CN107428555A - 生产结晶氧化钽颗粒的方法 - Google Patents
生产结晶氧化钽颗粒的方法 Download PDFInfo
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- CN107428555A CN107428555A CN201680013142.9A CN201680013142A CN107428555A CN 107428555 A CN107428555 A CN 107428555A CN 201680013142 A CN201680013142 A CN 201680013142A CN 107428555 A CN107428555 A CN 107428555A
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- Prior art keywords
- acid
- tantalum
- preferred
- alkoxide
- particle
- Prior art date
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- 239000002245 particle Substances 0.000 title claims abstract description 43
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910001936 tantalum oxide Inorganic materials 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- -1 tantalum alkoxide Chemical class 0.000 claims abstract description 31
- 239000002253 acid Substances 0.000 claims abstract description 23
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000002105 nanoparticle Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 22
- 239000002887 superconductor Substances 0.000 claims description 18
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 10
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 8
- 150000001412 amines Chemical class 0.000 claims description 7
- 150000002910 rare earth metals Chemical class 0.000 claims description 6
- 239000004215 Carbon black (E152) Substances 0.000 claims description 5
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- BZRSOWBAZCOWRN-UHFFFAOYSA-N butan-1-ol;tantalum Chemical compound [Ta].CCCCO BZRSOWBAZCOWRN-UHFFFAOYSA-N 0.000 claims description 2
- LVNAMAOHFNPWJB-UHFFFAOYSA-N methanol;tantalum Chemical compound [Ta].OC.OC.OC.OC.OC LVNAMAOHFNPWJB-UHFFFAOYSA-N 0.000 claims description 2
- GJAORVQUNCMFTG-UHFFFAOYSA-N ethanol;tantalum(5+) Chemical compound [Ta+5].CCO GJAORVQUNCMFTG-UHFFFAOYSA-N 0.000 claims 1
- 239000000758 substrate Substances 0.000 description 21
- 239000000243 solution Substances 0.000 description 20
- 150000002736 metal compounds Chemical class 0.000 description 12
- 229910052727 yttrium Inorganic materials 0.000 description 12
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- 125000004185 ester group Chemical group 0.000 description 7
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- 239000002184 metal Substances 0.000 description 7
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 7
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- 239000005642 Oleic acid Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
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- 150000007942 carboxylates Chemical class 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 3
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 3
- YWWVWXASSLXJHU-AATRIKPKSA-N (9E)-tetradecenoic acid Chemical compound CCCC\C=C\CCCCCCCC(O)=O YWWVWXASSLXJHU-AATRIKPKSA-N 0.000 description 2
- GQEZCXVZFLOKMC-UHFFFAOYSA-N 1-hexadecene Chemical compound CCCCCCCCCCCCCCC=C GQEZCXVZFLOKMC-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- DTQVDTLACAAQTR-UHFFFAOYSA-M Trifluoroacetate Chemical compound [O-]C(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-M 0.000 description 2
- 235000021322 Vaccenic acid Nutrition 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- MBMBGCFOFBJSGT-KUBAVDMBSA-N all-cis-docosa-4,7,10,13,16,19-hexaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCC(O)=O MBMBGCFOFBJSGT-KUBAVDMBSA-N 0.000 description 2
- YZXBAPSDXZZRGB-DOFZRALJSA-N arachidonic acid Chemical compound CCCCC\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O YZXBAPSDXZZRGB-DOFZRALJSA-N 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
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- 230000008901 benefit Effects 0.000 description 2
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- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
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- 150000001991 dicarboxylic acids Chemical class 0.000 description 2
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- 238000002296 dynamic light scattering Methods 0.000 description 2
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- MMXKVMNBHPAILY-UHFFFAOYSA-N ethyl laurate Chemical compound CCCCCCCCCCCC(=O)OCC MMXKVMNBHPAILY-UHFFFAOYSA-N 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- MNWFXJYAOYHMED-UHFFFAOYSA-N heptanoic acid Chemical compound CCCCCCC(O)=O MNWFXJYAOYHMED-UHFFFAOYSA-N 0.000 description 2
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- CMXPERZAMAQXSF-UHFFFAOYSA-M sodium;1,4-bis(2-ethylhexoxy)-1,4-dioxobutane-2-sulfonate;1,8-dihydroxyanthracene-9,10-dione Chemical compound [Na+].O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=CC=C2O.CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC CMXPERZAMAQXSF-UHFFFAOYSA-M 0.000 description 2
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- C—CHEMISTRY; METALLURGY
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Abstract
本发明为生产氧化钽颗粒的方法的领域。具体而言，本发明涉及生产结晶氧化钽纳米颗粒的方法，其包括将包含以下组分的无水溶液加热：(a)钽醇盐，(b)酸，和(c)溶剂。
Description
本发明是生产氧化钽颗粒的方法的领域。本发明进一步涉及结晶氧化钽颗粒及其在氧化物超导体中作为钉扎中心的用途。
氧化钽颗粒具有各种应用，例如抗腐蚀层、显像剂、作为光致发光和光催化材料、作为催化剂或者作为氧化物超导体的钉扎中心。在这些应用中的大多数中，有利的是使用小结晶纳米颗粒。生产氧化钽颗粒的方法由现有技术已知。
Bonitatibus等人在ACS Nano，第6卷(2012)，第6650-6658页中公开了氧化钽纳米颗粒合成。
然而，至今没有报告得到具有非常小粒度的结晶颗粒的方法。非常小粒度的颗粒具有这一优点：与具有较大粒度的颗粒相比，1g材料构成更多颗粒，这提高了颗粒的效果。同时，结晶度帮助防止颗粒在其环境中部分或完全溶解，特别是在加热至高温时。因此，本发明的目的是提供生产小粒度的结晶氧化钽颗粒的方法。旨在用仪器容易的并容许易按规模放大至工业规模的方法。
该目的通过生产结晶氧化钽颗粒的方法实现，所述方法包括将包含以下组分的无水溶液加热：
(a)钽醇盐，
(b)酸，和
(c)溶剂。
本发明进一步涉及包含氧化钽且具有1-20nm的重均直径的结晶颗粒在超导体中作为钉扎中心的用途。
本发明的优选实施方案可在说明书和权利要求书中找到。不同实施方案的组合落入本发明的范围内。
本发明方法包括将无水溶液加热。在本发明上下文中，无水通常意指溶液具有小于500ppm，优选小于200ppm，特别是小于100ppm，例如小于50ppm的水含量。术语“ppm”指常用的份每百万份。溶液的水含量可通过直接滴定根据例如DIN 51777-1，部分1(1983)中详述的Karl Fischer测定。
在加热以前，溶液优选为均匀的，这意指所有化合物都溶解。溶液优选在常压下在0-400℃，更优选25-350℃，例如50-300℃下为液体。
根据本发明，无水溶液包含钽醇盐。优选，钽醇盐中的钽为+5氧化态的。醇盐包括线性和支化醇盐。线性醇盐的实例为甲醇盐、乙醇盐、正丙醇盐、正丁醇盐、正戊醇盐、正己醇盐、正庚醇盐、正辛醇盐、正壬醇盐、正癸醇盐。支化醇盐的实例为异丙醇盐、异丁醇盐、仲丁醇盐、叔丁醇盐、2-甲基-戊醇盐、2-乙基-己醇盐、环丙醇盐、环己醇盐、茚满醇盐、降冰片醇盐。优选，醇盐为C1-C12醇盐，更优选C1-C8醇盐，特别是C1-C4醇盐。钽醇盐中的醇盐可为全都相同或者彼此不同的，优选，它们为全都相同的。钽醇盐的优选实例为甲醇钽(V)、乙醇钽(V)、正丁醇钽(V)。
无水溶液中钽醇盐的浓度优选为10-200毫摩尔/升，更优选30-150毫摩尔/升，特别是50-100毫摩尔/升。
根据本发明，无水溶液包含酸。酸优选能够与钽醇盐的醇盐形成酯。酸包括羧酸、膦酸、磷酸、磺酸。优选羧酸。羧酸包括线性饱和酸，例如甲酸、乙酸、丙酸、丁酸、戊酸、己酸、庚酸、辛酸、壬酸、癸酸、十一烷酸、月桂酸、十三烷酸、肉豆蔻酸、十五烷酸、棕榈酸、十七烷酸、硬脂酸、十九烷酸、二十烷酸。羧酸进一步包括不饱和线性酸，例如肉豆蔻脑酸、棕榈油酸、十六碳烯酸(sapienic acid)、油酸、反油酸、异油酸、亚油酸、反式亚油酸、花生四烯酸、二十碳五烯酸、芥酸、二十二碳六烯酸、羧酸进一步包括支化羧酸，例如仲丁酸或新戊酸。优选C1-C26羧酸，更优选C4-C24羧酸，特别是C8-C22羧酸，例如油酸。
无水溶液中酸与钽醇盐的摩尔比优选为2.5-50，更优选5-30，特别是10-20。
根据本发明，无水溶液包含溶剂。可使用溶解钽醇盐和胺的所有溶剂。优选非极性溶剂。非极性溶剂通常具有1.65D(Debye)或更小，优选1.6D或更小，特别是1.5D或更小的偶极动量。溶剂包括烃，包括饱和脂族烃，例如己烷、辛烷、癸烷、异十一烷、十六烷、十氢化萘；不饱和脂族烃，例如辛烯、十一碳烯、十六碳烯；和芳族烃，例如二甲苯、荚、萘满、硝基苯。其它合适的溶剂为醚，例如二己醚或二苯醚；酰胺，例如二甲基甲酰胺或二甲基乙酰胺；酯，例如丁酸丁酯、月桂酸乙酯；亚砜，例如二甲亚砜或环丁砜。优选烃，更优选C6-C30烃，特别是C12-C24烃。
根据本发明，将无水溶液加热。优选，将无水溶液加热至120-400℃，更优选150℃至320℃，特别是180-260℃的温度。优选将无水溶液在该温度下保持1分钟至5小时，更优选5-60分钟，特别是10-30分钟。优选将无水溶液以1-100℃/min，更优选5-50℃/min，特别是10-30℃/min的加热速率加热。加热通常通过电加热或蒸汽系统的换热器进行。作为选择，微波辅助加热是可能的。优选，在加热时使无水溶液保持运动以确保化合物和热的均匀分布，例如通过搅拌。
不愿受任何理论束缚，认为无水溶液中的酸在加热时与钽醇盐的醇盐形成酯，由此提供非常小且恰好足够量的水，其导致形成结晶氧化钽颗粒。
优选，无水溶液进一步包含胺。可使用可溶于无水溶液中的任何胺。优选，使用伯胺，特别是单烷基胺，其中烷基链可以为线性或支化的，可被取代并且可包含不饱和键，例如双键或三键。单烷基胺的实例为癸胺、十二胺、十六胺、2-乙基己胺、环己胺、油胺。胺与钽的摩尔比优选为2.5-50，更优选5-30，特别是10-20。
本发明方法得到包含氧化钽的结晶颗粒。这些具有1-20nm，优选2-15nm，更优选3-10nm，特别是4-8nm的重均直径。重均直径优选通过根据ISO 22412(2008)的动态光散射，优选通过使用Mie理论而测量。颗粒具有通过动态光散射测量的低粒度分布分散性D90/D50，优选1.2或更小，更优选1.15或更小，特别是1.1或更小的D90/D50值。
颗粒为结晶的。在本发明上下文中，结晶意指颗粒的结晶度为至少50％，优选至少70％，特别是至少90％。结晶度定义为在HR-TEM中目测观察到的颗粒的重均半径与通过使用Debye-Scherrer方程式评估X射线衍射图(XRD)的主峰的半峰全宽(FWHM)而测定的粒度半径的比。1的比确定100％的结晶度。
当悬浮于非极性溶剂中时，颗粒是稳定的以防聚集。优选，颗粒在其表面上具有充当稳定剂的酸，更优选如上所述羧酸。
结晶颗粒特别适用作氧化物超导体中的钉扎中心。结晶颗粒的优点是小粒度得到高钉扎效应，同时颗粒在高温下形成超导体期间不会部分地溶解，因此不污染超导体材料。优选，超导体包含REBa2Cu3O7-x，其中RE代表稀土金属或钇，且x为0.01-0.3，更优选超导体包含YBa2Cu3O7-x。
优选，超导体通过包含以下组分的油墨化学溶液沉积而制备：
(a)含钇或稀土金属化合物，
(b)含碱土金属化合物，
(c)含过渡金属化合物，
(d)醇，和
(e)本发明颗粒。
含钇或稀土金属化合物、含碱土金属化合物和含过渡金属化合物包括氧化物、氢氧化物、卤化物、羧酸盐、烷氧基化物、硝酸盐或硫酸盐。优选羧酸盐，特别是乙酸盐或丙酸盐。羧酸盐和烷氧基化物可优选被氟取代，例如二氟乙酸盐、三氟乙酸盐或者部分或完全氟化的丙酸盐。
含稀土金属或钇化合物、含碱土金属化合物和含过渡金属化合物中的至少一种包含氟。优选，含碱土金属化合物包含氟，例如作为三氟乙酸盐。
优选，钇或稀土金属为钇、镝或铒，特别是钇。优选，碱土金属为钡。优选，过渡金属为铜。
优选，油墨中含过渡金属化合物与含钇或稀土金属化合物的摩尔比为3:0.7-3:2，更优选3:1.2-3:1.4。优选，油墨中含过渡金属化合物与含碱土金属化合物的摩尔比为3:1-3:2，更优选3:1.7-3:1.9。
油墨进一步包含如上文关于方法所述的醇。优选，醇为甲醇和C2-C12醇的混合物。
油墨包含对超导体生长和/或性能而言最佳的摩尔比的含稀土金属或钇化合物、含碱土金属化合物和含过渡金属化合物，其中考虑待生产的超导体中各金属的摩尔组成。因此，它们的浓度取决于待生产的超导体。一般而言，溶液中它们的浓度相互独立地为0.01-10摩尔/升，优选0.1-1摩尔/升。
优选，油墨包含一定浓度的氧化钽颗粒，在该浓度下，氧化钽颗粒中的金属与含钇或稀土金属化合物的摩尔比为1-30％，更优选3-20％，特别是5-15％。在许多情况下，这相当于相对于油墨0.1-5重量％氧化钽颗粒。
优选，包含氧化钽的结晶颗粒另外通过包含至少一个磷酸基团和酯基团或者至少2个羧酸基团的有机化合物稳定化。更优选，包含氧化钽的结晶颗粒另外通过通式(I)的化合物稳定化：
其中a为0-5，且
b和c相互独立地为1-14，且
n为1-5。
优选，a为0。优选，b为2-10，更优选3-8。优选，c为2-10，更优选3-6。优选，n为2-4。在一个优选实例中，a为0，b为6，c为5，n为3。
还优选，包含至少一个磷酸基团和酯基团或者至少2个羧酸基团的有机化合物为通式(II)的化合物：
其中R1和R2相互独立地为H、OH或COOH，且m为1-12。
如果m大于1，则R1和R2可能是全都相同或者彼此不同的。通式(II)化合物的实例包括其中R1和R2为氢的二羧酸，例如丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、壬二酸、癸二酸；具有羟基的二羧酸，例如丙醇二酸、苹果酸、酒石酸；或者三羧酸，例如柠檬酸或异柠檬酸。
另一优选的包含至少一个磷酸基团和酯基团或者至少2个羧酸基团的有机化合物为通式(III)的化合物：
其中e和f相互独立地为0-12。优选，e为0。优选，f为2-6。
另一优选的包含至少一个磷酸基团和酯基团或者至少2个羧酸基团的有机化合物为通式(IV)的化合物：
其中f为0-5，且
p和q相互独立地为1-14，优选2-12。p与q的比优选为20:80-80:20，特别是40:60-60:40。
通过高极性溶剂如丙酮使结晶颗粒从悬浮液中沉淀，将沉淀物分离，并使沉淀物随着包含至少一个磷酸基团和酯基团或者至少2个羧酸基团的有机化合物再分散于醇中而使包含至少一个磷酸基团和酯基团或者至少2个羧酸基团的有机化合物与包含氧化钽的结晶颗粒接触。作为选择，将包含至少一个磷酸基团和酯基团或者至少2个羧酸基团的有机化合物加入结晶颗粒的悬浮液中，加入高沸点醇并通过蒸发除去较低沸点溶剂。
优选，油墨进一步包含稳定剂、润湿剂和/或其它添加剂。这些化合物的量相对于所用干化合物的总重量可以为0-30重量％。可能需要添加剂以调整粘度。添加剂包括路易斯碱；胺，例如TEA(三乙醇胺)、DEA(二乙醇胺)；表面活性剂；聚羧酸，例如PMAA(聚甲基丙烯酸)和PAA(聚丙烯酸)、PVP(聚乙烯吡咯烷酮)、乙基纤维素。
优选将油墨加热和/或搅拌以使所有成分均化，例如以回流。另外，油墨可进一步包含各种添加剂以提高溶液的稳定性和促进沉积过程。这类添加剂的实例包括润湿剂、胶凝剂和抗氧化剂。
为制备具有本发明油墨的超导体，通常使油墨沉积到基底上。油墨的沉积可以以各种方法进行。油墨可例如通过浸涂(将基底浸入油墨中)、旋涂(将油墨施涂于旋转基底上)、喷涂(将油墨喷雾或雾化到基底上)、毛细管涂覆(借助毛细管施涂油墨)、夹缝式挤压型涂覆(通过窄狭缝施涂油墨)和喷墨印刷施涂。优选夹缝式挤压型涂覆和喷墨印刷。
优选，在沉积以后将油墨在溶剂沸点以下的温度，例如溶剂沸点以下10-100℃，优选溶剂沸点以下20-50℃下蒸发以形成膜。
基底可以为能够支撑缓冲和/或超导体层的任何材料。例如，合适的基底公开于EP830 218、EP 1 208 244、EP 1 198 846、EP 2 137 330中。通常，基底为金属和/或合金条/带，由此金属和/或合金可以为镍、银、铜、锌、铝、铁、铬、钒、钯、钼、钨和/或其合金。优选，基底为镍基的。更优选，基底为镍基的并且包含1-10原子％，特别是3-9原子％钨。层压金属带、涂有第二金属如电镀涂层的带或者具有合适表面的任何其它多材料带也可用作基底。
基底优选为有纹理的，即它具有有纹理的表面。基底通常为20-200μm厚，优选40-100μm。长度通常为大于1m，宽度通常为1cm至1m。
优选，在将包含钇或稀土金属、碱土金属和过渡金属的膜沉积到其上以前，例如通电抛光将基底表面平面化。通常有利的是使因此平面化的基底经受热处理。该热处理包括将基底加热至600-1000℃2-15小时，其中时间指基底在最大温度下期间的时间。优选，热处理在还原气氛如含氢气氛下进行。平面化和/或热处理可重复。
优选，基底表面具有根据DIN EN ISO 4287和4288小于15nm的rms粗糙度。粗糙度指在基底表面的晶粒边界内10×10μm的面积，使得金属基底的颗粒边界不影响所述粗糙度测量。
优选，在基底与膜之间存在一个或多个缓冲层。缓冲层可包含能够支撑超导体层的任何材料。缓冲层材料的实例包括金属和金属氧化物，例如银、镍、TbOx、GaOx、CeO2、氧化钇稳定化的氧化锆(YSZ)、Y2O3、LaAlO3、SrTiO3、Gd2O3、LaNiO3、LaCuO3、SrRuO3、NdGaO3、NdAlO3和/或如本领域技术人员所知的一些氮化物。优选的缓冲层材料为钇稳定化的氧化锆(YSZ)；各种锆酸盐，例如锆酸钆、锆酸镧；钛酸盐，例如钛酸锶；和简单氧化物，例如氧化铈或氧化镁。更优选，缓冲层包含锆酸镧、氧化铈、氧化钇、钆掺杂的氧化铈和/或钛酸锶。甚至更优选，缓冲层包含锆酸镧和/或氧化铈。
为增强纹理转移度和作为扩散层的效率，各自包含不同缓冲剂材料的多个缓冲层在基底与膜之间。优选，基底包括两个或三个缓冲层，例如包含锆酸镧的第一缓冲层和包含氧化铈的第二缓冲层。
优选将膜加热至300-600℃，优选350-450℃的温度以除去前体的其余有机部分。将基底在该温度下保持1-30分钟，优选5-15分钟。
其后，优选将膜在包含水和氧气的气氛中加热至700-900℃，优选750-850℃的温度以使膜结晶。水的分压为气氛总分压的1-99.5％，氧气的分压为气氛总分压的0.5-90％，优选2-90％。甚至更优选，在加热至700-900℃的第一阶段期间，水的分压为气氛总分压的1-20％，优选1.5-5％，且在该加热的第二阶段期间，水的分压为总分压的90-99.5％，优选95-99％。
通常将超导体线切割成较小的带并通过例如通过电沉积用导电金属如铜涂覆而稳定化。
实施例
实施例1
将4.3mL油酸和9mL十八碳烯在真空下在120℃下除气1小时。然后将温度提高至180℃并将0.25mL乙醇钽快速注入混合物中。将反应混合物进一步加热至260℃并在该温度下保持15分钟，其后使试样冷却至室温。使颗粒沉淀并再溶于氯仿中。该提纯程序重复两次。图1所述透射电子显微镜(TEM)分析显示颗粒的粒度是均匀的(5nm直径)，并且从高分辨率图像中可以总结出颗粒为结晶的。图2显示所得试样的X射线衍射图，其中峰指定为氧化钽的晶面。
Claims (14)
1.生产结晶氧化钽纳米颗粒的方法，其包括将包含以下组分的无水溶液加热：
(a)钽醇盐，
(b)酸，和
(c)溶剂。
2.根据权利要求1的方法，其中溶剂为烃。
3.根据权利要求1或2的方法，其中溶剂为C12-C24烃。
4.根据权利要求1-3中任一项的方法，其中酸为羧酸。
5.根据权利要求1-4中任一项的方法，其中羧酸为C8-C22羧酸。
6.根据权利要求1-5中任一项的方法，其中酸与钽醇盐的摩尔比为5-30。
7.根据权利要求1-6中任一项的方法，其中无水溶液中钽醇盐的浓度为10-200毫摩尔/升。
8.根据权利要求1-7中任一项的方法，其中钽醇盐为甲醇钽(V)、乙醇钽(V)或正丁醇钽(V)。
9.根据权利要求1-8中任一项的方法，其中酸与钽醇盐的摩尔比为2.5-50。
10.根据权利要求1-9中任一项的方法，其中将无水溶液加热至120-400℃的温度。
11.根据权利要求1-10中任一项的方法，其中无水溶液进一步包含胺。
12.根据权利要求11的方法，其中胺为单烷基胺。
13.包含氧化钽且具有1-20nm的重均直径的结晶颗粒在超导体中作为钉扎中心的用途。
14.根据权利要求13的用途，其中超导体包含REBa2Cu3O7-x，其中RE代表稀土金属且x为0.01-0.3。
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP15157159 | 2015-03-02 | ||
| EP15157159.3 | 2015-03-02 | ||
| PCT/EP2016/051581 WO2016139013A1 (en) | 2015-03-02 | 2016-01-26 | Process for producing crystalline tantalum oxide particles |
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| EP (1) | EP3265430B1 (zh) |
| JP (1) | JP6751098B2 (zh) |
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| CN (1) | CN107428555A (zh) |
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| WO (1) | WO2016139013A1 (zh) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115818977A (zh) * | 2022-11-03 | 2023-03-21 | 广西大学 | 一种用于电致变色器件对电极的氧化钽纳米线薄膜的制备方法及电致变色器件 |
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| KR101848027B1 (ko) | 2016-08-16 | 2018-04-12 | 주식회사 고영테크놀러지 | 정위수술용 수술로봇 시스템 및 정위수술용 로봇의 제어방법 |
| US11623211B2 (en) * | 2019-04-26 | 2023-04-11 | The Regents Of The University Of California | Template-free tuned light driven photocatalyst and method |
| EP4284550A1 (en) * | 2021-01-29 | 2023-12-06 | Ecovyst Catalyst Technologies LLC | Method for manufacturing a supported tantalum catalyst |
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| JPH01111713A (ja) * | 1987-10-23 | 1989-04-28 | Tanaka Kikinzoku Kogyo Kk | 超電導体インク |
| US20050159298A1 (en) * | 2004-01-16 | 2005-07-21 | American Superconductor Corporation | Oxide films with nanodot flux pinning centers |
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| WO2013139843A2 (de) * | 2012-03-21 | 2013-09-26 | Basf Se | Verfahren zur herstellung von nanoteilchen sowie deren verwendung bei der herstellung von hochtemperatursupraleitern |
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| US5741377A (en) | 1995-04-10 | 1998-04-21 | Martin Marietta Energy Systems, Inc. | Structures having enhanced biaxial texture and method of fabricating same |
| PT1208244E (pt) | 1999-04-03 | 2004-09-30 | Leibniz Inst Festkorper Werkst | Material metalico a base de niquel e um metodo para a sua producao |
| AU2915401A (en) | 1999-07-23 | 2001-05-10 | American Superconductor Corporation | Control of oxide layer reaction rates |
| DE102004016131A1 (de) * | 2004-04-01 | 2005-10-20 | Max Planck Gesellschaft | Herstellung von Metalloxid-Nanoteilchen hoher Kristallinität und hoher Reinheit |
| DE102008016222B4 (de) | 2007-04-17 | 2010-12-30 | Leibniz-Institut für Festkörper und Werkstoffforschung e.V. | Metallfolie |
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2016
- 2016-01-26 CN CN201680013142.9A patent/CN107428555A/zh active Pending
- 2016-01-26 US US15/554,756 patent/US10233091B2/en not_active Expired - Fee Related
- 2016-01-26 WO PCT/EP2016/051581 patent/WO2016139013A1/en active Application Filing
- 2016-01-26 ES ES16701635T patent/ES2743951T3/es active Active
- 2016-01-26 KR KR1020177027625A patent/KR20170126961A/ko unknown
- 2016-01-26 DK DK16701635.1T patent/DK3265430T3/da active
- 2016-01-26 JP JP2017546619A patent/JP6751098B2/ja not_active Expired - Fee Related
- 2016-01-26 EP EP16701635.1A patent/EP3265430B1/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH01111713A (ja) * | 1987-10-23 | 1989-04-28 | Tanaka Kikinzoku Kogyo Kk | 超電導体インク |
| US20050159298A1 (en) * | 2004-01-16 | 2005-07-21 | American Superconductor Corporation | Oxide films with nanodot flux pinning centers |
| US20100117503A1 (en) * | 2005-09-22 | 2010-05-13 | Sony Corporation | Metal oxide nanoparticles, production method thereof, light-emitting element assembly, and optical material |
| WO2013139843A2 (de) * | 2012-03-21 | 2013-09-26 | Basf Se | Verfahren zur herstellung von nanoteilchen sowie deren verwendung bei der herstellung von hochtemperatursupraleitern |
| CN103274468A (zh) * | 2013-05-29 | 2013-09-04 | 复旦大学 | 一种球形五氧化二钽的制备方法及应用 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115818977A (zh) * | 2022-11-03 | 2023-03-21 | 广西大学 | 一种用于电致变色器件对电极的氧化钽纳米线薄膜的制备方法及电致变色器件 |
| CN115818977B (zh) * | 2022-11-03 | 2024-04-30 | 广西大学 | 一种用于电致变色器件对电极的氧化钽纳米线薄膜的制备方法及电致变色器件 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP3265430B1 (en) | 2019-06-05 |
| KR20170126961A (ko) | 2017-11-20 |
| JP6751098B2 (ja) | 2020-09-02 |
| JP2018513086A (ja) | 2018-05-24 |
| EP3265430A1 (en) | 2018-01-10 |
| DK3265430T3 (da) | 2019-08-26 |
| US10233091B2 (en) | 2019-03-19 |
| WO2016139013A1 (en) | 2016-09-09 |
| US20180044199A1 (en) | 2018-02-15 |
| ES2743951T3 (es) | 2020-02-21 |
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