CN106141189A - 一种放电等离子烧结非晶合金涂层的表面改性方法 - Google Patents
一种放电等离子烧结非晶合金涂层的表面改性方法 Download PDFInfo
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Abstract
本发明公开一种放电等离子烧结非晶合金涂层的表面改性方法，包括如下步骤：S1、采用放电等离子烧结炉，利用脉冲能、放电脉冲压力和焦耳热产生的瞬时高温场对非晶粉末进行烧结，从而得到烧结样品非晶态合金涂层；S2、将得到的非晶态合金涂层用激光焊接机进行激光重熔，得到最终的非晶合金涂层。并且本发明通过对制得试样进行如下的表征试验：对激光重熔前后的样品进行XRD表征；采用体视显微镜对重熔后样品的表面形貌进行观察；采用显微硬度计测定重熔后的表面硬度；采用扫描电镜观察试样横断面的显微组织，得出该方法将放电等离子烧结技术与激光重熔技术相结合，可以获得硬度强度更高及耐磨性更好的非晶涂层表面，从而可提高工件的寿命。
Description
技术领域
本发明属于环境保护技术领域，具体涉及一种放电等离子烧结非晶合金涂层的表面改性方法。
背景技术
非晶合金是一种玻璃结构，同时兼有金属材料和玻璃材料的物理化学性能及力学性能的新型金属材料。非晶合金原子具有短程有序，长程无序的特点，结构上不具有晶体材料的周期性分布特点，可以说其晶体结构是无缺陷的。基于这种结构特点，非晶态具有比常规晶态金属材料更为优异的硬度、强度、耐蚀性，近年来广为人们所关注。
对于非晶合金的制备来说，关键是减少冷却过程中的非均匀形核，所以在制备非晶合金时有两个注意点：一、对合金母材反复熔炼，提高熔体的纯度，消除非均匀成核点；二、采用高惰性气体保护，尽量减少氧含量。
目前，非晶合金的制备方法主要有以下几类：水淬法、电弧熔炼铜模吸铸法、感应加热铜模浇注法、射流成型法、压力模型铸造法、定向凝固法、粉末冶金冶金等。各非晶合金制备方法都有各自的优缺点：水淬法操作简单，设备简单，工艺容易控制，但有一定的局限性，对于那些与石英管有强烈反应的合金熔体不宜采用此方法。此外，熔体冷却速度速不如铜模吸铸法。电弧熔炼铜模吸铸法，电弧熔炼合金无污染、均匀性好，铜模冷却速率较快，制备效率高，但制备的样品尺寸比较小；感应加热铜模浇注法，在制备合金的过程中采用密封的石英管系统，冷却速率较快，但易于形成气孔，且样品的尺寸有限；射流成型法，适合制备小尺寸的金属玻璃样品，采用水冷铜模冷却，样品无明显气孔；压力模型铸造法，在提高铸件质量等方面极具潜力，在制备金属玻璃的过程中冷却速率快，能有效避免气孔和收缩等缺陷；定向凝固法适用于横截面积不大但比较长的样品，且要求玻璃形成能力较高。粉末冶金冶金制备出的非晶合金，不仅要求密实，而且要求避免晶化，因而在纯度，致密度，尺寸和成型等方面都受到很大限制。
放电等离子烧结(SPS)是近年来发展起来的一种新型的快速烧结技术。由于等离子活化烧结技术融等离子活化、热压、电阻加热为一体，因而具有升温速度快、烧结时间短、晶粒均匀、有利于控制烧结体的细微结构、获得的材料致密度高、性能好等特点。采用放电等离子烧结(SPS)技术制备非晶合金能够获得非晶特性的非晶合金涂层，然而，烧结得到的非晶涂层主要呈颗粒聚集状态，内部结构较为疏松，并存在较多孔洞，较大程度的影响了涂层的性能。因此，本领域技术人员有必要提供一种可获得硬度强度更高及耐磨性更好的非晶涂层表面的放电等离子烧结非晶合金涂层的表面改性方法。
发明内容
针对上述现有技术中的不足，本发明提供了一种能够制备出拥有更高硬度、强度表面并且非晶特性保持良好的非晶合金涂层的放电等离子烧结非晶合金涂层的表面改性方法。该方法将放电等离子烧结技术与激光重熔技术相结合，可以获得硬度强度更高及耐磨性更好的非晶涂层表面，从而提高工件的寿命，促进非晶涂层在耐磨耐腐等方面的应用。
为实现上述目的，本发明采用了以下技术方案：
一种放电等离子烧结非晶合金涂层的表面改性方法，包括如下步骤：
S1、采用放电等离子烧结炉，利用脉冲能、放电脉冲压力和焦耳热产生的瞬时高温场对非晶粉末进行烧结，从而得到烧结样品非晶态合金涂层；
S2、将得到的非晶态合金涂层用激光焊接机进行激光重熔，得到最终的非晶合金涂层。
优选的，步骤S1中烧结炉设备的压力保持在50～90MPa，烧结温度低于非晶涂层的晶化温度。
进一步的，步骤S1中，以100℃/min的速率快速加热至烧结温度，保持一定的时间，最后使用氮气吹扫快速冷却得到烧结样品。
优选的，在进行步骤S2激光重熔前，对烧结样品进行预热，预热温度低于晶化温度。
进一步的，对烧结样品的预热采用HP-05陶瓷封闭式恒温电炉。
优选的，步骤S2中，所述的激光焊接机的型号为GD-YAG-W200/W300，利用该型号焊接机进行激光重熔的工艺参数为：激光功率1.8～4.6kw、扫描速度180～250mm/min、激光加工路径轨迹间距0.4～0.6mm，并且在激光重熔过程中使用氩气做保护气沿激光加工方向吹气保护。
进一步的，其特征在于该方法还包括如下的表征步骤：对激光重熔前后的样品进行XRD表征；采用体视显微镜对重熔后样品的表面形貌进行观察；采用显微硬度计测定重熔后的表面硬度；采用扫描电镜观察试样横断面的显微组织。
本发明的有益效果在于：
1)、本发明将放电等离子烧结技术与激光重熔技术相结合，通过激光重熔，非晶颗粒瞬时熔化成液态后再凝固形成涂层，消除了颗粒的聚集状态，极大地减少涂层中的孔洞，进而大幅提高涂层的性能。通过试验验证，将放电等离子烧结技术与激光重熔技术相结合，可以获得硬度强度更高及耐磨性更好的非晶涂层表面，从而提高工件的寿命，促进非晶涂层在耐磨耐腐等方面的应用。
2)、本发明在进行激光重熔前，对烧结样品进行预热，预热温度低于晶化温度，而试验表明预热对减少非晶涂层表面裂纹有着显著的效果，进一步为通过本发明方法获得性能更优的非晶合金涂层提供了有效保障。
附图说明
图1为本发明的方法流程图。
图2为本发明SPS/激光重熔前后样品的XRD光谱图。
图3a为未经过预热直接激光重熔后的非晶涂层表面形貌图。
图3b为经过预热之后再激光重熔后的非晶涂层表面形貌图。
图4为本发明SPS/激光重熔后非晶合金涂层横断面的表面形貌图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明中的技术方案进行清楚、完整地描述。以下实施例仅用于更加清楚地说明本发明的技术方案，而不能以此来限制本发明的保护范围。
一种放电等离子烧结非晶合金涂层的表面改性方法，如图1所示，包括如下步骤：
S1、采用放电等离子烧结方法，利用脉冲能、放电脉冲压力和焦耳热产生的瞬时高温场进行烧结过程，从而得到非晶态合金涂层；
S2、将得到的非晶态合金涂层用激光焊接机进行激光重熔，得到最终的非晶合金涂层，从图1中可看出通过激光重熔，非晶颗粒瞬时熔化成液态后再凝固形成涂层，在涂层的表面消除了颗粒的聚集状态，大幅提高了涂层的性能。
实施例
S1、采用市售Fe48Cr15Mo14Y2C15B6(纯度99.9％，粒度10～30μm)非晶粉末为实验原料，使用放电等离子烧结设备制备非晶涂层，保持设备在高真空的压力下，设置压力为50～90MPa之间，温度设置为低于非晶涂层的晶化温度575℃。典型的制备周期分为三个部分：以100℃/min的速率快速加热至烧结温度，保持一定的时间，最后使用氮气吹扫达到快速冷却的目的。烧结所得的圆柱型样品的高为10mm，直径大小为15mm。
S2、采用光大激光生产的YAG能量反馈激光焊接机(型号为GD-YAG-W200/W300)对烧结所得的非晶涂层进行激光重熔；重熔前采用HP-05陶瓷封闭式恒温电炉对样品进行预热，温度设定为低于晶化温度。选取关键参数激光功率、扫描速度、激光扫描间距，在合理范围内控制单一变量测试参数的影响，最终选定比较合适的工艺参数范围：激光功率1.8～4.6kw、扫描速度180～250mm/min、激光加工路径轨迹间距0.4～0.6mm，并且使用氩气做保护气沿激光加工方向吹气保护，最终得到非晶合金涂层。
对上述实施例进行样品表征试验
采用X-ray Pert MPD PRO X射线衍射仪对激光重熔前后的样品进行XRD测试，分析激光重熔前后样品的物相。结果如图2所示，为放电等离子烧结技术制备得到的非晶态涂层激光重熔前后的XRD光谱图。通过比较我们可以看到，激光重熔前后的XRD都只有一个宽的漫散射锋并且位置相同，都在42°附近，这说明激光重熔前后试样皆为非晶态，并且没有发生晶化现象。激光重熔后的XRD图显示在30°附近有一个尖锐的杂锋，但结晶度较低，并不影响样品的非晶结构。
采用体式显微镜将激光重熔后的试样置于专业图像测量处理软件(scope photo)下观察并拍照，分析宏观形貌。未经过预热直接激光重熔后的非晶涂层表面形貌如图3a所示、经过预热之后再激光重熔后的非晶涂层表面形貌如图3b所示，可以看出非晶涂层的表面均比较平整，熔池的形状比较均匀，纹路略变形，重叠搭接处呈现明显的堆积线。具体的，图3a中可以看到树枝状的裂纹横穿整个界面，裂纹是激光实验普遍存在的问题，这是因为激光重熔后的非晶涂层表面硬度较大，韧性较差，并且激光会在材料表面会形成冲击波，故而样品表面易形成裂纹。可以通过适当降低激光功率以及对样品进行预热的办法来减少激光重熔后产生的裂纹。将非晶样品预热到低于晶化温度，可以看到图3b中基本看不出裂纹的存在，这说明预热对减少非晶涂层表面裂纹有着显著的效果。
切割试样得到非晶涂层的横断面，用Vickers显微硬度计对激光重熔后的部分进行硬度测试，选取十个点取平均值，得到最终值。并且使用FEI Quanta 200扫描电镜观察试样横断面的显微组织，如图4所示给出了SPS/激光重熔后非晶合金涂层的表面形貌，从图4中可以看出非晶涂层在激光重熔前比较疏松而且存在裂纹、气孔、夹杂等，激光重熔后可以看到非晶表面孔隙率明显降低，这说明重熔后周围的金属液体流向气孔，从而使气孔数量逐渐减少甚至得以消除，裂纹数量也得以减少。对激光重熔后的样品进行硬度测试，选取十个点取平均值，得到最终值。激光重熔后的非晶硬度非常高，这对要求高耐磨高硬度的工件意义重大。
综上所述，通过SPS/激光重熔后的非晶涂层孔洞明显减少，孔隙率明显降低，涂层组织均匀致密，并且硬度得到明显的提高，能够达到1000HV～1600HV，这对要求高耐磨高硬度的工件意义重大，拓宽了应用范围。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变形，这些改进和变形也应视为本发明的保护范围。
Claims (7)
1.一种放电等离子烧结非晶合金涂层的表面改性方法，其特征在于包括如下步骤：
S1、采用放电等离子烧结设备，利用脉冲能、放电脉冲压力和焦耳热产生的瞬时高温场对非晶粉末进行烧结，从而得到烧结样品非晶态合金涂层；
S2、将得到的非晶态合金涂层用激光焊接机进行激光重熔，得到最终的非晶合金涂层。
2.根据权利要求1所述的一种放电等离子烧结非晶合金涂层的表面改性方法，其特征在于，步骤S1中烧结设备的压力保持在50～90MPa，烧结温度低于非晶涂层的晶化温度。
3.根据权利要求2所述的一种放电等离子烧结非晶合金涂层的表面改性方法，其特征在于：步骤S1中，以100℃/min的速率快速加热至烧结温度，保持一定的时间，最后使用氮气吹扫快速冷却得到烧结样品。
4.根据权利要求1所述的一种放电等离子烧结非晶合金涂层的表面改性方法，其特征在于：在进行步骤S2激光重熔前，对烧结样品进行预热，预热温度低于晶化温度。
5.根据权利要求4所述的一种放电等离子烧结非晶合金涂层的表面改性方法，其特征在于：对烧结样品的预热采用HP-05陶瓷封闭式恒温电炉。
6.根据权利要求1所述的一种放电等离子烧结非晶合金涂层的表面改性方法，其特征在于：步骤S2中，所述的激光焊接机的型号为GD-YAG-W200/W300，利用该型号焊接机进行激光重熔的工艺参数为：激光功率1.8～4.6kw、扫描速度180～250mm/min、激光加工路径轨迹间距0.4～0.6mm，并且在激光重熔过程中使用氩气做保护气沿激光加工方向吹气保护。
7.根据权利要求1至6任一项所述的一种放电等离子烧结非晶合金涂层的表面改性方法，其特征在于该方法还包括如下的表征步骤：对激光重熔前后的样品进行XRD表征；采用体视显微镜对重熔后样品的表面形貌进行观察；采用显微硬度计测定重熔后的表面硬度；采用扫描电镜观察试样横断面的显微组织。
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