CN109437889A - 一种Ti位Cu/Ta共掺杂钛酸铋高温压电陶瓷材料的制备方法 - Google Patents
一种Ti位Cu/Ta共掺杂钛酸铋高温压电陶瓷材料的制备方法 Download PDFInfo
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- 229910002115 bismuth titanate Inorganic materials 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 46
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 22
- 229910052802 copper Inorganic materials 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 7
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 115
- 238000000498 ball milling Methods 0.000 claims description 36
- 239000004570 mortar (masonry) Substances 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 28
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 28
- 238000000227 grinding Methods 0.000 claims description 28
- 229910052709 silver Inorganic materials 0.000 claims description 28
- 239000004332 silver Substances 0.000 claims description 28
- 239000002002 slurry Substances 0.000 claims description 28
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 21
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 21
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 21
- 239000011812 mixed powder Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 19
- 229910052573 porcelain Inorganic materials 0.000 claims description 18
- 238000002791 soaking Methods 0.000 claims description 17
- 239000004615 ingredient Substances 0.000 claims description 15
- 239000000853 adhesive Substances 0.000 claims description 14
- 230000001070 adhesive effect Effects 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 14
- 238000010304 firing Methods 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 238000010348 incorporation Methods 0.000 claims description 13
- 230000010287 polarization Effects 0.000 claims description 10
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000007650 screen-printing Methods 0.000 claims description 7
- 229920002545 silicone oil Polymers 0.000 claims description 7
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims 2
- 239000000919 ceramic Substances 0.000 abstract description 45
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 9
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 10
- 150000001621 bismuth Chemical class 0.000 description 9
- 239000000126 substance Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- -1 bismuth laminated bismuth Chemical class 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 5
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000028161 membrane depolarization Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
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Abstract
本发明公开了一种Ti位Cu/Ta共掺杂钛酸铋高温压电陶瓷材料的制备方法,采用Bi4Ti3O12体系压电材料为基础,在Ti位按照一定的摩尔比掺入Cu、Ta,采用固相合成方法,制备得到此类新型铋层状结构压电陶瓷材料,该压电陶瓷材料的通式为Bi4Ti3‑x(Cu1/3Ta2/3)xO12,其中0<x≤0.03。与现有技术相比,本发明获得的压电陶瓷材料,主要性能参数d33=34pC/N,TC=677℃,在500℃时,ρ=9.02×106Ω·cm,此外制备工艺稳定可靠,生产成本低,易于实现工业化生产,在高温领域具有良好的应用前景。利用这种材料制得的陶瓷元件,组装成各种压电传感器,能够运用在航天航空、石油化工等特殊高温环境下。
Description
技术领域
本发明涉及一种铋层状结构钛酸铋高温压电陶瓷材料的制备方法,具体涉及一种Cu/Ta共掺杂的铋层状结构钛酸铋(Bi4Ti3O12)压电陶瓷材料的制备,属于压电陶瓷材料领域。
背景技术
目前,应用最广的压电材料主要是钙钛矿结构的PZT基压电陶瓷,但是这类压电陶瓷的居里温度一般在390℃以下,由于压电材料退极化现象的存在,压电材料在居里温度以下无法正常工作。随着航空航天、地质勘探等工业的飞速发展和人类社会可持续发展的需求,因此有必要寻求一种居里温度高,压点性能优异的环境友好型压电材料。
由于居里温度高、耐疲劳性能好,铋层状结构的陶瓷被认为是高温压电材料的理想选择。铋层状结构的陶瓷材料是由(Bi2O2)2+层和钙钛矿结构的晶格层相互交替叠加而成的,其化学通式为(Bi2O2)2+(Am-1BmO3m+1)2-,上式中A为适合十二面体配位的离子,如Na+,Ca2+,La3+等,B为适合八面体配位的离子,如Ti4+,Nb5+,Ta5+等,m为整数,取值为1到6。钛酸铋(Bi4Ti3O12)是m=3的铋层状结构材料,其居里温度高达675℃,压电常数d33约为8pC/N,与实际应用相比,虽然居里温度满足高温下的使用要求,但是其压电性能达不到应用要求(d33>30pC/N)。因此,如何在不降低居里温度的同时提高压电性能以获得高温范围内稳定使用的铋层状压电陶瓷材料成为压电陶瓷材料领域研究的一个重要课题。
目前,尚未见以Cu/Ta共掺杂来提高铋层状结构钛酸铋(Bi4Ti3O12)压电陶瓷材料性能的相关报道。
发明内容
针对上述现有技术不足,本发明的目的是提供一种铋层状结构钛酸铋高温压电陶瓷材料的制备方法,利用Cu、Ta元素对铋层状结构钛酸铋(Bi4Ti3O12)压电陶瓷材料进行共掺杂改性,在不降低居里温度温度的同时,提高其压电性能,制备出一种新型的、环境友好型的压电陶瓷材料。
为了克服现有技术存在的缺陷,本发明提供以下技术方案:
一种铋层状结构钛酸铋高温压电陶瓷材料的制备方法,步骤如下:
配料:以Bi2O3粉体、TiO2粉体、CuO粉体和Ta2O5粉体为原料,按通式Bi4Ti3-x(Cu1/ 3Ta2/3)xO12中Bi、Ti、Cu和Ta的化学计量进行配料,其中0<x≤0.03;
一次球磨:向上述混合物中加入与混合物等量的无水乙醇,持续球磨12~24小时,使粉体混合均匀形成浆料,由此可以进一步的提高钛酸铋高温压电陶瓷材料的综合性能;
烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨,得到粉料;
压片预烧:将粉料置于磨具中预压成料块,将料块预烧,预烧温度为675~750℃,保温时间2~4小时;
二次球磨:将预烧后的料块在研钵中,经碾碎研磨后得到初级粉料,向得到的初级粉料中加入与初级粉料等量的无水乙醇,持续球磨12~24小时,使粉体混合均匀形成浆料;
烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨成粉料;
造粒成型:将蒸馏水以及浓度为8%的聚乙烯醇溶液(PVA)作为粘合剂掺入粉料中,掺入的蒸馏水的质量是粉料质量的2.5%,掺入的粘合剂的质量是粉料质量的5%,在研钵中混合均匀;将混合后的粉料置于磨具中,压制成生坯;将生坯在研钵中磨碎成粉料,通过60目和120目的筛子过筛,取60目和120目筛子中间层的粉料,得到了颗粒大小合适的粉料;将粉料置于磨具中,在200MPa的压强下压制成生坯;
排胶:将生坯排胶,在650℃的温度下煅烧3小时,排除生坯中的PVA,得到瓷坯;
烧结:将瓷坯进行烧结,烧结温度为1000~1100℃,保温时间2~4小时,得到陶瓷片;
涂电极:将陶瓷片清洗、烘干、丝网印刷涂银电极、烧银,烧银温度500~600℃,保温时间1~2小时;
极化:将镀好银电极的陶瓷片置于120~160℃的硅油中,极化电压为12kV/mm~15kV/mm,极化时间为20min~40min。
优选地,在所述一次球磨和二次球磨过程中,所述球磨时间为12小时。
优选地,在所述预烧过程中,所述预烧温度为725℃,所述保温时间为4小时。
优选地,在所述烧结过程中,所述烧结温度为1050℃,所述保温时间为4小时。
优选的,x=0.01。
优选的,x=0.015。
优选的,x=0.02。
优选的,x=0.025。
优选的,x=0.03。
与现有技术相比较,本发明的技术方案,通过Cu和Ta取代B位的Ti,并控制掺杂元素的加入量,有效提高了钛酸铋高温压电陶瓷材料的压电性能。需要说明的是,现有技术中虽然有许多关于对压电陶瓷材料进行元素掺杂的报道,但是不同的掺杂元素,掺杂元素不同的加入量,都会对压电陶瓷材料的整体性能产生较大影响,则需要在试验过程中不断摸索,反复试验才能得到,发明人在前期研究中也尝试了多种不同元素对钛酸铋高温压电陶瓷材料的掺杂,但对于其他元素的掺杂,采用本发明的Cu和Ta元素共掺杂,制备得到的铋层状结构钛酸铋高温压电材料表现出更为优异的压电性能。
实验数据表明,本发明具有优异的性能:
本发明Cu、Ta元素共掺杂改性的铋层状钛酸铋(Bi4Ti3O12)压电陶瓷材料,居里温度为677℃,压电常数d33高达34pC/N,并具有良好的高温稳定性,在500℃时,电阻率ρ=9.02×106Ω·cm,在高温领域具有良好的应用前景。
另外,该发明通过传统压电陶瓷工业制得,制备成本低,工业简单且适合于大批量工业化生产,掺杂改性后的陶瓷材料的压电性能较之前提高了四倍以上,推进了高温压电材料的进展。
附图说明
图1是实施例1中制备的Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.01陶瓷的XRD衍射图,以及介电常数随温度变化的曲线;
图2是实施例2中制备的Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.015陶瓷的XRD衍射图,以及介电常数随温度变化的曲线;
图3是实施例3中制备的Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.02陶瓷的XRD衍射图,以及介电常数随温度变化的曲线;
图4是实施例4中制备的Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.025陶瓷的XRD衍射图,以及介电常数随温度变化的曲线;
图5是实施例5中制备的Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.03陶瓷的XRD衍射图,以及介电常数随温度变化的曲线;
图6是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的居里温度变化图;
图7是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的室温压电系数变化图;
图8是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的500℃时电阻率变化图。
具体实施方式
下面结合实施例对本发明做进一步的说明。
实施例1
制备符合化学组成Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.01的Cu/Ta共掺杂改性的钛酸铋(Bi4Ti3O12)无铅压电陶瓷,包括以下几个步骤:
(1)配料:以Bi2O3粉体、TiO2粉体、CuO粉体和Ta2O5粉体为原料,按通式中Bi、Ti、Cu和Ta的化学计量进行配料;
(2)一次球磨:向上述混合物中加入与混合物等量的无水乙醇,持续球磨12小时,使粉体混合均匀形成浆料,由此可以进一步的提高钛酸铋高温压电陶瓷材料的综合性能;
(3)烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨,得到粉料;
(4)压片预烧:将粉料置于磨具中预压成料块,将料块预烧,预烧温度为725℃,保温时间4小时;
(5)二次球磨:将预烧后的料块在研钵中,经碾碎研磨后得到初级粉料,向得到的初级粉料中加入与初级粉料等量的无水乙醇,持续球磨12小时,使粉体混合均匀形成浆料;
(6)烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨成粉料;
(7)造粒成型:将蒸馏水以及浓度为8%的聚乙烯醇溶液(PVA)作为粘合剂掺入粉料中,掺入的蒸馏水的质量是粉料质量的2.5%,掺入的粘合剂的质量是粉料质量的5%,在研钵中混合均匀;将混合后的粉料置于磨具中,压制成生坯;将生坯在研钵中磨碎成粉料,通过60目和120目的筛子过筛,取60目和120目筛子中间层的粉料,得到了颗粒大小合适的粉料;将粉料置于磨具中,在200MPa的压强下压制成生坯;
(8)排胶:将生坯排胶,在650℃的温度下煅烧3小时,排除生坯中的PVA,得到瓷坯;
(9)烧结:将瓷坯进行烧结,烧结温度为1050℃,保温时间4小时,得到陶瓷片;
(10)涂电极:将陶瓷片清洗、烘干、丝网印刷涂银电极、烧银,烧银温度500~600℃,保温时间1~2小时;
(11)极化:将镀好银电极的陶瓷片置于120~160℃的硅油中,极化电压为12kV/mm~15kV/mm,极化时间为20min~40min。
如图1中所示为实施例1中制备的Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.01陶瓷的XRD衍射图,以及介电常数随温度变化的曲线;图6是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的居里温度变化图;图7是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的室温压电系数变化图;图8是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的500℃时电阻率变化图。
由图1可以看出,本实施例制备的Cu/Ta共掺杂改性的钛酸铋无铅压电陶瓷与纯相的钛酸铋压电陶瓷的XRD图谱基本一致。
测试结果如下:d33=29pC/N,TC=677℃,500℃时电阻率ρ=4.28×105Ω·cm。
实施例2
制备符合化学组成Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.015的Cu/Ta共掺杂改性的钛酸铋(Bi4Ti3O12)无铅压电陶瓷,包括以下几个步骤:
(1)配料:以Bi2O3粉体、TiO2粉体、CuO粉体和Ta2O5粉体为原料,按通式中Bi、Ti、Cu和Ta的化学计量进行配料;
(2)一次球磨:向上述混合物中加入与混合物等量的无水乙醇,持续球磨12小时,使粉体混合均匀形成浆料,由此可以进一步的提高钛酸铋高温压电陶瓷材料的综合性能;
(3)烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨,得到粉料;
(4)压片预烧:将粉料置于磨具中预压成料块,将料块预烧,预烧温度为725℃,保温时间4小时;
(5)二次球磨:将预烧后的料块在研钵中,经碾碎研磨后得到初级粉料,向得到的初级粉料中加入与初级粉料等量的无水乙醇,持续球磨12小时,使粉体混合均匀形成浆料;
(6)烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨成粉料;
(7)造粒成型:将蒸馏水以及浓度为8%的聚乙烯醇溶液(PVA)作为粘合剂掺入粉料中,掺入的蒸馏水的质量是粉料质量的2.5%,掺入的粘合剂的质量是粉料质量的5%,在研钵中混合均匀;将混合后的粉料置于磨具中,压制成生坯;将生坯在研钵中磨碎成粉料,通过60目和120目的筛子过筛,取60目和120目筛子中间层的粉料,得到了颗粒大小合适的粉料;将粉料置于磨具中,在200MPa的压强下压制成生坯;
(8)排胶:将生坯排胶,在650℃的温度下煅烧3小时,排除生坯中的PVA,得到瓷坯;
(9)烧结:将瓷坯进行烧结,烧结温度为1050℃,保温时间4小时,得到陶瓷片;
(10)涂电极:将陶瓷片清洗、烘干、丝网印刷涂银电极、烧银,烧银温度500~600℃,保温时间1~2小时;
(11)极化:将镀好银电极的陶瓷片置于120~160℃的硅油中,极化电压为12kV/mm~15kV/mm,极化时间为20min~40min。
如图2中所示为实施例2中制备的Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.015陶瓷的XRD衍射图,以及介电常数随温度变化的曲线;图6是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的居里温度变化图;图7是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的室温压电系数变化图;图8是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的500℃时电阻率变化图。
由图2可以看出,本实施例制备的Cu/Ta共掺杂改性的钛酸铋无铅压电陶瓷与纯相的钛酸铋压电陶瓷的XRD图谱基本一致。
测试结果如下:d33=34pC/N,TC=677℃,500℃时电阻率ρ=9.02×106Ω·cm。
实施例3
制备符合化学组成Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.02的Cu/Ta共掺杂改性的钛酸铋(Bi4Ti3O12)无铅压电陶瓷,包括以下几个步骤:
(1)配料:以Bi2O3粉体、TiO2粉体、CuO粉体和Ta2O5粉体为原料,按通式中Bi、Ti、Cu和Ta的化学计量进行配料;
(2)一次球磨:向上述混合物中加入与混合物等量的无水乙醇,持续球磨12小时,使粉体混合均匀形成浆料,由此可以进一步的提高钛酸铋高温压电陶瓷材料的综合性能;
(3)烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨,得到粉料;
(4)压片预烧:将粉料置于磨具中预压成料块,将料块预烧,预烧温度为725℃,保温时间4小时;
(5)二次球磨:将预烧后的料块在研钵中,经碾碎研磨后得到初级粉料,向得到的初级粉料中加入与初级粉料等量的无水乙醇,持续球磨12小时,使粉体混合均匀形成浆料;
(6)烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨成粉料;
(7)造粒成型:将蒸馏水以及浓度为8%的聚乙烯醇溶液(PVA)作为粘合剂掺入粉料中,掺入的蒸馏水的质量是粉料质量的2.5%,掺入的粘合剂的质量是粉料质量的5%,在研钵中混合均匀;将混合后的粉料置于磨具中,压制成生坯;将生坯在研钵中磨碎成粉料,通过60目和120目的筛子过筛,取60目和120目筛子中间层的粉料,得到了颗粒大小合适的粉料;将粉料置于磨具中,在200MPa的压强下压制成生坯;
(8)排胶:将生坯排胶,在650℃的温度下煅烧3小时,排除生坯中的PVA,得到瓷坯;
(9)烧结:将瓷坯进行烧结,烧结温度为1050℃,保温时间4小时,得到陶瓷片;
(10)涂电极:将陶瓷片清洗、烘干、丝网印刷涂银电极、烧银,烧银温度500~600℃,保温时间1~2小时;
(11)极化:将镀好银电极的陶瓷片置于120~160℃的硅油中,极化电压为12kV/mm~15kV/mm,极化时间为20min~40min。
如图3中所示为实施例3中制备的Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.02陶瓷的XRD衍射图,以及介电常数随温度变化的曲线;图6是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的居里温度变化图;图7是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的室温压电系数变化图;图8是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的500℃时电阻率变化图。
由图3可以看出,本实施例制备的Cu/Ta共掺杂改性的钛酸铋无铅压电陶瓷与纯相的钛酸铋压电陶瓷的XRD图谱基本一致。
测试结果如下:d33=29pC/N,TC=676℃,500℃时电阻率ρ=2.67×107Ω·cm。
实施例4
制备符合化学组成Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.025的Cu/Ta共掺杂改性的钛酸铋(Bi4Ti3O12)无铅压电陶瓷,包括以下几个步骤:
(1)配料:以Bi2O3粉体、TiO2粉体、CuO粉体和Ta2O5粉体为原料,按通式中Bi、Ti、Cu和Ta的化学计量进行配料;
(2)一次球磨:向上述混合物中加入与混合物等量的无水乙醇,持续球磨12小时,使粉体混合均匀形成浆料,由此可以进一步的提高钛酸铋高温压电陶瓷材料的综合性能;
(3)烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨,得到粉料;
(4)压片预烧:将粉料置于磨具中预压成料块,将料块预烧,预烧温度为725℃,保温时间4小时;
(5)二次球磨:将预烧后的料块在研钵中,经碾碎研磨后得到初级粉料,向得到的初级粉料中加入与初级粉料等量的无水乙醇,持续球磨12小时,使粉体混合均匀形成浆料;
(6)烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨成粉料;
(7)造粒成型:将蒸馏水以及浓度为8%的聚乙烯醇溶液(PVA)作为粘合剂掺入粉料中,掺入的蒸馏水的质量是粉料质量的2.5%,掺入的粘合剂的质量是粉料质量的5%,在研钵中混合均匀;将混合后的粉料置于磨具中,压制成生坯;将生坯在研钵中磨碎成粉料,通过60目和120目的筛子过筛,取60目和120目筛子中间层的粉料,得到了颗粒大小合适的粉料;将粉料置于磨具中,在200MPa的压强下压制成生坯;
(8)排胶:将生坯排胶,在650℃的温度下煅烧3小时,排除生坯中的PVA,得到瓷坯;
(9)烧结:将瓷坯进行烧结,烧结温度为1050℃,保温时间4小时,得到陶瓷片;
(10)涂电极:将陶瓷片清洗、烘干、丝网印刷涂银电极、烧银,烧银温度500~600℃,保温时间1~2小时;
(11)极化:将镀好银电极的陶瓷片置于120~160℃的硅油中,极化电压为12kV/mm~15kV/mm,极化时间为20min~40min。
如图4中所示为实施例4中制备的Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.025陶瓷的XRD衍射图,以及介电常数随温度变化的曲线;图6是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的居里温度变化图;图7是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的室温压电系数变化图;图8是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的500℃时电阻率变化图。
由图4可以看出,本实施例制备的Cu/Ta共掺杂改性的钛酸铋无铅压电陶瓷与纯相的钛酸铋压电陶瓷的XRD图谱基本一致。
测试结果如下:d33=29pC/N,TC=676℃,500℃时电阻率ρ=2.31×107Ω·cm。
实施例5
制备符合化学组成Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.03的Cu/Ta共掺杂改性的钛酸铋(Bi4Ti3O12)无铅压电陶瓷,包括以下几个步骤:
(1)配料:以Bi2O3粉体、TiO2粉体、CuO粉体和Ta2O5粉体为原料,按通式中Bi、Ti、Cu和Ta的化学计量进行配料;
(2)一次球磨:向上述混合物中加入与混合物等量的无水乙醇,持续球磨12小时,使粉体混合均匀形成浆料,由此可以进一步的提高钛酸铋高温压电陶瓷材料的综合性能;
(3)烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨,得到粉料;
(4)压片预烧:将粉料置于磨具中预压成料块,将料块预烧,预烧温度为725℃,保温时间4小时;
(5)二次球磨:将预烧后的料块在研钵中,经碾碎研磨后得到初级粉料,向得到的初级粉料中加入与初级粉料等量的无水乙醇,持续球磨12小时,使粉体混合均匀形成浆料;
(6)烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨成粉料;
(7)造粒成型:将蒸馏水以及浓度为8%的聚乙烯醇溶液(PVA)作为粘合剂掺入粉料中,掺入的蒸馏水的质量是粉料质量的2.5%,掺入的粘合剂的质量是粉料质量的5%,在研钵中混合均匀;将混合后的粉料置于磨具中,压制成生坯;将生坯在研钵中磨碎成粉料,通过60目和120目的筛子过筛,取60目和120目筛子中间层的粉料,得到了颗粒大小合适的粉料;将粉料置于磨具中,在200MPa的压强下压制成生坯;
(8)排胶:将生坯排胶,在650℃的温度下煅烧3小时,排除生坯中的PVA,得到瓷坯;
(9)烧结:将瓷坯进行烧结,烧结温度为1050℃,保温时间4小时,得到陶瓷片;
(10)涂电极:将陶瓷片清洗、烘干、丝网印刷涂银电极、烧银,烧银温度500~600℃,保温时间1~2小时;
(11)极化:将镀好银电极的陶瓷片置于120~160℃的硅油中,极化电压为12kV/mm~15kV/mm,极化时间为20min~40min。
如图5中所示为实施例5中制备的Bi4Ti3-x(Cu1/3Ta2/3)xO12,x=0.03陶瓷的XRD衍射图,以及介电常数随温度变化的曲线;图6是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的居里温度变化图;图7是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的室温压电系数变化图;图8是不同量的Cu/Ta掺杂Bi4Ti3-x(Cu1/3Ta2/3)xO12陶瓷的500℃时电阻率变化图。
由图5可以看出,本实施例制备的Cu/Ta共掺杂改性的钛酸铋无铅压电陶瓷与纯相的钛酸铋压电陶瓷的XRD图谱基本一致。
测试结果如下:d33=27pC/N,TC=674℃,500℃时电阻率ρ=1.91×107Ω·cm。
以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求的保护范围内。
对所公开的实施例的上述说明,使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的,本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下,在其它实施例中实现。因此,本发明将不会被限制于本文所示的这些实施例,而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (9)
1.一种Ti位Cu/Ta共掺杂钛酸铋高温压电陶瓷材料的制备方法,包括配料、一次球磨、烘干、压片预烧、二次球磨、烘干、造粒成型、排胶、烧结、涂电极、极化,其特征在于,步骤如下:
配料:以Bi2O3粉体、TiO2粉体、CuO粉体和Ta2O5粉体为原料,按通式Bi4Ti3-x(Cu1/3Ta2/3)xO12中Bi、Ti、Cu和Ta的化学计量进行配料,其中0<x≤0.03;
一次球磨:向上述混合物中加入与混合物等量的无水乙醇,持续球磨12~24小时,使粉体混合均匀形成浆料,由此可以进一步的提高钛酸铋高温压电陶瓷材料的综合性能;
烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨,得到粉料;
压片预烧:将粉料置于磨具中预压成料块,将料块预烧,预烧温度为675~750℃,保温时间2~4小时;
二次球磨:将预烧后的料块在研钵中,经碾碎研磨后得到初级粉料,向得到的初级粉料中加入与初级粉料等量的无水乙醇,持续球磨12~24小时,使粉体混合均匀形成浆料;
烘干:将上述浆料置于恒温烘箱中烘烤,去除无水乙醇,并在研钵中研磨成粉料;
造粒成型:将蒸馏水以及浓度为8%的聚乙烯醇溶液(PVA)作为粘合剂掺入粉料中,掺入的蒸馏水的质量是粉料质量的2.5%,掺入的粘合剂的质量是粉料质量的5%,在研钵中混合均匀;将混合后的粉料置于磨具中,压制成生坯;将生坯在研钵中磨碎成粉料,通过60目和120目的筛子过筛,取60目和120目筛子中间层的粉料,得到了颗粒大小合适的粉料;将粉料置于磨具中,在200MPa的压强下压制成生坯;
排胶:将生坯排胶,在650℃的温度下煅烧3小时,排除生坯中的PVA,得到瓷坯;
烧结:将瓷坯进行烧结,烧结温度为1000~1100℃,保温时间2~4小时,得到陶瓷片;
涂电极:将陶瓷片清洗、烘干、丝网印刷涂银电极、烧银,烧银温度500~600℃,保温时间1~2小时;
极化:将镀好银电极的陶瓷片置于120~160℃的硅油中,极化电压为12kV/mm~15kV/mm,极化时间为20min~40min。
2.根据权利要求1所述的Ti位Cu/Ta共掺杂钛酸铋高温压电陶瓷材料的制备方法,其特征在于,在所述一次球磨和二次球磨过程中,所述球磨时间为12小时。
3.根据权利要求1所述的Ti位Cu/Ta共掺杂钛酸铋高温压电陶瓷材料的制备方法,其特征在于,在所述预烧过程中,所述预烧温度为725℃,所述保温时间为4小时。
4.根据权利要求1所述的Ti位Cu/Ta共掺杂钛酸铋高温压电陶瓷材料的制备方法,其特征在于,在所述烧结过程中,所述烧结温度为1050℃,所述保温时间为4小时。
5.根据权利要求1所述的Ti位Cu/Ta共掺杂钛酸铋高温压电陶瓷材料的制备方法,其特征在于,x=0.01。
6.根据权利要求1所述的Ti位Cu/Ta共掺杂钛酸铋高温压电陶瓷材料的制备方法,其特征在于,x=0.015。
7.根据权利要求1所述的Ti位Cu/Ta共掺杂钛酸铋高温压电陶瓷材料的制备方法,其特征在于,x=0.02。
8.根据权利要求1所述的Ti位Cu/Ta共掺杂钛酸铋高温压电陶瓷材料的制备方法,其特征在于,x=0.025。
9.根据权利要求1所述的Ti位Cu/Ta共掺杂钛酸铋高温压电陶瓷材料的制备方法,其特征在于,x=0.03。
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