CN1746328B - 复合材料 - Google Patents

复合材料 Download PDF

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CN1746328B
CN1746328B CN2005100991433A CN200510099143A CN1746328B CN 1746328 B CN1746328 B CN 1746328B CN 2005100991433 A CN2005100991433 A CN 2005100991433A CN 200510099143 A CN200510099143 A CN 200510099143A CN 1746328 B CN1746328 B CN 1746328B
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matrix material
copper
graphite
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carbide
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CN1746328A (zh
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B·舍德勒
Th·胡贝尔
Th·弗里德里克
D·舍德勒
A·察贝尼格
K·沙伊贝尔
H·D·弗里德尔
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Plansee SE
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Abstract

本发明涉及一种复合材料，其包括至少一个铜或铜合金区，至少一个以石墨为主的材料区和至少一个位于二者之间的连接区，其中该连接区包括一个或多个IVb、Vb、VIb族过渡金属的碳化物以及一个或多个由Si、B、Al、Ge、Mn、Sn组成的元素。优选其通过连铸的方法制造得到。

Description

复合材料
技术领域
本发明涉及一种复合材料，其包括至少一个铜或铜合金区，至少一个以石墨为主的材料区和至少一个位于二者之间的连接区，以及其制造方法。
背景技术
使用这种复合材料的一般例子是冷却设备，例如聚变反应堆的分流器和限流器。这种复合材料通常包括纯铜例如低氧铜(OFHC)区，和石墨例如碳纤维增强的石墨(CFC)区，它们整体上互相连接。正如在EP 0 663 670 B1中所描述，可以通过连铸(back-casting)来达到完整的结合。然而，还可以使用焊接或辅助压力连接技术(例如HIP)。界定铜区与石墨区的连接区域可以是平坦的或是弯曲的。平坦型的例子是扁砖分流器。弯曲的连接区域存在于例如管型分流器元件中。在此，石墨部分具有一个孔，其壁整体上与纯铜相连接，纯铜依次整体上与冷冻剂流过的铜合金(如Cu-Cr-Zr)管相连接。整体上与石墨材料相连接的纯铜具有确保驱热的功能。另外，当石墨通过纯铜中间层与高强度铜合金(如Cu-Cr-Zr)相连接时，它还具有应力消散的功能。除了石墨和一个或多个铜材料区以外，这种冷却设备还可以具有其它区，例如钢或钨合金(例如La2O3重量的W-1％)。
在所有情况下，石墨与铜之间的连接区是这种复合材料的弱点。生产具有改善该连接区强度的冷却设备的方法在EP 0 663 670 B1中有所描述。在此，使冷却设备的金属处于熔融状态与耐热材料部分接触，其中在连接过程中，使一定数量的一个或多个元素周期表的过渡族IV和/或V金属存在于连接区中。
用这种方法生产的复合材料，特别是CFC-铜复合物，具有明显改善的强度。对于经受高应力的复合材料，例如聚变反应堆的冷却元件，仍然还需要提高这种强度水平。
发明内容
因此本发明的目的在于提供一种具有改善强度的，尤其是在铜/石墨连接区中具有更高强度的复合材料，以及其生产方法。
根据本发明，这可以通过公开于权利要求1中的复合材料来实现。
本发明的复合材料包括一个铜或铜合金区，一个以石墨为主的材料区和一个位于二者之间的连接区。对于本发明的目的，连接区是铜/铜合金与石墨材料整体相连接的区。该连接区通过需要连接的材料的连接区域来结合，并且，除了这些连接区域，还包括加入到连接对之间的或在连接过程中形成的相成分。根据本发明的连接区包括一个或多个由IVb、Vb、VIb族过渡金属中的至少一个元素和一个或多个选自Si、B、Al、Ge、Sn、Mn的元素形成的碳化物或混合碳化物。Si、B、Al、Ge、Sn和Mn在其中的连接形式并不重要。因此，已经在本发明的复合材料中检测到以碳化物形式，作为金属间相，在该情况中仍旧优选与IVb、Vb、VIb过渡金属元素一起以元素形式和/或作为溶液存在的这些元素。
根据现有技术(EP 0 663 670 B1)，仅有很强碳化物形成元素，优选钛，可以加入到铜与石墨材料之间的连接区中。该方法也被称作活化作用。在连接过程中，例如在连铸过程中，邻接的碳化钛层形成于石墨材料上而且这对铜浸润性能有良好的作用。通过钛的活化作用使得碳化铜/钛界面中具有非常高的强度。然而，碳化钛经过而进入石墨材料的区域通常成为弱点。
现在已经惊奇地发现，用一个或多个IVb、Vb、VIb族过渡金属元素和一个或多个，由弱碳化物形成元素中的Si、B、Al、Ge、Sn、Mn、构成的元素所进行的活化作用来形成一个或多个由IVb、Vb、VIb族过渡金属元素的碳化物或混合碳化物，可能实现连接强度的明显增强，特别是在连接区中的切变强度，该切变强度主要由碳化钛经过并进入石墨材料区的强度来决定。Si、B、Al、Ge、Sn和/或Mn碳化物的相区和/或上述提到的形成碳化物的元素的金属间相以岛状存在是有利的。特别有利地，强碳化物形成元素包括Y、Ti、V和Mo，而使用Ti可以获得最好的结果。基本上，应该提到，强和弱碳化物形成元素在连接区中也可以以元素形式存在。另外，它们可以存在于石墨材料(例如作为碳化物)中和存在于铜/铜合金(例如作为溶液或作为沉淀物)中，其在各自的连接区中以较高浓度存在是有利的。通过用存在于连接区域中的TiC、Ti5Si3和SiC来进行的Ti和Si活化作用可以获得最好的结果。这种情况下，连接区中的切变强度要比CFC中的大。由于碳纤维增强的石墨(CFC)以及纯铜例如低氧铜(OFHC)的高热传导性，该材料对尤其适合于生产本发明的复合材料。在这种情况下的CFC也可以含有SiC部分或其它具有良好热传导性的相成分。以石墨为主的材料和铜/铜合金之间的连接强度可以通过以石墨为主的材料的结构来改进。该结构可以通过例如用激光产生空穴的方法来获得。
生产本发明复合材料的一个特别有用的方法是连铸。在连铸方法中，使熔融状态的铜/铜合金与石墨接触。该过程在由耐热材料制成的模型中实现，且该模型的负轮廓大致与复合材料的正轮廓相对应。
IVb、Vb、VIb族过渡金属元素，Si、B、Al、Ge、Sn和Mn能够通过例如将一个或两个连接对进行涂覆或者通过在连接对之间放置一个或更多金属薄片的方法来加入。合适的涂覆方法是例如电解方法以及化学气相淀积(CVD)和物理气相淀积(PVD)方法。IVb、Vb、VIb族过渡金属元素，Si、B、Al、Ge、Sn和Mn优选以元素的形式存在于涂覆层中或金属薄片中。在IVb、Vb、VIb族过渡金属元素与Si、B、Al、Ge、Sn、Mn之间，会出现与固体和液体温度的降低有关的恒定转换，这使得浸润性能得到了改善。
然而，这些元素理论上可以以另一种形式存在，例如作为化合物或合金。然而，IVb、Vb、VIb族过渡金属化合物的生成能必须小于其各碳化物的生成能。
如果通过涂覆的方法来加入，将有利于该涂覆层被淀积在石墨部分上。这确保形成碳化物的元素与碳源即石墨之间的密切接触。已经发现，涂覆层/金属薄片的合适厚度为10至50μm。在分离过程步骤中，形成碳化物的元素也可以被熔融或部分转化成碳化物。有利的是由Si、B、Al、Ge、Sn、Mn组成的元素的比例基于IVb、Vb、VIb族过渡金属元素的比例来进行选择而使得由此形成的合金包括共晶相部分。
另外，已经发现，有利的是一个或多个由Si，B，Al，Ge，Sn，Mn组成的弱碳化物形成元素以元素形式淀积在石墨部分上或以元素金属薄片用于石墨部分。在下一个步骤中，将石墨部分和涂覆层/金属薄片加热到高于弱碳化物形成元素熔点的温度。当合金层或合金金属薄片存在时，将石墨部分和涂覆层/金属薄片加热到至少大于固态点的温度。当使用包括例如两个或多个形成碳化物的元素的合金时，使用具有共晶微结构成分的合金有利。共晶或近共晶合金特别有利。
如果使用多于一个形成碳化物的元素，该过程也可以以多个阶段来实现。
可以通过用Si或Ge来涂覆石墨材料的方法来实现石墨与铜/铜合金之间特别高强度的连接，该方法的涂覆表面具有表面结构。用Si进行涂覆可以通过例如向石墨部分应用含硅浆料来实现。然后将用这种涂覆方法得到的部分在保护气体下或在减压下加热到高于Si的熔点的温度。强碳化物形成元素，优选Ti，以例如金属薄片的形式运用到以这种方法生产的部分中。优选Si的比例和Ti的比例以使其在反应时形成共晶微结构成分。在下一个步骤中，Ti金属薄片在保护气体下或在减压下熔融。然而，Si和Ti的熔融还可以在一个工艺步骤中实现。在这种情况下，温度必须至少在各合金的固态点温度之上。
然后熔融物渗入石墨结构表面的微孔中或大孔中。这使得Ti与石墨部分的C进行部分反应形成TiC。作为更弱碳化物形成元素Si，仅与少量C反应以及与Ti一起形成金属间相Ti5Si3。另外，可以检测到小部分SiO2，这可能是由于吸收的氧或该工艺环境中的少量O而生成。将用这种方法进行预处理过的石墨部分放在由耐热材料制成的模型中，并且用所需用量的铜或铜合金将其处理过的表面进行覆盖。然后将全部复合物加热直到铜/铜合金液化。存在的金属Ti在短时间内溶解在铜熔融物中。在铜或铜合金固化后，可以使铜和铜合金与石墨部分之间的连接较强且较紧密，并且在连接区域区Ti富集在Cu中。
本发明的复合材料有利于用作冷却元件并且在这种情况下优选作为聚变反应堆中的分流器和限流器
具体实施方式
下面将借助如下的实施例来对本发明进行说明。
为制作根据本发明的复合材料，将具有200×100×50 mm3尺寸的碳纤维增强的石墨(CFC)的棱柱部分在200×100 mm2侧面上引入与该表面垂直的空穴的方法来进行结构化，并且通过激光方法测量其直径约为100μm。在清洁石墨部分之后，依赖于所进行的实验，将已经分散各种弱碳化物形成元素的浆料应用到由这种方法结构化的表面上。所使用的量以其理论上与各元素覆盖6μm厚度相对应来进行计算。所用的元素如表1所示。在减压下，将这种方法处理的部分在高于各弱碳化物形成元素的液态点温度40℃的温度下加热60分钟。在下一个步骤中，依赖于所进行的实验，用20 μm厚的钛或钒金属薄片覆盖处理过的表面并且再次将该部分在减压下加热到1720℃(Ti)或1950℃(V)温度。在该温度下保持60分钟。冷却至室温后，将用超声清洁处理的具有200×100×50mm3尺寸的铜块放在钛或钒覆盖的区上并且将该层叠物加到一个长度和宽度实质上与该材料层叠物的长度(200mm)和宽度(100mm)相一致的石墨模型中。然后该材料层叠物在诱导加热炉中加热到1150℃。在以这种方法生产的复合材料移出加热炉之后，让其经受切变测试。作为比较，现有技术复合材料在除了没有加入弱碳化物形成元素而其它过程顺序相同的情况下进行生产。在切变测试中，与现有技术(实施例1-2)相比较，根据本发明生产的复合材料(实施例3-8)显示出具有明显改善的切变强度。
表1
  实验号   实验中生产的部分   弱碳化物形成元素   强碳化物形成元素   切变强度[MPa]
  1   现有技术   Ti   33
  2   现有技术   V   25
  3   根据本发明   Si   Ti   67
  4   根据本发明   Ge   Ti   70
  5   根据本发明   Al   Ti   49
  6   根据本发明   Si   V   54
  7   根据本发明   Ge   V   54
  8   根据本发明   Al   V   44

Claims (24)

1.一种复合材料，包括：至少一个铜或铜合金区，至少一个以石墨为主的材料区和至少一个位于二者之间的连接区，其特征在于，所述的连接区包括一个或多个由Si、B、Al、Ge、Sn、Mn组成的元素的碳化物或混合碳化物以及一个或多个IVb、Vb、VIb族过渡金属元素的至少一种碳化物，所述的至少一种碳化物在连接区中并不形成邻接层而为岛状。
2.如权利要求1所述的复合材料，其特征在于，所述的连接区包括至少一个元素Ti、V和/或Mo的碳化物或混合碳化物。
3.如权利要求1所述的复合材料，其特征在于，将IVb、Vb、VIb族过渡金属元素、Si、B、Al、Ge、Sn、Mn中的至少一种元素溶解在铜或铜合金中。
4.如权利要求3所述的复合材料，其特征在于，所述的IVb、Vb、VIb族过渡金属元素、Si、B、Al、Ge、Sn、Mn中的至少一种元素是富集在铜连接区中。
5.如权利要求1所述的复合材料，其特征在于，所述的连接区包括碳化钛。
6.如权利要求1所述的复合材料，其特征在于，所述的连接区包括Si和/或Ge。
7.如权利要求1所述的复合材料，其特征在于，所述的连接区包括碳化钛和碳化硅。
8.如权利要求1所述的复合材料，其特征在于，所述的连接区包括元素形式的IVb、Vb、VIb族过渡金属元素、Si、B、Al、Ge、Sn、Mn中的一个或多个元素。
9.如权利要求1所述的复合材料，其特征在于，所述的连接区包括一个或多个Si、B、Al、Ge、Sn、Mn与一个或多个IVb、Vb、VIb族过渡金属元素形成的至少一个金属间相。
10.如权利要求1所述的复合材料，其特征在于，所述的IVb、Vb、VIb族过渡金属元素、Si、B、Al、Ge、Sn、Mn中的一个或多个元素存在于以石墨为主的材料区中。
11.如权利要求1所述的复合材料，其特征在于，所述的连接区的厚度为0.05至30μm。
12.如权利要求1所述的复合材料，其特征在于，所述的以石墨为主的材料区包括碳纤维增强的石墨。
13.如权利要求1所述的复合材料，其特征在于，所述的以石墨为主的材料区通过其连接区上的空穴来进行结构化。
14.如权利要求1所述的复合材料，其特征在于，所述的铜或铜合金区包括低氧铜。
15.如权利要求1所述的复合材料用作冷却元件的用途。
16.如权利要求15所述的复合材料用作第一壁元件的用途。
17.如权利要求16所述的复合材料用作第一壁元件的用途，其特征在于，所述的第一壁元件是聚变反应堆中的分流器和限流器。
18.一种生产复合材料的方法，包括：将铜加热到高于其熔点的温度或将铜合金加热到高于其固态点温度的温度，且使其与以石墨为主的材料接触，其中，在连接过程中，使一个或多个由Si、B、Al、Ge、Sn、Mn组成的元素的量和一个或多个IVb、Vb、VIb族过渡金属元素的量存在于连接区中，然后通过冷却将铜或铜合金进行固化。
19.如权利要求18所述的生产复合材料的方法，其特征在于，所述的一个或多个由Si、B、Al、Ge、Sn、Mn组成的元素的量基于一个或多个IVb、Vb、VIb族过渡金属元素的量进行选择，以使得由此形成的合金包括共晶相部分。
20.如权利要求18或19所述的生产复合材料的方法，其特征在于，所述的铜合金加热到高于其液态点温度的温度。
21.如权利要求18或19所述的生产复合材料的方法，其特征在于，所述的一个或多个由Si、B、Al、Ge、Sn、Mn组成的元素以元素的形式、作为化合物和/或作为合金应用到以石墨为主的材料中，用这种方法处理的该以石墨为主的材料加热到高于该元素或化合物或合金固态点温度的温度，以产生以石墨为主的材料的局部浸润；然后一个或多个IVb、Vb、VIb族过渡金属元素的一个或多个金属薄片应用到以石墨为主的材料中，并且与处理过的以石墨为主的材料一起加热到形成碳化物的温度，再由耐热材料制成的模型中用铜或铜合金覆盖该处理过的以石墨为主的材料表面，并且将全部复合物加热到高于铜或铜合金液态点温度的温度。
22.如权利要求18或19所述的生产复合材料的方法，其特征在于，所述的复合材料用作冷却元件。
23.如权利要求22所述的生产复合材料的方法，其特征在于，所述的复合材料用作第一壁元件。
24.如权利要求23所述的生产复合材料的方法，其特征在于，所述第一壁元件是聚变反应堆中的分流器和限流器。
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KR101200578B1 (ko) 2012-11-12
US20060052249A1 (en) 2006-03-09
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ATE445582T1 (de) 2009-10-15
US8557383B2 (en) 2013-10-15
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