CN109321796A - 一种硅铝钾钨合金板材的制备方法 - Google Patents

一种硅铝钾钨合金板材的制备方法 Download PDF

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CN109321796A
CN109321796A CN201811361608.1A CN201811361608A CN109321796A CN 109321796 A CN109321796 A CN 109321796A CN 201811361608 A CN201811361608 A CN 201811361608A CN 109321796 A CN109321796 A CN 109321796A
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李光宗
赵腾飞
唐光明
傅崇伟
李柏明
刘伟
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Zhuzhou Cemented Carbide Group Co Ltd
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Abstract

本发明公开了一种硅铝钾钨合金板材的制备方法,属于钨合金加工技术领域,制备流程为:(1)硅铝钾钨粉的制取;(2)硅铝钾钨粉的掺杂,掺杂剂为稀土氧化物、钨粉、碳化钨中的一种或多种混合物;(3)等静压压制成型;(4)将压坯在保护性气氛下,于2250~2400℃的温度下进行烧结;(5)压力加工与热处理;(6)机械加工。本发明通过掺杂技术、烧结工艺和烧结板坯形状的创新,将烧结坯料的密度、晶粒度控制在一定的标准范围内,有效地保证了烧结坯料的轧制加工性能;通过对轧制工艺和退火工艺的创新,解决了轧制开裂问题,满足了机械加工性能和使用性能的要求,轧制总变形量在85%以上,收率在90%以上,实现硅铝钾钨板材的批量生产。

Description

一种硅铝钾钨合金板材的制备方法
技术领域
本发明属于钨合金加工技术领域,具体涉及一种硅铝钾钨合金板材的制备方法。
背景技术
MOCVD(气相外延生长)设备是半导体制造中的关键设备,一直以来依赖进口,价格昂贵。近几年来,国内生产商大力投资研发,国产化设备已逐步走向市场,这种设备的加热器的加热元件采用纯钨片,使用寿命在2~3个月,远低于国外设备的使用寿命(国外设备通常为1年左右),其失效方式主要表现为变形、断裂。
硅铝钾钨合金材料由于钾泡效应,材料具有优异的抗震性能和高温抗蠕变性能,大量用于生产抗震钨丝及高温炉用钨合金元部件。目前,硅铝钾钨合金的生产工艺路线为:硅铝钾钨粉的制取、钢模压制成型、垂熔烧结、旋锻拉拔,生产能耗高,成材率低,是一种低效率的加工方式。
中国专利CN 201410608333.2A公开了一种钨合金板材的轧制工艺,该方法需要进行2次中间退火和1次再结晶退火(温度为2000℃~2300℃,保温时间为1~2小时),制备的钨合金晶粒较粗,容易导致钨合金板材变形、开裂,而且其制备工艺复杂,加工周期长,再结晶温度高,增加了生产成本。
发明内容
针对现有技术的不足,本发明的目的在于提供一种硅铝钾钨合金板材的制备方法,解决了轧制过程容易开裂的问题,制备得到抗震性能好、耐高温的硅铝钾钨合金板材。
为了实现上述技术目的,本发明提供以下技术方案:
本发明提供一种硅铝钾钨合金板材的制备方法,包括以下步骤:
(1)硅铝钾钨粉的制取:
其中,K含量为0.005~0.05wt%;
Si含量为≤0.045wt%;
Al含量为≤0.035wt%;
其余为钨粉,总量之和为100wt%;
(2)将硅铝钾钨粉进行掺杂,掺杂剂为稀土氧化物、钨粉、碳化钨中的一种或多种混合物,得到掺杂后的硅铝钾钨粉;
(3)将步骤(2)所得掺杂后的硅铝钾钨粉进行等静压压制成型,得到压坯;
(4)将步骤(3)所得压坯在保护性气氛下,于2250~2400℃的温度下进行烧结,得到金属坯料;
(5)压力加工与热处理:
将步骤(4)所得金属坯料在1200~1600℃温度范围内进行压力加工,经过14~18道次轧制,第一道次轧制后回炉加热温度递减,保温时间为12~25min,道次变形率控制在15~30%之间,总变形量85%以上,中间不需退火处理,达到所需厚度后在1300~1450℃温度范围内进行再结晶热处理,得到板材半成品;
(6)将步骤(5)所得板材半成品进行机械加工,得到硅铝钾钨合金板材成品。
作为优选,步骤(2)中,所述掺杂剂的添加量为0.01~2wt%,掺杂后进行混合、过筛,得到掺杂后的硅铝钾钨粉。
作为优选,步骤(4)中,所述烧结在中频炉中进行,烧结工艺是采用随炉升降温的方式,从室温开始升温,在800~2200℃之间设有多个阶段保温台阶,高温保温温度为2250℃~2400℃,保温时间为6~12h。
作为优选,步骤(4)中,金属坯料的形状为板状或块状,棱边角为圆弧状。
作为优选,步骤(4)中,金属坯料的密度控制在17.2~18.2g/cm3,晶粒度控制在400个/mm2以上。
作为优选,步骤(4)中,金属坯料中钾含量控制在0.002~0.015wt%,硅含量控制在≤0.01wt%,铝含量控制在≤0.01wt%的范围内。
作为优选,步骤(5)中,第一道次轧制前,将金属坯料置于1520~1600℃的温度下进行保温60~120min。
作为优选,步骤(5)中,所述再结晶热处理的时间为40~120min。
作为优选,步骤(6)中,所述硅铝钾钨合金板材成品的形状为方板形、方片形、圆片形中的一种。
在硅铝钾钨合金片材研制初期,采用硅铝钾钨粉直接冷等静压压制、中频烧结后进行轧制,轧制开裂严重,成材率几乎为零,调整轧制工艺情况也得不到改善。通过分析发现,纯钨轧制板坯的晶粒度一般在400~3000个/mm2之间,而硅铝钾钨板坯的晶粒度在50~300之间,分析认为晶粒粗大可能是轧制开裂的主要原因。为此,对板坯制造工艺进行了改进,采用在硅铝钾钨粉中掺杂的方案来达到细化晶粒的目的。试验表明在硅铝钾钨粉中掺杂稀土氧化物、W、WC及这些物质的混合物可以明显细化硅铝钾钨板坯的晶粒,晶粒度达到了纯钨板坯的要求,同时对轧制工艺进行了创新,轧制过程无需进行退火,再结晶温度也大大降低,轧制试验效果很好,成材率达到了90%以上。
与现有技术相比,本发明的有益技术效果为:
本发明通过掺杂技术、烧结工艺和烧结板坯形状的创新,将烧结坯料的密度、晶粒度控制在一定的标准范围内,有效地保证了烧结坯料的轧制加工性能;通过对轧制工艺和退火工艺的创新,解决了轧制开裂问题,满足了机械加工性能和使用性能的要求,轧制总变形量在85%以上,收率在90%以上,实现硅铝钾钨板材的批量生产。
本发明提供的硅铝钾钨合金板材,经过MOCVD设备上机测试,硅铝钾钨片材制作的加热元件抗蠕变性能非常优异,提高了加热元件的使用寿命,产品使用寿命接近国外产品,得到了市场的认可。
本发明通过调整合金成分,改变压制和烧结方式,采用等静压压制和中频烧结方式,实现了硅铝钾钨合金批量生产,产品能耗低,成材率高,生产出的烧结态板块产品,产品适合轧制、锻造制造板和片产品,大规格片材(如2.3*315*624、2.3*330*640)已小批量投入市场,使用性能良好,满足了用户的需求。
附图说明
图1是本发明所述硅铝钾钨合金板材的制备方法的流程图。
图2为实施例1中烧结后的金属坯料外形图,其中(a)为外形设计图;(b)为实物图。
图3为实施例1中板材半成品的外形图。
图4为实施例1中所得磨光的硅铝钾钨方片产品的外形图。
图5为实施例2中烧结后金属坯料的金相图。
图6为实施例2中轧制后板材的金相图。
图7为实施例2中板材半成品的外形图。
图8为实施例2中所得磨光的硅铝钾钨圆片产品的外形图。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅是本发明一部分实施例,而不是全部实施例,基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
下面结合具体实施例和附图对本发明进行进一步说明:
实施例1
本发明提供一种硅铝钾钨合金板材的制备方法,工艺流程如图1所示,包括以下步骤:
(1)称取99.5kg的硅铝钾钨粉,其中,K含量为0.012wt%,Si含量为0.018wt%,Al含量为0.012wt%;
(2)将硅铝钾钨粉进行掺杂,掺杂剂(钨粉和氧化镧按1:1混合)0.5kg,混合4h,过筛;
(3)将掺杂后的硅铝钾钨粉进行等静压压制成型,得到压坯;
(4)将压坯置于中频炉中进行烧结,通入氢气,采用随炉升降温的方式,从室温开始升温,在800~2200℃之间设有多个阶段保温台阶,然后控制在2300℃保温8h,得到金属坯料,如图2所示;
制造出35*120*260的硅铝钾钨板坯,钨板坯的密度为17.38克/立方厘米,晶粒度为1800个/平方毫米,钾含量为0.0068wt%,硅含量控制在≤0.01wt%,铝含量控制在≤0.01wt%的范围内;
(5)压力加工与热处理:
将金属坯料在1550℃进行开坯轧制,经过14~18道次轧制,第一道次轧制前,将金属坯料置于1600℃的温度下进行保温80min,第一道次轧制后回炉加热温度递减,保温时间为12~25min,道次变形率控制在15~30%之间,总变形量85%以上,中间不需退火处理,轧制至尺寸为3.2*330~360*640~700,在1360℃下进行再结晶热处理60min,得到板材半成品,如图3所示;
(6)将板材半成品经水切割成3.2*315*624方片,再经磨削加工成2.3*315*624的磨光硅铝钾钨方片产品,如图4所示。
实施例2
本发明提供一种硅铝钾钨合金板材的制备方法,包括以下步骤:
(1)称取49.8kg的硅铝钾钨粉,其中,K含量为0.01wt%,Si含量为0.024wt%,Al含量为0.008wt%;
(2)将硅铝钾钨粉进行掺杂,掺杂氧化铈0.2kg,混合4h,过筛;
(3)将掺杂后的硅铝钾钨粉进行等静压压制成型,得到压坯;
(4)将压坯置于中频炉中进行烧结,通入氢气,采用随炉升降温的方式,从室温开始升温,在800~2200℃之间设有多个阶段保温台阶,然后控制在2300℃保温8h,得到金属坯料,其金相图如图5所示;
制造出24*160*270的硅铝钾钨板坯,钨板坯的密度为17.55克/立方厘米,晶粒度为2000个/平方毫米,钾含量为0.0064wt%,硅含量控制在≤0.01wt%,铝含量控制在≤0.01wt%的范围内;
(5)压力加工与热处理:
将金属坯料在1550℃进行开坯轧制,经过14~18道次轧制,第一道次轧制后回炉加热温度递减,保温时间为12~25min,道次变形率控制在15~30%之间,总变形量85%以上,中间不需退火处理,轧制至尺寸为2.2*410~430*4100~430,轧制后板材的金相图如图6所示,在1360℃下进行再结晶热处理80min,得到板材半成品,如图7所示;
(6)将板材半成品经水切割成的圆片,再经磨削加工成的磨光硅铝钾钨圆片产品,如图8所示。
实施例3
本发明提供一种硅铝钾钨合金板材的制备方法,包括以下步骤:
(1)称取79.6kg的硅铝钾钨粉,其中,K含量为0.0099wt%,Si含量为0.019wt%,Al含量为0.09wt%;
(2)将硅铝钾钨粉进行掺杂,掺杂氧化镧0.4kg,混合4h,过筛;
(3)将掺杂后的硅铝钾钨粉进行等静压压制成型,得到压坯;
(4)将压坯置于中频炉中进行烧结,通入氢气,采用随炉升降温的方式,从室温开始升温,在800~2200℃之间设有多个阶段保温台阶,然后控制在2300℃保温8h,得到金属坯料;
制造出24*160*270的硅铝钾钨板坯,钨板坯的密度为17.32克/立方厘米,晶粒度为1500个/平方毫米,钾含量为0.0063wt%,硅含量控制在≤0.01wt%,铝含量控制在≤0.01wt%的范围内;
(5)压力加工与热处理:将金属坯料在1550℃进行开坯轧制,轧制至尺寸为3.1*260~280*1100~1300,在1350℃下进行再结晶热处理100min,得到板材半成品;
(6)将板材半成品经水切割成3.1*250*500两件,再经磨削加工成2*250*500磨光的硅铝钾钨片产品。

Claims (10)

1.一种硅铝钾钨合金板材的制备方法,其特征在于,包括以下步骤:
(1)硅铝钾钨粉的制取:
其中,K含量为0.005~0.05wt%;
Si含量为≤0.045wt%;
Al含量为≤0.035wt%;
其余为钨粉,总量之和为100wt%;
(2)将硅铝钾钨粉进行掺杂,掺杂剂为稀土氧化物、钨粉、碳化钨中的一种或多种混合物,得到掺杂后的硅铝钾钨粉;
(3)将步骤(2)所得掺杂后的硅铝钾钨粉进行等静压压制成型,得到压坯;
(4)将步骤(3)所得压坯在保护性气氛下,于2250~2400℃的温度下进行烧结,得到金属坯料;
(5)压力加工与热处理:
将步骤(4)所得金属坯料在1200~1600℃温度范围内进行压力加工,经过14~18道次轧制,第一道次轧制后回炉加热温度递减,保温时间为12~25min,道次变形率控制在15~30%之间,总变形量85%以上,中间不需退火处理,达到所需厚度后在1300~1450℃温度范围内进行再结晶热处理,得到板材半成品;
(6)将步骤(5)所得板材半成品进行机械加工,得到硅铝钾钨合金板材成品。
2.根据权利要求1所述硅铝钾钨合金板材的制备方法,其特征在于,步骤(2)中,所述掺杂剂的添加量为0.01~2wt%,掺杂后进行混合、过筛,得到掺杂后的硅铝钾钨粉。
3.根据权利要求1所述硅铝钾钨合金板材的制备方法,其特征在于,步骤(4)中,所述烧结在中频炉中进行,烧结工艺是采用随炉升降温的方式,从室温开始升温,在800~2200℃之间设有多个阶段保温台阶,高温保温温度为2250℃~2400℃,保温时间为6~12h。
4.根据权利要求1所述硅铝钾钨合金板材的制备方法,其特征在于,步骤(4)中,金属坯料的形状为板状或块状,棱边角为圆弧状。
5.根据权利要求1所述硅铝钾钨合金板材的制备方法,其特征在于,步骤(4)中,金属坯料的密度控制在17.2~18.2g/cm3,晶粒度控制在400个/mm2以上。
6.根据权利要求1~5中任一项所述硅铝钾钨合金板材的制备方法,其特征在于,步骤(4)中,金属坯料中钾含量控制在0.002~0.015wt%,硅含量控制在≤0.01wt%,铝含量控制在≤0.01wt%的范围内。
7.根据权利要求1所述硅铝钾钨合金板材的制备方法,其特征在于,步骤(5)中,第一道次轧制前,将金属坯料置于1520~1600℃的温度下进行保温60~120min。
8.根据权利要求1所述硅铝钾钨合金板材的制备方法,其特征在于,步骤(5)中,所述再结晶热处理的时间为40~120min。
9.根据权利要求1所述硅铝钾钨合金板材的制备方法,其特征在于,步骤(6)中,所述硅铝钾钨合金板材成品的形状为方板形、方片形、圆片形中的一种。
10.一种根据权利要求1~9中任一项所述硅铝钾钨合金板材的制备方法制备得到的硅铝钾钨合金板材。
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