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 PDFInfo
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- 238000009766 low-temperature sintering Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 28
- 238000000498 ball milling Methods 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 14
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- -1 CO3O4 Inorganic materials 0.000 claims abstract description 4
- 239000005751 Copper oxide Substances 0.000 claims abstract description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 4
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 4
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000010955 niobium Substances 0.000 claims abstract description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 30
- 238000012360 testing method Methods 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000010009 beating Methods 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 3
- 238000000462 isostatic pressing Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract description 14
- 239000011787 zinc oxide Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 229960001296 zinc oxide Drugs 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 3
- 238000005520 cutting process Methods 0.000 abstract description 2
- 238000005538 encapsulation Methods 0.000 abstract 1
- 230000036632 reaction speed Effects 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- UOJLTGJDEASXFF-UHFFFAOYSA-N [Mn].[Co].[Fe] Chemical compound [Mn].[Co].[Fe] UOJLTGJDEASXFF-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 235000013409 condiments Nutrition 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 240000008415 Lactuca sativa Species 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000027648 face development Effects 0.000 description 1
- 239000010946 fine silver Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 235000012045 salad Nutrition 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 235000013555 soy sauce Nutrition 0.000 description 1
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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
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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