CN102482096B - 富勒烯型多层碳纳米颗粒 - Google Patents
富勒烯型多层碳纳米颗粒 Download PDFInfo
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Abstract
本发明涉及一种具有0.34-0.36nm层间距的环状的多层碳纳米颗粒，所述多层碳纳米颗粒的环状多层体的外径和厚度的比为(10-3)∶1，且平均尺寸为15-100nm。
Description
技术领域
本发明涉及碳的化学，特别是，涉及富勒烯型(fulleroid type)多层碳纳米颗粒的获得。
富勒烯型颗粒具有呈现由σ和π键交互的5元环，6元环组成的连续网状的典型结构。
多层颗粒具有等于0.34-0.36nm的层间距。富勒烯型纳米颗粒的结构决定了它们具有低强度的、强的或异常高的弥散相互作用(dispersion interaction)的性能，该性能通过进入所述颗粒的电磁波的电场强度的可行性增长得到证实。
背景技术
富勒烯型多层碳纳米颗粒—多层碳纳米管—是管状纳米颗粒，具有相当大范围的尺寸：长度为10-100000nm；外径为1-500nm；壁厚为0.1-200nm。纳米管通过提取由石墨阳极的电弧蒸发得到的阴极沉积物而获得(申请JP 07-165406，M.cl.C01B，31/00,1995)。
所述的多层纳米管在包含这些纳米颗粒的阴极的自发射中在电极间隙中对相互作用力几乎没有影响。此外，在包含纳米管的阴极表面上实现的电场增益系数值很小，不允许在各种介质的边界上获得高水平的弥散相互作用。
具有0.34-0.36nm的层间距以及60-200nm的平均颗粒尺寸的富勒烯型多面体多层碳纳米颗粒是已知的(RU专利号2196731，M.cl.C01B，31/02，2003)。
所述多面体多层碳纳米颗粒是具有内部裂缝状毛细管的4-7面多面体。它们也可以具有分枝形式并可不包含所述的内部毛细管，或者它们可具有拉平的多面体的形式，其外径超出纳米颗粒的长度。
所述富勒烯型多面体多层纳米颗粒从电弧过程中石墨阳极的蒸发得到的阴极沉积物的外壳中提取获得。制备方法包括研磨过的阴极沉淀物外壳的气相氧化以及随后的碳粉在氢氧化物和硝酸钾的混合物熔体中的液相氧化，如在RU2196731中所示的。
所述多面体多层碳纳米颗粒具有很多有价值的特性：它们有助于构造混凝土(RU专利号2233254，2004)，增强合金的耐磨性(RU专利号2281341，2003)，高抗热降解性(RU专利号2196731，2003)等等。然而，它们在尺寸和形状分布的随机性不允许在从由这些纳米颗粒制成的阴极自电子发射的过程中实现在电极间隙间相互作用力的效果，也不允许在它们表面上获得高的电场增益系数，高的电场增益系数在各种介质的相界面上提供最高水平的弥散相互作用。
发明内容
本发明的目的是获得富勒烯型多层碳纳米颗粒，在由所述颗粒制成的阴极自电子发射过程中所述颗粒在电极间隙间提供高值的相互作用力。
根据本发明，层间距为0.34-0.36nm的富勒烯型多层碳纳米颗粒具有环形形状，环状多层体的外径与厚度的比为(10-3)∶1且纳米颗粒的平均尺寸为15-100nm。
所述富勒烯型环形多层碳纳米颗粒通过它们在电场中的分离来选择多层碳纳米颗粒的尺寸和形状而获得，如Brozdnichenko A.N.&all.的论文中所述(Journal ofSurface Investigation.X-ray，Synchrotron and Neutron Techniques，2007，No2，p.69-73)。为了获得所述形状的纳米颗粒，阴极板被放置在真空体中；由先前的操作通过氧化得到的多层碳纳米颗粒置于阴极板上，并且与之平行放置由非磁性材料例如钽制成的阳极板。将阳极和阴极连接到高压电源后，提供电压并且逐渐提高在电极间隙间的电位差。当场强度达到800-1000V/mm时，开始产生自发射电流。如果自发射电流增大，通过一个在其上固定所述阳极板的真空功率计记录阳极/阴极吸引力的出现。以某个自发射电流值开始，一部分多层碳纳米颗粒从阴极迁移到阳极，同时，在电极间隙中作用的力停止增加。随后，移除施加在阴极和阳极上的电压，用惰性气体填充所述真空体，收集积聚在阳极板上的多层碳纳米颗粒。
用这种方式分离的多层碳纳米颗粒具有环形形状，所述环状多层体的外径与厚度的比等于(10-3)∶1，正如在透射电子显微镜，例如JEM-100C的帮助下的研究所示。
附图说明
所得纳米颗粒的微观照片如图1-2所示。
图1显示了聚集成一束的圆环形状的富勒烯型多层碳纳米颗粒的照片。
图2显示了富勒烯型环状多层碳纳米颗粒在可确定环状外径与其主体厚度的比的高放大倍率下的照片。
具体实施方式
本发明通过实施例进一步说明但不限于这些实施例。
实施例1
在80-200A/cm2的电流密度和20-28V的电弧压降下在40-100Torr压力的氦气气氛中通过截面积为30-160mm2的阳极石墨棒的电弧侵蚀来获得阴极沉积。从松散的中部分离阴极沉积物的致密外壳，将其研磨并将其放置在置于频率为2.5GHz且功率为500-1500Wt的超高频场中的转动的石英管中。在这些条件下经过100-150min的气相氧化，冷却所得到的粉末并将其置于真空体中的阴极上，处于阴极和阳极之间的极间空间中。随后增大阴极和阳极间的电位差直到出现自发射电流。随着自发射电流的增大，一部分多层碳纳米颗粒迁移到阳极。在该过程的最后，从阳极表面被收集多层碳纳米颗粒并在有机溶剂例如二甲基甲酰胺中转化为分散体。
实施例2
如实施例1所述得到产品，但气相氧化在包含过量氧气，例如，20％-60％氧气的气氛下进行。
实施例3
如实施例1所述得到产品，但在气相氧化后，多层碳纳米颗粒另外在包含氯化合物的含水电解液中电化学氧化。
实施例4
如实施例1所述得到产品，但环状多层碳纳米颗粒的分离在具有高的介电渗透性值的介电介质(例如石油溶剂油)中在电场下实施。
实施例5
如实施例1所述得到产品，但在气相氧化后，通过将多层碳纳米颗粒放置在液化气体介质(氮，氦)中进行附加冷却，鼓泡并从液相中分离沉积物，随后蒸发液化气体获得两种类型的碳粉末，并如实施例1所述进一步处理，。
为了确定电物理学特性，将产物从溶剂中分离并测定以下参数：
—放射学地测定多层碳纳米颗粒的层间距，测得层间距等于0.34-0.36nm，该值是富勒烯型碳化合物的特征；
—使用透射电子显微镜，例如JEM-100C，和乳胶珠标准样，测定了多层碳纳米颗粒的尺寸、形状以及环状纳米颗粒的外径和多层体厚度之间的比。
通过将所得到的环状纳米颗粒涂覆在电传导基体上制造自发射阴极。根据RU2196731，具有多层纳米管和多面体多层碳纳米颗粒的自发射阴极已用相似的方式制造。
测定了所述自发射阴极的电极间隙中的相互作用力。参数列于表中。
下表显示了当负极由富勒烯型环状多层碳纳米颗粒制造时电极间隙中的作用力，与根据RU2196731得到的多层纳米管和富勒烯型多面体多层碳纳米颗粒的电极的这些力的值不同。
表根据本发明的技术方案的由富勒烯型多层碳纳米颗粒
制备的电极的相互作用力
由于在这些富勒烯型环状多层碳纳米颗粒表面上的电场的增益系数的高值，制得的产物可以应用于利用在自电子发射过程中电极间隙中相互作用力的效应的电子设备(动态参数传感器)；作为非线性光学介质的组分；也可用作结构复合材料的增强剂和作为建筑中混凝土的增塑剂。
Claims (10)
1.富勒烯型多层碳纳米颗粒，其具有0.34-0.36nm的层间距，特征在于：所述富勒烯型多层碳纳米颗粒具有环形形状，环状纳米颗粒的多层体的外径和厚度的比等于(10-3):1，且平均尺寸为15-100nm，所述平均尺寸通过透射电子显微镜测定。
2.制备根据权利要求1所述的富勒烯型多层碳纳米颗粒的方法，所述方法包括：
-将阴极板和由非磁性材料制成的阳极板放置在具有介电介质的真空体中，调节所述阴极板和阳极板使得形成电极间隙，
-通过气相氧化获得源自多层碳纳米结构的粉末，
其特征在于，所述方法进一步包括：
-将先前通过气相氧化获得的源自多层碳纳米结构的粉末放置在所述阴极板上；
-将所述阳极板固定在功率计上；
-将所述阴极板和所述阳极板连接至电源；
-通过给所述阴极板和所述阳极板施加电压将所述粉末暴露在电场中；
-增加所述阴极板和所述阳极板之间的电位差直到在电极间隙间中出现自发射电流；
-通过所述功率计记录阳极/阴极吸引力作为自发射电流的函数；
-当在电极间隙中作用的力停止增加，移除施加在所述阴极板和所述阳极板上的电位差；
-用惰性气体填充所述真空体；
-收集积聚在所述阳极板的富勒烯型多层碳纳米颗粒；
-用放射学方法测定富勒烯型多层碳纳米颗粒的层间距；
-使用透射电子显微镜测定富勒烯型多层碳纳米颗粒的平均尺寸、形状以及外径和多层体厚度之间的比值；且
特征在于，
所述多层碳纳米颗粒是根据权利要求1所述的富勒烯型多层碳纳米颗粒。
3.根据权利要求2所述的方法，其特征在于，所述方法还包括：
-在氦气气氛中通过阳极石墨棒的电弧侵蚀来获得阴极沉积；
-从松散的中部分离阴极沉积物的致密外壳；
-研磨该致密外壳；
-借助于该致密外壳的气相氧化获得多层碳纳米结构。
4.根据权利要求3所述的方法，其特征在于，所述方法还包括：将在阳极板上收集的富勒烯型多层碳纳米颗粒在有机溶剂中转化为分散体。
5.根据权利要求4所述的方法，其特征在于，所述有机溶剂是二甲基甲酰胺。
6.根据权利要求5所述的方法，其特征在于，所述方法还包括将该致密外壳置于超高频场中，以及特征在于，
-阳极石墨棒的截面积为30-160mm2；
-在80-200A/cm2的电流密度和20-28V的电弧压降下在40-100Torr压力的氦气气氛中进行阳极石墨棒的电弧侵蚀；
-超高频场的频率为2.5GHz且功率为500-1500Wt；
-致密外壳的气相氧化在100-150min的时间内实现。
7.根据权利要求6所述的方法，其特征在于，所述致密外壳的气相氧化在包含氧气的气氛中进行，并且所述气氛包含的氧气量为20％-60％。
8.根据权利要求6所述的方法，其特征在于，在气相氧化之后，多层碳纳米结构另外在包含氯化合物溶液的含水电解液中被电化学氧化。
9.根据权利要求6所述的方法，其特征在于，在气相氧化之后，对多层碳纳米结构另外进行处理，该另外的处理包括：
-通过将多层碳纳米结构放置在液化气体中将其冷却；
-对包含该液化气体和该多层碳纳米结构的介质进行鼓泡；
-从该介质的液相中分离介质的固相；
-通过蒸发所述液相从介质的液相中获得粉末。
10.通过权利要求2的方法所获得的权利要求1的富勒烯型多层碳纳米颗粒在以下应用之一中的用途：(a)作为利用在自电子发射过程中电极间隙中相互作用力的效应的电子设备中的动态参数传感器；(b)作为非线性光学介质的组分；(c)用作结构复合材料的增强剂；和(d)作为建筑中混凝土的增塑剂。
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| ES2369811B1 (es) * | 2010-05-04 | 2012-10-15 | Consejo Superior De Investigaciones Científicas (Csic) | Procedimiento de obtención de materiales nanocompuestos. |
| GB201118586D0 (en) | 2011-10-27 | 2011-12-07 | Turzi Antoine | New A-PRP medical device, manufacturing machine and process |
| FR3000426A1 (fr) * | 2012-12-28 | 2014-07-04 | Andrey Ponomarev | Composition et procede de revetement d'un support |
| GB201421013D0 (en) | 2014-11-26 | 2015-01-07 | Turzi Antoine | New standardizations & medical devices for the preparation of platelet rich plasma (PRP) or bone marrow centrate (BMC) |
| CN116254545A (zh) | 2018-10-29 | 2023-06-13 | C2Cnt有限责任公司 | 以低碳足迹生产的碳纳米材料用于生产具有低co2排放的复合材料的用途 |
| CN110527257B (zh) * | 2019-09-18 | 2022-03-18 | 东莞泰合复合材料有限公司 | 一种碳纤维复合材料及其制备方法和应用 |
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| CN102482096A (zh) | 2012-05-30 |
| EP2460764A4 (en) | 2013-11-13 |
| EP2460764A1 (en) | 2012-06-06 |
| US9090752B2 (en) | 2015-07-28 |
| WO2011010946A1 (ru) | 2011-01-27 |
| US8742001B2 (en) | 2014-06-03 |
| CN102471064B (zh) | 2014-11-05 |
| US20120114946A1 (en) | 2012-05-10 |
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| US20120142821A1 (en) | 2012-06-07 |
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| WO2011010948A1 (ru) | 2011-01-27 |
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