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四元系Mn-Ni(Co)-Fe-Zn-O 热敏陶瓷材料的制备及电学性能研究
谢鲜鲜
学位类型硕士
导师常爱民
2017-05-25
学位授予单位中国科学院大学
学位授予地点北京
学位专业材料工程
关键词Ntc热敏电阻 硫酸盐 Xrd Sem 稳定性
其他摘要

NTC常温热敏电阻(-60 ℃ ~ 300 ℃)以由于测量温区较宽,研究比较成熟,广泛地应用于家用电器,移动设备以及汽车电子等民用领域。随着消费电子的发展,具有目标参数的ρ25=10(±3%) KW?cm, B25/50=3950(±3%) K的常温热敏电阻需求量逐渐增大。因此,制备符合市场需求的常温热敏电阻是目前主要研究方向之一。Mn-Ni-Fe-O与Mn-Co-Fe-O氧化物材料体系由于具有较宽B值(1000 K ~ 6000 K)和电阻率(100 ~ 105 KΩ·cm)在民用领域中应用较多。为了制备具有特定目标参数的 NTC 热敏电阻,本文选用 Zn 元素对 Mn-Ni-Fe-O氧化物陶瓷材料进行掺杂,调节热敏电阻的电学性能;采用微波烧结、二步烧结、常规烧结制备具有目标参数的Mn-Co-Fe-Zn-O 氧化物陶瓷材料,研究不同烧结方法对材料的一致性以及稳定性的影响;并采用硫酸盐共沉淀法对比硝酸盐共沉淀法制备Mn-Co-Fe-Zn-O 氧化物陶瓷材料,研究不同原材料对热敏电阻一致性以及稳定性的影响。主要研究内容与得到的结论如下:(1)采用共沉淀制备ZnxFe2.5-xNi2Mn1.5O8(0≤x≤0.8) 陶瓷粉体,结合XRD分析确定了最佳烧结温度为700 ℃,烧结后陶瓷晶粒平均尺寸范围为3 mm ~2 mm,随着Zn含量的增加,相对密度先从94.74 %增加到97.12 %,随后减少到 92.57 %,当掺杂量为x=0.2时,材料相对密度达到最大97.12 %。Zn元素的掺杂有效地改善了陶瓷材料的致密性。(2)随着Zn含量的增加,陶瓷样品的B25/50值从5375 K 减少至3911 K以及r25从9042 KW?cm 减少至 18 KW?cm。说明ZnxFe2.5-xNi2Mn1.5O8(0≤x≤0.8) 陶瓷具有较高的温度灵敏度,可根据调整Zn的掺杂量,得到相应的电学性能参数。(3)ZnxFe2.5-xNi2Mn1.5O8(0≤x≤0.8) 陶瓷样品在125 ℃下老化600 h,材料的△R/R0范围为0.64% ~0.99%,在x=0.2时得到最小值的△R/R0=0.58 %,(4)采用共沉淀制备Zn0.4Fe2.1Co2Mn1.5O8 热敏陶瓷粉体,对比硫酸盐与硝酸盐共沉淀法制备得到陶瓷样品在1200 ℃烧结后SEM分析,硫酸盐共沉淀法制备得到的Zn0.4Fe2.1Co2Mn1.5O8陶瓷样品致密度较高。(5)硫酸盐共沉淀法制备得到的Zn0.4Fe2.1Co2Mn1.5O8热敏陶瓷样品,其电学参数B25/50=4036 K,r25=13 KΩ·cm,△R/R0 =0.2 ‰;硝酸盐共沉淀制备得到的陶瓷样品其电学参数B25/50=3955 K,r25=11 KΩ·cm,△R/R0 =0.5 ‰;利用数据统计分析可知,硫酸盐共沉淀法所制备的陶瓷元器件其B25/50值的一致性较高,稳定性较好。

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Room temperature thermistor (60 ℃ ~ 300 ℃) has been widely used in home equipment, mobile devices and automotive electronics and other civilian areas with the wide temperature range of measurement and mature skills. As development of consumer electronics, Room temperature thermistor with ρ25=10(±3%) KW?cm, B25/50=3950(±3%) K demand increased gradually. Therefore, it is main research direction to prepare the normal temperature thermistor in accordance with market demand. Mn-Ni-Fe-O and Mn-Co-Fe-O oxide system is widely applied on the civilian areas as a wide range of resistivity(100 ~ 105 KΩ·cm), as well as B value(1000 K ~ 6000 K).Through microwave sintering, two step sintering and conventional sintering to prepare Mn-Co-Fe-Zn-O oxide ceramic material with target parameters. The effect of different sintering methods on the consistency and stability of material is studied. And sulfate coprecipitation method is used to contrast the nitrate coprecipitation preparation of Mn-Co-Fe-Zn-O oxide ceramic material, which study the influence of different raw materials for thermistor consistency and stability.The main contents are as follows:(1).The most appropriate ZnxFe2.5-xNi2Mn1.5O8(0≤x≤0.8) ceramic calcined temperature is 700 ℃ by XRD. The average grain size and relative density of the as-sintered samples decrease range from 3 mm to 2 mm and 97.12 % to 92.57%, respectively. The relative density presents a maximum value 97.12% with the Zn content of x = 0.2, which shows Zn-doping can improve the relative density of ceramic material.(2).The values of B and ρ25 of the ceramic samples with increasing Zn content are in the range of 5375 ~4177 K and 9042 KΩ?cm ~ 18 KΩ?cm, respectively. ZnxFe2.5-xNi2Mn1.5O8(0≤x≤0.8) have a high temperature sensitivity coefficient and we can adjust the electronic performance parameters by Zn content.(3).The resistivity drift of ZnxFe2.5-xNi2Mn1.5O8(0≤x≤0.8) ceramic samples is range from 0.58% ~0.99% and present a minimum value 0.58 % with the Zn content of x = 0.2 after aging at 125 ℃ for 600 h. (4).Zn0.4Fe2.1Co2Mn1.5O8 ceramic precursor powders are prepared by coprecipitation method with sulfate and nitrate as raw material and sintered at 1200 ℃. From SEM analysis, sulfate as raw materials might be prepared high density Zn0.4Fe2.1Co2Mn1.5O8 ceramic material.(5).The values of electronic performance parameters of Zn0.4Fe2.1Co2Mn1.5O8 ceramic prepared by both sulfate and nitrate material are B=4036 K, r25 = 13KΩ·cm, △R/R0=0.2 ‰ and B = 3955 K,r25=11 KΩ·cm, △R/R0=0.5 ‰ respectively. By data statistical analysis, the consistency of B value and stability is higher when ceramic components were prepared by sulfate material.

文献类型学位论文
条目标识符http://ir.xjipc.cas.cn/handle/365002/4943
专题材料物理与化学研究室
作者单位中国科学院新疆理化技术研究所
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谢鲜鲜. 四元系Mn-Ni(Co)-Fe-Zn-O 热敏陶瓷材料的制备及电学性能研究[D]. 北京. 中国科学院大学,2017.
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