CN114956823B - 一种导电碲化镉靶材的制备方法 - Google Patents

一种导电碲化镉靶材的制备方法 Download PDF

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CN114956823B
CN114956823B CN202210584839.9A CN202210584839A CN114956823B CN 114956823 B CN114956823 B CN 114956823B CN 202210584839 A CN202210584839 A CN 202210584839A CN 114956823 B CN114956823 B CN 114956823B
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周荣艳
文崇斌
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Vital Thin Film Materials Guangdong Co Ltd
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Abstract

本发明属于太阳能电池领域，公开了一种导电碲化镉靶材的制备方法，包括以下步骤：（1）将Cd粉、CdTe粉混匀，得到混合物料；（2）将步骤（1）的混合物料装入石墨模具，置于热压炉中进行预压；（3）预压完成后，抽真空处理，至真空度<10pa开始加热升温，升温速率为10~20℃/min，加热到500~750℃后保温；（4）达到保温时间后进行加压处理；（5）加压处理后降至室温，出炉、脱模，得毛坯靶材，毛坯靶材经机床加工后得导电碲化镉靶材。本发明所述的制备方法通过掺杂游离镉来破坏碲化镉的结晶方式，降低碲化镉靶材的电阻率，改善碲化镉薄膜的导电性。

Description

一种导电碲化镉靶材的制备方法
技术领域
本发明属于太阳能电池领域，更具体的，涉及一种导电碲化镉靶材的制备方法。
背景技术
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。
溅射所用的材料，称之为靶材。碲化镉（CdTe）是一种II-VI族化合物半导体材料，CdTe材料的禁带宽度为1.46eV，光谱响应与太阳光谱十分吻合，光吸收系数高达10-5cm-1，理论光电转换效率达到29%，因此，碲化镉靶材是公认高效、廉价的薄膜太阳能电池吸收材料。目前，CdTe在薄膜太阳能电池吸收材料的应用过程中，有以下问题需要得到解决：
（1）CdTe中碲和镉的相对原子序数比较大，导致CdTe靶材中经常含有本征点缺陷和杂质缺陷，形成载流子复合中心，减少非平衡载流子寿命，造成CdTe载流子浓度低，薄膜电阻率大，影响电池的电流输出；
（2）CdTe本身具有很强的自补偿效应，很难像硅等半导体一样通过掺入杂质元素来调控电学性能。
发明内容
针对现有技术中存在的上述问题，本发明的目的在于提供一种导电碲化镉靶材的制备方法，该方法通过掺杂游离镉来破坏碲化镉的结晶方式，降低碲化镉靶材的电阻率，改善碲化镉薄膜的导电性。
为实现上述目的，本发明所采用的技术方案是：
一种导电碲化镉靶材的制备方法，包括以下步骤：
（1）将Cd粉、CdTe粉混匀，得到混合物料；
（2）将步骤（1）的混合物料装入石墨模具，置于热压炉中进行预压；
（3）预压完成后，抽真空处理，至真空度<10pa开始加热升温，升温速率为10~20℃/min，加热到500~750℃后保温；
（4）达到保温时间后进行加压处理；
（5）加压处理后降至室温，出炉、脱模，得毛坯靶材；毛坯靶材经机床加工后得导电碲化镉靶材。
作为优选方案之一，步骤（1）中，Cd粉、CdTe粉的纯度均为5N以上，Cd粉粒径为10~100μm，CdTe粉粒径为150~300μm。
作为优选方案之一，步骤（1）中，Cd粉、CdTe粉的摩尔比为0.1~1：1。本发明采用碲化镉掺杂一定比例的游离镉原料，镉粉掺杂量需要精确控制，如掺杂的镉含量较低，对碲化镉组件没有实质的改善作用；如掺杂量太多，镉含量/碲含量会形成杂质缺陷，形成载流子复合中心，减少非平衡载流子寿命，造成CdTe载流子浓度低，薄膜电阻率大，影响电池的电流输出。
作为优选方案之一，步骤（1）中，混匀的具体操作为：采用均质机进行物理翻滚运行均质，均质时间为3~10h。
作为优选方案之一，步骤（2）中，预压压力为10~30T。
作为优选方案之一，步骤（3）中，保温时间为100~200min。
作为优选方案之一，步骤（4）中，加压压力为40~45MPa，压力的输出功率0.2~2w，保压时间为60~150min。
作为优选方案之一，步骤（5）中，加压处理后开始降温，当温度低于450℃时，停止抽真空，通氮气冷却到室温。进一步优选所述降温采用自然降温方式。
与现有技术相比，本发明的有益效果为：
本发明的导电碲化镉靶材的制备方法，采用碲化镉掺杂一定比例的游离镉原料，其反应合成的温度更低，靶材的生产效率更高，制得的靶材的电阻率更低，改善了碲化镉薄膜的光电利用率。
因为碲化镉本身是不导电的，碲化镉熔点1041℃，镉熔点320℃，直接制备高密度的碲化镉靶材，需要的热压温度更高，且电阻率很高，在溅射靶材时需要用到成本更高的交流电磁控溅射，光电转化效率成本更高。掺杂一定含量的镉，可以降低热压温度，在温度更低时获得高密度靶材，同时镉有一定的导电性，可选用成本更低的直流电磁控溅射。
本发明采用石墨模具，石墨模具耐高温高压，且装料会有石墨纸将物料与模具分开，易于脱模且坯体表面的石墨纸易于去除，也可减少杂质的引入。
本发明的制备方法工艺简单，对设备要求较低，成本较低，制得的靶材纯度和密度均较高。
具体实施方式
为了便于理解本发明，下文将结合说明书和较佳的实施例对本发明作更全面、细致地描述，但本发明的保护范围并不限于以下具体的实施例。
除非另有定义，下文中所使用的所有专业术语与本领域技术人员通常理解的含义相同。本文中所使用的专业术语只是为了描述具体实施例的目的，并不旨在限制本发明的保护范围。
除非另有特别说明，本发明中用到的各种原材料、试剂、仪器和设备等均可通过市场购买得到或者可通过现有方法制备得到。
实施例1
本实施例公开了一种导电碲化镉靶材的制备方法，包括以下步骤：
（1）称取Cd粉、CdTe粉，采用均质机进行物理翻滚运行均质6h，其中，Cd粉、CdTe粉的纯度均为5N，Cd粉粒径为10~100μm、CdTe粉粒径为150~300μm，Cd粉、CdTe粉的摩尔比为0.2：1；
（2）将上述混合均质的物料装入石墨模具中，其中石墨模具的大小为163×116mm，装料为1.15kg；将装有物料的石墨模具置于热压炉中进行预压，预压压力25T；
（3）预压完成后依次开粗抽阀、机械泵、开罗茨泵对炉体抽真空，在炉体真空度<10pa开始加热；从室温加热到650℃，加热的升温速率为15℃/min，加热到650℃后保温120min；
（4）到达保温设定时间后开始加压处理，加压压力为40MPa，压力的输出功率0.5w，保压时间为80min；
（5）加压处理后开始自然降温，温度低于450℃后，依次关闭粗抽阀、罗茨泵、机械泵，最后通N2降温到室温后出炉，进行脱模处理，得到碲化镉掺杂的毛坯靶材，通过CNC加工，得到碲化镉掺杂靶材。
实施例2
本实施例公开了一种导电碲化镉靶材的制备方法，包括以下步骤：
（1）称取Cd粉、CdTe粉，采用均质机进行物理翻滚运行均质6h，其中，Cd粉、CdTe粉的纯度均为5N，Cd粉粒径为10~100μm、CdTe粉粒径为150~300μm，Cd粉、CdTe粉的摩尔比为0.4：1；
（2）将上述混合均质的物料装入石墨模具中，其中石墨模具的大小为163×116mm，装料为1.15kg；将装有物料的石墨模具置于热压炉中进行预压，预压压力25T；
（3）预压完成后依次开粗抽阀、机械泵、开罗茨泵对炉体抽真空，在炉体真空度<10pa开始加热；从室温加热到680℃，加热的升温速率为15℃/min，加热到680℃后保温120min；
（4）到达保温设定时间后开始加压处理，加压压力为40MPa，压力的输出功率0.5w，保压时间为80min；
（5）加压处理后开始自然降温，温度低于450℃后，依次关闭粗抽阀、罗茨泵、机械泵，最后通N2降温到室温后出炉，进行脱模处理，得到碲化镉掺杂的毛坯靶材，通过CNC加工，得到碲化镉掺杂靶材。
实施例3
本实施例公开了一种导电碲化镉靶材的制备方法，包括以下步骤：
（1）称取Cd粉、CdTe粉，采用均质机进行物理翻滚运行均质6h，其中，Cd粉、CdTe粉的纯度均为5N，Cd粉粒径为10~100μm、CdTe粉粒径为150~300μm，Cd粉、CdTe粉的摩尔比为0.8：1；
（2）将上述混合均质的物料装入石墨模具中，其中石墨模具的大小为163×116mm，装料为1.15kg；将装有物料的石墨模具置于热压炉中进行预压，预压压力25T；
（3）预压完成后依次开粗抽阀、机械泵、开罗茨泵对炉体抽真空，在炉体真空度<10pa开始加热；从室温加热到700℃，加热的升温速率为15℃/min，加热到700℃后保温120min；
（4）到达保温设定时间后开始加压处理，加压压力为40MPa，压力的输出功率0.5w，保压时间为80min；
（5）加压处理后开始自然降温，温度低于450℃后，依次关闭粗抽阀、罗茨泵、机械泵，最后通N2降温到室温后出炉，进行脱模处理，得到碲化镉掺杂的毛坯靶材，通过CNC加工，得到碲化镉掺杂靶材。
对比例1
本对比例公开了一种碲化镉靶材的制备方法，包括以下步骤：
（1）称取CdTe粉采用均质机进行物理翻滚运行均质6h，CdTe粉粒径为150~300μm，纯度为5N；
（2）将上述混合均质的物料装入石墨模具中，其中装料模具的大小为163×116mm，装料为1.15kg，将装有物料的石墨模具置于热压炉中进行预压，预压压力25T；
（3）预压完成后依次开粗抽阀、机械泵、开罗茨泵对炉体抽真空，在炉体真空度<10pa开始加热；从室温加热到780℃，加热的升温速率为10℃/min，加热到780℃后保温100min；
（4）到达保温设定时间后开始加压处理，加压压力为40MPa，压力的输出功率0.5w，保压时间为100min；
（5）加压处理后开始自然降温，温度低于450℃后，依次关闭粗抽阀、罗茨泵、机械泵，最后通N2降温到室温后出炉，进行脱模处理，得到碲化镉掺杂的毛坯靶材，通过CNC加工，得到碲化镉靶材。
对比例2
本对比例公开了一种碲化镉靶材的制备方法，包括以下步骤：
（1）称取Cd粉、CdTe粉，采用均质机进行物理翻滚运行均质6h，其中，Cd粉、CdTe粉的纯度均为5N，Cd粉粒径为10~100μm、CdTe粉粒径为150~300μm，Cd粉、CdTe粉的摩尔比为0.05：1；
（2）将上述混合均质的物料装入石墨模具中，其中石墨模具的大小为163×116mm，装料为1.15kg；将装有物料的石墨模具置于热压炉中进行预压，预压压力25T；
（3）预压完成后依次开粗抽阀、机械泵、开罗茨泵对炉体抽真空，在炉体真空度<10pa开始加热；从室温加热到650℃，加热的升温速率为15℃/min，加热到650℃后保温120min；
（4）到达保温设定时间后开始加压处理，加压压力为40MPa，压力的输出功率0.5w，保压时间为80min；
（5）加压处理后开始自然降温，温度低于450℃后，依次关闭粗抽阀、罗茨泵、机械泵，最后通N2降温到室温后出炉，进行脱模处理，得到碲化镉掺杂的毛坯靶材，通过CNC加工，得到碲化镉掺杂靶材。
对比例3
本对比例公开了一种碲化镉靶材的制备方法，包括以下步骤：
（1）称取Cd粉、CdTe粉，采用均质机进行物理翻滚运行均质6h，其中，Cd粉、CdTe粉的纯度均为5N，Cd粉粒径为10~100μm、CdTe粉粒径为150~300μm，Cd粉、CdTe粉的摩尔比为1.2：1；
（2）将上述混合均质的物料装入石墨模具中，其中石墨模具的大小为163×116mm，装料为1.15kg；将装有物料的石墨模具置于热压炉中进行预压，预压压力25T；
（3）预压完成后依次开粗抽阀、机械泵、开罗茨泵对炉体抽真空，在炉体真空度<10pa开始加热；从室温加热到650℃，加热的升温速率为15℃/min，加热到650℃后保温120min；
（4）到达保温设定时间后开始加压处理，加压压力为40MPa，压力的输出功率0.5w，保压时间为80min；
（5）加压处理后开始自然降温，温度低于450℃后，依次关闭粗抽阀、罗茨泵、机械泵，最后通N2降温到室温后出炉，进行脱模处理，得到碲化镉掺杂的毛坯靶材，通过CNC加工，得到碲化镉掺杂靶材。
对实施例1~3、对比例1~3所得靶材进行测试。具体数据如下如表1所示：
实施例1~3中，靶材电阻率均小于80000 Ω.cm；
对比例1~3中，靶材电阻率大于100000 Ω.cm。
表1
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包含范围之内。

Claims (5)

1.一种导电碲化镉靶材的制备方法，其特征在于，包括以下步骤：
（1）将Cd粉、CdTe粉混匀，得到混合物料，Cd粉、CdTe粉的摩尔比为0.1~1：1；Cd粉、CdTe粉的纯度均为5N以上，Cd粉粒径为10~100μm，CdTe粉粒径为150~300μm；
（2）将步骤（1）的混合物料装入石墨模具，置于热压炉中进行预压，预压压力为10~30T；
（3）预压完成后，抽真空处理，至真空度<10pa开始加热升温，升温速率为10~20℃/min，加热到500~750℃后保温；
（4）达到保温时间后进行加压处理；加压压力为40~45MPa，压力的输出功率0.2~2w；保压时间为60~150min；
（5）加压处理后降至室温，出炉、脱模，得毛坯靶材；毛坯靶材经机床加工后得导电碲化镉靶材。
2.如权利要求1所述的导电碲化镉靶材的制备方法，其特征在于，步骤（1）中，混匀的具体操作为：采用均质机进行物理翻滚运行均质，均质时间为3~10h。
3.如权利要求1所述的导电碲化镉靶材的制备方法，其特征在于，步骤（3）中，保温时间为100~200min。
4.如权利要求1所述的导电碲化镉靶材的制备方法，其特征在于，步骤（5）中，加压处理后开始降温，当温度低于450℃时，停止抽真空，通氮气冷却到室温。
5.如权利要求4所述的导电碲化镉靶材的制备方法，其特征在于，所述降温采用自然降温方式。
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