CN1749170A - Method for preparing monodisperse rare-earth fluoride nano particles - Google Patents
Method for preparing monodisperse rare-earth fluoride nano particles Download PDFInfo
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- CN1749170A CN1749170A CN 200510109218 CN200510109218A CN1749170A CN 1749170 A CN1749170 A CN 1749170A CN 200510109218 CN200510109218 CN 200510109218 CN 200510109218 A CN200510109218 A CN 200510109218A CN 1749170 A CN1749170 A CN 1749170A
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- Prior art keywords
- fluoride
- rare earth
- rare
- polar solvent
- organic polar
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- -1 rare-earth fluoride Chemical class 0.000 title claims description 35
- 229910052761 rare earth metal Inorganic materials 0.000 title claims description 31
- 239000002105 nanoparticle Substances 0.000 title claims description 28
- 238000000034 method Methods 0.000 title claims description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 239000002798 polar solvent Substances 0.000 claims abstract description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 7
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 17
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 150000002632 lipids Chemical class 0.000 claims description 12
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 11
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 11
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 11
- 239000005642 Oleic acid Substances 0.000 claims description 11
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 11
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 11
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 11
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 claims description 8
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 7
- 235000013024 sodium fluoride Nutrition 0.000 claims description 7
- 239000011775 sodium fluoride Substances 0.000 claims description 7
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 5
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 5
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 4
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 claims description 4
- 229910052691 Erbium Inorganic materials 0.000 claims description 4
- 229910052693 Europium Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 230000001186 cumulative effect Effects 0.000 claims description 4
- 150000002910 rare earth metals Chemical class 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 229910052689 Holmium Inorganic materials 0.000 claims description 3
- 229910052772 Samarium Inorganic materials 0.000 claims description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 3
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 3
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 3
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 3
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- 229910052771 Terbium Inorganic materials 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 2
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 2
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 16
- 238000004458 analytical method Methods 0.000 abstract description 15
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 1
- 235000014113 dietary fatty acids Nutrition 0.000 abstract 1
- 229930195729 fatty acid Natural products 0.000 abstract 1
- 239000000194 fatty acid Substances 0.000 abstract 1
- 150000004665 fatty acids Chemical class 0.000 abstract 1
- 150000002736 metal compounds Chemical class 0.000 abstract 1
- 238000005303 weighing Methods 0.000 description 36
- 239000012046 mixed solvent Substances 0.000 description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 238000000634 powder X-ray diffraction Methods 0.000 description 18
- 239000000047 product Substances 0.000 description 13
- 230000005540 biological transmission Effects 0.000 description 12
- 238000005119 centrifugation Methods 0.000 description 12
- 238000001035 drying Methods 0.000 description 12
- 239000002244 precipitate Substances 0.000 description 12
- 229910001220 stainless steel Inorganic materials 0.000 description 12
- 239000010935 stainless steel Substances 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- 238000005406 washing Methods 0.000 description 12
- 239000000843 powder Substances 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 10
- 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 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- QCXKVMQEFRVUMD-UHFFFAOYSA-N [F].[Yb] Chemical compound [F].[Yb] QCXKVMQEFRVUMD-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- BOTHRHRVFIZTGG-UHFFFAOYSA-K praseodymium(3+);trifluoride Chemical compound F[Pr](F)F BOTHRHRVFIZTGG-UHFFFAOYSA-K 0.000 description 3
- 238000010189 synthetic method Methods 0.000 description 3
- FWQVINSGEXZQHB-UHFFFAOYSA-K trifluorodysprosium Chemical compound F[Dy](F)F FWQVINSGEXZQHB-UHFFFAOYSA-K 0.000 description 3
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 description 3
- RBORBHYCVONNJH-UHFFFAOYSA-K yttrium(iii) fluoride Chemical compound F[Y](F)F RBORBHYCVONNJH-UHFFFAOYSA-K 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- XVLAAJGISPCYOA-UHFFFAOYSA-N hydroxy-octadecoxy-octadecylsulfanyl-sulfanylidene-lambda5-phosphane Chemical compound CCCCCCCCCCCCCCCCCCOP(O)(=S)SCCCCCCCCCCCCCCCCCC XVLAAJGISPCYOA-UHFFFAOYSA-N 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229940105963 yttrium fluoride Drugs 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- QCCDYNYSHILRDG-UHFFFAOYSA-K cerium(3+);trifluoride Chemical compound [F-].[F-].[F-].[Ce+3] QCCDYNYSHILRDG-UHFFFAOYSA-K 0.000 description 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 229910003440 dysprosium oxide Inorganic materials 0.000 description 1
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(iii) oxide Chemical compound O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- ZXGIFJXRQHZCGJ-UHFFFAOYSA-N erbium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Er+3].[Er+3] ZXGIFJXRQHZCGJ-UHFFFAOYSA-N 0.000 description 1
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- RJOJUSXNYCILHH-UHFFFAOYSA-N gadolinium(3+) Chemical compound [Gd+3] RJOJUSXNYCILHH-UHFFFAOYSA-N 0.000 description 1
- OWCYYNSBGXMRQN-UHFFFAOYSA-N holmium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ho+3].[Ho+3] OWCYYNSBGXMRQN-UHFFFAOYSA-N 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- CZMAIROVPAYCMU-UHFFFAOYSA-N lanthanum(3+) Chemical compound [La+3] CZMAIROVPAYCMU-UHFFFAOYSA-N 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- RECVMTHOQWMYFX-UHFFFAOYSA-N oxygen(1+) dihydride Chemical compound [OH2+] RECVMTHOQWMYFX-UHFFFAOYSA-N 0.000 description 1
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 description 1
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 description 1
- 235000012736 patent blue V Nutrition 0.000 description 1
- WCWKKSOQLQEJTE-UHFFFAOYSA-N praseodymium(3+) Chemical compound [Pr+3] WCWKKSOQLQEJTE-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- FDIFPFNHNADKFC-UHFFFAOYSA-K trifluoroholmium Chemical class F[Ho](F)F FDIFPFNHNADKFC-UHFFFAOYSA-K 0.000 description 1
- XRADHEAKQRNYQQ-UHFFFAOYSA-K trifluoroneodymium Chemical class F[Nd](F)F XRADHEAKQRNYQQ-UHFFFAOYSA-K 0.000 description 1
- 229910003454 ytterbium oxide Inorganic materials 0.000 description 1
- 229940075624 ytterbium oxide Drugs 0.000 description 1
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- Luminescent Compositions (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention prepares monodisperse nanometer RE fluoride particles through reaction between RE metal compound and fluoride inside the mixture system comprising alkali metal hydroxide, fatty acid and organic polar solvent. The prepared nanometer RE fluoride particle may find wide application in biological, medicinal, catalyst, analysis and other fields. The present invention is simple, safe, low in cost and wide in adaptability, and has wide application foreground.
Description
Technical field
The present invention relates to nanometer particle process method, particularly relate to a kind of method for preparing monodisperse rare-earth fluoride nano particles.
Background technology
Rare-earth fluoride nano particles has widely in fields such as luminous, medical, analysis and biologies to be used.Developed at present the method for multiple synthesizing rare-earth fluoride nano particles.In " nanometer communication ", reported to be that protective material prepares LaF in 2002 as people such as Stouwdam J.W. with di-n-octadecyldithiophosphate
3Nanocrystalline synthetic method, synthetic use (the Nano Letters that has related to a large amount of organic solvent hexanaphthenes of protective material di-n-octadecyldithiophosphate, 2002,2:733-737), product is the mixture of sphere in irregular shape or rod-like nano crystalline substance; Li Yadongs etc. reported that the auxiliary ultrasonic synthetic method of hydro-thermal prepared YF in 2005 on " advanced function material " magazine
3The method of nanoparticle, but the synthetic nanoparticle have relatively poor dispersiveness and monodispersity (Adv.Func.Mater.2005,15:763); Yi GS etc. reported that the auxiliary direct precipitation of EDTA synthesized NaYF in 2004 in " nanometer communication "
4Nanocrystalline method, but the TEM show sample that is provided still has reunion to a certain degree, still has dispersion problem; People such as Zhang YW reported LaF in 2005 on " American Chemical Society's meeting will "
3Synthesizing of nanometer sheet, this method has adopted the organometallics raw material, and pyrolytic decomposition preparation in the octadecene system (J.Am.Chem.Soc.2005,127:3260-3261).
In sum, the synthetic method of the domestic and international rare-earth fluoride nano particles of reporting has generally used a large amount of organic solvents to be liquid-phase system at present, has dispersed, the uneven first-class problem of pattern.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing monodisperse rare-earth fluoride nano particles.
The method for preparing monodisperse rare-earth fluoride nano particles provided by the present invention, be that rare earth compound and fluorochemical are reacted in the mixed system of alkali metal hydroxide, lipid acid and organic polar solvent, obtain described monodisperse rare-earth fluoride nano particles.
Wherein, the step of above-mentioned reaction is: earlier alkali metal hydrogen oxygen compound, lipid acid are mixed with organic polar solvent, add rare earth ion solution and fluoride aqueous solution then, reaction obtains described monodisperse rare-earth fluoride nano particles under 20-300 ℃.
In reaction, the volume ratio of lipid acid and organic polar solvent is 1: 0.5-10; The concentration of used rare earth ion is 0.01-0.5mol/L, and the mol ratio of fluorion and rare earth ion is 3-10: 1; The cumulative volume of rare earth ion solution and fluoride aqueous solution is 1 with the cumulative volume ratio of lipid acid and organic polar solvent: 1-5; Alkali metal hydroxide: the mol ratio of rare earth ion is 1-10: 1.
Rare earth metal commonly used is lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, yttrium, holmium, erbium or ytterbium etc., can be with the soluble salt of these rare earth metals, and waiting as nitrate provides, and perhaps, waits with its oxide compound and nitric acid to be formulated as solution.Fluorochemical can be selected Sodium Fluoride, Neutral ammonium fluoride or ammonium bifluoride etc., and lipid acid is oleic acid, stearic acid or capric acid.The optional ethanol of organic polar solvent, acetone, ethylene glycol, glycerol, n-Octanol or the trimethyl carbinol etc.
It is raw material that the present invention adopts rare earth compound, alkali metal hydroxide, fluorochemical, in the mixed system of lipid acid, water, organic polar solvent, react, promptly can obtain the rare earth fluorine particle of dispersed nano level, prepared rare-earth fluoride nano particles is widely used in fields such as biological, medicine, catalysis and analyses.The present invention constitutes reaction system with water, lipid acid and organic polar solvent, overcome and adopted cost and the problem of environmental pollution that a large amount of organic solvent brought in the existing method, the inventive method is easy, safety, cost is low, suitability is wide, is with a wide range of applications.
Description of drawings
Fig. 1 is the prepared lanthanum trifluoride X-ray powder diffraction figure of embodiment 1;
Fig. 2 is that embodiment 1 prepared lanthanum trifluoride TEM Electronic Speculum detects figure;
Fig. 3 is three prepared praseodymium fluoride X-ray powder diffraction figure of embodiment 3;
Fig. 4 is that embodiment 3 three prepared praseodymium fluoride TEM Electronic Speculum detect figure;
Fig. 5 is three prepared dysprosium fluoride X-ray powder diffraction figure of embodiment 7;
Fig. 6 is that embodiment 7 three prepared dysprosium fluoride TEM Electronic Speculum detect figure;
Fig. 7 is three prepared yttrium fluoride X-ray powder diffraction figure of embodiment 8;
Fig. 8 is that embodiment 8 three prepared yttrium fluoride TEM Electronic Speculum detect figure;
Fig. 9 is the prepared tetrafluoro yttrium acid sodium X-ray powder diffraction figure of embodiment 9;
Figure 10 is that embodiment 9 prepared tetrafluoro yttrium acid sodium TEM Electronic Speculum detect figure;
Figure 11 is the prepared fluorine ytterbium acid sodium X-ray powder diffraction figure of embodiment 12;
Figure 12 is that embodiment 12 prepared fluorine ytterbium acid sodium TEM Electronic Speculum detect figure.
Embodiment
Embodiment 1,
Taking by weighing 0.5gNaOH adds in 10ml oleic acid, the 8ml ethanol mixed solvent, fully behind the about 30mins of reaction, taking by weighing 0.5g analytical pure lanthanum nitrate is dissolved in the 9mL water, take by weighing 0.5g analytical pure Sodium Fluoride and be dissolved in the 9mL water, and lanthanum ion, the fluorion solution that is made into is added in the mixed solvent simultaneously, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 140 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains white powder.Product is accredited as lanthanum trifluoride through X-ray powder diffraction as shown in Figure 1; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 2 its pattern is the dispersed nano particle, and particle diameter is between 6-7nm.
Embodiment 2,
Taking by weighing 0.5gKOH adding 20ml is dissolved with in the stearic ethylene glycol solvent of 5g, fully behind the about 30mins of reaction, taking by weighing 2g analytical pure cerous nitrate is dissolved in the 10mL water, take by weighing 3g analytical pure Neutral ammonium fluoride and be dissolved in the 10mL water, and cerium ion, the fluorion solution that is made into is added in the mixed solvent simultaneously, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 180 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains black powder.Product is accredited as cerous fluoride through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is between 8-10nm.
Embodiment 3,
Take by weighing 2gNaOH and add in 5ml oleic acid, the 20ml ethanol mixed solvent, fully behind the about 30mins of reaction, take by weighing 0.8g analytical pure Praseodymium trioxide in the dense HNO of 1mL analytical pure
3Thin up is to 7mL after the middle heating for dissolving, taking by weighing 1g analytical pure Neutral ammonium fluoride is dissolved in the 8mL water, add the praseodymium ion, the fluorion solution that are made in the mixed solvent simultaneously, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 120 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains white powder.Product is accredited as three praseodymium fluorides through X-ray powder diffraction as shown in Figure 3; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 4 its pattern is the dispersed nano particle, and particle diameter is between 15-20nm.
Embodiment 4,
Take by weighing 2gKOH and add in the mixed solvent of 10ml oleic acid, 20ml acetone, fully behind the about 30mins of reaction, take by weighing 0.5g analytical pure Neodymium trioxide in the dense HNO of 1mL analytical pure
3Thin up is to 5mL after the middle heating for dissolving, taking by weighing 0.5g analytical pure ammonium bifluoride is dissolved in the 5mL water, the neodymium ion, the fluorion solution that are made into are added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 180 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains the sky-blue powder.Product is accredited as three neodymium fluorides through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is between 20-30nm.
Embodiment 5,
Take by weighing 3gKOH and add in the mixed solvent of 5ml capric acid, 20ml n-Octanol, fully behind the about 30mins of reaction, take by weighing 0.6g analytical pure Samarium trioxide in the dense HNO of 1mL analytical pure
3Thin up is to 7mL water after the middle heating for dissolving, taking by weighing 1g analytical pure Sodium Fluoride is dissolved in the 8mL water, add the samarium ion, the fluorion solution that are made in the mixed solvent simultaneously, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 120 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains the yellow-white powder.Product is accredited as three samaric fluorides through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is between 20-30nm.
Embodiment 6,
Take by weighing 1gKOH and add in the mixed solvent of 6ml oleic acid, 20ml glycerol, fully behind the about 30mins of reaction, take by weighing 1g analytical pure europium sesquioxide in the dense HNO of 1mL analytical pure
3Thin up is to 7mL after the middle heating for dissolving, taking by weighing 0.5g analytical pure ammonium bifluoride is dissolved in the 7mL water, add the europium ion, the fluorion solution that are made in the mixed solvent simultaneously, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 180 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains white powder.Product is accredited as three europium through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is between 50-60nm.
Embodiment 7,
Take by weighing 1.5gKOH and add in the mixed solvent of 11ml oleic acid, 9ml ethylene glycol, fully behind the about 30mins of reaction, take by weighing 1.0g analytical pure dysprosium oxide in the dense HNO of 1mL analytical pure
3Thin up is to 8mL after the middle heating for dissolving, taking by weighing 2.5g analytical pure Sodium Fluoride is dissolved in the 8mL water, add the dysprosium ion, the fluorion solution that are made in the mixed solvent simultaneously, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 120 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains white powder.Product is accredited as three dysprosium fluorides through X-ray powder diffraction as shown in Figure 5; (TEM) carries out morphology analysis to it with transmission electron microscope, and its pattern is single shuttle type nano particle that disperses as can see from Figure 6, and particle diameter is between 200-300nm.
Embodiment 8,
Take by weighing 2gKOH and add in the mixed solvent of 10ml capric acid, the 10ml trimethyl carbinol, fully behind the about 30mins of reaction, take by weighing 1.5g analytical pure yttrium oxide in the dense HNO of 1mL analytical pure
3Thin up is to 10mL after the middle heating for dissolving, taking by weighing 2.5g analytical pure Neutral ammonium fluoride is dissolved in the 10mL water, add the gadolinium ion, the fluorion solution that are made in the mixed solvent simultaneously, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 120 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains white powder.Product is accredited as three yttrium fluorides through X-ray powder diffraction as shown in Figure 7; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 8 its pattern is single shuttle type nano particle that disperses, and particle diameter is between 300-400nm.
Embodiment 9,
Take by weighing 1gNaOH and add in 6ml oleic acid, the 18ml ethanol mixed solvent, fully behind the about 30mins of reaction, take by weighing 1.0g analytical pure yttrium oxide in the dense HNO of 1mL analytical pure
3Thin up is to 8mL water after the middle heating for dissolving, taking by weighing 2g analytical pure Sodium Fluoride is dissolved in the 8mL water, the ruthenium ion, the fluorion solution that are made into are added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 170 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains white powder.Product is accredited as tetrafluoro yttrium acid sodium through X-ray powder diffraction as shown in Figure 9; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 10 its pattern is single shuttle type nano particle that disperses, and particle diameter is between 300-500nm.
Take by weighing 1gNaOH and add in 10ml oleic acid, the 10ml ethanol mixed solvent, fully behind the about 30mins of reaction, take by weighing 1.0g analytical pure Holmium trioxide in the dense HNO of 1mL analytical pure
3Thin up is to 8mL water after the middle heating for dissolving, taking by weighing 2g analytical pure Neutral ammonium fluoride is dissolved in the 8mL water, the holmium ion, the fluorion solution that are made into are added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 170 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains white powder.Product is accredited as three holmium fluorides through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is between 2-3nm.
Embodiment 11,
Take by weighing 1gNaOH and add in 15ml oleic acid, the 5ml ethanol mixed solvent, fully behind the about 30mins of reaction, take by weighing 1.0g analytical pure Erbium trioxide in the dense HNO of 1mL analytical pure
3Thin up is to 10mL water after the middle heating for dissolving, taking by weighing 2g analytical pure Neutral ammonium fluoride is dissolved in the 10mL water, the erbium ion, the fluorion solution that are made into are added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 70 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains pink powder.Product is accredited as three through X-ray powder diffraction and fluoridizes erbium; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is between 2-3nm.
Embodiment 12,
Take by weighing 1gNaOH and add in 12ml oleic acid, the 8ml ethanol mixed solvent, fully behind the about 30mins of reaction, take by weighing 1.0g analytical pure ytterbium oxide in the dense HNO of 1mL analytical pure
3Thin up is to 10mL water after the middle heating for dissolving, taking by weighing 2g analytical pure Sodium Fluoride is dissolved in the 10mL water, the ytterbium ion, the fluorion solution that are made into are added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 250 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains white powder.Product is accredited as fluorine ytterbium acid sodium through X-ray powder diffraction as shown in figure 11; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 12 its pattern is the dispersed nano particle, and particle diameter is between 4-5nm.
Claims (7)
1, a kind of method for preparing monodisperse rare-earth fluoride nano particles, be that rare earth compound and fluorochemical are reacted in the mixed system of alkali metal hydroxide, lipid acid and organic polar solvent, obtain described monodisperse rare-earth fluoride nano particles.
2, method according to claim 1, it is characterized in that: the step of described reaction is: earlier alkali metal hydrogen oxygen compound, lipid acid are mixed with organic polar solvent, add rare earth ion solution and fluoride aqueous solution then, reaction obtains described monodisperse rare-earth fluoride nano particles under 20-300 ℃.
3, method according to claim 2 is characterized in that: the volume ratio of described lipid acid and described organic polar solvent is 1: 0.5-10; The concentration of described rare earth ion is 0.01-0.5mol/L, and the mol ratio of described fluorion and rare earth ion is 3-10: 1; The cumulative volume of rare earth ion solution and fluoride aqueous solution is 1 with the cumulative volume ratio of lipid acid and organic polar solvent: 1-5; Described alkali metal hydroxide: the mol ratio of described rare earth ion is 1-10: 1.
4, according to claim 1 or 2 or 3 or described method, it is characterized in that: described rare earth metal is lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, yttrium, holmium, erbium or ytterbium.
5, according to claim 1 or 2 or 3 described methods, it is characterized in that: described fluorochemical is Sodium Fluoride, Neutral ammonium fluoride or ammonium bifluoride.
6, according to claim 1 or 2 or 3 described methods, it is characterized in that: described lipid acid is oleic acid, stearic acid or capric acid.
7, according to claim 1 or 2 or 3 described methods, it is characterized in that: described organic polar solvent is ethanol, acetone, ethylene glycol, glycerol, n-Octanol or the trimethyl carbinol.
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CN101870863A (en) * | 2010-06-17 | 2010-10-27 | 复旦大学 | Preparation method of amphiphilic rare earth nanomaterial with adjustable surface functional group |
CN102205948A (en) * | 2011-05-26 | 2011-10-05 | 河南大学 | Fatty acid modified lanthanum series rare earth fluoride nanoparticle and preparation method thereof |
WO2021134785A1 (en) * | 2020-01-03 | 2021-07-08 | 大连民族大学 | Environment-friendly and large-scale fluoride nanomaterial preparation method |
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CN1017985B (en) * | 1989-07-07 | 1992-08-26 | 甘肃稀土公司 | Preparation method of rare earth fluoride |
CN1053635C (en) * | 1997-09-18 | 2000-06-21 | 吉林大学 | Water-heating preparation method for fluoride and composite fluoride material under mild condition |
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CN101870863A (en) * | 2010-06-17 | 2010-10-27 | 复旦大学 | Preparation method of amphiphilic rare earth nanomaterial with adjustable surface functional group |
CN101870863B (en) * | 2010-06-17 | 2014-05-21 | 复旦大学 | Preparation method of amphiphilic rare earth nanomaterial with adjustable surface functional group |
CN102205948A (en) * | 2011-05-26 | 2011-10-05 | 河南大学 | Fatty acid modified lanthanum series rare earth fluoride nanoparticle and preparation method thereof |
WO2021134785A1 (en) * | 2020-01-03 | 2021-07-08 | 大连民族大学 | Environment-friendly and large-scale fluoride nanomaterial preparation method |
US11866341B2 (en) | 2020-01-03 | 2024-01-09 | Dalian Minzu University | Environmentally friendly large-scale preparation method of fluoride nanomaterial |
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