CN108275983A - 一种无铅压电陶瓷材料的制备方法及其应用 - Google Patents
一种无铅压电陶瓷材料的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种无铅压电陶瓷材料的制备方法及其应用,该方法采用将氧化铝、三氧化二硼、钛酸钡、碳酸钾、氧化钴球磨后预烧制,将预烧料再次球磨成粉后加入聚乙二醇、正硅酸乙酯、硅锆酸钠、磷脂酰丝氨酸进行热反应,再经冷却、陈化、干燥成浆料后置于惰性气体氛围中加入无水乙醇、色粉保温、排塑得到排塑坯料,最后将排塑坯料加入粘结剂压制成型、烧结,冷却后得到成品无铅压电陶瓷材料。制备而成的无铅压电陶瓷材料,其力学性能好、机械品质高,在电子元件制造中具有良好的应用前景。
Description
技术领域
本发明涉及电子材料技术领域,具体涉及一种无铅压电陶瓷材料的制备方法及其应用。
背景技术
压电材料是指一类具有压电效应的功能材料,利用压电材料的正逆压电效应,可用于制备水声换能器、超声换能器、电声器件、滤波器、传感器、微位移驱动器等,在能源、医疗等领域得到广泛应用。
其中,压电陶瓷是一类具有压电特性的电子陶瓷材料。与典型的不包含铁电成分的压电石英晶体的主要区别是:构成其主要成分的晶相都是具有铁电性的晶粒。由于陶瓷是晶粒随机取向的多晶聚集体,因此其中各个铁电晶粒的自发极化矢量也是混乱取向的。为了使陶瓷能表现出宏观的压电特性,就必须在压电陶瓷烧成并于端面被复电极之后,将其置于强直流电场下进行极化处理,以使原来混乱取向的各自发极化矢量沿电场方向择优取向。经过极化处理后的压电陶瓷,在电场取消之后,会保留一定的宏观剩余极化强度,从而使陶瓷具有了一定的压电性质。
压电陶瓷除具有压电性外,还具有介电性、弹性等,已被广泛应用于医学成像、声传感器、声换能器、超声马达等。压电陶瓷利用其材料在机械应力作用下,引起内部正负电荷中心相对位移而发生极化,导致材料两端表面出现符号相反的束缚电荷即压电效应而制作,具有敏感的特性,压电陶瓷主要用于制造超声换能器、水声换能器、电声换能器、陶瓷滤波器、陶瓷变压器、陶瓷鉴频器、高压发生器、红外探测器、声表面波器件、电光器件、引燃引爆装置和压电陀螺等。
随着人们对生态环境的越来越重视以及电子器件的高速发展,对无铅压电陶瓷的需求越来越旺盛。然而,目前压电陶瓷普遍使用的是锆钛酸铅、铌锑酸铅等铅基材料制备而成,其中铅的含量高达70%,且铅在高温下易挥发,给人体身体健康和环境造成了严重危害。
发明内容
为解决上述技术问题,本发明提供一种无铅压电陶瓷材料的制备方法及其应用,该方法采用将氧化铝、三氧化二硼、钛酸钡、碳酸钾、氧化钴球磨后预烧制,将预烧料再次球磨成粉后加入聚乙二醇、正硅酸乙酯、硅锆酸钠、磷脂酰丝氨酸进行热反应,再经冷却、陈化、干燥成浆料后置于惰性气体氛围中加入无水乙醇、色粉保温、排塑得到排塑坯料,最后将排塑坯料加入粘结剂压制成型、烧结,冷却后得到成品无铅压电陶瓷材料。制备而成的无铅压电陶瓷材料,其力学性能好、机械品质高,在电子元件制造中具有良好的应用前景。
本发明的目的可以通过以下技术方案实现:
一种无铅压电陶瓷材料的制备方法,包括以下步骤:
(1)将氧化铝20-30份、三氧化二硼12-16份、钛酸钡8-10份、碳酸钾6-8份、氧化钴2-4份放入球磨机中混合均匀,经球磨处理得到均一的粉末;
(2)将步骤(1)经球磨处理后得到的粉末置于马弗炉中,调整马弗炉的温度至1200-1300℃,预烧制18-20小时;
(3)将步骤(2)经烧制得到的预烧料采用破碎机破碎,再次置于球磨机中,以无水乙醇为介质,经球磨处理得到均一的粉末;
(4)向将步骤(3)得到的粉末中加入其5倍质量的聚乙二醇,再加入正硅酸乙酯8-12份、硅锆酸钠7-9份、磷脂酰丝氨酸4-6份,边搅拌边加热至130℃,在该温度下维持20-40分钟,得到热反应产物;
(5)将步骤(4)得到的热反应产物冷却至室温,静置陈化24小时,随后置于干燥箱中于60℃下干燥至热反应产物形成粘稠的浆料;
(6)将步骤(5)的粘稠浆料置于惰性气体氛围中,加入无水乙醇5-9份、色粉3-5份,升温至600℃,保温2小时得到坯料,随后将得到的坯料放入马弗炉中加热排塑,排塑温度为750-800℃,排塑时间为2-3小时;
(7)将步骤(6)得到的排塑坯料加入粘结剂压制成型,压力为120MPa,在1400-1500℃中烧结3-5小时,随炉冷却,获得无铅压电陶瓷材料。
进一步的,所述步骤(1)中球磨机的转速为280-320转/分钟,球磨时间为2-4小时,处理后的粉末粒径为200-300nm。
进一步的,所述步骤(3)中球磨机的转速为350-380转/分钟,球磨时间为3-5小时,处理后的粉末粒径为80-100nm。
进一步的,所述步骤(6)中的惰性气体选自氮气、氦气、氩气中的任意一种。
进一步的,所述步骤(7)中的粘结剂优选为质量比为3:3:2的聚乙烯醇缩丁醛、甲基纤维素和硅酸钠的混合物。
进一步的,本发明还公开了所述制备方法制得的无铅压电陶瓷材料在电子元件制造中的应用。
本发明与现有技术相比,其有益效果为:
(1)本发明的无铅压电陶瓷材料的制备方法采用将氧化铝、三氧化二硼、钛酸钡、碳酸钾、氧化钴球磨后预烧制,将预烧料再次球磨成粉后加入聚乙二醇、正硅酸乙酯、硅锆酸钠、磷脂酰丝氨酸进行热反应,再经冷却、陈化、干燥成浆料后置于惰性气体氛围中加入无水乙醇、色粉保温、排塑得到排塑坯料,最后将排塑坯料加入粘结剂压制成型、烧结,冷却后得到成品无铅压电陶瓷材料。制备而成的无铅压电陶瓷材料,其力学性能好、机械品质高,在电子元件制造中具有良好的应用前景。
(2)本发明采用了氧化钴、正硅酸乙酯、硅锆酸钠、磷脂酰丝氨酸这几种原料参与制备无铅压电陶瓷材料,对无铅压电陶瓷材料进行了有效的性能提升,虽然这些材料并非首次应用于无铅压电陶瓷材料中,但按照一定配比量组合后,辅以相应的处理方式,给最后制备得到的无铅压电陶瓷材料带来了使用性能上的大幅度提高,这在以往的研究中是不曾报道过的,对于实现本发明的技术效果起到了决定性的作用。
具体实施方式
下面结合具体实施例对发明的技术方案进行详细说明。
实施例1
(1)将氧化铝20份、三氧化二硼12份、钛酸钡8份、碳酸钾6份、氧化钴2份放入球磨机中混合均匀,调整球磨机的转速为280转/分钟,球磨时间为2小时,经球磨处理得到均一的粉末,处理后的粉末粒径为200nm;
(2)将步骤(1)经球磨处理后得到的粉末置于马弗炉中,调整马弗炉的温度至1200℃,预烧制18小时;
(3)将步骤(2)经烧制得到的预烧料采用破碎机破碎,再次置于球磨机中,以无水乙醇为介质,调整球磨机的转速为350转/分钟,球磨时间为3小时,经球磨处理得到均一的粉末,处理后的粉末粒径为80nm;
(4)向将步骤(3)得到的粉末中加入其5倍质量的聚乙二醇,再加入正硅酸乙酯8份、硅锆酸钠7份、磷脂酰丝氨酸4份,边搅拌边加热至130℃,在该温度下维持20分钟,得到热反应产物;
(5)将步骤(4)得到的热反应产物冷却至室温,静置陈化24小时,随后置于干燥箱中于60℃下干燥至热反应产物形成粘稠的浆料;
(6)将步骤(5)的粘稠浆料置于氮气气体氛围中,加入无水乙醇5份、色粉3份,升温至600℃,保温2小时得到坯料,随后将得到的坯料放入马弗炉中加热排塑,排塑温度为750℃,排塑时间为2小时;
(7)将步骤(6)得到的排塑坯料加入粘结剂压制成型,粘结剂为质量比为3:3:2的聚乙烯醇缩丁醛、甲基纤维素和硅酸钠的混合物,压力为120MPa,在1400℃中烧结3小时,随炉冷却,获得无铅压电陶瓷材料。
制得的无铅压电陶瓷材料的性能测试结果如表1所示。
实施例2
(1)将氧化铝25份、三氧化二硼14份、钛酸钡9份、碳酸钾7份、氧化钴3份放入球磨机中混合均匀,调整球磨机的转速为300转/分钟,球磨时间为3小时,经球磨处理得到均一的粉末,处理后的粉末粒径为250nm;
(2)将步骤(1)经球磨处理后得到的粉末置于马弗炉中,调整马弗炉的温度至1250℃,预烧制19小时;
(3)将步骤(2)经烧制得到的预烧料采用破碎机破碎,再次置于球磨机中,以无水乙醇为介质,调整球磨机的转速为365转/分钟,球磨时间为4小时,经球磨处理得到均一的粉末,处理后的粉末粒径为90nm;
(4)向将步骤(3)得到的粉末中加入其5倍质量的聚乙二醇,再加入正硅酸乙酯10份、硅锆酸钠8份、磷脂酰丝氨酸5份,边搅拌边加热至130℃,在该温度下维持30分钟,得到热反应产物;
(5)将步骤(4)得到的热反应产物冷却至室温,静置陈化24小时,随后置于干燥箱中于60℃下干燥至热反应产物形成粘稠的浆料;
(6)将步骤(5)的粘稠浆料置于氦气气体氛围中,加入无水乙醇7份、色粉4份,升温至600℃,保温2小时得到坯料,随后将得到的坯料放入马弗炉中加热排塑,排塑温度为775℃,排塑时间为2.5小时;
(7)将步骤(6)得到的排塑坯料加入粘结剂压制成型,粘结剂为质量比为3:3:2的聚乙烯醇缩丁醛、甲基纤维素和硅酸钠的混合物,压力为120MPa,在1450℃中烧结4小时,随炉冷却,获得无铅压电陶瓷材料。
制得的无铅压电陶瓷材料的性能测试结果如表1所示。
实施例3
(1)将氧化铝30份、三氧化二硼16份、钛酸钡10份、碳酸钾8份、氧化钴4份放入球磨机中混合均匀,调整球磨机的转速为320转/分钟,球磨时间为4小时,经球磨处理得到均一的粉末,处理后的粉末粒径为300nm;
(2)将步骤(1)经球磨处理后得到的粉末置于马弗炉中,调整马弗炉的温度至1300℃,预烧制20小时;
(3)将步骤(2)经烧制得到的预烧料采用破碎机破碎,再次置于球磨机中,以无水乙醇为介质,调整球磨机的转速为380转/分钟,球磨时间为5小时,经球磨处理得到均一的粉末,处理后的粉末粒径为100nm;
(4)向将步骤(3)得到的粉末中加入其5倍质量的聚乙二醇,再加入正硅酸乙酯12份、硅锆酸钠9份、磷脂酰丝氨酸6份,边搅拌边加热至130℃,在该温度下维持40分钟,得到热反应产物;
(5)将步骤(4)得到的热反应产物冷却至室温,静置陈化24小时,随后置于干燥箱中于60℃下干燥至热反应产物形成粘稠的浆料;
(6)将步骤(5)的粘稠浆料置于氩气气体氛围中,加入无水乙醇9份、色粉5份,升温至600℃,保温2小时得到坯料,随后将得到的坯料放入马弗炉中加热排塑,排塑温度为800℃,排塑时间为3小时;
(7)将步骤(6)得到的排塑坯料加入粘结剂压制成型,粘结剂为质量比为3:3:2的聚乙烯醇缩丁醛、甲基纤维素和硅酸钠的混合物,压力为120MPa,在1500℃中烧结5小时,随炉冷却,获得无铅压电陶瓷材料。
制得的无铅压电陶瓷材料的性能测试结果如表1所示。
对比例1
(1)将氧化铝25份、三氧化二硼14份、钛酸钡9份、碳酸钾7份放入球磨机中混合均匀,调整球磨机的转速为300转/分钟,球磨时间为3小时,经球磨处理得到均一的粉末,处理后的粉末粒径为250nm;
(2)将步骤(1)经球磨处理后得到的粉末置于马弗炉中,调整马弗炉的温度至1250℃,预烧制19小时;
(3)将步骤(2)经烧制得到的预烧料采用破碎机破碎,再次置于球磨机中,以无水乙醇为介质,调整球磨机的转速为365转/分钟,球磨时间为4小时,经球磨处理得到均一的粉末,处理后的粉末粒径为90nm;
(4)向将步骤(3)得到的粉末中加入其5倍质量的聚乙二醇,再加入正硅酸乙酯10份、硅锆酸钠8份、磷脂酰丝氨酸5份,边搅拌边加热至130℃,在该温度下维持30分钟,得到热反应产物;
(5)将步骤(4)得到的热反应产物冷却至室温,静置陈化24小时,随后置于干燥箱中于60℃下干燥至热反应产物形成粘稠的浆料;
(6)将步骤(5)的粘稠浆料置于氦气气体氛围中,加入无水乙醇7份、色粉4份,升温至600℃,保温2小时得到坯料,随后将得到的坯料放入马弗炉中加热排塑,排塑温度为775℃,排塑时间为2.5小时;
(7)将步骤(6)得到的排塑坯料加入粘结剂压制成型,粘结剂为质量比为3:3:2的聚乙烯醇缩丁醛、甲基纤维素和硅酸钠的混合物,压力为120MPa,在1450℃中烧结4小时,随炉冷却,获得无铅压电陶瓷材料。
制得的无铅压电陶瓷材料的性能测试结果如表1所示。
对比例2
(1)将氧化铝25份、三氧化二硼14份、钛酸钡9份、碳酸钾7份、氧化钴3份放入球磨机中混合均匀,调整球磨机的转速为300转/分钟,球磨时间为3小时,经球磨处理得到均一的粉末,处理后的粉末粒径为250nm;
(2)将步骤(1)经球磨处理后得到的粉末置于马弗炉中,调整马弗炉的温度至1250℃,预烧制19小时;
(3)将步骤(2)经烧制得到的预烧料采用破碎机破碎,再次置于球磨机中,以无水乙醇为介质,调整球磨机的转速为365转/分钟,球磨时间为4小时,经球磨处理得到均一的粉末,处理后的粉末粒径为90nm;
(4)向将步骤(3)得到的粉末中加入其5倍质量的聚乙二醇,再加入硅锆酸钠8份、磷脂酰丝氨酸5份,边搅拌边加热至130℃,在该温度下维持30分钟,得到热反应产物;
(5)将步骤(4)得到的热反应产物冷却至室温,静置陈化24小时,随后置于干燥箱中于60℃下干燥至热反应产物形成粘稠的浆料;
(6)将步骤(5)的粘稠浆料置于氦气气体氛围中,加入无水乙醇7份、色粉4份,升温至600℃,保温2小时得到坯料,随后将得到的坯料放入马弗炉中加热排塑,排塑温度为775℃,排塑时间为2.5小时;
(7)将步骤(6)得到的排塑坯料加入粘结剂压制成型,粘结剂为质量比为3:3:2的聚乙烯醇缩丁醛、甲基纤维素和硅酸钠的混合物,压力为120MPa,在1450℃中烧结4小时,随炉冷却,获得无铅压电陶瓷材料。
制得的无铅压电陶瓷材料的性能测试结果如表1所示。
对比例3
(1)将氧化铝25份、三氧化二硼14份、钛酸钡9份、碳酸钾7份、氧化钴3份放入球磨机中混合均匀,调整球磨机的转速为300转/分钟,球磨时间为3小时,经球磨处理得到均一的粉末,处理后的粉末粒径为250nm;
(2)将步骤(1)经球磨处理后得到的粉末置于马弗炉中,调整马弗炉的温度至1250℃,预烧制19小时;
(3)将步骤(2)经烧制得到的预烧料采用破碎机破碎,再次置于球磨机中,以无水乙醇为介质,调整球磨机的转速为365转/分钟,球磨时间为4小时,经球磨处理得到均一的粉末,处理后的粉末粒径为90nm;
(4)向将步骤(3)得到的粉末中加入其5倍质量的聚乙二醇,再加入正硅酸乙酯10份、磷脂酰丝氨酸5份,边搅拌边加热至130℃,在该温度下维持30分钟,得到热反应产物;
(5)将步骤(4)得到的热反应产物冷却至室温,静置陈化24小时,随后置于干燥箱中于60℃下干燥至热反应产物形成粘稠的浆料;
(6)将步骤(5)的粘稠浆料置于氦气气体氛围中,加入无水乙醇7份、色粉4份,升温至600℃,保温2小时得到坯料,随后将得到的坯料放入马弗炉中加热排塑,排塑温度为775℃,排塑时间为2.5小时;
(7)将步骤(6)得到的排塑坯料加入粘结剂压制成型,粘结剂为质量比为3:3:2的聚乙烯醇缩丁醛、甲基纤维素和硅酸钠的混合物,压力为120MPa,在1450℃中烧结4小时,随炉冷却,获得无铅压电陶瓷材料。
制得的无铅压电陶瓷材料的性能测试结果如表1所示。
对比例4
(1)将氧化铝25份、三氧化二硼14份、钛酸钡9份、碳酸钾7份、氧化钴3份放入球磨机中混合均匀,调整球磨机的转速为300转/分钟,球磨时间为3小时,经球磨处理得到均一的粉末,处理后的粉末粒径为250nm;
(2)将步骤(1)经球磨处理后得到的粉末置于马弗炉中,调整马弗炉的温度至1250℃,预烧制19小时;
(3)将步骤(2)经烧制得到的预烧料采用破碎机破碎,再次置于球磨机中,以无水乙醇为介质,调整球磨机的转速为365转/分钟,球磨时间为4小时,经球磨处理得到均一的粉末,处理后的粉末粒径为90nm;
(4)向将步骤(3)得到的粉末中加入其5倍质量的聚乙二醇,再加入正硅酸乙酯10份、硅锆酸钠8份,边搅拌边加热至130℃,在该温度下维持30分钟,得到热反应产物;
(5)将步骤(4)得到的热反应产物冷却至室温,静置陈化24小时,随后置于干燥箱中于60℃下干燥至热反应产物形成粘稠的浆料;
(6)将步骤(5)的粘稠浆料置于氦气气体氛围中,加入无水乙醇7份、色粉4份,升温至600℃,保温2小时得到坯料,随后将得到的坯料放入马弗炉中加热排塑,排塑温度为775℃,排塑时间为2.5小时;
(7)将步骤(6)得到的排塑坯料加入粘结剂压制成型,粘结剂为质量比为3:3:2的聚乙烯醇缩丁醛、甲基纤维素和硅酸钠的混合物,压力为120MPa,在1450℃中烧结4小时,随炉冷却,获得无铅压电陶瓷材料。
制得的无铅压电陶瓷材料的性能测试结果如表1所示。
将实施例1-3和对比例1-4的制得的无铅压电陶瓷材料分别按照国家或行业标准中的测试方法进行拉伸强度、弯曲强度、机械品质因数这几项性能测试。
表1
本发明的无铅压电陶瓷材料的制备方法采用将氧化铝、三氧化二硼、钛酸钡、碳酸钾、氧化钴球磨后预烧制,将预烧料再次球磨成粉后加入聚乙二醇、正硅酸乙酯、硅锆酸钠、磷脂酰丝氨酸进行热反应,再经冷却、陈化、干燥成浆料后置于惰性气体氛围中加入无水乙醇、色粉保温、排塑得到排塑坯料,最后将排塑坯料加入粘结剂压制成型、烧结,冷却后得到成品无铅压电陶瓷材料。制备而成的无铅压电陶瓷材料,其力学性能好、机械品质高,在电子元件制造中具有良好的应用前景。并且,本发明采用了氧化钴、正硅酸乙酯、硅锆酸钠、磷脂酰丝氨酸这几种原料参与制备无铅压电陶瓷材料,对无铅压电陶瓷材料进行了有效的性能提升,虽然这些材料并非首次应用于无铅压电陶瓷材料中,但按照一定配比量组合后,辅以相应的处理方式,给最后制备得到的无铅压电陶瓷材料带来了使用性能上的大幅度提高,这在以往的研究中是不曾报道过的,对于实现本发明的技术效果起到了决定性的作用。
以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书内容所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围内。
Claims (6)
1.一种无铅压电陶瓷材料的制备方法,其特征在于,包括以下步骤:
(1)将氧化铝20-30份、三氧化二硼12-16份、钛酸钡8-10份、碳酸钾6-8份、氧化钴2-4份放入球磨机中混合均匀,经球磨处理得到均一的粉末;
(2)将步骤(1)经球磨处理后得到的粉末置于马弗炉中,调整马弗炉的温度至1200-1300℃,预烧制18-20小时;
(3)将步骤(2)经烧制得到的预烧料采用破碎机破碎,再次置于球磨机中,以无水乙醇为介质,经球磨处理得到均一的粉末;
(4)向将步骤(3)得到的粉末中加入其5倍质量的聚乙二醇,再加入正硅酸乙酯8-12份、硅锆酸钠7-9份、磷脂酰丝氨酸4-6份,边搅拌边加热至130℃,在该温度下维持20-40分钟,得到热反应产物;
(5)将步骤(4)得到的热反应产物冷却至室温,静置陈化24小时,随后置于干燥箱中于60℃下干燥至热反应产物形成粘稠的浆料;
(6)将步骤(5)的粘稠浆料置于惰性气体氛围中,加入无水乙醇5-9份、色粉3-5份,升温至600℃,保温2小时得到坯料,随后将得到的坯料放入马弗炉中加热排塑,排塑温度为750-800℃,排塑时间为2-3小时;
(7)将步骤(6)得到的排塑坯料加入粘结剂压制成型,压力为120MPa,在1400-1500℃中烧结3-5小时,随炉冷却,获得无铅压电陶瓷材料。
2.根据权利要求1所述的无铅压电陶瓷材料的制备方法,其特征在于,所述步骤(1)中球磨机的转速为280-320转/分钟,球磨时间为2-4小时,处理后的粉末粒径为200-300nm。
3.根据权利要求1所述的无铅压电陶瓷材料的制备方法,其特征在于,所述步骤(3)中球磨机的转速为350-380转/分钟,球磨时间为3-5小时,处理后的粉末粒径为80-100nm。
4.根据权利要求1所述的无铅压电陶瓷材料的制备方法,其特征在于,所述步骤(6)中的惰性气体选自氮气、氦气、氩气中的任意一种。
5.根据权利要求1所述的无铅压电陶瓷材料的制备方法,其特征在于,所述步骤(7)中的粘结剂优选为质量比为3:3:2的聚乙烯醇缩丁醛、甲基纤维素和硅酸钠的混合物。
6.根据权利要求1-5任一项所述制备方法制得的无铅压电陶瓷材料在电子元件制造中的应用。
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