CN116444269A - 一种掺杂型钼靶材的制备方法 - Google Patents

一种掺杂型钼靶材的制备方法 Download PDF

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CN116444269A
CN116444269A CN202310330102.9A CN202310330102A CN116444269A CN 116444269 A CN116444269 A CN 116444269A CN 202310330102 A CN202310330102 A CN 202310330102A CN 116444269 A CN116444269 A CN 116444269A
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oxide powder
doped molybdenum
sodium
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张莉兰
杨彪
钟小华
高建成
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Leading Film Materials Anhui Co ltd
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Abstract

本发明公开了一种掺杂型钼靶材的制备方法，属于靶材制备技术领域，包括以下步骤：将聚乙烯吡咯烷酮和聚乙二醇加入去离子水中搅拌溶解，加入氧化钼粉和二水合钼酸钠，球磨，喷雾干燥，得到钠掺杂钼粉；向钠掺杂钼粉中加入氧化铋粉和无水乙醇，球磨后进行喷雾干燥处理，得到坯体粉料；经过低压预压制和烧结成型，得到掺杂型钼靶材，本发明以氧化钼粉和二水合钼酸钠为原料，以聚乙烯吡咯烷酮为粘结剂，聚乙二醇为分散剂，得到钠掺杂钼粉，组分均一，形态良好，本发明在坯体粉料中引入了助熔剂氧化铋粉，可以增强靶材烧结成型过程中的晶界运动，促进晶粒生长，降低材料内部的空隙，有效提高粉体的粘接性和靶材的致密度。

Description

一种掺杂型钼靶材的制备方法
技术领域
本发明属于太阳能电池制备技术领域，具体涉及一种掺杂型钼靶材的制备方法。
背景技术
铜铟镓硒(CIGS)薄膜太阳能电池具有稳定性高、光吸率高、抗辐射能力强和使用寿命长等特点，其能力转化率基本保持在20％作用，已有研究表明，通过掺杂Li、Na、K等碱金属可以明显提升CIGS太阳能电池的转化效率，其中Na的提升效果最为明显。
目前研究的热点和难点是，采用何种Na源向CIGS吸收层提供充足与稳定的Na，现有的技术手段是在电池板的基板和Mo背极板层间添加Mo-Na层作为Na源材料，能够有效地将Na均匀地掺杂至CIGS吸收层中，且容易控制。Mo-Na层由直流磁控溅射沉积而成，与制备Mo背极板的工艺相同，只需将Mo靶材换成Mo-Na靶材即可，操作简单，适合工艺生产使用。
由于Na原子的化学活泼性和Mo原子的化学稳定性的巨大差异，以及Mo高熔点与Na低熔点的物理性质差异，导致Mo-Na合金靶材在制备过程难以保证钠元素的均匀分布和稳定存在，因此，有必要提供一种性能更好的掺杂型钼靶材。
发明内容
本发明的目的在于提供一种掺杂型钼靶材的制备方法，以解决背景技术中的问题。
本发明的目的可以通过以下技术方案实现：
一种掺杂型钼靶材的制备方法，包括以下步骤：
第一步、将聚乙烯吡咯烷酮和聚乙二醇加入去离子水中搅拌至聚乙烯吡咯烷酮和聚乙二醇完全溶解，得到分散液；向分散液中加入氧化钼粉和二水合钼酸钠，搅拌均匀后，转移至球磨机中，球磨1-10h，得到浆料；
第二步、将上述所得浆料利用喷雾干燥塔进行喷雾干燥处理，得到钠掺杂钼粉；
第三步、向钠掺杂氧化钼粉中加入氧化铋粉和无水乙醇，转移至球磨机中，球磨10h，进行喷雾干燥处理，得到坯体粉料；
第四步、将坯体粉料进行低压预压制，得到初始压坯体；
第五步、将初始压坯体置于石墨模具中，之后将石墨模具置于PSP烧结炉中在真空条件下进行放电等离子烧结，经过卸压、冷却，打磨、抛光，得到掺杂型钼靶材。
本发明主要是通过钼靶材掺杂金属钠提升太阳能电池的转化效率，且制备方法简单，易实施，对设备要求不高，除此之外，和已经发表的钠掺杂的靶材相比具有更好的均匀性以及高致密性。
作为本发明的进一步方案，氧化钼粉和二水合钼酸钠质量比为75.7-92.7：7.26-24.3，去离子水用量为氧化钼粉和二水合钼酸钠质量和的60-80％。
作为本发明的进一步方案，聚乙烯吡咯烷酮用量为氧化钼粉和钼酸钠质量和的3-5％，聚乙二醇用量为氧化钼粉和二水合钼酸钠质量和的0.5％。
作为本发明的进一步方案，氧化钼粉的平均粒度为2-3μm，氧化钼粉质量纯度大于等于99.95％，二水合钼酸钠的平均粒度为75-100μm，二水合钼酸钠质量纯度大于等于99.0％。
作为本发明的进一步方案，球磨转速为600-1200r/min。
作为本发明的进一步方案，喷雾干燥处理的具体工艺参数为：进风口温度为200-240℃，出风口温度为80-150℃，喷雾干燥塔中雾化器的转速为0.8×104-1.5×104r/min。
作为本发明的进一步方案，氧化铋粉为钠掺杂氧化钼粉质量的1-2％，无水乙醇加入质量为氧化铋粉和钠掺杂氧化钼粉质量之和，氧化铋粉的平均粒度为145-155μm。
作为本发明的进一步方案，低压预压制采用冷等静压法，具体参数为：压力100-130MPa，保压时间10-15min。
作为本发明的进一步方案，放电等离子烧结具体过程如下：
烧结压强35MPa，烧结温度300-600℃，保温时间2-8h，由室温升温至150度速度为0.03-1.5℃/min，150-250℃的速度为0.3-2℃/min，250-300℃或250-600℃的速度0.8-5℃/min。
本发明的有益效果：
1、本发明以氧化钼粉和二水合钼酸钠为原料，以聚乙烯吡咯烷酮为粘结剂，聚乙二醇为分散剂，通过球磨、喷雾干燥、得到钠掺杂氧化钼粉，相比于直接湿法球磨而言，以高分子聚合物作为分散剂和粘接剂，得到的钠掺杂氧化钼粉，组分均一，形态良好，原因在于分散剂和粘结剂的加入在不改变钠掺杂氧化钼粉组分的前提下，发挥粘合和隔离的作用，从而获得流动性和分散性极好的球状粉末，并且聚乙二醇和聚乙烯吡咯烷酮具有高温易分解的特点，能够在较低的温度和较快的时间完成脱碳处理，减少残留碳对靶材的影响。
2、本发明制备的钠掺杂氧化钼粉，其中二水合钼酸钠被均匀地包覆在氧化钼粉颗粒内部，钠元素分布均匀，且在烧结过程中，钠不会分布晶界上，而是被包覆在晶粒内部，减少高温烧结时低熔点钠的损失，使掺杂靶材内部钠元素分布均匀并且稳定存在。
3、本发明在坯体粉料中引入了助熔剂氧化铋粉，氧化铋粉的引入可以增强靶材烧结成型过程中的晶界运动，促进晶粒生长，降低材料内部的空隙，有效提高粉体的粘接性和靶材的致密度。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，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作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
实施例1
一种掺杂型钼靶材的制备方法，包括以下步骤：
第一步、将2.5g聚乙烯吡咯烷酮和0.4g聚乙二醇加入50g去离子水中搅拌至聚乙烯吡咯烷酮和聚乙二醇完全溶解，得到分散液；向分散液中加入75.7g氧化钼粉和7.26g二水合钼酸钠，搅拌均匀后，转移至球磨机中，转速为600r/min，球磨1h，得到浆料；
第二步、将上述所得浆料利用喷雾干燥塔进行喷雾干燥处理，得到钠掺杂钼粉；
第三步、向钠掺杂氧化钼粉中加入氧化铋粉和无水乙醇，氧化铋粉为钠掺杂氧化钼粉质量的1％，无水乙醇加入质量为氧化铋粉和钠掺杂氧化钼粉质量之和，氧化铋粉的平均粒度为145-155μm，转移至球磨机中，转速600r/min球磨1h，球磨结束后，进行喷雾干燥处理，得到坯体粉料；
第四步、将坯体粉料进行低压预压制，具体为压力100MPa，保压时间15min，得到初始压坯体；
第五步、将初始压坯体置于石墨模具中，之后将石墨模具置于PSP烧结炉中，烧结压强35MPa，烧结温度300℃，保温时间2h，由室温升温至150℃速度为0.03℃/min，150-250℃的速度为0.3℃/min，250-300℃的速度0.8℃/min；经过卸压、冷却，打磨、抛光，得到掺杂型钼靶材。
其中，氧化钼粉的平均粒度为2-3μm，氧化钼粉质量纯度大于等于99.95％，二水合钼酸钠的平均粒度为75-100μm，二水合钼酸钠质量纯度大于等于99.0％；喷雾干燥处理的具体工艺参数为：进风口温度为200℃，出风口温度为80℃，喷雾干燥塔中雾化器的转速为0.8×104r/min。
实施例2
一种掺杂型钼靶材的制备方法，包括以下步骤：
第一步、将3.5g聚乙烯吡咯烷酮和0.44g聚乙二醇加入63g去离子水中搅拌至聚乙烯吡咯烷酮和聚乙二醇完全溶解，得到分散液；向分散液中加入78.6g氧化钼粉和10.5g二水合钼酸钠，搅拌均匀后，转移至球磨机中，转速为1000r/min，球磨5h，得到浆料；
第二步、将上述所得浆料利用喷雾干燥塔进行喷雾干燥处理，得到钠掺杂钼粉；
第三步、向钠掺杂氧化钼粉中加入氧化铋粉和无水乙醇，氧化铋粉为钠掺杂氧化钼粉质量的1.5％，无水乙醇加入质量为氧化铋粉和钠掺杂氧化钼粉质量之和，氧化铋粉的平均粒度为145-155μm，转移至球磨机中，转速1000r/min球磨5h，球磨结束后，进行喷雾干燥处理，得到坯体粉料；
第四步、将坯体粉料进行低压预压制，具体为压力100MPa，保压时间13min，得到初始压坯体；
第五步、将初始压坯体置于石墨模具中，之后将石墨模具置于PSP烧结炉中，烧结压强35MPa，烧结温度600℃，保温时间5h，由室温升温至150℃速度为1℃/min，150-250℃的速度为1℃/min，250-600℃的速度2.5℃/min，经过卸压、冷却，打磨、抛光，得到掺杂型钼靶材。
其中，氧化钼粉的平均粒度为2-3μm，氧化钼粉质量纯度大于等于99.95％，二水合钼酸钠的平均粒度为75-100μm，二水合钼酸钠质量纯度大于等于99.0％；喷雾干燥处理的具体工艺参数为：进风口温度为220℃，出风口温度为130℃，喷雾干燥塔中雾化器的转速为1.0×104/min。
实施例3
一种掺杂型钼靶材的制备方法，包括以下步骤：
第一步、将5g聚乙烯吡咯烷酮和0.5g聚乙二醇加入80g去离子水中搅拌至聚乙烯吡咯烷酮和聚乙二醇完全溶解，得到分散液；向分散液中加入92.7g氧化钼粉和7.26g二水合钼酸钠，搅拌均匀后，转移至球磨机中，转速为1200r/min，球磨时间10h，得到浆料；
第二步、将上述所得浆料利用喷雾干燥塔进行喷雾干燥处理，得到钠掺杂钼粉；
第三步、向钠掺杂氧化钼粉中加入氧化铋粉和无水乙醇，转移至球磨机中，转速1200r/min球磨10h，球磨结束后，氧化铋粉为钠掺杂氧化钼粉质量的2％，无水乙醇加入质量为氧化铋粉和钠掺杂氧化钼粉质量之和，氧化铋粉的平均粒度为145-155μm，进行喷雾干燥处理，喷雾干燥工艺参数，处理结束后，得到坯体粉料；
第四步、将坯体粉料进行低压预压制，具体为压力130MPa，保压时间10min，得到初始压坯体；
第五步、将初始压坯体置于石墨模具中，之后将石墨模具置于PSP烧结炉中，烧结温度600℃，保温时间8h，由室温升温至150℃速度为1.5℃/min，150-250℃的速度为2℃/min，250-600℃的速度5℃/min，经过卸压、冷却，打磨、抛光，得到掺杂型钼靶材。
其中，氧化钼粉的平均粒度为2-3μm，氧化钼粉质量纯度大于等于99.95％，二水合钼酸钠的平均粒度为75-100μm，二水合钼酸钠质量纯度大于等于99.0％；喷雾干燥处理的具体工艺参数为：进风口温度为220℃，出风口温度为100℃，喷雾干燥塔中雾化器的转速为1×104r/min。
对比例1
与实施例1相比，将实施例1中聚乙烯吡咯烷酮和聚乙二醇去除，其余原料及制备过程同实施例1。
对比例2
与实施例1相比，将实施例1中第三步除去，即不添加氧化铋粉，其余原料及制备过程同实施例1。
对实施例1-3和对比例1-2所得掺杂钼靶材进行性能测试，利用DX-6000型密度测试仪，测量靶材的密度，并计算相对密度，测试结果如表1所示：
表1
项目 实施例1 实施例2 实施例3 对比例1 对比例2
密度(g/cm3) 9.56 9.59 9.67 9.32 9.11
相对密度(％) 97.1 97.9 98.6 96.2 95.3
由表1可以看出，相比于对比例1-2，实施例1-3所制备的掺杂型钼靶材密度较高，内部空隙少。
需要说明的是，在本文中，诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来，而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。

Claims (8)

1.一种掺杂型钼靶材的制备方法，其特征在于，包括以下步骤：
第一步、将聚乙烯吡咯烷酮和聚乙二醇加入去离子水中搅拌均匀，加入氧化钼粉和二水合钼酸钠，搅拌后转移至球磨机中，球磨，得到浆料；
第二步、将上述所得浆料进行喷雾干燥处理，得到钠掺杂钼粉；
第三步、向钠掺杂氧化钼粉中加入氧化铋粉和无水乙醇，转移至球磨机中，球磨，进行喷雾干燥处理，得到坯体粉料；
第四步、将坯体粉料进行低压预压制，得到初始压坯体；
第五步、将初始压坯体置于石墨模具中，之后将石墨模具置于PSP烧结炉中在真空条件下进行放电等离子烧结，经过卸压、冷却，打磨、抛光，得到掺杂型钼靶材。
2.根据权利要求1所述的一种掺杂型钼靶材的制备方法，其特征在于，氧化钼粉和二水合钼酸钠质量比为75.7-92.7：7.26-24.3，去离子水用量为氧化钼粉和二水合钼酸钠质量和的60-80％。
3.根据权利要求1所述的一种掺杂型钼靶材的制备方法，其特征在于，聚乙烯吡咯烷酮用量为氧化钼粉和钼酸钠质量和的3-5％，聚乙二醇用量为氧化钼粉和二水合钼酸钠质量和的0.5％。
4.根据权利要求1所述的一种掺杂型钼靶材的制备方法，其特征在于，氧化铋粉为钠掺杂氧化钼粉质量的1-2％，无水乙醇加入质量为氧化铋粉和钠掺杂氧化钼粉质量之和，氧化铋粉的平均粒度为145-155μm。
5.根据权利要求1所述的一种掺杂型钼靶材的制备方法，其特征在于，氧化钼粉的平均粒度为2-3μm，氧化钼粉质量纯度大于等于99.95％，二水合钼酸钠的平均粒度为75-100μm，二水合钼酸钠质量纯度大于等于99.0％。
6.根据权利要求1所述的一种掺杂型钼靶材的制备方法，其特征在于，喷雾干燥处理的具体工艺参数为：进风口温度为200-240℃，出风口温度为80-150℃，喷雾干燥塔中雾化器的转速为0.8×104-1.5×104r/min。
7.根据权利要求1所述的一种掺杂型钼靶材的制备方法，其特征在于，低压预压制采用冷等静压法，具体参数为：压力100-130MPa，保压时间10-15min。
8.根据权利要求1所述的一种掺杂型钼靶材的制备方法，其特征在于，放电等离子烧结具体过程如下：
烧结压强35MPa，烧结温度300-600℃，保温时间2-8h。
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