CN116768604A - 一种高密度izto靶材的制备方法 - Google Patents
一种高密度izto靶材的制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 81
- 238000000498 ball milling Methods 0.000 claims abstract description 37
- 239000011787 zinc oxide Substances 0.000 claims abstract description 34
- 238000005245 sintering Methods 0.000 claims abstract description 33
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 22
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 20
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 20
- 239000007921 spray Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000013077 target material Substances 0.000 claims abstract description 10
- 238000004321 preservation Methods 0.000 claims abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005469 granulation Methods 0.000 claims abstract description 8
- 230000003179 granulation Effects 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- 239000001301 oxygen Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 229910001868 water Inorganic materials 0.000 claims description 17
- 239000002002 slurry Substances 0.000 claims description 14
- 210000001161 mammalian embryo Anatomy 0.000 claims description 9
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 7
- 239000011324 bead Substances 0.000 claims description 7
- 238000005056 compaction Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052726 zirconium Inorganic materials 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 102220043159 rs587780996 Human genes 0.000 claims description 2
- 238000000462 isostatic pressing Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 21
- 239000010408 film Substances 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 7
- 239000010409 thin film Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000007405 data analysis Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- HRHKULZDDYWVBE-UHFFFAOYSA-N indium;oxozinc;tin Chemical compound [In].[Sn].[Zn]=O HRHKULZDDYWVBE-UHFFFAOYSA-N 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920001621 AMOLED Polymers 0.000 description 1
- 230000005355 Hall effect Effects 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001552 radio frequency sputter deposition Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 1
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
本发明涉及靶材技术领域，具体涉及一种高密度IZTO靶材的制备方法，所述制备方法包括如下步骤：S1原材料选择、S2氧化锌球磨、S3混合球磨、S4喷雾造粒、S5压力成型、S6靶材烧结。本发明选用特定BET值的氧化铟、氧化锡和氧化锌作为原材料，通过搅拌球磨使粉末混合均匀，经离心式喷雾造粒机干燥造成IZTO粉末，再使用等静压成型机将IZTO粉末压缩成素胚，然后在常压氧气气氛下进行烧结处理，控制升温速率和保温时间以实现高密度靶材的制备。与传统工艺相比，该方案可大幅度提高靶材的密度和均匀性，具有显著的应用价值。
Description
技术领域
本发明涉及靶材技术领域，尤其涉及一种高密度IZTO靶材的制备方法。
背景技术
近年来，液晶显示(LCD)、有源有机发光二极管显示(AMOLED)以及柔性显示等平板显示技术迅猛发展，作为核心部件的薄膜晶体管(thin-film transistors，TFT)的重要性不言而喻。其中，基于氧化物半导体的TFT以其高的载流子浓度、良好的电学均匀性、高的可见光透过性、较低的成本等优势受到学界和产业界的广泛关注。
TFT中半导体层的性能很大程度上决定了整个器件的性能，在氧化物半导体中，铟锌锡氧化物(IZTO)半导体具有大的禁带宽度(＞3ev)，可满足大尺寸、高分辨率、高开口率等显示要求，具有极大的应用潜力。然而，制备高迁移率、高密度、均匀性好的IZTO薄膜是一项挑战，主要是由于IZO薄膜的材料特性和制备过程的复杂性。其中，靶材作为制备薄膜的关键原材料，对薄膜质量和性能具有重要影响。传统的IZTO靶材制备方法主要有物理气相沉积(PVD)、射频磁控溅射(RF sputtering)等，但也存在一些问题，如靶材密度低、均匀性差、组分不稳定等。
发明内容
有鉴于此，本发明的目的在于提出一种高密度IZTO靶材的制备方法，以得一种高密度的IZTO靶材。
基于上述目的，本发明提供了一种高密度IZTO靶材的制备方法，具体制备步骤如下：
S1原材料选择：氧化铟的BET为5-10m2/g，氧化锡的BET为10-15m2/g，氧化锌的BET为10-20m2/g；
S2氧化锌球磨：在装有φ1-2mm锆珠的球磨罐中加入纯水和氧化锌，纯水加入量与氧化锌的加入量相同，球磨时间16-24h，得到氧化锌浆料；
S3混合球磨：在氧化锌浆料中加入纯水、氧化铟和氧化锡，纯水加入量与氧化铟的加入量相同，球磨时间24-48h，得到IZTO浆料；
S4喷雾造粒：将IZTO浆料使用离心式喷雾造粒机进行干燥造粒，进风温度200-230℃，出风温度80-100℃，得到IZTO粉末；
S5压力成型：将IZTO粉末装入模具中进行等静压成型，成型压力280-300MPa，得到IZTO素胚；
S6靶材烧结：将IZTO素胚放入常压氧气气氛高温烧结炉中进行烧结，烧结温度1450℃，保温时间20-40h，其中1300℃到1450℃的升温速率为0.03-0.05℃/min，得到高密度IZTO靶材。
其中，所述步骤S1中氧化铟质量百分比为40％-60％、氧化锡质量百分比为5％-10％和氧化锌质量百分比为30％-55％，氧化铟、氧化锡和氧化锡的氧化锡质量百分比总和为100％。
其中，所述步骤S4中IZTO粉末额的粒径D50＝35-50um，松装密度1.2-1.5g/cm3。
其中，所述步骤S5中IZTO素胚的内径为155-160mm，外径为190-200mm。
其中，所述步骤S6中高密度IZTO靶材的相对密度为99.91-99.95％，晶粒尺寸为3-3.2um。
进一步的，本发明提供了一种高密度IZTO靶材，所述高密度高迁移率IZTO靶材根据上述高密度IZTO靶材的制备方法得到。
进一步的，本发明提供了一种高密度IZTO靶材在薄膜晶体管上的应用。
本发明的有益效果：
本发明提供了一种高密度IZTO靶材的制备方法，采用了高比表面积的氧化锌，通过预磨的方式降低氧化锌的粒径，提高烧结活性，并且氧化铟和氧化锡在氧化锌预磨后加入，分散更为均匀。
本发明提供了一种高密度IZTO靶材的制备方法，在烧结规程中，将1300℃到最高温度1450℃的升温速率控制在0.03-0.05℃/min，在该温度区间慢速升温可以使氧化铟锌反应完全，先形成Zn3In2O6相，再通过高温保温使靶材内部气孔闭合，有助于提高靶材密度，并且采用本发明的高密度IZTO靶材制备的半导体薄膜具有较高的迁移率。
综上，本发明通过采用BET 10-20m2/g的氧化锌粉末，采用先预球磨氧化锌的方式使高活性纳米氧化锌均匀和氧化铟锡混合，通过烧结过程中1300℃以上进行慢速升温，使氧化铟锌锡充分反应，得到高密度的IZTO靶材。
附图说明
为了更清楚地说明本发明或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本发明实施例1制备的IZTO靶材断面SEM图片。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚明白，以下结合具体实施例，对本发明进一步详细说明。
实施例1
一种高密度的IZTO靶材，具体制备方法如下：
S1原材料选择：氧化铟的BET为7.5m2/g，氧化锡的BET为11.8m2/g，氧化锌的BET为10.5m2/g；
S2氧化锌球磨：在装有φ1mm锆珠的球磨罐中加入30g纯水和30g氧化锌，球磨时间16h，得到氧化锌浆料；
S3混合球磨：在氧化锌浆料中加入60g纯水、60g氧化铟和10g氧化锡，球磨时间24h，得到IZTO浆料；
S4喷雾造粒：将IZTO浆料使用离心式喷雾造粒机进行干燥造粒，进风温度200℃，出风温度80℃，得到IZTO粉末；
S5压力成型：将IZTO粉末装入模具中进行等静压成型，成型压力280Mpa，得到内径为155mm，外径为190mm的IZTO素胚；
S6靶材烧结：将IZTO素胚放入常压氧气气氛高温烧结炉中进行烧结，烧结温度1450℃，保温时间20h，其中1300℃到1450℃的升温速率为0.03℃/min，得到高密度IZTO靶材。
实施例2
一种高密度的IZTO靶材，具体制备方法如下：
S1原材料选择：氧化铟的BET为7.5m2/g，氧化锡的BET为11.8m2/g，氧化锌的BET为15.4m2/g；
S2氧化锌球磨：在装有φ2mm锆珠的球磨罐中加入40g纯水和40g氧化锌，球磨时间20h，得到氧化锌浆料；
S3混合球磨：在氧化锌浆料中加入50g纯水、50g氧化铟和10g氧化锡，球磨时间36h，得到IZTO浆料；
S4喷雾造粒：将IZTO浆料使用离心式喷雾造粒机进行干燥造粒，进风温度210℃，出风温度90℃，得到IZTO粉末；
S5压力成型：将IZTO粉末装入模具中进行等静压成型，成型压力280Mpa，得到内径为160mm，外径为195mm的IZTO素胚；
S6靶材烧结：将IZTO素胚放入常压氧气气氛高温烧结炉中进行烧结，烧结温度1450℃，保温时间20h，其中1300℃到1450℃的升温速率为0.04℃/min，得到高密度IZTO靶材。
实施例3
一种高密度的IZTO靶材，具体制备方法如下：
S1原材料选择：氧化铟的BET为7.5m2/g，氧化锡的BET为11.8m2/g，氧化锌的BET为19.4m2/g；
S2氧化锌球磨：在装有φ2mm锆珠的球磨罐中加入55g纯水和55g氧化锌，球磨时间24h，得到氧化锌浆料；
S3混合球磨：在氧化锌浆料中加入40g纯水、40g氧化铟和5g氧化锡，球磨时间48h，得到IZTO浆料；
S4喷雾造粒：将IZTO浆料使用离心式喷雾造粒机进行干燥造粒，进风温度230℃，出风温度100℃，得到IZTO粉末；
S5压力成型：将IZTO粉末装入模具中进行等静压成型，成型压力300Mpa，得到内径为160mm，外径为200mm的IZTO素胚；
S6靶材烧结：将IZTO素胚放入常压氧气气氛高温烧结炉中进行烧结，烧结温度1450℃，保温时间40h，其中1300℃到1450℃的升温速率为0.05℃/min，得到高密度IZTO靶材。
对比例1
对比例1与实施例1的不同在于：1300℃到1450℃的升温速率为0.5℃/min。
对比例2
对比例2与实施例1的不同在于：1300℃到1450℃的升温速率为1℃/min。
对比例3
对比例3与实施例1的不同在于：1300℃到1450℃的升温速率为3℃/min。
对比例4
对比例4与实施例1的不同在于：氧化锌的BET为7.4m2/g；
对比例5
一种IZTO靶材，具体制备方法如下：
S1原材料选择：氧化铟的BET为7.5m2/g，氧化锡的BET为11.8m2/g，氧化锌的BET为10.5m2/g；
S2混合球磨：在装有φ1mm锆珠的球磨罐中加入90g纯水、30g氧化锌、60g氧化铟和10g氧化锡，球磨时间24h，得到IZTO浆料；
S3喷雾造粒：将IZTO浆料使用离心式喷雾造粒机进行干燥造粒，进风温度200℃，出风温度80℃，得到IZTO粉末；
S4压力成型：将IZTO粉末装入模具中进行等静压成型，成型压力280Mpa，得到内径为155mm，外径为190mm的IZTO素胚；
S5靶材烧结：将IZTO素胚放入常压氧气气氛高温烧结炉中进行烧结，烧结温度1450℃，保温时间20h，其中1300℃到1450℃的升温速率为0.03℃/min，得到IZTO靶材。
对比例6
一种IZO靶材，具体制备方法如下：
S1原材料选择：氧化铟的BET为7.5m2/g，氧化锌的BET为10.5m2/g；
S2氧化锌球磨：在装有φ2mm锆珠的球磨罐中加入40g纯水和40g氧化锌，球磨时间20h，得到氧化锌浆料；
S3混合球磨：在氧化锌浆料中加入50g纯水、50g氧化铟，球磨时间36h，得到IZO浆料；
S4喷雾造粒：将IZO浆料使用离心式喷雾造粒机进行干燥造粒，进风温度210℃，出风温度90℃，得到IZO粉末；
S5压力成型：将IZTO粉末装入模具中进行等静压成型，成型压力280Mpa，得到内径为160mm，外径为195mm的IZO素胚；
S6靶材烧结：将IZTO素胚放入常压氧气气氛高温烧结炉中进行烧结，烧结温度1450℃，保温时间20h，其中1300℃到1450℃的升温速率为0.03℃/min，得到IZO靶材。
性能测试
表1实施例1-3，对比例1-5制备的靶材的相对密度和晶粒尺寸
数据分析：从实施例1-3可以看出，本发明制备的靶材具有超高的相对密度，从实施例1和对比例1-3可以看出，温度区间慢速升温有助于超高密度靶材的生成，从实施例1和对比例4-5可以看出，高比表面积的氧化锌和氧化锌的预磨有助于超高密度靶材的生成，从实施例1和对比例6可以看出，氧化锡的引入对于超高密度靶材的生成具有至关重要的作用。
半导体薄膜制备：
使用实施例1和对比例1-3、6的靶材制备半导体薄膜，采用脉冲直流磁控溅射技术，在玻璃衬底沉积半导体薄膜，使用霍尔效应测试其迁移率，磁场5000高斯，温度300K，测试结果如表2所示。
表2实施例1、对比例1-3靶材制备的薄膜的迁移率
| 迁移率/cm2/Vs | |
| 实施例1 | 43.0 |
| 对比例1 | 28.5 |
| 对比例2 | 24.3 |
| 对比例3 | 22.4 |
| 对比例6 | 25.4 |
数据分析：从实施例1和对比例1-3、6可以看出，采用本发明制备方法得到的靶材制备的薄膜具有较高的迁移率，温度区间慢速升温有助于较高迁移率薄膜的制备。
所属领域的普通技术人员应当理解：以上任何实施例的讨论仅为示例性的，并非旨在暗示本发明的范围(包括权利要求)被限于这些例子；在本发明的思路下，以上实施例或者不同实施例中的技术特征之间也可以进行组合，步骤可以以任意顺序实现，并存在如上所述的本发明的不同方面的许多其它变化，为了简明它们没有在细节中提供。
本发明旨在涵盖落入所附权利要求的宽泛范围之内的所有这样的替换、修改和变型。因此，凡在本发明的精神和原则之内，所做的任何省略、修改、等同替换、改进等，均应包含在本发明的保护范围。
Claims (6)
1.一种高密度IZTO靶材的制备方法，其特征在于，具体制备步骤如下：
S1原材料选择：氧化铟的BET为5-10m2/g，氧化锡的BET为10-15m2/g，氧化锌的BET为10-20m2/g；
S2氧化锌球磨：在装有φ1-2mm锆珠的球磨罐中加入纯水和氧化锌，纯水加入量与氧化锌的加入量相同，球磨时间16-24h，得到氧化锌浆料；
S3混合球磨：在氧化锌浆料中加入纯水、氧化铟和氧化锡，纯水加入量与氧化铟的加入量相同，球磨时间24-48h，得到IZTO浆料；
S4喷雾造粒：将IZTO浆料使用离心式喷雾造粒机进行干燥造粒，进风温度200-230℃，出风温度80-100℃，得到IZTO粉末；
S5压力成型：将IZTO粉末装入模具中进行等静压成型，成型压力280-300MPa，得到IZTO素胚；
S6靶材烧结：将IZTO素胚放入常压氧气气氛高温烧结炉中进行烧结，烧结温度1450℃，保温时间20-40h，其中1300℃到1450℃的升温速率为0.03-0.05℃/min，得到高密度IZTO靶材。
2.根据权利要求1所述的高密度IZTO靶材的制备方法，其特征在于，所述步骤S1中氧化铟质量百分比为40％-60％、氧化锡质量百分比为5％-10％和氧化锌质量百分比为30％-55％，氧化铟、氧化锡和氧化锡的氧化锡质量百分比总和为100％。
3.根据权利要求1所述的高密度IZTO靶材的制备方法，其特征在于，所述步骤S4中IZTO粉末额的粒径D50＝35-50um，松装密度＝1.2-1.5g/cm3。
4.根据权利要求1所述的高密度IZTO靶材的制备方法，其特征在于，所述步骤S5中IZTO素胚的内径为155-160mm，外径为190-200mm。
5.根据权利要求1所述的高密度IZTO靶材的制备方法，其特征在于，所述步骤S6中高密度IZTO靶材的相对密度为99.91-99.95％，晶粒尺寸为3-3.2um。
6.一种高密度IZTO靶材，其特征在于，所述高密度IZTO靶材根据权利要求1-5任一项所述的高密度IZTO靶材的制备方法得到。
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