CN102822114A - 具有受控的热膨胀系数的导电性复合材料 - Google Patents
具有受控的热膨胀系数的导电性复合材料 Download PDFInfo
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- CN102822114A CN102822114A CN2010800609857A CN201080060985A CN102822114A CN 102822114 A CN102822114 A CN 102822114A CN 2010800609857 A CN2010800609857 A CN 2010800609857A CN 201080060985 A CN201080060985 A CN 201080060985A CN 102822114 A CN102822114 A CN 102822114A
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- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- HEHRHMRHPUNLIR-UHFFFAOYSA-N aluminum;hydroxy-[hydroxy(oxo)silyl]oxy-oxosilane;lithium Chemical compound [Li].[Al].O[Si](=O)O[Si](O)=O.O[Si](=O)O[Si](O)=O HEHRHMRHPUNLIR-UHFFFAOYSA-N 0.000 description 1
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- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及包含陶瓷成分和碳纳米细丝的复合材料、其获得方法、以及其在微电子学、精密光学、航空和航天学中作为导电体的用途,所述陶瓷成分的特征在于其具有负的热膨胀系数。
Description
技术领域
本发明涉及包含陶瓷成分和碳纳米细丝的复合材料、其获得方法以及其在微电子学、精密光学、航空和航天学中作为导电体的用途,所述陶瓷成分的特征在于其具有负的热膨胀系数。
背景技术
具有低热膨胀系数(CTE)的材料在极为不同的领域中都具有广泛的应用。在许多类型的精密仪器中,以及在高技术系统中、在微电子工业和精密光学中的装置设备中都需要这些类型的材料。简言之,在所有这些应用中,随着温度的变化,都必须保证精密元件的维度稳定性,这需要降低形成这些元件的材料的CTE。此外,使用不同材料制造的原件的热膨胀的失衡还可以使用具有所需(且均匀的)CTE的复合材料的设计方案来解决。具有定制CTE的这些材料的设计方案可以使用具有正和负膨胀的成分的结合来处理。可以针对不同的温度实施复合材料CTE的定制设计方案,使得具有零CTE的成分的最终应用领域取决于用于所述应用所需的特定功能性的其他特征是否实现。锂陶瓷、玻璃陶瓷(LAS)、以及硅酸镁铝(堇青石)家族在许多应用领域(由玻璃陶瓷用于厨房到镜子用于卫星)中通常用于所述的这种目的。这些家族的一些矿物相具有负CTE,这使得它们可用于具有受控的且定制的CTE的复合材料中。通常,由于具有负CTE的材料负性是由于在不同的晶体取向之间具有强的各向异性(其中负行为通常在它们中的一者中发现,而正行为在其他两者中发现),所以具有负CTE的材料的抗折性较低。各向异性通常导致微纤维,这得到了这些材料的机械性质的值较低的结果。因此,加入氧化的/非氧化的陶瓷相能够得到具有改善的机械性质的材料。这些具有受控的CTE的材料受到关注地用于工程、光子、电子和/或结构的应用中(Roy,R.et al.,Annual Review ofMaterials Science,1989,19,59-81)。
在LAS系统中具有负膨胀的相为β-锂霞石(LiAlSiO4),这是由于其一个晶体轴方向的负膨胀较大。锂辉石(LiAlSi2O6)和透锂长石(LiAlSi4O10)相具有接近于零的CTE。制造具有LAS组合物的材料的传统方法为对玻璃进行加工,从而生产出玻璃陶瓷。该方法涉及将后期形成的玻璃在低温下施加热处理,以用于随后结晶LAS相的沉淀,并由此控制其CTE。偶尔,这种方法会产生不均匀的材料,并且由于该材料为玻璃,所以与其他陶瓷物质相比,其机械性质(刚性和抗性)当然不足以高达许多工业应用。这就是(由Schott出售)广泛地用于大量的应用中、但是对折断值具有较低的抗性的情况。因此,如果需要更好的机械性质,则需要玻璃陶瓷的备选物。目前存在其他的CTE接近于零的陶瓷材料,例如在US4403017或中公开的堇青石。制备具有低CTE的材料的备选方法由向其CTE为负的陶瓷成分中加入正热膨胀系数的第二相构成,如在US6953538、JP2007076949或JP2002220277以及专利申请P200803530中所述的情况。这种最后的选择极受关注,并且可以通过在基质中加入合适比例的第二相来调节CTE的值和其他性质。另一方面并且要记住的是材料的最终性质是两种或多种成分的组合中的结果,这些复合材料的主要问题在于进行操纵以便在广泛的温度范围内控制CTE的值。因此,在US6953538、JP2007076949或JP2002220277中,其中取得高的维度稳定性的温度范围为大约30-50℃。在专利申请P200803530中,用于CTE值接近于零的范围被扩展。
在专利P200803530中,使用了硅酸镁铝(堇青石)和硅酸锂铝。申请号为P200803530的专利公开了在溶液中由高岭土、碳酸锂、以及二氧化硅和氧化铝的前体合成硅酸锂铝的方法,由此可以得到具有受控的CTE和àla carte的LAS陶瓷,从而选择具有Al2O3∶Li2O∶SiO2相图的不同组合物。
发明内容
本发明提供了包含陶瓷基质和碳纳米细丝的复合材料,所述的材料可表征为其具有优异的机械性、导电性和热性质。此外,本发明还提供了所述材料的获得方法,以及其在制造用于微电子学、精密光学、航空和航天学的装置中作为导电体的用途。
本发明的第一个方面涉及这样的材料,其包含:
a.陶瓷成分,以及
b.碳纳米细丝,
其中所述的材料的热膨胀系数为-6x10-6℃-1至6.01x10-6℃-1。
这种材料为复合材料,并且这些碳纳米细丝起到导电体的作用;此外,这些碳纳米细丝在本发明所公开的材料的陶瓷基质(具有负的热膨胀系数)中起到增强作用。这形成了所述材料的导电性。
在本发明中,“复合材料”被理解为这样的材料,该材料由彼此不同的两种或多种成分形成,其具有得自这些成分的组合中的性质,而该性质优于分别形成的材料。
在本发明中的陶瓷成分起到了复合材料的基质的作用,由此为陶瓷基质。
在本发明中,“导电性”被理解为具有允许电流或电子从头至尾通过的能力的材料。
在本发明中,“热膨胀系数(CTE)”被理解为反映了当被加热时材料所发生的体积变化的参数。
在优选的实施方案中,所述的材料可表征为其进一步包含体积百分率低于80%的氧化的或非氧化的陶瓷化合物。
陶瓷成分优选地选自Li2O∶Al2O3∶SiO2体系或MgO∶Al2O3∶SiO2体系,这种基质为更优选的β-锂霞石或堇青石。
在优选的实施方案中,具有负的热膨胀系数的陶瓷成分占最终的材料的百分率高于10体积%。
在所述的基质中所包含的起到增强作用的碳纳米细丝可以为碳纳米纤维或纳米管,在作为碳纳米纤维的优选实施方案中,这些碳纳米纤维更优选地具有20至80nm的直径,长度/直径的比值更优选的是大于100,并且所述的碳纳米纤维更优选地具有超过70%的石墨结构。
在本发明中,“碳纳米纤维”被理解为具有高度的石墨结构的碳丝。
氧化的或非氧化的陶瓷优选地选自碳化物、氮化物、膨化物、金属氧化物或它们的组合中的任意一者。更优选的是,氧化的或非氧化的陶瓷选自:SiC,TiC,AlN,Si3N4,TiB2,Al2O3,ZrO2和MgAl2O4。
甚至更优选的是,氧化的陶瓷为氧化铝(Al2O3)的粒径更优选的为20至1000nm的Al2O3。并且如果陶瓷为非氧化的,则其更优选的为SiC;甚至更优选的是,所选的这种碳化硅的粒径小于10μm。
在高温下控制构成复合材料的相之间的反应性,以及控制复合材料的CTE使得可以根据人们想给予所述材料的应用来创造具有广泛的温度范围的CTE的导电性陶瓷材料。一方面,在这些复合材料中使用导电性相的益处在于可以得到具有高导电性的材料,另一方面,保持CTE和低密度,使得氧化的/非氧化的陶瓷能够得到具有改善的机械性质的材料。
具有陶瓷基质的导电性复合材料可表征为其具有受控的维度稳定性,其中所述的复合材料的特征在于在其组合物中包含碳纳米细丝,并且所述的陶瓷基质的组合物具有负的热膨胀系数,并且可以具有低于10体积%的孔隙率,而且电阻值低于1x104Ωcm,在-150℃至450℃的温度范围内可根据组成调节的热膨胀系数为-6x10-6℃-1至6.01x10-6℃-1,抗折性高于60Mpa,以及较低绝对密度。
本发明的第二个方面涉及如之前所述的材料的获得方法,其包括以下阶段:
a.将所述的陶瓷成分与所述的纳米细丝在溶剂中混合,
b.使在(a)中所获得的混合物干燥,
c.使在(b)中所获得的材料成形,
d.使在(c)中所获得的材料烧结。
在优选的实施方案中,在如之前所述的阶段(a)中加入氧化的或非氧化的陶瓷。
在阶段(a)中使用的溶剂选自水、无水醇或它们组合中的任意一者,并且甚至更优选的是无水醇为无水乙醇。
阶段(a)的混合优选的是在100至400rpm下实施的。这种混合可以在磨碎机中实施。
在优选的实施方案中,阶段(b)的干燥是通过雾化实施的。
在本发明中,“雾化”被理解为通过溶液的粉碎以及使用气流的悬浮的干燥方法。
阶段(c)的形式优选的是通过冷等静压制或者通过热压制实施的。
在本发明中,“等静压制”被理解为压紧方法,其是通过将通常为粉末形式的材料密封地封闭在模具中,通过流体施加流体静压,由此得到的部分具有均一且各向同性的性质。
当实施冷等静压制时,更优选的是在100至400Mpa的压力下实施。
如果实施热压制,在加热斜坡(heating ramp)为2至50℃/分钟的条件下在900℃至1600℃的温度下,施加5至150Mpa的单轴压力,并在该温度保持0.5至10小时。
阶段(d)的烧结温度优选在700至1600℃。可以在未施加压力或未施加单向压力的条件下实施烧结的阶段(d)。
当在未施加压力的条件下进行烧结时,可以在传统的烤箱中实施烧结,而且当在烧结过程中施加单向压力时,可以通过放电等离子烧结(SPS)或热压制进行烧结。
当在未施加压力的条件下实施烧结时,所述的烧结是通过以下过程进行的:在加热斜坡为2至10℃/分钟的条件下在1100℃至1600℃的温度下在惰性气氛中进行,并在该温度保持0.5至10小时。甚至更优选的是,惰性气氛为氩气。
可能甚至更优选的是,使用2至10℃/分钟的斜坡进行随后冷却至900℃。
如果所述的烧结是通过以下过程使用施加单轴压力进行的:在加热斜坡为2至300℃/分钟的条件下在700℃至1600℃的温度下施加5至150MPa的单轴压力,在该温度保持1至30分钟。这种烧结方法能够在短期时间内得到具有受控的粒径的材料。
通过简单的制造方法进行制备,这些方法是在固态下通过不同的技术形成和烧结的,从而避免了玻璃的形成,并且结果得到了改善的机械性质。
如果选择硅酸锂铝或硅酸镁铝基质以及导电性相,并且所述的导电性相可以加入第三种氧化的或非氧化的相而在高温下在相之间不会存在任何的反应,按照这种方式会改善机械性、电性和热性质,从而简化获得方法,得到致密的且超轻型的材料。这种控制是由于特别适用了具有负CTE的相。
本发明所提供的备选方法为获得是导电性的、在广泛的温度范围内具有受控的热膨胀系数的(这使得这些材料适用于大量的机械应用中)并且是低密度的(轻质的)陶瓷材料。除了为导电体以外,所述的方法开启了这样的可能性:可以使用电腐蚀技术对这些材料进行加工,从而能够制备得到具有所需形状的成分。
本发明的第三个方面涉及之前所述的材料作为导电体和/或作为在制造具有高维度稳定性的陶瓷成分的材料中的用途。所述的材料应用于微电子领域、精密光学或航空领域。在优选的实施方案中,所述的导电体材料可用于制造高精密测量仪器、用于空间观测系统的镜子、照相平板扫描仪、全息术、激光仪器或散热仪。
简言之,这些复合材料可以用于制造需要高维度稳定性的成分,更具体而言可用于制造卫星中的天文望远镜和x射线望远镜中的镜子结构、彗星探测器、气象卫星和微光刻中的光学元件、环形激光陀螺仪中的镜子和底座、共振中的激光距离指示仪、高精密测量技术中的测量棒和标准品等。
在整个说明书和权利要求书中,词语“包含”及其变体无意于排除其他的技术特征、添加剂、成分或步骤。对于本领域的技术人员而言,本发明的其他目标、益处和特征部分由说明书推断,部分由本发明的实施推断。通过举例的方式提供以下附图和实施例,并且这些附图和实施例无意于限定本发明。
附图说明
图1.Li2O-Al2O3-SiO2系统的相图,其示出了在实施方案的实施例中使用的组合物。
图2.与通过在SPS中烧结而得到的LAS材料-碳纳米纤维、通过传统的烤箱得到的堇青石-碳纳米纤维、通过热压制烧结而得到的LAS-碳纳米纤维-SiC以及通过在SPS中烧结得到的LAS-碳纳米纤维-Al2O3相应的热膨胀系数(α曲线)。
实施例
下文中,通过本发明人实施的测试来说明本发明,这些测试作为本发明的方法目标的具体实施方案,在(-150,+450)℃范围内具有受控的CTE的导电性复合材料的特异性和效力。
实施例1
起始材料为:
a)具有组成LiAlSiO4(图1中的组成A)的LAS粉末,其平均粒径为1μm,密度为2.39g/cm3。
b)碳纳米纤维,其直径为大约20-80nm,密度为1.97g/cm3。
c)无水乙醇(纯度为99.97%)。
使用700g LAS,其分散在1400g的乙醇中。然后,将其与由146.4g碳纳米纤维在2000g乙醇中形成的悬浮液混合。通过机械搅拌60分钟使结合物均化,然后在粉碎机中通过在300rpm下操作再研磨60分钟。由此制备的悬浮液通过雾化干燥,从而得到纳米复合物颗粒,同时由所述的过程回收乙醇。研磨阶段能够制备均匀和纳米尺寸的粉末,这会改善最终的材料的增稠作用。
将如此得到的干燥产物经历使用了放电等离子烧结(SPS)的成形和烧结过程。如此,将14.5克的材料引入到直径为40mm的石墨模具中,并在10MPa下单轴应力。接着,通过施加80MPa的最大压力并以100℃/分钟的加热斜坡加热至1200℃并停留1分钟来进行烧结。
通过所得材料的真密度(氦比重仪)、表观密度(Archimedes方法)、杨氏模量(在Grindosonic单元中的共振频率方法)、抗折性(在INSTRON8562单元中的四点弯曲方法)、以及热膨胀系数(直径,制造:METZCH,型号:DIL402C)来表征所得的材料。相应的值示于表1中。在所述的温度下热膨胀系数的变化在图2中呈现。
性质 | Ex.1 |
理论密度%,100x(d表观/d真) | 99.8 |
抗折性(MPa) | 165 |
CTE(x10-6℃-1)(-150,150)℃ | -1.34 |
CTE(x10-6℃-1)(-150,450)℃ | -0.69 |
表1:通过SPS烧结,由LAS和碳纳米纤维形成的复合材料的表征而得到的结果。
实施例2
起始材料为:
a)具有组成2Al2O3·5SiO2·2MgO的堇青石粉末,其密度为2.65g/cm3。
b)碳纳米纤维,其直径为大约20-80nm,密度为1.97g/cm3。
c)无水乙醇(纯度为99.97%)。
使用900g堇青石,其分散在1600g的乙醇中。然后,将其与由21g碳纳米纤维在400g乙醇中形成的悬浮液混合。通过机械搅拌60分钟使结合物均化,然后在粉碎机中通过在300rpm下操作再研磨60分钟。由此制备的悬浮液通过雾化干燥,从而得到纳米复合物颗粒,同时由所述的过程回收乙醇。
在200MPa下使干燥产物经历使用了冷等静压制的成形过程。得到成形的材料,该材料在1400℃下在氩气气氛中,在传统的烤箱中烧结,其中停留120分钟并且加热斜坡为5℃/分钟。
通过所得材料的真密度(氦比重仪)、表观密度(Archimedes方法)、杨氏模量(在Grindosonic单元中的共振频率方法)、抗折性(在INSTRON8562单元中的四点弯曲方法)、以及热膨胀系数(直径,制造商:METZCH,型号:DIL402C)来表征所得的材料。相应的值示于表2中。在所述的温度下热膨胀系数的变化在图2中呈现。
性质 | Ex.2 |
理论密度%,100x(d表观/d真) | 99.1 |
抗折性(MPa) | 120 |
CTE(x10-6℃-1)(-150,150)℃ | -0.02 |
CTE(x10-6℃-1)(-150,450)℃ | 0.91 |
表2:通过在传统的烤箱中烧结,由堇青石和碳纳米纤维形成的复合材料的表征而得到的结果。
实施例3
起始材料为:
a)具有组成LiAlSiO4(图1中的组成)的LAS粉末,其平均粒径为1μm,密度为2.39g/cm3。
b)碳纳米纤维,其直径为大约20-80nm,密度为1.97g/cm3。
c)SiC粉末,其平均粒径小于100nm,密度为3.20g/cm3。
d)无水乙醇(纯度为99.97%)。
使用600g LAS,其分散在1300g的乙醇中。然后,将其与由63g碳纳米纤维在1100g乙醇中形成的悬浮液以及由143.8g n-SiC在1000g乙醇中形成的悬浮液混合。通过机械搅拌60分钟使结合物均化,然后在粉碎机中通过在300rpm下操作再研磨60分钟。由此制备的悬浮液通过雾化干燥,从而得到纳米复合物颗粒,同时由所述的过程回收乙醇。
将如此得到的干燥产物经历使用了热压制的成形和烧结过程。如此,将30克的材料引入到直径为50mm的石墨模具中,并在5MPa下单轴应力。接着,通过施加35MPa的最大压力并以5℃/分钟的加热斜坡加热至1150℃并停留120分钟来进行烧结。
通过所得材料的真密度(氦比重仪)、表观密度(Archimedes方法)、杨氏模量(在Grindosonic单元中的共振频率方法)、抗折性(在INSTRON8562单元中的四点弯曲方法)、以及热膨胀系数(直径,制造商:METZCH,型号:DIL402C)来表征所得的材料。相应的值示于表3中。在所述的温度下热膨胀系数的变化在图2中呈现。
性质 | Ex.3 |
理论密度%,100x(d表观/d真) | 98.8 |
抗折性(MPa) | 144 |
CTE(x10-6℃-1)(-150,150)℃ | -0.34 |
CTE(x10-6℃-1)(-150,450)℃ | 0.35 |
表3:通过热压制烧结,由LAS和碳纳米纤维形成的复合材料的表征而得到的结果。
实施例4
起始材料为:
a)具有组成LiAlSiO4(图1中的组成)的LAS粉末,其平均粒径为1μm,密度为2.39g/cm3。
b)碳纳米纤维,其直径为大约20-80nm,密度为1.97g/cm3。
c)氧化铝粉末,其平均粒径小于160nm,密度为3.93g/cm3。
d)无水乙醇(纯度为99.97%)。
使用250g LAS,其分散在800g的乙醇中。然后,将其与由104.6g碳纳米纤维在1300g乙醇中形成的悬浮液以及由411.2g Al2O3在1000g乙醇中形成的悬浮液混合。通过机械搅拌60分钟使结合物均化,然后在粉碎机中通过在300rpm下操作再研磨60分钟。由此制备的悬浮液通过雾化干燥,从而得到纳米复合物颗粒,同时由所述的过程回收乙醇。
将如此得到的干燥产物经历使用了放电等离子烧结(SPS)的成形和烧结过程。如此,将18.4克的材料引入到直径为40mm的石墨模具中,并在10MPa下单轴应力。接着,通过施加80MPa的最大压力并以100℃/分钟的加热斜坡加热至1250℃并停留1分钟来进行烧结。
通过所得材料的真密度(氦比重仪)、表观密度(Archimedes方法)、杨氏模量(在Grindosonic单元中的共振频率方法)、抗折性(在INSTRON8562单元中的四点弯曲方法)、以及热膨胀系数(直径,制造商:METZCH,型号:DIL402C)来表征所得的材料。相应的值示于表4中。在所述的温度下热膨胀系数的变化在图2中呈现。
性质 | Ex.4 |
理论密度%,100x(d表观/d真) | 98.9 |
抗折性(MPa) | 310 |
CTE(x10-6℃-1)(-150,150)℃ | 2.83 |
CTE(x10-6℃-1)(-150,450)℃ | 3.88 |
表4:通过放电等离子烧结(SPS),由LAS和碳纳米纤维形成的复合材料的表征而得到的结果。
Claims (32)
1.一种材料,包含:
a.陶瓷成分,以及
b.碳纳米细丝,
其中所述的材料的特征在于其热膨胀系数为-6x10-6℃-1至6.01x10-6℃-1。
2.根据权利要求1所述的材料,其中其进一步包含体积百分率低于80%的氧化的或非氧化的陶瓷。
3.根据权利要求1所述的材料,其中所述的陶瓷成分选自Li2O∶Al2O3∶SiO2或MgO∶Al2O3∶SiO2。
4.根据权利要求3所述的材料,其中所述的陶瓷成分为β-锂霞石或堇青石。
5.根据权利要求1至4中任意一项所述的材料,其中所述的陶瓷成分占最终的材料的体积百分率大于10%。
6.根据权利要求1至5中任意一项所述的材料,其中所述的碳纳米细丝为碳纳米纤维。
7.根据权利要求6所述的材料,其中所述的碳纳米纤维的直径为20nm至80nm。
8.根据权利要求6或7中任意一项所述的材料,其中所述的碳纳米纤维具有大于100的长度/直径比。
9.根据权利要求6或8中任意一项所述的材料,其中所述的碳纳米纤维具有大于70%的石墨结构。
10.根据权利要求1至9中任意一项所述的材料,其中所述的氧化的或非氧化的陶瓷选自:碳化物、氮化物、硼化物、金属氧化物或它们组合中的任意一者。
11.根据权利要求10所述的材料,其中所述的氧化的或非氧化的陶瓷选自:SiC,TiC,AlN,Si3N4,TiB2,Al2O3,ZrO2和MgAl2O4。
12.根据权利要求11所述的材料,其中所述的氧化的陶瓷为Al2O3。
13.根据权利要求12所述的材料,其中所述的Al2O3的粒径为20nm至1000nm。
14.根据权利要求11所述的材料,其中所述的非氧化的陶瓷为SiC。
15.根据权利要求14所述的材料,其中所述的SiC的粒径小于10μm。
16.一种获得根据权利要求1至15所述的材料的方法,包括以下阶段:
a.将所述的陶瓷成分与所述的纳米细丝在溶剂中混合,
b.使在(a)中所获得的混合物干燥,
c.使在(b)中所获得的材料成形,
d.使在(c)中所获得的材料烧结。
17.根据权利要求16所述的方法,其中在阶段(a)进一步加入氧化的或非氧化的陶瓷。
18.根据权利要求16或17中任意一项所述的方法,其中所述的溶剂选自:水、无水醇或它们的组合中的任意一者。
19.根据权利要求18所述的方法,其中所述的无水醇为无水乙醇。
20.根据权利要求16至19中任意一项所述的方法,其中所述的阶段(a)的混合是在100rpm至400rpm间进行的。
21.根据权利要求16至20中任意一项所述的方法,其中所述的阶段(b)的干燥是通过雾化进行的。
22.根据权利要求16至21中任意一项所述的方法,其中所述的阶段(c)的成形是通过冷或热等静压制进行的。
23.根据权利要求22所述的方法,其中所述的冷等静压制是在100至400MPa的压力下进行的。
24.根据权利要求22所述的方法,其中所述的热压制是通过以下过程进行的:在加热斜坡为2至50℃/分钟的条件下在900℃至1600℃的温度下,施加5至150Mpa的单轴应力,并在该温度保持0.5至10小时。
25.根据权利要求16至24中任意一项所述的方法,其中所述的阶段(d)的烧结是在700℃至1600℃的温度下进行的。
26.根据权利要求25所述的方法,其中所述的阶段(d)的烧结是在未施加压力或施加单轴压力的条件下进行的。
27.根据权利要求25或26中任意一项所述的方法,其中所述的烧结是通过以下过程进行的:在加热斜坡为2至10℃/分钟的条件下在1100℃至1600℃的温度下在惰性气氛中进行,并在该温度保持0.5至10小时。
28.根据权利要求27所述的方法,其中所述的惰性气氛为氩气。
29.根据权利要求27或28中任意一项所述的方法,其中使用2至10℃/分钟的斜坡进行随后冷却至900℃。
30.根据权利要求25或26中任意一项所述的方法,其中所述的烧结是通过以下过程进行的:在加热斜坡为2至300℃/分钟的条件下在700℃至1600℃的温度下施加5至150MPa的单轴压力,并在该温度保持1至30分钟。
31.根据权利要求1至15中任意一项所述的材料在制造具有高维度稳定性的陶瓷成分中作为导电体和/或材料的用途。
32.根据权利要求31所述的材料在制造高精密测量仪器、用于空间观测系统的镜子、照相平板扫描仪、全息术、激光仪器或散热仪中的用途。
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PCT/ES2010/070827 WO2011073483A1 (es) | 2009-12-16 | 2010-12-14 | Material compuesto de electroconductor con coeficiente de expansión térmica controlado |
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CN105859272A (zh) * | 2016-05-11 | 2016-08-17 | 河南工程学院 | 低温烧结制备纳米负膨胀陶瓷LiAlSiO4的方法 |
CN112876228A (zh) * | 2021-01-26 | 2021-06-01 | 中国兵器工业第五二研究所烟台分所 | 一种高模量堇青石基低热膨胀陶瓷及其制备方法 |
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ES2341081B1 (es) | 2008-12-12 | 2011-05-23 | Consejo Superior De Investigaciones Cientificas (Csic) | Materiales basados en aluminosilicatos de litio con coeficiente de expansion termica negativos en un amplio intervalo de temperatura, procedimiento de preparacion y uso. |
CN103208735A (zh) * | 2012-01-12 | 2013-07-17 | 郑州大学 | 用于大功率半导体激光器列阵的热膨胀系数可调节热沉 |
CN112358296A (zh) * | 2014-08-14 | 2021-02-12 | 清华大学 | 一种硫氧化钆闪烁陶瓷制备方法 |
CN107188527B (zh) * | 2017-06-19 | 2019-10-11 | 西安交通大学 | 一种由纳米线构筑的SiC弹性陶瓷及其制备方法 |
CN111995418B (zh) * | 2020-08-27 | 2021-07-20 | 东华大学 | 一种高强度高韧性的碳化硅纳米线增强碳化硅陶瓷复合材料的制备方法 |
CN115043644B (zh) * | 2022-04-13 | 2023-03-24 | 山东电盾科技股份有限公司 | 一种具有防静电功能的陶瓷手模及其制备工艺 |
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CN112876228A (zh) * | 2021-01-26 | 2021-06-01 | 中国兵器工业第五二研究所烟台分所 | 一种高模量堇青石基低热膨胀陶瓷及其制备方法 |
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ES2578014T3 (es) | 2016-07-20 |
EP2514732A4 (en) | 2015-06-03 |
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