CN114854416A - Near-infrared silver-gold-selenium fluorescent quantum dot and preparation method and application thereof - Google Patents
Near-infrared silver-gold-selenium fluorescent quantum dot and preparation method and application thereof Download PDFInfo
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- CN114854416A CN114854416A CN202110073230.0A CN202110073230A CN114854416A CN 114854416 A CN114854416 A CN 114854416A CN 202110073230 A CN202110073230 A CN 202110073230A CN 114854416 A CN114854416 A CN 114854416A
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 89
- IANXFCFDMBNAHB-UHFFFAOYSA-N gold selanylidenesilver Chemical compound [Au].[Ag]=[Se] IANXFCFDMBNAHB-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- KDSXXMBJKHQCAA-UHFFFAOYSA-N disilver;selenium(2-) Chemical compound [Se-2].[Ag+].[Ag+] KDSXXMBJKHQCAA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002243 precursor Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 23
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 22
- 229910052737 gold Inorganic materials 0.000 claims abstract description 20
- 239000010931 gold Substances 0.000 claims abstract description 20
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 18
- 239000011669 selenium Substances 0.000 claims abstract description 18
- 239000002798 polar solvent Substances 0.000 claims abstract description 15
- 238000004729 solvothermal method Methods 0.000 claims abstract description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052709 silver Inorganic materials 0.000 claims abstract description 12
- 239000004332 silver Substances 0.000 claims abstract description 12
- 238000005341 cation exchange Methods 0.000 claims abstract description 9
- 229940091258 selenium supplement Drugs 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 238000006862 quantum yield reaction Methods 0.000 claims description 7
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 claims description 6
- 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 6
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 claims description 3
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 claims description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 3
- PMYDPQQPEAYXKD-UHFFFAOYSA-N 3-hydroxy-n-naphthalen-2-ylnaphthalene-2-carboxamide Chemical compound C1=CC=CC2=CC(NC(=O)C3=CC4=CC=CC=C4C=C3O)=CC=C21 PMYDPQQPEAYXKD-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- 229910021612 Silver iodide Inorganic materials 0.000 claims description 3
- KZNMRPQBBZBTSW-UHFFFAOYSA-N [Au]=O Chemical compound [Au]=O KZNMRPQBBZBTSW-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- YWWZCHLUQSHMCL-UHFFFAOYSA-N diphenyl diselenide Chemical compound C=1C=CC=CC=1[Se][Se]C1=CC=CC=C1 YWWZCHLUQSHMCL-UHFFFAOYSA-N 0.000 claims description 3
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 3
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 3
- 229910001922 gold oxide Inorganic materials 0.000 claims description 3
- ZVUZTTDXWACDHD-UHFFFAOYSA-N gold(3+);trinitrate Chemical compound [Au+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O ZVUZTTDXWACDHD-UHFFFAOYSA-N 0.000 claims description 3
- 229910021505 gold(III) hydroxide Inorganic materials 0.000 claims description 3
- WDZVNNYQBQRJRX-UHFFFAOYSA-K gold(iii) hydroxide Chemical compound O[Au](O)O WDZVNNYQBQRJRX-UHFFFAOYSA-K 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- QJAOYSPHSNGHNC-UHFFFAOYSA-N octadecane-1-thiol Chemical compound CCCCCCCCCCCCCCCCCCS QJAOYSPHSNGHNC-UHFFFAOYSA-N 0.000 claims description 3
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 3
- KZCOBXFFBQJQHH-UHFFFAOYSA-N octane-1-thiol Chemical compound CCCCCCCCS KZCOBXFFBQJQHH-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 claims description 3
- 229910001958 silver carbonate Inorganic materials 0.000 claims description 3
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 claims description 3
- 229940045105 silver iodide Drugs 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- KZJPVUDYAMEDRM-UHFFFAOYSA-M silver;2,2,2-trifluoroacetate Chemical compound [Ag+].[O-]C(=O)C(F)(F)F KZJPVUDYAMEDRM-UHFFFAOYSA-M 0.000 claims description 3
- NSVHDIYWJVLAGH-UHFFFAOYSA-M silver;n,n-diethylcarbamodithioate Chemical compound [Ag+].CCN(CC)C([S-])=S NSVHDIYWJVLAGH-UHFFFAOYSA-M 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 229960001881 sodium selenate Drugs 0.000 claims description 3
- 235000018716 sodium selenate Nutrition 0.000 claims description 3
- 239000011655 sodium selenate Substances 0.000 claims description 3
- VPQBLCVGUWPDHV-UHFFFAOYSA-N sodium selenide Chemical compound [Na+].[Na+].[Se-2] VPQBLCVGUWPDHV-UHFFFAOYSA-N 0.000 claims description 3
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052946 acanthite Inorganic materials 0.000 claims description 2
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 claims description 2
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229910000367 silver sulfate Inorganic materials 0.000 claims description 2
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 claims description 2
- 229940056910 silver sulfide Drugs 0.000 claims description 2
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 claims description 2
- 229960001471 sodium selenite Drugs 0.000 claims description 2
- 235000015921 sodium selenite Nutrition 0.000 claims description 2
- 239000011781 sodium selenite Substances 0.000 claims description 2
- 238000003384 imaging method Methods 0.000 claims 1
- KRRRBSZQCHDZMP-UHFFFAOYSA-N selanylidenesilver Chemical class [Ag]=[Se] KRRRBSZQCHDZMP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000047 product Substances 0.000 description 7
- 238000001132 ultrasonic dispersion Methods 0.000 description 7
- 238000012984 biological imaging Methods 0.000 description 6
- 229910001385 heavy metal Inorganic materials 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 231100000331 toxic Toxicity 0.000 description 6
- 230000002588 toxic effect Effects 0.000 description 6
- 239000012467 final product Substances 0.000 description 5
- 238000000799 fluorescence microscopy Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002073 fluorescence micrograph Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000011503 in vivo imaging Methods 0.000 description 1
- 229910052981 lead sulfide Inorganic materials 0.000 description 1
- 229940056932 lead sulfide Drugs 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000001748 luminescence spectrum Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- VCEXCCILEWFFBG-UHFFFAOYSA-N mercury telluride Chemical compound [Hg]=[Te] VCEXCCILEWFFBG-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- GGYFMLJDMAMTAB-UHFFFAOYSA-N selanylidenelead Chemical compound [Pb]=[Se] GGYFMLJDMAMTAB-UHFFFAOYSA-N 0.000 description 1
- 229940065287 selenium compound Drugs 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- H01L33/50—Wavelength conversion elements
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Abstract
The invention discloses a near-infrared silver-gold-selenium fluorescent quantum dot and a preparation method and application thereof. The preparation method comprises the following steps: carrying out solvothermal reaction on a first uniform mixed reaction system containing a silver source, a selenium source and a weak polar solvent to prepare a silver selenide quantum dot precursor; and (3) carrying out cation exchange reaction for 10-72 h at 0-200 ℃ on a second uniformly mixed reaction system containing the silver selenide quantum dot precursor and the gold source to obtain the near-infrared silver-gold-selenium fluorescent quantum dot, wherein the wavelength of a fluorescence emission peak of the fluorescent quantum dot is 800-1350 nm. The silver selenide quantum dots are prepared by a simple high-temperature solvothermal method, and then the silver gold selenium quantum dots are obtained by a cation exchange method.
Description
Technical Field
The invention relates to a near-infrared fluorescent quantum dot and a preparation method thereof, in particular to a near-infrared silver gold selenium fluorescent quantum dot with high quantum efficiency and a preparation method and application thereof, belonging to the field of material science.
Background
The fluorescence imaging technology has the advantages of non-contact, visual and real-time images, high sensitivity, economy, convenience, no radiation hazard and the like, and has wide application prospect in biomedical research and clinical practice, particularly in the aspect of fluorescence image operation navigation. According to the wavelength range of fluorescence imaging, the fluorescence imaging method mainly comprises visible light fluorescence imaging (400-. In biological imaging, near infrared light can be divided into two optical windows: near infrared I region (650-900nm, NIR-I) and near infrared (900-1700nm, NIR-II). NIR-fluorescence is a new fluorescence window discovered in vivo fluorescence imaging studies in the last decade, and the attenuation coefficient of NIR-II photons in living tissue is significantly reduced compared to the visible region and NIR-I region (j.am.chem.soc.2020, 142, 14789-.
The quantum dot as an excellent NIR-II fluorescent probe has the following characteristics in vivo imaging research: high biocompatibility, high quantum efficiency, tunable excitation and emission wavelengths, easy surface functionalization, and the like. However, the existing infrared fluorescent quantum dots, such as lead sulfide, cadmium telluride, lead selenide, mercury telluride, silver selenide and the like, have low absolute fluorescent quantum yield, and meanwhile, part of the existing infrared fluorescent quantum dots contain toxic heavy metal elements, so that the fluorescent intensity and the toxicity are difficult to be both complete. Therefore, the development of a novel fluorescent quantum dot probe with continuously adjustable single emission in the NIR-II full window (900-.
Disclosure of Invention
The invention mainly aims to provide a near-infrared silver-gold-selenium fluorescent quantum dot with high quantum efficiency and a preparation method thereof, so that the defects in the prior art are overcome.
The invention also aims to provide application of the near-infrared silver-gold-selenium fluorescent quantum dot.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a preparation method of near-infrared silver-gold-selenium fluorescent quantum dots, which comprises the following steps:
carrying out solvothermal reaction on a first uniform mixed reaction system containing a silver source, a selenium source and a weak polar solvent to prepare a silver selenide quantum dot precursor;
and (3) carrying out cation exchange reaction on a second uniformly mixed reaction system containing the silver selenide quantum dot precursor and the gold source at the temperature of 0-200 ℃ for 10-72 h to obtain the near-infrared silver-gold-selenium fluorescent quantum dot.
In some embodiments, the method of making comprises: and carrying out solvothermal reaction on the first uniformly mixed reaction system at 100-300 ℃ for 0.5-24 h to prepare the silver selenide quantum dot precursor.
The embodiment of the invention also provides the near-infrared silver-gold-selenium fluorescent quantum dot prepared by the method.
Furthermore, the diameter of the near-infrared silver gold selenium fluorescent quantum dot is 2-20 nm, and the size distribution is uniform.
Furthermore, the wavelength of a fluorescence emission peak of the near-infrared silver-gold-selenium fluorescence quantum dot is 800-1350 nm.
Further, the absolute fluorescence quantum yield of the near-infrared silver gold selenium fluorescence quantum dots is larger than 90%.
The embodiment of the invention also provides application of any near-infrared silver gold selenium fluorescent quantum dot in the fields of biological imaging, biomedicine or near-infrared devices (such as near-infrared light-emitting diodes) and the like.
Compared with the prior art, the invention has the beneficial effects that:
1) the silver selenide quantum dots are prepared by a simple high-temperature solvothermal method, and then the silver gold selenium quantum dots are obtained by a cation exchange method, so that the synthetic process is simple in step, controllable in experimental conditions, simple and easily available in used reagents, high in final product yield and suitable for large-scale production;
2) the prepared final product near-infrared silver-gold-selenium fluorescent quantum dots are uniform in size distribution, the fluorescence emission is in near infrared, the wavelength of an emission peak is 800-1350 nm, the final product has ultrahigh absolute quantum efficiency (more than 90%) and excellent light stability, does not contain any toxic heavy metal element, and has wide application prospects in the fields of biological imaging, near-infrared devices and the like;
3) the preparation process can be expanded to other preparation processes of near-infrared silver-gold-selenium fluorescent quantum dots, and is high in yield and easy to amplify reaction scale.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings needed to be used in the description of the embodiment or the prior art will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIGS. 1 a-1 b are the transmission electron microscope photograph and the high resolution transmission electron microscope photograph of the near infrared silver gold selenium fluorescent quantum dot in example 1 of the present invention, respectively;
FIG. 2 is a powder X-ray diffraction pattern of the near-infrared silver-gold-selenium fluorescent quantum dots in example 1 of the present invention;
FIG. 3 is an energy dispersive X-ray spectrum of a near-infrared silver-gold-selenium fluorescent quantum dot in example 1 of the present invention;
fig. 4 a-4 b are fluorescence emission spectra and quantum efficiency measurement spectra of the near-infrared silver gold selenium fluorescence quantum dots in example 1 of the present invention.
Detailed Description
As described above, in view of the deficiencies of the prior art, the inventors of the present invention found, after long-term research and extensive practice: the silver-gold-selenium quantum dot which is an alloying product of the gold element and the silver-selenium quantum dot has good near-infrared optical property, the absolute quantum efficiency of the silver-gold-selenium quantum dot is up to more than 90%, and meanwhile, the silver-gold-selenium quantum dot does not contain any toxic heavy metal elements. The technical solution of the present invention will be explained in more detail as follows.
As one aspect of the technical scheme of the invention, the related preparation method of the near-infrared silver-gold-selenium fluorescent quantum dot comprises the following steps:
carrying out solvothermal reaction on a first uniform mixed reaction system containing a silver source, a selenium source and a weak polar solvent to prepare a silver selenide quantum dot precursor;
and (3) carrying out cation exchange reaction on a second uniformly mixed reaction system containing the silver selenide quantum dot precursor and the gold source at the temperature of 0-200 ℃ for 10-72 h to obtain the near-infrared silver-gold-selenium fluorescent quantum dot.
In some embodiments, the method of making consists essentially of: uniformly mixing a silver source and a selenium source in a weak polar solvent, and carrying out solvothermal reaction to prepare a silver selenide quantum dot; and mixing the silver selenide quantum dots with a gold source, and carrying out a room-temperature cation exchange reaction to obtain the near-infrared silver gold selenium quantum dots with high quantum efficiency, wherein the wavelength of a fluorescence emission peak of the near-infrared silver gold selenium quantum dots is 800-1350 nm.
In some preferred embodiments, the method for preparing the high quantum efficiency near infrared silver gold selenium fluorescent quantum dot may specifically include:
uniformly mixing a silver source with a low-polarity solvent, and adding a selenium source to perform solvothermal reaction to prepare a silver selenide quantum dot precursor;
and mixing and reacting the silver selenide precursor and a gold source at 0-200 ℃ to obtain the silver-gold-selenium fluorescent quantum dot, wherein the wavelength of a fluorescence emission peak is 800-1350 nm, and the absolute fluorescence quantum yield is more than 90%.
In some embodiments, the method of making comprises: firstly, uniformly mixing a silver source and a weak polar solvent, and then adding a selenium source to form the first uniformly mixed reaction system.
In some embodiments, the method of making specifically comprises: and carrying out solvothermal reaction on the first uniformly mixed reaction system at 100-300 ℃ for 0.5-24 h to prepare the silver selenide quantum dot precursor.
In some embodiments, the mass ratio of the silver source to the selenium source is 1-10: 1-10. That is, the production method comprises: dissolving a silver source and a selenium source in a weak polar solvent according to the mass ratio of 1-10: 1-10.
The preparation process of the silver selenide precursor provided by the invention is a solvothermal reaction, the steps are simple, the experimental conditions are controllable, the used reagents are simple and easy to obtain, the yield of the final product is high, and the preparation method is suitable for large-scale production.
In some embodiments, the method of making comprises: and uniformly mixing the silver selenide quantum dot precursor, the gold source and the weak-polarity solvent to form the second uniformly-mixed reaction system.
In some embodiments, the mass ratio of the silver selenide quantum dot precursor to the gold source is 1-10: 1-10. That is, the production method comprises: dissolving a silver selenide quantum dot precursor and a gold source in a weak polar solvent according to a mass ratio of 1-10: 1-10.
In some embodiments, the silver salt includes any one or a combination of two or more of silver chloride, silver bromide, silver iodide, silver sulfate, silver nitrate, silver carbonate, silver sulfide, silver trifluoroacetate, silver diethyldithiocarbamate, and the like, but is not limited thereto.
In some embodiments, the selenium source includes any one or a combination of two or more of selenium dioxide, selenium powder, sodium selenate, sodium selenite, sodium selenide, diphenyl diselenide, and the like, but is not limited thereto.
In some embodiments, the weakly polar solvent includes any one or a combination of two or more of oleylamine, oleic acid, octadecene, octadecylamine, dodecylamine, tetradecylamine, dodecylmercaptan, octylmercaptan, octadecylmercaptan, etc., but is not limited thereto.
In some embodiments, the gold source includes any one or a combination of two or more of sodium chloroaurate, chloroauric acid, gold nitrate, gold chloride, gold hydroxide, gold oxide, gold nanorods, gold particles, and the like, but is not limited thereto.
The aforementioned silver salt, selenium source, weakly polar solvent, gold source, and the like may be selected from, but not limited to, the above listed species.
Further, in an exemplary embodiment, the preparation method may include: firstly, dissolving silver nitrate in oleylamine, adding a selenium source, reacting for 1-6 h at 100-300 ℃, and then cleaning to obtain a target product, namely a silver selenide quantum dot precursor.
Further, the mass ratio of the silver salt to the selenium source is 0.1-1 g: 0.1-1 g.
In some preferred embodiments, the preparation method may comprise: dissolving silver salt with the mass of 0.1-1 g in a weak polar solvent.
Further, the preparation method specifically comprises the following steps: and mixing the silver selenide precursor with a gold source, and reacting at 100-200 ℃ to obtain the near-infrared silver-gold-selenium fluorescent quantum dot.
Further, the preparation method further comprises the following steps: and after the reaction is finished, cleaning the obtained silver-gold-selenium fluorescent quantum dots.
Wherein, as a more specific embodiment, the preparation method may comprise the steps of:
I. mixing silver salt and a weak polar solvent, and then performing ultrasonic uniform dispersion;
II. Adding a selenium source into the mixed solution finally obtained in the step I, uniformly mixing and dispersing, and reacting at 100-300 ℃ for 0.5-24 h:
III, separating a product obtained by the solvothermal reaction in the step II, cleaning and drying;
and IV, reacting the product obtained in the step III with a gold source at the temperature of 0-200 ℃ for 10-72 hours to obtain the near-infrared silver-gold-selenium fluorescent quantum dot.
The near-infrared silver-gold-selenium fluorescent quantum dots prepared by the method have uniform size distribution, the wavelength of a fluorescence emission peak of the near-infrared silver-gold-selenium fluorescent quantum dots is 800-1350 nm, preferably 800-1200 nm, the near-infrared silver-gold-selenium fluorescent quantum dots have ultrahigh absolute fluorescent quantum efficiency (more than 90 percent), and the near-infrared silver-gold-selenium fluorescent quantum dots do not contain any toxic heavy metal elements. And the yield of the final product is high, and the preparation process is easy to enlarge the reaction scale.
Furthermore, the preparation process can be expanded to other preparation processes of near-infrared silver-gold-selenium fluorescent quantum dots, and is high in yield and easy to amplify reaction scale.
As another aspect of the technical scheme, the invention also relates to the near-infrared silver gold selenium fluorescent quantum dot prepared by the method.
Further, the diameter of the near-infrared silver gold selenium fluorescent quantum dot is 2-20 nm.
Furthermore, the wavelength of a fluorescence emission peak of the near-infrared silver-gold-selenium fluorescence quantum dot is 800-1350 nm, preferably 800-1200 nm, the absolute fluorescence quantum yield is greater than 90%, and the near-infrared silver-gold-selenium fluorescence quantum dot does not contain any toxic heavy metal elements.
As another aspect of the technical scheme, the invention also provides the near-infrared silver-gold-selenium fluorescent quantum dot which is uniform in shape and size, high in absolute quantum yield, free of any toxic heavy metal element and has important application prospects in the fields of biological imaging, biomedicine or near-infrared devices and the like.
The embodiment of the invention also provides application of any near-infrared silver, gold and selenium fluorescent quantum dot in the fields of biological imaging, biomedicine or near-infrared devices and the like.
Further, the near infrared device may be a near infrared light emitting diode, but is not limited thereto.
In summary, according to the technical scheme, the silver selenide quantum dots are prepared by a simple high-temperature solvothermal method, and then the silver gold selenium quantum dots are obtained by a cation exchange method, so that the synthesis process is simple and controllable, the yield is high, the silver gold selenium quantum dots can be prepared in a large scale, the obtained product is uniform in size, the fluorescence emission is near infrared, the high quantum efficiency and the excellent light stability are achieved, and the silver gold selenium quantum dots have wide application prospects in the fields of biological imaging, near infrared devices and the like.
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention are further described in detail with reference to some preferred embodiments, but the present invention is not limited to the following embodiments, and those skilled in the art can make insubstantial improvements and modifications within the spirit of the present invention and still fall within the scope of the present invention. Unless otherwise specified, various reagents used in the following examples are well known to those skilled in the art and available from commercial sources and the like. However, the experimental methods in the following examples, in which specific conditions are not specified, are generally performed under conventional conditions or under conditions recommended by the manufacturers.
Example 1
Dissolving 0.06g of silver nitrate in 20mL of oleylamine, performing ultrasonic dispersion uniformly, then adding 0.06g of selenium powder, reacting for 5h at 200 ℃ to obtain a silver selenide quantum dot precursor (0.6g), then adding 0.06g of chloroauric acid, and reacting for 48h at 100 ℃ to obtain the near-infrared silver-gold-selenium fluorescent quantum dot.
As can be seen from fig. 1 a-1 b, the near-infrared silver-gold-selenium fluorescent quantum dot product obtained in this example has uniform morphology and size, and the size is about 4.8nm, where fig. 1a is a transmission electron microscope photograph of the near-infrared silver-gold-selenium fluorescent quantum dot, and fig. 1b is a high-resolution transmission electron microscope photograph. Referring to fig. 2 and 3, it can be seen from the powder X-ray diffraction and energy dispersive X-ray spectra that the nanoparticle material is silver-gold-selenium compound.
And dispersing the silver-gold-selenium quantum dots in chloroform. The luminescence spectrum and absolute fluorescence quantum yield were tested using a near infrared fluorescence spectrometer. As can be seen from FIG. 4a and FIG. 4b, the silver-gold-selenium fluorescent quantum dots emit light at 800-1200 nm, and the absolute quantum efficiency is 90.3%.
Example 2
Dissolving 0.06g of silver carbonate in 20mL of octyl mercaptan, performing ultrasonic dispersion uniformly, then adding 0.8g of selenium dioxide, reacting for 2h at 250 ℃ to obtain a silver selenide quantum dot precursor (0.05g), and then adding 0.5g of gold nitrate, reacting for 10h at 200 ℃ to obtain the near-infrared silver-gold-selenium fluorescent quantum dot.
Example 3
Dissolving 0.6g of silver bromide in 20mL of oleic acid, performing ultrasonic dispersion uniformly, then adding 0.6g of sodium selenate, reacting for 1h at 200 ℃ to obtain a silver selenide quantum dot precursor (0.1g), then adding 0.1g of sodium chloroaurate, and reacting for 48h at 100 ℃ to obtain the near-infrared silver gold selenium fluorescent quantum dot.
Example 4
Dissolving 0.06g of silver chloride in 20mL of dodecanethiol, performing ultrasonic dispersion uniformly, then adding 0.06g of sodium selenide, reacting for 5 hours at 100 ℃ to obtain a silver selenide quantum dot precursor (0.06g), then adding 0.06g of gold chloride, and reacting for 72 hours at 0 ℃ to obtain the near-infrared silver-gold-selenium fluorescent quantum dot.
Example 5
Adding 0.06g of silver iodide into 20g of octadecylamine, performing ultrasonic dispersion uniformly, then adding 0.06g of diphenyl diselenide, reacting for 24h at 200 ℃ to obtain a silver selenide quantum dot precursor (0.03g), then adding 0.05g of gold hydroxide, and reacting for 72h at 0 ℃ to obtain the near-infrared silver-gold-selenium fluorescent quantum dot.
Example 6
Dissolving 0.06g of silver diethyldithiocarbamate in 20mL of octadecanethiol, performing ultrasonic dispersion uniformly, then adding 0.06 selenium powder, reacting at 300 ℃ for 0.5h to obtain a silver selenide quantum dot precursor (0.06g), then adding 0.06g of gold oxide, and reacting at 0 ℃ for 72h to obtain the near-infrared silver-gold-selenium fluorescent quantum dot.
Example 7
Dissolving 0.06g of silver trifluoroacetate in 20mL of octadecene, performing ultrasonic dispersion uniformly, then adding 0.06 selenium powder, reacting for 24h at 200 ℃ to obtain a silver selenide quantum dot precursor (0.06g), then adding 0.06g of gold nanorod, and reacting for 72h at 0 ℃ to obtain the near-infrared silver-gold-selenium fluorescent quantum dot.
In addition, the inventor also carries out corresponding experiments by using other raw materials and other process conditions listed above to replace various raw materials and corresponding process conditions in the embodiment l-7, so that the obtained near-infrared silver-gold-selenium fluorescent quantum dot has ideal morphology, performance and the like, and is basically similar to the product of the embodiment l-7.
The silver selenide quantum dots are prepared by a simple high-temperature solvothermal method, and then the silver gold selenium quantum dots are obtained by a cation exchange method.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
The use of headings and chapters in this disclosure is not meant to limit the disclosure; each section may apply to any aspect, embodiment, or feature of the disclosure.
Throughout this specification, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the composition of the present teachings also consist essentially of, or consist of, the recited components, and the process of the present teachings also consist essentially of, or consist of, the recited process steps.
Unless specifically stated otherwise, use of the terms "comprising", "including", "having" or "having" is generally to be understood as open-ended and not limiting.
It should be understood that the order of steps or the order in which particular actions are performed is not critical, so long as the teachings of the invention remain operable. Further, two or more steps or actions may be performed simultaneously.
While the invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims. Moreover, unless specifically stated any use of the terms first, second, etc. do not denote any order or importance, but rather the terms first, second, etc. are used to distinguish one element from another.
Claims (10)
1. A preparation method of near-infrared silver gold selenium fluorescent quantum dots is characterized by comprising the following steps:
carrying out solvothermal reaction on a first uniform mixed reaction system containing a silver source, a selenium source and a weak polar solvent to prepare a silver selenide quantum dot precursor;
and (3) carrying out cation exchange reaction on a second uniformly mixed reaction system containing the silver selenide quantum dot precursor and the gold source at the temperature of 0-200 ℃ for 10-72 h to obtain the near-infrared silver-gold-selenium fluorescent quantum dot.
2. The method of claim i, comprising: firstly, uniformly mixing a silver source and a weak polar solvent, and then adding a selenium source to form the first uniformly mixed reaction system.
3. The production method according to claim 1 or 2, characterized in that: the mass ratio of the silver source to the selenium source is 1-10: 1 to 10.
4. The production method according to claim 1 or 2, characterized by comprising: and carrying out solvothermal reaction on the first uniformly mixed reaction system at 100-300 ℃ for 0.5-24 h, preferably 1-6 h, so as to prepare the silver selenide quantum dot precursor.
5. The production method according to claim 1, characterized by comprising: uniformly mixing a silver selenide quantum dot precursor, a gold source and a weak polar solvent to form a second uniformly mixed reaction system;
and/or the mass ratio of the silver selenide quantum dot precursor to the gold source is 1-10: 1-10.
6. The method of claim 1, wherein: the silver salt comprises any one or the combination of more than two of silver chloride, silver bromide, silver iodide, silver sulfate, silver nitrate, silver carbonate, silver sulfide, silver trifluoroacetate and silver diethyldithiocarbamate.
7. The method of claim 1, wherein: the selenium source comprises one or more of selenium dioxide, selenium powder, sodium selenate, sodium selenite, sodium selenide and diphenyl diselenide;
and/or the weak polar solvent comprises any one or the combination of more than two of oleylamine, oleic acid, octadecene, octadecylamine, dodecylamine, tetradecylamine, dodecanethiol, octanethiol and octadecanethiol.
8. The method of claim 1, wherein: the gold source comprises one or the combination of more than two of sodium chloroaurate, chloroauric acid, gold nitrate, gold chloride, gold hydroxide, gold oxide, gold nanorods and gold particles.
9. The near-infrared silver-gold-selenium fluorescent quantum dot prepared by the method of any one of claims l-8, which has the diameter of 2-20 nm, is uniform in size distribution, has a fluorescence emission peak wavelength of 800-1350 nm, preferably 800-1200 nm, and has an absolute fluorescence quantum yield of more than 90%.
10. Use of the near-infrared silver gold selenium fluorescent quantum dots according to claim 9 in the fields of bio-imaging, biomedicine or near-infrared devices, preferably the near-infrared devices comprise near-infrared light emitting diodes.
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| US17/785,420 US20230247846A1 (en) | 2021-01-20 | 2021-12-21 | Fluorescent quantum dots as well as preparation method and use thereof |
| EP21920841.0A EP4092095B1 (en) | 2021-01-20 | 2021-12-21 | Fluorescent quantum dots and preparation method therefor and use thereof |
| PCT/CN2021/140056 WO2022156467A1 (en) | 2021-01-20 | 2021-12-21 | Fluorescent quantum dots and preparation method therefor and use thereof |
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| CN104513664A (en) * | 2013-09-27 | 2015-04-15 | 深圳先进技术研究院 | Near-infrared silver-indium-selenium quantum dot and preparation method thereof |
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