CN102883839A - 用于制造硬质合金产品的方法 - Google Patents
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Abstract
本发明涉及一种使用粘结剂体系注射成型或挤出硬质合金或金属陶瓷部件的方法，该粘结剂体系包括20-70wt％的烯烃聚合物和30-80wt％的蜡。根据本发明，所述烯烃聚合物是聚乙烯与聚(α-烯烃)的共聚物。通过使用根据本发明的粘结剂体系，达到了更高的生坯材料韧性性能和更低的注射成型或挤出温度。
Description
技术领域
本发明涉及一种利用粉末注射成型法制造碳化钨基硬质合金工具或部件的方法。
背景技术
碳化钨基硬质合金是包括了粘结相中的至少一种小颗粒(μm级别)硬质相的复合物。这些材料通常包括硬质相碳化钨(WC)。另外，还可包括具有(Ti，Nb，Ta，W)C等基本组成的其它金属碳化物，以及金属碳氮化物，例如Ti(C，N)。所述粘结相经常包括钴(Co)。也可使用其它组成的粘结相，例如，Co、Ni和Fe的组合，或者Ni和Fe的组合。
工业制造碳化钨基硬质合金通常包括，使用研磨液体在湿润状态下将给定比例的原料粉末和添加剂共混。这种液体通常为醇，例如乙醇或水，或者两者结合。然后将混合物研磨成均一的浆液。湿磨操作的目的是解团聚和充分地混合原料。单个的原料颗粒也被粉碎到一定程度。然后将获得的浆液干燥和颗粒化，例如，通过喷雾干燥器。可将获得的颗粒用于单轴压制生坯或挤出或注射成型。
注射成型经常用在塑料工业中，其中将包括热塑性或热固性聚合物的材料加热并被强迫进入到设定形状的模具中。当在粉末技术中使用时这种方法经常被称为粉末注射成型(PIM)。这种方法优选用于具有复杂几何形状的部件。
在碳化钨基硬质合金部件的粉末注射成型中，使用四个连续步骤：
1、将颗粒状硬质合金粉末和粘结剂体系混合。粘结剂体系作为粉末的载体并占所得到的材料的25-60体积％，经常被称为原料。具体的浓度取决于成型中所要的工艺性能。通过把组分加入混料器进行混合，所述混料器被加热到有机粘结剂的熔点以上的温度。获得尺寸大约为4×4mm的原料粒料。
2、使用所述混合的原料进行注射成型。材料被加热至有机组分熔化和原料为粘性的温度，从而可用普通的注射成型机进行加工。然后所述粘性的原料被强迫进入预定形状的空腔中。获得的部件通过冷却或硬化而被固化，然后从空腔取出。
3、从获得的部件中去除粘结剂。所述去除可通过在适合的溶剂中提取所述部件和/或通过在合适气氛的加热炉中加热而进行。这种步骤通常被称为脱脂步骤。
4、烧结所述部件。使用硬质合金的常规烧结步骤。
原料挤出包括上述的1、3、4步骤。代替原料被强迫进入预定形状的空腔中，原料被连续地强迫通过具有预定截面的模具。
常规的粘结剂体系包括两种主要的有机材料和少量的化学加工助剂。所述化学加工助剂可以是表面活性剂，增塑剂，即流变控制剂，而且，化学加工助剂用于在喷雾干燥过程中形成颗粒。所述两种主要的有机材料具有在注射成型过程中作为粉末颗粒载体的常规功能。当注射成型成生坯时，它们具有不同的功能。其中的一种有机材料作为将部件保持在一起的“骨架”直到部件烧结。通常，这种“骨架”是聚合物。另一种有机材料作为可移除的部分。当可移除的部分去除后，部件上留下开口的孔隙。这种孔隙用于在后续通过在炉中热解去除粘结剂的过程中放出裂解气。这些有机材料必须要化学兼容，却一定不可混溶。一部分的粘结剂在加热前通过用非极性溶剂提取而移除，所述非极性溶剂例如为在超临界物理条件下的二氧化碳、正己烷或其它的脂肪族烷烃。
配制上面描述的粘结剂体系的常用方式是使用聚丙烯或聚乙烯或它们的结合或聚丙烯和聚乙烯的共聚物作为骨架聚合物，以及脂肪烃蜡，例如微晶蜡、费托蜡或固体石蜡或它们的结合作为可移除的有机材料。蜡的移除可以通过用非极性溶剂提取而进行，所述非极性溶剂例如为在超临界物理条件下的二氧化碳、正己烷或其它任何的脂肪族烷烃。
当使用聚丙烯或聚乙烯或它们的结合或聚丙烯和聚乙烯的共聚物作为制造硬质合金原料的骨架聚合物时，固化的原料经常变脆。这种脆性可导致在提取时部件破裂，其中在蜡熔化时的膨胀在部件中产生应力。上面提到的一些骨架聚合物甚至在室温储藏时导致部件破裂。脆性材料的另一个缺点是在处理部件时部件容易被损坏。再就是，使用上面提到的聚合物作为原料制剂中的骨架时，使得原料需要相对较高的处理温度。高温导致化学加工助剂挥发，在材料中形成泡。高处理温度还可导致在材料中形成缩痕和收缩泡。
发明内容
本发明的目的是提供一种具有低的处理温度并且没有脆性特性的原料。
令人惊讶地发现，通过使用聚乙烯与聚(α-烯烃)的共聚物作为骨架聚合物，原料的骨架聚合物和可移除的有机材料间既有化学兼容性又不可混溶，可制备出没有前面所述问题的原料。
本发明包括下面的步骤：
1)在水或醇或两者的组合中湿磨原料，优选80wt％的乙醇和20％的水，同时含有0.1-1.2wt％、优选0.25-0.55wt％的羧酸，优选硬脂酸，作为随后干燥的造粒剂。硬质成分的颗粒尺寸越小则需要越多的羧酸。
2)干燥在上述湿磨工艺步骤中形成的浆液。
3)通过捏和使干燥粉末与粘结剂体系混合，该粘结剂体系包括20-70wt％的聚乙烯与聚(α-烯烃)的共聚物，优选密度在0.860-0.915g/ml范围内、更优选在0.880-0.915g/ml范围内、最优选在0.890-0.915g/ml范围内的聚(乙烯-共-(α-辛烯))，30-80wt％的蜡以及优选的2.5-10wt％的凡士林。在分批混料机或双螺杆挤出机中进行混合，加热至50-200℃形成尺寸大约为4×4mm的粒料。
4)在传统的注射成型机中将原料注射成型。可选地，将原料在单螺杆、双螺杆或柱塞式挤出机中挤出。材料被加热至100-240℃，优选100-150℃，然后在注射成型的情形下，其被强迫进入预定形状的空腔中。在挤出时，材料被强迫通过具有预定截面的模具。将注射成型获得的部件冷却然后从空腔中移走。将挤出材料切割成预定长度的块。
5)制得部件的脱脂。脱脂分为两个步骤。
5a)优选在非极性溶剂中，在31-70℃，优选地在45-60℃提取所述可移除的有机材料，所述非极性溶剂例如为在超临界物理条件下的二氧化碳、正己烷或其它任何的脂肪族烷烃，优选在超临界物理条件下的二氧化碳。本领域技术范围内的技术人员根据这些描述可通过实验确定避免形成裂纹和其它缺陷需要的条件。
5b)在炉中加热，优选在流动气体介质的氛围中，在2毫巴至大气压力下加热至450℃。本领域技术范围内的技术人员根据这些描述可通过实验确定避免形成裂纹和其它缺陷需要的条件。
6)在脱脂炉中，在真空下，在900-1250℃、优选在约1200℃下预烧结部件。
7)使用传统的烧结技术烧结部件。
本发明还涉及一种用于注射成型或挤出硬质合金或金属陶瓷的粘结剂体系，该体系包括20-70wt％的烯烃聚合物和30-80wt％的蜡，其中所述烯烃聚合物是聚乙烯与聚(α-烯烃)的共聚物。
本发明可用于所有组成的硬质合金和所有平常使用尺寸的WC颗粒，还可用于钛碳氮化物基材料。
具体实施方式
实施例1
通过在由乙醇和水(重量比为80∶20)组成的1.6L研磨液体中湿磨780g Co粉(OMG超细)、38.66g Cr3C2(H C Starck)、5161g WC(H C Starck DS80)、20.44g W金属粉末、16g费托蜡(Sasol H1)和22g硬脂酸40小时制成亚微米的WC-13wt％Co硬质合金粉末。当喷雾干燥浆液时，硬脂酸在此阶段加入作为颗粒形成剂。制成的浆液被喷雾干燥成颗粒粉末。
实施例2(对比)
通过将2500g实施例1的粉末与50.97g聚丙烯-聚乙烯共聚物(RD360MO，Borealis)、45.87g固体石蜡(Sasol Wax)和5.06g凡士林(Merkur VARA AB)在曲拐式强力混合机(Werner&Pfleiderer LUK1.0)中捏和，而将实施例1制备的粉末混合。
实施例3(本发明)
通过将2500g实施例1的粉末与50.97g密度大约为0.895g/ml的聚(乙烯-共-(α-辛烯)(Engage 8440，Dow Plastics)、45.87g固体石蜡(Sasol Wax)和5.06g凡士林(Merkur VARA AB)在曲拐式强力混合机(Werner&Pfleiderer LUK 1.0)中捏和，而将实施例1制备的粉末混合。
实施例4(对比)
将实施例2中制备的原料送入注射成型机中(Battenfeld HM60/130/22)。此机器用于注射成型山高刀具Minimaster的10mm立式铣刀的生坯。用于注射成型的材料温度为160℃。切断部件用于检查，在一些部件中发现了气泡。
实施例5(本发明)
将实施例3中制备的原料送入注射成型机中(Battenfeld HM60/130/22)。此机器用于注射成型山高刀具Minimaster的10mm立式铣刀的生坯。用于注射成型的材料温度为125℃。切断部件用来检查，没有发现气泡。
实施例6(对比)
通过在超临界物理条件下的二氧化碳中即在35MPa和58℃下提取，将实施例4中的部件脱脂20小时。在提取后检查部件。肉眼能够看到部件表面的裂纹。
实施例7(本发明)
通过在超临界物理条件下的二氧化碳中即在35MPa和58℃下提取，将实施例5中的部件脱脂20小时。在提取后检查部件。肉眼没有看到部件表面的裂纹，在50倍放大率下观察时也没发现裂纹。
Claims (10)
1.一种注射成型或挤出硬质合金或金属陶瓷部件的方法，该方法包括下面的步骤：
-在水或醇或其组合中湿磨原材料，
-干燥在湿磨工艺步骤中形成的浆液，
-通过捏和使干燥粉末和粘结剂体系混合，该粘结剂体系由20-70wt％的聚乙烯与聚(α-烯烃)的共聚物和30-80wt％的蜡组成，
-在注射成型机中将原料注射成型或在单螺杆、双螺杆或柱塞式挤出机中将原料挤出，以及
-对制得的部件脱脂。
2.根据权利要求1所述的方法，其特征在于所述的聚乙烯与聚(α-烯烃)的共聚物是聚(乙烯-共-(α-辛烯))。
3.根据权利要求2所述的方法，其特征在于所述的聚(乙烯-共-(α-辛烯))的密度范围是0.860-0.915g/ml。
4.根据权利要求3所述的方法，其特征在于所述的聚(乙烯-共-(α-辛烯))的密度范围是0.880-0.915g/ml。
5.根据权利要求4所述的方法，其特征在于所述的聚(乙烯-共-(α-辛烯))的密度范围是0.890-0.915g/ml。
6.一种用于注射成型或挤出硬质合金或金属陶瓷部件的粘结剂体系，该粘结剂体系包括20-70wt％的烯烃聚合物和30-80wt％的蜡，其特征在于所述烯烃聚合物是聚乙烯与聚(α-烯烃)的共聚物。
7.根据权利要求6所述的粘结剂体系，其特征在于所述聚乙烯与聚(α-烯烃)的共聚物是聚(乙烯-共-(α-辛烯))。
8.根据权利要求7所述的粘结剂体系，其特征在于所述的聚(乙烯-共-(α-辛烯))的密度范围是0.860-0.915g/ml。
9.根据权利要求8所述的粘结剂体系，其特征在于所述的聚(乙烯-共-(α-辛烯))的密度范围是0.880-0.915g/ml。
10.根据权利要求9所述的粘结剂体系，其特征在于所述的聚(乙烯-共-(α-辛烯))的密度范围是0.890-0.915g/ml。
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| SE1050388A SE533797C2 (sv) | 2010-04-20 | 2010-04-20 | Sätt att tillverka hårdmetallprodukter |
| SE1050388-6 | 2010-04-20 | ||
| PCT/SE2011/050483 WO2011133100A1 (en) | 2010-04-20 | 2011-04-20 | Method for producing cemented carbide products |
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| EP (1) | EP2560777A4 (zh) |
| KR (1) | KR20130059334A (zh) |
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| SE533922C2 (sv) * | 2008-12-18 | 2011-03-01 | Seco Tools Ab | Sätt att tillverka hårdmetallprodukter |
| KR20130083840A (ko) * | 2010-05-26 | 2013-07-23 | 쎄코 툴스 에이비 | 초경합금 제품의 제조 방법 |
| DE102012212018A1 (de) * | 2012-07-10 | 2014-01-16 | Robert Bosch Gmbh | Bindersystem für Pulverspritzgussmasse |
| IN2013CH04500A (zh) | 2013-10-04 | 2015-04-10 | Kennametal India Ltd |
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| DE4407760A1 (de) * | 1994-03-08 | 1995-09-14 | Bayer Ag | Thermoplastische Formmassen sowie deren Verwendung |
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| US5809848A (en) * | 1996-02-12 | 1998-09-22 | Credo Tool Company | Method of making a carbide cutting insert |
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| SE532448C2 (sv) * | 2007-11-01 | 2010-01-19 | Seco Tools Ab | Sätt att tillverka hårdmetallprodukter |
| US8524818B2 (en) * | 2008-01-18 | 2013-09-03 | Lubrizol Advanced Materials, Inc. | Thermoplastic composition |
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- 2011-04-20 CN CN2011800196238A patent/CN102883839A/zh active Pending
- 2011-04-20 KR KR1020127027425A patent/KR20130059334A/ko not_active Application Discontinuation
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- 2011-04-20 EP EP11772329.6A patent/EP2560777A4/en not_active Withdrawn
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| DE4407760A1 (de) * | 1994-03-08 | 1995-09-14 | Bayer Ag | Thermoplastische Formmassen sowie deren Verwendung |
| WO1998018973A1 (en) * | 1996-10-25 | 1998-05-07 | Sandvik Ab (Publ) | Method of making cemented carbide by powder injection molding |
| CN1268909A (zh) * | 1997-09-01 | 2000-10-04 | 赫加奈斯公司 | 冶金粉末组合物用的润滑剂 |
| WO2009024398A1 (de) * | 2007-08-20 | 2009-02-26 | Robert Bosch Gmbh | Formmasse und verfahren zur herstellung einer formmasse |
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| CN102256728A (zh) * | 2008-12-18 | 2011-11-23 | 山高刀具公司 | 制备硬质合金产品的方法 |
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| EP2560777A1 (en) | 2013-02-27 |
| SE1050388A1 (sv) | 2011-01-18 |
| BR112012027007A2 (pt) | 2016-07-19 |
| KR20130059334A (ko) | 2013-06-05 |
| SE533797C2 (sv) | 2011-01-18 |
| RU2012149283A (ru) | 2014-05-27 |
| EP2560777A4 (en) | 2014-11-26 |
| US20130064708A1 (en) | 2013-03-14 |
| WO2011133100A1 (en) | 2011-10-27 |
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