CN116462164A - 一种制备碲基超薄半导体纳米片的方法 - Google Patents
一种制备碲基超薄半导体纳米片的方法 Download PDFInfo
- Publication number
- CN116462164A CN116462164A CN202310373393.XA CN202310373393A CN116462164A CN 116462164 A CN116462164 A CN 116462164A CN 202310373393 A CN202310373393 A CN 202310373393A CN 116462164 A CN116462164 A CN 116462164A
- Authority
- CN
- China
- Prior art keywords
- tellurium
- inorganic
- salt
- solution
- ultrathin semiconductor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 37
- 239000004065 semiconductor Substances 0.000 title claims abstract description 32
- 239000002135 nanosheet Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 41
- 239000002184 metal Substances 0.000 claims abstract description 41
- 239000002243 precursor Substances 0.000 claims abstract description 31
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 150000003973 alkyl amines Chemical class 0.000 claims abstract description 9
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 229910010277 boron hydride Inorganic materials 0.000 claims abstract description 7
- 239000003446 ligand Substances 0.000 claims abstract description 7
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims description 15
- -1 boron hydride compound Chemical class 0.000 claims description 7
- 150000000918 Europium Chemical class 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 4
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 4
- 150000001462 antimony Chemical class 0.000 claims description 4
- 150000001621 bismuth Chemical class 0.000 claims description 4
- 150000001661 cadmium Chemical class 0.000 claims description 4
- 150000001879 copper Chemical class 0.000 claims description 4
- 150000002471 indium Chemical class 0.000 claims description 4
- 150000002696 manganese Chemical class 0.000 claims description 4
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 4
- 159000000008 strontium salts Chemical class 0.000 claims description 4
- 150000003751 zinc Chemical class 0.000 claims description 4
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 3
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 3
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 3
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 3
- FDIOSTIIZGWENY-UHFFFAOYSA-N n-[bis(diethylamino)phosphanyl]-n-ethylethanamine Chemical compound CCN(CC)P(N(CC)CC)N(CC)CC FDIOSTIIZGWENY-UHFFFAOYSA-N 0.000 claims description 3
- XVDBWWRIXBMVJV-UHFFFAOYSA-N n-[bis(dimethylamino)phosphanyl]-n-methylmethanamine Chemical compound CN(C)P(N(C)C)N(C)C XVDBWWRIXBMVJV-UHFFFAOYSA-N 0.000 claims description 3
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- VOADVZVYWFSHSM-UHFFFAOYSA-L sodium tellurite Chemical compound [Na+].[Na+].[O-][Te]([O-])=O VOADVZVYWFSHSM-UHFFFAOYSA-L 0.000 claims description 3
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 claims description 3
- TUQOTMZNTHZOKS-UHFFFAOYSA-N tributylphosphine Chemical compound CCCCP(CCCC)CCCC TUQOTMZNTHZOKS-UHFFFAOYSA-N 0.000 claims description 3
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 claims description 3
- ZMBHCYHQLYEYDV-UHFFFAOYSA-N trioctylphosphine oxide Chemical compound CCCCCCCCP(=O)(CCCCCCCC)CCCCCCCC ZMBHCYHQLYEYDV-UHFFFAOYSA-N 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 239000002064 nanoplatelet Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- SKJCKYVIQGBWTN-UHFFFAOYSA-N (4-hydroxyphenyl) methanesulfonate Chemical compound CS(=O)(=O)OC1=CC=C(O)C=C1 SKJCKYVIQGBWTN-UHFFFAOYSA-N 0.000 description 2
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 description 2
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 2
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- QYIGOGBGVKONDY-UHFFFAOYSA-N 1-(2-bromo-5-chlorophenyl)-3-methylpyrazole Chemical compound N1=C(C)C=CN1C1=CC(Cl)=CC=C1Br QYIGOGBGVKONDY-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical compound C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical class [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910000011 cadmium carbonate Inorganic materials 0.000 description 1
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 description 1
- GKDXQAKPHKQZSC-UHFFFAOYSA-L cadmium(2+);carbonate Chemical compound [Cd+2].[O-]C([O-])=O GKDXQAKPHKQZSC-UHFFFAOYSA-L 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- JVLRYPRBKSMEBF-UHFFFAOYSA-K diacetyloxystibanyl acetate Chemical compound [Sb+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JVLRYPRBKSMEBF-UHFFFAOYSA-K 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- LNYNHRRKSYMFHF-UHFFFAOYSA-K europium(3+);triacetate Chemical compound [Eu+3].CC([O-])=O.CC([O-])=O.CC([O-])=O LNYNHRRKSYMFHF-UHFFFAOYSA-K 0.000 description 1
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 description 1
- NNMXSTWQJRPBJZ-UHFFFAOYSA-K europium(iii) chloride Chemical compound Cl[Eu](Cl)Cl NNMXSTWQJRPBJZ-UHFFFAOYSA-K 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
- 229940046892 lead acetate Drugs 0.000 description 1
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 1
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229940071125 manganese acetate Drugs 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 description 1
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 1
- 229940071536 silver acetate Drugs 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 229910001631 strontium chloride Inorganic materials 0.000 description 1
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 description 1
- FAKFSJNVVCGEEI-UHFFFAOYSA-J tin(4+);disulfate Chemical compound [Sn+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FAKFSJNVVCGEEI-UHFFFAOYSA-J 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明公开了一种制备碲基超薄半导体纳米片的方法，其方法步骤为：（1）取金属前驱体溶解在烷基胺和非配体溶液中，在惰性环境下通过搅拌、加热使溶液澄清，降温后即获得金属前驱体溶液；（2）取碲源溶解在有机膦溶液中，在惰性环境下通过搅拌、加热使溶液澄清，降温后即获得碲前驱体溶液；（3）将金属前驱体溶液和碲前驱体溶液以及金属硼氢化合物放入反应釜中，在惰性气体保护下进行反应，即可获得碲基超薄半导体纳米片。本合成方法操作简便、反应条件温和、可适用多个反应体系；利用该方法可制备出厚度小于3纳米的碲基超薄半导体纳米片；制备的产品在光电探测、光电催化等领域具有巨大的应用前景。
Description
技术领域
本发明涉及一种纳米片的制备方法，尤其是一种制备碲基超薄半导体纳米片的方法。
背景技术
超薄半导体纳米片是指在厚度方向小于3纳米，其他维度方向没有限制的二维半导体材料。相比于常规厚度（厚度大于3纳米）的半导体纳米片，超薄半导体纳米片具有更大的比表面积和更显著的量子限域效应，使其成为光电子器件最理想的构筑单元。因此，人们将超薄半导体纳米片的合成和应用视作研究的热点。
近年来，科研工作者虽然已经通过气相沉积法、模板法、液相非催化法等策略合成了常规厚度的半导体纳米片，但是，遗憾的是，上述方法由于需要高的合成温度或厚度大于3纳米的模板，使其想要制备出直径小于3纳米的超薄半导体纳米片是非常困难的。更不用说将其发展成为一种制备超薄纳米片的普适性方法。
发明内容
本发明要解决的技术问题是提供一种工艺简单的制备碲基超薄半导体纳米片的方法。
为解决上述技术问题，本发明所采取的方法步骤为：
（1）取金属前驱体溶解在烷基胺和非配体溶液中，在惰性环境下通过搅拌、加热使溶液澄清，降温后即获得金属前驱体溶液；
（2）取碲源溶解在有机膦溶液中，在惰性环境下通过搅拌、加热使溶液澄清，降温后即获得碲前驱体溶液；
（3）将金属前驱体溶液和碲前驱体溶液以及金属硼氢化合物放入反应釜中，在惰性气体保护下进行反应，即可获得碲基超薄半导体纳米片。
进一步的，所述步骤（1）中，金属前驱体选自无机锌盐、无机镉盐、无机铅盐、无机银盐、无机锡盐、无机锑盐、无机铋盐、无机铜盐、无机锰盐、无机铕盐、无机锶盐和无机铟盐中的一种；烷基胺选自油胺、十二胺、辛胺、十六胺和十八胺中的一种或几种。
进一步的，所述步骤（2）中，碲源为碲粉、二氧化碲和/或亚碲酸钠；有机膦选自三正辛基膦、三正辛基氧膦、三（二乙胺基）膦、三正丁基膦、三（二甲胺基）膦中的一种或几种。
进一步的，所述步骤（3）中，金属硼氢化合物为硼氢化钠、三乙基硼氢化锂和/或三仲丁基硼氢化锂。
进一步的，所述步骤（3）中，反应温度在70～130℃，反应时间在8～24h。
进一步的，所述步骤（1）中，取0.1～0.5mmol的金属前驱体溶解在6～12mL的烷基胺和4～10mL的非配体溶液中；所述步骤（2）中，取0.1～0.5mmol的碲源，溶解在2～10mL的有机膦溶液中；所述步骤（3）中，金属硼氢化合物加入量为0.01～0.2mmol。
采用上述技术方案所产生的有益效果在于：本发明所述合成方法操作简便、反应条件温和、可适用多个反应体系；利用该方法可制备出厚度小于3纳米的碲基超薄半导体纳米片；制备的产品在光电探测、光电催化等领域具有巨大的应用前景。
附图说明
下面结合附图和具体实施方式对本发明作进一步详细的说明。
图1是本发明实施例1所得碲化锌超薄纳米片的透射电镜图；
图2是本发明实施例4所得碲化铜超薄纳米片的透射电镜图；
图3是本发明实施例7所得碲化铋超薄纳米片的透射电镜图。
具体实施方式
本制备碲基超薄半导体纳米片的方法，所述碲基超薄半导体为MTe超薄半导体，M金属选自Ag金属盐、Zn金属盐、Pb金属盐、Sn金属盐、镉金属盐、Sb金属盐、Bi金属盐、Cu金属盐、Mn金属盐、Eu金属盐、Sr金属盐和In金属盐中的一种；该制备方法包括以下步骤：
（1）制备金属前驱体溶液：称取0.1～0.5mmol的金属前驱体，使其溶解在6～12mL的烷基胺和4～10mL的非配体溶液中，反应溶液中通入氮气排出空气使其保持无氧的惰性环境，然后通过搅拌、加热使反应溶液澄清，澄清的溶液降温后即获得金属前驱体溶液。
所述金属前驱体选自无机锌盐、无机镉盐、无机铅盐、无机银盐、无机锡盐、无机锑盐、无机铋盐、无机铜盐、无机锰盐、无机铕盐、无机锶盐和无机铟盐中的一种。所述无机锌盐包括乙酸锌、硝酸锌和/或氯化锌；所述无机镉盐包括氯化镉、硝酸镉和/或碳酸镉；所述无机铅盐包括乙酸铅、硝酸铅和/或氯化铅；所述无机银盐包括乙酸银和/或硝酸银；所述无机锡盐包括氯化锡和/或硫酸锡；所述无机锑盐包括三氯化锑和/或醋酸锑；所述无机铋盐包括氯化铋、硝酸铋和/或乙酸铋；所述无机铜盐包括氯化铜、乙酸铜和/或硝酸铜；所述无机锰盐包括氯化锰、硝酸锰和/或乙酸锰；所述无机铕盐包括氯化铕、硝酸铕和/或乙酸铕；所述无机锶盐包括氯化锶、乙酸锶和/或碳酸锶；所述无机铟盐包括硝酸铟和/或三氯化铟。所述烷基胺包括油胺、十二胺、辛胺、十六胺和/或十八胺。所述非配体溶液包括十八烯和/或二苯醚。
（2）制备碲前驱体溶液：称取0.1～0.5mmol的碲源，溶解在2～10mL的有机膦溶液中，反应溶液中通入氮气排出空气使其保持无氧的惰性环境，然后通过搅拌、加热使反应溶液澄清，澄清的溶液降温后即获得碲前驱体溶液。所述碲源包括碲粉、二氧化碲和/或亚碲酸钠；所述有机膦为三正辛基膦、三正辛基氧膦、三（二乙胺基）膦、三正丁基膦和/或三（二甲胺基）膦。
（3）合成MTe超薄半导体纳米片：将步骤（1）所得金属前驱体溶液和步骤（2）所得碲前驱体溶液以及0.01～0.2mmol的金属硼氢化合物放入反应釜中，在惰性气体保护下，控制反应温度在70～130℃、反应时间调控在8～24h，即可获得MTe超薄半导体纳米片。所述金属硼氢化合物包括硼氢化钠、三乙基硼氢化锂和/或三仲丁基硼氢化锂。所合成的MTe超薄半导体纳米片的厚度能达到1～3nm，横向长度能达到0.3～6μm。
实施例1-32：本制备碲基超薄半导体纳米片的方法采用下述具体工艺。
1）采用上述工艺步骤，各实施例步骤（1）制备金属前驱体溶液和步骤（2）制备碲前驱体溶液所采用的原料及其用量见表1；
表1：各实施例前驱体溶液的原料及其用量
2）各实施例步骤（3）合成MTe超薄半导体纳米片所采用的原料及用量和工艺参数见表2，所得MTe超薄半导体纳米片的厚度和横向长度等尺寸见表2；
表2：各实施例合成工艺参数及产品尺寸
图1、图2和图3分别为实施例1、实施例4和实施例7所得碲化锌超薄纳米片的透射电镜图；由图1、图2和图3可以看出，所得纳米片为超薄的片层材料。
Claims (6)
1.一种制备碲基超薄半导体纳米片的方法，其特征在于，其方法步骤为：
（1）取金属前驱体溶解在烷基胺和非配体溶液中，在惰性环境下通过搅拌、加热使溶液澄清，降温后即获得金属前驱体溶液；
（2）取碲源溶解在有机膦溶液中，在惰性环境下通过搅拌、加热使溶液澄清，降温后即获得碲前驱体溶液；
（3）将金属前驱体溶液和碲前驱体溶液以及金属硼氢化合物放入反应釜中，在惰性气体保护下进行反应，即可获得碲基超薄半导体纳米片。
2.根据权利要求1所述的一种制备碲基超薄半导体纳米片的方法，其特征在于：所述步骤（1）中，金属前驱体选自无机锌盐、无机镉盐、无机铅盐、无机银盐、无机锡盐、无机锑盐、无机铋盐、无机铜盐、无机锰盐、无机铕盐、无机锶盐和无机铟盐中的一种；烷基胺选自油胺、十二胺、辛胺、十六胺和十八胺中的一种或几种。
3.根据权利要求1所述的一种制备碲基超薄半导体纳米片的方法，其特征在于：所述步骤（2）中，碲源为碲粉、二氧化碲和/或亚碲酸钠；有机膦选自三正辛基膦、三正辛基氧膦、三（二乙胺基）膦、三正丁基膦、三（二甲胺基）膦中的一种或几种。
4.根据权利要求1所述的一种制备碲基超薄半导体纳米片的方法，其特征在于：所述步骤（3）中，金属硼氢化合物为硼氢化钠、三乙基硼氢化锂和/或三仲丁基硼氢化锂。
5.根据权利要求1所述的一种制备碲基超薄半导体纳米片的方法，其特征在于：所述步骤（3）中，反应温度在70～130℃，反应时间在8～24h。
6.根据权利要求1-5任意一项所述的一种制备碲基超薄半导体纳米片的方法，其特征在于：所述步骤（1）中，取0.1～0.5mmol的金属前驱体溶解在6～12mL的烷基胺和4～10mL的非配体溶液中；所述步骤（2）中，取0.1～0.5mmol的碲源，溶解在2～10mL的有机膦溶液中；所述步骤（3）中，金属硼氢化合物加入量为0.01～0.2mmol。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310373393.XA CN116462164A (zh) | 2023-04-10 | 2023-04-10 | 一种制备碲基超薄半导体纳米片的方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310373393.XA CN116462164A (zh) | 2023-04-10 | 2023-04-10 | 一种制备碲基超薄半导体纳米片的方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116462164A true CN116462164A (zh) | 2023-07-21 |
Family
ID=87176436
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310373393.XA Pending CN116462164A (zh) | 2023-04-10 | 2023-04-10 | 一种制备碲基超薄半导体纳米片的方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116462164A (zh) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110300076A1 (en) * | 2008-10-03 | 2011-12-08 | Life Technologies Corporation | METHODS FOR PREPARATION OF ZnTe NANOCRYSTALS |
| KR20130094599A (ko) * | 2012-02-16 | 2013-08-26 | 고려대학교 산학협력단 | 용액 합성법을 이용한 카드뮴 텔러라이드 나노선의 제조방법 및 이에 의해 제조된 카드뮴 텔러라이드 나노선 |
| KR101493937B1 (ko) * | 2013-09-06 | 2015-02-17 | 한국전기연구원 | 초음파를 이용하여 형성된 이차원 나노시트 및 그 제조방법 |
| CN105200520A (zh) * | 2015-10-09 | 2015-12-30 | 广东工业大学 | 一种制备Bi2(SexTe1-x)3单晶纳米片的方法 |
| CN106670498A (zh) * | 2016-12-13 | 2017-05-17 | 中国海洋大学 | 铜铟碲超薄规则半导体纳米片的制备方法 |
| CN106976848A (zh) * | 2016-01-15 | 2017-07-25 | 中国药科大学 | 碲(Te)的新型溶解方法、碲化物Zn-Ag-In-Te的合成及其在肿瘤热疗和太阳能电池方面的应用 |
| CN108394872A (zh) * | 2017-02-07 | 2018-08-14 | 北京师范大学 | 一种制备金属硫族化合物半导体超细超长纳米线的方法及所制备的特征纳米线 |
| CN108821246A (zh) * | 2018-07-23 | 2018-11-16 | 山西师范大学 | 一种硫属化合物纳米片及其制备方法 |
| CN110697663A (zh) * | 2019-10-30 | 2020-01-17 | 深圳技术大学 | 一种碲掺杂铜锌锡硫纳米颗粒的制备方法 |
| CN112941627A (zh) * | 2021-01-29 | 2021-06-11 | 中南大学 | 一种垂直生长的超薄Cr2Te3单晶纳米片的制备方法 |
-
2023
- 2023-04-10 CN CN202310373393.XA patent/CN116462164A/zh active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110300076A1 (en) * | 2008-10-03 | 2011-12-08 | Life Technologies Corporation | METHODS FOR PREPARATION OF ZnTe NANOCRYSTALS |
| KR20130094599A (ko) * | 2012-02-16 | 2013-08-26 | 고려대학교 산학협력단 | 용액 합성법을 이용한 카드뮴 텔러라이드 나노선의 제조방법 및 이에 의해 제조된 카드뮴 텔러라이드 나노선 |
| KR101493937B1 (ko) * | 2013-09-06 | 2015-02-17 | 한국전기연구원 | 초음파를 이용하여 형성된 이차원 나노시트 및 그 제조방법 |
| CN105200520A (zh) * | 2015-10-09 | 2015-12-30 | 广东工业大学 | 一种制备Bi2(SexTe1-x)3单晶纳米片的方法 |
| CN106976848A (zh) * | 2016-01-15 | 2017-07-25 | 中国药科大学 | 碲(Te)的新型溶解方法、碲化物Zn-Ag-In-Te的合成及其在肿瘤热疗和太阳能电池方面的应用 |
| CN106670498A (zh) * | 2016-12-13 | 2017-05-17 | 中国海洋大学 | 铜铟碲超薄规则半导体纳米片的制备方法 |
| CN108394872A (zh) * | 2017-02-07 | 2018-08-14 | 北京师范大学 | 一种制备金属硫族化合物半导体超细超长纳米线的方法及所制备的特征纳米线 |
| CN108821246A (zh) * | 2018-07-23 | 2018-11-16 | 山西师范大学 | 一种硫属化合物纳米片及其制备方法 |
| CN110697663A (zh) * | 2019-10-30 | 2020-01-17 | 深圳技术大学 | 一种碲掺杂铜锌锡硫纳米颗粒的制备方法 |
| CN112941627A (zh) * | 2021-01-29 | 2021-06-11 | 中南大学 | 一种垂直生长的超薄Cr2Te3单晶纳米片的制备方法 |
Non-Patent Citations (2)
| Title |
|---|
| ZHENG, WR ET AL: "Few-layertellurium: cathodic exfoliation and doping for collaborative hydrogen evolution", 《SMALL》, vol. 17, no. 18, 18 March 2021 (2021-03-18), pages 1 - 10 * |
| 黄国波;: "绿色纳米合成技术在纳米材料研究中的应用", 《浙江化工》, no. 04, 15 April 2008 (2008-04-15), pages 8 - 12 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20200215509A1 (en) | Method of manufacturing a large-grain crystallized metal chalcogenide film, and a crystallized metal chalcogenide film prepared using the method | |
| Banerjee et al. | Recent developments in the emerging field of crystalline p-type transparent conducting oxide thin films | |
| Khan et al. | Progress in selenium based metal-organic precursors for main group and transition metal selenide thin films and nanomaterials | |
| US7586033B2 (en) | Metal-doped semiconductor nanoparticles and methods of synthesis thereof | |
| US7829059B2 (en) | Rapid synthesis of ternary, binary and multinary chalcogenide nanoparticles | |
| US20130037111A1 (en) | Process for Preparation of Elemental Chalcogen Solutions and Method of Employing Said Solutions in Preparation of Kesterite Films | |
| US9353433B2 (en) | Method of fabricating liquid for oxide thin film | |
| CN1384047A (zh) | 合成多种金属硒化物及碲化物半导体材料的方法 | |
| Lou et al. | Rod-shaped thiocyanate-induced abnormal band gap broadening in SCN− doped CsPbBr 3 perovskite nanocrystals | |
| US20080220593A1 (en) | Nanoparticles | |
| CA2424415A1 (en) | Synthesis of colloidal nanocrystals | |
| Chen et al. | The chemistry of colloidal semiconductor nanocrystals: From metal-chalcogenides to emerging perovskite | |
| JP2017511784A (ja) | ナトリウム又はアンチモンによるＣｕ（Ｉｎ，Ｇａ）（Ｓ，Ｓｅ）２ナノ粒子のドーピング方法 | |
| CN1191193C (zh) | 一种微米级硒化锌空心球的合成方法 | |
| CN115627163A (zh) | 一种高荧光量子产率紫光钙钛矿量子点的制备方法 | |
| Fazal et al. | Optoelectronic analysis of bismuth sulfide and copper-doped bismuth sulfide thin films | |
| CN113817467A (zh) | 一种球磨制备掺杂双钙钛矿荧光粉的方法 | |
| CN116462164A (zh) | 一种制备碲基超薄半导体纳米片的方法 | |
| Chawla et al. | Transition from CZTSe to CZTS via multicomponent CZTSSe: Potential low cost photovoltaic absorbers | |
| CN104692340A (zh) | 用于制备金属硒化物纳米材料的硒前躯体 | |
| Gull et al. | Deep red emission from Cs4PbI6/CsPbI3/ZnS heterostructure for enhanced stability and photoluminescence quantum yield | |
| WO2022211739A1 (en) | Ambient scalable synthesis of surfactant-free nanostructured chalcogenide particles for near room-temperature thermoelectric applications | |
| Zubair et al. | Precursor-Mediated Colloidal Synthesis of Compositionally Tunable Cu–Sb–M–S (M= Zn, Co, and Ni) Nanocrystals and Their Transport Properties | |
| JP7475839B2 (ja) | 亜鉛含有ナノ粒子の合成方法 | |
| CN110627125B (zh) | 一种合成硫化锰与硫化铅核壳结构纳米棒的方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |