CN113004037A - 一种压电陶瓷材料的制备方法 - Google Patents

一种压电陶瓷材料的制备方法 Download PDF

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CN113004037A
CN113004037A CN201911307641.0A CN201911307641A CN113004037A CN 113004037 A CN113004037 A CN 113004037A CN 201911307641 A CN201911307641 A CN 201911307641A CN 113004037 A CN113004037 A CN 113004037A
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田德辉
王宝
朱军吉
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Wuxi Huifeng Piezoeletric Co ltd
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Abstract

本发明提供一种压电陶瓷材料的制备方法,包括以下步骤:(1)配料;(2)混料;(3)压滤;(4)烘干压块;(5)预烧;(6)二次球磨;(7)喷雾造粒;(8)成型;(9)排塑;(10)烧结。通过本发明,以解决现有技术存在的压电陶瓷材料居里温度低、温度系数差导致的压电陶瓷材料使用寿命短的问题。

Description

一种压电陶瓷材料的制备方法
技术领域
本发明涉及压电材料技术领域,具体地说涉及一种压电陶瓷材料的制备方法。
背景技术
现如今,利用压电材料构成的压电器件广泛用于电子学的各个领域。压电陶瓷作为重要的功能材料不仅在电子材料工业领域占据相当大的比重,而且遍及日常生活。压电陶瓷材料被广泛应用于医学成像、声传感器、声换能器、超声马达、定位传感器等领域。
发明内容
本发明提供一种压电陶瓷材料的制备方法,以解决现有技术存在的压电陶瓷材料居里温度低、温度系数差导致的压电陶瓷材料使用寿命短的问题。
为解决上述技术问题,本发明提供一种压电陶瓷材料的制备方法,包括以下步骤:
(1)配料:按如下重量百分比的原料选料配比:四氧化三铅62~70%、二氧化锆12~15%、二氧化钛12~18%、稀土4~8%;
(2)混料:使用球磨机将加入去离子水的各种原材料磨成粒径为1~3um的浆料;
(3)压滤:将上述浆料用压滤机过滤脱水;
(4)烘干压块:将过滤脱水的浆料烘干,并使用压块机预压成块状的料块;
(5)预烧:将料块进行预烧,预烧温度为801~900℃,预烧时间为3~5h;
(6)二次球磨:使用球磨机将加入去离子水的预烧后料块磨成粒径为1~3um的料浆,使用砂磨机将所得料浆磨成粒径为0.6~1um的浆料;
(7)喷雾造粒:在二次球磨获取的浆料中加入粘合剂并配以搅拌,控制进入喷雾塔内的浆料温度,进行喷雾造粒;
(8)成型:将喷雾造粒获得的粉体使用模压工艺成形;
(9)排塑:将成型后的材料加热至600~800℃,并保持10-30min;
(10)烧结:将排塑处理后的成型材料送至烧结炉中烧结,烧结温度为900~1200℃,烧结时间为2~4h。
优选地,所述混料步骤中,所述去离子水的重量为原材料重量的50~70%。
优选地,所述二次球磨步骤中,所述去离子水的重量为原材料重量的50~70%。
优选地,所述喷雾造粒步骤中,加入的粘合剂的重量为原料量重量的7%、进口温度控制在250~299℃、出口温度控制在100℃~120℃。
优选地,所述喷雾造粒步骤中,加入的粘合剂的配方为:聚乙烯醇15%、甘油7%、酒精3%、蒸馏水75%。
本发明带来的有益效果:与现有技术相比,本发明的压电陶瓷材料具有较高的居里温度,并且温度系数良好,具有良好的稳定性和机械强度,能够显著提高压电陶瓷材料的使用寿命。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,对本发明作进一步地详细说明。
实施例1
将四氧化三铅粉体62克、二氧化锆粉体15克、二氧化钛粉体18克、稀土粉体5克混合在一起,在混合粉体中加入50克去离子水,使用球磨机将其磨成粒径为1um的浆料。使用压滤机将浆料过滤脱水,将过滤脱水的浆料烘干,并使用压块机预压成块状的料块。将料块进行预烧,预烧温度为900℃,预烧3h后,在预烧料块中加入50克去离子水,使用球磨机将预烧后料块磨成粒径为1um的料浆,使用砂磨机将所得料浆磨成粒径为0.6um的浆料。
在粒径为0.6um的浆料中加入粘合剂7克并配以搅拌。按重量百分比计,所述粘合剂的组成如下:聚乙烯醇15%、甘油7%、酒精3%、蒸馏水75%。控制进入喷雾塔内的浆料温度,进行喷雾造粒。进口温度控制在250℃、出口温度控制在100℃。将喷雾造粒获得的粉体使用模压工艺成形,将成型后的材料加热至800℃,并保持30min,将排塑处理后的成型材料送至烧结炉中烧结,烧结温度为900℃,烧结时间为2h。
实施例2
将四氧化三铅粉体70克、二氧化锆粉体12克、二氧化钛粉体12克、稀土粉体6克混合在一起,在混合粉体中加入70克去离子水,使用球磨机将其磨成粒径为3um的浆料。使用压滤机将浆料过滤脱水,将过滤脱水的浆料烘干,并使用压块机预压成块状的料块。将料块进行预烧,预烧温度为801℃,预烧5h后,在预烧料块中加入70克去离子水,使用球磨机将预烧后料块磨成粒径为3um的料浆,使用砂磨机将所得料浆磨成粒径为1um的浆料。
在粒径为1um的浆料中加入粘合剂7克并配以搅拌。按重量百分比计,所述粘合剂的组成如下:聚乙烯醇15%、甘油7%、酒精3%、蒸馏水75%。控制进入喷雾塔内的浆料温度,进行喷雾造粒。进口温度控制在299℃、出口温度控制在120℃。将喷雾造粒获得的粉体使用模压工艺成形,将成型后的材料加热至600℃,并保持10min,将排塑处理后的成型材料送至烧结炉中烧结,烧结温度为1200℃,烧结时间为4h。
实施例3
将四氧化三铅粉体66克、二氧化锆粉体15克、二氧化钛粉体15克、稀土粉体4克混合在一起,在混合粉体中加入55克去离子水,使用球磨机将其磨成粒径为2um的浆料。使用压滤机将浆料过滤脱水,将过滤脱水的浆料烘干,并使用压块机预压成块状的料块。将料块进行预烧,预烧温度为850℃,预烧4h后,在预烧料块中加入60克去离子水,使用球磨机将预烧后料块磨成粒径为2um的料浆,使用砂磨机将所得料浆磨成粒径为0.8um的浆料。
在粒径为0.8um的浆料中加入粘合剂7克并配以搅拌。按重量百分比计,所述粘合剂的组成如下:聚乙烯醇15%、甘油7%、酒精3%、蒸馏水75%。控制进入喷雾塔内的浆料温度,进行喷雾造粒。进口温度控制在270℃、出口温度控制在110℃。将喷雾造粒获得的粉体使用模压工艺成形,将成型后的材料加热至700℃,并保持20min,将排塑处理后的成型材料送至烧结炉中烧结,烧结温度为1100℃,烧结时间为3h。
实施例4
将四氧化三铅粉体64克、二氧化锆粉体13克、二氧化钛粉体15克、稀土粉体8克混合在一起,在混合粉体中加入60克去离子水,使用球磨机将其磨成粒径为2um的浆料。使用压滤机将浆料过滤脱水,将过滤脱水的浆料烘干,并使用压块机预压成块状的料块。将料块进行预烧,预烧温度为850℃,预烧4h后,在预烧料块中加入55克去离子水,使用球磨机将预烧后料块磨成粒径为2um的料浆,使用砂磨机将所得料浆磨成粒径为0.8um的浆料。
在粒径为0.8um的浆料中加入粘合剂7克并配以搅拌。按重量百分比计,所述粘合剂的组成如下:聚乙烯醇15%、甘油7%、酒精3%、蒸馏水75%。控制进入喷雾塔内的浆料温度,进行喷雾造粒。进口温度控制在280℃、出口温度控制在110℃。将喷雾造粒获得的粉体使用模压工艺成形,将成型后的材料加热至700℃,并保持20min,将排塑处理后的成型材料送至烧结炉中烧结,烧结温度为1000℃,烧结时间为3h。
本发明的压电陶瓷材料居里温度达370~430℃,电容温度稳定性控制在0.2~0.4%K-1/Tmax,0.2~0.4%K-1/Tmin,有效机电耦合系数稳定性控制在-0.1~0.025K-1/Tmax,-0.35~0.10K-1/Tmax。
综上所述,本发明的压电陶瓷材料具有较高的居里温度,并且温度系数良好,具有良好的稳定性和机械强度,能够显著提高压电陶瓷材料的使用寿命。
以上所述仅为本发明的实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的权利要求范围之内。

Claims (5)

1.一种压电陶瓷材料的制备方法,其特征在于:包括以下步骤:
(1)配料:按如下重量百分比的原料选料配比:四氧化三铅62~70%、二氧化锆12~15%、二氧化钛12~18%、稀土4~8%;
(2)混料:使用球磨机将加入去离子水的各种原材料磨成粒径为1~3um的浆料;
(3)压滤:将上述浆料用压滤机过滤脱水;
(4)烘干压块:将过滤脱水的浆料烘干,并使用压块机预压成块状的料块;
(5)预烧:将料块进行预烧,预烧温度为801~900℃,预烧时间为3~5h;
(6)二次球磨:使用球磨机将加入去离子水的预烧后料块磨成粒径为1~3um的料浆,使用砂磨机将所得料浆磨成粒径为0.6~1um的浆料;
(7)喷雾造粒:在二次球磨获取的浆料中加入粘合剂并配以搅拌,控制进入喷雾塔内的浆料温度,进行喷雾造粒;
(8)成型:将喷雾造粒获得的粉体使用模压工艺成形;
(9)排塑:将成型后的材料加热至600~800℃,并保持10-30min;
(10)烧结:将排塑处理后的成型材料送至烧结炉中烧结,烧结温度为900~1200℃,烧结时间为2~4h。
2.如权利要求1所述的压电陶瓷材料的制备方法,其特征在于,所述混料步骤中,所述去离子水的重量为原材料重量的50~70%。
3.如权利要求1所述的压电陶瓷材料的制备方法,其特征在于,所述二次球磨步骤中,所述去离子水的重量为原材料重量的50~70%。
4.如权利要求1所述的压电陶瓷材料的制备方法,其特征在于,所述喷雾造粒步骤中,加入的粘合剂的重量为原料量重量的7%、进口温度控制在250~299℃、出口温度控制在100℃~120℃。
5.如权利要求4所述的压电陶瓷材料的制备方法,其特征在于,所述喷雾造粒步骤中,加入的粘合剂的配方为:聚乙烯醇15%、甘油7%、酒精3%、蒸馏水75%。
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