CN113481477A - 高透过率硅旋转溅射靶材的制备方法 - Google Patents
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Abstract
本发明提供一种高透过率硅旋转溅射靶材的制备方法，通过采用6N多晶硅重掺原料和5N多晶硅高阻原料进行破碎成粉得到6N多晶硅半成品原料和5N多晶硅半成品半成品原料，将6N多晶硅半成品原料和5N多晶硅半成品半成品原料混合稀释制得杂质含量低的高纯硅粉末，这样喷涂制得的靶材杂质含量降低，尤其是B，提高靶材在镀膜过程产品的透过率，LAB值≥93%，减低客户使用成本及满足客户大尺寸产品镀膜需求。
Description
技术领域
本发明涉及硅靶材领域，尤其涉及一种高透过率硅旋转溅射靶材的制备方法。
背景技术
物理气相沉积(Physical Vapour Deposition，PVD)指的是，在真空条件下，采用低电压、大电流的电弧放电技术，利用气体放电使材料源蒸发并使被蒸发物质与气体都发生电离，然后通过电场的加速作用，使被蒸发物质及其反应产物沉积在工件上形成某种特殊功能的薄膜。PVD技术半导体芯片制造业、太阳能行业、LCD制造业等多种行业的核心技术，主要方法有真空蒸镀、电弧等离子体镀、离子镀膜、分子束外延和溅射镀膜等。
溅射是制备薄膜材料的主要技术之一，它利用离子源产生的离子，在真空中经过加速聚集，而形成高速度能的离子束流，轰击固体表面，离子和固体表面原子发生动能交换，使固体表面的原子离开固体并沉积在基底表面，被轰击的固体是制备溅射法沉积薄膜的原材料，一般被称为溅射靶材。
随着社会经济的快速发展，电子产品已经成为我们生活中不可或缺的工具和必需品。电子产品中一个非常关键的部件就是液晶显示屏，同时要对液晶显示屏进行镀膜，玻璃镀膜是通过磁控溅射镀膜工艺来实现的，而该工艺的材料则为旋转靶材。目前，中国及亚太地区旋转靶材的市场需求量超过世界总需求量的70％，市场前景广阔。磁控溅射镀膜有两个极其重要的指标参数，分别是透过率和电阻率，磁控溅射镀膜指标参数能否达标取决于旋转靶材的品质，而旋转靶材的品质是由其生产工艺和原材料粉末配方决定的。归根溯源，影响旋转靶材的品质最根本的问题是旋转靶材的配方及生产工艺。
现有技术专利 CN109267019A公开了一种硅旋转靶材及其制备方法，通过采用等离子体喷涂工艺形成环绕所述基体管的硅靶材层，获得尺寸满足工艺需求、结构致密度较高、无裂纹的硅旋转靶材，且使所述硅旋转靶材的尺寸一体化，所述硅旋转靶材的长度和厚度不受限制。但是现有的配方为纯度≥99.9％硅，其余为杂质，生产工艺也较为简单，这种配方和工艺得到的产品可以满足一定的使用要求，但是也存在较为明显的缺陷：其电阻率较高，透过率低，从而导致客户使用该靶材异常发生率高，这将严重影响到电子行业的快速发展。为了适应市场的需求，迫切需要解决上述问题。
为了使硅旋转溅射靶材在进行真空溅镀时发挥良好的性能，要求硅旋转溅射靶材具有较高的致密度、纯度、较低的含氧量等条件。
目前硅靶材的制备方法分为真空熔炼+绑定、大气等离子喷涂等多种方法，但是由于其制备工艺的限制，其靶材制备时存在以下问题：1、要使用高温设备，制备成本高；2、含氧量高、电阻率高、纯度低使用透过率不达标，满足不了（LAB值）≥93%。因此，解决硅旋转溅射靶材制造时出现的成本高、电阻率及高透过率的问题就显得尤为重要了。
发明内容
为解决上述问题，本发明提供一种高透过率硅旋转溅射靶材的制备方法，通过采用6N多晶硅重掺原料和5N多晶硅高阻原料进行破碎成粉得到6N多晶硅半成品原料和5N多晶硅半成品半成品原料，将6N多晶硅半成品原料和5N多晶硅半成品半成品原料混合稀释制得杂质含量低的高纯硅粉末，这样喷涂制得的靶材杂质含量降低，尤其是B，提高靶材在镀膜过程产品的透过率，LAB值≥93%，减低客户使用成本及满足客户大尺寸产品镀膜需求，解决了背景技术中出现的问题。
本发明的目的是提供一种高透过率硅旋转溅射靶材的制备方法，其特征在于：包括如下步骤：
步骤一：分别选取6N多晶硅重掺原料和5N多晶硅高阻原料，其中所述6N多晶硅重掺原料电阻率要求0.0001-0.0009Ω.cm，所述5N多晶硅高阻原料电阻率要求≥0.05Ω.cm；
分别对两种原料进行：打磨清洁原料外表→破碎制成10-100目粗粉→磁选除铁→进一步气流粉碎制成100-500目粉末→气流分级后形成100-400目的半成品原料，分别测试两种半成品原料的杂质含量；
步骤二：将6N多晶硅半成品原料和5N多晶硅半成品半成品原料混合稀释，制得高纯硅粉末；
所述高纯硅粉末中氧含量≤800ppm，氮≤100ppm；除气体元素外，其他杂质含量如下：B≤10ppm，Fe≤10ppm，Al≤10ppm，Ca≤10ppm，P+As的含量≤700ppm；除O、N外，Si总体纯度≥99.99%；
步骤三：对由不锈钢或钛制成的背管进行机加工至；
之后将步骤二制得的高纯硅粉末进行等离子喷涂到背管得到靶材；再对靶材进行表面抛光，最后进行机加工。
进一步改进在于：所述等离子喷涂为：
使用工装把背管装配至等离子喷涂设备，所述等离子喷涂工艺的参数为：冷却水温：0-80℃；喷嘴：直口，口径6-12mm；枪距50-500 mm；弧电流150-1000 A；弧电压30-300 V；送粉量10-100g/ g/min/路；Ar流量1000-5000L/H，压力0.3-0.8Mpa；H2流量100-1500L/H，压力0.3-0.8Mpa；载气流量50-500 L/H；风量＞1 m/s，旋转转速10-500r/min，行走速度5-500mm/s。
进一步改进在于：喷涂采用真空喷涂，确保腔体负压，氧含量为0%VOL；或采用气氛保护喷涂，气氛保护喷涂的气体为氦气、氮气、氩气中的任意一种。
进一步改进在于：气氛保护喷涂的气体为氮气，流量1-1000Nm3/h，微正压，氧含量为0%VOL进行喷涂，喷涂单边厚度控制在1-15mm。
进一步改进在于：所述步骤三中对背管机加工后还包括对其进行表面先进行喷砂粗化再进行电弧喷涂粗化。
进一步改进在于：所述抛光采用60-400目金刚石砂带进行抛光。
进一步改进在于：所述机加工包括对两端及管口进行车两端、精修。
本发明的有益效果：本发明通过采用6N多晶硅重掺原料和5N多晶硅高阻原料进行破碎成粉得到6N多晶硅半成品原料和5N多晶硅半成品半成品原料，将6N多晶硅半成品原料和5N多晶硅半成品半成品原料混合稀释制得杂质含量低的高纯硅粉末，再对背管进行等离子喷涂得到靶材，制得的靶材N≤100ppm，B≤10ppm，Fe≤10ppm，Al≤10ppm，Ca≤10ppm，P+As作为电阻率补偿控制含量≤700ppm，除O、N外Si总体纯度≥99.99%，电阻率≤2Ω.cm，密度≥2.21g/cm3，整个方法降低杂质含量，尤其是B，提高靶材在镀膜过程产品的透过率，LAB值≥93%，减低客户使用成本及满足客户大尺寸产品镀膜需求。
具体实施方式
为了加深对本发明的理解，下面将结合实施例对本发明作进一步的详述，本实施例仅用于解释本发明，并不构成对本发明保护范围的限定。
本实施例提供一种高透过率硅旋转溅射靶材的制备方法，具体步骤如下：
S1：选取6N多晶硅重掺原料，6N多晶硅重掺原料的电阻率为0.0001-0.0009Ω.cm，对原料进行打磨清洁原料外表→破碎制成50目粗粉→磁选除铁→进一步气流粉碎制成300目粉末→气流分级后形成100目的6N多晶硅半成品原料，测试半成品原料的杂质含量；
S2：选取5N多晶硅高阻原料，5N多晶硅高阻原料的电阻率为≥0.05Ω.cm，对原料进行打磨清洁原料外表→破碎制成50目粗粉→磁选除铁→进一步气流粉碎制成300目粉末→气流分级后形成100目的5N多晶硅半成品半成品原料，测试半成品原料的杂质含量；
S3：依据对两种半成品原料的杂质含量的测试结果，对6N多晶硅半成品原料及5N多晶硅半成品半成品原料混合稀释，制得高纯硅粉末；该高纯硅粉末中：氧含量≤800ppm，氮≤100ppm；除气体元素外，其他杂质含量B≤10ppm，Fe≤10ppm，Al≤10ppm，Ca≤10ppm，P+As的含量≤700ppm，除O、N外Si总体纯度≥99.99%；
S4：对不锈钢或钛管的背管进行机加工至标准范围；
S5：对背管使用喷砂机对表面进行喷砂粗化，然后采用线径直径2mm的镍铝丝进行电弧喷涂进行打底，进一步粗化背管表面，提高涂层与底层的结合强度；
S6：使用工装把背管装配至等离子喷涂设备，等离子喷涂工艺的参数为：冷却水温：40℃；喷嘴：直口，口径10mm；枪距300 mm；弧电流600 A；弧电压150 V；送粉量10-100g/g/min/路；Ar流量2000L/H，压力0.5Mpa；H2流量1000L/H，压力0.5Mpa；载气流量200 L/H；风量＞1 m/s，旋转转速：200r/min，行走速度：200mm/s；
喷涂采用气氛保护喷涂，气氛保护喷涂的气体为氮气，流量500Nm3/h，微正压，氧含量为0%VOL进行喷涂，喷涂单边厚度控制在10mm，待靶材喷涂完成，关闭等离子喷涂设备，靶材下管；
S7：对靶材采用金刚石砂带，200目，进行表面抛光；
S8：对抛光好的靶材两端及管口进行车两端、精修，确保靶材美观，达到客户要求，产品检验后包装。
本实施例将破碎成粉的6N多晶硅半成品原料和5N多晶硅半成品半成品原料进行混合稀释制得杂质含量低的高纯硅粉末，这样可以很好对原材料进行控制杂质含量，再对背管进行等离子喷涂得到靶材，制得的靶材N≤100ppm，B≤10ppm，Fe≤10ppm，Al≤10ppm，Ca≤10ppm，P+As作为电阻率补偿控制含量≤700ppm，除O、N外Si总体纯度≥99.99%，电阻率≤2Ω.cm，密度≥2.21g/cm3，整个方法降低杂质含量，尤其是B，提高靶材在镀膜过程产品的透过率，LAB值≥93%，减低客户使用成本及满足客户大尺寸产品镀膜需求。
Claims (7)
1.一种高透过率硅旋转溅射靶材的制备方法，其特征在于：包括如下步骤：
步骤一：分别选取6N多晶硅重掺原料和5N多晶硅高阻原料，其中所述6N多晶硅重掺原料电阻率要求0.0001-0.0009Ω.cm，所述5N多晶硅高阻原料电阻率要求≥0.05Ω.cm；
分别对两种原料进行：打磨清洁原料外表→破碎制成10-100目粗粉→磁选除铁→进一步气流粉碎制成100-500目粉末→气流分级后形成100-400目的半成品原料，分别测试两种半成品原料的杂质含量；
步骤二：将6N多晶硅半成品原料和5N多晶硅半成品半成品原料混合稀释，制得高纯硅粉末；
所述高纯硅粉末中氧含量≤800ppm，氮≤100ppm；除气体元素外，其他杂质含量如下：B≤10ppm，Fe≤10ppm，Al≤10ppm，Ca≤10ppm，P+As的含量≤700ppm；除O、N外，Si总体纯度≥99.99%；
步骤三：对由不锈钢或钛制成的背管进行机加工；
之后将步骤二制得的高纯硅粉末进行等离子喷涂到背管得到靶材；再对靶材进行表面抛光，最后进行机加工。
2.如权利要求1所述高透过率硅旋转溅射靶材的制备方法，其特征在于：所述等离子喷涂为：
使用工装把背管装配至等离子喷涂设备，所述等离子喷涂工艺的参数为：冷却水温：0-80℃；喷嘴：直口，口径6-12mm；枪距50-500 mm；弧电流150-1000 A；弧电压30-300 V；送粉量10-100g/ g/min/路；Ar流量1000-5000L/H，压力0.3-0.8Mpa；H2流量100-1500L/H，压力0.3-0.8Mpa；载气流量50-500 L/H；风量＞1 m/s，旋转转速10-500r/min，行走速度5-500mm/s。
3.如权利要求2所述高透过率硅旋转溅射靶材的制备方法，其特征在于：喷涂采用真空喷涂，确保腔体负压，氧含量为0%VOL；或采用气氛保护喷涂，气氛保护喷涂的气体为氦气、氮气、氩气中的任意一种。
4.如权利要求3所述高透过率硅旋转溅射靶材的制备方法，其特征在于：气氛保护喷涂的气体为氮气，流量1-1000Nm3/h，微正压，氧含量为0%VOL进行喷涂，喷涂单边厚度控制在1-15mm。
5.如权利要求1所述高透过率硅旋转溅射靶材的制备方法，其特征在于：所述步骤三中对背管机加工后还包括对其进行表面先进行喷砂粗化再进行电弧喷涂粗化。
6.如权利要求1所述高透过率硅旋转溅射靶材的制备方法，其特征在于：所述抛光采用60-400目金刚石砂带进行抛光。
7.如权利要求1所述高透过率硅旋转溅射靶材的制备方法，其特征在于：所述机加工包括对两端及管口进行车两端、精修。
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