CN109665831A - 一种低温烧结高稳定ntc热敏电阻体及其制备方法 - Google Patents

一种低温烧结高稳定ntc热敏电阻体及其制备方法 Download PDF

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CN109665831A
CN109665831A CN201811356779.5A CN201811356779A CN109665831A CN 109665831 A CN109665831 A CN 109665831A CN 201811356779 A CN201811356779 A CN 201811356779A CN 109665831 A CN109665831 A CN 109665831A
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林德智
蒋璐莲
蒋朝伦
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ZHAOQING JINLONGBAO ELECTRONICS CO Ltd
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Abstract

本发明涉及一种低温烧结高稳定NTC热敏电阻体及其制造方法，属于电阻体制备技术领域；该电阻体含有如下重量百分比的组分：23~30 mol%Mn、31~36mol%Co、22~26mol%Fe、8~13mol%Al，并掺杂氧化锌、氧化铜、三氧化二铌、二氧化锆；具体是以Mn3O4、CO3O4、Fe2O3、Al2O3、CuO、Nd2O3、ZrO2为原材料，通过球磨、烘干、预烧、二次球磨、烘干、打粉、压锭、烧结、切割、上电极、划片、封装等工序来制备；该电阻具有成本低，稳定性好、重复性强等特点，普遍应用于高灵敏、高反应速度的领域。

Description

一种低温烧结高稳定NTC热敏电阻体及其制备方法
技术领域
本发明涉及一种热敏电阻体及其制备方法，具体涉及一种低温烧结高稳定NTC热敏电阻体及其制备方法，属于半导体制备技术领域。。
背景技术
NTC是Negative Temperature Coefficient 的缩写，意思是负的温度系数，泛指负温度系数很大的半导体材料或元器件，所谓NTC热敏电阻器就是负温度系数热敏电阻器。它是以锰、钴、镍、铁等金属氧化物为主要材料，采用陶瓷工艺制造而成的。这些金属氧化物材料都具有半导体性质，因为在导电方式上完全类似锗、硅等半导体材料。温度低时，这些氧化物材料的载流子（电子和孔穴）数目少，所以其电阻值较高；随着温度的升高，载流子数目增加，所以电阻值降低。NTC热敏电阻器在室温下的变化范围在10O~1000000欧姆，温度系数-2%~-6.5%。NTC热敏电阻器可广泛应用于温度测量、温度补偿、抑制浪涌电流等场合。
电子信息技术的发展和数字化趋势对电子设备提出了小型化、轻型化、智能化方面发展。电子元件的开发和生产必须向小型化、智能化方向发展。同时，对电子元件的高可靠性和高稳定性提出更高的要求。
要实现热敏电阻的高可靠性和高稳定性，对热敏电阻配方有更高的要求。配方的稳定性和生产成本的降低，都是需要解决的关键问题所在。开发新配方，对加快我国NTC热敏电阻发展步伐，具有重要的意义，对热敏技术行业的技术提升和经济效益有很高的应用价值。
中国发明：201110370713.3；公开一种高B值、高稳定性的NTC热敏电阻材料及其生产方法，该热敏电阻材料烧结温度比较高，因此，开发一种低温烧结高稳定NTC热敏电阻体及其制备方法具有十分重要的意义。
发明内容
本发明提供一种烧结温度更低的NTC热敏电阻体，技术方案如下：一种低温烧结高稳定NTC热敏电阻体，该热敏电阻体的各个原材料成分以及比例为：23~30 mol%Mn、31~36mol %Co、22~26 mol %Fe、8~13 mol %Al，并掺杂氧化锌0~2mol%、氧化铜1~3mol%、三氧化二铌1~4mol%、二氧化锆1~2mol%。
该低温烧结高稳定NTC热敏电阻体通过下属步骤制备得出：
步骤1：配料
主要原材料有Mn3O4 、CO3O4、Fe2O3、Al2O3、CuO、Nd2O3、ZrO2，在使用前测试水份，测试温度115℃，恒温时间6min；
步骤2：球磨
将已配好的各原材料混合均匀，并将其小型球磨机研磨细化，细度为50目；
步骤3：烘干
用专用不锈钢烘盘盛装研磨好的料，烘料温度控制在320℃，烘料时间8~10小时，出烘炉的粉料需冷却1.2h后再倒入装料桶；
步骤4：打粉
将烘干后未预烧的粉料块用专用打粉机打粉，用60目筛网进行，用专用或干净装料桶盛装；
步骤5：预烧
将已打粉的粉料，用专用坩锅装八至九成满，放在纳博炉或马沸炉预烧合成，合成温度为950℃，保温h，自然冷却至室温出炉；
步骤6：二次球磨
将预烧后的粉料二次球磨，其中，料：球：水的比例为1：1.5：0.6，球磨时间4小时，粒度在150-200目；
步骤7：烘干
用专用不锈钢烘盘盛装二次球磨的料，烘料温度控制在320℃，烘料时间6~8小时，出烘炉的粉料需冷却1.2h后再倒入装料桶；
步骤8：压制成型
使用模具成型为圆锭形状，并用薄膜抽真空密封，然后在等静压机中，使用250个大气压下将粉料进行压制成型；
步骤9：高温烧结
将步骤8中的圆锭样品进行高温烧结，温度曲线：室温经过6小时升温到150℃，保温8小时，8小时均匀升温至350℃，保温3小时，6小时均匀升温至800℃，保温8小时，2小时均匀升温至1150℃，保温8小时，8小时降温至800℃，保温8小时，8小时降温至300℃，保温4小时，自然降温至室温，然后取出。
所制备的NTC热敏电阻电阻体电阻率ρ在11000~12000Ω·cm，B值在3900~4000K之间。
本发明是这样实现的将主体框架从橱柜框拉出来，大件放置区域用于放置厨房备用品如大桶色拉油、酱油等高瓶、大瓶装调料，不会经常使用的物品和具有较高的厨房用品，大件放置区和小件放置区之间设置的底板，所述的底板将大件放置区和小件放置区分隔开，将刀具、筷子、高瓶装调料物品等烹饪时使用频率高物品放置在小件放置区，同时根据需要可将常用的食用调味料放置在放置槽中，当需要使用放置槽下方小件放置区内使用频率低的其他物品时，先拉出主体框架后只需轻推放置槽，放置槽在铰链杆的摆动作用下，可推开放置槽使用小件放置区内的其他物品。
有益效果是：与其他电阻相比，本发明属于锰-钴-铁三元系结构配方；就三元系配方而言，烧结温度在1200度，本发明中添加了氧化锌ZnO，使得其烧结温度降低了50摄氏度，也能够很好地烧结成型；并可节省在高温保温区的电能；可方便调节材料的电阻率和B值，使芯片的尺寸更合理，方便生产，提高效率；最重要的是，能有效地提高产品的高精度、合格率和高温的稳定性。
附图说明
图1为实施例在电子显微镜下的成相图。
具体实施方式
一低温烧结高稳定NTC热敏电阻体，该热敏电阻体的各个原材料成分以及比例为：24.2 mol%Mn、32.3mol %Co、25.5 mol %Fe、10 .1mol %Al，并掺杂氧化锌1.1mol%、氧化铜2.6mol%、三氧化二铌3.1mol%、二氧化锆1.2mol%
该低温烧结高稳定NTC热敏电阻体通过下属步骤制备得出：
步骤1：配料
主要原材料有Mn3O4 、CO3O4、Fe2O3、Al2O3、CuO、Nd2O3、ZrO2，在使用前测试水份，测试温度115℃，恒温时间6min；
步骤2：球磨
将已配好的各原材料混合均匀，并将其小型球磨机研磨细化，细度为50目；
步骤3：烘干
用专用不锈钢烘盘盛装研磨好的料，烘料温度控制在320℃，烘料时间8~10小时，出烘炉的粉料需冷却1.2h后再倒入装料桶；
步骤4：打粉
将烘干后未预烧的粉料块用专用打粉机，型号为CJL-01，打粉，用60目筛网进行，用专用或干净装料桶盛装；
步骤5：预烧
将已打粉的粉料，用专用坩锅装八至九成满，放在纳博炉或马沸炉预烧合成，合成温度为950℃，保温h，自然冷却至室温出炉；
步骤6：二次球磨
将预烧后的粉料二次球磨，其中，料：球：水的比例为1：1.5：0.6，球磨时间4小时，粒度在150-200目；
步骤7：烘干
用专用不锈钢烘盘盛装二次球磨的料，烘料温度控制在320℃，烘料时间6~8小时，出烘炉的粉料需冷却1.2h后再倒入装料桶；
步骤8：压制成型
使用模具成型为圆锭形状，并用薄膜抽真空密封，然后在等静压机中，型号为JYc350，使用250个大气压下将粉料进行压制成型；
步骤9：高温烧结
将步骤8中的圆锭样品进行高温烧结，温度曲线：室温经过6小时升温到150℃，保温8小时，8小时均匀升温至350℃，保温3小时，6小时均匀升温至800℃，保温8小时，2小时均匀升温至1150℃，保温8小时，8小时降温至800℃，保温8小时，8小时降温至300℃，保温4小时，自然降温至室温，然后取出。
为测试高温烧结后的样品效果还包括如下步骤：
步骤10：切片
使用内圆切割机J55090，将圆锭切割成0.1mm厚度的薄片；
步骤11：上电极
在薄片两边涂覆上YD352型纯银浆，并在800度烧结，得到芯片的电极；
步骤12：划片
使用HW1601精密划片机，将薄片切割成1mm×1mm的小方片，即为成品；
步骤13：测试
使用THY-3010G恒温水油槽作为测试介质，使用高精度万用表测试阻值，得到电阻体电阻率ρ在11256Ω·cm，B值在3934K。
有益效果是：与其他电阻相比，本发明属于锰-钴-铁三元系结构配方；就三元系配方而言，烧结温度在1200度，本发明中添加了氧化锌ZnO，使得其烧结温度降低了50摄氏度，也能够很好地烧结成型；并可节省在高温保温区的电能；可方便调节材料的电阻率和B值，使芯片的尺寸更合理，方便生产，提高效率；最重要的是，能有效地提高产品的高精度、合格率和高温的稳定性。

Claims (3)

1.一种低温烧结高稳定NTC热敏电阻体，其特征在于： 该热敏电阻体的各个原材料成分以及比例为：23~30 mol%Mn、31~36 mol %Co、22~26 mol %Fe、8~13 mol %Al，并掺杂氧化锌0~2mol%、氧化铜1~3mol%、三氧化二铌1~4mol%、二氧化锆1~2mol%。
2.根据权利要求1所述的一种低温烧结高稳定NTC热敏电阻体，其特征在于：所述的电阻体电阻率ρ在11000~12000Ω·cm，B值在3900~4000K之间。
3. 一种制备权利要求1-2中低温烧结高稳定NTC热敏电阻体的制备方法，其特征在于：其制备工艺为：
步骤1：配料
主要原材料有Mn3O4 、CO3O4、Fe2O3、Al2O3、CuO、Nd2O3、ZrO2，在使用前测试水份，测试温度115℃，恒温时间6min；
步骤2：球磨
将已配好的各原材料混合均匀，并将其小型球磨机研磨细化，细度为50目；
步骤3：烘干
用专用不锈钢烘盘盛装研磨好的料，烘料温度控制在320℃，烘料时间8~10小时，出烘炉的粉料需冷却1.2h后再倒入装料桶；
步骤4：打粉
将烘干后未预烧的粉料块用专用打粉机打粉，用60目筛网进行，用专用或干净装料桶盛装；
步骤5：预烧
将已打粉的粉料，用专用坩锅装八至九成满，放在纳博炉或马沸炉预烧合成，合成温度为950℃，保温h，自然冷却至室温出炉；
步骤6：二次球磨
将预烧后的粉料二次球磨，其中，料：球：水的比例为1：1.5：0.6，球磨时间4小时，粒度在150-200目；
步骤7：烘干
用专用不锈钢烘盘盛装二次球磨的料，烘料温度控制在320℃，烘料时间6~8小时，出烘炉的粉料需冷却1.2h后再倒入装料桶；
步骤8：压制成型
使用模具成型为圆锭形状，并用薄膜抽真空密封，然后在等静压机中，使用250个大气压下将粉料进行压制成型；
步骤9：高温烧结
将步骤8中的圆锭样品进行高温烧结，温度曲线：室温经过6小时升温到150℃，保温8小时，8小时均匀升温至350℃，保温3小时，6小时均匀升温至800℃，保温8小时，2小时均匀升温至1150℃，保温8小时，8小时降温至800℃，保温8小时，8小时降温至300℃，保温4小时，自然降温至室温，然后取出。
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110357586A (zh) * 2019-06-13 2019-10-22 山东格仑特电动科技有限公司 一种一致性好的ntc热敏电阻材料及其制备方法
CN112366052A (zh) * 2020-11-09 2021-02-12 肇庆市金龙宝电子有限公司 一种医疗体温测量用高精度热敏电阻芯片及其制备方法
CN116230340A (zh) * 2023-03-03 2023-06-06 肇庆市金龙宝电子有限公司 一种耐高温的陶瓷薄膜ntc热敏电阻及其制备方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101618963A (zh) * 2009-07-28 2010-01-06 四川西汉电子科技有限责任公司 一种高均匀性高稳定性负温度系数热敏材料及其制备方法
CN101659544A (zh) * 2009-07-29 2010-03-03 四川西汉电子科技有限责任公司 一种低成本负温度系数热敏材料及其制备方法
CN102515737A (zh) * 2011-11-21 2012-06-27 肇庆市金龙宝电子有限公司 高b值、高稳定性的ntc热敏电阻材料及其生产方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101618963A (zh) * 2009-07-28 2010-01-06 四川西汉电子科技有限责任公司 一种高均匀性高稳定性负温度系数热敏材料及其制备方法
CN101659544A (zh) * 2009-07-29 2010-03-03 四川西汉电子科技有限责任公司 一种低成本负温度系数热敏材料及其制备方法
CN102515737A (zh) * 2011-11-21 2012-06-27 肇庆市金龙宝电子有限公司 高b值、高稳定性的ntc热敏电阻材料及其生产方法

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
刘旭: ""Mn-Co-Fe-(Zn)-O 系热敏材料制备及稳定性研究"", 《中国优秀硕士学位论文全文数据库 信息科技辑》 *
天津大学无线电材料与元件教研室编: "《电阻器》", 30 April 1981, 技术标准出版社 *
汪啸穆主编: "《陶瓷工艺学》", 31 May 1994, 北京：中国轻工业出版社 *
王迎军主编: "《新型材料科学与技术 无机材料卷 上》", 31 October 2016, 广州：华南理工大学出版社 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110357586A (zh) * 2019-06-13 2019-10-22 山东格仑特电动科技有限公司 一种一致性好的ntc热敏电阻材料及其制备方法
CN112366052A (zh) * 2020-11-09 2021-02-12 肇庆市金龙宝电子有限公司 一种医疗体温测量用高精度热敏电阻芯片及其制备方法
CN116230340A (zh) * 2023-03-03 2023-06-06 肇庆市金龙宝电子有限公司 一种耐高温的陶瓷薄膜ntc热敏电阻及其制备方法
CN116230340B (zh) * 2023-03-03 2024-02-13 肇庆市金龙宝电子有限公司 一种耐高温的陶瓷薄膜ntc热敏电阻及其制备方法

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