WO2019096335A1 - 一种复合型热敏电阻材料及其制备方法和应用 - Google Patents

一种复合型热敏电阻材料及其制备方法和应用 Download PDF

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WO2019096335A1
WO2019096335A1 PCT/CN2018/123419 CN2018123419W WO2019096335A1 WO 2019096335 A1 WO2019096335 A1 WO 2019096335A1 CN 2018123419 W CN2018123419 W CN 2018123419W WO 2019096335 A1 WO2019096335 A1 WO 2019096335A1
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oxide
thermistor
powder
thermistor material
composite
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PCT/CN2018/123419
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English (en)
French (fr)
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倪立
姜胜林
苏东
李明亚
冯安琪
张超
赵青
张博
周洋
方菊
方礼龙
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首凯汽车零部件（江苏）有限公司
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Priority to GB1904929.5A priority Critical patent/GB2582185B/en
Priority to US16/341,880 priority patent/US10622124B2/en
Publication of WO2019096335A1 publication Critical patent/WO2019096335A1/zh

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  • Compositions Of Oxide Ceramics (AREA)

Abstract

一种复合型热敏电阻材料及其制备方法和应用，将钙钛矿结构氧化物和烧绿石结构氧化物复合，采用固相反应法进行球磨、烘干、成型后煅烧制成圆片型坯体，然后经过高温烧结而形成耐高温可控B值的热敏电阻陶瓷，随后通过涂敷铂浆制成热敏电阻圆形片，切片后焊接铂丝作为引线形成热敏电阻元件。该热敏电阻能够实现由室温至1000℃范围的温度测量并且具有良好的负温度系数热敏电阻特性，并且可通过两相比率的改变实现调节热敏电阻系数B以满足不同系统中的要求。

Description

一种复合型热敏电阻材料及其制备方法和应用 技术领域
本发明属于温度传感器技术，具体涉及一种复合型热敏电阻材料及其制备方法和应用。
背景技术
负温度系数热敏电阻是一种电阻随温度的升高而下降的一种热敏材料，其作为电路补偿器件广泛应用于各种电路系统中，而作为温度探测元件，其相对于传统的热电偶，热电阻等器件，热敏电阻的主要特点在于其拥有高灵敏度，体积小，良好的线性特性并且价格低廉。高温热敏电阻材料相对于传统热敏电阻材料具有更好的稳定性并可以实现由室温至1000℃高温的宽温区测量，同时这种热敏电阻在汽车尾气环境下更稳定。因此相对于其他温度探测器而言，热敏电阻是更好的选择，因此这种可以耐高温的热敏电阻广泛应用在汽车石油地质钻探等领域。由于国内尚未形成成熟的热敏电阻制造体系，很难自主制造满足各类要求的高温热敏电阻，因此目前尾气温度传感器的热敏电阻芯片主要依赖于进口。
热敏电阻的主要参数在于其电阻率和其热敏电阻系数B值，热敏电阻系数B值是衡量热敏电阻温度与电阻变化的重要参量。对于高温热敏电阻为实现0-1000℃的测量要求材料具有高的电阻率和低的B值。然而过高的B值导致电阻下降的过快在高温区电阻过小测量精度受到限制，过低的B值将造成热敏电阻灵敏度的下降。常用高温热敏电阻的热敏电阻系数B值的范围为2000—4000。对于负温度系数热敏电阻NTC来说材料的电阻率调节比较容易，而材料的B值因其导电机制每种材料体系的B值基本固定很难改变。因此实现2000-4000范围内B值的调节是生产不同要求的负温度系数热敏电阻材料的关键。
发明内容
发明目的：本发明的目的在于解决现有技术中存在的不足，提供一种复合型热敏电阻材料及其制备方法和应用，本发明利用两种特性不同的高温热敏电阻材料复合以得到合适的热敏电阻系数，不但能够保证良好的高温特性以及热敏电阻特性，同时还实现不同比率的热敏电阻的热敏电阻系数B值在2000-4000的范围内通过两种物质比率的改变实现调节，能够制作参数要求不同的高温热敏电阻。
技术方案：本发明的一种复合型热敏电阻材料，包括钙钛矿结构氧化物和烧绿石结构氧化物，且二者的摩尔比为(70:30)～(90:10)，且钙钛矿结构氧化物中含有钇、锰和铬，烧绿石结构氧化物中含有钙、钛、钨和铈。
进一步的，所述钙钛矿氧化物和烧绿石氧化物分别为YCr 0.5Mn 0.5O 3和CaWO 4-CeTi 2O 6。
进一步的，所述钙钛矿结构氧化物中钇锰铬的摩尔质量比为(2～2.5)：(0.8～1.2)：(0.8～1.2)，所述烧绿石氧化物中钙钛钨铈的摩尔质量比(0.8～1.2)：(0.8～1.2)：(0.8～1.2)：(2～2.5)。
例如，钙钛矿结构氧化物中钇锰铬的摩尔质量比为2：1：1，所述烧绿石氧化物中钙钛钨铈的摩尔质量比1：1：1：2，采用此处的摩尔质量比能够使得制备后的复合型热敏电阻材料达到最优电阻率和B值，性能优越。
本发明还公开了一种复合型热敏电阻材料的制备方法，依次包括以下步骤：
(1)称取分析纯的Y 2O 3，Mn 2O 3和Cr 2O 3混合研磨，且三者之间的摩尔质量比为2：1：1；然后在1200℃下将研磨后的混合物煅烧1-2小时得到YCr 0.5Mn 0.5O3氧化物粉料；
(2)称取分析纯的CaCO 3，CeO 2，TiO 2和WO 3混合研磨，且四者之间的摩尔质量比为2：2：2：1；然后将研磨烘干后的粉料在1000℃下煅烧3h得到CaWO 4-CeTi 2O 6氧化物粉料；
(3)称取步骤(1)制备好的钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体，并加入PVA粘合剂使该钙钛矿氧化物粉料成颗粒状均匀分散，将均匀分散的颗粒直接在1400-1600℃下烧结1-2h；
(4)称取步骤(3)烧结后钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体，以及步骤(2)中制备好的烧绿石氧化物CaWO 4-CeTi 2O 6粉体，将二者混合研磨4-8h使其均匀，此处钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体与烧绿石氧化物CaWO 4-CeTi 2O 6粉体的摩尔比为(70:30)～(90:10)；
(5)将步骤(4)中混合研磨均匀的粉体加入PVA粘合剂，使其再次形成粒状的均匀分散颗粒，然后将均匀分散的颗粒经过模具成型后形成圆片；
(6)将成型后的圆片在1400摄氏度下烧结形成B值可调节的热敏电阻材料；
(7)将铂浆涂敷在步骤(6)中烧结好的热敏电阻材料表面，然后将其在1200℃下保温2h；
(8)将步骤(7)中所得的热敏电阻材料按照需求进行切割处理，对切割后的热敏电阻芯片焊接铂制引线。
进一步的，所述步骤(3)中，将加入PVA粘合剂后的钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体经过造粒处理后，不经过模具成型直接将均匀分散的颗粒在1400-1500℃下烧结。
本发明还公开了一种复合型热敏电阻材料的应用，将该复合型热敏电阻材料用于制备复合型热敏电阻，具体方法为：将相应长度的铂线末端涂敷铂浆，并将该铂线粘结在切割处理后的热敏电阻芯片两端，经过1200℃的高温处理后形成带有引线的高温热敏电阻。
本发明还公开了一种复合型热敏电阻材料的应用，将该复合型热敏电阻材料用于制备高温密质成瓷热敏电阻温度传感器。
有益效果：本发明中的复合型热敏电阻材料，根据其复合材料的比例不同，获得的热敏电阻系数B值不同，可实现由2000-4000的B值调节以满足不同工业生产的要求。本发明可广泛应用在汽车尾气测量以及各种温度测量领域中，是一种价格低廉，性能稳定的热敏电阻材料。
附图说明
图1为实施例1中阻温特性曲线示意图；
图2为实施例2中阻温特性曲线示意图；
图3为实施例3中阻温特性曲线示意图；
图4为实施例4中阻温特性曲线示意图。
具体实施方式
下面对本发明技术方案进行详细说明，但是本发明的保护范围不局限于所述实施例。
本发明的一种复合型热敏电阻材料，包括钙钛矿结构氧化物和烧绿石结构氧化物，且二者的摩尔比为(70:30)～(90:10)，且钙钛矿结构氧化物中含有钇、锰和铬，烧绿石结构氧化物中含有钙、钛、钨和铈。其中，钙钛矿氧化物和烧绿石氧化物分别为YCr 0.5Mn 0.5O 3和CaWO 4-CeTi 2O 6；钙钛矿结构氧化物中钇锰铬 的摩尔质量比为2：1：1，烧绿石氧化物中钙钛钨铈的摩尔质量比1：1：1：2。
上述复合型热敏电阻材料的制备方法，依次包括以下步骤：
(1)称取分析纯的Y 2O 3，Mn 2O 3和Cr 2O 3混合研磨，且三者之间的摩尔质量比为2：1：1；然后在1100℃-1300℃(例如1200℃)下将研磨后的混合物煅烧1-2小时得到YCr 0.5Mn 0.5O3氧化物粉料；
(2)称取分析纯的CaCO 3，CeO 2，TiO 2和WO 3混合研磨，且四者之间的摩尔质量比为2：2：2：1；然后将研磨烘干后的粉料在950℃—1050℃(例如1000℃)下煅烧3h得到CaWO 4-CeTi 2O 6氧化物粉料；
(3)称取步骤(1)制备好的钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体，并加入PVA粘合剂使该钙钛矿氧化物粉料成颗粒状均匀分散，将均匀分散的颗粒直接在1400-1600℃下烧结1-2h；
(4)称取步骤(3)烧结后钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体，以及步骤(2)中制备好的烧绿石氧化物CaWO 4-CeTi 2O 6粉体，将二者混合研磨4-8h使其均匀，此处钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体与烧绿石氧化物CaWO 4-CeTi 2O 6粉体的摩尔比为(70:30)～(90:10)；
(5)将步骤(4)中混合研磨均匀的粉体加入PVA粘合剂，使其再次形成粒状的均匀分散颗粒，然后将均匀分散的颗粒经过模具成型后形成圆片；
(6)将成型后的圆片在1400摄氏度下烧结形成B值可调节的热敏电阻材料；
(7)将铂浆涂敷在步骤(6)中烧结好的热敏电阻材料表面，然后将其在1200℃下保温2h；
(8)将步骤(7)中所得的热敏电阻材料按照需求进行切割处理，对切割后的热敏电阻芯片焊接铂制引线。
上述复合型热敏电阻材料可用于制备复合型热敏电阻，具体方法为：将涂敷有铂的热敏电阻材料按照需求进行切割处理，然后将相应长度的铂线末端涂敷铂浆，并粘结在切割处理后的热敏电阻芯片两端，经过1200℃的高温处理后形成带有引线的高温热敏电阻。
上述复合型热敏电阻材料还可用于制备高温密质成瓷热敏电阻温度传感器。
实施例1：
(1)称取已制备好的钙钛矿氧化物YCr 0.5Mn 0.5O 3，并加入PVA粘合剂使原粉料成粒状分散均匀后，将均匀分散的粉体在1400-1600℃下烧结1-2h。
(2)称取烧结后钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体，并与制备好的烧绿石氧化物CaWO 4-CeTi 2O 6粉体以摩尔比为70：30的比例进行混合研磨4-8h使其均匀。
(3)将均匀的粉体加入粘合剂使其再次形成粒状的均匀分散粉体，经过模具成型后形成圆片。
(4)将成型后的圆片在1400-1500温度下烧结形成B值可调节的热敏电阻材料
(5)将铂浆涂敷在烧结好的热敏电阻材料表面，在1200℃下保温2h。
(6)将涂敷有铂的热敏电阻材料按照需求进行切割处理，对切割后的热敏电阻芯片焊接铂制引线。
(7)将制好的热敏电阻进行电学性能测试其室温电阻率(25℃)为2540(kΩ*cm)高温电阻率(900℃)0.0076(kΩ*cm)其B值(25-200)为4378，B值(200-800)为4797，阻温特性曲线如图1。
实施例2：
(1)称取已制备好的钙钛矿氧化物YCr 0.5Mn 0.5O 3，并加入粘合剂使原粉料成粒状分散均匀后，将均匀分散的粉体在1400-1600℃下烧结1-2h。
(2)称取烧结后钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体，并与制备好的烧绿石氧化物CaWO 4-CeTi 2O 6粉体以摩尔比为80：20的比例进行混合研磨4-8h使其均匀。
(3)将均匀的粉体加入粘合剂使其再次形成粒状的均匀分散粉体，经过模具成型后形成圆片。
(4)将成型后的圆片在1400-1500温度下烧结形成B值可调节的热敏电阻材料
(5)将铂浆涂敷在烧结好的热敏电阻材料表面，在1200℃下保温2h。
(6)将涂敷有铂的热敏电阻材料按照需求进行切割处理，对切割后的热敏电阻芯片焊接铂制引线。
(7)将制好的热敏电阻进行电学性能测试其室温电阻率(25℃)为151.62(kΩ*cm)高温电阻率(900℃)0.0048(kΩ*cm)其B值(25-200)为3798其B值(200-800)为4370阻温特性曲线如图2。
实施例3：
(1)称取已制备好的钙钛矿氧化物YCr 0.5Mn 0.5O 3，并加入粘合剂使原粉料成粒状分散均匀后，将均匀分散的粉体在1400-1600℃下烧结1-2h。
(2)称取烧结后钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体，并与制备好的烧绿石氧化物CaWO 4-CeTi 2O 6粉体以摩尔比为90：10的比例进行混合研磨4-8h使其均匀。
(3)将均匀的粉体加入粘合剂使其再次形成粒状的均匀分散粉体，经过模具成型后形成圆片。
(4).将成型后的圆片在1400-1500温度下烧结形成B值可调节的热敏电阻材料。
(5).将铂浆涂敷在烧结好的热敏电阻材料表面，在1200℃下保温2h。
(6)将涂敷有铂的热敏电阻材料按照需求进行切割处理，对切割后的热敏电阻芯片焊接铂制引线。
(7)将制好的热敏电阻进行电学性能测试其室温电阻率(25℃)为30(kΩ*cm)高温电阻率(900℃)0.0022(kΩ*cm)其B值(25-200)为3263，B值(200-800)为4135阻温特性曲线如图3。
实施例4：
(1)称取分析纯的Y 2O 3Mn 2O 3Cr 2O 3以摩尔质量比为2：1：1混合研磨后，在1200℃下煅烧1-2h得到YCr 0.5Mn 0.5O 3氧化物粉料。
(2)将步骤(1)中所得粉料烘干后加入粘合剂使其成粒状分散均匀，经过成型工艺形成圆片。
(3)将成型后的圆片在1400-1500温度下烧结形成热敏电阻。
(4)将铂浆涂敷在烧结好的热敏电阻材料表面，在1200℃下保温2h。
(5).将涂敷有铂的热敏电阻材料按照需求进行切割处理，对切割后的热敏电阻芯片焊接铂制引线。
(6)将制好的热敏电阻进行电学性能测试其室温电阻率(25℃)为21.54(kΩ*cm)高温电阻率(800℃)0.01864(kΩ*cm)其B值(25-200)为2881，B值(200-800)为3083阻温特性曲线如图4。
通过上述实施例可以看出，通过本发明获得的复合型热敏电阻材料以及复合型热敏电阻，其电学性能极其优越：室温电阻率(25℃)变化范围为2540-21.54 (kΩ*cm)，高温电阻率(900℃)变化范围为0.0076-0.0022(kΩ*cm)，其B值变化范围(25-200)为4378-2881，B值(200-800)变化范围为4797-3083。

Claims (8)

  1. 一种复合型热敏电阻材料，其特征在于：包括钙钛矿结构氧化物和烧绿石结构氧化物，且二者的摩尔比为(70:30)～(90:10)，且钙钛矿结构氧化物中含有钇、锰和铬，烧绿石结构氧化物中含有钙、钛、钨和铈。
  2. 根据权利要求1所述的复合型热敏电阻材料，其特征在于：所述钙钛矿氧化物和烧绿石氧化物分别为YCr 0.5Mn 0.5O 3和CaWO 4-CeTi 2O 6。
  3. 根据权利要求1所述的复合型热敏电阻材料，其特征在于：所述钙钛矿结构氧化物中钇锰铬的摩尔质量比为(2～2.5)：(0.8～1.2)：(0.8～1.2)，所述烧绿石氧化物中钙钛钨铈的摩尔质量比(0.8～1.2)：(0.8～1.2)：(0.8～1.2)：(2～2.5)。
  4. 根据权利要求3所述的复合型热敏电阻材料，其特征在于：所述钙钛矿结构氧化物中钇锰铬的摩尔质量比为2：1：1，所述烧绿石氧化物中钙钛钨铈的摩尔质量比1：1：1：2。
  5. 根据权利要求1至4任意一项所述的复合型热敏电阻材料的制备方法，其特征在于：依次包括以下步骤：
    (1)称取分析纯的Y 2O 3，Mn 2O 3和Cr 2O 3混合研磨，且三者之间的摩尔质量比为2：1：1；然后在1100℃-1300℃将研磨后的混合物煅烧1-2小时得到YCr 0.5Mn 0.5O3氧化物粉料；
    (2)称取分析纯的CaCO 3，CeO 2，TiO 2和WO 3混合研磨，且四者之间的摩尔质量比为2：2：2：1；然后将研磨烘干后的粉料在950℃—1050℃下煅烧3h得到CaWO 4-CeTi 2O 6氧化物粉料；
    (3)称取步骤(1)所有制备好的钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体，并加入PVA粘合剂使该钙钛矿氧化物粉料成颗粒状均匀分散，将均匀分散的颗粒直接在1400-1600℃下烧结1-2h；
    (4)称取步骤(3)烧结后钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体，以及步骤(2)中制备好的烧绿石氧化物CaWO 4-CeTi 2O 6粉体，将二者混合研磨4-8h使其均匀，此处钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体与烧绿石氧化物CaWO 4-CeTi 2O 6粉体的摩尔比为(70:30)～(90:10)；
    (5)将步骤(4)中混合研磨均匀的粉体加入PVA粘合剂，使其再次形成粒状的均匀分散颗粒，然后将均匀分散的颗粒经过模具成型后形成圆片；
    (6)将成型后的圆片在1400摄氏度下烧结形成B值可调节的热敏电阻材 料；
    (7)将铂浆涂敷在步骤(6)中烧结好的热敏电阻材料表面，然后将其在1200℃下保温2h；
    (8)将步骤(7)中所得的热敏电阻材料按照需求进行切割处理，对切割后的热敏电阻芯片焊接铂制引线。
  6. 根据权利要求5所述的复合型热敏电阻材料的制备方法，其特征在于：所述步骤(3)中，将加入PVA粘合剂后的钙钛矿氧化物YCr 0.5Mn 0.5O 3粉体经过造粒处理后，不经过模具成型直接将均匀分散的颗粒在1400-1500℃下烧结。
  7. 一种根据权利要求1至4任意一项所述的复合型热敏电阻材料的应用，其特征在于：将该复合型热敏电阻材料用于制备复合型热敏电阻，具体方法为：将相应长度的铂线末端涂敷铂浆，并将该铂线粘结在切割处理后的热敏电阻芯片两端，经过1200℃的高温处理后形成带有引线的高温热敏电阻。
  8. 一种根据权利要求1至4任意一项所述的复合型热敏电阻材料的应用，其特征在于：将该复合型热敏电阻材料用于制备高温密质成瓷热敏电阻温度传感器。
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