CN114195512A - 一种钛酸钡ptc陶瓷膜片流延浆料及其制备方法与应用 - Google Patents
一种钛酸钡ptc陶瓷膜片流延浆料及其制备方法与应用 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 69
- 239000002002 slurry Substances 0.000 title claims abstract description 53
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 38
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000010345 tape casting Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000007613 slurry method Methods 0.000 title description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000000498 ball milling Methods 0.000 claims abstract description 33
- 238000005266 casting Methods 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000005303 weighing Methods 0.000 claims abstract description 9
- 239000011230 binding agent Substances 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 6
- 239000002270 dispersing agent Substances 0.000 claims abstract description 6
- 239000004014 plasticizer Substances 0.000 claims abstract description 6
- 238000012216 screening Methods 0.000 claims abstract description 6
- 239000012528 membrane Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 24
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical group CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical group CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical group CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 4
- 239000004359 castor oil Substances 0.000 claims description 3
- 235000019438 castor oil Nutrition 0.000 claims description 3
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 14
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 abstract description 14
- 239000004677 Nylon Substances 0.000 abstract description 13
- 229920001778 nylon Polymers 0.000 abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052681 coesite Inorganic materials 0.000 abstract description 6
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 6
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000377 silicon dioxide Substances 0.000 abstract description 6
- 229910052682 stishovite Inorganic materials 0.000 abstract description 6
- 229910052905 tridymite Inorganic materials 0.000 abstract description 6
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract 1
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- 238000001354 calcination Methods 0.000 description 5
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 5
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- 238000000691 measurement method Methods 0.000 description 3
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
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- 239000007787 solid Substances 0.000 description 2
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- 229910052726 zirconium Inorganic materials 0.000 description 2
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- YPQJHZKJHIBJAP-UHFFFAOYSA-N [K].[Bi] Chemical compound [K].[Bi] YPQJHZKJHIBJAP-UHFFFAOYSA-N 0.000 description 1
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- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 description 1
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- 229910052700 potassium Inorganic materials 0.000 description 1
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- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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Abstract
本发明涉及一种钛酸钡PTC陶瓷膜片流延浆料及其制备方法与应用,将下述组分按质量比顺序称取入尼龙球磨罐:PTC陶瓷粉料100,其中PTC陶瓷粉料主要成分为摩尔组分比混合:BaCO3 80~90,Pb3O4 15~20,TiO2 100,Y2O3 0.1~0.3,Nb2O5 0.01~0.05,SiO2 0~0.15,有机溶剂15~25,分散剂0.1~0.3,消泡剂0.1~0.3,增塑剂0.3~0.8,有机粘结剂15~40;称取一定重量的氧化锆球入尼龙罐中,氧化锆球的质量:粉料质量为3:1,氧化锆球直径分别为
Description
技术领域
本发明属于电子陶瓷元件制备技术领域,尤其是涉及一种钛酸钡PTC陶瓷膜片流延浆料及其制备方法与应用。
背景技术
随着科学技术的发展,新能源汽车和智能绿色家电等新兴产业欣欣向荣,同时也对用于电路保护和智能控温加热的PTC陶瓷材料与元件提出了更高的要求。钛酸钡是应用最多,最具代表性的PTC陶瓷,被人们称为“电子陶瓷产业的支柱”。
钛酸钡PTC陶瓷的制备方法包括固相法、水热法、流延法等,传统的固相法、水热法制备钛酸钡陶瓷,存在加工困难,生产效率低,成本高等缺点。流延成型是一种制备陶瓷薄膜材料的方法,被用于制备单层或多层陶瓷材料。相对于其他陶瓷成型方法,流延法具有以下几点优点:可以制备出面积大、厚度小、表面平整光滑的陶瓷器件;操作比较简单,劳动强度相对小;材料利用率较高;材料呈二维分布,缺陷小;生产效率高,生产可连续性。通过流延法制备厚度均一、抗拉性能好、固含量高的膜片是生产高性能片式PTC陶瓷的关键。
中国专利CN109761602B公开了一种低阻热敏陶瓷材料及制备方法与应用,该热敏陶瓷材料的主要成分的化学式为((Bi0.5Q0.5)xBam-x)TiO3;其中Q为碱金属元素Na或K;其中m的取值范围为1≤m≤1.007,x的取值范围为0.001≤x≤0.007。制备方法为将钛酸铋钠或钛酸铋钾陶瓷粉末与碳酸钡粉末、二氧化钛粉混合后进行煅烧,再依次通过流延、叠片、压片和切片,得到成型生坯;将成型生坯在温度大于等于280℃条件下分解流延过程中混入的有机物,再在还原气氛中煅烧,得到陶瓷块体;再将陶瓷块体再在含氧气氛中煅烧。该专利公开的方法需要首先进行煅烧,再依次通过流延、叠片、压片和切片,得到成型生坯,然后继续煅烧,其通过成分控制,主要解决的问题是:制得的片式钛酸钡基热敏陶瓷具有极低的室温电阻率,较高的升阻比,较高的温度系数。
中国专利CN102509601B公布了一种钛酸钡PTC陶瓷的制备方法,①将下述化合物按摩尔组分比混合:BaCO3 99~101,TiO2 100,Y2O3 0.1~0.5,SiO2 0~0.01;②进行高能超细球磨,获得粒径500nm以下的粉体混合物;③将所得浆料进行烘干、预烧处理,合成均匀微量掺杂的钛酸钡粉体;④将所得粉体配制成流延浆料,流延出生坯膜片;⑤层压并印刷Ni内电极,制作成叠层片式结构;⑥切割成含有内电极的器件;⑦在还原气氛中烧结,然后在空气中进行再氧化,获得所需的叠层片式陶瓷电阻。该专利采用较高的预烧温度和较低的烧结温度,制备出的陶瓷粒径细小均匀,易于在较低的温度下再氧化,所制备的半导体陶瓷的瓷体晶粒大小可以达到2.0μm以下,室温电阻率在1~200Ω.cm之间,叠层器件升阻比达103以上。
如上所述,现有技术中存在结合流延方法来制备钛酸钡PTC陶瓷的技术,但是这些现有技术在得到流延浆料以前都需要进行煅烧或预烧程序,而且这些现有技术强调的主要是电阻性能。
而如何实现流延出的膜片厚度均一、抗拉性能好、固含量高,现有技术中并没有给出需要配置怎样的流延浆料。
发明内容
本发明的目的在于提供一种钛酸钡PTC陶瓷膜片流延浆料及其制备方法与应用。通过调整流延浆料的配比,达到合适的粘度、流动性、分散性,进而得到膜片拉力、膜片拉伸量、膜片厚度综合性能优化的PTC陶瓷膜片。
本发明的目的可以通过以下技术方案来实现:
本发明提供一种钛酸钡PTC陶瓷膜片流延浆料的制备方法,包括以下步骤:
1)将粉料加入球磨罐,所述粉料由以下质量份的组分组成:PTC陶瓷粉料100,有机溶剂15~25,分散剂0.1~0.3,消泡剂0.1~0.3,增塑剂0.3~0.8,有机粘结剂15~40;
2)称取氧化锆球入球磨罐,中,氧化锆球的质量与粉料质量为3:1,所述氧化锆球采用三种不同直径大小球体的混合物;
3)将配好料的球磨罐放入球磨机球磨24~48h;
4)将球磨好的浆料过筛后倒入真空搅拌桶中,真空搅拌得到用于制备钛酸钡PTC陶瓷膜片的流延浆料,倒入流延机流延得到PTC陶瓷膜片。
在本发明的一个实施方式中,步骤1)中,所述PTC陶瓷粉料由以下摩尔用量的组分组成:BaCO3 80~90,Pb3O415~20,TiO2 100,Y2O3 0.1~0.3,Nb2O50.01~0.05,SiO2 0~0.15。
在本发明的一个实施方式中,步骤1)中,所述有机溶剂选择甲苯、乙醇或异丙醇中的一种或几种。有机溶剂主要用于溶解组分,使粉体和其他添加剂均匀化,同时可以快速挥发。
在本发明的一个实施方式中,步骤1)中,所述分散剂选择磷酸三丁酯或蓖麻油。分散剂用于分散颗粒,保持浆料颗粒均匀悬浮性。
在本发明的一个实施方式中,步骤1)中,所述消泡剂选择正丁醇或乙二醇。消泡剂用于抑制浆料中气泡的产生。
在本发明的一个实施方式中,步骤1)中,所述增塑剂为邻苯二甲酸二丁酯或二苯甲酸酯。增塑剂用于软化粘结剂聚合物链,充当润滑剂的作用。
在本发明的一个实施方式中,步骤1)中,所述有机粘结剂为PVB或聚甲基丙烯酸甲酯。有机粘结剂15~40用于粉体颗粒的聚合,为膜片提供柔韧性、成型性和易加工性。
在本发明的一个实施方式中,步骤1)、2)中,所述球磨罐采用尼龙球磨罐。
在本发明的一个实施方式中,步骤2)中,所述氧化锆球采用三种不同直径大小分别为和球体的混合物,3种直径的氧化锆球质量比为1:1:1。本发明中采用不同级配比的直径的锆球球磨,不仅可以使浆料混合均匀,而且通过小直径的锆球能充分研磨,大大减少浆料中小团聚的出现,提高研磨效率。
在本发明的一个实施方式中,在步骤3)进行球磨时,球磨的具体时间可以依据配料的量决定,配料越多,相应球磨时间越长。
在本发明的一个实施方式中,步骤4)中,真空搅拌的条件为:抽真空并且搅拌30min。
本发明通过调整有机溶剂、有机粘合剂的选择以及用量,制备得到膜片拉力大于4N/4cm,膜片拉伸量>15%及膜片厚度精度为±3μm之内的PTC陶瓷膜片。
本发明还提供基于上述方法制备得到的一种钛酸钡PTC陶瓷膜片流延浆料。
本发明还提供基于上述方法制备得到的钛酸钡PTC陶瓷膜片流延浆料的应用,所述钛酸钡PTC陶瓷膜片流延浆料用于制备得到钛酸钡PTC陶瓷膜片。
与现有技术相比,本发明具有以下优点及有益效果:
1.基于本发明钛酸钡PTC陶瓷膜片流延浆料,粉料分布均匀,无团聚,粘度适中,成型性能好,制备得到的钛酸钡PTC陶瓷膜片致密性好,孔隙率低,平整度好,厚度均一性好,无分层无开裂,抗拉性能好。
2.本发明提供的流延浆料配置方法,实用性强,可操作性高,可用于多种陶瓷粉料的流延浆料配置。
总之,基于本发明方法制备的PTC陶瓷膜片,采用拉伸测试仪,测得膜片拉力大于5N/4cm,膜片拉伸量>15%;采用五点测厚法测得不同位置膜片厚度相差在±3μm之内,因此,基于本发明方法制备出的膜片厚度均一性好。
具体实施方式
下面结合具体实施例对本发明进行详细说明。
实施例1
1)将下述组分按质量比顺序称取入尼龙球磨罐:PTC陶瓷粉料1000g,其中PTC陶瓷粉料主要成分为摩尔组分比混合:BaCO3 85,Pb3O415,TiO2 100,Y2O3 0.15,Nb2O50.02,SiO20.1,甲苯100g,乙醇100g,蓖麻油2g,乙二醇3g,邻苯二甲酸二丁6g,PVB(聚乙烯醇缩丁醛)300g;
3)将配好料的尼龙球磨罐放入球磨机球磨24h;
4)将球磨好的浆料过筛后倒入真空搅拌桶中,抽真空并且搅拌30min得到用于制备钛酸钡PTC陶瓷膜片流延浆料,倒入流延机流延得到PTC陶瓷膜片。
5)采用拉伸测试仪,测得膜片拉力为5.6N/4CM,拉伸率为18%;采用五点测厚法,测得膜片平均厚度为45μm。
实施例2
1)将下述组分按质量比顺序称取入尼龙球磨罐:PTC陶瓷粉料1000g,其中PTC陶瓷粉料主要成分为摩尔组分比混合:BaCO3 85,Pb3O415,TiO2 100,Y2O3 0.15,Nb2O50.02,SiO20.1,甲苯100g,乙醇60g,异丙醇40g,磷酸三丁酯2g,正丁醇2g,二苯甲酸酯6g,聚甲基丙烯酸甲酯250g;
3)将配好料的尼龙球磨罐放入球磨机球磨24h;
4)将球磨好的浆料过筛后倒入真空搅拌桶中,抽真空并且搅拌30min得到用于制备钛酸钡PTC陶瓷膜片流延浆料,倒入流延机流延得到PTC陶瓷膜片。
实施例3
1)将下述组分按质量比顺序称取入尼龙球磨罐:PTC陶瓷粉料1000g,其中PTC陶瓷粉料主要成分为摩尔组分比混合:BaCO3 85,Pb3O415,TiO2 100,Y2O3 0.15,Nb2O50.02,SiO20.1,甲苯100g,乙醇75g,异丙醇25g,磷酸三丁酯2g,乙二醇2g,邻苯二甲酸二丁酯5g,PVB(聚乙烯醇缩丁醛)250g;
3)将配好料的尼龙球磨罐放入球磨机球磨24h;
4)将球磨好的浆料过筛后倒入真空搅拌桶中,抽真空并且搅拌30min得到用于制备钛酸钡PTC陶瓷膜片流延浆料,倒入流延机流延得到PTC陶瓷膜片。
以上实施例中,采用拉伸测试仪测量膜片拉力以及拉伸率的方法为参照拉伸测试仪说明书进行。
以上实施例中,采用五点测厚法的方法为:在膜片的四角处以及中心处,一共5个位置,使用三丰/Mitutoyo ABSLOUTE数显指示表,分别测量这5个不同位置处膜片的厚度,然后取这5点不同位置处膜片的厚度的平均值,作为膜片的平均厚度。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和使用发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改,并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此,本发明不限于上述实施例,本领域技术人员根据本发明的揭示,不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。
Claims (10)
1.一种钛酸钡PTC陶瓷膜片流延浆料的制备方法,其特征在于,包括以下步骤:
1)将粉料加入球磨罐,所述粉料由以下质量份的组分组成:PTC陶瓷粉料100,有机溶剂15~25,分散剂0.1~0.3,消泡剂0.1~0.3,增塑剂0.3~0.8,有机粘结剂15~40;
2)称取氧化锆球入球磨罐,中,氧化锆球的质量与粉料质量为3:1,所述氧化锆球采用三种不同直径大小球体的混合物;
3)将配好料的球磨罐放入球磨机球磨24~48h;
4)将球磨好的浆料过筛后倒入真空搅拌桶中,真空搅拌得到用于制备钛酸钡PTC陶瓷膜片的流延浆料。
2.根据权利要求1所述的一种钛酸钡PTC陶瓷膜片流延浆料的制备方法,其特征在于,步骤1)中,所述有机溶剂选择甲苯、乙醇或异丙醇中的一种或几种。
3.根据权利要求1所述的一种钛酸钡PTC陶瓷膜片流延浆料的制备方法,其特征在于,步骤1)中,所述分散剂选择磷酸三丁酯或蓖麻油。
4.根据权利要求1所述的一种钛酸钡PTC陶瓷膜片流延浆料的制备方法,其特征在于,步骤1)中,所述消泡剂选择正丁醇或乙二醇。
5.根据权利要求1所述的一种钛酸钡PTC陶瓷膜片流延浆料的制备方法,其特征在于,步骤1)中,所述增塑剂为邻苯二甲酸二丁酯或二苯甲酸酯。
6.根据权利要求1所述的一种钛酸钡PTC陶瓷膜片流延浆料的制备方法,其特征在于,步骤1)中,所述有机粘结剂为PVB或聚甲基丙烯酸甲酯。
8.根据权利要求1所述的一种钛酸钡PTC陶瓷膜片流延浆料的制备方法,其特征在于,步骤4)中,真空搅拌的条件为:抽真空并且搅拌30min。
9.基于权利要求1-8中任一项所述方法制备得到的一种钛酸钡PTC陶瓷膜片流延浆料。
10.权利要求9所述钛酸钡PTC陶瓷膜片流延浆料的应用,其特征在于,所述钛酸钡PTC陶瓷膜片流延浆料用于制备得到钛酸钡PTC陶瓷膜片。
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