CN106169386B - 用于制备含镀Ag CNTs的电触头材料的方法 - Google Patents

用于制备含镀Ag CNTs的电触头材料的方法 Download PDF

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CN106169386B
CN106169386B CN201610340703.8A CN201610340703A CN106169386B CN 106169386 B CN106169386 B CN 106169386B CN 201610340703 A CN201610340703 A CN 201610340703A CN 106169386 B CN106169386 B CN 106169386B
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carbon nanotube
solution
electrical contact
contact material
mixed
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CN106169386A (zh
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赵昱东
文喆东
崔贤贞
金元泳
白承铉
李东穆
沈正贤
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LS Electric Co Ltd
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Abstract

当制备电触头材料时，本发明通过在碳纳米管中包含银以抑制碳纳米管的团聚而具有在材料中均匀分散碳纳米管的效果。

Description

用于制备含镀Ag CNTs的电触头材料的方法
技术领域
本发明涉及一种用于制备含镀Ag碳纳米管(CNTs)的电触头材料的方法，更特别地，涉及一种用于制备含镀Ag CNTs的电触头材料的方法，其使所述材料具有优异的性能同时降低银的含量。
背景技术
一般情况下，电触头材料是在电气设备中当电路开启或关闭时在接触部分使用的用于电传导的接触元件例如断路器或转换器，并被应用于电动开关、互换机、MCB、小型发动机和灯具、汽车、家用电器等。
此外，电触头材料要求多种性能，例如高熔点、优异的导电性和导热性、低接触电阻、优异的抗熔焊性、平稳地开和关、与耐磨性相关的高硬度和在接触表面中小的变形。
电触头材料可被分为用于低电流(1A或更低)的触头材料、用于中度电流(1A至600A)的触头材料和用于高电流(600A或更高)的触头材料。
一般而言，具有优异导电性的材料被用作用于低电流的电触头材料，具有优异导电性、高耐磨性、高熔点等的材料被用作用于中度电流的电触头材料，并且具有高熔点的材料被用作用于高电流的电触头材料。
进一步地，电触头材料也可被分为钨基电触头材料、银氧化物基电触头材料和贵金属基电触头材料。
在它们当中，如图1所示，当使用银镍合金制备电触头材料时，当银镍基电触头材料用于低电流和中度电流时，目前已使用含量约为8wt％或更高的银。
最近，已提出通过将碳基化合物添加至金属中来制备电触头材料以改善电触头材料的耐磨性、电性能等，且中国专利号102324335、001624175和001256450已公开了包括Ag粉末和碳纳米管的电触头材料。
然而，如上所述的相关领域中的电触头材料包括CNTs以改善电触头材料的电特性，但仍具有高含量的银(Ag)，因此存在制备成本增加和制备过程复杂的问题。
发明内容
因此，详细描述的一个方面是提供一种用于制备包括镀Ag碳纳米管的电触头材料的方法，其使所述材料具有优异的性能同时降低银的含量。
为实现这些或其他优势且根据本说明书的目的，正如本文所呈现和广泛描述的，提供一种制备包括镀Ag碳纳米管的电触头材料的方法，所述方法包括：(a)将碳纳米管放入硝酸银溶液中并使碳纳米管经受超声分散和酸处理；(b)洗涤在步骤(a)中经受超声分散和酸处理的碳纳米管；(c)通过随后将洗涤后的碳纳米管与氯化锡与盐酸的混合溶液和氯化钯与盐酸的混合溶液混合，然后各自对其应用超声波，使锡和钯与碳纳米管的表面结合；(d)将水性硝酸银溶液和水性氨溶液放入容器中并混合所形成的溶液直至溶液变为无色，然后将步骤(c)中制备的碳纳米管与所述溶液混合；(e)通过将水性乙醛酸溶液与水性氢氧化钠溶液混合，然后用去离子水洗涤所形成的纳米管来制备镀Ag碳纳米管；和(f)通过将镀Ag碳纳米管与其中金属被混合的合金混合制备粉末混合物。
此外，在步骤(f)中构成与碳纳米管混合的合金的金属的特征是具有14.3MS/m或更高的电导率。
此外，所述合金由选自由铜、镍和金组成的组中的一种或多种金属组成。
此外，所述方法在步骤(f)后进一步包括：使所述粉末混合物经受超声分散，并真空干燥所述粉末混合物；和(h)烧结所述真空干燥的粉末混合物。
此外，步骤(b)的特征在于所述碳纳米管被洗涤直至达到pH 7。
此外，步骤(e)的特征在于所述水性乙醛酸溶液与水性氢氧化钠溶液被混合直至达到pH 9。
此外，所述水性乙醛酸溶液与水性氢氧化钠溶液的特征为被去离子水洗涤直至达到pH 7。
此外，步骤(a)的特征在于所述碳纳米管经受超声分散5分钟并经受酸处理2小时。
此外，步骤(e)的特征在于当所述溶液混合时，所述水性乙醛酸溶液与水性氢氧化钠溶液在90℃下彼此反应1小时。
此外，步骤(h)的特征在于通过放电等离子烧结法实施。
为实现这些或其他优势且根据本发明的目的，正如本文呈现和广泛描述的，也提供一种制备包括镀Ag碳纳米管的电触头材料的方法，所述方法包括：(a)使碳纳米管经受超声分散和酸处理，然后将锡和钯与碳纳米管的表面结合；(b)将水性乙醛酸溶液与水性氢氧化钠溶液混合，然后将在步骤(a)中制备的碳纳米管与所述溶液混合；和(c)通过将水性乙醛酸溶液与水性氢氧化钠溶液混合制备镀Ag碳纳米管，然后通过将所述镀Ag碳纳米管与其中金属被混合的合金混合制备粉末混合物。
此外，在步骤(c)中构成与碳纳米管混合的合金的金属的特征是具有14.3MS/m或更高的电导率。
此外，所述合金由选自由铜、镍和金组成的组中的一种或多种金属组成。
此外，所述方法在步骤(c)后进一步包括：(d)使所述粉末混合物经受超声分散，并真空干燥所述粉末混合物；和(e)烧结所述真空干燥的粉末混合物。
如上所述，本发明的制备包括镀Ag碳纳米管的电触头材料的方法具有如下效果：当制备所述电触头材料时，通过在碳纳米管中包括Ag以抑制碳纳米管的团聚而使碳纳米管在材料中均匀分散。
此外，具有通过降低用于电触头材料的Ag的含量而降低总体制备成本的效果。
此外，当在碳纳米管中使用少量的Ag时，通过使电触头材料具有优异的性能，具有显著改善其中使用电触头材料的断路器等的功能的效果。
从下文给出的详细描述中本发明的进一步应用范围将变得更加明显。然而，应理解的是尽管指出了本发明的优选实施方案，所述详细描述和具体实施例仅以示例性方式给出，因为在本发明的精神和范围内的各种改变和修饰将从详细描述中对于本领域技术人员变得明显。
附图说明
被包括以提供本发明的进一步理解且被并入和构成本说明书的一部分的附图示出了示例性实施方案并连同描述用来解释本发明的原则。
在附图中：
图1是示出在相关领域中的银-镍基电触头材料的构型视图；
图2是示出其中根据本发明的电触头材料包括镀Ag碳纳米管的状态的构型视图；
图3是示出包括在根据本发明的电触头中的碳纳米管的SEM图；
图4是示出包括在根据本发明的电触头中的镀Ag碳纳米管的SEM图；
图5是示出包括在根据本发明的电触头中的镀Ag碳纳米管的SEM图；
图6是示出包括在根据本发明的电触头中的镀Ag碳纳米管的TEM图；
图7是包括在根据本发明的电触头中的镀Ag碳纳米管的EDS分析；
图8是示出制备根据本发明的电触头材料的过程的流程图；和
图9是示出制备根据本发明的镀Ag碳纳米管的过程的流程图。
具体实施方式
在下文中，将参考附图详细描述根据本发明的一个示例性实施方案的用于制备包括镀Ag碳纳米管的电触头材料的方法。
图2是示出其中根据本发明的电触头材料包括镀Ag碳纳米管的状态的构型视图，图3是示出包括在根据本发明的电触头中的碳纳米管的SEM图，图4是示出包括在根据本发明的电触头中的镀Ag碳纳米管的SEM图，和图5是示出包括在根据本发明的电触头中的镀Ag碳纳米管的SEM图。
此外，图6是示出包括在根据本发明的电触头中的镀Ag碳纳米管的TEM图，图7是包括在根据本发明的电触头中的镀Ag碳纳米管的EDS分析，图8是示出制备根据本发明的电触头材料的过程的流程图，和图9是示出制备根据本发明的镀Ag碳纳米管的过程的流程图。
如在图2中所示，由根据本发明的方法制备的电触头材料包括镀Ag碳纳米管10。
在该情况下，组成所述电触头材料以包括一种或多种选自由银(Ag)、铜(Cu)、镍(Ni)和金(Au)组成的组中的金属，所述银(Ag)、铜(Cu)、镍(Ni)和金(Au)可提高电触头材料的密度、电导率、硬度、热导率、伸长率和电寿命，所述电触头材料将在下面通过使用电导率分别为63MS/m、59MS/m、14.3MS/m和45.2MS/m或更高的那些进行描述。
银(Ag)具有优异的导电性和导热性和低接触电阻，因此经常用作电触头材料的基础材料，镍(Ni)具有比银(Ag)更低的导电性和导热性但具有高的机械强度，因此与银(Ag)一起作为电触头材料。
在该情况下，优选所述金属颗粒的尺寸为1μm-10μm。
此外，在银-镍基合金中银(Ag)的含量不特别限定，但优选为55wt％-65wt％。当所述含量小于55wt％时，所述银-镍基合金由于低导电性不可用作电触头材料，且当所述含量高于65wt％时，耐磨性和耐耗性劣化且制备成本显著增加。
相应地，镍(Ni)的含量优选为35wt％-45wt％。
碳纳米管(CNT)是一种新材料，其中碳原子通过sp2彼此连接键合形成六边形蜂窝结构并具有管状形状，且CNT的直径大约在数个至数十个纳米(nm)的范围内。
CNT具有优异的电性能、机械性能和热性能，并因此可被用作复合材料的增强材料，并作为电桥，并因此可提高电触头材料的电性能和机械性能。
尽管上面的优点，当与金属键合时CNT具有一些问题，包括难以分散等。
即，当碳纳米管(CNTs)用在电触头材料中时，由于碳纳米管之间的团聚存在在所述材料中难以均匀分散碳纳米管的问题，且存在不均匀性的分散影响材料性能的问题。
因此，本发明通过使用镀银(Ag)碳纳米管制备所述材料允许碳纳米管均匀分散在电触头材料中。
即，如图2中所示，当使用镀银(Ag)碳纳米管时，碳纳米管均匀分散在材料间的界面处，并因此提高了在电接头处所需的导热性和耐磨性。
如在图3-7中所示，通过使用投射电子显微镜(TEM)或扫描电子显微镜(SEM)证实碳纳米管(CNT)或包括银(Ag)的碳纳米管的状态，且如在图7中所示，当检测各组分时清楚显示强度。
下文中，将参考图8和9详细描述制备镀Ag碳纳米管的方法。
首先，通过将镀Ag碳纳米管与包括银和镍的合金混合制备粉末混合物(S101)。
在该情况下，对于镀Ag碳纳米管，0.04g的碳纳米管被放入7M硝酸银溶液中，并分别经受超声分散和和酸处理5分钟和2小时(S201)。
此后，通过使用真空过滤用去离子水洗涤通过步骤(S201)超声分散和酸处理的碳纳米管直至达到pH 7(S203)。
此后，通过步骤(S203)洗涤的碳纳米管依次与氯化锡(SnCl2)与盐酸(HCl)的混合溶液和氯化钯(PdCl2)与盐酸(HCl)的混合溶液混合，并对其应用超声波，从而使锡(Sn2+)和钯(Pd2+)与碳纳米管的表面结合(S205)。
此后，将0.3M的水性硝酸银(AgNO3)溶液和水性氨溶液放入容器中并混合直至溶液变为无色，然后与步骤(S205)中制备的碳纳米管混合(S207)。
此后，将0.1M水性乙醛酸溶液与0.5M水性氢氧化钠(NaOH)溶液混合直至达到pH9，然后使混合的溶液在90℃下反应1小时，然后使用真空过滤以用去离子水洗涤所述碳纳米管直至达到pH 7，从而制备镀Ag碳纳米管(S209)。
此后，将所述镀Ag碳纳米管与合金混合，从而制备粉末混合物(S211)。
此后，使在步骤(S211)中制备的粉末混合物经受超声分散和真空干燥(S103)，然后烧结所述真空干燥的粉末混合物(S105)。
在该情况下，在750-830℃的温度下烧结所述粉末混合物1分钟并维持该温度，且作为烧结方法，使用放电等离子烧结(SPS)法。
所述放电等离子烧结法是当在石墨模具中被压时，通过对原料颗粒直接应用脉冲电流使用在原料颗粒间产生的放电等离子体作为主要热源的烧结方法。
通过所述方法，高能量的放电等离子体可被有效应用于热扩散、电场的作用等。
此外，由于通过放电等离子烧结法在相对低的温度下短的时间内温度可能突然增加，颗粒的生长可被控制，短的时间内可得到致密的复合物，且甚至可轻易烧结难以烧结的材料(难烧结材料)。
<实验实施例>
[表]
如在表中所示，显示了在根据本发明的方法制备的包括镀Ag碳纳米管的电触头材料中，密度、电导率、电寿命等显著提高。
因此，在本发明中，当制备电触头材料时，通过在碳纳米管中包括Ag以抑制碳纳米管的团聚，碳纳米管均匀分散在材料中。
此外，通过降低在电触头材料中使用的Ag的含量降低总制备成本。
此外，当在碳纳米管中使用少量的Ag时，通过使电触头材料具有优异的性能，显著改善了其中使用电触头材料的断路器等的功能。
由于本发明的特征可体现为多种形式而不偏离其特征，应理解的是上述实施方案不被任何前面描述的细节限制，除非另有说明，更确切地说应在权利要求中限定的范围内广泛解释，因此权利要求旨在包含落在权利要求的公认范围内的所有改变和修饰或这样的公认范围的等同物。

Claims (8)

1.一种用于制备含镀Ag碳纳米管的电触头材料的方法，其特征在于，所述方法包含：
(a)将碳纳米管放入硝酸银溶液中并使碳纳米管经受超声分散和酸处理；
(b)洗涤在步骤(a)中经受超声分散和酸处理的碳纳米管；
(c)通过随后将洗涤后的碳纳米管与氯化锡与盐酸的混合溶液和氯化钯与盐酸的混合溶液混合，然后各自对其应用超声波，使锡和钯与碳纳米管的表面结合；
(d)将水性硝酸银溶液和水性氨溶液放入容器中并混合所形成的溶液直至溶液变为无色，然后将步骤(c)中制备的碳纳米管与所述溶液混合；
(e)通过将水性乙醛酸溶液和水性氢氧化钠溶液混合直至达到pH 9和使混合溶液在90℃下反应1小时，然后用去离子水洗涤所形成的纳米管来制备镀Ag碳纳米管；和
(f)通过将镀Ag碳纳米管与其中金属被混合的合金混合制备粉末混合物；
其中，
金属颗粒的尺寸为1μm-10μm；
合金中银(Ag)的含量为55wt％-65wt％；
合金中镍(Ni)的含量为35wt％-45wt％。
2.根据权利要求1所述的方法，其中在步骤(f)中构成与碳纳米管混合的合金的金属具有14.3MS/m或更高的电导率。
3.根据权利要求1所述的方法，其中所述合金由选自由铜、镍和金组成的组中的一种或多种金属组成。
4.根据权利要求1所述的方法，其进一步包含：
(g)使所述粉末混合物经受超声分散，并真空干燥所述粉末混合物；和
(h)烧结所述真空干燥的粉末混合物。
5.根据权利要求1所述的方法，其中在步骤(b)中，所述碳纳米管被洗涤直至达到pH 7。
6.根据权利要求1所述的方法，其中在步骤(e)中，所述水性乙醛酸溶液与水性氢氧化钠溶液被去离子水洗涤直至达到pH 7。
7.根据权利要求1所述的方法，其中在步骤(a)中，所述碳纳米管经受超声分散5分钟并经受酸处理2小时。
8.根据权利要求4所述的方法，其中通过放电等离子烧结法实施步骤(h)。
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