶法合成的粉体采用放电等离子体烧结(SPS烧结)制备出莫来石透明陶瓷(Transparent mulliteceramic from single-phase gel by spark plasma sintering.Journal of theEuropean Ceramic Society,2009.29:2705-2711),目前,莫来石粉体的合成方法主要是溶胶凝胶法,存在工艺步骤繁琐、周期长、释放酸性气体等问题,影响了粉体的合成效率,并对环境造成了一定的污染,同时目前报道的莫来石透明陶瓷的烧结方法(热压烧结、SPS烧结等)难以制备出复杂形状和大尺寸的陶瓷,极大限制了莫来石透明陶瓷的制备和应用发展,因此找到一种步骤简单、无污染且容易制备大尺寸和复杂形状莫来石透明陶瓷的制备方法具有重要的意义。
固相反应烧结法的优点是步骤少、效率高、环境友好,同时真空条件下烧结容易制备大尺寸复杂形状透明陶瓷,但用固相反应烧结莫来石透明陶瓷存在诸多难点,如原料纯度、铝硅比、烧结工艺等对制备莫来石透明陶瓷均有较大影响,还未见有报道用此方法制备出莫来石透明陶瓷;因此本发明为了解决目前存在的问题,以高纯氧化物粉体为原料,通过调整铝硅比,寻找适合的工艺参数,加入烧结助剂并采用真空固相反应烧结制备莫来石透明陶瓷。
发明内容
本发明的目的是提供一种工艺步骤简单、制备周期短且没有污染的制备透红外莫来石透明陶瓷的新方法。
一种制备莫来石红外透明陶瓷的方法,包括:
按摩尔比1.70~1.94:1称取氧化铝和二氧化硅,球磨得到混合粉体;将所得混合粉体于700~900℃煅烧2~4小时;将经煅烧处理的混合粉体成型得到素坯;以及对所得素坯于700~900℃进行预烧结处理2~3小时,然后于1700~1800℃下真空无压烧结4~8小时得到莫来石红外透明陶瓷。
本发明采用摩尔比为1.70~1.94:1的氧化铝和二氧化硅为原料,可以使二氧化硅完全反应形成莫来石;在成型之前,对原料混合粉体于700~900℃煅烧2~4小时,除去实验过程中引入水分等其他杂质;将混合粉体按照两步成型方法形成素坯,提高素坯的密度;成型后素坯在烧结前在700~900℃进行预烧结处理2~3小时,有效去除制备过程引入的有机物等杂质,提高素坯密度;最后于1700~1800℃下真空无压烧结4~8小时,升温速率为6~10℃/分钟。
较佳地,混合粉体煅烧升温速率为1~3℃/分钟。
较佳地,在球磨之前,还加入氧化镁作为烧结助剂,氧化镁的加入量占氧化铝和二氧化硅总质量的0.03~0.3wt%;加入一定量的氧化镁能获得高致密度纯相莫来石陶瓷。
具体地,氧化镁作用如下:能在较低温下形成于氧化铝和二氧化硅形成液相促进莫来石的致密化过程,提高莫来石陶瓷的致密度;氧化镁在高温下易挥发,相对于其他烧结助剂不产生第二相,同时还能带走一部分析出的氧化铝;氧化镁的加入能降低莫来石陶瓷的烧结温度,减小其晶粒尺寸提高其力学性能,因此,氧化镁的加入有助于提高透红外性能和力学性能。
较佳地,所述高纯氧化铝主晶相为α-Al2O3,所述氧化铝和二氧化硅粉体采用高纯原料,例如纯度均在99.99%以上,以此减少杂质的影响。
较佳地,球磨后所述粉体粒径为100~200nm,高纯二氧化硅的中位粒径为600~800nm,优选所述中位粒径为0.7μm;氧化铝粉体和二氧化硅粉体粒度较小,烧结活性好,同时它们的纯度高,杂质含量少有利于提高红外透过率,此外粉体粒径较为均匀有利于其反应生成莫来石。
较佳地,球磨介质优选为酒精,其中氧化铝和二氧化硅的总质量:球:酒精质量比为1:4~8:1.2~1.6;以酒精作为球磨介质有利于打开粉体的团聚来减小粉体的粒径,从而提高其烧结活性。
较佳地,球磨后的粉体在60℃~70℃下干燥24小时,过200目筛。
较佳地,所述形成素坯的方法为:在700~1600N的压力下保压1~3分钟进行干压预成型后,再在180~230N的压力下保压1~3分钟进行等静压处理成型,提高素坯密度,促进烧结过程。
较佳地,所述预烧的气氛为空气气氛,升温速率为1~3℃分钟。
较佳地,真空烧结中,真空度在10-3~10-2Pa之间,升温速率为6~10℃/分钟。
根据本发明制备的莫来石红外透明陶瓷,莫来石中Al元素折算成氧化铝的摩尔含量为63-66%,且所述莫来石红外透明陶瓷在中红外区域透过率可达到70%,中红外波段透过截止波长为5.5μm。
附图说明
图1为本发明实施例1和2中制备莫来石陶瓷的XRD图谱;
图2为本发明实施例1和2中制备莫来石陶瓷的红外波段透过曲线;
图3为本发明实施例1中制备莫来石陶瓷的显微结构。
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;在下述说明中,莫来石红外透明陶瓷也可以称为莫来石透明陶瓷。
本发明采用高纯氧化铝和高纯二氧化硅为原料,其中,高纯氧化铝主晶相为α-Al2O3,粉体粒径可为100~200nm;高纯二氧化硅的中位粒径为600~800nm;高纯氧化铝和/或高纯二氧化硅的纯度优选为99.99%以上。
加入氧化镁作为烧结助剂,所述氧化镁的加入量占氧化铝和二氧化硅总质量的0.03~0.3wt%。
原料粉体可采用湿法球磨进行混合、干燥,例如,球磨介质可采用酒精,其中,原料粉体、球、球磨介质的重量比可为1:4~8:1.2~1.6,例如1:6:1.4;干燥可在60~70℃烘箱中进行,干燥后的粉体优选再进行过筛处理,例如过200目筛。
在成型前,对混合粉体进行煅烧处理,煅烧温度可为700~900℃,煅烧时间可为2~4小时,升温速率为1~3℃/分钟,经过煅烧处理的粉体,可去除实验过程中引入的水分和其他有机物杂质。
经煅烧处理的混合粉体在700~1600N的压力下保压1~3分钟进行干压预成型后,再在180~230N的压力下保压1~3分钟进行等静压处理成型;分步两次成型能提高素坯密度。
所得素坯先经预烧结处理然后可进行真空烧结,所述真空度优选为10-3~10-2Pa;其中预烧结处理的温度在700~900℃之间,时间在2~3小时,升温速率在1~3℃/分钟;真空烧结温度在1700~1800℃之间,时间在4~8小时,升温速率为6~10℃/分钟;先预烧结再真空烧结,可以得到较高致密度的莫来石透明陶瓷。
实施例1
选择纯度在99.99%以上高纯氧化铝和高纯二氧化硅粉体为原料,高纯氧化铝粉体的粒径在100~200nm,高纯二氧化硅粉体的中位粒径在700nm,氧化铝和二氧化硅摩尔比为1.7:1;以酒精为介质球磨混合粉体,原料:球:酒精质量比为1:6:1.4,粉体在60℃干燥24小时后经200目过筛,在800℃煅烧处理3小时,升温速率为2℃/分钟;采用干压和冷等静压成型,成型具体过程是:干压压力为1000N,对所述混合粉体进行双面加压并保压1分钟,然后将干压预成型素坯在200MPa压力下进行冷等静压处理3分钟;所得成型素坯经800℃预烧处理3小时后,在真空条件下反应烧结,真空度为5×10-3Pa,升温速率为8℃/分钟,烧结温度为1780℃,保温时间为6小时,即可得到莫来石透明陶瓷。
实施例2
选择纯度在99.99%以上高纯氧化铝和高纯二氧化硅粉体为原料,加入0.2wt%氧化镁作为烧结助剂,高纯氧化铝粉体的粒径在100~200nm,高纯二氧化硅粉体的中位粒径在700nm,氧化铝和二氧化硅摩尔比为1.7:1;以酒精为介质球磨混合粉体,原料:球:酒精质量比为1:6:1.4,粉体在60℃干燥24小时后经200目过筛,在800℃煅烧处理3小时后,升温速率为2℃/分钟;采用干压和冷等静压成型,成型具体过程是:干压压力为1000N,对所述混合粉体进行双面加压并保压1分钟,然后将干压预成型素坯在200MPa压力下进行冷等静压处理3分钟;所得成型素坯经800℃预烧处理3小时后,在真空条件下烧结,真空度为5×10-3Pa,升温速率为8℃/分钟,烧结温度为1780℃,保温时间为6小时,即可得到莫来石透明陶瓷。
实施例3
选择纯度在99.99%以上高纯氧化铝和高纯二氧化硅粉体为原料,加入0.05wt%氧化镁作为烧结助剂,高纯氧化铝粉体的粒径在100~200nm,高纯二氧化硅粉体的中位粒径在700nm,氧化铝和二氧化硅摩尔比为1.7:1;以酒精为介质球磨混合粉体,原料:球:酒精质量比为1:6:1.4,粉体在70℃干燥24小时后经200目过筛,在800℃煅烧处理3小时,升温速率为1℃/分钟;采用干压和冷等静压成型,成型具体过程是:干压压力为1570N,对所述混合粉体进行双面加压并保压1分钟,然后将干压预成型素坯在230MPa压力下进行冷等静压处理2分钟;所得成型素坯经800℃预烧处理2小时后,在真空条件下反应烧结,真空度为10- 3Pa,烧结温度为1750℃,保温时间为5小时,即可得到莫来石透明陶瓷。
实施例4
选择纯度在99.99%以上高纯氧化铝和高纯二氧化硅粉体为原料,加入0.1wt%氧化镁作为烧结助剂高纯氧化铝粉体的粒径在100~200nm,高纯二氧化硅粉体的中位粒径在700nm,氧化铝和二氧化硅摩尔比为1.8:1;以酒精为介质球磨混合粉体,原料:球:酒精质量比为1:6:1.4,粉体在70℃干燥24小时后经200目过筛,在800℃煅烧处理3小时,升温速率为1.5℃/分钟;采用干压和冷等静压成型,成型具体过程是:干压压力为1000N,对所述混合粉体进行双面加压并保压1分钟,然后将干压预成型素坯在180MPa压力下进行冷等静压处理1分钟;所得成型素坯经800℃预烧处理2小时后,在真空条件下烧结,真空度为8×10-3Pa,升温速率为8℃/分钟,烧结温度为1780℃,保温时间为5小时,即可得到莫来石透明陶瓷。
实施例5
选择纯度在99.99%以上高纯氧化铝和高纯二氧化硅粉体为原料,高纯氧化铝粉体的粒径在100~200nm,高纯二氧化硅粉体的中位粒径在700nm,氧化铝和二氧化硅摩尔比为1.9:1;以酒精为介质球磨混合粉体,原料:球:酒精质量比为1:6:1.4,粉体在70℃干燥24小时后经200目过筛,在800℃煅烧处理3小时,升温速率为1.5℃/分钟;采用干压和冷等静压成型,成型具体过程是:干压压力为1570N,对所述混合粉体进行双面加压并保压1分钟,然后将干压预成型素坯在230MPa压力下进行冷等静压处理1分钟;所得成型素坯经800℃预烧处理3小时后,在真空条件下烧结,真空度为10-2Pa,升温速率为8℃/分钟,烧结温度为1780℃,保温时间为6小时,即可得到莫来石透明陶瓷。
图1XRD表明不加入烧结助剂MgO的样品在1780℃烧结时除了莫来石相还有少量氧化铝相,加入0.2wt%MgO可得到纯相的莫来石陶瓷;图2红外波段透过曲线表明加入氧化镁有利于提高红外透过率;由图3中的抛光腐蚀面可以看出,陶瓷气孔较少。
Claims (8)
1.一种固相反应烧结法制备纯相莫来石红外透明陶瓷的方法,其特征在于,包括:
按摩尔比1.70~1.94:1称取氧化铝和二氧化硅,加入0.03~0.3wt%氧化镁作为烧结助剂,球磨得到混合粉体;
将所得混合粉体于700~900℃煅烧2~4小时;
将经煅烧处理的混合粉体成型得到素坯;以及
对所得素坯于700~900℃进行预烧结处理2~3小时,然后于真空条件下在1700~1800℃烧结4~8小时,升温速率为6~10℃/分钟,得到莫来石红外透明陶瓷。
2.根据权利要求1所述的制备纯相莫来石红外透明陶瓷的方法,其特征在于,混合粉体煅烧升温速率为1~3℃/分钟。
3.根据权利要求1所述的制备纯相莫来石红外透明陶瓷的方法,其特征在于,所述氧化铝为高纯氧化铝,所述高纯氧化铝主晶相为α-Al2O3,且所述氧化铝和二氧化硅的纯度为99.99%以上。
4.根据权利要求1所述的制备纯相莫来石红外透明陶瓷的方法,其特征在于,所述二氧化硅为高纯二氧化硅,球磨后所述氧化铝粉体粒径为100~200nm,高纯二氧化硅的中位粒径为600~800nm。
5.根据权利要求1所述的制备纯相莫来石红外透明陶瓷的方法,其特征在于,球磨介质为酒精,其中氧化铝和二氧化硅的总质量:球:酒精质量比为1:4~8:1.2~1.6。
6.根据权利要求1所述的制备纯相莫来石红外透明陶瓷的方法,其特征在于,所述成型的方法为:在700~1600N的压力下保压1~3分钟进行干压预成型后,再在180~230N的压力下保压1~3分钟进行等静压处理成型。
7.根据权利要求1所述的制备纯相莫来石红外透明陶瓷的方法,其特征在于,所述预烧结的气氛为空气气氛,升温速率为1~3℃/分钟。
8.根据权利要求1-7中任一项所述的制备纯相莫来石红外透明陶瓷的方法,其特征在于,烧结方法为真空烧结,真空度为10-3~10-2Pa。
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