CN113788669A - 一种ito溅射靶材的制备方法 - Google Patents
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- 238000005477 sputtering target Methods 0.000 title claims abstract description 10
- 239000013077 target material Substances 0.000 title abstract description 34
- 238000005245 sintering Methods 0.000 claims abstract description 49
- 239000000843 powder Substances 0.000 claims abstract description 37
- 235000015895 biscuits Nutrition 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 30
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 28
- 239000002002 slurry Substances 0.000 claims abstract description 25
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000005238 degreasing Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 15
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- 239000000463 material Substances 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 9
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- 239000010963 304 stainless steel Substances 0.000 claims description 6
- 229910001209 Low-carbon steel Inorganic materials 0.000 claims description 6
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 10
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Abstract
本发明提供了一种ITO溅射靶材的制备方法,包括以下步骤:将纯度为99.995%的In2O3粉体和SnO2粉体按质量比为(90~97):(10~3)进行湿法球磨混合,球磨过程加入少量分散剂和粘结剂,得到高固含量、高流动性能的ITO浆料;将所得的ITO浆料注入石膏模具中进行粉浆浇注成型,得到大尺寸ITO素坯;ITO素坯干燥脱模进行低温脱脂去除有机添加剂;将脱脂后的ITO素坯进行热等静压烧结制备ITO溅射靶材。本发明可用于大尺寸、高致密度ITO靶材的制备,且发明工艺中的热等静压烧结可以降低靶材的烧结温度和烧结时间,有效地提高生产效率,该方法适用于工业化生产。
Description
技术领域
本发明涉及先进陶瓷靶材制备领域,具体涉及到一种ITO溅射靶材的制备方法。
背景技术
ITO薄膜是一种性能优异的透明导电薄膜,其可见光透过率高于95%、电阻率达10-4Ω·cm,载流子浓度高达1021 cm-3,红外线反射率高达80%以上,且具有优良的化学蚀刻性、热稳定性等特点,广泛应用于平面显示器、太阳能面板、 有机发光二极管、防辐射玻璃等领域上。
ITO溅射靶材是制备ITO薄膜的原料,ITO靶材的综合质量对ITO薄膜性能产生重要影响。
目前,ITO素坯成型方式主要有两种:(1)模压+冷等静压(2)粉浆浇注。前者属于干法成型,虽具有生产效率高、易于操作等特点,但设备昂贵,且无法制备大尺寸坯体。粉浆浇注成型不仅造价低廉、方便操作,而且可以用于大尺寸板坯的制备上。
目前,ITO靶材烧结方式主要有三种(1)常压气氛烧结;(2)热压烧结;(3)热等静压烧结。热等静压烧结相比于常压气氛烧结,可以进一步降低烧结温度和烧结时间,缩短生产周期;相比于热压烧结可以解决热压中施力不均的问题。热等静压烧结对于提高ITO靶材品质和生产效率等方面有着至关重要的意义。
专利CN 105130416 A提供一种低电阻ITO靶材制备方法,该发明中采用粉浆浇注成型制备出高强度素坯,坯体采用常压氧气烧结法制备ITO靶材,该工艺烧结温度较高、烧结时间较长,生产周期较长。
专利CN 101575203 A中提供了一种热压烧结制备ITO溅射靶材的方法,在热压过程中会发生氧化物分解、受力不均、材料污染等问题。
专利文献
张元松,叶有明,熊爱臣等. 一种低电阻率ITO靶材的制备方法. CN 105130416 A[P].2015.
扈百直,孙本双,刘孝宁等. ITO溅射靶材的制备方法. CN101575203A[P].2009。
发明内容
针对现有靶材制备技术中存在的板坯尺寸小、生产效率低等问题。本发明提供了一种ITO溅射靶材的制备方法,包括以下步骤:
(1)将In2O3粉末和SnO2粉末进行湿法球磨混合,(1)将In2O3粉体和SnO2粉体进行湿法球磨混合,得到高固含量、高流动性能的ITO浆料;
(2)将步骤(1)中所得的ITO浆料进行粉浆浇注成型,干燥脱模后得到ITO素坯;
(3)将步骤(2)中所得的ITO素坯进行脱脂烧结,去除有机添加剂;
(4)将步骤(3)中所得的ITO素坯进行热等静压烧结制备出大尺寸、高致密度的ITO靶材。
进一步地,所述步骤(1)中,In2O3粉体和SnO2粉体的纯度为99.995%;In2O3粉体的平均粒径为60~110 nm,SnO2粉体的平均粒径为100~180 nm。
进一步地,所述步骤(1)中,In2O3: SnO2质量比为90:10、93:7、95:5、97:3。
进一步地,所述步骤(1)中,In2O3粉末和SnO2粉末进行湿法球磨混合,其过程包括:
在In2O3原料粉和SnO2原料粉中加入去离子水、聚丙烯酸类分散剂球磨混合,球磨时间36~48 h,球磨速度200~250 r/min。粉料混合均匀后加入少量粘结剂继续球磨30~45 min,得到的ITO浆料抽真空排气泡。
进一步地,所述步骤(1)中所得的ITO浆料固含量为70~80 wt%、粘度为80~160mPa·s(25 °C,转速3.96 S-1)。
进一步地,所述步骤(2)中,ITO浆料进行粉浆浇注成型后得到直径为60~90cm、厚度10~15cm、致密度为45~60%的ITO素坯。
进一步地,所述步骤(3)中,ITO素坯进行脱脂烧结,去除球磨过程中加入的少量有机添加剂,避免后续在热等静压烧结过程中有机物分解挥发产生的气体造成包套鼓包的现象。脱脂温度700~800 °C、脱脂时间12~18 h。
进一步地,所述步骤(4)中,脱脂后的ITO素坯进行热等静压烧结,烧结温度1000~1200 °C、保压压力150~180 MPa、保压时间3~5 h。
进一步地,所述步骤(4)中,热等静压处理过程中包套材料选用低碳钢,隔离材料选用304不锈钢,包套密封前先进行抽真空排气。
进一步地,所述步骤(4)中,包套焊接采用氩弧焊接方式。
进一步地,所述步骤(4)中,热等静压结束后采用机械切割方法剥离包套。
进一步地,所制备的ITO靶材直径50~80cm、厚度8~12cm、致密度高于99%、电阻率为1.6~2.0×10-4 mΩ·cm。
本发明与现有技术相比具有以下优点:
通过粉浆浇注成型工艺,制得大尺寸、高强度的ITO素坯,可以减少热压过程中包套在HIP环节中的收缩量,防止包套变形度太大导致的开裂。
通过热等静压(HIP )烧结工艺,使ITO素坯在烧结过程中均匀受力,与热压烧结相比,避免了靶材密度不均、开裂变形等问题;与传统常压氧气烧结,进一步降低烧结所需要的温度和时间,缩短靶材制备周期。本发明可适用于工业化生产。
附图说明
图1为本发明ITO靶材制备方法的工艺流程图。
具体实施方式
下面将结合具体实施例对本发明作进一步说明,但是不限于所举实例。
实施例1
称取In2O3: SnO2质量比为90:10的原料粉,按要求加入纯水、聚丙烯酸类分散剂、粘结剂球磨混合制备出固含量为75%的ITO浆料;
将ITO浆料注入石膏模具中,得到直径为80cm、厚度为15cm、致密度为58%的ITO生坯;
ITO素坯温度800 °C条件下脱脂10h;
脱脂后的ITO素坯装入低碳钢包套内,包套与ITO素坯之间加入304不锈钢隔离材料,进行热等静压烧结,热等静压温度1100 °C、保压压力150 MPa、保压时间3 h;
热等静压烧结后得到的ITO靶材直径为56cm、厚度为10cm、致密度为98.2%、电阻率为2×10-4 mΩ·cm。靶材与包套剥离过程中,隔离材料没有与靶材发生反应,靶材形状完好,无开裂现象。
实施例2
称取In2O3: SnO2质量比为90:10的原料粉,按要求加入纯水、聚丙烯酸类分散剂、粘结剂球磨混合制备出固含量为75%的ITO浆料;
将ITO浆料注入石膏模具中,得到直径为80cm、厚度为15cm、致密度为58%的ITO生坯;
ITO素坯温度800 °C条件下脱脂10h;
脱脂后的ITO素坯装入低碳钢包套内,包套与ITO素坯之间加入304不锈钢隔离材料,进行热等静压烧结,热等静压温度1200 °C、保压压力150 MPa、保压时间3 h;
热等静压烧结后得到的ITO靶材直径为54cm、厚度为9.7cm、致密度为99%、电阻率为1.9×10-4 mΩ·cm。靶材与包套剥离过程中,隔离材料没有与靶材发生反应,靶材形状完好,无开裂现象。
实施例3
称取In2O3: SnO2质量比为90:10的原料粉,按要求加入纯水、聚丙烯酸类分散剂、粘结剂球磨混合制备出固含量为75%的ITO浆料;
将ITO浆料注入石膏模具中,得到直径为80cm、厚度为15cm、致密度为58%的ITO生坯;
ITO素坯温度800 °C条件下脱脂10h;
脱脂后的ITO素坯装入低碳钢包套内,包套与ITO素坯之间加入304不锈钢隔离材料,进行热等静压烧结,热等静压温度1200 °C、保压压力180 MPa、保压时间3 h;
热等静压烧结后得到的ITO靶材直径为52cm、厚度为9.3cm、致密度为99.5%、电阻率为1.7×10-4 mΩ·cm。靶材与包套剥离过程中,隔离材料没有与靶材发生反应,靶材形状完好,无开裂现象。
实施例4
称取In2O3: SnO2质量比为90:10的原料粉,按要求加入纯水、聚丙烯酸类分散剂、粘结剂球磨混合制备出固含量为75%的ITO浆料;
将ITO浆料注入石膏模具中,得到直径为80cm、厚度为15cm、致密度为58%的ITO生坯;
ITO素坯温度800 °C条件下脱脂10h;
脱脂后的ITO素坯装入低碳钢包套内,包套与ITO素坯之间加入304不锈钢隔离材料,进行热等静压烧结,热等静压温度1200 °C、保压压力180 MPa、保压时间5 h;
热等静压烧结后得到的ITO靶材直径为53cm、厚度为9.6cm、致密度为99.1%、电阻率为1.8×10-4 mΩ·cm。靶材与包套剥离过程中,隔离材料没有与靶材发生反应,靶材形状完好,有轻度开裂现象。
对比例1
称取In2O3: SnO2质量比为90:10的原料粉,按要求加入纯水、聚丙烯酸类分散剂、粘结剂球磨混合制备出固含量为75%的ITO浆料;
将ITO浆料注入石膏模具中,得到直径为80cm、厚度为15cm、致密度为58%的ITO生坯;
ITO素坯温度800 °C条件下脱脂10h;
脱脂后的ITO素坯进行常压氧气烧结,烧结温度1600 °C、保温时间时间5 h;
常压氧气烧结后得到的ITO靶材直径为58cm、厚度为11.5cm、致密度为98%、电阻率为2×10-4 mΩ·cm
对比例2
称取In2O3: SnO2质量比为90:10的原料粉,按要求加入纯水、聚丙烯酸类分散剂、粘结剂球磨混合制备出固含量为75%的ITO浆料;
将ITO浆料注入石膏模具中,得到直径为80cm、厚度为15cm、致密度为58%的ITO生坯;
ITO素坯温度800 °C条件下脱脂10h;
脱脂后的ITO素坯进行常压氧气烧结,烧结温度1600 °C、保温时间时间10 h;
常压氧气烧结后得到的ITO靶材直径为56cm、厚度为10.5cm、致密度为98.5%、电阻率为1.8×10-4 mΩ·cm
以上所述为本发明的优选实施例,并非对本发明作任何限制。凡是根据本发明实质对前述各实施例的技术方案进行修改,或等效替换其部分技术特征,均应包含在本发明的保护范围内。
Claims (10)
1.一种ITO溅射靶材的制备方法,其特征在于,具体操作步骤如下:
(1)将In2O3粉体和SnO2粉体进行湿法球磨混合,得到高固含量、高流动性能的ITO浆料;
(2)将步骤(1)中所得的ITO浆料进行粉浆浇注成型,干燥脱模后得到ITO素坯;
(3)将步骤(2)中所得的ITO素坯进行脱脂烧结,去除有机添加剂;
(4)将步骤(3)中所得的ITO素坯进行热等静压烧结制备出大尺寸、高致密度的ITO靶材。
2.根据权利要求1所述的制备方法,其特征在于,所述步骤(1)中,In2O3粉体和SnO2粉体的纯度为99.995%;In2O3粉体的平均粒径为60~110 nm,SnO2粉体的平均粒径为100~180nm。
3.根据权利要求1所述的制备方法,其特征在于,所述步骤(1)中,In2O3: SnO2质量比为90:10、93:7、95:5、97:3。
4.根据权利要求1所述的制备方法,其特征在于,所述步骤(1)中,In2O3粉末和SnO2粉末进行湿法球磨混合,其过程包括:
在In2O3原料粉和SnO2原料粉中加入去离子水、聚丙烯酸类分散剂球磨混合,球磨时间36~48 h,球磨速度200~250 r/min。粉料混合均匀后加入少量粘结剂继续球磨30~45min,得到的ITO浆料抽真空排气泡。
5.根据权利要求1所述的制备方法,其特征在于,所述步骤(1)中所得的ITO浆料固含量为70~80 wt%、粘度为80~160 mPa·s(25 °C,转速3.96 S-1)。
6.根据权利要求1所述的制备方法,其特征在于,所述步骤(2)中,ITO浆料进行粉浆浇注成型后得到直径为60~90cm、厚度10~15cm、致密度为45~60%的ITO素坯。
7.根据权利要求1所述的制备方法,其特征在于,所述步骤(3)中,ITO素坯进行脱脂烧结,去除球磨过程中加入的少量有机添加剂,避免后续在热等静压烧结过程中有机物分解挥发产生的气体造成包套鼓包的现象。脱脂温度700~800 °C、脱脂时间12~18 h。
8.根据权利要求1所述的制备方法,其特征在于,所述步骤(4)中,脱脂后的ITO素坯进行热等静压烧结,烧结温度1000~1200 °C、保压压力150~180 MPa、保压时间3~5 h。
9.根据权利要求1所述的制备方法,其特征在于,所述步骤(4)中,热等静压处理过程中包套材料选用低碳钢,隔离材料选用304不锈钢,包套密封前先进行抽真空排气。包套焊接采用氩弧焊接方式。
10.根据权利要求1所述的制备方法,其特征在于,所述步骤(4)中,热等静压结束后采用机械切割方法剥离包套。
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