CN108164262A - 一种热膨胀系数连续可调的nzp族陶瓷的制备方法 - Google Patents
一种热膨胀系数连续可调的nzp族陶瓷的制备方法 Download PDFInfo
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Abstract
本发明涉及具有热膨胀系数连续可调的NZP族陶瓷材料制备方法,属精细陶瓷材料技术领域。本发明以MⅠMⅡ3Zr2(PO4)3为基体,采用一定量的Ca2+和Sr2+离子分别取代MI、MⅡ位置,用Hf4+离子取代少量的Zr4+离子位置,制备出CaxSr1‑x(HfyZr1‑y)4P6O24(0≤x≤1,0≤y≤1)陶瓷材料。本发明的陶瓷粉体制备工艺采用化学共沉淀法,即把含Ca2+、Sr2+、Zr4+、Hf4+阳离子离子的盐溶液滴加到(NH4)2HPO4的沉淀剂溶液中,在反应过程中控制溶液浓度及PH值,经沉淀、清洗、烘干、煅烧、研磨后可以得到粒度分布均匀、烧结活性好的NZP族陶瓷粉体。粉体经添加适量ZnO、MgO、SiO2、Ta2O5或Nb2O5为烧结助剂,经高温烧结后可以获得热膨胀系数连续可调的陶瓷体材料。本发明的陶瓷产品具有热膨胀系数连续可调、抗压强度高、耐热冲击性好、可加工性强等优点。
Description
技术领域
本发明涉及一种共沉淀工艺制备NZP族陶瓷的方法,属于精细陶瓷技术领域。
背景技术
NZP族磷酸盐陶瓷材料是指与NaZr2P3O12具有相同晶体结构、但化学组分可调的的一类陶瓷材料,因其具有典型的负膨胀至零的膨胀性能而受到广泛关注。NZP的一般分子式可以表示为MⅠMⅡ3Zr2(PO4)3,其中MⅠ、MⅡ、Zr、P等位置均可被其他多种阳离子所取代,所衍生出的一系列化合物统称为NZP族化合物,由这些化合物制成的陶瓷材料称为NZP族陶瓷。
NZP族陶瓷化学性质非常稳定,不被强酸强碱腐蚀,极难氧化,即使在高温条件下也难与其他物质发生反应。并且,NZP族陶瓷通过MⅠ、MⅡ、Zr、P等位置不同离子取代及化学组分不同,可获得热膨胀系数从负值到正值连续可调的多元NZP陶瓷材料。
目前报导的NZP粉体制备普遍采用溶胶-凝胶法,另有少部分是固相反应法和水热合成法。固相反应法虽简单易行,但合成粉料的温度高,时间长,往往难以得到单一相的粉体,且制成的粉体粒径粗,烧结活性小,不易致密化。水热法和溶胶-凝胶法虽可在较低温度下合成单相NZP粉体,粉体的粒度分布均匀,烧结活性高,但设备要求高,合成周期长,产率低,不利于批量生产,限制了这两种方法的应用。
发明内容
针对上述技术现状,本发明采用一定量的Ca2+和Sr2+离子分别取代MI、MⅡ位置,用Hf4+离子取代少量的Zr4+离子位置,制备出CaxSr1-x(HfyZr1-y)4P6O24(0≤x≤1,0≤y≤1)陶瓷材料,该体系材料科在降低材料的整体热膨胀系数的同时,提升其抗热震性能。
本发明采用共沉淀工艺制备热膨胀系数可控的NZP族陶瓷材料。本发明制备NZP族陶瓷材料为CaxSr1-x(HfyZr1-y)4P6O24(0≤x≤1,0≤y≤1)的方法,包括NZP族陶瓷粉体的制备、NZP陶瓷坯体成型及烧结。
具体步骤如下:
(1)按上述化学式CaxSr1-x(HfyZr1-y)4P6O24(0≤x≤1,0≤y≤1)中摩尔配比进行配料,即CaCO3、SrCO3、HfOCl2·8H2O、ZrOCl2·8H2O、(NH4)2HPO4的摩尔份数比为x:(1-x):4y:4(1-y):6,原料选用分析纯CaCO3、SrCO3、HfOCl2·8H2O、ZrOCl2·8H2O、(NH4)2HPO4的化学试剂。将含有Ca2+、Sr2+、Zr4+、Hf4+阳离子离子的盐溶液滴加到过量的(NH4)2HPO4的沉淀剂溶液中,在此过程中控制溶液的PH在7-9之间。(2)将共沉淀工艺制备的悬浮液离心后获得沉淀物,加入大量蒸馏水后分散处理,再次离心处理,多次清洗后,将获得的沉淀物在80℃条件下烘干,过筛后进行900-1200℃煅烧,研磨后即可得到0.5-5μm的CaxSr1-x(HfyZr1-y)4P6O24粉体。(3)在上述方法所制备的粉体中参入适量ZnO、MgO、SiO2、Ta2O5或Nb2O5为烧结助剂,压制成型后,在1100-1300℃烧结后即可得到抗压强度高、热膨胀系数可调的CaxSr1-x(HfyZr1-y)4P6O24陶瓷。
本发明具有如下优点:
1、本发明的粉体制备工艺采用共沉淀法,该方法简单易行,具有制备的产品纯度高、粉体烧结活性好等优点。
2、沉淀物的干燥采取先用大量蒸馏水清洗、再低温烘干的方式,可以洗去沉淀物中的可溶性盐及Cl-离子,可以有效的克服干燥过程中粉体颗粒团聚问题。这种沉淀物经过煅烧后可以到质地疏松的、粒度分布均匀的、烧结活性好的NZP粉体。
3、本发明制备的NZP陶瓷材料,具有抗压强度高、热膨胀系数可调的优点。
具体实施方式
实施例1
(1)取x=0.5,y=0.5按照化学式中Ca0.5Sr0.5(Hf0.5Zr0.5)4P6O24进行配料取样,将4.6g的CaCO3、6.8g的SrCO3、37.8g的HfOCl2·8H2O溶解在276mL的浓度为0.5mol/L的ZrOCl2·8H2O溶液中,将上述混合盐溶液缓慢滴加至607mL浓度为1Mol/L的(NH4)2HPO4中,控制溶液pH=8。
(2)将悬浮液陈腐24h后离心后获得沉淀物,将沉淀物加入蒸馏水分散处理,再次离心,循环5次后,将获得的沉淀物于80℃下烘干,过200目筛。
(3)将沉淀物进行1100℃高温煅烧1h,即获得质量约为100g的Ca0.5Sr0.5(Hf0.5Zr0.5)4P6O24粉体。
(4)将粉体中加入占粉体总质量1%的氧化镁作为烧结助剂,氧化镁的纯度为3%,干压成型后进行1300℃高温煅烧,即获得Ca0.5Sr0.5(Hf0.5Zr0.5)4P6O24陶瓷体材料,经检测,所获得的陶瓷抗压强度124MPa、热膨胀系数5.2×10-7。
实施例2
(1)取x=0.8,y=0.8按照化学式中Ca0.8Sr0.2(Hf0.8Zr0.2)4P6O24进行配料取样,将7.76g的CaCO3、2.86g的SrCO3、19.86g的HfOCl2·8H2O溶解在340ml的浓度为0.5mol/L的ZrOCl2·8H2O溶液中,将上述溶液缓慢滴加至640ml浓度为1Mol/L的(NH4)2HPO4中,控制溶液PH=8。
(2)将悬浮液陈腐24h后离心后获得沉淀物,将沉淀物加入大量蒸馏水分散处理,再次离心,循环5次后,将获得的沉淀物于80℃下烘干,过200目筛。
(3)将沉淀物进行1000℃高温煅烧1h,即获得质量约为100g的Ca0.8Sr0.2(Hf0.8Zr0.2)4P6O24粉体。
(4)将粉体中加入占粉体总质量3%的氧化镁作为烧结助剂,氧化镁的纯度为3%,,干压成型后进行1100℃高温煅烧,即获得Ca0.8Sr0.2(Hf0.8Zr0.2)4P6O24陶瓷体材料,经检测,所获得的陶瓷抗压强度105MPa、热膨胀系数7.8×10-7。
实施例3
(1)当x=0,y=0时,按照化学式SrZr4P6O24中的化学配比,进行配料取样;将14.5gSrCO3溶解在783mL的浓度为0.5mol/L的ZrOCl2·8H2O溶液中,得到混合盐溶液,将所述混合盐溶液滴加到646ml浓度为1Mol/L(NH4)2HPO4的溶液中,在滴加过程中控制溶液pH=7,得到共沉淀工艺制备的悬浮液;
(2)将上述共沉淀工艺制备的悬浮液陈腐12h后离心,获得沉淀物,向沉淀物中加入蒸馏水分散处理,再次离心处理、清洗5次后,将获得的沉淀物在80℃条件下烘干,过200目筛。
(3)过筛后的粉体进行900℃煅烧2小时,研磨后即可得到0.5-5μm的SrZr4P6O24粉体;
(4)将粉体中加入占粉体总质量5%的氧化镁作为烧结助剂,氧化镁的纯度为3%,,干压成型后进行1100℃高温煅烧2小时,即获得SrZr4P6O24陶瓷体材料,经检测,所获得的陶瓷抗压强度87MPa、热膨胀系数9.6×10-7。
实施例4
(1)取x=1,y=1按照化学式中CaHf4P6O24进行配料取样,将8.3g的CaCO3、139g的HfOCl2·8H2O溶解在664ml蒸馏水溶液中,将上述溶液缓慢滴加至548ml浓度为1Mol/L的(NH4)2HPO4中,控制溶液PH=8。
(2)将悬浮液陈腐24h后离心后获得沉淀物,将沉淀物加入大量蒸馏水分散处理,再次离心,循环5次后,将获得的沉淀物于80℃下烘干,过200目筛。
(3)将沉淀物进行1200℃高温煅烧1h,即获得质量约为100g的CaHf4P6O24粉体。
(4)将粉体中加入占粉体总质量2%的氧化镁作为烧结助剂,氧化镁的纯度为3%,,干压成型后进行1300℃高温煅烧,即获得CaHf4P6O24陶瓷体材料,经检测,所获得的陶瓷抗压强度152MPa、热膨胀系数8.4×10-7。
Claims (2)
1.一种热膨胀系数连续可调的NZP族陶瓷的制备方法,其特征在于,包括以下步骤:
(1)原料选用CaCO3、SrCO3、HfOCl2·8H2O、ZrOCl2·8H2O以及(NH4)2HPO4,按照化学式CaxSr1-x(HfyZr1-y)4P6O24(0≤x≤1,0≤y≤1)中的化学配比,进行配料;
(2)将上述原料CaCO3、SrCO3、HfOCl2·8H2O溶解在ZrOCl2·8H2O溶液中,得到含有Ca2+、Sr2+、Zr4+、Hf4+阳离子的混合盐溶液,将所述混合盐溶液滴加到(NH4)2HPO4的溶液中,在滴加过程中控制溶液pH在7-9之间,得到共沉淀工艺制备的悬浮液;
(3)将上述共沉淀工艺制备的悬浮液陈腐12-24h后离心,获得沉淀物,向沉淀物中加入蒸馏水分散处理,再次离心处理、清洗3到5次后,将获得的沉淀物在80℃条件下烘干,过筛后进行900-1200℃煅烧,研磨后即可得到0.5-5μm的CaxSr1-x(HfyZr1-y)4P6O24粉体;
(4)在上述制备的粉体中参入占粉体总质量1%~5%的烧结助剂,压制成型后,在1100-1300℃烧结后即可得CaxSr1-x(HfyZr1-y)4P6O24陶瓷。
2.根据权利要求1所述的一种热膨胀系数连续可调的NZP族陶瓷的制备方法,其特征在于,所述步骤(4)中的烧结助剂为ZnO、MgO、SiO2、Ta2O5、Nb2O5中的一种或几种。
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