CN107188555A - 一种陶瓷靶材的制备方法 - Google Patents

一种陶瓷靶材的制备方法 Download PDF

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CN107188555A
CN107188555A CN201710481516.6A CN201710481516A CN107188555A CN 107188555 A CN107188555 A CN 107188555A CN 201710481516 A CN201710481516 A CN 201710481516A CN 107188555 A CN107188555 A CN 107188555A
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彭彪林
徐梦星
李路成
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Guangxi University
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Abstract

本发明提供一种陶瓷靶材的制备方法，[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3，其中M为Hf、Zr和Sn中的一种；具体步骤为(1)烘料，将起始原料Bi2O3、Na2CO3、BaCO3、TiO2、La2O3、MO2置于烘箱中烘料；(2)配料，将步骤(1)烘干的原料按照[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3相应的化学计量比称量；(3)球磨，将步骤(2)称量好的原料置于以酒精为介质、氧化锆球为磨球的尼龙罐中进行混料；(4)干燥，将步骤(3)制得的均匀浆料烘干；(5)煅烧，将步骤(4)烘干的粉料过筛并轻压成块状坯体置于马弗炉中；(6)球磨，将步骤(5)煅烧后的粉料研磨成细粉；(7)制坯，将步骤(6)制成的陶瓷粉料采用钢模手压成样片；(8)烧结，将步骤(7)制成的陶瓷坯体置于马弗炉中；(9)冷却，自然冷却至室温。本发明制备方法相对简单，整个过程没有使用含铅的原料，是一种绿色制备技术。

Description

一种陶瓷靶材的制备方法
技术领域
本发明属于功能材料领域，涉及[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3陶瓷靶材的制备方法。
背景技术
随着电子、信息和控制技术朝着微型化、高集成化方向的发展，以及可再生动力能源设备(如电动汽车、电网中的大型能量调节器等移动能源设备)的发展和使用，高密度储能电容器的发展已经被提上日程。作为铁电体材料的一类分支，反铁电体材料因其具有更高的储能密度而使得其逐渐成为高密度储能电容器的优秀候选材料。目前对反铁电材料储能效应的研究主要集中在锆钛酸铅(PZT)为基的含铅材料体系中，如Sn掺杂的Pb(Zr,Sn,Ti)O3(PZST)陶瓷材料以及La掺杂的Pb0.97La0.02(Zr0.65Sn0.24Ti0.11)O3薄膜材料。
材料一般以两种形态应用于电荷的存储，即体相及薄膜。体相陶瓷材料由于耐击穿电场强度不高，且操作电压过高，不易控制，难以获得大的电场强度用来提高体系的储能密度。材料薄膜化后，在较低的操作电压下，可获得高于体相材料击穿场强几十倍甚至上百倍的电场强度，从而能够获得高的储能密度。
[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3是一种无铅环保的反铁电体材料，以高温固相合成法制备出的[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3陶瓷为靶材，利用磁控溅射或脉冲沉积法轰击陶瓷靶材从而制备出具有击穿场强高、极化强度大的高储能密度反铁电薄膜。本实验制备出的[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti(1-x)MxO3陶瓷靶材将可以作为生长[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti(1-x)MxO3薄膜所用的靶材，有利于击穿场强高、极化强度大、剩余极化强度低的高储能密度[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3反铁电薄膜的制备。
发明内容
本申请在现有技术的基础上，通过不断研究和改进，得到一种全新的陶瓷靶材制备工艺。
本发明的目的是提供一种[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3陶瓷靶材的制备方法，其中M为Hf、Zr和Sn中的一种；具体步骤为：
(1)烘料：称量前将起始原料Bi2O3、Na2CO3、BaCO3、TiO2、La2O3、MO2置于烘箱中烘料3～6小时，烘料温度为100～120℃；
(2)配料：将步骤(1)烘干的原料按照[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3相应的化学计量比称量；
(3)球磨：将步骤(2)称量好的原料置于以酒精为介质、氧化锆球为磨球的尼龙罐中进行混料，混料时间为4～12小时，制成均匀浆料；
(4)干燥：将步骤(3)制得的均匀浆料烘干；
(5)煅烧：将步骤(4)烘干的粉料过筛并轻压成块状坯体置于马弗炉中，在800～950℃煅烧4～8小时，制成煅烧粉料；
(6)球磨：将步骤(5)煅烧后的粉料研磨成细粉，再次球磨、烘干得到陶瓷粉料；
(7)制坯：将步骤(6)制成的陶瓷粉料采用钢模手压成直径5～20mm、厚度约0.5～1.2mm的样片，将样片放入冷等静压机中，施加200～350MPa的压力，保压60～180s，制得[(Bi1/ 2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3陶瓷坯体，其中M为Hf、Zr和Sn中的一种；
(8)烧结：将步骤(7)制成的陶瓷坯体置于马弗炉中，在1100～1200℃烧结4～6小时；
(9)冷却：自然冷却至室温，即制得[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3陶瓷靶材。
进一步，步骤(1)中所述的起始原料的重量份数配比为：Bi2O3：40～50份，Na2CO3：5～15份，BaCO3：4～7份，TiO2：30～35份，La2O3：1～2份，MO2：1～3份。
进一步，步骤(5)中所述的煅烧温度为900℃。
进一步，步骤(5)中所述的煅烧时间为6小时。
进一步，步骤(8)中所述的烧结时间为5小时。
本发明的有益效果是：通过上述制备方法参数的限制，获得一种具有无铅、纯度高、致密性好、平均晶粒尺寸小、高介电常数、电场击穿强度大、储能密度高等优点的陶瓷；本发明制备方法相对简单，整个过程没有使用含铅的原料，是一种绿色制备技术。
附图说明
图1(a)、(b)、(c)分别为本发明实施例1、2制得的[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Hf0.04O3、[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Zr0.04O3和[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Sn0.04O3陶瓷靶材的SEM图谱；
图2为本发明实施例2制得的[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Zr0.04O3陶瓷靶材的XRD图谱；
图3为本发明实施例2制得的[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Zr0.04O3陶瓷靶材的介电温谱；
图4为本发明实施例2制得的[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Zr0.04O3陶瓷靶材的电滞回线。
具体实施方式
实施例1
(1)烘料：称量前将起始原料Bi2O3、Na2CO3、BaCO3、TiO2、La2O3、HfO2置于烘箱中烘料3小时，烘料温度为120℃。
(2)配料：步骤(1)烘干的原料按照[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Hf0.04O3相应的化学计量比称量。
(3)球磨：将步骤(2)称量好的原料置于以酒精为介质、氧化锆球为磨球的尼龙罐中进行混料，混料时间为8小时，制成均匀浆料。
(4)干燥：将步骤(3)制得的均匀浆料烘干。
(5)煅烧：将步骤(4)烘干的粉料过筛并轻压成块状坯体，在800℃煅烧4小时，制成煅烧粉料。
(6)球磨：将步骤(5)煅烧后的粉料研磨成细粉，再次球磨、烘干得到陶瓷粉料。
(7)制坯：将步骤(6)制成的陶瓷粉料采用钢模手压成直径12mm、厚度约0.5mm的样片，将样片放入冷等静压机中，施加200MPa的压力，保压120s，制得[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Hf0.04O3陶瓷坯体。
(8)烧结：将步骤(7)制成的陶瓷坯体置于马弗炉中，在1100摄氏度烧结5小时。
(9)冷却：自然冷却至室温，即制得[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Hf0.04O3陶瓷靶材。
附图1(a)为实施例1制得的[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Hf0.04O3陶瓷靶材的SEM图谱，从SEM照片中可以看出，样品呈现出致密的显微结构，没有明显的孔洞，且样品平均粒径为4μm。
实施例2
(1)烘料：称量前将起始原料Bi2O3、Na2CO3、BaCO3、TiO2、La2O3、ZrO2置于烘箱中烘料4小时，烘料温度为110℃。
(2)配料：步骤(1)烘干的原料按照[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Zr0.04O3相应的化学计量比称量。
(3)球磨：将步骤(2)称量好的原料置于以酒精为介质、氧化锆球为磨球的尼龙罐中进行混料，混料时间为4小时，制成均匀浆料。
(4)干燥：将步骤(3)制得的均匀浆料烘干。
(5)煅烧：将步骤(4)烘干的粉料过筛并轻压成块状坯体，在900℃煅烧6小时，制成煅烧粉料。
(6)球磨：将步骤(5)煅烧后的粉料研磨成细粉，再次球磨、烘干得到陶瓷粉料。
(7)制坯：将步骤(6)制成的陶瓷粉料采用钢模手压成直径10mm、厚度约1mm的样片，将样片放入冷等静压机中，施加300MPa的压力，保压60s，制得[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Zr0.04O3陶瓷坯体。
(8)烧结：将步骤(7)制成的陶瓷坯体置于马弗炉中，在1150摄氏度烧结6小时。
(9)冷却：自然冷却至室温，即制得[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Zr0.04O3陶瓷靶材。
附图1(b)为实施例2制得的[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Zr0.04O3陶瓷靶材的SEM图谱，从SEM照片中可以看出，样品呈现出致密的显微结构，没有明显的孔洞，且样品平均粒径为4μm。
附图2为实施例2制得的[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Zr0.04O3陶瓷靶材的XRD图谱，从图中可以看出，通过本方法烧结制备出的陶瓷靶材为纯的钙钛矿相结构，无焦绿石相等杂相存在。
附图3为实施例2制得的[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Zr0.04O3陶瓷靶材的介电温谱，从介电温谱中可以得到样品的介电常数为3068，较其它的陶瓷的介电常数高，低温段的介电常数峰有明显的频率色散特征，而其高温段介电常数峰的频率色散特征却很弱。
附图4为实施例2制得的[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Zr0.04O3陶瓷靶材的电滞回线，从图中可以看出，回线包围的面积很小，代表着样品的能量损耗很小。最大电场击穿强度为90kv/cm，通过根据能量密度计算公式得到样品的储能密度为0.9627(J/cm3)。
实施例3
(1)烘料：称量前将起始原料Bi2O3、Na2CO3、BaCO3、TiO2、La2O3、SnO2置于烘箱中烘料6小时，烘料温度为100℃。
(2)配料：步骤(1)烘干的原料按照[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Sn0.04O3相应的化学计量比称量。
(3)球磨：将步骤(2)称量好的原料置于以酒精为介质、氧化锆球为磨球的尼龙罐中进行混料，混料时间为12小时，制成均匀浆料。
(4)干燥：将步骤(3)制得的均匀浆料烘干。
(5)煅烧：将步骤(4)烘干的粉料过筛并轻压成块状坯体，在950℃煅烧8小时，制成煅烧粉料。
(6)球磨：将步骤(5)煅烧后的粉料研磨成细粉，再次球磨、烘干得到陶瓷粉料。
(7)制坯：将步骤(6)制成的陶瓷粉料采用钢模手压成直径20mm、厚度约1.2mm的样片，将样片放入冷等静压机中，施加350MPa的压力，保压180s，制得[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Sn0.04O3陶瓷坯体。
(8)烧结：将步骤(7)制成的陶瓷坯体置于马弗炉中，在1200摄氏度烧结4小时。
(9)冷却：自然冷却至室温，即制得[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Sn0.04O3陶瓷靶材。
附图1(c)为实施例3制得的[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Sn0.04O3陶瓷靶材的SEM图谱，从SEM照片中可以看出，样品呈现出致密的显微结构，没有明显的孔洞，且样品平均粒径为4μm。

Claims (5)

1.一种陶瓷靶材的制备方法，具体为[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3陶瓷靶材，其中M为Hf、Zr和Sn中的一种，其特征在于具体步骤为：
(1)烘料：称量前将起始原料Bi2O3、Na2CO3、BaCO3、TiO2、La2O3、MO2置于烘箱中烘料3～6小时，烘料温度为100～120℃；
(2)配料：将步骤(1)烘干的原料按照[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3相应的化学计量比称量；
(3)球磨：将步骤(2)称量好的原料置于以酒精为介质、氧化锆球为磨球的尼龙罐中进行混料，混料时间为4～12小时，制成均匀浆料；
(4)干燥：将步骤(3)制得的均匀浆料烘干；
(5)煅烧：将步骤(4)烘干的粉料过筛并轻压成块状坯体置于马弗炉中，在800～950℃煅烧4～8小时，制成煅烧粉料；
(6)球磨：将步骤(5)煅烧后的粉料研磨成细粉，再次球磨、烘干得到陶瓷粉料；
(7)制坯：将步骤(6)制成的陶瓷粉料采用钢模手压成直径5～20mm、厚度约0.5～1.2mm的样片，将样片放入冷等静压机中，施加200～350MPa的压力，保压60～180s，制得[(Bi1/ 2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3陶瓷坯体，其中M为Hf、Zr和Sn中的一种；(样片厚度0.5mm的端点值在具体实施例中并未有体现)
(8)烧结：将步骤(7)制成的陶瓷坯体置于马弗炉中，在1100～1200℃烧结4～6小时；
(9)冷却：自然冷却至室温，即制得[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96M0.04O3陶瓷靶材。
2.根据权利要求1所述的一种陶瓷靶材制备方法，其特征在于，步骤(1)中所述的起始原料的重量份数配比为：Bi2O3：40～50份，Na2CO3：5～15份，BaCO3：4～7份，TiO2：30～35份，La2O3：1～2份，MO2：1～3份。
3.根据权利要求1所述的一种陶瓷靶材制备方法，其特征在于，步骤(5)中所述的煅烧温度为900℃。
4.根据权利要求1所述的一种陶瓷靶材制备方法，其特征在于，步骤(5)中所述的煅烧时间为6小时。
5.根据权利要求1所述的一种陶瓷靶材制备方法，其特征在于，步骤(8)中所述的烧结时间为5小时。
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