CN113233897A - 一种碲硫镉靶材及其制备方法与应用 - Google Patents
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Abstract
本发明公开了一种碲硫镉靶材的制备方法,包括:(1)将碲化镉粉末和硫化镉粉末混合均匀,得到混合粉末;(2)将混合粉末在500~700℃下烧结1~2h,得到初烧结粉末;(3)将初烧结粉末进行球磨混合,得到球磨粉末;(4)将球磨粉末转入模具中,然后在真空环境下进行热压烧结,其中,先加热至400~500℃保温30~50min,再加热至700~900℃保温60~100min,压力为30~50MPa,烧结完成后,随炉冷却,得到靶材毛坯;(5)对靶材毛坯进行机加工,制成目标尺寸的碲硫镉靶材成品。本发明的制备方法具有节能、耗材少、操作简单、以及可批量生产等优点,所制备的碲硫镉靶材具有较高的密度,相对密度>95%,溅射性能好。
Description
技术领域
本发明涉及薄膜材料技术领域,具体涉及一种碲硫镉靶材及其制备方法与应用。
背景技术
随着电子信息产业的飞速发展,薄膜科学应用日益广泛,溅射法是制备薄膜材料的主要技术之一。溅射镀膜是指在真空中利用荷能粒子轰击靶表面,使被轰击出的粒子沉积在基片上的技术。与传统的蒸发镀膜相比,溅射镀膜具有可镀制任何材料,特别是高熔点材料,膜层致密,附着牢固,镀膜过程易于控制,镀膜速率稳定等系列优点。
而溅射所用的材料,称之为靶材。碲硫镉属于II-VI族化合物半导体,碲硫镉靶材是用来溅射制备太阳能薄膜的原料。其中,碲化镉(CdTe)太阳能薄膜电池是一种以p型CdTe和n型CdS所组成的异质结为基础的薄膜太阳能电池。CdTe为吸收层,是CdTe电池的主体吸光层,其与n型的CdS窗口层形成的p-n结是整个电池最核心的部分。而碲硫镉可作为p-n结之间的中间过渡层,有利于提高电池的光电转换效率。
靶材密度是衡量靶材性能的重要指标,为了减少靶材中的气孔,提高溅射薄膜的性能,通常要求靶材具有较高的密度。靶材的密度不仅影响溅射速率,还影响着薄膜的电学和光学性能。
因此,提供一种高密度的碲硫镉靶材成为尚待解决的技术问题。
发明内容
为解决上述现有技术中存在的缺点和不足,本发明的目的在于提供一种碲硫镉靶材及其制备方法与应用,本发明制备的碲硫镉靶材的相对密度>95%,具有较好的溅射性能。
为实现上述目的,本发明采取的技术方案为:
一种碲硫镉靶材的制备方法,包括如下步骤:
(1)将碲化镉粉末和硫化镉粉末混合均匀,得到混合粉末;
(2)将混合粉末在500~700℃下烧结1~2h,得到初烧结粉末;
(3)将初烧结粉末进行球磨混合,得到球磨粉末;
(4)将球磨粉末转入模具中,然后在真空环境下进行热压烧结,其中,先加热至400~500℃保温30~50min,再加热至700~900℃保温60~100min,压力为30~50MPa,烧结完成后,随炉冷却,得到靶材毛坯;
(5)对靶材毛坯进行机加工,制成目标尺寸的碲硫镉靶材成品。
优选地,所述步骤(1)中,碲化镉粉末与硫化镉粉末混合的质量比为,碲化镉粉末:硫化镉粉末=90~99.8:0.2~10。
优选地,所述碲化镉粉末和硫化镉粉末的平均粒径D50<5μm。
优选地,所述步骤(3)中,球磨混合的球料比为3~3.5:1,球磨时间为4~6h。
优选地,所述步骤(4)中,真空环境的真空度<5Pa,加热的升温速率为2~5℃/min。
本发明上述制备方法中,各步骤之间相互关联且相互影响,如:前阶段的步骤会影响后阶段的热压烧结效果,而后阶段的热压烧结会影响靶材的密度,碲硫镉靶的相对密度过小会导致其在溅射时容易产生结瘤。而按照本发明的制备方法进行各步骤时,可成功制得相对密度>95%的碲硫镉靶,该相对密度的碲硫镉靶具有较好的溅射性能,在溅射时不容易产生结瘤,溅射所得薄膜的厚度均匀性和组分均匀性均较好。
本发明还提供了一种碲硫镉靶材,其由本发明上述的制备方法制得。
本发明还提供了所述碲硫镉靶材在溅射制备太阳能薄膜中的用途。
与现有技术相比,本发明的有益效果在于:本发明的制备方法具有节能、耗材少、操作简单、以及可批量生产等优点,所制备的碲硫镉靶材具有较高的密度,相对密度>95%,溅射性能好。
具体实施方式
为更好的说明本发明的目的、技术方案和优点,下面将通过下列实施例进一步说明。应理解,以下实施例仅用于说明本发明而非用于限制本发明的范围。实施例中,所用方法如无特别说明,均为常规方法。实施例中使用的碲化镉粉末和硫化镉粉末均为申请人生产的市售产品,它们的纯度均为5N,平均粒径D50<5μm。
实施例1
一种碲硫镉靶材的制备方法,步骤如下:
(1)将碲化镉粉末和硫化镉粉末装入混料机中,碲化镉粉末与硫化镉粉末的质量比为97:3,混合均匀,得到混合粉末;
(2)将步骤(1)得到的混合粉末在600℃下烧结1.5h,得到初烧结粉末;
(3)将步骤(2)得到的初烧结粉末转入球磨桶中进行球磨混合,球料比为3:1,球磨时间为6h,得到球磨粉末;
(4)将步骤(3)得到的球磨粉末转入模具中,然后连带模具一起放入真空热压炉中,对真空热压炉进行抽真空,当真空度<5Pa后,开启加热,先以2℃/min加热至450℃保温40min,再以2℃/min加热至800℃保温80min,烧结过程的加压压力为30MPa,烧结完成后,随炉冷却,得到靶材毛坯;
(5)对靶材毛坯进行机加工,制成目标尺寸,即得碲硫镉靶材成品。
实施例2
一种碲硫镉靶材的制备方法,步骤如下:
(1)将碲化镉粉末和硫化镉粉末装入混料机中,碲化镉粉末与硫化镉粉末的质量比为90:10,混合均匀,得到混合粉末;
(2)将步骤(1)得到的混合粉末在700℃下烧结2h,得到初烧结粉末;
(3)将步骤(2)得到的初烧结粉末转入球磨桶中进行球磨混合,球料比为3.2:1,球磨时间为5h,得到球磨粉末;
(4)将步骤(3)得到的球磨粉末转入模具中,然后连带模具一起放入真空热压炉中,对真空热压炉进行抽真空,当真空度<5Pa后,开启加热,先以3℃/min加热至500℃保温50min,再以3℃/min加热至900℃保温100min,烧结过程的加压压力为45MPa,烧结完成后,随炉冷却,得到靶材毛坯;
(5)对靶材毛坯进行机加工,制成目标尺寸,即得碲硫镉靶材成品。
实施例3
一种碲硫镉靶材的制备方法,步骤如下:
(1)将碲化镉粉末和硫化镉粉末装入混料机中,碲化镉粉末与硫化镉粉末的质量比为99.8:0.2,混合均匀,得到混合粉末;
(2)将步骤(1)得到的混合粉末在500℃下烧结1h,得到初烧结粉末;
(3)将步骤(2)得到的初烧结粉末转入球磨桶中进行球磨混合,球料比为3:1,球磨时间为6h,得到球磨粉末;
(4)将步骤(3)得到的球磨粉末转入模具中,然后连带模具一起放入真空热压炉中,对真空热压炉进行抽真空,当真空度<5Pa后,开启加热,先以5℃/min加热至400℃保温30min,再以5℃/min加热至700℃保温60min,烧结过程的加压压力为35MPa,烧结完成后,随炉冷却,得到靶材毛坯;
(5)对靶材毛坯进行机加工,制成目标尺寸,即得碲硫镉靶材成品。
对比例1
一种碲硫镉靶材的制备方法,步骤如下:
(1)将碲化镉粉末和硫化镉粉末装入混料机中,碲化镉粉末与硫化镉粉末的质量比为97:3,混合均匀,得到混合粉末;
(2)将步骤(1)得到的混合粉末在400℃下烧结2h,得到初烧结粉末;
(3)将步骤(2)得到的初烧结粉末转入球磨桶中进行球磨混合,球料比为2:1,球磨时间为6h,得到球磨粉末;
(4)将步骤(3)得到的球磨粉末转入模具中,然后连带模具一起放入真空热压炉中,对真空热压炉进行抽真空,当真空度<5Pa后,开启加热,先以8℃/min加热至450℃保温40min,再以8℃/min加热至600℃保温80min,烧结过程的加压压力为60MPa,烧结完成后,随炉冷却,得到靶材毛坯;
(5)对靶材毛坯进行机加工,制成目标尺寸,即得碲硫镉靶材成品。
对比例2
一种碲硫镉靶材的制备方法,步骤如下:
(1)将碲化镉粉末和硫化镉粉末装入混料机中,碲化镉粉末与硫化镉粉末的质量比为97:3,混合均匀,得到混合粉末;
(2)将步骤(1)得到的混合粉末在800℃下烧结2h,得到初烧结粉末;
(3)将步骤(2)得到的初烧结粉末转入球磨桶中进行球磨混合,球料比为3:1,球磨时间为6h,得到球磨粉末;
(4)将步骤(3)得到的球磨粉末转入模具中,然后连带模具一起放入真空热压炉中,对真空热压炉进行抽真空,当真空度<5Pa后,开启加热,先以2℃/min加热至450℃保温40min,再以2℃/min加热至1000℃保温80min,烧结过程的加压压力为20MPa,烧结完成后,随炉冷却,得到靶材毛坯;
(5)对靶材毛坯进行机加工,制成目标尺寸,即得碲硫镉靶材成品。
相对密度测定(阿基米德排水法):
实施例1~3和对比例1~2的碲硫镉靶材的相对密度如下表所示。
碲硫镉靶材 | 相对密度 |
实施例1 | 95.3% |
实施例2 | 95.7% |
实施例3 | 96.0% |
对比例1 | 90.4% |
对比例2 | 92.3% |
从上表数据可看出,本发明的制备方法可制得相对密度>95%的碲硫镉靶材,而制备过程控制的条件会对靶材的密度产生影响。
最后所应当说明的是,以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制,尽管参照较佳实施例对本发明作了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。
Claims (8)
1.一种碲硫镉靶材的制备方法,其特征在于,包括如下步骤:
(1)将碲化镉粉末和硫化镉粉末混合均匀,得到混合粉末;
(2)将混合粉末在500~700℃下烧结1~2h,得到初烧结粉末;
(3)将初烧结粉末进行球磨混合,得到球磨粉末;
(4)将球磨粉末转入模具中,然后在真空环境下进行热压烧结,其中,先加热至400~500℃保温30~50min,再加热至700~900℃保温60~100min,压力为30~50MPa,烧结完成后,随炉冷却,得到靶材毛坯;
(5)对靶材毛坯进行机加工,制成目标尺寸的碲硫镉靶材成品。
2.如权利要求1所述的碲硫镉靶材的制备方法,其特征在于,所述步骤(1)中,碲化镉粉末与硫化镉粉末混合的质量比为,碲化镉粉末:硫化镉粉末=90~99.8:0.2~10。
3.如权利要求1所述的碲硫镉靶材的制备方法,其特征在于,所述碲化镉粉末和硫化镉粉末的平均粒径D50<5μm。
4.如权利要求1所述的碲硫镉靶材的制备方法,其特征在于,所述步骤(3)中,球磨混合的球料比为3~3.5:1,球磨时间为4~6h。
5.如权利要求1所述的碲硫镉靶材的制备方法,其特征在于,所述步骤(4)中,真空环境的真空度<5Pa。
6.如权利要求1所述的碲硫镉靶材的制备方法,其特征在于,所述步骤(4)中,加热的升温速率为2~5℃/min。
7.一种碲硫镉靶材,其特征在于,由如权利要求1~6任一项所述的碲硫镉靶材的制备方法制得。
8.如权利要求7所述的碲硫镉靶材在溅射制备太阳能薄膜中的应用。
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