CN113004048A - 一种碳氮氧化钛陶瓷粉体的制备方法 - Google Patents
一种碳氮氧化钛陶瓷粉体的制备方法 Download PDFInfo
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- 238000002441 X-ray diffraction Methods 0.000 description 1
- WFJCMBBIZUEKJJ-UHFFFAOYSA-N [C+4].N.[O-2].[Ti+4] Chemical compound [C+4].N.[O-2].[Ti+4] WFJCMBBIZUEKJJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种碳氮氧化钛陶瓷粉体的制备方法及其制备方法,本发明以Ti粉、Al粉、C粉为原料,经真空高温烧结得到的化合物在空气中高温氧化,然后在含氟化锂和盐酸的混合溶液中刻蚀得到。本发明所合成粉体纯度较高,合成可控,可以作为一种结构功能材料应用于金属陶瓷,机械加工,航天航空等领域。
Description
技术领域
本发明涉及陶瓷粉体材料领域,特别涉及一种碳氮氧化钛陶瓷粉体的制备方法。
背景技术
碳氮化钛属于过渡金属碳氮化物,是一种重要的功能结构材料,应用于金属陶瓷,机械加工,航天航空等领域。在金属切削加工中,碳氮化钛粉体作为一种涂层材料具有良好耐磨性和耐高温性。而氧化物作为涂层材料在抗润滑性,抗氧化性等方面提供更好的性能。碳氮氧化钛可以看做碳氮化钛和氧化钛形成的固溶体,其物相主要是作为一种中间产物被发现(参见文献W.J.Yao,G.H.Bao,et al.Growth Characteristics of TiCxNy Ceramicsunder Laser Melting Conditions,Materials and Manufacturing Processes,2014,29:715–720.),其陶瓷粉体的制备在文献中鲜有报道。授予小阿尔弗雷德·S·盖茨和班志刚的专利CN102965639A介绍了一种具有碳氮氧化钛涂层的切削镶片及其制造方法,用包含乙腈的气态混合物通过化学气相沉积(CVD)沉积得到碳氮氧化钛涂覆层,说明碳氮氧化钛作为涂层具有一定的优异性能。工业上碳氮化钛及氧化物作为涂层材料主要是将粉体喷涂到金属基体上,碳氮氧化钛作为涂层材料的应用以及像碳氮化钛一样作为一种功能结构材料广泛应用在各领域首先要合成制备出其陶瓷粉体。
发明内容
本发明所要解决的技术问题:本发明提供一种碳氮氧化钛陶瓷粉体的制备方法,其化学式为Ti(O0.19C0.53N0.32)。所采用的具体方案为:以Ti粉、Al粉、C粉为原料,经真空高温烧结得到的化合物在空气中高温氧化,然后在含氟化锂和盐酸的混合溶液中刻蚀得到。
为解决上述技术问题,本发明提供以下的技术方案:
一种碳氮氧化钛陶瓷粉体的制备方法,采用Ti粉、Al粉、C粉为原料,经真空高温烧结得到的化合物在空气中高温氧化,然后在含氟化锂和盐酸的混合溶液中刻蚀得到化学式为Ti(O0.19C0.53N0.32)的碳氮氧化钛陶瓷粉体。
优选地,碳氮氧化钛陶瓷粉体的具体制备步骤如下:
(1)称取Ti粉、Al粉、C粉为原料,纯度大于98%,摩尔配比为Ti:Al:C=2:(1.0~1.3):1。将称取的粉末放入球磨罐,加入无水乙醇湿混12-36h,在烘箱中50-80℃烘干;
(2)将步骤(1)中干燥的粉末真空无压烧结,以3~8℃/min的升温速率加热到1250~1400℃,保温2~5h,随炉冷却;
(3)将步骤(2)中得到的粉体研磨,过筛200目,放置于氧化铝方舟中,铺平,在马弗炉中以3~8℃/min升温速率升温至350~450℃,保温2~6小时,随炉降温;
(4)将步骤(3)中得到的粉体按每1g放置于20mL的LiF和盐酸的混合溶液中磁力搅拌,水浴加热;
(5)将步骤(4)中的混合溶液进行离心处理,使离心后上层清液的PH值达到5~7,用去离子水清洗沉淀,用手摇晃,让沉淀物混合均匀,用滤膜抽滤,将滤膜上的粉体干燥,温度50~120℃,时间12~24h,得到碳氮氧化钛粉体。
优选地,所述LiF和盐酸的混合溶液中LiF的含量为0.07~0.09g/mL,盐酸的浓度为6-10mol/L。
优选地,所述步骤(4)中水浴温度为30-80℃,时间为24-48h。
优选地,所述步骤(5)中离心速率为2500-6000rpm。
本发明获得的有益效果:
本发明成功制备了一种碳氮氧化钛陶瓷粉体,纯度高,制备工艺可控,可以作为一种功能结构材料广泛应用于金属陶瓷,机械加工,航天航空等领域。
附图说明
图1为实施例1中所制备的碳氮氧化钛陶瓷粉体的X射线衍射图谱及Ti(O0.19C0.53N0.32)标准PDF卡片。
图2为实施例1中所制备的碳氮氧化钛陶瓷粉体的扫描电镜图谱。
具体实施方式
下面通过对实施例的描述,对本发明的具体实施方式作进一步详细的说明,以帮助本领域的技术人员对本发明的发明构思、技术方案有更完整、准确和深入的理解。
实施例1:按如下方法制备碳氮氧化钛陶瓷粉体:
1)称取Ti粉、Al粉、C粉为原料,纯度大于98%,摩尔配比为Ti:Al:C=2:1.1:1。将称取的粉末放入球磨罐,加入无水乙醇湿混24h,在烘箱中50℃烘干。
2)将干燥的粉末真空无压烧结,以5℃的升温速率加热到1300℃,保温3h,随炉冷却。
3)将烧结得到的粉体研磨,过筛200目,放置于氧化铝方舟中,铺平,在马弗炉中以5℃/min升温速率升温至400℃,保温3小时,随炉降温。
4)将氧化后得到的粉体称量1g放置于LiF和盐酸的混合溶液中磁力搅拌,水浴加热。LiF的质量为1.6g,盐酸的浓度为9mol/L,体积20ml。水浴温度50℃,时间24h。
5)将水浴加热的混合溶液用去离子水清洗,3500rpm离心处理,倾倒上层溶液,直到上层溶液的PH值达到6,继续将去离子水倒入置有沉淀物的离心试管中,用手摇晃,让沉淀物混合均匀,用滤膜抽滤,将滤膜上的粉体真空70℃干燥20h,得到碳氮氧化钛粉体。
根据图1可知,比照标准PDF卡片,所合成的粉体为一种碳氮氧化钛化合物,物相纯度较高,含有少量杂质。从图2可以观察所合成粉体的微观形貌。
实施例2:
1)称取Ti粉、Al粉、C粉为原料,纯度大于98%,摩尔配比为Ti:Al:C=2:1.2:1。将称取的粉末放入球磨罐,加入无水乙醇湿混20h,在烘箱中60℃烘干。
2)将干燥的粉末真空无压烧结,以8℃/min的升温速率加热到1350℃,保温2h,随炉冷却。
3)将烧结得到的粉体研磨,过筛200目,放置于氧化铝方舟中,铺平,在马弗炉中以3℃/min升温速率升温至350℃,保温4小时,随炉降温。
4)将氧化后得到的粉体称量1g放置于LiF和盐酸的混合溶液中磁力搅拌,水浴加热。LiF的质量为1.5g,盐酸的浓度为7mol/L,体积20ml。水浴温度60℃,时间30h。
5)将水浴加热的混合溶液用去离子水清洗,3000rpm离心处理,倾倒上层溶液,直到上层溶液的PH值达到5,继续将去离子水倒入置有沉淀物的离心试管中,用手摇晃,让沉淀物混合均匀,用滤膜抽滤,将滤膜上的粉体真空80℃干燥24h,得到碳氮氧化钛粉体。
实施例3:
1)称取Ti粉、Al粉、C粉为原料,纯度大于98%,摩尔配比为Ti:Al:C=2:1.0:1。将称取的粉末放入球磨罐,加入无水乙醇湿混30h,在烘箱中70℃烘干。
2)将干燥的粉末真空无压烧结,以7℃/min的升温速率加热到1400℃,保温4h,随炉冷却。
3)将烧结得到的粉体研磨,过筛200目,放置于氧化铝方舟中,铺平,在马弗炉中以6℃/min升温速率升温至450℃,保温2小时,随炉降温。
4)将氧化后得到的粉体称量1g放置于LiF和盐酸的混合溶液中磁力搅拌,水浴加热。LiF的质量为1.8g,盐酸的浓度为10mol/L,体积20ml。水浴温度40℃,时间36h。
5)将水浴加热的混合溶液用去离子水清洗,5000rpm离心处理,倾倒上层溶液,直到上层溶液的PH值达到7,继续将去离子水倒入置有沉淀物的离心试管中,用手摇晃,让沉淀物混合均匀,用滤膜抽滤,将滤膜上的粉体真空60℃干燥30h,得到碳氮氧化钛粉体。
以上实施例仅为说明本发明的技术思想,不能以此限定本发明的保护范围,凡是按照本发明提出的技术思想,在技术方案基础上所做的任何改动,均落入本发明保护范围之内;本发明未涉及的技术均可通过现有技术加以实现。
Claims (5)
1.一种碳氮氧化钛陶瓷粉体的制备方法,其特征在于,采用Ti粉、Al粉、C粉为原料,经真空高温烧结得到的化合物在空气中高温氧化,然后在含氟化锂和盐酸的混合溶液中刻蚀得到化学式为Ti(O0.19C0.53N0.32)的碳氮氧化钛陶瓷粉体。
2.根据权利要求1中所述的一种碳氮氧化钛陶瓷粉体的制备方法,其特征在于,具体步骤如下:
(1)称取Ti粉、Al粉、C粉为原料,纯度大于98%,摩尔配比为Ti:Al:C=2:(1.0~1.3):1。将称取的粉末放入球磨罐,加入无水乙醇湿混12-36h,在烘箱中50-80℃烘干;
(2)将步骤(1)中干燥的粉末真空无压烧结,以3~8℃/min的升温速率加热到1250~1400℃,保温2~5h,随炉冷却;
(3)将步骤(2)中得到的粉体研磨,过筛200目,放置于氧化铝方舟中,铺平,在马弗炉中以3~8℃/min升温速率升温至350~450℃,保温2~6小时,随炉降温;
(4)将步骤(3)中得到的粉体按每1g放置于20mL的LiF和盐酸的混合溶液中磁力搅拌,水浴加热;
(5)将步骤(4)中的混合溶液进行离心处理,使离心后上层清液的PH值达到5~7,用去离子水清洗沉淀,用手摇晃,让沉淀物混合均匀,用滤膜抽滤,将滤膜上的粉体干燥,温度50~120℃,时间12~24h,得到碳氮氧化钛粉体。
3.根据权利要求2中所述的一种碳氮氧化钛陶瓷粉体的制备方法,其特征在于:所述LiF和盐酸的混合溶液中LiF的含量为0.07~0.09g/mL,盐酸的浓度为6-10mol/L。
4.根据权利要求2中所述的一种碳氮氧化钛陶瓷粉体的制备方法,其特征在于:所述步骤(4)中水浴温度为30-80℃,时间为24-48h。
5.根据权利要求2中所述的一种碳氮氧化钛陶瓷粉体的制备方法,其特征在于:所述步骤(5)中离心速率为2500-6000rpm。
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