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Article(id=1241768037557272580, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241768035548205179, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.01.029, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1692806400000, receivedDateStr=2023-08-24, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773990171088, onlineDateStr=2026-03-20, pubDate=1706716800000, pubDateStr=2024-02-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773990171088, onlineIssueDateStr=2026-03-20, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773990171087, creator=13701087609, updateTime=1773990171087, updator=13701087609, issue=Issue{id=1241768035548205179, tenantId=1146029695717560320, journalId=1235980550691926019, year='2024', volume='44', issue='1', pageStart='1', pageEnd='178', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773990170609, creator=13701087609, updateTime=1773993209826, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241780783011140021, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241768035548205179, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241780783015334326, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241768035548205179, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=134, endPage=137, ext={EN=ArticleExt(id=1241768037972508681, articleId=1241768037557272580, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Effects of Molding Pressure on Properties of Indium Tin Oxide (ITO) Sputtering Target, columnId=1236276108207902848, journalTitle=Mining and Metallurgical Engineering, columnName=MATERIALS, runingTitle=null, highlight=null, articleAbstract=

Nano ITO powders prepared by chemical coprecipitation plus calcination process were used as raw materials to prepare ITO sputtering target by molding and cold isostatic pressing, as well as conventional sintering. The effects of molding pressure on the relative density, resistivity, and grain size of ITO target were investigated. The results show that with the molding pressure of 60 MPa and the appropriate sintering conditions, the prepared ITO target has the relative density of 99.81% and resistivity of 1.707×10-4 Ω·cm, with an average grain size of 7.62 μm. The research results can provide reference for densification and large-scale production of ITO sputtering targets.

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以化学共沉淀-煅烧法制备的纳米ITO粉体为原料，通过模压、冷等静压成型，采用常压烧结法制备了ITO靶材，研究了模压成型压力对ITO靶材相对密度、电阻率和晶粒尺寸的影响。结果表明，模压成型压力60 MPa且烧结条件适宜时，制得的ITO靶材相对密度为99.81%、电阻率为1.707×10-4Ω·cm、平均晶粒尺寸为7.62 μm。研究结果可为ITO靶材的致密化与大型化生产提供借鉴。

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曾纪术（1974—），男，湖南洞口人，博士，正高级工程师，主要研究方向为材料冶金物理化学、光电材料。E-mail：；
方志杰（1979—），男，广西南宁人，博士，教授，主要研究方向为材料物理、计算材料学。E-mail：
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姜峰（1985—），男，江西玉山人，博士，高级工程师，主要研究方向为材料加工、粉末冶金技术。E-mail：

, authorsList=姜峰, 谭泽旦, 黄誓成, 方志杰, 陆映东, 覃立仁, 王永清, 曾纪术)}, authors=[Author(id=1241779782015320382, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241768037557272580, orderNo=0, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=18277202672@163.com, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1241779782132760905, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241768037557272580, authorId=1241779782015320382, language=EN, stringName=Feng JIANG, firstName=Feng, middleName=null, lastName=JIANG, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1.School of Mechanical and Automotive Engineering, Guangxi University of Science and Technology, Liuzhou 545616, Guangxi, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1241779782271172946, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241768037557272580, authorId=1241779782015320382, language=CN, stringName=姜峰, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1.广西科技大学　机械与汽车工程学院，广西　柳州　545616, bio={"content":"

姜峰（1985—），男，江西玉山人，博士，高级工程师，主要研究方向为材料加工、粉末冶金技术。E-mail：

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姜峰（1985—），男，江西玉山人，博士，高级工程师，主要研究方向为材料加工、粉末冶金技术。E-mail：

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模压成型压力对氧化铟锡（ITO）靶材性能影响研究
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姜峰 1 , 谭泽旦 1, 2 , 黄誓成 2 , 方志杰 3 , 陆映东 2 , 覃立仁 1 , 王永清 3 , 曾纪术 3
矿冶工程杂志 | 材料 2024,44(1): 134-137
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矿冶工程杂志 | 材料 2024, 44(1): 134-137
模压成型压力对氧化铟锡（ITO）靶材性能影响研究
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姜峰1 , 谭泽旦1, 2, 黄誓成2, 方志杰3 , 陆映东2, 覃立仁1, 王永清3, 曾纪术3
作者信息
  • 1.广西科技大学　机械与汽车工程学院，广西　柳州　545616
  • 2.广西晶联光电材料有限责任公司，广西　柳州　545036
  • 3.广西科技大学　电子工程学院，广西　柳州　545006

    • 姜峰（1985—），男，江西玉山人，博士，高级工程师，主要研究方向为材料加工、粉末冶金技术。E-mail：

通讯作者:

曾纪术（1974—），男，湖南洞口人，博士，正高级工程师，主要研究方向为材料冶金物理化学、光电材料。E-mail：；
方志杰（1979—），男，广西南宁人，博士，教授，主要研究方向为材料物理、计算材料学。E-mail：
Effects of Molding Pressure on Properties of Indium Tin Oxide (ITO) Sputtering Target
Feng JIANG1 , Zedan TAN1, 2, Shicheng HUANG2, Zhijie FANG3 , Yingdong LU2, Liren QIN1, Yongqing WANG3, Jishu ZENG3
Affiliations
  • 1.School of Mechanical and Automotive Engineering, Guangxi University of Science and Technology, Liuzhou 545616, Guangxi, China
  • 2.Guangxi Crystal Union Photoelectric Materials Co Ltd, Liuzhou 545036, Guangxi, China
  • 3.School of Electronic Engineering, Guangxi University of Science and Technology, Liuzhou 545006, Guangxi, China
出版时间: 2024-02-01 doi: 10.3969/j.issn.0253-6099.2024.01.029
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摘要
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以化学共沉淀-煅烧法制备的纳米ITO粉体为原料，通过模压、冷等静压成型，采用常压烧结法制备了ITO靶材，研究了模压成型压力对ITO靶材相对密度、电阻率和晶粒尺寸的影响。结果表明，模压成型压力60 MPa且烧结条件适宜时，制得的ITO靶材相对密度为99.81%、电阻率为1.707×10-4Ω·cm、平均晶粒尺寸为7.62 μm。研究结果可为ITO靶材的致密化与大型化生产提供借鉴。

模压成型  /  氧化铟锡  /  导电薄膜  /  靶材  /  常压烧结  /  电阻率  /  致密化

Nano ITO powders prepared by chemical coprecipitation plus calcination process were used as raw materials to prepare ITO sputtering target by molding and cold isostatic pressing, as well as conventional sintering. The effects of molding pressure on the relative density, resistivity, and grain size of ITO target were investigated. The results show that with the molding pressure of 60 MPa and the appropriate sintering conditions, the prepared ITO target has the relative density of 99.81% and resistivity of 1.707×10-4 Ω·cm, with an average grain size of 7.62 μm. The research results can provide reference for densification and large-scale production of ITO sputtering targets.

molding  /  indium tin oxide (ITO)  /  conductive thin film  /  target material  /  conventional sintering  /  electrical resistivity  /  densification
姜峰, 谭泽旦, 黄誓成, 方志杰, 陆映东, 覃立仁, 王永清, 曾纪术. 模压成型压力对氧化铟锡（ITO）靶材性能影响研究. 矿冶工程杂志, 2024 , 44 (1) : 134 -137 . DOI: 10.3969/j.issn.0253-6099.2024.01.029
Feng JIANG, Zedan TAN, Shicheng HUANG, Zhijie FANG, Yingdong LU, Liren QIN, Yongqing WANG, Jishu ZENG. Effects of Molding Pressure on Properties of Indium Tin Oxide (ITO) Sputtering Target[J]. Mining and Metallurgical Engineering, 2024 , 44 (1) : 134 -137 . DOI: 10.3969/j.issn.0253-6099.2024.01.029
正文
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透明导电氧化物薄膜兼具透明与导电特性，被广泛应用于显示面板、太阳能电池、传感器、微电子器件和功能玻璃等领域[1-2]。氧化铟锡（Indium Tin Oxide，简称ITO）薄膜是一种极具代表性[3]的透明导电氧化物薄膜，通常由磁控溅射法制备。我国的高质量ITO靶材曾长期依赖进口，尽管近年来国产化速度加快，但仍面临致密性较低、尺寸放大后缺陷增多等问题。
高性能ITO靶材的特点为高纯度、高密度、低电阻率和高组织均匀性[4-7]，其中密度指标最为重要，如何制备高密度ITO靶材一直都是研究的焦点[8-11]。氧气气氛无压烧结是当前制备ITO靶材的主流技术，其中模压成型压力是影响ITO靶材密度的重要因素之一[12]。本文以化学共沉淀法制备的ITO粉体为原料制备氧化铟锡靶材，研究模压成型压力对ITO靶材密度、电阻率和晶粒尺寸的影响，以期为国产高密度大尺寸ITO靶材的制备提供借鉴。
1　实验
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1.1　实验原料
采用由广西晶联光电材料有限责任公司提供的铟、锡氢氧化物混合物，按氧化铟（In2O3）与氧化锡（SnO2）质量比9∶1进行配料并采用化学共沉淀法制备ITO前驱体。所得ITO前驱体纯度大于99.99%，微观形貌为均匀的纳米颗粒粉体，如图1所示。前驱体比表面积为35.55 m2/g，具有很高的烧结活性，这是制备高性能ITO靶材的前提条件。
1.2　实验方法与过程
ITO靶材的制备按照“前驱体煅烧→粉体造粒→压制成型→常压烧结”的工艺流程进行，主要工艺参数设定基于论文作者前期研究结果以及相关文献[13]，过程分述如下：①前驱体煅烧：前驱体置于马弗炉中950 ℃下煅烧，发生化学反应生成氧化铟锡粉体（即ITO粉体）。②粉体造粒：将煅烧所得ITO粉体、超纯水、聚丙烯酸铵（分析纯）等加入超细研磨机中，球磨至设定时间后加入聚乙烯醇（分析纯），继续球磨1 h后将浆料转移至离心喷雾造粒机进行喷雾造粒处理。③压制成型：采用模压结合冷等静压进行成型，将处理后的粉体均匀填充至300 mm×200 mm的高强度钢模中进行模压，模压成型压力15～120 MPa，保压时间1 min。将模压得到的ITO靶材生坯抽真空包装，之后置于冷等静压机中进行最终成型，冷等静压压力250 MPa，保压时间10 min。④常压烧结：将成型后的ITO靶材生坯放入钟罩式烧结炉中，采用常压烧结法进行烧结。采用分段式升降温程序，升温、降温速率控制在0.5～1.0 ℃/min，首先在空气气氛中进行脱脂，随后向烧结炉中通入高纯氧气进行程序升温烧结，最高烧结温度为1 585 ℃，最高烧结温度下的保温时间为8 h。
1.3　样品的测试表征
采用日本Rigaku Miniflex 600对煅烧后粉体进行X射线衍射（XRD）分析；采用捷克TESCAN MIRALMS扫描电子显微镜观察粉体样品；采用梅特勒托利多精密天平测试靶材样品相对密度；采用ST2258C型数字四探针测试仪测试靶材样品电阻率；采用光学显微镜（OM）观察靶材样品金相组织；利用Nano Measurer 1.2软件，取样品中的100个晶粒进行统计分析，得到靶材样品晶粒尺寸。
2　结果与讨论
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2.1　共沉淀前驱体的煅烧结果分析
图2为共沉淀前驱体经950 ℃煅烧后所得ITO粉体的形貌。与图1对比可以看出，煅烧后粉体颗粒形貌发生了改变，形状更规则，主要为立方状，晶粒粒径略微增大，但仍为纳米级，粉体比表面积由煅烧前的35.55 m2/g降至6.56 m2/g。
前驱体经950 ℃煅烧后所得ITO粉体的XRD图谱如图3所示。由图3可知，粉体中主要物相为立方相氧化铟，衍射峰与标准卡片PDF#71-2195相吻合；26.71°、33.99°和51.86°附近的衍射峰被标定为二氧化锡。采用共沉淀法制备ITO粉体，煅烧温度较低时，锡原子完全固溶进入In2O3晶格[14]，煅烧温度升至950 ℃后，过饱和固溶的二氧化锡脱溶析出，故在XRD图谱中可以发现二氧化锡的衍射峰，与文献[15]报道结果一致。
2.2　模压成型压力对ITO靶材相对密度及电阻率的影响
模压成型压力15～120 MPa条件下（再经250 MPa冷等静压成型）制备的ITO靶材相对密度和电阻率如图4所示。由图4可以看出，随着成型压力增加，ITO靶材相对密度逐渐增大，成型压力60 MPa时，靶材相对密度99.81%，达到了超高密度水平；成型压力超过60 MPa后，靶材相对密度变化较小。尽管ITO靶材的成型要经历模压-冷等静压两道工序，但模压过程对ITO靶材的致密化有重要影响。成型压力较小时，生坯中部分ITO颗粒仅发生形变而未破碎，颗粒形貌基本未发生改变。在未破碎的ITO颗粒之间，存在未贴合界面和交联点，生坯即使再经较高压力冷等静压处理，仍可见未破碎ITO颗粒，存在较大的孔隙缺陷，孔隙无法通过烧结消除[12]。当成型压力超过临界值后，颗粒在模具内受到挤压而发生重排，伴随破碎坍塌，破碎颗粒在压力作用下填充到孔隙中。成型压力的临界值与实际工艺条件有关，如原料粉体颗粒粒径、形貌、流动性、靶材生坯尺寸以及模具的摩擦阻力等。具体到本研究体系，临界压力约60 MPa，成型压力超过临界值后，继续增大成型压力，在一定压力范围内对靶材密度影响不大。但在ITO粉末颗粒之间以及生坯与模具之间存在因相对滑动产生的摩擦，使得生坯内部存在压力梯度，且随成型压力增加，生坯内部压力梯度进一步增大，生坯内部可能发生滑动，反而导致靶材密度降低[16-18]。在本研究中，模压成型压力60～120 MPa范围内，靶材相对密度稳定在99.7%以上，展现了较宽的加压成型窗口，显示了本工艺的优越性。较大的成型压力虽然能获得高致密的氧化铟锡靶材，但考虑设备寿命以及成本效益，本文将模压成型压力定为60 MPa。根据ITO靶材的国家标准GB/T 20510—2017《氧化铟锡靶材》，ITO靶材的密度可分为RD99.0、RD99.5、RD99.7三个等级，本研究产品密度显然已超过最高等级RD99.7的密度要求。
总体而言，在本文采用的成型压力范围内，电阻率变化不大，但一般情况下ITO靶材的电阻率与相对密度在一定程度上呈负相关，即靶材相对密度越高，其电阻率越小。ITO靶材作为一种电导率接近金属的半导体陶瓷，影响其电阻率的因素可归纳为两个方面，一个是载流子浓度，另一个是载流子的迁移率[19]。在ITO中，载流子主要来源于Sn4+掺杂取代In3+[20]，本研究各靶材样品掺杂量相同，理应具有近似的载流子浓度，故其电阻率的不同归因于载流子迁移率的不同。迁移率与载流子的有效质量和散射概率成反比，载流子的有效质量与材料有关，故可认为各靶材样品具有相同的载流子有效质量。半导体中载流子的散射在低温下主要为缺陷和杂质离子的散射，高温下主要为由原子晶格振动产生的声子的散射，散射越强，迁移率越低[19]。本研究各靶材样品掺杂量相同，故可认为杂质离子散射量相当，它们在低温下载流子迁移率的差异可进一步归结为缺陷的差异。
晶界是一种容易影响载流子迁移率的缺陷，晶粒越小，晶界越多，载流子散射越严重。从各靶材样品的金相组织图及晶粒度分析结果得知，各靶材样品平均晶粒尺寸没有较大变化，由此推测几种靶材的晶界散射区别不大。此外，ITO材料中载流子浓度高达1 021 cm-3，晶界势垒降低，载流子容易实现隧穿效应，晶界散射对载流子迁移率的影响可以忽略[21]。另外一种影响载流子迁移率的缺陷是材料内部的孔隙，孔隙的存在破坏了晶体的周期性，缩短了载流子迁移自由程。靶材相对密度越低，表明材料内部孔洞越多，载流子迁移的自由程越短，散射越严重，电阻率越高。成型压力15～60 MPa范围时，随着压力增大，靶材相对密度逐渐提高，靶材中孔隙缺陷不断减少，载流子缺陷散射逐渐降低，电阻率逐渐降低。模压成型压力60 MPa时，靶材电阻率降至最低值1.707×10-4Ω·cm；成型压力60～120 MPa范围时，靶材相对密度几乎不变，孔隙缺陷基本保持不变，导致载流子缺陷散射也几乎不变，故电阻率保持在相同水平。综上所述，在本研究体系中，成型压力约60 MPa时更易获得具有较低电阻率的ITO靶材。
2.3　模压成型压力对ITO靶材组织均匀性的影响
图5为不同模压成型压力条件下（再经250 MPa冷等静压成型）ITO靶材的金相组织结构图。由图5可以看出，模压成型压力15～120 MPa（再经250 MPa冷等静压成型），ITO靶材晶粒较为规则整齐，晶粒之间紧密结合。同时可以看出，成型压力小于60 MPa时，材料中孔隙缺陷相对较多；成型压力大于60 MPa后，孔隙缺陷很少。随着成型压力提高，ITO靶材平均晶粒尺寸没有表现出很大的变化趋势，平均晶粒尺寸主要集中在7.55～7.68 μm，如图6所示。由此可见，在本研究体系及成型压力范围内，ITO靶材晶粒尺寸受成型压力的影响较小。
3　结论
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1）以化学共沉淀法制备的ITO粉体前驱体为原料，在优化工艺条件下，制备了超高密度（相对密度99.81%）、低电阻率（1.707×10-4Ω·cm）及金相组织均匀的ITO靶材。
2）在950 ℃下煅烧以共沉淀法制备纳米前驱体时，可以得到比表面积6.56 m2/g的纳米ITO粉体。
3）模压成型压力15～60 MPa时，随着压力增大，ITO靶材相对密度逐渐提高，电阻率逐渐降低；成型压力60～120 MPa时，靶材相对密度和电阻率基本没有变化。
4）模压成型压力15～120 MPa时，ITO靶材晶粒尺寸变化很小，平均晶粒尺寸主要集中在7.55～7.68 μm。
基金
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  • 国家自然科学基金(11864005)
  • 广西重点研发项目(桂科AB21196007)
  • 广西科技计划项目(桂科AD20159079)
  • 柳州市科技计划项目(2020PAAA0608)
文献
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2024年第44卷第1期
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文章信息
doi: 10.3969/j.issn.0253-6099.2024.01.029
  • 接收时间：2023-08-24
  • 首发时间：2026-03-20
  • 出版时间：2024-02-01
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  • 收稿日期：2023-08-24
基金
国家自然科学基金(11864005)
广西重点研发项目(桂科AB21196007)
广西科技计划项目(桂科AD20159079)
柳州市科技计划项目(2020PAAA0608)
作者信息
    1.广西科技大学　机械与汽车工程学院，广西　柳州　545616
    2.广西晶联光电材料有限责任公司，广西　柳州　545036
    3.广西科技大学　电子工程学院，广西　柳州　545006

通讯作者:

曾纪术（1974—），男，湖南洞口人，博士，正高级工程师，主要研究方向为材料冶金物理化学、光电材料。E-mail：；
方志杰（1979—），男，广西南宁人，博士，教授，主要研究方向为材料物理、计算材料学。E-mail：
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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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