CN104310991A - 一种掺杂稀土的纳米钛-铌涂层及其制备方法 - Google Patents
一种掺杂稀土的纳米钛-铌涂层及其制备方法 Download PDFInfo
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Abstract
一种掺杂稀土的纳米钛-铌涂层及其制备方法，涉及材料技术领域，涂层的厚度为0.1-5um；涂层的主要成分包括氧化钛、碳化钛、氧化铌、二氧化硅、纳米氧化锡和稀土氧化物；其中，稀土氧化物为纳米氧化钇和纳米氧化镨；其中，钛和铌的物质的量比为2-5:1。纳米钛-铌涂层的制备方法，包括：（1）称量；（2）研磨混合；（3）高温固相；（4）冷却；（5）粉碎；（6）喷涂。本发明提供的掺杂稀土的纳米钛-铌涂层及其制备方法，涂层具有优良的强度和韧性，同时涂层稳定性和耐腐蚀性能较好，且涂层性能更为持久。
Description
技术领域
本发明属于材料技术领域，特别涉及一种高稳定性能的掺杂稀土的纳米钛-铌涂层及其制备方法。
背景技术
随着纳米技术的发展，将纳米技术与涂层技术相结合，给后者的发展带来巨大活力。传统的陶瓷材料普遍存在脆性大、抗震抗力低等缺点，在很多场合制约了陶瓷材料的使用。纳米陶瓷材料由于晶粒细化，晶界数量大幅增加，材料的强度、韧性和超韧性等性能都明显提高。而且，采用合适的方法制备的纳米结构陶瓷涂层的性能较之传统的陶瓷涂层，有显著的改善，因此，纳米陶瓷材料的涂层技术，是现今最为关注的技术之一。
在涂层中，不同的材料和含量的不同，会造成涂层性质的千差万别，涂层多样性发展和功能化发展，也是现今纳米陶瓷涂层技术领域的发展趋势。
申请号为201310384218.7的专利文献“低碳钢表面钛-氮-碳-铝-氧纳米陶瓷涂层及制备方法”，公开了一种纳米陶瓷涂层，该纳米陶瓷涂层构成如下：由钢基材表面向外顺序依次为氮化钛层，碳化钛层，氧化钛层和氧化铝层；所述纳米陶瓷涂层总厚度8～12微米，其各单层符合如下特征：氮化钛层厚度1～3微米，碳化钛层厚度2.5～3微米，氧化钛层厚度0.5～1微米，氧化铝层厚度4～5微米。由此可知，该纳米陶瓷涂层，是多层结构，每层有不同的纳米材料构成，因此，对于基材的保护较为理想，有一定的耐腐性能和耐磨性能，但多层结构，容易造成分布不均和强度韧性上的不足，不适合低碳钢的工作需求。
申请号为201210476363.3的专利文献“一种纳米复合涂层”，公开了一种纳米复合涂层，包括金属基体和纳米陶瓷涂层，在金属基体与纳米陶瓷涂层之间设有纳米金属打底层；所述纳米陶瓷涂层的成分为氧化铝和氧化铬化合物；所述金属打底层为镍铬；所述纳米陶瓷涂层中氧化铝成分重量比例为85％-95％，氧化铬成分重量比例为5％-15％。由此可知，该纳米复合涂层即是纳米陶瓷层，是以氧化铝为主要成分的陶瓷材料，性能还是以氧化铝和氧化铬性能为主，是传统意义上的陶瓷材料，不同之处在于，涂层使用了纳米技术，另外为增加金属基体与纳米陶瓷层之间的联系，在两层之间增加了纳米金属打底层，虽然如此，性能上也没有改进，而且仍旧缺乏足够的韧性。
发明内容
本发明解决的技术问题：针对现有技术的缺陷，克服现有技术的不足，本发明提供一种掺杂稀土的纳米钛-铌涂层及其制备方法。
本发明的技术方案：一种掺杂稀土的纳米钛-铌涂层：
涂层的厚度为0.1-5um；
涂层的主要成分包括氧化钛、碳化钛、氧化铌、二氧化硅、纳米氧化锡和稀土氧化物；
其中，稀土氧化物为纳米氧化钇和纳米氧化镨；
其中，钛和铌的物质的量比为2-5:1；钛、硅、锡和钇或镨的物质的量比为1:0.01-0.05：0.05-0.1：0.08-0.18。
作为优选，钛和铌的物质的量之比为2-4:1。
作为优选，氧化钛和碳化钛的物质的量之比为1:1。
一种掺杂稀土的纳米钛-铌涂层的制备方法，制备步骤如下：
(1)根据物质的量比称取各个组分；
(2)将组合混合在一起，放入球磨机混合至均匀；
(3)将混合均匀的混合料放入高温炉中进行煅烧，温度600-800℃，每小时升温50-100℃，时间3-6h；
(4)煅烧结束之后，混合料随炉冷却至室温，取出；
(5)将混合料粉碎至平均粒径为0.05-0.5um；
(6)通过热喷法进行喷射，即得到掺杂稀土的纳米钛-铌涂层。
作为优选，步骤(3)中高温煅烧的最高温度为1300℃。
作为优选，步骤(3)中高温煅烧的起始温度为800℃，每小时升温60℃，时间5h。
作为优选，步骤(5)中混合粉料的平均粒径为0.05-0.1nm。
作为优选，步骤(6)中的热喷法为等离子喷射法。
有益效果：本发明提供的掺杂稀土的纳米钛-铌涂层及其制备方法，是利用纳米技术改进涂层稳定性和可塑性的方法。涂层中以钛和铌为主要成分，钛以氧化钛和碳化钛的形式出现，增强了材料的强度的同时也没有保持了材料的韧性，二氧化硅、纳米氧化锡和稀土氧化物，改善了涂层稳定性和耐磨性能，而且具有一定的光泽。
在制备上述涂层材料时，高温固相法为前提，这有别于传统的直接热喷法，高温固相，可以各个组分结合在一起，形成基团，基团通过热喷法喷射形成的涂层，组分分布更为均匀，性能保持的更为持久。
具体实施方式
为了进一步理解本发明，下面结合实施例对本发明优选实施方案进行描述，但是应当理解，这些描述只是为进一步说明本发明的特征和优点，而不是对本发明权利要求的限制。
实施例1：
根据本发明提供的制备方法制备掺杂稀土的纳米钛-铌涂层，步骤如下：
(1)称取氧化钛、碳化钛、氧化铌、二氧化硅、纳米氧化锡和稀土氧化物；
其中，各个组分的物质的量比为0.5：0.5：0.2：0.01：0.05：0.08；
(2)将组合混合在一起，放入球磨机混合至均匀；
(3)将混合均匀的混合料放入高温炉中进行煅烧，温度600℃，每小时升温80℃，时间5h；
(4)煅烧结束之后，混合料随炉冷却至室温，取出；
(5)将混合料粉碎至平均粒径为0.05um；
(6)通过等离子喷射法进行喷射，即得到掺杂稀土的纳米钛-铌涂层，涂层厚度为1um。
实施例2：
根据本发明提供的制备方法制备掺杂稀土的纳米钛-铌涂层，步骤如下：
(1)称取氧化钛、碳化钛、氧化铌、二氧化硅、纳米氧化锡和稀土氧化物；
其中，各个组分的物质的量比为0.5：0.5：0.5：0.05：0.1：0.18；
(2)将组合混合在一起，放入球磨机混合至均匀；
(3)将混合均匀的混合料放入高温炉中进行煅烧，温度700℃，每小时升温60℃，时间7h；
(4)煅烧结束之后，混合料随炉冷却至室温，取出；
(5)将混合料粉碎至平均粒径为0.05um；
(6)通过等离子喷射法进行喷射，即得到掺杂稀土的纳米钛-铌涂层，涂层厚度为1um。
实施例3：
根据本发明提供的制备方法制备掺杂稀土的纳米钛-铌涂层，步骤如下：
(1)称取氧化钛、碳化钛、氧化铌、二氧化硅、纳米氧化锡和稀土氧化物；
其中，各个组分的物质的量比为0.5：0.5：0.3：0.03：0.07：0.12；
(2)将组合混合在一起，放入球磨机混合至均匀；
(3)将混合均匀的混合料放入高温炉中进行煅烧，温度800℃，每小时升温60℃，时间5h；
(4)煅烧结束之后，混合料随炉冷却至室温，取出；
(5)将混合料粉碎至平均粒径为0.05um；
(6)通过等离子喷射法进行喷射，即得到掺杂稀土的纳米钛-铌涂层，涂层厚度为1um。
实施例4：
根据本发明提供的制备方法制备掺杂稀土的纳米钛-铌涂层，步骤如下：
(1)称取氧化钛、碳化钛、氧化铌、二氧化硅、纳米氧化锡和稀土氧化物；
其中，各个组分的物质的量比为0.5：0.5：0.4：0.03：0.07：0.15；
(2)将组合混合在一起，放入球磨机混合至均匀；
(3)将混合均匀的混合料放入高温炉中进行煅烧，温度700℃，每小时升温80℃，时间5h；
(4)煅烧结束之后，混合料随炉冷却至室温，取出；
(5)将混合料粉碎至平均粒径为0.1um；
(6)通过等离子喷射法进行喷射，即得到掺杂稀土的纳米钛-铌涂层，涂层厚度为3um。
实施例5：
根据本发明提供的制备方法制备掺杂稀土的纳米钛-铌涂层，步骤如下：
(1)称取氧化钛、碳化钛、氧化铌、二氧化硅、纳米氧化锡和稀土氧化物；
其中，各个组分的物质的量比为0.5：0.5：0.35：0.04：0.08：0.1；
(2)将组合混合在一起，放入球磨机混合至均匀；
(3)将混合均匀的混合料放入高温炉中进行煅烧，温度800℃，每小时升温80℃，时间4h；
(4)煅烧结束之后，混合料随炉冷却至室温，取出；
(5)将混合料粉碎至平均粒径为0.6um；
(6)通过高速火焰喷射法进行喷射，即得到掺杂稀土的纳米钛-铌涂层，涂层厚度为2um。
申请号为201310384218.7的专利文献“低碳钢表面钛-氮-碳-铝-氧纳米陶瓷涂层及制备方法”公开的技术方案制备纳米陶瓷涂层，为对照组；测定上述实施例和对照组纳米陶瓷涂层的强度和韧性，结果如表1所示：
表1 纳米陶瓷涂层强度和韧性测定
| 项目 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 对照组 |
| 韧性/MPam1/2 | 9.8 | 11.1 | 10.4 | 10.5 | 10.4 | 7.2 |
| 强度 | 1130 | 1250 | 1180 | 1230 | 1150 | 980 |
由上表可知，实施例1-5的韧性较之实施例1-3高，其中实施例2的韧性最优；在涂层强度性能上，对照组明显低于实施例1-5，其中实施例2的在强度最佳。
对实施例1-5和对照组的涂层材料进行耐腐蚀性能测试，结果如表2所示：
表2 纳米陶瓷涂层材料耐腐蚀性能测定
由此可知，实施例1-5和对照组的耐碱性都合格，在耐酸性上，对照组有轻微起泡现象，因此对照组的耐酸性能一般。
综上所述，本发明掺杂稀土的纳米钛-铌涂层及其制备方法提高的纳米陶瓷涂层，具有优良的强度和韧性，同时耐腐蚀性能优良。
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (8)
1.一种掺杂稀土的纳米钛-铌涂层，其特征在于：
涂层的厚度为0.1-5um；
涂层的主要成分包括氧化钛、碳化钛、氧化铌、二氧化硅、纳米氧化锡和稀土氧化物；
其中，稀土氧化物为纳米氧化钇和纳米氧化镨；
其中，钛和铌的物质的量比为2-5:1；钛、硅、锡和钇或镨的物质的量比为1:0.01-0.05：0.05-0.1：0.08-0.18。
2.根据权利要求1所述的掺杂稀土的纳米钛-铌涂层，其特征在于：钛和铌的物质的量之比为2-4:1。
3.根据权利要求1所述的掺杂稀土的纳米钛-铌涂层，其特征在于：氧化钛和碳化钛的物质的量之比为1:1。
4.一种根据权利要求1-3任一项所述的掺杂稀土的纳米钛-铌涂层的制备方法，其特征在于，制备步骤如下：
（1）根据物质的量比称取各个组分；
（2）将组合混合在一起，放入球磨机混合至均匀；
（3）将混合均匀的混合料放入高温炉中进行煅烧，温度600-800℃，每小时升温50-100℃，时间3-6h；
（4）煅烧结束之后，混合料随炉冷却至室温，取出；
（5）将混合料粉碎至平均粒径为0.05-0.5um；
（6）通过热喷法进行喷射，即得到掺杂稀土的纳米钛-铌涂层。
5.根据权利要求4所述的掺杂稀土的纳米钛-铌涂层的制备方法，其特征在于：步骤（3）中高温煅烧的最高温度为1300℃。
6.根据权利要求4所述的掺杂稀土的纳米钛-铌涂层的制备方法，其特征在于：步骤（3）中高温煅烧的起始温度为800℃，每小时升温60℃，时间5h。
7.根据权利要求4所述的掺杂稀土的纳米钛-铌涂层的制备方法，其特征在于：步骤（5）中混合粉料的平均粒径为0.05-0.1nm。
8.根据权利要求4所述的掺杂稀土的纳米钛-铌涂层的制备方法，其特征在于：步骤（6）中的热喷法为等离子喷射法。
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