CN110300731B - 使用胺-金属配合物和缓慢释放硫的前体合成发光2d层状材料 - Google Patents
使用胺-金属配合物和缓慢释放硫的前体合成发光2d层状材料 Download PDFInfo
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- ZKKLPDLKUGTPME-UHFFFAOYSA-N diazanium;bis(sulfanylidene)molybdenum;sulfanide Chemical compound [NH4+].[NH4+].[SH-].[SH-].S=[Mo]=S ZKKLPDLKUGTPME-UHFFFAOYSA-N 0.000 description 1
- RJYMRRJVDRJMJW-UHFFFAOYSA-L dibromomanganese Chemical compound Br[Mn]Br RJYMRRJVDRJMJW-UHFFFAOYSA-L 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- CTNMMTCXUUFYAP-UHFFFAOYSA-L difluoromanganese Chemical compound F[Mn]F CTNMMTCXUUFYAP-UHFFFAOYSA-L 0.000 description 1
- QFEOTYVTTQCYAZ-UHFFFAOYSA-N dimanganese decacarbonyl Chemical compound [Mn].[Mn].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-] QFEOTYVTTQCYAZ-UHFFFAOYSA-N 0.000 description 1
- ASLHVQCNFUOEEN-UHFFFAOYSA-N dioxomolybdenum;dihydrochloride Chemical compound Cl.Cl.O=[Mo]=O ASLHVQCNFUOEEN-UHFFFAOYSA-N 0.000 description 1
- YWWZCHLUQSHMCL-UHFFFAOYSA-N diphenyl diselenide Chemical compound C=1C=CC=CC=1[Se][Se]C1=CC=CC=C1 YWWZCHLUQSHMCL-UHFFFAOYSA-N 0.000 description 1
- VRLFOXMNTSYGMX-UHFFFAOYSA-N diphenyl ditelluride Chemical compound C=1C=CC=CC=1[Te][Te]C1=CC=CC=C1 VRLFOXMNTSYGMX-UHFFFAOYSA-N 0.000 description 1
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012990 dithiocarbamate Substances 0.000 description 1
- ZTPZXOVJDMQVIK-UHFFFAOYSA-N dodecane-1-selenol Chemical compound CCCCCCCCCCCC[SeH] ZTPZXOVJDMQVIK-UHFFFAOYSA-N 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- UCSVJZQSZZAKLD-UHFFFAOYSA-N ethyl azide Chemical compound CCN=[N+]=[N-] UCSVJZQSZZAKLD-UHFFFAOYSA-N 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- UPWPDUACHOATKO-UHFFFAOYSA-K gallium trichloride Chemical compound Cl[Ga](Cl)Cl UPWPDUACHOATKO-UHFFFAOYSA-K 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PDPJQWYGJJBYLF-UHFFFAOYSA-J hafnium tetrachloride Chemical compound Cl[Hf](Cl)(Cl)Cl PDPJQWYGJJBYLF-UHFFFAOYSA-J 0.000 description 1
- FEEFWFYISQGDKK-UHFFFAOYSA-J hafnium(4+);tetrabromide Chemical compound Br[Hf](Br)(Br)Br FEEFWFYISQGDKK-UHFFFAOYSA-J 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical class CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- GYCHYNMREWYSKH-UHFFFAOYSA-L iron(ii) bromide Chemical compound [Fe+2].[Br-].[Br-] GYCHYNMREWYSKH-UHFFFAOYSA-L 0.000 description 1
- FZGIHSNZYGFUGM-UHFFFAOYSA-L iron(ii) fluoride Chemical compound [F-].[F-].[Fe+2] FZGIHSNZYGFUGM-UHFFFAOYSA-L 0.000 description 1
- SHXXPRJOPFJRHA-UHFFFAOYSA-K iron(iii) fluoride Chemical compound F[Fe](F)F SHXXPRJOPFJRHA-UHFFFAOYSA-K 0.000 description 1
- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 description 1
- 150000007527 lewis bases Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 229910000473 manganese(VI) oxide Inorganic materials 0.000 description 1
- QWYFOIJABGVEFP-UHFFFAOYSA-L manganese(ii) iodide Chemical compound [Mn+2].[I-].[I-] QWYFOIJABGVEFP-UHFFFAOYSA-L 0.000 description 1
- 229910052960 marcasite Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- RLCOZMCCEKDUPY-UHFFFAOYSA-H molybdenum hexafluoride Chemical compound F[Mo](F)(F)(F)(F)F RLCOZMCCEKDUPY-UHFFFAOYSA-H 0.000 description 1
- GICWIDZXWJGTCI-UHFFFAOYSA-I molybdenum pentachloride Chemical compound Cl[Mo](Cl)(Cl)(Cl)Cl GICWIDZXWJGTCI-UHFFFAOYSA-I 0.000 description 1
- ZSSVQAGPXAAOPV-UHFFFAOYSA-K molybdenum trichloride Chemical compound Cl[Mo](Cl)Cl ZSSVQAGPXAAOPV-UHFFFAOYSA-K 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- BMGNSKKZFQMGDH-FDGPNNRMSA-L nickel(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ni+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BMGNSKKZFQMGDH-FDGPNNRMSA-L 0.000 description 1
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 description 1
- 229910021508 nickel(II) hydroxide Inorganic materials 0.000 description 1
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 description 1
- BFSQJYRFLQUZKX-UHFFFAOYSA-L nickel(ii) iodide Chemical compound I[Ni]I BFSQJYRFLQUZKX-UHFFFAOYSA-L 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- KZCOBXFFBQJQHH-UHFFFAOYSA-N octane-1-thiol Chemical compound CCCCCCCCS KZCOBXFFBQJQHH-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- JKDRQYIYVJVOPF-FDGPNNRMSA-L palladium(ii) acetylacetonate Chemical compound [Pd+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O JKDRQYIYVJVOPF-FDGPNNRMSA-L 0.000 description 1
- INIOZDBICVTGEO-UHFFFAOYSA-L palladium(ii) bromide Chemical compound Br[Pd]Br INIOZDBICVTGEO-UHFFFAOYSA-L 0.000 description 1
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 description 1
- AOLPZAHRYHXPLR-UHFFFAOYSA-I pentafluoroniobium Chemical compound F[Nb](F)(F)(F)F AOLPZAHRYHXPLR-UHFFFAOYSA-I 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- SONJTKJMTWTJCT-UHFFFAOYSA-K rhodium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Rh+3] SONJTKJMTWTJCT-UHFFFAOYSA-K 0.000 description 1
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 150000003958 selenols Chemical class 0.000 description 1
- IYKVLICPFCEZOF-UHFFFAOYSA-N selenourea Chemical compound NC(N)=[Se] IYKVLICPFCEZOF-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- VPQBLCVGUWPDHV-UHFFFAOYSA-N sodium selenide Chemical compound [Na+].[Na+].[Se-2] VPQBLCVGUWPDHV-UHFFFAOYSA-N 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- MQRWPMGRGIILKQ-UHFFFAOYSA-N sodium telluride Chemical compound [Na][Te][Na] MQRWPMGRGIILKQ-UHFFFAOYSA-N 0.000 description 1
- 239000002195 soluble material Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- YJPVTCSBVRMESK-UHFFFAOYSA-L strontium bromide Chemical compound [Br-].[Br-].[Sr+2] YJPVTCSBVRMESK-UHFFFAOYSA-L 0.000 description 1
- 229910001625 strontium bromide Inorganic materials 0.000 description 1
- FVRNDBHWWSPNOM-UHFFFAOYSA-L strontium fluoride Chemical compound [F-].[F-].[Sr+2] FVRNDBHWWSPNOM-UHFFFAOYSA-L 0.000 description 1
- 229910001637 strontium fluoride Inorganic materials 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- YRGLXIVYESZPLQ-UHFFFAOYSA-I tantalum pentafluoride Chemical compound F[Ta](F)(F)(F)F YRGLXIVYESZPLQ-UHFFFAOYSA-I 0.000 description 1
- GCPVYIPZZUPXPB-UHFFFAOYSA-I tantalum(v) bromide Chemical compound Br[Ta](Br)(Br)(Br)Br GCPVYIPZZUPXPB-UHFFFAOYSA-I 0.000 description 1
- OEIMLTQPLAGXMX-UHFFFAOYSA-I tantalum(v) chloride Chemical compound Cl[Ta](Cl)(Cl)(Cl)Cl OEIMLTQPLAGXMX-UHFFFAOYSA-I 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- UBZYKBZMAMTNKW-UHFFFAOYSA-J titanium tetrabromide Chemical compound Br[Ti](Br)(Br)Br UBZYKBZMAMTNKW-UHFFFAOYSA-J 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 description 1
- NLLZTRMHNHVXJJ-UHFFFAOYSA-J titanium tetraiodide Chemical compound I[Ti](I)(I)I NLLZTRMHNHVXJJ-UHFFFAOYSA-J 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- FEONEKOZSGPOFN-UHFFFAOYSA-K tribromoiron Chemical compound Br[Fe](Br)Br FEONEKOZSGPOFN-UHFFFAOYSA-K 0.000 description 1
- SEDZOYHHAIAQIW-UHFFFAOYSA-N trimethylsilyl azide Chemical compound C[Si](C)(C)N=[N+]=[N-] SEDZOYHHAIAQIW-UHFFFAOYSA-N 0.000 description 1
- ZAKSIRCIOXDVPT-UHFFFAOYSA-N trioctyl(selanylidene)-$l^{5}-phosphane Chemical compound CCCCCCCCP(=[Se])(CCCCCCCC)CCCCCCCC ZAKSIRCIOXDVPT-UHFFFAOYSA-N 0.000 description 1
- PIOZWDBMINZWGJ-UHFFFAOYSA-N trioctyl(sulfanylidene)-$l^{5}-phosphane Chemical compound CCCCCCCCP(=S)(CCCCCCCC)CCCCCCCC PIOZWDBMINZWGJ-UHFFFAOYSA-N 0.000 description 1
- OFQPGOWZSZOUIV-UHFFFAOYSA-N tris(trimethylsilyl)arsane Chemical compound C[Si](C)(C)[As]([Si](C)(C)C)[Si](C)(C)C OFQPGOWZSZOUIV-UHFFFAOYSA-N 0.000 description 1
- OUMZKMRZMVDEOF-UHFFFAOYSA-N tris(trimethylsilyl)phosphane Chemical compound C[Si](C)(C)P([Si](C)(C)C)[Si](C)(C)C OUMZKMRZMVDEOF-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- HQYCOEXWFMFWLR-UHFFFAOYSA-K vanadium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[V+3] HQYCOEXWFMFWLR-UHFFFAOYSA-K 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 1
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- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/68—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing chromium, molybdenum or tungsten
- C09K11/681—Chalcogenides
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B22—CASTING; POWDER METALLURGY
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- B22F1/14—Treatment of metallic powder
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- B22F9/00—Making metallic powder or suspensions thereof
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- C07C211/02—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
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- C07F11/00—Compounds containing elements of Groups 6 or 16 of the Periodic Table
- C07F11/005—Compounds containing elements of Groups 6 or 16 of the Periodic Table compounds without a metal-carbon linkage
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- C09K11/0805—Chalcogenides
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Abstract
本发明公开了一种合成二维(2D)纳米粒子的方法,所述方法包括将第一纳米粒子前体和第二纳米粒子前体在一种或多种溶剂中混合以形成溶液,随后将溶液加热至第一温度,持续第一时间段,然后接着将溶液加热至第二温度,持续第二时间段,其中第二温度高于第一温度,以实现纳米粒子前体向2D纳米粒子的转化。在一个实施方案中,第一纳米粒子前体是金属‑胺配合物并且第二纳米粒子前体是缓释硫属元素源。
Description
相关申请的交叉引用:
本申请要求2017年2月2日提交的美国临时申请系列号62/453,780和2017年11月20日提交的美国临时申请系列号62/588,774的利益,所述申请的内容通过引用整体并入本文。
关于联邦政府资助研究或开发的声明:不适用
发明背景
1.发明领域
本发明总体上涉及二维(2D)材料。更特别地,其涉及2D纳米粒子。
2.包括根据37 CFR 1.97和1.98公开的信息的相关领域的描述。
通过机械剥离石墨的石墨烯的分离[K.S.Novoselov,A.K.Geim,S.V.Morozov,D.Jiang,Y.Zhang,S.V.Dubnos,I.V.Grigorieva和A.A.Firsov,Science,2004,306,666]已经引起了对二维(2D)层状材料的强烈兴趣。石墨烯的性质包括优异的强度以及高的导电性和导热性,同时重量轻、柔韧并且透明。这提供了一系列潜在应用的可能性,包括高速晶体管和传感器、阻隔材料、太阳能电池、蓄电池和复合材料。
其他种类的广泛的令人感兴趣2D材料包括过渡金属二硫属化物(transitionmetal dichalcogenide,TMDC)材料,六方氮化硼(h-BN),以及基于第14族元素的那些,诸如硅烯(silicene)和锗烯(germanene)。这些材料的性质的范围可以从半金属,例如NiTe2和VSe2,到半导体,例如WSe2和MoS2,到绝缘,例如h-BN。
对于范围从催化到传感、储能和光电设备的应用来说,TMDC材料的2D纳米片越来越令人感兴趣。
TMDC单层是MX2型的原子厚度半导体,其中M是过渡金属元素(Mo、W等)并且X是硫属元素(S、Se或Te)。单层的M原子夹在两层X原子之间。MoS2单层的厚度为在2D TMDC中,半导体WSe2和MoS2是特别令人感兴趣的,因为当材料的尺寸减小到单层或少层(few-layer)时,由于量子限制效应而产生另外的性质,同时在很大程度上保留了它们的块状性质。在WSe2和MoS2的情况下,这些包括当厚度减少到单个单层时展现出间接到直接的带隙跃迁,伴有强烈的激子效应。这导致光致发光效率的明显增强,为这样的材料在光电设备中的应用开辟了新的机会。其他特别令人感兴趣的材料包括WS2和MoSe2。
石墨烯的发现说明了当宏观尺寸的块状晶体(bulk crystal)减薄到一个原子层时,如何可以出现新的物理性质。与石墨一样,TMDC块状晶体由通过范德华引力彼此结合的单层形成。TMDC单层具有与半金属石墨烯明显不同的性质。例如,TMDC单层MoS2、WS2、MoSe2、WSe2和MoTe2具有直接带隙,并且可以在电子设备中用作晶体管并且在光学器件中用作发射器和检测器。第4族至第7族的TMDC主要以层状结构结晶,导致在其电学、化学、机械和热学性质方面的各向异性。每层都包括通过共价键夹在两层硫属元素原子之间的金属原子的六方堆积层。相邻的层通过范德华相互作用弱结合,其可以容易地通过机械或化学方法破坏以产生单层和少层结构。
TMDC单层晶体结构不具有反转中心,这允许获得新的电荷载子自由度,即k-能谷(k-valley)指数,并且开辟了新的物理学领域:“能谷电子学(valleytronics)”。
TMDC单层中的强自旋-轨道耦合导致价带中数百兆电子伏(meV)和导带中数兆电子伏的自旋轨道分裂,这允许通过调谐激发激光光子能量来控制电子自旋。
自从发现直接带隙以及在电子学和能谷物理学中的潜在应用以来,TMDC单层的工作是新兴的研究和开发领域。TMDC可以与其他2D材料(例如石墨烯和六方氮化硼)组合以制造范德华异质结构器件。
半导体可以吸收能量大于或等于其带隙的光子。这意味着吸收波长较短的光。如果导带能量的最小值在k-空间中与价带的最大值处于相同位置,即带隙是直接的,则半导体通常是有效的发射器。低至厚度为两个单层的块状TMDC材料的带隙仍然是间接的,因此与单层材料相比,发射效率较低。TMDC单层的发射效率比块状材料(bulk material)高约104倍。TMDC单层的带隙在可见光范围内(400nm至700nm之间)。直接发射显示由自旋-轨道耦合能量分开的两个跃迁(称为A和B)。能量最低,因此在强度上最重要的是A发射。由于它们的直接带隙,TMDC单层是有前景的用于光电应用的材料。
在其多层形式中,MoS2是银黑色固体,作为矿物辉钼矿(钼的主要矿石)存在。MoS2是相对不活跃的。它不受稀酸和氧的影响。MoS2在外观和感觉上类似于石墨。由于其低摩擦性和坚韧性,它被广泛用作固体润滑剂。作为TMDC,MoS2拥有一些石墨烯的理想品质(诸如机械强度和导电性),并且可以发光,开辟了可能的应用诸如光电探测器和晶体管。
对于高性能应用来说,需要平坦、无缺陷的材料,而对于在蓄电池和超级电容器中的应用来说,缺陷、空隙和孔洞是合乎需要的。
可以使用“自上而下”和“自下而上”的方法制备单层和少层2D纳米片。自上而下的方法涉及从块状材料(bulk material)中机械地或化学地移除层。这样的技术包括机械剥离、超声辅助液相剥离(LPE)和插层技术。自下而上的方法(其中由其组成元素生长2D层)包括化学气相沉积(CVD)、原子层沉积(ALD)和分子束外延(MBE)以及基于溶液的方法(包括热注入)。
在现有技术中已经描述了许多合成2D纳米片的方法,其中最常见的包括机械剥离、LPE和CVD,少数报道为主要利用热注射技术的基于溶液的方法。虽然机械剥离提供高度结晶的薄片,但是该方法产率低,厚度控制差,并且不可扩展(unscalable)。LPE提供了可扩展的制备2D纳米片的途径,并且可以在环境条件下使用比其他技术更少的危险化学品进行。然而,与机械剥离一样,它提供差的厚度控制,而且反应产率低,并且产生小的薄片。差的反应产率也是CVD合成的典型特征。该方法的优点包括大的面积可扩展性、均匀性和厚度控制。然而,所得材料的质量与机械剥离薄片的质量是不可比的,其中由此制备的薄片通常很小并且显示出差的长期稳定性。基于溶液的合成方法越来越受到关注,并且可能控制所得2D材料的尺寸、形状和均匀性。然而,需要进一步改进以提供可扩展的合成方法的最终组合,其产生具有所需的结晶相、可调的窄的尺寸和形状分布并且用挥发性配体封端的薄片。
通过“自下而上”方法制备的2D量子点的胶体合成的文献报道很少。大多数是“自上而下”的基于剥离的方法-即其中剥离块状材料以提供2D材料的方法。用于形成2D薄片的基于溶液的方法是非常理想的,因为它们可以控制所得材料的尺寸、形状和均匀性,并且使配体能够施加到材料的表面以提供溶解性,并且因此提供溶液可加工性。如对于CVD生长的样品所观察到的,将有机配体应用到材料表面还可以通过充当对氧气和其他外来物质的屏障来限制降解。所得材料是自立式的(free-standing),进一步促进了它们的可加工性。然而,迄今为止开发的基于溶液的方法并未提供可扩展的反应以生成具有所需结晶相、可调的窄的形状和尺寸分布以及挥发性封端配体的2D层状材料,这样的层状材料是理想的,因为它可以在器件处理期间容易地移除。MoS2的一个有前途的参考文献使用单源前体四硫钼酸铵((NH4)2MoS4)。[H.Lin,C.Wang,J.Wu,Z.Xu,Y.Huang和C.Zhang,New J.Chem.,2015,39,8492]。然而,所报道的方法产生不溶性材料。预期有机可溶性材料对于某些应用和/或易用性将是非常有利的。
制备2D层状材料的挑战之一是大规模地实现组成均匀性,无论是需要高质量、无缺陷还是有缺陷的材料。进一步的挑战包括形成具有均匀形状和尺寸分布的2D薄片。
因此,需要一种合成方法,所述方法产生可以是溶液加工的具有均匀性质的2D纳米粒子。
发明概述
在本文中描述了一种制备纳米粒子的方法。所述方法可以用于生产具有均匀性质的2D纳米粒子,其可以是溶液加工的。
在一个实施方案中,合成方法包括将第一纳米粒子前体和第二纳米粒子前体在一种或多种溶剂中组合以形成溶液,随后将溶液加热至第一温度,持续第一时间段,然后接着将溶液加热至第二温度,持续第二时间段,其中第二温度高于第一温度,以实现纳米粒子前体向2D纳米粒子的转化。
在一个实施方案中,第一纳米粒子前体是金属-胺配合物。在一个实施方案中,第二纳米粒子前体是缓释硫属元素源。
在一个实施方案中,合成方法包括将单源前体溶解在溶剂中以形成溶液,将溶液加热至第一温度,持续第一时间段,然后接着将溶液加热至第二温度,持续第二时间段,其中第二温度高于第一温度,以实现单源前体向2D纳米粒子的转化。
在一个实施方案中,2D纳米粒子是TMDC纳米粒子。
在一个实施方案中,2D纳米粒子是2D量子点(QD)。
附图的若干视图的简要说明
图1是根据实施例4制备的MoS22D纳米粒子的光致发光等高线图。
图2是根据实施例4制备的MoS22D纳米粒子的拉曼光谱。
发明详述
在本文中描述了一种制备纳米粒子的方法。所述方法可以用于生产具有均匀性质的2D纳米粒子。在一个实施方案中,2D纳米粒子通过一锅法制备。
如本文中使用的,术语“纳米粒子”用于描述尺寸在大约1至100nm的量级的粒子。术语“量子点”(QD)用于描述显示出量子限制效应的半导体纳米粒子。QD的尺寸通常但并不排他性地为1至10nm。术语“纳米粒子”和“量子点”并非意在暗示对粒子的形状的任何限制。术语“2D纳米粒子”用于描述横向尺寸在大约1至100nm的量级并且厚度为1至10个原子或分子层的粒子,并且其中横向尺寸大于厚度。术语“2D纳米薄片”用于描述横向尺寸在大约1至100nm的量级并且厚度为1至5个原子或分子层的粒子。
如本文中使用的,术语“一锅法”用于描述合成方法,其中纳米粒子前体在单个反应容器中转化为2D纳米粒子。
纳米粒子的组成不受限制。合适的材料包括但不限于:
氧化石墨烯和还原的氧化石墨烯;
过渡金属二硫属化物(TMDC),诸如例如WO2;WS2;WSe2;WTe2;MnO2;MoO2;MoS2;MoSe2;MoTe2;NiO2;NiTe2;NiSe2;VO2;VS2;VSe2;TaS2;TaSe2;RuO2;RhTe2;PdTe2;HfS2;NbS2;NbSe2;NbTe2;FeS2;TiO2;TiS2;TiSe2;和ZrS2;
过渡金属三硫属化物,诸如例如TaO3;MnO3;WO3;ZrS3;ZrSe3;HfS3;和HfSe3;
第13-16族(III-VI)化合物,诸如例如InS;InSe;GaS;GaSe;和GaTe;
第15-16族(V-VI)化合物,诸如例如Bi2Se3;和Bi2Te3;
氮化物,诸如例如h-BN;
氧化物,诸如例如LaVO3;LaMnO3;V2O5;LaNbO7;Ca2Nb3O10;Ni(OH)2;和Eu(OH)2;层状铜氧化物;云母;和铋锶钙铜氧化物(BSCCO);
磷化物,诸如例如Li7MnP4;和MnP4。
在上述材料中,相邻的层通过范德华相互作用保持在一起,其在合成期间可以容易地分离而形成2D薄片。在备选实施方案中,纳米粒子包括非层状半导体材料,包括但不限于:
第12-16族(II-VI)半导体,诸如例如ZnS;ZnSe;CdS;CdSe;CdTe;
第13-15族(III-V)材料,诸如例如GaN;GaP;GaAs;InN;InP;InAs;和
第I-III-VI族材料,诸如例如CuGaS2;CuGaSe2;CuGa(S,Se)2;CuInS2、CuInSe2;CuIn(S,Se)2;Cu(In,Ga)S2;Cu(In,Ga)Se2;Cu(In,Ga)(S,Se)2;CuInTe2;AgInS2;和AgInSe2;和
包括其掺杂物质和合金。
在一些实施方案中,2D纳米粒子是2D纳米薄片。在一些实施方案中,2D纳米粒子是2D QD。QD由于其来源于“量子限制效应”的独特的光学、电子和化学性质而已经得到广泛地研究-当半导体纳米粒子的尺寸降低至低于玻尔半径的两倍时,能级变得量子化,产生离散的能级。带隙随着粒度降低而增加,得到尺寸可调的光学、电子和化学性质,诸如尺寸依赖性光致发光。此外,已经发现,将2D纳米薄片的横向尺寸降低至量子限制区域(regime)可以产生又一种独特的性质,取决于2D纳米薄片的横向尺寸和层数这两者。在一些实施方案中,2D纳米薄片的横向尺寸可以处于量子限制区域,其中可以通过改变它们的横向尺寸来控制纳米粒子的光学、电子和化学性质。例如,横向尺寸为约10nm以下的材料(诸如MoSe2和WSe2)的金属硫属化物单层纳米薄片可以在激发时展现出诸如尺寸可调的发射的性质。这可以使得2D纳米薄片的电致发光最大值(ELmax)或光致发光(PLmax)能够通过控制纳米粒子的横向尺寸进行调节。如本文中使用的,“2D量子点”或“2D QD”是指横向尺寸处于量子限制区域并且厚度为1-5个原子或分子单层的半导体纳米粒子。如本文中使用的,“单层量子点”或“单层QD”是指横向尺寸处于量子限制区域并且厚度为单一单层的半导体纳米粒子。与常规QD相比,2D QD具有高得多的表面积与体积的比值,其随着单层数量减少而增加。对于单层QD看到了最高的表面积与体积的比值。这可以产生具有与常规QD非常不同的表面化学的2DQD,其可以用于诸如催化的应用。
在一个实施方案中,合成方法包括将第一纳米粒子前体和第二纳米粒子前体在一种或多种溶剂中组合以形成溶液,随后将溶液加热至第一温度,持续第一时间段,然后接着将溶液加热至第二温度,持续第二时间段,其中第二温度高于第一温度,以实现纳米粒子前体向2D纳米粒子的转化。
在一个备选的实施方案中,合成方法包括将单源前体溶解在溶剂中以形成溶液,将溶液加热至第一温度,持续第一时间段,然后接着将溶液加热至第二温度,持续第二时间段,其中第二温度高于第一温度,以实现单源前体向2D纳米粒子的转化。
在一个实施方案中,第一前体是金属前体。合适的金属前体可以包括但不限于,无机前体,例如:
金属卤化物,诸如WCln(n=4-6)、Mo6Cl12、MoCl3、[MoCl5]2、NiCl2、MnCl2、VCl3、TaCl5、RuCl3、RhCl3、PdCl2、HfCl4、NbCl5、FeCl2、FeCl3、TiCl4、SrCl2、SrCl2·6H2O、WO2Cl2、MoO2Cl2、CuCl2、ZnCl2、CdCl2、GaCl3、INCl3、WF6、MoF6、NiF2、MnF2、TaF5、NbF5、FeF2、FeF3、TiF3、TiF4、SrF2、NiBr2、MnBr2、VBr3、TaBr5、RuBr3·XH2O、RhBr3、PdBr2、HfBr4、NbBr5、FeBr2、FeBr3、TiBr4、SrBr2、NiI2、MnI2、RuI3、RhI3、Pdl2或TiI4;
(NH4)6H2W12O40或(NH4)6H2Mo12O40;
有机金属前体,诸如羰基金属盐,例如Mo(CO)6、W(CO)6、Ni(CO)4、Mn2(CO)10、Ru3(CO)12、Fe3(CO)12或Fe(CO)5及其烷基和芳基衍生物;
乙酸盐,例如Ni(ac)2·4H2O、Mn(ac)2·4H2O、Rh2(ac)4、Pd3(ac)6、Pd(ac)2、Fe(ac)2、Sr(ac)2、Cu(ac)2、Zn(ac)2、Cd(ac)2或In(ac)3,其中ac=OOCCH3;
乙酰丙酮酸盐,例如Ni(acac)2、Mn(acac)2、V(acac)3、Ru(acac)3、Rh(acac)3、Pd(acac)2、Hf(acac)4、Fe(acac)2、Fe(acac)3、Sr(acac)2、Sr(acac)2·2H2O、Cu(acac)2、Ga(acac)3或In(acac)3,其中acac=CH3C(O)CHC(O)CH3;
己酸盐,例如Mo[OOCH(C2H5)C4H9]x、Ni[OOCCH(C2H5)C4H9]2、Mn[OOCCH(C2H5)C4H9]2、Nb[OOCCH(C2H5)C4H9]4、Fe[OOCCH(C2H5)C4H9]3或Sr[OOCCH(C2H5)C4H9]2;
硬脂酸盐,例如Ni(st)2、Fe(st)2或Zn(st)2,其中st=O2C18H35;
胺前体,例如[M(CO)n(胺)6-n]形式的配合物,其中M是金属;
烷基金属前体,例如W(CH3)6;或
双(乙基苯)钼[(C2H5)yC6H6-y]2Mo(y=1-4)。
在一个实施方案中,第二前体是非金属前体。非限制性实例包括硫属元素前体,诸如但不限于:醇,烷基硫醇或烷基硒醇;羧酸;H2S或H2Se;有机-硫属元素化合物,例如硫脲或硒脲;无机前体,例如Na2S、Na2Se或Na2Te;膦硫属化物,例如三辛基硫化膦、三辛基硒化膦或三辛基碲化膦;硫化十八烯、硒化十八烯或碲化十八烯;二苯基二硫属化物,例如二苯二硫、二苯二硒或二苯二碲;或元素硫、硒或碲。特别合适的硫属元素前体包括直链烷基硒醇和硫醇(诸如辛烷硫醇、辛烷硒醇、十二烷硫醇或十二烷硒醇),或支链烷基硒醇和硫醇(诸如二叔丁基硒醇或叔壬基硫醇),它们可以充当硫属元素源和封端剂二者。已经发现,使用缓释硫属元素源在这样的2D纳米粒子合成方法中提供可控的生长。在本文中,“缓释硫属元素源”被定义为具有硫属元素-碳键的化合物,当该化合物在纳米粒子合成反应中充当硫属元素前体时,所述硫属元素-碳键断开。在另一个实施方案中,缓释硫属元素源最初可以通过硫属元素-硫属元素键的断裂而分解,然后在随后的步骤中,当该化合物在纳米粒子合成反应中充当硫属元素前体时,碳-硫属元素键断开。合适的缓释硫属元素前体包括但不限于:R-S-R’形式的化合物,其中R是烷基或芳基,X是硫属元素,并且R’是H、烷基、芳基或X-R”(其中R”是烷基或芳基)。在一个特别的实施方案中,缓释硫属元素源是缓释硫源,诸如1-十二烷硫醇(DDT)。
其他合适的非金属前体包括第15族前体,诸如但不限于:NR3、PR3、AsR3、SbR3(R=Me、Et、tBu、iBu、iPr、Ph等);NHR2、PHR2、AsHR2、SbHR2(R=Me、Et、Bu、Bu、Pr、Ph等);NH2R、PH2R、AsH2R、SbH2R3(R=Me、Et、tBu、iBu、Pri、Ph等);PH3、AsH3;M(NMe)3,其中M=P、As、Sb;二甲基联氨(Me2NNH2);叠氮乙烷(ethylazide)(Et-NNN);肼(H2NNH2);Me3SiN3;三(三甲基硅烷基)膦;和三(三甲基硅烷基)胂。
在一个实施方案中,单源前体可以充当金属前体和非金属前体二者。合适的单源前体的实例包括但不限于:二硫代氨基甲酸烷基酯;二硒代氨基甲酸烷基酯;与秋兰姆的配合物,例如WS3L2、MoS3L2或MoL4,其中L=E2CNR2,E=S和/或Se,并且R=甲基、乙基、丁基和/或己基;(NH4)2MoS4;(NH4)2WS4;或Mo(StBu)4。
将第一前体和第二前体在一种或多种溶剂中组合,或者将单源前体溶解在一种或多种溶剂中。一种或多种溶剂的沸点必须足够高以使一种或多种溶剂能够加热至足够高的温度以实现第一和第二纳米粒子前体或单源前体向纳米粒子的转化。在一些实施方案中,一种或多种溶剂可以包括配位溶剂。合适的配位溶剂的实例包括但不限于:饱和烷基胺,诸如例如C6-C50烷基胺;不饱和脂肪胺,诸如例如油胺;脂肪酸,诸如例如肉豆蔻酸、棕榈酸和油酸;膦类,诸如例如三辛基膦(TOP);氧化膦类,诸如例如三辛基氧化膦(TOPO);醇类,诸如例如十六醇、苯甲醇、乙二醇、丙二醇;并且可以包括伯、仲、叔和支链溶剂。在一些实施方案中,一种或多种溶剂可以包括非配位溶剂,诸如但不限于C11-C50烷烃。在一些实施方案中,溶剂的沸点为150℃至600℃,例如160℃至400℃,或更特别是180℃至360℃。在一个特别的实施方案中,溶剂是十六胺。在另一个实施方案中,溶剂是肉豆蔻酸。如果使用非配位溶剂,则反应可以在另外的配位剂的存在下进行,以充当配体或封端剂。封端剂通常是路易斯碱,例如膦类、氧化膦类和/或胺类,但是可以使用其他试剂,诸如油酸或有机聚合物,其在纳米粒子周围形成保护性外层覆盖物。其他合适的封端剂包括烷基硫醇或硒醇,包括直链烷基硒醇和硫醇(诸如辛烷硫醇、辛烷硒醇、十二烷硫醇或十二烷硒醇),或支链烷基硒醇和硫醇(诸如二叔丁基硒醇或叔壬基硫醇),它们可以充当硫属元素源和封端剂这二者。其他合适的配体包括可以使纳米粒子的表面与不同官能度的基团例如S-和O-端基配位的二齿配体。
在一个实施方案中,将溶液加热至第一温度,持续第一时间段。第一温度可以在50至550℃、例如150至450℃、或更特别是200至350℃的范围内。第一时间段可以在10秒至5小时、例如2分钟至2小时、或更特别是5分钟至50分钟的范围内。在特别的实例中,将溶液加热至约260℃的第一温度,持续约20分钟。
在一个实施方案中,随后将溶液加热至第二温度,持续第二时间段,其中第二温度高于第一温度。第二温度可以在80至600℃、例如200至500℃、或更特别是300至400℃的范围内。在一个特别的实施方案中,第二温度是溶液的沸点,并且将溶液加热至回流。第二时间段可以在5分钟至1周、例如10分钟至1天、或更特别是20分钟至5小时的范围内。在一个特别的实例中,将溶液加热至约330℃的第二温度,持续约20分钟。增加在第二温度加热溶液的持续时间可以增加产率和/或改变所得2D纳米粒子的尺寸。
可以通过任何合适的技术从反应溶液中分离2D纳米粒子。实例包括但不限于离心、过滤、透析和柱色谱。可以采用尺寸选择性分离程序来提取具有类似尺寸并且因此具有类似发射性质的2D纳米粒子。
在胶体溶液中合成纳米粒子是特别有利的,因为它们允许控制纳米粒子的形状、尺寸和组成,并且可以提供可扩展性。胶体纳米粒子也可以用配体(封端剂)进行表面官能化,其中可以选择配体以赋予在一系列溶剂中的溶解性。配体也可以用于控制所得纳米粒子的形状。在纳米粒子合成期间沉积在纳米粒子表面上的固有配体可以与替代配体交换以赋予特定功能,诸如在特定溶剂中改善的溶液可加工性。
可以调节试剂的选择和反应参数(诸如温度和时间),以控制2D纳米粒子的横向尺寸和厚度这两者,并且由此控制它们的发射性质,诸如发射的光的波长(颜色)。
通过本文所述方法制备的2D纳米粒子可以溶解或分散在合适的溶剂中以提供溶液可加工性。溶液可加工的2D纳米粒子对以下应用特别具有吸引力,诸如光致发光显示器和照明设备、电致发光显示器和照明设备、2D异质结构器件、催化(例如,析氢反应、析氧反应、催化脱硫等)、传感器和生物成像。
本发明的一个特别的示例性实施方案是制备MoS2的2D纳米粒子的简单方法。首先,形成包含钼和胺的配合物。六羰基钼可以用作钼源。关于金属羰基化合物中键合的讨论,参见例如C.Kraihanzel和F.Cotton,Inorg.Chem.,1963,2,533以及R.Dennenberg和D.Darensbourg,Inorg.Chem.,1972,11,72。油胺可以用作胺源,不仅因为它是液体并且易于使用,而且还因为双键可以通过π-键合到金属中心从而有助于极易于升华的挥发性Mo(CO)6的溶解,进而提供一些功能用途(参见S.Ghosh,S.Khamarui,M.Saha和S.K.De,RSCAdv.,2015,5,38971)。优选将胺彻底脱气,然后用于形成预先称重的钼源的悬浮液并且转移回到反应烧瓶中。由于Mo(CO)6易于升华,所以不能将其置于真空下,并且需要将其温和加热至~150℃以形成配合物。溶液在150℃变为黄绿色然后变为深黄色/褐色。此时,可以将其快速加热至约250℃至300℃。然后快速加入DDT并且将溶液放置一段时间。
在另一个示例性实施方案中,形成包含钼和胺的配合物。在150℃,加入硫源,并且将混合物转移至注射器中并且快速注入另外量的胺中。将溶液加热至260℃,持续第一时间段。随后将温度升至回流并且保持第二时间段。
实施例1:MoS2纳米粒子的制备
在手套箱中将0.132g Mo(CO)6加入至用橡胶隔片[SIGMA-ALDRICH CO.,LLC,3050Spruce Street,St.Louis MISSOURI 63103]盖住的小瓶中。
在圆底烧瓶中,将14mL油胺在100℃脱气2小时,然后冷却至室温。
用注射器取出10mL脱气油胺,并且将2-3mL注入到含有Mo(CO)6的小瓶中并且摇匀。使用用氮气吹扫三次的干净注射器/针头,将油胺/Mo(CO)6悬浮液转移回到圆底烧瓶中。
将另外的2-3mL油胺加入至含有Mo(CO)6的小瓶中。将其摇匀并且将内容物再次转移回到圆底烧瓶中。重复该过程直至将所有油胺和Mo(CO)6转移至圆底烧瓶中。
将反应混合物温和地温热至150℃并且摇动烧瓶以溶解任何升华的Mo(CO)6。
然后将反应混合物加热至250℃。
快速注入0.25mL DDT。
将反应放置30分钟,并且注入另外0.25mL DDT并且再次放置30分钟。
然后将反应加热至300℃,并且注入0.5mL DDT并且放置30分钟。
将反应混合物冷却至室温。
为了分离产物,加入20mL丙酮并且弃去上清液。
然后加入20mL甲苯,接着加入60mL丙酮。
将混合物离心并且弃去上清液。
然后加入10mL己烷,接着加入20mL丙酮,然后加入10mL乙腈,并且离心。弃去上清液,并且用丙酮冲洗固体,最后溶解在5mL己烷中。需要对固体进行简单的超声处理以获得完全溶解。
将溶液离心并且弃去任何剩余的固体。
实施例2:MoS2纳米粒子的制备
合成在惰性N2环境下进行。
在圆底烧瓶中将14g十八烷在100℃脱气2小时,然后冷却至室温。
在小瓶中将2g十六胺和2g十八烷在100℃脱气2小时,然后冷却至40-50℃,并且注入到含有Mo(CO)6的小瓶中并且摇匀。
将反应混合物温和地温热至150℃并且摇动小瓶以溶解任何升华的Mo(CO)6,然后冷却至室温以形成Mo(CO)6-胺配合物。
然后将圆底烧瓶(含有14g十八烷)加热至300℃。
将Mo(CO)6-胺配合物温和地温热至~40℃直至固体熔融,并且加入1.5mL的1-十二烷硫醇(DDT)。然后将其立即装入注射器中并且迅速注入圆底烧瓶中。将温度调节至~260℃。
将反应混合物在260℃放置8分钟。
为了分离产物,加入与混合有10mL乙腈的40mL丙醇,以4000rpm离心5分钟,并且弃去上清液。
实施例3:MoS2纳米粒子的制备
在200-mL小瓶中,将十六胺(10g)和十六烷(50mL)在80℃在真空下脱气。将十六胺/十六烷溶液加入至250-mL圆底烧瓶中的Mo(CO)6(0.66g)中,并且在120℃搅拌以形成溶液(“溶液A”)。
在1-L圆底烧瓶中,将十六烷(50mL)和十六胺(5g)在80℃在真空下加热1小时。在N2下将溶液加热至250℃,以形成溶液(“溶液B”)。在250℃,每5分钟向溶液B中加入5-mL份的溶液A(保持在120℃),持续1小时,以形成溶液(“溶液C”)。
随后使用注射泵将1-十二烷硫醇(7.5mL)在250℃在1小时内缓慢加入溶液C中,然后在250℃搅拌另外1小时。将溶液冷却至60℃,然后加入丙酮(400mL),随后离心。将残余的固体分散在己烷(125mL)中。
实施例4:MoS22D纳米粒子的制备
在小瓶中将十六胺(4g)在100℃脱气2小时,然后冷却至40-50℃,并且注入到含有Mo(CO)6的小瓶中,然后摇匀。
将反应混合物温和地温热至150℃并且摇动小瓶以溶解任何升华的Mo(CO)6,形成Mo(CO)6-x-(胺)x配合物(其中1≤x<6),并且将其保持在刚好高于溶液的熔点。
另外,在圆底烧瓶中将十六胺(14g)在100℃脱气2小时,然后冷却至室温。
将含有十六胺的圆底烧瓶加热至300℃。
将1-十二烷硫醇(1.5mL)加入Mo(CO)6-x-(胺)x配合物中,然后将混合物立即转移至注射器中并且快速注入含有十六胺的圆底烧瓶中。将温度调节至~260℃并且保持40分钟。
然后将温度升至回流(330℃)并且在该温度保持20分钟直至形成黑色沉淀物。
将烧瓶冷却至60℃,并且加入甲苯(30mL)。将混合物在7000rpm离心5分钟,并且分离和弃去黑色物质。将上清液在真空下干燥,然后加入乙腈(50mL),温热,并且将顶部澄清层倾析并弃去,以留下油层。将该过程重复三次以移除过量的十六胺。最后将该物质溶解在丙醇中,并且通过0.2-μm PTFE过滤器过滤。
溶液展现出亮蓝色发射。PL等高线图(参见图1)示出了对于MoS22D纳米粒子溶液,针对激发波长(y-轴)绘制的发射波长(x-轴)。该材料显示出激发波长依赖性发射,当在约370nm激发时,最高强度发射集中在约430nm。
拉曼光谱(图2)示出了375cm-1和403cm-1处的峰,其指示MoS2。注意:约300cm-1和500cm-1处的峰来自背景光谱。
前述内容呈现了体现本发明原理的系统的特定实施方案。本领域技术人员将能够设计出替代方案和变型,即使在本文中并未明确公开,这些替代方案和变型也体现了那些原理并且因此在本发明的范围内。虽然已经示出和描述了本发明的特定实施方案,但是它们并不旨在限制本专利所涵盖的内容。本领域技术人员将理解,如在字面上和等同地由所附权利要求所涵盖的,可以在不脱离本发明的范围的情况下进行各种改变和修改。
Claims (4)
1.一种制备MoS2纳米粒子的方法,所述方法包括:
在密封容器中搅拌六羰基钼(Mo(CO)6)和脱气油胺的混合物以产生油胺/Mo(CO)6的悬浮液;
将所述油胺/Mo(CO)6的悬浮液的至少一部分转移至含有脱气油胺的容器中以形成反应混合物;
将所述反应混合物加热至250℃;
将第一部分的1-十二烷硫醇加入所述反应混合物中;
将所述反应混合物在250℃加热30分钟;
将第二部分的1-十二烷硫醇加入所述反应混合物中;
将所述反应混合物在250℃加热30分钟;
然后将所述反应混合物加热至300℃;
然后将第三部分的1-十二烷硫醇加入所述反应混合物中;以及
将所述反应混合物在300℃加热30分钟。
2.根据权利要求1所述的方法,还包括:
分离所述纳米粒子;和
将分离的纳米粒子溶解在溶剂中。
3.一种制备MoS2纳米粒子的方法,所述方法包括:
在密封容器中搅拌六羰基钼(Mo(CO)6)、脱气十八烷和脱气十六胺的混合物以产生第一反应混合物;
将所述反应混合物加热至150℃,然后将所述第一反应混合物冷却至室温,以形成Mo(CO)6-胺配合物;
将一定体积的脱气十八烷加热至300℃;
将所述Mo(CO)6-胺配合物温热至40℃以使任何固体熔融;
将1-十二烷硫醇加入到温热的Mo(CO)6-胺配合物中以产生第二反应混合物;
将所述第二反应混合物加入到经加热的所述一定体积的脱气十八烷中,以形成第三反应混合物;以及,
将所述第三反应混合物加热至260℃,持续8分钟。
4.一种制备MoS2纳米粒子的方法,所述方法包括:
在120℃搅拌六羰基钼(Mo(CO)6)、脱气十六烷和脱气十六胺的混合物以产生第一溶液;
将十六烷和十六胺的混合物在80℃在真空下加热1小时,然后将所述十六烷和十六胺的混合物在N2下加热至250℃以形成第二溶液;
将保持在120℃的所述第一溶液的一部分加入到所述第二溶液中,每5分钟一次,持续1小时,以形成第三溶液;以及
在1小时的时间段内,将1-十二烷硫醇在250℃加入到所述第三溶液中。
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US20200067002A1 (en) * | 2018-08-23 | 2020-02-27 | Nanoco 2D Materials Limited | Photodetectors Based on Two-Dimensional Quantum Dots |
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2005056368A (ja) * | 2003-08-07 | 2005-03-03 | Digital Concept:Kk | プリントシステム |
CN101468793A (zh) * | 2007-12-26 | 2009-07-01 | 三星电机株式会社 | 制备层状结构纳米颗粒的方法 |
CN104692463A (zh) * | 2015-02-15 | 2015-06-10 | 清华大学 | 一种油溶性纳米二硫化钼的制备方法 |
CN105060347A (zh) * | 2015-07-20 | 2015-11-18 | 清华大学 | 一种合成超薄二硫化钼纳米晶的方法 |
KR20150143168A (ko) * | 2014-06-13 | 2015-12-23 | 주식회사 엘지화학 | 금속 칼코젠 나노시트의 제조 방법 |
CN105523585A (zh) * | 2016-02-26 | 2016-04-27 | 吉林大学 | 一种二维MoS2纳米片的制备方法 |
CN105800566A (zh) * | 2016-04-15 | 2016-07-27 | 中国科学院上海技术物理研究所 | 交替注入反应物生长单层和多层过渡金属硫化物的方法 |
Family Cites Families (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA2432993A1 (en) * | 2002-07-08 | 2004-01-08 | Infineum International Limited | Molybdenum-sulfur additives |
KR100621309B1 (ko) * | 2004-04-20 | 2006-09-14 | 삼성전자주식회사 | 황 전구체로서 싸이올 화합물을 이용한 황화 금속나노결정의 제조방법 |
JP2007169605A (ja) | 2005-11-24 | 2007-07-05 | National Institute Of Advanced Industrial & Technology | 蛍光体、及びその製造方法 |
JP2009082910A (ja) * | 2007-09-14 | 2009-04-23 | Toyota Motor Corp | 微粒子コンポジット、その製造方法、固体高分子型燃料電池用触媒、及び固体高分子型燃料電池 |
JP5019052B2 (ja) | 2007-12-28 | 2012-09-05 | 独立行政法人放射線医学総合研究所 | CdSe量子ドット及びその製造方法 |
IT1402163B1 (it) * | 2010-10-01 | 2013-08-28 | Univ Degli Studi Salerno | Sintesi "one-pot" di nano cristalli 1d, 2d, e 0d di calcogenuri di tungsteno e molibdeno (ws2, mos2) funzionalizzati con ammine e/o acidi grassi a lunga catena e/o tioli |
WO2014009815A2 (en) * | 2012-07-09 | 2014-01-16 | Nanoco Technologies, Ltd. | Group xiii selenide nanoparticles |
CN103896222B (zh) | 2012-12-24 | 2016-01-20 | 中国科学技术大学 | 超薄纳米片半导体材料的制备方法 |
US9196767B2 (en) * | 2013-07-18 | 2015-11-24 | Nanoco Technologies Ltd. | Preparation of copper selenide nanoparticles |
US10079144B2 (en) * | 2015-04-22 | 2018-09-18 | Samsung Electronics Co., Ltd. | Composition for layered transition metal chalcogenide compound layer and method of forming layered transition metal chalcogenide compound layer |
KR20180027629A (ko) * | 2015-07-30 | 2018-03-14 | 퍼시픽 라이트 테크놀로지스 코포레이션 | 카드뮴 함량이 낮은 나노결정질 양자점 헤테로구조물 |
CN105129748B (zh) | 2015-08-24 | 2018-03-06 | 南京邮电大学 | 一种制备过渡金属硫族化合物量子点的方法 |
US10059585B2 (en) | 2016-06-28 | 2018-08-28 | Nanoco Technologies Ltd. | Formation of 2D flakes from chemical cutting of prefabricated nanoparticles and van der Waals heterostructure devices made using the same |
CN106395765B (zh) | 2016-08-25 | 2019-03-01 | 中国石油大学(华东) | 一种二碲化钼电化学储能材料、制备方法及其应用 |
US10662074B2 (en) | 2016-12-30 | 2020-05-26 | Nanoco Technologies Ltd. | Template-assisted synthesis of 2D nanosheets using nanoparticle templates |
CN107416905B (zh) * | 2017-06-22 | 2019-03-08 | 河南大学 | 一种油溶性二硫化钨纳米片的制备方法 |
-
2018
- 2018-01-24 US US15/879,136 patent/US10883046B2/en active Active
- 2018-01-25 EP EP19189487.2A patent/EP3594181B1/en active Active
- 2018-01-25 CN CN201880008844.7A patent/CN110300731B/zh active Active
- 2018-01-25 CN CN202010051062.0A patent/CN111187613A/zh active Pending
- 2018-01-25 EP EP18703636.3A patent/EP3577075B1/en active Active
- 2018-01-25 JP JP2019541795A patent/JP6975988B2/ja active Active
- 2018-01-25 WO PCT/IB2018/050465 patent/WO2018142247A1/en unknown
- 2018-01-25 KR KR1020197021276A patent/KR102594243B1/ko active IP Right Grant
- 2018-02-02 TW TW107103901A patent/TWI679171B/zh active
- 2018-02-02 TW TW108146717A patent/TWI754869B/zh active
-
2020
- 2020-10-29 US US17/084,443 patent/US11274247B2/en active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2005056368A (ja) * | 2003-08-07 | 2005-03-03 | Digital Concept:Kk | プリントシステム |
CN101468793A (zh) * | 2007-12-26 | 2009-07-01 | 三星电机株式会社 | 制备层状结构纳米颗粒的方法 |
KR20150143168A (ko) * | 2014-06-13 | 2015-12-23 | 주식회사 엘지화학 | 금속 칼코젠 나노시트의 제조 방법 |
CN104692463A (zh) * | 2015-02-15 | 2015-06-10 | 清华大学 | 一种油溶性纳米二硫化钼的制备方法 |
CN105060347A (zh) * | 2015-07-20 | 2015-11-18 | 清华大学 | 一种合成超薄二硫化钼纳米晶的方法 |
CN105523585A (zh) * | 2016-02-26 | 2016-04-27 | 吉林大学 | 一种二维MoS2纳米片的制备方法 |
CN105800566A (zh) * | 2016-04-15 | 2016-07-27 | 中国科学院上海技术物理研究所 | 交替注入反应物生长单层和多层过渡金属硫化物的方法 |
Non-Patent Citations (2)
Title |
---|
Generalized and Facile Synthesis of Semiconducting Metal Sulfide Nanocrystals;Jin Joo et al.;《Journal of the American Chemical Society》;20030813;第125卷;第11100-11105页 * |
Large-Scale Synthesis of Ultrathin Bi2S3 Necklace Nanowires;Ludovico Cademartiri et al.;《Angewandte Chemie》;20080409;第120卷;第3874-3877页 * |
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