CN102815970A - 多孔制品致密化的方法 - Google Patents
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Abstract
一种多孔制品致密化的方法,特别是一种使用液体前驱体致密化诸如制动器预制件的多孔基材的方法,其中通过将用于致密化的液体前驱体维持在比纯净差些但是对于获得所需的致密化产品仍在化学上合适的纯度级别,减少了消耗“新鲜”或“新”液体前驱体的速率。
Description
本申请是申请号为200780037156.5,申请日为2007年8月7日,发明名称为“多孔制品致密化的方法”的中国专利申请的分案申请。
相关申请的交叉引用:
本申请要求2006年8月7日提交的美国临时申请No.60/821,596的优先权,在此引入其全部内容作为参考。
技术领域
本发明涉及对具有合意高生产率的多孔制品进行致密化的方法和装置,特别地但不一定唯一地,关于摩擦制动制品的领域,例如飞行器制动器。
背景技术
在摩擦材料领域,通常已知的是使用多孔材料制造摩擦构件,例如摩擦制动盘。
这种摩擦构件的制造通常以多孔预制件的构造作为开始。例如,在许多摩擦制动器应用中使用环状预制件。
可以使用若干不同的已知方法构造环状预制件。例如,碳纤维织物层能够缝合在一起,环状预制件能够从堆叠材料中切割下来。
而且,例如通过织造碳纤维或者通过将碳纤维编织成所需的形状可以形成近乎网形状的预制件。已知某些碳纤维织物具有便于以螺旋形式布置织物的织纹。在上下文中,“近乎网”是指形成具有与最终制品(例如环状制动盘)所需形状接近的形式的结构。
氧化聚丙烯腈(“PAN”)纤维或沥青基纤维是在这类应用中所用原料纤维的常见实例。接着,可以在高温处理步骤中碳化这些纤维。在另一常规方法中,使用树脂或沥青形成原料纤维,随后用诸如氮气的反应性气体固化所得的物质。接着碳化由此固化的物质从而获得半刚性预制件。
无论如何,期望进一步致密化所得的多孔预制件(特别是但不必只是具有含碳材料的多孔预制件),从而获得合意的摩擦和机械性质。
因此,化学气相渗透(“CVI”)是为获得碳/碳复合材料而广泛使用的常规技术。CVI使用含碳氢化合物气体渗入多孔预制件。CVI气体随后在高温下裂化从而将碳涂层留在预制件的纤维结构上。
常规的CVI通常需要数百个小时的处理,以便得到具有合意密度和机械性质的碳/碳(“C/C”)结构。举例而言,通常常规的CVI工艺包括进行例如大约300-500小时或更长的第一渗透周期。
然而,常规的CVI在预制件的内部部分被充分致密化之前,经常造成预制件的表面多孔结构的快速阻塞。为了“重新打开”表面多孔结构以允许进一步的致密化,有必要进行中间机械加工步骤。总体而言,这种中间机械加工(利用已知的方法,例如铣削)去除了具有碳阻塞孔的预制件的表面层,以暴露出预制件的开放孔,使得碳氢化合物气体能够再次渗入预制件结构。考虑到在典型的致密化工艺中数百个预制件被致密化,中间机械加工步骤使得整个常规CVI致密化工艺增加了多达48小时。
一旦完成了部分致密化制品的中间机械加工,就进行次级CVI工艺,以利用预制件重新打开的表面多孔结构。这种次级CVI工艺步骤能够持续例如另外的300-500小时或更长。其通常利用CVI完成常规的致密化工艺。
致密化多孔预制件的另一种方法使用液体而不是气态碳氢化合物前驱体。这种致密化方法在本领域中有时称为“膜状沸腾(film boiling)”或“快速致密化”。
膜状沸腾致密化通常包括将多孔预制件浸入液体碳氢化合物中,使得液体基本上完全渗入预制件的孔和空隙。其后,通过适当放置的诸如感应线圈的电气元件将浸入的预制件感应加热至液体碳氢化合物的分解温度以上的温度(通常为1000℃或更高)。更特别地,邻近感应加热的预制件结构的液体碳氢化合物在预制件多孔结构内离解为多种气相种类(species)。气相种类进一步的热分解导致在多孔材料的开放区域中在内表面上形成热解碳。例如,在美国专利No.4 472 454、No.5 389 152、No.5 397 595、No.5 733 611、No.5 547 717、No.5 981002和No.6 726 962中讨论了用于致密化的液体前驱体的使用。这些文件的各个文件以及每个文件都全部合并于此作为参考。
感应加热的概念在本领域通常是已知的,包括如前述参考文件中所述。然而,将预制件加热至高温(至少1000℃和高至1400℃)并将其完全浸入高挥发性碳氢化合物液体(例如,诸如环己烷)中引发非常重要的安全问题。
发明内容
本发明涉及使用液体前驱体致密化多孔基材的方法,其中通过将用于致密化的液体前驱体维持在比纯净差些但是对于致密化工艺仍在化学上合适的纯度级别,有利地减少了所用“新”或“新鲜”液体前驱体的体积。在效果上,本发明使用人工“老化”(就其中存在的杂质而言)的液体前驱体。
附图说明
参照附图将更清楚地理解本发明,其中:
图1是根据本发明所述使用液体前驱体进行致密化的装置的示意性代表图;
图2和图3是根据本发明所述用于致密化多孔制品的反应室的部分剖面侧视图和俯视图;
图4显示了致密化运行周期与以主要前驱体组分的浓度量化的液体前驱体纯度之间的实验导出关系;
图5显示了在数个循环中液体前驱体中的杂质水平的实验所得进展;
图6显示了在数个其中前驱体纯度被周期恢复的循环中的计算数据与实验数据的关系;以及
图7和8显示了在数个其中前驱体纯度被部分周期恢复的循环中的计算数据与实验数据的关系。
具体实施方式
通过举例说明的方式参照附图显示了本发明的方法和装置的特征和细节,但其并不作为本发明的限制。
仅仅通过实施例和/或图示,在下文提到了多孔预制件,例如用于制造摩擦制动盘的预制件。但是,需清楚地注意到,本发明一般更适用于以所述方式致密化其它类型的多孔基材。
在图1中显示了利用液体前驱体进行致密化的装置的高度示意性代表图。该系统包括远程液体前驱体存储场所100(包括例如液体传送系统)以管理新的和使用过的前驱体液体的传送。根据本系统使用的前驱体液体的一个实例是液体碳氢化合物,例如环己烷(C6H12).例如,可以提供用于液体前驱体的一个或多个远程存储罐的罐“场(farm)”(以100集中表示)。该罐场还可以包括一个或多个用于至少初始存储使用过的液体前驱体的罐。出于安全原因,期望或者甚至是需要(其取决于可应用的工业要求)至少使罐场100离其余装置有一定的距离。例如某些地方和/或国家条例要求离开数百英尺的量级。
如果需要的话,该装置可以任选包括相对较小的本地存储罐105以使相对少量的新前驱体液体靠近处理装备。
用于使装置的各部分互相连接的管道系统(包括泵及类似物)是常规的,其可以是适合所用液体前驱体(特别是但不必只是液体碳氢化合物)传送的任何构造和布置。液体传送系统优选但不必须是计算机控制的系统。可市购的计算机控制系统(例如但不限于可自OPTO 22公司市购的那些)可以是用于监测和控制这种液体传送的系统,包括从外部供应者装载新液体前驱体。
将液体前驱体从本地前驱体存储罐105供给一个或多个反应室(以110集中表示)。优选地,提供足量液体前驱体以将进行致密化的一个或多个预制件以及与其相连的感应加热线圈基本浸没在其中。
如前所述,膜状沸腾工艺产生部分引起热解碳形成在预制件多孔结构内表面上的气体种类。为了工艺中可能的再循环,尽可能地俘获前驱体蒸汽,并使其在常规冷凝器单元115中凝结。可利用商用冷却塔140以维持用于冷却冷凝器单元115的合适水温。
优选将仍剩余的废气传送至构造已知的热氧化器120从而燃尽废气中的残余碳氢化合物。
通过金属总线汇流条(bus bar)30将获自电源125的功率传送至感应线圈25,所述总线汇流条根据装置中元件的给定布置并根据合适的所需尺寸考虑构造。总线汇流条可以由例如铜制得,且优选但不必须地通过水冷网络50进行水冷。(参见图2。)
每个电源125都可以具有远程PID回路控制能力,并且能够由计算机控制终端监测和控制。通过已知方法的致密化工艺的功率密度控制、电压控制、电流控制、频率控制和/或温度控制也在预期布置的范围内。
图2显示了为在其中处理两个(例如)多孔预制件而构造和布置的反应室110。反应室110具有两个对应于待处理的每个预制件35的感应加热线圈组件25。优选地,使用非反应性热稳定支架将感应线圈组件25安装到位,所述支架由能承受例如液体碳氢化合物环境的诸如电非导电玻璃复合材料45(例如在本领域中已知的“G-10”)制成。感应加热线圈25优选为水冷扁平螺旋线圈,并且可以由铜金属制成。因此,需要提供专用于感应线圈25的水冷系统的热交换器135(参见图1)。使用时,通过直接与感应线圈25耦合加热正在被致密化的预制件(或者磨损的制动器)35。
在装载和卸载线圈/反应器室110的一个实例中,顶部盖板15具有用于密封室110的常规锁定机构。向每个反应器室110(与所提供的一样多)具有常用液体前驱体供给线路连接20和可操作地连接至冷凝器115和热氧化器120的常用排气线路10。
每个反应器室110可通过计算机控制系统进行所需的填充、排放和监测。冷凝来自致密化工艺的排放液体前驱体蒸汽并将其反馈至反应器室110,接着将残余的废气送至热氧化器120并进行燃烧。
因为挥发性液体碳氢化合物是在本发明中使用的液体前驱体的特定例子,所以需要(但不是必须的)提供氮气(N2)供给系统(未示出)用以例如冲洗管路系统并通常用惰性气体(代替含氧空气)填充系统中的空隙从而降低燃烧的危险。在特定的实例中,将在远程和本地液体前驱体存储罐中的空间维持在氮气(或其它常规已知的惰性气体)的轻微的、连续提供的超压下,从而阻止挥发性蒸汽的潜在危险积聚。将与排出的氮气混合的碳氢化合物种类送至热氧化器120使得在气体排出至外部之前能够燃尽碳氢化合物。
而且,由于系统使用了“湿”法,因此有用的是在系统中提供干燥炉130从而在致密化后干燥致密化的预制件。还优选将来自这样的干燥炉130的废气连接至热氧化器120以处理在所得废气中夹带的重芳烃和轻芳烃。出于安全考虑,使用在其中发生爆炸的情况下在结构上能够抵抗故障(倘若在干燥过程中在炉中存在挥发性气体)的炉结构是有用的。干燥工艺可以是例如计算机控制的从而简化工艺控制。
表1
表1提供了对在致密化工艺中产生的老化的C6H12和主要杂质的分析。在该研究中,采用专用功率曲线在三个反应器中对碳化预制件进行了八个致密化循环。特别地,目标是减少新或“新鲜”液体前驱体(其是相对昂贵的)的用量从而补充在生产过程中正在使用的前驱体。
收集获自八个连续运行的十六个老化的C6H12样品并送去分析。目标是将各污染物峰值关联至老化的C6H12。在每个致密化循环之前和之后收集样品并标记为A和B。
在第八个循环结束时的C6H12%浓度仍高于94%。所得主要杂质峰是苯、萘、甲苯、苯乙烯、环己烯、环戊二烯和茚。七个测定杂质中的六个杂质在整个八个循环中遵循了稳定、大体上增加的趋势。对老化研究进行的气相色谱(GC)分析表明,所有主要杂质和环己烷浓度是非常可预测的。所有杂质峰从一个循环至下一循环是一致重复的。
通过用各种杂质掺杂液体前驱体模拟老化的液体前驱体也是预期的。通过这种方式,有可能有益地延续液体前驱体的可用寿命和/或减少对高纯(因此相对昂贵)液体前驱体的需求。换句话说,一方面,可以确定前驱体纯度的“最小”级别,使得可以以高于该最小值的纯度级别使用前驱体(在用高纯前驱体取代之前)。另一方面,可以确定前驱体的可接受的较低纯度级别从而使得预期的致密化工艺在正在进行的基础上能使用该较低纯度前驱体。不管怎样,高纯度前驱体液体的用量得以合意地降低。
通过用各种前述杂质掺杂液体前驱体来模拟老化的液体前驱体从而接近在数个工艺循环后高纯液体前驱体的逐渐“退化”。开发模型以预测在各个循环中的环己烷浓度。基于由前述的八个连续运行获得的实验数据进行外推。图4显示了预测的环己烷浓度与连续工艺运行次数的关系。值得注意的是,计算的环己烷浓度在大约40次运行后基本达到了稳定状态,这主要是因为在致密化循环之前向处理罐中加入了新环己烷。
500加仑批料计算
注:混合物的计算密度为:0.790克/立方厘米。允许的罐容量为480加仑480加仑批料重量:0.790×480×3.785=1435(千克)
表2
自Alfa Aesar购买九种化学品以掺杂环己烷前驱体。表2提供了用于掺杂的有关化学品的信息。购买的化学品的纯度在从99.6%至80%的范围内。
表2提供了单个化学品的用量以获得90%的环己烷浓度。对于初始混合物使用90%环己烷浓度以模拟模型,尽管出于安全原因在混合物中不使用环戊二烯,因为该凝胶状材料在空气中极易燃烧。但是相信对测试的影响是很小的。使用初始90%混合物进行六个连续致密化循环。在每个循环之前和之后收集液体前驱体的样品并送去GC分析。
500加仑批料计算与GC测定的关系
表3
将获自六个连续循环的总共十二个老化的前驱体送至实验室进行气相色谱分析。在致密化循环之前和之后从500加仑罐中收集老化的前驱体样品。表3提供了模拟的90%混合物前驱体的GC分析。从表3中可以观察到,除了环戊二烯(由于其在空气中具有高易燃性而实际上并未使用)外,所有化学品报告的浓度紧密跟随了在90%混合物中所用的质量%。但是,相信在实际样品中去掉环戊二烯对测试的综合影响很小。
掺杂研究-六次连续运行
表4
表4显示了来自六次连续循环的主要污染物或者十二个前驱体样品的进展。在六次致密化循环后,纯度通常以90.3%开始,以88.4%结束。在多数情况下,除了苯外,污染物到达稳定状态或者缓慢下降。(参见,例如在表4中的环戊二烯、环己烯、甲苯、乙基苯、苯乙炔、苯乙烯、茚、萘、甲基萘、苊和芴。)这表明从环己烷(C6H12)至苯(C6H6)化学损坏的连续(continuation of chemical breakdown)很可能在较低C6H12浓度水平下继续。(参见,例如在图5中的苯浓度。)
实践中,可使用数个方法管理前驱体。下文描述了其中的一些方法。
可以使用相同的液体前驱体浴(bath)运行数个连续的循环,随后周期性地用新环己烷取代整个存储罐。以那种方式,环己烷浓度在新鲜环己烷浓度至低浓度之间变化,这取决于连续循环运行的次数。图6显示了每8个循环对存储罐进行排放的情况。
另一管理前驱体的方法是周期性取代存储罐中仅部分液体前驱体。该方法减小了浓度的变化,因此能更好地控制从该前驱体沉积的热解碳(微观结构、热-机械或摩擦性质)。有关于此,图7显示了在理论上环己烷浓度如何受到每4次运行后以新鲜环己烷取代半个存储罐的影响。
根据这两个方法,存储罐不再完全排放。根据分别对应于图6和7中的方法进行多次运行,通过气相色谱法分析使用过的环己烷样品。
表5a和5b分别提供了这些分析的结果。
表5A
表5B
实验数据证实了该计算是预测环己烷浓度与运行次数的关系的准确方法(参见图8)。值得注意的是图7和8还显示了8次循环实验数据,其进一步证实了就其综合曲率而言预期的环己烷降解速率。
而且,分析显示每个化学成分的浓度在数次运行后基本保持稳定。
尽管为了举例说明和解释本发明的目的而在上文参考某些特别实例描述了本发明,但应该理解本发明不仅仅通过参考而限于这些实例的特定细节。更具体而言,本领域技术人员将容易理解可以对优选的具体实施方案进行改变与展开而不脱离如所附权利要求书中所定义的本发明的范围。
Claims (17)
1.一种多孔制品致密化的方法,该方法包括:
在反应室内,将多孔基材浸没在液体前驱体中使得液体前驱体渗入多孔基材的孔中;以及
感应加热浸没的多孔基材至足以引起液体前驱体热解并在基材孔内沉积分解产物的温度,以致密化多孔基材,
其中,将液体前驱体的化学纯度级别控制在比化学纯低但足以获得具有所需物理特性的分解产物的化学纯度。
2.根据权利要求1所述的多孔制品致密化的方法,其中所述液体前驱体包括碳氢化合物。
3.根据权利要求1所述的多孔制品致密化的方法,其中所述分解产物包括碳。
4.根据权利要求2所述的多孔制品致密化的方法,其中所述碳氢化合物从由以下物质组成的组中选择:环戊烷、环己烯、1-己烯、汽油、甲苯、甲基环己烷、正己烷、煤油、加氢脱硫煤油、苯及其组合。
5.根据权利要求1所述的多孔制品致密化的方法,其中将液体前驱体的化学纯度级别控制在大约80%至大约99.9%之间。
6.根据权利要求5所述的多孔制品致密化的方法,其中在液体前驱体中存在杂质,且所述杂质包括环戊二烯、己烷、甲基环戊烷、苯、环己烯、庚烷、甲基环己烷、甲苯、乙基苯、苯乙炔、苯乙烯、壬烷、茚、萘、甲基萘、苊和氟中的一种或多种。
7.根据权利要求1-6所述的多孔制品致密化的方法,其中使用在线蒸馏工艺控制液体前驱体的化学纯度。
8.根据权利要求7所述的多孔制品致密化的方法,其中将液体前驱体的化学纯度控制在大约95%±5%的范围内。
9.根据权利要求7所述的多孔制品致密化的方法,其中通过混合一定量的化学纯液体前驱体和一定量的老化的液体前驱体来将液体前驱体的化学纯度控制在大约90%±5%的范围内,所述一定量的老化的液体前驱体包含反映在一个或多个在先致密化循环中的使用的一种或多种杂质。
10.根据权利要求1所述的多孔制品致密化的方法,其中所述液体前驱体包含有机硅烷。
11.根据权利要求10所述的多孔制品致密化的方法,其中有机硅烷从由以下物质组成的组中选择:甲基三氯硅烷、二甲基二氯硅烷、甲基二氯硅烷或三正甲基氨基硅烷。
12.根据权利要求10所述的多孔制品致密化的方法,其中所述分解产物包括碳化硅和氮化硅。
13.根据权利要求1所述的多孔制品致密化的方法,其中所述液体前驱体是有机硅烷和碳氢化合物的混合物。
14.根据权利要求12所述的多孔制品致密化的方法,其中所述分解产物是碳/碳化硅或碳/氮化硅之一。
15.一种利用液体基质前驱体致密化多孔预制件的反应器,包括:
反应室;
至少一个置于反应室中的感应线圈加热组件;
用于监测液体前驱体消耗的液位指示器;
在致密化工艺中加入液体前驱体的装置;
用惰性气体清洗反应室的装置;
与反应室相连,被构造和布置用于冷凝反应室中的前驱体蒸汽,并将冷凝的前驱体返回至反应器容器的蒸汽回收系统;
将蒸汽回收系统和清洗装置连接至热氧化器的排气系统;以及
在致密化工艺中,用于将反应器压力维持在大约760Torr至大约780Torr之间的加压装置。
16.根据权利要求1所述的多孔制品致密化的方法,其中感应加热浸没的多孔基材包括:
设置感应加热的初始频率和功率电平,该初始频率和功率电平对于在多孔基材的几何中心区域,并优先在位于多孔基材的几何中心区域的孔中积聚足够的热量以引起液体前驱体蒸汽的热解是有效的;
提供在初始频率下用于感应加热的初始功率电平,从而足以致密化多孔基材的几何中心区域,但同时不致密化多孔基材的其它部分;
在致密化多孔基材的几何中心区域之后,进一步调整提供的功率电平和频率从而在自多孔基材的几何中心区域向外的径向方向上逐渐致密化多孔基材的内部区域;以及
在致密化工艺的最后将功率电平斜线降低至零。
17.根据权利要求1所述的多孔制品致密化的方法,该方法进一步包括在致密化后进行热处理,所述热处理包括:
从反应室中完全排出液体前驱体;
用惰性气体清洗反应室;
在惰性气体氛围中在大约1600℃至大约2400℃之间的温度下并维持压力在大约760Torr至大约780Torr,感应加热致密化的多孔基材;以及
将感应加热斜线降至零以结束热处理。
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