CN106747452A - 一种电阻炉生产碳化硼结晶块的方法 - Google Patents

一种电阻炉生产碳化硼结晶块的方法 Download PDF

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CN106747452A
CN106747452A CN201611043734.3A CN201611043734A CN106747452A CN 106747452 A CN106747452 A CN 106747452A CN 201611043734 A CN201611043734 A CN 201611043734A CN 106747452 A CN106747452 A CN 106747452A
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boron carbide
boron
powder
reducing agent
resistance furnace
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邢鹏飞
高帅波
王帅
李欣
都兴红
李盼
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Northeastern University China
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Abstract

一种电阻炉生产碳化硼结晶块的方法,按以下步骤进行:(1)将碳还原剂破碎筛分;(2)将硼酸和碳还原剂粉混合;(3)加水压制成球团;(4)放入电阻炉中进行脱水,然后升温至1900~2500℃,冶炼20~48h,获得碳化硼结晶块。本发明的方法不仅实现了炉内温度的可控,同时还提高了原料利用率,保障了炉内反应原料的硼碳比,降低了生产成本,节约了能源,而且还提高了高品质碳化硼的产出率,此外,原料挥发较少,极大降低了粉尘污染,改善车间环境。

Description

一种电阻炉生产碳化硼结晶块的方法
技术领域
[0001]本发明属于材料技术领域,特别涉及一种电阻炉生产碳化硼结晶块的方法。
背景技术
[0002]碳化硼,别名黑钻石,分子式为B4C,通常为灰黑色微粉,具有一系列优良的性质: 莫氏硬度为9_ 3,显微硬度为55〜67GPa,仅次于金刚石和立方氮化硼;密度低,理论密度为 2.52X 103 kg/m3;耐腐蚀性好,化学性质稳定,常温下不与酸和碱等大多数物质反应。基于 以上优良性质,碳化硼材料被广泛应用在机械研磨、耐火材料、工程陶瓷、核工业和军事等 不同领域。
[0003]、近年来,蓝宝石被广泛用作LED最理想的衬底材料。同时由于其良好的机械强度、 耐磨耐摔和抗伤性等特性,又逐步应用于高端手机领域,如手机屏幕、触控键以及镜头等。 这些应用都将促使蓝宝石的用量大幅提高。然而以上应用都需要先将蓝宝石晶体切割成厚 度为800wn左右的晶片,然后再通过研磨和抛光工序将蓝宝石加工成7〇〇wn左右的晶片。其 中,研磨工序是蓝^石关键环节,过去主要是采用不同粒度的金刚石粉进行研磨,但是由于 金刚石价格昂贵且产量低,现在国内外逐渐采用价格相对低廉的碳化硼替代金刚石对蓝宝 石进行研磨。
[0004]目前碳化硼的工业生产主要方法就是在电弧炉内用碳还原剂还原硼酸或硼酐来 制备的。该方法是将硼酸或硼酐与碳还原剂均匀混合后放入电弧炉中,碳作为还原剂,在一 定温度下合成碳化硼粉末;但其存在着以下缺点:1、冶炼温度不可控,冶炼的能耗高(碳化 硼结晶块的吨电耗约在27500〜28500kwh);2、冶炼出的结晶块品质差、高品质碳化硼产出率 低;3、碳化硼冶炼粉尘大、污染重;4、B/C比难以控制,质量差。
发明内容
[0005] 针对目前碳化硼冶炼技术及其产品存在的上述不足之处,本发明提出了一种电阻 炉生产碳化硼结晶块的方法,通过将硼酸和碳还原剂混合制球,然后冶炼,提高碳化硼品质 的同时,降低生产成本。
[0006] 本发明的方法按照以下步骤进行: (1) 先将碳还原剂破碎成粉料,筛分得到粒度< lcm碳还原剂粉;所述的碳还原剂是石 油焦、石墨和炭黑中的一种或两种以上; (2) 将硼酸和碳还原剂粉混合,制成混合粉料,混合粉料中硼酸占总重量的65〜80%; (3) 将混合粉料加水压制成直径1〇〜1〇〇圓的球团; (4) 将球团放入电阻炉中进行脱水,脱水温度50〜500°C,时间2〜1 Oh;然后升温至1900〜 2500°C,冶炼20〜48h,获得碳化硼结晶块。
[0007]上述的碳化硼结晶按重量百分比总硼含量为77 • 2〜80 • 6%,总碳含量为16.5〜21%, 硼碳摩尔比为4.08〜5.40。
[0008]与现有冶炼技术相比,本发明的优点是:冶炼工艺不仅实现了炉内温度的可控,同 时还提f 了原料利用率,保障了炉内反应原料的硼碳比,降低了生产成本,节约了能源,而 且还提高了高品质碳化硼的产出率,此外,原料挥发较少,极大降低了粉尘污染,改善车间 环境。
附图说明
[0009]图1为本发明的电阻炉生产碳化硼结晶块以及制备粒度砂的方法流程示意图; 图2为本发明实施例1的碳化硼结晶块制备成粒度砂后的XRD图; 图3为本发明实施例1的碳化硼结晶块制备成粒度砂后的SEM图。
具体实施方式
[0010]本发明实施例中采用的硼酸为市购,纯度多98.0%。
[0011]本发明实施例中的石油焦、石墨和炭黑为市购产品,石墨纯度彡98.0%,石油焦纯 度彡85%,炭黑纯度彡95%。
[0012]本发明实施例中制备球团是采用制球机。
[0013]本发明实施例中制备碳化硼结晶块时硼的利用率多99%。
[0014]本发明的碳化硼结晶块按常规工艺经破碎、分级、酸洗和筛分后制成粒度砂(其余 部分为低品质碳化硼,用于制作耐火材料的),粒度砂的粒度为250〜350um,纯度高于 JB3249-83标准中对纯度的要求,符合做蓝宝石研磨的要求。
[0015] 本发明实施例中的常规工艺是采用公开号为CN103864077B所公开的方案进行。
[0016] 实施例1 采用石油焦、石墨和炭黑作为碳还原剂,先将碳还原剂破碎成粉料,筛分得到粒度< lcm碳还原剂粉; 将硼酸和碳还原剂粉混合,制成混合粉料,混合粉料中硼酸占总重量的65%,石油焦粉 15%,石墨粉10%,炭黑粉10%; 将混合粉料加水压制成直径25mm的球团; 将球团放入电阻炉中进行脱水,脱水温度50。(:,时间10h;然后升温至2500。(:,冶炼20h, 获得碳化硼结晶块; 上述的碳化硼结晶按重量百分比总硼含量为77.2%,总碳含量为21%,硼碳摩尔比为 4.08; 碳化硼结晶块按常规工艺经破碎、分级、酸洗和筛分后制成粒度砂,粒度砂的粒度为 250〜35〇Mi,XRD分析结果如图2所示,SEM分析结果如图3所示。
[0017] 实施例2 方法同实施例1,不同点在于: ⑴混合粉料中硼酸占总重量的70%,石油焦粉10%,石墨粉10%,炭黑粉1 〇%; (2) 压制成直径40mm的球团; (3) 脱水温度50(TC,时间2h;升温至1900 -C,冶炼48h; (4) 总硼含量为77 • 4%,总碳含量为20.2%,硼碳摩尔比为4 • 26。
[0018] 实施例3 方法同实施例1,不同点在于: (1) 混合粉料中硼酸占总重量的80%,石油焦粉5%,石墨粉10%,炭黑粉5%; (2) 压制成直径10mm的球团; (3) 脱水温度400 °C,时间3h;升温至2000 °C,冶炼24h; (4) 总硼含量为79.6%,总碳含量为17.4%,硼碳摩尔比为5.08。
[0019] 实施例4 方法同实施例1,不同点在于: (1) 混合粉料中硼酸占总重量的75%,石油焦粉15%,石墨粉5%,炭黑粉5%; (2) 压制成直径100mm的球团; (3) 脱水温度300 °C,时间4h;升温至2200 °C,冶炼30h; (4) 总硼含量为80.2%,总碳含量为16.5%,硼碳摩尔比为5.40。
[0020] 实施例5 方法同实施例1,不同点在于: (1) 混合粉料中硼酸占总重量的65%,石油焦粉35%; (2) 压制成直径60mm的球团; (3) 脱水温度200 °C,时间6h;升温至2000 °C,冶炼40h; (4) 总硼含量为79.8%,总碳含量为16.6%,硼碳摩尔比为5.34。
[0021] 实施例6 方法同实施例1,不同点在于: (1) 混合粉料中硼酸占总重量的70%,石墨粉30%; (2) 压制成直径75mm的球团; (3) 脱水温度100 °C,时间8h;升温至2500 °C,冶炼20h; (4) 总硼含量为78.4%,总碳含量为17.8%,硼碳摩尔比为4.89。
[0022] 实施例7 方法同实施例1,不同点在于: (1) 混合粉料中硼酸占总重量的80%,炭黑粉20%; (2) 压制成直径90mm的球团; (3) 脱水温度350 °C,时间5h;升温至1900 °C,冶炼48h; (4) 总硼含量为80.6%,总碳含量为18.7%,硼碳摩尔比为4.79。

Claims (3)

1. 一种电阻炉生产碳化硼结晶块的方法,其特征在于按以下步骤进行: (1) 先将碳还原剂破碎成粉料,筛分得到粒度<lcm碳还原剂粉;所述的碳还原剂是石 油焦、石墨和炭黑中的一种或两种以上; (2) 将硼酸和碳还原剂粉混合,制成混合粉料,混合粉料中硼酸占总重量的65〜8〇%; ⑶将混合粉料加水压制成直径10〜100mm的球团; (4)将球团放入电阻炉中进行脱水,脱水温度SO〜5〇〇,时间2〜1 Oh;然后升温至1900〜 2500°C,冶炼20〜48h,获得碳化硼结晶块。
2.根据权利要求1所述的一种电阻炉生产碳化硼结晶块的方法,其特征在于所述的碳 化硼结晶按重量百分比总硼含量为77 • 2〜8〇 • 6%,总碳含量为16 • 5〜21%,硼碳摩尔比为4.08〜 5.40。
3.根据权利要求1所述的一种电阻炉生产碳化硼结晶块的方法,其特征在于所述的碳 化硼结晶块按常规工艺经破碎、分级、酸洗和筛分后制成粒度砂,粒度砂的粒度为250~350U m〇
CN201611043734.3A 2016-11-24 2016-11-24 一种电阻炉生产碳化硼结晶块的方法 Pending CN106747452A (zh)

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Publication number Priority date Publication date Assignee Title
CN108821772A (zh) * 2018-07-20 2018-11-16 东北大学 一种添加氧化铝粉制备碳化硼铝系复合陶瓷粉的方法
CN109019605A (zh) * 2018-09-25 2018-12-18 金玛(通辽)硼材料有限公司 一种碳化硼材料的冶炼方法
CN109081697A (zh) * 2018-08-28 2018-12-25 东北大学 一种制备B4C/SiC复合陶瓷粉的方法

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CN101269967A (zh) * 2008-05-13 2008-09-24 武汉理工大学 一种制备碳化硼陶瓷的方法
CN102161586A (zh) * 2011-04-26 2011-08-24 大连金玛硼业科技集团有限公司 一种粒度可控的碳化硼陶瓷粉体的制备方法
CN105502404A (zh) * 2016-01-22 2016-04-20 东北大学 一种高品质碳化硼结晶块的冶炼制备方法

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CN101269967A (zh) * 2008-05-13 2008-09-24 武汉理工大学 一种制备碳化硼陶瓷的方法
CN102161586A (zh) * 2011-04-26 2011-08-24 大连金玛硼业科技集团有限公司 一种粒度可控的碳化硼陶瓷粉体的制备方法
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108821772A (zh) * 2018-07-20 2018-11-16 东北大学 一种添加氧化铝粉制备碳化硼铝系复合陶瓷粉的方法
CN108821772B (zh) * 2018-07-20 2021-11-05 东北大学 一种添加氧化铝粉制备碳化硼铝系复合陶瓷粉的方法
CN109081697A (zh) * 2018-08-28 2018-12-25 东北大学 一种制备B4C/SiC复合陶瓷粉的方法
CN109019605A (zh) * 2018-09-25 2018-12-18 金玛(通辽)硼材料有限公司 一种碳化硼材料的冶炼方法
CN109019605B (zh) * 2018-09-25 2022-03-11 通辽中硼新材料科技有限公司 一种碳化硼材料的冶炼方法

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