CN104119095B - 一种金属陶瓷复合制品及其制备方法 - Google Patents

一种金属陶瓷复合制品及其制备方法 Download PDF

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CN104119095B
CN104119095B CN201310150777.1A CN201310150777A CN104119095B CN 104119095 B CN104119095 B CN 104119095B CN 201310150777 A CN201310150777 A CN 201310150777A CN 104119095 B CN104119095 B CN 104119095B
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metal composite
base alloy
zirconium base
groove
composite product
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CN104119095A (zh
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宫清
林信平
林勇钊
张法亮
陈建新
徐述荣
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BYD Co Ltd
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BYD Co Ltd
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Priority to CN201310150777.1A priority Critical patent/CN104119095B/zh
Priority to PCT/CN2014/076235 priority patent/WO2014173321A1/en
Priority to US14/785,792 priority patent/US20160068448A1/en
Priority to EP14787406.9A priority patent/EP2989067B1/en
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Abstract

本发明提供了一种金属陶瓷复合制品及其制备方法，该金属陶瓷复合制品包括：陶瓷基体及金属复合材料，所述陶瓷基体表面具有图案纹路的凹槽，所述金属复合材料填充所述凹槽，所述金属复合材料为锆基合金/A的复合材料，所述A选自W、Mo、Ni、Cr、不锈钢、WC、TiC、SiC、ZrC或ZrO2中的一种或几种，以锆基合金/A的复合材料的总量为基准，所述A的体积百分含量为30-70%，金属与陶瓷基体的结合力强，金属与陶瓷基体间能无缝连接，金属硬度大，不易磨损，具有良好耐腐蚀性能，且无气孔、孔洞等缺陷，外观完美，能实现整体或陶瓷镜面效果和金属哑光效果。

Description

一种金属陶瓷复合制品及其制备方法
技术领域
本发明属于陶瓷金属复合材料领域，尤其涉及一种金属陶瓷复合制品及其制备方法。
背景技术
金属-陶瓷复合耐磨材料主要应用于冶金、建材、矿山、耐火材料及电力等领域物料破碎及研磨装备中的耐磨件，如辊套、衬板、磨环、磨盘等，是为了满足更高的耐磨性要求而研制开发的，金属-陶瓷复合材料的性能取决于金属的性能、陶瓷的性能及两者的结合强度。金属-陶瓷复合材料优良的性能使其在很多领域中得到应用。例如，现有研究也用来制备同时具有陶瓷或整体镜面效果和金属哑光效果的金属装饰陶瓷制品，具有良好的耐磨性使其应用广泛。
目前陶瓷-金属复合材料的制备方法主要有粉末冶金、共喷射沉积、搅拌混合、挤压铸造、原位生成等。目前的陶瓷-金属复合材料制作工艺复杂、成本较高，复合材料中陶瓷的位置及体积分数较难控制，陶瓷的分布不均匀，目前复合材料中陶瓷和金属的体积比以及陶瓷的分布情况均不能很好的保证材料良好的综合性能和耐磨性能。因此有人提出先对氧化锆-氧化铝复相蜂窝陶瓷进行预处理和表面活化处理，后固定于铸型中，然后采用铸造工艺浇注高温钢铁金属液的方法，但该方法制得的复合材料内部会存在气孔，影响复合材料的外观，并不能作为外观件的制作方法。一般金属装饰的陶瓷制品采用PVD（物理气相沉积法）工艺沉积金属来制备，但得到的金属层非常薄，与陶瓷基体的结合力不高，制备的金属装饰容易磨损，不仅良品率低，而且应用受限。
发明内容
本发明为解决现有金属装饰与陶瓷基体的结合力弱，装饰的金属容易磨损，制备过程中会大面积的成片，易出现气孔、孔洞等缺陷的技术问题，提供一种金属与陶瓷基体的结合力强，金属与陶瓷基体间能无缝连接，金属硬度大，不易磨损，具有良好耐腐蚀性能，且无气孔、孔洞等缺陷，外观完美，能实现整体或陶瓷镜面效果和金属哑光效果的，尤其能制备完美的金属装饰的陶瓷制品的金属陶瓷复合制品及其制备方法。
本发明的第一个目的是提供一种金属陶瓷复合制品，该金属陶瓷复合制品包括：陶瓷基体及金属复合材料，所述陶瓷基体表面具有图案纹路的凹槽，所述金属复合材料填充所述凹槽，所述金属复合材料为锆基合金/A的复合材料，所述A选自W、Mo、Ni、Cr、不锈钢、WC、TiC、SiC、ZrC或ZrO2中的一种或几种，以锆基合金/A的复合材料的总量为基准，所述A的体积百分含量为30-70%。
本发明的第二个目的是提供一种金属陶瓷复合制品的制备方法，其步骤包括：S1，在表面具有图案纹路凹槽的陶瓷基体的凹槽中填充A材料，后在保护气氛中于1000℃-1200℃下烧结，在凹槽中形成增强相骨架；S2，在填充有A材料的凹槽中熔渗锆基合金的熔液，冷却后得到金属陶瓷复合制品；所述A选自W、Mo、Ni、Cr、不锈钢、WC、TiC、SiC、ZrC或ZrO2中的一种或几种。
本发明意外发现本发明制备的金属陶瓷复合制品中复合材料与陶瓷基体间能实现无缝连接，金属与陶瓷基体的结合力强，所获得的复合制品陶瓷基体与金属复合材料的结合力大于50MPa（剪切强度），金属硬度大，不易磨损，金属硬度大于500Hv，通过中性盐雾实验具有良好耐腐蚀性能，且无气孔、孔洞等缺陷，外观完美，能实现整体或陶瓷镜面效果和金属哑光效果。金属复合材料中即有体积百分含量为30-70%的A材料形成的增强相骨架，具有增强复合材料耐磨的性能，在增强相骨架中又渗入有锆基合金，锆基合金不仅作为增强相颗粒的粘结剂同时作为复合材料与陶瓷基体粘结剂，意外发现此复合材料与陶瓷基体的粘结强度远高于单纯的锆基合金与陶瓷基体的粘结强度，使二者构成一个有机整体；同时复合材料的强度、硬度较金属也得到了明显的提高；同时选自W、Mo、Ni、Cr、不锈钢、WC、TiC、SiC、ZrC或ZrO2中的一种或几种的A材料的熔点高，例如W的熔点3410℃，Mo的熔点2610℃等，远比金属锆基合金熔点800-900℃要高，且W、Mo等材料与锆基合金液润湿性良好，可以保证在较短时间完成合金液完全渗入A材料烧结形成的骨架中，同时W、Mo等材料在锆基合金液中溶解度不高，保证合金相成分基本不受影响，进一步保证了复合材料的性能；且增强相骨架的存在也使锆基合金不会大面积的成片出现，制得的复合材料整体无气孔、孔洞等缺陷，制备的金属外观更完美，能实现更完美的整体或陶瓷镜面效果和金属哑光效果的陶瓷制备，尤其可作为金属装饰的外观件等，应用更广泛。
同时WC、TiC、SiC、ZrC等材料的熔点不仅比锆基合金熔点高很多，而且推测WC、TiC、SiC、ZrC等中的C元素还可能与锆基合金中Zr元素发生反应生成碳化锆，此反应主要在A材料颗粒与锆基合金液界面发生，也能改善A材料颗粒与锆基合金液的润湿性，使合金液能更好、更完全的渗入A材料烧结形成的骨架中，也能优化复合制品的性能，同时A材料颗粒与锆基合金的结合力也强，也提高了复合材料的性能，提高了复合制品的性能。
本发明的方法简单易实现，更易实现大规模的生产，产品良率高，成本低。
具体实施方式
为了使本发明所解决的技术问题、技术方案及有益效果更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
本发明提供了一种金属陶瓷复合制品，该金属陶瓷复合制品包括：陶瓷基体及金属复合材料，所述陶瓷基体表面具有图案纹路的凹槽，所述金属复合材料填充所述凹槽，所述金属复合材料为锆基合金/A的复合材料，所述A选自W、Mo、Ni、Cr、不锈钢、WC、TiC、SiC、ZrC或ZrO2中的一种或几种，以锆基合金/A的复合材料的总量为基准，所述A的体积百分含量为30-70%，复合材料与陶瓷基体间能实现无缝连接，金属与陶瓷基体的结合力强，所获得的金属陶瓷复合制品陶瓷基体与金属复合材料的结合力大于50MPa（剪切强度），金属硬度大，不易磨损，具有良好耐腐蚀性能，金属硬度大于500Hv，通过中性盐雾实验具有良好耐腐蚀性能，且无气孔、孔洞等缺陷，外观完美，能实现整体或陶瓷镜面效果和金属哑光效果，尤其能制备完美的金属装饰的陶瓷制品。
其中，图案纹路是指根据需要设计的图案的各部分组成线路，在陶瓷基体的表面根据图案的线路设计有凹槽，即陶瓷基体的表面的凹槽能组成所设计的图案。填充在凹槽中，可以刚好填满所述凹槽，在颜色、光泽上替代陶瓷，显示整体或陶瓷镜面效果和金属哑光效果的具有金属图案的陶瓷制品，外观完美。
优选，锆基合金/A的复合材料包括增强相骨架及锆基合金，所述增强相骨架中含有孔隙，所述锆基合金填充在所述增强相骨架的孔隙中，所述增强相骨架的材料为A。
优选，A材料为颗粒，所述A材料的颗粒的粒径为0.1-100μm。
其中，锆基合金本发明没有限制，可以是本领域技术人员公知的各种锆基合金，例如锆铝铜镍系合金等。
优选，陶瓷基体与金属复合材料的表面结合力大于50MPa。
陶瓷基体本发明没有限制，可以为本领域技术人员公知的各种陶瓷基体，本发明优选，陶瓷基体为氧化锆陶瓷，不仅与复合材料能更好的结合，而且其韧性较高，进一步优化陶瓷制品的性能。
优选，凹槽的深度大于0.1mm。
本发明同时提供了一种金属陶瓷复合制品的制备方法，其步骤包括：
S1，在表面具有图案纹路凹槽的陶瓷基体的凹槽中填充A材料，后在保护气氛中于1000℃-1200℃下烧结，在凹槽中形成增强相骨架，其中，A选自W、Mo、Ni、Cr、不锈钢、WC、TiC、SiC、ZrC或ZrO2中的一种或几种。一般填充材料颗粒，优选，颗粒的粒径为0.1-100μm。填充A材料可以采用常用的填充方法，本发明优选，将A材料溶解于溶剂中配置成浆料，将浆料灌充在凹槽中，有机溶剂其作用和种类已为本领域技术人员所公知。浆料中也可以含有粉末表面活性剂等改性添加剂，例如在浆料中添加硅烷偶联剂9116等，本发明没有限制，有机溶剂优选为甲基硅油，将甲基硅油作为A材料的载体，在烧结时易于除去，也有利于增强相骨架中孔的形成。其中，保护气氛可以为真空，也可以为惰性气氛例如氮气、氩气等。
其中，陶瓷基体的形状和结构本发明没有限制，可以根据需要进行选择，金属图案本发明没有限制，根据需要进行设计，例如可以是小的立体的商标图案，也可以是占据陶瓷基体表面大部分面积的大的金属块、花纹等。表面具有图案纹路凹槽的陶瓷基体可以是市购也可以是自行制备，制备表面具有图案纹路凹槽的陶瓷基体可以是在制备陶瓷基体的同时形成凹槽，例如在陶瓷基体预成型时，通过陶瓷坯体预成型表面具有图案纹路凹槽结构后烧结，具体说来，可以是在注射成型或热压铸成型的成型模具预先做出与图案纹路凹槽相对应的凸起纹路，使用传统的注射或热压铸成型工艺，便可以获得表面具有图案纹路凹槽的陶瓷坯体，然后经过排胶、烧结获得带表面具有图案纹路凹槽的陶瓷件。陶瓷基体的制备本发明没有限制，可以采用现有的制备方法制成，具体步骤可以包括：称取配方量的原料，原料可以包含陶瓷粉体、粘结剂、表面活性剂，采用干压、挤出、热压铸、注射等成型方法制备生坯，经排胶、烧结后制得陶瓷基体。所述干压、挤出、热压铸、注射等成型方法所采用的设备和制作步骤已为本领域技术人员所公知，实际成型时，可根据所选用的陶瓷粉体、粘结剂、表面活性剂的种类和含量的不同，适当的调节其制备条件和参数。也可以是在已有的陶瓷基体的表面加工出所需的图案纹路凹槽，例如，在陶瓷基体的表面通过激光加工出所需图案纹路凹槽，具体的可以是使用传统的注射或热压铸成型工艺制作陶瓷坯体，然后经过排胶、烧结获得所需形状的陶瓷基体，最后使用激光器在陶瓷基体表面打出所设计的图案纹路的凹槽，便可以获得表面具有图案纹路凹槽的陶瓷基体，一般激光加工的条件可以为激光器功率10-20W。
优选，增强相骨架的孔隙率为70-30%，上述孔隙为开孔，用于填充合金。所述孔隙率可利用现有的排水法进行测试。
其中，烧结主要是使A材料颗粒与颗粒之间粘结，形成具有孔隙的增强相骨架，使其获得一定的强度，并能够形成开孔的孔隙，以便锆基合金的熔液的渗入，形成复合材料。优选，烧结的时间为1h-2h，进一步优化复合材料的致密度，优化复合材料的强度。其中，烧结可以在烧结炉中等，可以包括多段升温的预烧结等，本发明没有限制。
S2，在填充有A材料的凹槽中熔渗锆基合金的熔液，冷却后得到金属陶瓷复合制品。
熔渗可以为压力熔渗也可以为无压熔渗，所述压力熔渗已为本领域技术人员所公知，在此不做赘述。本发明优选无压熔渗的方法，所述无压熔渗的条件为在真空中，在锆基合金的熔点之上的温度下进行，复合材料无气孔。优选锆基合金的熔点为T，所述熔渗的条件为在真空度不低于9X10-3Pa，温度为T+50℃～T+100℃。优选，熔渗的时间不少于5min，进一步保证锆基合金与陶瓷基体的润湿/反应时间，进一步提高复合材料与陶瓷基体的结合强度，具体的可以为5-30min，此时，合金熔液能够更好、更完全的通过孔隙的毛细管作用渗透到增强相骨架的孔隙中。优选，冷却的条件为：温度大于700℃时冷却速度大于100℃/min；温度大于400℃时冷却速度大于50℃/min。具体的可以是，将锆基合金置于陶瓷基体的凹槽表面上方，抽真空至真空度不低于9X10-3Pa，升温至锆基合金熔点以上50～100℃，保温不少于5min，锆基合金熔化并充分渗入增强相骨架，后迅速充入Ar快速冷却，700℃以上冷却速度大于100℃/min，400℃以上冷却速度大于50℃/min。
优选，步骤S2之后还包括磨抛及喷砂处理，制备所需外观更完美的金属陶瓷复合制品，其中，磨抛及喷砂处理工艺为常规的加工工艺，在此不在赘述。
下面通过具体实施例对本发明做进一步的具体描述。
实施例1
（1）称取300gW粉（粒径D50为1μm）及1.2g硅烷偶联剂9116溶于25g甲基硅油中，将二者搅拌约2h混合均匀，在真空干燥箱中脱泡30min，得含W浆料，将含W浆料涂覆在坯体预成型时形成的深度为0.20mm、宽度为0.5mm的氧化锆陶瓷的表面凹槽上，填满凹槽，并再次在真空干燥箱中脱泡30min，然后将氧化锆陶瓷放入真空电阻炉内烧结，以2℃/min升温至600℃，并在600℃保温1h，然后10℃/min升温至1100℃，保温1h，形成增强相骨架，采用排水法，测得增强相骨架的孔隙率为62.8%。
（2）将锆铝铜镍系合金置于上述制备的氧化锆陶瓷的表面凹槽的上方一起放入熔渗炉中，抽真空至真空度8X10-3Pa，升温至950℃，保温5min，锆铝铜镍系合金熔化并充分渗入增强相骨架中，后迅速充入Ar快速冷却，冷却速度120℃/min，冷却至室温后取出对表面进行磨抛及喷砂处理即得金属陶瓷复合制品样品S1。
实施例2-4
采用与实施例1相同的方法制备金属陶瓷复合制品样品S2-S7，不同的具体参数见表1。
对比例1
将锆铝铜镍系合金置于激光加工的氧化锆陶瓷的表面凹槽（深度为0.15mm、宽度为0.5mm）的上方一起放入熔渗炉中，抽真空至真空度9X10-3Pa，升温至1000℃，保温10min，锆铝铜镍系合金熔化并填充到凹槽中，填满后，后迅速充入Ar快速冷却，冷却速度120℃/min，冷却至室温后取出对表面进行磨抛及喷砂处理即得金属陶瓷复合制品样品DS1。
表1
性能测试
复合材料与陶瓷基体结合力：将制备好的A的浆料注入内径11mm、高10mm的氧化锆陶瓷环中，预烧后，熔渗锆基合金，（工艺同结构件制作工艺一致），获得氧化锆芯部带复合材料的测试样品；采用万能试验机将复合材料芯部压出，测试所需压力，并换算出剪切力，即为复合材料与陶瓷基体结合力，测试结果见表2。
复合材料硬度：对样品表面进行研磨、抛光至镜面，然后采用HVS-10Z型数显维氏硬度计测试，测试10点，取平均值，测试结果见表2。
外观：肉眼观察及光学显微镜放大50倍观察；外观是否有明显凹坑、凸起等缺陷，以及光泽是否均匀一致，测试结果见表2。
表2
本发明制备的金属陶瓷复合制品中金属与陶瓷基体的结合力强，金属与陶瓷基体间能无缝连接，装饰的金属硬度大，不易磨损，具有良好耐腐蚀性能，且无气孔、孔洞等缺陷，外观完美，能实现整体或陶瓷镜面效果和金属哑光效果，尤其适合作为金属装饰的陶瓷制品。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (15)

1.一种金属陶瓷复合制品，其特征在于，包括：陶瓷基体及金属复合材料，所述陶瓷基体表面具有图案纹路的凹槽，所述金属复合材料填充所述凹槽，所述金属复合材料为锆基合金/A的复合材料，所述A选自W、Mo、Ni、Cr、不锈钢、WC、TiC、SiC、ZrC或ZrO2中的一种或几种，以锆基合金/A的复合材料的总量为基准，所述A的体积百分含量为30-70％。
2.根据权利要求1所述的金属陶瓷复合制品，其特征在于，所述锆基合金/A的复合材料包括增强相骨架及锆基合金，所述增强相骨架中含有孔隙，所述锆基合金填充在所述增强相骨架的孔隙中，所述增强相骨架的材料为A。
3.根据权利要求2所述的金属陶瓷复合制品，其特征在于，所述A材料为颗粒，所述A材料的颗粒的粒径为0.1-100μm。
4.根据权利要求1所述的金属陶瓷复合制品，其特征在于，所述陶瓷基体与金属复合材料的表面结合力大于50MPa。
5.根据权利要求1所述的金属陶瓷复合制品，其特征在于，所述陶瓷基体为氧化锆陶瓷。
6.根据权利要求1所述的金属陶瓷复合制品，其特征在于，所述凹槽的深度大于0.1mm。
7.一种金属陶瓷复合制品的制备方法，其特征在于，步骤包括：
S1，在表面具有图案纹路凹槽的陶瓷基体的凹槽中填充A材料，后在保护气氛中于1000℃-1200℃下烧结，在凹槽中形成增强相骨架；
S2，在填充有A材料的凹槽中熔渗锆基合金的熔液，冷却后得到金属陶瓷复合制品；
所述A选自W、Mo、Ni、Cr、不锈钢、WC、TiC、SiC、ZrC或ZrO2中的一种或几种；
以锆基合金/A的复合材料的总量为基准，所述A的体积百分含量为30-70％。
8.根据权利要求7所述的制备方法，其特征在于，所述增强相骨架的孔隙率为70％-30％。
9.根据权利要求7所述的制备方法，其特征在于，所述烧结的时间为1h-2h。
10.根据权利要求7所述的制备方法，其特征在于，所述熔渗的时间不少于5min。
11.根据权利要求7所述的制备方法，其特征在于，所述熔渗采用无压熔渗的方法，所述无压熔渗的条件为在真空条件下，在锆基合金的熔点之上的温度下进行。
12.根据权利要求11所述的制备方法，其特征在于，所述锆基合金的熔点为T，所述熔渗的条件为在真空度不低于9X10-3Pa，温度为T+50℃～T+100℃。
13.根据权利要求12所述的制备方法，其特征在于，所述冷却的条件为：温度大于700℃时冷却速度大于100℃/min；温度大于400℃时冷却速度大于50℃/min。
14.根据权利要求7所述的制备方法，其特征在于，所述步骤S2之后还包括磨抛及喷砂处理。
15.根据权利要求7所述的制备方法，其特征在于，所述保护气氛为真空或惰性气氛。
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