CN102144004A - 改性颗粒及包含所述颗粒的分散体 - Google Patents
改性颗粒及包含所述颗粒的分散体 Download PDFInfo
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- CN102144004A CN102144004A CN200980134455XA CN200980134455A CN102144004A CN 102144004 A CN102144004 A CN 102144004A CN 200980134455X A CN200980134455X A CN 200980134455XA CN 200980134455 A CN200980134455 A CN 200980134455A CN 102144004 A CN102144004 A CN 102144004A
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Abstract
Description
本发明涉及经改性剂改性的颗粒以及包含该改性颗粒的分散体。
氧化锌为用于制造大型显示器或其他电子电路中的有利TFT电路的薄膜晶体管(TFT)中的具有前景的半导体。
制造这些金属氧化物半导体FET(MOSFET)的关键步骤为将氧化锌或其他半导体沉积在各基材上。
对将半导体沉积在聚合物基材或其他挠性基材上存在极大兴趣,因为其不仅在其低重量及机械稳定性方面有利,而且也可藉通过例如旋涂、浸涂或印刷技术的方法由分散体显著更有利地沉积而加工。但是,聚合物基材限定操作范围低于200℃。
为形成细碎纳米尺寸颗粒的均匀层,胶态稳定分散体对于沉积很重要。为此需要能有效防止初级颗粒聚结的添加剂(改性剂)。这种添加剂的使用一般由其他申请已经知道很长时间了。
WO 2006/138071与WO 2006/138072分别公开了由胶态分散体将半导体氧化锌层沉积于基材上的方法。该分散体优选在室温下施用且随后在低于300℃的温度下烘烤(退火)。所用的分散体经稳定化,但其未提及任何稳定剂或改性剂。
DE 102 57 388 A1阐述了一种用于化妆品配方中的表面改性的氧化锌纳米颗粒,其中表面改性包括用通式HOOC-R1-(CH2)n-R2-CH3的有机酸涂覆,其中R1=CH2-(O-CH2-CH2)m;其中m=0至11,n=0至30以及当m=0时,n大于11;且R2=CH2、CHCH2、C(CH3)2、亚苯基、O、S。对于优选改性剂,可提及月桂醚-11-聚乙二醇酸、辛醚-6-聚乙二醇酸、月桂醚-4-聚乙二醇酸、月桂醚-6-聚乙二醇酸、及/或月桂醚-8-聚乙二醇酸。
DE 10 2005 007 374 A1公开了经可生物降解聚合物改性的纳米颗粒,特别是聚酯、聚氰基丙烯酸酯、聚丙烯酸酯、聚甲基丙烯酸酯、聚环氧化物、聚氨酯及聚苯乙烯。EP 1630136 A1公开了经亲水性聚合物改性的二氧化钛颗粒,特别是聚羧酸。改性剂的羧基经由酯键与二氧化钛键合。其他改性剂阐述于DE 10 2005 047 807 A1中。
到目前为止所用的改性颗粒或分散体具有如下缺点:其在导电、半导电或电介质层的沉积期间会严重损害半导体组件的性能或需使用在会损坏基材的温度下的热处理以改进性能。当使用其热稳定性一般低于无机基材的聚合物基材时尤其如此。
因此,本发明的目的是提供颗粒,由这种颗粒可制造稳定的、易加工的分散体,且借助该分散体可制得仅具有低杂质含量(特别是归因于改性剂的杂质)的半导体组件中的导电、电介质或半导体层。
该目的根据本发明通过表面改性的金属、金属卤化物、金属硫属元素化物、金属氮化物、金属磷化物、金属硼化物或金属磷酸盐颗粒或其混合物而实现,其中该颗粒具有1至500nm的平均粒径并且其表面经一种或多种选自式(I)、(II)及(III)的改性剂改性
其中
X1选自O、S及Se,
X2选自OH、OCH3、OC2H5、CO2H、OSi(R1)3-x-y(R2)y(R3)x,
x、y各自彼此独立地为0、1、2或3并且x与y之和不大于3,
R1、R2、R3、R4独立地选自H、C1-C10烷基,
X3选自O、S、Se及CH2,
n、m、p各自彼此独立地为0、1、2或3,优选为0、1、2,特别优选为1,
X4选自O、S、Se、C=O、-R4C=CH-、OCH2,
X5选自H、OH、OCH3、OC2H5、OSi(R1)(3-x-y)(R2)x(R3)y、CO2R5、OCO2R5,
R5选自C1-C4烷基,
X6选自SH、NH2、Si(R1 3-x-y)(R2)y(R3)x,
X7选自C1-C10亚烷基、O、S、Se、Te,
r为1至1000的整数,
R6选自H、C1-C10烷基及卤素。
所述改性剂具有的分解温度为在此温度下不会观察到基材中的变形、扭曲、分解或其他热变化,特别是当将改性颗粒涂覆于聚合物基材时。这使得可将这种改性剂从施加至聚合物基材的层中去除,而不会不利影响基材的结构。
所用改性剂的分解温度优选低于250℃。该分解温度也应高于50℃,优选高于75℃,更优选高于100℃,以避免过早分解。该分解温度优选低于200℃,特别优选低于150℃。对于本专利申请,该分解温度为有机改性剂丧失其原始结构并分解为较小分子(例如CO2)的温度。
这种改性剂在低温下分解,其甚至在涂覆聚合物基材时也不会引起任何变形及形成挥发性化合物。该热分解可针对丙二酸单乙酯的实例阐述如下,但本发明并不受限于此:
气态CO2以及挥发性乙酸乙酯的检出可借助IR、1H及13C{1H}-NMR而特别容易地证实。
在式(I)的改性剂中,优选其中X1为O或S,特别优选为O的那些。
X2优选选自OH、OCH3、COOH、OSi(R1)3-x-y(R2)y(R3)x,特别优选选自OH及OSi(R1)3-x-y(R2)y(R3)x。
还优选X3选自O、S、CH2,特别是O及CH2。X3特别优选为CH2。
还优选x及y各自彼此独立地为0、1或2,特别优选0或1。
还优选R1、R2、R3及R4独立地选自H及C1-C4烷基,特别优选H、甲基及乙基。
还优选n、m、p各自彼此独立为0、1、2,特别优选0或1。特别优选m、n或p中至少一个为0。
还优选X4选自O、S、C=O、-R4C=CH-及OCH2。还优选基团X3、X4及X5中至少一个包括C=O。
还优选X5选自H、OH、OSi(R1)(3-x-y)(R2)x(R3)y、CO2R5、OCO2R5,特别优选选自CO2R5。
还优选R5选自甲基、乙基及叔丁基,特别优选选自乙基及叔丁基。
对于本发明,卤素为F、Cl、Br及I。X6优选选自SH、OSi(R1 3-x-y)(R2)y(R3)x,特别优选OSi(R1 3-x-y)(R2)y(R3)x。
还优选X7选自C1-C4亚烷基,特别优选选自-CH2-及-C2H4-。
还优选r为1至100的整数,特别优选为1至10。
R6还优选选自H及C1-C4烷基,特别优选选自甲基及乙基。
进一步优选的改性剂为式Ia至Ih的那些:
其中n、p、X1、X2、X4及X5为如上所定义且R1、R2、R3选自C1-C10烷基,特别优选甲基、乙基及叔丁基。
式(I)改性剂的进一步优选的实施例为那些其中:
-n为0或n为1且X3选自O、S、Se、C=O、-HC=CH-、CH2,
-m为0或m=1且X4为选自O、S、C=O及OCH2,
-p为0或1及
-X5选自OCH3、OC2H5、CO2R5及OCO2R5。
特别优选的改性剂为下列结构IV至IX的化合物:
非常特别优选结构(VI)的改性剂。
颗粒可为金属、金属硫属元素化物、金属磷化物、金属硼化物、金属氮化物或金属磷酸盐颗粒或其混合物。金属硫属元素化物、金属磷化物、金属硼化物、金属磷酸盐和/或金属氮化物颗粒,特别是金属氧化物颗粒,可以是掺杂或未经掺杂的。
适于本发明目的的金属卤化物为金属氟化物、金属氯化物、金属溴化物以及金属碘化物,优选氟化物及氯化物。特别优选金属氯化物。
适于本发明目的的金属硫属元素化物为氧化物、硫化物、硒化物及碲化物,优选氧化物及硫化物。用于沉积半导体层的合适的金属硫属元素化物为氧化物,及例如CdS、CdSe、CdTe、ZnS、ZnSe、ZnTe、Cu-In-Ga-Se。金属硫属元素化物颗粒特别优选为金属氧化物颗粒。
优选的金属氮化物为AlN、GaN、InN、Al-Ga-N、In-Ga-N、Al-Ga-In-N。优选的金属磷化物为GaP、InP、Al-Ga-P、Ga-As-P、Al-Ga-In-P。优选的金属磷酸盐为稀土族元素(镧、铈、铽)的磷酸盐。
该颗粒,特别是金属氧化物颗粒,可为电介质、半导电或导电化合物。二元体系的实例为第2族金属氧化物(例如MgO)、第3族金属氧化物(例如Y2O3)、第4族金属氧化物(例如TiO2、ZrO2、HfO2)、第5族金属氧化物(例如V2O5、Nb2O5、Ta2O5)、第6族金属氧化物(例如Cr2O3、MoO3、WO3)、第7族金属氧化物(例如MnO2)、第8族金属氧化物(例如Fe2O3、Fe3O4、RuO2)、第9族金属氧化物(例如CoO、Co3O4)、第10族金属氧化物(例如NiO)、第11族金属氧化物(例如CuO、Cu2O)、第12族金属氧化物(例如ZnO、CdO)、第13族金属氧化物(例如B2O3、Al2O3、Ga2O3、In2O3)、第14族金属氧化物(例如SiO2、GeO2、SnO2、PbO、Pb3O4)、第15族金属氧化物(例如Sb2O3、Bi2O3、Bi2O3*Bi2O5)、镧系金属氧化物(La2O3、CeO2)。当然这种氧化物也可包含用来改进电子、热、磁及其他特性的其他掺杂元素(例如Sn-、Ge-、Mo-、F-、Ti-、Zr-、Hf-、Nb-、Ta-、W-、Te-掺杂的In2O3,Sb-、F-、As-、Nb-、Ta-掺杂的SnO2,Al-、Ga-、B-、In-、Y-、Sc-、F-、V-、Si-、Ge-、Ti-、Zr-、Hf-掺杂的ZnO,In-、Sn-掺杂的CdO)。如果需要,也可使用三元体系(例如Zn2SnO4、ZnSnO3、Zn2In2O5、Zn3In2O6、In4Sn3O12、CdIn2O4、MgIn2O4、GaInO3、CaTiO3、BaTiO3、MnFe2O4)或四元体系(例如Zn-In-Sn-O、Zn-In-Li-O、In-Ga-Zn-O)或金属氧化物的混合物。
用于沉积半导体层的优选金属氧化物为例如ZnO、Ga2O3、GeO2、CdO、In2O3、SnO2及其混合物或者其反应产物(三元体系:Zn-Sn-O、Zn-In-O;四元体系:Ga-In-Zn-O、Zn-In-Sn-O)。
用于沉积半导体层的特别优选的金属氧化物为ZnO及In2O3。
就半导体化合物而言,通常使用掺杂In-、Al-、Ga-、OH-、H-或固有缺陷(在晶格间位置处的O空位或Zn插入)来增加n型迁移率。p型迁移率通过例如掺杂Li、N而增加。
用于沉积半导体层的特别优选的金属氧化物为Al-或Mg-掺杂的ZnO、Ga-掺杂的ZnO、Al-掺杂的MgO、Sn-掺杂的ZnO、Bi-掺杂的ZnO以及Sn-掺杂的In2O3。
除上述金属化合物的颗粒外,也可使用金属颗粒。合适的金属颗粒选自Ag、Cu、Au及其与其他金属的合金。
所用颗粒的平均直径为1至500nm,优选2至200nm,更优选5至100nm,特别优选10至50nm。粒度分布可为单峰、双峰或多峰。颗粒可为球形或具有似微盘形或似棒状的形态。特别优选似棒状形态。
本发明进一步提供分散体,其包含
(a)具有1至500nm的平均初级粒径的金属、金属硫属元素化物、金属卤化物、金属氮化物、金属磷化物、金属硼化物或金属磷酸盐颗粒,
(b)一种或多种选自具有上式中一种的化合物的改性剂,及
(c)分散介质。
合适的分散介质原则上为颗粒可在加工条件下分散于其中的所有流体。优选使用在室温及大气压下为液体的有机化合物。优选使用非质子极性有机液体。进一步优选为具有低于200℃,特别优选低于100℃的沸点的有机液体。分散介质的偶极矩优选为3·10-30C·m至10·10-30C·m。
特别优选使用THF、二氯甲烷及/或氯仿,非常特别优选二氯甲烷。
除了以有机液体作为分散介质之外,也可使用他们与水的混合物。
改性剂可使颗粒,优选金属氧化物颗粒,稳定在纳米尺寸状态。由于一应用为由这些分散体制造薄层(例如通过旋涂、印刷等等),因此使用尽可能少的改性剂为明智的,因为一般在施加层之后必须再去除改性剂。另一方面,有必要使用足够的稳定剂来实现分散体的持久稳定作用。改性剂与金属氧化物的摩尔比可在2∶1至1∶60的范围内变化。优选摩尔比为1∶1至1∶30,更优选1∶5至1∶25。
分散体中颗粒的含量可为0.01至30重量%,优选为0.1至10重量%,特别是1至5重量%。
对于本发明,基材可为任何导电、半导电或不导电物质。基材的电、机械及化学特性的选择主要取决于应用。用于沉积导电、半导电或不导电层的合适基材一般为本领域技术人员已知的。
本发明分散体由于其可在较低温度下分解而特别适合施加层至聚合物基材,其仍然可为导电、半导电或不导电的。
特别合适的聚合物基材为聚酰亚胺(PI,例如可以商品名KAPTON获得)、聚酯萘二甲酸酯(PEN,例如可以商品名TEONEX Q 51获得)以及聚对苯二甲酸乙二醇酯(PET,例如可以商品名Hostaphan获得)。
改性颗粒可通过以下步骤制得:
a)使未经处理的金属、金属硫属元素化物、金属卤化物、金属氮化物、金属磷化物、金属硼化物或金属磷酸盐颗粒悬浮于非质子溶剂中,及
b)随后将此悬浮液与一种或多种式(I)改性剂混合以形成改性颗粒。以此方式获得的分散体可直接使用或可蒸发至干燥以获得改性颗粒。
他们可直接出售或随后再分散于另一分散介质中。
本方法将针对ZnO分散体的优选制造实例阐述于下,但本发明并不受其所限制。
首先,提供新沉淀的ZnO,例如通过使Zn盐(例如氯化锌或Zn(CH3COO)2·2H2O)与碱(例如KOH或NaOH)在分散介质(例如在醇如甲醇、乙醇、异丙醇中)中反应。例如通过使Zn盐与适当金属盐(例如在Al掺杂的情况下为AlCl3、Al(OiPr)3、乙酰丙酮铝)的混合物与碱在分散介质中反应获得掺杂的ZnO颗粒。副产品的沉淀颗粒(例如醋酸钾、氯化钾)可以本身已知的方式如通过过滤或离心分离出来。如有需要,可在分离沉淀颗粒之前借助薄膜法如纳米过滤、超过滤、微过滤或交叉流过滤将ZnO分散体浓缩。在沉淀之后以及在官能化之前,也可进行溶剂交换(例如借助交叉流过滤)。
随后以预定比率添加适当改性剂以致于形成金属氧化物颗粒的透明分散体。在由室温至所使用分散介质的沸点之间的温度下进行官能化。压力一般为1毫巴至50巴,优选为大气压(约1.013巴)。
以此方法获得的稳定分散体可以借助所有惯用的、基于液体的沉积方法施加至基材。合适的沉积方法特别是浸涂或旋涂或印刷方法(丝网印刷、柔版印刷、凹版印刷、喷墨印刷),但不限于此。所沉积的层厚度一般为10nm至10μm,优选为10nm至2μm,特别优选为20nm至200nm。
为制得最终的层(导电、半导电、电介质),将该层在约50℃至500℃,优选75℃至300℃,更优选100℃至200℃的温度下热处理。最高温度以及处理时间取决于基材的热稳定性、改性剂的分解温度以及待沉积的层的所需纯度。
在热处理期间,改性剂分解并以挥发性物质的形式(即在处理中以气态形式存在的物质)从沉积层去除。分解成挥发性物质必须实质上完全,但应当为至少60重量%,优选75重量%,更优选85重量%,特别优选90重量%。该热处理可在空气、氧气、氮气、氩气、氢气、蒸汽或混合物等中进行。热处理的持续时间一般为约1分钟至约30小时,优选30分钟至12小时。同样可以使用各种气体以多个步骤处理。
作为替代或另外,用来分解改性剂的能量输入可通过借助具有特定波长的灯或激光引入而进行。可能的波长范围为UV至IR(150nm至2500nm)。
当使用灯如Hg灯或准分子灯时,辐照连续进行1秒至24小时,优选1分钟至1小时的时间,并且有效功率密度为1mW/cm2至300kW/cm2,或以辐射脉冲持续时间为10ns至10秒并且有效功率密度为0.02KW/cm2至300kW/cm2的脉冲进行。
当使用激光时,优选以10ns至10秒的辐射脉冲持续时间及0.02kW/cm2至300kW/cm2的有效功率密度进行辐照。
除特定能量输入之外,另一任选选择为用酸性、碱性或pH-中性的化学品(例如SO2、N2O、N2H4、NH3、H2O)的蒸气处理该层,以从金属氧化物表面完全去除相对应的改性。
以丙二酸单乙酯为例,检验分解产物。需要最高200℃的温度以使优选分子(化合物(IV)至(IX))分解;分解可在惰性氛围(Ar、N2)或空气中进行。
本发明进一步提供了本发明分散体用于制造导电层、电介质层和/或半导电层的用途。在导电层的情况下,制造导电性颗粒(特别是金属)的分散体,并将其施加至合适的基材。在电介质层的情况下,使用金属氧化物颗粒,以及在半导电层的情况下,使用掺杂或未经掺杂的金属氧化物、金属硫属元素化物、金属氮化物、金属磷化物、金属卤化物、金属硼化物或金属磷酸盐颗粒。
本发明进一步提供制造半导体组件如TFT的方法:
使用掺杂或未经掺杂的金属氧化物颗粒作为TFT的半导体层。该颗粒可由分散体例如通过浸涂、旋涂或印刷方法加工以形成TFT并(如必要的话)烘烤(退火)。TFT结构如底栅、顶栅、顶触点、底触点等并不受到任何限制。电介质可为所有可能的有机材料、无机材料或有机-无机混合材料。栅、源极及漏极接触材料为导电材料(例如Al、Au、Ag、Ti/Au、Cr/Au、ITO、Si、PEDOT/PSS等)。合适的基材还包括特别是具有低分解温度的聚合及挠性材料以及其他热不稳定性基材,但不受限于此。基材、栅、源极及漏极接触材料以及电介质并不受到任何基本的限制,并且可根据化学/物理相容性、加工方法以及期望用途而选择。金属、金属氧化物、金属氮化物、金属磷化物、金属卤化物、金属硼化物或金属磷酸盐颗粒以及本发明分散体同样可用于该TFT组件。
最后,本发明颗粒及分散体可用于沉积透明导电层,其可用于许多电子组件中并可取代迄今为止所使用的层。对于本专利申请,透明意指在400nm至800nm范围内的电磁辐射的透射超过80%。
实施例
实施例1:由Zn(OAc)2制备ZnO
首先将1118ml 2-丙醇及36.81g Zn(OAc)2*2H2O置于2L密闭的搅拌装置中并加热至75℃。同时(in parallel thereto)将584ml 2-丙醇中的16.38g氢氧化钾加热至75℃。随后将氢氧化钾/2-丙醇溶液添加至Zn(OAc)2悬浮液中。将该混合物在75℃下加热一小时同时以425rpm搅拌。冷却至室温后,使形成的氧化锌沉降过夜。借助抽吸滤出上清液2-丙醇并随后用每次500ml的THF洗涤该氧化锌两次。借助抽吸滤出上清液THF。
实施例2:借助乙基三甲基甲硅烷基丙二酸酯官能化ZnO
将来自实施例1的湿氧化锌与1L氯仿混合。将200g ZnO在氯仿中的悬浮液(ZnO含量为1.6g(19.66mmol))与3.93mmol乙基三甲基甲硅烷基丙二酸酯(来自Fluka)在室温下混合。在添加数秒后,该溶液变澄清。在室温下将该混合物另外搅拌15分钟并随后浓缩该分散体使ZnO含量成为4重量%。
具有平均直径约10nm的ZnO颗粒可通过粒度分布(图1)的测定及TEM分析(图2)而检测。
实施例3:3-氧代戊二酸单乙酯的合成
将14.45g(0.099mol)3-氧代戊二酸(1,3-丙酮二甲酸)添加至在100ml单颈烧瓶中的10.2g(0.10mol)醋酸酐中。用力摇晃生成的浆料直到固体变得均化为止从而形成黄色的油。当进一步摇晃时,该混合物变温热且白色固体(3-氧代戊二酸酐)自发地沉淀。再摇晃该混合物5分钟并使烧瓶在RT下静置12小时。随后将该混合物过滤并且用每次5ml的甲苯将固体洗涤三次,以及用7ml正己烷洗涤一次。随后将残留物在真空干燥箱中储存5小时。
在第二步骤中,将1.84g所形成的酸酐溶于30ml绝对乙醇中并立即将该溶液在旋转蒸发器(2.10-3毫巴,RT)上蒸发。留下浅黄色油,将其储存于-20℃下,使其固化。
实施例4:借助3-氧代戊二酸单乙酯改性ZnO(ZnO与改性剂的摩尔比=3∶1)
将来自实施例1的湿氧化锌与1L二氯甲烷混合。将200g ZnO在二氯甲烷中的悬浮液(ZnO含量为1.6g(19.66mmol))与来自实施例3的1.14g 3-氧代戊二酸单乙酯(6.55mmol)在室温下混合;该分散体立即变澄清。随后在旋转蒸发器上在40℃下将二氯甲烷馏出并将残留物在减压下另外干燥4小时。
根据所得干燥残留物的TG分析(加热速率3℃/min至200℃,在200℃下10min,然后3℃/min至400℃;在氩气中),在低于200℃的温度下已去除所用改性剂的91%。实验测得的质量损失为37.8重量%;所使用的改性剂/(ZnO+改性剂)比为41.6重量%。
相应的TG分析显示于图3。
实施例5:借助3-氧代戊二酸单乙酯改性ZnO(ZnO与改性剂的摩尔比=5∶1)
将氧化锌在二氯甲烷中的100g分散体(0.80g ZnO(9.83mmol))与来自实施例3的0.34g(1.97mmol)3-氧代戊二酸单乙酯通过搅拌混合。该分散体立即变澄清并随后将其蒸发至干燥。随后将所形成的浅黄色粉末在减压下干燥4小时。
根据相应干燥粉末的TG分析(加热速率3℃/min至200℃,在200℃下10分钟,然后3℃/min至400℃;在氩气中),在低于200℃的温度下已去除所用改性剂的88%。实验测得的质量损失为26.6重量%;所使用的改性剂/(ZnO+改性剂)比为30.1重量%。
相应的TG分析显示于图4。
实施例6:借助3-氧代戊二酸单乙酯改性ZnO(ZnO与改性剂的摩尔比=29∶1)
将来自实施例1的湿氧化锌与1L二氯甲烷混合。将200g ZnO在二氯甲烷中的悬浮液(ZnO含量为1.6g(19.66mmol))与0.12g 3-氧代戊二酸单乙酯(0.67mmol)在室温下混合;该分散体立即变澄清。随后在旋转蒸发器上在40℃下将二氯甲烷馏出并将残留物在减压下另外干燥4小时。
对比例A:借助2-[2-(2-甲氧基乙氧基)乙氧基]醋酸官能化ZnO
将来自实施例1的湿氧化锌与1L THF混合。添加3.5g 2-[2-(2-甲氧基乙氧基)乙氧基]醋酸(Fluka)至该悬浮液中。将形成的混合物在搅拌的同时加热至沸腾,并在此温度下维持30分钟。该悬浮液变澄清。随后在旋转蒸发器上在60℃下将THF馏出并将残留物在减压下另外干燥4小时。
根据所得官能化ZnO粉末的TG分析(加热速率5℃/min至200℃,在200℃下60分钟,然后5℃/min至500℃;在空气中),在低于200℃的温度下仅去除23%的有机成分。在室温至200℃的温度范围内的实验测得质量损失=5.8重量%;从室温至500℃的总损失=25.3重量%。
相应的TG分析显示于图5。
对比例B:借助乙氧基乙酸官能化ZnO
将来自实施例1的湿氧化锌与1L THF混合。将5g乙氧基乙酸(Fluka)加入该悬浮液中。将形成的混合物在搅拌的同时加热至沸腾并在此温度下维持30分钟。该悬浮液变澄清。随后在旋转蒸发器上在60℃下将THF馏出并将残留物在减压下另外干燥4小时。
根据所得官能化ZnO粉末的TG分析(加热速率5℃/min至200℃,在200℃下60分钟,然后5℃/min至500℃;在空气中),在低于200℃的温度下仅去除28%的有机成分(在室温至200℃的温度范围内的实验测得质量损失为8.7重量%;从室温至500℃的总损失为31.6重量%)。
相应的TG分析显示于图6。
实施例7:TFT(底栅、顶触点结构)的制造
将3滴根据实施例6的在二氯甲烷中的分散体(ZnO含量为4重量%)与5体积%丁基乙二醇混合并通过旋涂(4000rpm,30s)施加至具有SiO2电介质层(200nm)的清洁的Si(经掺杂)基材上。随后将该试样加热至200℃并在200℃下维持1小时。
通过铝的热气相沉积(thermal vapor deposition)制得顶触点源极/漏极结构。相应晶体管的代表性起始曲线(AK)与转移曲线(TK)描绘于图7和8(VD:源极与漏极之间的电压,VG:源极与栅之间的电压,ID:源极与漏极之间的电流)。
测得以下平均参数:迁移率μ:3*10-3cm2/(V*s),开/关比:105,VT阈电压:12V。
Claims (20)
1.包括金属、金属卤化物、金属硫属元素化物、金属氮化物、金属磷化物、金属磷酸盐、金属硼化物或其混合物的颗粒,其中所述颗粒具有1至500nm的平均粒径,并且它们的表面经一种或多种选自式(I)、(II)及(III)的改性剂改性:
其中
X1选自O、S及Se,
X2选自OH、OCH3、OC2H5、COOH、OSi(R1)3-x-y(R2)y(R3)x,
x、y各自彼此独立地为0、1、2或3且x与y之和不大于3,
R1、R2、R3、R4独立地选自H、C1-C10烷基,
X3选自O、S、Se及CH2,
n、m、p各自彼此独立地为0、1、2或3,优选为0、1、2,特别优选为1,
X4选自O、S、Se、C=O、-R4C=CH-、OCH2,
X5选自H、OH、OCH3、OC2H5、OSi(R1)(3-x-y)(R2)x(R3)y、COOR5、OCOOR5,
R5选自C1-C4烷基,
X6选自SH、NH2、OSi(R1 3-x-y)(R2)y(R3)x,
X7选自C1-C10亚烷基、O、S、Se、Te,
r为1至1000的整数,
R6选自H、C1-C10烷基及卤素。
2.根据权利要求1的颗粒,其中所述颗粒为金属氧化物。
3.根据权利要求2的颗粒,其中所述金属氧化物包含至少一种选自Ti、Zr、Zn、Ga、In、Ge、Sn、Ce、Sb、Bi的金属。
4.根据权利要求3的颗粒,其中所述金属氧化物选自ZnO、In2O3、SnO2、Ga2O3、Zn2SnO4、ZnSnO3、Zn2In2O5、Zn3In2O6、In4Sn3O12、GaInO3、无定型In-Ga-Zn氧化物。
5.根据前述权利要求中任一项的颗粒,其中所述颗粒选自Sn-、Al-、Sb-、Ga-、Bi-、In-、Mg-、Li-、H-、OH-、N-掺杂的ZnO,Al-的掺杂MgO以及Sn-掺杂的In2O3。
6.根据前述权利要求中任一项的颗粒,其中所述颗粒具有5至100nm,特别是10至50nm的平均直径。
9.根据前述权利要求中任一项的颗粒,其中所述改性剂与颗粒的摩尔比为2∶1至1∶60,尤其是1∶1至1∶30,特优优选1∶25至1∶5。
10.根据前述权利要求中任一项的颗粒,其中所述改性剂的分解温度低于250℃,尤其是低于200℃。
11.一种制造根据前述权利要求中任一项的改性颗粒的方法,其包括
a)将未经处理的颗粒悬浮于非质子溶剂中,及
b)随后将其与一种或多种如权利要求1所定义的式(I)改性剂混合以形成改性颗粒。
12.一种分散体,其包含
(a)具有1至500nm的平均粒径的金属、金属硫属元素化物、金属卤化物、金属氮化物、金属磷化物、金属硼化物、金属磷酸盐颗粒或其混合物,
(b)一种或多种式(I)、(II)或(III)的改性剂:
其中
X1选自O、S及Se,
X2选自OH、OCH3、OC2H5、COOH、OSi(R1)3-x-y(R2)y(R3)x,
x、y各自彼此独立地为0、1、2或3且x与y之和不大于3,
R1、R2、R3、R4独立地选自H、C1-C10烷基,
X3选自O、S、Se及CH2,
n、m、p各自彼此独立地为0、1、2或3,优选为0、1、2,特别优选为1,
X4选自O、S、Se、C=O、-R4C=CH-、OCH2,
X5选自H、OH、OCH3、OC2H5、OSi(R1)(3-x-y)(R2)x(R3)y、COOR5、OCOOR5,
R5选自C1-C4烷基,
X6选自SH、NH2、OSi(R1 3-x-y)(R2)y(R3)x,
X7选自C1-C10亚烷基、O、S、Se、Te,
r为1至1000的整数,
R6选自H、C1-C10烷基及卤素,
(c)分散介质。
13.根据权利要求12的分散体,其中所述分散介质选自具有低于100℃的沸点的有机液体。
14.根据权利要求12或13的分散体,其中所述分散介质选自具有3至10·10-30C·m的偶极矩的有机液体。
15.根据权利要求12至14中任一项的分散体,其中所述分散体具有0.1至10重量%,尤其是1至5重量%的分散颗粒含量。
16.一种将层沉积于基材上的方法,其包括下列步骤:
a)制造包含权利要求1至11中任一项的表面改性颗粒及分散介质的分散体,
b)将所述分散体施加至基材,
c)去除所述分散介质,
d)通过在100℃至500℃下的热处理或用电磁辐射照射将改性剂转化为挥发性物质。
17.根据权利要求16的方法,其中所述基材为聚合物基材。
18.一种复合物,其包含基材和可通过权利要求16或17的方法获得的层。
19.根据权利要求18的复合物,其中所述层为导电且透明的。
20.一种电子组件,尤其是FET,其包含可通过权利要求16或17的方法获得的层或根据权利要求18或19的复合物。
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AU2009324379A1 (en) | 2008-12-11 | 2011-07-28 | Basf Se | Enrichment of valuable ores from mine waste (tailings) |
US8940814B2 (en) * | 2008-12-12 | 2015-01-27 | Basf Se | Dispersions comprising functionalized oxidic nanoparticles |
EA022857B1 (ru) | 2009-03-04 | 2016-03-31 | Басф Се | Магнитное разделение руд цветных металлов путем многостадийного кондиционирования |
CN102612406A (zh) * | 2009-11-20 | 2012-07-25 | 巴斯夫欧洲公司 | 用于制备羧酸和/或羧酸酐的在至少一个催化剂层中具有锑酸钒的多层催化剂及具有低热点温度的制备邻苯二甲酸酐的方法 |
CN102668086B (zh) | 2009-12-18 | 2016-01-06 | 巴斯夫欧洲公司 | 位于具有可由溶液低温加工的电介质的机械柔性聚合物衬底上的金属氧化物场效应晶体管 |
US20110230668A1 (en) * | 2010-03-19 | 2011-09-22 | Basf Se | Catalyst for gas phase oxidations based on low-sulfur and low-calcium titanium dioxide |
TW201206896A (en) | 2010-04-13 | 2012-02-16 | Basf Se | Process for controlling a gas phase oxidation reactor for preparation of phthalic anhydride |
CN102947218B (zh) | 2010-04-23 | 2016-05-11 | 皮瑟莱根特科技有限责任公司 | 纳米晶体的合成、盖帽和分散 |
JP2013525250A (ja) | 2010-04-28 | 2013-06-20 | ビーエーエスエフ ソシエタス・ヨーロピア | 溶液中で亜鉛錯体を調製する方法 |
US8865000B2 (en) | 2010-06-11 | 2014-10-21 | Basf Se | Utilization of the naturally occurring magnetic constituents of ores |
US8859459B2 (en) | 2010-06-30 | 2014-10-14 | Basf Se | Multilayer catalyst for preparing phthalic anhydride and process for preparing phthalic anhydride |
US9212157B2 (en) | 2010-07-30 | 2015-12-15 | Basf Se | Catalyst for the oxidation of o-xylene and/or naphthalene to phthalic anhydride |
US9376457B2 (en) | 2010-09-03 | 2016-06-28 | Basf Se | Hydrophobic, functionalized particles |
JP2014503446A (ja) | 2010-10-27 | 2014-02-13 | ピクセリジェント・テクノロジーズ,エルエルシー | ナノ結晶の合成、キャップ形成および分散 |
US9359689B2 (en) | 2011-10-26 | 2016-06-07 | Pixelligent Technologies, Llc | Synthesis, capping and dispersion of nanocrystals |
KR101978835B1 (ko) * | 2012-03-16 | 2019-05-15 | 한국전자통신연구원 | 박막 트랜지스터 |
WO2014119592A1 (ja) * | 2013-02-04 | 2014-08-07 | 独立行政法人産業技術総合研究所 | 抵抗体、誘電体等の電子部品用無機材料ペースト及び該無機材料ペーストの製造方法 |
FI130559B (en) * | 2021-06-23 | 2023-11-21 | Turun Yliopisto | Semiconductor structure, semiconductor device and method |
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US2303330A (en) | 1942-02-02 | 1942-12-01 | New Jersey Zinc Co | Zinc oxide |
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DE10063092A1 (de) | 2000-12-18 | 2002-06-20 | Henkel Kgaa | Nanoskalige Materialien in Hygiene-Produkten |
JP2003073122A (ja) * | 2001-09-04 | 2003-03-12 | Mitsui Chemicals Inc | 無機微粒子分散液及びそれを用いて製造される複合材料組成物 |
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JP2004010807A (ja) * | 2002-06-10 | 2004-01-15 | Toyo Ink Mfg Co Ltd | 水性分散体の製造方法 |
US20050182153A1 (en) * | 2002-06-12 | 2005-08-18 | Koji Yokoi | Porous metal oxide material in flake form, method for producing the same and cosmetic, coating material resin composition ink composition and paper comprising the same |
JP2004182483A (ja) * | 2002-11-29 | 2004-07-02 | Mitsubishi Chemicals Corp | 酸化亜鉛超微粒子の製造方法 |
DE10257388A1 (de) | 2002-12-06 | 2004-06-24 | Sustech Gmbh & Co. Kg | Nanopartikuläres redispergierbares Zinkoxidpulver |
DE10304849A1 (de) | 2003-02-06 | 2004-08-19 | Institut für Neue Materialien gemeinnützige Gesellschaft mit beschränkter Haftung | Chemomechanische Herstellung von Funktionskolloiden |
WO2004087577A1 (ja) | 2003-03-31 | 2004-10-14 | Toto Ltd. | 表面改質二酸化チタン微粒子とその分散液、およびその製造方法 |
JP5014796B2 (ja) * | 2004-09-30 | 2012-08-29 | 株式会社カネカ | ポリマー修飾金属カルコゲン化物ナノ粒子の製造方法 |
DE102004048230A1 (de) | 2004-10-04 | 2006-04-06 | Institut für Neue Materialien Gemeinnützige GmbH | Verfahren zur Herstellung von Nanopartikeln mit maßgeschneiderter Oberflächenchemie und entsprechenden Kolloiden |
DE102005007374A1 (de) | 2005-02-17 | 2006-08-24 | Universität Ulm | Nanopartikel und deren Verwendung |
JP4918994B2 (ja) * | 2005-05-30 | 2012-04-18 | 住友電気工業株式会社 | 金属被膜の形成方法および金属配線 |
DE102005047807A1 (de) | 2005-06-04 | 2006-12-07 | Solvay Infra Bad Hönningen GmbH | Modifizierte Nanopartikel |
US7691666B2 (en) | 2005-06-16 | 2010-04-06 | Eastman Kodak Company | Methods of making thin film transistors comprising zinc-oxide-based semiconductor materials and transistors made thereby |
US7402506B2 (en) * | 2005-06-16 | 2008-07-22 | Eastman Kodak Company | Methods of making thin film transistors comprising zinc-oxide-based semiconductor materials and transistors made thereby |
JP4738931B2 (ja) * | 2005-07-29 | 2011-08-03 | 富士フイルム株式会社 | ナノ粒子分散液、それを用いた半導体デバイスの製造方法及び半導体デバイス |
KR100768632B1 (ko) * | 2006-10-30 | 2007-10-18 | 삼성전자주식회사 | 나노입자의 분산방법 및 이를 이용한 나노입자 박막의제조방법 |
KR20080108767A (ko) * | 2007-06-11 | 2008-12-16 | 삼성에스디아이 주식회사 | 전극 단자부 코팅재 및 이를 구비한 플라즈마 디스플레이패널 |
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- 2009-08-28 EP EP09782305A patent/EP2321373A1/de not_active Withdrawn
- 2009-08-28 KR KR1020117007826A patent/KR20110066162A/ko active IP Right Grant
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Publication number | Publication date |
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JP2012501941A (ja) | 2012-01-26 |
EP2321373A1 (de) | 2011-05-18 |
CN102144004B (zh) | 2014-11-26 |
JP5599797B2 (ja) | 2014-10-01 |
TWI488815B (zh) | 2015-06-21 |
US20110163278A1 (en) | 2011-07-07 |
TW201016614A (en) | 2010-05-01 |
US8734899B2 (en) | 2014-05-27 |
KR20110066162A (ko) | 2011-06-16 |
WO2010026102A1 (de) | 2010-03-11 |
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