CN108863342A - 一种高密度Nb-ZnO材料的制备 - Google Patents

一种高密度Nb-ZnO材料的制备 Download PDF

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CN108863342A
CN108863342A CN201710341423.3A CN201710341423A CN108863342A CN 108863342 A CN108863342 A CN 108863342A CN 201710341423 A CN201710341423 A CN 201710341423A CN 108863342 A CN108863342 A CN 108863342A
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zno
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zno material
sintering
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沈金城
尚福亮
王晨
肖超
董磊
朱佐祥
彭伟
高玲
杨海涛
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Shenzhen University
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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Abstract

一种高密度Nb‑ZnO材料的制备。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Nb‑ZnO材料制备技术。把(0.005‑1at％)的Nb2O5与ZnO粉末经过充分混合、成型、烧结可制备出致密度超过99.8％，抗弯强度超过100MPa，电阻率小于2×10‑2Ω·cm的Nb‑ZnO材料。这种Nb‑ZnO材料，可制成溅射镀膜靶材，在显示、薄膜太阳能电池、low‑E玻璃等领域有极其广泛的应用。

Description

一种高密度Nb-ZnO材料的制备
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
ZnO薄膜作为透明导电氧化物薄膜是一种被广泛研究的功能材料。ZnO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。
透明导电ZnO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薄膜需要使用高密度靶材，通过能量束轰击靶材将其气化，再沉积到基体表面形成透明导电膜。Nb2O5掺杂ZnO能大幅度降低ZnO靶材的烧结温度，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
本发明公开了一种高密度Nb-ZnO材料的制备。把(0.001-1at％)的Nb2O5、ZnO粉末，按水∶料比为3∶1制成混合料浆，湿磨72h，干燥过筛，粉末预烧后加入5wt％的PEG-2000溶液，继续湿磨2h后，干燥过筛，然后造粒、成型、烧结。在1100℃-1250℃温度下烧结，可制备出致密度超过99.8％，抗弯强度超过100MPa，电阻率小于2×10-2Ω·cm的Nb-ZnO(NZO)靶材，这种NZO靶材，可经济、高效的制成各种复杂形状。NZO透明导电薄膜有性能稳定、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。
本发明详细研究并掌握了掺杂比、球磨参数、烧结温度等对NZO烧结致密化过程的变化规律，从而可制备出高性能的烧结NZO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1：一种高密度Nb-ZnO材料的制备工艺流程图。
下面结合附图对本发明作进一步说明：
如附图1所示，本发明的高密度Nb-ZnO材料的制备工艺流程图：先将Nb2O5、ZnO粉末和成型剂加入到球磨机中于水溶液中湿磨混合，充分混合均匀后，经干燥过筛得到充分混合的Nb-ZnO粉体，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Nb掺杂ZnO烧结材料。
本发明的优点在于用微量Nb2O5掺杂，即可大幅度降低ZnO靶材的烧结温度，提高ZnO靶材致密度，通过对Nb-ZnO粉体进行烧结，可制备出高性能烧结Nb掺杂ZnO靶材。
具体实施方式：
实例1：0.05wt％Nb-ZnO粉体的制备
将市售纯度为99.9％ZnO、Nb2O5粉末按质量比99.95∶0.05混合加入1wt％-5wt％聚乙二醇(PEG)，在水溶液中置于球磨机中湿磨24-96h，干燥过筛后，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∶Nb2O5＝99.95∶0.05的Nb-ZnO粉体。
实例2：0.05wt％Nb-ZnO粉体1100℃烧结
将制备的Nb-ZnO粉体，在100-200MPa压力下压制成型，脱成型剂后，在高温炉内1100℃下于Ar中常压烧结60-180分钟，随炉冷却。这样制得的烧结NZO靶材，密度大于5.59g/cm3，相对密度≥99.8％，抗弯强度大于100MPa，电阻率小于2.0×10-2Ω·cm。
实例3：0.05wt％Nb-ZnO粉体1200℃烧结
将制备的Nb-ZnO粉，在100-200MPa压力下压制成型，脱成型剂后，在高温炉内1200℃下于Ar中常压烧结60-180分钟，随炉冷却。这样制得的烧结NZO靶材，密度大于5.58g/cm3，相对密度≥99.6％，抗弯强度大于75MPa，电阻率小于1×10-2Ω·cm。
实例4：0.05wt％Nb-ZnO粉体1250℃烧结
将制备的Nb-ZnO粉，在100-200MPa压力下压制成型，脱成型剂后，在高温炉内1250℃下于空气中常压烧结60-180分钟，随炉冷却。这样制得的烧结NZO靶材，密度大于5.56g/cm3，相对密度≥99.2％，抗弯强度大于100MPa，电阻率小于5×10-1Ω·cm。

Claims (3)

1.一种高密度Nb-ZnO材料的制备，实验采用球磨(加成型剂)-卸料-干燥-过筛-干压成型-烧结的制备工艺流程，可制备出密度达5.59g/cm3，抗弯强度大于100MPa，电阻率小于2.0×10-2Ω·cm的高性能靶材。
2.对权利要求1所述的Nb-ZnO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Nb-ZnO粉体直接热压而得到致密Nb-ZnO材料。
3.利用权利要求1所述Nb-ZnO粉体制备的Nb-ZnO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。
CN201710341423.3A 2017-05-11 2017-05-11 一种高密度Nb-ZnO材料的制备 Pending CN108863342A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109970096A (zh) * 2019-05-08 2019-07-05 扬州新达锌业有限公司 一种高密度氧化锌加工工艺
CN110655387A (zh) * 2019-11-08 2020-01-07 先导薄膜材料（广东）有限公司 一种低密度ito靶材及其制备方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109970096A (zh) * 2019-05-08 2019-07-05 扬州新达锌业有限公司 一种高密度氧化锌加工工艺
CN110655387A (zh) * 2019-11-08 2020-01-07 先导薄膜材料（广东）有限公司 一种低密度ito靶材及其制备方法
CN110655387B (zh) * 2019-11-08 2022-05-10 先导薄膜材料（广东）有限公司 一种低密度ito靶材及其制备方法

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Application publication date: 20181123