CN107793145A - 一种MoO3包覆TZO粉体的制备及其烧结方法 - Google Patents

一种MoO3包覆TZO粉体的制备及其烧结方法 Download PDF

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CN107793145A
CN107793145A CN201610817752.6A CN201610817752A CN107793145A CN 107793145 A CN107793145 A CN 107793145A CN 201610817752 A CN201610817752 A CN 201610817752A CN 107793145 A CN107793145 A CN 107793145A
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杨海涛
高玲
尚福亮
朱佐祥
彭伟
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Abstract

一种TZO‑MoO3包覆粉末的制备及其烧结方法。本发明属于非金属元素及其化合物。本发明公开了一种新的工艺来制备MoO3掺杂TZO靶材。本发明的优点在于用一种新的掺杂工艺来代替传统的球磨掺杂，得到充分混合、均匀掺杂的粉体。适用于微量(0.2‑0.5at％)的MoO3粉末掺杂，可制备出致密度超过99.9％，强度超过120MPa，电阻率小于5.0×10‑3Ω·cm的掺杂TZO靶材，这种掺杂TZO靶材，可经济、高效的制成各种复杂形状。TZO透明导电薄膜性能稳定、制备简单、成本低廉等优势，在光电学性能平板显示领域得到了极其广泛的应用，是新一代透明导电膜，最有可能替代昂贵的ITO，在薄膜太阳能电池和low‑E玻璃等领域，正显示出巨大的应用前景和市场，是一种被广泛研究的功能材料。

Description

一种MoO3包覆TZO粉体的制备及其烧结方法
技术领域：
本发明属于无机非金属元素及其化合物。
背景技术：
TZO(氧化锌钛)薄膜是一种被广泛研究的功能材料。TZO透明导电膜性能稳定、制备简单、成本低廉，是新一代透明导电膜，有可能替代昂贵的ITO，在薄膜，在平板显示、太阳能电池、节能玻璃、智能玻璃等领域有广泛的应用前景。
TZO薄膜的制备方法主要有：物理气相沉积、化学气相沉积、溶胶-凝胶等各种方法。由于物理气相沉积制备的TZO薄膜与基体的结合强度高、沉积效率高、工艺成熟稳定而被广泛应用。而用物理气相沉积制备TZO薄膜需要使用高密度TZO靶材，通过能量束轰击TZO靶材将其气化，再沉积到基体表面形成透明导电膜。微量的MoO3掺杂能降低TZO的烧结温度，促进其烧结的致密化，提高靶材的密度、强度及导电性，从而提高镀膜质量。
发明内容：
本发明公开了一种MoO3包覆TZO粉体的制备及其烧结方法。其特征是用钼酸铵溶于水的特性，将TZO粉体在钼酸铵水溶液中湿磨，干燥后在TZO粉体表面形成分散均匀的钼酸铵包覆层，然后通过钼酸铵在100-200℃下的热解在TZO表面形成分散均匀的的MoO3包覆层，从而制备出MoO3包覆TZO粉体，实现MoO3的均匀掺杂。通过对包覆粉体的烧结，可制备出相对密度高于99.9％，强度大于150MPa，电阻率小于4.5×10-4Ω·cm的MoO3掺杂TZO烧结材料，可作为溅射镀膜用的靶材。
本发明详细研究并掌握了掺杂比、球磨参数、热解温度等对TZO-MoO3包覆粉末制备过程的影响及其烧结致密化过程的变化规律，从而可制备出高性能的烧结MoO3掺杂TZO材料。这种材料可经济、高效的制成各种复杂形状的产品，主要是溅射镀膜用的靶材(包括平面靶和旋转靶)，也可用于制造多种导电零部件。
附图说明
下面结合附图对本发明作进一步说明：
附图1：MoO3包覆TZO粉体的制备工艺流程图。
附图2：TZO-MoO3包覆粉体的烧结工艺流程图。
下面结合附图对本发明作进一步说明：
如附图1所示，本发明的MoO3包覆TZO粉体的制备工艺流是：先将ZnO、TiO2粉末加入到球磨机中于钼酸铵水溶液中湿磨混合，充分混合均匀后，经干燥过筛得到在TZO粉体表面形成分散均匀的钼酸铵包覆层的混合料，将混合料于100-200℃加热，通过钼酸铵热解在TZO粉体表面形成分散均匀的的MoO3包覆层，从而制备出MoO3包覆TZO粉体。
如附图2所示，将MoO3包覆TZO粉体，加入成形剂聚乙二醇(PEG)，然后成型(干压、冷等静压、注射成型等)，得到生坯，经脱成型剂后，即可进行常压烧结或气压烧结，得到高强度高密度的MoO3掺杂TZO烧结材料。
本发明的优点在于用一种新的方法制备MoO3包覆TZO粉体，特别适用于微量MoO3掺杂，通过对MoO3包覆TZO粉体进行烧结，可制备出高性能烧结MoO3掺杂TZO材料。
具体实施方式：
实例1：0.2wt％MoO3包覆TZO粉体的制备
将市售纯度为99.9％ZnO、TiO2粉末按质量比99∶1混合，在用0.23wt％钼酸铵配制的水溶液中置于球磨机中湿磨24-96h，干燥过筛后，将粉体置于100-200℃的炉子中，钼酸铵热解生成MoO3包覆住ZnO、TiO2，得到各种粉料充分混合、粒径分布均匀、成型性好、各组分质量比为ZnO∶TiO2∶MoO3＝98.8∶1.0∶0.2的WO3包覆TZO粉体。
实例2：0.5wt％MoO3包覆TZO粉体的制备
将市售纯度为99.9％ZnO、TiO2粉末按质量比98∶1.5混合，在用0.57wt％钼酸铵配制的水溶液中置于球磨机中湿磨24-96h，干燥过筛后，将粉体置于100-200℃的炉子中，钼酸铵热解生成MoO3包覆住ZnO、TiO2，得到各种粉料充分混合、粒径分布均匀、成型性好、各组分质量比为ZnO∶TiO2∶MoO3＝98.5∶1.0∶0.5的MoO3包覆TZO粉体。
实例3：0.2wt％MoO3包覆TZO粉体的烧结
将制备的MoO3包覆TZO粉，掺1-5wt％聚乙二醇(PEG)作为成型剂，于球磨机中湿磨2h，再干燥过筛，在100-200MPa压力下压制成型，脱成型剂后，在高温炉内1400℃下于空气中常压烧结60-180分钟，随炉冷却。这样制得的烧结MoO3包覆TZO靶材，密度大于5.55g/cm3，相对密度≥99.2％，强度大于130MPa，电阻率小于8×10-4Ω·cm。
实例4：0.5wt％MoO3包覆TZO粉体的烧结
将制备的MoO3包覆TZO粉，掺1-5wt％聚乙二醇(PEG)作为成型剂，于球磨机中湿磨2h，再干燥过筛，在100-200MPa压力下压制成型，脱成型剂后，在高温炉内1380℃下于空气中常压烧结60-180分钟，随炉冷却。这样制得的烧结MoO3包覆TZO靶材，密度大于5.56g/cm3m，相对密度≥99.6％，强度大于120MPa，电阻率小于8×10-4Ω·cm。

Claims (4)

1.一种新的方法制备MoO3包覆TZO(氧化锌钛)粉体，其特征是用钼酸铵((NH4)6Mo7O24·4H2O)溶于水的特性，将TZO粉体在钼酸铵水溶液中湿磨，干燥后在TZO粉体表面形成分散均匀的钼酸铵包覆层，然后通过钼酸铵在100-200℃下的热解在TZO表面形成分散均匀的的MoO3包覆层，从而制备出MoO3包覆TZO粉体，实现MoO3的均匀掺杂。
2.对权利要求1所述的MoO3包覆TZO粉体，通过加成型剂-干燥-过筛-成型-烧结等工序，可制备出密度高于5.5g/cm3，抗弯强度大于100MPa，电阻率小于8×10-4Ω·cm的高性能高致密MoO3掺杂TZO材料。
3.对权利要求1所述的MoO3包覆TZO粉体的烧结，既可采用常压烧结工艺，也适用于气压烧结工艺，另外也可将权利要求1所述的MoO3包覆TZO粉体直接热压而得到致密MoO3掺杂TZO材料。
4.利用权利要求1所述的MoO3包覆TZO粉体制备的致密MoO3掺杂TZO材料，可制成各种复杂形状的制品，主要是溅射镀膜用的靶材(包括平面靶和旋转靶)，也可用于制造其它多种导电零部件。
CN201610817752.6A 2016-09-07 2016-09-07 一种MoO3包覆TZO粉体的制备及其烧结方法 Pending CN107793145A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112479683A (zh) * 2020-12-17 2021-03-12 中山智隆新材料科技有限公司 一种掺杂的igzo材料的制备方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112479683A (zh) * 2020-12-17 2021-03-12 中山智隆新材料科技有限公司 一种掺杂的igzo材料的制备方法

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