CN105541321B - 一种高介电常数p‑52压电陶瓷材料及其制作方法 - Google Patents

一种高介电常数p‑52压电陶瓷材料及其制作方法 Download PDF

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CN105541321B
CN105541321B CN201610075665.8A CN201610075665A CN105541321B CN 105541321 B CN105541321 B CN 105541321B CN 201610075665 A CN201610075665 A CN 201610075665A CN 105541321 B CN105541321 B CN 105541321B
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王新平
李丹
刘天阳
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ZHONGCHUAN HEAVY INDUSTRY HAISHENG SCIENCE-TECHNOLOGY Co Ltd
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Abstract

本发明属于水声接收产品领域,特别涉及一种高介电常数P‑52压电陶瓷材料及其制作方法。高介电常数P‑52压电陶瓷材料包括按重量份计以下原料制成:红丹粉45~65份,钛白粉6~15份,氧化钴15~25份,氧化镧0.3~1.2份,氧化铌0.2~1.2份,氧化铝0.8~1.8份。制作所述的材料包括配料、混料、干燥,压坯、合成,细化,脱水,增塑造粒、成型、排塑,烧结,机械加工、清洗、烘干,高温氧化等步骤。本发明制作的产品样品经过性能测试,介电常数高达3300~4500,压电系数为612×10‑12~810×10‑12c/N,该工艺制备的P‑52材料完全满足水声换能器的性能及使用要求。

Description

一种高介电常数P-52压电陶瓷材料及其制作方法
技术领域
本发明涉及水声接收产品领域,特别涉及一种高介电常数P-52压电陶瓷材料及其制作方法。
背景技术
中国船舶工业总公司部标准 CB 1125-98《水声用压电陶瓷材料规范》所要求的P-52压电陶瓷材料介电常数为3250±12.5%、压电系数为575×10-12c/N±12.5%,随着现代科学技术的不断发展,需要进一步提高P-52压电陶瓷的介电常数、压电系数,以满足灵敏度要求高、抗干扰能力强的水声换能器应用需求,缩小我国在军品开发上与发达国家的差距,并为相关院校、院所的科研提供新的技术支持和应用领域。
发明内容
本发明的主要目的在于提供一种高介电常数P-52压电陶瓷材料及其制作方法,使该材料性能达到一定的技术指标,满足水声换能器产品应用。
本发明的技术方案如下:
一种高介电常数P-52压电陶瓷材料,所述材料包括按重量份计以下原料制成:
红丹粉45~65份,钛白粉6~15份,氧化钴15~25份,氧化镧0.3~1.2份,氧化铌0.2~1.2份,氧化铝0.8~1.8份。
所述材料包括按重量份计以下原料制成:
红丹粉50~60份,钛白粉8~10份,氧化钴18~20份,氧化镧0.5~0.8份,氧化铌0.4~0.7份,氧化铝1~1.5份。
所述材料介电常数为3300~4500,压电系数为612×10-12~810×10-12c/N。
制作所述的材料,所述方法包括以下步骤:
1)配料、混料、干燥:按配方量称取原料,混合,干燥得到物料1;
2)压坯、合成:将物料1放入坩埚中压实,合成,得到物料2;
3)细化:将物料2球磨得到物料3;
4)脱水:将物料3进行干燥,得到物料4;
5)增塑造粒、成型、排塑:将物料4中加入增塑剂后造粒,烘干、压片、排塑,得到物料5;
6)烧结:将物料5置于马弗炉中烧结得到物料6;
7)机械加工、清洗、烘干:将物料6机械加工到所需的尺寸,并超声波清洗、烘干,得到物料7;
8)高温氧化:将物料7置于马福炉中,进行高温氧化,得到物料8;
9)上电极、烧渗、极化:将物料8进行上电极、烧渗、硅油中极化;
完成高介电常数P-52压电陶瓷材料的制作。
所述步骤2)合成温度为800-900℃,合成时间为0.5~1 h,
所述步骤3)细化过程中物料2中加入50%~70%的水进行球磨。
所述步骤3)物料3粒径<2μm。
所述步骤5)物料4中加入的增塑剂为聚乙烯醇或邻苯二甲酸二丁酯,加入量为5%~10%。
所述步骤6)于1280~1350℃下烧结2~3 h,
所述步骤8)高温氧化条件为按100~160℃/小时的速度升温,升至温度1150~1250℃,保温110~130 min。
所述步骤8)将加工到机械尺寸要求的压电陶瓷制品放置在同种材料加工的平整垫片上,置于敞口的坩埚中,再将坩埚放置于炉门微开的高温马福炉中,升温速度升至最高温度,并保温。
所述步骤1)物料1、步骤4)物料4的含水率≤10%。
本发明提供一种高介电常数P-52压电陶瓷材料及其制作方法,有益效果如下:
1、本发明在常规压电陶瓷材料制作工艺基础上,在机械加工和上电极之前加入高温氧化工艺,大大提高了P-52压电陶瓷材料的介电常数、压电系数,
2、本发明对P-52压电陶瓷材料的制作原料进行优化,针对高介电常数P-52压电陶瓷材料的需求,挑选了适宜的原材料;
3、本发明严格控制加工过程中物料的水分和粒径大小,保证最终产品品质均匀;
4、本发明对合成工艺进行控制,使各材料的固相化学反应充分均匀,生产组成固定的固溶体,减少瓷料的烧成收缩;
5、本发明对烧成工艺进行精确控制,让锆钛酸铅等化合物的松散颗粒状态在高温条件下溶固结合成一体。并在结晶过程中,使晶粒生长均匀、致密、具有某种显微组织结构和一定机械强度的物理性能;
6、本发明制作的产品样品经过性能测试,介电常数高达3300~4500,压电系数为612×10-12~810×10-12c/N,该工艺制备的P-52材料完全满足水声换能器的性能及使用要求。
具体实施方式
下面结合实施例来进一步说明本发明,但本发明要求保护的范围并不局限于实施例表述的范围。
实施例1
一种高介电常数P-52压电陶瓷材料,所述材料包括按重量份计以下原料制成:
红丹粉45份,钛白粉6份,氧化钴15份,氧化镧0.3份,氧化铌0.2份,氧化铝0.8份。
实施例2
一种高介电常数P-52压电陶瓷材料,所述材料包括按重量份计以下原料制成:
红丹粉65份,钛白粉15份,氧化钴25份,氧化镧1.2份,氧化铌1.2份,氧化铝1.8份。
所述材料介电常数为4300,压电系数为810×10-12c/N。
实施例3
一种高介电常数P-52压电陶瓷材料,所述材料包括按重量份计以下原料制成:
红丹粉50份,钛白粉8份,氧化钴18份,氧化镧0.5份,氧化铌0.4份,氧化铝1份。
所述材料介电常数为3300,压电系数为612×10-12c/N。
实施例4
一种高介电常数P-52压电陶瓷材料,所述材料包括按重量份计以下原料制成:
红丹粉60份,钛白粉10份,氧化钴20份,氧化镧0.8份,氧化铌0.7份,氧化铝1.5份。
所述材料介电常数为4500,压电系数为810×10-12c/N。
实施例5
一种高介电常数P-52压电陶瓷材料,所述材料包括按重量份计以下原料制成:
红丹粉55份,钛白粉9份,氧化钴19份,氧化镧0.6份,氧化铌0.6份,氧化铝1.4份。
所述材料介电常数为4400,压电系数为790×10-12c/N。
实施例6
制作高介电常数P-52压电陶瓷材料的方法,所述方法包括以下步骤:
1)配料、混料、干燥:按配方量称取原料,混合,干燥得到物料1;
2)压坯、合成:将物料1放入坩埚中压实,合成,合成温度为800-900℃,合成时间为0.5~1 h,得到物料2;
3)细化:将物料2中加入50%~70%的水,进行球磨得到物料3,物料3粒径<2μm;
4)脱水:将物料3进行干燥,得到物料4;
5)增塑造粒、成型、排塑:将物料4中加入增塑剂后造粒,烘干、压片、排塑,得到物料5;
6)烧结:将物料5置于马弗炉中于1280~1350℃下烧结2~3 h,得到物料6;
7)机械加工、清洗、烘干:将物料6机械加工到所需的尺寸,并超声波清洗、烘干,得到物料7;
8)高温氧化:将物料7置于马福炉中,进行高温氧化,高温氧化条件为按100~160℃/小时的速度升温,升至温度1150~1250 ℃,保温110~130 min,得到物料8;
9)上电极、烧渗、极化:将物料8进行上电极、烧渗、硅油中极化;
完成高介电常数P-52压电陶瓷材料的制作。
所述步骤5)物料4中加入的增塑剂为聚乙烯醇或邻苯二甲酸二丁酯,加入量为5%~10%。
所述步骤8)将加工到机械尺寸要求的压电陶瓷制品放置在同种材料加工的平整垫片上,置于敞口的坩埚中,再将坩埚放置于炉门微开的高温马福炉中,升温速度升至最高温度,并保温。
所述步骤1)物料1、步骤4)物料4的含水率≤10%。
上述的实施例仅为本发明的优选技术方案,而不应视为对于本发明的限制,本申请中的实施例及实施例中的特征在不冲突的情况下,可以相互任意组合。本发明的保护范围应以权利要求记载的技术方案,包括权利要求记载的技术方案中技术特征的等同替换方案为保护范围。即在此范围内的等同替换改进,也在本发明的保护范围之内。

Claims (3)

1.一种高介电常数P-52压电陶瓷材料,其特征在于,所述材料的制作原料包括按重量份计的以下组分:
红丹粉45~65份,钛白粉6~15份,氧化钴15~25份,氧化镧0.3~1.2份,氧化铌0.2~1.2份,氧化铝0.8~1.8份;
制作所述的材料,所述方法包括以下步骤:
1)配料、混料、干燥:按配方量称取原料,混合,干燥,得到物料1;
2)压坯、合成:将物料1放入坩埚中压实,合成,得到物料2;
3)细化:将物料2球磨得到物料3;
4)脱水:将物料3进行干燥,得到物料4;
5)增塑造粒、成型、排塑:将物料4中加入增塑剂后造粒,烘干、压片、排塑,得到物料5;
6)烧结:将物料5置于马弗炉中烧结得到物料6;
7)机械加工、清洗、烘干:将物料6机械加工到所需的尺寸,并超声波清洗、烘干,得到物料7;
8)高温氧化:将物料7置于马福炉中,进行高温氧化,得到物料8;
9)上电极、烧渗、极化:将物料8进行上电极、烧渗、硅油中极化;
完成高介电常数P-52压电陶瓷材料的制作;
所述步骤2)合成温度为800-900℃,合成时间为0.5~1 h;
所述步骤3)细化过程中物料2中加入50%~70%的水进行球磨;
所述步骤3)物料3粒径<2μm;
所述步骤5)物料4中加入的增塑剂为聚乙烯醇或邻苯二甲酸二丁酯,加入量为5%~10%;
所述步骤6)于1280~1350℃下烧结2~3 h;
所述步骤8)高温氧化条件为按100~160℃/小时的速度升温,升至温度1150~1250 ℃,保温110~130 min。
2.根据权利要求1所述的材料,其特征在于,所述材料包括按重量份计以下原料制成:
红丹粉50~60份,钛白粉8~10份,氧化钴18~20份,氧化镧0.5~0.8份,氧化铌0.4~0.7份,氧化铝1~1.5份。
3.根据权利要求1或2所述的材料,其特征在于:所述材料介电常数为3300~4500,压电系数为612×10-12~810×10-12c/N。
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