CN114853448B - 一种低温共烧用负温度系数热敏陶瓷材料制备方法 - Google Patents
一种低温共烧用负温度系数热敏陶瓷材料制备方法 Download PDFInfo
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Abstract
一种低温共烧用负温度系数热敏陶瓷材料制备方法,属于电子材料领域。包括如下工艺:通过高温熔炼制备Pb‑B‑Si玻璃,经冷却后,再通过气流粉碎进行粉碎,即制备出掺杂用玻璃粉助剂;将碳酸锰、三氧化二钴、氧化锌按一定的比例进行球磨混合、高温合成、过筛,即制备出合成的热敏电阻粉体;将玻璃粉助剂与热敏电阻粉体按一定的比例进行混合、烘干、过筛,即可制备成低温共烧用热敏陶瓷材料。解决了现有技术中负温度系数热敏陶瓷材料与金属电极浆料很难实现共烧的问题。可将烧结温度降低到1000℃以下,与银浆、金浆等金属电极浆料实现850℃~900℃烧结。广泛应用于负温度系数热敏陶瓷电阻的制作中。
Description
技术领域
本发明属于电子材料领域,进一步来说涉及电子陶瓷材料领域,具体来说,涉及一种低温共烧用负温度系数热敏陶瓷材料制备方法。
背景技术
负温度系数热敏陶瓷材料具备随温度升高电阻值降低的特性,通常由Mn、Co、Ni、Cu、Fe等过渡元素高温烧结而成,利用其阻值-温度特性,可用作测温及温度补偿,或利用其特有的伏安特性,制备功率计、放大器、低频振荡器,市场需求量较大。该类材料通常由固相法或者液相法制备,烧结温度在1100℃~1300℃之间,烧结温度较高,可与银钯电极等高温烧结电极材料制备多层片式NTC热敏电阻器,但常规烧结浆料如银浆、金浆等金属浆料,烧结温度在850℃左右,很难实现共烧。虽然国内部分热敏材料开发工作者,开展过相关工作,如通过共沉淀法、溶胶凝胶法提高粉体烧结活性,或者添加Bi2O3、B2O3等烧结助剂进行降温烧结,但烧结温度均在1000℃以上,均不能实现850℃~900℃烧结,无法与银电极浆料实现共烧,导致热敏电阻器生产成本较高。有鉴于此,特提出本发明。
发明内容
本发明所要解决的技术问题是:解决现有技术中负温度系数热敏陶瓷材料烧结温度过高,与烧结温度低的金属电极浆料很难实现共烧的问题。
本发明的发明构思是:通过高温熔炼法制备Pb-B-Si玻璃,再将玻璃粉作为热敏陶瓷材料烧结助剂进行掺杂,进而制备一种可与电极浆料共烧用负温度系数热敏陶瓷材料。
为此,本发明提供一种低温共烧用负温度系数热敏陶瓷材料制备方法,包括如下工艺:
(1)制备掺杂用玻璃粉助剂:通过高温熔炼制备Pb-B-Si玻璃,经冷却后,再通过气流粉碎进行粉碎,即制备出掺杂用玻璃粉助剂;
(2)制备热敏电阻粉体:将碳酸锰、三氧化二钴、氧化锌按一定的比例进行球磨混合、高温合成、过筛,即制备出合成的热敏电阻粉体;
(3)将玻璃粉助剂与热敏电阻粉体按一定的比例进行混合、烘干、过筛,即可制备成低温共烧用热敏陶瓷材料。
所述高温熔炼是在高温熔炼炉中进行。
所述冷却是在双辊冷却轧机中进行。
所述气流粉碎是在气流粉碎机中进行。
使用本发明方案制备的热敏陶瓷材料可将烧结温度降低到1000℃以下,与银浆、金浆等金属电极浆料实现850℃~900℃烧结,由传统先烧结热敏陶瓷,再烧结电极浆料的方式转变为低温共烧,从而大幅度降低生产成本。
可广泛应用于负温度系数热敏陶瓷电阻的制作中。
附图说明
图1为本发明负温度系数热敏陶瓷材料制备流程示意图。
具体实施方式
如图1所示,所述一种低温共烧用负温度系数热敏陶瓷材料制备方法,具体实施方式如下:
案例一:
(1)按质量百分比,将22wt%的氧化铅、5wt%的氧化硼、58wt%的氧化硅、10wt%的氧化钙进行配料,球磨混合4h,出料装入坩埚中。
(2)使用高温熔炼炉对混合粉料进行高温熔炼,熔炼温度为1400℃~1600℃,熔炼时间为2h~4h。
(3)高温熔炼完成后,熔融玻璃液,直接放入双辊冷却轧机,制备玻璃片。
(4)使用气流粉碎机对玻璃进行粉碎,制备掺杂用玻璃细粉,细粉粒径D50为0.5μm~2.0μm。
(5)按MnxCoyZnZ摩尔比,对碳酸锰、三氧化二钴、氧化锌三种材料进行配料,其中x为(1.0~1.3),y为(1.7~1.9),z为(0.01~0.2)进行配料。称量完成后加入球磨罐中,再添加适量去离子水,进行球磨混合,球磨转速为20r/min~200r/min,球磨时间为10h~50h。
(6)球磨完成后,进行喷雾干燥、高温烧结等常规工艺步骤,其中高温烧结温度为700℃~850℃之间,烧结时间为2h~4h。
(7)烧结完成热敏陶瓷粉体进行过筛备用。
(8)热敏陶瓷粉体与玻璃按质量百分比进行配料(70%~95%)∶(5%~30%),添加适量去离子水,然后使用球磨机进行混合。
球磨完成的浆料使用喷雾干燥塔进行喷雾干燥制备低温共烧用负温度系数热敏陶瓷材料。
案例二:
进一步地,在案例一的基础上:
(1)按质量比氧化铅22wt%、氧化硼5wt%、氧化硅58wt%,氧化钙10wt%进行配料,球磨混合4h,出料装入坩埚中。
(2)使用高温熔炼炉对混合粉料进行高温熔炼,熔炼温度为1400℃,熔炼时间为2h。
(3)高温熔融玻璃液,直接放入双辊冷却轧机,制备玻璃片。
(4)使用气流粉碎机对玻璃进行粉碎,制备掺杂用玻璃细粉,细粉粒径D50为1.0μm。
(5)按Mn1.1Co1.85Zn0.05进行配料,分别称量碳酸锰12.65Kg,三氧化钴15.34kg,氧化锌0.407Kg,添加30Kg去离子水,进行球磨混合,球磨转速为30r/min,混合时间为40h。
(6)球磨完成后,进行喷雾干燥、高温烧结,烧结温度为770℃,时间为2h。
(7)烧结完成的热敏陶瓷粉体过80目筛网备用。
(8)称量热敏陶瓷粉体20Kg,掺杂玻璃粉体3kg,进行球磨混合,再使用喷雾干燥设备制备负温度系数热敏陶瓷材料。
(9)使用PVA进行造粒、压片,双面印刷微量掺杂Pb-B-Si玻璃的电极浆料,再进行850℃高温烧结30分钟,制备共烧热敏电阻器,进行性能测试,材料B25/50值为3541,25℃电阻率为3103Ω·cm。
案例三:
(1)按照案例二方法制备Pb-B-Si玻璃粉,再按照Mn1.1Co1.8Zn0.1进行配料,制备热敏陶瓷粉体。
(2)称量热敏陶瓷粉体20Kg,掺杂玻璃粉体3kg,进行球磨混合,再使用喷雾干燥设备制备负温度系数热敏陶瓷材料。
(3)使用PVA进行造粒、压片,双面印刷微量掺杂Pb-B-Si玻璃的电阻银浆,再进行850℃高温烧结30分钟,制备共烧热敏电阻器,进行性能测试,材料B25/50值为3738,电阻率为4213Ω·cm。
最后应说明的是:上述实施例仅仅是为清楚地说明所作的举例,本发明包括但不限于以上实施例,这里无需也无法对所有的实施方式予以穷举。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。凡符合本发明要求的实施方案均属于本发明的保护范围。
Claims (3)
1.一种低温共烧用负温度系数热敏陶瓷材料制备方法,其特征在于,包括如下工艺:
(1)按质量百分比,将22wt%的氧化铅、5wt%的氧化硼、58wt%的氧化硅、10wt%的氧化钙进行配料,球磨混合4h,出料装入坩埚中;
(2)使用高温熔炼炉对混合粉料进行高温熔炼,熔炼温度为1400℃~1600℃,熔炼时间为2h~4h;
(3)高温熔炼完成后,熔融玻璃液,直接放入双辊冷却轧机,制备玻璃片;
(4)使用气流粉碎机对玻璃进行粉碎,制备掺杂用玻璃细粉,细粉粒径D50为0.5μm~2.0μm;
(5)按MnxCoyZnZ摩尔比,对碳酸锰、三氧化二钴、氧化锌三种材料进行配料,其中x为1.0~1.3,y为1.7~1.9,z为0.01~0.2;
(6)称量完成后加入球磨罐中,再添加适量去离子水,进行球磨混合,球磨转速为20r/min~200r/min,球磨时间为10h~50h;
(7)球磨完成后,进行喷雾干燥、高温烧结、过筛,高温烧结温度为700℃~850℃,烧结时间为2h~4h,制备成热敏陶瓷粉体;
(8)热敏陶瓷粉体与玻璃细粉按质量百分比(70%~95%)∶(5%~30%)进行配料,添加适量去离子水,然后使用球磨机进行混合。
2.如权利要求1所述的一种低温共烧用负温度系数热敏陶瓷材料制备方法,其特征在于:
(1)按质量比氧化铅22wt%、氧化硼5wt%、氧化硅58wt%,氧化钙10wt%进行配料,球磨混合4h,出料装入坩埚中;
(2)使用高温熔炼炉对混合粉料进行高温熔炼,熔炼温度为1400℃,熔炼时间为2h;
(3)高温熔融玻璃液,直接放入双辊冷却轧机,制备玻璃片;
(4)使用气流粉碎机对玻璃进行粉碎,制备掺杂用玻璃细粉,细粉粒径D50为1.0μm;
(5)按Mn1.1Co1.85Zn0.05进行配料,分别称量碳酸锰12.65kg,三氧化二钴15.34kg,氧化锌0.407kg,添加30kg去离子水,进行球磨混合,球磨转速为30r/min,混合时间为40h;
(6)球磨完成后,进行喷雾干燥、高温烧结,烧结温度为770℃,时间为2h;
(7)烧结完成的热敏陶瓷粉体过80目筛网备用;
(8)称量热敏陶瓷粉体20kg,掺杂玻璃粉体3kg,进行球磨混合,再使用喷雾干燥设备制备负温度系数热敏陶瓷材料;
(9)使用PVA进行造粒、压片,双面印刷微量掺杂Pb-B-Si玻璃的电极浆料,再进行850℃高温烧结30分钟,制备共烧热敏电阻器,进行性能测试,材料B25/50值为3541,25℃电阻率为3103Ω·cm。
3.如权利要求2所述的一种低温共烧用负温度系数热敏陶瓷材料制备方法,其特征在于:
(1)按照权利要求2的方法制备玻璃粉;
(2)按照Mn1.1Co1.8Zn0.1进行配料,制备热敏陶瓷粉体;
(3)称量热敏陶瓷粉体20kg,掺杂玻璃粉体3kg,进行球磨混合;
(4)使用喷雾干燥设备制备负温度系数热敏陶瓷材料;
(5)使用PVA进行造粒、压片,双面印刷微量掺杂Pb-B-Si玻璃的电阻银浆,再进行850℃高温烧结30分钟,制备共烧热敏电阻器;
所述共烧热敏电阻器的材料B25/50值为3738,电阻率为4213Ω·cm。
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