硅酸盐学报

高致密铟锡氧化物管状靶材的成型及性能

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文浪 ¹ , 赵天豪 ¹ , 徐华蕊 ¹ , 龙神峰 ¹ , 吴芳洲 ¹ , 许积文 ¹ , 朱归胜 ¹ , 黄誓成 ²

硅酸盐学报 | 研究论文 2025,53(8): 2239-2247

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硅酸盐学报 |研究论文 2025 , 53 (8) : 2239 -2247

高致密铟锡氧化物管状靶材的成型及性能

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文浪¹, 赵天豪¹, 徐华蕊¹, 龙神峰¹, 吴芳洲¹, 许积文¹, 朱归胜¹, 黄誓成²

作者信息

^1．桂林电子科技大学材料科学与工程学院，电子信息材料与器件教育部工程研究中心，广西信息材料重点实验室，广西桂林 541000

^2．广西晶联光电材料有限责任公司，广西柳州 545036

通讯作者:

朱归胜（1981—），男，博士，教授。

作者简介:

文浪（1998—），男，硕士研究生。

Molding and Performance of Highly Dense Indium Tin Oxide Tubular Targets

Lang WEN¹, Tianhao ZHAO¹, Huarui XU¹, Shenfeng LONG¹, Fangzhou WU¹, Jiwen XU¹, Guisheng ZHU¹, Shicheng HUANG²

Affiliations

^1.Guangxi Key Laboratory of Information Materials, Engineering Research Center of Electronic Information Materials and Devices, Ministry of Education, School of Materials Science and Engineering, Guilin University of Electronic Technology, Guilin 541004, Guangxi, China

^2.Guangxi Jinglian Photoelectric Material Co., Ltd, Liuzhou 545036, Guangxi, China

Corresponding Author:

ZHU Guisheng (1981-), male, Ph.D., Professor. E-mail: Zhuguisheng@guet.edu.cn

WEN Lang (1998-), male, Master candidate. E-mail: 15878397086@163.com

出版时间: 2025-08-20 doi: 10.14062/j.issn.0454-5648.20250017

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摘要

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高性能铟锡氧化物（ITO）靶材是平板显示、太阳能光伏电池的关键材料，制备出高致密、组织均匀的ITO素坯是制备高性能ITO靶材的关键，其中ITO靶材的成型尤为重要。本工作采用二元颗粒级配-喷雾造粒-冷等静压成型工艺，研究了不同颗粒级配比例、成型压力、保压时间和成型工艺对粉体、素坯和靶材性能的影响。结果表明：颗粒级配适当地提高了粉体密度，喷雾造粒适当地提高了粉体球形度，适当提高成型压力、延长保压时间能明显提升坯体密度。经复合式压制工艺在200 MPa保压9 min制备了相对密度为62.52%的素坯，通过烧结得到相对密度为99.85%、电阻率为1.333×10^-4 Ω·cm的ITO管状靶材。

关键词

铟锡氧化物 / 中空管状靶材 / 高致密度 / 冷等静压成型

Abstract

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Introduction

Indium tin oxide (ITO) film is an excellent transparent conductive material widely used in liquid crystal displays (LCDs), electroluminescent displays (EL/OLEDs) and various photovoltaic devices. In particular, heterojunction (HJT) solar cells have shown a broader development potential. In order to improve the photovoltaic conversion efficiency of heterojunction solar cells, transparent conductive films need to be deposited on curved or cylindrical solar collectors. The deposition of ITO conductive films on these non-planar substrates requires specially shaped ITO tubular targets as the deposition source. Therefore, the preparation of high-quality ITO tubular targets is a prerequisite for obtaining ITO films with excellent properties on curved or cylindrical substrates, and the shaping and high densification of ITO tubular targets have been a hot and difficult issue in this field. In this work, based on the theoretical model of binary particle grading and the composite spray granulation-cold isostatic pressing moulding process route, the effects of different grading ratios, moulding pressures, times and processes on the properties of powders, billets and targets were investigated.

Methods

In₂O₃ and SnO₂ powders (purity 99.99%, Hunan Ruyang Ruijin Electronic Technology Co., Ltd.) were ball-milled at a mass ratio of 9∶1 to formulate indium tin oxide powders with D₅₀ (the particle size corresponding to the cumulative particle size distribution percentage of the samples reaching 50%) of 50 nm and 323 nm, respectively, and were mixed in accordance with different grade ratios. After mixing, anhydrous ethanol (analytically pure, Xilong Science Co., Ltd.) was added to disperse the powder in a ball milling tank, and the mass ratio of zirconia balls to powder in the slurry was 3∶1, and the slurry was mixed and then milled in a planetary ball mill at 350 r/min for 8 h. The slurry was obtained at an inlet temperature of 190 ℃, with a slurry solids content of 60% (mass fraction) and 1.5% binder content, Spray granulation was carried out at a feed rate of 100 mL/h. The granulated powder was loaded into a cold isostatic pressing mould with an inner diameter of 6 mm and a length of 39 mm, and then fully vibrated and consolidated before bagging and sealing for vacuum treatment and cold isostatic pressing. The total holding time of the composite pressing curve was the same as that of the single-point pressing curve. The hollow tubular blanks were sintered in a tube furnace at a flow rate of 5 L/min in an oxygen atmosphere, at sintering temperature of 1550 ℃ and holding time of 8 h to produce ITO tubular targets.

X-ray diffractometer (XRD, D8 Advance, Bruker) was used to study the phase structure. Scanning electron microscope (SEM, Tecnai-450, FEI) was used to observe the microstructure and elemental distribution with an operating voltage of 8 kV. The particle size distribution of the powders was tested using a laser particle size analyser model LS-609 from Omec. The loose packing density of the powders was tested using a WLD-02 Hall flow meter (funnel method). The density of ITO target was tested by Archimedes method and compared with the theoretical density to calculate the relative density of ITO target. The resistivity was measured by a four-point probe meter (MCP-T700, Mitsubishi chemical).

Results and discussion

Based on the tightest stacking theory model, the stacking density of ITO powder is significantly improved by binary particle grading, because a reasonable grading ratio can achieve the fine particles to fill the gaps between the larger particles, which effectively improves the loose loading density of ITO powder.

The study of ITO tubular target prepared by cold isostatic pressing technology shows that the densification process of billet and target by forming pressure presents three-stage characteristics: Stage 1, the loose powder is rapidly rearranged under extrusion, with narrowing particle gaps and increasing bulk density, resulting in a lower resistivity; Stage 2, the resistance of internal friction between the particles increases, and the rate of densification tends to slow down; Stage 3, when the pressure exceeds the critical value (the limit), the particle plastic deformation or fragmentation occurs. deformation stress), the particles undergo plastic deformation or fragmentation, and the pores are further filled, but too high a pressure will form a pressure gradient due to the friction between the billet and the mould, which may, on the contrary, trigger internal slip leading to a decrease in density. The effect of holding time showed that within 5-11 min, extending the holding time significantly increased the relative density, which was attributed to the full displacement of the powder to fill the pores and the deformation of the particles, which increased the contact area and the interaction force; after more than 11 min, the pore filling tended to be saturated, and the density growth was stagnant. The composite pressing process effectively discharges the residual gas inside the billet through staged pressure release, eliminating the gas compression reaction force and achieving better densification results. The study reveals the key mechanism of cold isostatic pressure parameters on the microstructure regulation of ITO targets.

Conclusions

In this work, the effects of different grading ratios, moulding pressures, times and processes on the properties of powders, blanks and targets were investigated using a binary particle grading-spray granulation-cold isostatic pressing process. The results showed that particle grading improved the density of the powder, spray granulation improved the sphericity of the powder, and increasing the moulding pressure and prolonging the holding time improved the density of the billet. The billet with a relative density of 62.52% was prepared by the composite pressing process at a holding pressure of 200 MPa for 9 min, and the ITO tubular target with a relative density of 99.85% and a resistivity of 1.333×10^-4 Ω·cm was obtained by sintering.

Key words

indium tin oxide / hollow tubular target / high density / cold isostatic pressing

引用本文

文浪, 赵天豪, 徐华蕊, 龙神峰, 吴芳洲, 许积文, 朱归胜, 黄誓成. 高致密铟锡氧化物管状靶材的成型及性能. 硅酸盐学报, 2025 , 53 (8) : 2239 -2247 . DOI: 10.14062/j.issn.0454-5648.20250017

Lang WEN, Tianhao ZHAO, Huarui XU, Shenfeng LONG, Fangzhou WU, Jiwen XU, Guisheng ZHU, Shicheng HUANG. Molding and Performance of Highly Dense Indium Tin Oxide Tubular Targets[J]. Journal of the Chinese Ceramic Society, 2025 , 53 (8) : 2239 -2247 . DOI: 10.14062/j.issn.0454-5648.20250017

基金

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国家自然科学基金(U21A2065; 62354007)
广西科技基地与人才专项(AD23023013)
广西科技重大专项资助(AA21077018)
桂林市创新平台和人才计划(20220120-1)

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2025年第53卷第8期

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文章信息

doi: 10.14062/j.issn.0454-5648.20250017

接收时间：2025-01-08
首发时间：2026-10-21
出版时间：2025-08-20

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出版历史

收稿日期：2025-01-08
修回日期：2025-03-18

基金

国家自然科学基金(U21A2065; 62354007)

广西科技基地与人才专项(AD23023013)

广西科技重大专项资助(AA21077018)

桂林市创新平台和人才计划(20220120-1)

作者信息

^1．桂林电子科技大学材料科学与工程学院，电子信息材料与器件教育部工程研究中心，广西信息材料重点实验室，广西桂林 541000

^2．广西晶联光电材料有限责任公司，广西柳州 545036

通讯作者:

朱归胜（1981—），男，博士，教授。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20250017

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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