CN115504768A - 一种氧化铟镓锌靶材的制备方法 - Google Patents
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000013077 target material Substances 0.000 title claims abstract description 27
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 21
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052733 gallium Inorganic materials 0.000 title claims abstract description 20
- 229910052738 indium Inorganic materials 0.000 title claims abstract description 20
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 60
- 238000005245 sintering Methods 0.000 claims abstract description 41
- 235000015895 biscuits Nutrition 0.000 claims abstract description 29
- 239000002002 slurry Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 claims abstract description 19
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001195 gallium oxide Inorganic materials 0.000 claims abstract description 15
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 15
- 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 15
- 239000003292 glue Substances 0.000 claims abstract description 11
- 238000007599 discharging Methods 0.000 claims abstract description 10
- 239000007921 spray Substances 0.000 claims abstract description 10
- 238000004321 preservation Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001238 wet grinding Methods 0.000 claims abstract description 6
- 238000005469 granulation Methods 0.000 claims abstract description 5
- 230000003179 granulation Effects 0.000 claims abstract description 5
- 238000000748 compression moulding Methods 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract 3
- 239000007788 liquid Substances 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 12
- 229920002125 Sokalan® Polymers 0.000 claims description 9
- 239000004584 polyacrylic acid Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 5
- 239000000178 monomer Substances 0.000 claims description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 24
- 238000000498 ball milling Methods 0.000 description 11
- 239000011230 binding agent Substances 0.000 description 8
- 238000000227 grinding Methods 0.000 description 6
- 238000000889 atomisation Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000004576 sand Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
本发明公开了一种氧化铟镓锌靶材的制备方法,包括:将氧化铟粉末、氧化镓粉末和氧化锌粉末加入水中,并加入分散剂,搅拌制得IGZO前混液;将IGZO前混液加入球磨机中进行湿磨,制得IGZO浆料;将IGZO浆料依次进行喷雾造粒和压制成型,制得IGZO素坯;将IGZO素坯依次进行排胶、预烧结和高温烧结,制得IGZO靶材;其中,排胶温度为500℃~800℃,排胶时间≥24小时;预烧结温度为1000℃~1250℃,保温时间为6~12小时;高温烧结温度为1350℃~1450℃,保温时间为4~20小时。本发明增加了排胶后的预烧结工艺,使成型后的IGZO靶材具有强度高、密度大、平整度高、电阻率低等特点。
Description
技术领域
本发明涉及OLED平面显示用靶材技术领域,具体涉及一种氧化铟镓锌靶材的制备方法。
背景技术
氧化铟镓锌(IGZO)靶材应用于新一代显示领域,可作为ITO靶材的迭代产品,应用于以车载、IT显示屏(包括平板、笔电、显示器等)、工业品等显示应用为目标产品市场。作为第四代半导体材料亦可用于元宇宙显示芯片等领域,可生产分辨率超过5000ppi的元宇宙显示驱动芯片。
IGZO是一种新型半导体材料,有着比非晶硅(α-Si)更高的电子迁移率。电子迁移率越高则器件信息传输量越大,可使用更窄的通道传递信息,实现更高的分辨率,并具有高亮度、低功耗、窄边框的优势。
现有氧化铟镓锌靶材制备方法是在脱脂后直接进行烧结,没有预烧工序;烧结后变形量大、密度低、表面质量有时有缺陷。
发明内容
针对现有技术中存在的不足之处,本发明提供一种氧化铟镓锌靶材的制备方法。
本发明公开了一种氧化铟镓锌靶材的制备方法,包括:
将氧化铟粉末、氧化镓粉末和氧化锌粉末加入水中,并加入分散剂,搅拌均匀制得IGZO前混液;
将IGZO前混液加入球磨机中进行湿磨,制得IGZO浆料;
将IGZO浆料进行喷雾造粒,制得IGZO粉体;
将IGZO粉体进行压制成型,制得IGZO素坯;
将IGZO素坯依次进行排胶、预烧结和高温烧结,制得IGZO靶材;其中,排胶温度为500℃~800℃,排胶时间≥24小时;预烧结温度为1000℃~1250℃,保温时间为6~12小时;高温烧结温度为1350℃~1450℃,保温时间为4~20小时。
作为本发明的进一步改进,所述氧化铟粉末、氧化镓粉末和氧化锌粉末为纯度大于99.99%的单体粉末,所述氧化铟粉末、氧化镓粉末和氧化锌粉末按预设的原子比配置IGZO原料粉末。
作为本发明的进一步改进,所述IGZO前混液的固含量为30%~60%,所述分散剂为聚丙烯酸类分散剂,所述聚丙烯酸类分散剂的加入量为IGZO原料粉末总重的0.1~0.5%。
作为本发明的进一步改进,所述IGZO浆料的固含量为30%~50%,所述IGZO浆料的粒径为0.3μm~1.0μm,25℃时IGZO浆料的粘度为30~60mPa·S。
作为本发明的进一步改进,所述IGZO粉体的松装密度≥1.3g/cm3。
作为本发明的进一步改进,所述IGZO素坯的相对密度(相对IGZO靶材的真实密度)控制为40%~50%。
与现有技术相比,本发明的有益效果为:
本发明在压制素坯与高温烧结制得IGZO靶材之间增加了排胶以及排胶后的预烧结工艺,使成型后的IGZO靶材具有强度高、密度大、平整度高、电阻率低等特点。
附图说明
图1为本发明一种实施例公开的氧化铟镓锌靶材的制备方法的流程图。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例,都属于本发明保护的范围。
下面结合附图对本发明做进一步的详细描述:
如图1所示,本发明提供一种氧化铟镓锌靶材的制备方法,包括:
步骤1、将氧化铟粉末、氧化镓粉末和氧化锌粉末加入水中,并加入分散剂,采用高速分散机搅拌均匀制得IGZO前混液;其中,
氧化铟粉末、氧化镓粉末和氧化锌粉末为纯度大于99.99%的单体粉末,氧化铟粉末、氧化镓粉末和氧化锌粉末按预设的原子比配置IGZO原料粉末;IGZO前混液的固含量为30%~60%,分散剂为有机分散剂,优选为聚丙烯酸类分散剂,分散剂的加入量为IGZO原料粉末总重的0.1~0.5%,优选为0.3%。
步骤2、将IGZO前混液加入球磨机中进行湿磨,制得IGZO浆料;其中,
湿磨后的IGZO浆料的固含量为30%~50%,湿磨后的IGZO浆料中固体颗粒的平均粒径为0.3μm~1.0μm,25℃时IGZO浆料的粘度为30~60mPa·S。进一步,球磨介质可采用0.5mm的氧化锆球,锆球体积分数占腔体的70%,研磨转速1200r/min
步骤3、将IGZO浆料进行喷雾造粒,制得IGZO粉体;其中,
喷雾造粒制得的IGZO粉体的松装密度≥1.3g/cm3。
步骤4、将IGZO粉体进行压制成型,制得IGZO素坯;其中,
IGZO素坯的相对密度控制为40%~50%。
步骤5、将IGZO素坯进行排胶;其中,
排胶温度为500℃~800℃,排胶时间≥24小时。
步骤6、将排胶后的IGZO素坯进行预烧结;其中,
预烧结温度为1000℃~1250℃,保温时间为6~12小时;
步骤7、将预烧结后的IGZO素坯进行高温烧结,制得IGZO靶材;其中,
高温烧结温度为1350℃~1450℃,保温时间为4~20小时。
本发明通过增加预烧结工艺使成型后的IGZO靶材具有强度高、密度大、平整度高、电阻率低等特点的原理在于:IGZO靶材开始收缩温度在1200℃左右,预烧(低温保温)主要作用在烧结过程中使坯体排气充分以及促使陶瓷粉粒的均质化,从而促进烧结致密化。无低温预烧,由于粉体高烧结活性,由烧结牵引导致过高反作用力,使得烧结变形量较大,大尺寸靶材尤为明显。氧化物烧结体电阻炉与缺氧密度有关,低温预烧,有助于烧结后期电阻率降低。
本发明所制备的IGZO靶材可制备透明导电氧化物薄膜(Transparent conductiveoxide,简称TCO);其主要用途有:1、OLED显示器件;2、薄膜太阳能电池;3、功能玻璃;4、电磁防护屏;另外在红外材料、紫外探测器等其它方面也获得了广泛的应用。
对比例1:
一种氧化铟镓锌靶材的制备方法,包括:
1)、取纯度为99.99%的氧化铟、氧化镓、氧化锌粉末按原子比配成5kg IGZO原料粉末,按固含量60%称取定量水配置成IGZO前混液,并在搅拌过程中加入原料粉末总量0.3%的聚丙烯酸类分散剂。
2)、用卧式砂磨机对IGZO前混液进行球磨,球磨介质采用0.5mm的氧化锆球,锆球体积分数占腔体的70%,研磨转速1200r/min,控制浆料平均粒径为0.3~1.0μm,测量粘度值为55mPa·s;
3)、喷雾造粒机进风温度设定238℃,出风温度100℃,雾化转速15000rpm,制得IGZO粉体松装密度≥1.3g/cm3;
4)、IGZO粉末采用限位压制,控制素坯密度为40%~50%;
5)、素坯800℃排胶20小时后,在1450℃条件下烧结12小时。
靶材烧结体测试密度为95%,强度较低无法进行加工,烧结后靶材翘曲严重,无法加工目标尺寸,靶材电阻率95mΩ·cm。
对比例2
一种氧化铟镓锌靶材的制备方法,包括:
1)、取纯度为99.99%的氧化铟、氧化镓、氧化锌粉末按原子比配成5kg IGZO原料粉末,按固含量60%称取定量水配置成IGZO前混液,并在搅拌过程中加入原料粉末总量0.3%的聚丙烯酸类分散剂。
2)、用卧式砂磨机对IGZO前混液进行球磨,球磨介质采用0.5mm的氧化锆球,锆球体积分数占腔体的70%,研磨转速1200r/min,控制浆料平均粒径为0.3~1.0μm,测量粘度值为55mPa·s;
3)、喷雾造粒机进风温度设定238℃,出风温度100℃,雾化转速15000rpm,制得IGZO粉体松装密度≥1.3g/cm3;
4)、IGZO粉末采用限位压制,控制素坯密度为40%~50%;
5)、素坯800℃排胶20小时后,在1400℃条件下烧结12小时。
靶材烧结体测试密度为95%,具有一定强度,可进行加工,烧结后靶材翘曲严重,无法加工目标尺寸,靶材电阻率95mΩ·cm。
实施例1
一种氧化铟镓锌靶材的制备方法,包括:
1)、取纯度为99.99%的氧化铟、氧化镓、氧化锌粉末按原子比配成5kg IGZO原料粉末,按固含量60%称取定量水配置成IGZO前混液,并在搅拌过程中加入原料粉末总量0.3%的聚丙烯酸类分散剂。
2)、用卧式砂磨机对IGZO前混液进行球磨,球磨介质采用0.5mm的氧化锆球,锆球体积分数占腔体的70%,研磨转速1200r/min,控制浆料平均粒径为0.3~1.0μm,测量粘度值为55mPa·s;
3)、喷雾造粒机进风温度设定238℃,出风温度100℃,雾化转速15000rpm,制得IGZO粉体松装密度≥1.3g/cm3;
4)、IGZO粉末采用限位压制,控制素坯密度为40%~50%;
5)、素坯800℃排胶20小时后,在1250℃条件下进行预预烧,预烧时间5小时,再经1400℃条件下进行烧结,烧结时间12小时。
靶材烧结体的相对密度可达99.5%以上,靶材电阻率小于等于12mΩ·cm,靶材强度、平整度良好,可加工目标尺寸靶材。
实施例2
一种氧化铟镓锌靶材的制备方法,包括:
1)、取纯度为99.99%的氧化铟、氧化镓、氧化锌粉末按原子比配成5kg IGZO原料粉末,按固含量60%称取定量水配置成IGZO前混液,并在搅拌过程中加入原料粉末总量0.3%的聚丙烯酸类分散剂。
2)、用卧式砂磨机对IGZO前混液进行球磨,球磨介质采用0.5mm的氧化锆球,锆球体积分数占腔体的70%,研磨转速1200r/min,控制浆料平均粒径为0.3~1.0μm,测量粘度值为55mPa·s;
3)、喷雾造粒机进风温度设定238℃,出风温度100℃,雾化转速15000rpm,制得IGZO粉体松装密度≥1.3g/cm3;
4)、IGZO粉末采用限位压制,控制素坯密度为40%~50%;
5)、素坯800℃排胶20小时后,在1000℃条件下进行预预烧,预烧时间5小时,再经1400℃条件下进行烧结,烧结时间12小时。
靶材烧结体的相对密度可达99.0%以上,靶材电阻率小于等于17mΩ·cm,靶材强度、平整度良好,可加工目标尺寸靶材。
实施例3
一种氧化铟镓锌靶材的制备方法,包括:
1)、取纯度为99.99%的氧化铟、氧化镓、氧化锌粉末按原子比配成5kg IGZO原料粉末,按固含量60%称取定量水配置成IGZO前混液,并在搅拌过程中加入原料粉末总量0.3%的聚丙烯酸类分散剂。
2)、用卧式砂磨机对IGZO前混液进行球磨,球磨介质采用0.5mm的氧化锆球,锆球体积分数占腔体的70%,研磨转速1200r/min,控制浆料平均粒径为0.3~1.0μm,测量粘度值为55mPa·s;
3)、喷雾造粒机进风温度设定238℃,出风温度100℃,雾化转速15000rpm,制得IGZO粉体松装密度≥1.3g/cm3;
4)、IGZO粉末采用限位压制,控制素坯密度为40%~50%;
5)、素坯800℃排胶20小时后,在1150℃条件下进行预预烧,预烧时间5小时,再经1400℃条件下进行烧结,烧结时间12小时。
靶材烧结体的相对密度可达99.0%以上,靶材电阻率小于等于12mΩ·cm,靶材强度、平整度良好,可加工目标尺寸靶材。
本发明的优点为:
本发明在压制素坯与高温烧结制得IGZO靶材之间增加了排胶以及排胶后的预烧结工艺,使成型后的IGZO靶材具有强度高、密度大、平整度高、电阻率低等特点。
以上仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (6)
1.一种氧化铟镓锌靶材的制备方法,其特征在于,包括:
将氧化铟粉末、氧化镓粉末和氧化锌粉末加入水中,并加入分散剂,搅拌均匀制得IGZO前混液;
将IGZO前混液加入球磨机中进行湿磨,制得IGZO浆料;
将IGZO浆料进行喷雾造粒,制得IGZO粉体;
将IGZO粉体进行压制成型,制得IGZO素坯;
将IGZO素坯依次进行排胶、预烧结和高温烧结,制得IGZO靶材;其中,排胶温度为500℃~800℃,排胶时间≥24小时;预烧结温度为1000℃~1250℃,保温时间为6~12小时;高温烧结温度为1350℃~1450℃,保温时间为4~20小时。
2.如权利要求1所述的氧化铟镓锌靶材的制备方法,其特征在于,所述氧化铟粉末、氧化镓粉末和氧化锌粉末为纯度大于99.99%的单体粉末,所述氧化铟粉末、氧化镓粉末和氧化锌粉末按预设的原子比配置IGZO原料粉末。
3.如权利要求2所述的氧化铟镓锌靶材的制备方法,其特征在于,所述IGZO前混液的固含量为30%~60%,所述分散剂为聚丙烯酸类分散剂,所述聚丙烯酸类分散剂的加入量为IGZO原料粉末总重的0.1~0.5%。
4.如权利要求1所述的氧化铟镓锌靶材的制备方法,其特征在于,所述IGZO浆料的固含量为30%~50%,所述IGZO浆料的粒径为0.3μm~1.0μm,25℃时IGZO浆料的粘度为30~60mPa·S。
5.如权利要求1所述的氧化铟镓锌靶材的制备方法,其特征在于,所述IGZO粉体的松装密度≥1.3g/cm3。
6.如权利要求1所述的氧化铟镓锌靶材的制备方法,其特征在于,所述IGZO素坯的相对密度控制为40%~50%。
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CN118184311A (zh) * | 2024-05-16 | 2024-06-14 | 广州市尤特新材料有限公司 | 一种igzo靶材的烧结制备方法及其应用 |
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CN118184311A (zh) * | 2024-05-16 | 2024-06-14 | 广州市尤特新材料有限公司 | 一种igzo靶材的烧结制备方法及其应用 |
CN118184311B (zh) * | 2024-05-16 | 2024-08-13 | 广州市尤特新材料有限公司 | 一种igzo靶材的烧结制备方法及其应用 |
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