CN116854480B - 碳热还原法制备氮化铝粉体的方法 - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 28
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 27
- 230000008569 process Effects 0.000 title claims description 8
- 239000000463 material Substances 0.000 claims abstract description 73
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- 239000002994 raw material Substances 0.000 claims abstract description 51
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- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 34
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
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- 239000000758 substrate Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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Abstract
本发明涉及一种碳热还原法制备氮化铝粉体的方法,包括如下步骤:制备原料球,将氧化铝与炭黑配比混合,装入球磨机中混合磨料,过筛后造粒得到原料球备用;将上述制备好的原料球投入加热炉,所述加热炉内转动安装有载料容器,加热炉上连通的氮气管道,所述原料球投放在载料容器内;将氮气通过氮气管道通入加热炉,启动加热炉对炉内物体进行加热,加热温度在1600℃‑1800℃,加热时间为3h;将反应后的产物收集至除碳装置,并向除碳装置内通入空气,除碳装置内温度600℃‑650℃;对除碳装置内反应后的产物进行收集,即得到成品氮化铝粉体。本发明的碳热还原法制备氮化铝粉体的方法能够促进原料充分反应,制得的成品纯度高。
Description
技术领域
本发明涉及氮化铝粉体制备技术领域,特别是涉及一种碳热还原法制备氮化铝粉体的方法。
背景技术
氮化铝陶瓷(AIN陶瓷)由于高热导、低热膨胀系数以及高强度、高耐蚀性、绝缘、低电容率等优良的综合性能,已成为电子元件理想的封装和基板材料,氮化铝陶瓷的由氮化铝粉末烧结而成,氮化铝粉末的制备对最终氮化陶瓷的烧结、成型以及导热效率等性能有重要影响。氮化铝陶瓷粉末的合成方法很多,目前有铝粉直接氮化法、碳热还原法、化学气相沉积法、溶胶一凝胶法、自蔓延高温合成法和等离子化学合成法等多种方法,其中碳热还原法生产出来的产品纯度高、成型与烧结性能好,采用碳热还原法制备氮化铝粉末时,由于原料球在加热炉内受热时不会被搅动,且原料具有一定的厚度,原料球在与氮气反应时存在反应不均匀充分的情况,且当原料堆积的厚度增加后,表层的原料和内部的原料的反应程度会产生较大差异,导致最终的氮化铝粉体成分产生偏差。
发明内容
为克服现有技术存在的技术缺陷,本发明提供一种碳热还原法制备粉体的方法,其能够促进原料充分反应,制得的成品纯度高。
本发明采用的技术解决方案是:碳热还原法制备氮化铝粉体的方法,包括如下步骤
S1、制备原料球,将氧化铝与炭黑配比混合,装入球磨机中混合磨料,过筛后造粒得到原料球备用;
S2、将上述制备好的原料球投入加热炉,所述加热炉内转动安装有载料容器,加热炉上连通的氮气管道,所述原料球投放在载料容器内;
S3、将氮气通过氮气管道通入加热炉,启动加热炉对炉内物体进行加热,加热温度在1600℃-1800℃,加热时间为3h;
S4、将反应后的产物收集至除碳装置,并向除碳装置内通入空气,除碳装置内温度600℃-650℃;
S5、对除碳装置内反应后的产物进行收集,即得到成品氮化铝粉体。
优选地,所述氧化铝和炭黑的质量比为2:0.6-1.2。
优选地,向所述氧化铝和炭黑组成的原料球中加入其总重量11%的氮化铝晶种及总重量5%的烧结助剂。
优选地,所述加热炉包括炉体,所述载料容器可转动安装在炉体底部,炉体外设有驱动载料容器转动的驱动机构,所述载料容器内壁连接有载料板,所述炉体上端连接与所述载料容器连通的氮气通道,所述载料容器内壁连接有载料板,所述氮气管道的出气端对正所述载料板。
优选地,所述氮气通道包括穿设在炉体顶部的进气管道及连接在进气管道下端的多孔布气板,所述多孔布气板的上端设有与所述进气管道连通的进气孔,所述多孔布气板的下端设有多个出气孔,每个所述出气孔上设有棱锥体,所述棱锥体上设有通道,所述通道具有与出气孔连通的一个进气端和多个分布在棱锥体表面的出气端。
优选地,所述载料板为环形板,所述多孔布气板为扇形板,所述多孔布气板的进气孔设在其圆心处,所述多孔布气板的底端设有刮料板,所述刮料板设在多孔布气板的一条直边上且所述刮料板的底端高度高于棱锥体的底端高度,多个所述出气孔沿多条绕布气板圆心的弧形路径排布。
优选地,所述炉体的顶部穿设有粉末管道,所述粉末管道的下端对准所述载料板的顶面。
优选地,所述载料容器的转速为0.05r/min-0.1r/min。
本发明的有益效果在于:本发明的加热炉的炉体内可转动安装有载料容器,所述载料容器内壁连接有载料板,所述炉体上端连接与所述载料容器连通的进气管道,进气管道的下端连接有多孔布气板,作业时,将原料投放在载料板上,驱动机构驱动载料容器转动,多孔布气板上刮料板推动原料堆使其行成厚度均匀的原料层,同时多孔布气板下端的棱锥体进入原料层并向原料层内注入氮气,氮气在与原料反应的同时会推动原料翻滚,使得氮气和各种原料处于流动混合的状态,各个反应组分可充分反应,提高了产品的纯度。
附图说明
图1为本发明加热炉的结构示意图。
图2为图1中A处的局部放大图。
图3为本发明多孔布气板的仰视图。
图4为本发明多孔布气板的俯视图。
图5为本发明棱锥体的结构示意图。
附图标记说明:1、炉体;101、进气管道;1011、多孔布气板;10111、进气孔;10112、出气孔;1012、刮料板;1013、棱锥体;10131、进气端;10132、出气端;102、粉末管道;2、载料容器;201、载料板;202、驱动机构。
具体实施方式
下面结合附图对本发明作进一步说明:
如图1至5所示,本实施例提供一种碳热还原法制备氮化铝粉体的方法,包括如下步骤
S1、制备原料球,将氧化铝与炭黑配比混合,装入球磨机中混合磨料,过筛后造粒得到原料球备用;
S2、将上述制备好的原料球投入加热炉,所述加热炉内转动安装有载料容器2,加热炉上连通的氮气管道,所述原料球投放在载料容器2内;
S3、将氮气通过氮气管道通入加热炉,启动加热炉对炉内物体进行加热,加热温度在1600℃-1800℃,加热时间为3h;
S4、将反应后的产物收集至除碳装置,并向除碳装置内通入空气,除碳装置内温度600℃-650℃;
S5、对除碳装置内反应后的产物进行收集,即得到成品氮化铝粉体。
在本实施例中,所述氧化铝和炭黑的质量比为2:0.6-1.2,优选地,在制备原料球时向所述氧化铝和炭黑组成的原料球中加入其总重量11%的氮化铝晶种及总重量5%的烧结助剂。
在本实施例中,进行造粒时,将球磨后的粉体湿法球磨后得到浆料,在进行湿法球磨时,向混合物中加入粘结剂和分散剂,所述粘结剂与所述混合物的质量比为1~5:100,所述分散剂与所述混合物的质量比为0.1~1:100,在所述湿法球磨的过程中加入溶剂,得到的所述浆料的固含量为45%~65%,将得到后的浆料在搅拌状态下进行离心雾化,即可得到原料球。
在烧结时,若氧化铝粉末的平均粒度过小时,粉末容易团聚,不利于反应进行,平均粒度过大时,最终形成的氮化铝陶瓷的气孔率过高,所以在本实施例中,氧化铝粉末的平均粒径应保持在0.8um-1um,以保证反应的进行及最终产品的质量。
在本实施例中,所述加热炉包括炉体1,所述载料容器2可转动安装在炉体1底部,炉体1外设有驱动载料容器2转动的驱动机构202,所述载料容器2内壁连接有载料板201,所述炉体1上端连接与所述载料容器2连通的氮气通道,所述载料容器2内壁连接有载料板201,所述氮气管道的出气口对正所述载料板201,原料球在炉体1内加热时,驱动机构202驱动载料容器2转动,所述载料容器2和炉体1之间转动配合的同时密封配合,实现密封的结构采用工业回转窑炉常用的密封结构:旋转摩擦密封等,在此不再赘述,在加热过程中应持续向炉体1内通入氮气。
在本实施例中,所述氮气通道包括穿设在炉体1顶部的进气管道101及连接在进气管道101下端的多孔布气板1011,所述多孔布气板1011的上端设有与所述进气管道101连通的进气孔10111,所述多孔布气板1011的下端设有多个出气孔10112,每个所述出气孔10112上设有棱锥体1013,所述棱锥体1013上设有通道,所述通道具有与出气孔10112连通的一个进气端10131和多个分布在棱锥体1013表面的出气端10132,优选地,所述载料板201为环形板,所述多孔布气板1011为扇形板,所述多孔布气板1011的进气孔10111设在其圆心处,所述多孔布气板1011的底端设有刮料板1012,所述刮料板1012设在多孔布气板1011的一条直边上且所述刮料板1012的底端高度高于棱锥体1013的底端高度,多个所述出气孔10112沿多条绕布气板圆心的弧形路径排布。载料板201用于盛放原料球,原料球投放后,载料容器2开始转动,多孔布气板1011上的刮料板1012推动原料球,使得原料球在载料板201上形成厚度均匀的原料层,设在刮料板1012相对载料板201前进方向后方的棱锥体1013破开原料层进入到原料层内,同时向进气管道101内通入氮气,氮气由棱锥体1013上的多个出气端10132射出,在气流的推动下,原料在进行反应的反应的同时,未反应的氮气及反应生成的一氧化碳气体推动原料球不断翻滚,使得氮气和各种原料处于流动混合的状态,各个反应组分可充分反应,在反应过程中,应持续向炉体1内通入氮气,炉体1上有泄压阀,进入炉体1内氮气由泄压阀排出。
在本实施例中,所述炉体1的顶部穿设有粉末管道102,所述粉末管道102的下端对准所述载料板201的顶面,在投料时,不应将原料球投放至载料板201中部,以保证刮料板1012在初始时能够将所有原料刮平为均匀厚度的料层。
本实施例的加热炉在作业时,将原料投放在载料板201上,驱动机构202驱动载料容器2转动,多孔布气板1011上刮料板1012推动原料堆使其行成厚度均匀的原料层,同时多孔布气板1011下端的棱锥体1013进入原料层并向原料层内注入氮气,氮气在与原料反应的同时会推动原料翻滚,使得氮气和各种原料处于流动混合的状态,各个反应组分可充分反应,提高了产品的纯度,载料容器2在转时,刮料板1012不断抹平原料层,使得原料球能够被持续翻动。优选地,所述载料容器2的转速为0.05r/min-0.1r/min,以保证反应的稳定进行。
以上显示和描述了本发明创造的基本原理和主要特征及本发明的优点,本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明创造精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内,本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (5)
1.碳热还原法制备氮化铝粉体的方法,其特征在于:包括如下步骤
S1、制备原料球,将氧化铝与炭黑配比混合,装入球磨机中混合磨料,过筛后造粒得到原料球备用;
S2、将上述制备好的原料球投入加热炉,所述加热炉内转动安装有载料容器,加热炉上连通的氮气管道,所述原料球投放在载料容器内;
S3、将氮气通过氮气管道通入加热炉,启动加热炉对炉内物体进行加热,加热温度在1600℃-1800℃,加热时间为3h;
S4、将反应后的产物收集至除碳装置,并向除碳装置内通入空气,除碳装置内温度600℃-650℃;
S5、对除碳装置内反应后的产物进行收集,即得到成品氮化铝粉体;
所述加热炉包括炉体,所述载料容器可转动安装在炉体底部,炉体外设有驱动载料容器转动的驱动机构,所述载料容器内壁连接有载料板,所述炉体上端连接与所述载料容器连通的氮气通道,所述载料容器内壁连接有载料板,所述氮气管道的出气端对正所述载料板;
所述氮气通道包括穿设在炉体顶部的进气管道及连接在进气管道下端的多孔布气板,所述多孔布气板的上端设有与所述进气管道连通的进气孔,所述多孔布气板的下端设有多个出气孔,每个所述出气孔上设有棱锥体,所述棱锥体上设有通道,所述通道具有与出气孔连通的一个进气端和多个分布在棱锥体表面的出气端;
所述载料板为环形板,所述多孔布气板为扇形板,所述多孔布气板的进气孔设在其圆心处,所述多孔布气板的底端设有刮料板,所述刮料板设在多孔布气板的一条直边上且所述刮料板的底端高度高于棱锥体的底端高度,多个所述出气孔沿多条绕布气板圆心的弧形路径排布。
2.根据权利要求1所述的碳热还原法制备氮化铝粉体的方法,其特征在于:所述氧化铝和炭黑的质量比为2:0.6-1.2。
3.根据权利要求1所述的碳热还原法制备氮化铝粉体的方法,其特征在于:向所述氧化铝和炭黑组成的原料球中加入其总重量11%的氮化铝晶种及总重量5%的烧结助剂。
4.根据权利要求1所述的碳热还原法制备氮化铝粉体的方法,其特征在于:所述炉体的顶部穿设有粉末管道,所述粉末管道的下端对准所述载料板的顶面。
5.根据权利要求1所述的碳热还原法制备氮化铝粉体的方法,其特征在于:所述载料容器的转速为0.05r/min-0.1r/min。
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Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006219308A (ja) * | 2005-02-08 | 2006-08-24 | Sumitomo Metal Electronics Devices Inc | メタライズ層を有する窒化アルミニウム焼結体の製造方法および製造装置、メタライズ層を有する窒化アルミニウム焼結体、電子部品搭載用多層配線基板ならびに電子部品搭載モジュール |
CN201304335Y (zh) * | 2008-11-04 | 2009-09-09 | 攀钢集团研究院有限公司 | 流态化反应器装置 |
WO2011089790A1 (ja) * | 2010-01-22 | 2011-07-28 | コスモ石油株式会社 | 多結晶シリコンの製造方法 |
US8211356B1 (en) * | 2000-07-18 | 2012-07-03 | Surmet Corporation | Method of making aluminum oxynitride |
CN103553093A (zh) * | 2013-09-25 | 2014-02-05 | 中国科学院上海光学精密机械研究所 | 气流混合反应合成氧氮化铝粉体的方法及装置 |
CN104016316A (zh) * | 2014-06-18 | 2014-09-03 | 宁夏艾森达新材料科技有限公司 | 一种氮化铝粉连续制备方法及其设备 |
JP2014201474A (ja) * | 2013-04-03 | 2014-10-27 | 株式会社トクヤマ | 窒化アルミニウム粉末の製造方法 |
CN203946896U (zh) * | 2014-06-18 | 2014-11-19 | 宁夏艾森达新材料科技有限公司 | 一种连续生产氮化铝粉的设备 |
KR20210079870A (ko) * | 2019-12-20 | 2021-06-30 | 한국알루미나 주식회사 | 다공성 카본도가니를 활용한 질화알루미늄의 제조방법 |
CN113083010A (zh) * | 2021-04-23 | 2021-07-09 | 何静 | 一种烟气脱硫脱硝设备 |
JP2021123508A (ja) * | 2020-02-03 | 2021-08-30 | 株式会社トクヤマ | 窒化アルミニウム粉末の製造方法および製造装置 |
CN115215664A (zh) * | 2022-06-29 | 2022-10-21 | 宁夏北瓷新材料科技有限公司 | 一种低氧含量氮化铝微粉及其制备方法、应用和合成炉 |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9034199B2 (en) * | 2012-02-21 | 2015-05-19 | Applied Materials, Inc. | Ceramic article with reduced surface defect density and process for producing a ceramic article |
CN107429973A (zh) * | 2014-08-03 | 2017-12-01 | 普拉迪普金属有限公司 | 微波复合加热炉 |
-
2023
- 2023-06-26 CN CN202310758799.XA patent/CN116854480B/zh active Active
Patent Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8211356B1 (en) * | 2000-07-18 | 2012-07-03 | Surmet Corporation | Method of making aluminum oxynitride |
JP2006219308A (ja) * | 2005-02-08 | 2006-08-24 | Sumitomo Metal Electronics Devices Inc | メタライズ層を有する窒化アルミニウム焼結体の製造方法および製造装置、メタライズ層を有する窒化アルミニウム焼結体、電子部品搭載用多層配線基板ならびに電子部品搭載モジュール |
CN201304335Y (zh) * | 2008-11-04 | 2009-09-09 | 攀钢集团研究院有限公司 | 流态化反应器装置 |
WO2011089790A1 (ja) * | 2010-01-22 | 2011-07-28 | コスモ石油株式会社 | 多結晶シリコンの製造方法 |
JP2014201474A (ja) * | 2013-04-03 | 2014-10-27 | 株式会社トクヤマ | 窒化アルミニウム粉末の製造方法 |
CN103553093A (zh) * | 2013-09-25 | 2014-02-05 | 中国科学院上海光学精密机械研究所 | 气流混合反应合成氧氮化铝粉体的方法及装置 |
CN104016316A (zh) * | 2014-06-18 | 2014-09-03 | 宁夏艾森达新材料科技有限公司 | 一种氮化铝粉连续制备方法及其设备 |
CN203946896U (zh) * | 2014-06-18 | 2014-11-19 | 宁夏艾森达新材料科技有限公司 | 一种连续生产氮化铝粉的设备 |
KR20210079870A (ko) * | 2019-12-20 | 2021-06-30 | 한국알루미나 주식회사 | 다공성 카본도가니를 활용한 질화알루미늄의 제조방법 |
JP2021123508A (ja) * | 2020-02-03 | 2021-08-30 | 株式会社トクヤマ | 窒化アルミニウム粉末の製造方法および製造装置 |
CN113083010A (zh) * | 2021-04-23 | 2021-07-09 | 何静 | 一种烟气脱硫脱硝设备 |
CN115215664A (zh) * | 2022-06-29 | 2022-10-21 | 宁夏北瓷新材料科技有限公司 | 一种低氧含量氮化铝微粉及其制备方法、应用和合成炉 |
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