CN117229778A - Preparation method and application of rare earth oxygen carbonate - Google Patents
Preparation method and application of rare earth oxygen carbonate Download PDFInfo
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- CN117229778A CN117229778A CN202311117247.7A CN202311117247A CN117229778A CN 117229778 A CN117229778 A CN 117229778A CN 202311117247 A CN202311117247 A CN 202311117247A CN 117229778 A CN117229778 A CN 117229778A
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 49
- -1 rare earth oxygen carbonate Chemical class 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000006184 cosolvent Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 150000002910 rare earth metals Chemical class 0.000 claims description 16
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 8
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 5
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004323 potassium nitrate Substances 0.000 claims description 4
- 235000010333 potassium nitrate Nutrition 0.000 claims description 4
- 239000004317 sodium nitrate Substances 0.000 claims description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims description 4
- 230000004907 flux Effects 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 9
- 238000003786 synthesis reaction Methods 0.000 abstract description 9
- 239000011159 matrix material Substances 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000003889 chemical engineering Methods 0.000 abstract description 2
- 238000005253 cladding Methods 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 238000009423 ventilation Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 239000008213 purified water Substances 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 230000005284 excitation Effects 0.000 description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 4
- 239000004202 carbamide Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000000295 emission spectrum Methods 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000012190 activator Substances 0.000 description 3
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
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- 238000004321 preservation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003568 thioethers Chemical class 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
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- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000012612 commercial material Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
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- 239000010419 fine particle Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
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- 238000005424 photoluminescence Methods 0.000 description 1
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- 241000894007 species Species 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention belongs to the field of fine chemical engineering, and particularly relates to a preparation method and application of rare earth oxygen carbonate. The method comprises the following steps: 1) Taking rare earth carbonate as a precursor, and uniformly mixing the precursor with a cosolvent; 2) Calcining the mixture in air to obtain the rare earth oxygen carbonate. The rare earth oxygen carbonate prepared by the invention can be used for preparing luminescent materials taking the rare earth oxygen carbonate as a matrix. The preparation method has the advantages of simple synthesis process, low cost, no need of ventilation and cladding processes, short reaction time and low reaction temperature, can greatly reduce the energy consumption, and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the field of fine chemical engineering, and particularly relates to a preparation method and application of rare earth oxygen carbonate.
Background
The rare earth luminescent material has the advantages of narrow luminescent band, high color purity, bright color, high light conversion efficiency, strong absorption capacity and wavelength divisionThe cloth width and other advantages, and has been widely used in lighting, display, anti-fake, security inspection, optical fiber communication, medical care and other fields. For practical application of rare earth luminescent materials, the selection of matrix materials is particularly critical, which determines the luminescent properties of rare earth ions to a great extent, and the exploration of excellent matrix materials is always an important subject in the field of luminescence. Halides and sulfides are reported to generally have higher luminous efficiency due to lower phonon energy. However, halides and sulfides are inferior in chemical stability and mechanical processability and are severely contaminated in the production process. In contrast, oxides are mostly non-toxic and chemically very stable, being ideal choices for luminescent host materials. In rare earth oxides, hexagonal phase rare earth oxycarbonates (RE 2 O 2 CO 3 ) The material has excellent heat resistance, good chemical stability to water and carbon dioxide, and excellent luminescent matrix material. Various methods for preparing rare earth hexagonal phase rare earth oxygen carbonate exist at present, such as: carbonate thermal decomposition method [ 1 ] A.N.Shirsat, K.N.G.Kaimal, S.R.Bharadwaj, D.Das, thermochemical studies on RE 2 O 2 CO 3 (re=gd, nd) composition, journal of Physics and Chemistry of Solids (2005) 1122-1127; (2) Rheal P.Turcotte, james O.Sawyer, leroy effect, on the rare earth dioxymonocarbonates and their decomposition, inorganic Chemistry,8 (2) (1969) 238-246), carbonation of rare earth oxides or hydroxides [ 3 ] Anja Olafsen, helmer Fjellvag, synthesis of rare earth oxide carbonates and thermal stability of Nd 2 O 2 CO 3 II, journal of Materials Chemistry,9 (1999) 2697-2702 ], hydrothermal Process [ 4 ] Christensen A. Norlund, hydrothermal preparation and magnetic properties Dy 2 O 2 CO 3 ,Ho 2 O 2 CO 3 ,Er 2 O 2 CO 3 ,and Yb 2 O 2 CO 3 27 (1973) 1835-1837 ], precursor method [ 5 ] Zhilong Wang, yuhua Wang, jiachi Zhang, vacuum ultraviolet excited photoluminescence properties of Gd 2 O 2 CO 3 :Eu 3+ phosphor,Journal of Rare Earths,26 (3) (2008) 425-427), etc.
However, these methods require an excessively long preparation time (3 to 5 days or several weeks) or an excessively high pressure (1400 to 3400 atm), and are liable to generate tetragonal phase and monoclinic phase RE 2 O 2 CO 3 Impurities, which are poor in both thermal and chemical stability, are not suitable for use as light-emitting host materials.
Thus, in order to shorten the experimental period and simplify the experimental conditions, researchers have begun to explore new experimental methods to prepare a single hexagonal phase RE 2 O 2 CO 3 And have achieved some results such as fusion [ 6 ] Nobuhito Imanaka, toshiyuki Masui, yuhei Mayama, kazuhiko Koyabu, synthesis of crystalline yttrium oxycarbonate in single phase, journal of Solid State Chemistry,178 (2005) 3601-3603; (7) Toshiyuki Masui, yuhei Mayama, kazuhiko Koyabu, nobuhito Imanaka, synthesis of new green-emiting Gd 2 O 2 CO 3 :Tb 3+ fine particles with high luminescence intensities,Chemistry Letters,34(2005)1236-1237；(8)T.Masui,K.Koyabu,S.Tamura,N.Imanaka,Synthesis of a new green-emitting phosphor based on lanthanum oxycarbonate(La 2 O 2 CO 3 -Ⅱ),Journal of Materials Science,40(2005)4121-4123；(9)Kazuhiko Koyabu,Toshiyuki Masui,Shinji Tamura,Nobuhito Imanaka,Synthesis of a new phosphor based on rare earth oxycarbonate,Journal of Alloys and Compounds,408-412(2006)867-870；(10)Cristina Artini,Federico Locardi,Marcella Pani,Ilaria Nelli,Federico Caglieris,Roberto Masini,Jasper Rikkert Plaisier,Giorgio Andrea Costa,Yb-doped Gd 2 O 2 CO 3 Structure, microstructure, thermal and magnetic behaviour, journal of Physics and Chemistry of Solids,103 (2017) 59-66; (11) Mizuki Watanabe, yasuhiro Sejima, ryohei Oka, shantaro Ida, toshiyuki Masui, submicron-sized phosphors based on hexagonal rare earth oxycarbonate for near-infrared excitation and emission, journal of Asian Ceramic Societies,7 (2019) 502-508 ], in combination with SiO 2 Coated homogeneous precipitation [ 12 ] Wen Ge, zhiang Li, zhiwei Lei,Tong Chen,Zhengping Fu,Ranran Peng,Min Liu,Yalin Lu,Synthesis of hexagonal phase Gd 2 O 2 CO 3 :Yb 3+ ,Er 3+ upconversion nanoparticles via SiO 2 coating and Nd 3+ dopping, crystEngComm,17 (2015) 5702-5709 ]. However, these methods also suffer from significant disadvantages, such as the need for relatively high calcination temperatures (450-600 ℃) and the need for CO introduction during the synthesis process 2 /N 2 Mixed gas and cumbersome SiO 2 And (5) a coating process.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to prepare hexagonal phase rare earth oxygen carbonate RE by adopting a novel method 2 O 2 CO 3 。
In order to achieve the above object, the technical scheme of the present invention is as follows:
in one aspect, the invention provides a method for preparing rare earth oxycarbonate, comprising the steps of:
1) Taking rare earth carbonate as a precursor, and uniformly mixing the precursor with a cosolvent;
2) Calcining the mixture in air to obtain the rare earth oxygen carbonate.
In the step 1), the precursor can be made by self or can be a commercial material purchased directly; the single rare earth carbonate is used as a precursor to prepare the single rare earth carbonate, or the rare earth carbonate containing the activator is used as the precursor to prepare the rare earth carbonate doped with the activator.
In the above technical scheme, further, the carbonate is RE 2 CO 3 、RE 2 (OH) 2 CO 3 One or a mixture of two of the above, wherein RE is rare earth metal.
In the above technical scheme, the fluxing agent is one or more of potassium nitrate, sodium nitrate and lithium nitrate.
In the above technical scheme, further, the addition mass of the cosolvent is 0.5-50 times of the mass of the precursor.
In the technical scheme, the calcination temperature is 250-650 ℃ and the calcination time is 0.5-12 h.
The invention also provides rare earth oxygen carbonate prepared by the preparation method, and the rare earth oxygen carbonate is pure hexagonal phase.
In still another aspect, the present invention provides an application of the rare earth oxygen carbonate in preparing a luminescent material, and the luminescent material is prepared by using the rare earth oxygen carbonate as a matrix.
The beneficial effects of the invention are as follows:
the method has the advantages of simple synthesis process, low cost, no need of ventilation and cladding processes, short reaction time and low reaction temperature, can greatly reduce the energy consumption, and is suitable for large-scale production.
The method of the invention can prepare pure hexagonal phase RE 2 O 2 CO 3 。
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of the sample prepared in example 1;
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of the sample prepared in example 1 by calcining at 450℃for 2 hours;
FIG. 3 is an emission spectrum of the sample prepared in example 1 under 254nm ultraviolet excitation;
FIG. 4 is an emission spectrum of the sample prepared in example 2 under 254nm ultraviolet excitation.
Detailed Description
The following examples of the present invention are given as illustration, but the present invention is not limited to these examples.
Example 1
Gd 2 O 2 CO 3 Eu is prepared by the following steps:
(1) Gd (NO) was disposed at a concentration of 0.1mol/L 3 ) 3 And Eu (NO) 3 ) 3 The solutions were then separately weighed Gd (NO 3 ) 3 And Eu (NO) 3 ) 3 153.6ml and 6.4ml of solution are mixed with proper amount of purified water to prepare 800ml of aqueous solution, 96g of urea is weighed and dissolved in 320ml of purified water, and the rare earth nitrate solution and the urea are mixedMixing the raw materials, adding a proper amount of purified water to prepare a mixed solution with the total volume of 1.6L, heating the mixed solution to 82 ℃, continuously preserving heat and curing for 90min after turbidity of the mixed solution is observed, carrying out centrifugal separation (3000 rmp multiplied by 3 min) on the precipitate after heat preservation is finished, respectively washing 3 times by purified water and 1 time by ethanol, and drying the washed precipitate at 60 ℃ for 10h to obtain dry basic carbonate precursor powder;
(2) 1g of precursor, 12g of potassium nitrate and 10g of sodium nitrate are weighed and uniformly mixed in an agate mortar;
(3) Calcining the mixture in muffle furnace at 300 deg.C, 400 deg.C and 450 deg.C for 2 hr, washing the product with purified water, washing with ethanol for three times, and drying in 60 deg.C vacuum drying oven to obtain Gd 2 O 2 CO 3 :4％Eu。
FIG. 1 is an XRD pattern of the samples prepared in example 1, in which XRD diffraction peaks of all the samples are well matched with PDF38-0680 quasi-cards, showing that the samples prepared by calcining at 300 ℃, 400 ℃ and 450 ℃ for 2 hours are all pure hexagonal phase Gd 2 O 2 CO 3 。
FIG. 2 is an SEM photograph of a sample obtained by calcining at 450℃for 2 hours in example 1, and it can be seen from the figure that the sample has a regular morphology and is in the form of spheroidal particles having an average particle diameter of about 1.5. Mu.m.
FIG. 3 shows the emission spectra of the samples prepared in example 1 under 254nm ultraviolet excitation, and it can be seen that all the samples mainly exhibit red light emission at 600-636 nm, and the luminous intensity increases with the increase of the calcination temperature.
In this embodiment, the rare earth element species have little effect on the final product, either a single rare earth or a combination of rare earth elements. Therefore, the method can prepare single rare earth oxygen carbonate or rare earth oxygen carbonate luminescent material containing activator.
Example 2
Gd 2 O 2 CO 3 Tb is prepared by the following steps:
(1) Gd (NO) was weighed separately 3 ) 3 And Tb (NO) 3 ) 3 Solution of Tb 3+ Mixing rare earth nitrate mixed solution with a proper amount of purified water to prepare 800ml of aqueous solution, dissolving 96g of urea in 320ml of purified water, mixing the rare earth nitrate solution with the urea solution, adding a proper amount of purified water to prepare a mixed solution with the total volume of 1.6L, heating the mixed solution to 82 ℃, continuing to keep the temperature for curing for 90min after turbidity of the mixed solution is observed, centrifugally separating sediment (3000 rmp multiplied by 3 min) after the heat preservation is finished, washing the sediment with purified water for 3 times and ethanol for 1 time respectively, and drying the washed sediment at 60 ℃ for 10h to obtain dry basic carbonate precursor powder;
(2) 1g of precursor, 13g of potassium nitrate and 13g of sodium nitrate are respectively weighed and uniformly mixed in an agate mortar;
(3) Calcining the mixture in a muffle furnace at 450 ℃ for 2 hours, washing the product with purified water for three times, washing with ethanol once after the calcining, and drying in a 60 DEG vacuum drying oven to obtain Gd 2 O 2 CO 3 :Tb。
FIG. 4 shows the emission spectrum of the samples prepared in example 2 under 254nm ultraviolet excitation, and shows that the emission peaks of all the samples are similar, and Tb is shown 3+ The strongest peak of which was at 539nm, shows green emission with higher color purity. With Tb 3+ The emission intensity of the sample is gradually increased by increasing the doping concentration of the sample.
The above examples are only preferred embodiments of the present invention and are not limiting of the implementation. The protection scope of the present invention shall be subject to the scope defined by the claims. Other variations or modifications may be made in the various forms based on the above description. Obvious variations or modifications of the embodiments are within the scope of the invention.
Claims (7)
1. A preparation method of rare earth carbonate oxide is characterized in that: the method comprises the following steps:
1) Taking rare earth carbonate as a precursor, and uniformly mixing the precursor with a cosolvent;
2) Calcining the mixture in air to obtain the rare earth oxygen carbonate.
2. The method for preparing rare earth oxycarbonate according to claim 1, wherein the carbonate is RE 2 CO 3 、RE 2 (OH) 2 CO 3 One or a mixture of two of the above, wherein RE is rare earth metal.
3. The method for preparing rare earth oxycarbonate according to claim 1 wherein the flux is one or more of potassium nitrate, sodium nitrate, and lithium nitrate.
4. The method for preparing rare earth carbonate according to claim 1, wherein the addition mass of the cosolvent is 0.5 to 50 times the mass of the precursor.
5. The method for preparing rare earth oxygen carbonate according to claim 1, wherein the calcination temperature is 250-650 ℃ and the calcination time is 0.5-12 h.
6. A rare earth oxycarbonate produced by the process of any one of claims 1 to 5 wherein the rare earth oxycarbonate is in a pure hexagonal phase.
7. Use of the rare earth oxycarbonate of claim 6 in the preparation of a luminescent material.
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