CN104310990B - 一种气敏陶瓷材料及其制备方法 - Google Patents

一种气敏陶瓷材料及其制备方法 Download PDF

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CN104310990B
CN104310990B CN201410522662.5A CN201410522662A CN104310990B CN 104310990 B CN104310990 B CN 104310990B CN 201410522662 A CN201410522662 A CN 201410522662A CN 104310990 B CN104310990 B CN 104310990B
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翟红波
杨振枢
韦洪屹
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Tongxiang Tengfei Home Textile Co ltd
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Abstract

一种气敏陶瓷材料及其制备方法，涉及材料技术领域，气敏陶瓷材料主要成分为SnO2和ZnO，SnO2的含量为65‑85wt%，ZnO的含量为10‑25wt%，还包括以下质量百分比的添加剂，La2O3 0.3‑0.8wt%；Y2O3 0.5‑1.8wt%；Nb2O5 0.2‑0.5wt%；TiO2 1.2‑1.7wt%；V2O5 0.5‑1.5wt%；ZrO2 0.6‑1.2wt%；Cr2O3 0.3‑0.9wt%；CeO2 0.5‑1.1wt%。本发明气敏陶瓷材料及其制备方法提供的气敏陶瓷材料及对CO和H2S具有较高的灵敏度，具有响应快，测量范围宽，耐候性强等特点，是检测CO和H2S理想的气敏材料。

Description

一种气敏陶瓷材料及其制备方法
技术领域
本发明属于材料技术领域，特别涉及一种对CO和H2S具有较高灵敏度的气敏陶瓷材料及其制备方法。
背景技术
气敏陶瓷，亦称气敏半导体是用于吸收某种气体后电阻率发生变化的一种功能陶瓷。一般是用气敏氧化物材料经压制烧结而成的，对多种气体具有灵敏度。其应用也较为广泛，例如应用于气敏检漏仪等装置进行自动报警。
气敏材料的核心是对气体敏感的金属氧化物，即，气敏半导体材料，随着陶瓷技术的发展，多种金属氧化物被发现对多种不同的气体具有高度灵敏度。其中SnO2和Zn0就是优良的气敏半导体材料，配合不同的助剂，可改变对不同气体产生灵敏度。
申请号为201210190973.7的专利文献“一种气敏材料、应用其的一氧化碳气敏元件及制备方法”公开了一种气敏陶瓷材料，所述材料一种二氧化锡气敏材料，按质量百分比计由如下物质组成：二氧化锡88-94％，三氧化二锑1-5％，贵金属0.5-5％，金属氧化物0.5-4％，二氧化硅0.5-4％。由此可知，该技术方案中，以二氧化锡作为主材料，以三氧化二锑和贵金属作为辅助材料，金属氧化物和二氧化硅作为添加剂，合成一氧化碳气敏材料。但是在气敏材料领域，添加不同的金属氧化物作为添加剂对不同气体具有不同的灵敏度，一般二氧化锡、三氧化二锑和贵金属，特别是贵金属金，对CO气体具有很高的灵敏度，这也是现有技术，该方案中选择添加的金属氧化物和二氧化硅，反而会降低对CO气体的灵敏度，因此该气敏材料并不理想。
申请号为201210185865.0的专利文献“甲醛气敏材料及相应的甲醛气敏元件、该元件的制作方法”，公开了一种气敏陶瓷材料，所述气敏材料中含有SnO268-84wt％，In2O310-30wt％，WO31-8wt％，Pt和/或Pd1-5％，CaO1-4wt％。这也是一种利用SnO2优良的气敏半导体性能，加入其他助剂，使得SnO2能够对甲醛气体具有高度灵敏度，能够实现快速检测。
CO和H2S是有害气体，目前对于CO气体的气敏材料较多，而缺少同时对CO和H2S具有高度灵敏度的气敏材料，随着陶瓷技术和气敏半导体材料的发展，对多种有害气体同时具备高度灵敏度的气敏材料是发展趋势。
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，本发明提供一种气敏陶瓷材料及其制备方法。
本发明的技术方案：一种气敏陶瓷材料：
气敏陶瓷材料主要成分为SnO2和ZnO，SnO2的含量为65-85wt％，ZnO的含量为10-25wt％，还包括以下质量百分比的添加剂，
La2O30.3-0.8wt％；Y2O30.5-1.8wt％；Nb2O50.2-0.5wt％；TiO21.2-1.7wt％；V2O50.5-1.5wt％；ZrO20.6-1.2wt％；Cr2O30.3-0.9wt％；CeO20.5-1.1wt％。
作为优选，La2O3和Y2O3的质量之比为0.2-0.8：1。
作为优选，添加剂包括烧结助剂ThO21.1-2.7wt％。
一种气敏陶瓷材料的制备方法，制备步骤如下：
(1)准确称量各个组分，各个氧化物的纯度都在99％以上；
(2)将各个组分混合在一起，放入球磨机中进行研磨，研磨至均匀后过筛，干燥；
(3)将步骤(2)得到的混合物放入模具，进行高温煅烧，温度800-1500℃，时间2-5h；
(4)煅烧结束之后，随炉冷却至室温，取出，即制得气敏陶瓷材料。
作为优选，步骤(2)过筛筛孔的尺寸为100-200目，过筛次数为3次。
更优地，步骤(2)过筛筛孔的尺寸为200目，过筛次数为3次。
作为优选，步骤(3)中高温煅烧的温度为1000-1300℃。
更优地，步骤(4)中高温煅烧的温度为1150℃。
有益效果：本发明气敏陶瓷材料及其制备方法，是为同时对CO和H2S有害气体具备高度的灵敏度，为达到此性能，选择SnO2和ZnO两种气敏半导体材料作为主材料，其中控制SnO2的比例，太高会影响ZnO的性能，过低对于气体的灵敏度会降低，添加的金属氧化物，对材料有两个影响，第一提高气敏半导体对CO和H2S的灵敏度；第二，提高材料的机械性能和耐候性能。
另外，采用高温固相法制备上述气敏材料时，烧结温度对于两种气敏半导体具有明显影响，因此，本发明提供的制备方法中，对温度的控制极为严格，且在烧结过程中加入了烧结助剂，以改变烧结结构和温度，提供气敏半导体的性能。
因此，本发明气敏陶瓷材料及其制备方法提供的气敏陶瓷材料，对CO和H2S具有较高的灵敏度，具有响应快，测量范围宽，耐候性强等特点，是检测CO和H2S的理想气敏材料。
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：
一种气敏陶瓷材料，主要成分为SnO2和ZnO，其中SnO2的含量为85wt％，ZnO的含量为10wt％，还包括以下质量百分比的添加剂，
La2O30.3wt％；Y2O30.5wt％；Nb2O50.2wt％；TiO21.2wt％；V2O50.5wt％；ZrO20.6wt％；Cr2O30.3wt％；CeO20.5wt％；ThO21.2wt％。
一种气敏陶瓷材料的制备方法，制备步骤如下：
(1)准确称量各个组分，各个氧化物的纯度都在99％以上；
(2)将各个组分混合在一起，放入球磨机中进行研磨，研磨至均匀后过筛，筛孔的尺寸为200目，过筛次数为3次，然后干燥；
(3)将步骤(2)得到的混合物放入模具，进行高温煅烧，温度1300℃，时间3h；
(4)煅烧结束之后，随炉冷却至室温，取出，即制得气敏陶瓷材料。
实施例2：
一种气敏陶瓷材料，主要成分为SnO2和ZnO，其中SnO2的含量为65wt％，ZnO的含量为23wt％，还包括以下质量百分比的添加剂，
La2O30.8wt％；Y2O31.8wt％；Nb2O50.5wt％；TiO21.7wt％；V2O51.5wt％；ZrO20.6-1.2wt％；Cr2O30.9wt％；CeO21.1wt％；ThO22.5wt％。
一种气敏陶瓷材料的制备方法，制备步骤如下：
(1)准确称量各个组分，各个氧化物的纯度都在99％以上；
(2)将各个组分混合在一起，放入球磨机中进行研磨，研磨至均匀后过筛，筛孔的尺寸为200目，过筛次数为3次，然后干燥；
(3)将步骤(2)得到的混合物放入模具，进行高温煅烧，温度1400℃，时间3h；
(4)煅烧结束之后，随炉冷却至室温，取出，即制得气敏陶瓷材料。
实施例3：
一种气敏陶瓷材料，主要成分为SnO2和ZnO，其中SnO2的含量为72wt％，ZnO的含量为19wt％，还包括以下质量百分比的添加剂，
La2O30.6wt％；Y2O31.4wt％；Nb2O50.3wt％；TiO21.5wt％；V2O51.2wt％；ZrO21wt％；Cr2O30.5wt％；CeO20.7wt％；ThO21.8wt％。
作为优选，La2O3和Y2O3的质量之比为0.2-0.8：1。
一种气敏陶瓷材料的制备方法，制备步骤如下：
(1)准确称量各个组分，各个氧化物的纯度都在99％以上；
(2)将各个组分混合在一起，放入球磨机中进行研磨，研磨至均匀后过筛，筛孔的尺寸为200目，过筛次数为3次，然后干燥；
(3)将步骤(2)得到的混合物放入模具，进行高温煅烧，温度1150℃，时间3h；
(4)煅烧结束之后，随炉冷却至室温，取出，即制得气敏陶瓷材料。
实施例4：
一种气敏陶瓷材料，主要成分为SnO2和ZnO，其中SnO2的含量为75wt％，ZnO的含量为16wt％，还包括以下质量百分比的添加剂，
La2O30.6wt％；Y2O31.4wt％；Nb2O50.3wt％；TiO21.5wt％；V2O51.2wt％；ZrO21wt％；Cr2O30.5wt％；CeO20.7wt％；ThO21.8wt％。
一种气敏陶瓷材料的制备方法，制备步骤如下：
(1)准确称量各个组分，各个氧化物的纯度都在99％以上；
(2)将各个组分混合在一起，放入球磨机中进行研磨，研磨至均匀后过筛，筛孔的尺寸为200目，过筛次数为3次，然后干燥；
(3)将步骤(2)得到的混合物放入模具，进行高温煅烧，温度1300℃，时间3h；
(4)煅烧结束之后，随炉冷却至室温，取出，即制得气敏陶瓷材料。
实施例5：
一种气敏陶瓷材料，主要成分为SnO2和ZnO，其中SnO2的含量为71wt％，ZnO的含量为20wt％，还包括以下质量百分比的添加剂，
La2O30.8wt％；Y2O31wt％；Nb2O50.5wt％；TiO21.7wt％；V2O51wt％；ZrO21wt％；Cr2O30.5wt％；CeO20.5wt％；ThO22wt％。
一种气敏陶瓷材料的制备方法，制备步骤如下：
(1)准确称量各个组分，各个氧化物的纯度都在99％以上；
(2)将各个组分混合在一起，放入球磨机中进行研磨，研磨至均匀后过筛，筛孔的尺寸为100-200目，过筛次数为3次，然后干燥；
(3)将步骤(2)得到的混合物放入模具，进行高温煅烧，温度800℃，时间3h；
(4)煅烧结束之后，随炉冷却至室温，取出，即制得气敏陶瓷材料。
申请号为201210190973.7的专利文献“一种气敏材料、应用其的一氧化碳气敏元件及制备方法”公开的技术方案制备气敏陶瓷材料，为对照组；测定上述实施例和对照组的气体敏感性能：
(1)CO气敏性能，结果如表1所示：
表1 气敏陶瓷材料CO气敏性能
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
检测范围/ppm 10-2000 10-1500 10-1500 10-2000 10-1500 10-1200
工作温度/℃ 50-200 50-200 50-200 50-250 50-200 50-150
反应时间/s ＜7 ＜8 ＜8 ＜7 ＜8 ＜11
由上表可知，实施例1-5在的检测范围要关于对照组，其中实施例1和实施例4的检查范围最高；工作温度区间，实施例1-5优于对照组，实施例4最宽；在反应时间上，实施例1-5很明显交对照组反应快，其中实施例1和实施例4的反应时间最快。
(2)H2S气敏性能，结果如表2所示：
表2 气敏陶瓷材料H2S气敏性能
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
检测范围/ppm 10-1200 10-1500 10-1500 10-2000 10-1500 -
工作温度/℃ 50-200 50-200 50-200 50-250 50-200 -
反应时间/s ＜11 ＜8 ＜8 ＜7 ＜9 -
由表可知，对照组不能检测H2S，因此不再列明说明数据。在对H2S的检测中，实施例4的性能最优。
通过上述两个测定，实施例4在CO气敏性能和H2S气敏性能上表现均最为优异，说明本发明提供的气敏陶瓷材料对CO和H2S气体检测均具有灵敏度高、响应快和检测范围宽的优点。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)

1.一种气敏陶瓷材料，其特征在于：
气敏陶瓷材料主要成分为SnO2和ZnO，SnO2的含量为65-85wt%，ZnO的含量为10-25wt%，还包括以下质量百分比的添加剂，
La2O3 0.3-0.8wt%；Y2O3 0.5-1.8wt%；Nb2O5 0.2-0.5wt%；TiO2 1.2-1.7wt%；V2O5 0.5-1.5wt%；ZrO2 0.6-1.2wt%；Cr2O3 0.3-0.9wt%；CeO2 0.5-1.1wt%。
2.根据权利要求1所述的气敏陶瓷材料，其特征在于：La2O3和Y2O3的质量之比为0.2-0.8：1。
3.根据权利要求1所述的气敏陶瓷材料，其特征在于：添加剂包括烧结助剂ThO2 1.1-2.7wt%。
4.一种根据权利要求1-3任一项所述的气敏陶瓷材料的制备方法，其特征在于，制备步骤如下：
（1）准确称量各个组分，各个氧化物的纯度都在99%以上；
（2）将各个组分混合在一起，放入球磨机中进行研磨，研磨至均匀后过筛，干燥；
（3）将步骤（2）得到的混合物放入模具，进行高温煅烧，温度800-1500℃，时间2-5h；
（4）煅烧结束之后，随炉冷却至室温，取出，即制得气敏陶瓷材料。
5.根据权利要求4所述的气敏陶瓷材料的制备方法，其特征在于：步骤（2）过筛筛孔的尺寸为100-200目，过筛次数为3次。
6.根据权利要求5所述的气敏陶瓷材料的制备方法，其特征在于：步骤（2）过筛筛孔的尺寸为200目，过筛次数为3次。
7.根据权利要求4所述的气敏陶瓷材料的制备方法，其特征在于：步骤（3）中高温煅烧的温度为1000-1300℃。
8.根据权利要求7所述的气敏陶瓷材料的制备方法，其特征在于：步骤（3）中高温煅烧的温度为1150℃。
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