CN111097904B - 保留镍粉各向异性的银镍电接触材料及其制备方法 - Google Patents
保留镍粉各向异性的银镍电接触材料及其制备方法 Download PDFInfo
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- MOFOBJHOKRNACT-UHFFFAOYSA-N nickel silver Chemical compound [Ni].[Ag] MOFOBJHOKRNACT-UHFFFAOYSA-N 0.000 title claims abstract description 34
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- 229910000831 Steel Inorganic materials 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- ASMQPJTXPYCZBL-UHFFFAOYSA-N [O-2].[Cd+2].[Ag+] Chemical compound [O-2].[Cd+2].[Ag+] ASMQPJTXPYCZBL-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种保留镍粉各向异性的银镍电接触材料及其制备方法，其步骤包括单晶镍粉、银粉、添加物、粘结剂的3D喷头式粉末成型打印、保留镍粉各向异性、微波烧结致密化、后处理，最终获得各向异性电磁性能的AgNi材料。该材料通过电磁场的作用快速熄灭电弧，提高了触点材料在密封高温条件下的抗熔焊性能，且生产工序少，生产过程简单、流程短、易于批量生产。
Description
技术领域
本发明涉及电工触头材料领域，具体是指一种保留镍粉各向异性的银镍电接触材料及其制备方法。
背景技术
银镍电接触材料具有优良的抗熔焊性能、加工性能，被认为是银氧化镉最理想的替代材料之一，广泛应用于低压开关装置及继电器中。但是在密封、高温环境条件下，继电器内部热量无法散失，触点温度高、导致触点表面析出银包发生粘连现象。通过改善银镍材料抗熔焊性是改善该问题的一种重要途径。
现有技术中，银镍材料抗熔焊性的改善方法包括纤维增强、添加其它添加剂、组织均匀化、电沉积技术等，通过相关文献，检索到的相关专利如下：
(1)专利CN109306439A，一种纤维增强型银镍材料的制备方法，该技术方案中粉体中加入了微量元素，起到固溶强化的作用，材料更加耐磨，有利于改善材料的电气性能；经过多次的压型、烧结、挤压和拉拔进行多次的大塑性变形，镍质点在银基体中分散得非常均匀，纤维化程度非常高且整齐，采用此种方法制备出来的材料加工性能与电气性能均具有优良的性能；
(2)专利CN109207877A，一种银镍基电触头材料及其制备方法，该技术方案中通过在银粉中加入镍粉、石墨烯、钢纤维、碳化钽、金刚石微粉、氮化钛、氮化钒、勃姆石粉，在保证导电率的同时，不仅提高了材料的硬度，还提高了抗熔焊性和抗氧化性；
(3)专利CN107475552A，一种银镍合金材料的制备方法；该技术方案中不会引入诸如Na等杂质金属元素；
(4)专利CN108425137A，一种电沉积制备银镍合金电触头的方法，该技术方案使用了有机物作基础液进行电沉积，在环保方面也有提高，并且该方法消除了传统水溶剂在电镀时产生氢脆的现象。
然而上述文献中AgNi材料后续均通过挤压的方法制备AgNi材料，消除了Ni粉的各向异性特性，且均未涉及AgNi触点材料在密封、高温条件下抗熔焊性能的提高。因此有必要对此进行改进。
另一方面，3D打印技术出现在20世纪80年代，又被称作“快速成型技术”。其最大的优点是无需机械加工或磨具，就能直接从计算机设计出的图形数据中生成任何物体，从而极大地缩短产品的研发周期，提高生产率和降低生产成本。因此被广泛地应用在艺术界和工业界。3D打印技术，根据其成型方法的不同，可用于直接制造金属功能零件的主要金属3D打印工艺有：包括选择性激光烧结(Selective Laser Sintering，SLS)技术、直接金属粉末激光烧结(Direct Metal Laser Sintering，DMLS)、选择性激光熔化(Selective LaserMelting，SLM)技术、激光近净成形(Laser Engineered Net Shaping，LENS)技术和电子束选择性熔化(Electron Beam Selective Melting，EBSM)技术、喷头式粉末成型打印技术等。
发明内容
为解决现有技术存在的问题和不足，本发明的目的是提供一种保留镍粉各向异性的银镍电接触材料及其制备方法，本发明通过采用各向异性的单晶Ni粉，并配合3D打印技术，发挥镍粉的各向异性电磁性能，在密封高温条件下通过电磁场的作用快速熄灭电弧，从而大大降低触点表面的温度，减少银包现象的发生，从而提高触点在密封、高温条件下的抗熔焊性能。
为实现上述目的，本发明的第一个方面是提供一种保留镍粉各向异性的银镍电接触材料的制备方法，其包括有以下步骤：
(1)将银粉、单晶镍粉、粘结剂与添加物在3D喷头式粉末成型打印设备进行打印，形成银镍电触头坯件，该银镍电触头坯件中的单晶镍粉保留镍粉的各向异性特性；
(2)将步骤(1)的银镍电触头坯件在保护气氛或真空条件下通过微波方式进行烧结致密化处理，烧结后的银镍电触头坯件中的单晶镍粉保留镍粉的各向异性特性；微波烧结具有热效率高、加热均匀性优异、加热速度快等一系列特点，并配合步进加热方式，本发明人发现可以保留单晶镍粉的各向异性。
(3)将经步骤(2)处理的银镍电触头坯件进行清洗抛光和干燥处理获得成品。
进一步设置是所述步骤(1)中的银粉粒度分布范围为50-100微米、平均粒度60-90微、纯度≥99.99％，单晶镍粉粒度范围3-20微米、平均粒度5-18微米、纯度≥99.9％，粘结剂为用于粉体粘结的高分子材料，其平均粒度为3-10微米，添加物为碳氮化钛、碳氮化锆、碳氮化铪、碳氮化钒、碳氮化铌、碳氮化钽、碳氮化铬的一种或多种，其粒度范围3-20微米、平均粒度5-18微米、纯度≥99.9％。
进一步设置是所述步骤(1)中Ag、Ni、添加物的重量份数比为(50-92)：(7-49.9)：(0.1-1)。
进一步设置是步骤(1)中梯度分布打印具体为：将Ag粉、Ni粉、添加物、粘结剂置于3D打印设备。
进一步设置是所打印的银镍电触头坯件形状为铆钉型、片型或异型。
进一步设置是所述步骤(2)中的微波烧结温度为100-900℃、步进温度为50-100℃、每步保温10min。
进一步设置是所述步骤(3)中清洗、抛光、干燥工序是在惰性气体保护下进行。
本发明还提供一种通过上述制备方法所制备的保留镍粉各向异性的单晶银镍电接触材料。
本发明的优点是：
(1)传统的AgNi材料普遍采用原材料混合(或化学)→等静压压锭→挤压→拉拔、退火(或轧制、退火)→制打(或冲制)→后处理→成品获得最终铆钉、片材、型材产品。而在本发明中引入了3D打印技术，工艺步骤为原材料3D打印→致密化→后处理→成品，生产工序少，生产过程简单、流程短、易于批量生产。
(2)通过本发明工艺使得制备的银镍触头材料中的单晶镍粉的各向异性得到保留，从而使得该触头材料在应用于电气产品时，该各向异性电磁性能在密封高温条件下能快速熄灭电弧，从而提高触点在密封、高温条件下的抗熔焊性能。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性的前提下，根据这些附图获得其他的附图仍属于本发明的范畴。
图1本发明的工艺流程图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚，下面将结合附图对本发明作进一步地详细描述。
实施例一：
(1)银粉、镍粉、添加物含量分别为92、7、1％，平均粒度分别为60、5、5微米，添加物为碳氮化钛、碳氮化铪、碳氮化铌、碳氮化钽、碳氮化铬，含量分别为0.1、0.5、0.1、0.1、0.1％。将Ag粉、Ni粉、添加物、粘结剂置于3D喷头式粉末成型打印设备进行打印，样坯的规格为R4×1+2×1SR10；
(2)将坯体置于微波烧结炉中，氮气气体保护，初始温度100℃，终了温度900℃，步进温度50℃、每步保温10min。
(3)进行后处理，包括清洗、抛光、干燥工序。坯体先在六角滚桶、介质为去离子水进行清洗，清洗时间10min，然后在加入抛光剂，抛光时间10min，最后采用微波加热烘干，温度120℃，时间20min，保护气氛为氩气。烘干处理后即获得成品。
实施例二：
(1)银粉、镍粉、添加物含量分别为80、19.3、0.7％，平均粒度分别为70、9、8微米，添加物为碳氮化锆、碳氮化钒、碳氮化铬，含量分别为0.1、0.4、0.2％。将Ag粉、Ni粉、添加物、粘结剂置于3D喷头式粉末成型打印设备进行打印，样坯的规格为R4×1+2×1SR10；
(2)将坯体置于微波烧结炉中，氩气保护，初始温度100℃，终了温度800℃，步进温度100℃、每步保温10min。
(3)进行后处理，包括清洗、抛光、干燥工序。坯体先在六角滚桶、介质为去离子水进行清洗，清洗时间10min，然后在加入抛光剂，抛光时间10min，最后采用微波加热烘干，温度120℃，时间20min，保护气氛为氮气。烘干处理后即获得成品。
实施例三：
(1)银粉、镍粉、添加物含量分别为65、34.6、0.4％，平均粒度分别为80、13、12微米，添加物为碳氮化锆、碳氮化钽，含量分别为0.3、0.1％。将Ag粉、Ni粉、添加物、粘结剂3D喷头式粉末成型打印设备进行打印，样坯的规格为R4×1+2×1SR10；
(2)将坯体置于微波烧结炉中，惰性气体保护，初始温度100℃，终了温度850℃，步进温度50℃、每步保温10min。
(3)进行后处理，包括清洗、抛光、干燥工序。坯体先在六角滚桶、介质为去离子水进行清洗，清洗时间10min，然后在加入抛光剂，抛光时间10min，最后采用微波加热烘干，温度120℃，时间20min，保护气氛为氩气。烘干处理后即获得成品。
实施例四：
(1)银粉、镍粉、添加物含量分别为50、49.9、0.1％，平均粒度分别为90、18、18微米，添加物为碳氮化钛，含量分别为0.1％。将Ag粉、Ni粉、添加物、粘结剂置于3D打印设备，3D喷头式粉末成型打印设备进行打印，样坯的规格为R4×1+2×1SR10；
(2)将坯体置于微波烧结炉中，惰性气体保护，初始温度100℃，终了温度850℃，步进温度50℃、每步保温10min。
(3)进行后处理，包括清洗、抛光、干燥工序。坯体先在六角滚桶、介质为去离子水进行清洗，清洗时间10min，然后在加入抛光剂，抛光时间10min，最后采用微波加热烘干，温度120℃，保护气氛为氮气，时间20min。烘干处理后即获得成品。
将上述实施例的铆钉组装成继电器，在250V、15A、密封、85℃阻性负载试验材料下进行电性能试验，具体结果如下表所示。可见，4个实施例的燃弧时间、电寿命次数均优于比较例，其中燃弧时间减少1-5ms，Weibull分布95％置信区间，电寿命次数提高4-6.2万次。
其中，实施例三，燃弧时间最短、电寿命次数最高，分别为10ms、12.3万次。
表1 不同成分实施案例及电性能比较
另外，上述3D打印还可以采用梯度分布打印，其具体为：将Ag粉、Ni粉、添加物、粘结剂置于梯度分布3D打印设备，首先打印基层Ag粉、厚度50-100微米，随后打印一层Ni粉、厚度3-20微米，然后打印一层添加物、厚度3-20微米，最后打印一层粘结剂、厚度为1-10微米，以上四个步骤重复进行，直至达到所需要的规格厚度。
以上所揭露的仅为本发明较佳实施例而已，当然不能以此来限定本发明之权利范围，因此依本发明权利要求所作的等同变化，仍属本发明所涵盖的范围。
Claims (7)
1.一种保留镍粉各向异性的单晶银镍电接触材料的制备方法，其特征在于包括以下步骤：
（1）将银粉、单晶镍粉、粘结剂与添加物混合粉末在3D喷头式粉末成型打印设备进行打印，形成银镍电接触材料坯件，该银镍电接触材料坯件中的单晶镍粉保留镍粉的各向异性特性；
（2）将步骤（1）的银镍电接触材料坯件在保护气氛或真空条件下通过微波方式进行烧结致密化处理，烧结后的银镍电接触材料坯件中的单晶镍粉保留镍粉的各向异性特性；
（3）将经步骤（2）处理的银镍电接触材料坯件进行清洗抛光和干燥处理获得成品。
2.根据权利要求1所述的一种保留镍粉各向异性的单晶银镍电接触材料的制备方法，其特征在于：所述步骤（1）中的银粉粒度分布范围为50-100微米、平均粒度60-90微米 、纯度≥99.99%，单晶镍粉粒度范围3-20微米、平均粒度5-18微米、纯度≥99.9%，粘结剂为用于粉体粘结的高分子材料，其平均粒度为3-10微米，添加物为碳氮化钛、碳氮化锆、碳氮化铪、碳氮化钒、碳氮化铌、碳氮化钽、碳氮化铬的一种或多种，其粒度范围3-20微米、平均粒度5-18微米、纯度≥99.9%。
3.根据权利要求1所述的一种保留镍粉各向异性的单晶银镍电接触材料的制备方法，其特征在于：所述步骤（1）中Ag、Ni、添加物的重量份数比为（50-92）：（7-49.9）：（0.1-1）。
4.根据权利要求1所述的一种保留镍粉各向异性的单晶银镍电接触材料的制备方法，其特征在于：所打印的银镍电接触材料坯件形状为铆钉型、片型或异型。
5.根据权利要求1所述的一种保留镍粉各向异性的单晶银镍电接触材料的制备方法，其特征在于：所述步骤（2）中的微波烧结的初始温度100℃，终了温度900℃；步进温度50℃，每步保温10min，所述步骤(2)的保护气氛为：氮气。
6.根据权利要求1所述的一种保留镍粉各向异性的单晶银镍电接触材料的制备方法，其特征在于所述步骤（3）中清洗、抛光、干燥工序是在惰性气体保护下进行。
7.一种如权利要求1-6之一所述制备方法所制备的保留镍粉各向异性的单晶银镍电接触材料。
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