CN109400166A - 晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法 - Google Patents

晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法 Download PDF

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CN109400166A
CN109400166A CN201910029152.7A CN201910029152A CN109400166A CN 109400166 A CN109400166 A CN 109400166A CN 201910029152 A CN201910029152 A CN 201910029152A CN 109400166 A CN109400166 A CN 109400166A
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邢鹏飞
高帅波
刘坤
都兴红
王帅
孔剑
魏冬卉
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Northeastern University China
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Abstract

本发明提出了利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法。具体步骤如下:(1)将碳质还原剂破碎成粒径细小的颗粒;(2)将破碎好的碳质还原剂粉,硼酸粉和晶体硅金刚线切割废料按一定的配比进行混料;(3)向混合均匀的粉料中加入水并压制成球团;(4)将球团放入到烘箱中进行烘干,除去其中的自由水;(5)将球团放入感应炉内进行高温冶炼;(6)将得到的产品破碎并进行分级除杂;(7)将产品粉压块烧结,制备碳化硼碳化硅复合陶瓷。本方法可以有效改善炉况,增加炉料的透气性,实现节能减排;增加碳化硅和碳化硼均匀弥散,提高碳化硼复合陶瓷的性能;实现晶体硅切割废料的回收和二次利用,避免了废料的污染环境等问题。

Description

晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法
技术领域
本发明涉及一种利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法,属于碳化硼复合陶瓷的制备领域。
背景技术
复合材料通常具有良好综合性能,兼具两种或两种以上材料的特点,能改善单一材料的性能,如提高强度、增加韧性、抗冲击抗疲劳性能和改善化学稳定性、介电性能等。碳化硼复合陶瓷作为高温结构材料用的陶瓷复合材料,主要用于宇航,军工等部门。此外,在机械、化工、电子技术等领域也广泛采用各种陶瓷复合材料。
随着对太阳能的研究和发展,太阳能电池作为有效利用太阳能的一种装置,被广泛应用于相关行业。其中,晶体硅片因作为太阳能电池的主要组成部分,所以需求量得到了显著的提升。然而在晶体硅切割制备晶体硅片的过程中,有将近40%高纯硅以粉末的形式进入到切割废料浆中,因此,对这部分高纯度的硅粉进行回收利用是很有价值和意义的。
此外,传统的电弧炉冶炼碳化硼过程存在许多不足之处,如冶炼温度不均匀,弧区温度高,不可控;硼酸挥发损失严重;气体排放量高;氧化硼粘度高,阻碍了气体的及时排出,不利于碳化硼的生成,同时增加了炉况的复杂性和处理难度。鉴于存在的这些不足之处进行改善,直接向冶炼原料中加入晶体硅切割废料可以有效改善炉料的透气性,改善炉况。
本文通过直接冶炼过程中添加晶体硅金刚线切割废料冶炼,再烧结制备碳化硼碳化硅复合陶瓷,与传统制备碳化硼碳化硅复合陶瓷的原料(碳化硼粉、碳化硅粉)简单机械混合相比较,碳化硼和碳化硅在微观尺度上更紧密结合,具有更高的反应活性,有助于烧结致密化。
发明内容
针对传统电弧炉冶炼存在不足的问题和当前切割废料回收利用现状,针对复合陶瓷的优势,直接在原料中加入添加剂比传统冶炼过程存在的优势,本发明提出了一种利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法。
实现本发明可以按照以下步骤进行:
(1)将碳质还原剂破碎成粒径细小的颗粒,所述碳质还原剂是石墨、石油焦和活性炭的混合物;
(2)将破碎好的碳质还原剂粉、硼酸粉和晶体硅金刚线切割废料按重量配比进行混料;所述的重量配比为:硼酸粉20~60%,石油焦不大于35%,石墨不大于25%,活性炭不大于35%,晶体硅金刚线切割废料5~35%;
(3)向混合均匀的粉料中加入水并压制成球团;
(4)将球团放入到烘箱中进行烘干,除去其中的自由水;
(5)将球团放入感应炉内进行高温冶炼,冶炼温度控制在1000~2000℃,冶炼时间控制在20~80min;
(6)将得到的产品破碎并进行分级除杂;
(7)将产品粉压块烧结,制备碳化硼碳化硅复合陶瓷。
所述步骤(1)所述的碳质还原剂破碎的粒度不大于5mm。
所述步骤(3)所述的压制球团的压力为10~30Mpa,保压时间10~50s,球团的直径为15~35mm。
所述步骤(4)所述的烘干的温度控制在80~120℃,烘干时间为2~10h。
所述步骤(5)所述的感应炉可以快速升温速率可调。
所述步骤(6)所述的破碎的产品的颗粒的粒径不大于1mm。
所述步骤(7)所述的烧结温度控制在1400~2000℃之间,烧结时间控制在20~100min。
本发明的优点是:
(1)采用了直接在冶炼原料中添加碳化硅的方法,可以实现碳化硼和碳化硅的良好的结合,促进后续的烧结进行。
(2)直接向原料中加入切割废料,可以有效地改善冶炼炉况,提高原料的透气性,有利于反应的顺利进行,改善冶炼环境。
(3)有效的实现了晶体硅切割废料的二次利用,并达到了节能减排的目的。
附图说明
图1为本发明的一种利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法的新型冶炼工艺的流程图。
具体实施方式
实施例1
1、将碳质还原剂进行研磨,筛分;
2、将硼酸粉、碳质还原剂粉和晶体硅金刚线切割废料按照一定的重量比进行配料:硼酸20%,石墨20%,石油焦15%,活性炭15%,然后在配好的原料中加入30%的切割废料。
3、将混好的料在压球机上压制成15mm厚的团块;
4、将压制好的团块湿料进行烘干,烘干温度为90℃,烘干时间为7h;
5、将已烘干的团块放入感应炉内进行高温冶炼,冶炼温度为1300℃,冶炼时间为70min,制备成碳化硼复合陶瓷粗粉;
6、将碳化硼复合陶瓷粗粉进行破碎,并进行分级和除杂,得到碳化硼复合陶瓷精粉;
7、将产品粉压块,在1500℃下烧结,时间为90min,制备碳化硼碳化硅复合陶瓷。
实施例2
1、将碳质还原剂进行研磨,筛分;
2、将硼酸粉、碳质还原剂粉和晶体硅金刚线切割废料按照一定的重量比进行配料:硼酸40%,石墨10%,石油焦25%,活性炭5%,然后在配好的原料中加入20%的切割废料。
3、将混好的料在压球机上压制成25mm厚的团块;
4、将压制好的团块湿料进行烘干,烘干温度为100℃,烘干时间为9h;
5、将已烘干的团块放入感应炉内进行高温冶炼,冶炼温度为1500℃,冶炼时间为60min,制备成碳化硼复合陶瓷粗粉;
6、将碳化硼复合陶瓷粗粉进行破碎,并进行分级和除杂,得到碳化硼复合陶瓷精粉;
7、将产品粉压块,在1600℃下烧结,时间为80min,制备碳化硼碳化硅复合陶瓷。
实施例3
1、将碳质还原剂进行研磨,筛分;
2、将硼酸粉、碳质还原剂粉和晶体硅金刚线切割废料按照一定的重量比进行配料:硼酸50%,石墨10%,石油焦15%,活性炭15%,然后在配好的原料中加入10%的切割废料。
3、将混好的料在压球机上压制成30mm厚的团块;
4、将压制好的团块湿料进行烘干,烘干温度为110℃,烘干时间为4h;
5、将已烘干的团块放入感应炉内进行高温冶炼,冶炼温度为1750℃,冶炼时间为55min,制备成碳化硼复合陶瓷粗粉;
6、将碳化硼复合陶瓷粗粉进行破碎,并进行分级和除杂,得到碳化硼复合陶瓷精粉;
7、将产品粉压块,在1800℃下烧结,时间为65min,制备碳化硼碳化硅复合陶瓷。
实施例4
1、将碳质还原剂进行研磨,筛分;
2、将硼酸粉、碳质还原剂粉和晶体硅金刚线切割废料按照一定的重量比进行配料:硼酸45%,石墨25%,石油焦15%,活性炭10%,然后在配好的原料中加入5%切割废料。
3、将混好的料在压球机上压制成20mm厚的团块;
4、将压制好的团块湿料进行烘干,烘干温度为100℃,烘干时间为6.5h;
5、将已烘干的团块放入感应炉内进行高温冶炼,冶炼温度为1950℃,冶炼时间为50min,制备成碳化硼复合陶瓷粗粉;
6、将碳化硼复合陶瓷粗粉进行破碎,并进行分级和除杂,得到碳化硼复合陶瓷精粉;
7、将产品粉压块,在1900℃下烧结,时间为50min,制备碳化硼碳化硅复合陶瓷。
实施例5
1、将碳质还原剂进行研磨,筛分;
2、将硼酸粉、碳质还原剂粉和晶体硅金刚线切割废料按照一定的重量比进行配料:硼酸40%,石墨5%,石油焦35%,活性炭5%,然后在配好的原料中加入15%的切割废料。
3、将混好的料在压球机上压制成25mm厚的团块;
4、将压制好的团块湿料进行烘干,烘干温度为105℃,烘干时间为3h;
5、将已烘干的团块放入感应炉内进行高温冶炼,冶炼温度为1950℃,冶炼时间为45min,制备成碳化硼复合陶瓷粗粉;
6、将碳化硼复合陶瓷粗粉进行破碎,并进行分级和除杂,得到碳化硼复合陶瓷精粉;
7、将产品粉压块,在1700℃下烧结,时间为50min,制备碳化硼碳化硅复合陶瓷。

Claims (10)

1.一种利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法,其特征在于,包括如下步骤:
(1)将碳质还原剂破碎成粒径细小的颗粒,所述碳质还原剂是石墨、石油焦和活性炭的混合物;
(2)将破碎好的碳质还原剂粉、硼酸粉和晶体硅金刚线切割废料按重量配比进行混料;所述的重量配比为:硼酸粉20~60%,石油焦不大于35%,石墨不大于25%,活性炭不大于35%,晶体硅金刚线切割废料5~35%;
(3)向混合均匀的粉料中加入水并压制成球团;
(4)将球团放入到烘箱中进行烘干,除去其中的自由水;
(5)将球团放入感应炉内进行高温冶炼,冶炼温度控制在1000~2000℃,冶炼时间控制在20~80min;
(6)将得到的产品破碎并进行分级除杂;
(7)将产品粉压块烧结,制备碳化硼碳化硅复合陶瓷。
2.根据权利要求1所述的利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法,其特征在于,步骤(1)所述的碳质还原剂破碎的粒度不大于5mm。
3.根据权利要求1或2所述的利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法,其特征在于,步骤(3)所述的压制球团的压力为10~30Mpa,保压时间10~50s,球团的直径为15~35mm。
4.根据权利要求1或2所述的利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法,其特征在于,步骤(4)所述的烘干的温度控制在80~120℃,烘干时间为2~10h。
5.根据权利要求3所述的利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法,其特征在于,步骤(4)所述的烘干的温度控制在80~120℃,烘干时间为2~10h。
6.根据权利要求1或2或5所述的利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法,其特征在于,步骤(6)所述的破碎的产品的颗粒的粒径不大于1mm。
7.根据权利要求3所述的利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法,其特征在于,步骤(6)所述的破碎的产品的颗粒的粒径不大于1mm。
8.根据权利要求4所述的利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法,其特征在于,步骤(6)所述的破碎的产品的颗粒的粒径不大于1mm。
9.根据权利要求1或2或5或7或8所述的利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法,其特征在于,步骤(7)所述的烧结温度控制在1400~2000℃之间,烧结时间控制在20~100min。
10.根据权利要求3所述的利用晶体硅金刚线切割废料制备碳化硼碳化硅复合陶瓷的方法,其特征在于,步骤(7)所述的烧结温度控制在1400~2000℃之间,烧结时间控制在20~100min。
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