CN114959596A - 钼合金包覆热成型工艺 - Google Patents
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Abstract
本发明涉及一种钼合金包覆热成型工艺，包括如下步骤：原料挑选；真空干燥混料；粉末填充，同时完成纯钼包覆；对填充好粉末的包套揉压，抽真空除气，取出分隔套；冷等静压；生坯切割整形；通氢气热压烧结成型；轧制；消除应力退火。本发明制得的靶坯杂质含量更低，纯度更高；靶坯密度高；靶坯内部组织均匀；使用常规装备、制造成本低。
Description
技术领域：
本发明涉及靶材制造技术领域，尤其涉及一种钼合金包覆热成型工艺。
背景技术：
在钼合金靶材的制备过程中，为了得到内部组织均匀、高纯度且高密度的靶材，一般利用CIP冷等静压机进行钼合金粉末成型得到生坯，再对生坯进行包套除气封口，然后利用HIP热等静压机进行加压加热成型，接着对热成型坯进行二次包覆，最后再进行热轧和热处理工艺。但是如上所述，由于HIP热等静压热成型工艺中不锈钢包套的阻隔问题，靶坯内氧含量和其它杂质无法在热成型过程中挥发出去，造成靶坯纯度较低，同时热轧加工时较容易形成开裂报废。并且HIP热等静压机属于特殊装备，价格非常昂贵，使用维护成本特别高，故造成生产成本太高，产品在市场上没有竞争力。
CN110257784一种高致密度钼铌合金溅射靶材的制备工艺；CN108930020A钼铌靶材制作工艺；CN105441884B一种钼铌合金溅射靶材的制备方法；这3个专利均需要使用昂贵的热等静压设备；CN111590071A一种钼铌合金靶材及其制备方法，使用的是真空热成型，不施加压力，在没有压力的情况下，热成型温度需要很高，内部晶粒组织不均匀。而且直接在氢气炉中加热进行轧制，会造成开裂。
发明内容：
本发明的目的通过以下技术方案，使用常规设备，通过改进工艺，得到内部组织均匀、高密度，且纯度更高的钼合金靶材。
本发明在粉末填充时利用隔离套完成了生坯纯钼包覆，使用通氢加压热成型。纯钼包覆可以让坯料热成型和加热轧制时，避免合金组元发生氢脆，造成开裂。加压可大幅降低热成型温度，更容易获得内部晶粒组织均匀的坯料。
本发明是通过如下技术方案实现的：
本发明提供一种钼合金包覆热成型工艺，包括如下步骤：
(1)选择合适的粉末原料
a、合金粉末各组元粒度尺寸相当，且中位粒径3-10微米；
b、纯度大于3N5。
(2)真空干燥混料
a、采用回转真空混料机；
b、混料时间：4-8小时；
c、带真空系统；
采用回转真空混料机可以同时完成合金粉末混合和干燥。
(3)粉末填充
将上述混料后的填充于模具中，在生坯外包裹分隔套，在分隔套外包裹包套，最后在分隔套和包套之间填充纯钼粉末。
常规钼制品热成型炉都是氢气保护气氛热成型炉，氢还原反应可以保护胚体不会氧化，还能去除坯体内的部分氧含量，高温下其他杂质挥发，提高坯体纯度，但氢气对合金中其它组元会产生氢脆反应，造成内部组织不均匀，热轧时开裂等问题。因此本发明使用纯钼包覆，作用是阻隔氢气对合金中其它组元的氢脆反应。
(4)对填充好粉末的包套揉压，抽真空除气，取出分隔套；
a、采用双辊揉压机；
b、往复揉压5-20次，包套封口，连接管路，打开真空泵，抽出包套内的空气。
(5)冷等静压
a、压力：250-300Mpa；
b、保压时间：300-500s。
(6)生坯切割整形
a、采用电动钢丝锯，无需冷却液，避免生坯污染；
b、线锯条直径为1mm，可切割复杂形状，切割面平整，平面度小于0.3MM，粉末浪费少。
热压成型时，为了压力能够均匀的传递，避免坯料在压力下发生破裂，坯料表面平面度需小于0.3mm。
(7)通氢气热压成型
a、采用常规热压成型炉，氢气气氛下进行热压成型；
b、热压成型温度为1500-2500℃，压力为30-50Mpa。
在通氢热成型过程中，坯体在加热的同时施加一定的压力，可以降低热成型温度，更容易得到组织均匀，高密度，高纯度的靶坯。
(8)轧制
a、温度1100-1600℃；
b、压下量0-35％；
(9)消除应力退火
a、采用真空退火炉，真空度小于1.0e-2Pa；
b、温度1000-1200℃；
c、保温时间5-8小时。
本发明的有益效果是：
1、靶坯杂质含量更低，纯度更高；
2、靶坯密度高；
3、靶坯内部组织均匀；
4、使用常规装备、制造成本低。
附图说明：
图1为本发明钼合金包覆热成型工艺的流程图；
图2为本发明实施例1的金相图；
图3为本发明实施例2的金相图；
图4为本发明实施例3的金相图；
图5为本发明实施例4的金相图；
图6为本发明实施例5的金相图。
具体实施方式：
下面结合附图对本发明的较佳实施例进行详细阐述，以使本发明的优点和特征能更易被本领域人员理解，从而对本发明的保护范围做出更为清楚明确的界定。
如图1所示，本发明提供一种钼合金包覆热成型工艺，包括如下步骤：
(1)原料挑选；(2)真空干燥混料；(3)粉末填充，纯钼包覆；(4)对填充好粉末的包套揉压，抽真空除气，取出分隔套；(5)冷等静压；(6)生坯切割整形；(7)通氢气热压烧结成型；(8)轧制；(9)消除应力退火。
下面举例进行具体说明。
对上述各实施例检测分析：
实施例子1：基于实施例1的技术方案，参考图2的金相图可以看出，得到的板坯组织均匀，纯度高，但是由于热成型温度偏低了，坯料由海绵体长成连续金属时，能量不够，造成密度偏低。
实施例子2、3：
实施例子2、3为本发明的优选实施例，基于实施例2和实施例3的技术方案，参考图3、图4的金相图可以看出，得到的板坯组织均匀，纯度高，密度高。
实施例子4：
基于实施例4的技术方案，参考图5的金相图可以看出，由于未对钼合金胚体进行关键的包覆处理，烧结时合金组元在氢气氛中吸收大量的氢原子，形成了氢裂反应，造成热轧开裂，无法得到合格的板坯。
实施例子5：
基于实施例子5的技术方案，参考图6的金相图可以看出，得到的板坯组织均匀，但是由于热成型是未对胚体施加压力，坯料由海绵体长成连续金属时，能量不够，造成密度较低，由于未通氢气，胚体在烧结过程中发生了氧化反应，造成氧含量超标。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，比如，其它基合金在保护气氛(不局限于氢气)下进行的类似包覆热成型方式，这些都属于本发明的保护范围。
Claims (1)
1.一种钼合金包覆热成型工艺，其特征在于，包括如下步骤：
(1)选择合适的粉末原料
a、合金粉末各组元粒度尺寸相当，且中位粒径3-10微米；
b、纯度大于3N5；
(2)真空干燥混料
a、采用回转真空混料机；
b、混料时间：4-8小时；
c、带真空系统；
(3)粉末填充
将上述混料后的填充于模具中，通过分隔套及包套对生坯进行纯钼包覆；
(4)对填充好粉末的包套揉压，抽真空除气，取出分隔套；
a、采用双辊揉压机；
b、往复揉压5-20次，包套封口，连接管路，打开真空泵，抽出包套内的空气；
(5)冷等静压
a、压力：250-300Mpa；
b、保压时间：300-500s；
(6)生坯切割整形
a、采用电动钢丝锯；
b、线锯条直径为1mm，平面度小于0.3MM；
(7)通氢气热压成型
a、采用常规热压成型炉，氢气气氛下进行热压成型；
b、热压成型温度为1500-2500℃，压力为30-50Mpa；
(8)轧制
a、温度1100-1600℃；
b、压下量0-35％；
(9)消除应力退火
a、采用真空退火炉，真空度小于1.0e-2Pa；
b、温度1000-1200℃；
c、保温时间5-8小时。
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