CN106220188A - 一种窄粒度分布高纯氮化硅粉体的制备方法 - Google Patents
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Abstract
本发明涉及一种窄粒度分布高纯氮化硅粉体的制备方法,属于氮化硅粉体的制备技术领域。具体步骤为:首先在高纯硅粉中加入氮化硅稀释剂,混合均匀得到氮化反应原料,然后控制氮化反应条件得到氮化硅,最后将反应得到的氮化硅经气流磨磨细分级得到窄粒度分布的高纯氮化硅粉体。该工艺不使用添加剂,多级粒度精确配比的粒料层可以充分利用反应放出的热能,多级净化纯化保证产品纯度,是一条经济、高效、环保且可进行大规模生产的工艺。
Description
技术领域
本发明涉及一种窄粒度分布高纯氮化硅粉体的制备方法,属于氮化硅粉体的制备技术领域。
背景技术
氮化硅具有高硬度、耐磨损、耐高温,热膨胀系数小,抗腐蚀能力强,能抵抗冷热冲击等特点,应用范围极为广泛,其中高纯氮化硅主要应用于高性能陶瓷零件和光伏产业。高性能氮化硅陶瓷具有优异的机械性能、热学性能及化学稳定性,可以承受金属或高分子材料难以承受的严酷工作环境,要制得高性能陶瓷,关键在于氮化硅粉体的高纯度及窄粒度分布;多晶硅铸锭是光伏产业链的重要工序,硅锭的纯度直接影响太阳能电池片的光电转换效率,高纯氮化硅涂层用于多晶硅铸锭过程的脱模剂,同时隔绝坩埚杂质污染硅锭,氮化硅粉体的高纯度及窄粒度分布是涂层良好的致密性和结合性的保证。
从国内的指标测试来看,氮化硅粉体的粒度主要集中在0.5um~5um之间,粒度分布较宽,金属杂质含量高,很大程度上影响后期使用效果。因此,窄粒度分布高纯氮化硅粉体是氮化硅粉体行业的主要发展目标。
发明内容
针对现有技术中存在的缺陷,本发明的目的在于提供一种窄粒度分布高纯氮化硅粉体的制备方法。本发明的技术方案如下:
(1)在高纯硅粉中加入氮化硅稀释剂,不使用添加剂,混合均匀得到氮化反应原料;
(2)将步骤(1)中的氮化反应原料铺成多级粒度精确配比的粒料层置于烧结炉内,通入氮气以置换出炉内空气,继续通入氮气,加热到1400~1450℃,高纯硅粉与氮气充分反应得到氮化硅;
(3)冷却至室温后,将步骤(2)得到的氮化硅破碎后经气流磨磨细分级,得到窄粒度分布的高纯氮化硅粉体。
本发明所述高纯硅粉的粒度为10~50um。
本发明所述氮气纯度优选≥99.99%。
本发明所述氮化硅稀释剂的添加量为高纯硅粉的10%~20%。
本发明所述氮化反应时间为5~20h。
本发明多级净化纯化贯穿整个制备过程。
与现有技术相比,本发明的有益效果:本发明不使用添加剂,多级粒度精确配比的粒料层可以充分利用反应放出的热能,多级净化纯化保证产品纯度,是一条经济、高效、环保且可进行大规模生产的工艺。
具体实施方式
以下实施方式仅仅是为了说明本发明的原理而采用的示例性实施方式,然而本发明并不局限于此。对于本领域的普通技术人员而言,在不脱离本发明的精神和实质的情况下,可以做出各种变形和改进,这些变形和改进也视为本发明的保护范围。
实施例1
(1)在10~30um的高纯硅粉中加入氮化硅稀释剂,氮化硅稀释剂的添加量为高纯硅粉的10%,不使用添加剂,混合均匀得到氮化反应原料;
(2)将步骤(1)中的氮化反应原料铺成多级粒度精确配比的粒料层置于烧结炉内,通入氮气以置换出炉内空气,氮气纯度为99.99%,继续通入氮气,加热到1400℃,氮化反应5h,高纯硅粉与氮气充分反应得到氮化硅;
(3)冷却至室温后,将步骤(2)得到的氮化硅破碎后经气流磨磨细分级,得到窄粒度分布的高纯氮化硅粉体,高纯氮化硅粉体纯度为99.99%,粒度D10为0.89um,D50为1.16um,D90为1.47um。
实施例2
(1)在20~50um的高纯硅粉中加入氮化硅稀释剂,氮化硅稀释剂的添加量为高纯硅粉的20%,不使用添加剂,混合均匀得到氮化反应原料;
(2)将步骤(1)中的氮化反应原料铺成多级粒度精确配比的粒料层置于烧结炉内,通入氮气以置换出炉内空气,氮气纯度为99.99%,继续通入氮气,加热到1420℃,氮化反应20h,高纯硅粉与氮气充分反应得到氮化硅;
(3)冷却至室温后,将步骤(2)得到的氮化硅破碎后经气流磨磨细分级,得到窄粒度分布的高纯氮化硅粉体,高纯氮化硅粉体纯度为99.999%,粒度D10为1.53um,D50为1.98um,D90为2.17um。
实施例3
(1)在10~40um的高纯硅粉中加入氮化硅稀释剂,氮化硅稀释剂的添加量为高纯硅粉的12%,不使用添加剂,混合均匀得到氮化反应原料;
(2)将步骤(1)中的氮化反应原料铺成多级粒度精确配比的粒料层置于烧结炉内,通入氮气以置换出炉内空气,氮气纯度为99.999%,继续通入氮气,加热到1450℃,氮化反应10h,高纯硅粉与氮气充分反应得到氮化硅;
(3)冷却至室温后,将步骤(2)得到的氮化硅破碎后经气流磨磨细分级,得到窄粒度分布的高纯氮化硅粉体,高纯氮化硅粉体纯度为99.99%,粒度D10为1.45um,D50为1.86um,D90为2.27um。
实施例4
(1)在20~40um的高纯硅粉中加入氮化硅稀释剂,氮化硅稀释剂的添加量为高纯硅粉的15%,不使用添加剂,混合均匀得到氮化反应原料;
(2)将步骤(1)中的氮化反应原料铺成多级粒度精确配比的粒料层置于烧结炉内,通入氮气以置换出炉内空气,氮气纯度为99.99%,继续通入氮气,加热到1440℃,氮化反应15h,高纯硅粉与氮气充分反应得到氮化硅;
(3)冷却至室温后,将步骤(2)得到的氮化硅破碎后经气流磨磨细分级,得到窄粒度分布的高纯氮化硅粉体,高纯氮化硅粉体纯度为99.999%,粒度D10为0.39um,D50为0.86um,D90为1.17um。
Claims (6)
1.一种窄粒度分布高纯氮化硅粉体的制备方法,其特征在于,通过以下步骤实现:
(1)在高纯硅粉中加入氮化硅稀释剂,不使用添加剂,混合均匀得到氮化反应原料;
(2)将步骤(1)中的氮化反应原料铺成多级粒度精确配比的粒料层置于烧结炉内,通入氮气以置换出炉内空气,继续通入氮气,加热到1400~1450℃,高纯硅粉与氮气充分反应得到氮化硅;
(3)冷却至室温后,将步骤(2)得到的氮化硅破碎后经气流磨磨细分级,得到窄粒度分布的高纯氮化硅粉体。
2.根据权利要求1所述的一种窄粒度分布高纯氮化硅粉体的制备方法,其特征在于:所述高纯硅粉的粒度为10~50um。
3.根据权利要求1所述的一种窄粒度分布高纯氮化硅粉体的制备方法,其特征在于:所述氮气纯度优选≥99.99%。
4.根据权利要求1所述的一种窄粒度分布高纯氮化硅粉体的制备方法,其特征在于:所述氮化硅稀释剂的添加量为高纯硅粉的10%~20%。
5.根据权利要求1所述的一种窄粒度分布高纯氮化硅粉体的制备方法,其特征在于:所述氮化反应时间为5~20h。
6.根据权利要求1所述的一种窄粒度分布高纯氮化硅粉体的制备方法,其特征在于:多级净化纯化贯穿整个制备过程。
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CN109650904A (zh) * | 2017-10-10 | 2019-04-19 | 河北高富氮化硅材料有限公司 | 一种改善氮化硅粉体粒径及分布的球磨方法 |
CN112850665A (zh) * | 2021-01-30 | 2021-05-28 | 埃克诺新材料(大连)有限公司 | 一种氮化硅粉体的制备方法 |
CN113493191A (zh) * | 2020-04-08 | 2021-10-12 | 新疆晶硕新材料有限公司 | 制备高纯度α-氮化硅粉的方法及高纯度α-氮化硅粉 |
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CN102060538A (zh) * | 2010-11-30 | 2011-05-18 | 沈阳鑫劲粉体工程有限责任公司 | 利用高温旋转炉合成氮化硅粉末的方法 |
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CN109650904A (zh) * | 2017-10-10 | 2019-04-19 | 河北高富氮化硅材料有限公司 | 一种改善氮化硅粉体粒径及分布的球磨方法 |
CN113493191A (zh) * | 2020-04-08 | 2021-10-12 | 新疆晶硕新材料有限公司 | 制备高纯度α-氮化硅粉的方法及高纯度α-氮化硅粉 |
CN113493191B (zh) * | 2020-04-08 | 2022-11-22 | 新疆晶硕新材料有限公司 | 制备高纯度α-氮化硅粉的方法及高纯度α-氮化硅粉 |
CN112850665A (zh) * | 2021-01-30 | 2021-05-28 | 埃克诺新材料(大连)有限公司 | 一种氮化硅粉体的制备方法 |
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