Fabrication Ceramics Target and Transparent Conductive Oxide Films on Flexible Substrates

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Project title

Code/計畫編號

MOST108-2218-E262-001

Translated Name/計畫中文名

製備氧化鋅陶瓷靶材及透明導電膜於可撓性基材之研究

Project Coordinator/計畫主持人

Jihng-Kuo Ho

Funding Organization/主管機關

National Science and Technology Council

Co-Investigator(s)/共同執行人

許春耀

Department/Unit

Department of Mechanical Engineering,LHU

Website

https://www.grb.gov.tw/search/planDetail?id=13238740

Year

2019

Start date/計畫起

01-08-2019

Expected Completion/計畫迄

30-09-2020

Bugetid/研究經費

618千元

ResearchField/研究領域

機械工程

Transparent conducting oxide (TCO) film with optical transmission of more than 85% in the visible region and resistivity of less than 10-4 Ω-cm is used in various technological fields such as transparent electrodes, solar cells, gas sensors, piezoelectric transducers and surface acoustic wave devices. Tin-doped indium oxide has been the most popular commercial TCO material due to its excellent electrical and optical performance. Because of indium is toxic, rare and expensive, the development of alternative TCO materials is essential to solve this problem. Recently, zinc oxide (ZnO), an alternative TCO material, has received considerable attention due to its various advantages, such as its abundance in nature, non-toxicity and good stability in hydrogen plasma processes as compared to ITO and SnO2 films. In addition, ZnO can be doped with a wide variety of ions to meet the demands of several application fields. In order to increase its electrical and optical characteristics, ZnO is commonly doped with Group III elements, which have been reported as effective dopants for zinc oxide based films. In the research, sintering Al2O3-doped ZnO (AZO, Al2O3 1~2wt%), Ga2O3-doped ZnO (GZO, Ga2O3 1~2wt%), TiO2-doped ZnO (TZO, TiO2 1~2wt%), Al2O及Ga2O3- Co-doped ZnO (AGZO, Al2O and Ga2O3 1~2wt%) ceramics target was investigated. Process variables include types of powder, milling time, preload, uprising rate of temperature, holding temperature, holding time, holding load, descending rate of temperature. The Taguchi method which combine the experiment design theory and the quality loss function concept have been applied to the robust design of products and process and have solved some confusing problems in manufacturing. The optimal sintering parameters are determined through experiments planned, conducted and analysed using the Taguchi method. The experimental studies were conducted under different heating rates (1, 4, 8 oC /min), holding temperatures (1000, 1200, 1400 oC), holding pressure (1200, 1400, 2000 kg), holding time (3, 5, 8 hr) and cooling rates (10, 30, 60 oC /min). Taguchi method was used for executing the experiment, employing a generic signal-to-noise (S/N) ratio to quantify the present variation. The use of a grey-based Taguchi method to determine the deposition parameters of AZO, GZO, TZO, AGZO transparent conductive oxide film coated tools has been studied by considering multiple performance characteristics. A Taguchi method with the AZO, GZO, TZO, AGZO transparent conductive oxide film coated flexible substrates orthogonal array, signal-to-noise (S/N) ratio, and analysis of variance (ANOVA) is employed to investigate the performance characteristics in the deposition operations. The effect and optimization of AZO, GZO, TZO, AGZO transparent conductive oxide films deposition parameters: rf power (50, 100, 200 W), working pressure (10, 15, 20 mtorr), deposition time (25, 50, 70 min) and O2/(O2 + Ar) flow-rate ratios (10, 20, 30%) on the electrical, structural, morphological and optical properties of AZO, GZO, TZO, AGZO films was investigated. 透明導電膜用途廣泛，需求量大，值得投入經費研究。氧化銦摻雜錫(indium tin oxide , ITO) 透明導電膜，光、電性優良，製程成熟，但是ITO中的In元素產量有限，In元素有毒、價格昂貴、化學穩定性低、高溫應用不穩定象。與ITO 薄膜在光、電特性相抗衡的氧化鋅(ZnO)受到極大重視。本計畫的目的為靶材壓製及燒結研究，包括:Al2O3-doped ZnO (AZO), Ga2O3-doped ZnO (GZO)，TiO2-doped ZnO (TZO)，Al2O及Ga2O3- Co-doped ZnO (AGZO)等4種靶材。探討靶材燒結參數，包括: 升溫速率: 1、4、8 (oC /min)、持壓溫度: 1000、1200、1400 (oC)、持壓荷重: 1200、1400、2000 (kg)、持壓時間: 3、5、8 (hr)、降溫速率: 10、30、60 (oC /min)。靶材製作步驟包括:1.配粉(粉末依標準計量，並加入去離子及分散劑)。2. 球磨(粉末置入球磨罐中，進行球磨作業)。3烘乾(漿料烘乾，溫度為150°C，時間為24 hr)。4過篩研磨形成粉末，過篩得到粒度均勻細粉)。5.壓製生胚(離散劑)噴附於圓柱模具內，使粉末均勻，壓擠，保壓，獲得生胚。6. 燒結。本計畫以燒結完成的靶材(AZO, GZO, TZO, AGZO)應用射頻磁控濺鍍系統，沉積透明導電膜於可撓性塑膠(PET, PC)。田口實驗設計(Taguchi methods) L9 (34)直交表，探討製程參數: rf 功率 (100, 150, 200 W)、製程壓力 (10, 15, 20 mtorr)、沉積時間 (25, 50, 70 min)、氬氧比例 (10, 20, 30%)。分析AZO, GZO, TZO, AGZO透明導電膜沉積速率、電阻率、可見光穿透率、載子濃度與電子遷移率、結晶性、微結構(SEM、HRTEM、AFM、X-Ray、TEM)、薄膜附着性。訊號雜訊比(signal-noise ratio)及變異數分析(ANOVA)，獲得影響AZO, GZO, TZO, AGZO 透明導電膜沉積參數的重要因子。應用田口-灰關聯分析，獲得最佳AZO, GZO, TZO, AGZO透明導電膜沉積製程參數，完成實驗驗証及再現性測試，期望取代市售ITO透明導電膜。

Keyword(s)

transparent conductive oxide
sintering
ZnO
flexible substrates
grey Taguchi method

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Fabrication Ceramics Target and Transparent Conductive Oxide Films on Flexible Substrates

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