CN105492447B - 用于制备铟烷氧化物化合物的方法、可由该方法制备的铟烷氧化物化合物及其用途 - Google Patents
用于制备铟烷氧化物化合物的方法、可由该方法制备的铟烷氧化物化合物及其用途 Download PDFInfo
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- CN105492447B CN105492447B CN201480036888.2A CN201480036888A CN105492447B CN 105492447 B CN105492447 B CN 105492447B CN 201480036888 A CN201480036888 A CN 201480036888A CN 105492447 B CN105492447 B CN 105492447B
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- 229910052738 indium Inorganic materials 0.000 title claims abstract description 56
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- 238000000034 method Methods 0.000 title claims abstract description 31
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 150000001875 compounds Chemical class 0.000 claims abstract description 21
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 8
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 7
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 7
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 7
- 125000000467 secondary amino group Chemical class [H]N([*:1])[*:2] 0.000 claims abstract description 6
- 239000004020 conductor Substances 0.000 claims abstract 2
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- 239000000460 chlorine Substances 0.000 description 5
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- 229910044991 metal oxide Inorganic materials 0.000 description 5
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
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- 229910021617 Indium monochloride Inorganic materials 0.000 description 4
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Abstract
本发明涉及一种铟烷氧化物化合物,其可通过在通式ROH醇(其中R=烷基)的存在下将三卤化铟InX3(其中X=F、Cl、Br、I)与式R′2NH(其中R′=烷基)的仲胺以相对于三卤化铟8∶1至20∶1的摩尔比反应制备;本发明还涉及制备所述化合物的方法;及其用于制造含氧化铟或(半)导体层的用途。
Description
本发明涉及用于制备铟烷氧化物化合物的方法,可由该方法制备的铟烷氧化物化合物以及其用途。
相比于许多其它方法(例如化学气相沉积(CVD)),通过印刷和其它液体沉积方法制造半导体电子组件层能够获得低的多的制造成本,因为此处半导体可以连续操作沉积。此外,在相对低加工温度的情况下,也变得可在柔性基板上操作,并且可(特别是在非常薄层的情况下和尤其是在氧化的半导体的情况下)实现印刷层的光学透明度。应当理解此处和以下的半导体层是指对于在栅-源电压50V和源-漏电压为50V下通道长度为20μm的组件具有1-50cm2/Vs的载流子迁移率的层。
因为通过印刷方法制备的组件层的材料关键性地决定了特定的层性能,所以其选择对于含有该组件层的任何组件具有重要的影响。印刷半导体层的重要参数是其特定的载流子迁移率,及在其制备过程期间所使用的可印刷前驱体的加工性和加工温度。所述材料应当具有良好的载流子迁移率并且可以由溶液并且在显著低于500℃的温度下制备以适用于多种应用和基板。许多新型应用同样需要的是所获得的半导体层的光学透明度。
由于3.6eV和3.75eV之间的大的能带隙(针对通过气相沉积所施加的层测量,H.S.Kim,P.D.Byrne,A.Facchetti,T.J.Marks;J.Am.Chem.Soc.2008,130,12580-12581),氧化铟(氧化铟(III),In2O3)是有希望的并且因此广泛用于半导体。厚度数百纳米的薄膜在550nm下大于90%的可见光谱区域中可以额外地具有高透明度。在极度高度有序的氧化铟单晶中,额外可能测得最高160cm2/Vs的载流子迁移率。然而,迄今尚未可以通过溶液处理获得这种值(H.Nakazawa,Y.Ito,E.Matsumoto,K.Adachi,N.Aoki,Y.Ochiai;J.Appl.Phys.2006,100,093706;和A.Gupta,H.Cao,Parekh,K.K.V.Rao,A.R.Raju,U.V.Waghmare;J.Appl.Phys.2007,101,09N513)。
氧化铟通常特别与氧化锡(IV)(SnO2)一起使用作为半导体混合氧化物ITO。由于ITO层相对高的导电性和同时在可见光谱区域的透明度,所以其用途之一是用在液晶显示器(LCD)中,尤其用作“透明电极”。这些通常掺杂的金属氧化物层在工业上特别通过在高真空下高成本的气相沉积方法制备。归因于ITO涂覆基板的重大经济利益,目前存在一些用于含氧化铟层的涂覆方法,特别是基于溶胶-凝胶技术。
原则上,对于经由印刷方法制备氧化铟半导体存在两种选择:1)粒子概念,其中(纳米)颗粒存在于可印刷分散液中,并且在印刷操作之后通过烧结操作转化成所需的半导体层,和2)前驱体概念,其中至少一种可溶或可分散的前驱体,在印刷适当的组合物之后,转化成含氧化铟的层。相比于使用前驱体,颗粒概念具有两个显著的缺点:首先,颗粒分散液具有胶体不稳定性,其必须使用分散添加剂(其不利于后续层性能);第二,许多可使用的颗粒(例如由于钝化层)通过烧结仅不完全地形成层,使得一些微粒结构仍然在层中出现。在其颗粒边界处,存在相当高的颗粒-颗粒电阻,这降低了载流子迁移率并且增加一般层电阻。
存在多种制备氧化铟层的前驱体。例如,除了铟盐之外,可以使用铟烷氧化物(均配(homoleptic)化合物,即仅具有铟和烷氧化物基团的化合物)作为前驱体以制备含氧化铟的层。
例如,Marks等描述了使用包含溶解于甲氧基乙醇的盐InCl3和碱性单乙醇胺(MEA)的含前驱体的组合物制备的组分。在旋涂该组合物之后,通过在400℃下的热处理获得了相应的氧化铟层(H.S.Kim,P.D.Byrne,A.Facchetti,T.J.Marks;J.Am.Chem.Soc.2008,130,12580-12581和补充信息)。
WO 2011/072887 A1描述了制备卤化铟(III)二烷氧化物的方法及其制备含氧化铟层的用途。用于由这些卤化铟(III)二烷氧化物制备含氧化铟层的方法公开于WO 2011/073005 A2中。
然而,卤化铟(III)二烷氧化物,迄今仍未形成具有足够好的电性能的含氧化铟层。铟氧代烷氧化物获得更好的层性能,例如以下通式的化合物:In6O2X6(OR)6(R′CH(O)COOR″)2(HOR)x(HNR″′2)y、In7O2(OH)(OR)12X4(ROH)x和MxOy(OR)z[O(R′O)eH]aXbyc[R″OH]d,其公开于WO 2012/010427 A1、WO 2012/010464 A1和在本申请案的优先权日期尚未公开的德国申请DE 10 2012 209918。
尽管已知这种改善,但仍然需要有关层形成性能和所获得层性能的改进。更具体地,合适的前驱体应当:
-具有良好的加工性,尤其是在空气下的加工性,
-均匀地转化成氧化物,
-在最小温度下转化成氧化物,和
-形成具有优异电性能的层。
这种要求的复杂概况通过铟烷氧化物化合物实现,所述铟烷氧化物化合物可通过在通式ROH的醇(其中R=烷基)的存在下将
-三卤化铟InX3,其中X=F、Cl、Br、I
-与式R′2NH的仲胺,其中R′=烷基,以相对于三卤化铟8∶1至20∶1的摩尔比反应制备。
在反应中以相对于三卤化铟8∶1至15∶1,甚至更好的8∶1至12∶1的摩尔比使用仲胺时,可以以铟烷氧化物化合物制备特别良好的层。
应当理解本发明上下文中的铟烷氧化物化合物是指具有至少一个铟原子和至少一个烷氧化物基团的化合物,其可以在醇的存在下通过三卤化物与仲胺的上述反应制备。可通过根据本发明的方法获得的这些溶解的化合物的结构的测定是困难的。然而,假定得到的化合物是卤化的铟氧代烷氧化物化合物。相应的固态结构已经通过X射线结构分析测定。假设这些混合物的相似结构也存在于溶液中。铟氧代烷氧化物是可以离子形式存在并且通过氧代基团桥接的铟团簇,其中不由氧代基团配位的价态至少部分由烷氧基配位。对于可由根据本发明的方法获得的铟烷氧化物化合物,假设它们在合成后通常以盐的形式存在,尤其是以配位至阳离子的卤化铟氧代烷氧化物阴离子的形式存在。
特别优选的方法产物是通式[In6(O)(OR)12X6]2-Am z(ROH)x的铟烷氧化物化合物,其中R=烷基,X=F、Cl、Br、I,A=阳离子,z=阳离子的价态,m*z=2和x=0至10,其可以尤其使用9∶1至10∶1比率的仲胺制备。所述化合物可以通过醇分子ROH配位并且任选地在反应中存在其他溶剂。
典型的阳离子是铵离子[NHyR4-y]+,优选式[NH2R2]+的铵离子。
非常特别优选的化合物是[In6(O)(OMe)12Cl6]2-[NH2R2]+ 2(MeOH)2,其可以通过使用InCl3、Me2NH(后者以9∶1至10∶1的比例)和MeOH(甲醇)制备。经由X射线结构分析测定的其结构示于图1中。
本发明进一步提供了用于制备铟烷氧化物化合物的方法,其中在通式ROH的醇(其中R=烷基)的存在下将
-三卤化铟InX3,其中X=F、Cl、Br、I
-与式R′2NH的仲胺,其中R′=烷基,以相对于三卤化铟8∶1至20∶1的摩尔比反应。
式InX3的三卤化铟是本领域技术人员已知的并且可以从市面获得。
式R′2NH的仲胺(其中R′=烷基)同样形成现有技术的一部分。优选,烷基R′是式CnH2n+1(其中n=1至10)的直链、支化或环状C1-至C10-烷基。一个或两个不同仲胺的两个R′基团也可以一起形成亚烷基CnH2n。相应地,可使用的化合物为例如二甲胺、二乙胺、二丙胺、吡咯烷、哌啶和吡咯。优选的R′基团是甲基、乙基、正丙基和异丙基基团。最优选地,R′基团是甲基,因为其导致特别良好的产率和特别稳定的化合物。
所使用的醇ROH优选是具有式CnH2n+1(其中n=1至10)的直链、支化或环状C1-至C10-烷基的那些。此处优选的R基团也为甲基、乙基、正丙基和异丙基。最优选,R基团是甲基。
基于所有组分的总质量,三卤化铟优选以0.1-50wt%,更优选1-25wt%,最优选2-10wt%的比例使用。
三卤化铟可以溶解,即解离或以分子水平与溶剂分子/醇分子络合,或分散在液相中。
基于所有组分的总质量,醇ROH优选以50-99.9wt%,更优选75-99wt%,最优选80-96wt%的比例使用。
反应混合物可以进一步包括至少一种相对于反应惰性的液体溶剂或分散介质,即在反应条件下不与三卤化铟反应的溶剂/分散介质或多种溶剂/分散介质的混合物。优选可使用的是非质子溶剂,尤其是选自非质子非极性溶剂的组的那些,即烷烃、取代的烷烃、烯烃、炔烃、不具有或具有脂肪族或芳香族取代基的芳族化合物,卤代烃和四甲基硅烷,和选自非质子极性溶剂的组的那些,即醚、芳香醚、取代醚、酯或酸酐、酮、叔胺、硝基甲烷、DMF(二甲基甲酰胺)、DMSO(二甲亚砜)或碳酸丙烯酯。
如果至少一种相对于反应惰性的这种液体溶剂或分散介质存在于反应混合物中,那么其比例优选是1-50wt%,更优选1-25wt%,最优选1-10wt%,基于所有组分的总质量。
优选在反应中以相对于三卤化铟为8∶1至15∶1,甚至更好地以8∶1至12∶1的摩尔比使用仲胺,因为随后可以特别高的产率制备特别良好适用于层制造的铟烷氧化物化合物。
优选地,根据本发明的方法通过最初将三卤化铟加入到醇ROH中来进行。以气体形式,以液体形式或溶解在溶剂中(尤其是包含ROH作为溶剂)添加仲胺。
同样优选在SATP条件下(25℃和1.013巴)添加。
因为反应可以此方式特别有效地控制并且获得特别好的铟烷氧化物化合物,所以二烷基胺优选以每小时、相对于每摩尔卤化铟为0.5-5mol的速率添加,优选每小时、相对于每摩尔卤化铟为1.15-2.60mol。
进一步优选地,在添加所有的组分之后,加热反应混合物。优选地,反应混合物在1-10小时的时间内被加热至40℃和70℃之间的温度。进一步优选地,反应混合物在1-5小时的时间内被加热至45℃和60℃之间的温度。之后,将反应混合物冷却。
在反应结束之后,优选将通常沉淀出的产物或产物混合物与反应组合物的其它成分分开。这优选通过过滤进行。优选地,将分离的产物混合物额外干燥并且用合适的溶剂洗涤。
特别好的铟烷氧化物化合物是在分离和任选干燥和/或洗涤之后获得的产物或产物混合物重结晶的结果。优选地,重结晶在醇ROH中进行,所述醇ROH也可用于该化合物的合成。优选地,重结晶通过将分离的产物或产物混合物溶解在沸腾的醇中并且随后在-30℃至0℃的温度下重结晶进行。将上层溶剂丢弃并且可以进一步使用结晶产物。
本发明的化合物特别有利地适用于尤其通过湿化学方法制备具有改善电性能的含氧化铟涂层。该改善是令人意外的,因为金属氧化物的前驱体通常在具有最小结晶倾向的物质中寻找。然而,许多本发明化合物为因此已经具有微晶结构的团簇化合物。所需的金属氧化物层也应当与结晶特征相比具有更多的无定形特征,以具有特别良好的电性能。与预期相反的,使用本发明的化合物可以制备特别均匀的层。
在这种情况下含氧化铟的涂层应当被理解为是指氧化铟层和主要包含氧化铟和其它金属和/或金属氧化物的层。在本发明的上下文中氧化铟层应当被理解为是指可从所提及的铟烷氧化物制备的金属层,其主要具有铟原子或离子,铟原子或离子主要以氧化形式存在。任选地,氧化铟层还可以包括来自不完全转化的卤素或烷氧化物组分和/或氮、氢和/或碳。此也应用于主要包含氧化铟和其它金属和/或金属氧化物的层,条件是这些也包括其它金属和/或金属氧化物。
本发明化合物额外具有令人意外的优点,即其可以特别有效地用于制备电子组件的导电或半导体含氧化铟的层,尤其用于制造(薄膜)晶体管、二极管或太阳能电池。
以下实施例旨在进一步阐明本发明的主题,而本身无任何限制作用。
发明实施例
合成
在30L无残留水分的反应器中,通过搅拌将1.30kg的氯化铟(III)(InCl3,5.9mol)悬浮在17.38kg的干燥甲醇和保护性气体气氛中。在室温下通过质量流量控制器计量加入二甲胺(2.57kg,57mol)(0.86kg/h,约4小时),在此期间可以观察到略微放热反应。然后,将反应混合物保持在50℃的温度下2小时,冷却至室温并且过滤。用4×500ml的干燥甲醇洗涤滤渣并且在减压下(0.1毫巴)干燥8小时。将该材料溶解在沸腾的甲醇中并且在-20℃下结晶。
制备配制物
将获得的材料以50mg/ml的浓度溶解在1-甲氧基-2-丙醇中。所获得的浓缩物如下配制:1份浓缩物对2份1-甲氧基-2-丙醇对1份乙醇。向该配制物中加入另外3wt%的四氢糠醇(THFA,tetrahydrofurfurylalcohol)。所有使用的溶剂是无水的(<200ppm的H2O)并且混合在惰性条件下进行(同样无水)。所获得的配制物最终通过200nm PTFE过滤器过滤。
涂覆
使用100μl的上述配制物润湿具有约15mm边缘长度和具有约200nm氧化硅涂层厚度和ITO/金指状结构的掺杂硅基板。以2000rpm(30秒)进行旋涂。在此涂覆操作之后,立即用来自汞蒸汽灯且在150-300nm的波长范围的UV辐射照射涂覆的基板10分钟。随后,在加热板上350℃的温度下加热基板1小时。在转化之后,可在手套箱中在2VDS下测定μFET=14cm2/Vs的场效应移动性(mobility)值(处于线性范围)。
对比例
合成
在500ml无残留水分的玻璃圆底烧瓶中,在保护气体气氛下通过搅拌将5.0g的氯化铟(III)(InCl3,22.5mmol)溶解在250ml的干燥甲醇中,留下<10wt%的InCl3残余(基于起始重量)。通过质量流量控制器控制计量加入二乙胺碱(5.0g,对应于111mmol),并且在5小时期间于室温下以基于InCl3的化学计量的量添加,在起始时观察到稍微放热反应。随后,该溶液完全蒸发,剩余的固体用250ml的干燥甲醇提取,在保护气体(N2)下过滤,用干燥的甲醇重复洗涤(10次冲洗)并且在室温减压(<10毫巴)下干燥12小时。产率为>80mol%的氯化铟(III)二甲氧化物(indium(III)chlordimethoxide)。
制备配制物
将获得的材料以50mg/ml的浓度溶解在1-甲氧基-2-丙醇中。所获得的浓缩物如下配制:1份浓缩物对2份1-甲氧基-2-丙醇对1份乙醇。向该配制物中加入另外3wt%的四氢糠醇(THFA)。所有使用的溶剂是无水的(<200ppm的H2O)并且混合在惰性条件下进行(同样无水)。所获得的配制物最终过滤通过200nm PTFE过滤器。
使用100μl的上述配制物润湿具有约15mm边缘长度和具有约200nm氧化硅涂层厚度和ITO/金指状结构的掺杂硅基板。然后以2000rpm(30秒)进行旋涂。在此涂覆操作之后,立即用来自汞蒸汽灯且在150-300nm的波长范围的UV辐射照射涂覆的基板10分钟。随后,在加热板上350℃的温度下加热基板1小时。在转化之后,可在手套箱中在2VDS下测定μFET=8cm2/Vs的场效应移动性值(处于线性范围)。
Claims (13)
1.铟烷氧化物化合物,其可通过在通式ROH的醇存在下将
-三卤化铟InX3,其中X=F、Cl、Br、I
-与式R'2NH的仲胺以相对于三卤化铟8:1至20:1的摩尔比反应制备,其中R和R'是式CnH2n+1的直链、支化或环状C1-至C10-烷基,n=1至10。
2.根据权利要求1的铟烷氧化物化合物,其特征在于其可通过其中仲胺以相对于三卤化铟8:1至15:1,优选8:1至12:1的摩尔比存在的方法制备。
3.通式[In6(O)(OR)12X6]2-Am z(ROH)x的化合物
其中R=烷基,X=F、Cl、Br、I,A=阳离子,z=阳离子的价态,m*z=2和x=0至10。
4.根据权利要求3的化合物,其特征在于其具有通式[In6(O)(OMe)12Cl6]2-[NH2R'2]+ 2(MeOH)2。
5.制备铟烷氧化物化合物的方法,其中在通式ROH的醇存在下将
-三卤化铟InX3,其中X=F、Cl、Br、I
-与式R'2NH的仲胺以相对于三卤化铟8:1至20:1的摩尔比反应,其中R和R'是式CnH2n+1的直链、支化或环状C1-至C10-烷基,n=1至10。
6.根据权利要求5的方法,其特征在于所述摩尔比为8:1至15:1,优选8:1至12:1。
7.根据权利要求6的方法,其特征在于最初将三卤化铟加入到醇ROH中并且加入气态形式、液态形式或溶解于溶剂中的仲胺。
8.根据权利要求7的方法,其特征在于二烷基胺以每小时相对于每摩尔InX3为0.5mol至5mol的速率添加。
9.根据权利要求5-8任一项的方法,其特征在于在添加所有组分之后于1小时至10小时的时间将反应混合物加热至40℃和70℃之间的温度。
10.根据权利要求5-8任一项的方法,其特征在于将所形成的铟烷氧化物化合物与反应组合物的其它成分分开并且重结晶。
11.根据权利要求9的方法,其特征在于将所形成的铟烷氧化物化合物与反应组合物的其它成分分开并且重结晶。
12.根据权利要求1-4任一项的化合物或可由根据权利要求5-11的任一项方法制备的产物用于制造含氧化铟的涂层的用途。
13.根据权利要求1-4任一项的化合物或可由根据权利要求5-11的任一项方法制备的产物用于制造电子组件的半导体或导体层,尤其是用于制造(薄膜)晶体管、二极管或太阳能电池的用途。
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DE102013212017.6 | 2013-06-25 | ||
PCT/EP2014/059957 WO2014206634A1 (de) | 2013-06-25 | 2014-05-15 | Verfahren zur herstellung von indiumalkoxid-verbindungen, die nach dem verfahren herstellbaren indiumalkoxid-verbindungen und ihre verwendung |
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CN112480906A (zh) * | 2020-11-24 | 2021-03-12 | 苏州星烁纳米科技有限公司 | 一种铟氧簇合物及其制备方法、由其制备的量子点及该量子点的制备方法 |
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CN103003286A (zh) * | 2010-07-21 | 2013-03-27 | 赢创德固赛有限公司 | 用于制备含氧化铟层的铟氧桥醇盐 |
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AUPP027497A0 (en) * | 1997-11-07 | 1997-12-04 | Sustainable Technologies Australia Limited | Preparation of metal alkoxides |
RU2181389C2 (ru) * | 1999-06-29 | 2002-04-20 | Омский научно-исследовательский институт приборостроения | Способ получения прозрачной электропроводящей пленки на основе оксидов индия и олова |
KR100627631B1 (ko) * | 2005-02-18 | 2006-09-25 | 한국화학연구원 | 휘발성 인듐 아미노 알콕사이드 화합물 및 그 제조 방법 |
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DE102009009338A1 (de) | 2009-02-17 | 2010-08-26 | Evonik Degussa Gmbh | Indiumalkoxid-haltige Zusammensetzungen, Verfahren zu ihrer Herstellung und ihre Verwendung |
DE102009009337A1 (de) | 2009-02-17 | 2010-08-19 | Evonik Degussa Gmbh | Verfahren zur Herstellung halbleitender Indiumoxid-Schichten, nach dem Verfahren hergestellte Indiumoxid-Schichten und deren Verwendung |
DE102009028801B3 (de) | 2009-08-21 | 2011-04-14 | Evonik Degussa Gmbh | Verfahren zur Herstellung Indiumoxid-haltiger Schichten, nach dem Verfahren herstellbare Indiumoxid-haltige Schicht und deren Verwendung |
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CN103003286A (zh) * | 2010-07-21 | 2013-03-27 | 赢创德固赛有限公司 | 用于制备含氧化铟层的铟氧桥醇盐 |
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US9802964B2 (en) | 2017-10-31 |
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