CN101851749B - 低温流动层法制备氮化钒涂层方法及其装置 - Google Patents
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Abstract
低温流动层法制备氮化钒涂层方法及其装置，属于先进材料制备领域。反应器中粉体因进气口送入氨气而悬浮，粉末之间借助气流在分隔板上移动搅拌而形成流动层；反应器由钢板焊接而成，采用碳化硅制作圆柱形的炉膛。活化剂供给器提供氯化铵作为活化剂，在呈流动状态的粉末中装入模具，夹具在电机驱动下作旋转运动，按温度控制器设定的温度和时间进行处理，处理后的废气经过滤器后由出气口排出。本发明专利采用反应气体搅拌的方法，氮化钒涂层形成的均匀性好，可用于处理复杂形状的高精度模具表面低温强化处理。
Description
技术领域
本发明涉及在高精度模具钢表面制备高硬度氮化钒涂层方法，是采用低温流动层热辐射效应在高精度模具表面制备氮化钒的工艺方法及其装置，属于先进材料制备领域。
背景技术
作为表面改质技术的扩散处理或扩散渗透处理技术如渗碳、氮化，已在机械零件、模具和工具等表面处理得到广泛的应用。作为更高性能的表面扩散处理，1960年后期发明的TD工艺(反应原料为粉末熔融盐浴)与CVD法(反应原料全部为气态)和PVD法(反应原料为金属原子蒸发)一起，大幅地提高了模具、夹具和工具的性能和使用寿命。但是TD工艺与CVD法都是在1000℃左右的高温下进行的处理，变形比较大，不适用于进行精冲压模、注塑模以及压铸模具等高精度模具表面强化处理。PVD法虽然是在400～600℃低温条件下进行处理，降低了高温对模具变形的影响，但存在处理成本高、涂层密实度差及不均匀等缺陷。为了解决高精度模具表面强化处理变形的难题，本发明专利通过气流与粉体在500℃～600℃形成的流动层的热辐射特性，在高精度模具钢表面制备高耐磨高耐蚀的氮化钒涂层，提高模具的使用寿命，也适用于基材为碳素钢、低合金钢、不锈钢、锻钢、高速钢以及陶瓷、超硬合金等表面强化处理。
发明内容
本发明专利的特征在于通过气流使反应器中氧化铝粉和钒铁粉形成流动层，由反应气体氮气提供活性氮原子，流动层中钒铁粉发生还原反应生成钒原子，使活性氮原子与钒原子发生氮化反应在模具表面生成氮化钒涂层。本发明方法的装置主要包括：加热温度控制系统、流动层形成系统和反应器系统等组成。
低温流动层法制备氮化钒涂层方法，其特征在于：通入氮气使得氧化铝粉和钒铁粉形成流动层，将流动层加热至反应温度，放入高精度模具钢，再通入活络剂进行反应，得到氮化钒涂层。
上述制备方法中，反应温度500℃～600℃。
上述制备方法中，氧化铝粉末(80目)和钒铁粉末(100目～150目)质量比为5∶1～4∶1。
上述制备方法中，活络剂主要是增加流动层的流动性，取氯化铵作为活络剂，其质量为粉末5％。
上述制备方法中，氮化钒厚度随处理温度的增加而增加，与处理时间成正比。反应时间一般为5～12h，可形成3μm～10μm氮化钒涂层。
反应过程中，隔板孔径小于原料粉体粒径，气体流动速率为1.5m/s～2m/s时，上述混合粉末形成流动层。
本发明专利涉及的低温制备氮化钒涂层装置如图1所示，装置包括温度控制器、反应器、夹具，电机和热电偶；反应器设有圆柱形炉膛，在炉膛外圆槽内盘绕有电热丝，反应器底部设有进气口，两侧分别设有活络剂供给器和出气口，反应器下部设有分隔板，热电偶(4)由反应器门孔插入炉膛内，热电偶和电热丝与温度控制器相连接，夹具设在圆柱形炉膛内并位于隔板之上，并由电机驱动旋转。
上述的装置中，电热丝为铁铬铝合金丝。
上述的装置中，反应器炉膛由碳化硅制成。
上述的装置中，反应器与出气口之间设有过滤器。
本发明专利的关键是流动层的形成，容器中粉末因其进气口送入的氮气而悬浮，粉末之间借助氮气流便于移动搅拌而形成有空隙的粉末层。粉末一直处于搅拌流动状态中，流动层内温度分布变得及其均匀。粉末的热传导系数大，模具能够迅速被加热或冷却。这样在呈流动状态的粉末中装入模具，设定温度500℃～600℃和处理时间5～12h，不降低炉内温度取出被处理模具。
如图1所述，电热丝为铁铬铝合金丝，盘绕在炉膛外圆槽内，热电偶由反应器门孔插入炉膛内，二者与温度控制器相连接；反应器中粉体因进气口送入氨气而悬浮，粉末之间借助气流在分隔板上移动搅拌而形成流动层；反应器由钢板焊接而成，采用碳化硅制作圆柱形的炉膛。活络剂供给器提供氯化铵作为活络剂，在呈流动状态的粉末中装入模具，夹具在电机驱动下作旋转运动，按温度控制器设定的温度和时间进行处理，处理后的废气经过滤器后由出气口排出。本发明专利采用反应气体搅拌的方法，氮化钒涂层形成的均匀性好，可用于处理复杂形状的高精度模具表面低温强化处理。
附图说明
图1为低温流动层法氮化钒涂层制备装置示意图
1、温度控制器；2、活络剂供给器；3、反应器；4、热电偶；5、夹具；6、电机；7、过滤器；8、出气口；9、模具；10、电热丝；11、流动层；12、分隔板；13、进气口
图2为低温流动层法制备的氮化钒涂层金相组织(×1500)
具体实施方式
(1)将氧化铝粉末(80目)和钒铁粉末(120目)按5∶1比例混合装入图1反应器3中，进气气口10通入氮气使其形成流动层11，氮气的流动速率为1.7m/s；电热丝10将该流动层10加热至580℃，放入夹有复杂的高精度模具(包括精冲压模、注塑模以及压铸模具等)9，活络剂供给器2提供占粉末总重量5％的氯化铵作为活络剂，使模具9与流动层11进行反应8小时，生成氮化钒涂层，如图2所示。
(2)图2为氮化钒涂层表面金相组织，涂层表面均匀性好，其厚度随温度增加而增加，与处理时间成正比。氮化钒硬度为1500HV，具有优越耐磨性。
Claims (2)
1.低温流动层法制备氮化钒涂层方法，其特征在于：通入氮气使得氧化铝粉和钒铁粉形成流动层，将流动层加热至反应温度，放入高精度模具钢，再通入活络剂进行反应，得到氮化钒涂层；其中反应温度500℃～600℃，反应时间为5～12h；氧化铝粉末为80目，钒铁粉末为100目～150目，氧化铝粉末与钒铁粉末的质量比为5∶1～4∶1；活络剂为氯化铵，质量为氧化铝粉末和钒铁粉末总重量的5％；：氮气的流动速率为1.5m/s～2m/s。
2.如权利要求1所述的制备方法，其特征在于：氮化钒涂层厚度为3μm～10μm，氮化钒厚度随处理温度的增加而增加，与处理时间成正比。
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| CN102337517A (zh) * | 2011-05-03 | 2012-02-01 | 中国科学院福建物质结构研究所 | 氧化物薄膜生长用金属有机物化学气相沉积反应室 |
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| CN1562769A (zh) * | 2004-03-30 | 2005-01-12 | 上海大学 | 氮化钒的制备方法及其装置 |
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| US3745209A (en) * | 1970-09-09 | 1973-07-10 | Hollandse Metall Ind Billiton | Process for the preparation of vanadium(carbo)nitride |
| CN2347683Y (zh) * | 1998-10-30 | 1999-11-10 | 张凤焘 | 一种在风机风叶上涂覆防腐塑料涂层的装置 |
| CN1562769A (zh) * | 2004-03-30 | 2005-01-12 | 上海大学 | 氮化钒的制备方法及其装置 |
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Effective date of registration: 20190521 Address after: 213000 Lujiatou 176, Hongzhuang Village Committee, Yaoguan Town, Wujin District, Changzhou City, Jiangsu Province Patentee after: Changzhou Kane Chain Drive Technology Co.,Ltd. Address before: 213311 7 7, tou tou street, Dai tou Town, Liyang, Changzhou, Jiangsu Patentee before: Liyang Chang Technology Transfer Center Co.,Ltd. |
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Effective date of registration: 20220629 Address after: 213000 Hongzhuang Village, Yaoguan Town, Wujin District, Changzhou City, Jiangsu Province Patentee after: Changzhou Dongchuan chain drive technology Co.,Ltd. Address before: 213000 Lujiatou 176, Hongzhuang Village Committee, Yaoguan Town, Wujin District, Changzhou City, Jiangsu Province Patentee before: Changzhou Kane Chain Drive Technology Co.,Ltd. |
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Denomination of invention: Method and device for preparing vanadium nitride coating by low-temperature flow layer method Effective date of registration: 20230423 Granted publication date: 20120829 Pledgee: Bank of China Limited Changzhou Economic Development Zone sub branch Pledgor: Changzhou Dongchuan chain drive technology Co.,Ltd. Registration number: Y2023980038898 |
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