CN1084231C - 金属加工的润滑 - Google Patents

金属加工的润滑 Download PDF

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Publication number
CN1084231C
CN1084231C CN96195004A CN96195004A CN1084231C CN 1084231 C CN1084231 C CN 1084231C CN 96195004 A CN96195004 A CN 96195004A CN 96195004 A CN96195004 A CN 96195004A CN 1084231 C CN1084231 C CN 1084231C
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China
Prior art keywords
lubricant
metal
perfluor
wire
pipe
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Expired - Fee Related
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CN96195004A
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CN1189112A (zh
Inventor
R·W·巴雷特
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Materion Newton Inc
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HC Starck Inc
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    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/56—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing nitrogen
    • C10M105/58—Amines, e.g. polyalkylene polyamines, quaternary amines
    • C10M105/60—Amines, e.g. polyalkylene polyamines, quaternary amines having amino groups bound to an acyclic or cycloaliphatic carbon atom
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B45/00—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills
    • B21B45/02—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills for lubricating, cooling, or cleaning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B45/00—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills
    • B21B45/04—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills for de-scaling, e.g. by brushing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C43/00—Devices for cleaning metal products combined with or specially adapted for use with machines or apparatus provided for in this subclass
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
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    • B21C9/00—Cooling, heating or lubricating drawing material
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    • B21B45/0239—Lubricating
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    • B21B45/0248—Lubricating devices using liquid lubricants, e.g. for sections, for tubes
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Abstract

采用润滑剂加工难熔金属和其他金属的方法，该润滑剂包括全氟化碳化合物(PFC)，包括具有通式为CnF2n+2的脂族全氟化碳化合物(α-PFC)，具有通式为CnF2n+1ON的全氟吗啉类，全氟胺类(PFA)和高度氟化的胺类(HFA)，全氟醚类(PFE)和高度氟化的醚类(HFE)及其聚合产物。

Description

金属加工的润滑
本申请涉及润滑，特别是涉及各种金属加工方法包括非切削成形法和切削/机械加工法的润滑。成形法包括金属丝拉制、无缝管和有缝管的成形、管的轧制、锻造(包括镦锻、型锻和滚丝)、碾轧(包括扁平轧材和型材的碾轧)、挤压、薄板加工法包括下料、模压、深拉延、冲孔、剪切、旋压、冲压和拉伸成形、金属切削和机械加工作业包括切削、镗孔、扩孔、钻孔、端面加工、铣削、刨削、铰孔、锯切、攻丝、套孔和车削以及砂轮切割、磨削、喷砂清理、抛光和擦光。上述各种作业均在轧材和/或成品零件(工件)上进行。
许多金属加工的成形和切削方法采用润滑剂来冷却工件和工具、冲洗在切削过程中切掉的金属、降低工具和工件之间的摩擦力以及作为防止粘结或滞塞的阻挡层。在不同的金属加工方法以及用于不同金属的特定加工方法中，上述各种润滑所要求的程度是不同的。这可通过难熔金属(钽、铌、钼、钨、钛、锆、铪、及合金)、钢和普通黑色和有色金属(铁、铜、铝、镍和合金，例如INCONELTM和钢)以及贵金属(金、铂、钯、铑、铼)拉丝时润滑的要求情况加以说明。本文中所用的术语“金属”包括可采用基本上与金属相同的方法加工的例如金属陶瓷类的陶瓷，其中采用润滑的方法来降低工具的磨损和/或增进金属加工的过程。
由于工件和工具之间剧烈的滑动接触，在所有的金属加工作业中均采用润滑剂以便减少工件和工具之间的摩擦、冲洗工具以防止碎屑和污垢聚集在工具表面上、减少工件和工具之间的磨损和滞塞、除去塑性变形期间产生的热以及保护工件成品的表面特性。
当今加工普通金属所用的润滑剂是各种酯类；皂类；固体润滑剂，例如石墨、TEFLONTM、熔融氟化物、MoS2、WS2、MoSe2、MoTe2和类似的固体润滑剂以及其他特压润滑剂的复杂混合物。油基或聚乙二醇基的润滑剂常以浓度约为10％的水中的乳剂形式使用，有时用添加剂赋予该乳剂必需的去垢性以使工件和工具保持洁净。易于清洗是选择金属加工润滑剂的基本参数。在目前的工艺水平下，已发现这几类润滑剂例如在生产难熔金属丝时是不适应的。在这种情况下使用固体润滑剂容易出故障。
众所周知，特别是在难熔金属的拉丝和拔管时在工具和工件之间的摩擦力、工具的磨损和工件经受的应力方面呈现出最苛刻的条件。因此，仅为说明起见，以下的讨论将涉及难熔金属的拉丝和拔管，并应理解该论述同样适用于其他金属加工作业和其他冶金的工件。
在磷酸盐预涂层上已使用各种氯化油以及各种石墨和二硫化钼润滑剂的混合物，然而对于拉制难熔金属丝仅取得有限的成功。最近，粘度通常为20-150厘沲的氯三氟乙烯(CTFE)基的油类已成为生产难熔金属丝时选用的润滑剂。尽管CTFE润滑剂几乎是目前唯一用在生产电子级钽丝的润滑剂，但是它们显示出许多苛刻的操作限制。由于CTFE润滑剂的传热性很差，因而拉制速率必须很抵，通常为100-300FPM。而普通金属的拉丝速率通常为5000-20,000FPM。因此，相比之下难熔金属的拉制成本很高。
此外，CTFE润滑剂在减少金属丝和模具之间的磨损和滞塞以及将磨损生成物从模具的入口喇叭冲洗掉方面仅仅勉强合乎要求。这些问题是很明显的，当采用碳化物模具拉制钽丝时存在着模具寿命短(每套＜20磅)和持续产生表面粗糙度和尺寸控制(包括直径和圆度)的问题。所有这些与CTFE润滑剂有关的局限性使难熔金属丝的拉制固有地成为一种成本高且产品质量不令人满意的方法。
当试图从金属丝成品表面除去CTFE润滑剂时，发现了这类润滑剂更严重的局限性。通常，采用一些溶剂典型的是1，1，1-三氯乙烷来除去这类润滑剂。然而，由于这些溶剂具有易燃性、毒性、消耗臭氧、会使全球变暖，因而对溶剂的使用日益增加了限制，所以几乎完全不可能从金属丝成品上除去CTFE润滑剂。曾试图采用一些热的水性脱脂体系在有或没有超声波作用的情况下除去这类润滑剂，然而仅取得了有限的成功。电子级金属丝表面上的CTFE润滑剂残余物仍然是电子元件失灵的原因。
生产无缝金属管的第一个步骤通常是通过辊轧锻铸(rolling cast)或预先轧制成圆钢坯实现的。将轧制成的厚壁管用作毛坯管加以拉制。根据所需的管径和壁厚可采用一些不同的制造方法。生产无缝管的最古老方法是利用横向螺旋轧制原理的曼内斯曼式穿孔法。该机器包括其轴彼此倾斜的两个钢辊。它们以相同的方向旋转。两辊之间的距离会聚至称为咽喉(gorge)的最小宽度。恰在该咽喉之外的是一个穿孔心棒。将与这两个辊呈相反方向旋转的固体金属圆棒插入该两辊之间。当该圆棒的前端前进到该咽喉处时，就与该穿孔心棒相遇，而当圆棒继续前进通过该两辊时，穿孔心棒就会在圆棒中形成一个中心空腔。
随后可将采用曼内斯曼式穿孔法制成的厚壁管通过所谓皮尔格式轧管机中的专用轧辊减薄为薄壁管。这些轧辊在其圆周的周围的断面形状是不同的。固定在穿孔心棒上的管首先被这两个轧辊的狭窄部分夹持。由于专用轧辊的旋转，致使该专用轧辊逐渐加厚的部分与该管接触，并在该管的壁上产生增大的压力，从而使该管的壁厚减薄直至每个轧辊已旋转达到其断面的最宽部分的程度为止，这样，该管就不再被夹持。然后，再将该管拉回一定距离，使该管的厚壁部分再用该轧辊夹持。该穿孔心棒同时旋转，以保证在该管的整个圆周上施加均匀的轧辊压力。
第二种生产无缝金属管的普通方法是斯蒂费尔穿孔法，其中首先将圆棒在旋转的穿孔机上穿孔，然后将这样得到的厚壁管在第二道穿孔工序中在二辊式轧机平台上减薄以形成薄壁管。
第三种生产无缝金属管的普通方法是回旋式锻造法，其中将加热到轧制温度的方钢锭成形为一端封闭的毛坯管。然后将该毛坯管在回转式穿孔机上减薄并拉伸，最后通过按90°的间隔排列在该管周围的四套轧辊从而将其管径逐渐缩小。
第四种生产无缝金属毛坯管的普通方法是挤压法，其中将坯体在模具和穿孔心棒(为了保持该管的中心空腔)之间加压。然后采用上述方法中之一将挤出的毛坯管缩减到最终直径和壁厚。
挤压法是用来生产包括棒、管、空心断面、条、丝和带的长而直的金属产品的金属加工方法。在该方法中，将放置在密闭容器中的坯料在重载荷下强使其通过模具以生产具有所需截面的挤压件。根据待加工的金属或合金而定，挤压法可以在室温或高温下进行。
冷挤压法广泛用于挤压包括铅、锡、铝、黄铜和铜等低熔点的金属。在这种方法中，将坯料放置在腔室内并进行轴向加压。该金属穿过具有一个或多个孔的模具流出而形成被挤压产品的截面。
最广泛用于生产挤压成形制品的方法是直接热挤压法。在这种方法中，将加热了的固体金属坯料或含有金属或陶瓷粉的金属容器或预制件等放置在腔室内，然后通过柱塞轴向加压。在对着柱塞的缸体端装有一个具有所需形状的锐孔或有许多锐孔的模具。
与直接热挤压法一样，静液力挤压法包括在压力下强使固体金属坯料或含有金属或陶瓷粉的金属容器或预制件穿过适当形状的锐孔。在这两种方法中，均将工件或类似物件放置在腔室内，该腔室的一端装有一个具有所需形状的锐孔或有许多级形锐孔的模具。与直接热挤压法不同的是，直接热挤压法中作用在工件上的压力是通过工件和柱塞之间直接接触而产生的，而在静液力挤压法中则是通过工件周围的推力介质(液体或粉状物质)将压力间接传递到该工件上。由此可见，所有的压力都均匀地作用在工件上。静液力挤压法几乎已应用于所有的材料例如铝、铜、钢和陶瓷。
此外，金属的挤压法有各种不同的称谓：顶锻法、压制法、锻压法、挤压锻造法、冷挤压法以及冲击挤压法。冷镦法在钢和有色金属加工领域已很普及。这种原始的方法包括用来撞击已放置在模具空腔内待挤压的金属坯料(或锻造毛坯)的冲头(通常在高速下移动)。该冲头和模具壁之间留有间隙。当该冲头与坯料接触时，该金属除了通过冲头和模具之间的环形缝隙以外无处可去。该冲头移动的距离通过压机的设定控制。该距离确定了零件成品的基本轴向厚度。冷挤压法的优点是由于剧烈的应变硬化使得挤压件的强度较高、表面光洁度好、尺寸精确且所需的机械加工量最少。然而，坯料和模具之间增加的摩擦需要高效的润滑剂来确保挤压件符合所需的技术规格，且保证坯料不致堵塞在模具中。
通常将采用上述方法生产的空心圆筒或管通过拉拔进行冷精轧。采用冷拔法以获得更精密的尺寸公差、产生更好的光洁度、通过应变硬化改善管材的机械特性、生产出比热成形法能得到的壁更薄或直径更小的管材以及生产出异型管。
拔管法与拉丝法类似。在拉拔机或拉丝模上并用类似于拉丝时所用的模具来生产管材。然而，为了缩小壁厚和精确地控制内径，当管材通过模具时必须支护该管的内表面。通常，可在该管内插入一条心棒实现。通常将该心棒紧固在与拉拔机的一端连接的固定杆的端部，并加以定位，以使该心棒位于模具的咽喉处。该心棒可具有圆柱形或锥形截面。
也可以采用活动的心棒，或通过将长杆与该管一起拉过模具或将深拉延的毛坯管与冲头一起推过模具来拉制管材。由于用长杆作为心棒时有困难，因此用长杆的拔管法通常仅限于生产大直径的管材。对于小直径的管材，支护固定心棒用的杆太细而没有足够的强度。
另一种管成形法是在通过模具拔管时不用心棒支护该管内表面的无心棒拔管法。由于在无心棒拔管法中不对该管的内部支护，因而壁厚会增加或减小，这取决于该方法所施加的条件。在工业上，无心棒拔管法仅用于生产小管。然而，无心棒拔管法提出了一个重要的塑性成形理论问题，因为它作为带有心棒拔管的第一个步骤出现。为了能通过心棒的尺寸控制管材的尺寸，必须在管材通过模具的初期阶段采用无心棒拔管法将该管的内径减小到比该心棒的直径略小一些的值。
已从所有的普通金属包括钢、铜、铝、金、银等以及难熔金属包括钽、铌、钼、钨、钛、锆及其合金等生产管材。由于管材和模具之间以及管材和心棒之间剧烈的滑动接触，在管成形作业中采用润滑剂以便减少管材与成形工具之间的摩擦、冲洗工具以防止碎屑和污垢聚集在工具表面上、减少工具和管材之间的磨损和滞塞、除去塑性变形期间产生的热以及保护管材成品的表面特性。
与拉丝法一样，易于清洗是选择拔管润滑剂的基本参数。在目前的工艺水平下，已发现一些润滑剂在生产难熔金属管时是不适应的。
CTFE润滑剂的传热性很差极大地限制了拉制速率，通常仅为50-100FPM。而普通金属的拔管速率通常为1,000-4,000FPM。因此，相比之下难熔金属的拉制成本很高。此外，CTFE润滑剂在减少管材和模具之间的磨损和滞塞以及将磨损生成物从模具的入口喇叭冲洗掉方面仅仅勉强合乎要求。这些问题会导致模具寿命短以及表面粗糙度和尺寸控制(包括直径和圆度)的问题。另外，与拉丝法一样，CTFE润滑剂会留下难以清除的残余物(在成品管的外表面和内表面上)。
在生产不能盘卷的管材时会出现另一个问题。这些管材通常是在拉拔机上采用高达1000FPM的速率拉制成直长形的。因此，甚至在该管的外表面上部分形成流体动力膜的趋势被大大地降低。在内表面上的状况甚至更严重；甚至当采用浸涂法涂覆时，用拉拔膏或固体皂也不能保证充分的覆盖，而当润滑剂分解时，经常导致未被润滑的部分滞塞。
可以比较容易地将液体润滑剂涂覆在管材的内表面上，但是，很少有液体润滑剂是足以有效地避免某些金属与金属接触的边界润滑剂，而且有些润滑剂(例如氯化油)的确经常能促使心棒的腐蚀性磨损。由于在芯塞和模具上的环状磨损非常明显，因此，在任何情况下磨损都会加倍。当拉拔反应性较小的材料例如不锈钢或钛合金时，这些困难大大地增加。
本发明的目的是提供改进了的采用润滑性比常规润滑剂优越的润滑剂的金属加工方法。
本发明的另一个目的是采取避免上述问题的方式改进加工金属的方法。
本发明的第三个目的是在常规的金属加工方法中采用不易燃和无毒的润滑剂。
本发明的第四个目的是在常规的金属加工方法中采用具有零臭氧消耗潜力(ODP)的润滑剂。
本发明的第五个目的是在常规的金属加工方法中采用一种润滑剂，该润滑剂在大气中无光化学反应性而且既不是光化学烟雾的前体也不是各国和各国际组织定义的挥发性有机化合物(VOC)。
类似地，本发明的目的是提供一种改进了的方法，该方法提供的润滑性可避免上述问题。
本发明的再一个目的旨在减少通常不认为是金属加工过程然而涉及润滑的过程中金属和有关部件的磨损，所述过程是例如齿轮传动、链传动和润滑油箱中的或敞开式变速器的操作；以及在轴承、轴颈或轴瓦上转动或轴向运动的轴的操作。
本发明在用于拉丝、拔管、无心棒拔管或轧制管材、轧制带材、镦锻、模压、无缝金属管成形、锻造、型锻和挤压的方法和设备(机器)时优选使用完全氟化和高度氟化的润滑剂，更具体而言，优选用于生产难熔金属轧材和成品零件。这些优选的方法和设备使用的润滑剂包括一种或多种：(a)全氟化碳化合物(PFC)，包括通式为CnF2n+2的脂族全氟烷烃(α-PFC)，(b)通式为CnF2n+1ON的全氟吗啉类(PFM)，(c)全氟胺类(PFA)，(d)高度氟化的胺类(HFA)，及其各自的聚合产物。由于碳-氟键的强度使这些完全氟化和高度氟化的碳化合物呈现出很高的热稳定性和化学稳定性。PFC类的特征还在于其表面张力极低、粘度低和流体密度高。它们是清澈、无臭、无色的液体，其沸点约为30℃至约300℃。这些液体可以单独使用或与惰性载体例如润滑脂、糊剂、蜡、磨光剂等配合使用。
可用于本发明的氟化了的惰性液体可以是α-PFC、PFM、PFA和HFA类化合物中的一种或其混合物，这些化合物具有5-18个或更多的碳原子，任选含有一个或多个链状杂原子例如二价氧、六价硫或三价氮，H∶F之比低于1∶1，氢含量优选小于5％(重量)，最优选小于1％(重量)。这些材料可呈液相单独使用，也可与其他功能性的液体或载液混合或乳化和/或与固体微粒混合为糊剂(例如与已知的微粒状固体润滑剂如氟化钕、硫化钼、硫化钨、硒化钼、碲化钼、石墨、TEFLOWTM、熔融氟化物以及类似的固体润滑剂混合)。根据本发明的方法用于氟化液体的载体可以是例如润滑脂、糊剂、蜡和磨光剂。
具体而言，适用于本发明的氟化了的惰性液体可以包括例如全氟烷类例如全氟戊烷、全氟己烷、全氟庚烷和全氟辛烷；全氟胺类例如全氟三丁胺、全氟三乙胺、全氟三异丙胺、全氟三戊胺；全氟吗啉类例如全氟-N-甲基吗啉、全氟-N-乙基吗啉和全氟-N-异丙基吗啉；以及上述各类的聚合产物。
本说明书所用的前缀“全氟”意指所有的或基本上所有的氢原子均被氟原子取代。最初开发的全氟化碳液体供作传热液体之用。目前它们用于传热、气相焊接和电子测试方面的用途以及作为溶剂和清洁剂。本说明书所用的术语“高度氟化的”意指具有H∶F之比低于1∶1。
可用于本发明的市售的氟化了的惰性液体包括FC-40、FC-72、FC-75、FC-5311、FC-5312(可从3M公司以商品名Fluorinert，3MProduct Bulletin 98-02110534707(101.5)NP1(1990)买到)；LS-190、LS-215、LS-260(可从Montefluos Inc.，Italy买到)；HostinertTM175、216、272(可从Hoechst-Celanese买到)；K-6、K-7、K-8(可从DuPont买到)。
重要的是，因为PFC是高度或完全氟化了的，因此，它们不含氯或溴并具有零臭氧消耗潜力(ODP)。上述液体不易燃且无毒。此外，因为它们在大气中无光化学反应性，所以它们不是光化学烟雾的前体，也不是联邦定义的挥发性有机化合物(VOC)。
此外，PFC液体的价格显著低于目前使用的氯三氟乙烯油的价格。因此，这些氟化了的惰性液体对本说明书所述的各种方法都是有利的，目前，PFC类是高速拉制难熔金属细丝的优选润滑剂。
在拉丝方法中，全氟化碳液体已大大扩展了对工艺工程师有用的主要拉丝变数的范围。在使用CTFE类润滑剂时，每模具的缩减率局限于约15％。使用PFC类润滑剂可使缩减率大到每模具26％。这将使下一代拉丝设备更加多产。此外，操作速率可以提高10倍以上，从而大大减少在给定生产能力下所需的拉丝机的台数。CTFE类润滑剂局限于约200FPM，然而PFC类润滑剂已在2,000FPM以上的速率下使用仍未出现已达到上限的迹象。此外，可使模具的磨损降低到最低程度，并可将0.103英寸(2.5mm)的金属丝拉拔到最终直径为0.005英寸(0.127mm)而不发生退火且模具的寿命大于200磅成品硬拉丝。
在拔管法中，全氟化碳液体大大扩展了对工艺工程师有用的主要拉拔变数的范围。在使用常规的润滑剂时，每道次的缩减率局限于约10-15％。使用PFC类润滑剂可使缩减率大到30％。这可使新的和改进的拔管方法和设备更加多产。操作速率可以提高10倍以上，从而大大提高给定生产设备的生产能力。常规的润滑剂局限于约100FPM，然而PFC类润滑剂可在2,000FPM以上的速率下使用。本发明的PFC类润滑剂提高了一些小直径的管、特别是皮下注射针头和直径为0.005-0.125英寸(0.127-3.17mm)、壁厚为0.001-0.050英寸(0.025-1.27mm)的毛细管的生产能力。
在金属加工领域中拉拔钽丝和钽管时需要润滑是一种最苛刻的操作条件。本说明书所示的结果证实，对于不太苛求的金属加工方法和其他一些更有延展性和韧性的材料是可行的。
迄今评价了的所有等级的全氟化碳液体均已用于生产高质量的钽丝和钽管。从3M公司的沸点仅为30℃、粘度为0.4厘沲的PF-5050(C5F12)到通式CnF2n+3N的全氟胺，如3M公司的沸点为215℃、粘度为14厘沲的FC-70(全氟三丙胺(C3F9N)和全氟三丁胺(C4F11N)的掺合物)，到其他沸点至多为240℃、室温下的粘度为40厘沲的PFC类(例如全氟三丁胺、全氟三戊胺和全氟三丙胺)均已用于在高拉拔速率下生产高质量的钽丝和在高轧制速率和/或高拉拔速率下生产高质量的钽管。3M公司的FC-40(全氟三丙胺(C3F9N))由于售价低且沸点高(155℃)因而受到了广泛的评价。这种液体具有的粘度仅为2厘沲，室温下的蒸气压为3乇(3mmHg)。所有的数据表明许多其他的PFC类液体都是优良的金属加工润滑剂。
润滑特性与PFC类液体的粘度无关这一事实是这类液体所独有的，且在当今的金属加工润滑理论上还不了解。事实上，使用粘度小于1厘沲的金属加工润滑剂是与大多数润滑理论对立的。
此外，已观察到在上述拉制过程中产生的亚微细的钽微粒碎屑大量减少。当采用常规的润滑剂时，由于高含量的钽细粉使得该润滑剂在几小时内变成黑色和“焦油状”。当采用PFC液体时，采用简单的过滤器可保持该液体透明清澈。与常规的润滑剂相反，当管材离开机器时，PFC类可从该管的表面蒸发出来。因此，使用这类润滑剂不仅使所得产品比采用常规润滑剂可能得到的更光滑、更洁净和性能更好，而且与常规的润滑剂相比，不需要后续的清洗步骤。
各种金属加工作业可以通过上述方法改善。在有关生产用作钽电解电容器中阳极导线的细钽丝的上下文中已了解到这些特别的好处。将钽丝(直径通常为5密耳-20密耳(0.127mm-0.508mm))对焊到多孔的烧结粉末阳极上，或在烧结前将其嵌入该阳极中，烧结时使其与该阳极结合。采用这种阳极时，电容器的最小漏电量部分取决于导线的清洁度，而这是受到润滑剂的选择直接影响的。
采用本发明生产的钽丝已实现了导线的DC漏电显著降低。漏电现象直接与导线的表面形态以及仍然陷在导线表面缝隙和裂缝中的润滑剂量有关。DC漏电可以通过生产出光滑的导线表面和从导线表面消除残余的润滑剂降低。DC漏电可以通过将一定长度的导线阳极处理达到以氧化钽的介电薄膜完全覆盖该表面进行测定。将阳极处理过的导线放置在电解质中，并在该钽导线体上施加DC电压。在固定的电压下测定通过所述介电薄膜“漏泄”的DC电流。上述漏泄电流是介电薄膜的完整性的量度。介电薄膜完整性本身又是整个导线表面的表面粗糙度和清洁度的量度。通过产生出无残余润滑剂的光滑表面，可以生产改进的介电薄膜，从而可改进导线以及其上附有该导线的阳极的DC漏电特性。
此外，在有关生产用作热交换器管道的钽管的上下文中已了解到这些显著的好处。该钽管(直径通常为10-40mm)用于化学工业生产厂中的热交换用途，在这些工厂中没有任何其他金属材料可以保持完好。上述的那些好处在其他不太苛刻的操作条件下也可以了解到，这些条件包括其他的金属加工方法和采用其他更有延展性和韧性的材料或一些材料(即本文中所定义的呈现类似的或更加苛刻的金属加工作业的金属)。本发明也可以用于一般的润滑用途，例如箱式润滑(case lubrication)、轴承润滑等。
本发明通常不能在温度高于氟化液体分解温度(＞600℃)下进行的高温金属加工方法中应用。所指的温度是施加到金属加工机械的成形或切削表面和/或工件(例如挤压之前加热的坯料)上的外部热以及通过工具表面与工件之间的机械接触而产生的结果。在有润滑的金属加工过程结束时会发生沸腾，且经常在通过本发明增强的冷法和温法(甚至在正常的热法中)中发生。从氟化液体蒸发出来的蒸气可以通过利用冷却表面冷凝加以回收。冷凝液可以重复利用而无需再调节。
本发明还包括压缩粉末冶金的应用，其要点在于当将金属微粒在模具中或等压地压缩时，液体或固体状态的氟化了的惰性材料可用作例如呈初级或次级(预烧结)形式的粉状和/或片状金属微粒的涂层。可在混合器中以一种类似于采用常规润滑剂/粘合剂例如硬脂酸的常规涂覆方式将这些微粒与该液体一起翻滚，直到完全被覆盖为止。初始压制时在微粒中产生通常呈逐点熔结的多孔形式的紧凑的压块。然后，将该压块加热到高于氟化涂料的沸点以将该氟化物从该多孔物质中驱除而基本上不遗留其残余物。根据直接用户的用途，该压块可以直接使用或再采用冷压、热压、烧结或其他已知的工艺步骤加以压制和/或加热进一步使其压实和强化。
在粉末冶金压制中，氟化了的惰性液体可以单独使用或与辅助润滑剂一起使用。其用途可限于在压制之前涂覆该金属颗粒或(与包括辅助润滑剂在内的适宜固体材料配合)在压块中形成基体和/或将压块粘结在一起。在这种情况下，可在初始压制金属之后借助常规的除粘合剂的技术基本上将包含氟化了的惰性材料的基体整个地除去。优选将氟化了的惰性材料和辅助润滑剂蒸出。
图1所示为在200英尺/分钟(61米/分钟)下采用FC-40全氟化碳液体拉制的金属丝表面的300X和1000X扫描电子显微照片。
图2所示为在500英尺/分钟(152.4米/分钟)下采用FC-40 PFC液体拉制的金属丝表面的300X和1000X扫描电子显微照片。
图3所示为在1,000英尺/分钟(304.8米/分钟)下采用FC-40 PFC液体拉制的金属丝表面的300X和1000X扫描电子显微照片。
图4所示为在200英尺/分钟(61米/分钟)下采用CTFE润滑剂拉制的两种金属丝样品表面的1000X扫描电子显微照片。
图5所示为采用CTFE润滑剂拉制的TPX金属丝表面上50微米2区域的2500X的SPM显微照片。
图6所示为采用FC-40 PFC液体拉制的TPX金属丝表面上50微米2区域的2500X的SPM显微照片。
图7所示为采用CTFE润滑剂拉制的电容器级钽丝的表面上50微米2区域2500X的SPM显微照片。
图8所示为3M FC-40 PFC液体的微-FTIR参照谱图。
图9所示为从电容器级钽丝样品获得的提取物的微-FTIR谱图以及FC-40 PFC液体的微-FTIR参照谱图。
图10所示为从用于在生产规模拉制电容器级钽丝的超声波束清洗系统中清洗后的电容器级钽丝样品取得的提取物的微-FTIR谱图。
图11所示为附加在CTFE油和酯基线材轧制油的参照谱图上的清洗后的微-FTIR谱图。
图12所示为采用FC-40 PFC液体拉制的TPX金属丝来样的漏电率，以μA/cm2计。
图13所示为用于拉丝的PFC液体的收回和再循环装置的示意图。
图14 A-D所示为采用FC40和拉制铜的烃基润滑剂拉制的ETP铜丝的300X和4500X扫描电子显微镜图像。
图15 A-B所示为采用FC40和CTFE润滑剂拉拔的钽管的扫描电子显微镜图像。
图16 A-B所示为采用FC40和CTFE润滑剂拉拔的钽管表面的扫描探针显微镜图像。
图17所示为采用L13557全氟化碳液体拉制的.0993英寸的302不锈钢丝表面的扫描电子显微镜图像
图18 A-C所示为采用L13557全氟化碳液体机械加工的4mm钽螺母的表面。
根据其优选实施方案的本发明的实施通过以下非限制性实施例加以说明：
实施例1：
采用FC-40全氟化碳液体(3M公司)作为润滑剂通过Heinrich拉丝机(MODEL # 21W 21)拉制了169.5磅(77.1千克)0.0098英寸(0.0249厘米)的半硬回火钽丝。拉丝速率为200英尺/分钟(61米/分钟)至1386英尺/分钟(424.5米/分钟)。每盘金属丝开始时采用激光测微计测得平均圆度为1英寸的百万分之16(40.6微米)，每盘结束时的平均圆度为1英寸的百万分之18(45.7微米)。每套模具平均生产42.4磅钽丝。
实施例2：
与实施例1相同，采用3M公司的FC-40全氟化碳液体作为润滑剂，通过Heinrich拉丝机拉制了70.2磅(31.9千克)0.0079英寸(0.0201厘米)的特硬回火钽丝。拉丝速率为500英尺/分钟(152.4米/分钟)至1000英尺/分钟(304.8米/分钟)。每盘金属丝开始时的平均圆度为1英寸的百万分之11(27.9微米)，每盘结束时的平均圆度为1英寸的百万分之11(27.3微米)。每套模具平均生产35.1磅钽丝。
实施例3：
与实施例1相同，采用3M公司的FC-40全氟化碳液体作为润滑剂，通过Heinrich拉丝机拉制了231.8磅(105.4千克)0.0079英寸(0.0201厘米)的硬回火钽丝。拉丝速率为800英尺/分钟(243.8米/分钟)至1480英尺/分钟(451.1米/分钟)。每盘金属丝开始时的平均圆度为1英寸的百万分之12(30.5微米)，每盘结束时的平均圆度为1英寸的百万分之16(40.6微米)。每套模具平均生产46.4磅钽丝。
实施例4：
与实施例1相同，采用3M公司的FC-40全氟化碳液体作为润滑剂，通过Heinrich拉丝机拉制了49.4磅(22.5千克)0.0075英寸(0.0191厘米)的硬回火钽丝。拉丝速率为1480英尺/分钟(451.1米/分钟)至1600英尺/分钟(487.7米/分钟)。每盘金属丝开始时的平均圆度为1英寸的百万分之15(38.1微米)，每盘结束时的平均圆度为1英寸的百万分之17(43.2微米)。每套模具平均生产24.7磅钽丝。
实施例5：
与实施例1相同，采用3M公司的FC-40全氟化碳液体作为润滑剂，通过Heinrich拉丝机拉制了71.6磅(32.6千克)0.091英寸(0.0231厘米)的退火后的回火钽丝。拉丝速率为1200英尺/分钟(365.8米/分钟)。每盘金属丝开始和结束时的平均圆度为1英寸的百万分之20(50.8微米)。每套模具平均生产71.6磅钽丝。
实施例6：
除了在生产金属丝时对其进行的公称尺寸、目视的和机械特性的评价以外，采用扫描电子显微镜(SEM)评价了以全氟化碳润滑剂拉制的金属丝。
采用FC-40在200英尺/分钟(61米/分钟)、500英尺/分钟(152.4米/分钟)和1000英尺/分钟(304.8米/分钟)速率下，对电容器级钽丝拍摄的300X和1000X的扫描电子显微照片分别示于图1-3。300X的照片表明，随着拉丝速率的增高金属丝表面的质量实际上有所改进。总的说来，采用全氟化碳液体润滑剂拉制的金属丝表面上裂缝和缝隙的频度和深度随着拉丝速率的提高而递减。
实施例7：
采用CTFE润滑剂在200英尺/分钟(61米/分钟)下拉制的电容器级钽丝表面以1000X示于图4。该照片表明在采用常规氯三氟乙烯润滑剂拉制的钽丝上观察到的典型结构。可以看出，该金属丝显示出许多表面伤痕，特别是呈从该丝的表面撕开的较薄的小片状材料形式的伤痕。这似乎是一种机制，根据该机制观察到的大多数“细屑”是在拉细丝过程中产生的。采用全氟化碳液体润滑剂拉制金属丝时未观察到有细屑的事实表明，由于滞塞和卡住(由于润滑剂分解而造成的结果)而产生的这种小片状的表面伤痕已经被消除。
实施例8：
为了评价采用全氟化碳润滑剂生产的拉制后金属丝的总清洁度，将样品送去作微-FTIR红外分析。该3M FC-40润滑剂的参照谱图示于图8。取自采用全氟化碳润滑剂拉制的TPX 501G金属丝样品的二氯甲烷提取物的谱图以及FC-40的参照谱图示于图9。必须着重指出的是，在该金属丝上基本上没有发现任一种润滑剂的残余物，而且任何存在的残余物肯定不是FC-40。其总吸光度可与示于图10中的数据相比，该图示出了从用于除去CTFE润滑剂的超声波束清洗系统中清洗后的TPX 501G样品获得的提取物的FTIR谱图。在该装置中清洁了的金属丝的总吸光度通常约为0.1吸光度单位。一般而言，上述吸光度表示在该金属丝表面上的残余润滑剂小于一个单分子层。用全氟化碳拉制后的金属丝仅有小于20％的这种表面污染量，这确实是一种电子级洁净的材料。
图11所示为附加在金属丝生产过程的初期阶段使用的CTFE油和酯基线材轧制油的参照谱图上的清洗后的谱图。这两种材料基本上占我们未清洗的电容器级金属丝表面上发现的残余物的100％。未显示出有任何FC-40残余物存在。通过上述分析看来，似乎采用全氟化碳润滑剂拉制的金属丝在拉制后即可使用。随后的超声波清洗将仅仅起沾染金属丝表面的作用。
实施例9：
为了进一步用实验验证上述发现，将0.0079英寸(0.0201厘米)和0.0098英寸(0.0249厘米)直径的两种样品送去作来样的漏电测试。DC漏电可以通过将一定长度的导线阳极处理达到以氧化钽介电薄膜完全覆盖该表面进行测定。将阳极处理过的导线放置在电解质中，并在此钽导线体上施加DC电压。在固定的电压下测定通过所述介电薄膜“漏泄”的DC电流。上述漏泄电流是介电薄膜的完整性的量度。介电薄膜完整性本身又是整个导线表面的表面粗糙度和清洁度的量度。通过产生出无残余润滑剂的光滑表面，可以生产改进的介电薄膜，从而可改进导线的DC漏电特性。这些数据示于图12且表明拉制后的金属丝来样的漏电率在1-3μA/cm3范围内。与目前的生产相比它们当然是优越的，与工业上常见规格的最大值10μA/cm3相比它们更优越。
实施例10：
为了评价全氟化碳液体用于拉制铜丝作业中的效果，采用装有测量仪器的实验室拉丝机用FC40和粘度约为20厘沲的烃基拉制铜用油作为拉制润滑剂拉出直径为0.0120英寸的ETP铜丝。当将直径为0.0128英寸的铜丝通过末段模具拉制成直径为0.0120英寸的铜丝(缩减率为12.1％)时，测定其拉拔力。与采用烃基拉制铜用润滑剂时观察到的720克的力相比，当采用FC40时观察到的力仅为560克。
在放大倍数285X和4500X下拍摄的、用这两种润滑剂拉制的ETP铜丝的扫描电子显微镜图像示于图14。虽然用这两种润滑剂拉制的铜丝的表面在低放大倍数下是相似的，然而，高放大倍数的检查显示出，在烃基润滑剂拉制的样品上有许多反映出晶界分离的人字形裂纹，如果试图再拉拔，将会导致铜丝断裂。
实施例11：
用扫描电子显微镜检查了采用FC40和CTFE润滑剂拉拔的钽管表面。图15A示出了采用FC40拉拔的直径为0.250英寸、壁厚为0.010英寸的放大倍数为315X的管表面。图15B示出了采用CTFE油拉拔的直径为0.500英寸的放大倍数为319X的管表面。这些显微照片清楚地表明，采用CTFE油拉拔时，金属从该管的表面上大范围地损失。
为了量化这些管之间的表面粗糙度的差别，采用扫描探针显微镜检查了两种样品。图16A示出了采用FC40拉拔的平均表面粗糙度(Ra)为93.15nm的管表面的三维图像。图16B示出了采用CTFE油拉拔的平均表面粗糙度为294.92nm的管表面的三维图像。这些数据表明采用CTFE油拉拔的管表面粗糙度三倍于采用FC40全氟化碳液体拉拔的管表面粗糙度。
实施例12：
为了评价全氟化碳液体用于拉制不锈钢丝作业中的效果，从CarpenterTechnology得到直径为0.139英寸的302不锈钢丝，采用L13557全氟化碳液体作为润滑剂通过四次逐步缩减拉制成直径为0.0993英寸的丝。采用标准的拉制不锈钢的习惯做法，在不锈钢丝不退火且不用磷酸盐润滑剂载体再涂覆的情况下，只能经三次18％的缩减。
采用全氟化碳润滑剂拉制的0.0993英寸丝表面255X的SEM图像示于图17。该图像清楚地表明，四次18％的缩减后，在大部分不锈钢丝的表面上存在着磷酸盐润滑剂载体。
实施例13：
为了评价全氟化碳液体在钽的机械加工作业中的效果，将实验用的全氟胺液体代替通常用于生产4mm钽螺母的程序机械加工作业的CTFE油。这些螺母由冲了孔的坯料经过一系列包括钻孔、攻丝、车削和端面加工的机械加工作业进行生产。L13557的引入导致机械加工速率从每分钟表面切削200英尺达到每分钟表面切削＞850英尺，增加了4倍以上，与此同时工具的寿命至少增加10倍。当采用CTFE油时，每50-100个工件需要将端面车刀的刀头再磨锐。当使用L13557时，需要再磨锐工具的间隔大于2000个工件。还观察到用于钻孔和攻丝的工具寿命也有类似的增加。
一种4mm螺母断面的25X的SEM图像示于图18A。该图像示出了在最外螺纹表面以及削光面上所得的高质量的表面光洁度。始终如一地测得的平均表面光洁度(Ra)比32微英寸更好。该螺纹的31X的SEM图像示于图18B，该图示出了所得的极好螺纹形状且未显示出任何撕裂的迹象。一种采用L13557机械加工的4mm钽螺母表面25X和250X的SEM分裂图像示于图18C，该图表明在此放大倍数下完全没有通常在机械加工的钽螺母表面上会发现的撕裂和擦伤。
在使用3M公司的FC-40全氟化碳液体的实际生产试验中，观察到的最显著优点包括模具寿命增加5倍以上、拉丝速率增加10倍以上、电子级洁净的拉制后的金属丝以及每磅拉丝的润滑剂费用降低到五分之一。此外，已观察到产生的亚微细的钽微粒碎屑大量减少。当使用CTFE润滑剂时，在每生产班结束时都要更换拉丝机上的过滤器。当采用PFC液体时，这些过滤器每1-2个月才加以更换。同时，如13图所示，所用的PFC液体可以从拉丝机中收回并重复利用，从而降低操作费用，甚至对改善环境还可能有好处。
当拉拔任一种冶金的管材时，每道次(越过固定的圆柱形心棒)的最大理论缩减率可按下式计算： ( 1 ) q max = 1 - [ + 1 + 0.133 B ′ 1 + B ] - 1 / B ′
式中 B ′ = 2 f tan α 式中f对特定的润滑剂而言是模具与工件之间的摩擦系数，α为模具顶角的二分之一，在这种情况下该顶角保持恒定为12°
对通常的润滑剂而言，f通常在0.05-0.15之间变化。对PFC液体润滑剂而言，经计算f约为0.003-0.005。于是，
Figure C9619500400213
和 B ′ PFC = 2 ( 0.005 ) tan α = 0.095
因此，qmax(常规)＝35％，qmax(PFC)＝56％，与常规润滑剂相比，当采用PFC润滑剂时，每道次的最大理论缩减率可增加60％。
现在，可以明显地看出，其他实施方案、改进、细节和应用，对本领域的技术人员而言，可以在符合以上公开的内容和精神实质以及本申请的范围内作出，本专利仅受根据包括同等物原则的专利法解释的下述权利要求书限制。

Claims (26)

1.一种金属加工的方法，该方法包括在加工过程中采用氟化惰性液体润滑该金属，所述氟化惰性液体选自具有通式为CnF2n+2的全氟烷烃，其中n是一个5-18的数；具有通式CnF2n+1ON的全氟吗啉类，其中n是一个5-18的数，全氟环烷烃；和全氟胺类，其中所述氟化惰性液体能使金属加工过程相对于CTPE润滑在高速率下有效地进行，但是在该过程结束时没有除去氟化惰性润滑剂的润滑剂残余物的必要。
2.根据权利要求1的方法，其中所述氟化惰性液体是与选自润滑脂、糊剂、蜡和磨光剂的至少一种惰性载体一起提供的。
3.根据权利要求1的方法，其中该待加工的材料是难熔金属。
4.根据权利要求3的方法，其中该难熔金属是钽。
5.根据权利要求3的方法，其中该加工方法是采用复式模道的拉丝法，润滑剂液体是全氟化碳液体，拉制后的金属丝具有的平均直径为5密耳(0.127毫米)至20密耳(0.508毫米)。
6.根据权利要求1的方法，其中该氟化惰性液体化合物包括具有5-18个碳原子的氟化脂族化合物。
7.根据权利要求1的方法，其中该氟化惰性液体化合物包括至少一种链状杂原子，选自二价氧、六价硫或三价氮，且H∶F之比低于1∶1。
8.根据权利要求6的方法，其中该氟化惰性液体化合物具有的氢含量小于5％(重量)。
9.根据权利要求7的方法，其中该氟化惰性液体化合物具有的氢含量小于1％(重量)。
10.根据权利要求1的方法，其中该全氟烷烃液体选自全氟烷烃。
11.根据权利要求10的方法，其中全氟烷烃选自全氟戊烷、全氟己烷、全氟庚烷、全氟辛烷。
12.根据权利要求9的方法，其中该液体化合物是一种全氟胺。
13.根据权利要求12的方法，其中该全氟胺选自全氟三丁胺、全氟三乙胺、全氟三异丙胺和全氟三戊胺。
14.根据权利要求1的方法，其中该全氟烷烃液体是全氟吗啉。
15.根据权利要求14的方法，其中该全氟吗啉选自全氟-N-甲基吗啉、全氟-N-乙基吗啉和全氟-N-异丙基吗啉。
16.根据权利要求1-4中任一项的方法，其中将该金属拉制成细金属丝形式并作为导线与多孔的电极物质结合。
17.一种钽电解电容器阳极和所附的采用权利要求1的方法制成的导线。
18.根据权利要求1-4中任一项的方法，其中该金属加工方法是无缝金属管的轧制法，该方法包括以下一些步骤：将大直径的管材或棒材拉入具有至少一套轧缩辊的轧管机；在轧制过程中用选自具有通式为CnF2n+2的全氟化烷烃液体的液体润滑该材料；通过至少一套用全氟烷烃液体润滑的轧缩辊轧制该管材或棒材；重复这些过程直到获得所需的管尺寸为止。
19.根据权利要求18的方法，其中该管具有的平均直径为10mm-50mm，壁厚为0.5mm-10mm。
20.根据权利要求1-4中任一项的方法，其中该金属加工方法是采用复式模道拉制无缝金属管的方法，润滑剂是全氟烷烃液体，拉制后的管具有的平均直径为0.005英寸(0.127mm)-2.0英寸(50.8mm)且壁厚为0.001英寸-0.050英寸(0.025-1.27mm)。
21.一种提供润滑的方法，其中润滑剂是氟化惰性液体，该液体选自具有通式为CnF2n+2的脂族全氟化烷烃，具有通式为CnF2n+1ON的全氟吗啉类、全氟胺类和高度氟化的胺类；其中所述全氟胺类和高度氟化的胺类以取代的和未取代的形式出现，
22.根据权利要求21的方法，其中所述氟化惰性液体是与至少一种惰性载体选自润滑脂、糊剂、蜡和磨光剂的组合物一起提供的。
23.根据权利要求21或22的方法，其中该氟化惰性液体与一种固体润滑剂混合，并以糊剂、凝胶或其他固体形式提供。
24.根据权利要求23的方法，其中该固体润滑剂选自石墨、TEFLONTM、熔融的氟化物、MoS2、WS2、MoSe2、MoTe2和类似的固体润滑剂。
25.根据权利要求1-4中任一项的方法，其中该金属加工方法是采用所述惰性液体涂覆的金属颗粒的粉末冶金压制法。
26.根据权利要求1-4中任一项的方法，其中该金属加工方法是采用所述惰性液体和辅助润滑剂涂覆的金属颗粒的粉末冶金压制法。
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