CN111850370A - 一种粗晶WC-Co硬质合金的制备方法 - Google Patents
一种粗晶WC-Co硬质合金的制备方法 Download PDFInfo
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Abstract
本发明公开了一种粗晶WC‑Co硬质合金的制备方法，包括以下步骤：(1)预处理WC粉末；(2)配置活化液，再将WC粉末进行活化；(3)过滤、烘干活化后的WC粉末，并进行热处理还原得到表面附着有金属Co颗粒的WC活化粉体；(4)配置镀液；(5)将表面附着有金属Co颗粒的WC活化粉体、C粉和W粉置于镀液中进行化学镀，过滤、清洗并真空干燥得到WC/C/W/Co粗晶复合粉末；(6)将WC/C/W/Co粗晶复合粉末加入成型剂并压制成胚，并烧结成WC‑Co硬质合金。该方法利用原位反应烧结制备出晶粒度大于2μm的粗晶WC‑Co硬质合金，其晶粒度、硬度、横向断裂强度和冲击韧性优异。
Description
技术领域
本发明涉及一种硬质合金的制备方法；更具体地，涉及一种粗晶WC-Co硬质合金的制备方法。
背景技术
硬质合金是一种具有高硬度、高耐磨性能、优良的红硬性和热稳定性及耐腐蚀性、高强度与优良韧性的复合材料。其中，粗晶WC-Co硬质合金具有优良的硬度、耐磨性以及较高的韧性，被广泛应用于地矿工具、隧道掘进刀具等领域。粗晶的WC-Co硬质合金的制备，通常将平均粒度大于20mm的WC粉末，采用球磨强度适度的湿磨法制备得到粒度符合且分散均匀的WC/Co复合粉末，然而球磨时WC颗粒的粒度难以控制，从而导致烧制的合金中WC颗粒的分布低于或超出2～5mm粗晶标准的范围，最终仅得到具有宽峰晶粒分布的WC-Co硬质合金，晶粒度相同时，宽峰分布的粗晶WC-Co硬质合金的强度和韧性低于窄峰分布合金。此外，球磨获取高均匀性的复合粉末将给WC颗粒带来较高的残余应力，这也不利于合金性能的提升。
发明内容
发明目的：本发明的目的是提供一种能够制备出窄峰分布、硬度、横向断裂强度和冲击韧性好的粗晶WC-Co硬质合金的制备方法。
技术方案：本发明所述的粗晶WC-Co硬质合金的制备方法，包括以下步骤：
(1)将粗颗粒WC粉末进行球磨，清洗、真空干燥得到预处理的WC粉末；
(2)将CoSO4·7H2O和NaH2PO2·7H2O溶于中配置成活化液，再将步骤1中处理后的WC粉末加入活化液中进行活化；
(3)过滤、烘干活化后的WC粉末，并进行热处理还原得到表面附着有金属Co颗粒的WC活化粉体；
(4)将CoSO4·7H2O和Na2C6H5O7·2H2O溶于水中充分络合，依次加入H3BO3和NaH2PO2·7H2O配置成镀液；
(5)将表面附着有金属Co颗粒的WC活化粉体、C粉和W粉置于镀液中，在水浴下搅拌，调节镀液pH值为10～12，并在70～90℃下进行化学镀，过滤、清洗并真空干燥得到WC/C/W/Co粗晶复合粉末；
(6)将WC/C/W/Co粗晶复合粉末加入成型剂并压制成胚，并烧结成WC-Co硬质合金。
其中，步骤1中球磨采用直径为10～13mm的合金球，球料比为1～3:1；步骤2中活化液中CoSO4·7H2O和Na2C6H5O7·2H2O浓度分别为50～60g/L，体积比为1：1～2，活化温度为50～60℃，活化时间为20～30min；步骤3中热处理温度为300～400℃，时间为2～3h；步骤4中CoSO4·7H2O浓度为45～60g/L、Na2C6H5O7·2H2O浓度为50～60g/L、H3BO3浓度为25～30g/L、NaH2PO2·7H2O浓度为30～40g/L；步骤5中调节镀液pH值之前先将镀液预热到70～90℃；步骤5中WC/C/W/Co粗晶复合粉末中C粉和W粉总占比为5～10wt.％，C粉和W粉的质量比为1：15～16，Co镀层为5～10wt.％；步骤6中成型剂为SD-E橡胶，成型剂的含量占总料粉的1.5～2.5wt.％，压胚压制压力为20～100MPa，烧结时在真空条件下，烧结温度在1400～1450℃，烧结后在1～10Pa气压下保温1～2h。
合成原理：本发明中碳粉、钨粉协同包覆方式得到WC/C/W/Co粗晶复合粉末，两种粉末将于钴在碳化钨表面形核生长过程中填充到钴颗粒之间形成C/W/Co镀层，使两种粉体分散更均匀的同时保证了钴层的均匀生长，协同包覆最终获得的WC/C/W/Co粗晶的复合粉末是W和C颗粒镶嵌于Co镀层中的结构，最后在液相烧结过程中，碳粉和钨粉在钴的液相中原位反应，促进粗晶WC晶粒的快速生长的同时形成高性能的WC和高强度的相界面，最终获得具有高综合性能的粗晶WC-Co硬质合金。
有益效果：本发明与现有技术相比，其显著优点是：利用原位反应烧结制备出晶粒度大于2μm的粗晶WC-Co硬质合金，其晶粒度、硬度、横向断裂强度和冲击韧性优异。
具体实施方式
实施例1
(1)将500g粒度为10～15μm的粗WC粉，以无水酒精作为湿磨介质在滚筒式球磨机中球磨，无水酒精的含量为200mL/kg，磨球直径选用13mm，球料比为3:1；球磨12h后进行真空干燥得到预处理的WC粉末；
(2)将50g的CoSO4·7H2O和50g的NaH2PO2·7H2O溶解于蒸馏水中配置成1L活化液，再取100g预处理的WC粉末置于1L活化液中机械搅拌，在50℃下进行活化，活化时间为30min；
(3)过滤、烘干活化后的WC粉末，并在马弗炉中400℃下热处理2h得到表面附着有金属Co颗粒的WC活化粉体；
(4)将55g CoSO4·7H2O和50g Na2C6H5O7·2H2O溶解于800mL蒸馏水中充分络合，再依次加入25g H3BO3和40g NaH2PO2·7H2O配置成900mL镀液；
(5)然后将24.82g WC活化粉末、2.9g C粉和0.19g W粉置于上述镀液中，在80℃水浴下进行机械搅拌，采用NaOH调节pH为11，添加蒸馏水使镀液为1L，并在80℃下进行化学镀60min，化学镀后过滤、清洗并真空干燥得到31.04g WC/0.614wt.％C/9.386wt.％W/10wt.％Co复合粉末。
(6)在WC/0.614wt.％C/9.386wt.％W/10wt.％Co复合粉末中加入2.5wt.％的SD-E成型剂，并进行造粒，造粒后过80目的筛网，在20MPa的压力下压制成型；将压胚在置于真空条件下进行烧结，烧结温度在1400℃，保温时间为1h，得到WC-Co硬质合金。
实施例2
(1)将500g粒度为10～15μm的粗WC粉，以无水酒精作为湿磨介质在滚筒式球磨机中球磨，无水酒精的含量为200mL/kg，磨球直径选用13mm，球料球料比为3:1；球磨12h后进行真空干燥得到预处理的WC粉末；
(2)将50g的CoSO4·7H2O和50g的NaH2PO2·7H2O溶解于蒸馏水中配置成1L活化液，再取100g预处理的WC粉末置于1L活化液中机械搅拌，在50℃下进行活化，活化时间为30min；
(3)过滤、烘干活化后的WC粉末，并在马弗炉中300℃下热处理3h得到表面附着有金属Co颗粒的WC活化粉体；
(4)将50g CoSO4·7H2O和50g Na2C6H5O7·2H2O溶解于800mL蒸馏水中充分络合，再依次加入25g H3BO3和30g NaH2PO2·7H2O配置成900mL镀液；
(5)然后将15.6g WC活化粉末、0.12g C粉和1.83g W粉置于上述镀液中，在70℃水浴下进行机械搅拌，采用NaOH调节pH为11，添加蒸馏水使镀液为1L，并在70℃下进行化学镀60min，化学镀后过滤、清洗并真空干燥得到19.48g WC/0.307wt.％C/4.693wt.％W/8wt.％Co复合粉末。
(6)在WC/0.614wt.％C/9.386wt.％W/10wt.％Co复合粉末中加入2.5wt.％SD-E成型剂，并进行造粒，造粒后过80目的筛网，在20MPa的压力下压制成型；将压胚在置于真空条件下进行烧结，烧结温度在1450℃，保温时间为1h，得到WC-Co硬质合金。
对比例1
本对比例与实施例1的区别是：在化学镀的步骤中未添加C粉和W粉，化学镀后制得WC/10wt.％Co复合粉末。
对比例2
本对比例与实施例2的区别是：未对粗WC粉进行球磨预处理。
对实施例1～2和对比例1～2进行性能测试，结果如表1所示，从表中可以看出，四种粗晶硬质合金中孔隙基本一致，实施例1～2的硬质合金平均晶粒度大于2μm，包覆的C/W/Co镀层均匀，C和W颗粒分散均匀，所制备的粗晶硬质合金硬度、横向断裂强度和冲击韧性较优，而对比例1和对比例2，前者未添加碳粉和钨粉所制备的粗晶硬质合金晶粒度、硬度、强度和冲击韧性略低，后者因碳化钨粉未进行预处理导致合金粒度较大，且容易产生聚集态WC晶粒而导致性能下降。
表1实施例1～2和对比例1～2进行性能测试结果
Claims (10)
1.一种粗晶WC-Co硬质合金的制备方法，其特征在于，包括以下步骤：
(1)将粗颗粒WC粉末进行球磨，清洗、真空干燥得到预处理的WC粉末；
(2)将CoSO4·7H2O和NaH2PO2·7H2O溶于中配置成活化液，再将步骤1中处理后的WC粉末加入活化液中进行活化；
(3)过滤、烘干活化后的WC粉末，并进行热处理还原得到表面附着有金属Co颗粒的WC活化粉体；
(4)将CoSO4·7H2O和Na2C6H5O7·2H2O溶于水中充分络合，依次加入H3BO3和NaH2PO2·7H2O配置成镀液；
(5)将表面附着有金属Co颗粒的WC活化粉体、C粉和W粉置于镀液中，在水浴下搅拌，调节镀液pH值为10～12，并在70～90℃下进行化学镀，过滤、清洗并真空干燥得到WC/C/W/Co粗晶复合粉末；
(6)将WC/C/W/Co粗晶复合粉末加入成型剂并压制成胚，并烧结成WC-Co硬质合金。
2.根据权利要求1所述的粗晶WC-Co硬质合金的制备方法，其特征在于，所述步骤1中球磨采用直径为10～13mm的合金球，球料比为1～3:1。
3.根据权利要求1所述的粗晶WC-Co硬质合金的制备方法，其特征在于，所述步骤2中活化液中CoSO4·7H2O和Na2C6H5O7·2H2O浓度分别为50～60g/L，体积比为1：1～2，活化温度为50～60℃，活化时间为20～30min。
4.根据权利要求1所述的粗晶WC-Co硬质合金的制备方法，其特征在于，所述步骤3中热处理温度为300～400℃，时间为2～3h。
5.根据权利要求1所述的粗晶WC-Co硬质合金的制备方法，其特征在于，所述步骤4中CoSO4·7H2O浓度为45～60g/L、Na2C6H5O7·2H2O浓度为50～60g/L、H3BO3浓度为25～30g/L、NaH2PO2·7H2O浓度为30～40g/L。
6.根据权利要求1所述的粗晶WC-Co硬质合金的制备方法，其特征在于，所述步骤5中调节镀液pH值之前先将镀液预热到70～90℃。
7.根据权利要求1所述的粗晶WC-Co硬质合金的制备方法，其特征在于，所述步骤5中WC/C/W/Co粗晶复合粉末中C粉和W粉总占比为5～10wt.％，C粉和W粉的质量比为1：15～16，Co镀层为5～10wt.％。
8.根据权利要求1所述的粗晶WC-Co硬质合金的制备方法，其特征在于，所述步骤6中成型剂为SD-E橡胶，成型剂的含量占总料粉的1.5～2.5wt.％。
9.根据权利要求1所述的粗晶WC-Co硬质合金的制备方法，其特征在于，所述步骤6中压胚压制压力为20～100MPa。
10.根据权利要求1所述的粗晶WC-Co硬质合金的制备方法，其特征在于，所述步骤6中烧结时在真空条件下，烧结温度在1400～1450℃，烧结后在1～10Pa气压下保温1～2h。
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