CN103582621B - 碳化硅－碳复合材料的制造方法 - Google Patents

碳化硅－碳复合材料的制造方法 Download PDF

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CN103582621B
CN103582621B CN201280025810.1A CN201280025810A CN103582621B CN 103582621 B CN103582621 B CN 103582621B CN 201280025810 A CN201280025810 A CN 201280025810A CN 103582621 B CN103582621 B CN 103582621B
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silicon carbide
carbonaceous material
silicon
carbon composite
carbide
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CN103582621A (zh
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陈卫武
宫本钦生
东城哲朗
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Toyo Tanso Co Ltd
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Toyo Tanso Co Ltd
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Abstract

本发明提供一种新的碳化硅－碳复合材料的制造方法。通过对包含表面附着有氮化硅的碳质材料（2）的成型体进行烧制，制造碳化硅－碳复合材料（1）。

Description

碳化硅－碳复合材料的制造方法
技术领域
本发明涉及碳化硅－碳复合材料的制造方法。
背景技术
一直以来，已知有将石墨等碳与碳化硅复合化而得到的碳化硅－碳复合材料。例如，在专利文献1中公开了使碳基材与SiO2气体反应，制造被碳化硅覆盖的碳基材的方法。并且，在专利文献2中公开了将碳与碳化硅混合后进行烧制，制造碳化硅与碳的复合材料的方法。
在先技术文献
专利文献
专利文献1：日本特开2011－51866号公报
专利文献2：日本特开2011－51867号公报
发明内容
发明要解决的技术问题
需求碳化硅－碳复合材料的更有效的制造方法。
本发明是鉴于这一点而完成的，其目的在于提供一种新的碳化硅－碳复合材料的制造方法。
用于解决技术问题的手段
本发明的碳化硅－碳复合材料的制造方法具备对含有氮化硅和碳质材料的成型体进行烧制的工序。优选在碳质材料的表面附着有氮化硅。
在本发明的碳化硅－碳复合材料的制造方法中，优选将氮化硅、碳质材料和粘合剂混合，得到含有表面附着有氮化硅的碳质材料的混合物，对混合物进行成型，得到成型体。
在本发明的碳化硅－碳复合材料的制造方法中，可以通过凝胶浇注法得到成型体。
在本发明的碳化硅－碳复合材料的制造方法中，可以使用颗粒状的氮化硅。
优选氮化硅的粒径在碳质材料的粒径的1／100～1／5的范围内。
在本发明的碳化硅－碳复合材料的制造方法中，优选使用氮化硅与碳质材料的体积比为5：95～50：50的成型体。
在本发明的碳化硅－碳复合材料的制造方法中，优选以1700℃以上进行成型体的烧制。
本发明的碳化硅－碳复合材料的制造方法是用于制作具有碳化硅的碳化硅－碳复合材料的方法，该碳化硅覆盖多个碳质材料、并且将多个碳质材料连接。
发明效果
根据本发明，能够提供一种新的碳化硅－碳复合材料的制造方法。
附图说明
图1是由本发明的一个实施方式的制造方法制得的碳化硅－碳复合材料的示意截面图。
图2是实施例1中得到的碳化硅－石墨复合材料的扫描型电子显微镜照片（（a）表面（b）断裂面）。
图3是实施例2中得到的碳化硅－石墨复合材料的扫描型电子显微镜照片（（a）表面（b）断裂面）。
图4是实施例3中得到的碳化硅－石墨复合材料的扫描型电子显微镜照片（（a）表面（b）断裂面）。
图5是实施例4中得到的碳化硅－石墨复合材料的扫描型电子显微镜照片（（a）表面（b）断裂面）。
图6是实施例5中得到的碳化硅－石墨复合材料的扫描型电子显微镜照片（（a）表面（b）断裂面）。
图7是比较例1中得到的碳化硅－石墨复合材料表面的扫描型电子显微镜照片。
图8是比较例2中得到的碳化硅－石墨复合材料表面的扫描型电子显微镜照片。
具体实施方式
下面，对本发明的优选实施方式的一个例子进行说明。但下述的实施方式仅仅是例示。本发明完全不限定于下述的实施方式。
实施方式等中参照的附图是示意性的记载，附图中绘出的物体的尺寸的比例等有时与现实物体的尺寸的比例等不同。具体的物体的尺寸比例等应该参照以下的说明来判断。
（碳化硅－碳复合材料1）
图1是表示由本实施方式的制造方法制得的碳化硅－碳复合材料的示意截面图。首先，参照图1对由本实施方式的制造方法制得的碳化硅－碳复合材料的结构进行说明。
碳化硅－碳复合材料1是包括多个碳质材料2和碳化硅3的复合材料。
碳质材料2例如优选使用鳞状石墨、鳞片状石墨、土状石墨等构成的天然石墨，以焦炭或中间相小球体为原料的人造石墨等。碳质材料可以为颗粒状。即碳质材料2可以为碳颗粒。碳质材料2的粒径优选为50nm～500μm左右，更优选为1μm～250μm左右，进一步优选为5μm～100μm左右。在碳质材料2的粒径过小时，可能会发生凝聚。一旦碳质材料2过度凝聚，则有时碳化硅－碳复合材料1不能得到碳的特性。另一方面，在碳质材料2的粒径过大时，有时烧制得到的陶瓷－碳复合材料的强度降低。多个碳质材料2可以仅包括1种碳质材料2，也可以包括多种碳质材料2。
碳化硅3形成于多个碳质材料2之间。碳化硅3覆盖多个碳质材料2、并且将多个碳质材料2连接。优选碳化硅3具有连续的结构。更优选碳化硅3具有三维网状结构。即，优选多个碳质材料2通过具有三维网状结构的碳化硅3而一体化。在碳化硅－碳复合材料1中，优选碳化硅3中分散有碳颗粒2。在碳化硅3中碳颗粒2可以以块状分散。
其中，碳化硅3可以由连续的一个块构成，也可以由孤立的多个块构成。
碳化硅－碳复合材料1中的碳质材料2与碳化硅3的体积比（碳质材料2的体积：碳化硅3的体积）优选为95：5～50：50，更优选为90：10～70：30。
碳化硅3的厚度优选为100nm～10μm左右。
碳化硅－碳复合材料1可以含有来自烧结助剂的化合物。作为烧结助剂，可以列举Y2O3等的氧化钇、Al2O3等的氧化铝、CaO等的氧化钙、SiO2等的氧化硅、其他的稀土氧化物等。
接着，对碳化硅－碳复合材料1的制造方法的一个例子进行说明。
（成型体制作工序）
制作包含表面附着有氮化硅的碳质材料2的成型体。
附着于碳质材料2的表面的氮化硅的形状没有特别限定。例如可以列举颗粒状、覆膜状等。
在氮化硅为颗粒状的情况下，氮化硅的粒径优选为50nm～10μm左右，更优选为100nm～1μm左右。
优选氮化硅的粒径在碳质材料2的粒径的1／100～1／5的范围内。在这种情况下，能够由氮化硅覆盖碳质材料2的实质上的全部表面。更优选氮化硅的粒径在碳质材料2的粒径的1／50～1／10的范围内，进一步优选在1／40～1／20的范围内。
氮化硅与碳质材料2的混合比例（氮化硅的体积：碳质材料2的体积（体积比））优选为5：95～50：50，更优选为10：90～30：70。
使氮化硅附着于碳质材料2的表面的方法没有特别限定。例如将碳质材料2与氮化硅混合即可。作为具体例，可以列举气相法、液相法、使用混合机等将氮化硅与碳质材料2混合的机械混合法、浆料法或者将这些方法组合的方法。作为气相法的具体例，可以列举化学气相蒸镀法（CVD法）、转化法（CVR法）等。作为液相法的具体例，例如可以列举化学沉淀法等。作为浆料法的具体例，例如可以列举凝胶浇注法、滑移浇铸法、带式浇注法等。
将表面附着有氮化硅的碳质材料2成型的方法没有特别限定。例如可以利用凝胶浇注法，同时进行氮化硅在碳质材料2的表面的附着和成型。利用凝胶浇注法，将作为液体的溶剂和粘合剂混合制成浆料，在该浆料中添加碳质材料，进行混合，之后使其干燥，得到固态混合物。例如，在加入有作为粘合剂的丙烯酰胺和N,N′－亚甲基双丙烯酰胺的异丙醇有机溶剂中添加碳粉末和氮化硅粉末，利用自转·公转混合机进行搅拌，从而制备浆料，将该浆料加入模具中并使其干燥，得到成型体。
（烧制工序）
接着对成型体进行烧制。作为烧制方法，例如可以列举放电等离子体烧结法等。
成型体的烧制温度和烧制时间、烧制气氛的种类、烧制气氛的压力等可以根据所使用的材料的种类、形状、大小等适当设定。烧制温度例如可以为1700℃以上。烧制温度优选为1700℃～2100℃左右，更优选为1800℃～2000℃左右。烧制时间例如可以为5分钟～2小时左右。烧制气氛的种类例如可以为真空、氮、氩等的不活泼气体气氛。烧制气氛的压力例如可以为0.01MPa～10MPa左右。
在烧制工序中，在碳质材料2的表面形成碳化硅3。此时，碳化硅3形成于多个碳质材料2之间。即，在烧制工序中，多个碳质材料2由碳化硅3覆盖，并且由碳化硅3连接。其中，碳化硅－碳复合材料1中可以残留有氮化硅。
由本实施方式的制造方法制得的碳化硅－碳复合材料1，与将碳化硅作为原料制得的碳化硅－碳复合材料相比，在强度、热传导系数等方面优异。可以认为这是由于与使用碳化硅作为原料的情况相比，使用氮化硅作为原料时，在烧制工序中容易以更低的温度在碳质材料2的表面形成碳化硅3，容易进行碳化硅的烧结。即，在将碳化硅作为原料时，烧结的驱动力仅依赖于颗粒表面能量的减少，而在以氮化硅为原料时，由氮化硅转化为碳化硅的化学反应进一步促进烧结。可以认为烧结越进行，碳化硅－碳复合材料1中的碳化硅3的连续性越高，碳化硅3的连续性越高，强度和热传导系数越高。即，可以认为在本实施方式的制造方法中，由于使用氮化硅作为原料，能够得到强度、热传导系数等方面优异的碳化硅－碳复合材料1。
根据本实施方式的制造方法，即使不使用碳化硅作为原料，也能够以更低的温度简便地制造碳化硅－碳复合材料1。
下面，基于具体的实施例进一步对本发明进行详细地说明。本发明完全不限定于以下的实施例。在不改变本发明的要点的范围内可以适当进行变更而实施。
（实施例1）
如下所述操作，制作实质上具有与碳化硅－碳复合材料1同样结构的碳化硅－碳复合材料。
作为碳质材料2使用石墨（中间相小球体、东洋炭素株式会社生产）。作为氮化硅，使用宇部兴产株式会社生产的Si3N4。
将石墨（10g）、氮化硅（4.63g）和作为烧结助剂的Al2O3（0.31g）以及Y2O3（0.15g）混合，得到混合粉末，通过凝胶浇注法将得到的混合粉末与在异丙醇（45g）中溶解有丙烯酰胺（8g）和N,N′－亚甲基双丙烯酰胺（1g）的粘合剂溶液（3.57g）混合，将该混合物浇注在塑料模具中。混合物中的石墨与陶瓷的体积比为80：20。将得到的混合物在常压下、以80℃干燥12小时，得到干燥物。接着，将干燥物在真空中、以700℃加热1小时，除去作为粘合剂的丙烯酰胺。进一步利用放电等离子体烧结法，施加30MPa的压力，并且以1700℃、5分钟、真空条件进行脉冲通电烧结。结果，作为碳化硅－碳复合材料，得到碳化硅－石墨复合材料。
以下述方法测定得到的碳化硅－石墨复合材料的体积密度、相对密度、弯曲强度和热传导系数。将结果示于下述的表1。
〔体积密度〕
利用阿基米德法测定体积密度。具体而言基于JISA1509－3进行测定。
〔相对密度〕
由通过上述方法测得的体积密度与相同样品的理论密度（没有气孔的状态下的密度）之比，计算相对密度（参照JISZ2500－3407）。
〔弯曲强度〕
通过3点弯曲强度试验测定弯曲强度。具体而言基于JISA1509－4进行测定。
〔热传导系数〕
利用激光闪光法测定热传导系数。具体而言基于JISR1650－3进行测定。
将实施例1中得到的碳化硅－石墨复合材料的扫描型电子显微镜照片（（a）表面（b）断裂面）示于图2（倍率1000倍）。
（实施例2）
除了以1750℃进行脉冲通电烧结以外，与实施例1同样操作，得到碳化硅－石墨复合材料。与实施例1同样操作，测定得到的碳化硅－石墨复合材料的体积密度、相对密度、弯曲强度和热传导系数。将结果示于下述的表1。将实施例2中得到的碳化硅－石墨复合材料的扫描型电子显微镜照片（（a）表面（b）断裂面）示于图3（倍率1000倍）。
（实施例3）
除了以1800℃进行脉冲通电烧结以外，与实施例1同样操作，得到碳化硅－石墨复合材料。与实施例1同样操作，测定得到的碳化硅－石墨复合材料的体积密度、相对密度、弯曲强度和热传导系数。将结果示于下述的表1。将实施例3中得到的碳化硅－石墨复合材料的扫描型电子显微镜照片（（a）表面（b）断裂面）示于图4（倍率1000倍）。
（实施例4）
除了以1900℃进行脉冲通电烧结以外，与实施例1同样操作，得到碳化硅－石墨复合材料。与实施例1同样操作，测定得到的碳化硅－石墨复合材料的体积密度、相对密度、弯曲强度和热传导系数。将结果示于下述的表1。将实施例4中得到的碳化硅－石墨复合材料的扫描型电子显微镜照片（（a）表面（b）断裂面）示于图5（倍率1000倍）。
（实施例5）
将石墨（10g）、氮化硅（5.96g）和作为烧结助剂的Al2O3（0.39g）以及Y2O3（0.20g）混合，得到混合粉末，通过凝胶浇注法将得到的混合粉末与含有丙烯酰胺作为有机单体的1－丙醇（3.83g）混合，除此以外与实施例4同样操作，得到碳化硅－石墨复合材料。混合物中的石墨与陶瓷的体积比为80：20。
与实施例1同样操作，测定得到的碳化硅－石墨复合材料的体积密度、相对密度、弯曲强度和热传导系数。将结果示于下述的表1。
将实施例5中得到的碳化硅－石墨复合材料的扫描型电子显微镜照片（（a）表面（b）断裂面）示于图6（（a）为倍率500倍、（b）为倍率1000倍）。
（比较例1）
将石墨（10g）、碳化硅（SiC4.50g）和作为烧结助剂的Al2O3（0.30g）以及Y2O3（0.15g）混合，得到混合粉末，通过凝胶浇注法将得到的混合粉末与在异丙醇（45g）中溶解有丙烯酰胺（8g）和N,N′－亚甲基双丙烯酰胺（1g）的粘合剂溶液（3.03g）混合，除此以外与实施例4同样操作，得到碳化硅－石墨复合材料。混合物中的石墨与陶瓷的体积比为75：25。
与实施例1同样操作，测定得到的碳化硅－石墨复合材料的体积密度、相对密度、弯曲强度和热传导系数。将结果示于下述的表1。将比较例1中得到的碳化硅－石墨复合材料表面的扫描型电子显微镜照片示于图7（倍率1000倍）。
（比较例2）
将石墨（10g）、碳化硅（SiC5.96g）和作为烧结助剂的Al2O3（0.39g）以及Y2O3（0.20g）混合，得到混合粉末，通过凝胶浇注法将得到的混合粉末与含有丙烯酰胺作为有机单体的1－丙醇（3.24g）混合，除此以外与实施例4同样操作，得到碳化硅－石墨复合材料。混合物中的石墨与陶瓷的体积比为70：30。
与实施例1同样操作，测定得到的碳化硅－石墨复合材料的体积密度、相对密度、弯曲强度和热传导系数。将结果示于下述的表1。将比较例2中得到的碳化硅－石墨复合材料表面的扫描型电子显微镜照片示于图8（倍率1000倍）。
（比较例3）
将石墨（10g）、氮化铝（AlN3.54g）和作为烧结助剂的Y2O3（0.19g）混合，得到混合粉末，通过凝胶浇注法将得到的混合粉末与在异丙醇（45g）中溶解有丙烯酰胺（8g）和N,N′－亚甲基双丙烯酰胺（1g）的粘合剂溶液（2.49g）混合，除此以外与实施例4同样操作，得到碳化硅－石墨复合材料。混合物中的石墨与陶瓷的体积比为70：30。
与实施例1同样操作，测定得到的碳化硅－石墨复合材料的体积密度、相对密度、弯曲强度和热传导系数。将结果示于下述的表1。
[表1]
符号说明
1：碳化硅－碳复合材料；
2：碳质材料；
3：碳化硅。

Claims (3)

1.一种碳化硅－碳复合材料的制造方法，该碳化硅－碳复合材料中，碳化硅覆盖多个碳质材料，并且连接所述多个碳质材料，所述制造方法的特征在于，包括：
将颗粒状的氮化硅和颗粒状的碳质材料混合、成型，得到成型体的步骤；和
以1700℃以上2100℃以下并在加压下进行所述成型体的烧制，由此得到所述碳化硅－碳复合材料的步骤，
所述碳质材料的粒径在1μm～500μm的范围内，
所述氮化硅的粒径在所述碳质材料的粒径的1/100～1/5的范围内，
连接所述多个碳质材料的所述碳化硅是在对所述成型体进行烧制时、通过所述氮化硅与所述碳质材料反应而形成的碳化硅。
2.如权利要求1所述的碳化硅－碳复合材料的制造方法，其特征在于：将所述氮化硅、所述碳质材料和粘合剂混合，得到含有表面附着有所述氮化硅的所述碳质材料的混合物，对所述混合物进行成型，由此得到所述成型体。
3.如权利要求1所述的碳化硅－碳复合材料的制造方法，其特征在于：使用所述氮化硅与碳质材料的体积比为5：95～50：50的成型体。
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