CN108675770A - 一种金属铅增韧的氧化铅陶瓷及其制备方法 - Google Patents
一种金属铅增韧的氧化铅陶瓷及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种金属铅增韧的氧化铅陶瓷及其制备方法,其制作步骤如下:步骤一:制陶瓷的原料的准备;步骤二:陶瓷坯体压制成型;步骤三:对制作的陶瓷体进行高温烧结;步骤四:上釉料。该一种金属铅增韧的氧化铅陶瓷及其制备方法,在本发明中通过细化氧化铅和Al2O3‑ZrO2复相粉体的基本晶粒和裂纹屏蔽作用,耗散裂纹前进的动力,从而进行增韧,当弥散颗粒比基体的热膨胀系数相差很多时,热应力韧化就成为氧化铅陶瓷中重要的韧化机制,增韧颗粒尺寸,基体晶粒尺寸都能对氧化铅陶瓷起到增韧的目的。
Description
技术领域
本发明涉及氧化铅陶瓷增韧技术领域,具体为一种金属铅增韧的氧化铅陶瓷及其制备方法。
背景技术
氧化铅陶瓷是一种以氧化铅为主体的陶瓷材料,用于厚膜集成电路。氧化铝陶瓷有较好的传导性、机械强度和耐高温性。需要注意的是需用超声波进行洗涤。氧化铅陶瓷是一种用途广泛的陶瓷,因为其优越的性能,在现代社会的应用已经越来越广泛,为了满足日常的使用的需求对传统的制作氧化铅进行改进。改进后的氧化铅能够大幅度的提高自身的韧性,并且在制作过程中使用微波进行烧结,避免了陶瓷本次的受热不均出现裂缝。
发明内容
本发明的目的在于提供一种金属铅增韧的氧化铅陶瓷及其制备方法,以解决现有的技术缺陷和不能达到的技术要求。
为实现上述目的,本发明提供如下技术方案:一种金属铅增韧的氧化铅陶瓷及其制备方法,其制作步骤如下:步骤一:制陶瓷的原料的准备;步骤二:陶瓷坯体压制成型;步骤三:对制作的陶瓷体进行高温烧结;步骤四:上釉料。
优选的,所述制陶瓷的原料的准备:泥料、氧化铅、二氧化铅、四氧化三铅、AlCl3·6H2O和ZrOCl·8H2O;制备陶泥:将泥料:水质量比为5:1制得生陶泥;第一阶段先制取复相粉体,以AlCl3·6H2O和ZrOCl·8H2O为前驱体,采用沉淀法制备平均晶粒尺寸为20nm的Al2O3-ZrO2复相粉体,将该粉体均匀的散落于生陶泥中,反复揉捏使其混合均匀;第二阶段制取铅溶液:将氧化铅、二氧化铅和四氧化三铅三元原料通过质量配比1:2:3,将其原料采用烧结的方式进行加热,加热温度为550℃,得到高纯度的黄色四方晶系粉末氧化铅,将氧化铅粉末倒至氯化铵溶液中溶解;然后将溶解有氧化铅粉末的氯化铵溶液倒至含有Al2O3-ZrO2复相粉体的生陶泥中进行揉捏得到半成品陶泥。
优选的,所述陶瓷坯体压制成型:第一步:粉末造粒:取一定质量的半成品陶泥,在半成品陶泥中添加4%质量分数的去离子水,再充分混合研磨均匀,在8MPa的压力下压制3分钟;第二步:加压过程:将预处理的粉末装入模具中,以0.1MPa/S的加压速率加压至15MPa,保存5分钟后以0.1MPa/S的降压速率泄压,得到金属陶瓷压坯。
优选的,所述对制作的陶瓷体进行高温烧结:采用微波烧结,微波频率范围为300MHz~300GHz之间;微波先加热陶坯表面,热量再逐渐传递到陶坯内部,使其温度逐渐上升至600℃,烧制2h后取出置于室温中冷却,得到平均晶粒尺寸为50nm的致密陶瓷。
优选的,所述上釉料:将烧结后的陶瓷本体浸泡于提前制取好的釉料中,静置5min后取出,将取出后的陶瓷本体置于烧制窑中烤制,烤制温度设为300℃,烤制40min,使釉料与陶瓷本体结为一体。
与现有技术相比,本发明的有益效果如下:
1.在本发明中通过细化氧化铅和Al2O3-ZrO2复相粉体的基本晶粒和裂纹屏蔽作用,耗散裂纹前进的动力,从而进行增韧,当弥散颗粒比基体的热膨胀系数相差很多时,热应力韧化就成为氧化铅陶瓷中重要的韧化机制,增韧颗粒尺寸,基体晶粒尺寸都能对氧化铅陶瓷起到增韧的目的。
2.在本发明中使用微波对陶瓷本体进行烧结,微波比其它用于辐射加热的电磁波,如红外线、远红外线等波长更长,因此具有更好的穿透性;微波透入介质时,由于介质损耗引起的介质温度的升高,使介质材料内部、外部几乎同时加热升温,形成休热源状态,大大缩短了常规加热中的热传导时间,且在条件为介质损耗因数与介质温度呈负相关关系时,物料内外加热均匀一致。
具体实施方式
下面将结合本发明,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
本发明提供一种技术方案:一种金属铅增韧的氧化铅陶瓷及其制备方法,其制作步骤如下:步骤一:制陶瓷的原料的准备;步骤二:陶瓷坯体压制成型;步骤三:对制作的陶瓷体进行高温烧结;步骤四:上釉料。
制陶瓷的原料的准备:泥料、氧化铅、二氧化铅、四氧化三铅、AlCl3·6H2O和ZrOCl·8H2O;制备陶泥:将泥料:水质量比为5:1制得生陶泥;第一阶段先制取复相粉体,以AlCl3·6H2O和ZrOCl·8H2O为前驱体,采用沉淀法制备平均晶粒尺寸为20nm的Al2O3-ZrO2复相粉体,将该粉体均匀的散落于生陶泥中,反复揉捏使其混合均匀;第二阶段制取铅溶液:将氧化铅、二氧化铅和四氧化三铅三元原料通过质量配比1:2:3,将其原料采用烧结的方式进行加热,加热温度为550℃,得到高纯度的黄色四方晶系粉末氧化铅,将氧化铅粉末倒至氯化铵溶液中溶解;然后将溶解有氧化铅粉末的氯化铵溶液倒至含有Al2O3-ZrO2复相粉体的生陶泥中进行揉捏得到半成品陶泥。
陶瓷坯体压制成型:第一步:粉末造粒:取一定质量的半成品陶泥,在半成品陶泥中添加4%质量分数的去离子水,再充分混合研磨均匀,在8MPa的压力下压制3分钟;第二步:加压过程:将预处理的粉末装入模具中,以0.1MPa/S的加压速率加压至15MPa,保存5分钟后以0.1MPa/S的降压速率泄压,得到金属陶瓷压坯。
对制作的陶瓷体进行高温烧结:采用微波烧结,微波频率范围为300MHz~300GHz之间;微波先加热陶坯表面,热量再逐渐传递到陶坯内部,使其温度逐渐上升至600℃,烧制2h后取出置于室温中冷却,得到平均晶粒尺寸为50nm的致密陶瓷。
上釉料:将烧结后的陶瓷本体浸泡于提前制取好的釉料中,静置5min后取出,将取出后的陶瓷本体置于烧制窑中烤制,烤制温度设为300℃,烤制40min,使釉料与陶瓷本体结为一体。
本发明一种金属铅增韧的氧化铅陶瓷及其制备方法,先制取生陶泥,然后制取复相粉体,以AlCl3·6H2O和ZrOCl·8H2O为前驱体,制得Al2O3-ZrO2复相粉体,然后再制取铅溶液,将氧化铅、二氧化铅和四氧化三铅采用烧结的方式进行加热,加热温度为550℃得到高纯度的黄色四方晶系粉末氧化铅,将Al2O3-ZrO2复相粉体均匀的散落至生陶泥中,再将含有氧化铅的氯化铵溶液倒至生陶泥中进行揉捏制成半成品陶泥;对半成品陶泥进行压制成型制得陶坯,向半成品陶泥中加入4%质量分数的去离子水,在8MPa的压力下压制3分钟,得到金属陶瓷压坯;然后采用微波烧结的方式对其进行烧结,最终得到晶粒尺寸为50nm的致密陶瓷;然后将陶瓷成品置于提前配制好的釉料中浸泡5分钟取出进行烤制。
在本发明中通过细化氧化铅和Al2O3-ZrO2复相粉体的基本晶粒和裂纹屏蔽作用,耗散裂纹前进的动力,从而进行增韧,当弥散颗粒比基体的热膨胀系数相差很多时,热应力韧化就成为氧化铅陶瓷中重要的韧化机制,增韧颗粒尺寸,基体晶粒尺寸都能对氧化铅陶瓷起到增韧的目的。2.在本发明中使用微波对陶瓷本体进行烧结,微波比其它用于辐射加热的电磁波,如红外线、远红外线等波长更长,因此具有更好的穿透性;微波透入介质时,由于介质损耗引起的介质温度的升高,使介质材料内部、外部几乎同时加热升温,形成休热源状态,大大缩短了常规加热中的热传导时间,且在条件为介质损耗因数与介质温度呈负相关关系时,物料内外加热均匀一致
将变形后的陶瓷与未变性做对比得到如下实验数据:
数据一:
种类 | 晶体晶粒/nm | 裂纹长度/mm | 强度/MP | 韧性/KJ·M2 |
普通陶瓷 | 5 | 18 | 359 | 58 |
加铅陶瓷 | 4 | 12 | 418 | 37 |
数据二:
种类 | 波长/mm | 温度/℃ | 热传导时间/s | 介质损耗/tgδ |
微波 | 50 | 500 | 7.8 | 3.5 |
红外线 | 0.9 | 300 | 5.3 | 2.7 |
远红外线 | 0.5 | 200 | 4.2 | 2.1 |
结论:制作而成的变性成品氧化铅陶瓷,使其陶瓷的韧性得到大幅度的提升。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (5)
1.一种金属铅增韧的氧化铅陶瓷及其制备方法,其特征在于:其制作步骤如下:步骤一:制陶瓷的原料的准备;步骤二:陶瓷坯体压制成型;步骤三:对制作的陶瓷体进行高温烧结;步骤四:上釉料。
2.根据权利要求1所述的一种金属铅增韧的氧化铅陶瓷及其制备方法,其特征在于:制陶瓷的原料的准备:泥料、氧化铅、二氧化铅、四氧化三铅、AlCl3·6H2O和ZrOCl·8H2O;制备陶泥:将泥料:水质量比为5:1制得生陶泥;第一阶段先制取复相粉体,以AlCl3·6H2O和ZrOCl·8H2O为前驱体,采用沉淀法制备平均晶粒尺寸为20nm的Al2O3-ZrO2复相粉体,将该粉体均匀的散落于生陶泥中,反复揉捏使其混合均匀;第二阶段制取铅溶液:将氧化铅、二氧化铅和四氧化三铅三元原料通过质量配比1:2:3,将其原料采用烧结的方式进行加热,加热温度为550℃,得到高纯度的黄色四方晶系粉末氧化铅,将氧化铅粉末倒至氯化铵溶液中溶解;然后将溶解有氧化铅粉末的氯化铵溶液倒至含有Al2O3-ZrO2复相粉体的生陶泥中进行揉捏得到半成品陶泥。
3.根据权利要求1所述的一种金属铅增韧的氧化铅陶瓷及其制备方法,其特征在于:陶瓷坯体压制成型:第一步:粉末造粒:取一定质量的半成品陶泥,在半成品陶泥中添加4%质量分数的去离子水,再充分混合研磨均匀,在8MPa的压力下压制3分钟;第二步:加压过程:将预处理的粉末装入模具中,以0.1MPa/S的加压速率加压至15MPa,保存5分钟后以0.1MPa/S的降压速率泄压,得到金属陶瓷压坯。
4.根据权利要求1所述的一种金属铅增韧的氧化铅陶瓷及其制备方法,其特征在于:对制作的陶瓷体进行高温烧结:采用微波烧结,微波频率范围为300MHz~300GHz之间;微波先加热陶坯表面,热量再逐渐传递到陶坯内部,使其温度逐渐上升至600℃,烧制2h后取出置于室温中冷却,得到平均晶粒尺寸为50nm的致密陶瓷。
5.根据权利要求1所述的一种金属铅增韧的氧化铅陶瓷及其制备方法,其特征在于:上釉料:将烧结后的陶瓷本体浸泡于提前制取好的釉料中,静置5min后取出,将取出后的陶瓷本体置于烧制窑中烤制,烤制温度设为300℃,烤制40min,使釉料与陶瓷本体结为一体。
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